#------------------------------------------------------------------------------ #$Date: 2023-11-02 01:39:04 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287228 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247631.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_7247631 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, C19 H18 P' _chemical_formula_sum 'C19 H18 Br3 P Pb' _chemical_formula_weight 724.22 _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 iterative _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 22.601(2) _cell_length_b 7.8074(7) _cell_length_c 24.284(2) _cell_measurement_reflns_used 3661 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.5050 _cell_measurement_theta_min 3.8520 _cell_volume 4285.0(6) _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 'olex2.solve (Bourhis et al., 2015)' _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 -51.00 33.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 -57.0000 -180.0000 84 #__ type_ start__ end____ width___ exp.time_ 2 omega -25.00 55.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 -99.0000 -90.0000 80 #__ type_ start__ end____ width___ exp.time_ 3 omega 35.00 88.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 178.0000 120.0000 53 #__ type_ start__ end____ width___ exp.time_ 4 omega -11.00 14.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 15.8569 77.0000 -150.0000 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0187265000 _diffrn_orient_matrix_UB_12 0.0249888000 _diffrn_orient_matrix_UB_13 0.0220311000 _diffrn_orient_matrix_UB_21 0.0116363000 _diffrn_orient_matrix_UB_22 -0.0670550000 _diffrn_orient_matrix_UB_23 0.0164743000 _diffrn_orient_matrix_UB_31 0.0223022000 _diffrn_orient_matrix_UB_32 0.0560487000 _diffrn_orient_matrix_UB_33 0.0098812000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1042 _diffrn_reflns_av_unetI/netI 0.1011 _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 -27 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 16987 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.214 _diffrn_reflns_theta_max 25.318 _diffrn_reflns_theta_min 3.168 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 13.543 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.11823 _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 red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.245 _exptl_crystal_description prism _exptl_crystal_F_000 2672 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _refine_diff_density_max 2.020 _refine_diff_density_min -2.040 _refine_diff_density_rms 0.255 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 218 _refine_ls_number_reflns 3915 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0708 _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^)+(0.0726P)^2^+13.1542P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1525 _refine_ls_wR_factor_ref 0.1775 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2336 _reflns_number_total 3915 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 61.res created by SHELXL-2014/7 TITL 170313_LGN_ZJL_B89 in Pbca #61 REM reset to Pbca #61 CELL 0.71 22.601067 7.80742 24.284161 90 90 90 ZERR 8 0.001981 0.000694 0.00196 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 152 144 24 8 8 DELU 0.01 0.02 C5 C6 L.S. 50 0 0 PLAN 5 TEMP 20(2) BOND fmap 2 53 acta SHEL 999 0.83 OMIT 0 0 4 OMIT 19 4 14 REM REM REM WGHT 0.072600 13.154201 FVAR 0.92736 PB1 5 0.249282 0.166531 0.589539 11.00000 0.04575 0.03279 = 0.03490 0.00078 0.00119 0.00018 BR1 3 0.310295 -0.080183 0.668695 11.00000 0.05523 0.05892 = 0.03403 -0.00430 -0.00375 -0.00159 BR2 3 0.353507 0.412305 0.594893 11.00000 0.03720 0.06844 = 0.05573 0.00790 0.00317 -0.00071 BR3 3 0.290733 -0.080810 0.501085 11.00000 0.05741 0.05258 = 0.03472 0.00298 0.00854 0.01107 P1 4 0.400903 0.433894 0.382781 11.00000 0.03536 0.04429 = 0.03891 -0.00490 0.00665 0.00038 C1 1 0.434951 0.592078 0.339876 11.00000 0.04140 0.03688 = 0.03970 0.00855 0.00733 0.00078 C2 1 0.494168 0.634716 0.347059 11.00000 0.05212 0.06019 = 0.04764 0.00029 0.01181 -0.01300 AFIX 43 H2 2 0.517335 0.574384 0.372069 11.00000 -1.20000 AFIX 0 C3 1 0.518074 0.765324 0.317272 11.00000 0.06100 0.06962 = 0.05680 0.00828 0.00126 -0.01885 AFIX 43 H3 2 0.557373 0.795646 0.323088 11.00000 -1.20000 AFIX 0 C4 1 0.485965 0.851844 0.279456 11.00000 0.07484 0.04493 = 0.07758 0.01056 0.02879 -0.00861 AFIX 43 H4 2 0.503439 0.939605 0.259305 11.00000 -1.20000 AFIX 0 C5 1 0.427064 0.810337 0.270561 11.00000 0.06786 0.05670 = 0.09301 0.01576 0.00091 0.01859 AFIX 43 H5 2 0.404956 0.868386 0.244199 11.00000 -1.20000 AFIX 0 C6 1 0.401723 0.680680 0.301696 11.00000 0.04782 0.04428 = 0.09525 0.01470 -0.00073 0.00467 AFIX 43 H6 2 0.362026 0.653293 0.296785 11.00000 -1.20000 AFIX 0 C7 1 0.358073 0.280279 0.342634 11.00000 0.02666 0.04317 = 0.04766 -0.00316 0.01222 -0.00155 C8 1 0.355716 0.280998 0.286640 11.00000 0.05019 0.05836 = 0.04292 0.00014 0.01342 -0.01197 AFIX 43 H8 2 0.376730 0.362442 0.266677 11.00000 -1.20000 AFIX 0 C9 1 0.322390 0.161689 0.260080 11.00000 0.05905 0.08418 = 0.03365 0.00335 -0.01743 -0.00809 AFIX 43 H9 2 0.320818 0.160661 0.221813 11.00000 -1.20000 AFIX 0 C10 1 0.291087 0.042820 0.289855 11.00000 0.03674 0.04910 = 0.08670 -0.01358 -0.02324 -0.00334 AFIX 43 H10 2 0.267312 -0.036073 0.271589 11.00000 -1.20000 AFIX 0 C11 1 0.294508 0.039042 0.346784 11.00000 0.04982 0.06747 = 0.05684 0.03526 -0.00708 -0.02061 AFIX 43 H11 2 0.274409 -0.045292 0.366318 11.00000 -1.20000 AFIX 0 C12 1 0.327423 0.159165 0.374585 11.00000 0.06162 0.06356 = 0.03532 -0.00534 0.00178 -0.02055 AFIX 43 H12 2 0.329334 0.160275 0.412838 11.00000 -1.20000 AFIX 0 C13 1 0.457722 0.318844 0.418967 11.00000 0.02810 0.04219 = 0.04586 -0.00175 0.01011 -0.00264 C14 1 0.461309 0.322384 0.475452 11.00000 0.07918 0.04875 = 0.04556 -0.00354 -0.01942 -0.00665 AFIX 43 H14 2 0.433776 0.383759 0.495961 11.00000 -1.20000 AFIX 0 C15 1 0.506511 0.233285 0.501582 11.00000 0.09515 0.05193 = 0.05931 -0.00584 -0.02311 -0.00986 AFIX 43 H15 2 0.508317 0.229998 0.539827 11.00000 -1.20000 AFIX 0 C16 1 0.547677 0.151742 0.471300 11.00000 0.07116 0.06853 = 0.09594 -0.00353 -0.04327 -0.01896 AFIX 43 H16 2 0.578758 0.097089 0.489220 11.00000 -1.20000 AFIX 0 C17 1 0.545309 0.146604 0.415052 11.00000 0.04742 0.07716 = 0.12732 0.01053 0.01194 0.01356 AFIX 43 H17 2 0.573778 0.086762 0.395191 11.00000 -1.20000 AFIX 0 C18 1 0.499235 0.233029 0.387523 11.00000 0.05652 0.06397 = 0.06058 -0.00717 0.01117 -0.00347 AFIX 43 H18 2 0.496821 0.232359 0.349293 11.00000 -1.20000 AFIX 0 C19 1 0.352762 0.538587 0.430704 11.00000 0.05468 0.05450 = 0.06781 -0.01545 0.01108 0.01009 AFIX 137 H19A 2 0.325971 0.611972 0.411096 11.00000 -1.50000 H19B 2 0.375848 0.605702 0.455913 11.00000 -1.50000 H19C 2 0.330655 0.454215 0.450795 11.00000 -1.50000 AFIX 0 HKLF 4 REM 170313_LGN_ZJL_B89 in Pbca #61 REM R1 = 0.0708 for 2336 Fo > 4sig(Fo) and 0.1174 for all 3915 data REM 218 parameters refined using 1 restraints END WGHT 0.0726 13.2706 REM Highest difference peak 2.020, deepest hole -2.040, 1-sigma level 0.255 Q1 1 0.2967 0.4198 0.4995 11.00000 0.05 2.02 Q2 1 0.2484 0.2417 0.5375 11.00000 0.05 1.95 Q3 1 0.2512 0.2395 0.6428 11.00000 0.05 1.90 Q4 1 0.2473 0.0374 0.5910 11.00000 0.05 1.74 Q5 1 0.2506 0.3031 0.5900 11.00000 0.05 1.70 REM The information below was added by Olex2. REM REM R1 = 0.0708 for 2336 Fo > 4sig(Fo) and 0.1174 for all 21179 data REM n/a parameters refined using n/a restraints REM Highest difference peak 2.02, deepest hole -2.04 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1174 REM R1_gt = 0.0708 REM wR_ref = 0.1775 REM GOOF = 1.044 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 21179 REM Reflections_gt = 2336 REM Parameters = n/a REM Hole = -2.04 REM Peak = 2.02 REM Flack = n/a ; _cod_data_source_file d3ce00931a2.cif _cod_data_source_block cmp4 _cod_original_cell_volume 4285.1(6) _cod_database_code 7247631 _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 At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints C5, C6 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 3.a 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.b Idealised Me refined as rotating group: C19(H19A,H19B,H19C) ; _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 99.62 _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+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 0.24928(2) 0.16653(7) 0.58954(2) 0.0378(2) Uani 1 1 d . . . . . Br1 Br 0.31030(6) -0.08018(19) 0.66870(7) 0.0494(4) Uani 1 1 d . . . . . Br2 Br 0.35351(6) 0.4123(2) 0.59489(7) 0.0538(5) Uani 1 1 d . . . . . Br3 Br 0.29073(7) -0.08081(18) 0.50109(6) 0.0482(4) Uani 1 1 d . . . . . P1 P 0.40090(15) 0.4339(5) 0.38278(17) 0.0395(9) Uani 1 1 d . . . . . C1 C 0.4350(6) 0.5921(16) 0.3399(6) 0.039(3) Uani 1 1 d . . . . . C2 C 0.4942(6) 0.6347(19) 0.3471(7) 0.053(4) Uani 1 1 d . . . . . H2 H 0.5173 0.5744 0.3721 0.064 Uiso 1 1 calc R . . . . C3 C 0.5181(8) 0.765(2) 0.3173(8) 0.062(5) Uani 1 1 d . . . . . H3 H 0.5574 0.7956 0.3231 0.075 Uiso 1 1 calc R . . . . C4 C 0.4860(8) 0.852(2) 0.2795(9) 0.066(5) Uani 1 1 d . . . . . H4 H 0.5034 0.9396 0.2593 0.079 Uiso 1 1 calc R . . . . C5 C 0.4271(8) 0.810(2) 0.2706(9) 0.073(6) Uani 1 1 d . U . . . H5 H 0.4050 0.8684 0.2442 0.087 Uiso 1 1 calc R . . . . C6 C 0.4017(7) 0.6807(17) 0.3017(8) 0.062(5) Uani 1 1 d . U . . . H6 H 0.3620 0.6533 0.2968 0.075 Uiso 1 1 calc R . . . . C7 C 0.3581(5) 0.2803(17) 0.3426(6) 0.039(4) Uani 1 1 d . . . . . C8 C 0.3557(6) 0.2810(19) 0.2866(7) 0.050(4) Uani 1 1 d . . . . . H8 H 0.3767 0.3624 0.2667 0.061 Uiso 1 1 calc R . . . . C9 C 0.3224(7) 0.162(2) 0.2601(7) 0.059(4) Uani 1 1 d . . . . . H9 H 0.3208 0.1607 0.2218 0.071 Uiso 1 1 calc R . . . . C10 C 0.2911(6) 0.0428(18) 0.2899(8) 0.058(5) Uani 1 1 d . . . . . H10 H 0.2673 -0.0361 0.2716 0.069 Uiso 1 1 calc R . . . . C11 C 0.2945(7) 0.039(2) 0.3468(8) 0.058(5) Uani 1 1 d . . . . . H11 H 0.2744 -0.0453 0.3663 0.070 Uiso 1 1 calc R . . . . C12 C 0.3274(7) 0.1592(18) 0.3746(7) 0.054(4) Uani 1 1 d . . . . . H12 H 0.3293 0.1603 0.4128 0.064 Uiso 1 1 calc R . . . . C13 C 0.4577(5) 0.3188(17) 0.4190(7) 0.039(4) Uani 1 1 d . . . . . C14 C 0.4613(8) 0.3224(19) 0.4755(8) 0.058(5) Uani 1 1 d . . . . . H14 H 0.4338 0.3838 0.4960 0.069 Uiso 1 1 calc R . . . . C15 C 0.5065(8) 0.2333(19) 0.5016(8) 0.069(5) Uani 1 1 d . . . . . H15 H 0.5083 0.2300 0.5398 0.083 Uiso 1 1 calc R . . . . C16 C 0.5477(9) 0.152(2) 0.4713(11) 0.079(7) Uani 1 1 d . . . . . H16 H 0.5788 0.0971 0.4892 0.094 Uiso 1 1 calc R . . . . C17 C 0.5453(8) 0.147(2) 0.4151(11) 0.084(7) Uani 1 1 d . . . . . H17 H 0.5738 0.0868 0.3952 0.101 Uiso 1 1 calc R . . . . C18 C 0.4992(6) 0.2330(19) 0.3875(8) 0.060(4) Uani 1 1 d . . . . . H18 H 0.4968 0.2324 0.3493 0.072 Uiso 1 1 calc R . . . . C19 C 0.3528(6) 0.5386(19) 0.4307(8) 0.059(5) Uani 1 1 d . . . . . H19A H 0.3260 0.6120 0.4111 0.088 Uiso 1 1 calc GR . . . . H19B H 0.3758 0.6057 0.4559 0.088 Uiso 1 1 calc GR . . . . H19C H 0.3307 0.4542 0.4508 0.088 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 0.0457(4) 0.0328(3) 0.0349(4) 0.0008(3) 0.0012(3) 0.0002(2) Br1 0.0552(9) 0.0589(9) 0.0340(9) -0.0043(8) -0.0038(7) -0.0016(7) Br2 0.0372(8) 0.0684(10) 0.0557(11) 0.0079(9) 0.0032(7) -0.0007(7) Br3 0.0574(9) 0.0526(9) 0.0347(9) 0.0030(8) 0.0085(7) 0.0111(7) P1 0.0354(18) 0.044(2) 0.039(2) -0.0049(19) 0.0066(18) 0.0004(16) C1 0.041(8) 0.037(7) 0.040(9) 0.009(8) 0.007(7) 0.001(6) C2 0.052(9) 0.060(9) 0.048(11) 0.000(8) 0.012(9) -0.013(7) C3 0.061(10) 0.070(11) 0.057(12) 0.008(11) 0.001(10) -0.019(9) C4 0.075(12) 0.045(9) 0.078(15) 0.011(10) 0.029(12) -0.009(8) C5 0.068(12) 0.057(10) 0.093(17) 0.016(10) 0.001(11) 0.019(8) C6 0.048(9) 0.044(9) 0.095(16) 0.015(9) -0.001(10) 0.005(7) C7 0.027(6) 0.043(8) 0.048(10) -0.003(8) 0.012(7) -0.002(6) C8 0.050(9) 0.058(9) 0.043(10) 0.000(9) 0.013(9) -0.012(7) C9 0.059(10) 0.084(11) 0.034(10) 0.003(9) -0.017(9) -0.008(9) C10 0.037(8) 0.049(9) 0.087(15) -0.014(10) -0.023(10) -0.003(7) C11 0.050(9) 0.067(11) 0.057(12) 0.035(10) -0.007(9) -0.021(8) C12 0.062(10) 0.064(9) 0.035(10) -0.005(8) 0.002(9) -0.021(8) C13 0.028(7) 0.042(8) 0.046(11) -0.002(7) 0.010(7) -0.003(6) C14 0.079(12) 0.049(9) 0.046(11) -0.004(8) -0.019(10) -0.007(8) C15 0.095(14) 0.052(10) 0.059(13) -0.006(12) -0.023(12) -0.010(11) C16 0.071(13) 0.069(13) 0.096(19) -0.004(13) -0.043(15) -0.019(10) C17 0.047(11) 0.077(13) 0.13(2) 0.011(14) 0.012(13) 0.014(9) C18 0.057(10) 0.064(10) 0.061(12) -0.007(10) 0.011(9) -0.003(9) C19 0.055(9) 0.054(10) 0.068(13) -0.015(9) 0.011(9) 0.010(7) 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(5) . 7_665 ? Br1 Pb1 Br2 84.65(4) . 7_655 ? Br1 Pb1 Br3 170.09(4) . 7_665 ? Br2 Pb1 Br1 84.63(4) . 7_665 ? Br2 Pb1 Br1 91.22(4) . . ? Br2 Pb1 Br1 93.34(4) 7_655 7_665 ? Br2 Pb1 Br2 174.93(7) . 7_655 ? Br2 Pb1 Br3 81.48(4) . 7_665 ? Br3 Pb1 Br1 84.53(4) . . ? Br3 Pb1 Br1 83.94(4) 7_665 7_665 ? Br3 Pb1 Br1 171.19(4) . 7_665 ? Br3 Pb1 Br2 81.47(4) . 7_655 ? Br3 Pb1 Br2 102.95(4) 7_665 7_655 ? Br3 Pb1 Br2 101.10(4) . . ? Br3 Pb1 Br3 90.26(5) . 7_665 ? Pb1 Br1 Pb1 79.27(4) . 7_655 ? Pb1 Br2 Pb1 79.59(3) . 7_665 ? Pb1 Br3 Pb1 79.74(4) . 7_655 ? C1 P1 C7 111.8(7) . . ? C1 P1 C13 108.8(6) . . ? C1 P1 C19 108.9(7) . . ? C13 P1 C7 108.2(6) . . ? C19 P1 C7 109.0(7) . . ? C19 P1 C13 110.2(8) . . ? C2 C1 P1 120.4(12) . . ? C6 C1 P1 120.2(11) . . ? C6 C1 C2 119.2(13) . . ? C3 C2 C1 119.6(16) . . ? C4 C3 C2 121.5(16) . . ? C3 C4 C5 120.3(16) . . ? C6 C5 C4 118.8(17) . . ? C1 C6 C5 120.5(15) . . ? C8 C7 P1 123.5(11) . . ? C8 C7 C12 122.3(14) . . ? C12 C7 P1 114.1(12) . . ? C9 C8 C7 119.5(15) . . ? C8 C9 C10 119.9(16) . . ? C9 C10 C11 120.8(14) . . ? C12 C11 C10 120.4(14) . . ? C11 C12 C7 117.0(15) . . ? C14 C13 P1 121.3(12) . . ? C14 C13 C18 121.4(15) . . ? C18 C13 P1 117.2(13) . . ? C13 C14 C15 119.3(17) . . ? C16 C15 C14 120(2) . . ? C15 C16 C17 122(2) . . ? C16 C17 C18 119(2) . . ? C13 C18 C17 118.1(19) . . ? 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 3.0690(15) 7_665 ? Pb1 Br1 3.0507(16) . ? Pb1 Br2 3.0410(16) . ? Pb1 Br2 3.0583(16) 7_655 ? Pb1 Br3 3.0366(15) . ? Pb1 Br3 3.0534(16) 7_665 ? Br1 Pb1 3.0691(15) 7_655 ? Br2 Pb1 3.0584(15) 7_665 ? Br3 Pb1 3.0534(16) 7_655 ? P1 C1 1.790(13) . ? P1 C7 1.824(14) . ? P1 C13 1.797(14) . ? P1 C19 1.791(15) . ? C1 C2 1.390(19) . ? C1 C6 1.38(2) . ? C2 C3 1.36(2) . ? C3 C4 1.35(2) . ? C4 C5 1.39(2) . ? C5 C6 1.39(2) . ? C7 C8 1.36(2) . ? C7 C12 1.406(19) . ? C8 C9 1.36(2) . ? C9 C10 1.37(2) . ? C10 C11 1.38(2) . ? C11 C12 1.37(2) . ? C13 C14 1.37(2) . ? C13 C18 1.383(19) . ? C14 C15 1.39(2) . ? C15 C16 1.35(2) . ? C16 C17 1.37(3) . ? C17 C18 1.41(2) . ?