#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 23/03/2015' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section C' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section C' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; ? # name ; ; ? # footnote ; ; ? # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _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. # enable this reference if Diamond ver. 2 was used for visualization #Brandenburg, K. (1999). DIAMOND. Version. 2.1c. #Crystal Impact GbR, Bonn, Germany. # enable this reference if Diamond ver. 3 was used for visualization #Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. #Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. # enable this reference if SIR97 was used for solving of the structure #Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., #Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R. (1997). #SIR97. A Package for Crystal Structure Solution by Direct Methods #and Refinement, Bari, Rome, Italy. # use this reference if SIR2002 was used for solving of the structure #Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., #Polidori, G., Spagna, R. #SIR2002: the program, J. Appl. Cryst, (2003). 36, 1103 # use this reference if SIR2011 was used for solving of the structure #Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, #G.L., Giacovazzo, C., Mallamo. M., Mazzone, A., Polidori, G., Spagna, R. #SIR2011: a new package for crystal structure determination and refinement, #J.Appl.Cryst. (2012) 45, 357-361 # enable this reference if bond valences were calculated #Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # enable this reference if Xshape wase used for crystal shape refinement #Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. # enable this reference if Flack coefficient was refined #Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'K1.727 Na2.273 O8 S2' _chemical_formula_weight 311.9 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3 m 1' _symmetry_space_group_name_Hall '-P 3;-2"' _symmetry_Int_Tables_number 164 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 _cell_length_a 5.6014(3) _cell_length_b 5.6014(3) _cell_length_c 7.1507(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 194.30(2) 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 0.535(5) 1 0 0 0 1 0 0 0 1 2 0.465(5) -1 0 0 0 -1 0 0 0 1 _cell_formula_units_Z 1 _cell_measurement_reflns_used 2234 _cell_measurement_theta_min 4.1600 _cell_measurement_theta_max 31.4550 _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.6655 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 154 _exptl_absorpt_coefficient_mu 1.75 _exptl_crystal_description 'crystal chip' _exptl_crystal_size_max 0.6609 _exptl_crystal_size_mid 0.3567 _exptl_crystal_size_min 0.3501 _exptl_crystal_size_rad ? _exptl_crystal_colour 'yellow' _exptl_absorpt_correction_T_min 0.53148 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_probe 'x-ray' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Sapphire3' _diffrn_detector_area_resol_mean 16.0630 _diffrn_ambient_temperature 293 _diffrn_measurement_method ? _diffrn_measurement_specimen_support ? _diffrn_reflns_number 3814 _diffrn_reflns_theta_min 4.2 _diffrn_reflns_theta_max 31.49 _diffrn_reflns_theta_full 31.49 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_unetI/netI 0.0089 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _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 ? ? ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 274 _reflns_number_gt 272 _reflns_threshold_expression 'I>2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_gt 0.0842 _refine_ls_R_factor_all 0.0285 _refine_ls_wR_factor_ref 0.0844 _refine_ls_goodness_of_fit_ref 1.18 _refine_ls_goodness_of_fit_gt 1.18 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 274 _refine_ls_number_parameters 22 _refine_ls_number_restraints 0 _refine_ls_number_constraints 4 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0049000001I^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0480 _refine_ls_shift/su_mean 0.0145 _refine_diff_density_max 0.21 _refine_diff_density_min -0.23 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _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 K 0.2009 0.2494 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Na 0.0362 0.0249 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 '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_ _restr_distance_atom_site_label_1 _restr_distance_site_symmetry_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param ? ? ? ? ? ? loop_ _restr_angle_atom_site_label_1 _restr_angle_site_symmetry_1 _restr_angle_atom_site_label_2 _restr_angle_site_symmetry_2 _restr_angle_atom_site_label_3 _restr_angle_site_symmetry_3 _restr_angle_target _restr_angle_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_torsion_atom_site_label_1 _restr_torsion_site_symmetry_1 _restr_torsion_atom_site_label_2 _restr_torsion_site_symmetry_2 _restr_torsion_atom_site_label_3 _restr_torsion_site_symmetry_3 _restr_torsion_atom_site_label_4 _restr_torsion_site_symmetry_4 _restr_torsion_angle_target _restr_torsion_weight_param ? ? ? ? ? ? ? ? ? ? loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_site_symmetry_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param ? ? ? ? ? ? loop_ _restr_equal_angle_atom_site_label_1 _restr_equal_angle_site_symmetry_1 _restr_equal_angle_atom_site_label_2 _restr_equal_angle_site_symmetry_2 _restr_equal_angle_atom_site_label_3 _restr_equal_angle_site_symmetry_3 _restr_equal_angle_class_class_id _restr_equal_angle_class_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_equal_torsion_atom_site_label_1 _restr_equal_torsion_site_symmetry_1 _restr_equal_torsion_atom_site_label_2 _restr_equal_torsion_site_symmetry_2 _restr_equal_torsion_atom_site_label_3 _restr_equal_torsion_site_symmetry_3 _restr_equal_torsion_atom_site_label_4 _restr_equal_torsion_site_symmetry_4 _restr_equal_torsion_class_class_id _restr_equal_torsion_class_target_weight_param ? ? ? ? ? ? ? ? ? ? #======================================================================= # 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 _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0 0 0.5 Uani 0.0344(4) 1 1 d . . . Na1 Na 0 0 0 Uani 0.0181(5) 1 1 d . . . Na3 Na 0.666667 0.333333 -0.18900(19) Uani 0.0217(4) 2 0.637(12) d . . . S1 S 0.333333 0.666667 0.73541(12) Uani 0.0164(2) 2 1 d . . . O1 O 0.19098(18) 0.80902(18) 0.8006(6) Uani 0.0571(10) 6 1 d . . . O2 O 0.333333 0.666667 0.5319(7) Uani 0.0475(11) 2 1 d . . . Na3_k K 0.666667 0.333333 -0.18900(19) Uani 0.0217(4) 2 0.364(12) 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 K1 K 0.0438(4) 0.0438(4) 0.0157(7) 0.0219(2) 0 0 Na1 Na 0.0154(5) 0.0154(5) 0.0236(10) 0.0077(3) 0 0 Na3 Na 0.0209(5) 0.0209(5) 0.0232(7) 0.0104(2) 0 0 S1 S 0.0144(3) 0.0144(3) 0.0204(4) 0.00720(13) 0 0 O1 O 0.0670(11) 0.0670(11) 0.0642(14) 0.0537(12) 0.0120(5) -0.0120(5) O2 O 0.0614(15) 0.0614(15) 0.0199(18) 0.0307(7) 0 0 Na3_k K 0.0209(5) 0.0209(5) 0.0232(7) 0.0104(2) 0 0 loop_ _jana_atom_site_ADP_C_label _jana_atom_site_ADP_C_type_symbol _jana_atom_site_ADP_C_111 _jana_atom_site_ADP_C_112 _jana_atom_site_ADP_C_113 _jana_atom_site_ADP_C_122 _jana_atom_site_ADP_C_123 _jana_atom_site_ADP_C_133 _jana_atom_site_ADP_C_222 _jana_atom_site_ADP_C_223 _jana_atom_site_ADP_C_233 _jana_atom_site_ADP_C_333 ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_D_label _jana_atom_site_ADP_D_type_symbol _jana_atom_site_ADP_D_1111 _jana_atom_site_ADP_D_1112 _jana_atom_site_ADP_D_1113 _jana_atom_site_ADP_D_1122 _jana_atom_site_ADP_D_1123 _jana_atom_site_ADP_D_1133 _jana_atom_site_ADP_D_1222 _jana_atom_site_ADP_D_1223 _jana_atom_site_ADP_D_1233 _jana_atom_site_ADP_D_1333 _jana_atom_site_ADP_D_2222 _jana_atom_site_ADP_D_2223 _jana_atom_site_ADP_D_2233 _jana_atom_site_ADP_D_2333 _jana_atom_site_ADP_D_3333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_E_label _jana_atom_site_ADP_E_type_symbol _jana_atom_site_ADP_E_11111 _jana_atom_site_ADP_E_11112 _jana_atom_site_ADP_E_11113 _jana_atom_site_ADP_E_11122 _jana_atom_site_ADP_E_11123 _jana_atom_site_ADP_E_11133 _jana_atom_site_ADP_E_11222 _jana_atom_site_ADP_E_11223 _jana_atom_site_ADP_E_11233 _jana_atom_site_ADP_E_11333 _jana_atom_site_ADP_E_12222 _jana_atom_site_ADP_E_12223 _jana_atom_site_ADP_E_12233 _jana_atom_site_ADP_E_12333 _jana_atom_site_ADP_E_13333 _jana_atom_site_ADP_E_22222 _jana_atom_site_ADP_E_22223 _jana_atom_site_ADP_E_22233 _jana_atom_site_ADP_E_22333 _jana_atom_site_ADP_E_23333 _jana_atom_site_ADP_E_33333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_ADP_F_label _jana_atom_site_ADP_F_type_symbol _jana_atom_site_ADP_F_111111 _jana_atom_site_ADP_F_111112 _jana_atom_site_ADP_F_111113 _jana_atom_site_ADP_F_111122 _jana_atom_site_ADP_F_111123 _jana_atom_site_ADP_F_111133 _jana_atom_site_ADP_F_111222 _jana_atom_site_ADP_F_111223 _jana_atom_site_ADP_F_111233 _jana_atom_site_ADP_F_111333 _jana_atom_site_ADP_F_112222 _jana_atom_site_ADP_F_112223 _jana_atom_site_ADP_F_112233 _jana_atom_site_ADP_F_112333 _jana_atom_site_ADP_F_113333 _jana_atom_site_ADP_F_122222 _jana_atom_site_ADP_F_122223 _jana_atom_site_ADP_F_122233 _jana_atom_site_ADP_F_122333 _jana_atom_site_ADP_F_123333 _jana_atom_site_ADP_F_133333 _jana_atom_site_ADP_F_222222 _jana_atom_site_ADP_F_222223 _jana_atom_site_ADP_F_222233 _jana_atom_site_ADP_F_222333 _jana_atom_site_ADP_F_223333 _jana_atom_site_ADP_F_233333 _jana_atom_site_ADP_F_333333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 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 K1 Na1 . . 3.5754(5) ? K1 Na1 . 1_556 3.5754(5) ? K1 Na3 . 1_446 3.9248(9) ? K1 Na3 . 1_456 3.9248(8) ? K1 Na3 . 1_556 3.9248(9) ? K1 Na3 . 4_445 3.9248(9) ? K1 Na3 . 4_545 3.9248(8) ? K1 Na3 . 4_555 3.9248(9) ? K1 S1 . 1_445 3.6458(6) ? K1 S1 . 1_545 3.6458(4) ? K1 S1 . . 3.6458(6) ? K1 S1 . 4_446 3.6458(6) ? K1 S1 . 4_456 3.6458(4) ? K1 S1 . 4_556 3.6458(6) ? K1 O1 . 1_545 2.838(3) ? K1 O1 . 2_665 2.838(3) ? K1 O1 . 3_455 2.838(3) ? K1 O1 . 4_456 2.838(3) ? K1 O1 . 5_666 2.838(3) ? K1 O1 . 6_546 2.838(3) ? K1 O2 . 1_445 3.2420(6) ? K1 O2 . 1_545 3.2420(4) ? K1 O2 . . 3.2420(6) ? K1 O2 . 4_446 3.2420(6) ? K1 O2 . 4_456 3.2420(4) ? K1 O2 . 4_556 3.2420(6) ? K1 Na3_k . 1_446 3.9248(9) ? K1 Na3_k . 1_456 3.9248(8) ? K1 Na3_k . 1_556 3.9248(9) ? K1 Na3_k . 4_445 3.9248(9) ? K1 Na3_k . 4_545 3.9248(8) ? K1 Na3_k . 4_555 3.9248(9) ? Na1 Na3 . 1_445 3.5050(7) ? Na1 Na3 . 1_455 3.5050(6) ? Na1 Na3 . . 3.5050(7) ? Na1 Na3 . 4_445 3.5050(7) ? Na1 Na3 . 4_545 3.5050(6) ? Na1 Na3 . 4_555 3.5050(7) ? Na1 S1 . 1_444 3.7468(6) ? Na1 S1 . 1_544 3.7468(4) ? Na1 S1 . 1_554 3.7468(6) ? Na1 S1 . 4_446 3.7468(6) ? Na1 S1 . 4_456 3.7468(4) ? Na1 S1 . 4_556 3.7468(6) ? Na1 O1 . 1_544 2.338(3) ? Na1 O1 . 2_664 2.338(3) ? Na1 O1 . 3_454 2.338(3) ? Na1 O1 . 4_456 2.338(3) ? Na1 O1 . 5_666 2.338(3) ? Na1 O1 . 6_546 2.338(3) ? Na1 Na3_k . 1_445 3.5050(7) ? Na1 Na3_k . 1_455 3.5050(6) ? Na1 Na3_k . . 3.5050(7) ? Na1 Na3_k . 4_445 3.5050(7) ? Na1 Na3_k . 4_545 3.5050(6) ? Na1 Na3_k . 4_555 3.5050(7) ? Na3 S1 . 1_544 3.2788(6) ? Na3 S1 . 1_554 3.2788(3) ? Na3 S1 . 1_654 3.2788(6) ? Na3 S1 . 4_555 3.9071(17) ? Na3 S1 . 4_556 3.2436(17) ? Na3 O1 . 1_544 2.8116(9) ? Na3 O1 . 1_654 2.8116(9) ? Na3 O1 . 2_664 2.8116(15) ? Na3 O1 . 2_764 2.8116(13) ? Na3 O1 . 3_554 2.8116(13) ? Na3 O1 . 3_564 2.8116(15) ? Na3 O1 . 4_556 3.102(4) ? Na3 O1 . 5_666 3.102(4) ? Na3 O1 . 6_656 3.102(4) ? Na3 O2 . 1_544 3.800(3) ? Na3 O2 . 1_554 3.800(3) ? Na3 O2 . 1_654 3.800(3) ? Na3 O2 . 4_555 2.452(5) ? Na3 Na3_k . . 0 ? S1 O1 . . 1.4575(19) ? S1 O1 . 2_665 1.4575(19) ? S1 O1 . 3_565 1.4575(19) ? S1 O2 . . 1.455(5) ? S1 O2 . 4_456 3.757(3) ? S1 O2 . 4_556 3.757(3) ? S1 O2 . 4_566 3.757(3) ? S1 Na3_k . 1_456 3.2788(6) ? S1 Na3_k . 1_556 3.2788(3) ? S1 Na3_k . 1_566 3.2788(6) ? S1 Na3_k . 4_555 3.9071(17) ? S1 Na3_k . 4_556 3.2436(17) ? O1 O1 . 2_665 2.392(2) ? O1 O1 . 2_675 3.210(2) ? O1 O1 . 3_465 3.210(2) ? O1 O1 . 3_565 2.392(2) ? O1 O1 . 5_677 3.401(5) ? O1 O1 . 6_557 3.401(5) ? O1 O2 . . 2.366(5) ? O1 O2 . 4_456 3.681(4) ? O1 O2 . 4_566 3.681(4) ? O1 Na3_k . 1_456 2.8116(9) ? O1 Na3_k . 1_566 2.8116(9) ? O1 Na3_k . 4_556 3.102(4) ? O2 O2 . 4_456 3.2660(11) ? O2 O2 . 4_556 3.2660(10) ? O2 O2 . 4_566 3.2660(11) ? O2 Na3_k . 1_456 3.800(3) ? O2 Na3_k . 1_556 3.800(3) ? O2 Na3_k . 1_566 3.800(3) ? O2 Na3_k . 4_555 2.452(5) ? 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 ? ? ? ? ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 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_observed_status 0 2 0 290.15 313.67 1.25 o -1 3 0 32.50 40.82 0.22 o 0 3 0 1994.09 1927.13 7.30 o -2 4 0 2567.87 2411.91 12.53 o -1 4 0 21.38 25.47 0.22 o 0 4 0 49.47 43.61 0.44 o -2 5 0 50.67 46.72 0.39 o -1 5 0 790.32 781.00 2.60 o 0 5 0 1.28 1.43 0.11 o -3 6 0 547.73 535.26 3.75 o -2 6 0 10.52 10.53 0.21 o -1 6 0 3.38 3.59 0.13 o 0 6 0 319.14 315.23 2.29 o -3 7 0 0.86 1.15 0.10 o -2 7 0 239.62 226.33 1.59 o -1 7 0 16.45 16.35 0.36 o 0 7 0 9.82 12.20 1.29 o -4 8 0 154.66 165.30 2.55 o -3 8 0 8.54 8.45 0.40 o -1 1 1 421.70 432.30 3.28 o 0 1 1 443.42 437.15 2.70 o -2 2 1 263.75 306.33 1.25 o -1 2 1 126.09 147.59 0.50 o 0 2 1 288.35 323.99 1.16 o -3 3 1 94.47 108.92 0.58 o -2 3 1 21.98 18.69 0.14 o -1 3 1 19.93 17.71 0.14 o 0 3 1 83.94 97.19 0.62 o -4 4 1 2.60 2.37 0.11 o -3 4 1 45.45 42.36 0.28 o -2 4 1 0.20 0.24 0.03 o -1 4 1 42.51 40.11 0.28 o 0 4 1 2.46 2.66 0.11 o -5 5 1 7.77 8.91 0.28 o -4 5 1 12.15 11.43 0.20 o -3 5 1 53.25 54.70 0.42 o -2 5 1 57.17 56.43 0.45 o -1 5 1 12.10 11.66 0.20 o 0 5 1 8.59 9.44 0.26 o -6 6 1 0.82 0.99 0.13 o -5 6 1 5.48 5.26 0.16 o -4 6 1 4.10 4.06 0.13 o -3 6 1 0.65 0.69 0.07 o -2 6 1 3.97 3.97 0.15 o -1 6 1 5.54 5.30 0.17 o 0 6 1 0.92 0.91 0.13 o -7 7 1 13.74 14.51 0.80 o -6 7 1 9.60 9.62 0.30 o -5 7 1 3.82 3.77 0.17 o -4 7 1 4.70 4.99 0.19 o -3 7 1 4.45 4.80 0.19 o -2 7 1 4.02 3.86 0.17 o -1 7 1 9.20 9.59 0.28 o 0 7 1 13.74 14.81 1.25 o -5 8 1 5.11 6.09 0.43 o -4 8 1 0.27 0.56 0.11 o -3 8 1 5.02 5.64 0.37 o 0 0 2 1148.05 1299.11 18.99 o -1 1 2 1347.00 1398.56 10.28 o 0 1 2 1468.94 1411.03 20.60 o -2 2 2 2174.70 2076.84 19.89 o -1 2 2 0.84 0.99 0.04 o 0 2 2 1904.93 1859.52 7.68 o -3 3 2 53.84 61.94 0.45 o -2 3 2 496.45 506.56 1.71 o -1 3 2 567.17 579.58 1.76 o 0 3 2 46.88 55.58 0.37 o -4 4 2 463.80 442.32 2.73 o -3 4 2 474.67 478.52 1.82 o -2 4 2 199.17 193.45 0.79 o -1 4 2 427.97 443.15 1.71 o 0 4 2 518.74 520.19 2.82 o -5 5 2 140.28 137.08 1.42 o -4 5 2 52.55 51.19 0.49 o -3 5 2 329.24 327.74 1.62 o -2 5 2 354.47 342.88 1.53 o -1 5 2 56.90 56.38 0.50 o 0 5 2 123.33 123.94 1.19 o -6 6 2 51.30 51.12 0.87 o -5 6 2 113.64 104.17 0.84 o -4 6 2 175.93 173.73 1.21 o -3 6 2 49.29 44.78 0.49 o -2 6 2 157.56 157.13 1.12 o -1 6 2 129.18 120.91 0.93 o 0 6 2 50.68 50.24 0.87 o -7 7 2 51.74 46.35 2.60 o -6 7 2 89.65 88.70 0.89 o -5 7 2 37.74 33.65 0.52 o -4 7 2 70.50 65.44 0.77 o -3 7 2 80.23 74.21 0.79 o -2 7 2 35.88 32.23 0.52 o -1 7 2 80.89 80.68 0.91 o -5 8 2 59.07 51.11 1.33 o -4 8 2 31.03 34.13 1.33 o -3 8 2 52.61 46.67 1.35 o 0 0 3 2188.71 2417.66 35.11 o -1 1 3 119.64 93.76 0.64 o 0 1 3 134.75 110.37 0.74 o -2 2 3 100.03 96.87 0.64 o -1 2 3 214.77 199.50 0.75 o 0 2 3 108.30 109.12 0.67 o -3 3 3 82.25 79.33 0.59 o -2 3 3 47.71 45.93 0.27 o -1 3 3 43.78 40.48 0.29 o 0 3 3 88.65 83.70 0.62 o -4 4 3 23.98 24.25 0.45 o -3 4 3 75.08 74.24 0.47 o -2 4 3 183.88 173.00 0.83 o -1 4 3 67.17 67.15 0.48 o 0 4 3 27.47 27.57 0.47 o -5 5 3 19.82 22.23 0.51 o -4 5 3 32.28 32.31 0.42 o -3 5 3 61.86 60.29 0.51 o -2 5 3 70.58 67.19 0.53 o -1 5 3 30.00 30.22 0.41 o 0 5 3 21.55 24.62 0.52 o -6 6 3 4.79 5.51 0.32 o -5 6 3 21.38 22.96 0.39 o -4 6 3 14.37 13.12 0.30 o -3 6 3 20.13 19.18 0.34 o -2 6 3 13.07 11.97 0.28 o -1 6 3 22.52 23.99 0.42 o 0 6 3 5.21 6.18 0.31 o -6 7 3 24.00 24.48 0.50 o -5 7 3 3.13 3.48 0.18 o -4 7 3 13.83 14.09 0.36 o -3 7 3 13.83 14.35 0.34 o -2 7 3 3.58 4.12 0.19 o -1 7 3 21.39 22.22 0.49 o 0 0 4 1904.17 1895.73 15.96 o -1 1 4 99.01 98.17 0.73 o 0 1 4 85.98 79.53 0.64 o -2 2 4 437.60 450.34 2.29 o -1 2 4 916.85 970.59 3.37 o 0 2 4 452.22 462.15 2.31 o -3 3 4 613.79 656.54 3.12 o -2 3 4 142.09 150.15 0.70 o -1 3 4 129.66 133.88 0.69 o 0 3 4 580.38 602.81 2.98 o -4 4 4 107.88 109.24 1.08 o -3 4 4 64.94 64.55 0.50 o -2 4 4 570.73 595.79 2.37 o -1 4 4 70.68 69.05 0.54 o 0 4 4 107.40 107.48 1.25 o -5 5 4 52.17 52.64 0.74 o -4 5 4 219.68 226.77 1.35 o -3 5 4 31.17 37.40 0.41 o -2 5 4 29.94 36.21 0.42 o -1 5 4 229.78 234.82 1.40 o 0 5 4 53.79 53.04 0.91 o -6 6 4 117.13 126.13 1.66 o -5 6 4 47.78 48.53 0.61 o -4 6 4 47.25 54.34 0.68 o -3 6 4 140.28 141.60 1.09 o -2 6 4 47.07 53.86 0.65 o -1 6 4 46.03 48.20 0.63 o 0 6 4 115.30 121.87 1.74 o -6 7 4 19.98 20.54 1.84 o -5 7 4 90.22 88.30 0.98 o -4 7 4 34.18 37.16 0.66 o -3 7 4 33.55 35.66 0.60 o -2 7 4 86.42 84.52 0.99 o -1 7 4 19.24 19.92 1.19 o 0 0 5 94.57 122.54 1.72 o -1 1 5 304.15 292.46 1.72 o 0 1 5 326.65 321.14 2.29 o -2 2 5 293.47 286.77 1.68 o -1 2 5 14.08 12.04 0.19 o 0 2 5 262.82 250.60 1.76 o -3 3 5 4.77 5.12 0.18 o -2 3 5 210.36 203.77 1.02 o -1 3 5 209.20 201.09 1.03 o 0 3 5 5.43 6.02 0.20 o -4 4 5 93.14 88.89 1.06 o -3 4 5 154.26 143.36 0.90 o -1 4 5 145.80 135.76 0.89 o 0 4 5 102.07 94.65 1.11 o -5 5 5 56.89 57.77 0.86 o -3 5 5 84.85 83.82 0.71 o -2 5 5 92.98 91.03 0.76 o 0 5 5 59.60 60.35 0.94 o -6 6 5 0.22 0.24 0.12 < -5 6 5 56.08 54.28 0.69 o -4 6 5 41.69 39.03 0.59 o -2 6 5 40.35 40.55 0.55 o -1 6 5 55.76 53.55 0.74 o 0 6 5 0.25 0.27 0.10 o -5 7 5 0.01 0.32 0.28 < -4 7 5 36.28 35.77 0.83 o -3 7 5 34.95 34.99 0.73 o -1 1 6 248.79 277.49 2.35 o 0 1 6 286.55 322.49 2.64 o -2 2 6 399.98 429.96 2.49 o 0 2 6 353.52 369.26 2.78 o -3 3 6 16.89 17.06 0.38 o -2 3 6 212.65 222.10 1.35 o -1 3 6 245.07 255.95 1.49 o 0 3 6 18.93 18.43 0.41 o -4 4 6 129.58 129.21 1.48 o -3 4 6 115.43 117.42 0.89 o -2 4 6 11.83 11.36 0.25 o -1 4 6 100.31 102.13 0.85 o 0 4 6 148.26 142.96 1.61 o -5 5 6 88.56 79.04 1.26 o -4 5 6 6.86 8.16 0.26 o -3 5 6 63.94 66.81 0.70 o -2 5 6 73.56 77.91 0.75 o -1 5 6 6.05 7.25 0.26 o 0 5 6 76.89 70.33 1.27 o -5 6 6 43.25 42.52 0.66 o -4 6 6 72.23 74.01 0.86 o -3 6 6 3.43 3.27 0.16 o -2 6 6 62.99 67.81 0.83 o -1 6 6 49.47 47.62 0.76 o 0 0 7 21.40 19.86 0.96 o -1 1 7 95.52 105.24 1.27 o 0 1 7 85.24 90.01 1.20 o -2 2 7 113.05 118.92 1.31 o 0 2 7 120.01 125.52 1.46 o -3 3 7 2.51 1.98 0.18 o -2 3 7 102.25 106.56 0.87 o -1 3 7 91.84 92.93 0.79 o 0 3 7 2.71 2.19 0.16 o -4 4 7 54.47 52.25 0.98 o -3 4 7 63.07 58.63 0.70 o -2 4 7 1.84 1.91 0.13 o -1 4 7 68.81 63.77 0.70 o 0 4 7 51.94 48.10 1.01 o -5 5 7 38.89 36.79 0.81 o -4 5 7 2.43 2.51 0.16 o -3 5 7 38.58 41.88 0.61 o -2 5 7 36.30 39.65 0.56 o -1 5 7 2.13 2.43 0.16 o 0 5 7 42.79 40.89 0.98 o -4 6 7 29.05 28.82 0.99 o -3 6 7 2.40 2.51 0.20 o -2 6 7 30.94 27.05 1.35 o 0 0 8 27.66 24.67 1.16 o -1 1 8 58.76 60.38 1.00 o 0 1 8 53.71 52.57 0.94 o -2 2 8 56.94 59.58 1.11 o -1 2 8 51.13 56.78 0.73 o 0 2 8 64.61 74.19 1.14 o -3 3 8 35.26 37.24 0.88 o -2 3 8 26.77 29.21 0.52 o -1 3 8 23.59 24.18 0.44 o 0 3 8 35.04 37.07 0.76 o -4 4 8 28.50 30.93 0.96 o -3 4 8 22.38 19.78 0.45 o -2 4 8 19.41 23.19 0.47 o -1 4 8 25.07 22.35 0.46 o 0 4 8 24.76 26.66 0.78 o -4 5 8 13.24 13.62 1.00 o -3 5 8 21.87 18.68 0.46 o -2 5 8 19.22 17.00 0.49 o -1 5 8 13.57 15.45 1.57 o 0 0 9 65.52 55.45 1.93 o -1 1 9 70.70 67.81 1.25 o 0 1 9 70.05 68.02 1.16 o -2 2 9 82.41 85.36 1.43 o -1 2 9 64.46 68.73 0.83 o 0 2 9 82.60 87.99 1.36 o -3 3 9 40.80 49.18 1.09 o -2 3 9 56.42 59.52 0.79 o -1 3 9 55.48 56.82 0.74 o 0 3 9 42.12 50.97 0.95 o -3 4 9 35.96 36.25 1.03 o -2 4 9 28.74 31.43 0.76 o -1 4 9 37.60 36.60 1.39 o 0 0 10 20.47 24.39 1.33 o -1 1 10 32.65 28.71 0.86 o 0 1 10 36.85 37.52 0.89 o -1 2 10 8.72 7.01 0.46 o 0 2 10 23.47 22.49 1.88 o loop_ _twin_refln_datum_id _twin_refln_individual_id _twin_refln_index_h _twin_refln_index_k _twin_refln_index_l _twin_refln_F_squared_calc _twin_refln_F_squared_meas _twin_refln_F_squared_sigma _twin_refln_include_status ? ? ? ? ? ? ? ? ?