#------------------------------------------------------------------------------ #$Date: 2024-01-06 09:57:03 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288789 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247634.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_7247634 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, C21 H22 P' _chemical_formula_sum 'C21 H22 Br3 P Pb' _chemical_formula_weight 752.27 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 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 95.977(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.3422(12) _cell_length_b 8.1688(8) _cell_length_c 21.4738(18) _cell_measurement_reflns_used 2575 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.1050 _cell_measurement_theta_min 3.5630 _cell_volume 2327.7(4) _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 '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 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -3.00 85.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 37.0000 90.0000 88 #__ type_ start__ end____ width___ exp.time_ 2 omega -51.00 33.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 -57.0000 -90.0000 84 #__ type_ start__ end____ width___ exp.time_ 3 omega -25.00 22.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -16.9507 -99.0000 60.0000 47 #__ type_ start__ end____ width___ exp.time_ 4 omega 35.00 88.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 178.0000 150.0000 53 #__ type_ start__ end____ width___ exp.time_ 5 omega -85.00 -34.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -16.9507 -77.0000 -120.0000 51 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0071618000 _diffrn_orient_matrix_UB_12 -0.0803502000 _diffrn_orient_matrix_UB_13 0.0121553000 _diffrn_orient_matrix_UB_21 0.0076357000 _diffrn_orient_matrix_UB_22 -0.0290629000 _diffrn_orient_matrix_UB_23 -0.0302831000 _diffrn_orient_matrix_UB_31 0.0524103000 _diffrn_orient_matrix_UB_32 0.0152277000 _diffrn_orient_matrix_UB_33 0.0062869000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_unetI/netI 0.0610 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 13335 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.349 _diffrn_reflns_theta_min 3.070 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 12.470 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.21804 _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 yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.147 _exptl_crystal_description prism _exptl_crystal_F_000 1400 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.388 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.129 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 4248 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 0.979 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0370 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0175P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.0673 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2906 _reflns_number_total 4248 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 14.res created by SHELXL-2014/7 TITL 170329_lgn_zjl_b90_a.res in P2(1)/n REM Old TITL 170329_LGN_ZJL_B90 in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.120, Rweak 0.095, Alpha 0.099, Orientation as input REM Formula found by SHELXT: C20 Br3 P Pb CELL 0.71073 13.3422 8.1688 21.4738 90 95.977 90 ZERR 4 0.0012 0.0008 0.0018 0 0.008 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Br P Pb UNIT 84 88 12 4 4 ISOR 0.02 0.04 C20 L.S. 30 PLAN 20 SIZE 0.08 0.15 0.38 TEMP 20(2) BOND $H list 4 fmap 2 acta SHEL 999 0.83 REM REM REM WGHT 0.017500 FVAR 0.22833 PB1 5 0.751971 0.794395 0.751956 11.00000 0.04459 0.04816 = 0.04080 0.00089 0.00458 0.00031 BR1 3 0.879007 1.021936 0.689157 11.00000 0.05225 0.06828 = 0.06672 0.00852 0.02307 -0.00051 BR2 3 0.722755 0.605556 0.640916 11.00000 0.06633 0.08226 = 0.04151 -0.00868 0.00232 0.00299 BR3 3 0.576972 1.001191 0.719804 11.00000 0.04542 0.08922 = 0.06607 0.01136 -0.00042 0.01061 P1 4 0.220036 0.130331 0.564022 11.00000 0.04855 0.04706 = 0.03589 -0.00090 0.00996 0.00095 C1 1 0.314908 0.280140 0.583059 11.00000 0.03881 0.04126 = 0.04291 0.00375 0.00653 0.00195 C2 1 0.368303 0.297052 0.640762 11.00000 0.07426 0.06342 = 0.06001 0.00280 -0.00190 -0.00297 AFIX 43 H2 2 0.356598 0.224248 0.672505 11.00000 -1.20000 AFIX 0 C3 1 0.438275 0.418089 0.652857 11.00000 0.06460 0.07969 = 0.08902 -0.01676 -0.02465 0.01030 AFIX 43 H3 2 0.473920 0.427404 0.692284 11.00000 -1.20000 AFIX 0 C4 1 0.455339 0.526341 0.605771 11.00000 0.04165 0.05285 = 0.16936 -0.01916 0.02903 -0.00612 AFIX 43 H4 2 0.502573 0.609606 0.613345 11.00000 -1.20000 AFIX 0 C5 1 0.402945 0.511013 0.548273 11.00000 0.07134 0.06809 = 0.09684 0.00660 0.02822 -0.00299 AFIX 43 H5 2 0.414262 0.584387 0.516638 11.00000 -1.20000 AFIX 0 C6 1 0.333609 0.388218 0.536640 11.00000 0.05948 0.05646 = 0.06212 0.00038 0.00955 -0.01443 AFIX 43 H6 2 0.298896 0.377927 0.496975 11.00000 -1.20000 AFIX 0 C7 1 0.223023 -0.024967 0.623575 11.00000 0.05566 0.04757 = 0.04131 -0.00171 0.01472 0.00160 C8 1 0.133214 -0.084274 0.641617 11.00000 0.06721 0.05431 = 0.05206 -0.00466 0.00916 -0.00435 AFIX 43 H8 2 0.072191 -0.037190 0.626141 11.00000 -1.20000 AFIX 0 C9 1 0.135420 -0.216230 0.683519 11.00000 0.11065 0.07135 = 0.05787 0.00483 0.03531 -0.01288 AFIX 43 H9 2 0.075498 -0.258222 0.695433 11.00000 -1.20000 AFIX 0 C10 1 0.226049 -0.283736 0.707051 11.00000 0.14507 0.05853 = 0.06818 0.02322 0.03884 0.02393 AFIX 43 H10 2 0.226954 -0.372461 0.734242 11.00000 -1.20000 AFIX 0 C11 1 0.315336 -0.220933 0.690649 11.00000 0.11822 0.07349 = 0.06811 0.01337 0.03308 0.02594 AFIX 43 H11 2 0.376362 -0.264858 0.707799 11.00000 -1.20000 AFIX 0 C12 1 0.314250 -0.092371 0.648617 11.00000 0.07628 0.06026 = 0.05457 0.00590 0.02763 0.00978 AFIX 43 H12 2 0.374562 -0.050944 0.637084 11.00000 -1.20000 AFIX 0 C13 1 0.100378 0.230285 0.558348 11.00000 0.04740 0.04226 = 0.03801 -0.00096 0.00529 -0.00556 C14 1 0.035459 0.228754 0.504174 11.00000 0.05464 0.05114 = 0.05703 -0.00443 0.01153 -0.00780 AFIX 43 H14 2 0.053924 0.175673 0.468794 11.00000 -1.20000 AFIX 0 C15 1 -0.057745 0.306326 0.502105 11.00000 0.04990 0.05631 = 0.06861 -0.00323 -0.00935 -0.00766 AFIX 43 H15 2 -0.101599 0.306158 0.465486 11.00000 -1.20000 AFIX 0 C16 1 -0.083813 0.382707 0.554685 11.00000 0.04900 0.05287 = 0.09217 0.00416 0.02543 -0.00076 AFIX 43 H16 2 -0.146301 0.433572 0.553832 11.00000 -1.20000 AFIX 0 C17 1 -0.020346 0.385430 0.607742 11.00000 0.07583 0.05280 = 0.06638 -0.00294 0.02633 0.00961 AFIX 43 H17 2 -0.039127 0.439206 0.642893 11.00000 -1.20000 AFIX 0 C18 1 0.072122 0.309279 0.610402 11.00000 0.06137 0.07252 = 0.04374 -0.00336 0.00981 0.01338 AFIX 43 H18 2 0.115364 0.311220 0.647273 11.00000 -1.20000 AFIX 0 C19 1 0.239316 0.038161 0.490029 11.00000 0.06787 0.04906 = 0.05328 -0.00687 0.02234 0.00427 AFIX 23 H19A 2 0.185398 -0.039166 0.478476 11.00000 -1.20000 H19B 2 0.236302 0.122501 0.458091 11.00000 -1.20000 AFIX 0 C20 1 0.343109 -0.052825 0.492053 11.00000 0.14759 0.09454 = 0.06006 -0.01030 0.02001 0.05628 AFIX 23 H20A 2 0.396876 0.025307 0.502820 11.00000 -1.20000 H20B 2 0.346591 -0.135051 0.524796 11.00000 -1.20000 AFIX 0 C21 1 0.359044 -0.129535 0.434658 11.00000 0.18102 0.15989 = 0.05398 0.00324 0.01666 0.07084 AFIX 137 H21A 2 0.363706 -0.047615 0.403035 11.00000 -1.50000 H21B 2 0.303704 -0.201491 0.422139 11.00000 -1.50000 H21C 2 0.420508 -0.191423 0.439949 11.00000 -1.50000 AFIX 0 HKLF 4 REM 170329_lgn_zjl_b90_a.res in P2(1)/n REM R1 = 0.0370 for 2906 Fo > 4sig(Fo) and 0.0686 for all 4248 data REM 236 parameters refined using 6 restraints END WGHT 0.0175 0.0000 REM Highest difference peak 1.388, deepest hole -0.882, 1-sigma level 0.129 Q1 1 0.5975 0.9997 0.6827 11.00000 0.05 1.39 Q2 1 0.7435 0.9286 0.7361 11.00000 0.05 0.80 Q3 1 0.7519 0.5522 0.7588 11.00000 0.05 0.75 Q4 1 0.7392 0.6620 0.7217 11.00000 0.05 0.69 Q5 1 0.5950 1.0128 0.7371 11.00000 0.05 0.66 Q6 1 0.7159 0.7828 0.7957 11.00000 0.05 0.63 Q7 1 0.5209 0.9281 0.7110 11.00000 0.05 0.61 Q8 1 0.6518 0.7816 0.6880 11.00000 0.05 0.60 Q9 1 0.6770 1.0824 0.7761 11.00000 0.05 0.59 Q10 1 0.4202 -0.0350 0.4834 11.00000 0.05 0.58 Q11 1 0.7934 0.8011 0.7128 11.00000 0.05 0.57 Q12 1 0.6620 1.1188 0.7354 11.00000 0.05 0.56 Q13 1 0.8277 0.7083 0.7576 11.00000 0.05 0.54 Q14 1 0.5831 1.1637 0.7105 11.00000 0.05 0.54 Q15 1 0.8331 1.0113 0.7277 11.00000 0.05 0.54 Q16 1 0.8211 0.8217 0.7821 11.00000 0.05 0.54 Q17 1 0.6814 1.0052 0.7719 11.00000 0.05 0.53 Q18 1 0.7172 0.4985 0.6401 11.00000 0.05 0.53 Q19 1 0.5807 0.5113 0.7223 11.00000 0.05 0.52 Q20 1 0.9278 1.0486 0.7229 11.00000 0.05 0.50 REM The information below was added by Olex2. REM REM R1 = 0.0370 for 2906 Fo > 4sig(Fo) and 0.0686 for all 16244 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.39, deepest hole -0.88 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0686 REM R1_gt = 0.0370 REM wR_ref = 0.0673 REM GOOF = 0.977 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 16244 REM Reflections_gt = 2906 REM Parameters = n/a REM Hole = -0.88 REM Peak = 1.39 REM Flack = n/a ; _cod_data_source_file d3ce00931a2.cif _cod_data_source_block cmp6 _cod_depositor_comments 'Adding full bibliography for 7247629--7247634.cif.' _cod_database_code 7247634 _chemical_oxdiff_formula 'C H N P 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. Uiso/Uaniso restraints and constraints Uanis(C20) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 3.a Secondary CH2 refined with riding coordinates: C19(H19A,H19B), C20(H20A,H20B) 3.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18) 3.c Idealised Me refined as rotating group: C21(H21A,H21B,H21C) ; _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 99.59 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _shelx_estimated_absorpt_t_min 0.088 _shelx_estimated_absorpt_t_max 0.435 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 0.75197(2) 0.79440(3) 0.75196(2) 0.04451(10) Uani 1 1 d . . . . . Br1 Br 0.87901(6) 1.02194(10) 0.68916(4) 0.0612(2) Uani 1 1 d . . . . . Br2 Br 0.72276(6) 0.60556(11) 0.64092(4) 0.0636(2) Uani 1 1 d . . . . . Br3 Br 0.57697(6) 1.00119(11) 0.71980(4) 0.0673(3) Uani 1 1 d . . . . . P1 P 0.22004(14) 0.1303(2) 0.56402(9) 0.0434(5) Uani 1 1 d . . . . . C1 C 0.3149(5) 0.2801(8) 0.5831(3) 0.0408(18) Uani 1 1 d . . . . . C2 C 0.3683(6) 0.2971(11) 0.6408(4) 0.067(2) Uani 1 1 d . . . . . H2 H 0.3566 0.2242 0.6725 0.080 Uiso 1 1 calc R . . . . C3 C 0.4383(7) 0.4181(13) 0.6529(5) 0.080(3) Uani 1 1 d . . . . . H3 H 0.4739 0.4274 0.6923 0.096 Uiso 1 1 calc R . . . . C4 C 0.4553(7) 0.5263(11) 0.6058(7) 0.087(4) Uani 1 1 d . . . . . H4 H 0.5026 0.6096 0.6133 0.104 Uiso 1 1 calc R . . . . C5 C 0.4029(7) 0.5110(11) 0.5483(5) 0.077(3) Uani 1 1 d . . . . . H5 H 0.4143 0.5844 0.5166 0.093 Uiso 1 1 calc R . . . . C6 C 0.3336(6) 0.3882(10) 0.5366(4) 0.059(2) Uani 1 1 d . . . . . H6 H 0.2989 0.3779 0.4970 0.071 Uiso 1 1 calc R . . . . C7 C 0.2230(6) -0.0250(9) 0.6236(3) 0.0475(19) Uani 1 1 d . . . . . C8 C 0.1332(6) -0.0843(9) 0.6416(4) 0.058(2) Uani 1 1 d . . . . . H8 H 0.0722 -0.0372 0.6261 0.069 Uiso 1 1 calc R . . . . C9 C 0.1354(8) -0.2162(12) 0.6835(4) 0.078(3) Uani 1 1 d . . . . . H9 H 0.0755 -0.2582 0.6954 0.094 Uiso 1 1 calc R . . . . C10 C 0.2260(10) -0.2837(11) 0.7071(5) 0.089(3) Uani 1 1 d . . . . . H10 H 0.2270 -0.3725 0.7342 0.106 Uiso 1 1 calc R . . . . C11 C 0.3153(8) -0.2209(11) 0.6906(4) 0.085(3) Uani 1 1 d . . . . . H11 H 0.3764 -0.2649 0.7078 0.102 Uiso 1 1 calc R . . . . C12 C 0.3142(7) -0.0924(10) 0.6486(4) 0.062(2) Uani 1 1 d . . . . . H12 H 0.3746 -0.0509 0.6371 0.075 Uiso 1 1 calc R . . . . C13 C 0.1004(5) 0.2303(8) 0.5583(3) 0.0425(18) Uani 1 1 d . . . . . C14 C 0.0355(6) 0.2288(9) 0.5042(4) 0.054(2) Uani 1 1 d . . . . . H14 H 0.0539 0.1757 0.4688 0.065 Uiso 1 1 calc R . . . . C15 C -0.0577(6) 0.3063(9) 0.5021(4) 0.059(2) Uani 1 1 d . . . . . H15 H -0.1016 0.3062 0.4655 0.071 Uiso 1 1 calc R . . . . C16 C -0.0838(6) 0.3827(10) 0.5547(5) 0.063(2) Uani 1 1 d . . . . . H16 H -0.1463 0.4336 0.5538 0.076 Uiso 1 1 calc R . . . . C17 C -0.0203(7) 0.3854(10) 0.6077(4) 0.064(2) Uani 1 1 d . . . . . H17 H -0.0391 0.4392 0.6429 0.076 Uiso 1 1 calc R . . . . C18 C 0.0721(6) 0.3093(9) 0.6104(4) 0.059(2) Uani 1 1 d . . . . . H18 H 0.1154 0.3112 0.6473 0.071 Uiso 1 1 calc R . . . . C19 C 0.2393(6) 0.0382(9) 0.4900(3) 0.056(2) Uani 1 1 d . . . . . H19A H 0.1854 -0.0392 0.4785 0.067 Uiso 1 1 calc R . . . . H19B H 0.2363 0.1225 0.4581 0.067 Uiso 1 1 calc R . . . . C20 C 0.3431(8) -0.0528(11) 0.4921(4) 0.100(3) Uani 1 1 d . U . . . H20A H 0.3969 0.0253 0.5028 0.120 Uiso 1 1 calc R . . . . H20B H 0.3466 -0.1351 0.5248 0.120 Uiso 1 1 calc R . . . . C21 C 0.3590(8) -0.1295(14) 0.4347(4) 0.131(5) Uani 1 1 d . . . . . H21A H 0.3637 -0.0476 0.4030 0.197 Uiso 1 1 calc GR . . . . H21B H 0.3037 -0.2015 0.4221 0.197 Uiso 1 1 calc GR . . . . H21C H 0.4205 -0.1914 0.4399 0.197 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 0.04459(18) 0.04816(18) 0.04080(18) 0.00089(15) 0.00458(13) 0.00031(15) Br1 0.0523(5) 0.0683(6) 0.0667(6) 0.0085(5) 0.0231(4) -0.0005(4) Br2 0.0663(6) 0.0823(6) 0.0415(5) -0.0087(4) 0.0023(4) 0.0030(5) Br3 0.0454(5) 0.0892(7) 0.0661(6) 0.0114(5) -0.0004(4) 0.0106(4) P1 0.0486(12) 0.0471(12) 0.0359(11) -0.0009(10) 0.0100(10) 0.0009(10) C1 0.039(4) 0.041(4) 0.043(5) 0.004(4) 0.007(4) 0.002(3) C2 0.074(7) 0.063(6) 0.060(6) 0.003(5) -0.002(5) -0.003(5) C3 0.065(7) 0.080(7) 0.089(8) -0.017(6) -0.025(6) 0.010(6) C4 0.042(6) 0.053(6) 0.169(12) -0.019(8) 0.029(7) -0.006(5) C5 0.071(7) 0.068(7) 0.097(9) 0.007(6) 0.028(6) -0.003(6) C6 0.059(6) 0.056(5) 0.062(6) 0.000(5) 0.010(5) -0.014(5) C7 0.056(5) 0.048(5) 0.041(5) -0.002(4) 0.015(4) 0.002(4) C8 0.067(6) 0.054(5) 0.052(5) -0.005(4) 0.009(4) -0.004(4) C9 0.111(9) 0.071(7) 0.058(6) 0.005(5) 0.035(6) -0.013(6) C10 0.145(11) 0.059(6) 0.068(7) 0.023(5) 0.039(7) 0.024(7) C11 0.118(9) 0.073(7) 0.068(7) 0.013(6) 0.033(7) 0.026(6) C12 0.076(6) 0.060(6) 0.055(6) 0.006(5) 0.028(5) 0.010(5) C13 0.047(5) 0.042(4) 0.038(5) -0.001(4) 0.005(4) -0.006(4) C14 0.055(5) 0.051(5) 0.057(6) -0.004(4) 0.012(5) -0.008(4) C15 0.050(5) 0.056(5) 0.069(6) -0.003(5) -0.009(4) -0.008(4) C16 0.049(6) 0.053(5) 0.092(7) 0.004(5) 0.025(6) -0.001(4) C17 0.076(7) 0.053(5) 0.066(7) -0.003(5) 0.026(6) 0.010(5) C18 0.061(6) 0.073(6) 0.044(5) -0.003(4) 0.010(4) 0.013(5) C19 0.068(6) 0.049(5) 0.053(5) -0.007(4) 0.022(4) 0.004(4) C20 0.148(9) 0.095(7) 0.060(6) -0.010(5) 0.020(6) 0.056(6) C21 0.181(12) 0.160(11) 0.054(7) 0.003(7) 0.017(7) 0.071(9) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 174.44(2) . 2_646 ? Br2 Pb1 Br1 89.63(3) . . ? Br2 Pb1 Br1 85.42(2) . 2_646 ? Br2 Pb1 Br3 94.58(3) . . ? Br3 Pb1 Br1 90.62(3) . . ? Br3 Pb1 Br1 92.30(2) . 2_646 ? Pb1 Br1 Pb1 83.846(18) . 2_656 ? C1 P1 C7 111.1(4) . . ? C1 P1 C13 108.1(3) . . ? C1 P1 C19 109.1(3) . . ? C7 P1 C19 109.7(3) . . ? C13 P1 C7 108.9(3) . . ? C13 P1 C19 109.9(4) . . ? C2 C1 P1 124.6(6) . . ? C2 C1 C6 118.3(7) . . ? C6 C1 P1 117.0(6) . . ? C1 C2 H2 119.1 . . ? C3 C2 C1 121.7(8) . . ? C3 C2 H2 119.1 . . ? C2 C3 H3 120.5 . . ? C2 C3 C4 119.1(9) . . ? C4 C3 H3 120.5 . . ? C3 C4 H4 120.1 . . ? C5 C4 C3 119.9(9) . . ? C5 C4 H4 120.1 . . ? C4 C5 H5 119.8 . . ? C4 C5 C6 120.4(9) . . ? C6 C5 H5 119.8 . . ? C1 C6 H6 119.7 . . ? C5 C6 C1 120.6(8) . . ? C5 C6 H6 119.7 . . ? C8 C7 P1 119.3(6) . . ? C8 C7 C12 120.1(7) . . ? C12 C7 P1 120.5(6) . . ? C7 C8 H8 120.4 . . ? C7 C8 C9 119.2(8) . . ? C9 C8 H8 120.4 . . ? C8 C9 H9 119.9 . . ? C10 C9 C8 120.2(9) . . ? C10 C9 H9 119.9 . . ? C9 C10 H10 119.8 . . ? C11 C10 C9 120.5(9) . . ? C11 C10 H10 119.8 . . ? C10 C11 H11 120.0 . . ? C10 C11 C12 120.0(9) . . ? C12 C11 H11 120.0 . . ? C7 C12 H12 120.0 . . ? C11 C12 C7 120.1(8) . . ? C11 C12 H12 120.0 . . ? C14 C13 P1 122.2(6) . . ? C14 C13 C18 119.3(7) . . ? C18 C13 P1 118.5(6) . . ? C13 C14 H14 119.9 . . ? C13 C14 C15 120.3(7) . . ? C15 C14 H14 119.9 . . ? C14 C15 H15 120.5 . . ? C16 C15 C14 119.0(8) . . ? C16 C15 H15 120.5 . . ? C15 C16 H16 119.5 . . ? C17 C16 C15 121.0(8) . . ? C17 C16 H16 119.5 . . ? C16 C17 H17 119.7 . . ? C16 C17 C18 120.6(8) . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 119.9(8) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? P1 C19 H19A 109.1 . . ? P1 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C20 C19 P1 112.4(6) . . ? C20 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? C19 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C21 C20 C19 113.4(8) . . ? C21 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 3.1728(8) 2_646 ? Pb1 Br1 2.9364(8) . ? Pb1 Br2 2.8326(9) . ? Pb1 Br3 2.9062(9) . ? Br1 Pb1 3.1728(8) 2_656 ? P1 C1 1.777(7) . ? P1 C7 1.799(7) . ? P1 C13 1.786(7) . ? P1 C19 1.801(7) . ? C1 C2 1.370(10) . ? C1 C6 1.374(9) . ? C2 H2 0.9300 . ? C2 C3 1.366(11) . ? C3 H3 0.9300 . ? C3 C4 1.380(12) . ? C4 H4 0.9300 . ? C4 C5 1.360(13) . ? C5 H5 0.9300 . ? C5 C6 1.370(11) . ? C6 H6 0.9300 . ? C7 C8 1.385(9) . ? C7 C12 1.392(10) . ? C8 H8 0.9300 . ? C8 C9 1.402(11) . ? C9 H9 0.9300 . ? C9 C10 1.376(12) . ? C10 H10 0.9300 . ? C10 C11 1.376(12) . ? C11 H11 0.9300 . ? C11 C12 1.384(10) . ? C12 H12 0.9300 . ? C13 C14 1.376(9) . ? C13 C18 1.377(9) . ? C14 H14 0.9300 . ? C14 C15 1.392(10) . ? C15 H15 0.9300 . ? C15 C16 1.366(10) . ? C16 H16 0.9300 . ? C16 C17 1.347(10) . ? C17 H17 0.9300 . ? C17 C18 1.378(10) . ? C18 H18 0.9300 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.568(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C21 1.418(11) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ?