#------------------------------------------------------------------------------ #$Date: 2023-11-02 01:39:04 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287228 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247632.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_7247632 loop_ _publ_author_name 'Gao, Cheng-Cheng' 'Tang, Xue-Na' 'Miao, Jin-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_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00931A _journal_year 2023 _chemical_formula_moiety 'Br3 Pb, C20 H20 P' _chemical_formula_sum 'C20 H20 Br3 P Pb' _chemical_formula_weight 738.25 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _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 8 _cell_length_a 22.2970(12) _cell_length_b 7.9480(4) _cell_length_c 25.2706(11) _cell_measurement_reflns_used 1791 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.2770 _cell_measurement_theta_min 3.2290 _cell_volume 4478.4(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 35.00 88.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 15.7007 178.0000 90.0000 53 #__ type_ start__ end____ width___ exp.time_ 2 omega -25.00 52.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 15.7007 -99.0000 -90.0000 77 #__ type_ start__ end____ width___ exp.time_ 3 omega -15.00 28.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 15.7007 -37.0000 0.0000 43 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0127732000 _diffrn_orient_matrix_UB_12 0.0529725000 _diffrn_orient_matrix_UB_13 -0.0195801000 _diffrn_orient_matrix_UB_21 0.0233334000 _diffrn_orient_matrix_UB_22 0.0221109000 _diffrn_orient_matrix_UB_23 0.0177594000 _diffrn_orient_matrix_UB_31 0.0174438000 _diffrn_orient_matrix_UB_32 -0.0683628000 _diffrn_orient_matrix_UB_33 -0.0094187000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_unetI/netI 0.0977 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 13237 _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 25.499 _diffrn_reflns_theta_min 3.180 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 12.961 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.20324 _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 2.190 _exptl_crystal_description prism _exptl_crystal_F_000 2736 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.241 _refine_diff_density_min -1.342 _refine_diff_density_rms 0.181 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 4151 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.996 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0499 _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^)+(0.0141P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.1022 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2156 _reflns_number_total 4151 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 61.res created by SHELXL-2014/7 TITL 170122_LGN_ZJL_639 in Pbca #61 REM reset to Pbca #61 CELL 0.71073 22.29702 7.94798 25.27059 90 90 90 ZERR 8 0.00116 0.00039 0.00107 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H Br P Pb UNIT 160 160 24 8 8 L.S. 50 PLAN 5 TEMP 20(2) BOND fmap 2 acta OMIT -3 51 OMIT 2 1 3 OMIT 1 2 2 REM REM REM WGHT 0.014100 FVAR 0.45334 PB1 5 0.749744 0.743980 0.412716 11.00000 0.04392 0.03377 = 0.03446 -0.00171 0.00204 0.00001 BR1 3 0.689958 0.981681 0.336228 11.00000 0.05635 0.05307 = 0.02997 -0.00510 -0.00551 -0.00357 BR2 3 0.643792 0.522086 0.409689 11.00000 0.03711 0.05211 = 0.05401 0.00636 0.00024 -0.00474 BR3 3 0.703863 0.972181 0.495687 11.00000 0.05589 0.05629 = 0.03319 -0.00372 0.00800 0.00938 P1 4 0.603852 0.637755 0.628018 11.00000 0.03630 0.04856 = 0.03112 -0.00245 -0.00023 0.00554 C1 1 0.548764 0.730886 0.586823 11.00000 0.03950 0.04079 = 0.05046 0.00648 0.01191 0.00304 C2 1 0.546106 0.704012 0.532375 11.00000 0.06074 0.05146 = 0.03604 0.00490 -0.01662 -0.00343 AFIX 43 H2 2 0.576324 0.643598 0.515569 11.00000 -1.20000 AFIX 0 C3 1 0.498610 0.767036 0.503300 11.00000 0.08990 0.06421 = 0.05598 0.01598 -0.03193 -0.02810 AFIX 43 H3 2 0.496868 0.751083 0.466874 11.00000 -1.20000 AFIX 0 C4 1 0.454478 0.852761 0.528883 11.00000 0.05046 0.04117 = 0.11505 0.00528 -0.01187 0.00585 AFIX 43 H4 2 0.421896 0.892222 0.509547 11.00000 -1.20000 AFIX 0 C5 1 0.456521 0.882847 0.582326 11.00000 0.05841 0.07217 = 0.08584 0.00070 0.02060 0.01510 AFIX 43 H5 2 0.426520 0.945048 0.598787 11.00000 -1.20000 AFIX 0 C6 1 0.502439 0.821104 0.610321 11.00000 0.05168 0.05027 = 0.04988 0.00971 0.00903 0.01271 AFIX 43 H6 2 0.503411 0.839098 0.646675 11.00000 -1.20000 AFIX 0 C7 1 0.567550 0.478738 0.667209 11.00000 0.04500 0.05058 = 0.02538 -0.00822 0.00742 -0.00785 C8 1 0.511092 0.419168 0.654581 11.00000 0.05702 0.06109 = 0.04529 0.00098 0.00786 -0.01275 AFIX 43 H8 2 0.490088 0.466807 0.626538 11.00000 -1.20000 AFIX 0 C9 1 0.485963 0.291622 0.682752 11.00000 0.06796 0.08167 = 0.06924 0.00492 0.01610 -0.03160 AFIX 43 H9 2 0.447589 0.253993 0.674511 11.00000 -1.20000 AFIX 0 C10 1 0.517531 0.218323 0.723537 11.00000 0.10922 0.05460 = 0.06856 0.00963 0.02309 -0.00211 AFIX 43 H10 2 0.500291 0.130035 0.742297 11.00000 -1.20000 AFIX 0 C11 1 0.572023 0.271007 0.736632 11.00000 0.07932 0.05084 = 0.06493 0.03727 0.02004 0.01476 AFIX 43 H11 2 0.592074 0.222127 0.765005 11.00000 -1.20000 AFIX 0 C12 1 0.598719 0.397547 0.708292 11.00000 0.04647 0.05652 = 0.05353 0.01089 -0.00160 0.00339 AFIX 43 H12 2 0.637756 0.429962 0.716298 11.00000 -1.20000 AFIX 0 C13 1 0.639982 0.798996 0.667807 11.00000 0.05389 0.03357 = 0.04545 0.00441 0.00302 0.00695 C14 1 0.642971 0.795541 0.722594 11.00000 0.04789 0.05489 = 0.02837 0.00554 0.00023 0.00475 AFIX 43 H14 2 0.623887 0.710515 0.741455 11.00000 -1.20000 AFIX 0 C15 1 0.674737 0.920256 0.749106 11.00000 0.07122 0.05788 = 0.03638 -0.01627 -0.02075 -0.00103 AFIX 43 H15 2 0.677467 0.917900 0.785821 11.00000 -1.20000 AFIX 0 C16 1 0.701721 1.045229 0.721479 11.00000 0.04804 0.04403 = 0.07016 -0.01882 0.00001 0.01052 AFIX 43 H16 2 0.723837 1.126503 0.739373 11.00000 -1.20000 AFIX 0 C17 1 0.696807 1.053281 0.667458 11.00000 0.05248 0.06588 = 0.05448 -0.00114 0.01320 0.00054 AFIX 43 H17 2 0.714561 1.141433 0.649011 11.00000 -1.20000 AFIX 0 C18 1 0.665764 0.931536 0.640697 11.00000 0.07805 0.04847 = 0.03642 0.01155 0.00559 -0.00094 AFIX 43 H18 2 0.662002 0.938029 0.604102 11.00000 -1.20000 AFIX 0 C19 1 0.662234 0.536658 0.589857 11.00000 0.02983 0.05848 = 0.04885 -0.00360 -0.00497 -0.00015 AFIX 23 H19A 2 0.676246 0.614869 0.563110 11.00000 -1.20000 H19B 2 0.695729 0.512495 0.613144 11.00000 -1.20000 AFIX 0 C20 1 0.643392 0.374620 0.562773 11.00000 0.07861 0.03924 = 0.05143 -0.01141 0.01157 0.01028 AFIX 137 H20A 2 0.673316 0.342714 0.537369 11.00000 -1.50000 H20B 2 0.605755 0.391474 0.545102 11.00000 -1.50000 H20C 2 0.639188 0.287180 0.588717 11.00000 -1.50000 AFIX 0 HKLF 4 REM 170122_LGN_ZJL_639 in Pbca #61 REM R1 = 0.0499 for 2156 Fo > 4sig(Fo) and 0.1182 for all 4151 data REM 227 parameters refined using 0 restraints END WGHT 0.0141 0.0000 REM Highest difference peak 1.241, deepest hole -1.342, 1-sigma level 0.181 Q1 1 0.7548 0.8881 0.4116 11.00000 0.05 1.24 Q2 1 0.7529 0.5960 0.4128 11.00000 0.05 1.12 Q3 1 0.7015 0.4782 0.4949 11.00000 0.05 1.03 Q4 1 0.7487 1.0464 0.4674 11.00000 0.05 1.02 Q5 1 0.6480 0.5347 0.3856 11.00000 0.05 0.88 REM The information below was added by Olex2. REM REM R1 = 0.0499 for 2156 Fo > 4sig(Fo) and 0.1182 for all 16564 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.24, deepest hole -1.34 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1182 REM R1_gt = 0.0499 REM wR_ref = 0.1022 REM GOOF = 0.996 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 16564 REM Reflections_gt = 2156 REM Parameters = n/a REM Hole = -1.34 REM Peak = 1.24 REM Flack = n/a ; _cod_data_source_file d3ce00931a2.cif _cod_data_source_block cmp5 _cod_database_code 7247632 _chemical_oxdiff_formula 'C H 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.a Secondary CH2 refined with riding coordinates: C19(H19A,H19B) 2.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) 2.c Idealised Me refined as rotating group: 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 99.57 _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, 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 0.74974(2) 0.74398(6) 0.41272(2) 0.03738(16) Uani 1 1 d . . . . . Br1 Br 0.68996(6) 0.98168(17) 0.33623(4) 0.0465(3) Uani 1 1 d . . . . . Br2 Br 0.64379(5) 0.52209(17) 0.40969(5) 0.0477(3) Uani 1 1 d . . . . . Br3 Br 0.70386(6) 0.97218(17) 0.49569(4) 0.0485(4) Uani 1 1 d . . . . . P1 P 0.60385(15) 0.6378(4) 0.62802(12) 0.0387(8) Uani 1 1 d . . . . . C1 C 0.5488(6) 0.7309(15) 0.5868(5) 0.044(3) Uani 1 1 d . . . . . C2 C 0.5461(6) 0.7040(16) 0.5324(5) 0.049(4) Uani 1 1 d . . . . . H2 H 0.5763 0.6436 0.5156 0.059 Uiso 1 1 calc R . . . . C3 C 0.4986(8) 0.7670(19) 0.5033(7) 0.070(5) Uani 1 1 d . . . . . H3 H 0.4969 0.7511 0.4669 0.084 Uiso 1 1 calc R . . . . C4 C 0.4545(7) 0.8528(18) 0.5289(8) 0.069(5) Uani 1 1 d . . . . . H4 H 0.4219 0.8922 0.5095 0.083 Uiso 1 1 calc R . . . . C5 C 0.4565(7) 0.883(2) 0.5823(7) 0.072(5) Uani 1 1 d . . . . . H5 H 0.4265 0.9450 0.5988 0.087 Uiso 1 1 calc R . . . . C6 C 0.5024(6) 0.8211(16) 0.6103(5) 0.051(4) Uani 1 1 d . . . . . H6 H 0.5034 0.8391 0.6467 0.061 Uiso 1 1 calc R . . . . C7 C 0.5675(5) 0.4787(16) 0.6672(4) 0.040(3) Uani 1 1 d . . . . . C8 C 0.5111(6) 0.4192(17) 0.6546(5) 0.054(4) Uani 1 1 d . . . . . H8 H 0.4901 0.4668 0.6265 0.065 Uiso 1 1 calc R . . . . C9 C 0.4860(7) 0.292(2) 0.6828(6) 0.073(5) Uani 1 1 d . . . . . H9 H 0.4476 0.2540 0.6745 0.088 Uiso 1 1 calc R . . . . C10 C 0.5175(9) 0.218(2) 0.7235(7) 0.077(5) Uani 1 1 d . . . . . H10 H 0.5003 0.1300 0.7423 0.093 Uiso 1 1 calc R . . . . C11 C 0.5720(8) 0.2710(18) 0.7366(6) 0.065(5) Uani 1 1 d . . . . . H11 H 0.5921 0.2221 0.7650 0.078 Uiso 1 1 calc R . . . . C12 C 0.5987(6) 0.3975(17) 0.7083(5) 0.052(4) Uani 1 1 d . . . . . H12 H 0.6378 0.4300 0.7163 0.063 Uiso 1 1 calc R . . . . C13 C 0.6400(6) 0.7990(15) 0.6678(5) 0.044(3) Uani 1 1 d . . . . . C14 C 0.6430(6) 0.7955(16) 0.7226(5) 0.044(3) Uani 1 1 d . . . . . H14 H 0.6239 0.7105 0.7415 0.052 Uiso 1 1 calc R . . . . C15 C 0.6747(6) 0.9203(18) 0.7491(5) 0.055(4) Uani 1 1 d . . . . . H15 H 0.6775 0.9179 0.7858 0.066 Uiso 1 1 calc R . . . . C16 C 0.7017(6) 1.0452(17) 0.7215(6) 0.054(4) Uani 1 1 d . . . . . H16 H 0.7238 1.1265 0.7394 0.065 Uiso 1 1 calc R . . . . C17 C 0.6968(6) 1.0533(18) 0.6675(6) 0.058(4) Uani 1 1 d . . . . . H17 H 0.7146 1.1414 0.6490 0.069 Uiso 1 1 calc R . . . . C18 C 0.6658(6) 0.9315(17) 0.6407(5) 0.054(4) Uani 1 1 d . . . . . H18 H 0.6620 0.9380 0.6041 0.065 Uiso 1 1 calc R . . . . C19 C 0.6622(5) 0.5367(15) 0.5899(5) 0.046(3) Uani 1 1 d . . . . . H19A H 0.6762 0.6149 0.5631 0.055 Uiso 1 1 calc R . . . . H19B H 0.6957 0.5125 0.6131 0.055 Uiso 1 1 calc R . . . . C20 C 0.6434(6) 0.3746(15) 0.5628(5) 0.056(4) Uani 1 1 d . . . . . H20A H 0.6733 0.3427 0.5374 0.085 Uiso 1 1 calc GR . . . . H20B H 0.6058 0.3915 0.5451 0.085 Uiso 1 1 calc GR . . . . H20C H 0.6392 0.2872 0.5887 0.085 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 0.0439(3) 0.0338(3) 0.0345(3) -0.0017(3) 0.0020(3) 0.0000(2) Br1 0.0564(8) 0.0531(8) 0.0300(6) -0.0051(7) -0.0055(6) -0.0036(8) Br2 0.0371(6) 0.0521(8) 0.0540(8) 0.0064(7) 0.0002(7) -0.0047(7) Br3 0.0559(8) 0.0563(9) 0.0332(6) -0.0037(7) 0.0080(6) 0.0094(8) P1 0.0363(18) 0.049(2) 0.0311(18) -0.0025(17) -0.0002(17) 0.0055(18) C1 0.039(7) 0.041(8) 0.050(8) 0.006(7) 0.012(8) 0.003(7) C2 0.061(9) 0.051(9) 0.036(8) 0.005(7) -0.017(8) -0.003(8) C3 0.090(12) 0.064(10) 0.056(9) 0.016(9) -0.032(9) -0.028(11) C4 0.050(10) 0.041(10) 0.115(15) 0.005(10) -0.012(11) 0.006(8) C5 0.058(11) 0.072(11) 0.086(13) 0.001(11) 0.021(11) 0.015(9) C6 0.052(9) 0.050(9) 0.050(9) 0.010(8) 0.009(8) 0.013(8) C7 0.045(7) 0.051(8) 0.025(6) -0.008(7) 0.007(6) -0.008(8) C8 0.057(9) 0.061(10) 0.045(8) 0.001(8) 0.008(8) -0.013(8) C9 0.068(11) 0.082(13) 0.069(11) 0.005(10) 0.016(11) -0.032(10) C10 0.109(15) 0.055(11) 0.069(12) 0.010(9) 0.023(13) -0.002(11) C11 0.079(12) 0.051(10) 0.065(11) 0.037(9) 0.020(10) 0.015(9) C12 0.046(8) 0.057(9) 0.054(9) 0.011(8) -0.002(8) 0.003(8) C13 0.054(8) 0.034(7) 0.045(8) 0.004(7) 0.003(8) 0.007(7) C14 0.048(8) 0.055(9) 0.028(7) 0.006(7) 0.000(7) 0.005(7) C15 0.071(10) 0.058(9) 0.036(8) -0.016(8) -0.021(8) -0.001(8) C16 0.048(9) 0.044(9) 0.070(10) -0.019(8) 0.000(8) 0.011(7) C17 0.052(9) 0.066(10) 0.054(9) -0.001(8) 0.013(8) 0.001(8) C18 0.078(11) 0.048(9) 0.036(8) 0.012(7) 0.006(8) -0.001(8) C19 0.030(6) 0.058(9) 0.049(8) -0.004(7) -0.005(6) 0.000(7) C20 0.079(10) 0.039(8) 0.051(9) -0.011(7) 0.012(9) 0.010(8) 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 102.15(4) . 7_755 ? Br1 Pb1 Br3 79.40(3) 7_755 7_755 ? Br1 Pb1 Br3 172.58(4) . 7_755 ? Br2 Pb1 Br1 90.22(4) . . ? Br2 Pb1 Br1 85.99(4) . 7_755 ? Br2 Pb1 Br3 96.21(4) . . ? Br2 Pb1 Br3 82.62(4) . 7_755 ? Br3 Pb1 Br1 85.25(4) . . ? Br3 Pb1 Br1 172.30(4) . 7_755 ? Br3 Pb1 Br3 93.54(4) . 7_755 ? Pb1 Br1 Pb1 80.34(3) . 7_765 ? Pb1 Br3 Pb1 80.60(3) . 7_765 ? C1 P1 C7 107.8(6) . . ? C1 P1 C13 109.7(6) . . ? C1 P1 C19 111.8(6) . . ? C7 P1 C13 113.0(6) . . ? C7 P1 C19 107.8(6) . . ? C19 P1 C13 106.8(6) . . ? C2 C1 P1 123.1(11) . . ? C6 C1 P1 118.6(10) . . ? C6 C1 C2 118.0(13) . . ? C3 C2 C1 120.1(14) . . ? C4 C3 C2 118.9(15) . . ? C3 C4 C5 122.1(16) . . ? C6 C5 C4 118.8(15) . . ? C5 C6 C1 122.1(13) . . ? C8 C7 P1 121.6(10) . . ? C8 C7 C12 117.6(12) . . ? C12 C7 P1 120.4(10) . . ? C9 C8 C7 120.7(14) . . ? C8 C9 C10 119.8(15) . . ? C11 C10 C9 121.4(16) . . ? C10 C11 C12 119.9(15) . . ? C11 C12 C7 120.5(13) . . ? C14 C13 P1 124.0(10) . . ? C18 C13 P1 116.6(10) . . ? C18 C13 C14 119.4(12) . . ? C13 C14 C15 119.4(12) . . ? C16 C15 C14 120.0(12) . . ? C15 C16 C17 120.8(13) . . ? C18 C17 C16 120.0(13) . . ? C17 C18 C13 120.3(12) . . ? C20 C19 P1 114.7(8) . . ? 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 3.1449(13) 7_755 ? Pb1 Br1 3.0137(13) . ? Pb1 Br2 2.9491(13) . ? Pb1 Br3 2.9551(13) . ? Pb1 Br3 3.1832(13) 7_755 ? Br1 Pb1 3.1448(13) 7_765 ? Br3 Pb1 3.1832(13) 7_765 ? P1 C1 1.772(13) . ? P1 C7 1.798(12) . ? P1 C13 1.817(13) . ? P1 C19 1.808(11) . ? C1 C2 1.394(16) . ? C1 C6 1.391(15) . ? C2 C3 1.383(17) . ? C3 C4 1.360(19) . ? C4 C5 1.37(2) . ? C5 C6 1.338(18) . ? C7 C8 1.382(16) . ? C7 C12 1.406(15) . ? C8 C9 1.360(18) . ? C9 C10 1.377(19) . ? C10 C11 1.327(19) . ? C11 C12 1.371(17) . ? C13 C14 1.386(15) . ? C13 C18 1.382(16) . ? C14 C15 1.390(16) . ? C15 C16 1.355(17) . ? C16 C17 1.371(17) . ? C17 C18 1.368(17) . ? C19 C20 1.518(15) . ?