#------------------------------------------------------------------------------ #$Date: 2024-01-06 09:57:03 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288789 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247629.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_7247629 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 'Br3 Pb, C8 H8 N S' _chemical_formula_sum 'C8 H8 Br3 N Pb S' _chemical_formula_weight 597.13 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _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 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.7383(4) _cell_length_b 11.5787(7) _cell_length_c 14.7269(12) _cell_measurement_reflns_used 1992 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.5100 _cell_measurement_theta_min 3.2240 _cell_volume 1319.52(15) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _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 'SIR2004 (Burla et al., 2007)' _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 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 35.00 88.00 1.00 20.00 -- 15.86 178.00 90.00 53 2 \w 41.00 88.00 1.00 20.00 -- 15.86 178.00 -90.00 47 3 \w 35.00 80.00 1.00 20.00 -- 15.86 178.00-180.00 45 4 \w -24.00 13.00 1.00 20.00 -- -16.95 -99.00 -90.00 37 5 \w 15.00 55.00 1.00 20.00 -- 15.70 -99.00 30.00 40 6 \w -11.00 42.00 1.00 20.00 -- 15.70 77.00-180.00 53 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0766429000 _diffrn_orient_matrix_UB_12 -0.0300414000 _diffrn_orient_matrix_UB_13 0.0119650000 _diffrn_orient_matrix_UB_21 0.0443052000 _diffrn_orient_matrix_UB_22 0.0267179000 _diffrn_orient_matrix_UB_23 -0.0366035000 _diffrn_orient_matrix_UB_31 0.0239828000 _diffrn_orient_matrix_UB_32 0.0462200000 _diffrn_orient_matrix_UB_33 0.0288766000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_unetI/netI 0.1140 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 6548 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.338 _diffrn_reflns_theta_min 3.166 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 21.992 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.09374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 3.006 _exptl_crystal_description prism _exptl_crystal_F_000 1064 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _refine_diff_density_max 4.290 _refine_diff_density_min -1.914 _refine_diff_density_rms 0.280 _refine_ls_abs_structure_details ; Flack x determined using 468 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.012(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 2397 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 0.914 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0491 _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^)+(0.0394P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1027 _refine_ls_wR_factor_ref 0.1111 _reflns_Friedel_coverage 0.715 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 1541 _reflns_number_total 2397 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 19.res created by SHELXL-2014/7 TITL 170508_lgn_zjlb175_a.res in P2(1)2(1)2(1) REM Old TITL 170508_lgn_zjlb175_b.res in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.124, Rweak 0.017, Alpha 0.018, Orientation as input REM Flack x = 0.028 ( 0.020 ) from Parsons' quotients REM Formula found by SHELXT: Br3 Pb S C1 N CELL 0.71073 7.7383 11.5787 14.7269 90 90 90 ZERR 4 0.0004 0.0007 0.0012 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC Br Pb S C N H UNIT 12 4 4 32 4 32 ISOR 0.02 0.04 C4 ISOR 0.002 0.004 C2 L.S. 50 PLAN 20 TEMP 20(2) BOND $H list 4 fmap 2 acta SHEL 999 0.83 OMIT 0 2 1 OMIT 0 3 6 OMIT 0 2 5 OMIT 0 6 1 OMIT 0 3 4 OMIT 0 8 7 OMIT 6 2 1 OMIT 4 0 0 REM REM REM WGHT 0.039400 FVAR 0.21161 PB1 2 0.075945 0.750306 0.501125 11.00000 0.02661 0.03116 = 0.03883 -0.00304 0.00055 -0.00130 BR1 1 0.308029 0.688107 0.349335 11.00000 0.05298 0.04444 = 0.03086 -0.00497 0.00009 -0.00006 BR2 1 0.305815 0.610017 0.618623 11.00000 0.05498 0.04158 = 0.04175 0.00595 -0.00590 -0.00353 BR3 1 -0.152474 0.551984 0.463799 11.00000 0.03938 0.02949 = 0.05796 -0.00820 -0.00364 -0.00174 S1 3 0.988491 0.747865 0.175551 11.00000 0.04811 0.09846 = 0.08221 -0.02812 -0.00629 0.00628 N1 5 0.753353 0.603650 0.199812 11.00000 0.06175 0.07228 = 0.04791 -0.00322 0.00376 0.01621 C1 4 0.676451 0.684955 0.151984 11.00000 0.07405 0.01350 = 0.02971 -0.00323 -0.00703 0.02183 C2 4 0.504317 0.690643 0.124523 11.00000 0.04390 0.04326 = 0.04345 -0.00049 0.00072 -0.00012 AFIX 43 H2 6 0.427482 0.630759 0.136402 11.00000 -1.20000 AFIX 0 C3 4 0.452354 0.789617 0.078629 11.00000 0.04923 0.05019 = 0.03527 -0.01183 -0.01011 -0.00795 AFIX 43 H3 6 0.338849 0.792859 0.058031 11.00000 -1.20000 AFIX 0 C4 4 0.550696 0.877390 0.062593 11.00000 0.08431 0.05452 = 0.07249 0.01045 0.00904 0.00989 AFIX 43 H4 6 0.505649 0.944269 0.036850 11.00000 -1.20000 AFIX 0 C5 4 0.730560 0.869889 0.085188 11.00000 0.07055 0.03306 = 0.07267 -0.00588 0.02926 -0.02957 AFIX 43 H5 6 0.807296 0.927210 0.066994 11.00000 -1.20000 AFIX 0 C6 4 0.788113 0.775104 0.134906 11.00000 0.04675 0.03040 = 0.05918 -0.00839 0.00719 -0.00041 C7 4 0.914974 0.618189 0.218009 11.00000 0.08184 0.05379 = 0.03670 0.00906 0.00110 0.03492 AFIX 43 H7 6 0.982798 0.565656 0.249818 11.00000 -1.20000 AFIX 0 C8 4 0.667141 0.491522 0.228836 11.00000 0.10011 0.03228 = 0.09417 -0.02227 -0.01083 0.00593 AFIX 137 H8A 6 0.752411 0.440274 0.253702 11.00000 -1.50000 H8B 6 0.613620 0.455876 0.177135 11.00000 -1.50000 H8C 6 0.580978 0.507642 0.273990 11.00000 -1.50000 AFIX 0 HKLF 4 REM 170508_lgn_zjlb175_a.res in P2(1)2(1)2(1) REM R1 = 0.0491 for 1541 Fo > 4sig(Fo) and 0.0852 for all 2397 data REM 128 parameters refined using 12 restraints END WGHT 0.0390 0.0000 REM Highest difference peak 4.290, deepest hole -1.914, 1-sigma level 0.280 Q1 1 -0.0634 0.7510 0.5013 11.00000 0.05 4.29 Q2 1 0.2071 0.7496 0.5023 11.00000 0.05 3.93 Q3 1 -0.0179 0.5549 0.4665 11.00000 0.05 1.72 Q4 1 0.4394 0.6104 0.6177 11.00000 0.05 1.65 Q5 1 0.1833 0.6125 0.6167 11.00000 0.05 1.51 Q6 1 -0.2996 0.5564 0.4641 11.00000 0.05 1.45 Q7 1 0.1754 0.6956 0.3534 11.00000 0.05 1.40 Q8 1 0.4476 0.6895 0.3547 11.00000 0.05 1.37 Q9 1 0.5415 1.0536 0.0063 11.00000 0.05 1.01 Q10 1 0.3131 0.7384 0.3214 11.00000 0.05 0.85 Q11 1 0.8402 1.0621 0.0105 11.00000 0.05 0.83 Q12 1 -0.1531 0.5973 0.4308 11.00000 0.05 0.78 Q13 1 0.4038 1.0216 -0.0188 11.00000 0.05 0.77 Q14 1 0.0786 0.8054 0.5468 11.00000 0.05 0.74 Q15 1 -0.1592 0.5118 0.4504 11.00000 0.05 0.70 Q16 1 -0.0841 0.4963 0.5237 11.00000 0.05 0.68 Q17 1 0.0726 0.7056 0.5537 11.00000 0.05 0.66 Q18 1 0.3115 0.5573 0.6071 11.00000 0.05 0.65 Q19 1 0.9787 0.9583 0.0686 11.00000 0.05 0.64 Q20 1 -0.1380 0.5969 0.4953 11.00000 0.05 0.64 REM The information below was added by Olex2. REM REM R1 = 0.0491 for 1541 Fo > 4sig(Fo) and 0.0852 for all 7638 data REM n/a parameters refined using n/a restraints REM Highest difference peak 4.29, deepest hole -1.91 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0852 REM R1_gt = 0.0491 REM wR_ref = 0.1111 REM GOOF = 0.916 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 7638 REM Reflections_gt = 1541 REM Parameters = n/a REM Hole = -1.91 REM Peak = 4.29 REM Flack = -0.012(19) ; _cod_data_source_file d3ce00931a2.cif _cod_data_source_block cmp1 _cod_depositor_comments 'Adding full bibliography for 7247629--7247634.cif.' _cod_database_code 7247629 _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 At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(C2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C7(H7) 3.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 6.163 _oxdiff_exptl_absorpt_empirical_full_min 0.451 _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 99.62 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 0.07595(11) 0.75031(12) 0.50113(8) 0.0322(3) Uani 1 1 d . . . . . Br1 Br 0.3080(5) 0.6881(2) 0.34934(16) 0.0428(8) Uani 1 1 d . . . . . Br2 Br 0.3058(5) 0.6100(2) 0.61862(18) 0.0461(8) Uani 1 1 d . . . . . Br3 Br -0.1525(4) 0.5520(2) 0.46380(19) 0.0423(7) Uani 1 1 d . . . . . S1 S 0.9885(12) 0.7479(12) 0.1756(6) 0.076(3) Uani 1 1 d . . . . . N1 N 0.753(4) 0.604(3) 0.1998(18) 0.061(8) Uani 1 1 d . . . . . C1 C 0.676(5) 0.685(2) 0.1520(16) 0.039(7) Uani 1 1 d . . . . . C2 C 0.504(4) 0.691(3) 0.1245(19) 0.044(8) Uani 1 1 d . U . . . H2 H 0.4275 0.6308 0.1364 0.052 Uiso 1 1 calc R . . . . C3 C 0.452(4) 0.790(3) 0.0786(19) 0.045(8) Uani 1 1 d . . . . . H3 H 0.3388 0.7929 0.0580 0.054 Uiso 1 1 calc R . . . . C4 C 0.551(5) 0.877(3) 0.063(2) 0.070(11) Uani 1 1 d . U . . . H4 H 0.5056 0.9443 0.0368 0.085 Uiso 1 1 calc R . . . . C5 C 0.731(5) 0.870(3) 0.085(2) 0.059(10) Uani 1 1 d . . . . . H5 H 0.8073 0.9272 0.0670 0.071 Uiso 1 1 calc R . . . . C6 C 0.788(4) 0.775(2) 0.1349(19) 0.045(8) Uani 1 1 d . . . . . C7 C 0.915(5) 0.618(3) 0.218(2) 0.057(10) Uani 1 1 d . . . . . H7 H 0.9828 0.5657 0.2498 0.069 Uiso 1 1 calc R . . . . C8 C 0.667(5) 0.492(2) 0.229(2) 0.076(11) Uani 1 1 d . . . . . H8A H 0.7524 0.4403 0.2537 0.113 Uiso 1 1 calc GR . . . . H8B H 0.6136 0.4559 0.1771 0.113 Uiso 1 1 calc GR . . . . H8C H 0.5810 0.5076 0.2740 0.113 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 0.0266(4) 0.0312(5) 0.0388(5) -0.0030(6) 0.0006(5) -0.0013(5) Br1 0.053(2) 0.0444(16) 0.0309(14) -0.0050(13) 0.0001(16) -0.0001(17) Br2 0.055(2) 0.0416(16) 0.0418(15) 0.0060(13) -0.0059(18) -0.0035(16) Br3 0.0394(16) 0.0295(14) 0.0580(17) -0.0082(13) -0.0036(15) -0.0017(15) S1 0.048(5) 0.098(7) 0.082(6) -0.028(8) -0.006(5) 0.006(7) N1 0.06(2) 0.07(2) 0.048(16) -0.003(15) 0.004(16) 0.016(18) C1 0.07(2) 0.013(13) 0.030(14) -0.003(11) -0.007(18) 0.022(17) C2 0.044(8) 0.043(8) 0.043(8) 0.000(3) 0.001(3) 0.000(3) C3 0.05(2) 0.05(2) 0.035(15) -0.012(14) -0.010(14) -0.008(15) C4 0.08(2) 0.055(18) 0.07(2) 0.010(17) 0.009(18) 0.010(18) C5 0.07(3) 0.033(17) 0.07(2) -0.006(16) 0.03(2) -0.030(17) C6 0.047(19) 0.030(18) 0.059(18) -0.008(13) 0.007(16) 0.000(15) C7 0.08(3) 0.05(2) 0.037(19) 0.009(17) 0.00(2) 0.03(2) C8 0.10(3) 0.032(18) 0.09(2) -0.022(18) -0.01(3) 0.01(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 175.56(11) . 4_466 ? Br1 Pb1 Br2 80.65(8) 4_466 4_466 ? Br1 Pb1 Br2 86.76(9) . . ? Br1 Pb1 Br2 95.97(9) . 4_466 ? Br1 Pb1 Br3 99.33(8) 4_466 4_566 ? Br1 Pb1 Br3 84.02(8) . 4_566 ? Br2 Pb1 Br1 96.45(9) . 4_466 ? Br2 Pb1 Br2 175.68(11) . 4_466 ? Br2 Pb1 Br3 84.39(8) . 4_566 ? Br3 Pb1 Br1 84.89(8) . 4_466 ? Br3 Pb1 Br1 91.92(9) . . ? Br3 Pb1 Br2 92.39(9) . . ? Br3 Pb1 Br2 84.18(8) . 4_466 ? Br3 Pb1 Br2 99.21(8) 4_566 4_466 ? Br3 Pb1 Br3 174.94(9) . 4_566 ? Pb1 Br1 Pb1 79.25(6) . 4_566 ? Pb1 Br2 Pb1 77.99(6) . 4_566 ? Pb1 Br3 Pb1 78.67(6) . 4_466 ? C6 S1 C7 89.3(17) . . ? C1 N1 C8 124(3) . . ? C7 N1 C1 117(4) . . ? C7 N1 C8 119(3) . . ? N1 C1 C2 128(3) . . ? N1 C1 C6 111(3) . . ? C6 C1 C2 121(3) . . ? C1 C2 H2 121.4 . . ? C3 C2 C1 117(3) . . ? C3 C2 H2 121.4 . . ? C2 C3 H3 117.7 . . ? C4 C3 C2 125(3) . . ? C4 C3 H3 117.7 . . ? C3 C4 H4 120.6 . . ? C3 C4 C5 119(3) . . ? C5 C4 H4 120.6 . . ? C4 C5 H5 120.6 . . ? C6 C5 C4 119(3) . . ? C6 C5 H5 120.6 . . ? C1 C6 S1 112(2) . . ? C1 C6 C5 119(3) . . ? C5 C6 S1 129(2) . . ? S1 C7 H7 124.5 . . ? N1 C7 S1 111(3) . . ? N1 C7 H7 124.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 2.957(3) . ? Pb1 Br1 3.107(3) 4_466 ? Pb1 Br2 3.177(3) 4_466 ? Pb1 Br2 2.966(3) . ? Pb1 Br3 3.150(3) 4_566 ? Pb1 Br3 2.950(3) . ? Br1 Pb1 3.108(3) 4_566 ? Br2 Pb1 3.177(3) 4_566 ? Br3 Pb1 3.150(3) 4_466 ? S1 C6 1.69(3) . ? S1 C7 1.72(4) . ? N1 C1 1.32(4) . ? N1 C7 1.29(4) . ? N1 C8 1.52(4) . ? C1 C2 1.39(4) . ? C1 C6 1.38(4) . ? C2 H2 0.9300 . ? C2 C3 1.39(4) . ? C3 H3 0.9300 . ? C3 C4 1.29(4) . ? C4 H4 0.9300 . ? C4 C5 1.43(4) . ? C5 H5 0.9300 . ? C5 C6 1.39(4) . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ?