#------------------------------------------------------------------------------ #$Date: 2024-01-06 09:57:03 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288789 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247633.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7247633 loop_ _publ_author_name 'Gao, Cheng-Cheng' 'Tang, Xue-Na' 'Miao, Jing-Ling' 'Li, Yu' 'Li, Cuncheng' 'Liu, Guang-Ning' _publ_section_title ; Regulating the crystal and electronic structures and optical properties of hybrid bromoplumbates with alkylated N, S- or P-containing aromatic cations ; _journal_issue 47 _journal_name_full CrystEngComm _journal_page_first 6556 _journal_page_last 6567 _journal_paper_doi 10.1039/D3CE00931A _journal_volume 25 _journal_year 2023 _chemical_formula_moiety 'Br8 Pb3, 2(C10 H12 N S)' _chemical_formula_sum 'C20 H24 Br8 N2 Pb3 S2' _chemical_formula_weight 1617.38 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2023-09-20 _audit_creation_method ; FinalCif V106 by Daniel Kratzert, Freiburg 2023, https://dkratzert.de/finalcif.html ; _audit_update_record ; 2023-09-21 deposited with the CCDC. 2023-11-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.913(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.8791(4) _cell_length_b 21.8322(14) _cell_length_c 17.9977(10) _cell_measurement_reflns_used 2929 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.8660 _cell_measurement_theta_min 3.0050 _cell_volume 3486.9(3) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (G. Sheldrick)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0355 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -53.00 35.00 1.0000 28.6000 omega____ theta____ kappa____ phi______ frames - 15.8569 -37.0000 -30.0000 88 #__ type_ start__ end____ width___ exp.time_ 2 omega -3.00 85.00 1.0000 28.6000 omega____ theta____ kappa____ phi______ frames - 15.8569 37.0000 150.0000 88 #__ type_ start__ end____ width___ exp.time_ 3 omega -25.00 22.00 1.0000 28.6000 omega____ theta____ kappa____ phi______ frames - -16.9507 -99.0000 120.0000 47 #__ type_ start__ end____ width___ exp.time_ 4 omega 35.00 88.00 1.0000 28.6000 omega____ theta____ kappa____ phi______ frames - 15.8569 178.0000 -120.0000 53 #__ type_ start__ end____ width___ exp.time_ 5 omega -85.00 -49.00 1.0000 28.6000 omega____ theta____ kappa____ phi______ frames - -16.9507 -77.0000 -30.0000 36 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0750795000 _diffrn_orient_matrix_UB_12 0.0062571000 _diffrn_orient_matrix_UB_13 -0.0099777000 _diffrn_orient_matrix_UB_21 0.0081234000 _diffrn_orient_matrix_UB_22 -0.0307687000 _diffrn_orient_matrix_UB_23 -0.0118533000 _diffrn_orient_matrix_UB_31 -0.0262791000 _diffrn_orient_matrix_UB_32 0.0083367000 _diffrn_orient_matrix_UB_33 -0.0362487000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_unetI/netI 0.1725 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19454 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.348 _diffrn_reflns_theta_min 2.958 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 23.751 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.20429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 3.081 _exptl_crystal_description prism _exptl_crystal_F_000 2864 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _refine_diff_density_max 4.591 _refine_diff_density_min -1.908 _refine_diff_density_rms 0.319 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 318 _refine_ls_number_reflns 6330 _refine_ls_number_restraints 37 _refine_ls_restrained_S_all 0.878 _refine_ls_R_factor_all 0.1354 _refine_ls_R_factor_gt 0.0707 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1343 _refine_ls_wR_factor_ref 0.1591 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3025 _reflns_number_total 6330 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 14.res created by SHELXL-2014/7 TITL 170509_lgn_zjl_b172_a.res in P2(1)/c REM Old TITL 170509_LGN_ZJL_B172 in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.177, Rweak 0.012, Alpha 0.095, Orientation as input REM Formula found by SHELXT: C14 N2 S2 Br8 Pb3 rem ISOR 0.01 0.02 C6 C17 C20 rem ISOR 0.002 0.004 C4 C7 C11 C12 C13 C19 CELL 0.71073 8.8791 21.8322 17.9977 90 91.913 90 ZERR 4 0.0004 0.0014 0.001 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N S Br Pb UNIT 80 96 8 8 32 12 DELU 0.01 0.02 C9 C10 SIMU 0.01 0.02 2 C9 C10 ISOR 0.002 0.004 C4 C7 C11 C12 C20 L.S. 60 PLAN 10 TEMP 20(2) BOND $H list 4 fmap 2 acta SHEL 999 0.83 OMIT -6 6 1 OMIT 6 6 5 OMIT -6 1 2 OMIT 6 1 12 OMIT -8 1 6 OMIT -6 6 5 OMIT -2 1 11 OMIT 8 1 4 OMIT 1 3 0 OMIT -6 1 8 OMIT 6 7 0 OMIT 2 4 1 OMIT 2 6 0 OMIT 0 3 6 OMIT 0 1 6 OMIT 0 2 6 OMIT 0 4 6 OMIT 4 0 0 OMIT 0 5 7 OMIT 6 5 0 OMIT -2 5 1 OMIT 0 7 7 OMIT 6 5 1 OMIT 0 0 6 OMIT 0 2 5 OMIT 0 3 3 OMIT 0 4 4 OMIT -4 13 12 OMIT 0 5 6 OMIT 0 2 3 OMIT 0 1 9 OMIT -8 2 1 OMIT 0 1 8 OMIT 0 3 10 OMIT 2 3 1 OMIT 0 7 8 OMIT 0 3 11 OMIT 8 1 0 OMIT 0 9 7 OMIT 6 5 4 OMIT 6 7 4 OMIT 0 4 12 OMIT 0 1 10 REM REM REM WGHT 0.027400 FVAR 0.06872 PB1 6 -0.244911 0.498464 0.999676 11.00000 0.03727 0.04209 = 0.02976 0.00338 0.00206 0.00416 PB2 6 -0.021097 0.582035 0.790039 11.00000 0.03748 0.03502 = 0.03194 0.00170 0.00084 -0.00252 PB3 6 0.480683 0.573135 0.792671 11.00000 0.03762 0.03752 = 0.03123 0.00132 0.00207 -0.00004 BR1 5 -0.489636 0.590725 0.976341 11.00000 0.05691 0.03343 = 0.04847 -0.00584 0.00271 0.00914 BR2 5 -0.221769 0.518442 1.166677 11.00000 0.05047 0.03381 = 0.03426 -0.00224 0.00362 -0.00105 BR3 5 -0.011948 0.596965 0.974691 11.00000 0.05414 0.03937 = 0.03808 -0.00213 0.00443 0.00702 BR4 5 -0.256255 0.480881 0.828917 11.00000 0.04937 0.03583 = 0.03696 -0.00300 0.00169 -0.00256 BR5 5 -0.023461 0.554565 0.638338 11.00000 0.05247 0.03865 = 0.03620 -0.00153 0.00054 -0.00739 BR6 5 0.235440 0.669126 0.774966 11.00000 0.04988 0.02874 = 0.05659 -0.00371 -0.00137 -0.00275 BR7 5 0.472297 0.529688 0.645636 11.00000 0.05091 0.04116 = 0.03605 -0.00096 0.00155 -0.00367 BR8 5 0.712469 0.669710 0.767399 11.00000 0.04556 0.03046 = 0.06486 0.00653 0.00214 -0.00568 S1 4 0.659145 0.581338 0.494514 11.00000 0.03836 0.04370 = 0.05394 0.01308 0.00416 -0.00183 PART 1 N1 3 0.750795 0.688740 0.525796 11.00000 0.01331 0.04705 = 0.03280 0.00828 -0.00281 -0.00629 PART 0 C1 1 0.814810 0.678875 0.456661 11.00000 0.03538 0.02594 = 0.03927 0.00771 0.01194 -0.00292 C2 1 0.898610 0.716785 0.411992 11.00000 0.02808 0.03164 = 0.11287 0.01815 0.02495 0.01222 AFIX 43 H2 2 0.921411 0.756995 0.425194 11.00000 -1.20000 AFIX 0 C3 1 0.944185 0.692057 0.349239 11.00000 0.03691 0.03220 = 0.04053 0.00083 0.00701 -0.01102 AFIX 43 H3 2 1.007231 0.715618 0.320495 11.00000 -1.20000 AFIX 0 C4 1 0.906706 0.634866 0.322917 11.00000 0.03383 0.03380 = 0.03307 0.00058 0.00140 0.00019 AFIX 43 H4 2 0.942824 0.621624 0.277741 11.00000 -1.20000 AFIX 0 C5 1 0.819609 0.598573 0.361451 11.00000 0.02824 0.05458 = 0.05061 -0.01515 -0.00686 -0.00510 AFIX 43 H5 2 0.788997 0.560787 0.342471 11.00000 -1.20000 AFIX 0 C6 1 0.774467 0.617796 0.430839 11.00000 0.05361 0.05771 = 0.02175 0.01249 0.00403 -0.02416 C7 1 0.677956 0.641389 0.546614 11.00000 0.03809 0.03806 = 0.03820 0.00062 0.00188 -0.00096 AFIX 43 H7 2 0.634724 0.641577 0.592973 11.00000 -1.20000 AFIX 0 C8 1 0.782211 0.743913 0.566510 11.00000 0.04930 0.04194 = 0.04477 -0.02367 0.01657 -0.00353 AFIX 23 H8A 2 0.713644 0.747362 0.607145 11.00000 -1.20000 H8B 2 0.766465 0.778991 0.534097 11.00000 -1.20000 AFIX 0 C9 1 0.945837 0.743856 0.597595 11.00000 0.05797 0.09011 = 0.06143 -0.02483 -0.00842 -0.00835 AFIX 23 H9A 2 0.964796 0.706445 0.625437 11.00000 -1.20000 H9B 2 1.014450 0.745001 0.556794 11.00000 -1.20000 AFIX 0 C10 1 0.973125 0.796033 0.645405 11.00000 0.07372 0.09240 = 0.08783 -0.02871 -0.02229 0.00338 AFIX 137 H10A 2 0.950892 0.833003 0.618322 11.00000 -1.50000 H10B 2 1.076877 0.796324 0.662213 11.00000 -1.50000 H10C 2 0.909757 0.793479 0.687481 11.00000 -1.50000 AFIX 0 S2 4 1.193226 0.564670 0.467753 11.00000 0.05259 0.02800 = 0.06413 0.00398 0.00897 -0.00963 N2 3 1.291268 0.633069 0.366633 11.00000 0.03016 0.04679 = 0.03655 0.01551 -0.00540 0.00434 C11 1 1.313178 0.668206 0.437287 11.00000 0.02659 0.02586 = 0.02671 0.00142 0.00060 -0.00001 C12 1 1.373125 0.728064 0.443617 11.00000 0.05288 0.05226 = 0.05261 0.00038 0.00175 -0.00085 AFIX 43 H12 2 1.403513 0.751048 0.403273 11.00000 -1.20000 AFIX 0 C13 1 1.381426 0.748109 0.514068 11.00000 0.09884 0.04567 = 0.06617 0.00515 -0.02318 -0.05426 AFIX 43 H13 2 1.425594 0.786152 0.522928 11.00000 -1.20000 AFIX 0 C14 1 1.329842 0.716801 0.573720 11.00000 0.08195 0.03680 = 0.01417 -0.01084 -0.01043 -0.00006 AFIX 43 H14 2 1.337011 0.734962 0.620446 11.00000 -1.20000 AFIX 0 C15 1 1.266780 0.658527 0.566971 11.00000 0.06301 0.02994 = 0.07887 -0.00609 -0.03647 0.00031 AFIX 43 H15 2 1.229236 0.637655 0.607418 11.00000 -1.20000 AFIX 0 PART 1 C16 1 1.263667 0.633769 0.496249 11.00000 0.04427 0.02444 = 0.04831 -0.00390 -0.00193 0.01190 PART 0 C17 1 1.239805 0.579673 0.381970 11.00000 0.07988 0.01417 = 0.05738 -0.01000 0.00155 -0.01409 AFIX 43 H17 2 1.229077 0.549982 0.345121 11.00000 -1.20000 AFIX 0 C18 1 1.334733 0.655902 0.298525 11.00000 0.06889 0.01881 = 0.05267 0.00669 0.00308 0.00058 AFIX 23 H18A 2 1.312940 0.699431 0.297050 11.00000 -1.20000 H18B 2 1.273244 0.636578 0.259617 11.00000 -1.20000 AFIX 0 C19 1 1.501560 0.646703 0.280629 11.00000 0.04276 0.06804 = 0.04969 0.03338 0.02288 -0.00974 AFIX 23 H19A 2 1.564152 0.668389 0.317161 11.00000 -1.20000 H19B 2 1.526068 0.603487 0.284267 11.00000 -1.20000 AFIX 0 C20 1 1.537198 0.669619 0.203165 11.00000 0.05156 0.04941 = 0.04953 0.00269 0.00573 -0.00104 AFIX 137 H20A 2 1.491873 0.642821 0.166516 11.00000 -1.50000 H20B 2 1.644394 0.670213 0.197793 11.00000 -1.50000 H20C 2 1.497769 0.710255 0.196401 11.00000 -1.50000 AFIX 0 HKLF 4 REM 170509_lgn_zjl_b172_a.res in P2(1)/c REM R1 = 0.0707 for 3025 Fo > 4sig(Fo) and 0.1354 for all 6330 data REM 318 parameters refined using 37 restraints END WGHT 0.0274 0.0000 REM Highest difference peak 4.591, deepest hole -1.908, 1-sigma level 0.319 Q1 1 0.1077 0.5809 0.7924 11.00000 0.05 4.59 Q2 1 0.6079 0.5738 0.7913 11.00000 0.05 4.25 Q3 1 -0.1158 0.4999 0.9985 11.00000 0.05 4.24 Q4 1 -0.3820 0.4995 0.9999 11.00000 0.05 4.00 Q5 1 0.3473 0.5725 0.7974 11.00000 0.05 3.31 Q6 1 -0.1597 0.5807 0.7949 11.00000 0.05 3.06 Q7 1 0.3767 0.6677 0.7683 11.00000 0.05 1.87 Q8 1 0.6003 0.5297 0.6398 11.00000 0.05 1.84 Q9 1 0.1095 0.5528 0.6378 11.00000 0.05 1.76 Q10 1 -0.1133 0.4796 0.8266 11.00000 0.05 1.68 REM The information below was added by Olex2. REM REM R1 = 0.0707 for 3025 Fo > 4sig(Fo) and 0.1354 for all 23364 data REM n/a parameters refined using n/a restraints REM Highest difference peak 4.59, deepest hole -1.91 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1354 REM R1_gt = 0.0707 REM wR_ref = 0.1591 REM GOOF = 0.880 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 23364 REM Reflections_gt = 3025 REM Parameters = n/a REM Hole = -1.91 REM Peak = 4.59 REM Flack = n/a ; _cod_data_source_file d3ce00931a2.cif _cod_data_source_block cmp3 _cod_depositor_comments 'Adding full bibliography for 7247629--7247634.cif.' _cod_database_code 7247633 _chemical_oxdiff_formula 'C H N S Br Pb' _shelx_shelxl_version_number 2014/7 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints C9, C10 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 3. Uiso/Uaniso restraints and constraints C9 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 4.a Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C9(H9A,H9B), C18(H18A,H18B), C19(H19A,H19B) 4.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17) 4.c Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C20(H20A,H20B,H20C) ; _olex2_submission_special_instructions 'No special instructions were received' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.71 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb -0.24491(8) 0.49846(4) 0.99968(4) 0.0364(3) Uani 1 1 d . . . . . Pb2 Pb -0.02110(9) 0.58204(4) 0.79004(5) 0.0348(2) Uani 1 1 d . . . . . Pb3 Pb 0.48068(9) 0.57314(4) 0.79267(5) 0.0354(3) Uani 1 1 d . . . . . Br1 Br -0.4896(3) 0.59073(10) 0.97634(13) 0.0462(6) Uani 1 1 d . . . . . Br2 Br -0.2218(2) 0.51844(10) 1.16668(12) 0.0395(6) Uani 1 1 d . . . . . Br3 Br -0.0119(2) 0.59696(10) 0.97469(12) 0.0438(6) Uani 1 1 d . . . . . Br4 Br -0.2563(2) 0.48088(10) 0.82892(12) 0.0407(6) Uani 1 1 d . . . . . Br5 Br -0.0235(2) 0.55456(10) 0.63834(13) 0.0425(6) Uani 1 1 d . . . . . Br6 Br 0.2354(2) 0.66913(10) 0.77497(13) 0.0451(6) Uani 1 1 d . . . . . Br7 Br 0.4723(2) 0.52969(10) 0.64564(12) 0.0427(6) Uani 1 1 d . . . . . Br8 Br 0.7125(2) 0.66971(10) 0.76740(14) 0.0470(6) Uani 1 1 d . . . . . S1 S 0.6591(6) 0.5813(3) 0.4945(3) 0.0453(15) Uani 1 1 d . . . . . N1 N 0.7508(15) 0.6887(8) 0.5258(9) 0.031(4) Uani 1 1 d . . . A 1 C1 C 0.815(2) 0.6789(9) 0.4567(12) 0.033(5) Uani 1 1 d . . . . . C2 C 0.899(2) 0.7168(11) 0.4120(16) 0.057(8) Uani 1 1 d . . . . . H2 H 0.9214 0.7570 0.4252 0.068 Uiso 1 1 calc R . . . . C3 C 0.944(2) 0.6921(10) 0.3492(12) 0.036(5) Uani 1 1 d . . . . . H3 H 1.0072 0.7156 0.3205 0.044 Uiso 1 1 calc R . . . . C4 C 0.907(2) 0.6349(9) 0.3229(12) 0.034(5) Uani 1 1 d . U . . . H4 H 0.9428 0.6216 0.2777 0.040 Uiso 1 1 calc R . . . . C5 C 0.820(2) 0.5986(11) 0.3615(13) 0.045(6) Uani 1 1 d . . . . . H5 H 0.7890 0.5608 0.3425 0.054 Uiso 1 1 calc R . . . . C6 C 0.774(2) 0.6178(11) 0.4308(12) 0.044(6) Uani 1 1 d . . . . . C7 C 0.678(2) 0.6414(10) 0.5466(12) 0.038(5) Uani 1 1 d . U . . . H7 H 0.6347 0.6416 0.5930 0.046 Uiso 1 1 calc R . . A . C8 C 0.782(2) 0.7439(10) 0.5665(12) 0.045(6) Uani 1 1 d . . . . . H8A H 0.7136 0.7474 0.6071 0.054 Uiso 1 1 calc R . . A . H8B H 0.7665 0.7790 0.5341 0.054 Uiso 1 1 calc R . . A . C9 C 0.946(3) 0.7439(13) 0.5976(15) 0.070(7) Uani 1 1 d . U . . . H9A H 0.9648 0.7064 0.6254 0.084 Uiso 1 1 calc R . . . . H9B H 1.0145 0.7450 0.5568 0.084 Uiso 1 1 calc R . . . . C10 C 0.973(3) 0.7960(13) 0.6454(16) 0.085(8) Uani 1 1 d . U . . . H10A H 0.9509 0.8330 0.6183 0.128 Uiso 1 1 calc GR . . . . H10B H 1.0769 0.7963 0.6622 0.128 Uiso 1 1 calc GR . . . . H10C H 0.9098 0.7935 0.6875 0.128 Uiso 1 1 calc GR . . . . S2 S 1.1932(6) 0.5647(3) 0.4678(4) 0.0481(16) Uani 1 1 d . . . . . N2 N 1.2913(17) 0.6331(8) 0.3666(10) 0.038(5) Uani 1 1 d . . . . . C11 C 1.313(2) 0.6682(9) 0.4373(11) 0.026(4) Uani 1 1 d . U . . . C12 C 1.373(2) 0.7281(11) 0.4436(14) 0.053(6) Uani 1 1 d . U . . . H12 H 1.4035 0.7510 0.4033 0.063 Uiso 1 1 calc R . . . . C13 C 1.381(3) 0.7481(11) 0.5141(15) 0.071(9) Uani 1 1 d . . . . . H13 H 1.4256 0.7862 0.5229 0.085 Uiso 1 1 calc R . . . . C14 C 1.330(3) 0.7168(10) 0.5737(11) 0.045(6) Uani 1 1 d . . . . . H14 H 1.3370 0.7350 0.6204 0.053 Uiso 1 1 calc R . . . . C15 C 1.267(2) 0.6585(10) 0.5670(15) 0.058(8) Uani 1 1 d . . . . . H15 H 1.2292 0.6377 0.6074 0.070 Uiso 1 1 calc R . . B . C16 C 1.264(2) 0.6338(9) 0.4962(13) 0.039(6) Uani 1 1 d . . . C 1 C17 C 1.240(3) 0.5797(10) 0.3820(13) 0.050(7) Uani 1 1 d . . . . . H17 H 1.2291 0.5500 0.3451 0.061 Uiso 1 1 calc R . . . . C18 C 1.335(2) 0.6559(9) 0.2985(13) 0.047(6) Uani 1 1 d . . . . . H18A H 1.3129 0.6994 0.2970 0.056 Uiso 1 1 calc R . . . . H18B H 1.2732 0.6366 0.2596 0.056 Uiso 1 1 calc R . . . . C19 C 1.502(2) 0.6467(12) 0.2806(12) 0.053(7) Uani 1 1 d . . . . . H19A H 1.5642 0.6684 0.3172 0.064 Uiso 1 1 calc R . . . . H19B H 1.5261 0.6035 0.2843 0.064 Uiso 1 1 calc R . . . . C20 C 1.537(2) 0.6696(10) 0.2032(12) 0.050(6) Uani 1 1 d . U . . . H20A H 1.4919 0.6428 0.1665 0.075 Uiso 1 1 calc GR . . . . H20B H 1.6444 0.6702 0.1978 0.075 Uiso 1 1 calc GR . . . . H20C H 1.4978 0.7103 0.1964 0.075 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0373(5) 0.0421(6) 0.0298(5) 0.0034(4) 0.0021(4) 0.0042(4) Pb2 0.0375(5) 0.0350(5) 0.0319(5) 0.0017(4) 0.0008(4) -0.0025(4) Pb3 0.0376(5) 0.0375(5) 0.0312(5) 0.0013(4) 0.0021(4) 0.0000(4) Br1 0.0569(15) 0.0334(14) 0.0485(15) -0.0058(11) 0.0027(12) 0.0091(11) Br2 0.0505(13) 0.0338(13) 0.0343(13) -0.0022(10) 0.0036(10) -0.0011(11) Br3 0.0541(14) 0.0394(14) 0.0381(14) -0.0021(11) 0.0044(11) 0.0070(11) Br4 0.0494(13) 0.0358(13) 0.0370(13) -0.0030(11) 0.0017(11) -0.0026(11) Br5 0.0525(14) 0.0386(13) 0.0362(13) -0.0015(11) 0.0005(11) -0.0074(11) Br6 0.0499(14) 0.0287(13) 0.0566(16) -0.0037(11) -0.0014(12) -0.0027(11) Br7 0.0509(14) 0.0412(14) 0.0361(13) -0.0010(11) 0.0015(11) -0.0037(11) Br8 0.0456(14) 0.0305(13) 0.0649(17) 0.0065(12) 0.0021(12) -0.0057(11) S1 0.038(3) 0.044(4) 0.054(4) 0.013(3) 0.004(3) -0.002(3) N1 0.013(8) 0.047(12) 0.033(11) 0.008(9) -0.003(7) -0.006(8) C1 0.035(12) 0.026(12) 0.039(13) 0.008(10) 0.012(10) -0.003(10) C2 0.028(12) 0.032(14) 0.11(2) 0.018(15) 0.025(14) 0.012(11) C3 0.037(12) 0.032(13) 0.041(14) 0.001(11) 0.007(11) -0.011(10) C4 0.034(5) 0.034(5) 0.033(5) 0.001(2) 0.001(2) 0.000(2) C5 0.028(12) 0.055(16) 0.051(16) -0.015(13) -0.007(11) -0.005(11) C6 0.054(15) 0.058(17) 0.022(12) 0.012(12) 0.004(11) -0.024(12) C7 0.038(6) 0.038(6) 0.038(6) 0.001(2) 0.002(2) -0.001(2) C8 0.049(14) 0.042(15) 0.045(15) -0.024(12) 0.017(12) -0.004(12) C9 0.058(14) 0.090(19) 0.061(16) -0.025(13) -0.008(13) -0.008(14) C10 0.074(15) 0.09(2) 0.088(18) -0.029(14) -0.022(14) 0.003(15) S2 0.053(4) 0.028(3) 0.064(4) 0.004(3) 0.009(3) -0.010(3) N2 0.030(10) 0.047(12) 0.037(11) 0.016(10) -0.005(9) 0.004(9) C11 0.027(5) 0.026(5) 0.027(5) 0.001(2) 0.001(2) 0.000(2) C12 0.053(7) 0.052(7) 0.053(7) 0.000(2) 0.002(2) -0.001(2) C13 0.10(2) 0.046(17) 0.07(2) 0.005(15) -0.023(16) -0.054(15) C14 0.082(18) 0.037(14) 0.014(12) -0.011(11) -0.010(12) 0.000(13) C15 0.063(16) 0.030(15) 0.08(2) -0.006(14) -0.036(15) 0.000(12) C16 0.044(13) 0.024(12) 0.048(15) -0.004(11) -0.002(12) 0.012(11) C17 0.080(18) 0.014(12) 0.057(17) -0.010(12) 0.002(14) -0.014(12) C18 0.069(16) 0.019(12) 0.053(16) 0.007(12) 0.003(13) 0.001(12) C19 0.043(14) 0.068(18) 0.050(16) 0.033(13) 0.023(11) -0.010(13) C20 0.052(7) 0.049(7) 0.050(7) 0.003(4) 0.006(4) -0.001(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Pb1 Br1 83.69(7) . 3_467 ? Br1 Pb1 Br2 93.86(7) . . ? Br1 Pb1 Br3 179.41(7) . 3_567 ? Br1 Pb1 Br3 89.86(7) . . ? Br1 Pb1 Br3 96.65(6) 3_467 3_567 ? Br1 Pb1 Br4 86.82(6) . . ? Br2 Pb1 Br1 88.80(6) . 3_467 ? Br2 Pb1 Br3 85.67(6) . 3_567 ? Br2 Pb1 Br4 177.68(7) . . ? Br3 Pb1 Br1 173.53(6) . 3_467 ? Br3 Pb1 Br2 91.20(6) . . ? Br3 Pb1 Br3 89.81(6) . 3_567 ? Br3 Pb1 Br4 86.58(6) . . ? Br4 Pb1 Br1 93.48(6) . 3_467 ? Br4 Pb1 Br3 93.64(6) . 3_567 ? Br4 Pb2 Br2 84.83(6) . 3_567 ? Br5 Pb2 Br2 94.29(7) . 3_567 ? Br5 Pb2 Br4 94.79(7) . . ? Br5 Pb2 Br6 91.65(7) . . ? Br5 Pb2 Br8 91.35(7) . 1_455 ? Br6 Pb2 Br2 87.02(6) . 3_567 ? Br6 Pb2 Br4 169.96(6) . . ? Br6 Pb2 Br8 100.27(6) . 1_455 ? Br8 Pb2 Br2 170.66(7) 1_455 3_567 ? Br8 Pb2 Br4 87.29(6) 1_455 . ? Br4 Pb3 Br2 95.07(6) 1_655 3_567 ? Br6 Pb3 Br2 86.33(6) . 3_567 ? Br6 Pb3 Br4 173.34(7) . 1_655 ? Br7 Pb3 Br2 90.45(6) . 3_567 ? Br7 Pb3 Br4 88.58(7) . 1_655 ? Br7 Pb3 Br6 97.93(7) . . ? Br7 Pb3 Br8 95.25(7) . . ? Br8 Pb3 Br2 173.38(7) . 3_567 ? Br8 Pb3 Br4 88.45(6) . 1_655 ? Br8 Pb3 Br6 89.55(6) . . ? Pb1 Br1 Pb1 96.31(7) . 3_467 ? Pb1 Br2 Pb2 99.65(7) . 3_567 ? Pb1 Br2 Pb3 96.48(6) . 3_567 ? Pb3 Br2 Pb2 89.97(6) 3_567 3_567 ? Pb1 Br3 Pb1 90.20(6) . 3_567 ? Pb1 Br4 Pb2 97.73(6) . . ? Pb1 Br4 Pb3 97.25(7) . 1_455 ? Pb2 Br4 Pb3 89.89(6) . 1_455 ? Pb2 Br6 Pb3 95.61(7) . . ? Pb3 Br8 Pb2 94.11(7) . 1_655 ? C7 S1 C6 87.7(11) . . ? C1 N1 C8 120.4(17) . . ? C7 N1 C1 111.0(19) . . ? C7 N1 C8 128.3(19) . . ? N1 C1 C6 108.8(17) . . ? C2 C1 N1 132(2) . . ? C2 C1 C6 120(2) . . ? C1 C2 H2 122.1 . . ? C3 C2 C1 116(2) . . ? C3 C2 H2 122.1 . . ? C2 C3 H3 117.0 . . ? C2 C3 C4 126(2) . . ? C4 C3 H3 117.0 . . ? C3 C4 H4 119.9 . . ? C5 C4 C3 120(2) . . ? C5 C4 H4 119.9 . . ? C4 C5 H5 120.6 . . ? C4 C5 C6 119(2) . . ? C6 C5 H5 120.6 . . ? C1 C6 S1 110.5(16) . . ? C5 C6 S1 130.0(19) . . ? C5 C6 C1 119(2) . . ? S1 C7 H7 119.1 . . ? N1 C7 S1 121.8(18) . . ? N1 C7 H7 119.1 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 C9 110.5(17) . . ? H8A C8 H8B 108.1 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C10 C9 C8 111(2) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C17 S2 C16 90.3(11) . . ? C17 N2 C11 108.7(18) . . ? C17 N2 C18 129(2) . . ? C18 N2 C11 122.3(18) . . ? C12 C11 N2 125.6(19) . . ? C16 C11 N2 109.8(17) . . ? C16 C11 C12 125(2) . . ? C11 C12 H12 123.6 . . ? C13 C12 C11 113(2) . . ? C13 C12 H12 123.6 . . ? C12 C13 H13 117.6 . . ? C12 C13 C14 125(2) . . ? C14 C13 H13 117.6 . . ? C13 C14 H14 118.9 . . ? C13 C14 C15 122(2) . . ? C15 C14 H14 118.9 . . ? C14 C15 H15 122.2 . . ? C16 C15 C14 116(2) . . ? C16 C15 H15 122.2 . . ? C11 C16 S2 111.9(16) . . ? C15 C16 S2 128.2(19) . . ? C15 C16 C11 120(2) . . ? S2 C17 H17 120.5 . . ? N2 C17 S2 119.0(18) . . ? N2 C17 H17 120.5 . . ? N2 C18 H18A 108.3 . . ? N2 C18 H18B 108.3 . . ? N2 C18 C19 115.8(17) . . ? H18A C18 H18B 107.4 . . ? C19 C18 H18A 108.3 . . ? C19 C18 H18B 108.3 . . ? C18 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C20 C19 C18 112.3(18) . . ? C20 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 Br1 2.982(2) . ? Pb1 Br1 3.099(3) 3_467 ? Pb1 Br2 3.037(2) . ? Pb1 Br3 3.028(2) . ? Pb1 Br3 3.112(2) 3_567 ? Pb1 Br4 3.095(2) . ? Pb2 Br2 3.155(2) 3_567 ? Pb2 Br4 3.134(2) . ? Pb2 Br5 2.795(2) . ? Pb2 Br6 2.986(2) . ? Pb2 Br8 3.060(2) 1_455 ? Pb3 Br2 3.151(2) 3_567 ? Pb3 Br4 3.136(2) 1_655 ? Pb3 Br6 3.031(2) . ? Pb3 Br7 2.810(2) . ? Pb3 Br8 2.992(2) . ? Br1 Pb1 3.099(2) 3_467 ? Br2 Pb2 3.155(2) 3_567 ? Br2 Pb3 3.151(2) 3_567 ? Br3 Pb1 3.112(2) 3_567 ? Br4 Pb3 3.136(2) 1_455 ? Br8 Pb2 3.060(2) 1_655 ? S1 C6 1.75(2) . ? S1 C7 1.62(2) . ? N1 C1 1.40(2) . ? N1 C7 1.28(2) . ? N1 C8 1.43(2) . ? C1 C2 1.39(3) . ? C1 C6 1.45(3) . ? C2 H2 0.9300 . ? C2 C3 1.33(3) . ? C3 H3 0.9300 . ? C3 C4 1.37(3) . ? C4 H4 0.9300 . ? C4 C5 1.32(3) . ? C5 H5 0.9300 . ? C5 C6 1.39(3) . ? C7 H7 0.9300 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.54(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.44(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? S2 C16 1.71(2) . ? S2 C17 1.64(2) . ? N2 C11 1.49(2) . ? N2 C17 1.29(2) . ? N2 C18 1.39(3) . ? C11 C12 1.41(3) . ? C11 C16 1.38(3) . ? C12 H12 0.9300 . ? C12 C13 1.34(3) . ? C13 H13 0.9300 . ? C13 C14 1.36(3) . ? C14 H14 0.9300 . ? C14 C15 1.39(3) . ? C15 H15 0.9300 . ? C15 C16 1.38(3) . ? C17 H17 0.9300 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C19 1.54(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.52(3) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ?