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#\#CIF_1.0 ################################################################################ # # # This CIF is a part of the B-IncStrDB # # (Bilbao Incommensurate Structures Database) # # http://www.cryst.ehu.eus/bincstrdb/ # # # # Please note that the structure of the CIF file may differ from the one # # deposited, as it may have been modified to comply with the standard. The # # file has been validated against official dictionaries as well as local # # dictionaries including non-standard data names used by SHELXL (Sheldrick, # # G. M. (2008). Acta Cryst. A 64, 112-122) and JANA (Petricek, V., Dusek, M. # # and Palatinus, L. (2014), Z. Kristallogr. 229, 345-352). # # # # For comments and/or criticisms, please e-mail to administrador-bcs@ehu.es # # # ################################################################################ data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 02/04/2022' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic 2022-11-08 _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted 2023-01-09 _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code BM5150SUP1 _journal_coeditor_notes ; ? ; _journal_techeditor_code B230021 _iucr_compatibility_tag ACTA95 _journal_paper_category FA _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section B' _journal_year 2023 _journal_volume 79 _journal_issue 2 _journal_page_first 148 _journal_page_last 156 _journal_paper_doi https://doi.org/10.1107/S2052520623000215 #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name 'Dey, Somnath' _publ_contact_author_address ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; _publ_contact_author_email somnathdey226@gmail.com _publ_contact_author_fax ? _publ_contact_author_phone ? #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Asymmetric rotations and dimerization driven by normal to modulated phase transition in 4-biphenylcarboxy coupled L-phenylalaninates ; loop_ _publ_author_name _publ_author_address 'Dey, Somnath' ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; 'Sasmal, Supriya' ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; 'Mondal, Saikat' ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; 'Kumar, Santosh' ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; 'Chowdhury, Rituparno' ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; 'Sarkar, Debashrita' ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; 'Reddy, C. Malla' ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; 'Peters, Lars' ;Institute of Crystallography RWTH Aachen University Jaegertrasse 17-19 52066 Aachen Germany ; 'Roth, Georg' ;Institute of Crystallography RWTH Aachen University Jaegertrasse 17-19 52066 Aachen Germany ; 'Haldar, Debasish' ;Department of Chemical Sciences Indian Institute of Science Education and Research Kolkata Mohanpur 741246 India ; #======================================================================= data_I_phaseII_modulated #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C23 H21 N1 O3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C23 H21 N1 O3' _chemical_formula_weight 359.4 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_ssg_name 'P21(\a0\g)0' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2+1/2,-x3,-x4 _cell_length_a 5.0377(2) _cell_length_b 8.5898(3) _cell_length_c 42.0432(14) _cell_angle_alpha 90 _cell_angle_beta 90.884(3) _cell_angle_gamma 90 _cell_volume 1819.11(11) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.9758(7) 1 0 0 0 1 0 0 0 1 2 0.0242(7) 1 0 0 0 -1 0 0 0 -1 _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.500000 0.000000 0.500000 _jana_cell_commen_supercell_matrix_1_1 2 _jana_cell_commen_supercell_matrix_1_2 0 _jana_cell_commen_supercell_matrix_1_3 0 _jana_cell_commen_supercell_matrix_2_1 0 _jana_cell_commen_supercell_matrix_2_2 1 _jana_cell_commen_supercell_matrix_2_3 0 _jana_cell_commen_supercell_matrix_3_1 0 _jana_cell_commen_supercell_matrix_3_2 0 _jana_cell_commen_supercell_matrix_3_3 2 _jana_cell_commen_t_section_1 0.25 _cell_formula_units_Z 4 _cell_measurement_reflns_used 3948 _cell_measurement_theta_min 4.19 _cell_measurement_theta_max 65.68 _cell_measurement_temperature 99.97(16) _cell_special_details ? _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 1.3124 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.696 _exptl_crystal_description 'rectangular' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_colour colorless _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 99.97 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Cu K\a' #_diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 7.9580 _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 13838 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 65.79 _diffrn_reflns_theta_full 65.45 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_unetI/netI 0.0414 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ? _reflns_number_total 8898 _reflns_number_gt 5940 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_gt 0.0483 _refine_ls_R_factor_all 0.0642 _refine_ls_wR_factor_ref 0.0526 _refine_ls_goodness_of_fit_ref 1.40 _refine_ls_goodness_of_fit_gt 1.60 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 8898 _refine_ls_number_parameters 662 _refine_ls_number_restraints 0 _refine_ls_number_constraints 403 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'mixed' _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 0.28 _refine_diff_density_min -0.26 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 2000(200) _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ; 2293 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0492 0.0322 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_cell_refinement 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group O1a O 0.3281(4) 0.0586(3) 0.45604(4) Uani 0.0324(6) 2 1 d . . . O1b O 0.8601(3) 0.5767(3) 0.04224(4) Uani 0.0245(5) 2 1 d . . . O2a O 0.1716(5) 0.2539(3) 0.48497(5) Uani 0.0528(8) 2 1 d . . . O2b O 0.6592(4) 0.3891(3) 0.01379(4) Uani 0.0357(6) 2 1 d . . . O3a O 0.8641(3) 0.2662(3) 0.39922(4) Uani 0.0268(5) 2 1 d . . . O3b O 0.5649(3) 0.4034(3) 0.09454(4) Uani 0.0242(5) 2 1 d . . . N1a N 0.4221(4) 0.253675 0.40734(4) Uani 0.0202(6) 2 1 d . . . N1b N 1.0017(4) 0.3687(3) 0.08786(4) Uani 0.0174(5) 2 1 d . . . C1a C 0.2019(6) -0.0493(4) 0.47735(6) Uani 0.0344(9) 2 1 d . . . C1b C 0.7017(5) 0.6894(4) 0.02465(6) Uani 0.0290(8) 2 1 d . . . C2a C 0.2943(5) 0.2079(4) 0.46273(5) Uani 0.0246(7) 2 1 d . . . C2b C 0.8090(4) 0.4294(4) 0.03488(5) Uani 0.0214(7) 2 1 d . . . C3a C 0.4348(5) 0.3147(4) 0.43962(5) Uani 0.0215(7) 2 1 d . . . C3b C 0.9674(5) 0.3156(4) 0.05526(5) Uani 0.0193(6) 2 1 d . . . C4a C 0.3236(5) 0.4818(4) 0.44133(5) Uani 0.0229(7) 2 1 d . . . C4b C 0.8374(5) 0.1516(3) 0.05272(5) Uani 0.0220(7) 2 1 d . . . C5a C 0.4652(5) 0.5942(4) 0.41993(5) Uani 0.0232(7) 2 1 d . . . C5b C 0.9455(5) 0.0347(3) 0.07633(5) Uani 0.0223(7) 2 1 d . . . C6a C 0.3934(5) 0.6056(4) 0.38805(6) Uani 0.0271(7) 2 1 d . . . C6b C 0.8291(5) 0.0212(4) 0.10608(5) Uani 0.0245(7) 2 1 d . . . C7a C 0.5263(5) 0.7059(4) 0.36807(6) Uani 0.0287(8) 2 1 d . . . C7b C 0.9184(5) -0.0881(4) 0.12781(6) Uani 0.0273(7) 2 1 d . . . C8a C 0.7338(5) 0.7984(4) 0.37965(6) Uani 0.0273(7) 2 1 d . . . C8b C 1.1270(5) -0.1852(4) 0.12056(6) Uani 0.0290(8) 2 1 d . . . C9a C 0.8041(5) 0.7890(4) 0.41150(6) Uani 0.0288(8) 2 1 d . . . C9b C 1.2478(5) -0.1728(4) 0.09106(6) Uani 0.0285(8) 2 1 d . . . C10a C 0.6718(5) 0.6877(4) 0.43153(6) Uani 0.0254(7) 2 1 d . . . C10b C 1.1568(5) -0.0635(4) 0.06929(5) Uani 0.0246(7) 2 1 d . . . C11a C 0.6357(4) 0.2417(4) 0.38927(5) Uani 0.0193(7) 2 1 d . . . C11b C 0.7942(4) 0.4048(4) 0.10536(5) Uani 0.0177(6) 2 1 d . . . C12a C 0.5851(4) 0.1990(4) 0.35516(5) Uani 0.0193(6) 2 1 d . . . C12b C 0.8486(4) 0.4459(4) 0.13957(5) Uani 0.0182(6) 2 1 d . . . C13a C 0.7508(5) 0.2571(4) 0.33255(5) Uani 0.0250(7) 2 1 d . . . C13b C 0.6799(5) 0.5475(4) 0.15426(6) Uani 0.0369(9) 2 1 d . . . C14a C 0.7120(5) 0.2217(4) 0.30072(6) Uani 0.0267(8) 2 1 d . . . C14b C 0.7182(5) 0.5891(4) 0.18587(6) Uani 0.0371(9) 2 1 d . . . C15a C 0.5115(4) 0.1245(4) 0.29032(5) Uani 0.0203(6) 2 1 d . . . C15b C 0.9251(4) 0.5269(3) 0.20397(5) Uani 0.0185(6) 2 1 d . . . C16a C 0.3465(5) 0.0658(4) 0.31327(6) Uani 0.0256(8) 2 1 d . . . C16b C 1.0894(5) 0.4230(4) 0.18885(5) Uani 0.0334(8) 2 1 d . . . C17a C 0.3818(5) 0.1034(4) 0.34520(5) Uani 0.0233(7) 2 1 d . . . C17b C 1.0577(5) 0.3836(4) 0.15712(6) Uani 0.0310(8) 2 1 d . . . C18a C 0.4741(4) 0.0871(4) 0.25609(5) Uani 0.0193(6) 2 1 d . . . C18b C 0.9603(4) 0.5671(4) 0.23844(5) Uani 0.0202(7) 2 1 d . . . C19a C 0.6345(5) 0.1510(4) 0.23310(6) Uani 0.0286(8) 2 1 d . . . C19b C 0.7931(5) 0.6736(4) 0.25293(5) Uani 0.0304(8) 2 1 d . . . C20a C 0.6015(6) 0.1174(4) 0.20114(6) Uani 0.0314(8) 2 1 d . . . C20b C 0.8211(5) 0.7084(4) 0.28498(6) Uani 0.0311(8) 2 1 d . . . C21a C 0.4041(5) 0.0168(4) 0.19119(6) Uani 0.0270(7) 2 1 d . . . C21b C 1.0142(4) 0.6378(4) 0.30348(5) Uani 0.0232(7) 2 1 d . . . C22a C 0.2431(5) -0.0484(4) 0.21341(6) Uani 0.0311(8) 2 1 d . . . C22b C 1.1828(5) 0.5347(4) 0.28921(6) Uani 0.0293(8) 2 1 d . . . C23a C 0.2771(5) -0.0138(4) 0.24536(6) Uani 0.0272(8) 2 1 d . . . C23b C 1.1584(5) 0.4989(4) 0.25727(6) Uani 0.0262(7) 2 1 d . . . H1c3a H 0.618836 0.318816 0.445839 Uiso 0.0322 2 1 d . . . H1c3b H 1.144647 0.308885 0.047295 Uiso 0.029 2 1 d . . . H1c4a H 0.137775 0.480681 0.435915 Uiso 0.0343 2 1 d . . . H2c4a H 0.334422 0.518391 0.462889 Uiso 0.0343 2 1 d . . . H1c4b H 0.64889 0.160976 0.055154 Uiso 0.033 2 1 d . . . H2c4b H 0.857399 0.112158 0.031532 Uiso 0.033 2 1 d . . . H1c6a H 0.250178 0.543224 0.379746 Uiso 0.0325 2 1 d . . . H1c6b H 0.684882 0.088689 0.111512 Uiso 0.0294 2 1 d . . . H1c7a H 0.475132 0.711883 0.346022 Uiso 0.0345 2 1 d . . . H1c7b H 0.834829 -0.096535 0.148107 Uiso 0.0328 2 1 d . . . H1c8a H 0.826414 0.867424 0.365715 Uiso 0.0327 2 1 d . . . H1c8b H 1.188658 -0.260863 0.13576 Uiso 0.0347 2 1 d . . . H1c9a H 0.945149 0.853008 0.419823 Uiso 0.0346 2 1 d . . . H1c9b H 1.393387 -0.239779 0.08587 Uiso 0.0342 2 1 d . . . H1c10a H 0.722958 0.681826 0.453577 Uiso 0.0305 2 1 d . . . H1c10b H 1.240567 -0.055308 0.049001 Uiso 0.0295 2 1 d . . . H1n1a H 0.253(5) 0.254(3) 0.3989(6) Uiso 0.0243 2 1 d . . . H1n1b H 1.172(5) 0.381(3) 0.0954(5) Uiso 0.0208 2 1 d . . . H1c13a H 0.893824 0.322492 0.339022 Uiso 0.03 2 1 d . . . H1c13b H 0.532889 0.590411 0.14245 Uiso 0.0443 2 1 d . . . H1c14a H 0.826301 0.26514 0.285403 Uiso 0.032 2 1 d . . . H1c14b H 0.599656 0.662307 0.195409 Uiso 0.0446 2 1 d . . . H1c16a H 0.206194 -0.001581 0.306925 Uiso 0.0307 2 1 d . . . H1c16b H 1.231637 0.376016 0.200867 Uiso 0.0401 2 1 d . . . H1c17a H 0.263687 0.062576 0.360572 Uiso 0.028 2 1 d . . . H1c17b H 1.180054 0.313485 0.147303 Uiso 0.0371 2 1 d . . . H1c19a H 0.772211 0.220388 0.239673 Uiso 0.0343 2 1 d . . . H1c19b H 0.656647 0.723683 0.240543 Uiso 0.0365 2 1 d . . . H1c20a H 0.714746 0.16355 0.185851 Uiso 0.0376 2 1 d . . . H1c20b H 0.704435 0.7827 0.294451 Uiso 0.0373 2 1 d . . . H1c22a H 0.106273 -0.118415 0.206696 Uiso 0.0374 2 1 d . . . H1c22b H 1.320725 0.486353 0.301714 Uiso 0.0352 2 1 d . . . H1c23a H 0.162843 -0.059866 0.26048 Uiso 0.0326 2 1 d . . . H1c23b H 1.279065 0.426399 0.247926 Uiso 0.0314 2 1 d . . . H1c21a H 0.380038 -0.007098 0.169026 Uiso 0.0324 2 1 d . . . H1c21b H 1.030215 0.660313 0.325786 Uiso 0.0279 2 1 d . . . H1c1a H 0.237302 -0.153941 0.470628 Uiso 0.0516 2 1 d . . . H2c1a H 0.270779 -0.034204 0.498543 Uiso 0.0516 2 1 d . . . H3c1a H 0.013797 -0.031416 0.477042 Uiso 0.0516 2 1 d . . . H1c1b H 0.75009 0.792587 0.031285 Uiso 0.0436 2 1 d . . . H2c1b H 0.733216 0.677993 0.002307 Uiso 0.0436 2 1 d . . . H3c1b H 0.517047 0.672102 0.028702 Uiso 0.0436 2 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1a O 0.0429(11) 0.0232(9) 0.0314(9) 0.0014(8) 0.0128(8) 0.0012(7) O1b O 0.0298(9) 0.0186(8) 0.0249(8) -0.0019(7) -0.0074(6) 0.0017(7) O2a O 0.0936(17) 0.0291(11) 0.0369(11) 0.0007(12) 0.0360(11) -0.0019(9) O2b O 0.0507(11) 0.0247(9) 0.0309(9) -0.0020(9) -0.0218(8) -0.0008(8) O3a O 0.0145(8) 0.0396(10) 0.0265(9) -0.0001(8) -0.0001(6) -0.0032(8) O3b O 0.0147(8) 0.0325(9) 0.0252(8) -0.0002(7) -0.0029(6) -0.0009(8) N1a N 0.0163(10) 0.0250(10) 0.0193(9) 0.0005(8) -0.0008(7) -0.0013(8) N1b N 0.0137(9) 0.0189(9) 0.0193(9) -0.0022(8) -0.0018(7) 0.0001(7) C1a C 0.0492(17) 0.0277(14) 0.0265(13) -0.0096(13) 0.0037(11) 0.0022(11) C1b C 0.0399(15) 0.0202(12) 0.0269(12) 0.0048(12) -0.0037(10) 0.0032(10) C2a C 0.0254(13) 0.0282(13) 0.0202(11) -0.0010(11) 0.0001(9) -0.0050(10) C2b C 0.0229(12) 0.0230(12) 0.0184(11) -0.0007(10) 0.0019(9) 0.0003(9) C3a C 0.0217(12) 0.0235(12) 0.0192(11) 0.0012(10) -0.0020(9) -0.0028(9) C3b C 0.0193(12) 0.0210(11) 0.0177(11) -0.0004(10) -0.0013(8) -0.0008(9) C4a C 0.0210(12) 0.0249(12) 0.0228(12) 0.0033(10) 0.0020(9) -0.0042(10) C4b C 0.0248(13) 0.0161(11) 0.0249(12) -0.0011(10) -0.0056(9) -0.0016(9) C5a C 0.0253(13) 0.0184(12) 0.0261(12) 0.0040(10) 0.0043(9) -0.0010(9) C5b C 0.0248(13) 0.0151(11) 0.0270(12) -0.0039(10) -0.0048(9) -0.0040(9) C6a C 0.0227(13) 0.0277(13) 0.0308(13) 0.0028(11) -0.0041(9) -0.0032(11) C6b C 0.0243(13) 0.0182(11) 0.0310(13) 0.0012(10) -0.0021(9) -0.0027(10) C7a C 0.0297(13) 0.0321(14) 0.0245(12) 0.0009(12) 0.0002(10) 0.0034(11) C7b C 0.0331(13) 0.0229(12) 0.0259(12) 0.0006(11) -0.0010(10) -0.0001(10) C8a C 0.0309(14) 0.0206(12) 0.0304(13) 0.0022(11) 0.0032(10) 0.0034(10) C8b C 0.0313(14) 0.0213(12) 0.0340(14) 0.0003(11) -0.0081(10) 0.0030(11) C9a C 0.0294(14) 0.0249(13) 0.0321(13) -0.0023(11) -0.0020(10) -0.0046(11) C9b C 0.0265(13) 0.0217(12) 0.0372(14) 0.0038(10) -0.0026(10) -0.0031(10) C10a C 0.0271(13) 0.0245(12) 0.0244(12) 0.0006(11) -0.0022(9) -0.0024(10) C10b C 0.0255(12) 0.0217(12) 0.0264(12) -0.0030(11) -0.0001(9) -0.0051(10) C11a C 0.0121(11) 0.0200(12) 0.0259(11) -0.0001(9) 0.0008(8) 0.0012(9) C11b C 0.0116(11) 0.0157(11) 0.0258(11) 0.0002(9) -0.0005(8) 0.0030(9) C12a C 0.0165(11) 0.0194(11) 0.0221(11) 0.0013(10) 0.0005(8) 0.0000(9) C12b C 0.0168(11) 0.0174(11) 0.0204(11) -0.0020(9) 0.0040(8) 0.0018(9) C13a C 0.0166(12) 0.0324(14) 0.0260(12) -0.0046(11) -0.0011(9) -0.0031(11) C13b C 0.0315(15) 0.0518(18) 0.0272(13) 0.0237(14) -0.0088(10) -0.0068(13) C14a C 0.0248(13) 0.0309(14) 0.0245(12) -0.0032(12) 0.0057(10) 0.0018(11) C14b C 0.0381(15) 0.0444(16) 0.0287(13) 0.0247(14) -0.0076(11) -0.0112(12) C15a C 0.0195(11) 0.0169(11) 0.0244(11) 0.0031(10) 0.0002(8) 0.0005(9) C15b C 0.0166(11) 0.0162(11) 0.0227(11) -0.0004(9) 0.0009(8) 0.0006(9) C16a C 0.0244(13) 0.0254(13) 0.0268(13) -0.0040(11) 0.0001(10) -0.0021(11) C16b C 0.0297(14) 0.0460(16) 0.0243(12) 0.0194(13) -0.0057(10) -0.0048(12) C17a C 0.0180(12) 0.0249(13) 0.0272(12) -0.0028(11) 0.0063(9) -0.0005(10) C17b C 0.0239(13) 0.0430(16) 0.0258(12) 0.0144(12) -0.0041(9) -0.0079(11) C18a C 0.0164(11) 0.0168(11) 0.0247(11) 0.0038(9) -0.0014(8) -0.0023(9) C18b C 0.0212(12) 0.0179(11) 0.0217(11) -0.0053(10) 0.0042(8) -0.0004(9) C19a C 0.0279(14) 0.0289(14) 0.0290(13) -0.0055(12) 0.0015(10) -0.0032(11) C19b C 0.0287(14) 0.0391(16) 0.0233(12) 0.0120(12) -0.0030(10) -0.0001(11) C20a C 0.0376(15) 0.0338(15) 0.0227(12) -0.0031(13) 0.0025(11) -0.0038(11) C20b C 0.0298(14) 0.0365(15) 0.0271(12) 0.0071(12) 0.0044(10) -0.0069(11) C21a C 0.0321(14) 0.0258(13) 0.0228(12) 0.0068(11) -0.0048(9) -0.0063(10) C21b C 0.0211(12) 0.0266(12) 0.0220(12) -0.0074(10) 0.0003(9) -0.0018(10) C22a C 0.0315(15) 0.0300(15) 0.0318(14) -0.0040(12) -0.0048(11) -0.0057(12) C22b C 0.0290(14) 0.0314(14) 0.0273(13) 0.0038(12) -0.0078(10) -0.0003(11) C23a C 0.0245(13) 0.0297(14) 0.0273(13) -0.0045(12) 0.0007(10) -0.0015(11) C23b C 0.0266(13) 0.0259(13) 0.0260(12) 0.0056(11) -0.0008(9) -0.0039(10) loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id O1ax1 O1a x 1 O1ay1 O1a y 1 O1az1 O1a z 1 O1bx1 O1b x 1 O1by1 O1b y 1 O1bz1 O1b z 1 O2ax1 O2a x 1 O2ay1 O2a y 1 O2az1 O2a z 1 O2bx1 O2b x 1 O2by1 O2b y 1 O2bz1 O2b z 1 O3ax1 O3a x 1 O3ay1 O3a y 1 O3az1 O3a z 1 O3bx1 O3b x 1 O3by1 O3b y 1 O3bz1 O3b z 1 N1ax1 N1a x 1 N1ay1 N1a y 1 N1az1 N1a z 1 N1bx1 N1b x 1 N1by1 N1b y 1 N1bz1 N1b z 1 C1ax1 C1a x 1 C1ay1 C1a y 1 C1az1 C1a z 1 C1bx1 C1b x 1 C1by1 C1b y 1 C1bz1 C1b z 1 C2ax1 C2a x 1 C2ay1 C2a y 1 C2az1 C2a z 1 C2bx1 C2b x 1 C2by1 C2b y 1 C2bz1 C2b z 1 C3ax1 C3a x 1 C3ay1 C3a y 1 C3az1 C3a z 1 C3bx1 C3b x 1 C3by1 C3b y 1 C3bz1 C3b z 1 C4ax1 C4a x 1 C4ay1 C4a y 1 C4az1 C4a z 1 C4bx1 C4b x 1 C4by1 C4b y 1 C4bz1 C4b z 1 C5ax1 C5a x 1 C5ay1 C5a y 1 C5az1 C5a z 1 C5bx1 C5b x 1 C5by1 C5b y 1 C5bz1 C5b z 1 C6ax1 C6a x 1 C6ay1 C6a y 1 C6az1 C6a z 1 C6bx1 C6b x 1 C6by1 C6b y 1 C6bz1 C6b z 1 C7ax1 C7a x 1 C7ay1 C7a y 1 C7az1 C7a z 1 C7bx1 C7b x 1 C7by1 C7b y 1 C7bz1 C7b z 1 C8ax1 C8a x 1 C8ay1 C8a y 1 C8az1 C8a z 1 C8bx1 C8b x 1 C8by1 C8b y 1 C8bz1 C8b z 1 C9ax1 C9a x 1 C9ay1 C9a y 1 C9az1 C9a z 1 C9bx1 C9b x 1 C9by1 C9b y 1 C9bz1 C9b z 1 C10ax1 C10a x 1 C10ay1 C10a y 1 C10az1 C10a z 1 C10bx1 C10b x 1 C10by1 C10b y 1 C10bz1 C10b z 1 C11ax1 C11a x 1 C11ay1 C11a y 1 C11az1 C11a z 1 C11bx1 C11b x 1 C11by1 C11b y 1 C11bz1 C11b z 1 C12ax1 C12a x 1 C12ay1 C12a y 1 C12az1 C12a z 1 C12bx1 C12b x 1 C12by1 C12b y 1 C12bz1 C12b z 1 C13ax1 C13a x 1 C13ay1 C13a y 1 C13az1 C13a z 1 C13bx1 C13b x 1 C13by1 C13b y 1 C13bz1 C13b z 1 C14ax1 C14a x 1 C14ay1 C14a y 1 C14az1 C14a z 1 C14bx1 C14b x 1 C14by1 C14b y 1 C14bz1 C14b z 1 C15ax1 C15a x 1 C15ay1 C15a y 1 C15az1 C15a z 1 C15bx1 C15b x 1 C15by1 C15b y 1 C15bz1 C15b z 1 C16ax1 C16a x 1 C16ay1 C16a y 1 C16az1 C16a z 1 C16bx1 C16b x 1 C16by1 C16b y 1 C16bz1 C16b z 1 C17ax1 C17a x 1 C17ay1 C17a y 1 C17az1 C17a z 1 C17bx1 C17b x 1 C17by1 C17b y 1 C17bz1 C17b z 1 C18ax1 C18a x 1 C18ay1 C18a y 1 C18az1 C18a z 1 C18bx1 C18b x 1 C18by1 C18b y 1 C18bz1 C18b z 1 C19ax1 C19a x 1 C19ay1 C19a y 1 C19az1 C19a z 1 C19bx1 C19b x 1 C19by1 C19b y 1 C19bz1 C19b z 1 C20ax1 C20a x 1 C20ay1 C20a y 1 C20az1 C20a z 1 C20bx1 C20b x 1 C20by1 C20b y 1 C20bz1 C20b z 1 C21ax1 C21a x 1 C21ay1 C21a y 1 C21az1 C21a z 1 C21bx1 C21b x 1 C21by1 C21b y 1 C21bz1 C21b z 1 C22ax1 C22a x 1 C22ay1 C22a y 1 C22az1 C22a z 1 C22bx1 C22b x 1 C22by1 C22b y 1 C22bz1 C22b z 1 C23ax1 C23a x 1 C23ay1 C23a y 1 C23az1 C23a z 1 C23bx1 C23b x 1 C23by1 C23b y 1 C23bz1 C23b z 1 H1c3ax1 H1c3a x 1 H1c3ay1 H1c3a y 1 H1c3az1 H1c3a z 1 H1c3bx1 H1c3b x 1 H1c3by1 H1c3b y 1 H1c3bz1 H1c3b z 1 H1c4ax1 H1c4a x 1 H1c4ay1 H1c4a y 1 H1c4az1 H1c4a z 1 H2c4ax1 H2c4a x 1 H2c4ay1 H2c4a y 1 H2c4az1 H2c4a z 1 H1c4bx1 H1c4b x 1 H1c4by1 H1c4b y 1 H1c4bz1 H1c4b z 1 H2c4bx1 H2c4b x 1 H2c4by1 H2c4b y 1 H2c4bz1 H2c4b z 1 H2c6ax1 H1c6a x 1 H1c6ay1 H1c6a y 1 H1c6az1 H1c6a z 1 H1c6bx1 H1c6b x 1 H1c6by1 H1c6b y 1 H1c6bz1 H1c6b z 1 H1c7ax1 H1c7a x 1 H1c7ay1 H1c7a y 1 H1c7az1 H1c7a z 1 H1c7bx1 H1c7b x 1 H1c7by1 H1c7b y 1 H1c7bz1 H1c7b z 1 H1c8ax1 H1c8a x 1 H1c8ay1 H1c8a y 1 H1c8az1 H1c8a z 1 H1c8bx1 H1c8b x 1 H1c8by1 H1c8b y 1 H1c8bz1 H1c8b z 1 H1c9ax1 H1c9a x 1 H1c9ay1 H1c9a y 1 H1c9az1 H1c9a z 1 H1c9bx1 H1c9b x 1 H1c9by1 H1c9b y 1 H1c9bz1 H1c9b z 1 H1c10ax1 H1c10a x 1 H1c10ay1 H1c10a y 1 H1c10az1 H1c10a z 1 H1c10bx1 H1c10b x 1 H1c10by1 H1c10b y 1 H1c10bz1 H1c10b z 1 H1n1ax1 H1n1a x 1 H1n1ay1 H1n1a y 1 H1n1az1 H1n1a z 1 H1n1bx1 H1n1b x 1 H1n1by1 H1n1b y 1 H1n1bz1 H1n1b z 1 H1c13ax1 H1c13a x 1 H1c13ay1 H1c13a y 1 H1c13az1 H1c13a z 1 H1c13bx1 H1c13b x 1 H1c13by1 H1c13b y 1 H1c13bz1 H1c13b z 1 H1c14ax1 H1c14a x 1 H1c14ay1 H1c14a y 1 H1c14az1 H1c14a z 1 H1c14bx1 H1c14b x 1 H1c14by1 H1c14b y 1 H1c14bz1 H1c14b z 1 H1c16ax1 H1c16a x 1 H1c16ay1 H1c16a y 1 H1c16az1 H1c16a z 1 H1c16bx1 H1c16b x 1 H1c16by1 H1c16b y 1 H1c16bz1 H1c16b z 1 H1c17ax1 H1c17a x 1 H1c17ay1 H1c17a y 1 H1c17az1 H1c17a z 1 H1c17bx1 H1c17b x 1 H1c17by1 H1c17b y 1 H1c17bz1 H1c17b z 1 H1c19ax1 H1c19a x 1 H1c19ay1 H1c19a y 1 H1c19az1 H1c19a z 1 H1c19bx1 H1c19b x 1 H1c19by1 H1c19b y 1 H1c19bz1 H1c19b z 1 H1c20ax1 H1c20a x 1 H1c20ay1 H1c20a y 1 H1c20az1 H1c20a z 1 H1c20bx1 H1c20b x 1 H1c20by1 H1c20b y 1 H1c20bz1 H1c20b z 1 H1c22ax1 H1c22a x 1 H1c22ay1 H1c22a y 1 H1c22az1 H1c22a z 1 H1c22bx1 H1c22b x 1 H1c22by1 H1c22b y 1 H1c22bz1 H1c22b z 1 H1c23ax1 H1c23a x 1 H1c23ay1 H1c23a y 1 H1c23az1 H1c23a z 1 H1c23bx1 H1c23b x 1 H1c23by1 H1c23b y 1 H1c23bz1 H1c23b z 1 H1c21ax1 H1c21a x 1 H1c21ay1 H1c21a y 1 H1c21az1 H1c21a z 1 H1c21bx1 H1c21b x 1 H1c21by1 H1c21b y 1 H1c21bz1 H1c21b z 1 H1c1ax1 H1c1a x 1 H1c1ay1 H1c1a y 1 H1c1az1 H1c1a z 1 H2c1ax1 H2c1a x 1 H2c1ay1 H2c1a y 1 H2c1az1 H2c1a z 1 H3c1ax1 H3c1a x 1 H3c1ay1 H3c1a y 1 H3c1az1 H3c1a z 1 H1c1bx1 H1c1b x 1 H1c1by1 H1c1b y 1 H1c1bz1 H1c1b z 1 H2c1bx1 H2c1b x 1 H2c1by1 H2c1b y 1 H2c1bz1 H2c1b z 1 H3c1bx1 H3c1b x 1 H3c1by1 H3c1b y 1 H3c1bz1 H3c1b z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin O1ax1 0 0.0014(5) O1ay1 0 0.0078(3) O1az1 0 -0.00070(6) O1bx1 0 -0.0010(4) O1by1 0 -0.0014(2) O1bz1 0 0.00017(4) O2ax1 0.0036(6) 0 O2ay1 0.0084(3) 0 O2az1 -0.00074(6) 0 O2bx1 0 -0.0086(8) O2by1 0 -0.0033(4) O2bz1 0 0.00115(10) O3ax1 -0.0011(5) 0 O3ay1 0.0109(3) 0 O3az1 0.00070(6) 0 O3bx1 0.0009(4) 0 O3by1 -0.0029(2) 0 O3bz1 0.00082(5) 0 N1ax1 0 -0.0006(5) N1ay1 0 0.0071(3) N1az1 0 -0.00095(6) N1bx1 -0.0049(15) 0 N1by1 0.0021(8) 0 N1bz1 -0.00092(18) 0 C1ax1 0 0.0003(12) C1ay1 0 0.0116(6) C1az1 0 -0.00081(13) C1bx1 0 -0.0017(9) C1by1 0 -0.0023(5) C1bz1 0 0.00022(10) C2ax1 0 0.0031(7) C2ay1 0 0.0086(4) C2az1 0 -0.00076(9) C2bx1 0 -0.0033(6) C2by1 0 -0.0015(3) C2bz1 0 0.00047(7) C3ax1 0 0.0024(6) C3ay1 0 0.0058(3) C3az1 0 -0.00080(7) C3bx1 0 -0.0016(5) C3by1 0 -0.0009(3) C3bz1 0 0.00032(6) C4ax1 0 0.0081(7) C4ay1 0 0.0085(4) C4az1 0 -0.00081(9) C4bx1 0 -0.0009(5) C4by1 0 -0.0013(3) C4bz1 0 0.00041(7) C5ax1 0 0.0069(5) C5ay1 0 0.0071(3) C5az1 0 -0.00063(7) C5bx1 0 -0.0014(5) C5by1 0 -0.0009(3) C5bz1 0 0.00058(6) C6ax1 0 0.0048(7) C6ay1 0 0.0102(4) C6az1 0 -0.00069(9) C6bx1 0 -0.0002(5) C6by1 0 -0.0001(3) C6bz1 0 0.00074(7) C7ax1 0 -0.0009(5) C7ay1 0 0.0110(3) C7az1 0 -0.00052(7) C7bx1 0 -0.0013(6) C7by1 0 0.0000(3) C7bz1 0 0.00068(7) C8ax1 0 -0.0008(6) C8ay1 0 0.0109(3) C8az1 0 -0.00041(7) C8bx1 0 -0.0039(8) C8by1 0 -0.0013(4) C8bz1 0 0.00090(10) C9ax1 0 0.0043(7) C9ay1 0 0.0106(4) C9az1 0 -0.00078(9) C9bx1 0 -0.0077(11) C9by1 0 -0.0042(6) C9bz1 0 0.00134(15) C10ax1 0 0.0067(5) C10ay1 0 0.0060(3) C10az1 0 -0.00078(7) C10bx1 0 -0.0027(7) C10by1 0 -0.0023(4) C10bz1 0 0.00085(9) C11ax1 0 -0.0005(5) C11ay1 0 -0.0015(3) C11az1 0 -0.00067(6) C11bx1 0 0.0007(5) C11by1 0 -0.0018(3) C11bz1 0 0.00045(7) C12ax1 0 -0.0034(5) C12ay1 0 -0.0016(3) C12az1 0 -0.00061(6) C12bx1 0 0.0028(5) C12by1 0 -0.0014(3) C12bz1 0 0.00050(6) C13ax1 0 0.0215(5) C13ay1 0 -0.0221(3) C13az1 0 -0.00007(7) C13bx1 0 -0.0034(7) C13by1 0 -0.0074(4) C13bz1 0 0.00103(8) C14ax1 0 0.0218(5) C14ay1 0 -0.0221(3) C14az1 0 0.00000(6) C14bx1 0 -0.0029(6) C14by1 0 -0.0068(4) C14bz1 0 0.00093(7) C15ax1 0 -0.0038(6) C15ay1 0 -0.0031(3) C15az1 0 -0.00066(8) C15bx1 0 0.0051(5) C15by1 0 -0.0021(3) C15bz1 0 0.00048(6) C16ax1 -0.0298(6) 0 C16ay1 0.0189(4) 0 C16az1 -0.00142(7) 0 C16bx1 0 0.0163(9) C16by1 0 0.0041(6) C16bz1 0 0.00031(11) C17ax1 -0.0329(7) 0 C17ay1 0.0208(4) 0 C17az1 -0.00150(8) 0 C17bx1 0 0.0107(7) C17by1 0 0.0033(5) C17bz1 0 0.00007(9) C18ax1 0 -0.0047(7) C18ay1 0 -0.0032(4) C18az1 0 -0.00111(9) C18bx1 0 0.0049(6) C18by1 0 -0.0012(4) C18bz1 0 0.00052(8) C19ax1 0 -0.0251(6) C19ay1 0 0.0159(4) C19az1 0 -0.00106(7) C19bx1 0 0.0127(6) C19by1 0 0.0053(4) C19bz1 0 -0.00010(7) C20ax1 0 -0.0287(7) C20ay1 0 0.0184(4) C20az1 0 -0.00119(8) C20bx1 0 0.0084(6) C20by1 0 0.0059(4) C20bz1 0 -0.00025(7) C21ax1 -0.0016(6) 0 C21ay1 -0.0007(3) 0 C21az1 -0.00079(7) 0 C21bx1 0 -0.0066(9) C21by1 0 -0.0030(5) C21bz1 0 0.00095(12) C22ax1 0.0193(6) 0 C22ay1 -0.0157(3) 0 C22az1 -0.00058(7) 0 C22bx1 0.0092(6) 0 C22by1 0.0066(3) 0 C22bz1 -0.00115(7) 0 C23ax1 0.0183(5) 0 C23ay1 -0.0183(3) 0 C23az1 -0.00038(7) 0 C23bx1 0.0069(6) 0 C23by1 0.0072(3) 0 C23bz1 -0.00099(7) 0 H1c3ax1 -0.0016 0.0024 H1c3ay1 -0.0021 0.0031 H1c3az1 0.0005 -0.0008 H1c3bx1 0.001 -0.0017 H1c3by1 0.0004 -0.0007 H1c3bz1 -0.0001 0.0002 H1c4ax1 0.0042 0.0062 H1c4ay1 0.0059 0.0086 H1c4az1 -0.0003 -0.0004 H2c4ax1 -0.0009 0.0092 H2c4ay1 -0.0008 0.0078 H2c4az1 0.0001 -0.0008 H1c4bx1 -0.0006 -0.0009 H1c4by1 -0.0008 -0.0013 H1c4bz1 0.0001 0.0002 H2c4bx1 0 0.0001 H2c4by1 0 -0.0017 H2c4bz1 0 0.0005 H2c6ax1 0.0029 0.0056 H1c6ay1 0.0041 0.008 H1c6az1 -0.0003 -0.0006 H1c6bx1 0.0005 0.001 H1c6by1 0.0003 0.0006 H1c6bz1 0.0003 0.0007 H1c7ax1 -0.0009 -0.0039 H1c7ay1 0.003 0.0126 H1c7az1 -0.0001 -0.0004 H1c7bx1 -0.0002 -0.0009 H1c7by1 0.0001 0.0006 H1c7bz1 0.0001 0.0007 H1c8ax1 0.0008 -0.0033 H1c8ay1 -0.0031 0.0123 H1c8az1 0.0001 -0.0003 H1c8bx1 0.0011 -0.0045 H1c8by1 0.0003 -0.0013 H1c8bz1 -0.0002 0.0009 H1c9ax1 -0.002 0.004 H1c9ay1 -0.0048 0.0094 H1c9az1 0.0004 -0.0007 H1c9bx1 0.0046 -0.0097 H1c9by1 0.0027 -0.0057 H1c9bz1 -0.0005 0.0012 H1c10ax1 -0.0023 0.0097 H1c10ay1 -0.0009 0.0039 H1c10az1 0.0002 -0.0009 H1c10bx1 0.0004 -0.0018 H1c10by1 0.0005 -0.0026 H1c10bz1 -0.0002 0.0009 H1n1ax1 0 -0.006(12) H1n1ay1 0 0.009(7) H1n1az1 0 -0.0009(15) H1n1bx1 -0.002(7) 0 H1n1by1 -0.001(4) 0 H1n1bz1 0.0002(9) 0 H1c13ax1 -0.0174 0.0344 H1c13ay1 0.0161 -0.0318 H1c13az1 -0.0001 0.0002 H1c13bx1 -0.0041 -0.0076 H1c13by1 -0.0054 -0.0099 H1c13bz1 0.0006 0.0012 H1c14ax1 -0.0125 0.0388 H1c14ay1 0.0111 -0.0346 H1c14az1 -0.0001 0.0004 H1c14bx1 -0.0026 -0.0072 H1c14by1 -0.0035 -0.0098 H1c14bz1 0.0004 0.0012 H1c16ax1 -0.0407 -0.0821 H1c16ay1 0.028 0.0564 H1c16az1 -0.0015 -0.0031 H1c16bx1 -0.0112 0.0212 H1c16by1 -0.0043 0.0082 H1c16bz1 0.0001 -0.0001 H1c17ax1 -0.0191 -0.0571 H1c17ay1 0.0131 0.0393 H1c17az1 -0.0007 -0.0022 H1c17bx1 -0.005 0.0135 H1c17by1 -0.0024 0.0064 H1c17bz1 0.0001 -0.0003 H1c19ax1 0.0184 -0.0377 H1c19ay1 -0.0122 0.025 H1c19az1 0.0005 -0.0011 H1c19bx1 0.0093 0.0184 H1c19by1 0.0044 0.0088 H1c19bz1 -0.0003 -0.0005 H1c20ax1 0.0143 -0.045 H1c20ay1 -0.0097 0.0305 H1c20az1 0.0004 -0.0014 H1c20bx1 0.0049 0.0139 H1c20by1 0.0037 0.0104 H1c20bz1 -0.0003 -0.0008 H1c22ax1 -0.1051 -0.2171 H1c22ay1 0.0794 0.1641 H1c22az1 0.0017 0.0035 H1c22bx1 0.0787 -0.154 H1c22by1 0.0515 -0.1007 H1c22bz1 -0.0081 0.0158 H1c23ax1 0.1492 0.4633 H1c23ay1 -0.1333 -0.4139 H1c23az1 -0.0008 -0.0024 H1c23bx1 0.0156 -0.0428 H1c23by1 0.0148 -0.0406 H1c23bz1 -0.0018 0.0049 H1c21ax1 -0.0001 -0.0008 H1c21ay1 -0.0003 -0.0023 H1c21az1 -0.0004 -0.0026 H1c21bx1 0.0018 -0.0148 H1c21by1 0.0006 -0.0052 H1c21bz1 -0.0001 0.0011 H1c1ax1 0.0001 -0.0014 H1c1ay1 -0.001 0.0113 H1c1az1 0.0001 -0.0008 H2c1ax1 -0.0003 0.001 H2c1ay1 -0.0032 0.011 H2c1az1 0.0002 -0.0008 H3c1ax1 0.0003 0.0004 H3c1ay1 0.007 0.0104 H3c1az1 -0.0004 -0.0006 H1c1bx1 -0.0001 0.0003 H1c1by1 0.0004 -0.0021 H1c1bz1 0 -0.0001 H2c1bx1 0.0001 -0.004 H2c1by1 0.0001 -0.0036 H2c1bz1 0 0.0002 H3c1bx1 -0.0008 -0.0012 H3c1by1 -0.0006 -0.001 H3c1bz1 0.0003 0.0004 #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag O1a C1a . . 1.443(4) 1.438(4) 1.448(4) ? O1a C2a . . 1.324(5) 1.324(5) 1.324(5) ? O1b C1b . . 1.450(5) 1.450(5) 1.450(5) ? O1b C2b . . 1.327(5) 1.326(5) 1.327(5) ? O2a C2a . . 1.196(5) 1.193(5) 1.199(5) ? O2b C2b . . 1.206(4) 1.205(4) 1.206(4) ? O3a C11a . . 1.238(6) 1.236(6) 1.239(6) ? O3b C11b . . 1.235(6) 1.230(6) 1.240(6) ? N1a C3a . . 1.455(4) 1.454(4) 1.457(4) ? N1a C11a . . 1.332(6) 1.331(6) 1.334(6) ? N1a H1n1a . . 0.92(3) 0.91(3) 0.92(3) ? N1b C3b . . 1.453(4) 1.453(4) 1.453(4) ? N1b C11b . . 1.324(5) 1.320(5) 1.329(5) ? N1b H1n1b . . 0.92(3) 0.91(3) 0.92(3) ? C1a H1c1a . . 1.0(5) 1.0(6) 1.0(6) ? C1a H2c1a . . 1(2) 1(2) 1(2) ? C1a H3c1a . . 0.960(6) 0.960(6) 0.960(6) ? C1b H1c1b . . 1.0(9) 1.0(9) 1.0(9) ? C1b H2c1b . . 1.0(19) 1.0(19) 1.0(19) ? C1b H3c1b . . 0.96(2) 0.96(2) 0.96(2) ? C2a C3a . . 1.519(5) 1.519(5) 1.520(5) ? C2b C3b . . 1.519(5) 1.518(5) 1.520(5) ? C3a C4a . . 1.543(5) 1.542(5) 1.545(5) ? C3a H1c3a . . 1.0(11) 1.0(12) 1.0(12) ? C3b C4b . . 1.556(5) 1.555(5) 1.556(5) ? C3b H1c3b . . 1.0(11) 1.0(11) 1.0(11) ? C4a C5a . . 1.507(5) 1.504(5) 1.509(5) ? C4a H1c4a . . 0.96(6) 0.96(6) 0.96(6) ? C4a H2c4a . . 1(3) 1(3) 1(3) ? C4b C5b . . 1.508(5) 1.506(5) 1.511(5) ? C4b H1c4b . . 1.0(3) 1.0(3) 1.0(3) ? C4b H2c4b . . 1(3) 1(3) 1(3) ? C5a C6a . . 1.387(5) 1.385(5) 1.389(5) ? C5a C10a . . 1.397(6) 1.390(6) 1.404(6) ? C5b C6b . . 1.395(5) 1.392(5) 1.397(5) ? C5b C10b . . 1.394(6) 1.392(6) 1.395(6) ? C6a C7a . . 1.383(5) 1.383(5) 1.384(5) ? C6a H1c6a . . 1.0(3) 1.0(3) 1.0(3) ? C6b C7b . . 1.380(5) 1.376(5) 1.384(5) ? C6b H1c6b . . 1.0(8) 1.0(8) 1.0(8) ? C7a C8a . . 1.395(6) 1.393(6) 1.396(6) ? C7a H1c7a . . 1(3) 1(3) 1(3) ? C7b C8b . . 1.379(6) 1.379(6) 1.380(6) ? C7b H1c7b . . 1(4) 1(4) 1(4) ? C8a C9a . . 1.382(5) 1.379(5) 1.386(5) ? C8a H1c8a . . 1.0(18) 1.0(18) 1.0(18) ? C8b C9b . . 1.394(5) 1.391(5) 1.397(5) ? C8b H1c8b . . 1.0(8) 1.0(8) 1.0(8) ? C9a C10a . . 1.389(5) 1.386(5) 1.392(5) ? C9a H1c9a . . 1.0(3) 1.0(3) 1.0(3) ? C9b C10b . . 1.384(5) 1.383(5) 1.385(5) ? C9b H1c9b . . 0.960(7) 0.960(7) 0.960(7) ? C10a H1c10a . . 1(3) 1(3) 1(3) ? C10b H1c10b . . 1.0(14) 1.0(14) 1.0(14) ? C11a C12a . . 1.498(5) 1.498(5) 1.498(5) ? C11b C12b . . 1.502(5) 1.497(5) 1.508(5) ? C12a C13a . . 1.385(6) 1.383(6) 1.388(6) ? C12a C17a . . 1.386(6) 1.384(6) 1.388(6) ? C12b C13b . . 1.373(6) 1.371(6) 1.374(6) ? C12b C17b . . 1.385(6) 1.383(6) 1.387(6) ? C13a C14a . . 1.384(5) 1.381(5) 1.386(5) ? C13a H1c13a . . 1.0(7) 1.0(7) 1.0(7) ? C13b C14b . . 1.387(5) 1.387(5) 1.387(5) ? C13b H1c13b . . 1.0(6) 1.0(6) 1.0(6) ? C14a C15a . . 1.392(6) 1.388(7) 1.396(7) ? C14a H1c14a . . 1(3) 1(3) 1(3) ? C14b C15b . . 1.389(6) 1.386(6) 1.392(6) ? C14b H1c14b . . 1.0(12) 1.0(13) 1.0(13) ? C15a C16a . . 1.394(5) 1.384(6) 1.404(6) ? C15a C18a . . 1.484(4) 1.476(4) 1.491(4) ? C15b C16b . . 1.380(5) 1.377(5) 1.383(5) ? C15b C18b . . 1.498(4) 1.497(4) 1.499(4) ? C16a C17a . . 1.389(5) 1.386(5) 1.393(5) ? C16a H1c16a . . 0.960(5) 0.960(5) 0.960(5) ? C16b C17b . . 1.383(4) 1.376(4) 1.390(4) ? C16b H1c16b . . 0.96(10) 0.96(10) 0.96(10) ? C17a H1c17a . . 1.0(4) 1.0(4) 1.0(4) ? C17b H1c17b . . 1.0(5) 1.0(5) 1.0(5) ? C18a C19a . . 1.394(5) 1.390(5) 1.399(5) ? C18a C23a . . 1.399(6) 1.393(6) 1.404(6) ? C18b C19b . . 1.392(6) 1.391(6) 1.394(6) ? C18b C23b . . 1.396(6) 1.392(6) 1.399(6) ? C19a C20a . . 1.382(5) 1.381(5) 1.383(5) ? C19a H1c19a . . 1.0(13) 1.0(13) 1.0(13) ? C19b C20b . . 1.385(5) 1.378(5) 1.392(5) ? C19b H1c19b . . 1(2) 1(2) 1(2) ? C20a C21a . . 1.389(6) 1.386(7) 1.392(7) ? C20a H1c20a . . 1(3) 1(3) 1(3) ? C20b C21b . . 1.380(6) 1.375(6) 1.384(6) ? C20b H1c20b . . 1.0(19) 1(2) 1(2) ? C21a C22a . . 1.376(6) 1.371(6) 1.381(6) ? C21a H1c21a . . 0.96(10) 0.96(10) 0.96(10) ? C21b C22b . . 1.373(6) 1.371(6) 1.375(6) ? C21b H1c21b . . 1.0(8) 1.0(8) 1.0(8) ? C22a C23a . . 1.384(5) 1.382(5) 1.387(5) ? C22a H1c22a . . 1.0(4) 1.0(4) 1.0(4) ? C22b C23b . . 1.381(5) 1.374(5) 1.389(5) ? C22b H1c22b . . 1.0(3) 1.0(3) 1.0(3) ? C23a H1c23a . . 0.96(16) 0.96(17) 0.96(17) ? C23b H1c23b . . 0.960(14) 0.960(15) 0.960(15) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag C1a O1a C2a . . . 115.5(3) 115.5(3) 115.6(3) ? C1b O1b C2b . . . 114.5(3) 114.4(3) 114.5(3) ? C3a N1a C11a . . . 122.4(3) 122.0(3) 122.7(3) ? C3a N1a H1n1a . . . 113(4) 112(4) 113(4) ? C11a N1a H1n1a . . . 122(4) 121(4) 124(4) ? C3b N1b C11b . . . 121.0(2) 120.4(2) 121.5(2) ? C3b N1b H1n1b . . . 117.3(15) 117.2(15) 117.5(15) ? C11b N1b H1n1b . . . 121.6(15) 121.0(15) 122.2(15) ? O1a C1a H1c1a . . . 109.47 109.47 109.47 ? O1a C1a H2c1a . . . 109.47 109.47 109.47 ? O1a C1a H3c1a . . . 109.47 109.47 109.47 ? H1c1a C1a H2c1a . . . 109.47 109.47 109.47 ? H1c1a C1a H3c1a . . . 109.47 109.47 109.47 ? H2c1a C1a H3c1a . . . 109.47 109.47 109.47 ? O1b C1b H1c1b . . . 109.47 109.47 109.47 ? O1b C1b H2c1b . . . 109.47 109.47 109.47 ? O1b C1b H3c1b . . . 109.47 109.47 109.47 ? H1c1b C1b H2c1b . . . 109.47 109.47 109.47 ? H1c1b C1b H3c1b . . . 109.47 109.47 109.47 ? H2c1b C1b H3c1b . . . 109.47 109.47 109.47 ? O1a C2a O2a . . . 123.8(3) 123.4(3) 124.2(3) ? O1a C2a C3a . . . 112.7(3) 112.5(3) 112.9(3) ? O2a C2a C3a . . . 123.5(4) 123.4(4) 123.7(4) ? O1b C2b O2b . . . 124.2(4) 124.1(4) 124.3(4) ? O1b C2b C3b . . . 112.6(3) 112.5(3) 112.6(3) ? O2b C2b C3b . . . 123.2(4) 123.2(4) 123.3(4) ? N1a C3a C2a . . . 111.4(3) 111.0(3) 111.8(3) ? N1a C3a C4a . . . 111.6(3) 111.4(3) 111.7(3) ? N1a C3a H1c3a . . . 107.2 107.06 107.35 ? C2a C3a C4a . . . 111.0(3) 110.9(3) 111.1(3) ? C2a C3a H1c3a . . . 107.81 107.43 108.19 ? C4a C3a H1c3a . . . 107.62 107.44 107.8 ? N1b C3b C2b . . . 112.6(3) 112.5(3) 112.7(3) ? N1b C3b C4b . . . 113.1(3) 112.9(3) 113.4(3) ? N1b C3b H1c3b . . . 104.51 104.21 104.81 ? C2b C3b C4b . . . 109.1(3) 109.0(3) 109.1(3) ? C2b C3b H1c3b . . . 108.98 108.94 109.01 ? C4b C3b H1c3b . . . 108.35 108.22 108.48 ? C3a C4a C5a . . . 113.1(3) 112.6(3) 113.6(3) ? C3a C4a H1c4a . . . 109.47 109.47 109.47 ? C3a C4a H2c4a . . . 109.47 109.47 109.47 ? C5a C4a H1c4a . . . 109.47 109.47 109.47 ? C5a C4a H2c4a . . . 109.47 109.47 109.47 ? H1c4a C4a H2c4a . . . 105.58 105.05 106.1 ? C3b C4b C5b . . . 114.2(3) 114.1(3) 114.3(3) ? C3b C4b H1c4b . . . 109.47 109.47 109.47 ? C3b C4b H2c4b . . . 109.47 109.47 109.47 ? C5b C4b H1c4b . . . 109.47 109.47 109.47 ? C5b C4b H2c4b . . . 109.47 109.47 109.47 ? H1c4b C4b H2c4b . . . 104.28 104.2 104.36 ? C4a C5a C6a . . . 120.3(3) 120.1(3) 120.5(3) ? C4a C5a C10a . . . 121.1(3) 120.9(3) 121.3(3) ? C6a C5a C10a . . . 118.6(3) 118.6(3) 118.6(3) ? C4b C5b C6b . . . 119.5(3) 119.2(3) 119.9(3) ? C4b C5b C10b . . . 122.2(3) 122.1(3) 122.3(3) ? C6b C5b C10b . . . 118.3(4) 118.0(3) 118.5(4) ? C5a C6a C7a . . . 120.7(3) 120.5(3) 120.8(3) ? C5a C6a H1c6a . . . 119.68 119.62 119.73 ? C7a C6a H1c6a . . . 119.67 119.61 119.73 ? C5b C6b C7b . . . 120.9(3) 120.7(3) 121.0(3) ? C5b C6b H1c6b . . . 119.57 119.5 119.63 ? C7b C6b H1c6b . . . 119.57 119.5 119.63 ? C6a C7a C8a . . . 120.7(3) 120.3(3) 121.1(3) ? C6a C7a H1c7a . . . 119.67 119.47 119.87 ? C8a C7a H1c7a . . . 119.67 119.46 119.87 ? C6b C7b C8b . . . 120.4(4) 120.4(4) 120.4(4) ? C6b C7b H1c7b . . . 119.79 119.78 119.8 ? C8b C7b H1c7b . . . 119.79 119.78 119.8 ? C7a C8a C9a . . . 119.0(4) 118.6(4) 119.4(4) ? C7a C8a H1c8a . . . 120.51 120.32 120.69 ? C9a C8a H1c8a . . . 120.51 120.33 120.7 ? C7b C8b C9b . . . 119.7(4) 119.7(4) 119.7(4) ? C7b C8b H1c8b . . . 120.16 120.14 120.17 ? C9b C8b H1c8b . . . 120.16 120.14 120.17 ? C8a C9a C10a . . . 120.4(3) 120.1(3) 120.6(3) ? C8a C9a H1c9a . . . 119.81 119.68 119.94 ? C10a C9a H1c9a . . . 119.81 119.68 119.94 ? C8b C9b C10b . . . 119.7(3) 119.6(3) 119.7(3) ? C8b C9b H1c9b . . . 120.16 120.13 120.19 ? C10b C9b H1c9b . . . 120.16 120.13 120.19 ? C5a C10a C9a . . . 120.7(3) 120.5(3) 120.9(3) ? C5a C10a H1c10a . . . 119.64 119.54 119.74 ? C9a C10a H1c10a . . . 119.64 119.54 119.74 ? C5b C10b C9b . . . 121.1(4) 121.1(4) 121.1(4) ? C5b C10b H1c10b . . . 119.46 119.45 119.47 ? C9b C10b H1c10b . . . 119.46 119.45 119.47 ? O3a C11a N1a . . . 123.5(3) 123.3(3) 123.6(3) ? O3a C11a C12a . . . 120.6(3) 120.3(3) 120.8(3) ? N1a C11a C12a . . . 116.0(3) 115.8(3) 116.1(3) ? O3b C11b N1b . . . 122.3(3) 122.0(3) 122.7(3) ? O3b C11b C12b . . . 120.7(3) 120.7(3) 120.8(3) ? N1b C11b C12b . . . 116.9(3) 116.7(3) 117.2(3) ? C11a C12a C13a . . . 118.2(3) 117.8(3) 118.5(3) ? C11a C12a C17a . . . 123.3(3) 122.7(3) 123.9(3) ? C13a C12a C17a . . . 118.5(3) 118.2(3) 118.8(3) ? C11b C12b C13b . . . 118.3(3) 118.2(3) 118.5(3) ? C11b C12b C17b . . . 123.1(3) 123.0(3) 123.1(3) ? C13b C12b C17b . . . 118.6(3) 118.4(3) 118.7(3) ? C12a C13a C14a . . . 120.5(3) 120.4(4) 120.6(3) ? C12a C13a H1c13a . . . 119.75 119.71 119.79 ? C14a C13a H1c13a . . . 119.75 119.71 119.79 ? C12b C13b C14b . . . 121.2(4) 121.1(4) 121.2(4) ? C12b C13b H1c13b . . . 119.42 119.4 119.45 ? C14b C13b H1c13b . . . 119.42 119.39 119.45 ? C13a C14a C15a . . . 121.7(3) 121.6(4) 121.9(3) ? C13a C14a H1c14a . . . 119.13 119.06 119.2 ? C15a C14a H1c14a . . . 119.13 119.06 119.2 ? C13b C14b C15b . . . 121.2(4) 121.0(4) 121.4(4) ? C13b C14b H1c14b . . . 119.41 119.32 119.51 ? C15b C14b H1c14b . . . 119.41 119.32 119.51 ? C14a C15a C16a . . . 117.3(3) 117.3(3) 117.3(3) ? C14a C15a C18a . . . 121.0(3) 121.0(3) 121.1(3) ? C16a C15a C18a . . . 121.6(3) 121.5(3) 121.7(3) ? C14b C15b C16b . . . 116.6(3) 116.3(3) 117.0(3) ? C14b C15b C18b . . . 121.2(3) 120.6(3) 121.8(3) ? C16b C15b C18b . . . 122.1(3) 121.8(3) 122.4(3) ? C15a C16a C17a . . . 121.0(3) 120.9(3) 121.0(3) ? C15a C16a H1c16a . . . 119.52 119.48 119.56 ? C17a C16a H1c16a . . . 119.52 119.48 119.56 ? C15b C16b C17b . . . 122.7(3) 122.3(3) 123.2(3) ? C15b C16b H1c16b . . . 118.63 118.42 118.83 ? C17b C16b H1c16b . . . 118.63 118.42 118.83 ? C12a C17a C16a . . . 120.9(3) 120.9(3) 120.9(3) ? C12a C17a H1c17a . . . 119.54 119.54 119.54 ? C16a C17a H1c17a . . . 119.54 119.53 119.54 ? C12b C17b C16b . . . 119.7(4) 119.6(4) 119.7(4) ? C12b C17b H1c17b . . . 120.16 120.13 120.2 ? C16b C17b H1c17b . . . 120.17 120.13 120.2 ? C15a C18a C19a . . . 121.4(3) 120.9(3) 121.9(3) ? C15a C18a C23a . . . 121.7(3) 121.6(3) 121.9(3) ? C19a C18a C23a . . . 116.9(3) 116.3(3) 117.4(3) ? C15b C18b C19b . . . 120.8(3) 120.7(3) 120.9(3) ? C15b C18b C23b . . . 121.7(3) 121.7(3) 121.7(3) ? C19b C18b C23b . . . 117.5(3) 117.4(3) 117.7(3) ? C18a C19a C20a . . . 122.0(4) 121.4(4) 122.6(4) ? C18a C19a H1c19a . . . 118.99 118.71 119.28 ? C20a C19a H1c19a . . . 118.99 118.71 119.28 ? C18b C19b C20b . . . 120.9(4) 120.4(3) 121.5(4) ? C18b C19b H1c19b . . . 119.54 119.26 119.82 ? C20b C19b H1c19b . . . 119.53 119.25 119.81 ? C19a C20a C21a . . . 119.8(3) 119.5(3) 120.1(3) ? C19a C20a H1c20a . . . 120.09 119.95 120.24 ? C21a C20a H1c20a . . . 120.09 119.95 120.24 ? C19b C20b C21b . . . 121.0(4) 120.6(4) 121.3(4) ? C19b C20b H1c20b . . . 119.52 119.36 119.69 ? C21b C20b H1c20b . . . 119.52 119.36 119.69 ? C20a C21a C22a . . . 119.4(3) 119.4(3) 119.4(3) ? C20a C21a H1c21a . . . 120.31 120.3 120.32 ? C22a C21a H1c21a . . . 120.31 120.3 120.32 ? C20b C21b C22b . . . 118.4(3) 118.3(3) 118.5(3) ? C20b C21b H1c21b . . . 120.8 120.75 120.86 ? C22b C21b H1c21b . . . 120.8 120.75 120.85 ? C21a C22a C23a . . . 120.5(4) 120.0(3) 121.0(4) ? C21a C22a H1c22a . . . 119.76 119.51 120.01 ? C23a C22a H1c22a . . . 119.76 119.51 120 ? C21b C22b C23b . . . 121.4(3) 121.3(3) 121.6(3) ? C21b C22b H1c22b . . . 119.29 119.2 119.37 ? C23b C22b H1c22b . . . 119.29 119.2 119.38 ? C18a C23a C22a . . . 121.4(3) 120.7(3) 122.2(3) ? C18a C23a H1c23a . . . 119.28 118.9 119.66 ? C22a C23a H1c23a . . . 119.28 118.9 119.66 ? C18b C23b C22b . . . 120.7(3) 120.6(3) 120.8(3) ? C18b C23b H1c23b . . . 119.64 119.6 119.68 ? C22b C23b H1c23b . . . 119.64 119.6 119.68 ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_index_m_1 _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_include_status 1 0 0 0 1.73 6.91 2.78 < 2 0 0 0 2722.38 2268.02 55.75 o 3 0 0 0 91.14 107.95 5.84 o 4 0 0 0 68.35 86.71 9.36 o 5 0 0 0 81.25 81.02 8.12 o 1 -1 0 0 5573.46 5406.39 47.29 o 2 1 0 0 434.33 399.63 24.37 o 2 -1 0 0 433.00 395.77 22.43 o 3 1 0 0 315.07 343.02 10.47 o 3 -1 0 0 317.16 343.89 10.54 o 4 1 0 0 73.92 94.83 6.88 o 4 -1 0 0 73.99 97.52 10.34 o 5 1 0 0 41.81 22.52 5.54 o 5 -1 0 0 42.43 34.42 5.87 o 0 2 0 0 1438.00 1465.45 26.61 o 1 2 0 0 6472.50 6299.67 78.09 o 1 -2 0 0 6465.88 6462.72 57.66 o 2 2 0 0 87.89 110.15 14.21 o 2 -2 0 0 87.16 109.34 7.45 o 3 2 0 0 104.71 112.17 6.66 o 4 2 0 0 86.21 102.69 9.83 o 4 -2 0 0 86.99 100.00 10.41 o 5 2 0 0 45.09 87.29 8.51 o 5 -2 0 0 45.22 41.02 6.23 o 1 3 0 0 552.68 518.48 24.61 o 2 3 0 0 240.45 253.40 12.39 o 2 -3 0 0 236.92 237.18 11.71 o 3 3 0 0 404.43 402.23 17.34 o 3 -3 0 0 403.98 381.33 17.72 o 4 3 0 0 1241.05 1209.98 34.55 o 4 -3 0 0 1238.62 1275.88 35.95 o 0 4 0 0 36.52 42.74 4.11 o 1 4 0 0 91.37 87.36 4.64 o 2 4 0 0 1625.17 1611.50 21.28 o 3 4 0 0 197.78 169.80 12.38 o 4 4 0 0 156.98 170.27 13.50 o 4 -4 0 0 158.51 187.76 14.59 o 5 -4 0 0 17.99 19.65 4.32 o 1 5 0 0 193.66 195.04 7.38 o 2 5 0 0 299.80 247.23 13.75 o 3 5 0 0 297.07 279.55 16.31 o 4 -5 0 0 381.70 401.20 14.14 o 5 -5 0 0 30.36 24.16 4.17 o 0 6 0 0 866.12 939.69 25.28 o 1 6 0 0 67.84 76.08 5.37 o 2 6 0 0 33.89 37.39 6.34 o 3 6 0 0 398.71 388.95 19.70 o 3 -6 0 0 397.93 430.66 15.02 o 4 -6 0 0 47.29 56.58 4.93 o 1 7 0 0 659.70 693.65 25.00 o 2 7 0 0 891.01 868.00 29.40 o 2 -7 0 0 891.00 913.57 21.34 o 3 -7 0 0 1.53 6.93 3.15 < 4 -7 0 0 26.52 37.79 4.22 o 1 -8 0 0 255.99 266.88 17.95 o 2 -8 0 0 142.95 128.73 8.02 o 3 -8 0 0 30.22 32.22 3.69 o 1 -9 0 0 329.87 296.90 11.56 o 0 -10 0 0 96.68 105.21 7.71 o 1 -10 0 0 134.59 135.91 8.75 o -5 0 1 -1 0.09 1.74 1.81 < -4 0 1 -1 29.19 30.48 4.42 o -3 0 1 -1 53.75 57.42 4.75 o -2 0 1 -1 0.54 -0.01 1.61 < -1 0 1 -1 25.47 23.26 4.85 o 0 0 0 1 0.06 -1.43 0.94 < 1 0 0 1 105.38 83.91 8.80 o 2 0 0 1 1.94 -1.75 2.23 < 3 0 0 1 37.92 29.10 3.55 o 4 0 0 1 17.70 19.22 2.95 o 5 0 0 1 1.48 -0.05 1.92 < -5 1 1 -1 23.84 27.57 4.41 o -5 -1 1 -1 23.83 25.11 4.59 o -4 1 1 -1 20.04 23.22 3.43 o -4 -1 1 -1 20.05 17.68 3.82 o -3 1 1 -1 5.23 6.96 2.29 o -3 -1 1 -1 5.22 5.44 2.99 < -2 1 1 -1 0.81 0.68 1.29 < -2 -1 1 -1 0.80 0.73 1.33 < -1 1 1 -1 13.43 8.61 3.37 < -1 -1 1 -1 13.44 7.80 2.28 o 0 1 1 -1 1.62 2.39 2.05 < 0 -1 1 -1 1.62 2.88 1.21 < 0 -1 0 1 7.22 3.88 1.42 < 1 1 0 1 37.88 31.81 6.27 o 1 -1 0 1 37.92 32.85 3.92 o 2 1 0 1 9.08 11.69 1.94 o 2 -1 0 1 9.11 11.53 2.18 o 3 1 0 1 17.15 19.51 3.20 o 3 -1 0 1 17.23 13.54 3.45 o 4 1 0 1 42.59 39.25 7.04 o 4 -1 0 1 42.59 40.87 4.49 o 5 1 0 1 12.97 11.58 3.76 o 5 -1 0 1 12.97 13.28 3.19 o -5 2 1 -1 6.34 4.69 1.95 < -5 -2 1 -1 6.37 4.32 2.92 < -4 2 1 -1 14.82 11.44 3.66 o -4 -2 1 -1 14.83 15.98 3.71 o -3 2 1 -1 13.89 10.30 2.57 o -3 -2 1 -1 13.90 4.99 2.67 < -2 2 1 -1 14.90 15.77 2.23 o -2 -2 1 -1 14.93 16.84 2.45 o -1 2 1 -1 40.82 37.98 7.71 o 0 2 1 -1 8.47 11.35 3.42 o 0 2 0 1 34.92 23.72 4.33 o 1 2 0 1 5.20 6.57 3.63 < 2 2 0 1 36.71 30.68 2.95 o 2 -2 0 1 36.64 35.81 3.43 o 3 2 0 1 2.11 2.53 1.73 < 3 -2 0 1 2.12 2.63 2.37 < 4 2 0 1 24.17 14.20 3.75 o 4 -2 0 1 24.19 22.89 4.16 o 5 2 0 1 3.90 1.90 1.22 < 5 -2 0 1 3.91 6.18 2.50 < -4 -3 1 -1 4.71 6.87 2.86 < -3 3 1 -1 10.47 13.56 3.32 o -3 -3 1 -1 10.53 18.33 4.17 o -2 3 1 -1 40.88 45.53 5.40 o -2 -3 1 -1 40.83 37.48 5.09 o -1 3 1 -1 11.07 15.55 3.23 o 0 3 1 -1 75.57 71.58 7.94 o 0 3 0 1 145.99 121.52 10.76 o 1 3 0 1 21.64 19.98 2.45 o 2 3 0 1 13.86 10.65 3.04 o 2 -3 0 1 13.88 11.53 3.90 < 3 3 0 1 0.60 1.71 2.07 < 3 -3 0 1 0.61 -1.79 2.46 < 4 -3 0 1 1.29 5.26 2.05 < -4 -4 1 -1 0.68 -0.30 2.34 < -3 4 1 -1 4.49 0.54 2.64 < -2 4 1 -1 56.73 53.73 6.45 o -1 4 1 -1 11.65 8.69 1.38 o 0 4 1 -1 141.29 140.11 5.22 o 0 4 0 1 84.22 83.11 4.18 o 1 4 0 1 10.12 8.56 1.75 o 2 4 0 1 11.23 8.65 3.33 < 3 4 0 1 5.67 5.59 2.38 < 4 -4 0 1 2.22 0.73 2.22 < -4 -5 1 -1 3.95 7.54 3.65 < -3 5 1 -1 23.28 30.15 5.69 o -3 -5 1 -1 23.33 26.88 3.66 o -2 5 1 -1 27.77 23.92 4.67 o -1 5 1 -1 57.00 55.63 4.20 o 0 5 1 -1 74.19 81.17 4.69 o 0 5 0 1 45.37 51.43 3.79 o 1 5 0 1 69.40 71.08 4.80 o 2 5 0 1 2.81 -1.87 2.20 < 3 5 0 1 1.52 1.87 3.00 < 3 -5 0 1 1.49 2.22 1.92 < 4 -5 0 1 0.84 0.22 2.29 < -4 -6 1 -1 9.14 13.94 2.76 o -3 -6 1 -1 74.77 81.89 5.22 o -2 6 1 -1 2.94 3.69 2.37 < -2 -6 1 -1 2.95 -2.53 2.25 < -1 6 1 -1 78.90 60.29 7.19 o 0 6 1 -1 81.74 80.55 5.36 o 0 6 0 1 28.02 28.78 3.31 o 1 6 0 1 145.74 155.62 11.41 o 2 6 0 1 4.06 3.23 2.28 < 2 -6 0 1 4.09 0.13 1.36 < 3 -6 0 1 19.40 16.12 3.63 o 4 -6 0 1 1.10 1.96 2.40 < -3 -7 1 -1 4.32 7.15 2.00 o -2 -7 1 -1 9.52 7.47 2.11 o -1 7 1 -1 4.27 3.67 2.62 < -1 -7 1 -1 4.27 6.63 2.24 < 0 7 1 -1 10.01 9.02 2.06 o 0 7 0 1 3.00 2.64 1.63 < 1 7 0 1 73.95 80.80 9.10 o 1 -7 0 1 74.03 78.47 4.56 o 2 -7 0 1 45.48 38.65 3.33 o 3 -7 0 1 1.28 3.86 1.91 < -3 -8 1 -1 2.83 2.93 1.48 < -2 -8 1 -1 23.34 21.90 3.58 o -1 -8 1 -1 7.05 4.85 2.15 < 0 -8 1 -1 16.21 12.04 2.23 o 0 -8 0 1 6.45 8.04 1.96 o 1 -8 0 1 45.66 45.30 3.52 o 2 -8 0 1 31.38 30.28 4.01 o 3 -8 0 1 2.17 2.61 1.35 < -2 -9 1 -1 5.62 7.91 2.49 o -1 -9 1 -1 3.00 3.55 2.38 < 0 -9 1 -1 20.95 19.28 2.77 o 0 -9 0 1 11.39 11.50 2.46 o 1 -9 0 1 2.83 3.63 2.82 < 2 -9 0 1 6.57 5.06 1.64 o 0 -10 1 -1 14.06 26.06 4.25 o 0 -10 0 1 5.85 9.42 2.63 o -5 0 1 0 15.73 9.14 3.92 < -4 0 1 0 1.38 12.32 4.47 < -3 0 1 0 66.11 61.81 4.56 o -2 0 1 0 12.82 0.98 5.56 < -1 0 1 0 4764.23 4953.02 61.73 o 1 0 1 0 16477.80 17022.00 102.13 o 2 0 1 0 510.88 515.21 25.78 o 3 0 1 0 143.27 161.81 7.29 o 4 0 1 0 1.35 2.96 2.36 < 5 0 1 0 9.20 12.35 3.84 o -5 1 1 0 28.78 42.82 6.43 o -4 1 1 0 487.03 500.08 21.62 o -4 -1 1 0 488.76 483.30 21.77 o -3 1 1 0 21.94 28.65 3.53 o -3 -1 1 0 22.28 30.81 5.48 o -2 1 1 0 95.34 109.33 14.35 o -2 -1 1 0 96.69 97.48 11.56 o -1 -1 1 0 9388.23 9412.12 67.04 o 0 1 1 0 1483.23 1440.07 13.18 o 1 -1 1 0 8663.20 8499.15 44.47 o 2 1 1 0 1013.42 1035.82 38.92 o 2 -1 1 0 1007.19 1051.46 36.05 o 3 1 1 0 137.07 131.70 6.48 o 3 -1 1 0 134.96 116.54 6.20 o 4 1 1 0 190.05 199.65 9.55 o 4 -1 1 0 190.21 207.66 14.62 o -5 -2 1 0 65.42 67.62 5.66 o -4 2 1 0 451.33 444.96 20.28 o -4 -2 1 0 451.41 412.34 20.49 o -3 2 1 0 1121.87 1080.04 18.91 o -3 -2 1 0 1125.91 1058.60 27.54 o -2 2 1 0 979.45 1064.47 41.80 o -2 -2 1 0 984.20 1007.94 21.62 o -1 2 1 0 5766.71 5699.22 73.67 o -1 -2 1 0 5795.63 5875.90 58.59 o 0 2 1 0 13981.60 14876.60 62.41 o 1 2 1 0 5571.95 5377.49 73.37 o 2 2 1 0 186.04 185.77 9.90 o 2 -2 1 0 185.70 186.62 10.42 o 3 2 1 0 362.15 304.94 14.44 o 3 -2 1 0 360.99 307.86 10.64 o 4 2 1 0 29.06 37.36 6.55 o 4 -2 1 0 29.90 32.96 6.41 o -5 -3 1 0 437.01 461.31 20.02 o -4 3 1 0 57.06 109.58 11.29 o -3 3 1 0 257.30 274.30 14.28 o -3 -3 1 0 258.56 249.67 14.57 o -2 3 1 0 53.80 41.22 5.48 o -1 3 1 0 259.68 237.44 17.02 o 0 3 1 0 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106.36 127.00 11.34 o -4 -1 3 0 106.50 124.90 11.53 o -3 1 3 0 295.33 307.91 9.84 o -3 -1 3 0 296.36 312.91 14.37 o -2 1 3 0 681.01 701.44 32.59 o -2 -1 3 0 682.46 636.24 19.63 o -1 1 3 0 12990.60 13117.30 102.94 o -1 -1 3 0 13014.80 12883.10 63.27 o 0 1 3 0 1867.74 1829.85 16.88 o 1 -1 3 0 5318.93 5442.79 32.59 o 2 1 3 0 329.90 371.00 23.32 o 2 -1 3 0 329.77 390.55 20.99 o 3 1 3 0 65.94 68.60 4.72 o 3 -1 3 0 66.25 66.92 4.99 o 4 1 3 0 239.82 272.80 16.32 o 4 -1 3 0 240.33 267.98 11.41 o 5 1 3 0 161.40 218.81 14.08 o -5 -2 3 0 124.93 129.68 10.13 o -4 2 3 0 232.82 220.85 14.53 o -4 -2 3 0 232.76 204.15 14.71 o -3 2 3 0 275.52 279.43 9.74 o -3 -2 3 0 274.20 286.38 14.41 o -2 2 3 0 149.96 159.08 17.58 o -2 -2 3 0 150.70 143.54 9.63 o -1 2 3 0 2938.62 2799.33 51.58 o -1 -2 3 0 2925.91 2857.17 44.74 o 0 2 3 0 9620.59 10077.40 51.02 o 1 2 3 0 1702.12 1695.58 41.11 o 2 2 3 0 1668.42 1656.92 29.52 o 2 -2 3 0 1675.65 1639.91 27.84 o 3 2 3 0 667.82 654.36 21.23 o 3 -2 3 0 670.04 655.67 15.39 o 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1571.31 27.28 o 0 4 5 0 163.77 174.54 8.76 o 1 4 5 0 1684.35 1721.09 22.44 o 1 -4 5 0 1688.09 1694.74 28.14 o 2 4 5 0 1421.39 1378.09 30.03 o 3 4 5 0 26.80 16.55 4.68 o 4 -4 5 0 27.13 35.21 6.27 o -5 -5 5 0 94.28 110.21 8.56 o -4 -5 5 0 138.95 144.83 8.74 o -3 5 5 0 197.90 190.65 13.76 o -2 5 5 0 56.82 65.03 7.36 o -1 5 5 0 291.34 320.14 13.95 o 0 5 5 0 444.08 479.85 11.17 o 1 5 5 0 187.60 185.29 7.38 o 2 5 5 0 36.13 34.35 3.69 o 3 5 5 0 505.60 492.18 14.69 o 4 -5 5 0 30.23 27.38 5.64 o 5 -5 5 0 17.71 19.99 2.59 o -4 -6 5 0 10.75 13.52 4.14 o -3 -6 5 0 40.09 42.59 4.85 o -2 6 5 0 9.84 2.38 4.22 < -1 6 5 0 224.04 201.58 12.61 o 0 6 5 0 164.70 186.93 11.33 o 1 6 5 0 7.71 14.25 2.84 o 2 6 5 0 336.37 311.85 11.44 o 3 -6 5 0 32.40 42.66 6.92 o 4 -6 5 0 12.65 16.79 4.42 o -4 -7 5 0 54.38 51.01 3.98 o -3 -7 5 0 26.10 38.54 3.76 o -2 7 5 0 22.16 22.91 5.73 o -2 -7 5 0 21.37 39.98 6.53 o -1 7 5 0 340.37 337.58 18.12 o 0 7 5 0 18.60 16.21 4.55 o 1 7 5 0 731.26 717.72 17.57 o 2 7 5 0 183.54 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25.56 3.95 o -2 0 43 0 12.49 18.50 3.15 o -1 0 43 0 11.03 6.51 2.56 < 0 0 43 0 43.04 43.56 4.80 o 1 0 43 0 3.03 9.08 3.49 < 2 0 43 0 18.93 20.96 4.33 o -3 1 43 0 48.52 54.08 5.91 o -2 1 43 0 23.23 15.29 2.78 o -2 -1 43 0 23.35 18.81 2.98 o -1 1 43 0 25.78 23.53 4.96 o 0 1 43 0 62.37 65.29 8.00 o 0 -1 43 0 62.35 57.48 7.57 o 1 1 43 0 3.68 5.04 3.31 < 1 -1 43 0 3.56 1.67 1.95 < 2 1 43 0 69.78 58.20 6.61 o 2 -1 43 0 69.93 64.71 7.11 o -2 2 43 0 193.51 215.79 9.06 o -2 -2 43 0 194.84 218.52 12.48 o -1 2 43 0 68.21 62.04 7.73 o 0 2 43 0 55.03 59.02 7.15 o 0 -2 43 0 55.47 57.24 5.22 o 1 2 43 0 166.64 166.96 11.48 o 1 -2 43 0 166.95 161.08 8.18 o 2 2 43 0 36.88 37.13 5.01 o 2 -2 43 0 35.60 40.02 3.92 o -2 3 43 0 31.18 39.92 5.03 o -1 3 43 0 68.43 88.13 8.85 o 0 3 43 0 5.04 7.48 2.56 < 0 -3 43 0 4.97 2.33 2.28 < 1 -3 43 0 44.38 46.42 6.60 o 2 -3 43 0 8.92 7.83 3.20 < -1 -4 43 0 3.45 1.67 1.85 < 0 4 43 0 21.72 31.97 4.81 o 0 -4 43 0 21.83 28.71 4.98 o 1 -4 43 0 15.88 21.89 4.32 o 0 -5 43 0 3.88 5.21 1.37 o -2 0 44 -1 0.92 1.66 2.25 < -1 0 44 -1 0.17 0.29 1.95 < 0 0 44 -1 0.24 -1.50 2.14 < 0 0 43 1 0.13 0.68 2.88 < 1 0 43 1 1.65 0.03 2.90 < 2 0 43 1 0.53 -1.81 1.79 < -2 1 44 -1 2.56 -2.75 2.17 < -2 -1 44 -1 2.57 -0.40 1.77 < -1 1 44 -1 0.58 2.22 1.99 < 0 1 44 -1 1.86 -0.48 2.76 < 0 1 43 1 0.36 2.52 2.98 < 0 -1 43 1 0.35 -1.81 3.37 < 1 1 43 1 1.76 6.82 2.64 < 1 -1 43 1 1.77 5.44 2.64 < 2 1 43 1 3.86 5.60 1.65 o 2 -1 43 1 3.84 11.15 3.11 o -2 2 44 -1 1.05 1.47 1.85 < -1 2 44 -1 2.01 7.70 2.40 o -1 -2 44 -1 1.97 0.92 1.73 < 0 2 44 -1 0.37 -1.43 2.82 < 0 2 43 1 4.94 4.96 2.53 < 0 -2 43 1 4.93 3.89 1.87 < 1 2 43 1 0.07 -3.03 1.62 < 1 -2 43 1 0.07 -3.01 1.89 < -1 3 44 -1 0.38 2.60 2.04 < 0 3 44 -1 0.74 2.46 2.16 < 0 -3 43 1 1.23 3.19 3.14 < 1 -3 43 1 0.30 4.12 3.11 < -1 -4 44 -1 5.34 6.46 3.69 < 0 4 44 -1 2.78 1.67 1.53 < 0 -4 44 -1 2.78 5.13 2.30 < 0 4 43 1 2.98 1.16 2.12 < 0 -4 43 1 3.02 5.65 1.83 o 1 -4 43 1 1.76 5.70 2.66 < -2 0 44 0 0.48 1.37 1.51 < -1 0 44 0 5.77 10.61 3.76 < 0 0 44 0 3.39 4.76 2.04 < 1 0 44 0 204.46 210.33 13.57 o 2 0 44 0 15.81 20.67 4.04 o -2 1 44 0 45.30 40.91 4.13 o -2 -1 44 0 45.36 50.72 4.40 o -1 1 44 0 74.05 80.47 8.58 o 0 1 44 0 1.13 -0.25 1.70 < 0 -1 44 0 1.07 1.66 3.26 < 1 1 44 0 157.35 144.69 11.13 o 1 -1 44 0 157.64 152.69 11.52 o 2 1 44 0 6.58 1.66 1.82 < 2 -1 44 0 6.58 4.84 2.27 < -2 2 44 0 162.28 178.16 7.81 o -2 -2 44 0 160.81 168.56 10.50 o -1 2 44 0 158.12 181.67 12.66 o 0 2 44 0 18.78 22.01 4.81 o 0 -2 44 0 18.16 26.21 5.70 o 1 2 44 0 14.18 11.74 3.45 o 1 -2 44 0 13.97 10.85 2.32 o 2 2 44 0 11.94 16.06 3.61 o 2 -2 44 0 11.73 16.85 2.49 o -2 3 44 0 37.93 35.19 4.62 o -1 3 44 0 87.73 84.03 8.26 o 0 3 44 0 7.94 10.60 3.08 o 1 -3 44 0 13.14 10.97 3.20 o 2 -3 44 0 229.97 242.40 12.03 o -1 -4 44 0 15.02 15.43 3.66 o 0 4 44 0 22.68 19.29 4.11 o 0 -4 44 0 22.22 19.12 3.57 o 1 -4 44 0 25.54 22.34 3.94 o -2 0 45 -1 1.73 0.35 1.44 < -1 0 45 -1 0.00 1.57 2.41 < 0 0 45 -1 1.03 0.47 1.97 < 0 0 44 1 4.88 -0.05 2.55 < 1 0 44 1 0.00 -1.18 2.16 < 2 0 44 1 0.17 1.50 1.65 < -2 1 45 -1 1.13 -0.62 2.14 < -1 1 45 -1 1.97 0.63 2.54 < 0 1 45 -1 0.67 0.86 2.36 < 0 1 44 1 1.82 -1.33 2.88 < 0 -1 44 1 1.84 1.32 2.65 < 1 1 44 1 0.09 2.55 2.61 < 1 -1 44 1 0.09 0.11 2.29 < -1 2 45 -1 4.50 2.64 1.71 < -1 -2 45 -1 4.56 7.20 2.97 < 0 2 45 -1 0.07 0.96 2.45 < 0 2 44 1 1.66 1.59 2.46 < 0 -2 44 1 1.66 2.59 1.76 < 1 2 44 1 3.55 3.62 1.74 < 1 -2 44 1 3.59 4.54 1.77 < -1 3 45 -1 0.45 0.15 1.53 < 0 3 45 -1 0.71 -1.41 2.33 < 0 -3 44 1 0.24 -1.39 2.93 < 1 -3 44 1 0.48 0.24 1.65 < 0 -4 45 -1 0.92 -3.29 2.04 < 0 4 44 1 1.22 3.76 1.70 < -2 0 45 0 30.36 28.24 3.43 o -1 0 45 0 0.60 3.25 2.41 < 0 0 45 0 48.74 56.17 4.96 o 1 0 45 0 14.08 14.49 4.27 o 2 0 45 0 85.22 69.96 6.97 o -2 1 45 0 132.23 132.68 6.88 o -2 -1 45 0 133.36 145.19 10.10 o -1 1 45 0 20.64 28.00 5.31 o 0 1 45 0 23.16 29.71 3.78 o 1 1 45 0 17.60 28.81 5.46 o 1 -1 45 0 17.56 21.71 4.34 o 2 1 45 0 169.73 162.77 10.29 o 2 -1 45 0 168.79 171.35 10.17 o -2 2 45 0 41.57 47.98 5.95 o -1 2 45 0 28.84 34.95 5.86 o 0 2 45 0 5.77 7.14 3.62 < 1 2 45 0 45.44 45.80 5.60 o 1 -2 45 0 45.81 45.51 4.03 o 2 -2 45 0 1.15 -1.57 2.82 < -1 3 45 0 1.55 2.88 2.36 < 0 3 45 0 86.18 78.66 8.01 o 1 -3 45 0 55.87 49.38 6.16 o -1 0 46 -1 0.24 3.22 1.88 < 0 0 46 -1 0.26 -2.96 2.76 < 0 0 45 1 0.63 -1.81 1.79 < 1 0 45 1 2.34 5.06 3.04 < -1 1 46 -1 1.57 2.51 1.53 < -1 -1 46 -1 1.54 3.77 2.44 < 0 1 46 -1 1.61 0.38 2.32 < 0 1 45 1 2.16 2.93 2.86 < 0 -1 45 1 2.16 1.29 1.96 < 1 1 45 1 3.24 -1.98 1.98 < 1 -1 45 1 3.23 2.28 2.31 < -1 2 46 -1 0.78 0.36 1.48 < -1 -2 46 -1 0.77 0.25 2.14 < 0 2 46 -1 0.16 -0.69 2.43 < 0 2 45 1 0.68 -0.01 2.61 < 0 -2 45 1 0.67 2.86 1.33 < 1 2 45 1 0.78 1.88 1.43 < 1 -2 45 1 0.78 0.07 1.37 < -1 3 46 -1 2.15 1.47 1.82 < 0 3 46 -1 0.38 4.35 2.47 < 0 3 45 1 0.87 3.32 2.00 < 1 -3 45 1 1.01 1.06 1.56 < -2 0 46 0 15.59 9.87 1.78 o -1 0 46 0 50.44 45.46 6.08 o 0 0 46 0 10.39 4.15 2.23 < 1 0 46 0 43.07 33.23 5.21 o 2 0 46 0 3.07 -0.03 1.51 < -2 1 46 0 12.41 10.69 2.04 o -2 -1 46 0 12.25 14.55 3.51 o -1 1 46 0 9.65 11.43 3.93 < 0 1 46 0 54.69 55.33 6.91 o 1 1 46 0 73.90 74.13 7.40 o 1 -1 46 0 74.32 73.71 7.45 o 2 1 46 0 78.94 102.72 7.49 o 2 -1 46 0 78.57 106.16 7.61 o -2 2 46 0 3.89 -2.14 2.33 < -1 2 46 0 31.93 34.95 5.07 o 0 2 46 0 39.72 31.61 5.34 o 1 2 46 0 19.71 22.60 4.20 o 1 -2 46 0 19.36 15.53 2.53 o -1 3 46 0 25.91 28.26 4.32 o 0 3 46 0 55.33 57.58 6.31 o 1 -3 46 0 11.40 18.20 3.77 o -1 0 47 -1 8.40 5.98 1.62 o 0 0 47 -1 0.02 0.41 1.82 < 0 0 46 1 0.88 3.72 2.13 < 1 0 46 1 0.47 -4.25 2.73 < -1 1 47 -1 0.43 2.51 1.81 < -1 -1 47 -1 0.45 -1.03 1.91 < 0 1 47 -1 0.27 1.56 2.08 < 0 1 46 1 0.30 1.64 1.65 < 0 -1 46 1 0.30 2.51 2.30 < 1 1 46 1 0.41 -1.40 2.47 < 1 -1 46 1 0.42 2.37 2.02 < -1 2 47 -1 1.83 2.54 1.41 < -1 -2 47 -1 1.82 4.80 1.89 < 0 2 47 -1 0.77 4.55 2.55 < 0 2 46 1 0.51 2.44 2.25 < 0 3 47 -1 6.38 2.82 1.49 < 0 3 46 1 0.61 -1.02 2.45 < -2 0 47 0 35.10 35.17 5.11 o -1 0 47 0 1.85 -2.43 2.89 < 0 0 47 0 41.87 44.29 5.89 o 1 0 47 0 0.87 4.32 1.67 < -1 1 47 0 63.19 52.37 6.27 o 0 1 47 0 211.47 237.55 13.36 o 1 1 47 0 56.50 56.34 6.16 o 1 -1 47 0 56.94 50.12 5.95 o -1 2 47 0 92.22 94.26 5.64 o -1 -2 47 0 92.71 104.22 8.07 o 0 2 47 0 6.90 6.56 2.84 < 1 2 47 0 19.14 12.43 2.82 o 1 -2 47 0 18.92 13.78 2.13 o 0 3 47 0 40.33 55.94 5.95 o -1 0 48 -1 0.97 1.28 1.21 < 0 0 48 -1 0.14 -0.41 1.76 < 0 0 47 1 0.00 -0.35 1.44 < 1 0 47 1 1.69 0.10 2.02 < -1 1 48 -1 1.52 0.63 1.17 < -1 -1 48 -1 1.51 -2.41 2.13 < 0 1 48 -1 5.63 8.47 3.62 < 0 1 47 1 2.22 1.85 1.73 < 1 1 47 1 1.38 -0.72 2.19 < 1 -1 47 1 1.35 7.45 3.06 < 0 2 48 -1 0.35 2.40 2.49 < 0 2 47 1 0.04 -5.11 3.02 < -1 0 48 0 44.72 42.55 5.20 o 0 0 48 0 1.45 7.01 2.73 < 1 0 48 0 75.43 79.59 6.93 o -1 1 48 0 5.33 2.90 2.08 < 0 1 48 0 29.40 41.85 5.51 o 1 1 48 0 24.73 34.82 3.36 o 1 -1 48 0 25.08 29.31 3.96 o -1 2 48 0 80.91 94.16 7.53 o 0 2 48 0 29.89 37.71 5.04 o 0 0 49 -1 0.55 3.04 2.04 < 0 0 48 1 4.48 10.14 2.65 o 0 1 49 -1 2.78 0.08 1.91 < 0 1 48 1 1.81 1.06 2.21 < 0 2 49 -1 4.41 7.13 1.96 o 0 2 48 1 1.55 0.77 2.18 < 0 0 49 0 58.22 70.78 6.44 o 0 1 49 0 209.56 242.79 11.95 o # start Validation Reply Form #_vrf_SYMM003_I #; #PROBLEM: _symmetry_space_group_name_H-M is missing #RESPONSE: The present structural model is in #superspace. Checkcif cannot formally deal #superspace groups. #; #_vrf_SYMM004_I #; #PROBLEM: _symmetry_equiv_pos_as_xyz loop is missing. #RESPONSE: see response to comment _vrf_SYMM003_I #; #_vrf_GEOM003_I #; #PROBLEM: _geom_bond_distance is missing #RESPONSE: Modulated structure model reports #average, minimum and maximum distances. #; #_vrf_GEOM008_I #; #PROBLEM: _geom_angle is missing #RESPONSE: Modulated structure model reports #average, minimum and maximum angles. #; # end Validation Reply Form #======================================================================= data_I_phaseI #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C23 H21 N1 O3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C23 H21 N1 O3' _chemical_formula_weight 359.4 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration syn #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' _space_group_IT_number 4 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y+1/2,-z _cell_length_a 5.0479(2) _cell_length_b 8.6330(4) _cell_length_c 42.1525(15) _cell_angle_alpha 90 _cell_angle_beta 90.513(3) _cell_angle_gamma 90 _cell_volume 1836.87(13) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.9760(8) 1 0 0 0 1 0 0 0 1 2 0.0240(8) 1 0 0 0 -1 0 0 0 -1 _cell_formula_units_Z 4 _cell_measurement_reflns_used 3437 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 65.36 _cell_measurement_temperature 160.00(10) _cell_special_details ? _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.2997 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.69 _exptl_crystal_description 'rectrangular' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_colour colorless _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 160 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Cu K\a' #_diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 7.9580 _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 6108 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 65.26 _diffrn_reflns_theta_full 65.26 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ? _reflns_number_total 4555 _reflns_number_gt 4219 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_gt 0.0481 _refine_ls_R_factor_all 0.0423 _refine_ls_wR_factor_ref 0.0492 _refine_ls_goodness_of_fit_ref 1.54 _refine_ls_goodness_of_fit_gt 1.57 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 4555 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_number_constraints 163 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'mixed' _refine_ls_shift/su_max 0.0003 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 0.17 _refine_diff_density_min -0.15 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 3400(300) _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ; 1218 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0492 0.0322 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_cell_refinement 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group O1a O 0.3209(5) 0.0596(4) 0.45564(5) Uani 0.0488(8) 2 1 d . . . O1b O 0.8559(4) 0.5788(4) 0.04235(4) Uani 0.0340(6) 2 1 d . . . O2a O 0.1752(8) 0.2511(5) 0.48507(7) Uani 0.0852(14) 2 1 d . . . O2b O 0.6560(6) 0.3932(4) 0.01419(5) Uani 0.0533(9) 2 1 d . . . O3a O 0.8541(4) 0.2654(4) 0.39851(5) Uani 0.0383(7) 2 1 d . . . O3b O 0.5560(4) 0.4070(4) 0.09509(4) Uani 0.0330(6) 2 1 d . . . N1a N 0.4147(5) 0.253675 0.40714(5) Uani 0.0265(7) 2 1 d . . . N1b N 0.9919(4) 0.3722(4) 0.08810(5) Uani 0.0235(7) 2 1 d . . . C1a C 0.1977(9) -0.0488(6) 0.47710(8) Uani 0.0552(14) 2 1 d . . . C1b C 0.7025(7) 0.6917(5) 0.02466(7) Uani 0.0414(11) 2 1 d . . . C2a C 0.2913(6) 0.2070(5) 0.46255(6) Uani 0.0335(9) 2 1 d . . . C2b C 0.8031(6) 0.4325(5) 0.03514(6) Uani 0.0291(9) 2 1 d . . . C3a C 0.4295(6) 0.3143(5) 0.43929(6) Uani 0.0281(8) 2 1 d . . . C3b C 0.9592(6) 0.3187(5) 0.05575(6) Uani 0.0255(8) 2 1 d . . . C4a C 0.3154(6) 0.4788(5) 0.44110(7) Uani 0.0336(9) 2 1 d . . . C4b C 0.8291(6) 0.1568(5) 0.05334(6) Uani 0.0296(9) 2 1 d . . . C5a C 0.4559(6) 0.5923(5) 0.41986(6) Uani 0.0316(9) 2 1 d . . . C5b C 0.9369(6) 0.0394(5) 0.07655(6) Uani 0.0288(8) 2 1 d . . . C6a C 0.3833(7) 0.6055(5) 0.38816(7) Uani 0.0388(10) 2 1 d . . . C6b C 0.8186(6) 0.0248(5) 0.10632(7) Uani 0.0331(9) 2 1 d . . . C7a C 0.5160(7) 0.7071(6) 0.36839(7) Uani 0.0431(11) 2 1 d . . . C7b C 0.9087(6) -0.0847(5) 0.12755(7) Uani 0.0384(10) 2 1 d . . . C8a C 0.7185(7) 0.7981(5) 0.37988(7) Uani 0.0414(11) 2 1 d . . . C8b C 1.1171(7) -0.1809(5) 0.12010(8) Uani 0.0398(10) 2 1 d . . . C9a C 0.7912(7) 0.7871(5) 0.41144(8) Uani 0.0435(11) 2 1 d . . . C9b C 1.2378(6) -0.1683(5) 0.09081(8) Uani 0.0380(10) 2 1 d . . . C10a C 0.6598(6) 0.6856(5) 0.43137(7) Uani 0.0369(10) 2 1 d . . . C10b C 1.1468(6) -0.0567(5) 0.06921(7) Uani 0.0352(10) 2 1 d . . . C11a C 0.6282(5) 0.2414(5) 0.38875(6) Uani 0.0275(8) 2 1 d . . . C11b C 0.7833(5) 0.4085(5) 0.10570(6) Uani 0.0236(8) 2 1 d . . . C12a C 0.5746(5) 0.1993(5) 0.35478(6) Uani 0.0271(8) 2 1 d . . . C12b C 0.8386(5) 0.4494(5) 0.13964(6) Uani 0.0235(8) 2 1 d . . . C13a C 0.7404(7) 0.2577(6) 0.33210(7) Uani 0.0489(12) 2 1 d . . . C13b C 0.6711(7) 0.5509(6) 0.15456(7) Uani 0.0430(11) 2 1 d . . . C14a C 0.7010(7) 0.2228(6) 0.30031(7) Uani 0.0505(13) 2 1 d . . . C14b C 0.7094(7) 0.5917(6) 0.18620(7) Uani 0.0439(11) 2 1 d . . . C15a C 0.5008(6) 0.1252(5) 0.29014(6) Uani 0.0274(8) 2 1 d . . . C15b C 0.9146(5) 0.5288(5) 0.20401(6) Uani 0.0248(8) 2 1 d . . . C16a C 0.3368(7) 0.0662(6) 0.31326(7) Uani 0.0439(11) 2 1 d . . . C16b C 1.0803(6) 0.4268(6) 0.18894(7) Uani 0.0414(11) 2 1 d . . . C17a C 0.3717(7) 0.1040(5) 0.34503(7) Uani 0.0430(11) 2 1 d . . . C17b C 1.0469(6) 0.3877(6) 0.15710(7) Uani 0.0393(10) 2 1 d . . . C18a C 0.4636(6) 0.0879(5) 0.25594(6) Uani 0.0275(8) 2 1 d . . . C18b C 0.9493(5) 0.5681(5) 0.23843(6) Uani 0.0279(8) 2 1 d . . . C19a C 0.6213(7) 0.1549(6) 0.23294(7) Uani 0.0482(12) 2 1 d . . . C19b C 0.7833(7) 0.6755(6) 0.25305(7) Uani 0.0419(11) 2 1 d . . . C20a C 0.5851(8) 0.1201(6) 0.20106(7) Uani 0.0535(13) 2 1 d . . . C20b C 0.8104(7) 0.7094(6) 0.28491(7) Uani 0.0442(11) 2 1 d . . . C21a C 0.3936(7) 0.0194(5) 0.19124(7) Uani 0.0363(10) 2 1 d . . . C21b C 1.0040(6) 0.6387(5) 0.30308(7) Uani 0.0354(10) 2 1 d . . . C22a C 0.2357(8) -0.0474(6) 0.21338(8) Uani 0.0497(13) 2 1 d . . . C22b C 1.1728(7) 0.5358(6) 0.28887(7) Uani 0.0418(11) 2 1 d . . . C23a C 0.2706(7) -0.0139(6) 0.24550(7) Uani 0.0488(12) 2 1 d . . . C23b C 1.1471(7) 0.5003(5) 0.25696(7) Uani 0.0356(10) 2 1 d . . . H1c1a H 0.251308 -0.152259 0.471816 Uiso 0.0828 2 1 d . . . H2c1a H 0.25145 -0.025677 0.498482 Uiso 0.0828 2 1 d . . . H3c1a H 0.008574 -0.040418 0.475241 Uiso 0.0828 2 1 d . . . H1c1b H 0.742097 0.793688 0.032416 Uiso 0.062 2 1 d . . . H2c1b H 0.746415 0.685269 0.002591 Uiso 0.062 2 1 d . . . H3c1b H 0.517087 0.670854 0.02725 Uiso 0.062 2 1 d . . . H1c3a H 0.613348 0.319577 0.445211 Uiso 0.0421 2 1 d . . . H1c3b H 1.136613 0.311321 0.047862 Uiso 0.0382 2 1 d . . . H1c4a H 0.130402 0.476416 0.435663 Uiso 0.0504 2 1 d . . . H2c4a H 0.323956 0.514785 0.462634 Uiso 0.0504 2 1 d . . . H1c4b H 0.641145 0.166454 0.056025 Uiso 0.0444 2 1 d . . . H2c4b H 0.846895 0.117959 0.032128 Uiso 0.0444 2 1 d . . . H1c6a H 0.240255 0.543918 0.379864 Uiso 0.0465 2 1 d . . . H1c6b H 0.674133 0.091404 0.111932 Uiso 0.0397 2 1 d . . . H1c7a H 0.465776 0.714034 0.346419 Uiso 0.0517 2 1 d . . . H1c7b H 0.825345 -0.094164 0.147836 Uiso 0.0461 2 1 d . . . H1c8a H 0.80861 0.868643 0.366076 Uiso 0.0497 2 1 d . . . H1c8b H 1.178532 -0.256411 0.13517 Uiso 0.0477 2 1 d . . . H1c9a H 0.933146 0.849834 0.419618 Uiso 0.0522 2 1 d . . . H1c9b H 1.382187 -0.2354 0.085392 Uiso 0.0456 2 1 d . . . H1c10a H 0.710185 0.679619 0.453352 Uiso 0.0442 2 1 d . . . H1c10b H 1.231312 -0.046782 0.048999 Uiso 0.0422 2 1 d . . . H1n1a H 0.248(7) 0.240(4) 0.3988(7) Uiso 0.0319 2 1 d . . . H1n1b H 1.162(7) 0.384(4) 0.0961(7) Uiso 0.0282 2 1 d . . . H1c13a H 0.885181 0.323399 0.338318 Uiso 0.0586 2 1 d . . . H1c13b H 0.524743 0.594576 0.142923 Uiso 0.0515 2 1 d . . . H1c14a H 0.816527 0.267965 0.284877 Uiso 0.0606 2 1 d . . . H1c14b H 0.591423 0.664648 0.195856 Uiso 0.0527 2 1 d . . . H1c16a H 0.195607 -0.002446 0.307208 Uiso 0.0527 2 1 d . . . H1c16b H 1.223823 0.38108 0.200739 Uiso 0.0496 2 1 d . . . H1c17a H 0.251917 0.062771 0.360457 Uiso 0.0516 2 1 d . . . H1c17b H 1.168626 0.317575 0.147232 Uiso 0.0472 2 1 d . . . H1c19a H 0.757737 0.226421 0.239165 Uiso 0.0578 2 1 d . . . H1c19b H 0.648297 0.726572 0.24074 Uiso 0.0503 2 1 d . . . H1c20a H 0.697303 0.167937 0.185617 Uiso 0.0642 2 1 d . . . H1c20b H 0.693164 0.782965 0.294526 Uiso 0.0531 2 1 d . . . H1c21a H 0.370444 -0.004103 0.169127 Uiso 0.0436 2 1 d . . . H1c21b H 1.02055 0.661099 0.325313 Uiso 0.0425 2 1 d . . . H1c22a H 0.099024 -0.118109 0.206831 Uiso 0.0596 2 1 d . . . H1c22b H 1.310666 0.487709 0.301235 Uiso 0.0502 2 1 d . . . H1c23a H 0.157745 -0.062754 0.260734 Uiso 0.0586 2 1 d . . . H1c23b H 1.267223 0.427894 0.247501 Uiso 0.0427 2 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1a O 0.0640(16) 0.0383(14) 0.0445(12) 0.0019(13) 0.0228(10) 0.0012(11) O1b O 0.0440(12) 0.0249(11) 0.0329(10) -0.0020(10) -0.0108(8) 0.0036(9) O2a O 0.158(3) 0.0436(17) 0.0553(16) 0.001(2) 0.0651(19) -0.0016(14) O2b O 0.0797(18) 0.0361(14) 0.0434(12) -0.0009(14) -0.0347(12) -0.0036(12) O3a O 0.0195(10) 0.0602(16) 0.0353(10) -0.0008(10) -0.0001(7) -0.0064(10) O3b O 0.0208(10) 0.0468(14) 0.0313(9) 0.0018(10) -0.0034(7) -0.0025(10) N1a N 0.0209(12) 0.0303(14) 0.0284(11) -0.0013(10) -0.0008(8) -0.0034(10) N1b N 0.0198(11) 0.0259(13) 0.0249(10) -0.0004(9) -0.0014(8) 0.0007(9) C1a C 0.085(3) 0.043(2) 0.0381(18) -0.013(2) 0.0091(17) 0.0025(16) C1b C 0.061(2) 0.0283(18) 0.0349(16) 0.0089(17) -0.0082(14) 0.0049(14) C2a C 0.0415(17) 0.0342(18) 0.0249(13) -0.0037(15) 0.0040(11) -0.0021(13) C2b C 0.0370(16) 0.0278(16) 0.0223(13) 0.0022(14) -0.0005(11) -0.0006(11) C3a C 0.0256(14) 0.0322(16) 0.0263(13) 0.0045(12) -0.0004(10) -0.0023(12) C3b C 0.0254(14) 0.0271(15) 0.0239(12) -0.0002(12) -0.0019(10) -0.0021(11) C4a C 0.0326(16) 0.0375(18) 0.0308(14) 0.0030(14) 0.0045(11) -0.0038(13) C4b C 0.0318(15) 0.0243(16) 0.0326(14) -0.0010(13) -0.0085(11) -0.0028(12) C5a C 0.0329(16) 0.0294(17) 0.0326(13) 0.0073(14) 0.0033(11) -0.0013(13) C5b C 0.0310(15) 0.0199(15) 0.0353(14) -0.0038(12) -0.0068(10) -0.0042(12) C6a C 0.0339(17) 0.046(2) 0.0368(15) 0.0045(15) -0.0047(12) -0.0014(15) C6b C 0.0351(17) 0.0240(16) 0.0402(15) 0.0008(14) 0.0001(12) -0.0006(13) C7a C 0.0454(19) 0.049(2) 0.0349(16) -0.0011(18) -0.0040(13) 0.0042(16) C7b C 0.0430(18) 0.0356(19) 0.0367(15) 0.0029(16) 0.0008(12) 0.0040(15) C8a C 0.0457(18) 0.037(2) 0.0415(17) 0.0004(16) 0.0035(14) 0.0080(15) C8b C 0.0402(17) 0.0327(18) 0.0463(17) 0.0021(15) -0.0080(13) 0.0059(15) C9a C 0.0418(18) 0.039(2) 0.0498(18) -0.0041(17) -0.0031(14) -0.0038(16) C9b C 0.0302(15) 0.0296(17) 0.0541(18) 0.0079(14) -0.0053(13) -0.0047(15) C10a C 0.0410(17) 0.0364(19) 0.0332(14) 0.0029(15) -0.0050(12) -0.0035(13) C10b C 0.0363(17) 0.0317(18) 0.0375(15) -0.0026(14) -0.0012(12) -0.0049(13) C11a C 0.0212(14) 0.0305(17) 0.0310(13) 0.0052(12) 0.0016(10) -0.0016(12) C11b C 0.0198(13) 0.0196(14) 0.0313(13) -0.0011(12) -0.0013(10) 0.0048(12) C12a C 0.0227(14) 0.0294(16) 0.0292(13) 0.0027(13) 0.0016(10) -0.0006(12) C12b C 0.0234(14) 0.0205(14) 0.0266(13) -0.0004(11) 0.0027(10) 0.0043(11) C13a C 0.0408(18) 0.075(3) 0.0307(15) -0.030(2) -0.0011(12) -0.0045(17) C13b C 0.0400(18) 0.055(2) 0.0342(15) 0.0240(18) -0.0087(12) -0.0056(15) C14a C 0.0467(19) 0.076(3) 0.0287(15) -0.030(2) 0.0036(13) -0.0016(17) C14b C 0.051(2) 0.048(2) 0.0327(15) 0.0240(18) -0.0020(13) -0.0091(15) C15a C 0.0240(14) 0.0252(15) 0.0329(14) 0.0049(12) -0.0006(10) 0.0004(12) C15b C 0.0245(14) 0.0210(14) 0.0289(13) -0.0025(12) 0.0029(10) 0.0020(11) C16a C 0.0418(18) 0.054(2) 0.0364(16) -0.0222(18) 0.0073(12) -0.0131(16) C16b C 0.0320(16) 0.062(2) 0.0299(14) 0.0177(17) -0.0071(11) -0.0015(15) C17a C 0.0427(18) 0.051(2) 0.0360(15) -0.0205(17) 0.0161(13) -0.0070(15) C17b C 0.0368(17) 0.052(2) 0.0290(14) 0.0170(16) -0.0018(11) -0.0084(14) C18a C 0.0284(14) 0.0230(15) 0.0311(13) 0.0058(12) -0.0018(10) -0.0019(12) C18b C 0.0266(14) 0.0295(16) 0.0276(13) -0.0071(12) 0.0038(10) 0.0010(12) C19a C 0.049(2) 0.062(3) 0.0340(16) -0.0229(19) 0.0062(14) -0.0102(16) C19b C 0.0378(18) 0.056(2) 0.0322(15) 0.0116(17) 0.0000(12) -0.0031(15) C20a C 0.057(2) 0.073(3) 0.0305(16) -0.020(2) 0.0074(14) -0.0092(17) C20b C 0.0421(18) 0.056(2) 0.0348(15) 0.0056(18) 0.0049(13) -0.0107(16) C21a C 0.0432(18) 0.0365(18) 0.0292(14) 0.0057(15) -0.0022(11) -0.0042(13) C21b C 0.0386(17) 0.0373(18) 0.0305(14) -0.0119(15) 0.0021(12) -0.0024(13) C22a C 0.056(2) 0.053(3) 0.0402(17) -0.0184(19) -0.0129(15) -0.0022(17) C22b C 0.0415(18) 0.047(2) 0.0372(15) 0.0021(17) -0.0076(12) 0.0007(15) C23a C 0.053(2) 0.059(2) 0.0346(16) -0.0252(19) -0.0022(14) 0.0054(16) C23b C 0.0422(18) 0.0329(18) 0.0316(15) 0.0049(15) -0.0021(12) -0.0058(13) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1a C1a . . 1.446(5) ? O1a C2a . . 1.314(6) ? O1b C1b . . 1.447(5) ? O1b C2b . . 1.326(5) ? O2a C2a . . 1.183(5) ? O2b C2b . . 1.198(4) ? O3a C11a . . 1.227(3) ? O3b C11b . . 1.228(3) ? N1a C3a . . 1.454(3) ? N1a C11a . . 1.337(3) ? N1a H1n1a . . 0.92(3) ? N1b C3b . . 1.448(3) ? N1b C11b . . 1.331(4) ? N1b H1n1b . . 0.92(3) ? C1a H1c1a . . 0.96 ? C1a H2c1a . . 0.96 ? C1a H3c1a . . 0.96 ? C1b H1c1b . . 0.96 ? C1b H2c1b . . 0.96 ? C1b H3c1b . . 0.96 ? C2a C3a . . 1.523(5) ? C2b C3b . . 1.526(5) ? C3a C4a . . 1.534(6) ? C3a H1c3a . . 0.96 ? C3b C4b . . 1.547(5) ? C3b H1c3b . . 0.96 ? C4a C5a . . 1.509(5) ? C4a H1c4a . . 0.96 ? C4a H2c4a . . 0.96 ? C4b C5b . . 1.507(5) ? C4b H1c4b . . 0.96 ? C4b H2c4b . . 0.96 ? C5a C6a . . 1.387(4) ? C5a C10a . . 1.391(5) ? C5b C6b . . 1.400(4) ? C5b C10b . . 1.383(5) ? C6a C7a . . 1.387(5) ? C6a H1c6a . . 0.96 ? C6b C7b . . 1.376(5) ? C6b H1c6b . . 0.96 ? C7a C8a . . 1.373(5) ? C7a H1c7a . . 0.96 ? C7b C8b . . 1.379(5) ? C7b H1c7b . . 0.96 ? C8a C9a . . 1.380(5) ? C8a H1c8a . . 0.96 ? C8b C9b . . 1.386(5) ? C8b H1c8b . . 0.96 ? C9a C10a . . 1.387(5) ? C9a H1c9a . . 0.96 ? C9b C10b . . 1.400(5) ? C9b H1c9b . . 0.96 ? C10a H1c10a . . 0.96 ? C10b H1c10b . . 0.96 ? C11a C12a . . 1.500(4) ? C11b C12b . . 1.498(4) ? C12a C13a . . 1.372(5) ? C12a C17a . . 1.374(5) ? C12b C13b . . 1.374(5) ? C12b C17b . . 1.384(4) ? C13a C14a . . 1.386(4) ? C13a H1c13a . . 0.96 ? C13b C14b . . 1.391(4) ? C13b H1c13b . . 0.96 ? C14a C15a . . 1.381(5) ? C14a H1c14a . . 0.96 ? C14b C15b . . 1.385(5) ? C14b H1c14b . . 0.96 ? C15a C16a . . 1.381(5) ? C15a C18a . . 1.487(4) ? C15b C16b . . 1.374(5) ? C15b C18b . . 1.499(4) ? C16a C17a . . 1.388(4) ? C16a H1c16a . . 0.96 ? C16b C17b . . 1.393(4) ? C16b H1c16b . . 0.96 ? C17a H1c17a . . 0.96 ? C17b H1c17b . . 0.96 ? C18a C19a . . 1.386(5) ? C18a C23a . . 1.381(5) ? C18b C19b . . 1.397(5) ? C18b C23b . . 1.391(5) ? C19a C20a . . 1.387(5) ? C19a H1c19a . . 0.96 ? C19b C20b . . 1.380(4) ? C19b H1c19b . . 0.96 ? C20a C21a . . 1.362(6) ? C20a H1c20a . . 0.96 ? C20b C21b . . 1.379(5) ? C20b H1c20b . . 0.96 ? C21a C22a . . 1.361(5) ? C21a H1c21a . . 0.96 ? C21b C22b . . 1.372(6) ? C21b H1c21b . . 0.96 ? C22a C23a . . 1.394(5) ? C22a H1c22a . . 0.96 ? C22b C23b . . 1.385(4) ? C22b H1c22b . . 0.96 ? C23a H1c23a . . 0.96 ? C23b H1c23b . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1a O1a C2a . . . 115.9(3) ? C1b O1b C2b . . . 114.7(3) ? C3a N1a C11a . . . 122.3(2) ? C3a N1a H1n1a . . . 116.2(19) ? C11a N1a H1n1a . . . 120.6(19) ? C3b N1b C11b . . . 121.1(2) ? C3b N1b H1n1b . . . 118.5(19) ? C11b N1b H1n1b . . . 120.4(19) ? O1a C1a H1c1a . . . 109.47 ? O1a C1a H2c1a . . . 109.47 ? O1a C1a H3c1a . . . 109.47 ? H1c1a C1a H2c1a . . . 109.47 ? H1c1a C1a H3c1a . . . 109.47 ? H2c1a C1a H3c1a . . . 109.47 ? O1b C1b H1c1b . . . 109.47 ? O1b C1b H2c1b . . . 109.47 ? O1b C1b H3c1b . . . 109.47 ? H1c1b C1b H2c1b . . . 109.47 ? H1c1b C1b H3c1b . . . 109.47 ? H2c1b C1b H3c1b . . . 109.47 ? O1a C2a O2a . . . 123.2(4) ? O1a C2a C3a . . . 113.1(3) ? O2a C2a C3a . . . 123.6(4) ? O1b C2b O2b . . . 124.1(3) ? O1b C2b C3b . . . 112.4(2) ? O2b C2b C3b . . . 123.5(4) ? N1a C3a C2a . . . 111.2(3) ? N1a C3a C4a . . . 111.3(2) ? N1a C3a H1c3a . . . 107.52 ? C2a C3a C4a . . . 110.9(3) ? C2a C3a H1c3a . . . 107.97 ? C4a C3a H1c3a . . . 107.8 ? N1b C3b C2b . . . 112.6(3) ? N1b C3b C4b . . . 113.2(3) ? N1b C3b H1c3b . . . 104.4 ? C2b C3b C4b . . . 109.1(2) ? C2b C3b H1c3b . . . 108.93 ? C4b C3b H1c3b . . . 108.3 ? C3a C4a C5a . . . 113.1(3) ? C3a C4a H1c4a . . . 109.47 ? C3a C4a H2c4a . . . 109.47 ? C5a C4a H1c4a . . . 109.47 ? C5a C4a H2c4a . . . 109.47 ? H1c4a C4a H2c4a . . . 105.54 ? C3b C4b C5b . . . 114.5(2) ? C3b C4b H1c4b . . . 109.47 ? C3b C4b H2c4b . . . 109.47 ? C5b C4b H1c4b . . . 109.47 ? C5b C4b H2c4b . . . 109.47 ? H1c4b C4b H2c4b . . . 103.95 ? C4a C5a C6a . . . 120.2(3) ? C4a C5a C10a . . . 121.3(3) ? C6a C5a C10a . . . 118.5(3) ? C4b C5b C6b . . . 119.2(3) ? C4b C5b C10b . . . 122.1(3) ? C6b C5b C10b . . . 118.7(3) ? C5a C6a C7a . . . 120.4(3) ? C5a C6a H1c6a . . . 119.81 ? C7a C6a H1c6a . . . 119.81 ? C5b C6b C7b . . . 120.2(3) ? C5b C6b H1c6b . . . 119.89 ? C7b C6b H1c6b . . . 119.89 ? C6a C7a C8a . . . 120.8(3) ? C6a C7a H1c7a . . . 119.61 ? C8a C7a H1c7a . . . 119.61 ? C6b C7b C8b . . . 120.9(3) ? C6b C7b H1c7b . . . 119.54 ? C8b C7b H1c7b . . . 119.54 ? C7a C8a C9a . . . 119.4(4) ? C7a C8a H1c8a . . . 120.29 ? C9a C8a H1c8a . . . 120.29 ? C7b C8b C9b . . . 119.9(3) ? C7b C8b H1c8b . . . 120.06 ? C9b C8b H1c8b . . . 120.06 ? C8a C9a C10a . . . 120.2(4) ? C8a C9a H1c9a . . . 119.9 ? C10a C9a H1c9a . . . 119.9 ? C8b C9b C10b . . . 119.3(3) ? C8b C9b H1c9b . . . 120.37 ? C10b C9b H1c9b . . . 120.37 ? C5a C10a C9a . . . 120.7(3) ? C5a C10a H1c10a . . . 119.64 ? C9a C10a H1c10a . . . 119.64 ? C5b C10b C9b . . . 121.0(3) ? C5b C10b H1c10b . . . 119.51 ? C9b C10b H1c10b . . . 119.51 ? O3a C11a N1a . . . 122.9(3) ? O3a C11a C12a . . . 121.4(2) ? N1a C11a C12a . . . 115.7(2) ? O3b C11b N1b . . . 122.4(2) ? O3b C11b C12b . . . 121.1(2) ? N1b C11b C12b . . . 116.5(2) ? C11a C12a C13a . . . 118.1(3) ? C11a C12a C17a . . . 123.9(3) ? C13a C12a C17a . . . 118.0(3) ? C11b C12b C13b . . . 118.5(3) ? C11b C12b C17b . . . 123.5(3) ? C13b C12b C17b . . . 118.0(3) ? C12a C13a C14a . . . 120.7(4) ? C12a C13a H1c13a . . . 119.64 ? C14a C13a H1c13a . . . 119.64 ? C12b C13b C14b . . . 121.3(3) ? C12b C13b H1c13b . . . 119.37 ? C14b C13b H1c13b . . . 119.37 ? C13a C14a C15a . . . 122.0(3) ? C13a C14a H1c14a . . . 118.98 ? C15a C14a H1c14a . . . 118.98 ? C13b C14b C15b . . . 121.2(4) ? C13b C14b H1c14b . . . 119.41 ? C15b C14b H1c14b . . . 119.41 ? C14a C15a C16a . . . 116.6(3) ? C14a C15a C18a . . . 121.2(3) ? C16a C15a C18a . . . 122.2(3) ? C14b C15b C16b . . . 117.1(3) ? C14b C15b C18b . . . 121.1(3) ? C16b C15b C18b . . . 121.8(3) ? C15a C16a C17a . . . 121.5(4) ? C15a C16a H1c16a . . . 119.25 ? C17a C16a H1c16a . . . 119.24 ? C15b C16b C17b . . . 122.1(3) ? C15b C16b H1c16b . . . 118.93 ? C17b C16b H1c16b . . . 118.93 ? C12a C17a C16a . . . 121.1(3) ? C12a C17a H1c17a . . . 119.44 ? C16a C17a H1c17a . . . 119.45 ? C12b C17b C16b . . . 120.2(3) ? C12b C17b H1c17b . . . 119.88 ? C16b C17b H1c17b . . . 119.88 ? C15a C18a C19a . . . 121.3(3) ? C15a C18a C23a . . . 121.9(3) ? C19a C18a C23a . . . 116.7(3) ? C15b C18b C19b . . . 120.8(3) ? C15b C18b C23b . . . 121.7(3) ? C19b C18b C23b . . . 117.5(3) ? C18a C19a C20a . . . 121.1(4) ? C18a C19a H1c19a . . . 119.47 ? C20a C19a H1c19a . . . 119.47 ? C18b C19b C20b . . . 121.0(3) ? C18b C19b H1c19b . . . 119.48 ? C20b C19b H1c19b . . . 119.48 ? C19a C20a C21a . . . 121.3(4) ? C19a C20a H1c20a . . . 119.35 ? C21a C20a H1c20a . . . 119.35 ? C19b C20b C21b . . . 120.7(4) ? C19b C20b H1c20b . . . 119.67 ? C21b C20b H1c20b . . . 119.67 ? C20a C21a C22a . . . 118.7(3) ? C20a C21a H1c21a . . . 120.64 ? C22a C21a H1c21a . . . 120.64 ? C20b C21b C22b . . . 119.0(3) ? C20b C21b H1c21b . . . 120.52 ? C22b C21b H1c21b . . . 120.52 ? C21a C22a C23a . . . 120.6(4) ? C21a C22a H1c22a . . . 119.72 ? C23a C22a H1c22a . . . 119.72 ? C21b C22b C23b . . . 120.9(3) ? C21b C22b H1c22b . . . 119.53 ? C23b C22b H1c22b . . . 119.53 ? C18a C23a C22a . . . 121.6(3) ? C18a C23a H1c23a . . . 119.19 ? C22a C23a H1c23a . . . 119.19 ? C18b C23b C22b . . . 120.8(3) ? C18b C23b H1c23b . . . 119.58 ? C22b C23b H1c23b . . . 119.58 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1a C2a C3a N1a . . . . 36.2(3) ? O1b C2b C3b N1b . . . . 36.4(3) ? C2a C3a N1a C11a . . . . -130.1(3) ? C2b C3b N1b C11b . . . . 56.1(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C4a H1c4a O3a . . 1_455 0.96 2.77 3.459(4) 129.24 ? C10a H1c10a O2a . . 2_656 0.96 2.72 3.656(4) 163.61 ? C10b H1c10b O2b . . 2_745 0.96 2.78 3.688(4) 158.56 ? N1a H1n1a O3a . . 1_455 0.92(3) 2.00(3) 2.852(3) 154(3) ? N1b H1n1b O3b . . 1_655 0.92(3) 2.00(3) 2.876(3) 157(3) ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_include_status 2 0 0 2645.57 2186.22 70.37 o 3 0 0 69.78 76.57 7.28 o 4 0 0 51.94 72.70 8.60 o 5 0 0 57.36 53.68 7.24 o 1 1 0 6242.81 5820.08 73.76 o 2 -1 0 346.67 287.40 25.43 o 3 1 0 294.85 344.34 15.93 o 3 -1 0 296.60 322.67 15.25 o 4 1 0 114.64 129.24 11.37 o 4 -1 0 114.91 126.15 11.50 o 5 1 0 14.96 12.37 2.54 o 5 -1 0 15.09 12.80 4.20 o 0 2 0 1716.45 1718.64 38.16 o 1 2 0 6907.50 6614.98 65.93 o 2 2 0 30.01 43.83 11.05 o 3 2 0 73.61 68.58 7.17 o 3 -2 0 72.63 74.94 7.67 o 4 2 0 111.58 123.41 11.10 o 5 -2 0 48.21 52.56 7.67 o 1 3 0 398.92 378.59 26.52 o 2 3 0 318.50 323.31 30.94 o 2 -3 0 314.39 329.57 13.70 o 3 3 0 296.72 297.92 15.24 o 3 -3 0 296.18 293.44 15.38 o 4 -3 0 918.58 986.05 33.00 o 5 -3 0 21.93 42.98 7.19 o 0 4 0 57.88 56.46 10.86 o 1 4 0 89.05 95.22 15.36 o 1 -4 0 89.19 89.62 6.69 o 2 -4 0 1531.40 1482.64 31.74 o 3 4 0 207.21 193.57 13.36 o 4 4 0 191.93 204.71 13.26 o 4 -4 0 192.62 199.57 15.08 o 5 -4 0 16.92 20.84 4.25 o 1 -5 0 180.19 205.90 11.72 o 2 5 0 261.16 226.65 14.46 o 3 5 0 214.84 227.76 16.01 o 4 5 0 253.67 272.49 11.29 o 4 -5 0 253.58 267.77 16.56 o 5 -5 0 12.81 12.01 3.41 o 0 -6 0 855.06 898.89 26.73 o 1 -6 0 80.06 88.68 6.11 o 2 6 0 23.85 24.16 5.93 o 3 6 0 209.56 208.44 10.39 o 4 6 0 21.94 32.22 5.66 o 1 -7 0 473.02 488.26 22.02 o 2 7 0 708.07 740.31 16.51 o 2 -7 0 707.90 728.13 27.80 o 3 7 0 5.55 18.27 6.20 < 4 7 0 42.13 69.75 7.69 o 0 8 0 215.41 218.81 15.75 o 1 8 0 142.31 116.37 11.91 o 2 8 0 91.95 73.95 9.04 o 3 8 0 15.51 23.06 5.91 o 1 9 0 239.00 243.94 15.48 o 2 9 0 29.59 39.46 8.23 o 0 10 0 33.66 36.09 5.07 o 0 -10 0 33.16 37.26 4.74 o 1 10 0 100.55 69.16 6.93 o -5 0 1 1.59 0.19 1.59 < -4 0 1 3.73 3.37 1.70 < -3 0 1 130.22 129.24 9.66 o -2 0 1 29.06 12.37 7.79 < -1 0 1 4931.66 4903.43 53.45 o 1 0 1 15024.50 16385.30 130.57 o 2 0 1 480.29 494.00 32.61 o 3 0 1 292.42 314.98 14.93 o 4 0 1 3.85 2.38 1.30 < 5 0 1 17.75 19.26 4.38 o -5 1 1 71.28 78.57 6.36 o -5 -1 1 71.33 72.73 8.73 o -4 1 1 247.35 236.11 15.15 o -4 -1 1 248.45 267.26 16.46 o -3 1 1 20.91 27.25 4.78 o -3 -1 1 21.18 23.97 4.18 o -2 -1 1 128.93 198.96 22.21 o -1 1 1 9122.69 9054.49 95.45 o 0 1 1 1514.84 1405.84 22.74 o 1 1 1 8693.59 8688.91 89.53 o 2 -1 1 1083.22 1044.79 48.24 o 3 1 1 79.57 76.94 7.39 o 3 -1 1 77.86 79.88 7.61 o 4 1 1 132.69 140.31 11.91 o 5 1 1 10.74 9.88 4.06 < 5 -1 1 10.64 12.80 3.66 o -5 2 1 51.18 55.52 7.67 o -5 -2 1 50.98 56.11 7.73 o -4 2 1 332.28 293.57 16.86 o -4 -2 1 332.35 325.12 18.27 o -3 2 1 866.82 769.75 23.01 o -3 -2 1 868.72 793.91 24.65 o -2 2 1 1058.65 1106.06 46.80 o -1 2 1 5004.28 4810.34 56.40 o 0 2 1 14115.90 14277.60 82.83 o 1 2 1 5662.51 5350.22 58.47 o 2 2 1 163.26 169.71 22.23 o 3 2 1 201.16 186.54 11.93 o 3 -2 1 200.37 191.60 11.91 o 4 2 1 17.16 21.41 5.61 o 5 -2 1 56.87 57.01 7.68 o -5 -3 1 359.78 339.22 18.04 o -4 -3 1 90.15 107.93 11.59 o -3 3 1 273.45 281.55 14.96 o -3 -3 1 274.86 280.63 15.16 o -2 3 1 17.11 4.02 5.57 < -2 -3 1 16.85 12.88 3.66 o -1 3 1 198.88 197.76 19.55 o 0 3 1 3.61 6.12 2.20 < 1 3 1 853.72 811.26 39.11 o 2 3 1 591.77 554.93 40.49 o 2 -3 1 591.43 563.90 17.55 o 3 3 1 33.84 40.19 5.85 o 4 -3 1 162.38 199.36 14.87 o 5 -3 1 73.59 91.64 9.79 o -5 -4 1 35.47 35.49 5.50 o -4 4 1 372.33 385.11 17.97 o -4 -4 1 373.74 373.16 20.55 o -3 4 1 153.58 170.71 12.75 o -2 -4 1 137.43 127.25 9.75 o -1 4 1 890.64 894.91 45.40 o -1 -4 1 891.28 922.08 21.54 o 0 4 1 4474.93 4671.00 67.10 o 1 4 1 111.35 146.89 19.53 o 1 -4 1 109.95 164.52 9.08 o 2 -4 1 920.88 817.11 23.48 o 3 4 1 15.70 12.46 3.51 o 4 4 1 567.19 603.55 22.54 o 4 -4 1 564.41 559.54 24.73 o 5 -4 1 18.63 17.84 3.80 o -5 -5 1 21.24 18.39 3.53 o -4 5 1 33.61 38.51 6.10 o -4 -5 1 33.34 30.71 6.13 o -3 5 1 51.43 48.88 7.20 o -2 -5 1 106.53 107.86 9.32 o -1 -5 1 95.56 96.69 7.97 o 0 -5 1 80.35 76.36 4.88 o 1 5 1 40.33 40.95 5.53 o 1 -5 1 39.09 34.50 4.95 o 2 5 1 64.50 54.39 7.08 o 3 5 1 138.72 138.44 13.31 o 4 5 1 161.03 169.76 11.98 o 4 -5 1 159.95 166.34 12.98 o 5 -5 1 66.62 80.31 7.11 o -4 6 1 2.92 4.25 1.92 < -4 -6 1 3.01 6.07 3.03 < -3 6 1 19.70 134.79 9.46 o -2 6 1 73.30 71.94 8.99 o -1 -6 1 73.72 72.53 5.67 o 0 -6 1 217.70 220.35 9.32 o 1 -6 1 193.14 216.88 13.60 o 2 6 1 97.97 85.16 9.28 o 3 6 1 193.60 233.32 11.07 o 4 6 1 30.66 27.95 5.45 o -4 7 1 137.40 147.79 10.97 o -3 7 1 46.24 49.10 7.29 o -2 7 1 145.99 127.26 7.18 o -2 -7 1 145.49 144.60 8.76 o -1 -7 1 112.41 116.73 10.79 o 0 -7 1 371.83 405.80 13.95 o 1 -7 1 219.16 209.45 14.76 o 2 7 1 85.61 85.33 5.88 o 2 -7 1 86.36 87.74 9.89 o 3 7 1 46.07 39.00 7.26 o 4 7 1 145.98 162.31 11.11 o 4 -7 1 146.10 137.28 9.35 o -3 8 1 78.55 62.95 7.97 o -2 8 1 30.18 62.75 8.66 o -1 8 1 264.47 266.17 17.42 o 0 8 1 295.82 340.32 14.38 o 1 8 1 181.50 186.41 14.48 o 2 8 1 15.25 21.82 4.99 o 3 8 1 29.99 29.13 4.88 o -2 9 1 67.64 79.87 8.23 o -1 9 1 18.00 33.37 7.36 o -1 -9 1 17.47 12.17 3.36 o 0 9 1 37.42 38.47 4.38 o 1 9 1 1.82 41.31 6.54 o 2 9 1 84.58 88.29 8.97 o -1 10 1 8.76 6.83 3.16 < 0 10 1 41.20 35.48 3.59 o 0 -10 1 39.82 50.10 5.47 o 1 10 1 4.97 30.49 4.73 o -5 0 2 1.41 2.84 1.54 < -4 0 2 8.41 15.22 3.52 o -3 0 2 355.10 416.35 17.46 o -2 0 2 68.28 65.68 14.95 o -1 0 2 1178.68 1084.66 18.21 o 0 0 2 0.04 0.99 0.27 o 1 0 2 2046.24 1763.83 42.21 o 2 0 2 2133.34 1886.09 63.55 o 3 0 2 344.96 370.43 16.12 o 4 0 2 117.52 129.56 11.29 o 5 0 2 26.06 25.07 4.80 o -5 1 2 129.35 139.33 8.35 o -5 -1 2 129.23 145.40 8.55 o -4 1 2 174.04 159.74 12.63 o -4 -1 2 174.15 157.30 13.03 o -3 1 2 99.40 112.24 9.32 o -3 -1 2 99.46 97.33 8.37 o -2 1 2 2056.57 1963.78 67.69 o -2 -1 2 2055.16 1942.20 66.99 o -1 1 2 455.15 412.47 19.98 o 0 1 2 485.53 465.36 11.96 o 1 1 2 1574.17 1445.90 26.68 o 2 -1 2 248.67 253.04 24.53 o 3 -1 2 98.16 90.47 8.16 o 4 1 2 492.48 485.95 21.86 o 4 -1 2 490.45 465.27 21.31 o 5 1 2 65.80 70.97 8.74 o 5 -1 2 66.09 84.11 9.61 o -5 2 2 67.79 77.67 8.42 o -5 -2 2 68.68 75.07 8.95 o -4 2 2 344.16 295.70 16.73 o -4 -2 2 344.08 317.77 18.24 o -3 -2 2 1.76 5.44 2.23 < -2 2 2 550.68 531.70 32.69 o -1 2 2 10121.20 10280.50 85.30 o 0 2 2 8360.75 8400.37 61.82 o 1 2 2 11518.30 11650.50 87.23 o 2 2 2 206.03 216.79 23.66 o 2 -2 2 207.23 215.98 22.92 o 3 2 2 17.90 10.90 3.07 o 4 2 2 17.90 21.92 5.62 o 4 -2 2 18.07 17.24 4.47 o 5 -2 2 173.36 197.78 14.16 o -5 -3 2 639.82 619.91 24.43 o -4 -3 2 673.64 686.66 27.63 o -3 -3 2 177.35 183.16 12.42 o -2 3 2 841.81 834.28 49.84 o -2 -3 2 840.40 780.17 21.44 o -1 3 2 2112.73 2047.12 40.38 o 0 3 2 2702.46 2730.65 42.35 o 1 3 2 1862.85 1858.27 60.31 o 2 -3 2 1316.69 1247.80 25.91 o 3 3 2 208.40 215.37 13.21 o 4 3 2 138.04 123.79 10.13 o 4 -3 2 138.52 140.57 12.67 o 5 -3 2 44.56 34.28 6.21 o -5 -4 2 23.02 26.83 4.86 o -4 -4 2 29.16 34.55 7.23 o -3 4 2 428.58 412.38 19.99 o -3 -4 2 427.85 409.54 19.52 o -2 -4 2 460.88 464.36 18.05 o -1 4 2 327.45 338.86 28.02 o -1 -4 2 326.90 341.16 13.31 o 0 4 2 6.54 8.83 5.64 < 0 -4 2 6.40 12.99 2.75 o 1 4 2 902.89 1078.87 51.32 o 1 -4 2 899.89 962.62 21.58 o 2 4 2 700.53 688.50 22.67 o 3 4 2 122.18 137.44 11.51 o 4 4 2 198.58 210.46 13.36 o 4 -4 2 198.37 208.62 14.90 o 5 -4 2 22.04 24.98 4.75 o -5 -5 2 0.16 4.53 2.22 < -4 5 2 51.73 61.35 5.44 o -4 -5 2 51.76 53.69 7.66 o -3 5 2 44.06 64.13 9.74 o -2 -5 2 24.57 19.58 4.22 o -1 -5 2 172.71 191.50 11.33 o 0 -5 2 1762.66 1814.95 23.45 o 1 5 2 140.95 144.67 10.05 o 2 5 2 27.68 20.43 4.35 o 3 5 2 1063.65 1054.08 33.84 o 4 5 2 51.22 59.06 5.39 o 4 -5 2 52.05 67.10 8.37 o 5 -5 2 5.42 8.13 2.67 o -4 6 2 5.39 12.45 3.78 o -4 -6 2 5.44 2.29 1.98 < -3 6 2 453.10 454.29 15.32 o -3 -6 2 451.24 463.32 22.09 o -2 6 2 136.01 108.77 10.77 o -2 -6 2 135.98 120.91 11.38 o -1 -6 2 462.36 477.02 14.26 o 0 -6 2 115.65 102.83 6.38 o 1 6 2 248.96 261.40 15.16 o 1 -6 2 248.17 255.19 15.01 o 2 6 2 408.79 362.03 19.51 o 3 6 2 80.48 111.96 7.96 o 4 6 2 219.79 222.86 9.67 o -4 7 2 25.03 29.08 5.94 o -3 7 2 11.91 20.33 5.05 o -2 7 2 231.94 245.87 9.69 o -2 -7 2 230.80 229.18 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9.58 o 1 -2 38 180.45 180.96 9.23 o 2 2 38 44.87 44.72 3.48 o 2 -2 38 44.78 47.24 4.60 o 3 2 38 8.50 4.79 1.87 < 3 -2 38 8.32 5.88 2.10 < -3 3 38 68.56 76.71 4.78 o -2 3 38 4.58 9.06 2.17 o -1 3 38 23.77 23.58 3.61 o 0 3 38 125.59 120.47 11.16 o 0 -3 38 124.93 123.78 10.70 o 1 3 38 70.95 55.48 7.79 o 1 -3 38 70.75 59.15 7.27 o 2 3 38 43.81 45.95 5.56 o 2 -3 38 43.74 44.87 6.03 o 3 3 38 81.77 99.48 7.32 o 3 -3 38 82.09 107.07 7.87 o -3 4 38 4.35 4.83 1.90 < -2 4 38 40.10 39.56 3.72 o -1 4 38 34.00 32.38 4.96 o -1 -4 38 34.09 36.93 5.55 o 0 4 38 43.60 47.75 6.10 o 0 -4 38 43.12 48.48 6.51 o 1 4 38 29.67 24.51 5.06 o 1 -4 38 29.37 30.69 5.34 o 2 4 38 26.90 29.96 4.28 o 2 -4 38 26.85 31.96 4.72 o -2 5 38 0.95 1.19 0.79 < -1 5 38 19.08 18.62 3.81 o -1 -5 38 19.79 18.45 3.79 o 0 5 38 88.04 83.46 7.72 o 0 -5 38 89.61 87.45 8.32 o 1 5 38 5.53 7.29 2.31 o 1 -5 38 5.33 2.84 1.89 < 2 -5 38 35.02 35.98 4.43 o -1 6 38 114.78 106.90 5.33 o -1 -6 38 115.90 102.26 7.67 o 0 6 38 6.44 10.42 2.66 o 0 -6 38 6.16 8.53 2.24 o 1 6 38 3.30 1.63 0.35 o 1 -6 38 3.27 3.57 1.45 < -3 0 39 67.00 65.80 7.28 o -2 0 39 256.08 255.94 15.70 o -1 0 39 0.86 0.80 2.09 < 0 0 39 184.92 169.73 13.64 o 1 0 39 19.19 12.16 2.37 o 2 0 39 76.88 67.01 5.65 o 3 0 39 1.71 0.63 0.98 < -3 1 39 64.08 76.40 7.88 o -3 -1 39 64.85 70.22 7.12 o -2 1 39 55.73 46.17 6.60 o -2 -1 39 55.80 54.80 7.08 o -1 1 39 98.49 102.32 10.91 o 0 1 39 153.69 133.73 12.21 o 1 1 39 803.78 782.37 20.15 o 1 -1 39 802.12 773.91 19.34 o 2 1 39 7.11 4.61 1.48 o 2 -1 39 7.17 5.92 1.94 o 3 1 39 32.31 37.51 4.75 o 3 -1 39 32.08 30.02 4.43 o -3 2 39 50.93 61.35 4.62 o -2 2 39 91.54 88.73 6.22 o -1 2 39 43.21 55.77 7.99 o 0 2 39 389.49 409.48 21.18 o 1 2 39 90.75 79.66 6.29 o 1 -2 39 90.86 79.47 6.04 o 2 2 39 113.68 115.19 6.54 o 2 -2 39 112.68 122.50 7.25 o 3 2 39 91.82 98.32 7.38 o 3 -2 39 90.94 95.75 7.85 o -3 3 39 98.91 114.07 5.56 o -2 3 39 74.52 83.30 5.78 o -1 3 39 141.57 126.99 7.48 o 0 3 39 34.82 26.91 5.49 o 0 -3 39 35.01 23.03 4.84 o 1 3 39 61.05 57.37 7.66 o 1 -3 39 60.03 58.83 7.48 o 2 3 39 29.38 30.43 4.65 o 2 -3 39 28.78 28.32 4.74 o 3 3 39 66.31 72.02 5.97 o 3 -3 39 65.92 65.69 5.96 o -2 4 39 31.65 38.39 5.02 o -1 4 39 1.25 -0.42 1.10 < -1 -4 39 1.08 1.14 0.10 o 0 4 39 34.24 33.69 5.04 o 0 -4 39 33.98 38.04 5.63 o 1 4 39 0.91 2.46 1.37 < 1 -4 39 0.85 0.21 1.39 < 2 -4 39 16.96 15.30 3.33 o -2 5 39 65.08 68.32 4.28 o -1 5 39 66.03 62.39 6.52 o -1 -5 39 65.84 64.44 6.68 o 0 5 39 50.58 49.20 5.76 o 0 -5 39 50.12 52.13 6.45 o 1 5 39 39.71 46.16 5.10 o 1 -5 39 39.55 41.29 5.31 o 2 -5 39 25.21 25.97 3.63 o -1 6 39 62.35 61.17 5.68 o -1 -6 39 62.22 55.57 5.39 o 0 6 39 71.22 80.77 6.56 o 0 -6 39 70.56 70.96 6.57 o -3 0 40 5.33 10.58 2.82 o -2 0 40 36.16 28.88 5.20 o -1 0 40 227.60 217.73 15.11 o 0 0 40 227.13 214.23 15.23 o 1 0 40 461.22 476.10 15.55 o 2 0 40 7.70 8.14 2.03 o 3 0 40 74.00 83.57 5.02 o -3 1 40 15.72 16.19 3.38 o -3 -1 40 15.67 15.64 3.26 o -2 1 40 73.91 76.90 8.57 o -2 -1 40 74.31 73.85 8.03 o -1 1 40 48.66 46.93 7.14 o 0 1 40 74.55 69.26 8.62 o 1 1 40 125.37 111.76 7.60 o 1 -1 40 125.43 124.52 7.66 o 2 1 40 14.17 11.78 2.15 o 2 -1 40 13.63 10.84 2.19 o 3 1 40 87.47 85.93 6.86 o 3 -1 40 87.29 90.09 7.68 o -3 2 40 24.11 28.23 4.27 o -2 2 40 95.85 102.10 9.51 o -1 2 40 13.71 21.45 5.13 o 0 2 40 60.39 59.65 7.82 o 1 2 40 36.14 32.22 4.06 o 1 -2 40 36.64 35.69 3.98 o 2 2 40 73.76 75.68 6.97 o 2 -2 40 73.89 60.55 7.14 o 3 2 40 60.14 71.62 5.97 o 3 -2 40 60.59 67.42 6.29 o -3 3 40 51.25 58.84 5.50 o -2 3 40 87.11 93.83 5.95 o -1 3 40 37.96 35.46 4.01 o 0 3 40 1.44 2.10 1.25 < 0 -3 40 1.45 -0.09 0.32 < 1 3 40 199.04 208.76 14.36 o 1 -3 40 201.33 215.13 13.61 o 2 3 40 19.33 16.36 3.21 o 2 -3 40 19.03 22.66 4.27 o -2 4 40 10.22 11.07 2.67 o -1 4 40 36.67 33.37 4.96 o 0 4 40 11.95 14.19 3.12 o 0 -4 40 12.25 9.97 2.35 o 1 4 40 9.43 12.54 3.49 o 1 -4 40 9.19 5.44 1.94 < 2 -4 40 8.04 10.59 2.42 o -2 5 40 27.53 30.06 3.90 o -1 5 40 26.46 20.03 3.51 o -1 -5 40 25.97 24.61 3.94 o 0 5 40 40.55 38.89 5.12 o 0 -5 40 40.41 42.55 5.45 o 1 5 40 30.81 20.66 3.25 o 1 -5 40 30.90 21.80 3.98 o 0 6 40 40.13 48.02 4.78 o 0 -6 40 39.61 41.56 4.74 o -3 0 41 8.29 5.79 1.71 o -2 0 41 32.93 32.79 5.40 o -1 0 41 566.09 596.59 24.51 o 0 0 41 29.76 24.82 5.47 o 1 0 41 14.03 24.22 4.30 o 2 0 41 123.20 112.41 6.86 o 3 0 41 1.18 1.56 0.90 < -3 1 41 30.87 29.91 4.30 o -3 -1 41 31.20 32.88 4.64 o -2 1 41 72.31 69.16 7.99 o -2 -1 41 71.95 69.88 7.79 o -1 1 41 131.85 150.83 12.54 o 0 1 41 23.11 28.05 5.48 o 1 1 41 187.40 199.82 10.05 o 1 -1 41 188.35 199.68 9.57 o 2 1 41 132.58 134.90 7.30 o 2 -1 41 133.29 133.72 7.43 o 3 1 41 31.54 29.00 3.73 o 3 -1 41 31.53 37.43 4.56 o -3 2 41 60.59 69.00 6.66 o -2 2 41 32.15 29.68 4.94 o -1 2 41 53.85 49.27 6.87 o 0 2 41 13.11 15.31 4.97 o 1 2 41 9.99 9.80 2.12 o 1 -2 41 10.34 10.08 2.07 o 2 -2 41 86.13 86.81 8.15 o 3 2 41 12.66 12.82 2.41 o 3 -2 41 13.36 11.86 2.68 o -2 3 41 12.12 12.05 2.07 o -1 3 41 55.15 54.98 7.51 o 0 3 41 1.16 0.26 1.51 < 0 -3 41 1.14 -0.40 1.45 < 1 3 41 25.25 26.80 5.19 o 1 -3 41 25.40 30.97 5.13 o 2 3 41 30.98 33.47 4.28 o 2 -3 41 30.55 33.02 4.67 o -2 4 41 35.91 42.98 5.10 o -1 4 41 5.62 8.09 2.24 o 0 4 41 20.59 20.56 3.55 o 0 -4 41 20.32 21.00 4.30 o 1 4 41 32.57 35.07 5.41 o 1 -4 41 32.34 34.51 4.86 o 2 -4 41 30.48 29.00 4.06 o -1 5 41 78.42 86.42 7.09 o -1 -5 41 77.95 87.29 7.03 o 0 5 41 66.87 74.30 6.61 o 0 -5 41 66.55 68.71 6.73 o 1 5 41 81.34 85.62 6.49 o 1 -5 41 81.72 80.02 7.00 o -3 0 42 37.66 42.35 5.09 o -2 0 42 44.66 40.59 5.83 o -1 0 42 103.17 106.29 10.32 o 0 0 42 0.08 -1.33 1.55 < 1 0 42 42.49 39.60 4.46 o 2 0 42 26.96 21.36 2.95 o -3 1 42 5.05 1.98 0.88 < -3 -1 42 5.08 4.24 1.53 < -2 1 42 16.01 22.40 4.53 o -2 -1 42 15.99 13.99 3.20 o -1 1 42 6.00 7.30 3.31 < 0 1 42 269.31 257.03 16.42 o 1 1 42 159.58 173.24 9.16 o 1 -1 42 159.29 161.86 8.42 o 2 1 42 16.15 19.76 3.62 o 2 -1 42 16.16 18.07 3.94 o 3 -1 42 20.22 19.80 3.09 o -2 2 42 2.82 6.94 3.47 < -1 2 42 117.44 108.13 10.17 o 0 2 42 2.40 4.56 1.63 < 0 -2 42 2.36 0.40 0.80 < 1 2 42 7.56 9.41 2.22 o 1 -2 42 7.63 8.50 2.03 o 2 -2 42 62.35 58.33 6.65 o -2 3 42 22.57 23.95 2.82 o -1 3 42 35.96 33.69 5.30 o 0 3 42 14.53 16.32 4.00 o 0 -3 42 14.81 19.47 4.19 o 1 3 42 8.39 8.93 3.35 < 1 -3 42 8.10 10.22 3.28 o 2 3 42 25.62 24.58 3.62 o 2 -3 42 25.58 26.96 4.19 o -2 4 42 32.68 30.38 4.07 o -1 4 42 33.04 34.82 4.76 o 0 -4 42 19.79 20.79 3.95 o 1 4 42 5.02 4.61 1.79 < 1 -4 42 5.13 6.75 2.71 < 2 -4 42 38.28 53.71 5.26 o -1 5 42 7.75 5.77 1.81 o 0 5 42 19.96 19.01 3.15 o 0 -5 42 19.60 21.77 3.67 o 1 -5 42 15.86 17.29 3.20 o -2 0 43 13.43 11.06 2.91 o -1 0 43 8.07 3.65 2.18 < 0 0 43 42.66 48.27 7.07 o 1 0 43 1.56 1.42 0.96 < 2 0 43 15.88 21.31 4.00 o -2 1 43 22.28 19.61 4.00 o -2 -1 43 22.32 23.29 4.02 o -1 1 43 22.55 25.31 5.05 o 0 1 43 52.47 53.08 7.13 o 1 1 43 1.96 2.72 1.41 < 1 -1 43 1.88 1.73 1.43 < 2 1 43 40.13 36.20 4.89 o 2 -1 43 40.05 45.90 5.66 o -2 2 43 145.79 161.05 11.11 o -1 2 43 51.05 58.51 7.58 o 0 2 43 38.93 43.60 4.37 o 0 -2 43 39.29 36.95 5.53 o 1 2 43 117.03 109.13 6.83 o 1 -2 43 117.19 110.77 6.56 o 2 -2 43 26.68 27.98 4.40 o -2 3 43 19.10 21.41 2.63 o -1 3 43 56.89 66.54 7.39 o 0 3 43 3.59 2.11 0.92 < 0 -3 43 3.52 5.85 2.90 < 1 3 43 36.26 35.17 5.59 o 1 -3 43 36.08 38.42 5.48 o 2 -3 43 2.52 4.66 2.06 < -1 4 43 1.68 1.81 0.44 o 0 -4 43 14.22 11.25 2.65 o 1 -4 43 11.67 12.33 2.60 o 0 -5 43 2.56 3.25 1.72 < -2 0 44 0.73 -0.08 0.27 < -1 0 44 3.87 8.80 2.76 o 0 0 44 3.72 4.06 0.92 o 1 0 44 129.19 114.50 7.17 o 2 0 44 2.19 2.45 1.55 < -2 1 44 31.38 39.89 5.58 o -2 -1 44 31.41 34.85 4.84 o -1 1 44 61.14 72.62 8.22 o 0 1 44 3.18 4.76 2.13 < 0 -1 44 3.10 5.84 2.71 < 1 1 44 107.36 108.73 6.98 o 1 -1 44 107.64 109.32 6.57 o 2 1 44 6.62 4.66 1.75 < 2 -1 44 6.67 4.94 1.89 < -2 2 44 111.50 124.68 9.53 o -1 2 44 114.49 130.01 10.94 o 0 2 44 12.96 18.25 2.88 o 0 -2 44 12.55 18.68 4.07 o 1 2 44 5.33 5.08 1.81 < 1 -2 44 5.24 6.60 1.60 o 2 -2 44 11.78 13.24 2.87 o -2 3 44 33.75 41.68 4.90 o -1 3 44 68.37 76.84 7.85 o 0 3 44 1.96 2.46 2.23 < 0 -3 44 1.94 0.81 1.16 < 1 3 44 10.84 14.35 3.62 o 1 -3 44 10.71 9.64 2.82 o 2 -3 44 148.52 174.54 9.66 o -1 4 44 4.52 3.21 0.62 o 0 -4 44 14.88 15.00 2.98 o 1 -4 44 13.53 14.20 2.85 o -2 0 45 36.94 27.05 4.54 o -1 0 45 0.16 -0.67 1.26 < 0 0 45 46.38 41.67 4.35 o 1 0 45 4.94 3.77 0.94 o 2 0 45 70.59 49.24 5.35 o -2 1 45 95.19 99.35 8.64 o -1 1 45 15.65 19.08 4.18 o 0 1 45 21.36 23.19 3.41 o 0 -1 45 21.37 18.40 4.18 o 1 1 45 10.18 14.85 2.51 o 1 -1 45 10.07 15.63 2.27 o 2 -1 45 95.65 102.85 7.87 o -2 2 45 19.27 22.93 4.21 o -1 2 45 23.37 24.84 4.60 o 0 2 45 4.88 5.08 1.44 o 0 -2 45 4.70 5.38 2.06 < 1 2 45 25.78 27.74 3.17 o 1 -2 45 25.89 27.06 3.11 o 2 -2 45 1.37 3.42 1.32 < -1 3 45 2.47 2.77 1.90 < 0 3 45 49.46 41.09 5.71 o 0 -3 45 49.23 46.52 5.46 o 1 3 45 38.60 33.75 4.92 o 1 -3 45 38.35 40.43 5.00 o 0 -4 45 18.34 26.30 3.77 o -2 0 46 10.20 12.50 2.73 o -1 0 46 41.96 42.04 5.78 o 0 0 46 7.75 5.51 1.42 o 1 0 46 24.62 18.77 2.58 o 2 0 46 0.60 2.13 1.05 < -2 1 46 10.47 7.33 1.97 o -1 1 46 4.61 5.25 2.87 < 0 1 46 34.68 37.43 3.86 o 0 -1 46 34.50 43.68 5.75 o 1 1 46 43.96 42.13 3.97 o 1 -1 46 44.22 47.55 5.79 o 2 -1 46 40.59 62.81 5.86 o -1 2 46 19.51 18.05 3.51 o 0 2 46 23.02 25.17 3.06 o 0 -2 46 22.76 20.94 3.53 o 1 2 46 12.56 12.42 1.96 o 1 -2 46 12.37 10.60 1.78 o -1 3 46 22.74 23.98 3.94 o 0 3 46 34.00 36.10 5.02 o 1 -3 46 5.19 7.25 2.13 o -1 0 47 2.39 4.13 1.88 < 0 0 47 24.50 24.61 3.03 o 1 0 47 1.34 1.55 0.77 < -1 1 47 39.89 36.79 5.33 o 0 1 47 140.96 151.40 7.59 o 0 -1 47 141.27 157.12 10.57 o 1 1 47 39.14 38.72 3.60 o 1 -1 47 39.35 40.44 5.04 o -1 2 47 57.31 64.24 4.51 o -1 -2 47 57.63 65.22 6.16 o 0 2 47 7.44 7.45 1.66 o 0 -2 47 7.67 8.85 2.31 o 1 2 47 12.35 9.49 1.67 o 1 -2 47 12.11 7.41 1.49 o 0 3 47 34.02 34.14 4.67 o -1 0 48 30.25 33.20 4.52 o 0 0 48 2.41 5.33 1.59 o 1 0 48 61.68 61.90 4.32 o -1 1 48 5.70 8.17 2.58 o -1 -1 48 5.34 8.37 2.50 o 0 1 48 16.95 17.39 2.52 o 0 -1 48 17.08 14.32 2.98 o 1 1 48 8.35 9.25 1.54 o 1 -1 48 8.48 8.49 2.00 o -1 2 48 43.51 57.46 6.15 o 0 2 48 14.32 19.04 2.46 o 0 -2 48 14.79 18.72 3.31 o -1 0 49 3.39 1.09 1.02 < 0 0 49 32.12 36.35 3.33 o 0 1 49 132.15 142.86 6.54 o 0 -1 49 131.92 145.76 9.07 o #======================================================================= data_I_phaseII #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C23 H21 N1 O3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C23 H21 N1 O3' _chemical_formula_weight 359.4 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'B21' _space_group_name_Hall ? _space_group_IT_number 4 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y+1/2,-z+1/2 3 x+1/2,y,z+1/2 4 -x+1/2,y+1/2,-z _cell_length_a 10.0754(2) _cell_length_b 8.5898(3) _cell_length_c 84.0864(14) _cell_angle_alpha 90 _cell_angle_beta 90.884(3) _cell_angle_gamma 90 _cell_volume 7276.4(3) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.97583 1 0 0 0 1 0 0 0 1 2 0.02417 1 0 0 0 -1 0 0 0 -1 _cell_formula_units_Z 16 _cell_measurement_reflns_used 3948 _cell_measurement_theta_min 4.19 _cell_measurement_theta_max 65.68 _cell_measurement_temperature 99.97 _cell_special_details ? _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.3124 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 0.696 _exptl_crystal_description 'rectrangular' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_colour colorless _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.966 _exptl_absorpt_correction_T_max 1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 99.97 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Cu K\a' #_diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 7.9580 _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 13838 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 65.79 _diffrn_reflns_theta_full 65.45 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_unetI/netI 0.0414 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -87 _diffrn_reflns_limit_l_max 98 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; The superstructure model was derived from the commensurately modulated structure model using JANA2006. The scale factor has been refined with a damping factor of 1. ; _reflns_number_total 8898 _reflns_number_gt 5940 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_gt 0.0483 _refine_ls_R_factor_all 0.0642 _refine_ls_wR_factor_ref 0.0526 _refine_ls_goodness_of_fit_ref 1.35 _refine_ls_goodness_of_fit_gt 1.51 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 8898 _refine_ls_number_parameters 1 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1309 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 0.22 _refine_diff_density_min -0.21 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 1998.78 _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ; 2293 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0492 0.0322 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group O1a-1 O 0.163487 0.052529 0.228295 Uani 0.0324 4 1 d . . . O1a-2 O 0.664614 0.064725 0.227747 Uani 0.0324 4 1 d . . . O1b-1 O 0.430515 0.577937 0.021036 Uani 0.0246 4 1 d . . . O1b-2 O 0.929536 0.575363 0.021203 Uani 0.0246 4 1 d . . . O2a-1 O 0.084228 0.246474 0.242814 Uani 0.0528 4 1 d . . . O2a-2 O 0.587399 0.26123 0.24216 Uani 0.0528 4 1 d . . . O2b-1 O 0.331843 0.390845 0.006598 Uani 0.0356 4 1 d . . . O2b-2 O 0.827385 0.387425 0.007195 Uani 0.0356 4 1 d . . . O3a-1 O 0.43166 0.274224 0.199869 Uani 0.0268 4 1 d . . . O3a-2 O 0.932486 0.25823 0.19935 Uani 0.0268 4 1 d . . . O3b-1 O 0.282052 0.405893 0.04691 Uani 0.0241 4 1 d . . . O3b-2 O 0.782848 0.400887 0.047626 Uani 0.0241 4 1 d . . . N1a-1 N 0.211317 0.247607 0.204082 Uani 0.0202 4 1 d . . . N1a-2 N 0.710829 0.259743 0.203261 Uani 0.0202 4 1 d . . . N1b-1 N 0.500153 0.369328 0.043804 Uani 0.0174 4 1 d . . . N1b-2 N 0.001505 0.368136 0.044058 Uani 0.0174 4 1 d . . . C1a-1 C 0.100894 0.944551 0.23889 Uani 0.0344 4 1 d . . . C1a-2 C 0.60104 0.956921 0.238457 Uani 0.0344 4 1 d . . . C1b-1 C 0.351409 0.690829 0.012251 Uani 0.029 4 1 d . . . C1b-2 C 0.850318 0.687877 0.012396 Uani 0.029 4 1 d . . . C2a-1 C 0.14603 0.201635 0.231639 Uani 0.0246 4 1 d . . . C2a-2 C 0.648296 0.214085 0.231092 Uani 0.0246 4 1 d . . . C2b-1 C 0.405925 0.430677 0.017232 Uani 0.0214 4 1 d . . . C2b-2 C 0.903035 0.428071 0.017644 Uani 0.0214 4 1 d . . . C3a-1 C 0.216302 0.309353 0.220179 Uani 0.0215 4 1 d . . . C3a-2 C 0.718538 0.319971 0.219442 Uani 0.0215 4 1 d . . . C3b-1 C 0.484508 0.316487 0.027472 Uani 0.0193 4 1 d . . . C3b-2 C 0.982939 0.314639 0.027789 Uani 0.0193 4 1 d . . . C4a-1 C 0.158771 0.475486 0.220967 Uani 0.0229 4 1 d . . . C4a-2 C 0.664785 0.488078 0.220368 Uani 0.0229 4 1 d . . . C4b-1 C 0.419107 0.152866 0.026168 Uani 0.0221 4 1 d . . . C4b-2 C 0.918275 0.150434 0.026552 Uani 0.0221 4 1 d . . . C5a-1 C 0.229353 0.587552 0.21026 Uani 0.0232 4 1 d . . . C5a-2 C 0.735811 0.60076 0.20967 Uani 0.0232 4 1 d . . . C5b-1 C 0.473491 0.035571 0.037878 Uani 0.0223 4 1 d . . . C5b-2 C 0.972047 0.033825 0.038454 Uani 0.0223 4 1 d . . . C6a-1 C 0.194869 0.597681 0.194289 Uani 0.0271 4 1 d . . . C6a-2 C 0.698568 0.613437 0.193756 Uani 0.0271 4 1 d . . . C6b-1 C 0.414649 0.021264 0.05268 Uani 0.0246 4 1 d . . . C6b-2 C 0.914428 0.021042 0.053399 Uani 0.0246 4 1 d . . . C7a-1 C 0.26359 0.695481 0.184279 Uani 0.0287 4 1 d . . . C7a-2 C 0.762692 0.716269 0.183793 Uani 0.0287 4 1 d . . . C7b-1 C 0.459853 0.911893 0.063573 Uani 0.0273 4 1 d . . . C7b-2 C 0.958555 0.911945 0.064241 Uani 0.0273 4 1 d . . . C8a-1 C 0.367291 0.788099 0.190015 Uani 0.0273 4 1 d . . . C8a-2 C 0.866526 0.808613 0.189635 Uani 0.0273 4 1 d . . . C8b-1 C 0.56489 0.815782 0.05996 Uani 0.029 4 1 d . . . C8b-2 C 0.06208 0.813908 0.060604 Uani 0.029 4 1 d . . . C9a-1 C 0.400367 0.780795 0.206053 Uani 0.0289 4 1 d . . . C9a-2 C 0.903725 0.797301 0.205446 Uani 0.0289 4 1 d . . . C9b-1 C 0.625762 0.829213 0.045206 Uani 0.0285 4 1 d . . . C9b-2 C 0.122021 0.825157 0.045855 Uani 0.0285 4 1 d . . . C10a-1 C 0.332722 0.681949 0.216134 Uani 0.0254 4 1 d . . . C10a-2 C 0.839083 0.693409 0.215393 Uani 0.0254 4 1 d . . . C10b-1 C 0.579408 0.938201 0.034321 Uani 0.0246 4 1 d . . . C10b-2 C 0.077377 0.934709 0.034965 Uani 0.0246 4 1 d . . . C11a-1 C 0.318083 0.243194 0.194968 Uani 0.0193 4 1 d . . . C11a-2 C 0.817629 0.240256 0.194303 Uani 0.0193 4 1 d . . . C11b-1 C 0.396749 0.406579 0.052466 Uani 0.0177 4 1 d . . . C11b-2 C 0.897428 0.403107 0.05289 Uani 0.0177 4 1 d . . . C12a-1 C 0.294194 0.200624 0.177882 Uani 0.0194 4 1 d . . . C12a-2 C 0.790885 0.19742 0.17728 Uani 0.0194 4 1 d . . . C12b-1 C 0.422945 0.447288 0.069534 Uani 0.0182 4 1 d . . . C12b-2 C 0.925695 0.444504 0.070034 Uani 0.0182 4 1 d . . . C13a-1 C 0.365049 0.278518 0.166312 Uani 0.0251 4 1 d . . . C13a-2 C 0.885782 0.23577 0.166243 Uani 0.0251 4 1 d . . . C13b-1 C 0.341469 0.553878 0.076683 Uani 0.0369 4 1 d . . . C13b-2 C 0.838477 0.541066 0.077577 Uani 0.0369 4 1 d . . . C14a-1 C 0.345082 0.243792 0.150358 Uani 0.0266 4 1 d . . . C14a-2 C 0.866869 0.199564 0.150363 Uani 0.0266 4 1 d . . . C14b-1 C 0.360514 0.595601 0.092492 Uani 0.0371 4 1 d . . . C14b-2 C 0.857707 0.582685 0.093377 Uani 0.0371 4 1 d . . . C15a-1 C 0.257305 0.127034 0.145429 Uani 0.0203 4 1 d . . . C15a-2 C 0.75423 0.12205 0.144896 Uani 0.0203 4 1 d . . . C15b-1 C 0.460215 0.528879 0.101764 Uani 0.0185 4 1 d . . . C15b-2 C 0.964887 0.524965 0.102202 Uani 0.0185 4 1 d . . . C16a-1 C 0.186303 0.049166 0.15726 Uani 0.0256 4 1 d . . . C16a-2 C 0.660159 0.082366 0.156014 Uani 0.0256 4 1 d . . . C16b-1 C 0.539487 0.42035 0.094326 Uani 0.0334 4 1 d . . . C16b-2 C 0.049938 0.425602 0.094526 Uani 0.0334 4 1 d . . . C17a-1 C 0.203339 0.087675 0.173167 Uani 0.0233 4 1 d . . . C17a-2 C 0.678455 0.119107 0.172033 Uani 0.0233 4 1 d . . . C17b-1 C 0.524686 0.381024 0.078531 Uani 0.0309 4 1 d . . . C17b-2 C 0.03304 0.386204 0.078585 Uani 0.0309 4 1 d . . . C18a-1 C 0.238591 0.089201 0.128414 Uani 0.0193 4 1 d . . . C18a-2 C 0.735507 0.084931 0.127681 Uani 0.0193 4 1 d . . . C18b-1 C 0.478159 0.568063 0.119009 Uani 0.0203 4 1 d . . . C18b-2 C 0.982124 0.566101 0.119431 Uani 0.0203 4 1 d . . . C19a-1 C 0.328726 0.136433 0.117037 Uani 0.0286 4 1 d . . . C19a-2 C 0.805763 0.165611 0.116062 Uani 0.0286 4 1 d . . . C19b-1 C 0.390287 0.668374 0.126518 Uani 0.0304 4 1 d . . . C19b-2 C 0.90284 0.678854 0.126417 Uani 0.0304 4 1 d . . . C20a-1 C 0.312446 0.102443 0.101053 Uani 0.0313 4 1 d . . . C20a-2 C 0.789079 0.132399 0.100084 Uani 0.0313 4 1 d . . . C20b-1 C 0.406594 0.702864 0.142607 Uani 0.0311 4 1 d . . . C20b-2 C 0.914526 0.713984 0.142371 Uani 0.0311 4 1 d . . . C21a-1 C 0.202813 0.017388 0.095973 Uani 0.027 4 1 d . . . C21a-2 C 0.701251 0.016128 0.095218 Uani 0.027 4 1 d . . . C21b-1 C 0.508855 0.639448 0.151483 Uani 0.0232 4 1 d . . . C21b-2 C 0.005305 0.63623 0.151997 Uani 0.0232 4 1 d . . . C22a-1 C 0.111974 0.967204 0.106991 Uani 0.0312 4 1 d . . . C22a-2 C 0.631089 0.936044 0.106417 Uani 0.0312 4 1 d . . . C22b-1 C 0.595985 0.541221 0.144036 Uani 0.0293 4 1 d . . . C22b-2 C 0.086864 0.528113 0.145179 Uani 0.0293 4 1 d . . . C23a-1 C 0.129465 0.004474 0.12287 Uani 0.0271 4 1 d . . . C23a-2 C 0.647678 0.967932 0.122491 Uani 0.0271 4 1 d . . . C23b-1 C 0.582533 0.505886 0.12816 Uani 0.0262 4 1 d . . . C23b-2 C 0.075902 0.49196 0.129113 Uani 0.0262 4 1 d . . . H1c3a-1 H 0.308079 0.315318 0.22336 Uiso 0.0322 4 1 d . . . H1c3a-2 H 0.810757 0.322314 0.222479 Uiso 0.0322 4 1 d . . . H1c3b-1 H 0.573299 0.309717 0.02355 Uiso 0.029 4 1 d . . . H1c3b-2 H 0.071348 0.308053 0.023745 Uiso 0.029 4 1 d . . . H1c4a-1 H 0.066109 0.472973 0.218143 Uiso 0.0343 4 1 d . . . H1c4a-2 H 0.571666 0.488389 0.217772 Uiso 0.0343 4 1 d . . . H2c4a-1 H 0.163778 0.512583 0.231728 Uiso 0.0343 4 1 d . . . H2c4a-2 H 0.670644 0.524199 0.231161 Uiso 0.0343 4 1 d . . . H1c4b-1 H 0.324951 0.16239 0.027458 Uiso 0.033 4 1 d . . . H1c4b-2 H 0.823939 0.159562 0.027696 Uiso 0.033 4 1 d . . . H2c4b-1 H 0.428636 0.113769 0.015551 Uiso 0.033 4 1 d . . . H2c4b-2 H 0.928763 0.110547 0.015981 Uiso 0.033 4 1 d . . . H1c6a-1 H 0.122659 0.5363 0.190133 Uiso 0.0325 4 1 d . . . H1c6a-2 H 0.627519 0.550148 0.189613 Uiso 0.0325 4 1 d . . . H1c6b-1 H 0.341911 0.087998 0.055361 Uiso 0.0294 4 1 d . . . H1c6b-2 H 0.842971 0.08938 0.056151 Uiso 0.0294 4 1 d . . . H1c7a-1 H 0.23947 0.699648 0.173198 Uiso 0.0345 4 1 d . . . H1c7a-2 H 0.735662 0.724118 0.172824 Uiso 0.0345 4 1 d . . . H1c7b-1 H 0.417869 0.902862 0.073703 Uiso 0.0328 4 1 d . . . H1c7b-2 H 0.91696 0.904068 0.074404 Uiso 0.0328 4 1 d . . . H1c8a-1 H 0.414822 0.855555 0.183001 Uiso 0.0327 4 1 d . . . H1c8a-2 H 0.911592 0.879293 0.182714 Uiso 0.0327 4 1 d . . . H1c8b-1 H 0.595982 0.740072 0.067543 Uiso 0.0347 4 1 d . . . H1c8b-2 H 0.092676 0.738202 0.068217 Uiso 0.0347 4 1 d . . . H1c9a-1 H 0.470817 0.844811 0.210225 Uiso 0.0346 4 1 d . . . H1c9a-2 H 0.974332 0.861205 0.209598 Uiso 0.0346 4 1 d . . . H1c9b-1 H 0.699297 0.763289 0.042627 Uiso 0.0342 4 1 d . . . H1c9b-2 H 0.19409 0.757153 0.043243 Uiso 0.0342 4 1 d . . . H1c10a-1 H 0.356763 0.678027 0.227218 Uiso 0.0305 4 1 d . . . H1c10a-2 H 0.866195 0.685625 0.226359 Uiso 0.0305 4 1 d . . . H1c10b-1 H 0.620997 0.94671 0.024162 Uiso 0.0295 4 1 d . . . H1c10b-2 H 0.11957 0.942674 0.024839 Uiso 0.0295 4 1 d . . . H1n1a-1 H 0.127816 0.249207 0.19967 Uiso 0.0243 4 1 d . . . H1n1a-2 H 0.624953 0.257895 0.199267 Uiso 0.0243 4 1 d . . . H1n1b-1 H 0.585063 0.380409 0.047749 Uiso 0.0208 4 1 d . . . H1n1b-2 H 0.086833 0.382395 0.04762 Uiso 0.0208 4 1 d . . . H1c13a-1 H 0.428304 0.356965 0.169377 Uiso 0.03 4 1 d . . . H1c13a-2 H 0.96552 0.288019 0.169645 Uiso 0.03 4 1 d . . . H1c13b-1 H 0.270187 0.60023 0.070637 Uiso 0.0443 4 1 d . . . H1c13b-2 H 0.762702 0.580592 0.071813 Uiso 0.0443 4 1 d . . . H1c14a-1 H 0.392772 0.301432 0.142507 Uiso 0.032 4 1 d . . . H1c14a-2 H 0.933529 0.228848 0.142896 Uiso 0.032 4 1 d . . . H1c14b-1 H 0.30346 0.672277 0.097105 Uiso 0.0446 4 1 d . . . H1c14b-2 H 0.796196 0.652337 0.098304 Uiso 0.0446 4 1 d . . . H1c16a-1 H 0.125129 0.968157 0.154293 Uiso 0.0307 4 1 d . . . H1c16a-2 H 0.581065 0.028681 0.152632 Uiso 0.0307 4 1 d . . . H1c16b-1 H 0.608131 0.370041 0.100477 Uiso 0.0401 4 1 d . . . H1c16b-2 H 0.123506 0.381991 0.10039 Uiso 0.0401 4 1 d . . . H1c17a-1 H 0.151548 0.035466 0.181034 Uiso 0.028 4 1 d . . . H1c17a-2 H 0.612139 0.089686 0.179538 Uiso 0.028 4 1 d . . . H1c17b-1 H 0.584427 0.308168 0.07377 Uiso 0.0371 4 1 d . . . H1c17b-2 H 0.095627 0.318802 0.073533 Uiso 0.0371 4 1 d . . . H1c19a-1 H 0.405301 0.194961 0.120408 Uiso 0.0343 4 1 d . . . H1c19a-2 H 0.86691 0.245815 0.119265 Uiso 0.0343 4 1 d . . . H1c19b-1 H 0.318109 0.713946 0.120563 Uiso 0.0365 4 1 d . . . H1c19b-2 H 0.838538 0.73342 0.11998 Uiso 0.0365 4 1 d . . . H1c20a-1 H 0.376603 0.137492 0.093527 Uiso 0.0376 4 1 d . . . H1c20a-2 H 0.838143 0.189608 0.092324 Uiso 0.0376 4 1 d . . . H1c20b-1 H 0.345269 0.772259 0.147603 Uiso 0.0373 4 1 d . . . H1c20b-2 H 0.859166 0.793141 0.146848 Uiso 0.0373 4 1 d . . . H1c22a-1 H 0.036695 0.906439 0.103616 Uiso 0.0374 4 1 d . . . H1c22a-2 H 0.569578 0.856731 0.10308 Uiso 0.0374 4 1 d . . . H1c22b-1 H 0.667944 0.496266 0.150079 Uiso 0.0352 4 1 d . . . H1c22b-2 H 0.152781 0.47644 0.151635 Uiso 0.0352 4 1 d . . . H1c23a-1 H 0.064232 0.970852 0.13033 Uiso 0.0326 4 1 d . . . H1c23a-2 H 0.598611 0.909416 0.13015 Uiso 0.0326 4 1 d . . . H1c23b-1 H 0.645499 0.43771 0.123283 Uiso 0.0314 4 1 d . . . H1c23b-2 H 0.133566 0.415088 0.124643 Uiso 0.0314 4 1 d . . . H1c21a-1 H 0.190142 0.993581 0.084899 Uiso 0.0324 4 1 d . . . H1c21a-2 H 0.689896 0.992223 0.084127 Uiso 0.0324 4 1 d . . . H1c21b-1 H 0.519154 0.663135 0.162591 Uiso 0.0279 4 1 d . . . H1c21b-2 H 0.011061 0.657491 0.163195 Uiso 0.0279 4 1 d . . . H1c1a-1 H 0.119033 0.840002 0.235523 Uiso 0.0516 4 1 d . . . H1c1a-2 H 0.618269 0.852116 0.235105 Uiso 0.0516 4 1 d . . . H2c1a-1 H 0.135119 0.959694 0.249495 Uiso 0.0516 4 1 d . . . H2c1a-2 H 0.63566 0.971898 0.249048 Uiso 0.0516 4 1 d . . . H3c1a-1 H 0.006755 0.96189 0.238721 Uiso 0.0516 4 1 d . . . H3c1a-2 H 0.507042 0.975278 0.238321 Uiso 0.0516 4 1 d . . . H1c1b-1 H 0.374943 0.793967 0.015669 Uiso 0.0436 4 1 d . . . H1c1b-2 H 0.875147 0.791207 0.015616 Uiso 0.0436 4 1 d . . . H2c1b-1 H 0.367915 0.680374 0.001088 Uiso 0.0436 4 1 d . . . H2c1b-2 H 0.865301 0.675612 0.001219 Uiso 0.0436 4 1 d . . . H3c1b-1 H 0.259001 0.672879 0.014181 Uiso 0.0436 4 1 d . . . H3c1b-2 H 0.758046 0.671325 0.014521 Uiso 0.0436 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1a-1 O 0.04287 0.023246 0.031514 0.001385 0.01283 0.001207 O1a-2 O 0.04287 0.023246 0.031514 0.001385 0.01283 0.001207 O1b-1 O 0.029795 0.018585 0.025068 -0.001925 -0.007423 0.00172 O1b-2 O 0.029795 0.018585 0.025068 -0.001925 -0.007423 0.00172 O2a-1 O 0.093617 0.029089 0.036885 0.000701 0.035958 -0.001939 O2a-2 O 0.093617 0.029089 0.036885 0.000701 0.035958 -0.001939 O2b-1 O 0.050726 0.024678 0.030798 -0.00199 -0.021841 -0.000842 O2b-2 O 0.050726 0.024678 0.030798 -0.00199 -0.021841 -0.000842 O3a-1 O 0.014473 0.039555 0.0265 -0.000132 -0.000129 -0.00322 O3a-2 O 0.014473 0.039555 0.0265 -0.000132 -0.000129 -0.00322 O3b-1 O 0.014694 0.032498 0.025068 -0.000237 -0.002918 -0.000915 O3b-2 O 0.014694 0.032498 0.025068 -0.000237 -0.002918 -0.000915 N1a-1 N 0.016299 0.025018 0.019338 0.000495 -0.000772 -0.001281 N1a-2 N 0.016299 0.025018 0.019338 0.000495 -0.000772 -0.001281 N1b-1 N 0.013733 0.018933 0.019338 -0.002183 -0.001845 0.000146 N1b-2 N 0.013733 0.018933 0.019338 -0.002183 -0.001845 0.000146 C1a-1 C 0.049199 0.027665 0.0265 -0.009592 0.00369 0.002159 C1a-2 C 0.049199 0.027665 0.0265 -0.009592 0.00369 0.002159 C1b-1 C 0.039919 0.020163 0.026858 0.004752 -0.00369 0.00322 C1b-2 C 0.039919 0.020163 0.026858 0.004752 -0.00369 0.00322 C2a-1 C 0.025425 0.02824 0.020054 -0.000964 0.000129 -0.005012 C2a-2 C 0.025425 0.02824 0.020054 -0.000964 0.000129 -0.005012 C2b-1 C 0.022926 0.022977 0.018264 -0.000719 0.001931 0.000293 C2b-2 C 0.022926 0.022977 0.018264 -0.000719 0.001931 0.000293 C3a-1 C 0.021707 0.023512 0.019338 0.001175 -0.001974 -0.002817 C3a-2 C 0.021707 0.023512 0.019338 0.001175 -0.001974 -0.002817 C3b-1 C 0.01926 0.020951 0.017547 -0.000368 -0.001287 -0.000768 C3b-2 C 0.01926 0.020951 0.017547 -0.000368 -0.001287 -0.000768 C4a-1 C 0.020967 0.024929 0.022919 0.003349 0.002017 -0.004244 C4a-2 C 0.020967 0.024929 0.022919 0.003349 0.002017 -0.004244 C4b-1 C 0.024777 0.016144 0.025068 -0.001083 -0.005621 -0.00161 C4b-2 C 0.024777 0.016144 0.025068 -0.001083 -0.005621 -0.00161 C5a-1 C 0.025286 0.018406 0.026142 0.003959 0.004291 -0.000988 C5a-2 C 0.025286 0.018406 0.026142 0.003959 0.004291 -0.000988 C5b-1 C 0.024792 0.01506 0.026858 -0.003858 -0.004806 -0.004025 C5b-2 C 0.024792 0.01506 0.026858 -0.003858 -0.004806 -0.004025 C6a-1 C 0.022659 0.027657 0.030798 0.002762 -0.004076 -0.003256 C6a-2 C 0.022659 0.027657 0.030798 0.002762 -0.004076 -0.003256 C6b-1 C 0.024294 0.018178 0.031156 0.001162 -0.002103 -0.002707 C6b-2 C 0.024294 0.018178 0.031156 0.001162 -0.002103 -0.002707 C7a-1 C 0.029667 0.032076 0.024352 0.000947 0.000257 0.003403 C7a-2 C 0.029667 0.032076 0.024352 0.000947 0.000257 0.003403 C7b-1 C 0.033127 0.022914 0.025784 0.000561 -0.00103 -0.00011 C7b-2 C 0.033127 0.022914 0.025784 0.000561 -0.00103 -0.00011 C8a-1 C 0.030931 0.020645 0.030439 0.002218 0.003175 0.003366 C8a-2 C 0.030931 0.020645 0.030439 0.002218 0.003175 0.003366 C8b-1 C 0.031332 0.021262 0.034021 0.000329 -0.008067 0.002964 C8b-2 C 0.031332 0.021262 0.034021 0.000329 -0.008067 0.002964 C9a-1 C 0.029389 0.024869 0.03223 -0.002275 -0.001974 -0.004573 C9a-2 C 0.029389 0.024869 0.03223 -0.002275 -0.001974 -0.004573 C9b-1 C 0.02651 0.021706 0.037244 0.003775 -0.002575 -0.00311 C9b-2 C 0.02651 0.021706 0.037244 0.003775 -0.002575 -0.00311 C10a-1 C 0.027137 0.024521 0.024352 0.000636 -0.002188 -0.002378 C10a-2 C 0.027137 0.024521 0.024352 0.000636 -0.002188 -0.002378 C10b-1 C 0.025538 0.021718 0.0265 -0.003051 -0.000086 -0.005049 C10b-2 C 0.025538 0.021718 0.0265 -0.003051 -0.000086 -0.005049 C11a-1 C 0.012134 0.019979 0.025784 -0.000092 0.000815 0.001171 C11a-2 C 0.012134 0.019979 0.025784 -0.000092 0.000815 0.001171 C11b-1 C 0.011568 0.015662 0.025784 0.000219 -0.000515 0.003037 C11b-2 C 0.011568 0.015662 0.025784 0.000219 -0.000515 0.003037 C12a-1 C 0.016484 0.019393 0.022203 0.001306 0.000515 0 C12a-2 C 0.016484 0.019393 0.022203 0.001306 0.000515 0 C12b-1 C 0.016823 0.017426 0.020412 -0.001999 0.004034 0.001829 C12b-2 C 0.016823 0.017426 0.020412 -0.001999 0.004034 0.001829 C13a-1 C 0.016623 0.032371 0.026142 -0.004599 -0.001073 -0.00311 C13a-2 C 0.016623 0.032371 0.026142 -0.004599 -0.001073 -0.00311 C13b-1 C 0.031523 0.051782 0.027216 0.023748 -0.008796 -0.006769 C13b-2 C 0.031523 0.051782 0.027216 0.023748 -0.008796 -0.006769 C14a-1 C 0.024767 0.030894 0.024352 -0.003187 0.005664 0.001756 C14a-2 C 0.024767 0.030894 0.024352 -0.003187 0.005664 0.001756 C14b-1 C 0.038068 0.044441 0.028649 0.024682 -0.007595 -0.011232 C14b-2 C 0.038068 0.044441 0.028649 0.024682 -0.007595 -0.011232 C15a-1 C 0.019512 0.016948 0.024352 0.00313 0.000172 0.000549 C15a-2 C 0.019512 0.016948 0.024352 0.00313 0.000172 0.000549 C15b-1 C 0.016617 0.01623 0.022561 -0.000416 0.000944 0.000585 C15b-2 C 0.016617 0.01623 0.022561 -0.000416 0.000944 0.000585 C16a-1 C 0.024433 0.02537 0.026858 -0.003954 0.000043 -0.002049 C16a-2 C 0.024433 0.02537 0.026858 -0.003954 0.000043 -0.002049 C16b-1 C 0.029723 0.045985 0.024352 0.019355 -0.005707 -0.004829 C16b-2 C 0.029723 0.045985 0.024352 0.019355 -0.005707 -0.004829 C17a-1 C 0.01797 0.024891 0.027216 -0.002845 0.006308 -0.000476 C17a-2 C 0.01797 0.024891 0.027216 -0.002845 0.006308 -0.000476 C17b-1 C 0.023872 0.043002 0.025784 0.014353 -0.004119 -0.007939 C17b-2 C 0.023872 0.043002 0.025784 0.014353 -0.004119 -0.007939 C18a-1 C 0.016437 0.016825 0.02471 0.003832 -0.001416 -0.002342 C18a-2 C 0.016437 0.016825 0.02471 0.003832 -0.001416 -0.002342 C18b-1 C 0.021178 0.017939 0.021845 -0.0053 0.004248 -0.000402 C18b-2 C 0.021178 0.017939 0.021845 -0.0053 0.004248 -0.000402 C19a-1 C 0.027877 0.028861 0.029007 -0.005449 0.001459 -0.00322 C19a-2 C 0.027877 0.028861 0.029007 -0.005449 0.001459 -0.00322 C19b-1 C 0.028715 0.039137 0.023277 0.011951 -0.003004 -0.000073 C19b-2 C 0.028715 0.039137 0.023277 0.011951 -0.003004 -0.000073 C20a-1 C 0.037615 0.033776 0.022561 -0.003104 0.002446 -0.003805 C20a-2 C 0.037615 0.033776 0.022561 -0.003104 0.002446 -0.003805 C20b-1 C 0.02979 0.036456 0.027216 0.007128 0.00442 -0.006878 C20b-2 C 0.02979 0.036456 0.027216 0.007128 0.00442 -0.006878 C21a-1 C 0.032063 0.025841 0.022919 0.006795 -0.004806 -0.00633 C21a-2 C 0.032063 0.025841 0.022919 0.006795 -0.004806 -0.00633 C21b-1 C 0.021106 0.026641 0.021845 -0.007378 0.000257 -0.001793 C21b-2 C 0.021106 0.026641 0.021845 -0.007378 0.000257 -0.001793 C22a-1 C 0.031456 0.030027 0.031872 -0.004007 -0.004763 -0.005671 C22a-2 C 0.031456 0.030027 0.031872 -0.004007 -0.004763 -0.005671 C22b-1 C 0.029039 0.031425 0.027216 0.003753 -0.00781 -0.000293 C22b-2 C 0.029039 0.031425 0.027216 0.003753 -0.00781 -0.000293 C23a-1 C 0.024489 0.029721 0.027216 -0.004537 0.000644 -0.0015 C23a-2 C 0.024489 0.029721 0.027216 -0.004537 0.000644 -0.0015 C23b-1 C 0.026602 0.025908 0.026142 0.005611 -0.000815 -0.003915 C23b-2 C 0.026602 0.025908 0.026142 0.005611 -0.000815 -0.003915 #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1a-1 C1a-1 . 1_545 1.43841(6) ? O1a-1 C2a-1 . . 1.32361(9) ? O1a-2 C1a-2 . 1_545 1.44797(6) ? O1a-2 C2a-2 . . 1.32423(9) ? O1b-1 C1b-1 . . 1.45021(6) ? O1b-1 C2b-1 . . 1.32714(8) ? O1b-2 C1b-2 . . 1.44958(6) ? O1b-2 C2b-2 . . 1.32633(8) ? O2a-1 C2a-1 . . 1.19879(5) ? O2a-2 C2a-2 . . 1.19341(5) ? O2b-1 C2b-1 . . 1.20546(5) ? O2b-2 C2b-2 . . 1.20589(5) ? O3a-1 C11a-1 . . 1.23928(5) ? O3a-2 C11a-2 . . 1.23611(5) ? O3b-1 C11b-1 . . 1.23979(5) ? O3b-2 C11b-2 . . 1.23014(5) ? N1a-1 C3a-1 . . 1.45389(4) ? N1a-1 C11a-1 . . 1.33092(6) ? N1a-1 H1n1a-1 . . 0.91432(4) ? N1a-2 C3a-2 . . 1.45659(4) ? N1a-2 C11a-2 . . 1.33353(6) ? N1a-2 H1n1a-2 . . 0.92342(4) ? N1b-1 C3b-1 . . 1.45263(5) ? N1b-1 C11b-1 . . 1.31975(6) ? N1b-1 H1n1b-1 . . 0.91773(4) ? N1b-2 C3b-2 . 1_455 1.45248(5) ? N1b-2 C11b-2 . 1_455 1.32868(6) ? N1b-2 H1n1b-2 . . 0.91426(4) ? C1a-1 H1c1a-1 . . 0.96003(6) ? C1a-1 H2c1a-1 . . 0.95996(4) ? C1a-1 H3c1a-1 . . 0.96000(4) ? C1a-2 H1c1a-2 . . 0.95997(6) ? C1a-2 H2c1a-2 . . 0.96007(4) ? C1a-2 H3c1a-2 . . 0.96000(4) ? C1b-1 H1c1b-1 . . 0.96000(6) ? C1b-1 H2c1b-1 . . 0.96001(3) ? C1b-1 H3c1b-1 . . 0.96001(4) ? C1b-2 H1c1b-2 . . 0.96000(6) ? C1b-2 H2c1b-2 . . 0.95998(3) ? C1b-2 H3c1b-2 . . 0.95998(4) ? C2a-1 C3a-1 . . 1.51890(6) ? C2a-2 C3a-2 . . 1.51959(6) ? C2b-1 C3b-1 . . 1.51965(6) ? C2b-2 C3b-2 . . 1.51790(6) ? C3a-1 C4a-1 . . 1.54209(9) ? C3a-1 H1c3a-1 . . 0.95999(4) ? C3a-2 C4a-2 . . 1.54461(9) ? C3a-2 H1c3a-2 . . 0.96000(4) ? C3b-1 C4b-1 . . 1.55543(9) ? C3b-1 H1c3b-1 . . 0.95998(4) ? C3b-2 C4b-2 . . 1.55650(9) ? C3b-2 H1c3b-2 . 1_655 0.96001(4) ? C4a-1 C5a-1 . . 1.50422(6) ? C4a-1 H1c4a-1 . . 0.96002(4) ? C4a-1 H2c4a-1 . . 0.95992(3) ? C4a-2 C5a-2 . . 1.50931(6) ? C4a-2 H1c4a-2 . . 0.95999(4) ? C4a-2 H2c4a-2 . . 0.96007(3) ? C4b-1 C5b-1 . . 1.50608(6) ? C4b-1 H1c4b-1 . . 0.95999(4) ? C4b-1 H2c4b-1 . . 0.96002(3) ? C4b-2 C5b-2 . . 1.51052(6) ? C4b-2 H1c4b-2 . . 0.96001(4) ? C4b-2 H2c4b-2 . . 0.95998(3) ? C5a-1 C6a-1 . . 1.38470(5) ? C5a-1 C10a-1 . . 1.40366(5) ? C5a-2 C6a-2 . . 1.38846(5) ? C5a-2 C10a-2 . . 1.39001(5) ? C5b-1 C6b-1 . . 1.39230(5) ? C5b-1 C10b-1 . 1_545 1.39200(5) ? C5b-2 C6b-2 . . 1.39671(5) ? C5b-2 C10b-2 . 1_645 1.39527(5) ? C6a-1 C7a-1 . . 1.38260(5) ? C6a-1 H1c6a-1 . . 0.96000(4) ? C6a-2 C7a-2 . . 1.38426(5) ? C6a-2 H1c6a-2 . . 0.96002(4) ? C6b-1 C7b-1 . 1_545 1.38425(5) ? C6b-1 H1c6b-1 . . 0.96000(4) ? C6b-2 C7b-2 . 1_545 1.37640(5) ? C6b-2 H1c6b-2 . . 0.96000(4) ? C7a-1 C8a-1 . . 1.39344(5) ? C7a-1 H1c7a-1 . . 0.95996(3) ? C7a-2 C8a-2 . . 1.39611(5) ? C7a-2 H1c7a-2 . . 0.96004(4) ? C7b-1 C8b-1 . . 1.37977(5) ? C7b-1 H1c7b-1 . . 0.96001(4) ? C7b-2 C8b-2 . 1_655 1.37859(5) ? C7b-2 H1c7b-2 . . 0.95998(4) ? C8a-1 C9a-1 . . 1.38556(5) ? C8a-1 H1c8a-1 . . 0.96002(4) ? C8a-2 C9a-2 . . 1.37916(5) ? C8a-2 H1c8a-2 . . 0.96000(4) ? C8b-1 C9b-1 . . 1.39716(6) ? C8b-1 H1c8b-1 . . 0.95993(4) ? C8b-2 C9b-2 . . 1.39113(6) ? C8b-2 H1c8b-2 . . 0.96001(4) ? C9a-1 C10a-1 . . 1.38629(5) ? C9a-1 H1c9a-1 . . 0.95999(4) ? C9a-2 C10a-2 . . 1.39175(5) ? C9a-2 H1c9a-2 . . 0.96001(4) ? C9b-1 C10b-1 . . 1.38532(5) ? C9b-1 H1c9b-1 . . 0.95999(3) ? C9b-2 C10b-2 . . 1.38335(5) ? C9b-2 H1c9b-2 . . 0.96002(4) ? C10a-1 H1c10a-1 . . 0.95994(3) ? C10a-2 H1c10a-2 . . 0.95998(4) ? C10b-1 H1c10b-1 . . 0.96004(4) ? C10b-2 H1c10b-2 . . 0.95997(4) ? C11a-1 C12a-1 . . 1.49836(5) ? C11a-2 C12a-2 . . 1.49834(5) ? C11b-1 C12b-1 . . 1.49667(5) ? C11b-2 C12b-2 . . 1.50766(5) ? C12a-1 C13a-1 . . 1.38754(5) ? C12a-1 C17a-1 . . 1.38753(6) ? C12a-2 C13a-2 . . 1.38252(6) ? C12a-2 C17a-2 . . 1.38381(5) ? C12b-1 C13b-1 . . 1.37433(5) ? C12b-1 C17b-1 . . 1.38679(6) ? C12b-2 C13b-2 . . 1.37102(5) ? C12b-2 C17b-2 . 1_655 1.38330(6) ? C13a-1 C14a-1 . . 1.38592(5) ? C13a-1 H1c13a-1 . . 0.96000(4) ? C13a-2 C14a-2 . . 1.38137(5) ? C13a-2 H1c13a-2 . . 0.96000(4) ? C13b-1 C14b-1 . . 1.38726(5) ? C13b-1 H1c13b-1 . . 0.95996(4) ? C13b-2 C14b-2 . . 1.38654(5) ? C13b-2 H1c13b-2 . . 0.96002(4) ? C14a-1 C15a-1 . . 1.39588(6) ? C14a-1 H1c14a-1 . . 0.96001(4) ? C14a-2 C15a-2 . . 1.38799(5) ? C14a-2 H1c14a-2 . . 0.96000(4) ? C14b-1 C15b-1 . . 1.38609(6) ? C14b-1 H1c14b-1 . . 0.95999(4) ? C14b-2 C15b-2 . . 1.39208(6) ? C14b-2 H1c14b-2 . . 0.96000(4) ? C15a-1 C16a-1 . . 1.40385(5) ? C15a-1 C18a-1 . . 1.47642(5) ? C15a-2 C16a-2 . . 1.38414(6) ? C15a-2 C18a-2 . . 1.49138(5) ? C15b-1 C16b-1 . . 1.38332(6) ? C15b-1 C18b-1 . . 1.49686(5) ? C15b-2 C16b-2 . 1_655 1.37712(5) ? C15b-2 C18b-2 . . 1.49868(5) ? C16a-1 C17a-1 . . 1.38595(5) ? C16a-1 H1c16a-1 . 1_545 0.96000(4) ? C16a-2 C17a-2 . . 1.39294(5) ? C16a-2 H1c16a-2 . . 0.95999(4) ? C16b-1 C17b-1 . . 1.37630(4) ? C16b-1 H1c16b-1 . . 0.95998(4) ? C16b-2 C17b-2 . . 1.39040(5) ? C16b-2 H1c16b-2 . . 0.96000(4) ? C17a-1 H1c17a-1 . . 0.96003(4) ? C17a-2 H1c17a-2 . . 0.95998(4) ? C17b-1 H1c17b-1 . . 0.96003(4) ? C17b-2 H1c17b-2 . . 0.95999(4) ? C18a-1 C19a-1 . . 1.38972(6) ? C18a-1 C23a-1 . . 1.39286(5) ? C18a-2 C19a-2 . . 1.39900(5) ? C18a-2 C23a-2 . 1_545 1.40415(6) ? C18b-1 C19b-1 . . 1.39363(5) ? C18b-1 C23b-1 . . 1.39938(6) ? C18b-2 C19b-2 . . 1.39129(6) ? C18b-2 C23b-2 . 1_655 1.39190(5) ? C19a-1 C20a-1 . . 1.38267(5) ? C19a-1 H1c19a-1 . . 0.96000(4) ? C19a-2 C20a-2 . . 1.38122(5) ? C19a-2 H1c19a-2 . . 0.96000(4) ? C19b-1 C20b-1 . . 1.39218(5) ? C19b-1 H1c19b-1 . . 0.95999(4) ? C19b-2 C20b-2 . . 1.37830(4) ? C19b-2 H1c19b-2 . . 0.95998(4) ? C20a-1 C21a-1 . . 1.38630(5) ? C20a-1 H1c20a-1 . . 0.95999(4) ? C20a-2 C21a-2 . . 1.39168(6) ? C20a-2 H1c20a-2 . . 0.95999(4) ? C20b-1 C21b-1 . . 1.37536(6) ? C20b-1 H1c20b-1 . . 0.95999(4) ? C20b-2 C21b-2 . 1_655 1.38382(5) ? C20b-2 H1c20b-2 . . 0.96002(4) ? C21a-1 C22a-1 . 1_545 1.38130(6) ? C21a-1 H1c21a-1 . 1_545 0.95996(3) ? C21a-2 C22a-2 . 1_545 1.37122(5) ? C21a-2 H1c21a-2 . 1_545 0.96006(3) ? C21b-1 C22b-1 . . 1.37537(5) ? C21b-1 H1c21b-1 . . 0.95999(3) ? C21b-2 C22b-2 . . 1.37148(5) ? C21b-2 H1c21b-2 . . 0.96002(3) ? C22a-1 C23a-1 . 1_565 1.38169(5) ? C22a-1 H1c22a-1 . . 0.96000(4) ? C22a-2 C23a-2 . . 1.38666(5) ? C22a-2 H1c22a-2 . . 0.96000(4) ? C22b-1 C23b-1 . . 1.37369(4) ? C22b-1 H1c22b-1 . . 0.96000(4) ? C22b-2 C23b-2 . . 1.38890(4) ? C22b-2 H1c22b-2 . . 0.96004(4) ? C23a-1 H1c23a-1 . 1_545 0.96000(4) ? C23a-2 H1c23a-2 . . 0.96002(4) ? C23b-1 H1c23b-1 . . 0.96001(4) ? C23b-2 H1c23b-2 . . 0.95999(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1a-1 O1a-1 C2a-1 1_545 . . 115.5571(17) ? C1a-2 O1a-2 C2a-2 1_545 . . 115.4634(17) ? C1b-1 O1b-1 C2b-1 . . . 114.5492(19) ? C1b-2 O1b-2 C2b-2 . . . 114.4180(19) ? C3a-1 N1a-1 C11a-1 . . . 121.995(2) ? C3a-1 N1a-1 H1n1a-1 . . . 112.993(3) ? C11a-1 N1a-1 H1n1a-1 . . . 120.904(2) ? C3a-2 N1a-2 C11a-2 . . . 122.707(2) ? C3a-2 N1a-2 H1n1a-2 . . . 112.457(3) ? C11a-2 N1a-2 H1n1a-2 . . . 123.513(2) ? C3b-1 N1b-1 C11b-1 . . . 121.496(3) ? C3b-1 N1b-1 H1n1b-1 . . . 117.457(3) ? C11b-1 N1b-1 H1n1b-1 . . . 120.984(2) ? C3b-2 N1b-2 C11b-2 1_455 . 1_455 120.443(3) ? C3b-2 N1b-2 H1n1b-2 1_455 . . 117.240(3) ? C11b-2 N1b-2 H1n1b-2 1_455 . . 122.198(2) ? O1a-1 C1a-1 H1c1a-1 1_565 . . 109.4666(19) ? O1a-1 C1a-1 H2c1a-1 1_565 . . 109.4709(19) ? O1a-1 C1a-1 H3c1a-1 1_565 . . 109.470(2) ? H1c1a-1 C1a-1 H2c1a-1 . . . 109.4760(8) ? H1c1a-1 C1a-1 H3c1a-1 . . . 109.4692(9) ? H2c1a-1 C1a-1 H3c1a-1 . . . 109.475(3) ? O1a-2 C1a-2 H1c1a-2 1_565 . . 109.4754(19) ? O1a-2 C1a-2 H2c1a-2 1_565 . . 109.4722(19) ? O1a-2 C1a-2 H3c1a-2 1_565 . . 109.472(2) ? H1c1a-2 C1a-2 H2c1a-2 . . . 109.4669(8) ? H1c1a-2 C1a-2 H3c1a-2 . . . 109.4732(9) ? H2c1a-2 C1a-2 H3c1a-2 . . . 109.468(3) ? O1b-1 C1b-1 H1c1b-1 . . . 109.470(2) ? O1b-1 C1b-1 H2c1b-1 . . . 109.4726(19) ? O1b-1 C1b-1 H3c1b-1 . . . 109.4704(19) ? H1c1b-1 C1b-1 H2c1b-1 . . . 109.4716(9) ? H1c1b-1 C1b-1 H3c1b-1 . . . 109.4701(10) ? H2c1b-1 C1b-1 H3c1b-1 . . . 109.472(3) ? O1b-2 C1b-2 H1c1b-2 . . . 109.470(2) ? O1b-2 C1b-2 H2c1b-2 . . . 109.4703(19) ? O1b-2 C1b-2 H3c1b-2 . . . 109.4716(19) ? H1c1b-2 C1b-2 H2c1b-2 . . . 109.4728(9) ? H1c1b-2 C1b-2 H3c1b-2 . . . 109.4709(10) ? H2c1b-2 C1b-2 H3c1b-2 . . . 109.472(3) ? O1a-1 C2a-1 O2a-1 . . . 123.34942(14) ? O1a-1 C2a-1 C3a-1 . . . 112.9495(17) ? O2a-1 C2a-1 C3a-1 . . . 123.6704(18) ? O1a-2 C2a-2 O2a-2 . . . 124.15365(19) ? O1a-2 C2a-2 C3a-2 . . . 112.4815(17) ? O2a-2 C2a-2 C3a-2 . . . 123.3520(19) ? O1b-1 C2b-1 O2b-1 . . . 124.09 ? O1b-1 C2b-1 C3b-1 . . . 112.6403(19) ? O2b-1 C2b-1 C3b-1 . . . 123.2516(18) ? O1b-2 C2b-2 O2b-2 . . . 124.29 ? O1b-2 C2b-2 C3b-2 . . . 112.4791(19) ? O2b-2 C2b-2 C3b-2 . . . 123.1901(18) ? N1a-1 C3a-1 C2a-1 . . . 111.018(2) ? N1a-1 C3a-1 C4a-1 . . . 111.7145(13) ? N1a-1 C3a-1 H1c3a-1 . . . 107.347(3) ? C2a-1 C3a-1 C4a-1 . . . 110.9325(19) ? C2a-1 C3a-1 H1c3a-1 . . . 108.190(2) ? C4a-1 C3a-1 H1c3a-1 . . . 107.4408(9) ? N1a-2 C3a-2 C2a-2 . . . 111.773(2) ? N1a-2 C3a-2 C4a-2 . . . 111.4350(13) ? N1a-2 C3a-2 H1c3a-2 . . . 107.060(3) ? C2a-2 C3a-2 C4a-2 . . . 111.0949(18) ? C2a-2 C3a-2 H1c3a-2 . . . 107.430(2) ? C4a-2 C3a-2 H1c3a-2 . . . 107.7979(8) ? N1b-1 C3b-1 C2b-1 . . . 112.456(2) ? N1b-1 C3b-1 C4b-1 . . . 112.8710(13) ? N1b-1 C3b-1 H1c3b-1 . . . 104.809(3) ? C2b-1 C3b-1 C4b-1 . . . 109.077(2) ? C2b-1 C3b-1 H1c3b-1 . . . 108.941(2) ? C4b-1 C3b-1 H1c3b-1 . . . 108.4857(11) ? N1b-2 C3b-2 C2b-2 1_655 . . 112.688(2) ? N1b-2 C3b-2 C4b-2 1_655 . . 113.4114(13) ? N1b-2 C3b-2 H1c3b-2 1_655 . 1_655 104.213(3) ? C2b-2 C3b-2 C4b-2 . . . 109.045(2) ? C2b-2 C3b-2 H1c3b-2 . . 1_655 109.010(2) ? C4b-2 C3b-2 H1c3b-2 . . 1_655 108.2185(11) ? C3a-1 C4a-1 C5a-1 . . . 112.6439(19) ? C3a-1 C4a-1 H1c4a-1 . . . 109.4703(9) ? C3a-1 C4a-1 H2c4a-1 . . . 109.4739(13) ? C5a-1 C4a-1 H1c4a-1 . . . 109.468(2) ? C5a-1 C4a-1 H2c4a-1 . . . 109.469(2) ? H1c4a-1 C4a-1 H2c4a-1 . . . 106.104(3) ? C3a-2 C4a-2 C5a-2 . . . 113.5559(19) ? C3a-2 C4a-2 H1c4a-2 . . . 109.4717(8) ? C3a-2 C4a-2 H2c4a-2 . . . 109.4683(12) ? C5a-2 C4a-2 H1c4a-2 . . . 109.475(2) ? C5a-2 C4a-2 H2c4a-2 . . . 109.472(2) ? H1c4a-2 C4a-2 H2c4a-2 . . . 105.050(3) ? C3b-1 C4b-1 C5b-1 . . . 114.138(2) ? C3b-1 C4b-1 H1c4b-1 . . . 109.4713(11) ? C3b-1 C4b-1 H2c4b-1 . . . 109.4700(15) ? C5b-1 C4b-1 H1c4b-1 . . . 109.471(2) ? C5b-1 C4b-1 H2c4b-1 . . . 109.4722(19) ? H1c4b-1 C4b-1 H2c4b-1 . . . 104.363(3) ? C3b-2 C4b-2 C5b-2 . . . 114.277(2) ? C3b-2 C4b-2 H1c4b-2 . . . 109.4715(11) ? C3b-2 C4b-2 H2c4b-2 . . . 109.4729(15) ? C5b-2 C4b-2 H1c4b-2 . . . 109.470(2) ? C5b-2 C4b-2 H2c4b-2 . . . 109.4710(19) ? H1c4b-2 C4b-2 H2c4b-2 . . . 104.195(3) ? C4a-1 C5a-1 C6a-1 . . . 120.4522(18) ? C4a-1 C5a-1 C10a-1 . . . 120.940(2) ? C6a-1 C5a-1 C10a-1 . . . 118.599(2) ? C4a-2 C5a-2 C6a-2 . . . 120.0749(19) ? C4a-2 C5a-2 C10a-2 . . . 121.339(2) ? C6a-2 C5a-2 C10a-2 . . . 118.586(2) ? C4b-1 C5b-1 C6b-1 . . . 119.2000(17) ? C4b-1 C5b-1 C10b-1 . . 1_545 122.268(2) ? C6b-1 C5b-1 C10b-1 . . 1_545 118.520(2) ? C4b-2 C5b-2 C6b-2 . . . 119.8970(17) ? C4b-2 C5b-2 C10b-2 . . 1_645 122.107(2) ? C6b-2 C5b-2 C10b-2 . . 1_645 117.986(2) ? C5a-1 C6a-1 C7a-1 . . . 120.5364(19) ? C5a-1 C6a-1 H1c6a-1 . . . 119.732(2) ? C7a-1 C6a-1 H1c6a-1 . . . 119.731(2) ? C5a-2 C6a-2 C7a-2 . . . 120.7703(18) ? C5a-2 C6a-2 H1c6a-2 . . . 119.619(2) ? C7a-2 C6a-2 H1c6a-2 . . . 119.611(2) ? C5b-1 C6b-1 C7b-1 . . 1_545 120.7397(17) ? C5b-1 C6b-1 H1c6b-1 . . . 119.627(2) ? C7b-1 C6b-1 H1c6b-1 1_545 . . 119.633(2) ? C5b-2 C6b-2 C7b-2 . . 1_545 120.9956(17) ? C5b-2 C6b-2 H1c6b-2 . . . 119.503(2) ? C7b-2 C6b-2 H1c6b-2 1_545 . . 119.501(2) ? C6a-1 C7a-1 C8a-1 . . . 121.068(2) ? C6a-1 C7a-1 H1c7a-1 . . . 119.4654(19) ? C8a-1 C7a-1 H1c7a-1 . . . 119.467(2) ? C6a-2 C7a-2 C8a-2 . . . 120.252(2) ? C6a-2 C7a-2 H1c7a-2 . . . 119.8756(19) ? C8a-2 C7a-2 H1c7a-2 . . . 119.872(2) ? C6b-1 C7b-1 C8b-1 1_565 . . 120.400(2) ? C6b-1 C7b-1 H1c7b-1 1_565 . . 119.7996(17) ? C8b-1 C7b-1 H1c7b-1 . . . 119.800(2) ? C6b-2 C7b-2 C8b-2 1_565 . 1_655 120.447(2) ? C6b-2 C7b-2 H1c7b-2 1_565 . . 119.7769(17) ? C8b-2 C7b-2 H1c7b-2 1_655 . . 119.776(2) ? C7a-1 C8a-1 C9a-1 . . . 118.610(2) ? C7a-1 C8a-1 H1c8a-1 . . . 120.693(2) ? C9a-1 C8a-1 H1c8a-1 . . . 120.6975(19) ? C7a-2 C8a-2 C9a-2 . . . 119.352(2) ? C7a-2 C8a-2 H1c8a-2 . . . 120.324(2) ? C9a-2 C8a-2 H1c8a-2 . . . 120.3242(19) ? C7b-1 C8b-1 C9b-1 . . . 119.656(2) ? C7b-1 C8b-1 H1c8b-1 . . . 120.176(2) ? C9b-1 C8b-1 H1c8b-1 . . . 120.1676(17) ? C7b-2 C8b-2 C9b-2 1_455 . . 119.716(2) ? C7b-2 C8b-2 H1c8b-2 1_455 . . 120.141(2) ? C9b-2 C8b-2 H1c8b-2 . . . 120.1432(17) ? C8a-1 C9a-1 C10a-1 . . . 120.6469(19) ? C8a-1 C9a-1 H1c9a-1 . . . 119.677(2) ? C10a-1 C9a-1 H1c9a-1 . . . 119.676(2) ? C8a-2 C9a-2 C10a-2 . . . 120.1175(18) ? C8a-2 C9a-2 H1c9a-2 . . . 119.942(2) ? C10a-2 C9a-2 H1c9a-2 . . . 119.941(2) ? C8b-1 C9b-1 C10b-1 . . . 119.6262(17) ? C8b-1 C9b-1 H1c9b-1 . . . 120.183(2) ? C10b-1 C9b-1 H1c9b-1 . . . 120.191(2) ? C8b-2 C9b-2 C10b-2 . . . 119.7471(17) ? C8b-2 C9b-2 H1c9b-2 . . . 120.132(2) ? C10b-2 C9b-2 H1c9b-2 . . . 120.121(2) ? C5a-1 C10a-1 C9a-1 . . . 120.514(2) ? C5a-1 C10a-1 H1c10a-1 . . . 119.743(2) ? C9a-1 C10a-1 H1c10a-1 . . . 119.7425(19) ? C5a-2 C10a-2 C9a-2 . . . 120.918(2) ? C5a-2 C10a-2 H1c10a-2 . . . 119.541(2) ? C9a-2 C10a-2 H1c10a-2 . . . 119.5413(19) ? C5b-1 C10b-1 C9b-1 1_565 . . 121.054(2) ? C5b-1 C10b-1 H1c10b-1 1_565 . . 119.473(2) ? C9b-1 C10b-1 H1c10b-1 . . . 119.4725(17) ? C5b-2 C10b-2 C9b-2 1_465 . . 121.098(2) ? C5b-2 C10b-2 H1c10b-2 1_465 . . 119.451(2) ? C9b-2 C10b-2 H1c10b-2 . . . 119.4511(17) ? O3a-1 C11a-1 N1a-1 . . . 123.557(2) ? O3a-1 C11a-1 C12a-1 . . . 120.344(3) ? N1a-1 C11a-1 C12a-1 . . . 116.089(3) ? O3a-2 C11a-2 N1a-2 . . . 123.347(2) ? O3a-2 C11a-2 C12a-2 . . . 120.815(3) ? N1a-2 C11a-2 C12a-2 . . . 115.827(3) ? O3b-1 C11b-1 N1b-1 . . . 122.009(2) ? O3b-1 C11b-1 C12b-1 . . . 120.798(3) ? N1b-1 C11b-1 C12b-1 . . . 117.183(3) ? O3b-2 C11b-2 N1b-2 . . 1_655 122.666(2) ? O3b-2 C11b-2 C12b-2 . . . 120.670(3) ? N1b-2 C11b-2 C12b-2 1_655 . . 116.660(3) ? C11a-1 C12a-1 C13a-1 . . . 118.545(2) ? C11a-1 C12a-1 C17a-1 . . . 122.6925(19) ? C13a-1 C12a-1 C17a-1 . . . 118.7599(19) ? C11a-2 C12a-2 C13a-2 . . . 117.823(2) ? C11a-2 C12a-2 C17a-2 . . . 123.933(2) ? C13a-2 C12a-2 C17a-2 . . . 118.229(2) ? C11b-1 C12b-1 C13b-1 . . . 118.516(2) ? C11b-1 C12b-1 C17b-1 . . . 123.035(2) ? C13b-1 C12b-1 C17b-1 . . . 118.4445(19) ? C11b-2 C12b-2 C13b-2 . . . 118.168(2) ? C11b-2 C12b-2 C17b-2 . . 1_655 123.111(2) ? C13b-2 C12b-2 C17b-2 . . 1_655 118.694(2) ? C12a-1 C13a-1 C14a-1 . . . 120.420(2) ? C12a-1 C13a-1 H1c13a-1 . . . 119.7925(19) ? C14a-1 C13a-1 H1c13a-1 . . . 119.788(2) ? C12a-2 C13a-2 C14a-2 . . . 120.579(2) ? C12a-2 C13a-2 H1c13a-2 . . . 119.710(2) ? C14a-2 C13a-2 H1c13a-2 . . . 119.711(2) ? C12b-1 C13b-1 C14b-1 . . . 121.099(2) ? C12b-1 C13b-1 H1c13b-1 . . . 119.4538(19) ? C14b-1 C13b-1 H1c13b-1 . . . 119.447(2) ? C12b-2 C13b-2 C14b-2 . . . 121.210(2) ? C12b-2 C13b-2 H1c13b-2 . . . 119.394(2) ? C14b-2 C13b-2 H1c13b-2 . . . 119.396(2) ? C13a-1 C14a-1 C15a-1 . . . 121.5932(19) ? C13a-1 C14a-1 H1c14a-1 . . . 119.203(2) ? C15a-1 C14a-1 H1c14a-1 . . . 119.2036(19) ? C13a-2 C14a-2 C15a-2 . . . 121.873(2) ? C13a-2 C14a-2 H1c14a-2 . . . 119.062(2) ? C15a-2 C14a-2 H1c14a-2 . . . 119.064(2) ? C13b-1 C14b-1 C15b-1 . . . 121.366(2) ? C13b-1 C14b-1 H1c14b-1 . . . 119.314(2) ? C15b-1 C14b-1 H1c14b-1 . . . 119.3206(19) ? C13b-2 C14b-2 C15b-2 . . . 120.979(2) ? C13b-2 C14b-2 H1c14b-2 . . . 119.512(2) ? C15b-2 C14b-2 H1c14b-2 . . . 119.509(2) ? C14a-1 C15a-1 C16a-1 . . . 117.3464(19) ? C14a-1 C15a-1 C18a-1 . . . 121.1133(19) ? C16a-1 C15a-1 C18a-1 . . . 121.533(2) ? C14a-2 C15a-2 C16a-2 . . . 117.345(2) ? C14a-2 C15a-2 C18a-2 . . . 120.968(2) ? C16a-2 C15a-2 C18a-2 . . . 121.684(2) ? C14b-1 C15b-1 C16b-1 . . . 116.2843(19) ? C14b-1 C15b-1 C18b-1 . . . 121.842(2) ? C16b-1 C15b-1 C18b-1 . . . 121.8421(19) ? C14b-2 C15b-2 C16b-2 . . 1_655 117.007(2) ? C14b-2 C15b-2 C18b-2 . . . 120.576(2) ? C16b-2 C15b-2 C18b-2 1_655 . . 122.380(2) ? C15a-1 C16a-1 C17a-1 . . . 120.884(2) ? C15a-1 C16a-1 H1c16a-1 . . 1_545 119.5603(19) ? C17a-1 C16a-1 H1c16a-1 . . 1_545 119.5552(19) ? C15a-2 C16a-2 C17a-2 . . . 121.034(2) ? C15a-2 C16a-2 H1c16a-2 . . . 119.483(2) ? C17a-2 C16a-2 H1c16a-2 . . . 119.483(2) ? C15b-1 C16b-1 C17b-1 . . . 123.1610(19) ? C15b-1 C16b-1 H1c16b-1 . . . 118.4227(19) ? C17b-1 C16b-1 H1c16b-1 . . . 118.416(2) ? C15b-2 C16b-2 C17b-2 1_455 . . 122.335(2) ? C15b-2 C16b-2 H1c16b-2 1_455 . . 118.830(2) ? C17b-2 C16b-2 H1c16b-2 . . . 118.834(2) ? C12a-1 C17a-1 C16a-1 . . . 120.929(2) ? C12a-1 C17a-1 H1c17a-1 . . . 119.5354(19) ? C16a-1 C17a-1 H1c17a-1 . . . 119.535(2) ? C12a-2 C17a-2 C16a-2 . . . 120.925(2) ? C12a-2 C17a-2 H1c17a-2 . . . 119.539(2) ? C16a-2 C17a-2 H1c17a-2 . . . 119.536(2) ? C12b-1 C17b-1 C16b-1 . . . 119.595(2) ? C12b-1 C17b-1 H1c17b-1 . . . 120.1985(19) ? C16b-1 C17b-1 H1c17b-1 . . . 120.206(2) ? C12b-2 C17b-2 C16b-2 1_455 . . 119.743(2) ? C12b-2 C17b-2 H1c17b-2 1_455 . . 120.131(2) ? C16b-2 C17b-2 H1c17b-2 . . . 120.126(2) ? C15a-1 C18a-1 C19a-1 . . . 121.855(2) ? C15a-1 C18a-1 C23a-1 . . . 121.850(2) ? C19a-1 C18a-1 C23a-1 . . . 116.295(2) ? C15a-2 C18a-2 C19a-2 . . . 120.940(2) ? C15a-2 C18a-2 C23a-2 . . 1_545 121.6248(19) ? C19a-2 C18a-2 C23a-2 . . 1_545 117.4349(19) ? C15b-1 C18b-1 C19b-1 . . . 120.654(2) ? C15b-1 C18b-1 C23b-1 . . . 121.693(2) ? C19b-1 C18b-1 C23b-1 . . . 117.653(2) ? C15b-2 C18b-2 C19b-2 . . . 120.9003(19) ? C15b-2 C18b-2 C23b-2 . . 1_655 121.669(2) ? C19b-2 C18b-2 C23b-2 . . 1_655 117.4222(19) ? C18a-1 C19a-1 C20a-1 . . . 122.583(2) ? C18a-1 C19a-1 H1c19a-1 . . . 118.709(2) ? C20a-1 C19a-1 H1c19a-1 . . . 118.708(2) ? C18a-2 C19a-2 C20a-2 . . . 121.446(2) ? C18a-2 C19a-2 H1c19a-2 . . . 119.2752(19) ? C20a-2 C19a-2 H1c19a-2 . . . 119.2792(19) ? C18b-1 C19b-1 C20b-1 . . . 120.369(2) ? C18b-1 C19b-1 H1c19b-1 . . . 119.816(2) ? C20b-1 C19b-1 H1c19b-1 . . . 119.814(2) ? C18b-2 C19b-2 C20b-2 . . . 121.4917(19) ? C18b-2 C19b-2 H1c19b-2 . . . 119.2560(19) ? C20b-2 C19b-2 H1c19b-2 . . . 119.252(2) ? C19a-1 C20a-1 C21a-1 . . . 119.526(2) ? C19a-1 C20a-1 H1c20a-1 . . . 120.237(2) ? C21a-1 C20a-1 H1c20a-1 . . . 120.237(2) ? C19a-2 C20a-2 C21a-2 . . . 120.0995(19) ? C19a-2 C20a-2 H1c20a-2 . . . 119.948(2) ? C21a-2 C20a-2 H1c20a-2 . . . 119.9525(19) ? C19b-1 C20b-1 C21b-1 . . . 121.281(2) ? C19b-1 C20b-1 H1c20b-1 . . . 119.359(2) ? C21b-1 C20b-1 H1c20b-1 . . . 119.360(2) ? C19b-2 C20b-2 C21b-2 . . 1_655 120.624(2) ? C19b-2 C20b-2 H1c20b-2 . . . 119.6901(19) ? C21b-2 C20b-2 H1c20b-2 1_655 . . 119.6859(19) ? C20a-1 C21a-1 C22a-1 . . 1_545 119.396(2) ? C20a-1 C21a-1 H1c21a-1 . . 1_545 120.302(2) ? C22a-1 C21a-1 H1c21a-1 1_545 . 1_545 120.301(2) ? C20a-2 C21a-2 C22a-2 . . 1_545 119.3616(19) ? C20a-2 C21a-2 H1c21a-2 . . 1_545 120.3176(19) ? C22a-2 C21a-2 H1c21a-2 1_545 . 1_545 120.321(2) ? C20b-1 C21b-1 C22b-1 . . . 118.293(2) ? C20b-1 C21b-1 H1c21b-1 . . . 120.855(2) ? C22b-1 C21b-1 H1c21b-1 . . . 120.852(2) ? C20b-2 C21b-2 C22b-2 1_455 . . 118.5023(19) ? C20b-2 C21b-2 H1c21b-2 1_455 . . 120.748(2) ? C22b-2 C21b-2 H1c21b-2 . . . 120.7501(19) ? C21a-1 C22a-1 C23a-1 1_565 . 1_565 119.993(2) ? C21a-1 C22a-1 H1c22a-1 1_565 . . 120.003(2) ? C23a-1 C22a-1 H1c22a-1 1_565 . . 120.004(2) ? C21a-2 C22a-2 C23a-2 1_565 . . 120.972(2) ? C21a-2 C22a-2 H1c22a-2 1_565 . . 119.5131(19) ? C23a-2 C22a-2 H1c22a-2 . . . 119.5145(19) ? C21b-1 C22b-1 C23b-1 . . . 121.594(2) ? C21b-1 C22b-1 H1c22b-1 . . . 119.204(2) ? C23b-1 C22b-1 H1c22b-1 . . . 119.202(2) ? C21b-2 C22b-2 C23b-2 . . . 121.254(2) ? C21b-2 C22b-2 H1c22b-2 . . . 119.3688(19) ? C23b-2 C22b-2 H1c22b-2 . . . 119.378(2) ? C18a-1 C23a-1 C22a-1 . . 1_545 122.192(2) ? C18a-1 C23a-1 H1c23a-1 . . 1_545 118.905(2) ? C22a-1 C23a-1 H1c23a-1 1_545 . 1_545 118.903(2) ? C18a-2 C23a-2 C22a-2 1_565 . . 120.6793(19) ? C18a-2 C23a-2 H1c23a-2 1_565 . . 119.6587(19) ? C22a-2 C23a-2 H1c23a-2 . . . 119.662(2) ? C18b-1 C23b-1 C22b-1 . . . 120.802(2) ? C18b-1 C23b-1 H1c23b-1 . . . 119.596(2) ? C22b-1 C23b-1 H1c23b-1 . . . 119.602(2) ? C18b-2 C23b-2 C22b-2 1_455 . . 120.643(2) ? C18b-2 C23b-2 H1c23b-2 1_455 . . 119.6810(19) ? C22b-2 C23b-2 H1c23b-2 . . . 119.676(2) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C3b-1 H1c3b-1 O2b-2 . . . 0.96 3.00 3.9236 161.88 ? C4a-1 H1c4a-1 O3a-2 . . 1_455 0.96 2.77 3.4434 128.27 ? C4a-1 H1c4a-1 C10a-2 . . 1_455 0.96 2.98 3.7486 138.45 ? C4a-2 H1c4a-2 O3a-1 . . . 0.96 2.75 3.4260 127.83 ? C4a-2 H1c4a-2 C10a-1 . . . 0.96 2.93 3.7492 144.34 ? C6b-1 H1c6b-1 O3b-1 . . . 0.96 2.88 3.5939 131.70 ? C6b-2 H1c6b-2 O3b-2 . . . 0.96 2.83 3.5523 132.43 ? C7a-1 H1c7a-1 C21b-2 . . . 0.96 2.99 3.7658 139.35 ? C7a-2 H1c7a-2 C21b-1 . . . 0.96 2.97 3.7607 140.04 ? C7b-2 H1c7b-2 C21a-2 . . 1_565 0.96 2.97 3.8098 146.59 ? C9a-1 H1c9a-1 C1a-2 . . . 0.96 2.86 3.6920 145.38 ? C9a-2 H1c9a-2 O1a-1 . . 1_665 0.96 2.95 3.8977 168.76 ? C9a-2 H1c9a-2 C1a-1 . . 1_655 0.96 2.85 3.6445 141.06 ? C10a-1 H1c10a-1 O2a-2 . . 2_655 0.96 2.72 3.6500 162.63 ? C10a-2 H1c10a-2 O2a-1 . . 2_655 0.96 2.68 3.6154 163.78 ? C10b-1 H1c10b-1 O2b-2 . . 4_655 0.96 2.74 3.6551 158.90 ? C10b-2 H1c10b-2 O2b-1 . . 4_555 0.96 2.73 3.6457 159.21 ? N1a-1 H1n1a-1 O3a-2 . . 1_455 0.91 1.97 2.8328 156.81 ? N1a-2 H1n1a-2 O3a-1 . . . 0.92 1.95 2.8255 156.64 ? N1b-1 H1n1b-1 O3b-2 . . . 0.92 2.00 2.8742 158.48 ? N1b-2 H1n1b-2 O3b-1 . . . 0.91 1.98 2.8516 159.03 ? C13a-1 H1c13a-1 C21b-1 . . . 0.96 2.97 3.6499 128.46 ? C13b-1 H1c13b-1 C8b-2 . . . 0.96 2.90 3.8241 161.36 ? C13b-2 H1c13b-2 C8b-1 . . . 0.96 3.00 3.9032 157.77 ? C14a-1 H1c14a-1 C22b-1 . . . 0.96 2.91 3.6389 134.03 ? C14a-1 H1c14a-1 C23b-1 . . . 0.96 2.88 3.7966 161.21 ? C14a-2 H1c14a-2 C23b-2 . . 1_655 0.96 2.93 3.7487 144.46 ? C16b-1 H1c16b-1 C19a-2 . . . 0.96 2.95 3.8955 169.74 ? C16b-1 H1c16b-1 C20a-2 . . . 0.96 2.74 3.5551 143.47 ? C17a-2 H1c17a-2 O3a-1 . . . 0.96 2.97 3.6900 132.51 ? C19a-2 H1c19a-2 C15b-2 . . . 0.96 2.97 3.6762 131.32 ? C19a-2 H1c19a-2 C18b-2 . . . 0.96 2.99 3.8803 155.54 ? C19b-2 H1c19b-2 C22a-2 . . . 0.96 2.94 3.8812 168.06 ? C19b-2 H1c19b-2 C23a-2 . . . 0.96 2.80 3.5858 140.21 ? C20a-1 H1c20a-1 C16b-1 . . . 0.96 2.93 3.6124 128.84 ? C20a-1 H1c20a-1 C17b-1 . . . 0.96 2.87 3.7430 151.33 ? C20a-2 H1c20a-2 C16b-2 . . 1_655 0.96 2.95 3.6752 133.58 ? C20a-2 H1c20a-2 C17b-2 . . 1_655 0.96 2.85 3.7683 160.85 ? C20b-1 H1c20b-1 C16a-1 . . 1_565 0.96 2.99 3.9214 164.76 ? C22a-2 H1c22a-2 C18b-1 . . . 0.96 2.97 3.6792 131.58 ? C22b-2 H1c22b-2 C13a-1 . . . 0.96 2.98 3.9315 169.21 ? C22b-2 H1c22b-2 C14a-1 . . . 0.96 2.79 3.5900 141.73 ? C23a-1 H1c23a-1 C20b-2 1_565 . 1_455 0.96 2.87 3.7033 146.27 ? C23a-2 H1c23a-2 C19b-1 . . . 0.96 2.96 3.6726 131.95 ? C23a-2 H1c23a-2 C20b-1 . . . 0.96 2.84 3.7513 159.42 ? C23b-1 H1c23b-1 C19a-2 . . . 0.96 2.91 3.8350 162.08 ? C21a-1 H1c21a-1 C7b-2 1_565 . 1_455 0.96 2.97 3.7140 135.14 ? C21a-1 H1c21a-1 C8b-2 1_565 . . 0.96 2.85 3.7122 149.51 ? C21a-2 H1c21a-2 C7b-1 1_565 . . 0.96 2.95 3.6875 134.39 ? C21a-2 H1c21a-2 C8b-1 1_565 . . 0.96 2.82 3.6760 149.45 ? C21b-1 H1c21b-1 C8a-1 . . . 0.96 2.99 3.7822 141.12 ? C21b-2 H1c21b-2 C8a-2 . . 1_455 0.96 2.97 3.7816 142.49 ? C1b-1 H1c1b-1 C5b-1 . . 1_565 0.96 2.95 3.8528 156.47 ? C1b-1 H1c1b-1 C10b-1 . . . 0.96 2.85 3.6200 137.59 ? C1b-2 H1c1b-2 C5b-2 . . 1_565 0.96 2.99 3.8798 155.14 ? C1b-2 H1c1b-2 C10b-2 . . 1_655 0.96 2.87 3.6327 137.52 ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_include_status 2 0 0 27.61 110.52 44.55 < 4 0 0 43557.60 36295.60 892.23 o 6 0 0 1458.17 1727.56 93.47 o 8 0 0 1093.46 1387.70 149.82 o 10 0 0 1300.07 1296.56 129.96 o 2 -1 0 89175.50 86519.60 756.74 o 4 1 0 6949.23 6395.43 389.94 o 4 -1 0 6927.98 6333.58 358.99 o 6 1 0 5041.13 5489.46 167.48 o 6 -1 0 5074.50 5503.42 168.67 o 8 1 0 1182.78 1517.52 110.14 o 8 -1 0 1183.84 1560.60 165.50 o 10 1 0 668.99 360.33 88.68 o 10 -1 0 678.84 550.79 94.01 o 0 2 0 23008.00 23451.90 425.91 o 2 2 0 103560.00 100815.00 1249.74 o 2 -2 0 103454.00 103424.00 922.69 o 4 2 0 1406.32 1762.75 227.45 o 4 -2 0 1394.55 1749.82 119.27 o 6 2 0 1675.29 1795.06 106.64 o 8 2 0 1379.38 1643.43 157.37 o 8 -2 0 1391.83 1600.34 166.56 o 10 2 0 721.44 1396.94 136.24 o 10 -2 0 723.49 656.45 99.70 o 2 3 0 8842.99 8297.39 393.90 o 4 3 0 3847.15 4055.16 198.35 o 4 -3 0 3790.59 3795.58 187.47 o 6 3 0 6470.75 6437.05 277.57 o 6 -3 0 6463.39 6102.50 283.58 o 8 3 0 19856.60 19363.50 552.85 o 8 -3 0 19817.70 20418.10 575.38 o 0 4 0 584.26 684.04 65.74 o 2 4 0 1462.06 1398.10 74.31 o 4 4 0 26003.30 25789.20 340.52 o 6 4 0 3164.52 2717.35 198.11 o 8 4 0 2511.61 2724.94 216.07 o 8 -4 0 2536.07 3004.80 233.51 o 10 -4 0 287.80 314.51 69.16 o 2 5 0 3098.49 3121.35 118.14 o 4 5 0 4796.52 3956.48 220.07 o 6 5 0 4752.91 4473.75 261.05 o 8 -5 0 6106.88 6420.51 226.32 o 10 -5 0 485.60 386.58 66.76 o 0 6 0 13857.90 15038.10 404.56 o 2 6 0 1085.37 1217.58 85.90 o 4 6 0 542.22 598.36 101.54 o 6 6 0 6379.57 6224.42 315.30 o 6 -6 0 6367.13 6892.00 240.40 o 8 -6 0 756.52 905.54 78.88 o 2 7 0 10555.00 11100.60 400.13 o 4 7 0 14256.50 13890.80 470.57 o 4 -7 0 14256.40 14620.00 341.48 o 6 -7 0 24.53 110.86 50.48 < 8 -7 0 424.35 604.80 67.55 o 2 -8 0 4096.01 4270.91 287.20 o 4 -8 0 2287.17 2060.13 128.32 o 6 -8 0 483.38 515.65 59.04 o 2 -9 0 5277.88 4751.36 184.94 o 0 -10 0 1546.75 1683.68 123.32 o 2 -10 0 2153.62 2174.97 140.05 o -11 0 1 1.51 27.87 28.95 < -9 0 1 466.97 487.76 70.69 o -7 0 1 859.97 918.98 76.04 o -5 0 1 8.65 -0.16 25.71 < -3 0 1 407.48 372.26 77.66 o 1 0 1 0.97 -22.81 15.12 < 3 0 1 1686.25 1342.89 140.75 o 5 0 1 31.00 -27.95 35.67 < 7 0 1 606.66 465.62 56.83 o 9 0 1 283.24 307.52 47.16 o 11 0 1 23.65 -0.82 30.72 < -11 1 1 381.44 441.28 70.50 o -11 -1 1 381.33 401.92 73.50 o -9 1 1 320.67 371.60 54.88 o -9 -1 1 320.82 283.00 61.13 o -7 1 1 83.61 111.36 36.70 o -7 -1 1 83.46 86.99 47.92 < -5 1 1 12.95 10.91 20.60 < -5 -1 1 12.81 11.62 21.31 < -3 1 1 214.92 137.76 53.91 < -3 -1 1 215.08 124.90 36.52 o -1 1 1 25.94 38.28 32.85 < -1 -1 1 25.88 46.11 19.31 < 1 -1 1 115.44 62.15 22.74 < 3 1 1 606.01 509.08 100.40 o 3 -1 1 606.70 525.71 62.78 o 5 1 1 145.27 187.15 31.03 o 5 -1 1 145.76 184.49 34.85 o 7 1 1 274.39 312.21 51.13 o 7 -1 1 275.68 216.63 55.22 o 9 1 1 681.52 628.13 112.71 o 9 -1 1 681.55 654.06 71.84 o 11 1 1 207.52 185.24 60.17 o 11 -1 1 207.51 212.56 51.01 o -11 2 1 101.48 75.11 31.14 < -11 -2 1 101.94 69.15 46.79 < -9 2 1 237.12 183.13 58.51 o -9 -2 1 237.25 255.77 59.31 o -7 2 1 222.18 164.78 41.18 o -7 -2 1 222.34 79.85 42.65 < -5 2 1 238.41 252.30 35.65 o -5 -2 1 238.91 269.51 39.20 o -3 2 1 653.21 607.83 123.40 o -1 2 1 135.51 181.58 54.65 o 1 2 1 558.66 379.64 69.26 o 3 2 1 83.14 105.18 58.13 < 5 2 1 587.34 491.05 47.26 o 5 -2 1 586.25 573.12 54.93 o 7 2 1 33.80 40.55 27.74 < 7 -2 1 33.99 42.15 37.88 < 9 2 1 386.68 227.23 60.07 o 9 -2 1 387.08 366.36 66.57 o 11 2 1 62.32 30.48 19.52 < 11 -2 1 62.55 98.98 40.02 < -9 -3 1 75.37 109.96 45.71 < -7 3 1 167.54 216.97 53.16 o -7 -3 1 168.38 293.26 66.68 o -5 3 1 654.12 728.63 86.49 o -5 -3 1 653.33 599.72 81.38 o -3 3 1 177.21 248.87 51.74 o -1 3 1 1209.02 1145.57 127.12 o 1 3 1 2335.66 1944.77 172.27 o 3 3 1 346.18 319.75 39.23 o 5 3 1 221.73 170.47 48.72 o 5 -3 1 222.04 184.54 62.34 < 7 3 1 9.66 27.37 33.14 < 7 -3 1 9.75 -28.64 39.33 < 9 -3 1 20.65 84.20 32.88 < -9 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3 1 93 6.42 -22.42 39.49 < 3 -1 93 6.65 37.88 32.30 < -3 2 93 29.28 40.65 22.52 < -3 -2 93 29.04 76.74 30.32 < -1 2 93 12.21 72.79 40.78 < 1 2 93 7.91 39.02 36.01 < -1 3 93 102.02 45.15 23.82 < 1 3 93 9.86 -16.28 39.20 < -4 0 94 563.29 562.80 81.74 o -2 0 94 28.64 -38.83 46.23 < 0 0 94 678.89 708.77 94.22 o 2 0 94 13.79 69.18 26.74 < -2 1 94 1015.17 838.06 100.39 o 0 1 94 3375.36 3801.52 213.88 o 2 1 94 903.46 901.60 98.57 o 2 -1 94 910.53 802.14 95.20 o -2 2 94 1480.47 1508.41 90.21 o -2 -2 94 1488.40 1667.88 129.17 o 0 2 94 109.78 105.04 45.39 < 2 2 94 310.36 198.93 45.09 o 2 -2 94 306.76 220.56 34.02 o 0 3 94 648.30 895.28 95.17 o -3 0 95 15.65 20.47 19.34 < -1 0 95 2.15 -6.53 28.19 < 1 0 95 0.08 -5.53 23.10 < 3 0 95 27.19 1.66 32.35 < -3 1 95 24.37 10.09 18.68 < -3 -1 95 24.13 -38.57 34.09 < -1 1 95 90.21 135.52 57.96 < 1 1 95 35.47 29.56 27.71 < 3 1 95 21.86 -11.51 35.01 < 3 -1 95 21.48 119.21 48.92 < -1 2 95 5.49 38.41 39.78 < 1 2 95 0.58 -81.83 48.34 < -2 0 96 720.02 680.88 83.19 o 0 0 96 21.54 112.15 43.65 < 2 0 96 1199.71 1273.74 110.98 o -2 1 96 85.36 46.37 33.35 < 0 1 96 470.95 669.72 88.10 o 2 1 96 397.70 557.16 53.74 o 2 -1 96 403.38 469.12 63.33 o -2 2 96 1290.87 1506.80 120.50 o 0 2 96 480.71 603.41 80.73 o -1 0 97 8.76 48.63 32.67 < 1 0 97 71.13 162.31 42.39 o -1 1 97 44.71 1.26 30.51 < 1 1 97 29.05 16.97 35.38 < -1 2 97 71.07 114.04 31.35 o 1 2 97 24.91 12.38 34.91 < 0 0 98 917.23 1132.70 103.07 o 0 1 98 3357.71 3885.35 191.16 o # start Validation Reply Form #_vrf_SYMMG01_I #; #PROBLEM: Unrecognised _symmetry_space_group_name_H-M #RESPONSE: The standard space group symmetry for B21 #reported here is P21. #The non-standard setting is used in order to maintain #unique phase relations with the crystal structure at T = 160 K #; #_vrf_SYMMG02_I #; #PROBLEM: Supplied _symmetry_space_group_name_H-M not recognised #RESPONSE: see response to _vrf_SYMMG01_I #; #_vrf_PLAT027_I #; #PROBLEM: _diffrn_reflns_theta_full value (too) Low ...... 65.45 Degree #RESPONSE: CuKalpha wavelength necessarily limits data resolution #using in-house sources. #; #_vrf_PLAT075_I #; #PROBLEM: Occupancy 2.000 Greater Than 1.0 for ...... C4A-2 #RESPONSE: Checkcif reports occupancy of 2 because it performs #the checks using B2 while the correct symmetry is B21. #; #_vrf_PLAT310_I #; #PROBLEM: H999 Deleted (Close to C20B-1 ) Dist ... 0.144 Ang. #RESPONSE: Checkcif reports occupancy of 2 because it performs #the checks using B2 while the correct symmetry is B21. #; #_vrf_PLAT413_I #; #PROBLEM: Short Inter XH3 .. XHn H2C1B-2 ..H3C1B-1 . 1.79 Ang. #RESPONSE: see response to _vrf_PLAT075_I #; #_vrf_PLAT430_I #; #PROBLEM: Short Inter D...A Contact O2A-1 ..O2A-2 . 2.16 Ang. #RESPONSE: see response to _vrf_PLAT075_I #; #_vrf_PLAT727_I #; #PROBLEM: D...A Calc 20.3366(7), Rep 3.65000 Dev... 16.69 Ang. #RESPONSE: see response to _vrf_PLAT075_I #; # end Validation Reply Form