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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_Cd4Na1P3_298 #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Cd4 Na1 P3' _chemical_formula_weight 565.6 _chemical_melting_point ? #======================================================================= # 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 4.3445(5) _cell_length_b 4.3445(5) _cell_length_c 33.197(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 542.64(12) _cell_formula_units_Z 3 _cell_measurement_reflns_used 2479 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 32.17 _cell_measurement_temperature 298 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 5.192 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 12.309 _exptl_crystal_description plate _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.010 _exptl_crystal_size_rad ? _exptl_crystal_colour black _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'Jana2006' _exptl_absorpt_correction_T_min 0.3914 _exptl_absorpt_correction_T_max 0.8087 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 3 -1 15 0.0399 0 0 1 0.0094 1 -1 30 0.0190 1 0 -30 0.0139 -30 17 -21 0.0491 0 -1 -15 0.0234 -1 2 -30 0.0177 #======================================================================= # 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 1219 _diffrn_reflns_theta_min 3.7 _diffrn_reflns_theta_max 31.97 _diffrn_reflns_theta_full 31.97 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_unetI/netI 0.0332 _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 48 _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 _refine_special_details ? _reflns_number_total 160 _reflns_number_gt 128 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_gt 0.0699 _refine_ls_R_factor_all 0.0492 _refine_ls_wR_factor_ref 0.0719 _refine_ls_goodness_of_fit_ref 1.91 _refine_ls_goodness_of_fit_gt 2.10 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 160 _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 0.0047 _refine_ls_shift/su_mean 0.0018 _refine_diff_density_max 1.31 _refine_diff_density_min -1.87 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 490(50) _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 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' P 0.1048 0.0969 '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 0.09768(6) Uani 0.0324(6) 6 1 d . . . P1 P 0 0 0.22205(12) Uani 0.0101(11) 6 1 d . . . Cd2 Cd 0 0 0.29950(4) Uani 0.0313(6) 6 1 d . . . Na1 Na 0 0 0.5 Uani 0.029(3) 3 1 d . . . P2 P 0 0 0 Uani 0.0153(16) 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 0.0120(6) 0.0120(6) 0.0733(13) 0.0060(3) 0 0 P1 P 0.0095(13) 0.0095(13) 0.011(2) 0.0047(7) 0 0 Cd2 Cd 0.0405(7) 0.0405(7) 0.0130(7) 0.0202(4) 0 0 Na1 Na 0.027(4) 0.027(4) 0.034(7) 0.013(2) 0 0 P2 P 0.0112(17) 0.0112(17) 0.023(3) 0.0056(9) 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 P1 . 16_445 2.5486(11) ? Cd1 P1 . 16_455 2.5486(8) ? Cd1 P1 . 16_555 2.5486(11) ? Cd1 Na1 . 25_444 3.3966(15) ? Cd1 Na1 . 25_544 3.3966(13) ? Cd1 Na1 . 25_554 3.3966(15) ? P1 Cd2 . . 2.571(4) ? P1 Na1 . 25_444 3.110(2) ? P1 Na1 . 25_544 3.110(2) ? P1 Na1 . 25_554 3.110(2) ? Cd2 P2 . 13_445 2.7483(10) ? Cd2 P2 . 13_455 2.7483(7) ? Cd2 P2 . 13_555 2.7483(10) ? 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 P1 Cd1 P1 16_445 . 16_455 116.93(4) ? P1 Cd1 P1 16_445 . 16_555 116.93(4) ? P1 Cd1 Na1 16_445 . 25_444 61.13(6) ? P1 Cd1 Na1 16_445 . 25_544 61.13(6) ? P1 Cd1 Na1 16_445 . 25_554 127.39(11) ? P1 Cd1 P1 16_455 . 16_555 116.93(4) ? P1 Cd1 Na1 16_455 . 25_444 61.13(6) ? P1 Cd1 Na1 16_455 . 25_544 127.39(11) ? P1 Cd1 Na1 16_455 . 25_554 61.13(6) ? P1 Cd1 Na1 16_555 . 25_444 127.39(11) ? P1 Cd1 Na1 16_555 . 25_544 61.13(6) ? P1 Cd1 Na1 16_555 . 25_554 61.13(6) ? Na1 Cd1 Na1 25_444 . 25_544 79.52(4) ? Na1 Cd1 Na1 25_444 . 25_554 79.52(4) ? Na1 Cd1 Na1 25_544 . 25_554 79.52(4) ? Cd1 P1 Cd1 16_445 . 16_455 116.93(5) ? Cd1 P1 Cd1 16_445 . 16_555 116.93(5) ? Cd1 P1 Cd2 16_445 . . 79.79(10) ? Cd1 P1 Na1 16_445 . 25_444 73.02(4) ? Cd1 P1 Na1 16_445 . 25_544 73.02(4) ? Cd1 P1 Na1 16_445 . 25_554 153.97(15) ? Cd1 P1 Cd1 16_455 . 16_555 116.93(5) ? Cd1 P1 Cd2 16_455 . . 79.79(10) ? Cd1 P1 Na1 16_455 . 25_444 73.02(4) ? Cd1 P1 Na1 16_455 . 25_544 153.97(15) ? Cd1 P1 Na1 16_455 . 25_554 73.02(4) ? Cd1 P1 Cd2 16_555 . . 79.79(10) ? Cd1 P1 Na1 16_555 . 25_444 153.97(15) ? Cd1 P1 Na1 16_555 . 25_544 73.02(4) ? Cd1 P1 Na1 16_555 . 25_554 73.02(4) ? Cd2 P1 Na1 . . 25_444 126.24(6) ? Cd2 P1 Na1 . . 25_544 126.24(6) ? Cd2 P1 Na1 . . 25_554 126.24(6) ? Na1 P1 Na1 25_444 . 25_544 88.61(8) ? Na1 P1 Na1 25_444 . 25_554 88.61(8) ? Na1 P1 Na1 25_544 . 25_554 88.61(8) ? P1 Cd2 P2 . . 13_445 114.12(3) ? P1 Cd2 P2 . . 13_455 114.12(3) ? P1 Cd2 P2 . . 13_555 114.12(3) ? P2 Cd2 P2 13_445 . 13_455 104.45(3) ? P2 Cd2 P2 13_445 . 13_555 104.45(3) ? P2 Cd2 P2 13_455 . 13_555 104.45(3) ? Cd1 Na1 Cd1 13_445 . 13_455 79.52(3) ? Cd1 Na1 Cd1 13_445 . 13_555 79.52(3) ? Cd1 Na1 Cd1 13_445 . 28_445 100.48(3) ? Cd1 Na1 Cd1 13_445 . 28_545 100.48(3) ? Cd1 Na1 Cd1 13_445 . 28_555 180.0(5) ? Cd1 Na1 P1 13_445 . 13_445 78.64(6) ? Cd1 Na1 P1 13_445 . 13_455 134.14(3) ? Cd1 Na1 P1 13_445 . 13_555 134.14(3) ? Cd1 Na1 P1 13_445 . 28_445 45.86(3) ? Cd1 Na1 P1 13_445 . 28_545 45.86(3) ? Cd1 Na1 P1 13_445 . 28_555 101.36(6) ? Cd1 Na1 Cd1 13_455 . 13_555 79.52(3) ? Cd1 Na1 Cd1 13_455 . 28_445 100.48(3) ? Cd1 Na1 Cd1 13_455 . 28_545 180.0(5) ? Cd1 Na1 Cd1 13_455 . 28_555 100.48(3) ? Cd1 Na1 P1 13_455 . 13_445 134.14(3) ? Cd1 Na1 P1 13_455 . 13_455 78.64(6) ? Cd1 Na1 P1 13_455 . 13_555 134.14(3) ? Cd1 Na1 P1 13_455 . 28_445 45.86(3) ? Cd1 Na1 P1 13_455 . 28_545 101.36(6) ? Cd1 Na1 P1 13_455 . 28_555 45.86(3) ? Cd1 Na1 Cd1 13_555 . 28_445 180.0(5) ? Cd1 Na1 Cd1 13_555 . 28_545 100.48(3) ? Cd1 Na1 Cd1 13_555 . 28_555 100.48(3) ? Cd1 Na1 P1 13_555 . 13_445 134.14(3) ? Cd1 Na1 P1 13_555 . 13_455 134.14(3) ? Cd1 Na1 P1 13_555 . 13_555 78.64(6) ? Cd1 Na1 P1 13_555 . 28_445 101.36(6) ? Cd1 Na1 P1 13_555 . 28_545 45.86(3) ? Cd1 Na1 P1 13_555 . 28_555 45.86(3) ? Cd1 Na1 Cd1 28_445 . 28_545 79.52(3) ? Cd1 Na1 Cd1 28_445 . 28_555 79.52(3) ? Cd1 Na1 P1 28_445 . 13_445 45.86(3) ? Cd1 Na1 P1 28_445 . 13_455 45.86(3) ? Cd1 Na1 P1 28_445 . 13_555 101.36(6) ? Cd1 Na1 P1 28_445 . 28_445 78.64(6) ? Cd1 Na1 P1 28_445 . 28_545 134.14(3) ? Cd1 Na1 P1 28_445 . 28_555 134.14(3) ? Cd1 Na1 Cd1 28_545 . 28_555 79.52(3) ? Cd1 Na1 P1 28_545 . 13_445 45.86(3) ? Cd1 Na1 P1 28_545 . 13_455 101.36(6) ? Cd1 Na1 P1 28_545 . 13_555 45.86(3) ? Cd1 Na1 P1 28_545 . 28_445 134.14(3) ? Cd1 Na1 P1 28_545 . 28_545 78.64(6) ? Cd1 Na1 P1 28_545 . 28_555 134.14(3) ? Cd1 Na1 P1 28_555 . 13_445 101.36(6) ? Cd1 Na1 P1 28_555 . 13_455 45.86(3) ? Cd1 Na1 P1 28_555 . 13_555 45.86(3) ? Cd1 Na1 P1 28_555 . 28_445 134.14(3) ? Cd1 Na1 P1 28_555 . 28_545 134.14(3) ? Cd1 Na1 P1 28_555 . 28_555 78.64(6) ? P1 Na1 P1 13_445 . 13_455 88.61(6) ? P1 Na1 P1 13_445 . 13_555 88.61(6) ? P1 Na1 P1 13_445 . 28_445 91.39(6) ? P1 Na1 P1 13_445 . 28_545 91.39(6) ? P1 Na1 P1 13_445 . 28_555 180.0(5) ? P1 Na1 P1 13_455 . 13_555 88.61(6) ? P1 Na1 P1 13_455 . 28_445 91.39(6) ? P1 Na1 P1 13_455 . 28_545 180.0(5) ? P1 Na1 P1 13_455 . 28_555 91.39(6) ? P1 Na1 P1 13_555 . 28_445 180.0(5) ? P1 Na1 P1 13_555 . 28_545 91.39(6) ? P1 Na1 P1 13_555 . 28_555 91.39(6) ? P1 Na1 P1 28_445 . 28_545 88.61(6) ? P1 Na1 P1 28_445 . 28_555 88.61(6) ? P1 Na1 P1 28_545 . 28_555 88.61(6) ? Cd2 P2 Cd2 25_444 . 25_544 104.45(2) ? Cd2 P2 Cd2 25_444 . 25_554 104.45(2) ? Cd2 P2 Cd2 25_444 . 16_445 75.55(2) ? Cd2 P2 Cd2 25_444 . 16_455 75.55(2) ? Cd2 P2 Cd2 25_444 . 16_555 180.0(5) ? Cd2 P2 Cd2 25_544 . 25_554 104.45(2) ? Cd2 P2 Cd2 25_544 . 16_445 75.55(2) ? Cd2 P2 Cd2 25_544 . 16_455 180.0(5) ? Cd2 P2 Cd2 25_544 . 16_555 75.55(2) ? Cd2 P2 Cd2 25_554 . 16_445 180.0(5) ? Cd2 P2 Cd2 25_554 . 16_455 75.55(2) ? Cd2 P2 Cd2 25_554 . 16_555 75.55(2) ? Cd2 P2 Cd2 16_445 . 16_455 104.45(2) ? Cd2 P2 Cd2 16_445 . 16_555 104.45(2) ? Cd2 P2 Cd2 16_455 . 16_555 104.45(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 247783.00 238415.00 9121.67 o 0 3 0 99968.80 95836.50 748.71 o -2 4 0 70252.50 67016.60 705.55 o -1 1 1 23012.70 23216.50 357.93 o 0 2 1 15099.20 14891.90 153.03 o -2 3 1 11800.80 11327.80 107.30 o -4 4 1 6974.50 6320.55 222.06 o -1 4 1 8179.19 8795.93 109.63 o -3 5 1 5991.98 5828.71 122.13 o 0 1 2 13289.50 14006.60 203.53 o -2 2 2 5307.82 5083.18 135.68 o -1 3 2 2523.04 2702.28 88.26 o -3 4 2 645.48 694.41 102.40 o 0 4 2 321.36 470.24 161.54 < -2 5 2 151.21 348.62 123.14 < -1 2 3 5025.84 4593.13 97.00 o -3 3 3 905.28 1029.29 131.26 o 0 3 3 905.28 726.74 144.07 o -2 4 3 374.23 479.89 97.58 o -1 1 4 25.21 140.72 159.91 < 0 2 4 85.90 148.73 140.73 < -2 3 4 162.43 340.66 91.16 o -4 4 4 281.19 647.76 163.14 o -1 4 4 248.78 259.10 102.36 < -3 5 4 307.55 641.36 119.96 o 0 1 5 162678.00 169454.00 3019.12 o -2 2 5 88589.40 84598.50 1560.60 o -1 3 5 52602.60 51350.20 421.94 o -3 4 5 22249.30 22081.50 112.77 o 0 4 5 15514.00 15087.40 393.97 o -2 5 5 11204.90 11602.50 145.25 o 0 0 6 12554.10 15816.80 1443.51 o -1 2 6 8720.62 8409.04 96.06 o -3 3 6 5782.65 5126.43 135.24 o 0 3 6 5782.65 6158.48 185.16 o -2 4 6 4944.44 4943.55 104.46 o -1 1 7 1657.13 1906.17 157.51 o 0 2 7 327.68 380.78 115.19 o -2 3 7 15.38 108.73 92.74 < -4 4 7 235.29 443.01 169.53 < -1 4 7 130.68 135.93 111.94 < -3 5 7 319.28 513.41 124.75 o 0 1 8 4465.26 3844.09 153.89 o -2 2 8 1614.98 1555.38 133.09 o -1 3 8 522.57 451.23 88.01 o -3 4 8 15.83 204.67 108.73 < 0 4 8 3.03 73.55 143.91 < -2 5 8 25.33 22.39 127.92 < 0 0 9 26197.40 32107.50 1171.39 o -1 2 9 16585.80 16924.70 227.69 o -3 3 9 11166.40 12559.00 285.06 o 0 3 9 11166.40 11153.10 179.78 o -2 4 9 9545.03 10352.70 166.28 o -1 1 10 220461.00 213434.00 5628.22 o 0 2 10 126831.00 120956.00 1510.38 o -2 3 10 80949.80 79177.50 476.76 o -4 4 10 28476.70 28779.30 337.58 o -1 4 10 38911.50 38215.70 414.63 o -3 5 10 21370.50 21953.10 136.66 o 0 1 11 3951.07 4271.95 156.61 o -2 2 11 3301.99 3161.94 155.93 o -1 3 11 2814.90 2983.12 93.07 o -3 4 11 2169.19 1884.29 110.56 o 0 4 11 1938.20 2155.87 158.57 o 0 0 12 5729.04 7634.05 794.94 o -1 2 12 2028.34 2270.54 96.28 o -3 3 12 221.97 292.69 137.55 < 0 3 12 221.97 647.75 169.54 o -2 4 12 45.08 188.69 105.54 < -1 1 13 32727.00 31664.90 959.70 o 0 2 13 18487.80 17060.60 254.81 o -2 3 13 11598.50 11433.80 145.94 o -4 4 13 3666.26 4053.33 178.04 o -1 4 13 5246.74 4907.17 107.66 o 0 1 14 2097.84 2166.39 157.38 o -2 2 14 949.54 1024.79 156.92 o -1 3 14 473.06 495.97 95.99 o -3 4 14 106.48 151.92 116.74 < 0 4 14 41.76 27.18 155.11 < 0 0 15 151721.00 163392.00 1374.11 o -1 2 15 87747.30 86849.50 670.96 o -3 3 15 36894.30 37289.20 667.81 o 0 3 15 36894.30 36840.60 1056.53 o -2 4 15 25704.40 25437.60 219.43 o -1 1 16 8201.22 9137.81 288.95 o 0 2 16 6713.55 6763.67 284.04 o -2 3 16 5718.23 5489.81 162.55 o -4 4 16 3781.45 3392.54 186.07 o -1 4 16 4317.12 4393.43 113.97 o 0 1 17 8058.23 8864.30 220.55 o -2 2 17 4012.11 4099.38 147.90 o -1 3 17 2095.47 2046.69 100.97 o -3 4 17 574.44 574.33 118.39 o 0 4 17 285.74 316.67 268.69 < 0 0 18 2199.16 2422.89 659.91 o -1 2 18 636.24 683.38 108.83 o -3 3 18 6.32 137.51 155.10 < 0 3 18 6.32 -63.96 147.11 < -2 4 18 27.91 75.15 110.33 < -1 1 19 714.31 622.72 206.51 o 0 2 19 929.25 1136.61 145.68 o -2 3 19 1057.13 1229.41 107.25 o -1 4 19 1106.27 1232.40 112.04 o 0 1 20 65725.70 68356.40 1217.51 o -2 2 20 40050.40 42298.50 1380.26 o -1 3 20 25792.50 26456.40 298.85 o -3 4 20 12059.10 12835.10 130.85 o 0 0 21 1639.32 2185.11 609.20 o -1 2 21 1550.71 1720.66 115.35 o -3 3 21 1356.63 1071.10 172.91 o 0 3 21 1356.63 1344.88 158.50 o -2 4 21 1256.28 1096.50 126.46 o -1 1 22 57.81 297.44 171.11 < 0 2 22 40.73 284.63 155.11 < -2 3 22 218.45 307.07 118.35 < -1 4 22 554.18 639.89 118.38 o 0 1 23 23183.10 23613.80 430.24 o -2 2 23 15087.10 16287.70 409.71 o -1 3 23 10239.40 10681.50 122.74 o -3 4 23 5099.22 5838.41 139.70 o 0 0 24 555.78 1382.58 564.87 < -1 2 24 173.73 487.79 113.55 o -3 3 24 1.12 -87.94 174.29 < 0 3 24 1.12 167.89 169.49 < -2 4 24 6.40 231.85 137.51 < -1 1 25 54871.50 55277.40 824.35 o 0 2 25 36030.70 36546.10 678.68 o -2 3 25 24644.10 24320.80 235.55 o 0 1 26 2.25 147.11 166.29 < -2 2 26 21.03 196.68 172.70 < -1 3 26 49.29 179.10 127.93 < 0 0 27 15232.90 15158.00 568.28 o -1 2 27 9612.14 8949.71 198.63 o -3 3 27 4139.66 3547.84 195.76 o 0 3 27 4139.66 3636.09 189.35 o -1 1 28 4363.10 4701.06 178.34 o 0 2 28 2454.71 2969.96 189.13 o -2 3 28 1411.85 1876.35 129.68 o 0 1 29 2372.34 3743.04 179.54 o -2 2 29 1436.41 1831.72 182.53 o -1 3 29 885.39 1204.96 142.42 o 0 0 30 29376.80 29465.00 618.49 o -1 2 30 19007.70 18378.30 252.32 o -1 1 31 2288.51 2370.29 177.89 o 0 2 31 2113.98 1925.64 203.46 o -2 3 31 1920.92 1558.31 147.34 o 0 1 32 458.12 241.55 174.37 < -2 2 32 106.51 81.56 190.30 < -1 3 32 7.70 -73.55 156.70 < 0 0 33 6433.23 6511.48 593.71 o -1 2 33 4063.60 4663.32 155.66 o -1 1 34 276.49 886.06 215.92 o 0 2 34 102.01 737.20 214.28 o 0 1 35 12057.60 10705.00 378.17 o -2 2 35 7866.52 6884.96 238.19 o 0 0 36 1726.38 2259.64 621.36 o -1 2 36 1213.20 1464.55 145.65 o -1 1 37 5528.26 5127.89 184.74 o 0 1 38 6307.84 6011.53 192.88 o 0 0 39 1675.31 3223.25 618.07 o #======================================================================= data_Cd4Na1P3_130_mod #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Cd4 Na1 P3' _chemical_formula_weight 565.6 _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 7.5098(8) _cell_length_b 13.0065(10) _cell_length_c 11.2885(11) _cell_angle_alpha 90 _cell_angle_beta 102.827(8) _cell_angle_gamma 90 _cell_volume 1075.10(18) 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(9) 1 0 0 0 1 0 0 0 1 2 0.55(9) -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 -0.040000 0.000000 0.342262 _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 5.2411 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 12.425 _exptl_crystal_description plate _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.010 _exptl_crystal_size_rad ? _exptl_crystal_colour black _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'Jana2006' _exptl_absorpt_correction_T_min 0.1598 _exptl_absorpt_correction_T_max 0.2853 #======================================================================= # 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 ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '??integration method??' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 27871 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 29.38 _diffrn_reflns_theta_full 29.38 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_unetI/netI 0.0832 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _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 _refine_special_details ? _reflns_number_total 8466 _reflns_number_gt 2895 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_gt 0.0661 _refine_ls_R_factor_all 0.1331 _refine_ls_wR_factor_ref 0.0927 _refine_ls_goodness_of_fit_ref 0.89 _refine_ls_goodness_of_fit_gt 1.11 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 8466 _refine_ls_number_parameters 211 _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 0.0043 _refine_ls_shift/su_mean 0.0011 _refine_diff_density_max 2.18 _refine_diff_density_min -1.53 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 316(11) _refine_ls_abs_structure_details ; 4172 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0.55(9) _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' P 0.1048 0.0969 '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' 0.0768 0.0274 0.0661 Sat1 '1st-order satellites' 0.2345 0.0552 0.1984 #======================================================================= # 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 0.1767(3) 0.1661(2) 0.0315(2) Uani 0.0216(6) 4 1 d . . . Cd2 Cd 0.3729(3) 0.1670(2) 0.6203(2) Uani 0.0220(6) 4 1 d . . . Cd3 Cd 0.6842(5) 0 0.0525(3) Uani 0.0153(7) 2 1 d . . . Cd4 Cd 0.8809(6) 0 0.6409(4) Uani 0.0229(9) 2 1 d . . . Cd5 Cd 0.0689(3) 0.3257(2) 0.2300(2) Uani 0.0214(5) 4 1 d . . . Cd6 Cd 0.4707(3) 0.3403(3) 0.4339(2) Uani 0.0195(5) 4 1 d . . . Cd7 Cd 0.0921(5) 0 0.2298(4) Uani 0.0221(7) 2 1 d . . . Cd8 Cd 0.4926(5) 0 0.4325(4) Uani 0.0207(7) 2 1 d . . . P1 P 0.2767(9) 0.1665(7) 0.3312(7) Uani 0.0121(11) 4 1 d . . . P2 P 0.7744(9) 0 0.3197(7) Uani 0.009(2) 2 1 d . . . P3 P 0.0019(8) 0.3330(5) 0.0005(5) Uiso 0.0015(9) 4 1 d . . . P4 P 0.0600(10) 0.1683(5) 0.6720(7) Uani 0.0153(12) 4 1 d . . . P5 P 0.0007(15) 0 0.0001(10) Uiso 0.0034(15) 2 1 d . . . P6 P 0.5561(16) 0 0.6687(12) Uani 0.0163(18) 2 1 d . . . Na1 Na 0.2694(17) 0.334(2) 0.8353(9) Uani 0.0150(12) 4 1 d . . . Na2 Na 0.288(2) 0 0.8353(11) 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 0.0107(8) 0.0095(8) 0.0473(12) 0.0004(7) 0.0120(7) 0.0008(8) Cd2 Cd 0.0124(8) 0.0126(8) 0.0422(12) 0.0002(7) 0.0085(7) 0.0010(9) Cd3 Cd 0.0055(10) 0.0024(10) 0.0387(14) 0 0.0068(9) 0 Cd4 Cd 0.0105(11) 0.0056(12) 0.055(2) 0 0.0123(12) 0 Cd5 Cd 0.0250(8) 0.0266(9) 0.0126(6) 0.0018(7) 0.0041(5) 0.0020(6) Cd6 Cd 0.0239(8) 0.0203(9) 0.0136(7) 0.0030(7) 0.0028(6) -0.0001(6) Cd7 Cd 0.0256(13) 0.0246(14) 0.0142(10) 0 0.0001(9) 0 Cd8 Cd 0.0193(11) 0.0278(15) 0.0146(10) 0 0.0030(9) 0 P1 P 0.009(2) 0.0096(18) 0.0181(18) 0.0003(7) 0.0036(13) -0.0008(11) P2 P 0.009(4) 0.007(3) 0.011(3) 0 0.004(2) 0 P4 P 0.0129(16) 0.0133(15) 0.020(2) -0.0009(10) 0.0042(13) -0.0015(14) P6 P 0.010(2) 0.011(2) 0.028(4) 0 0.0049(19) 0 Na1 Na 0.0142(18) 0.016(2) 0.0164(18) -0.001(3) 0.0058(14) 0.0002(19) 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 P1x1 P1 x 1 P1y1 P1 y 1 P1z1 P1 z 1 P3x1 P3 x 1 P3y1 P3 y 1 P3z1 P3 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 -0.0077(4) 0.000(2) Cd1y1 -0.0005(4) 0.0009(3) Cd1z1 -0.0207(4) 0.001(6) Cd2x1 -0.0035(17) -0.0055(11) Cd2y1 -0.0002(3) 0.0007(3) Cd2z1 -0.009(6) -0.021(2) Cd5x1 0.021(2) 0.007(6) Cd5y1 -0.0065(8) -0.0026(19) Cd5z1 0.0009(3) -0.0005(4) Cd6x1 0.015(4) 0.016(4) Cd6y1 0.0057(16) 0.0056(16) Cd6z1 -0.0003(4) 0.0010(3) Cd7x1 0 0 Cd7y1 0.0136(16) 0.006(4) Cd7z1 0 0 Cd8x1 0 0 Cd8y1 -0.012(3) -0.011(3) Cd8z1 0 0 P1x1 0.0037(9) 0.0023(14) P1y1 -0.0007(8) 0.0006(6) P1z1 0.0100(18) 0.006(3) P3x1 -0.0019(4) -0.0007(6) P3y1 0.0024(4) 0.0003(7) P3z1 0.0013(8) -0.0027(4) Na1x1 0.0089(19) 0.001(4) Na1y1 -0.001(3) -0.0038(19) Na1z1 0.0022(13) -0.0011(19) Na2x1 0 0 Na2y1 0.0(9) 0.012(2) 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 Na1U111 Na1 U11 1 Na1U221 Na1 U22 1 Na1U331 Na1 U33 1 Na1U121 Na1 U12 1 Na1U131 Na1 U13 1 Na1U231 Na1 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Cd1U111 0.0012(10) 0.0017(11) Cd1U221 0.0036(8) 0.0000(12) Cd1U331 -0.0123(15) 0.001(4) Cd1U121 -0.0003(10) -0.0009(11) Cd1U131 -0.0050(13) 0.0031(18) Cd1U231 -0.0005(15) -0.0025(15) Cd2U111 0.0000(12) 0.0020(9) Cd2U221 0.0019(16) 0.0048(10) Cd2U331 -0.014(9) -0.031(4) Cd2U121 -0.0002(11) -0.0003(9) Cd2U131 -0.0040(19) -0.0057(14) Cd2U231 -0.0030(15) 0.0001(15) Cd5U111 0.0103(12) 0.001(3) Cd5U221 -0.007(2) -0.006(2) Cd5U331 0.0006(6) -0.0005(6) Cd5U121 0.002(2) 0.0077(12) Cd5U131 -0.0013(9) -0.0016(6) Cd5U231 0.0005(17) 0.0045(10) Cd7U111 0 0 Cd7U221 0 0 Cd7U331 0 0 Cd7U121 -0.0156(15) 0.001(4) Cd7U131 0 0 Cd7U231 -0.0038(13) 0.0003(17) Na1U111 0.000(6) -0.004(5) Na1U221 0.003(6) 0.003(5) Na1U331 -0.004(5) -0.001(5) Na1U121 -0.002(6) -0.001(6) Na1U131 -0.001(5) -0.008(3) Na1U231 -0.001(6) 0.014(6) #======================================================================= # 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 P3 . . 2.527(11) 2.517(14) 2.540(14) ? Cd1 P3 . 4_5555 2.548(18) 2.54(3) 2.56(3) ? Cd1 P5 . . 2.521(9) 2.485(11) 2.567(11) ? Cd1 Na1 . 1_5545 3.30(4) 3.17(6) 3.44(6) ? Cd1 Na1 . 4_4545 3.36(3) 3.26(4) 3.45(4) ? Cd1 Na2 . 1_5545 3(4) 3(8) 3(8) ? Cd2 P4 . . 2.55(2) 2.49(3) 2.62(3) ? Cd2 P4 . 4_5555 2.563(11) 2.522(14) 2.614(14) ? Cd2 P6 . . 2.571(10) 2.522(13) 2.630(13) ? Cd2 Na1 . . 3.48(5) 3.36(6) 3.60(6) ? Cd2 Na1 . 4_5555 3.40(3) 3.23(4) 3.58(4) ? Cd2 Na2 . . 3(4) 3(7) 4(7) ? Cd3 P3 . 3_5455 2.565(9) 2.544(11) 2.586(11) ? Cd3 P3 . 4_5555 2.565(9) 2.544(11) 2.586(11) ? Cd3 P5 . 1_6555 2.573(13) 2.573(13) 2.573(13) ? Cd3 Na1 . 3_5445 3.43(3) 3.38(3) 3.47(3) ? Cd3 Na1 . 4_5545 3.43(3) 3.38(3) 3.47(3) ? Cd3 Na2 . 1_5545 3.41(13) 3.4(3) 3.4(3) ? Cd4 P4 . 1_6555 2.552(7) 2.552(7) 2.552(7) ? Cd4 P4 . 2_6555 2.552(7) 2.552(7) 2.552(7) ? Cd4 P6 . . 2.527(13) 2.527(13) 2.527(13) ? Cd4 Na1 . 3_5455 3.31(3) 3.29(3) 3.33(3) ? Cd4 Na1 . 4_5555 3.31(3) 3.29(3) 3.33(3) ? Cd4 Na2 . 1_6555 3.35(13) 3.3(3) 3.3(3) ? Cd5 P1 . . 2.69(2) 2.60(3) 2.79(3) ? Cd5 P1 . 4_4555 2.70(3) 2.60(5) 2.80(5) ? Cd5 P3 . . 2.534(10) 2.508(12) 2.556(12) ? Cd6 P1 . . 2.80(3) 2.70(3) 2.91(3) ? Cd6 P1 . 4_5555 2.80(4) 2.71(4) 2.90(4) ? Cd6 P2 . 3_4555 2.71(2) 2.70(2) 2.72(2) ? Cd6 P4 . 4_5555 2.627(9) 2.614(9) 2.639(9) ? Cd7 P1 . . 2.69(3) 2.59(4) 2.80(4) ? Cd7 P1 . 2_5555 2.69(3) 2.59(4) 2.80(4) ? Cd7 P5 . . 2.534(12) 2.531(12) 2.538(12) ? Cd8 P1 . . 2.80(4) 2.70(4) 2.91(4) ? Cd8 P1 . 2_5555 2.80(4) 2.70(4) 2.91(4) ? Cd8 P2 . . 2.705(9) 2.701(9) 2.709(9) ? Cd8 P6 . . 2.607(14) 2.603(14) 2.611(14) ? P3 Na1 . 1_5545 3.03(3) 2.98(3) 3.08(3) ? P3 Na1 . 4_4545 3.13(3) 3.07(3) 3.20(3) ? P3 Na2 . 3_4545 3(4) 3(8) 3(8) ? P4 Na1 . . 3.04(3) 2.99(3) 3.09(3) ? P4 Na1 . 4_4555 3.15(3) 3.11(3) 3.19(3) ? P4 Na2 . . 3(4) 3(8) 3(8) ? P5 Na1 . 3_4445 3.11(3) 3.06(3) 3.16(3) ? P5 Na1 . 4_4545 3.11(3) 3.06(3) 3.16(3) ? P5 Na2 . 1_5545 3.15(14) 3.1(3) 3.2(3) ? P6 Na1 . 3_5455 3.07(3) 3.01(3) 3.12(3) ? P6 Na1 . 4_5555 3.07(3) 3.01(3) 3.12(3) ? P6 Na2 . . 3.05(14) 3.0(3) 3.0(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 P3 Cd1 P3 . . 4_5555 117.2(7) 115.5(4) 118.2(5) ? P3 Cd1 P5 . . . 118.2(5) 115.2(3) 120.5(3) ? P3 Cd1 Na1 . . 1_5545 61.0(8) 57.6(6) 64.1(7) ? P3 Cd1 Na1 . . 4_4545 62.5(7) 59.6(6) 65.3(7) ? P3 Cd1 Na2 . . 1_5545 131.9(13) 122.0(5) 141.7(5) ? P3 Cd1 P5 4_5555 . . 118.1(7) 114.7(4) 120.8(4) ? P3 Cd1 Na1 4_5555 . 1_5545 63.3(8) 62.0(6) 64.5(8) ? P3 Cd1 Na1 4_5555 . 4_4545 132.3(14) 124.4(6) 140.2(6) ? P3 Cd1 Na2 4_5555 . 1_5545 61.3(7) 57.7(4) 64.8(4) ? P5 Cd1 Na1 . . 1_5545 131.4(13) 122.4(6) 140.4(6) ? P5 Cd1 Na1 . . 4_4545 62.1(7) 59.0(6) 65.1(7) ? P5 Cd1 Na2 . . 1_5545 63.3(7) 61.4(5) 65.1(6) ? Na1 Cd1 Na1 1_5545 . 4_4545 81.8(9) 76.2(6) 87.4(7) ? Na1 Cd1 Na2 1_5545 . 1_5545 82.2(11) 75.6(8) 88.7(8) ? Na1 Cd1 Na2 4_4545 . 1_5545 83.6(9) 78.5(6) 88.6(6) ? P4 Cd2 P4 . . 4_5555 115.2(9) 111.1(8) 118.6(6) ? P4 Cd2 P6 . . . 115.5(9) 111.2(8) 119.3(6) ? P4 Cd2 Na1 . . . 58.2(9) 54.8(7) 61.7(7) ? P4 Cd2 Na1 . . 4_5555 123.0(17) 114.5(12) 131.9(14) ? P4 Cd2 Na2 . . . 60.9(8) 56.6(6) 65.1(6) ? P4 Cd2 P6 4_5555 . . 114.4(6) 110.8(6) 117.6(5) ? P4 Cd2 Na1 4_5555 . . 60.8(8) 58.0(8) 63.4(8) ? P4 Cd2 Na1 4_5555 . 4_5555 59.4(8) 57.3(7) 61.4(7) ? P4 Cd2 Na2 4_5555 . . 123.3(15) 113.7(11) 133.3(12) ? P6 Cd2 Na1 . . . 125.1(16) 116.5(12) 134.0(13) ? P6 Cd2 Na1 . . 4_5555 59.9(8) 56.2(7) 63.7(7) ? P6 Cd2 Na2 . . . 59.0(7) 57.4(7) 60.6(7) ? Na1 Cd2 Na1 . . 4_5555 78.5(10) 74.1(10) 83.1(11) ? Na1 Cd2 Na2 . . . 78.3(12) 71.3(9) 85.5(10) ? Na1 Cd2 Na2 4_5555 . . 76.2(10) 70.7(8) 82.0(9) ? P3 Cd3 P3 3_5455 . 4_5555 115.7(3) 115.7(3) 115.7(3) ? P3 Cd3 P5 3_5455 . 1_6555 114.9(2) 114.1(2) 115.6(2) ? P3 Cd3 Na1 3_5455 . 3_5445 58.6(6) 57.2(6) 60.1(6) ? P3 Cd3 Na1 3_5455 . 4_5545 122.9(5) 121.5(5) 124.3(5) ? P3 Cd3 Na2 3_5455 . 1_5545 59.9(5) 57.5(5) 62.4(5) ? P3 Cd3 P5 4_5555 . 1_6555 114.9(2) 114.1(2) 115.6(2) ? P3 Cd3 Na1 4_5555 . 3_5445 122.9(5) 121.5(5) 124.3(5) ? P3 Cd3 Na1 4_5555 . 4_5545 58.6(6) 57.2(6) 60.1(6) ? P3 Cd3 Na2 4_5555 . 1_5545 60.0(5) 57.5(5) 62.4(5) ? P5 Cd3 Na1 1_6555 . 3_5445 60.5(6) 59.5(6) 61.5(6) ? P5 Cd3 Na1 1_6555 . 4_5545 60.5(6) 59.5(6) 61.5(6) ? P5 Cd3 Na2 1_6555 . 1_5545 122.5(4) 122.5(4) 122.5(4) ? Na1 Cd3 Na1 3_5445 . 4_5545 77.9(8) 77.8(8) 77.9(8) ? Na1 Cd3 Na2 3_5445 . 1_5545 76.0(5) 73.9(6) 78.0(6) ? Na1 Cd3 Na2 4_5545 . 1_5545 76.0(5) 73.9(6) 78.0(6) ? P4 Cd4 P4 1_6555 . 2_6555 118.1(3) 118.1(3) 118.1(3) ? P4 Cd4 P6 1_6555 . . 118.5(2) 118.5(2) 118.5(2) ? P4 Cd4 Na1 1_6555 . 3_5455 132.0(5) 131.2(5) 132.9(5) ? P4 Cd4 Na1 1_6555 . 4_5555 63.5(6) 62.4(6) 64.6(6) ? P4 Cd4 Na2 1_6555 . 1_6555 62.1(5) 59.5(5) 64.8(5) ? P4 Cd4 P6 2_6555 . . 118.5(2) 118.5(2) 118.5(2) ? P4 Cd4 Na1 2_6555 . 3_5455 63.5(6) 62.4(6) 64.6(6) ? P4 Cd4 Na1 2_6555 . 4_5555 132.0(5) 131.2(5) 132.9(5) ? P4 Cd4 Na2 2_6555 . 1_6555 62.2(5) 59.5(5) 64.8(5) ? P6 Cd4 Na1 . . 3_5455 61.6(6) 60.4(6) 62.8(6) ? P6 Cd4 Na1 . . 4_5555 61.6(6) 60.4(6) 62.8(6) ? P6 Cd4 Na2 . . 1_6555 133.2(4) 133.2(4) 133.3(4) ? Na1 Cd4 Na1 3_5455 . 4_5555 81.1(8) 81.1(8) 81.2(8) ? Na1 Cd4 Na2 3_5455 . 1_6555 84.0(5) 81.5(5) 86.4(5) ? Na1 Cd4 Na2 4_5555 . 1_6555 83.9(5) 81.5(5) 86.4(5) ? P1 Cd5 P1 . . 4_4555 107.3(8) 107.1(6) 107.5(9) ? P1 Cd5 P3 . . . 115.5(9) 107.0(7) 123.9(8) ? P1 Cd5 P3 4_4555 . . 115.9(11) 107.5(7) 124.5(7) ? P1 Cd6 P1 . . 4_5555 101.6(8) 101.0(8) 102.0(9) ? P1 Cd6 P2 . . 3_4555 104.0(8) 101.4(8) 106.4(8) ? P1 Cd6 P4 . . 4_5555 112.3(9) 105.1(9) 119.7(9) ? P1 Cd6 P2 4_5555 . 3_4555 103.6(7) 100.9(7) 106.1(7) ? P1 Cd6 P4 4_5555 . 4_5555 112.2(11) 104.9(10) 119.3(11) ? P2 Cd6 P4 3_4555 . 4_5555 120.4(8) 119.7(8) 120.9(8) ? P1 Cd7 P1 . . 2_5555 107.3(5) 107.1(5) 107.4(5) ? P1 Cd7 P5 . . . 115.8(12) 107.8(9) 123.7(9) ? P1 Cd7 P5 2_5555 . . 115.7(12) 107.8(9) 123.7(9) ? P1 Cd8 P1 . . 2_5555 101.5(5) 101.4(5) 101.7(4) ? P1 Cd8 P2 . . . 104.4(10) 101.4(10) 107.1(9) ? P1 Cd8 P6 . . . 112.1(12) 104.6(11) 119.7(12) ? P1 Cd8 P2 2_5555 . . 104.5(10) 101.4(10) 107.1(9) ? P1 Cd8 P6 2_5555 . . 112.2(12) 104.6(11) 119.7(12) ? P2 Cd8 P6 . . . 119.6(4) 119.3(4) 119.9(3) ? Cd5 P1 Cd5 . . 4_5555 103.7(10) 98.7(9) 108.5(8) ? Cd5 P1 Cd6 . . . 75.6(7) 75.1(8) 76.4(8) ? Cd5 P1 Cd6 . . 4_4555 75.5(7) 75.1(7) 76.0(6) ? Cd5 P1 Cd7 . . . 103.9(9) 99.1(9) 108.4(8) ? Cd5 P1 Cd8 . . . 175.0(11) 171.4(10) 179.5(10) ? Cd5 P1 Cd6 4_5555 . . 75.5(7) 75.1(8) 75.7(7) ? Cd5 P1 Cd6 4_5555 . 4_4555 174.7(10) 171.3(9) 179.5(8) ? Cd5 P1 Cd7 4_5555 . . 103.7(8) 99.0(8) 108.2(7) ? Cd5 P1 Cd8 4_5555 . . 75.4(5) 74.6(4) 76.0(5) ? Cd6 P1 Cd6 . . 4_4555 104.6(10) 100.3(10) 108.4(9) ? Cd6 P1 Cd7 . . . 175.0(12) 171.5(11) 179.9(12) ? Cd6 P1 Cd8 . . . 104.7(9) 99.8(9) 109.1(8) ? Cd6 P1 Cd7 4_4555 . . 75.8(5) 75.3(5) 76.3(5) ? Cd6 P1 Cd8 4_4555 . . 105.0(8) 100.4(8) 109.3(8) ? Cd7 P1 Cd8 . . . 75.5(8) 75.0(9) 75.9(8) ? Cd6 P2 Cd6 3_5455 . 4_5555 100.5(7) 100.4(7) 100.5(7) ? Cd6 P2 Cd8 3_5455 . . 100.2(9) 99.7(9) 100.7(9) ? Cd6 P2 Cd8 4_5555 . . 100.2(9) 99.7(9) 100.7(9) ? Cd1 P3 Cd1 . . 4_4555 118.2(6) 117.6(4) 119.1(5) ? Cd1 P3 Cd3 . . 3_4555 117.5(4) 115.9(3) 118.8(3) ? Cd1 P3 Cd5 . . . 81.2(11) 79.8(9) 82.4(9) ? Cd1 P3 Na1 . . 1_5545 72.2(10) 68.0(7) 76.7(7) ? Cd1 P3 Na1 . . 4_4545 71.8(8) 68.5(6) 75.3(6) ? Cd1 P3 Na2 . . 3_4545 151.4(10) 143.9(6) 158.9(6) ? Cd1 P3 Cd3 4_4555 . 3_4555 116.4(5) 116.1(6) 116.7(6) ? Cd1 P3 Cd5 4_4555 . . 80.7(13) 80.1(11) 81.3(11) ? Cd1 P3 Na1 4_4555 . 1_5545 150.8(10) 145.0(6) 156.5(6) ? Cd1 P3 Na1 4_4555 . 4_4545 70.2(8) 67.8(6) 72.6(6) ? Cd1 P3 Na2 4_4555 . 3_4545 72.1(6) 68.5(4) 75.8(4) ? Cd3 P3 Cd5 3_4555 . . 79.8(7) 79.0(7) 80.5(7) ? Cd3 P3 Na1 3_4555 . 1_5545 75.1(7) 73.9(7) 76.3(7) ? Cd3 P3 Na1 3_4555 . 4_4545 157.4(6) 155.5(6) 159.2(6) ? Cd3 P3 Na2 3_4555 . 3_4545 73.9(5) 71.6(4) 76.1(5) ? Cd5 P3 Na1 . . 1_5545 128.4(9) 123.3(7) 133.6(7) ? Cd5 P3 Na1 . . 4_4545 122.7(8) 121.5(9) 124.1(9) ? Cd5 P3 Na2 . . 3_4545 127.4(7) 121.2(5) 133.7(6) ? Na1 P3 Na1 1_5545 . 4_4545 89.8(8) 88.8(9) 90.7(8) ? Na1 P3 Na2 1_5545 . 3_4545 87.2(7) 85.4(7) 88.9(7) ? Na1 P3 Na2 4_4545 . 3_4545 89.0(7) 85.5(7) 92.4(7) ? Cd2 P4 Cd2 . . 4_4555 116.4(6) 115.9(6) 116.7(5) ? Cd2 P4 Cd4 . . 1_4555 116.6(4) 115.3(4) 117.8(4) ? Cd2 P4 Cd6 . . 4_4555 78.7(12) 77.0(9) 80.6(10) ? Cd2 P4 Na1 . . . 76.4(9) 73.1(7) 79.6(7) ? Cd2 P4 Na1 . . 4_4555 158.1(11) 152.9(10) 163.2(9) ? Cd2 P4 Na2 . . . 73.6(7) 70.4(6) 76.8(6) ? Cd2 P4 Cd4 4_4555 . 1_4555 116.1(4) 114.7(3) 117.5(3) ? Cd2 P4 Cd6 4_4555 . 4_4555 78.5(11) 76.9(9) 80.2(9) ? Cd2 P4 Na1 4_4555 . . 74.1(8) 71.0(7) 77.3(7) ? Cd2 P4 Na1 4_4555 . 4_4555 74.1(11) 71.3(9) 77.0(9) ? Cd2 P4 Na2 4_4555 . . 157.5(11) 150.7(8) 164.3(8) ? Cd4 P4 Cd6 1_4555 . 4_4555 79.4(6) 79.2(6) 79.6(6) ? Cd4 P4 Na1 1_4555 . . 151.4(6) 151.2(6) 151.6(6) ? Cd4 P4 Na1 1_4555 . 4_4555 70.1(7) 69.1(7) 71.0(7) ? Cd4 P4 Na2 1_4555 . . 71.6(4) 69.6(4) 73.5(5) ? Cd6 P4 Na1 4_4555 . . 129.1(8) 128.9(8) 129.3(8) ? Cd6 P4 Na1 4_4555 . 4_4555 123.0(9) 119.6(9) 126.5(9) ? Cd6 P4 Na2 4_4555 . . 124.0(7) 118.8(7) 129.2(7) ? Na1 P4 Na1 . . 4_4555 89.2(8) 87.4(7) 90.9(7) ? Na1 P4 Na2 . . . 89.8(7) 87.2(8) 92.4(7) ? Na1 P4 Na2 4_4555 . . 90.4(7) 89.5(7) 91.3(7) ? Cd1 P5 Cd1 . . 2_5555 118.5(6) 118.3(6) 118.6(6) ? Cd1 P5 Cd3 . . 1_4555 116.8(5) 115.1(3) 118.4(3) ? Cd1 P5 Cd7 . . . 80.9(13) 79.6(10) 82.3(10) ? Cd1 P5 Na1 . . 3_4445 152.1(11) 147.1(7) 157.1(7) ? Cd1 P5 Na1 . . 4_4545 72.3(8) 69.4(6) 75.1(6) ? Cd1 P5 Na2 . . 1_5545 71.1(9) 68.9(8) 73.2(8) ? Cd1 P5 Cd3 2_5555 . 1_4555 116.7(5) 115.1(3) 118.4(3) ? Cd1 P5 Cd7 2_5555 . . 80.9(13) 79.6(10) 82.3(10) ? Cd1 P5 Na1 2_5555 . 3_4445 72.3(8) 69.4(6) 75.1(6) ? Cd1 P5 Na1 2_5555 . 4_4545 152.2(11) 147.1(7) 157.1(7) ? Cd1 P5 Na2 2_5555 . 1_5545 71.1(9) 68.9(8) 73.2(8) ? Cd3 P5 Cd7 1_4555 . . 79.6(4) 79.6(4) 79.6(4) ? Cd3 P5 Na1 1_4555 . 3_4445 73.5(6) 72.5(6) 74.5(6) ? Cd3 P5 Na1 1_4555 . 4_4545 73.5(6) 72.5(6) 74.5(6) ? Cd3 P5 Na2 1_4555 . 1_5545 157.7(5) 157.6(5) 157.8(5) ? Cd7 P5 Na1 . . 3_4445 127.0(9) 123.2(7) 130.6(8) ? Cd7 P5 Na1 . . 4_4545 126.9(9) 123.2(7) 130.6(8) ? Cd7 P5 Na2 . . 1_5545 122.7(4) 122.6(4) 122.8(4) ? Na1 P5 Na1 3_4445 . 4_4545 87.6(9) 87.6(9) 87.7(9) ? Na1 P5 Na2 3_4445 . 1_5545 90.7(7) 88.6(7) 92.8(7) ? Na1 P5 Na2 4_4545 . 1_5545 90.7(7) 88.6(7) 92.8(7) ? Cd2 P6 Cd2 . . 2_5555 116.0(5) 115.8(5) 116.1(5) ? Cd2 P6 Cd4 . . . 117.4(6) 115.8(5) 118.9(4) ? Cd2 P6 Cd8 . . . 79.3(13) 78.0(11) 80.8(11) ? Cd2 P6 Na1 . . 3_5455 155.2(13) 149.0(11) 161.2(10) ? Cd2 P6 Na1 . . 4_5555 73.7(8) 69.4(7) 77.8(7) ? Cd2 P6 Na2 . . . 74.6(10) 73.2(10) 76.1(10) ? Cd2 P6 Cd4 2_5555 . . 117.4(6) 115.8(5) 118.9(4) ? Cd2 P6 Cd8 2_5555 . . 79.4(13) 78.0(11) 80.8(11) ? Cd2 P6 Na1 2_5555 . 3_5455 73.6(8) 69.4(7) 77.8(7) ? Cd2 P6 Na1 2_5555 . 4_5555 155.1(13) 149.0(11) 161.2(10) ? Cd2 P6 Na2 2_5555 . . 74.6(10) 73.2(10) 76.1(10) ? Cd4 P6 Cd8 . . . 80.5(4) 80.5(4) 80.5(4) ? Cd4 P6 Na1 . . 3_5455 71.9(6) 71.0(6) 72.8(7) ? Cd4 P6 Na1 . . 4_5555 71.9(6) 71.0(6) 72.8(7) ? Cd4 P6 Na2 . . . 149.9(5) 149.8(5) 149.9(5) ? Cd8 P6 Na1 . . 3_5455 125.4(10) 120.8(10) 130.1(10) ? Cd8 P6 Na1 . . 4_5555 125.5(10) 120.8(10) 130.1(10) ? Cd8 P6 Na2 . . . 129.6(5) 129.6(5) 129.7(5) ? Na1 P6 Na1 3_5455 . 4_5555 89.3(9) 89.2(9) 89.3(9) ? Na1 P6 Na2 3_5455 . . 87.1(7) 84.6(8) 89.5(8) ? Na1 P6 Na2 4_5555 . . 87.0(7) 84.6(8) 89.5(8) ? Cd1 Na1 Cd1 1_5565 . 4_5565 81.7(10) 80.7(10) 82.7(9) ? Cd1 Na1 Cd2 1_5565 . . 99.5(11) 94.1(11) 104.9(11) ? Cd1 Na1 Cd2 1_5565 . 4_4555 101.0(9) 97.5(8) 104.7(8) ? Cd1 Na1 Cd3 1_5565 . 3_4565 80.6(7) 78.1(5) 83.2(6) ? Cd1 Na1 Cd4 1_5565 . 3_4555 175.8(10) 173.7(6) 179.9(9) ? Cd1 Na1 P3 1_5565 . 1_5565 46.8(5) 45.7(4) 47.9(5) ? Cd1 Na1 P3 1_5565 . 4_5565 46.6(5) 45.2(5) 48.1(5) ? Cd1 Na1 P4 1_5565 . . 77.1(10) 73.1(8) 81.0(9) ? Cd1 Na1 P4 1_5565 . 4_5555 131.4(12) 129.3(12) 133.7(12) ? Cd1 Na1 P5 1_5565 . 3_5565 103.4(7) 99.6(5) 107.4(6) ? Cd1 Na1 P6 1_5565 . 3_4555 135.9(9) 133.1(7) 138.6(7) ? Cd1 Na1 Cd2 4_5565 . . 98.4(9) 94.3(9) 102.5(9) ? Cd1 Na1 Cd2 4_5565 . 4_4555 175.6(11) 171.5(11) 179.7(11) ? Cd1 Na1 Cd3 4_5565 . 3_4565 79.5(7) 78.2(5) 80.8(5) ? Cd1 Na1 Cd4 4_5565 . 3_4555 96.3(9) 92.7(7) 99.9(7) ? Cd1 Na1 P3 4_5565 . 1_5565 103.1(8) 101.0(6) 105.3(6) ? Cd1 Na1 P3 4_5565 . 4_5565 45.6(4) 44.9(4) 46.5(4) ? Cd1 Na1 P4 4_5565 . . 132.2(12) 129.7(12) 134.6(12) ? Cd1 Na1 P4 4_5565 . 4_5555 74.7(8) 70.6(4) 78.9(5) ? Cd1 Na1 P5 4_5565 . 3_5565 45.6(4) 45.4(4) 45.9(3) ? Cd1 Na1 P6 4_5565 . 3_4555 132.9(12) 130.4(12) 135.3(12) ? Cd2 Na1 Cd2 . . 4_4555 78.3(7) 77.3(6) 79.4(7) ? Cd2 Na1 Cd3 . . 3_4565 176.5(10) 174.3(10) 180.0(5) ? Cd2 Na1 Cd4 . . 3_4555 79.4(7) 77.5(6) 81.5(7) ? Cd2 Na1 P3 . . 1_5565 135.0(12) 133.1(12) 136.9(12) ? Cd2 Na1 P3 . . 4_5565 78.4(9) 73.7(9) 82.9(9) ? Cd2 Na1 P4 . . . 45.4(5) 45.2(5) 45.6(5) ? Cd2 Na1 P4 . . 4_5555 45.1(5) 44.5(4) 45.6(5) ? Cd2 Na1 P5 . . 3_5565 132.0(9) 129.9(8) 134.1(8) ? Cd2 Na1 P6 . . 3_4555 100.3(8) 97.7(8) 103.1(8) ? Cd2 Na1 Cd3 4_4555 . 3_4565 103.9(10) 100.2(10) 107.5(10) ? Cd2 Na1 Cd4 4_4555 . 3_4555 80.9(7) 78.8(6) 83.0(7) ? Cd2 Na1 P3 4_4555 . 1_5565 80.9(9) 76.8(10) 85.0(9) ? Cd2 Na1 P3 4_4555 . 4_5565 134.8(12) 133.6(11) 135.8(12) ? Cd2 Na1 P4 4_4555 . . 46.5(4) 45.2(3) 47.8(4) ? Cd2 Na1 P4 4_4555 . 4_5555 101.2(9) 97.8(7) 104.7(8) ? Cd2 Na1 P5 4_4555 . 3_5565 135.5(12) 133.0(12) 137.9(12) ? Cd2 Na1 P6 4_4555 . 3_4555 46.4(4) 45.6(3) 47.2(4) ? Cd3 Na1 Cd4 3_4565 . 3_4555 100.3(10) 99.1(9) 101.7(10) ? Cd3 Na1 P3 3_4565 . 1_5565 46.3(4) 45.6(4) 47.0(4) ? Cd3 Na1 P3 3_4565 . 4_5565 100.3(6) 99.3(6) 101.3(6) ? Cd3 Na1 P4 3_4565 . . 136.6(9) 134.7(7) 138.4(7) ? Cd3 Na1 P4 3_4565 . 4_5555 133.4(11) 131.9(11) 135.0(11) ? Cd3 Na1 P5 3_4565 . 3_5565 46.0(5) 45.4(5) 46.6(5) ? Cd3 Na1 P6 3_4565 . 3_4555 80.9(9) 79.6(8) 82.3(9) ? Cd4 Na1 P3 3_4555 . 1_5565 135.3(12) 132.9(12) 137.8(12) ? Cd4 Na1 P3 3_4555 . 4_5565 131.0(9) 129.3(7) 132.7(7) ? Cd4 Na1 P4 3_4555 . . 103.5(6) 102.7(6) 104.2(6) ? Cd4 Na1 P4 3_4555 . 4_5555 46.4(4) 46.1(4) 46.7(4) ? Cd4 Na1 P5 3_4555 . 3_5565 75.9(8) 75.0(8) 76.8(8) ? Cd4 Na1 P6 3_4555 . 3_4555 46.5(5) 46.0(5) 46.9(5) ? P3 Na1 P3 1_5565 . 4_5565 89.3(8) 88.2(7) 90.3(7) ? P3 Na1 P4 1_5565 . . 92.6(8) 91.5(7) 93.6(8) ? P3 Na1 P4 1_5565 . 4_5555 177.3(11) 175.1(10) 179.9(7) ? P3 Na1 P5 1_5565 . 3_5565 89.7(8) 89.1(8) 90.3(8) ? P3 Na1 P6 1_5565 . 3_4555 93.1(9) 90.8(8) 95.5(8) ? P3 Na1 P4 4_5565 . . 90.7(11) 89.0(10) 92.4(10) ? P3 Na1 P4 4_5565 . 4_5555 88.5(8) 86.8(8) 90.3(8) ? P3 Na1 P5 4_5565 . 3_5565 87.8(6) 86.8(5) 88.8(5) ? P3 Na1 P6 4_5565 . 3_4555 177.1(10) 176.1(10) 178.8(9) ? P4 Na1 P4 . . 4_5555 88.3(7) 87.3(8) 89.2(8) ? P4 Na1 P5 . . 3_5565 177.1(11) 174.9(11) 179.1(9) ? P4 Na1 P6 . . 3_4555 89.9(6) 88.5(5) 91.3(5) ? P4 Na1 P5 4_5555 . 3_5565 89.4(8) 88.1(7) 90.8(8) ? P4 Na1 P6 4_5555 . 3_4555 89.1(8) 88.8(8) 89.4(8) ? P5 Na1 P6 3_5565 . 3_4555 91.5(11) 90.2(10) 92.8(10) ? Cd1 Na2 Cd1 1_5565 . 2_5565 81(3) 81(2) 81(7) ? Cd1 Na2 Cd2 1_5565 . . 100(150) 90(60) 110(60) ? Cd1 Na2 Cd2 1_5565 . 2_5555 170(90) 170(60) 180(110) ? Cd1 Na2 Cd3 1_5565 . 1_5565 80(50) 80(100) 80(110) ? Cd1 Na2 Cd4 1_5565 . 1_4555 100(70) 90(70) 100(60) ? Cd1 Na2 P3 1_5565 . 3_5465 103(6) 101(19) 106(10) ? Cd1 Na2 P3 1_5565 . 4_5565 50(60) 46(19) 50(40) ? Cd1 Na2 P4 1_5565 . . 80(110) 70(90) 80(80) ? Cd1 Na2 P4 1_5565 . 2_5555 131(12) 130(8) 130(30) ? Cd1 Na2 P5 1_5565 . 1_5565 50(30) 45(8) 46(7) ? Cd1 Na2 P6 1_5565 . . 140(160) 130(70) 140(40) ? Cd1 Na2 Cd2 2_5565 . . 170(90) 170(60) 180(110) ? Cd1 Na2 Cd2 2_5565 . 2_5555 100(150) 90(60) 110(60) ? Cd1 Na2 Cd3 2_5565 . 1_5565 80(50) 80(100) 80(110) ? Cd1 Na2 Cd4 2_5565 . 1_4555 100(70) 90(70) 100(60) ? Cd1 Na2 P3 2_5565 . 3_5465 50(60) 46(19) 50(40) ? Cd1 Na2 P3 2_5565 . 4_5565 103(6) 101(19) 106(10) ? Cd1 Na2 P4 2_5565 . . 131(12) 130(8) 130(30) ? Cd1 Na2 P4 2_5565 . 2_5555 80(110) 70(90) 80(80) ? Cd1 Na2 P5 2_5565 . 1_5565 50(30) 45(8) 46(7) ? Cd1 Na2 P6 2_5565 . . 130(160) 130(70) 140(40) ? Cd2 Na2 Cd2 . . 2_5555 79(3) 79(4) 79.1(6) ? Cd2 Na2 Cd3 . . 1_5565 100(80) 99(4) 108(4) ? Cd2 Na2 Cd4 . . 1_4555 80(50) 79(15) 80(40) ? Cd2 Na2 P3 . . 3_5465 136(16) 136(15) 140(20) ? Cd2 Na2 P3 . . 4_5565 80(110) 73(10) 87(12) ? Cd2 Na2 P4 . . . 50(60) 40(20) 50(20) ? Cd2 Na2 P4 . . 2_5555 101(5) 98.1(5) 103.9(6) ? Cd2 Na2 P5 . . 1_5565 130(150) 130(20) 140(20) ? Cd2 Na2 P6 . . . 50(40) 50(50) 47(17) ? Cd2 Na2 Cd3 2_5555 . 1_5565 100(80) 99(4) 108(4) ? Cd2 Na2 Cd4 2_5555 . 1_4555 80(50) 79(15) 80(40) ? Cd2 Na2 P3 2_5555 . 3_5465 80(110) 73(10) 87(12) ? Cd2 Na2 P3 2_5555 . 4_5565 136(16) 136(15) 140(20) ? Cd2 Na2 P4 2_5555 . . 101(5) 98.1(5) 103.9(6) ? Cd2 Na2 P4 2_5555 . 2_5555 50(60) 40(20) 50(20) ? Cd2 Na2 P5 2_5555 . 1_5565 130(150) 130(20) 140(20) ? Cd2 Na2 P6 2_5555 . . 50(40) 50(50) 47(17) ? Cd3 Na2 Cd4 1_5565 . 1_4555 170(80) 170(20) 175(11) ? Cd3 Na2 P3 1_5565 . 3_5465 50(20) 45.9(3) 47(6) ? Cd3 Na2 P3 1_5565 . 4_5565 50(20) 45.9(3) 47(6) ? Cd3 Na2 P4 1_5565 . . 130(170) 130(30) 140(30) ? Cd3 Na2 P4 1_5565 . 2_5555 130(170) 130(30) 140(30) ? Cd3 Na2 P5 1_5565 . 1_5565 100(5) 100.1(19) 100.3(7) ? Cd3 Na2 P6 1_5565 . . 81(4) 81.4(14) 81.6(6) ? Cd4 Na2 P3 1_4555 . 3_5465 130(160) 130(40) 140(40) ? Cd4 Na2 P3 1_4555 . 4_5565 130(160) 130(40) 140(40) ? Cd4 Na2 P4 1_4555 . . 50(20) 46(5) 47(3) ? Cd4 Na2 P4 1_4555 . 2_5555 50(20) 46(5) 47(3) ? Cd4 Na2 P5 1_4555 . 1_5565 75(4) 74.9(13) 75.0(5) ? Cd4 Na2 P6 1_4555 . . 103(6) 103(2) 103.2(8) ? P3 Na2 P3 3_5465 . 4_5565 90(6) 90(5) 90.0(4) ? P3 Na2 P4 3_5465 . . 180(100) 170(30) 178(18) ? P3 Na2 P4 3_5465 . 2_5555 90(150) 90(30) 100(40) ? P3 Na2 P5 3_5465 . 1_5565 90(70) 87(8) 90(3) ? P3 Na2 P6 3_5465 . . 90(80) 90(20) 95(17) ? P3 Na2 P4 4_5565 . . 90(150) 90(30) 100(40) ? P3 Na2 P4 4_5565 . 2_5555 180(100) 170(30) 178(18) ? P3 Na2 P5 4_5565 . 1_5565 90(70) 87(8) 90(3) ? P3 Na2 P6 4_5565 . . 90(80) 90(20) 95(17) ? P4 Na2 P4 . . 2_5555 89(5) 89.0(17) 89.2(6) ? P4 Na2 P5 . . 1_5565 90(70) 87(12) 91(10) ? P4 Na2 P6 . . . 90(70) 87(13) 91(11) ? P4 Na2 P5 2_5555 . 1_5565 90(70) 87(12) 91(10) ? P4 Na2 P6 2_5555 . . 90(70) 87(13) 91(11) ? P5 Na2 P6 1_5565 . . 180(150) 170(30) 180(30) ? #======================================================================= # 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 54331.0 53676.0 819.0 o -2 0 0 0 54349.0 53202.0 801.0 o 4 0 0 0 482.0 535.0 404.0 < -4 0 0 0 495.0 546.0 330.0 < 6 0 0 0 26298.0 25201.0 675.0 o -6 0 0 0 26305.0 26143.0 523.0 o 8 0 0 0 556.0 765.0 488.0 < 10 0 0 0 57866.0 51856.0 2431.0 o -10 0 0 0 57885.0 56284.0 891.0 o 1 1 0 -1 0.0 -11.0 359.0 < -1 1 0 1 0.0 -9.0 269.0 < 1 1 0 0 102.0 25.0 485.0 < -1 1 0 0 103.0 -16.0 429.0 < 1 1 0 1 175.0 131.0 275.0 < -1 1 0 -1 176.0 97.0 303.0 < 3 1 0 -1 1636.0 1658.0 287.0 o -3 1 0 1 1636.0 1561.0 203.0 o 3 1 0 0 863.0 355.0 339.0 < -3 1 0 0 863.0 1136.0 298.0 o 3 1 0 1 20.0 65.0 257.0 < -3 1 0 -1 20.0 -7.0 169.0 < 5 1 0 -1 4984.0 5368.0 436.0 o -5 1 0 1 4985.0 5770.0 513.0 o 5 1 0 0 10347.0 7900.0 2317.0 o -5 1 0 0 10349.0 9894.0 330.0 o 5 1 0 1 6559.0 6781.0 823.0 o -5 1 0 -1 6558.0 6465.0 513.0 o 7 1 0 -1 232.0 251.0 214.0 < -7 1 0 1 232.0 553.0 293.0 < 7 1 0 0 1379.0 707.0 524.0 < -7 1 0 0 1378.0 966.0 463.0 < 7 1 0 1 1899.0 2066.0 284.0 o -7 1 0 -1 1900.0 1883.0 309.0 o 9 1 0 -1 5.0 102.0 327.0 < -9 1 0 1 5.0 -411.0 341.0 < 9 1 0 0 25.0 -151.0 470.0 < -9 1 0 0 25.0 54.0 535.0 < 9 1 0 1 6.0 72.0 377.0 < -9 1 0 -1 6.0 151.0 375.0 < 0 2 0 0 3.0 -18.0 343.0 < 0 2 0 1 70.0 77.0 332.0 < 0 2 0 -1 70.0 70.0 273.0 < 2 2 0 -1 23.0 -5.0 217.0 < -2 2 0 1 23.0 54.0 233.0 < 2 2 0 0 213.0 27.0 330.0 < -2 2 0 0 213.0 65.0 409.0 < 2 2 0 1 898.0 874.0 235.0 o -2 2 0 -1 898.0 953.0 266.0 o 4 2 0 -1 310.0 321.0 366.0 < -4 2 0 1 309.0 278.0 221.0 < 4 2 0 0 201.0 214.0 499.0 < -4 2 0 0 201.0 117.0 312.0 < 4 2 0 1 160.0 90.0 291.0 < -4 2 0 -1 160.0 36.0 201.0 < 6 2 0 -1 533.0 517.0 271.0 < -6 2 0 1 533.0 330.0 230.0 < 6 2 0 0 247.0 372.0 343.0 < -6 2 0 0 246.0 813.0 332.0 < 6 2 0 1 18.0 23.0 262.0 < -6 2 0 -1 18.0 126.0 248.0 < 8 2 0 -1 2165.0 2366.0 429.0 o -8 2 0 1 2164.0 2177.0 305.0 o 8 2 0 0 1168.0 650.0 415.0 < -8 2 0 0 1168.0 2014.0 750.0 < 8 2 0 1 313.0 253.0 284.0 < -8 2 0 -1 314.0 409.0 490.0 < 1 3 0 -1 2.0 7.0 264.0 < -1 3 0 1 2.0 -41.0 242.0 < 1 3 0 0 92729.0 92758.0 1445.0 o -1 3 0 0 92735.0 94001.0 1557.0 o 1 3 0 1 7.0 5.0 327.0 < -1 3 0 -1 6.0 29.0 210.0 < 3 3 0 -1 9.0 117.0 205.0 < -3 3 0 1 9.0 50.0 214.0 < 3 3 0 0 17994.0 18115.0 401.0 o -3 3 0 0 17984.0 17413.0 517.0 o 3 3 0 1 3.0 -54.0 228.0 < -3 3 0 -1 3.0 -27.0 230.0 < 5 3 0 -1 22.0 18.0 271.0 < -5 3 0 1 22.0 -149.0 214.0 < 5 3 0 0 216351.0 213210.0 815.0 o -5 3 0 0 216274.0 213476.0 719.0 o 5 3 0 1 9.0 38.0 296.0 < -5 3 0 -1 9.0 77.0 230.0 < 7 3 0 -1 7.0 -50.0 248.0 < -7 3 0 1 7.0 280.0 334.0 < 7 3 0 0 744.0 756.0 334.0 < -7 3 0 0 742.0 1029.0 359.0 < 7 3 0 1 8.0 -138.0 255.0 < -7 3 0 -1 8.0 -29.0 248.0 < 9 3 0 -1 15.0 88.0 298.0 < -9 3 0 1 15.0 -79.0 415.0 < 9 3 0 0 28917.0 28924.0 541.0 o -9 3 0 0 28915.0 29845.0 758.0 o 9 3 0 1 4.0 -11.0 314.0 < -9 3 0 -1 4.0 -9.0 456.0 < 0 4 0 0 2.0 -63.0 341.0 < 0 4 0 1 23.0 52.0 199.0 < 0 4 0 -1 23.0 0.0 237.0 < 2 4 0 -1 2190.0 2419.0 260.0 o -2 4 0 1 2191.0 2216.0 237.0 o 2 4 0 0 1986.0 1421.0 585.0 < -2 4 0 0 1984.0 2017.0 262.0 o 2 4 0 1 2139.0 2130.0 239.0 o -2 4 0 -1 2141.0 2313.0 190.0 o 4 4 0 -1 578.0 643.0 201.0 o -4 4 0 1 578.0 560.0 192.0 < 4 4 0 0 1187.0 1088.0 327.0 o -4 4 0 0 1186.0 1323.0 318.0 o 4 4 0 1 853.0 1206.0 226.0 o -4 4 0 -1 852.0 1111.0 257.0 o 6 4 0 -1 195.0 93.0 235.0 < -6 4 0 1 195.0 126.0 230.0 < 6 4 0 0 463.0 619.0 348.0 < -6 4 0 0 462.0 467.0 307.0 < 6 4 0 1 697.0 506.0 246.0 < -6 4 0 -1 698.0 519.0 219.0 < 8 4 0 -1 1329.0 187.0 382.0 < -8 4 0 1 1329.0 750.0 607.0 < 8 4 0 0 285.0 379.0 508.0 < -8 4 0 0 284.0 163.0 501.0 < 8 4 0 1 126.0 14.0 339.0 < -8 4 0 -1 126.0 36.0 298.0 < 1 5 0 -1 3155.0 3134.0 413.0 o -1 5 0 1 3156.0 3263.0 258.0 o 1 5 0 0 2890.0 2939.0 436.0 o -1 5 0 0 2890.0 2971.0 267.0 o 1 5 0 1 1578.0 1861.0 307.0 o -1 5 0 -1 1579.0 1522.0 178.0 o 3 5 0 -1 2625.0 2525.0 355.0 o -3 5 0 1 2624.0 2850.0 215.0 o 3 5 0 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1 37.0 -27.0 226.0 < -4 6 0 -1 37.0 5.0 226.0 < 6 6 0 -1 28.0 -122.0 251.0 < -6 6 0 1 28.0 0.0 235.0 < 6 6 0 0 21630.0 21044.0 396.0 o -6 6 0 0 21633.0 21633.0 396.0 o 6 6 0 1 19.0 18.0 208.0 < -6 6 0 -1 19.0 -52.0 230.0 < 8 6 0 -1 11.0 345.0 359.0 < -8 6 0 1 12.0 -106.0 372.0 < 8 6 0 0 695.0 370.0 415.0 < -8 6 0 0 697.0 948.0 510.0 < 8 6 0 1 1.0 90.0 300.0 < -8 6 0 -1 1.0 -52.0 377.0 < 1 7 0 -1 2461.0 2823.0 271.0 o -1 7 0 1 2461.0 2351.0 208.0 o 1 7 0 0 3951.0 4166.0 404.0 o -1 7 0 0 3949.0 4207.0 282.0 o 1 7 0 1 2737.0 2421.0 291.0 o -1 7 0 -1 2739.0 3054.0 185.0 o 3 7 0 -1 93.0 23.0 233.0 < -3 7 0 1 93.0 61.0 178.0 < 3 7 0 0 70.0 -18.0 350.0 < -3 7 0 0 70.0 138.0 255.0 < 3 7 0 1 1028.0 896.0 253.0 o -3 7 0 -1 1027.0 1041.0 181.0 o 5 7 0 -1 2987.0 3446.0 309.0 o -5 7 0 1 2986.0 3647.0 361.0 o 5 7 0 0 5460.0 6158.0 359.0 o -5 7 0 0 5464.0 5871.0 436.0 o 5 7 0 1 2851.0 2730.0 486.0 o -5 7 0 -1 2851.0 2902.0 237.0 o 7 7 0 -1 663.0 768.0 300.0 < -7 7 0 1 664.0 682.0 433.0 < 7 7 0 0 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1273.0 316.0 o -2 10 0 -1 1569.0 1795.0 181.0 o 4 10 0 -1 1435.0 1590.0 330.0 o -4 10 0 1 1435.0 1097.0 253.0 o 4 10 0 0 2456.0 2579.0 429.0 o -4 10 0 0 2455.0 2109.0 298.0 o 4 10 0 1 1698.0 1608.0 305.0 o -4 10 0 -1 1696.0 1926.0 226.0 o 6 10 0 -1 844.0 433.0 377.0 < -6 10 0 1 845.0 630.0 321.0 < 6 10 0 0 1717.0 903.0 583.0 < -6 10 0 0 1714.0 1657.0 463.0 o 6 10 0 1 1263.0 1149.0 325.0 o -6 10 0 -1 1265.0 824.0 278.0 < 8 10 0 -1 482.0 183.0 756.0 < -8 10 0 1 482.0 -72.0 467.0 < 8 10 0 0 8.0 -106.0 704.0 < -8 10 0 0 8.0 72.0 616.0 < 8 10 0 1 255.0 59.0 643.0 < -8 10 0 -1 254.0 -84.0 413.0 < 1 11 0 -1 2808.0 2500.0 246.0 o -1 11 0 1 2809.0 3198.0 273.0 o 1 11 0 0 3176.0 3218.0 377.0 o -1 11 0 0 3177.0 3277.0 314.0 o 1 11 0 1 1557.0 2068.0 298.0 o -1 11 0 -1 1559.0 1626.0 233.0 o 3 11 0 -1 1166.0 1066.0 298.0 o -3 11 0 1 1165.0 1219.0 235.0 o 3 11 0 0 1818.0 1894.0 440.0 o -3 11 0 0 1816.0 1576.0 282.0 o 3 11 0 1 1700.0 2147.0 266.0 o -3 11 0 -1 1700.0 1332.0 203.0 o 5 11 0 -1 874.0 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