#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 25/10/2015' # 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 'As3 Fe4 H14 K0.2 O21 Pb0.5' _chemical_formula_weight 909.7 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P -4 3 m' _symmetry_space_group_name_Hall 'P -4;2;3' _symmetry_Int_Tables_number 215 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,z 3 -x,y,-z 4 x,-y,-z 5 z,x,y 6 z,-x,-y 7 -z,-x,y 8 -z,x,-y 9 y,z,x 10 -y,z,-x 11 y,-z,-x 12 -y,-z,x 13 y,x,z 14 -y,-x,z 15 y,-x,-z 16 -y,x,-z 17 x,z,y 18 -x,z,-y 19 -x,-z,y 20 x,-z,-y 21 z,y,x 22 z,-y,-x 23 -z,y,-x 24 -z,-y,x _cell_length_a 7.9791 _cell_length_b 7.9791 _cell_length_c 7.9791 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 507.9977 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 ? ? ? ? ? ? ? ? ? ? ? _cell_formula_units_Z 1 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.9735 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 411 _exptl_absorpt_coefficient_mu 15.527 _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type X-ray _diffrn_radiation_source ? _diffrn_radiation_wavelength 0.80038 _diffrn_radiation_monochromator ? _diffrn_measurement_device ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_measurement_specimen_support ? _diffrn_reflns_number 3384 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 32.85 _diffrn_reflns_theta_full 32.85 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.1298 _diffrn_reflns_av_unetI/netI 0.0039 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _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 ? ? ? _diffrn_radiation_probe X-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 287 _reflns_number_gt 284 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.1007 _refine_ls_wR_factor_gt 0.1489 _refine_ls_R_factor_all 0.1008 _refine_ls_wR_factor_ref 0.1489 _refine_ls_goodness_of_fit_ref 12.92 _refine_ls_goodness_of_fit_gt 12.99 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 287 _refine_ls_number_parameters 16 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0492 _refine_ls_shift/su_mean 0.0179 _refine_diff_density_max 2.01 _refine_diff_density_min -3.26 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; 115 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As -0.2359 2.4582 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Fe 0.3576 1.0559 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.2369 0.3191 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0150 0.0081 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Pb -7.6102 10.6145 '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 Fe Fe 0.1431(3) 0.1431(3) 0.1431(3) Uani 0.0206(6) 4 1 d . . . As As 0.5 0 0 Uani 0.0317(10) 3 1 d . . . O1 O 0.1243(15) 0.381(2) 0.1243(15) Uiso 0.035(4) 12 1 d . . . O2 O 0.8865(13) 0.8865(13) 0.8865(13) Uiso 0.008(3) 4 1 d . . . Pb Pb 0 0.5 0.5 Uiso 0.12(2) 3 0.13(2) d . . . Ow1 O 0.685(7) 0.685(7) 0.685(7) Uiso 0.100(18) 4 0.6739 d . . . Ow2 O 0.219(10) 0.5 0.5 Uiso 0.100(18) 6 0.5671 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 Fe Fe 0.0206(11) 0.0206(11) 0.0206(11) -0.0047(8) -0.0047(8) -0.0047(8) As As 0.0143(17) 0.0404(17) 0.0404(17) 0 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 Fe O1 . . 1.908(16) ? Fe O1 . 5_555 1.908(16) ? Fe O1 . 9_555 1.908(16) ? Fe O2 . 2_664 2.074(11) ? Fe O2 . 3_646 2.074(11) ? Fe O2 . 4_466 2.074(11) ? As O1 . 9_555 1.695(14) ? As O1 . 10_655 1.695(14) ? As O1 . 11_555 1.695(14) ? As O1 . 12_655 1.695(14) ? As O2 . 1_544 3.339(11) ? As O2 . 2_664 3.339(11) ? As O2 . 3_646 3.339(11) ? As O2 . 4_566 3.339(11) ? Pb O1 . . 3.298(13) ? Pb O1 . 2_565 3.298(13) ? Pb O1 . 3_556 3.298(13) ? Pb O1 . 4_566 3.298(13) ? Pb O1 . 5_555 3.298(13) ? Pb O1 . 6_566 3.298(13) ? Pb O1 . 7_565 3.298(13) ? Pb O1 . 8_556 3.298(13) ? Pb Ow1 . 1_455 3.27(5) ? Pb Ow1 . 2_665 3.27(5) ? Pb Ow1 . 3_656 3.27(5) ? Pb Ow1 . 4_466 3.27(5) ? Pb Ow2 . . 1.75(8) ? Pb Ow2 . 2_565 1.75(8) ? 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 O1 Fe O1 . . 5_555 98.6(5) ? O1 Fe O1 . . 9_555 98.6(5) ? O1 Fe O2 . . 2_664 91.5(5) ? O1 Fe O2 . . 3_646 164.3(5) ? O1 Fe O2 . . 4_466 91.5(5) ? O1 Fe O1 5_555 . 9_555 98.6(5) ? O1 Fe O2 5_555 . 2_664 164.3(5) ? O1 Fe O2 5_555 . 3_646 91.5(5) ? O1 Fe O2 5_555 . 4_466 91.5(5) ? O1 Fe O2 9_555 . 2_664 91.5(5) ? O1 Fe O2 9_555 . 3_646 91.5(5) ? O1 Fe O2 9_555 . 4_466 164.3(5) ? O2 Fe O2 2_664 . 3_646 76.2(4) ? O2 Fe O2 2_664 . 4_466 76.2(4) ? O2 Fe O2 3_646 . 4_466 76.2(4) ? O1 As O1 9_555 . 10_655 108.4(6) ? O1 As O1 9_555 . 11_555 111.7(7) ? O1 As O1 9_555 . 12_655 108.4(6) ? O1 As O2 9_555 . 1_544 146.7(5) ? O1 As O2 9_555 . 2_664 58.8(5) ? O1 As O2 9_555 . 3_646 58.8(5) ? O1 As O2 9_555 . 4_566 101.6(5) ? O1 As O1 10_655 . 11_555 108.4(6) ? O1 As O1 10_655 . 12_655 111.7(7) ? O1 As O2 10_655 . 1_544 58.8(5) ? O1 As O2 10_655 . 2_664 101.6(5) ? O1 As O2 10_655 . 3_646 146.7(5) ? O1 As O2 10_655 . 4_566 58.8(5) ? O1 As O1 11_555 . 12_655 108.4(6) ? O1 As O2 11_555 . 1_544 101.6(5) ? O1 As O2 11_555 . 2_664 58.8(5) ? O1 As O2 11_555 . 3_646 58.8(5) ? O1 As O2 11_555 . 4_566 146.7(5) ? O1 As O2 12_655 . 1_544 58.8(5) ? O1 As O2 12_655 . 2_664 146.7(5) ? O1 As O2 12_655 . 3_646 101.6(5) ? O1 As O2 12_655 . 4_566 58.8(5) ? O2 As O2 1_544 . 2_664 148.5(3) ? O2 As O2 1_544 . 3_646 148.5(3) ? O2 As O2 1_544 . 4_566 45.1(3) ? O2 As O2 2_664 . 3_646 45.1(3) ? O2 As O2 2_664 . 4_566 148.5(3) ? O2 As O2 3_646 . 4_566 148.5(3) ? O1 Pb O1 . . 2_565 49.3(3) ? O1 Pb O1 . . 3_556 146.5(4) ? O1 Pb O1 . . 4_566 145.0(3) ? O1 Pb O1 . . 5_555 52.1(4) ? O1 Pb O1 . . 6_566 115.7(4) ? O1 Pb O1 . . 7_565 95.2(4) ? O1 Pb O1 . . 8_556 95.2(4) ? O1 Pb Ow1 . . 1_455 140.6(10) ? O1 Pb Ow1 . . 2_665 92.8(10) ? O1 Pb Ow1 . . 3_656 59.2(10) ? O1 Pb Ow1 . . 4_466 71.9(10) ? O1 Pb Ow2 . . . 72.5(2) ? O1 Pb Ow2 . . 2_565 107.5(2) ? O1 Pb O1 2_565 . 3_556 145.0(3) ? O1 Pb O1 2_565 . 4_566 146.5(4) ? O1 Pb O1 2_565 . 5_555 95.2(4) ? O1 Pb O1 2_565 . 6_566 95.2(4) ? O1 Pb O1 2_565 . 7_565 52.1(4) ? O1 Pb O1 2_565 . 8_556 115.7(4) ? O1 Pb Ow1 2_565 . 1_455 92.8(10) ? O1 Pb Ow1 2_565 . 2_665 140.6(10) ? O1 Pb Ow1 2_565 . 3_656 71.9(10) ? O1 Pb Ow1 2_565 . 4_466 59.2(10) ? O1 Pb Ow2 2_565 . . 107.5(2) ? O1 Pb Ow2 2_565 . 2_565 72.5(2) ? O1 Pb O1 3_556 . 4_566 49.3(3) ? O1 Pb O1 3_556 . 5_555 95.2(4) ? O1 Pb O1 3_556 . 6_566 95.2(4) ? O1 Pb O1 3_556 . 7_565 115.7(4) ? O1 Pb O1 3_556 . 8_556 52.1(4) ? O1 Pb Ow1 3_556 . 1_455 59.2(10) ? O1 Pb Ow1 3_556 . 2_665 71.9(10) ? O1 Pb Ow1 3_556 . 3_656 140.6(10) ? O1 Pb Ow1 3_556 . 4_466 92.8(10) ? O1 Pb Ow2 3_556 . . 107.5(2) ? O1 Pb Ow2 3_556 . 2_565 72.5(2) ? O1 Pb O1 4_566 . 5_555 115.7(4) ? O1 Pb O1 4_566 . 6_566 52.1(4) ? O1 Pb O1 4_566 . 7_565 95.2(4) ? O1 Pb O1 4_566 . 8_556 95.2(4) ? O1 Pb Ow1 4_566 . 1_455 71.9(10) ? O1 Pb Ow1 4_566 . 2_665 59.2(10) ? O1 Pb Ow1 4_566 . 3_656 92.8(10) ? O1 Pb Ow1 4_566 . 4_466 140.6(10) ? O1 Pb Ow2 4_566 . . 72.5(2) ? O1 Pb Ow2 4_566 . 2_565 107.5(2) ? O1 Pb O1 5_555 . 6_566 145.0(3) ? O1 Pb O1 5_555 . 7_565 146.5(4) ? O1 Pb O1 5_555 . 8_556 49.3(3) ? O1 Pb Ow1 5_555 . 1_455 140.6(10) ? O1 Pb Ow1 5_555 . 2_665 59.2(10) ? O1 Pb Ow1 5_555 . 3_656 92.8(10) ? O1 Pb Ow1 5_555 . 4_466 71.9(10) ? O1 Pb Ow2 5_555 . . 72.5(2) ? O1 Pb Ow2 5_555 . 2_565 107.5(2) ? O1 Pb O1 6_566 . 7_565 49.3(3) ? O1 Pb O1 6_566 . 8_556 146.5(4) ? O1 Pb Ow1 6_566 . 1_455 71.9(10) ? O1 Pb Ow1 6_566 . 2_665 92.8(10) ? O1 Pb Ow1 6_566 . 3_656 59.2(10) ? O1 Pb Ow1 6_566 . 4_466 140.6(10) ? O1 Pb Ow2 6_566 . . 72.5(2) ? O1 Pb Ow2 6_566 . 2_565 107.5(2) ? O1 Pb O1 7_565 . 8_556 145.0(3) ? O1 Pb Ow1 7_565 . 1_455 59.2(10) ? O1 Pb Ow1 7_565 . 2_665 140.6(10) ? O1 Pb Ow1 7_565 . 3_656 71.9(10) ? O1 Pb Ow1 7_565 . 4_466 92.8(10) ? O1 Pb Ow2 7_565 . . 107.5(2) ? O1 Pb Ow2 7_565 . 2_565 72.5(2) ? O1 Pb Ow1 8_556 . 1_455 92.8(10) ? O1 Pb Ow1 8_556 . 2_665 71.9(10) ? O1 Pb Ow1 8_556 . 3_656 140.6(10) ? O1 Pb Ow1 8_556 . 4_466 59.2(10) ? O1 Pb Ow2 8_556 . . 107.5(2) ? O1 Pb Ow2 8_556 . 2_565 72.5(2) ? Ow1 Pb Ow1 1_455 . 2_665 126.2(14) ? Ow1 Pb Ow1 1_455 . 3_656 126.2(14) ? Ow1 Pb Ow1 1_455 . 4_466 79.5(14) ? Ow1 Pb Ow2 1_455 . . 140.2(10) ? Ow1 Pb Ow2 1_455 . 2_565 39.8(10) ? Ow1 Pb Ow1 2_665 . 3_656 79.5(14) ? Ow1 Pb Ow1 2_665 . 4_466 126.2(14) ? Ow1 Pb Ow2 2_665 . . 39.8(10) ? Ow1 Pb Ow2 2_665 . 2_565 140.2(10) ? Ow1 Pb Ow1 3_656 . 4_466 126.2(14) ? Ow1 Pb Ow2 3_656 . . 39.8(10) ? Ow1 Pb Ow2 3_656 . 2_565 140.2(10) ? Ow1 Pb Ow2 4_466 . . 140.2(10) ? Ow1 Pb Ow2 4_466 . 2_565 39.8(10) ? Ow2 Pb Ow2 . . 2_565 180.0(5) ? 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 1 0 0 11171.40 6272.34 10.86 o 1 1 0 60.43 591.96 1.90 o 1 1 1 5806.83 3414.00 6.75 o 1 1 -1 5733.98 3297.79 4.48 o 2 0 0 7968.39 8605.43 6.76 o 2 1 0 281.37 521.71 1.18 o 2 1 1 6029.37 6321.70 4.52 o 2 1 -1 5593.77 6172.01 4.41 o 2 2 0 9726.15 11400.10 6.15 o 2 2 1 1518.42 1137.02 2.11 o 2 2 -1 1304.64 1086.08 2.26 o 2 2 2 5247.50 5618.00 9.09 o 2 2 -2 4123.07 5268.10 7.59 o 3 0 0 7264.36 6663.01 7.47 o 3 1 0 5104.50 5447.74 3.57 o 3 1 1 5864.91 5565.68 4.41 o 3 1 -1 5379.66 4699.51 5.23 o 3 2 0 351.82 539.52 1.55 o 3 2 1 808.89 1039.32 1.71 o 3 2 -1 706.74 952.75 1.93 o 3 2 2 470.88 503.91 1.86 o 3 2 -2 364.59 475.60 1.78 o 3 3 0 1509.12 1429.61 2.73 o 3 3 1 1228.55 1224.92 2.84 o 3 3 -1 1147.40 1048.50 2.68 o 3 3 2 1257.33 1475.60 3.79 o 3 3 -2 1246.47 1367.87 3.35 o 3 3 3 5561.75 6385.28 14.82 o 3 3 -3 5402.54 7214.81 12.75 o 4 0 0 1949.45 2358.17 6.01 o 4 1 0 2226.19 2322.69 2.84 o 4 1 1 2417.15 2651.99 4.31 o 4 1 -1 2629.23 2852.62 5.68 o 4 2 0 6399.23 6655.54 5.17 o 4 2 1 1041.41 907.21 1.98 o 4 2 -1 988.37 956.48 2.01 o 4 2 2 4694.70 4140.09 5.47 o 4 2 -2 4044.13 3046.54 5.24 o 4 3 0 5323.28 5635.34 5.05 o 4 3 1 271.16 258.59 1.26 o 4 3 -1 320.46 274.42 1.69 o 4 3 2 320.33 361.61 1.65 o 4 3 -2 286.80 322.38 1.67 o 4 3 3 2458.19 2350.09 4.76 o 4 3 -3 2539.00 2417.55 4.42 o 4 4 0 18718.20 18175.50 14.19 o 4 4 1 2856.32 3433.04 5.52 o 4 4 -1 2801.41 3205.79 6.19 o 4 4 2 1749.17 1778.81 3.99 o 4 4 -2 1852.27 1966.66 4.56 o 4 4 3 1065.95 1088.06 3.32 o 4 4 -3 1089.57 1026.24 3.71 o 4 4 4 312.10 366.60 5.29 o 4 4 -4 266.08 367.32 5.82 o 5 0 0 910.11 694.12 3.52 o 5 1 0 927.85 876.44 2.02 o 5 1 1 2889.82 2494.80 4.20 o 5 1 -1 3243.79 2794.00 5.62 o 5 2 0 229.41 311.69 1.64 o 5 2 1 2103.46 2065.33 3.16 o 5 2 -1 2243.74 2270.22 3.09 o 5 2 2 1173.04 1520.77 4.42 o 5 2 -2 1190.86 1372.33 4.74 o 5 3 0 91.43 260.42 1.92 o 5 3 1 1757.67 1994.93 3.09 o 5 3 -1 1929.59 2251.83 4.20 o 5 3 2 683.54 643.38 1.98 o 5 3 -2 764.23 767.96 2.33 o 5 3 3 1677.10 1769.88 5.39 o 5 3 -3 1806.96 2144.99 5.98 o 5 4 0 908.37 1019.49 2.75 o 5 4 1 349.20 337.02 1.70 o 5 4 -1 280.46 288.13 1.87 o 5 4 2 404.26 545.42 1.92 o 5 4 -2 420.60 608.92 2.36 o 5 4 3 489.61 512.50 2.19 o 5 4 -3 457.34 497.25 2.64 o 5 4 4 74.50 56.85 1.84 o 5 4 -4 52.35 32.53 2.39 o 5 5 0 137.34 269.36 3.24 o 5 5 1 2180.60 2331.68 4.99 o 5 5 -1 1974.54 2448.91 6.61 o 5 5 2 1442.36 1690.91 4.45 o 5 5 -2 1336.18 1228.94 5.66 o 5 5 3 945.88 1356.92 4.38 o 5 5 -3 800.80 1217.06 4.95 o 5 5 4 313.69 272.67 2.83 o 5 5 -4 334.13 264.93 3.63 o 5 5 5 1152.11 1680.53 8.88 o 5 5 -5 1303.46 1849.85 9.50 o 6 0 0 5636.03 5336.60 8.85 o 6 1 0 767.10 669.82 1.95 o 6 1 1 405.78 373.43 2.27 o 6 1 -1 435.72 370.07 2.91 o 6 2 0 1395.28 1449.69 3.40 o 6 2 1 385.02 313.83 1.77 o 6 2 -1 393.14 308.74 2.45 o 6 2 2 1467.33 1651.06 4.39 o 6 2 -2 1850.23 2059.98 5.88 o 6 3 0 41.74 123.14 1.84 o 6 3 1 545.37 453.80 2.20 o 6 3 -1 565.43 429.28 2.02 o 6 3 2 220.25 242.11 2.29 o 6 3 -2 276.95 298.77 2.12 o 6 3 3 74.97 82.51 3.15 o 6 3 -3 84.02 121.85 2.42 o 6 4 0 387.37 524.41 2.61 o 6 4 1 188.11 218.87 1.68 o 6 4 -1 208.12 199.73 2.04 o 6 4 2 1573.99 1504.37 3.50 o 6 4 -2 1735.06 1698.86 3.84 o 6 4 3 660.35 687.18 2.80 o 6 4 -3 702.40 752.82 2.89 o 6 4 4 1585.57 1643.93 4.96 o 6 4 -4 1570.98 1522.88 7.07 o 6 5 0 24.86 55.67 2.10 o 6 5 1 489.76 453.59 2.19 o 6 5 -1 435.96 449.41 2.75 o 6 5 2 422.16 465.91 2.20 o 6 5 -2 414.81 541.28 3.10 o 6 5 3 93.52 113.07 1.77 o 6 5 -3 86.01 126.33 2.43 o 6 5 4 223.16 305.66 2.33 o 6 5 -4 188.20 262.43 2.67 o 6 5 5 407.60 506.03 4.32 o 6 5 -5 418.29 472.24 6.30 o 6 6 0 1338.36 1432.60 5.89 o 6 6 1 366.72 560.25 3.82 o 6 6 -1 333.29 591.86 6.11 o 6 6 2 569.81 566.90 4.36 o 6 6 -2 420.39 515.89 4.78 o 6 6 3 9.04 51.66 2.80 o 6 6 -3 2.08 71.30 4.68 o 6 6 4 232.88 239.36 3.08 o 6 6 -4 168.40 275.56 5.17 o 6 6 5 73.92 183.59 3.20 o 6 6 -5 60.72 157.30 4.84 o 6 6 6 228.14 401.11 6.01 o 7 0 0 2461.50 1703.94 9.41 o 7 1 0 77.02 160.94 1.47 o 7 1 1 453.69 305.07 2.99 o 7 1 -1 501.20 364.55 2.96 o 7 2 0 18.28 41.94 1.48 o 7 2 1 385.00 372.81 2.19 o 7 2 -1 355.67 405.26 2.41 o 7 2 2 164.34 116.22 2.49 o 7 2 -2 191.33 145.90 2.57 o 7 3 0 1854.35 1637.54 3.88 o 7 3 1 1901.95 1800.27 4.16 o 7 3 -1 1921.87 1841.30 4.72 o 7 3 2 79.82 97.07 1.95 o 7 3 -2 57.69 127.37 2.03 o 7 3 3 16.31 27.07 3.49 o 7 3 -3 12.39 37.88 2.48 o 7 4 0 946.58 730.84 2.83 o 7 4 1 735.73 807.37 2.87 o 7 4 -1 718.84 762.57 3.03 o 7 4 2 114.81 155.75 2.07 o 7 4 -2 130.55 138.61 2.02 o 7 4 3 197.41 150.82 2.33 o 7 4 -3 202.43 204.50 2.40 o 7 4 4 832.82 1124.90 4.96 o 7 4 -4 835.17 962.66 6.43 o 7 5 0 291.72 361.31 2.77 o 7 5 1 541.15 615.92 3.05 o 7 5 -1 503.17 623.73 3.41 o 7 5 2 69.36 123.76 2.00 o 7 5 -2 74.96 169.64 2.40 o 7 5 3 283.35 377.24 2.99 o 7 5 -3 273.44 432.98 3.54 o 7 5 4 16.32 60.07 2.20 o 7 5 -4 23.26 58.46 4.11 o 7 5 5 304.46 404.10 3.51 o 7 5 -5 325.08 332.76 5.36 o 7 6 0 334.80 421.36 3.16 o 7 6 1 16.58 54.05 2.73 o 7 6 -1 18.75 52.06 2.73 o 7 6 2 100.29 56.08 2.50 o 7 6 -2 86.85 39.81 2.85 o 7 6 3 298.06 247.00 2.28 o 7 6 -3 324.91 316.72 4.77 o 7 6 4 61.87 47.46 2.61 o 7 6 -4 65.70 55.73 2.76 o 7 6 5 71.12 64.38 4.59 o 7 6 -5 64.81 126.11 6.84 o 7 7 0 177.12 195.74 4.75 o 7 7 1 24.44 51.23 3.55 o 7 7 -1 34.94 63.79 5.00 o 7 7 2 167.18 264.21 3.84 o 7 7 -2 198.02 291.04 4.42 o 7 7 3 902.58 1155.57 10.15 o 7 7 -3 929.87 1227.69 9.95 o 7 7 4 471.59 642.93 17.34 o 7 7 -4 488.39 705.53 10.70 o 8 0 0 4799.50 4302.45 21.51 o 8 1 0 985.49 840.04 2.75 o 8 1 1 314.36 254.93 3.70 o 8 1 -1 297.55 256.53 2.76 o 8 2 0 580.83 487.91 3.01 o 8 2 1 508.59 401.46 3.10 o 8 2 -1 564.17 412.35 2.74 o 8 2 2 1305.65 843.17 5.25 o 8 2 -2 1542.78 1210.10 5.44 o 8 3 0 186.87 167.73 2.08 o 8 3 1 294.71 241.23 2.67 o 8 3 -1 274.24 231.12 2.99 o 8 3 2 349.55 303.20 3.07 o 8 3 -2 400.64 345.55 2.62 o 8 3 3 167.09 157.59 4.00 o 8 3 -3 173.61 220.58 3.86 o 8 4 0 52.03 64.36 1.94 o 8 4 1 58.95 103.92 2.27 o 8 4 -1 34.16 77.56 2.92 o 8 4 2 622.24 606.11 3.46 o 8 4 -2 593.31 547.07 3.82 o 8 4 3 611.89 577.56 3.75 o 8 4 -3 619.66 597.69 4.24 o 8 4 4 1551.66 1440.96 7.39 o 8 4 -4 1555.89 1593.28 7.64 o 8 5 0 1.39 39.48 2.07 o 8 5 1 243.11 204.90 2.93 o 8 5 -1 246.07 216.77 3.33 o 8 5 2 413.99 423.30 3.21 o 8 5 -2 371.94 358.13 3.75 o 8 5 3 82.33 77.65 2.41 o 8 5 -3 94.63 111.45 3.08 o 8 5 4 156.12 244.53 4.07 o 8 5 -4 150.43 301.00 5.03 o 8 6 0 546.49 624.68 4.50 o 8 6 1 341.81 306.41 3.13 o 8 6 -1 292.05 305.20 3.19 o 8 6 2 491.99 472.66 5.70 o 8 6 -2 394.65 440.27 4.71 o 8 6 3 75.38 102.48 4.73 o 8 6 -3 64.99 160.68 3.21 o 8 7 0 315.72 369.79 7.52 o 8 7 -1 29.92 57.44 5.15 o 8 7 2 24.38 13.30 8.05 < 8 7 -2 19.14 16.37 6.22 < 9 0 0 8.52 16.18 4.21 o 9 1 0 153.67 208.48 2.44 o 9 1 1 918.35 569.60 5.81 o 9 1 -1 807.50 533.46 3.67 o 9 2 0 2.33 18.86 2.74 o 9 2 1 440.44 400.12 3.20 o 9 2 -1 388.34 324.33 3.07 o 9 2 2 328.36 286.21 4.65 o 9 2 -2 322.65 279.00 4.78 o 9 3 0 47.38 66.49 3.02 o 9 3 1 322.27 196.70 4.12 o 9 3 -1 263.30 185.95 2.55 o 9 3 2 179.60 230.20 4.04 o 9 3 -2 159.09 179.34 3.60 o 9 3 3 436.21 376.75 5.20 o 9 3 -3 400.48 328.81 4.60 o 9 4 0 1.59 11.87 2.25 o 9 4 1 91.03 90.01 2.88 o 9 4 -1 99.31 88.73 2.11 o 9 4 2 97.58 94.60 2.37 o 9 4 -2 92.63 91.59 2.84 o 9 4 3 100.90 160.93 3.16 o 9 4 -3 114.74 177.31 3.70 o 9 4 4 17.56 23.41 2.64 o 9 4 -4 10.36 12.15 6.17 < 9 5 0 61.89 73.37 4.79 o 9 5 1 395.79 267.16 3.74 o 9 5 -1 465.92 263.99 3.25 o 9 5 2 373.50 406.31 9.64 o 9 5 -2 405.10 403.23 4.26 o 9 5 3 295.45 236.82 10.03 o 9 5 -3 339.25 389.48 5.52 o 10 0 0 14.95 5.55 0.83 o 10 1 0 0.10 29.48 2.38 o 10 1 1 42.56 29.69 4.45 o 10 1 -1 39.31 39.71 2.81 o 10 2 0 411.91 180.33 3.82 o 10 2 1 134.33 78.83 3.79 o 10 2 -1 118.86 117.66 3.14 o 10 2 2 276.91 136.08 4.39 o 10 2 -2 191.31 129.52 4.63 o 10 3 0 396.74 194.55 3.59 o 10 3 1 70.78 44.55 3.27 o 10 3 -1 67.98 52.88 3.29 o 10 3 2 30.74 35.31 3.24 o 10 3 -2 16.54 34.20 4.95 o 10 4 0 580.70 348.59 6.05 o 10 4 -1 184.82 175.01 8.11 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 ? ? ? ? ? ? ? ? ?