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#\#CIF_1.1 ################################################################################ # # # 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 : 02/11/2015' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_name_full 'Inorganic Chemistry' _journal_year 2016 _journal_volume 55 _journal_page_first 7764 _journal_page_last 7776 _journal_paper_doi http://dx.doi.org/10.1021/acs.inorgchem.6b01233 #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name 'Nilges, Tom' _publ_contact_author_address ;Department of Chemistry Synthesis and Characterization of Innovative Materials Technical University Munich Lichtenbergstrasse 4 85747 Garching Germany ; _publ_contact_author_email 'tom.nilges@lrz.tum.de' _publ_contact_author_fax '+49-(0)89-289-13762' _publ_contact_author_phone '+49-(0)89-289-13110' #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ;Polymorphism in Zintl-Phases ACd~4~Pn~3~: The modulated structures of NaCd~4~Pn~3~ with Pn = P, As ; loop_ _publ_author_name _publ_author_address 'Grotz, Carolin' ;Department of Chemistry Synthesis and Characterization of Innovative Materials Technical University Munich Lichtenbergstrasse 4 85747 Garching Germany ; 'Baumgartner, Maximilian' ;Department of Chemistry Synthesis and Characterization of Innovative Materials Technical University Munich Lichtenbergstrasse 4 85747 Garching Germany ; 'Freitag, Katharina M.' ;Department of Chemistry Synthesis and Characterization of Innovative Materials Technical University Munich Lichtenbergstrasse 4 85747 Garching Germany ; 'Baumer, Franziska' ;Department of Chemistry Synthesis and Characterization of Innovative Materials Technical University Munich Lichtenbergstrasse 4 85747 Garching Germany ; 'Nilges, Tom' ;Department of Chemistry Synthesis and Characterization of Innovative Materials Technical University Munich Lichtenbergstrasse 4 85747 Garching Germany ; #======================================================================= # 4. TEXT _publ_section_references ; Petricek, V., Dusek, M. & Palatinus L. (2014). Z. Kristallogr. 229(5), 345-352. Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790. Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. ; #======================================================================= data_As3Cd4Na1_298 #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'As3 Cd4 Na1' _chemical_formula_weight 697.4 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system trigonal _space_group_name_H-M_alt 'R -3 m' _space_group_name_Hall '-R 3 2"' _space_group_IT_number 166 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 y,x,-z 5 x-y,-y,-z 6 -x,-x+y,-z 7 -x,-y,-z 8 y,-x+y,-z 9 x-y,x,-z 10 -y,-x,z 11 -x+y,y,z 12 x,x-y,z 13 x+2/3,y+1/3,z+1/3 14 -y+2/3,x-y+1/3,z+1/3 15 -x+y+2/3,-x+1/3,z+1/3 16 y+2/3,x+1/3,-z+1/3 17 x-y+2/3,-y+1/3,-z+1/3 18 -x+2/3,-x+y+1/3,-z+1/3 19 -x+2/3,-y+1/3,-z+1/3 20 y+2/3,-x+y+1/3,-z+1/3 21 x-y+2/3,x+1/3,-z+1/3 22 -y+2/3,-x+1/3,z+1/3 23 -x+y+2/3,y+1/3,z+1/3 24 x+2/3,x-y+1/3,z+1/3 25 x+1/3,y+2/3,z+2/3 26 -y+1/3,x-y+2/3,z+2/3 27 -x+y+1/3,-x+2/3,z+2/3 28 y+1/3,x+2/3,-z+2/3 29 x-y+1/3,-y+2/3,-z+2/3 30 -x+1/3,-x+y+2/3,-z+2/3 31 -x+1/3,-y+2/3,-z+2/3 32 y+1/3,-x+y+2/3,-z+2/3 33 x-y+1/3,x+2/3,-z+2/3 34 -y+1/3,-x+2/3,z+2/3 35 -x+y+1/3,y+2/3,z+2/3 36 x+1/3,x-y+2/3,z+2/3 _cell_length_a 4.4616(3) _cell_length_b 4.4616(3) _cell_length_c 33.783(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 582.38(7) _cell_formula_units_Z 3 _cell_measurement_reflns_used 6126 _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 32.27 _cell_measurement_temperature 298 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 5.9655 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 23.714 _exptl_crystal_description plate _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.040 _exptl_crystal_size_rad ? _exptl_crystal_colour black _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'Jana2006' _exptl_absorpt_correction_T_min 0.0173 _exptl_absorpt_correction_T_max 0.2693 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0233 70 -30 999 0.1057 -1 5 -30 0.1002 0 -1 -30 0.0388 1 5 -30 0.0734 -1 -2 -15 0.0943 21 -23 999 0.0386 1 0 -30 0.0608 -3 1 -30 0.1118 0 0 -1 0.0370 -1 1 15 0.1021 1 4 -30 0.0962 -1 -3 30 0.0860 0 1 30 0.0482 1 -1 -15 0.0851 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 298 _diffrn_source_power 2 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'IPDS Stoe' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '??integration method??' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 1353 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 31.91 _diffrn_reflns_theta_full 31.91 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_unetI/netI 0.0444 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _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 172 _reflns_number_gt 169 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_gt 0.1097 _refine_ls_R_factor_all 0.0485 _refine_ls_wR_factor_ref 0.1098 _refine_ls_goodness_of_fit_ref 3.68 _refine_ls_goodness_of_fit_gt 3.71 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 172 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0004I^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0049 _refine_ls_shift/su_mean 0.0017 _refine_diff_density_max 1.84 _refine_diff_density_min -2.39 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 1530(170) _refine_ls_abs_structure_details ? _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 As 0.0511 2.0283 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Cd -0.7834 1.2309 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Na 0.0374 0.0259 '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 Cd1 Cd 0 0 0.09583(5) Uani 0.0318(7) 6 1 d . . . As1 As 0 0 0.22070(5) Uani 0.0121(7) 6 1 d . . . Cd2 Cd 0 0 0.29896(4) Uani 0.0300(7) 6 1 d . . . Na1 Na 0 0 0.5 Uani 0.026(3) 3 1 d . . . As2 As 0 0 0 Uani 0.0157(8) 3 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 Cd1 Cd 0.0127(8) 0.0127(8) 0.0700(14) 0.0064(4) 0 0 As1 As 0.0098(8) 0.0098(8) 0.0165(12) 0.0049(4) 0 0 Cd2 Cd 0.0361(9) 0.0361(9) 0.0178(10) 0.0180(5) 0 0 Na1 Na 0.035(4) 0.035(4) 0.008(5) 0.018(2) 0 0 As2 As 0.0144(10) 0.0144(10) 0.0183(15) 0.0072(5) 0 0 #======================================================================= # 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 Cd1 As1 . 16_445 2.6377(7) ? Cd1 As1 . 16_455 2.6377(6) ? Cd1 As1 . 16_555 2.6377(7) ? Cd1 Na1 . 25_444 3.5159(13) ? Cd1 Na1 . 25_544 3.5159(13) ? Cd1 Na1 . 25_554 3.5159(13) ? As1 Cd2 . . 2.644(2) ? As1 Na1 . 25_444 3.1572(10) ? As1 Na1 . 25_544 3.1572(10) ? As1 Na1 . 25_554 3.1572(10) ? Cd2 As2 . 13_445 2.8255(7) ? Cd2 As2 . 13_455 2.8255(6) ? Cd2 As2 . 13_555 2.8255(7) ? 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 As1 Cd1 As1 16_445 . 16_455 115.50(3) ? As1 Cd1 As1 16_445 . 16_555 115.50(3) ? As1 Cd1 Na1 16_445 . 25_444 59.72(3) ? As1 Cd1 Na1 16_445 . 25_544 59.72(3) ? As1 Cd1 Na1 16_445 . 25_554 124.69(7) ? As1 Cd1 As1 16_455 . 16_555 115.50(3) ? As1 Cd1 Na1 16_455 . 25_444 59.72(3) ? As1 Cd1 Na1 16_455 . 25_544 124.69(7) ? As1 Cd1 Na1 16_455 . 25_554 59.72(3) ? As1 Cd1 Na1 16_555 . 25_444 124.69(7) ? As1 Cd1 Na1 16_555 . 25_544 59.72(3) ? As1 Cd1 Na1 16_555 . 25_554 59.72(3) ? Na1 Cd1 Na1 25_444 . 25_544 78.76(3) ? Na1 Cd1 Na1 25_444 . 25_554 78.76(3) ? Na1 Cd1 Na1 25_544 . 25_554 78.76(3) ? Cd1 As1 Cd1 16_445 . 16_455 115.50(3) ? Cd1 As1 Cd1 16_445 . 16_555 115.50(3) ? Cd1 As1 Cd2 16_445 . . 77.58(5) ? Cd1 As1 Na1 16_445 . 25_444 74.10(3) ? Cd1 As1 Na1 16_445 . 25_544 74.10(3) ? Cd1 As1 Na1 16_445 . 25_554 157.10(7) ? Cd1 As1 Cd1 16_455 . 16_555 115.50(3) ? Cd1 As1 Cd2 16_455 . . 77.58(5) ? Cd1 As1 Na1 16_455 . 25_444 74.10(3) ? Cd1 As1 Na1 16_455 . 25_544 157.10(7) ? Cd1 As1 Na1 16_455 . 25_554 74.10(3) ? Cd1 As1 Cd2 16_555 . . 77.58(5) ? Cd1 As1 Na1 16_555 . 25_444 157.10(7) ? Cd1 As1 Na1 16_555 . 25_544 74.10(3) ? Cd1 As1 Na1 16_555 . 25_554 74.10(3) ? Cd2 As1 Na1 . . 25_444 125.32(2) ? Cd2 As1 Na1 . . 25_544 125.32(2) ? Cd2 As1 Na1 . . 25_554 125.32(2) ? Na1 As1 Na1 25_444 . 25_544 89.92(3) ? Na1 As1 Na1 25_444 . 25_554 89.92(3) ? Na1 As1 Na1 25_544 . 25_554 89.92(3) ? As1 Cd2 As2 . . 13_445 114.27(3) ? As1 Cd2 As2 . . 13_455 114.27(3) ? As1 Cd2 As2 . . 13_555 114.27(3) ? As2 Cd2 As2 13_445 . 13_455 104.28(3) ? As2 Cd2 As2 13_445 . 13_555 104.28(3) ? As2 Cd2 As2 13_455 . 13_555 104.28(3) ? Cd1 Na1 Cd1 13_445 . 13_455 78.76(2) ? Cd1 Na1 Cd1 13_445 . 13_555 78.76(2) ? Cd1 Na1 Cd1 13_445 . 28_445 101.24(2) ? Cd1 Na1 Cd1 13_445 . 28_545 101.24(2) ? Cd1 Na1 Cd1 13_445 . 28_555 180.0(5) ? Cd1 Na1 As1 13_445 . 13_445 78.22(3) ? Cd1 Na1 As1 13_445 . 13_455 133.821(13) ? Cd1 Na1 As1 13_445 . 13_555 133.821(13) ? Cd1 Na1 As1 13_445 . 28_445 46.179(13) ? Cd1 Na1 As1 13_445 . 28_545 46.179(13) ? Cd1 Na1 As1 13_445 . 28_555 101.78(3) ? Cd1 Na1 Cd1 13_455 . 13_555 78.76(2) ? Cd1 Na1 Cd1 13_455 . 28_445 101.24(2) ? Cd1 Na1 Cd1 13_455 . 28_545 180.0(5) ? Cd1 Na1 Cd1 13_455 . 28_555 101.24(2) ? Cd1 Na1 As1 13_455 . 13_445 133.821(13) ? Cd1 Na1 As1 13_455 . 13_455 78.22(3) ? Cd1 Na1 As1 13_455 . 13_555 133.821(13) ? Cd1 Na1 As1 13_455 . 28_445 46.179(13) ? Cd1 Na1 As1 13_455 . 28_545 101.78(3) ? Cd1 Na1 As1 13_455 . 28_555 46.179(13) ? Cd1 Na1 Cd1 13_555 . 28_445 180.0(5) ? Cd1 Na1 Cd1 13_555 . 28_545 101.24(2) ? Cd1 Na1 Cd1 13_555 . 28_555 101.24(2) ? Cd1 Na1 As1 13_555 . 13_445 133.821(13) ? Cd1 Na1 As1 13_555 . 13_455 133.821(13) ? Cd1 Na1 As1 13_555 . 13_555 78.22(3) ? Cd1 Na1 As1 13_555 . 28_445 101.78(3) ? Cd1 Na1 As1 13_555 . 28_545 46.179(13) ? Cd1 Na1 As1 13_555 . 28_555 46.179(13) ? Cd1 Na1 Cd1 28_445 . 28_545 78.76(2) ? Cd1 Na1 Cd1 28_445 . 28_555 78.76(2) ? Cd1 Na1 As1 28_445 . 13_445 46.179(13) ? Cd1 Na1 As1 28_445 . 13_455 46.179(13) ? Cd1 Na1 As1 28_445 . 13_555 101.78(3) ? Cd1 Na1 As1 28_445 . 28_445 78.22(3) ? Cd1 Na1 As1 28_445 . 28_545 133.821(13) ? Cd1 Na1 As1 28_445 . 28_555 133.821(13) ? Cd1 Na1 Cd1 28_545 . 28_555 78.76(2) ? Cd1 Na1 As1 28_545 . 13_445 46.179(13) ? Cd1 Na1 As1 28_545 . 13_455 101.78(3) ? Cd1 Na1 As1 28_545 . 13_555 46.179(13) ? Cd1 Na1 As1 28_545 . 28_445 133.821(13) ? Cd1 Na1 As1 28_545 . 28_545 78.22(3) ? Cd1 Na1 As1 28_545 . 28_555 133.821(13) ? Cd1 Na1 As1 28_555 . 13_445 101.78(3) ? Cd1 Na1 As1 28_555 . 13_455 46.179(13) ? Cd1 Na1 As1 28_555 . 13_555 46.179(13) ? Cd1 Na1 As1 28_555 . 28_445 133.821(13) ? Cd1 Na1 As1 28_555 . 28_545 133.821(13) ? Cd1 Na1 As1 28_555 . 28_555 78.22(3) ? As1 Na1 As1 13_445 . 13_455 89.92(2) ? As1 Na1 As1 13_445 . 13_555 89.92(2) ? As1 Na1 As1 13_445 . 28_445 90.08(2) ? As1 Na1 As1 13_445 . 28_545 90.08(2) ? As1 Na1 As1 13_445 . 28_555 180.0(5) ? As1 Na1 As1 13_455 . 13_555 89.92(2) ? As1 Na1 As1 13_455 . 28_445 90.08(2) ? As1 Na1 As1 13_455 . 28_545 180.0(5) ? As1 Na1 As1 13_455 . 28_555 90.08(2) ? As1 Na1 As1 13_555 . 28_445 180.0(5) ? As1 Na1 As1 13_555 . 28_545 90.08(2) ? As1 Na1 As1 13_555 . 28_555 90.08(2) ? As1 Na1 As1 28_445 . 28_545 89.92(2) ? As1 Na1 As1 28_445 . 28_555 89.92(2) ? As1 Na1 As1 28_545 . 28_555 89.92(2) ? Cd2 As2 Cd2 25_444 . 25_544 104.28(2) ? Cd2 As2 Cd2 25_444 . 25_554 104.28(2) ? Cd2 As2 Cd2 25_444 . 16_445 75.72(2) ? Cd2 As2 Cd2 25_444 . 16_455 75.72(2) ? Cd2 As2 Cd2 25_444 . 16_555 180.0(5) ? Cd2 As2 Cd2 25_544 . 25_554 104.28(2) ? Cd2 As2 Cd2 25_544 . 16_445 75.72(2) ? Cd2 As2 Cd2 25_544 . 16_455 180.0(5) ? Cd2 As2 Cd2 25_544 . 16_555 75.72(2) ? Cd2 As2 Cd2 25_554 . 16_445 180.0(5) ? Cd2 As2 Cd2 25_554 . 16_455 75.72(2) ? Cd2 As2 Cd2 25_554 . 16_555 75.72(2) ? Cd2 As2 Cd2 16_445 . 16_455 104.28(2) ? Cd2 As2 Cd2 16_445 . 16_555 104.28(2) ? Cd2 As2 Cd2 16_455 . 16_555 104.28(2) ? #======================================================================= # 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 -1 2 0 410024.00 352571.00 42264.00 o 0 3 0 181183.00 174514.00 8163.94 o -2 4 0 130606.00 130172.00 2019.43 o -1 5 0 57313.90 63456.20 591.96 o -1 1 1 49911.00 45125.50 1479.59 o 0 2 1 33103.60 33007.60 292.14 o -2 3 1 25013.10 25608.50 356.77 o -4 4 1 13124.00 13107.40 139.14 o -1 4 1 15973.40 17389.70 539.16 o -3 5 1 10910.90 9862.32 1270.06 o 0 1 2 24550.90 21424.30 2010.98 o -2 2 2 12838.90 13374.10 49.77 o -1 3 2 7809.65 7398.47 714.93 o -3 4 2 3389.81 3256.07 36.86 o 0 4 2 2325.68 2440.26 32.93 o -2 5 2 1621.86 1551.87 29.07 o -1 2 3 5952.57 6060.06 137.02 o -3 3 3 1388.60 1498.97 17.71 o 0 3 3 1388.60 1352.23 54.39 o -2 4 3 682.55 769.52 84.52 o -4 5 3 50.64 133.47 17.63 o -1 5 3 50.64 95.70 30.22 o -1 1 4 18559.00 18108.10 607.44 o 0 2 4 10347.10 7832.77 2769.27 < -2 3 4 6713.10 6507.63 124.00 o -4 4 4 2111.25 1849.11 18.98 o -1 4 4 3081.60 3310.26 161.26 o -3 5 4 1451.35 1429.98 32.84 o 0 1 5 77052.50 67442.90 1260.22 o -2 2 5 39116.90 39649.00 1255.87 o -1 3 5 21682.00 20098.30 2711.05 o -3 4 5 8172.90 8739.77 93.98 o 0 4 5 5449.33 5737.09 264.14 o -2 5 5 3788.78 3671.49 297.17 o 0 0 6 13813.50 14467.40 417.24 o -1 2 6 9621.81 9777.02 98.36 o -3 3 6 6366.32 5992.34 39.85 o 0 3 6 6366.32 5480.66 1430.91 o -2 4 6 5454.13 5312.65 108.68 o -4 5 6 3699.39 3227.74 40.62 o -1 5 6 3699.39 3824.29 205.62 o -1 1 7 323.11 352.24 59.34 o 0 2 7 793.07 759.63 16.43 o -2 3 7 1182.36 1186.19 18.97 o -4 4 7 1618.65 1778.50 44.24 o -1 4 7 1565.54 1486.92 15.17 o -3 5 7 1617.85 1655.40 27.80 o 0 1 8 977.03 771.53 32.99 o -2 2 8 202.68 155.01 15.12 o -1 3 8 20.30 49.11 12.59 o -3 4 8 60.10 137.26 11.33 o 0 4 8 101.70 211.57 59.19 o -2 5 8 133.62 287.14 42.82 o 0 0 9 82403.40 96397.20 894.67 o -1 2 9 55399.80 46004.60 7791.24 o -3 3 9 34022.10 39480.40 226.20 o 0 3 9 34022.10 36774.30 474.74 o -2 4 9 27623.50 29781.40 492.04 o -1 1 10 298152.00 351633.00 38000.50 o 0 2 10 180879.00 146949.00 6630.71 o -2 3 10 119917.00 117717.00 4590.66 o -4 4 10 45054.90 48543.70 453.18 o -1 4 10 60567.30 62819.40 887.23 o -3 5 10 34245.50 36344.00 776.39 o 0 1 11 2296.55 2310.38 85.66 o -2 2 11 1766.61 1643.27 39.34 o -1 3 11 1445.35 1374.23 91.11 o -3 4 11 1085.05 893.93 16.41 o 0 4 11 969.37 1131.97 30.29 o -2 5 11 872.99 885.56 31.54 o 0 0 12 4379.28 5293.19 147.25 o -1 2 12 1847.98 2100.88 20.32 o -3 3 12 371.51 356.71 16.39 o 0 3 12 371.51 413.43 15.13 o -2 4 12 153.11 149.88 11.34 o -1 1 13 88984.10 56742.50 24848.60 < 0 2 13 57344.20 54828.20 256.43 o -2 3 13 39637.10 40280.30 194.09 o -4 4 13 15707.20 17058.50 240.21 o -1 4 13 20941.50 20492.70 498.79 o -3 5 13 11961.60 12248.70 301.08 o 0 1 14 36978.90 27458.00 6437.55 o -2 2 14 23978.80 23280.50 979.98 o -1 3 14 16467.10 15536.50 100.89 o -3 4 14 8386.04 7280.36 135.01 o 0 4 14 6131.52 6040.43 86.84 o 0 0 15 134347.00 139090.00 694.04 o -1 2 15 80098.40 68399.20 4261.81 o -3 3 15 35232.50 39893.10 2043.31 o 0 3 15 35232.50 28091.30 8453.63 o -2 4 15 25003.50 25751.80 447.67 o -1 1 16 22689.50 22157.80 635.33 o 0 2 16 17718.90 18032.70 350.89 o -2 3 16 14406.60 14206.90 290.90 o -4 4 16 8595.28 8281.88 404.40 o -1 4 16 10092.60 9969.03 41.30 o 0 1 17 10221.00 10172.10 259.03 o -2 2 17 5804.04 5420.92 962.01 o -1 3 17 3423.94 3390.79 33.08 o -3 4 17 1220.12 1149.13 30.31 o 0 4 17 718.25 733.95 73.14 o 0 0 18 3249.90 2952.22 92.18 o -1 2 18 3520.87 3148.20 96.99 o -3 3 18 3282.04 3126.56 157.54 o 0 3 18 3282.04 3245.98 38.11 o -2 4 18 2980.92 2505.02 281.58 o -1 1 19 4346.17 4462.56 29.51 o 0 2 19 4143.17 4592.65 144.32 o -2 3 19 3830.35 4419.47 169.34 o -4 4 19 2737.24 3783.66 127.94 o -1 4 19 3091.05 3435.85 43.12 o 0 1 20 53094.50 49798.30 620.78 o -2 2 20 32558.30 33627.20 1553.40 o -1 3 20 21015.00 18989.80 2138.91 o -3 4 20 9763.18 10418.00 245.99 o 0 4 20 6922.51 7310.31 40.90 o 0 0 21 1876.41 2175.68 78.70 o -1 2 21 1569.92 1620.32 53.17 o -3 3 21 1178.55 997.69 40.41 o 0 3 21 1178.55 1256.58 32.84 o -2 4 21 1038.71 941.56 15.15 o -1 1 22 7031.62 7034.89 149.98 o 0 2 22 6614.69 7254.60 210.80 o -2 3 22 6072.07 6443.85 236.81 o -1 4 22 4936.34 5565.52 92.95 o 0 1 23 66539.90 65353.90 579.64 o -2 2 23 47575.20 47342.70 980.63 o -1 3 23 35036.90 36510.70 472.34 o -3 4 23 20174.40 22404.20 550.20 o 0 0 24 6219.05 6762.39 99.22 o -1 2 24 3632.40 3315.76 304.33 o -3 3 24 1328.87 1043.36 37.89 o 0 3 24 1328.87 1313.68 25.26 o -2 4 24 816.80 732.86 37.84 o -1 1 25 66287.40 67371.10 150.97 o 0 2 25 45649.90 45992.10 1442.82 o -2 3 25 32575.00 32048.50 476.02 o -1 4 25 17916.60 18284.30 412.22 o 0 1 26 3.59 59.17 17.63 o -2 2 26 10.76 56.66 40.29 < -1 3 26 32.79 62.96 13.85 o 0 0 27 35011.00 35250.30 185.41 o -1 2 27 24500.50 21745.40 1035.50 o -3 3 27 12744.20 11072.90 495.24 o 0 3 27 12744.20 11966.10 435.60 o -1 1 28 149.28 996.33 162.49 o 0 2 28 47.96 355.09 51.63 o -2 3 28 19.80 237.97 12.59 o 0 1 29 7331.03 8728.72 222.46 o -2 2 29 5000.03 5678.99 39.53 o -1 3 29 3506.65 4058.54 85.06 o 0 0 30 21141.10 19490.20 132.39 o -1 2 30 13697.40 11918.00 322.07 o -3 3 30 6224.24 5590.91 162.11 o 0 3 30 6224.24 5846.21 225.93 o -1 1 31 10807.50 10329.90 82.95 o 0 2 31 8898.10 8711.51 383.40 o -2 3 31 7379.09 6594.36 197.15 o 0 1 32 4138.83 4221.89 71.28 o -2 2 32 3952.31 4110.42 44.49 o -1 3 32 3697.61 3868.07 163.76 o 0 0 33 9971.73 12556.70 107.27 o -1 2 33 7126.54 8807.32 137.03 o -1 1 34 385.15 717.07 35.29 o 0 2 34 152.25 379.10 20.15 o 0 1 35 8981.03 7594.13 47.60 o -2 2 35 6064.92 5258.26 67.64 o 0 0 36 7417.15 6942.01 91.00 o -1 2 36 5619.03 5745.30 71.40 o -1 1 37 11182.70 10255.10 111.08 o 0 1 38 5472.86 9735.69 1552.51 o 0 0 39 5284.07 7058.50 73.90 o #======================================================================= data_As3Cd4Na1_130_mod #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'As3 Cd4 Na1' _chemical_formula_weight 697.4 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_ssg_name 'Cm(\a0\g)s' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 x1,-x2,x3,x4+1/2 3 x1+1/2,x2+1/2,x3,x4 4 x1+1/2,-x2+1/2,x3,x4+1/2 _cell_length_a 7.7151(8) _cell_length_b 13.3673(10) _cell_length_c 11.5106(11) _cell_angle_alpha 90 _cell_angle_beta 102.905(8) _cell_angle_gamma 90 _cell_volume 1157.10(19) 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 0.45(4) 1 0 0 0 1 0 0 0 1 2 0.55(4) -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 -0.018589 0.000000 0.341400 _cell_formula_units_Z 6 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 130 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 6.0049 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1812 _exptl_absorpt_coefficient_mu 23.871 _exptl_crystal_description plate _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.040 _exptl_crystal_size_rad ? _exptl_crystal_colour black _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'Jana2006' _exptl_absorpt_correction_T_min 0.0253 _exptl_absorpt_correction_T_max 0.3386 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 130 _diffrn_source_power 2 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'IPDS Stoe' _diffrn_detector 'image plate' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '??integration method??' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 35411 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 32.12 _diffrn_reflns_theta_full 32.12 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.1032 _diffrn_reflns_av_unetI/netI 0.0741 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _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_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 11345 _reflns_number_gt 4609 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_gt 0.1082 _refine_ls_R_factor_all 0.1065 _refine_ls_wR_factor_ref 0.1270 _refine_ls_goodness_of_fit_ref 1.35 _refine_ls_goodness_of_fit_gt 1.82 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 11345 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_number_constraints 2 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0004I^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0029 _refine_ls_shift/su_mean 0.0006 _refine_diff_density_max 0.83 _refine_diff_density_min 0.00 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 1520(40) _refine_ls_abs_structure_details ; 5447 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0.55(4) _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As 0.0511 2.0283 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Cd -0.7834 1.2309 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Na 0.0374 0.0259 '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 ? loop_ _reflns_class_code _reflns_class_description _reflns_class_R_factor_all _reflns_class_R_factor_gt _reflns_class_wR_factor_all Main 'Main reflections' 0.0638 0.0415 0.1003 Sat1 '1st-order satellites' 0.2115 0.0705 0.2235 #======================================================================= # 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 Cd1 Cd 0.18304(19) 0.16637(13) 0.04866(15) Uani 0.0191(4) 4 1 d . . . Cd2 Cd 0.37447(18) 0.16657(13) 0.62437(15) Uani 0.0185(4) 4 1 d . . . Cd3 Cd 0.6870(2) 0 0.0616(2) Uani 0.0122(4) 2 1 d . . . Cd4 Cd 0.8806(3) 0 0.6383(2) Uani 0.0191(6) 2 1 d . . . Cd5 Cd 0.07468(17) 0.32821(15) 0.23742(11) Uani 0.0143(3) 4 1 d . . . Cd6 Cd 0.47674(19) 0.33765(19) 0.44323(15) Uani 0.0193(4) 4 1 d . . . Cd7 Cd 0.0894(2) 0 0.23684(19) Uani 0.0139(4) 2 1 d . . . Cd8 Cd 0.4913(3) 0 0.4424(2) Uani 0.0194(5) 2 1 d . . . As1 As 0.2810(3) 0.16670(17) 0.3420(2) Uani 0.0099(3) 4 1 d . . . As2 As 0.7793(3) 0 0.3340(2) Uani 0.0093(7) 2 1 d . . . As3 As 0.0015(3) 0.33377(13) 0.00046(16) Uiso 0.0096(3) 4 1 d . . . As4 As 0.0603(2) 0.16741(11) 0.67816(16) Uani 0.0048(2) 4 1 d . . . As5 As -0.0012(3) 0 -0.0010(3) Uiso 0.0098(4) 2 1 d . . . As6 As 0.5583(3) 0 0.6770(2) Uani 0.0042(3) 2 1 d . . . Na1 Na 0.2812(10) 0.3320(10) 0.8429(6) Uiso 0.0095(6) 4 1 d . . . Na2 Na 0.2895(12) 0 0.8435(8) Uiso 0.02 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 Cd1 Cd 0.0099(5) 0.0096(6) 0.0393(9) 0.0000(4) 0.0088(5) 0.0005(5) Cd2 Cd 0.0096(5) 0.0079(6) 0.0390(9) 0.0003(4) 0.0080(5) 0.0003(6) Cd3 Cd 0.0068(6) 0.0036(6) 0.0277(8) 0 0.0069(5) 0 Cd4 Cd 0.0077(6) 0.0016(7) 0.0505(14) 0 0.0120(7) 0 Cd5 Cd 0.0207(5) 0.0192(6) 0.0029(3) -0.0009(4) 0.0023(3) 0.0011(4) Cd6 Cd 0.0215(6) 0.0191(7) 0.0172(5) 0.0017(4) 0.0039(4) 0.0002(4) Cd7 Cd 0.0169(7) 0.0204(9) 0.0034(5) 0 0.0003(5) 0 Cd8 Cd 0.0165(6) 0.0240(10) 0.0175(7) 0 0.0038(5) 0 As1 As 0.0077(4) 0.0076(6) 0.0147(6) -0.00037(19) 0.0032(4) -0.0004(3) As2 As 0.0081(9) 0.0054(10) 0.0150(13) 0 0.0042(9) 0 As4 As 0.0049(3) 0.0019(3) 0.0083(4) -0.0003(2) 0.0033(2) 0.0004(3) As6 As 0.0043(5) 0.0019(5) 0.0072(5) 0 0.0030(3) 0 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 Cd1x1 Cd1 x 1 Cd1y1 Cd1 y 1 Cd1z1 Cd1 z 1 Cd2x1 Cd2 x 1 Cd2y1 Cd2 y 1 Cd2z1 Cd2 z 1 Cd5x1 Cd5 x 1 Cd5y1 Cd5 y 1 Cd5z1 Cd5 z 1 Cd6x1 Cd6 x 1 Cd6y1 Cd6 y 1 Cd6z1 Cd6 z 1 Cd7x1 Cd7 x 1 Cd7y1 Cd7 y 1 Cd7z1 Cd7 z 1 Cd8x1 Cd8 x 1 Cd8y1 Cd8 y 1 Cd8z1 Cd8 z 1 As1x1 As1 x 1 As1y1 As1 y 1 As1z1 As1 z 1 As3x1 As3 x 1 As3y1 As3 y 1 As3z1 As3 z 1 Na1x1 Na1 x 1 Na1y1 Na1 y 1 Na1z1 Na1 z 1 Na2x1 Na2 x 1 Na2y1 Na2 y 1 Na2z1 Na2 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Cd1x1 -0.0043(2) -0.0001(6) Cd1y1 -0.00032(16) 0.00041(15) Cd1z1 -0.0145(2) -0.0007(19) Cd2x1 -0.0024(7) -0.0047(4) Cd2y1 -0.00027(15) 0.00020(15) Cd2z1 -0.005(2) -0.0148(7) Cd5x1 0.0143(8) 0.0059(19) Cd5y1 -0.0047(3) -0.0020(7) Cd5z1 0.00096(18) -0.0008(2) Cd6x1 0.0108(17) 0.0129(15) Cd6y1 0.0038(6) 0.0043(5) Cd6z1 0.0001(2) 0.00048(18) Cd7x1 0 0 Cd7y1 0.0090(6) 0.0042(12) Cd7z1 0 0 Cd8x1 0 0 Cd8y1 -0.0077(11) -0.0083(11) Cd8z1 0 0 As1x1 0.0029(3) 0.0016(5) As1y1 -0.0005(2) 0.00068(17) As1z1 0.0064(7) 0.0052(9) As3x1 -0.00359(14) -0.0005(5) As3y1 0.00311(12) -0.0001(4) As3z1 0.0011(3) -0.00231(18) Na1x1 0.0055(10) -0.0006(15) Na1y1 0.0036(9) 0.0005(11) Na1z1 -0.0001(6) 0.0000(8) Na2x1 0 0 Na2y1 -0.0090(14) 0.0(13) Na2z1 0 0 loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id Cd1U111 Cd1 U11 1 Cd1U221 Cd1 U22 1 Cd1U331 Cd1 U33 1 Cd1U121 Cd1 U12 1 Cd1U131 Cd1 U13 1 Cd1U231 Cd1 U23 1 Cd2U111 Cd2 U11 1 Cd2U221 Cd2 U22 1 Cd2U331 Cd2 U33 1 Cd2U121 Cd2 U12 1 Cd2U131 Cd2 U13 1 Cd2U231 Cd2 U23 1 Cd5U111 Cd5 U11 1 Cd5U221 Cd5 U22 1 Cd5U331 Cd5 U33 1 Cd5U121 Cd5 U12 1 Cd5U131 Cd5 U13 1 Cd5U231 Cd5 U23 1 Cd7U111 Cd7 U11 1 Cd7U221 Cd7 U22 1 Cd7U331 Cd7 U33 1 Cd7U121 Cd7 U12 1 Cd7U131 Cd7 U13 1 Cd7U231 Cd7 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Cd1U111 0.0027(6) -0.0004(7) Cd1U221 0.0026(7) -0.0001(8) Cd1U331 0.0047(11) 0.0016(12) Cd1U121 0.0005(5) -0.0009(7) Cd1U131 0.0013(7) 0.0013(6) Cd1U231 0.0010(8) -0.0020(10) Cd2U111 -0.0003(6) 0.0014(5) Cd2U221 -0.0003(8) 0.0026(6) Cd2U331 -0.008(3) -0.0249(15) Cd2U121 -0.0008(6) 0.0000(5) Cd2U131 -0.0032(10) -0.0053(7) Cd2U231 0.0005(9) 0.0001(7) Cd5U111 0.0035(6) 0.0009(6) Cd5U221 -0.0031(8) -0.0020(8) Cd5U331 0.0003(3) -0.0003(3) Cd5U121 0.0020(7) 0.0009(7) Cd5U131 -0.0005(4) -0.0006(3) Cd5U231 0.0011(7) -0.0004(7) Cd7U111 0 0 Cd7U221 0 0 Cd7U331 0 0 Cd7U121 -0.0053(8) -0.0023(10) Cd7U131 0 0 Cd7U231 -0.0009(8) -0.0004(8) #======================================================================= # 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 Cd1 As3 . . 2.636(5) 2.619(7) 2.658(7) ? Cd1 As3 . 4_5555 2.639(8) 2.632(12) 2.648(12) ? Cd1 As5 . . 2.635(3) 2.601(4) 2.673(4) ? Cd1 Na1 . 1_5545 3.449(19) 3.38(2) 3.52(2) ? Cd1 Na1 . 4_4545 3.457(13) 3.384(16) 3.534(16) ? Cd1 Na2 . 1_5545 3(6) 3(12) 4(12) ? Cd2 As4 . . 2.636(8) 2.598(12) 2.678(12) ? Cd2 As4 . 4_5555 2.643(4) 2.605(5) 2.684(5) ? Cd2 As6 . . 2.640(4) 2.602(5) 2.682(5) ? Cd2 Na1 . . 3.545(19) 3.42(2) 3.67(2) ? Cd2 Na1 . 4_5555 3.559(14) 3.429(16) 3.688(16) ? Cd2 Na2 . . 4(6) 3(12) 4(12) ? Cd3 As3 . 3_5455 2.652(4) 2.628(6) 2.676(6) ? Cd3 As3 . 4_5555 2.652(4) 2.628(6) 2.676(6) ? Cd3 As5 . 1_6555 2.661(4) 2.661(4) 2.661(4) ? Cd3 Na1 . 3_5445 3.567(15) 3.552(16) 3.582(16) ? Cd3 Na1 . 4_5545 3.567(15) 3.552(16) 3.582(16) ? Cd3 Na2 . 1_5545 3.50(13) 3.5(3) 3.5(3) ? Cd4 As4 . 1_6555 2.6184(19) 2.6184(19) 2.6184(19) ? Cd4 As4 . 2_6555 2.6184(19) 2.6184(19) 2.6184(19) ? Cd4 As6 . . 2.622(4) 2.622(4) 2.622(4) ? Cd4 Na1 . 3_5455 3.462(16) 3.415(16) 3.509(16) ? Cd4 Na1 . 4_5555 3.462(16) 3.415(16) 3.509(16) ? Cd4 Na2 . 1_6555 3.49(13) 3.5(3) 3.5(3) ? Cd5 As1 . . 2.792(9) 2.724(11) 2.865(11) ? Cd5 As1 . 4_4555 2.797(12) 2.728(16) 2.869(16) ? Cd5 As2 . 3_4555 2.868(8) 2.863(10) 2.873(10) ? Cd5 As3 . . 2.663(4) 2.647(5) 2.678(5) ? Cd6 As1 . . 2.844(10) 2.764(10) 2.926(10) ? Cd6 As1 . 4_5555 2.846(13) 2.768(14) 2.931(14) ? Cd6 As2 . 3_4555 2.787(9) 2.782(9) 2.790(9) ? Cd6 As4 . 4_5555 2.639(3) 2.634(3) 2.646(3) ? Cd7 As1 . . 2.797(11) 2.734(14) 2.865(14) ? Cd7 As1 . 2_5555 2.799(11) 2.734(14) 2.865(14) ? Cd7 As2 . 1_4555 2.860(4) 2.859(4) 2.862(4) ? Cd7 As5 . . 2.671(4) 2.670(4) 2.673(4) ? Cd8 As1 . . 2.848(12) 2.769(13) 2.930(13) ? Cd8 As1 . 2_5555 2.846(12) 2.769(13) 2.930(13) ? Cd8 As2 . . 2.783(4) 2.781(4) 2.785(4) ? Cd8 As6 . . 2.636(4) 2.634(4) 2.638(4) ? As3 Na1 . 1_5545 3.114(13) 3.046(15) 3.181(15) ? As3 Na1 . 4_4545 3.117(16) 3.088(17) 3.145(17) ? As3 Na2 . 3_4545 3(6) 3(13) 3(13) ? As4 Na1 . . 3.147(15) 3.096(16) 3.197(16) ? As4 Na1 . 4_4555 3.171(13) 3.136(14) 3.207(14) ? As4 Na2 . . 3(6) 3(13) 3(13) ? As5 Na1 . 3_4445 3.121(15) 3.070(16) 3.172(16) ? As5 Na1 . 4_4545 3.121(15) 3.070(16) 3.172(16) ? As5 Na2 . 1_5545 3.17(15) 3.2(3) 3.2(3) ? As6 Na1 . 3_5455 3.190(15) 3.173(16) 3.208(16) ? As6 Na1 . 4_5555 3.191(15) 3.173(16) 3.208(16) ? As6 Na2 . . 3.12(15) 3.1(3) 3.1(3) ? 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 As3 Cd1 As3 . . 4_5555 115.5(3) 113.66(17) 116.96(18) ? As3 Cd1 As5 . . . 115.71(17) 113.25(10) 117.77(10) ? As3 Cd1 Na1 . . 1_5545 59.8(3) 57.3(3) 62.2(3) ? As3 Cd1 Na1 . . 4_4545 59.7(4) 58.2(3) 61.2(3) ? As3 Cd1 Na2 . . 1_5545 130(170) 120(180) 130(160) ? As3 Cd1 As5 4_5555 . . 115.8(3) 112.38(13) 119.02(13) ? As3 Cd1 Na1 4_5555 . 1_5545 59.8(3) 59.0(3) 60.6(3) ? As3 Cd1 Na1 4_5555 . 4_4545 126.3(5) 120.5(3) 132.1(3) ? As3 Cd1 Na2 4_5555 . 1_5545 60(110) 60(110) 60(110) ? As5 Cd1 Na1 . . 1_5545 125.9(5) 119.7(3) 132.0(3) ? As5 Cd1 Na1 . . 4_4545 59.9(4) 57.4(3) 62.3(3) ? As5 Cd1 Na2 . . 1_5545 60(180) 60(180) 60(180) ? Na1 Cd1 Na1 1_5545 . 4_4545 80.0(4) 76.5(3) 83.5(3) ? Na1 Cd1 Na2 1_5545 . 1_5545 100(200) 100(200) 100(200) ? Na1 Cd1 Na2 4_4545 . 1_5545 80(30) 80(40) 90(20) ? As4 Cd2 As4 . . 4_5555 114.8(3) 112.0(2) 117.30(19) ? As4 Cd2 As6 . . . 115.0(3) 112.2(2) 117.64(18) ? As4 Cd2 Na1 . . . 59.1(3) 56.6(3) 61.6(3) ? As4 Cd2 Na1 . . 4_5555 123.2(6) 117.6(4) 128.9(4) ? As4 Cd2 Na2 . . . 60(110) 60(110) 60(100) ? As4 Cd2 As6 4_5555 . . 114.7(2) 111.88(16) 117.24(14) ? As4 Cd2 Na1 4_5555 . . 59.6(3) 57.4(3) 61.8(3) ? As4 Cd2 Na1 4_5555 . 4_5555 58.8(4) 56.5(3) 61.1(4) ? As4 Cd2 Na2 4_5555 . . 120(170) 120(180) 130(170) ? As6 Cd2 Na1 . . . 123.2(5) 117.7(4) 129.0(4) ? As6 Cd2 Na1 . . 4_5555 59.8(4) 57.6(3) 62.1(3) ? As6 Cd2 Na2 . . . 60(180) 60(170) 60(190) ? Na1 Cd2 Na1 . . 4_5555 77.4(4) 74.3(4) 80.7(4) ? Na1 Cd2 Na2 . . . 100(200) 100(200) 100(200) ? Na1 Cd2 Na2 4_5555 . . 80(40) 70(50) 80(40) ? As3 Cd3 As3 3_5455 . 4_5555 113.86(14) 113.85(13) 113.87(15) ? As3 Cd3 As5 3_5455 . 1_6555 113.28(10) 112.25(9) 114.30(9) ? As3 Cd3 Na1 3_5455 . 3_5445 57.9(3) 56.1(3) 59.7(3) ? As3 Cd3 Na1 3_5455 . 4_5545 121.5(3) 121.0(3) 122.0(3) ? As3 Cd3 Na2 3_5455 . 1_5545 100(300) 100(300) 100(300) ? As3 Cd3 As5 4_5555 . 1_6555 113.26(10) 112.25(9) 114.30(9) ? As3 Cd3 Na1 4_5555 . 3_5445 121.5(3) 121.0(3) 122.0(3) ? As3 Cd3 Na1 4_5555 . 4_5545 57.9(3) 56.1(3) 59.7(3) ? As3 Cd3 Na2 4_5555 . 1_5545 100(300) 100(300) 100(300) ? As5 Cd3 Na1 1_6555 . 3_5445 58.0(2) 57.1(2) 58.9(2) ? As5 Cd3 Na1 1_6555 . 4_5545 58.0(2) 57.1(2) 58.9(2) ? As5 Cd3 Na2 1_6555 . 1_5545 120(4) 120(6) 120.4(2) ? Na1 Cd3 Na1 3_5445 . 4_5545 78.0(4) 78.0(4) 78.0(4) ? Na1 Cd3 Na2 3_5445 . 1_5545 80(190) 80(190) 100(200) ? Na1 Cd3 Na2 4_5545 . 1_5545 80(190) 80(190) 100(200) ? As4 Cd4 As4 1_6555 . 2_6555 117.44(9) 117.44(9) 117.44(9) ? As4 Cd4 As6 1_6555 . . 117.08(7) 117.08(7) 117.08(7) ? As4 Cd4 Na1 1_6555 . 3_5455 128.6(3) 127.9(3) 129.3(3) ? As4 Cd4 Na1 1_6555 . 4_5555 61.0(3) 60.9(3) 61.2(3) ? As4 Cd4 Na2 1_6555 . 1_6555 100(300) 100(300) 100(300) ? As4 Cd4 As6 2_6555 . . 117.08(7) 117.08(7) 117.08(7) ? As4 Cd4 Na1 2_6555 . 3_5455 61.0(3) 60.9(3) 61.2(3) ? As4 Cd4 Na1 2_6555 . 4_5555 128.6(3) 127.9(3) 129.3(3) ? As4 Cd4 Na2 2_6555 . 1_6555 100(300) 100(300) 100(300) ? As6 Cd4 Na1 . . 3_5455 61.4(2) 61.0(2) 61.8(2) ? As6 Cd4 Na1 . . 4_5555 61.4(2) 61.0(2) 61.8(2) ? As6 Cd4 Na2 . . 1_6555 129(5) 129(8) 129.2(3) ? Na1 Cd4 Na1 3_5455 . 4_5555 80.9(4) 80.9(4) 80.9(4) ? Na1 Cd4 Na2 3_5455 . 1_6555 80(190) 80(190) 100(200) ? Na1 Cd4 Na2 4_5555 . 1_6555 80(190) 80(190) 100(200) ? As1 Cd5 As1 . . 4_4555 105.7(3) 105.4(2) 106.1(3) ? As1 Cd5 As2 . . 3_4555 103.9(3) 101.9(2) 105.80(19) ? As1 Cd5 As3 . . . 115.8(3) 109.4(3) 122.1(3) ? As1 Cd5 As2 4_4555 . 3_4555 103.9(2) 102.2(2) 105.7(2) ? As1 Cd5 As3 4_4555 . . 115.7(4) 109.5(3) 122.0(3) ? As2 Cd5 As3 3_4555 . . 110.2(3) 109.5(2) 110.8(2) ? As1 Cd6 As1 . . 4_5555 103.1(3) 102.7(3) 103.4(3) ? As1 Cd6 As2 . . 3_4555 104.7(3) 102.5(3) 106.7(3) ? As1 Cd6 As4 . . 4_5555 112.6(3) 107.3(3) 118.1(3) ? As1 Cd6 As2 4_5555 . 3_4555 104.4(3) 102.3(3) 106.3(3) ? As1 Cd6 As4 4_5555 . 4_5555 112.7(4) 107.1(4) 118.1(4) ? As2 Cd6 As4 3_4555 . 4_5555 117.7(3) 117.3(3) 117.9(3) ? As1 Cd7 As1 . . 2_5555 105.63(16) 105.57(16) 105.68(16) ? As1 Cd7 As2 . . 1_4555 103.7(3) 101.8(2) 105.5(2) ? As1 Cd7 As5 . . . 115.9(4) 110.6(3) 121.2(3) ? As1 Cd7 As2 2_5555 . 1_4555 103.7(3) 101.8(2) 105.5(2) ? As1 Cd7 As5 2_5555 . . 115.8(4) 110.6(3) 121.2(3) ? As2 Cd7 As5 1_4555 . . 110.44(10) 110.34(10) 110.54(9) ? As1 Cd8 As1 . . 2_5555 103.05(15) 102.98(15) 103.11(15) ? As1 Cd8 As2 . . . 104.9(3) 102.6(4) 107.0(3) ? As1 Cd8 As6 . . . 112.3(4) 106.9(4) 117.8(4) ? As1 Cd8 As2 2_5555 . . 104.9(3) 102.6(4) 107.0(3) ? As1 Cd8 As6 2_5555 . . 112.4(4) 106.9(4) 117.8(4) ? As2 Cd8 As6 . . . 117.66(11) 117.51(11) 117.81(10) ? Cd5 As1 Cd5 . . 4_5555 103.4(4) 100.2(3) 106.6(3) ? Cd5 As1 Cd6 . . . 75.7(2) 75.3(3) 76.3(3) ? Cd5 As1 Cd6 . . 4_4555 75.5(3) 75.0(2) 76.1(2) ? Cd5 As1 Cd7 . . . 103.4(3) 100.1(3) 106.6(3) ? Cd5 As1 Cd8 . . . 176.4(4) 173.1(4) 180.0(5) ? Cd5 As1 Cd6 4_5555 . . 75.5(3) 75.4(3) 75.6(2) ? Cd5 As1 Cd6 4_5555 . 4_4555 176.1(3) 172.9(3) 179.6(3) ? Cd5 As1 Cd7 4_5555 . . 103.4(3) 100.0(3) 106.6(3) ? Cd5 As1 Cd8 4_5555 . . 75.50(19) 75.02(15) 75.99(17) ? Cd6 As1 Cd6 . . 4_4555 105.0(3) 101.9(4) 107.9(3) ? Cd6 As1 Cd7 . . . 176.4(4) 173.2(4) 179.7(3) ? Cd6 As1 Cd8 . . . 105.1(3) 101.7(3) 108.2(3) ? Cd6 As1 Cd7 4_4555 . . 75.83(19) 75.7(2) 76.0(2) ? Cd6 As1 Cd8 4_4555 . . 105.3(3) 102.1(3) 108.3(3) ? Cd7 As1 Cd8 . . . 75.6(3) 75.2(3) 76.0(3) ? Cd5 As2 Cd5 3_5455 . 4_5555 106.5(3) 106.5(3) 106.5(3) ? Cd5 As2 Cd6 3_5455 . 3_5455 75.5(2) 75.0(2) 75.9(3) ? Cd5 As2 Cd6 3_5455 . 4_5555 176.11(16) 175.85(16) 176.38(17) ? Cd5 As2 Cd7 3_5455 . 1_6555 106.6(3) 106.5(4) 106.6(4) ? Cd5 As2 Cd8 3_5455 . . 75.4(3) 74.9(3) 75.9(3) ? Cd5 As2 Cd6 4_5555 . 3_5455 176.11(16) 175.85(16) 176.38(17) ? Cd5 As2 Cd6 4_5555 . 4_5555 75.5(2) 75.0(2) 75.9(3) ? Cd5 As2 Cd7 4_5555 . 1_6555 106.5(3) 106.5(4) 106.6(4) ? Cd5 As2 Cd8 4_5555 . . 75.4(3) 74.9(3) 75.9(3) ? Cd6 As2 Cd6 3_5455 . 4_5555 102.4(3) 102.4(3) 102.4(2) ? Cd6 As2 Cd7 3_5455 . 1_6555 75.8(3) 75.5(3) 76.1(4) ? Cd6 As2 Cd8 3_5455 . . 102.1(3) 101.8(3) 102.3(3) ? Cd6 As2 Cd7 4_5555 . 1_6555 75.8(3) 75.5(3) 76.1(4) ? Cd6 As2 Cd8 4_5555 . . 102.1(3) 101.8(3) 102.3(3) ? Cd7 As2 Cd8 1_6555 . . 176.48(11) 176.46(12) 176.50(11) ? Cd1 As3 Cd1 . . 4_4555 115.6(3) 115.15(19) 116.2(2) ? Cd1 As3 Cd3 . . 3_4555 115.17(14) 114.44(12) 115.82(15) ? Cd1 As3 Cd5 . . . 77.2(4) 76.7(4) 77.8(4) ? Cd1 As3 Na1 . . 1_5545 73.2(4) 70.2(4) 76.4(4) ? Cd1 As3 Na1 . . 4_4545 73.3(4) 71.0(3) 75.8(3) ? Cd1 As3 Na2 . . 3_4545 160(160) 150(180) 160(140) ? Cd1 As3 Cd3 4_4555 . 3_4555 114.67(19) 113.88(15) 115.47(17) ? Cd1 As3 Cd5 4_4555 . . 77.2(4) 76.7(5) 77.7(6) ? Cd1 As3 Na1 4_4555 . 1_5545 157.3(4) 153.3(3) 161.1(3) ? Cd1 As3 Na1 4_4555 . 4_4545 73.1(3) 71.8(3) 74.5(3) ? Cd1 As3 Na2 4_4555 . 3_4545 70(70) 70(80) 80(60) ? Cd3 As3 Cd5 3_4555 . . 76.9(3) 76.0(3) 77.7(3) ? Cd3 As3 Na1 3_4555 . 1_5545 76.0(3) 74.8(3) 77.1(4) ? Cd3 As3 Na1 3_4555 . 4_4545 160.4(3) 159.6(3) 161.3(3) ? Cd3 As3 Na2 3_4555 . 3_4545 100(200) 100(200) 100(200) ? Cd5 As3 Na1 . . 1_5545 125.5(3) 121.7(3) 129.3(3) ? Cd5 As3 Na1 . . 4_4545 122.6(4) 122.3(3) 123.0(4) ? Cd5 As3 Na2 . . 3_4545 130(160) 120(140) 130(180) ? Na1 As3 Na1 1_5545 . 4_4545 90.8(4) 89.6(4) 92.0(4) ? Na1 As3 Na2 1_5545 . 3_4545 91(3) 90(4) 91(4) ? Na1 As3 Na2 4_4545 . 3_4545 100(200) 100(300) 100(200) ? Cd2 As4 Cd2 . . 4_4555 115.48(18) 115.3(2) 115.62(15) ? Cd2 As4 Cd4 . . 1_4555 115.72(13) 114.61(12) 116.83(11) ? Cd2 As4 Cd6 . . 4_4555 77.6(4) 76.8(3) 78.6(3) ? Cd2 As4 Na1 . . . 75.0(3) 72.3(3) 77.7(3) ? Cd2 As4 Na1 . . 4_4555 157.6(4) 154.0(3) 161.1(3) ? Cd2 As4 Na2 . . . 70(60) 70(70) 80(50) ? Cd2 As4 Cd4 4_4555 . 1_4555 116.03(12) 114.84(10) 117.16(11) ? Cd2 As4 Cd6 4_4555 . 4_4555 77.7(4) 76.8(3) 78.5(3) ? Cd2 As4 Na1 4_4555 . . 75.2(4) 72.6(3) 77.9(3) ? Cd2 As4 Na1 4_4555 . 4_4555 74.5(4) 71.9(4) 77.1(4) ? Cd2 As4 Na2 4_4555 . . 160(170) 150(170) 160(160) ? Cd4 As4 Cd6 1_4555 . 4_4555 78.5(2) 78.4(2) 78.5(2) ? Cd4 As4 Na1 1_4555 . . 153.8(3) 153.2(3) 154.5(3) ? Cd4 As4 Na1 1_4555 . 4_4555 72.7(3) 72.1(3) 73.3(3) ? Cd4 As4 Na2 1_4555 . . 100(200) 100(200) 100(200) ? Cd6 As4 Na1 4_4555 . . 127.7(3) 127.0(3) 128.4(4) ? Cd6 As4 Na1 4_4555 . 4_4555 124.7(3) 122.1(3) 127.4(3) ? Cd6 As4 Na2 4_4555 . . 120(170) 120(160) 130(170) ? Na1 As4 Na1 . . 4_4555 89.2(4) 88.8(4) 89.6(4) ? Na1 As4 Na2 . . . 100(200) 100(200) 100(200) ? Na1 As4 Na2 4_4555 . . 90.3(10) 89.4(18) 91.2(8) ? Cd1 As5 Cd1 . . 2_5555 115.36(17) 115.29(19) 115.44(17) ? Cd1 As5 Cd3 . . 1_4555 114.74(19) 113.23(10) 116.20(9) ? Cd1 As5 Cd7 . . . 76.9(4) 75.9(3) 77.9(3) ? Cd1 As5 Na1 . . 3_4445 158.0(4) 153.9(3) 162.1(3) ? Cd1 As5 Na1 . . 4_4545 73.3(3) 71.1(3) 75.5(3) ? Cd1 As5 Na2 . . 1_5545 100(300) 100(300) 100(300) ? Cd1 As5 Cd3 2_5555 . 1_4555 114.71(19) 113.23(10) 116.20(9) ? Cd1 As5 Cd7 2_5555 . . 76.9(4) 75.9(3) 77.9(3) ? Cd1 As5 Na1 2_5555 . 3_4445 73.3(3) 71.1(3) 75.5(3) ? Cd1 As5 Na1 2_5555 . 4_4545 158.1(4) 153.9(3) 162.1(3) ? Cd1 As5 Na2 2_5555 . 1_5545 100(300) 100(300) 100(300) ? Cd3 As5 Cd7 1_4555 . . 76.60(11) 76.59(11) 76.60(11) ? Cd3 As5 Na1 1_4555 . 3_4445 75.7(3) 75.2(3) 76.3(3) ? Cd3 As5 Na1 1_4555 . 4_4545 75.7(3) 75.2(3) 76.3(3) ? Cd3 As5 Na2 1_4555 . 1_5545 160(20) 160(40) 161.9(2) ? Cd7 As5 Na1 . . 3_4445 125.1(4) 122.0(3) 128.2(3) ? Cd7 As5 Na1 . . 4_4545 125.0(4) 122.0(3) 128.2(3) ? Cd7 As5 Na2 . . 1_5545 122(8) 122(7) 122(11) ? Na1 As5 Na1 3_4445 . 4_4545 92.0(4) 92.0(4) 92.0(4) ? Na1 As5 Na2 3_4445 . 1_5545 100(200) 100(200) 100(200) ? Na1 As5 Na2 4_4545 . 1_5545 100(200) 100(200) 100(200) ? Cd2 As6 Cd2 . . 2_5555 115.32(14) 115.23(16) 115.40(13) ? Cd2 As6 Cd4 . . . 116.24(19) 115.11(13) 117.37(12) ? Cd2 As6 Cd8 . . . 78.0(4) 77.2(3) 78.9(3) ? Cd2 As6 Na1 . . 3_5455 157.3(4) 153.6(3) 160.8(3) ? Cd2 As6 Na1 . . 4_5555 74.6(3) 71.8(3) 77.3(3) ? Cd2 As6 Na2 . . . 100(300) 100(300) 100(300) ? Cd2 As6 Cd4 2_5555 . . 116.27(19) 115.11(13) 117.37(12) ? Cd2 As6 Cd8 2_5555 . . 78.0(4) 77.2(3) 78.9(3) ? Cd2 As6 Na1 2_5555 . 3_5455 74.5(3) 71.8(3) 77.3(3) ? Cd2 As6 Na1 2_5555 . 4_5555 157.2(4) 153.6(3) 160.8(3) ? Cd2 As6 Na2 2_5555 . . 100(300) 100(300) 100(300) ? Cd4 As6 Cd8 . . . 78.60(11) 78.59(11) 78.61(11) ? Cd4 As6 Na1 . . 3_5455 72.4(3) 71.5(3) 73.2(3) ? Cd4 As6 Na1 . . 4_5555 72.3(3) 71.5(3) 73.2(3) ? Cd4 As6 Na2 . . . 153(16) 150(20) 152.8(4) ? Cd8 As6 Na1 . . 3_5455 124.7(4) 122.0(4) 127.5(4) ? Cd8 As6 Na1 . . 4_5555 124.8(4) 122.0(4) 127.5(4) ? Cd8 As6 Na2 . . . 129(16) 130(20) 129(7) ? Na1 As6 Na1 3_5455 . 4_5555 89.5(4) 89.5(4) 89.5(4) ? Na1 As6 Na2 3_5455 . . 100(200) 100(200) 100(200) ? Na1 As6 Na2 4_5555 . . 100(200) 100(200) 100(200) ? Cd1 Na1 Cd1 1_5565 . 4_5565 80.5(4) 80.2(4) 80.9(4) ? Cd1 Na1 Cd2 1_5565 . . 101.4(5) 97.7(5) 104.9(5) ? Cd1 Na1 Cd2 1_5565 . 4_4555 101.2(4) 98.3(4) 104.1(4) ? Cd1 Na1 Cd3 1_5565 . 3_4565 79.0(3) 77.8(2) 80.2(3) ? Cd1 Na1 Cd4 1_5565 . 3_4555 177.8(5) 176.3(4) 179.8(6) ? Cd1 Na1 As3 1_5565 . 1_5565 47.0(2) 46.3(2) 47.7(2) ? Cd1 Na1 As3 1_5565 . 4_5565 47.1(2) 46.3(2) 47.8(3) ? Cd1 Na1 As4 1_5565 . . 78.0(4) 74.7(4) 81.3(4) ? Cd1 Na1 As4 1_5565 . 4_5555 134.0(6) 132.9(5) 134.9(5) ? Cd1 Na1 As5 1_5565 . 3_5565 103.8(3) 101.8(3) 105.9(3) ? Cd1 Na1 As6 1_5565 . 3_4555 133.7(4) 132.0(4) 135.3(4) ? Cd1 Na1 Cd2 4_5565 . . 101.3(4) 99.4(4) 103.2(4) ? Cd1 Na1 Cd2 4_5565 . 4_4555 177.5(5) 174.9(5) 179.7(6) ? Cd1 Na1 Cd3 4_5565 . 3_4565 78.8(3) 77.8(2) 79.8(3) ? Cd1 Na1 Cd4 4_5565 . 3_4555 99.2(4) 96.1(3) 102.3(3) ? Cd1 Na1 As3 4_5565 . 1_5565 103.5(4) 101.6(3) 105.5(3) ? Cd1 Na1 As3 4_5565 . 4_5565 46.91(19) 45.91(17) 47.98(18) ? Cd1 Na1 As4 4_5565 . . 134.3(6) 133.9(5) 134.8(6) ? Cd1 Na1 As4 4_5565 . 4_5555 77.5(3) 74.5(2) 80.5(2) ? Cd1 Na1 As5 4_5565 . 3_5565 46.86(17) 46.62(16) 47.10(15) ? Cd1 Na1 As6 4_5565 . 3_4555 133.3(6) 130.9(5) 135.7(5) ? Cd2 Na1 Cd2 . . 4_4555 77.8(3) 77.1(3) 78.4(3) ? Cd2 Na1 Cd3 . . 3_4565 178.0(5) 177.3(5) 178.5(4) ? Cd2 Na1 Cd4 . . 3_4555 79.1(3) 77.4(3) 80.9(3) ? Cd2 Na1 As3 . . 1_5565 134.0(6) 132.4(5) 135.8(5) ? Cd2 Na1 As3 . . 4_5565 78.3(4) 76.0(4) 80.6(4) ? Cd2 Na1 As4 . . . 45.9(2) 45.3(2) 46.6(2) ? Cd2 Na1 As4 . . 4_5555 45.9(2) 45.4(2) 46.5(2) ? Cd2 Na1 As5 . . 3_5565 133.6(4) 132.0(4) 135.2(4) ? Cd2 Na1 As6 . . 3_4555 100.5(3) 98.5(3) 102.6(3) ? Cd2 Na1 Cd3 4_4555 . 3_4565 102.0(4) 100.7(4) 103.4(4) ? Cd2 Na1 Cd4 4_4555 . 3_4555 79.1(3) 77.5(3) 80.7(3) ? Cd2 Na1 As3 4_4555 . 1_5565 78.1(4) 75.8(4) 80.5(4) ? Cd2 Na1 As3 4_4555 . 4_5565 134.0(6) 132.8(6) 135.3(6) ? Cd2 Na1 As4 4_4555 . . 45.90(17) 45.11(15) 46.72(17) ? Cd2 Na1 As4 4_4555 . 4_5555 100.8(4) 98.8(3) 102.9(3) ? Cd2 Na1 As5 4_4555 . 3_5565 132.8(6) 131.9(5) 133.7(5) ? Cd2 Na1 As6 4_4555 . 3_4555 45.63(16) 45.16(16) 46.14(18) ? Cd3 Na1 Cd4 3_4565 . 3_4555 100.5(5) 99.3(4) 101.7(5) ? Cd3 Na1 As3 3_4565 . 1_5565 46.2(2) 45.5(2) 46.9(2) ? Cd3 Na1 As3 3_4565 . 4_5565 102.0(3) 101.6(3) 102.4(3) ? Cd3 Na1 As4 3_4565 . . 134.2(4) 132.8(4) 135.7(4) ? Cd3 Na1 As4 3_4565 . 4_5555 133.9(5) 131.9(5) 135.9(5) ? Cd3 Na1 As5 3_4565 . 3_5565 46.3(2) 45.9(2) 46.7(2) ? Cd3 Na1 As6 3_4565 . 3_4555 79.2(4) 78.7(4) 79.6(4) ? Cd4 Na1 As3 3_4555 . 1_5565 132.8(6) 132.3(6) 133.2(6) ? Cd4 Na1 As3 3_4555 . 4_5565 133.0(4) 132.3(4) 133.7(4) ? Cd4 Na1 As4 3_4555 . . 102.5(3) 102.5(3) 102.5(3) ? Cd4 Na1 As4 3_4555 . 4_5555 46.2(2) 45.62(18) 46.88(19) ? Cd4 Na1 As5 3_4555 . 3_5565 75.7(4) 74.4(3) 77.0(4) ? Cd4 Na1 As6 3_4555 . 3_4555 46.2(2) 45.7(2) 46.7(2) ? As3 Na1 As3 1_5565 . 4_5565 91.4(4) 90.9(4) 92.0(4) ? As3 Na1 As4 1_5565 . . 90.2(4) 88.9(3) 91.6(4) ? As3 Na1 As4 1_5565 . 4_5555 178.4(5) 177.7(4) 179.1(6) ? As3 Na1 As5 1_5565 . 3_5565 90.7(4) 90.2(4) 91.3(4) ? As3 Na1 As6 1_5565 . 3_4555 89.6(4) 88.5(3) 90.6(4) ? As3 Na1 As4 4_5565 . . 90.3(5) 89.7(5) 90.9(5) ? As3 Na1 As4 4_5565 . 4_5555 89.7(4) 89.4(4) 90.0(4) ? As3 Na1 As5 4_5565 . 3_5565 91.3(3) 91.2(3) 91.4(3) ? As3 Na1 As6 4_5565 . 3_4555 178.5(5) 178.0(4) 179.1(5) ? As4 Na1 As4 . . 4_5555 89.4(4) 89.1(3) 89.7(3) ? As4 Na1 As5 . . 3_5565 178.0(5) 176.8(5) 179.0(5) ? As4 Na1 As6 . . 3_4555 89.1(3) 88.5(2) 89.7(2) ? As4 Na1 As5 4_5555 . 3_5565 89.6(4) 88.1(3) 91.2(4) ? As4 Na1 As6 4_5555 . 3_4555 89.3(4) 88.4(3) 90.2(3) ? As5 Na1 As6 3_5565 . 3_4555 89.3(5) 88.0(5) 90.5(5) ? Cd1 Na2 Cd1 1_5565 . 2_5565 80(4) 80(9) 80(3) ? Cd1 Na2 Cd2 1_5565 . . 100(200) 100(60) 110(60) ? Cd1 Na2 Cd2 1_5565 . 2_5555 180(130) 170(90) 180(90) ? Cd1 Na2 Cd3 1_5565 . 1_5565 80(80) 80(110) 80(130) ? Cd1 Na2 Cd4 1_5565 . 1_4555 100(110) 95(7) 101(6) ? Cd1 Na2 As3 1_5565 . 3_5465 104(8) 102.4(3) 105.0(4) ? Cd1 Na2 As3 1_5565 . 4_5565 50(90) 50(100) 50(110) ? Cd1 Na2 As4 1_5565 . . 80(170) 73(10) 81(4) ? Cd1 Na2 As4 1_5565 . 2_5555 132(17) 131.5(11) 130(40) ? Cd1 Na2 As5 1_5565 . 1_5565 50(50) 50(20) 47(7) ? Cd1 Na2 As6 1_5565 . . 100(200) 131.1(7) 138.7(6) ? Cd1 Na2 Cd2 2_5565 . . 180(130) 170(90) 180(90) ? Cd1 Na2 Cd2 2_5565 . 2_5555 100(200) 100(60) 110(60) ? Cd1 Na2 Cd3 2_5565 . 1_5565 80(80) 80(110) 80(130) ? Cd1 Na2 Cd4 2_5565 . 1_4555 100(110) 95(7) 101(6) ? Cd1 Na2 As3 2_5565 . 3_5465 50(90) 50(100) 50(110) ? Cd1 Na2 As3 2_5565 . 4_5565 104(8) 102.4(3) 105.0(4) ? Cd1 Na2 As4 2_5565 . . 132(17) 131.5(11) 130(40) ? Cd1 Na2 As4 2_5565 . 2_5555 80(170) 73(10) 81(4) ? Cd1 Na2 As5 2_5565 . 1_5565 50(50) 50(20) 47(7) ? Cd1 Na2 As6 2_5565 . . 100(200) 131.1(7) 138.7(6) ? Cd2 Na2 Cd2 . . 2_5555 78(5) 78.0(9) 78(3) ? Cd2 Na2 Cd3 . . 1_5565 100(120) 100(100) 110(90) ? Cd2 Na2 Cd4 . . 1_4555 80(80) 80(110) 80(120) ? Cd2 Na2 As3 . . 3_5465 140(30) 134.5(12) 136.0(9) ? Cd2 Na2 As3 . . 4_5565 80(170) 70(130) 80(120) ? Cd2 Na2 As4 . . . 50(90) 44(17) 50(30) ? Cd2 Na2 As4 . . 2_5555 100(6) 99(10) 103(6) ? Cd2 Na2 As5 . . 1_5565 100(200) 129.0(14) 135.2(6) ? Cd2 Na2 As6 . . . 50(60) 50(40) 50(40) ? Cd2 Na2 Cd3 2_5555 . 1_5565 100(120) 100(100) 110(90) ? Cd2 Na2 Cd4 2_5555 . 1_4555 80(80) 80(110) 80(120) ? Cd2 Na2 As3 2_5555 . 3_5465 80(170) 70(130) 80(120) ? Cd2 Na2 As3 2_5555 . 4_5565 140(30) 134.5(12) 136.0(9) ? Cd2 Na2 As4 2_5555 . . 100(6) 99(10) 103(6) ? Cd2 Na2 As4 2_5555 . 2_5555 50(90) 44(17) 50(30) ? Cd2 Na2 As5 2_5555 . 1_5565 100(200) 129.0(14) 135.2(6) ? Cd2 Na2 As6 2_5555 . . 50(60) 50(40) 50(40) ? Cd3 Na2 Cd4 1_5565 . 1_4555 180(130) 175(3) 177(9) ? Cd3 Na2 As3 1_5565 . 3_5465 50(30) 50(30) 50(50) ? Cd3 Na2 As3 1_5565 . 4_5565 50(30) 50(30) 50(50) ? Cd3 Na2 As4 1_5565 . . 100(300) 131(4) 138(4) ? Cd3 Na2 As4 1_5565 . 2_5555 100(300) 131(4) 138(4) ? Cd3 Na2 As5 1_5565 . 1_5565 102(6) 102.2(3) 102.2(4) ? Cd3 Na2 As6 1_5565 . . 81(4) 81.0(3) 81.1(3) ? Cd4 Na2 As3 1_4555 . 3_5465 100(300) 128.9(7) 136.1(7) ? Cd4 Na2 As3 1_4555 . 4_5565 100(300) 128.9(7) 136.1(7) ? Cd4 Na2 As4 1_4555 . . 50(30) 45.3(6) 46.2(4) ? Cd4 Na2 As4 1_4555 . 2_5555 50(30) 45.3(6) 46.2(4) ? Cd4 Na2 As5 1_4555 . 1_5565 75(4) 74.6(2) 74.7(3) ? Cd4 Na2 As6 1_4555 . . 102(6) 101.9(3) 102.0(4) ? As3 Na2 As3 3_5465 . 4_5565 92(7) 91.8(3) 91.9(3) ? As3 Na2 As4 3_5465 . . 180(180) 175.0(15) 180(5) ? As3 Na2 As4 3_5465 . 2_5555 100(200) 86.4(14) 93.3(16) ? As3 Na2 As5 3_5465 . 1_5565 90(120) 90(40) 90(60) ? As3 Na2 As6 3_5465 . . 90(120) 89(8) 93(7) ? As3 Na2 As4 4_5565 . . 100(200) 86.4(14) 93.3(16) ? As3 Na2 As4 4_5565 . 2_5555 180(180) 175.0(15) 180(5) ? As3 Na2 As5 4_5565 . 1_5565 90(120) 90(40) 90(60) ? As3 Na2 As6 4_5565 . . 90(120) 89(8) 93(7) ? As4 Na2 As4 . . 2_5555 89(5) 88.6(3) 88.7(4) ? As4 Na2 As5 . . 1_5565 90(110) 86.7(17) 89.7(15) ? As4 Na2 As6 . . . 90(120) 87.8(18) 90.9(16) ? As4 Na2 As5 2_5555 . 1_5565 90(110) 86.7(17) 89.7(15) ? As4 Na2 As6 2_5555 . . 90(120) 87.8(18) 90.9(16) ? As5 Na2 As6 1_5565 . . 180(150) 174(4) 177(11) ? #======================================================================= # 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 2 0 0 0 99472.0 92347.0 3074.0 o -2 0 0 0 99456.0 69197.0 16982.0 o 4 0 0 0 43581.0 40384.0 2445.0 o -4 0 0 0 43630.0 38705.0 2456.0 o 6 0 0 0 25486.0 24554.0 554.0 o -6 0 0 0 25457.0 25358.0 2813.0 o 8 0 0 0 726.0 1472.0 637.0 < -8 0 0 0 746.0 605.0 155.0 o 10 0 0 0 130846.0 129818.0 500.0 o 1 1 0 -1 8.0 9.0 47.0 < -1 1 0 1 8.0 3.0 41.0 < 1 1 0 0 35.0 17.0 49.0 < -1 1 0 0 35.0 22.0 88.0 < 1 1 0 1 58.0 38.0 43.0 < -1 1 0 -1 58.0 25.0 47.0 < 3 1 0 -1 925.0 833.0 43.0 o -3 1 0 1 922.0 822.0 119.0 o 3 1 0 0 499.0 482.0 54.0 o -3 1 0 0 498.0 453.0 66.0 o 3 1 0 1 30.0 35.0 30.0 < -3 1 0 -1 30.0 33.0 39.0 < 5 1 0 -1 3331.0 3482.0 190.0 o -5 1 0 1 3327.0 2177.0 1123.0 < 5 1 0 0 5615.0 5461.0 258.0 o -5 1 0 0 5614.0 4164.0 1437.0 < 5 1 0 1 4320.0 4559.0 329.0 o -5 1 0 -1 4318.0 3045.0 1016.0 < 7 1 0 -1 250.0 360.0 63.0 o -7 1 0 1 249.0 183.0 92.0 < 7 1 0 0 1124.0 1266.0 71.0 o -7 1 0 0 1121.0 683.0 367.0 < 7 1 0 1 1482.0 1793.0 117.0 o -7 1 0 -1 1483.0 1139.0 581.0 < 9 1 0 -1 103.0 161.0 55.0 < -9 1 0 1 103.0 -24.0 125.0 < 9 1 0 0 193.0 190.0 95.0 < -9 1 0 0 195.0 -36.0 174.0 < 9 1 0 1 145.0 215.0 66.0 o 11 1 0 -1 3.0 -24.0 79.0 < -11 1 0 1 3.0 -44.0 101.0 < 11 1 0 0 111.0 32.0 190.0 < 11 1 0 1 44.0 36.0 52.0 < -11 1 0 -1 45.0 8.0 71.0 < 0 2 0 0 4.0 30.0 152.0 < 0 2 0 1 45.0 28.0 128.0 < 0 2 0 -1 45.0 24.0 79.0 < 2 2 0 -1 25.0 13.0 33.0 < -2 2 0 1 25.0 8.0 35.0 < 2 2 0 0 58.0 36.0 51.0 < -2 2 0 0 57.0 33.0 63.0 < 2 2 0 1 493.0 400.0 43.0 o -2 2 0 -1 493.0 400.0 46.0 o 4 2 0 -1 274.0 243.0 36.0 o -4 2 0 1 275.0 308.0 63.0 o 4 2 0 0 201.0 218.0 49.0 o -4 2 0 0 200.0 177.0 66.0 < 4 2 0 1 99.0 84.0 39.0 < -4 2 0 -1 100.0 68.0 55.0 < 6 2 0 -1 374.0 485.0 39.0 o -6 2 0 1 376.0 452.0 52.0 o 6 2 0 0 105.0 167.0 57.0 < -6 2 0 0 105.0 152.0 74.0 < 6 2 0 1 7.0 13.0 41.0 < -6 2 0 -1 7.0 0.0 39.0 < 8 2 0 -1 2214.0 2339.0 156.0 o -8 2 0 1 2214.0 2468.0 283.0 o 8 2 0 0 1254.0 1324.0 88.0 o -8 2 0 0 1253.0 1357.0 228.0 o 8 2 0 1 345.0 482.0 51.0 o -8 2 0 -1 348.0 376.0 92.0 o 10 2 0 -1 1452.0 1627.0 191.0 o -10 2 0 1 1459.0 1435.0 111.0 o 10 2 0 0 2784.0 2843.0 134.0 o 10 2 0 1 1701.0 1446.0 218.0 o 1 3 0 -1 5.0 3.0 74.0 < -1 3 0 1 5.0 -3.0 55.0 < 1 3 0 0 201434.0 203428.0 3266.0 o -1 3 0 0 201426.0 155757.0 35148.0 o 1 3 0 1 21.0 3.0 85.0 < -1 3 0 -1 21.0 5.0 62.0 < 3 3 0 -1 14.0 3.0 28.0 < -3 3 0 1 14.0 16.0 43.0 < 3 3 0 0 24932.0 22465.0 646.0 o -3 3 0 0 24912.0 24438.0 1452.0 o 3 3 0 1 6.0 -2.0 36.0 < -3 3 0 -1 6.0 2.0 39.0 < 5 3 0 -1 14.0 3.0 38.0 < -5 3 0 1 14.0 6.0 47.0 < 5 3 0 0 105408.0 81819.0 20136.0 o -5 3 0 0 105254.0 101643.0 1921.0 o 5 3 0 1 6.0 8.0 36.0 < -5 3 0 -1 6.0 0.0 44.0 < 7 3 0 -1 2.0 -28.0 43.0 < -7 3 0 1 2.0 -27.0 65.0 < 7 3 0 0 5549.0 6281.0 650.0 o -7 3 0 0 5549.0 5487.0 198.0 o 7 3 0 1 6.0 3.0 49.0 < -7 3 0 -1 6.0 -30.0 76.0 < 9 3 0 -1 4.0 13.0 74.0 < -9 3 0 1 4.0 -46.0 115.0 < 9 3 0 0 78119.0 92912.0 11174.0 o 9 3 0 1 1.0 35.0 81.0 < 11 3 0 -1 3.0 14.0 70.0 < -11 3 0 1 3.0 -46.0 95.0 < 11 3 0 0 5435.0 6937.0 1010.0 o 11 3 0 1 7.0 -55.0 98.0 < 0 4 0 0 9.0 54.0 147.0 < 0 4 0 1 54.0 25.0 115.0 < 0 4 0 -1 53.0 -5.0 96.0 < 2 4 0 -1 1050.0 917.0 117.0 o -2 4 0 1 1048.0 950.0 71.0 o 2 4 0 0 1022.0 888.0 128.0 o -2 4 0 0 1022.0 871.0 134.0 o 2 4 0 1 1422.0 1584.0 218.0 o -2 4 0 -1 1420.0 1235.0 79.0 o 4 4 0 -1 297.0 272.0 39.0 o -4 4 0 1 296.0 278.0 46.0 o 4 4 0 0 476.0 469.0 58.0 o -4 4 0 0 475.0 469.0 58.0 o 4 4 0 1 528.0 602.0 84.0 o -4 4 0 -1 525.0 599.0 66.0 o 6 4 0 -1 56.0 47.0 41.0 < -6 4 0 1 55.0 43.0 49.0 < 6 4 0 0 364.0 291.0 90.0 o -6 4 0 0 364.0 362.0 81.0 o 6 4 0 1 674.0 687.0 111.0 o -6 4 0 -1 673.0 810.0 55.0 o 8 4 0 -1 1321.0 1326.0 112.0 o -8 4 0 1 1321.0 1218.0 223.0 o 8 4 0 0 464.0 408.0 82.0 o -8 4 0 0 463.0 417.0 120.0 o 8 4 0 1 39.0 16.0 63.0 < -8 4 0 -1 39.0 70.0 70.0 < 10 4 0 -1 1273.0 1496.0 321.0 o -10 4 0 1 1280.0 1223.0 123.0 o 10 4 0 0 2264.0 2241.0 373.0 o -10 4 0 0 2268.0 2219.0 431.0 o 10 4 0 1 1211.0 796.0 114.0 o -10 4 0 -1 1218.0 518.0 175.0 < 1 5 0 -1 1504.0 1374.0 210.0 o -1 5 0 1 1503.0 1385.0 204.0 o 1 5 0 0 1148.0 1149.0 166.0 o -1 5 0 0 1148.0 759.0 253.0 < 1 5 0 1 942.0 839.0 119.0 o -1 5 0 -1 939.0 640.0 220.0 < 3 5 0 -1 1386.0 1427.0 147.0 o -3 5 0 1 1384.0 1301.0 58.0 o 3 5 0 0 1475.0 1266.0 96.0 o -3 5 0 0 1473.0 1366.0 92.0 o 3 5 0 1 1109.0 1013.0 68.0 o -3 5 0 -1 1108.0 943.0 62.0 o 5 5 0 -1 2224.0 2113.0 161.0 o -5 5 0 1 2219.0 2314.0 115.0 o 5 5 0 0 4484.0 4320.0 117.0 o -5 5 0 0 4485.0 4592.0 256.0 o 5 5 0 1 4284.0 4656.0 342.0 o -5 5 0 -1 4277.0 4495.0 172.0 o 7 5 0 -1 11.0 2.0 57.0 < -7 5 0 1 11.0 24.0 85.0 < 7 5 0 0 498.0 384.0 88.0 o -7 5 0 0 496.0 472.0 93.0 o 7 5 0 1 981.0 1172.0 161.0 o -7 5 0 -1 981.0 1052.0 122.0 o 9 5 0 -1 7.0 0.0 76.0 < -9 5 0 1 7.0 11.0 88.0 < 9 5 0 0 20.0 0.0 111.0 < -9 5 0 0 21.0 -2.0 169.0 < 9 5 0 1 21.0 44.0 81.0 < -9 5 0 -1 20.0 41.0 125.0 < 0 6 0 0 1727820.0 1963370.0 10321.0 o 0 6 0 1 21.0 13.0 100.0 < 0 6 0 -1 21.0 19.0 130.0 < 2 6 0 -1 44.0 -19.0 66.0 < -2 6 0 1 44.0 3.0 47.0 < 2 6 0 0 52855.0 53988.0 669.0 o -2 6 0 0 52838.0 50449.0 1699.0 o 2 6 0 1 44.0 -11.0 131.0 < -2 6 0 -1 44.0 5.0 46.0 < 4 6 0 -1 28.0 6.0 52.0 < -4 6 0 1 28.0 -16.0 54.0 < 4 6 0 0 29497.0 27699.0 1174.0 o -4 6 0 0 29542.0 27442.0 193.0 o 4 6 0 1 23.0 22.0 62.0 < -4 6 0 -1 23.0 13.0 47.0 < 6 6 0 -1 6.0 -3.0 55.0 < -6 6 0 1 6.0 -17.0 76.0 < 6 6 0 0 22052.0 21885.0 1136.0 o -6 6 0 0 22016.0 24168.0 1791.0 o 6 6 0 1 4.0 -14.0 63.0 < -6 6 0 -1 4.0 -6.0 52.0 < 8 6 0 -1 5.0 3.0 81.0 < -8 6 0 1 5.0 -14.0 96.0 < 8 6 0 0 963.0 904.0 149.0 o -8 6 0 0 985.0 806.0 145.0 o 8 6 0 1 8.0 11.0 82.0 < -8 6 0 -1 8.0 -24.0 95.0 < 10 6 0 -1 1.0 16.0 123.0 < -10 6 0 1 1.0 8.0 144.0 < 10 6 0 0 109222.0 132446.0 20717.0 o -10 6 0 0 109420.0 110367.0 8723.0 o 10 6 0 1 5.0 82.0 169.0 < -10 6 0 -1 5.0 44.0 118.0 < 1 7 0 -1 1143.0 1149.0 144.0 o -1 7 0 1 1143.0 1140.0 125.0 o 1 7 0 0 1506.0 1342.0 130.0 o -1 7 0 0 1506.0 1442.0 158.0 o 1 7 0 1 1350.0 1388.0 166.0 o -1 7 0 -1 1347.0 963.0 332.0 < 3 7 0 -1 122.0 139.0 58.0 < -3 7 0 1 120.0 147.0 43.0 o 3 7 0 0 7.0 52.0 77.0 < -3 7 0 0 7.0 36.0 73.0 < 3 7 0 1 488.0 548.0 77.0 o -3 7 0 -1 488.0 545.0 55.0 o 5 7 0 -1 2336.0 2442.0 131.0 o -5 7 0 1 2336.0 2504.0 180.0 o 5 7 0 0 3508.0 3544.0 161.0 o -5 7 0 0 3506.0 3659.0 326.0 o 5 7 0 1 2073.0 2428.0 243.0 o -5 7 0 -1 2075.0 2461.0 96.0 o 7 7 0 -1 628.0 814.0 74.0 o -7 7 0 1 627.0 708.0 190.0 o 7 7 0 0 1189.0 1231.0 130.0 o -7 7 0 0 1187.0 1273.0 250.0 o 7 7 0 1 1133.0 1394.0 228.0 o -7 7 0 -1 1135.0 1352.0 175.0 o 9 7 0 -1 374.0 294.0 133.0 < -9 7 0 1 376.0 253.0 144.0 < 9 7 0 0 564.0 395.0 179.0 < -9 7 0 0 567.0 256.0 202.0 < 9 7 0 1 341.0 300.0 114.0 < -9 7 0 -1 344.0 379.0 142.0 < 0 8 0 0 25.0 -66.0 212.0 < 0 8 0 1 107.0 77.0 136.0 < 0 8 0 -1 107.0 156.0 197.0 < 2 8 0 -1 397.0 420.0 161.0 < -2 8 0 1 395.0 248.0 114.0 < 2 8 0 0 184.0 204.0 234.0 < -2 8 0 0 185.0 109.0 88.0 < 2 8 0 1 9.0 19.0 126.0 < -2 8 0 -1 9.0 36.0 58.0 < 4 8 0 -1 1273.0 1305.0 131.0 o -4 8 0 1 1273.0 1296.0 115.0 o 4 8 0 0 1323.0 1397.0 160.0 o -4 8 0 0 1320.0 1427.0 96.0 o 4 8 0 1 1003.0 1182.0 117.0 o -4 8 0 -1 1007.0 1267.0 73.0 o 6 8 0 -1 1055.0 1329.0 155.0 o -6 8 0 1 1054.0 1196.0 398.0 o 6 8 0 0 848.0 973.0 130.0 o -6 8 0 0 851.0 1014.0 235.0 o 6 8 0 1 319.0 444.0 88.0 o -6 8 0 -1 320.0 329.0 136.0 < 8 8 0 -1 1980.0 2519.0 256.0 o -8 8 0 1 1981.0 2265.0 199.0 o 8 8 0 0 1484.0 1490.0 218.0 o -8 8 0 0 1483.0 1609.0 220.0 o 8 8 0 1 624.0 656.0 166.0 o -8 8 0 -1 629.0 872.0 115.0 o 10 8 0 -1 985.0 528.0 256.0 < 10 8 0 0 2258.0 1465.0 296.0 o -10 8 0 0 2263.0 1880.0 597.0 o 10 8 0 1 1459.0 814.0 400.0 < -10 8 0 -1 1465.0 414.0 156.0 < 1 9 0 -1 17.0 -22.0 101.0 < -1 9 0 1 17.0 17.0 128.0 < 1 9 0 0 108287.0 109912.0 2066.0 o -1 9 0 0 108338.0 110907.0 1403.0 o 1 9 0 1 72.0 9.0 95.0 < -1 9 0 -1 72.0 -14.0 79.0 < 3 9 0 -1 59.0 -35.0 229.0 < -3 9 0 1 59.0 17.0 55.0 < 3 9 0 0 7174.0 7944.0 575.0 o -3 9 0 0 7155.0 7433.0 279.0 o 3 9 0 1 25.0 28.0 175.0 < -3 9 0 -1 26.0 38.0 49.0 < 5 9 0 -1 67.0 -13.0 103.0 < -5 9 0 1 68.0 14.0 66.0 < 5 9 0 0 46684.0 46366.0 2300.0 o -5 9 0 0 46557.0 44696.0 292.0 o 5 9 0 1 27.0 -22.0 131.0 < -5 9 0 -1 27.0 -49.0 68.0 < 7 9 0 -1 15.0 11.0 156.0 < -7 9 0 1 15.0 57.0 147.0 < 7 9 0 0 6499.0 7586.0 327.0 o -7 9 0 0 6509.0 6971.0 220.0 o 7 9 0 1 34.0 27.0 128.0 < -7 9 0 -1 34.0 24.0 109.0 < 9 9 0 -1 19.0 58.0 325.0 < -9 9 0 1 19.0 -28.0 362.0 < 9 9 0 0 61832.0 64434.0 6373.0 o -9 9 0 0 61813.0 72535.0 1065.0 o 9 9 0 1 6.0 14.0 313.0 < -9 9 0 -1 6.0 -9.0 441.0 < 0 10 0 0 37.0 126.0 316.0 < 0 10 0 1 169.0 103.0 188.0 < 0 10 0 -1 169.0 46.0 201.0 < 2 10 0 -1 1402.0 1427.0 256.0 o -2 10 0 1 1397.0 1519.0 158.0 o 2 10 0 0 1238.0 1332.0 191.0 o -2 10 0 0 1238.0 959.0 354.0 < 2 10 0 1 1187.0 1237.0 133.0 o -2 10 0 -1 1184.0 743.0 370.0 < 4 10 0 -1 953.0 1305.0 379.0 o -4 10 0 1 951.0 1112.0 190.0 o 4 10 0 0 1348.0 1466.0 378.0 o -4 10 0 0 1350.0 1569.0 242.0 o 4 10 0 1 1210.0 1294.0 175.0 o -4 10 0 -1 1208.0 1359.0 79.0 o 6 10 0 -1 467.0 509.0 169.0 o -6 10 0 1 463.0 645.0 118.0 o 6 10 0 0 1279.0 1174.0 354.0 o -6 10 0 0 1279.0 1237.0 115.0 o 6 10 0 1 1330.0 942.0 378.0 < 8 10 0 -1 460.0 466.0 243.0 < -8 10 0 1 461.0 212.0 160.0 < 8 10 0 0 43.0 57.0 354.0 < -8 10 0 0 42.0 38.0 234.0 < 8 10 0 1 79.0 93.0 253.0 < -8 10 0 -1 79.0 164.0 103.0 < 1 11 0 -1 1691.0 2026.0 262.0 o -1 11 0 1 1690.0 1776.0 240.0 o 1 11 0 0 1584.0 1814.0 193.0 o -1 11 0 0 1582.0 1543.0 213.0 o 1 11 0 1 1204.0 1375.0 174.0 o -1 11 0 -1 1200.0 1381.0 141.0 o 3 11 0 -1 755.0 855.0 155.0 o -3 11 0 1 754.0 453.0 231.0 < 3 11 0 0 1123.0 1182.0 196.0 o -3 11 0 0 1121.0 1144.0 88.0 o 3 11 0 1 1278.0 1400.0 278.0 o -3 11 0 -1 1276.0 1356.0 180.0 o 5 11 0 -1 743.0 678.0 278.0 < -5 11 0 1 739.0 686.0 95.0 o 5 11 0 0 2033.0 2118.0 425.0 o -5 11 0 0 2035.0 2241.0 378.0 o 5 11 0 1 2255.0 2407.0 232.0 o -5 11 0 -1 2248.0 1963.0 161.0 o 7 11 0 -1 121.0 164.0 327.0 < -7 11 0 1 122.0 95.0 118.0 < 7 11 0 0 77.0 -141.0 509.0 < -7 11 0 0 77.0 49.0 209.0 < 7 11 0 1 346.0 550.0 378.0 < -7 11 0 -1 345.0 275.0 130.0 < 9 11 0 -1 86.0 62.0 231.0 < -9 11 0 1 86.0 60.0 90.0 < 9 11 0 0 117.0 130.0 602.0 < -9 11 0 0 118.0 -27.0 305.0 < 9 11 0 1 66.0 79.0 276.0 < -9 11 0 -1 65.0 77.0 196.0 < 0 12 0 0 639888.0 703844.0 3676.0 o 0 12 0 1 42.0 175.0 177.0 < 0 12 0 -1 43.0 66.0 156.0 < 2 12 0 -1 67.0 -5.0 145.0 < -2 12 0 1 67.0 -25.0 87.0 < 2 12 0 0 14174.0 15440.0 354.0 o -2 12 0 0 14158.0 13932.0 487.0 o 2 12 0 1 85.0 60.0 137.0 < -2 12 0 -1 85.0 46.0 66.0 < 4 12 0 -1 55.0 -11.0 185.0 < -4 12 0 1 56.0 -5.0 63.0 < 4 12 0 0 10335.0 10276.0 287.0 o -4 12 0 0 10382.0 9582.0 440.0 o 4 12 0 1 63.0 5.0 120.0 < -4 12 0 -1 63.0 14.0 65.0 < 6 12 0 -1 9.0 -25.0 362.0 < -6 12 0 1 9.0 0.0 107.0 < 6 12 0 0 16347.0 17657.0 1199.0 o -6 12 0 0 16292.0 16186.0 274.0 o 6 12 0 1 18.0 -77.0 313.0 < -6 12 0 -1 18.0 11.0 87.0 < 8 12 0 -1 16.0 -41.0 479.0 < -8 12 0 1 16.0 -11.0 90.0 < 8 12 0 0 1425.0 1297.0 559.0 < -8 12 0 0 1447.0 976.0 221.0 o 8 12 0 1 14.0 -63.0 265.0 < -8 12 0 -1 13.0 39.0 147.0 < 1 13 0 -1 1206.0 1421.0 209.0 o -1 13 0 1 1207.0 1348.0 207.0 o 1 13 0 0 1651.0 1901.0 333.0 o -1 13 0 0 1654.0 1748.0 272.0 o 1 13 0 1 1200.0 1340.0 216.0 o -1 13 0 -1 1196.0 1305.0 228.0 o 3 13 0 -1 4.0 16.0 164.0 < -3 13 0 1 4.0 -9.0 71.0 < 3 13 0 0 114.0 139.0 215.0 < -3 13 0 0 114.0 87.0 100.0 < 3 13 0 1 677.0 814.0 167.0 o -3 13 0 -1 676.0 493.0 243.0 < 5 13 0 -1 1057.0 1327.0 175.0 o -5 13 0 1 1058.0 1318.0 96.0 o 5 13 0 0 1516.0 1438.0 234.0 o -5 13 0 0 1513.0 1868.0 218.0 o 5 13 0 1 674.0 689.0 182.0 o -5 13 0 -1 677.0 684.0 100.0 o 7 13 0 -1 561.0 640.0 297.0 < -7 13 0 1 561.0 292.0 185.0 < 7 13 0 0 748.0 510.0 480.0 < -7 13 0 0 748.0 -212.0 243.0 < 7 13 0 1 516.0 586.0 355.0 < -7 13 0 -1 518.0 820.0 179.0 o 0 14 0 0 3.0 22.0 196.0 < 0 14 0 1 67.0 55.0 147.0 < 0 14 0 -1 67.0 66.0 131.0 < 2 14 0 -1 400.0 540.0 229.0 < -2 14 0 1 397.0 472.0 104.0 o 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