#------------------------------------------------------------------------------ #$Date: 2019-02-22 05:40:34 +0200 (Fri, 22 Feb 2019) $ #$Revision: 213785 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/15/2021524.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2021524 loop_ _publ_author_name 'Cheng, Ling' 'Cao, Yingjie' _publ_section_title ; A two-dimensional organic--inorganic hybrid perovskite-type semiconductor: poly[(2-azaniumylethyl)trimethylphosphanium [tetra-\m-bromido-plumbate(II)]] ; _journal_coeditor_code KU3234 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229619001712 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac '(C5 H16 N P) [Pb Br4]' _chemical_formula_moiety 'C5 H16 N P 2+, Br4 Pb1 2-' _chemical_formula_sum 'C5 H16 Br4 N P Pb' _chemical_formula_weight 647.99 _chemical_name_systematic ; Poly[(2-azaniumylethyl)trimethylphosphanium [tetra-\m-bromido-plumbate(II)]] ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90.43(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.0127(12) _cell_length_b 12.056(2) _cell_length_c 9.962(2) _cell_measurement_reflns_used 2927 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 3.380 _cell_volume 722.1(2) _computing_cell_refinement ; CrystalClear (Rigaku, 2005) ; _computing_data_collection ; CrystalClear (Rigaku, 2005) ; _computing_data_reduction ; CrystalClear (Rigaku, 2005) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2005) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 13.6612 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku SCXmini' _diffrn_measurement_method CCD_Profile_fitting _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_unetI/netI 0.0705 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 5045 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_min 3.380 _exptl_absorpt_coefficient_mu 22.820 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrystalClear; Rigaku, 2005) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.980 _exptl_crystal_description prism _exptl_crystal_F_000 580 _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _refine_diff_density_max 1.618 _refine_diff_density_min -1.797 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.501(17) _refine_ls_extinction_coef 0.0255(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2014 (Sheldrick, 2015) ; _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 3093 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0374 _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^)+(0.0192P)^2^+1.5138P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.0826 _reflns_number_gt 2927 _reflns_number_total 3093 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ku3234sup1.cif _cod_data_source_block I _cod_database_code 2021524 _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. ; _shelx_hkl_file ; 0 0 2 566.62 16.74 0 0 -2 606.89 16.32 0 0 3 1475.83 68.64 0 0 3 1801.76 72.66 0 0 4 1339.40 61.45 0 0 4 1257.54 64.26 0 0 5 293.54 13.18 0 0 5 306.47 14.13 0 0 6 388.28 19.99 0 0 6 337.60 14.71 0 0 7 1126.59 60.63 0 0 7 1167.63 75.27 0 0 8 51.20 5.59 0 0 8 44.28 3.68 0 0 9 34.84 5.31 0 0 9 35.32 3.55 0 0 10 211.16 11.54 0 0 10 224.29 18.90 0 0 11 61.55 8.71 0 0 12 11.46 4.94 0 -1 2 13.99 0.58 0 1 2 16.35 0.91 0 1 2 15.79 0.70 0 -1 2 15.77 0.97 0 -1 3 268.00 9.85 0 1 3 300.53 8.70 0 1 3 306.96 10.20 0 -1 3 291.66 7.72 0 1 4 131.13 4.71 0 -1 4 107.15 3.65 0 -1 4 119.48 5.38 0 1 4 131.39 5.57 0 1 5 101.29 5.27 0 1 5 96.31 4.82 0 -1 5 86.28 3.75 0 -1 5 98.96 5.42 0 -1 6 133.26 7.91 0 1 6 137.32 7.90 0 -1 6 128.99 5.80 0 1 6 134.43 7.68 0 1 7 234.78 13.88 0 -1 7 234.11 14.78 0 1 7 263.08 15.46 0 -1 7 211.76 9.93 0 -1 8 7.33 2.19 0 1 8 25.52 2.92 0 1 8 12.03 3.45 0 -1 8 16.72 3.58 0 1 9 12.13 3.40 0 1 9 12.59 2.13 0 -1 9 6.92 3.77 0 -1 9 6.40 1.72 0 -1 10 173.48 9.24 0 -1 10 149.05 14.58 0 1 10 161.53 14.62 0 1 10 162.69 10.87 0 1 11 91.61 11.11 0 -1 11 93.25 11.38 0 -1 12 7.18 4.09 0 1 12 0.65 3.94 0 2 0 656.34 12.36 0 -2 0 631.90 11.41 0 2 0 613.88 10.44 0 -2 1 584.81 11.61 0 2 1 601.40 13.42 0 2 -1 588.92 11.62 0 2 2 230.94 5.55 0 -2 2 245.60 6.32 0 2 2 228.73 5.38 0 2 -2 225.28 4.96 0 -2 3 1057.32 40.65 0 2 3 952.62 34.36 0 2 3 1025.20 38.51 0 2 -3 1073.74 31.76 0 2 4 866.62 38.45 0 2 4 843.71 34.54 0 -2 4 883.48 40.74 0 2 -4 966.28 32.87 0 -2 5 132.33 7.60 0 2 5 136.74 7.37 0 2 5 161.40 6.94 0 2 -5 151.73 5.05 0 2 6 649.39 33.18 0 -2 6 680.06 36.99 0 2 6 637.60 33.98 0 2 -6 622.06 25.34 0 -2 7 648.31 39.25 0 2 7 623.84 36.65 0 2 7 660.59 39.45 0 2 -7 625.82 27.59 0 2 8 360.86 23.99 0 2 8 373.04 24.78 0 -2 8 375.85 25.54 0 2 9 267.10 17.79 0 2 9 214.29 17.41 0 -2 9 207.47 17.63 0 2 10 331.86 21.81 0 -2 10 387.57 31.04 0 2 10 378.67 29.54 0 2 -10 422.20 22.22 0 -2 11 187.22 18.85 0 2 11 198.57 18.73 0 -2 12 45.00 8.02 0 2 12 41.74 8.13 0 3 0 2.27 0.51 0 -3 0 3.55 0.41 0 3 1 308.12 7.26 0 -3 1 296.19 6.25 0 3 -1 293.27 6.49 0 -3 2 29.91 1.26 0 3 2 31.43 1.32 0 3 -2 30.18 1.09 0 3 3 61.73 2.30 0 3 3 64.01 2.22 0 -3 3 61.03 2.49 0 3 -3 58.34 1.94 0 -3 4 268.11 11.10 0 3 4 259.92 9.65 0 3 4 276.82 10.70 0 3 -4 276.56 8.54 0 3 5 241.54 10.02 0 3 5 215.62 10.15 0 -3 5 215.90 10.93 0 3 -5 217.43 7.85 0 -3 6 39.50 3.99 0 3 6 43.69 3.65 0 3 6 34.13 3.74 0 3 -6 38.92 2.64 0 3 7 129.42 8.56 0 3 7 140.34 8.43 0 -3 7 134.21 9.26 0 3 -7 117.53 5.49 0 -3 8 185.71 12.81 0 3 8 143.72 11.50 0 3 8 185.03 12.71 0 3 -8 167.27 7.65 0 -3 9 14.87 4.13 0 3 9 11.64 3.75 0 3 9 21.33 3.53 0 -3 10 108.51 11.74 0 3 10 108.12 10.73 0 3 10 128.12 12.97 0 3 -10 102.25 7.27 0 3 11 47.75 8.63 0 -3 11 69.03 8.98 0 -3 12 11.45 4.67 0 3 12 10.41 4.95 0 -4 0 1541.40 50.01 0 4 0 1591.94 50.85 0 -4 1 987.46 26.64 0 4 1 982.11 30.64 0 -4 -1 968.64 26.22 0 4 -1 1004.28 29.92 0 -4 2 1043.74 32.98 0 4 2 983.98 30.07 0 4 2 1018.94 35.82 0 4 -2 1017.81 32.45 0 -4 3 1175.40 45.28 0 4 3 1122.33 45.16 0 4 3 1129.85 41.27 0 4 -3 1129.41 41.51 0 4 4 789.21 32.35 0 -4 4 831.94 34.90 0 4 4 782.75 32.75 0 4 -4 768.11 28.76 0 4 5 557.93 25.38 0 -4 5 544.73 25.65 0 4 5 542.02 24.46 0 4 -5 564.54 22.94 0 4 6 557.32 29.21 0 4 6 526.04 27.81 0 -4 6 548.84 30.64 0 4 -6 523.19 22.82 0 -4 7 448.26 27.36 0 4 7 437.16 26.26 0 4 7 458.82 27.02 0 4 -7 431.65 21.98 0 4 8 48.44 5.26 0 -4 8 49.24 6.28 0 4 8 59.88 5.40 0 4 -8 51.86 3.71 0 4 9 153.49 12.57 0 4 9 175.20 15.97 0 -4 9 168.19 14.38 0 4 -9 170.35 9.85 0 4 10 137.36 13.63 0 -4 10 126.65 12.67 0 4 10 125.82 11.91 0 -4 11 31.70 6.58 0 4 11 41.37 6.63 0 4 12 31.85 7.01 0 -4 12 32.98 7.22 0 -5 0 3.70 0.80 0 5 0 3.68 0.83 0 -5 1 232.05 6.02 0 5 1 221.08 7.12 0 5 -1 224.81 6.76 0 -5 -1 223.61 5.91 0 -5 2 81.86 2.66 0 5 2 87.97 3.43 0 5 -2 81.22 2.91 0 5 3 455.62 14.72 0 -5 3 403.02 14.47 0 5 3 413.11 15.79 0 5 -3 392.18 13.88 0 5 4 215.51 8.44 0 -5 4 229.57 10.22 0 5 4 219.43 9.11 0 5 -4 212.88 8.59 0 -5 5 89.68 5.25 0 5 5 91.66 5.11 0 5 5 91.23 4.84 0 5 -5 82.85 4.82 0 -5 6 268.32 14.78 0 5 6 268.77 13.46 0 5 6 280.26 14.50 0 5 -6 262.86 11.78 0 5 7 73.61 5.31 0 5 7 53.20 5.48 0 -5 7 56.80 5.75 0 5 -7 59.63 4.10 0 5 8 82.85 6.59 0 5 8 94.14 8.70 0 -5 8 70.76 7.19 0 5 -8 69.34 4.99 0 -5 9 64.42 7.55 0 5 9 67.04 6.83 0 5 9 78.75 8.72 0 5 -9 66.54 6.00 0 5 10 55.16 7.53 0 -5 10 75.66 8.78 0 5 10 65.43 10.19 0 5 11 91.85 10.80 0 -5 11 104.46 12.10 0 5 12 21.34 5.72 0 -5 12 20.23 6.12 0 -6 0 227.87 7.87 0 6 0 194.77 6.84 0 6 1 425.25 15.40 0 -6 1 439.66 13.94 0 -6 -1 439.06 13.00 0 6 -1 431.06 15.05 0 6 2 466.38 17.85 0 -6 2 468.43 15.21 0 6 -2 450.68 16.45 0 6 3 464.11 14.85 0 -6 3 435.54 16.15 0 6 3 451.28 18.47 0 6 -3 420.41 16.60 0 6 4 285.58 11.28 0 -6 4 289.36 12.45 0 6 4 302.13 13.36 0 6 -4 286.73 12.65 0 6 5 370.00 17.48 0 -6 5 379.02 18.13 0 6 5 385.81 18.50 0 6 -5 363.23 16.70 0 -6 6 684.62 38.48 0 6 6 613.94 32.80 0 6 6 681.92 38.63 0 6 -6 618.16 31.66 0 -6 7 191.31 12.18 0 6 7 171.05 10.86 0 6 7 180.79 10.92 0 6 -7 177.75 11.34 0 -6 8 269.35 19.20 0 6 8 287.59 19.57 0 6 8 260.59 19.94 0 6 -8 259.93 17.37 0 -6 9 361.76 27.76 0 6 9 388.91 28.58 0 6 9 337.52 26.62 0 6 -9 359.90 24.68 0 6 10 214.20 18.18 0 -6 10 194.92 18.37 0 6 10 177.66 15.31 0 6 11 53.56 7.74 0 -6 11 60.43 9.20 0 7 0 0.55 1.07 0 -7 0 0.01 0.95 0 -7 1 198.10 7.20 0 7 1 181.90 7.44 0 7 -1 174.54 7.27 0 -7 -1 191.31 5.70 0 -7 2 18.34 1.51 0 7 2 17.74 1.98 0 7 -2 16.91 1.71 0 7 3 17.86 2.07 0 7 3 11.30 1.25 0 -7 3 14.47 1.58 0 7 -3 16.37 1.74 0 -7 4 117.86 5.87 0 7 4 118.30 4.95 0 7 4 118.82 6.62 0 7 -4 119.09 6.66 0 -7 5 159.95 8.73 0 7 5 163.29 8.94 0 7 5 160.59 7.29 0 7 -5 155.75 8.29 0 -7 6 4.47 2.44 0 7 6 8.31 2.48 0 7 6 6.77 1.98 0 7 -6 11.46 2.13 0 7 7 63.62 6.23 0 7 7 65.62 5.90 0 -7 7 71.80 6.45 0 7 -7 59.46 5.19 0 7 8 184.35 13.89 0 -7 8 167.30 13.51 0 7 8 176.35 12.10 0 7 -8 163.10 11.31 0 7 9 30.23 5.33 0 7 9 28.18 5.29 0 -7 9 35.46 5.74 0 7 -9 27.29 4.12 0 7 10 37.91 7.45 0 -7 10 29.19 6.15 0 7 10 26.95 4.92 0 -7 11 26.64 6.13 0 7 11 18.27 4.98 0 8 0 524.92 23.45 0 -8 0 576.75 23.23 0 8 1 686.22 30.77 0 -8 1 697.28 29.37 0 8 -1 678.03 30.44 0 -8 -1 719.99 25.18 0 -8 2 947.05 41.80 0 8 2 961.64 35.68 0 8 2 945.08 45.95 0 8 -2 905.86 43.45 0 8 3 453.15 21.95 0 -8 3 452.44 20.23 0 8 -3 436.21 20.66 0 8 4 289.05 15.10 0 8 4 285.53 11.68 0 -8 4 266.96 13.21 0 8 -4 298.64 14.12 0 -8 5 568.02 29.99 0 8 5 578.88 31.34 0 8 5 539.25 24.32 0 8 -5 547.91 29.67 0 8 6 326.79 18.73 0 -8 6 357.63 20.69 0 8 6 342.71 22.17 0 8 -6 317.74 18.71 0 8 7 94.87 6.86 0 8 7 103.40 8.33 0 -8 7 107.76 8.64 0 8 -7 89.65 7.42 0 -8 8 79.41 8.57 0 8 8 72.01 6.89 0 8 8 108.71 9.20 0 8 -8 77.34 7.36 0 8 9 170.01 14.61 0 -8 9 148.31 17.02 0 8 9 127.90 12.60 0 8 -9 156.44 12.14 0 8 10 33.68 5.39 0 -8 10 45.13 7.65 0 8 10 47.89 9.11 0 -8 11 9.91 5.23 0 -9 0 1.36 1.15 0 9 0 -1.60 1.48 0 9 1 9.25 1.91 0 -9 1 3.74 1.63 0 -9 -1 3.36 1.19 0 9 -1 7.84 1.77 0 -9 2 36.52 3.06 0 9 2 31.06 3.17 0 9 2 31.63 1.80 0 9 -2 27.58 2.90 0 9 3 42.18 4.11 0 -9 3 41.51 3.08 0 9 3 51.40 2.55 0 9 -3 43.09 3.74 0 -9 4 51.35 4.02 0 9 4 67.72 5.15 0 9 -4 64.06 4.86 0 -9 5 114.53 7.32 0 9 5 103.54 8.07 0 9 5 105.57 5.10 0 9 -5 119.21 7.71 0 9 6 52.05 4.63 0 -9 6 52.70 5.18 0 9 6 56.85 5.59 0 9 -6 43.79 5.01 0 -9 7 23.49 3.91 0 9 7 18.81 4.01 0 9 7 10.69 3.47 0 9 -7 18.06 4.50 0 9 8 64.10 6.97 0 9 8 50.90 6.60 0 -9 8 55.00 8.97 0 9 -8 57.61 7.73 0 9 9 67.57 7.22 0 -9 9 89.56 12.52 0 9 9 119.57 12.13 0 -9 10 20.39 5.26 0 9 10 4.05 4.91 0 10 0 261.88 13.89 0 -10 0 270.36 11.64 0 -10 1 180.38 8.98 0 10 1 155.31 9.10 0 10 -1 142.07 8.61 0 -10 -1 151.03 6.30 0 -10 2 210.87 10.88 0 10 2 197.71 8.14 0 10 2 202.26 11.27 0 10 -2 190.07 10.96 0 10 3 183.86 7.26 0 -10 3 173.46 9.12 0 10 3 193.37 11.10 0 10 -3 174.45 10.55 0 10 4 158.61 10.61 0 -10 4 150.68 10.43 0 10 4 167.91 7.32 0 10 -4 165.50 10.48 0 10 5 253.34 16.45 0 -10 5 243.33 14.54 0 10 -5 240.07 15.56 0 10 6 179.99 13.60 0 -10 6 188.21 14.60 0 10 6 168.23 10.82 0 10 -6 181.67 13.37 0 -10 7 175.74 13.81 0 10 7 182.37 14.42 0 10 7 140.94 9.68 0 10 -7 168.81 15.50 0 10 8 186.77 15.85 0 -10 8 188.42 16.15 0 10 -8 160.36 15.41 0 10 9 177.03 17.35 0 -10 9 149.51 20.06 0 11 0 11.25 2.01 0 -11 0 0.03 1.16 0 -11 1 0.45 1.38 0 11 1 -0.70 1.94 0 11 -1 3.21 1.89 0 -11 -1 0.82 0.99 0 11 2 8.26 2.37 0 11 2 4.52 1.38 0 -11 2 7.65 2.31 0 11 -2 8.68 2.47 0 11 3 78.62 6.40 0 -11 3 82.02 5.54 0 11 3 70.60 4.06 0 11 -3 73.21 6.11 0 -11 4 9.95 2.96 0 11 4 12.71 3.10 0 11 4 10.63 1.90 0 11 -4 10.92 3.02 0 -11 5 41.40 4.56 0 11 5 37.42 5.40 0 11 -5 48.96 5.38 0 11 6 47.22 6.61 0 -11 6 57.15 5.86 0 11 -6 51.87 7.75 0 11 7 60.25 7.48 0 -11 7 42.89 6.52 0 11 -7 51.43 6.86 0 -11 8 23.78 5.90 0 11 8 34.99 6.19 0 11 -8 30.62 6.83 0 11 9 40.58 8.67 0 -11 9 57.85 10.17 0 -12 0 267.38 12.55 0 12 0 266.17 17.33 0 12 1 309.32 18.57 0 -12 1 302.86 15.05 0 12 -1 292.63 18.64 0 -12 2 367.67 20.98 0 12 2 278.38 18.66 0 12 -2 270.57 18.52 0 12 3 196.66 13.52 0 -12 3 200.96 12.58 0 12 -3 207.40 16.52 0 12 4 187.90 16.43 0 -12 4 200.59 15.45 0 12 -4 191.11 14.43 0 12 5 159.09 13.33 0 -12 5 173.19 12.80 0 12 -5 188.29 14.74 0 12 6 96.04 11.47 0 -12 6 91.73 8.98 0 12 -6 95.70 10.11 0 -12 7 63.75 7.84 0 12 7 65.19 8.96 0 12 -7 59.51 8.74 0 -12 8 83.79 10.35 0 12 8 74.52 10.17 0 13 0 -0.24 2.29 0 13 1 16.90 4.00 0 13 -1 26.38 3.90 0 13 2 16.95 3.57 0 13 -2 16.94 3.86 0 13 3 16.89 3.53 0 13 -3 9.29 3.81 0 13 4 12.27 3.93 0 13 -4 13.41 3.87 0 13 5 22.13 5.22 0 13 -5 36.73 5.65 0 13 6 44.83 6.97 0 13 -6 47.96 7.56 0 13 7 14.17 4.74 0 13 -7 6.28 4.90 0 14 0 85.03 8.58 0 14 1 37.45 5.74 0 14 -1 43.09 5.86 0 14 2 51.40 6.58 0 14 -2 49.50 6.56 0 14 3 60.29 7.26 0 14 -3 64.15 7.86 0 14 4 77.93 8.34 0 14 -4 64.30 9.04 0 14 5 65.41 8.05 0 14 -5 62.08 9.18 0 15 1 -0.82 2.71 0 15 -1 0.72 3.47 0 15 2 15.36 3.96 0 15 -2 6.74 4.33 0 15 3 40.34 7.42 0 15 -3 31.57 6.01 -1 0 12 -0.95 4.19 -1 0 11 32.94 6.47 -1 0 11 28.65 5.09 -1 0 10 35.83 6.07 -1 0 10 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113.51 13.80 -6 -1 6 94.62 12.66 -6 -1 6 70.62 10.21 -6 1 6 97.58 12.49 -6 1 6 77.95 9.08 -6 -1 5 0.83 3.95 -6 1 5 3.55 4.04 -6 -1 5 1.94 3.24 -6 1 5 3.01 2.98 -6 -1 4 40.99 6.88 -6 -1 4 38.25 5.86 -6 1 4 28.03 4.63 -6 1 4 30.13 6.68 -6 -1 3 97.20 9.34 -6 -1 3 96.39 11.04 -6 1 3 87.89 7.47 -6 1 3 101.48 10.64 -6 -1 2 39.01 6.16 -6 -1 2 38.48 5.93 -6 1 2 40.34 4.31 -6 1 2 36.65 6.07 -6 -1 1 0.64 1.79 -6 -1 1 -0.41 2.30 -6 1 1 -2.95 2.37 -6 1 1 -0.23 3.20 6 1 0 32.14 5.19 6 -1 0 55.71 5.36 -6 -1 0 36.91 5.15 -6 1 0 45.14 4.76 6 1 1 26.11 4.34 6 1 1 28.85 4.17 6 -1 1 21.45 3.67 -6 1 -1 28.94 3.31 6 1 2 5.75 3.56 6 1 2 6.69 2.12 6 -1 2 5.51 2.76 6 -1 2 3.30 1.75 6 1 3 4.72 3.41 6 -1 3 -2.62 2.34 6 1 4 15.10 4.56 6 -1 4 17.01 4.94 6 1 5 1.32 3.43 6 -1 5 2.39 3.53 6 1 6 24.48 6.35 6 -1 6 17.35 5.36 6 1 7 2.38 5.60 6 -1 7 5.26 4.39 6 1 8 -5.94 4.92 6 -1 8 0.79 5.98 -6 -2 8 84.94 15.14 -6 -2 8 122.03 16.21 -6 2 8 119.21 16.14 -6 -2 7 227.57 26.76 -6 2 7 231.84 30.35 -6 -2 7 195.61 24.74 -6 -2 6 212.01 23.36 -6 -2 6 185.28 19.45 -6 2 6 224.69 23.68 -6 -2 5 263.77 25.41 -6 -2 5 217.42 20.69 -6 2 5 251.85 25.11 -6 -2 4 222.17 18.58 -6 -2 4 217.75 19.76 -6 2 4 233.18 17.54 -6 2 4 231.04 22.59 6 2 -3 431.90 33.87 -6 -2 3 350.05 27.23 -6 2 3 360.87 31.16 -6 2 3 351.26 21.45 6 2 -2 357.46 28.01 -6 -2 2 306.05 22.06 -6 2 2 309.09 25.56 -6 2 2 314.04 18.26 6 2 -1 216.29 16.28 -6 -2 1 184.32 14.29 -6 2 1 191.54 15.84 6 2 0 478.05 35.08 6 -2 0 516.42 30.20 -6 -2 0 445.61 31.53 -6 2 0 449.82 33.91 6 2 1 263.29 17.52 6 2 1 336.73 21.85 6 -2 1 306.18 18.90 -6 2 -1 307.63 18.51 6 2 2 187.94 12.29 6 2 2 264.36 17.82 6 -2 2 221.45 13.82 6 2 3 256.07 19.45 6 -2 3 239.06 16.72 6 -2 4 326.93 29.10 6 2 4 354.18 29.07 6 2 5 173.19 18.42 6 -2 5 181.86 17.20 6 2 6 122.80 14.36 6 -2 6 82.26 11.60 6 2 7 229.88 25.15 6 -2 7 217.65 23.76 6 2 8 100.68 16.38 6 -2 8 127.99 15.80 6 3 -7 87.24 11.68 -6 -3 7 39.59 9.22 -6 3 7 47.14 10.38 6 3 -6 45.93 11.26 -6 -3 6 71.83 9.54 -6 3 6 63.23 11.31 6 3 -5 21.65 6.75 -6 -3 5 20.60 5.37 -6 3 5 20.04 6.79 6 3 -4 67.67 11.51 -6 -3 4 50.68 8.23 -6 3 4 56.21 9.45 6 3 -3 67.63 8.52 -6 -3 3 43.30 8.64 -6 3 3 43.89 8.21 6 3 -2 34.67 5.84 -6 -3 2 22.56 4.80 -6 3 2 26.57 5.54 6 3 -1 12.37 3.88 6 -3 -1 10.11 2.66 -6 -3 1 14.44 3.74 -6 3 1 16.04 4.14 6 3 0 38.41 4.71 6 -3 0 36.17 3.67 -6 -3 0 26.26 5.20 -6 3 0 25.37 4.48 6 3 1 14.17 3.39 6 3 1 8.00 3.55 6 -3 1 7.51 2.69 -6 3 -1 8.56 2.57 6 3 2 1.55 1.74 6 3 2 0.80 3.82 6 -3 2 2.96 1.98 6 3 3 44.29 6.08 6 -3 3 29.17 4.78 6 3 4 16.03 5.16 6 -3 4 21.23 3.93 6 3 5 2.04 4.01 6 -3 5 5.12 3.25 6 3 6 -7.29 4.55 6 -3 6 8.66 4.26 6 3 7 8.10 5.20 6 -3 7 -0.07 5.09 6 4 -7 59.56 11.85 -6 -4 7 58.74 12.22 -6 4 7 53.75 11.87 6 4 -6 215.45 25.25 -6 -4 6 187.33 25.03 -6 4 6 198.44 24.13 6 4 -5 176.11 20.17 -6 -4 5 124.88 15.44 -6 4 5 172.54 22.07 6 4 -4 221.11 22.38 -6 -4 4 174.45 18.92 -6 4 4 197.97 24.67 6 4 -3 330.57 29.27 -6 -4 3 292.30 25.48 -6 4 3 326.16 33.34 6 4 -2 405.03 33.76 -6 -4 2 371.79 29.02 -6 4 2 399.21 38.05 6 4 -1 306.74 25.39 -6 4 1 371.55 34.77 -6 -4 1 337.61 24.53 6 4 0 296.07 22.70 -6 -4 0 322.94 23.82 -6 4 0 316.13 23.55 6 4 1 427.90 30.25 -6 -4 -1 546.45 37.62 -6 4 -1 487.70 33.19 6 4 2 312.09 22.12 6 4 2 351.60 26.67 6 4 3 336.00 25.18 6 -4 3 267.27 18.08 6 4 4 394.48 30.91 6 -4 4 294.91 25.71 6 4 5 250.72 21.97 6 -4 5 198.30 18.08 6 4 6 206.88 21.52 6 -4 6 159.37 16.98 6 4 7 131.47 19.69 6 5 -7 40.34 9.43 -6 -5 7 30.58 8.68 -6 5 7 46.69 11.24 6 5 -6 30.66 8.54 -6 -5 6 31.21 8.01 -6 5 6 46.03 10.26 6 5 -5 43.09 9.46 -6 -5 5 37.06 8.85 -6 5 5 59.03 10.73 6 5 -4 36.00 8.05 -6 -5 4 32.56 7.16 -6 5 4 41.13 9.14 6 5 -3 17.82 6.03 -6 -5 3 26.19 6.69 -6 5 3 27.64 7.75 6 5 -2 45.25 6.88 -6 -5 2 32.13 6.03 -6 5 2 28.56 8.14 6 5 -1 41.64 6.50 -6 -5 1 42.16 6.32 -6 5 1 42.97 7.26 6 5 0 12.31 3.78 -6 -5 0 12.87 3.98 -6 5 0 12.26 4.20 6 5 1 14.64 4.49 -6 -5 -1 19.56 4.70 -6 5 -1 20.39 4.20 6 5 2 3.58 3.43 6 5 2 7.99 3.64 6 5 3 21.05 5.28 6 5 4 -3.10 3.98 6 5 5 20.52 6.05 6 5 6 28.58 7.83 6 5 7 15.86 7.32 6 6 -6 188.65 23.69 -6 -6 6 150.16 21.25 -6 6 6 207.53 28.32 6 6 -5 186.50 23.77 -6 6 5 228.32 29.29 -6 -6 5 178.14 21.98 6 6 -4 101.95 15.68 -6 -6 4 109.91 14.31 -6 6 4 124.54 18.24 6 6 -3 183.41 21.39 -6 -6 3 185.71 18.63 -6 6 3 208.85 25.19 6 6 -2 246.01 24.72 -6 -6 2 259.05 21.80 -6 6 2 265.46 30.02 6 6 -1 131.83 13.66 -6 -6 1 142.70 13.43 -6 6 1 142.71 17.28 6 6 0 151.61 14.17 -6 -6 0 171.73 14.90 -6 6 0 170.79 21.09 6 6 1 243.19 22.20 -6 -6 -1 240.41 20.21 -6 6 -1 241.07 22.23 6 6 2 212.54 19.02 6 6 2 219.06 18.87 6 6 3 144.87 14.91 6 6 4 142.80 15.39 6 6 5 182.66 20.62 6 6 6 120.53 15.46 6 7 -6 24.01 8.34 -6 -7 6 13.35 7.24 -6 7 6 29.98 9.92 6 7 -5 51.11 10.83 -6 -7 5 42.14 9.82 -6 7 5 52.34 15.74 6 7 -4 55.28 11.21 -6 -7 4 50.46 9.50 -6 7 4 71.32 12.35 6 7 -3 -1.09 4.65 -6 -7 3 1.81 4.81 -6 7 3 8.72 5.23 6 7 -2 20.06 6.36 -6 -7 2 26.00 5.59 -6 7 2 23.43 7.00 6 7 -1 50.00 7.96 -6 -7 1 49.45 7.15 -6 7 1 29.03 10.01 6 7 0 26.81 8.10 -6 -7 0 23.61 5.49 -6 7 0 22.45 5.88 6 7 1 0.10 3.36 -6 -7 -1 3.60 3.34 6 7 2 11.22 3.41 6 7 2 0.61 3.79 6 7 3 16.78 6.12 6 7 4 11.26 4.74 6 7 5 9.33 5.10 6 8 -5 100.67 17.81 -6 -8 5 87.23 15.17 -6 8 5 120.34 18.50 6 8 -4 86.10 15.32 -6 -8 4 98.74 13.62 -6 8 4 110.85 17.50 6 8 -3 127.81 18.49 -6 -8 3 139.38 14.81 -6 8 3 138.08 20.44 6 8 -2 181.05 23.26 -6 -8 2 197.18 19.35 -6 8 2 226.99 27.62 6 8 -1 275.26 28.49 -6 -8 1 209.65 20.34 -6 8 1 220.14 31.71 6 8 0 170.77 22.59 -6 -8 0 167.89 15.80 -6 8 0 152.65 23.04 6 8 1 232.31 21.83 -6 -8 -1 212.07 19.47 6 8 2 214.85 19.29 6 8 2 232.77 21.01 6 8 3 177.25 18.34 6 8 4 124.78 13.80 6 9 -3 0.12 5.52 -6 -9 3 0.81 4.07 -6 9 3 11.16 6.26 6 9 -2 17.65 8.30 -6 -9 2 15.39 5.07 -6 9 2 16.02 9.64 6 9 -1 53.31 9.94 -6 -9 1 30.80 7.22 -6 9 1 51.74 10.49 6 9 0 3.37 4.45 -6 -9 0 -4.93 3.59 6 9 1 21.48 5.18 -6 -9 -1 -4.21 4.09 6 9 2 2.81 3.43 6 9 2 1.73 3.55 6 9 3 -4.05 4.12 6 10 0 107.55 16.70 -6 -10 0 117.24 13.36 -7 0 5 32.33 8.54 -7 0 4 26.42 7.12 -7 0 3 88.09 11.97 -7 0 3 95.10 9.48 -7 0 2 31.45 5.23 -7 0 2 40.98 6.49 -7 0 1 27.93 4.75 -7 0 1 60.93 5.89 7 0 0 136.80 11.91 7 0 0 130.36 11.70 7 0 1 82.38 8.50 7 0 2 62.14 8.04 7 0 3 87.08 11.51 7 0 4 122.08 16.20 7 0 5 22.99 6.06 -7 -1 5 24.48 9.91 -7 -1 5 31.22 7.89 -7 1 5 34.52 8.28 -7 -1 4 21.42 6.16 -7 -1 4 24.82 6.74 -7 1 4 18.03 6.69 -7 -1 3 88.35 9.88 -7 1 3 97.52 12.21 7 1 -2 26.48 5.91 -7 -1 2 15.31 4.74 -7 1 2 28.89 5.56 7 1 -1 11.80 3.84 7 -1 -1 4.86 3.56 -7 -1 1 3.90 3.40 -7 1 1 7.25 3.56 7 1 0 28.17 4.50 7 1 0 17.10 4.56 7 -1 0 22.24 4.25 -7 1 0 22.35 4.23 7 1 1 28.07 5.18 7 -1 1 24.22 4.30 7 1 2 0.11 4.13 7 -1 2 5.84 3.12 7 1 3 11.76 4.79 7 -1 3 14.98 4.87 7 1 4 9.61 4.93 7 -1 4 16.08 4.53 7 -1 5 8.72 5.04 7 1 5 5.70 4.80 7 2 -5 39.15 8.59 -7 -2 5 20.42 6.41 -7 2 5 26.94 7.78 7 2 -4 85.82 12.27 -7 -2 4 58.59 8.88 -7 2 4 80.99 13.44 7 2 -3 49.56 9.29 -7 -2 3 46.96 7.01 -7 2 3 51.59 8.75 7 2 -2 78.91 9.60 -7 -2 2 59.25 7.98 -7 2 2 51.18 9.00 7 2 -1 21.28 5.55 -7 -2 1 27.47 5.27 -7 2 1 27.21 4.97 7 2 0 48.29 6.74 7 2 0 78.58 7.92 -7 2 0 54.50 6.78 7 2 1 80.33 9.70 7 2 2 5.68 3.73 7 2 3 81.64 12.95 7 2 4 53.75 10.60 7 2 5 28.00 9.03 7 3 -5 29.99 9.57 -7 -3 5 17.66 6.14 -7 3 5 24.46 7.58 7 3 -4 37.41 11.56 -7 -3 4 44.14 7.27 -7 3 4 47.28 9.19 7 3 -3 86.74 10.44 -7 -3 3 51.66 8.12 -7 3 3 48.06 9.89 7 3 -2 18.41 4.99 -7 -3 2 16.01 4.62 -7 3 2 8.37 5.19 7 3 -1 29.33 5.83 -7 -3 1 40.06 7.00 -7 3 1 19.35 6.89 7 3 0 25.08 5.47 -7 -3 0 20.02 5.27 7 3 1 7.51 3.74 7 3 2 -1.88 3.59 7 3 3 5.21 3.98 7 3 4 0.53 3.82 7 3 5 17.46 6.22 7 4 -4 33.59 7.23 -7 -4 4 15.58 6.01 -7 4 4 32.37 7.24 7 4 -3 99.45 12.58 -7 -4 3 72.86 10.87 -7 4 3 89.98 14.30 7 4 -2 77.91 10.89 -7 -4 2 58.38 8.51 -7 4 2 53.31 8.77 7 4 -1 73.16 7.82 -7 -4 1 48.13 7.89 -7 4 1 42.64 7.76 7 4 0 112.63 11.05 -7 -4 0 120.42 12.75 7 4 1 81.60 10.11 7 4 2 98.00 11.81 7 4 3 66.30 9.47 7 4 4 127.66 15.93 7 5 -4 42.43 9.23 -7 -5 4 36.11 7.82 -7 5 4 41.40 9.60 7 5 -3 37.79 7.14 -7 -5 3 18.45 6.00 -7 5 3 18.12 7.41 7 5 -2 28.34 6.28 -7 -5 2 12.84 5.44 -7 5 2 20.56 7.52 7 5 -1 19.07 6.07 -7 -5 1 6.56 4.94 -7 5 1 20.85 5.97 7 5 0 12.23 4.12 -7 -5 0 17.21 4.92 7 5 1 27.38 6.09 7 5 2 4.08 4.15 7 5 3 22.12 5.93 7 6 -2 93.57 12.06 -7 -6 2 73.59 10.36 -7 6 2 64.32 13.85 7 6 -1 24.84 6.52 -7 -6 1 38.50 6.72 7 6 0 28.63 5.86 -7 -6 0 26.88 6.40 7 6 1 67.60 9.67 7 6 2 37.21 7.62 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 87267 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P2(1) CELL 0.71073 6.0127 12.0565 9.9620 90.000 90.434 90.000 ZERR 2.00 0.0012 0.0024 0.0020 0.000 0.030 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N P Br Pb UNIT 10 32 2 2 8 2 L.S. 10 ACTA BOND FMAP 2 PLAN 20 HTAB C2 Br2_$1 HTAB C2 Br4_$1 HTAB C2 Br4_$5 HTAB N1 Br3_$2 HTAB N1 Br1_$4 HTAB N1 Br1 HTAB C5 Br4_$5 EQIV $5 -x+2, y-1/2, -z+2 HTAB C5 Br4_$4 EQIV $4 -x+1, y-1/2, -z+2 HTAB C1 Br1_$3 EQIV $3 -x+1, y-1/2, -z+1 HTAB C4 Br3_$2 EQIV $2 x-1, y, z HTAB C4 Br3 HTAB C3 Br4_$1 EQIV $1 x, y, z-1 TWIN -1 0 0 0 -1 0 0 0 -1 2 DFIX 1.54 C4 C5 WGHT 0.019200 1.513800 EXTI 0.025494 BASF 0.50120 FVAR 0.19828 MOLE 1 PB1 6 0.994408 0.475465 1.010835 11.00000 0.01156 0.01977 = 0.01761 -0.00125 0.00187 -0.00011 BR2 5 0.985753 0.221339 1.043421 11.00000 0.05156 0.01961 = 0.03320 0.00073 0.00738 0.00047 BR3 5 0.997601 0.407499 0.722788 11.00000 0.03305 0.04204 = 0.01919 -0.00492 -0.00243 0.00515 BR4 5 0.958640 0.508654 1.303956 11.00000 0.05070 0.05022 = 0.02108 -0.00896 0.00666 -0.01984 P1 4 0.594451 0.204729 0.425936 11.00000 0.01744 0.02518 = 0.02227 -0.00066 0.00334 0.00010 BR1 5 0.500767 0.492758 0.992299 11.00000 0.01115 0.04743 = 0.04801 -0.00853 -0.00074 0.00177 C3 1 0.490109 0.281952 0.288894 11.00000 0.01902 0.08331 = 0.03691 0.02955 -0.00072 0.00554 AFIX 137 H3A 2 0.585885 0.344129 0.272526 11.00000 -1.50000 H3B 2 0.343275 0.308059 0.309066 11.00000 -1.50000 H3C 2 0.484377 0.235697 0.210506 11.00000 -1.50000 AFIX 0 C4 1 0.503945 0.261316 0.579242 11.00000 0.02548 0.02433 = 0.02475 -0.00283 0.00863 -0.00376 AFIX 23 H4A 2 0.575526 0.332664 0.592154 11.00000 -1.20000 H4B 2 0.344970 0.274270 0.573137 11.00000 -1.20000 AFIX 0 C1 1 0.505901 0.066949 0.406675 11.00000 0.04490 0.04009 = 0.06042 -0.02650 0.01948 -0.01632 AFIX 137 H1A 2 0.356307 0.059785 0.438542 11.00000 -1.50000 H1B 2 0.602026 0.018850 0.457433 11.00000 -1.50000 H1C 2 0.510916 0.046822 0.313510 11.00000 -1.50000 AFIX 0 C5 1 0.550531 0.190058 0.700949 11.00000 0.02777 0.04352 = 0.02652 -0.01023 0.01156 0.00836 AFIX 23 H5A 2 0.484543 0.117465 0.687375 11.00000 -1.20000 H5B 2 0.709932 0.180244 0.710856 11.00000 -1.20000 AFIX 0 N1 3 0.462550 0.238559 0.823642 11.00000 0.06944 0.04886 = 0.02309 -0.00156 -0.00641 0.02956 AFIX 137 H1D 2 0.550024 0.294051 0.850196 11.00000 -1.50000 H1E 2 0.457961 0.187051 0.887557 11.00000 -1.50000 H1F 2 0.325957 0.264184 0.808071 11.00000 -1.50000 AFIX 0 C2 1 0.888222 0.206542 0.426685 11.00000 0.01724 0.04768 = 0.02726 0.00361 0.00842 -0.00966 AFIX 137 H2A 2 0.942964 0.161685 0.499375 11.00000 -1.50000 H2B 2 0.939652 0.281375 0.437905 11.00000 -1.50000 H2C 2 0.941703 0.177553 0.343182 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1 in P2(1) REM R1 = 0.0374 for 2927 Fo > 4sig(Fo) and 0.0404 for all 3093 data REM 115 parameters refined using 2 restraints END WGHT 0.0192 1.5139 REM Highest difference peak 1.618, deepest hole -1.797, 1-sigma level 0.268 Q1 1 1.0118 0.4234 0.9489 11.00000 0.05 1.62 Q2 1 1.0173 0.5260 0.9473 11.00000 0.05 1.50 Q3 1 0.9015 0.4202 1.0759 11.00000 0.05 1.28 Q4 1 1.0103 0.3786 1.0240 11.00000 0.05 1.25 Q5 1 0.9958 0.5395 1.0623 11.00000 0.05 1.15 Q6 1 1.0015 0.0860 1.1249 11.00000 0.05 1.12 Q7 1 1.0104 0.5733 1.0159 11.00000 0.05 1.05 Q8 1 0.9666 0.3925 1.1388 11.00000 0.05 1.03 Q9 1 0.9983 0.3562 0.8891 11.00000 0.05 1.02 Q10 1 0.9906 0.4667 1.2259 11.00000 0.05 0.96 Q11 1 1.0102 0.4814 0.5640 11.00000 0.05 0.95 Q12 1 1.0051 0.2729 0.9730 11.00000 0.05 0.94 Q13 1 1.0060 0.4437 0.6405 11.00000 0.05 0.92 Q14 1 1.0163 0.4868 0.6914 11.00000 0.05 0.91 Q15 1 1.0104 0.2636 0.5050 11.00000 0.05 0.91 Q16 1 0.9990 0.3578 0.6171 11.00000 0.05 0.89 Q17 1 0.9628 0.3603 0.7754 11.00000 0.05 0.89 Q18 1 1.0305 0.1221 0.5924 11.00000 0.05 0.87 Q19 1 0.9556 0.1204 0.4596 11.00000 0.05 0.85 Q20 1 1.0035 0.0874 0.3853 11.00000 0.05 0.85 ; _shelx_res_checksum 64504 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy Pb Pb1 0.99441(8) 0.47547(5) 1.01083(5) 0.01630(18) Uani d 1 Br Br2 0.9858(3) 0.22134(17) 1.04342(17) 0.0348(4) Uani d 1 Br Br3 0.9976(3) 0.40750(16) 0.72279(16) 0.0314(4) Uani d 1 Br Br4 0.9586(3) 0.50865(16) 1.30396(17) 0.0406(6) Uani d 1 P P1 0.5945(6) 0.2047(4) 0.4259(4) 0.0216(9) Uani d 1 Br Br1 0.5008(2) 0.4928(3) 0.99230(18) 0.0355(7) Uani d 1 C C3 0.490(3) 0.2820(19) 0.289(2) 0.046(6) Uani d 1 H H3A 0.5859 0.3441 0.2725 0.070 Uiso calc 1 H H3B 0.3433 0.3081 0.3091 0.070 Uiso calc 1 H H3C 0.4844 0.2357 0.2105 0.070 Uiso calc 1 C C4 0.504(3) 0.2613(12) 0.5792(17) 0.025(4) Uani d 1 H H4A 0.5755 0.3327 0.5922 0.030 Uiso calc 1 H H4B 0.3450 0.2743 0.5731 0.030 Uiso calc 1 C C1 0.506(3) 0.0669(16) 0.407(2) 0.048(6) Uani d 1 H H1A 0.3563 0.0598 0.4385 0.073 Uiso calc 1 H H1B 0.6020 0.0189 0.4574 0.073 Uiso calc 1 H H1C 0.5109 0.0468 0.3135 0.073 Uiso calc 1 C C5 0.551(3) 0.1901(15) 0.7009(16) 0.033(4) Uani d 1 H H5A 0.4845 0.1175 0.6874 0.039 Uiso calc 1 H H5B 0.7099 0.1802 0.7109 0.039 Uiso calc 1 N N1 0.463(3) 0.2386(14) 0.8236(14) 0.047(5) Uani d 1 H H1D 0.5500 0.2941 0.8502 0.071 Uiso calc 1 H H1E 0.4580 0.1871 0.8876 0.071 Uiso calc 1 H H1F 0.3260 0.2642 0.8081 0.071 Uiso calc 1 C C2 0.888(2) 0.2065(16) 0.4267(16) 0.031(4) Uani d 1 H H2A 0.9430 0.1617 0.4994 0.046 Uiso calc 1 H H2B 0.9397 0.2814 0.4379 0.046 Uiso calc 1 H H2C 0.9417 0.1776 0.3432 0.046 Uiso calc 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pb1 0.0116(3) 0.0198(3) 0.0176(3) -0.0001(2) 0.00187(18) -0.0012(3) Br2 0.0516(11) 0.0196(7) 0.0332(9) 0.0005(9) 0.0074(8) 0.0007(9) Br3 0.0330(10) 0.0420(9) 0.0192(8) 0.0051(8) -0.0024(7) -0.0049(7) Br4 0.0507(12) 0.0502(12) 0.0211(9) -0.0198(9) 0.0067(8) -0.0090(7) P1 0.0174(19) 0.025(2) 0.022(2) 0.0001(18) 0.0033(16) -0.0007(16) Br1 0.0111(7) 0.0474(19) 0.0480(10) 0.0018(8) -0.0007(7) -0.0085(9) C3 0.019(9) 0.083(15) 0.037(12) 0.006(10) -0.001(9) 0.030(11) C4 0.025(9) 0.024(8) 0.025(9) -0.004(7) 0.009(8) -0.003(6) C1 0.045(13) 0.040(10) 0.060(14) -0.016(10) 0.019(11) -0.026(11) C5 0.028(9) 0.044(11) 0.027(10) 0.008(9) 0.012(8) -0.010(8) N1 0.069(12) 0.049(10) 0.023(8) 0.030(9) -0.006(8) -0.002(7) C2 0.017(7) 0.048(10) 0.027(9) -0.010(8) 0.008(7) 0.004(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' N N 0.0061 0.0033 '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' 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br4 Pb1 Br1 . . 88.39(6) y Br4 Pb1 Br3 . . 171.02(6) y Br1 Pb1 Br3 . . 88.47(6) y Br4 Pb1 Br2 . . 91.67(5) y Br1 Pb1 Br2 . . 93.35(7) y Br3 Pb1 Br2 . . 80.13(5) y C1 P1 C4 . . 111.5(9) y C1 P1 C3 . . 108.0(12) y C4 P1 C3 . . 110.9(9) y C1 P1 C2 . . 108.3(9) y C4 P1 C2 . . 107.9(8) y C3 P1 C2 . . 110.3(8) y C5 C4 P1 . . 114.8(11) y N1 C5 C4 . . 112.2(14) y Br4 Pb1 Br2 . 2_757 92.71(5) ? Br1 Pb1 Br2 . 2_757 87.76(7) ? Br3 Pb1 Br2 . 2_757 95.57(5) ? Br4 Pb1 Br1 . 1_655 97.48(6) ? Br1 Pb1 Br1 . 1_655 169.41(10) ? Br3 Pb1 Br1 . 1_655 86.96(6) ? Br2 Pb1 Br1 2_757 1_655 83.19(7) ? Br2 Pb1 Br2 2_757 . 175.51(2) ? Br1 Pb1 Br2 1_655 . 95.26(7) ? Pb1 Br2 Pb1 2_747 . 163.28(6) ? Pb1 Br1 Pb1 . 1_455 169.41(10) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pb1 Br4 . 2.9568(18) y Pb1 Br1 . 2.9798(15) y Pb1 Br3 . 2.9844(17) y Pb1 Br2 2_757 3.016(2) ? Pb1 Br1 1_655 3.0587(16) ? Pb1 Br2 . 3.082(2) y C4 C5 . 1.510(17) y Br2 Pb1 2_747 3.016(2) ? P1 C1 . 1.754(18) y P1 C4 . 1.763(16) y P1 C3 . 1.764(17) y P1 C2 . 1.766(14) y Br1 Pb1 1_455 3.0587(15) ? C5 N1 . 1.46(2) y loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C2 H2C Br2 1_554 0.96 3.05 3.871(16) 144.9 C2 H2B Br4 1_554 0.96 3.05 3.866(19) 143.7 C2 H2A Br4 2_747 0.96 2.75 3.702(18) 170.1 N1 H1F Br3 1_455 0.89 2.75 3.596(15) 158.5 N1 H1E Br1 2_647 0.89 2.64 3.491(16) 160.0 N1 H1D Br1 . 0.89 2.80 3.502(16) 136.8 C5 H5B Br4 2_747 0.97 2.88 3.674(17) 140.1 C5 H5A Br4 2_647 0.97 2.97 3.762(19) 139.5 C1 H1C Br1 2_646 0.96 3.12 4.07(2) 176.0 C4 H4B Br3 1_455 0.97 3.04 3.806(17) 137.4 C4 H4A Br3 . 0.97 2.98 3.728(18) 134.5 C3 H3A Br4 1_554 0.96 3.01 3.93(2) 160.9 _cod_database_fobs_code 2021524