#------------------------------------------------------------------------------ #$Date: 2024-08-05 20:53:54 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293732 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/18/1571897.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_1571897 loop_ _publ_author_name 'Fan, Chang-Chun' 'Liu, Cheng-Dong' 'Liang, Bei-Dou' 'Ju, Tong-Yu' 'Wang, Wei' 'Jin, Ming-Liang' 'Chai, Chao-Yang' 'Zhang, Wen' _publ_section_title ; Chiral three-dimensional organic-inorganic lead iodide hybrid semiconductors. ; _journal_issue 29 _journal_name_full 'Chemical science' _journal_page_first 11374 _journal_page_last 11381 _journal_paper_doi 10.1039/d4sc00954a _journal_volume 15 _journal_year 2024 _chemical_absolute_configuration rmad _chemical_formula_moiety 'I6 Pb2, C7 H11 N2' _chemical_formula_sum 'C7 H11 I6 N2 Pb2' _chemical_formula_weight 1298.96 _space_group_crystal_system orthorhombic _space_group_IT_number 20 _space_group_name_Hall 'C 2c 2' _space_group_name_H-M_alt 'C 2 2 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-01-05 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-01-05 deposited with the CCDC. 2024-06-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 12.9873(5) _cell_length_b 18.8387(7) _cell_length_c 17.5741(8) _cell_measurement_reflns_used 5889 _cell_measurement_temperature 269.0(6) _cell_measurement_theta_max 30.7170 _cell_measurement_theta_min 2.2200 _cell_volume 4299.7(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 269.0(6) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.829 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 0.00 28.00 0.50 1.00 -- -6.24 -99.00 0.00 56 2 \w -15.00 28.00 0.50 1.00 -- -6.24 -99.00-120.00 86 3 \w -19.00 15.00 0.50 1.00 -- -6.24 57.00 150.00 68 4 \w 18.00 64.00 0.50 1.00 -- -6.24 78.00 150.00 92 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0032862000 _diffrn_orient_matrix_UB_12 -0.0011933000 _diffrn_orient_matrix_UB_13 0.0402848000 _diffrn_orient_matrix_UB_21 0.0289822000 _diffrn_orient_matrix_UB_22 -0.0318282000 _diffrn_orient_matrix_UB_23 -0.0024028000 _diffrn_orient_matrix_UB_31 0.0461462000 _diffrn_orient_matrix_UB_32 0.0200740000 _diffrn_orient_matrix_UB_33 -0.0013809000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_unetI/netI 0.0387 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.829 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 11070 _diffrn_reflns_point_group_measured_fraction_full 0.978 _diffrn_reflns_point_group_measured_fraction_max 0.758 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.503 _diffrn_reflns_theta_min 1.905 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 24.245 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.57418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'metallic dark red' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 4.013 _exptl_crystal_description block _exptl_crystal_F_000 4392 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 1.504 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.179 _refine_ls_abs_structure_details ; Flack x determined using 1538 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.006(8) _refine_ls_extinction_coef 0.000459(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 160 _refine_ls_number_reflns 4978 _refine_ls_number_restraints 60 _refine_ls_restrained_S_all 0.971 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0286 _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^)+(0.0266P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.0612 _reflns_Friedel_coverage 0.668 _reflns_Friedel_fraction_full 0.954 _reflns_Friedel_fraction_max 0.672 _reflns_number_gt 4276 _reflns_number_total 4978 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc00954a2.cif _cod_data_source_block 2R _cod_depositor_comments 'Adding full bibliography for 1571897--1571906.cif.' _cod_database_code 1571897 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C1 H1 N1 I1 Pb1' _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_estimated_absorpt_t_max 0.085 _shelx_estimated_absorpt_t_min 0.085 _olex2_refinement_description ; 1. Rigid body (RIGU) restrains C5, C1, H1A, H1B, H1C, C2, N1, H2, C3, H1D, H1E, H1F, C4, N2, H4, C7, H5, C6, H7, H6 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 2.a Ternary CH refined with riding coordinates: C2(H2) 2.b Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C7(H7), C6(H6) 2.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), N1(H1D,H1E,H1F) ; _shelx_res_file ; TITL fcc-126-02-1_a.res in C222(1) fcc-126-02-1.res created by SHELXL-2018/3 at 11:07:26 on 05-Jan-2024 CELL 0.71073 12.9873 18.8387 17.5741 90 90 90 ZERR 8 0.0005 0.0007 0.0008 0 0 0 LATT -7 SYMM -X,-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM +X,-Y,-Z SFAC C H I N Pb UNIT 56 88 48 16 16 RIGU C5 C1 H1a H1b H1c C2 N1 H2 C3 H1d H1e H1f C4 N2 H4 C7 H5 C6 H7 H6 L.S. 60 PLAN 1 SIZE 0.2 0.2 0.2 TEMP -24 CONF BOND LIST 4 MORE -1 BOND $H fmap 2 acta OMIT 7 5 11 OMIT 4 0 0 OMIT 0 4 4 OMIT 0 2 0 OMIT 2 0 0 OMIT 0 0 8 OMIT 4 4 4 OMIT -4 4 4 REM REM REM WGHT 0.026600 EXTI 0.000459 FVAR 0.05460 PB2 5 0.996154 0.376352 0.380892 11.00000 0.03688 0.03791 = 0.02850 0.00144 0.00062 0.00253 PB1 5 0.506569 0.377434 0.378983 11.00000 0.03574 0.03273 = 0.02561 0.00029 0.00121 -0.00039 I6 3 0.500000 0.500790 0.250000 10.50000 0.04089 0.03484 = 0.03146 0.00000 0.00487 0.00000 I5 3 0.539820 0.500000 0.500000 10.50000 0.05791 0.05329 = 0.04366 -0.02313 0.00000 0.00000 I8 3 0.500000 0.259558 0.250000 10.50000 0.03276 0.03255 = 0.03042 0.00000 -0.00399 0.00000 I4 3 0.754224 0.358739 0.362193 11.00000 0.02245 0.04086 = 0.06038 -0.00991 0.00033 0.00077 I9 3 0.257669 0.405115 0.393932 11.00000 0.02981 0.04998 = 0.05530 0.00637 0.00394 0.00474 I3 3 1.000000 0.254794 0.250000 10.50000 0.03122 0.03974 = 0.03692 0.00000 0.00450 0.00000 I1 3 0.958592 0.500000 0.500000 10.50000 0.05931 0.05631 = 0.03771 -0.01863 0.00000 0.00000 I7 3 0.484199 0.264063 0.508149 11.00000 0.09097 0.05080 = 0.04341 0.02086 0.01733 0.01184 C1 1 0.341554 0.125178 0.112117 11.00000 0.05992 0.09865 = 0.03208 -0.00301 0.00538 -0.01164 AFIX 137 H1A 2 0.353522 0.074933 0.120325 11.00000 -1.50000 H1B 2 0.397506 0.152260 0.134343 11.00000 -1.50000 H1C 2 0.338071 0.134668 0.057929 11.00000 -1.50000 AFIX 0 C4 1 0.252242 0.073466 0.273386 11.00000 0.03251 0.02796 = 0.04917 0.00038 -0.00383 0.00073 AFIX 43 H4 2 0.253356 0.030648 0.245935 11.00000 -1.20000 AFIX 0 C5 1 0.256368 0.072316 0.350731 11.00000 0.03722 0.04614 = 0.04539 0.01011 -0.00958 -0.00775 AFIX 43 H5 2 0.258757 0.028723 0.376695 11.00000 -1.20000 AFIX 0 C7 1 0.254502 0.197322 0.350735 11.00000 0.05009 0.05073 = 0.06769 -0.02315 0.00044 -0.00268 AFIX 43 H7 2 0.257278 0.240735 0.377022 11.00000 -1.20000 AFIX 0 N2 4 0.248273 0.198092 0.275790 11.00000 0.03112 0.03399 = 0.05629 -0.00678 0.00678 -0.00410 N1 4 0.155726 0.102536 0.118102 11.00000 0.05631 0.10276 = 0.05226 0.02171 -0.02090 -0.02401 AFIX 137 H1D 2 0.182129 0.062789 0.097448 11.00000 -1.50000 H1E 2 0.121823 0.127239 0.082134 11.00000 -1.50000 H1F 2 0.111893 0.090823 0.155728 11.00000 -1.50000 AFIX 0 C2 1 0.240360 0.146649 0.149422 11.00000 0.05437 0.04581 = 0.04123 0.01580 -0.00272 -0.00490 AFIX 13 H2 2 0.226321 0.197140 0.137747 11.00000 -1.20000 AFIX 0 C3 1 0.246412 0.137464 0.235013 11.00000 0.01961 0.03750 = 0.03788 0.00107 -0.00085 -0.00486 I2 3 1.000000 0.487464 0.250000 10.50000 0.03927 0.03230 = 0.02952 0.00000 0.00187 0.00000 C6 1 0.257048 0.135617 0.391341 11.00000 0.06021 0.07600 = 0.03700 -0.00490 -0.00588 -0.00541 AFIX 43 H6 2 0.259183 0.135910 0.444804 11.00000 -1.20000 AFIX 0 HKLF 4 REM fcc-126-02-1_a.res in C222(1) REM wR2 = 0.0612, GooF = S = 0.974, Restrained GooF = 0.971 for all data REM R1 = 0.0286 for 4276 Fo > 4sig(Fo) and 0.0361 for all 4978 data REM 160 parameters refined using 60 restraints END WGHT 0.0265 0.0000 REM Highest difference peak 1.504, deepest hole -0.848, 1-sigma level 0.179 Q1 1 0.4372 0.3747 0.3778 11.00000 0.05 1.50 ; _shelx_res_checksum 73933 _shelx_hkl_file ; 0 0 -2 10.06 0.58 0 0 2 10.11 0.60 0 0 3 0.26 0.41 0 0 -3 -0.13 0.40 0 0 -4 706.28 22.16 0 0 -5 0.63 0.68 0 0 -6 347.74 11.55 0 0 -7 0.22 0.92 0 0 -8 8842.74 270.59 0 0 -9 -0.38 1.25 0 0 -10 126.82 5.41 0 0 -11 0.81 1.46 0 0 -12 24.29 2.46 0 0 -13 -0.41 1.67 0 0 -14 352.29 13.01 0 0 -15 1.73 1.97 0 0 -16 2163.68 68.52 0 0 -17 1.05 2.33 0 0 -18 72.66 4.75 0 0 -19 -0.41 2.52 0 0 -20 14.56 3.06 0 0 -21 4.28 2.76 0 2 0 4.45 0.37 0 2 -1 2401.04 73.52 0 -2 -2 22.18 0.98 0 -2 -3 3031.51 92.81 0 -2 -4 14.25 1.04 0 -2 -5 2118.07 65.31 0 -2 -6 28.41 1.74 0 -2 -7 2992.14 92.25 0 -2 -8 9.83 1.38 0 -2 -9 780.52 25.24 0 -2 -10 64.36 3.44 0 -2 -11 1458.62 46.19 0 -2 -12 6.10 1.95 0 -2 -13 223.11 8.84 0 -2 -14 6.56 2.12 0 -2 -15 1017.13 33.42 0 -2 -16 5.39 2.26 0 -2 -17 38.40 3.50 0 -2 -18 12.97 2.77 0 -2 -19 249.17 10.55 0 -2 -20 7.84 2.82 0 -2 -21 5.49 2.77 0 4 0 708.70 22.27 0 4 -1 27.49 1.49 0 4 -1 28.68 1.18 0 4 -2 25.03 1.11 0 -4 -2 27.00 1.14 0 -4 -3 119.54 4.13 0 4 -3 119.71 4.12 0 4 -4 9999.00 303.17 0 -4 -4 9871.11 303.14 0 4 -5 12.72 1.10 0 -4 -5 16.57 1.22 0 4 -6 111.83 4.33 0 -4 -6 109.79 4.30 0 -4 -7 61.21 2.91 0 4 -7 61.77 2.91 0 -4 -8 137.22 5.40 0 4 -8 136.07 5.40 0 4 -9 22.95 1.92 0 -4 -9 22.00 1.94 0 4 -10 276.04 10.14 0 -4 -10 285.90 10.13 0 -4 -11 81.65 4.07 0 4 -11 70.72 3.92 0 -4 -12 4654.53 143.25 0 4 -12 4624.49 143.29 0 -4 -13 46.43 3.38 0 4 -13 47.17 3.40 0 -4 -14 87.49 4.75 0 4 -14 94.08 4.92 0 -4 -15 4.10 2.01 0 4 -15 5.04 2.05 0 -4 -16 17.55 2.62 0 4 -16 16.74 2.69 0 4 -17 9.14 2.47 0 -4 -17 12.56 2.51 0 4 -18 214.94 9.52 0 -4 -18 223.96 9.49 0 -4 -19 7.04 2.72 0 4 -19 1.43 2.61 0 4 -20 717.61 25.48 0 -4 -20 745.30 25.44 0 -4 -21 2.75 2.71 0 4 -21 2.66 2.77 0 -6 0 100.96 3.80 0 6 0 157.03 4.96 0 6 -1 1686.98 52.42 0 6 -1 1811.88 53.16 0 -6 -1 1680.53 53.05 0 6 -2 9.69 0.58 0 -6 -2 9.99 0.61 0 6 -2 8.04 0.73 0 6 -2 10.22 1.22 0 -6 -2 7.94 1.12 0 6 -3 3184.35 97.61 0 -6 -3 3226.90 97.61 0 6 -3 3109.27 98.38 0 6 -4 109.30 4.00 0 -6 -4 114.81 4.03 0 6 -4 108.55 4.65 0 6 -5 1979.99 61.13 0 -6 -5 1981.35 61.10 0 -6 -6 241.06 8.11 0 6 -6 228.82 8.07 0 6 -7 1059.63 33.53 0 -6 -7 1068.25 33.52 0 6 -8 1.93 1.15 0 -6 -8 2.65 1.09 0 -6 -9 743.68 24.02 0 6 -9 740.13 24.06 0 -6 -10 119.25 5.18 0 6 -10 120.90 5.23 0 -6 -11 1930.42 59.49 0 6 -11 1860.93 59.53 0 -6 -12 8.82 1.91 0 6 -12 10.29 1.93 0 6 -13 238.79 9.33 0 -6 -13 239.86 9.27 0 -6 -14 122.02 5.75 0 6 -14 119.45 5.76 0 -6 -15 227.74 9.27 0 6 -15 239.60 9.47 0 6 -16 10.44 2.50 0 -6 -16 12.39 2.41 0 6 -17 56.58 4.26 0 -6 -17 61.30 4.26 0 6 -18 12.57 2.76 0 -6 -18 16.40 2.85 0 -6 -19 492.97 17.61 0 6 -19 469.82 17.62 0 -6 -20 -0.20 2.45 0 6 -20 4.22 2.67 0 -6 -21 10.82 3.18 0 6 -21 5.24 2.95 0 -8 0 7355.78 232.48 0 8 0 7860.52 232.65 0 8 -1 14.95 1.68 0 -8 -1 13.47 1.02 0 -8 -1 12.36 1.47 0 -8 1 12.60 1.52 0 8 -1 15.05 1.15 0 8 -2 1.61 0.64 0 -8 -2 2.29 1.07 0 8 -2 1.24 1.14 0 8 -2 0.69 0.33 0 -8 -2 1.21 0.35 0 -8 2 2.21 1.02 0 8 -2 1.10 0.70 0 -8 -3 76.36 2.72 0 8 -3 73.48 2.71 0 -8 -3 70.45 3.51 0 8 -4 83.92 3.17 0 -8 -4 85.33 3.18 0 8 -4 93.03 4.21 0 -8 -5 11.59 1.05 0 8 -5 11.86 1.06 0 8 -5 12.82 1.78 0 -8 -6 70.63 3.04 0 8 -6 72.81 3.07 0 8 -6 69.46 3.91 0 8 -7 235.79 8.29 0 -8 -7 240.23 8.27 0 8 -7 230.39 9.26 0 -8 -8 5675.68 174.22 0 8 -8 5686.35 174.29 0 -8 -9 90.47 4.20 0 8 -9 96.09 4.27 0 -8 -10 23.64 2.05 0 8 -10 21.00 2.04 0 8 -11 40.91 2.82 0 -8 -11 41.62 2.78 0 -8 -12 19.35 2.25 0 8 -12 17.73 2.19 0 -8 -13 46.26 3.19 0 8 -13 47.72 3.28 0 8 -14 139.04 6.46 0 -8 -14 145.39 6.39 0 8 -15 66.99 4.28 0 -8 -15 62.43 4.10 0 -8 -16 1652.53 52.57 0 8 -16 1635.20 52.74 0 8 -17 38.79 3.65 0 -8 -17 38.11 3.50 0 8 -18 35.09 3.59 0 -8 -18 41.67 3.64 0 -8 -19 3.00 2.36 0 8 -19 2.66 2.53 0 8 -20 3.47 2.61 0 -8 -20 6.75 2.88 0 8 -21 7.03 2.75 0 -8 -21 6.86 2.83 0 -10 0 102.81 4.65 0 10 0 106.96 4.87 0 -10 1 1616.45 49.36 0 -10 -1 1564.07 49.25 0 10 -1 1673.05 49.64 0 -10 -1 1484.49 48.50 0 10 -1 1585.69 48.75 0 10 -2 72.85 2.76 0 -10 -2 78.09 3.14 0 10 -2 75.36 3.95 0 -10 -2 75.05 3.69 0 -10 2 81.15 3.87 0 10 -2 74.09 3.16 0 10 -3 339.18 12.10 0 10 -3 334.20 10.95 0 -10 -3 339.43 10.65 0 10 -3 337.16 10.64 0 -10 -3 322.32 11.76 0 -10 -4 2.84 0.65 0 10 -4 1.94 0.63 0 -10 -4 2.82 1.36 0 10 -4 1.97 1.47 0 10 -5 617.67 20.56 0 -10 -5 595.74 19.06 0 10 -5 605.24 19.09 0 10 -6 59.54 3.77 0 -10 -6 53.80 2.51 0 10 -6 54.90 2.56 0 10 -7 1651.26 52.63 0 -10 -7 1657.05 51.16 0 10 -7 1631.99 51.23 0 10 -8 31.90 3.09 0 -10 -8 33.64 2.18 0 10 -8 36.40 2.26 0 10 -9 579.10 20.08 0 10 -9 559.13 18.69 0 -10 -9 567.11 18.64 0 10 -10 257.50 10.58 0 10 -10 238.01 9.16 0 -10 -10 258.82 9.16 0 10 -11 126.60 6.60 0 -10 -11 122.83 5.25 0 10 -11 111.91 5.28 0 10 -12 -0.67 2.61 0 10 -12 2.67 1.69 0 -10 -12 2.44 1.62 0 10 -13 209.82 9.71 0 -10 -13 207.26 8.28 0 10 -13 212.75 8.46 0 -10 -14 49.24 3.54 0 10 -14 54.05 3.67 0 -10 -15 784.34 26.02 0 10 -15 779.20 26.25 0 -10 -16 3.96 2.31 0 10 -16 4.04 2.29 0 -10 -17 46.04 3.73 0 10 -17 41.78 3.71 0 10 -18 50.82 4.19 0 -10 -18 51.33 4.00 0 -10 -19 62.54 4.47 0 10 -19 54.32 4.48 0 10 -20 3.93 2.82 0 -10 -20 1.56 2.57 0 -10 -21 9.68 3.01 0 10 -21 9.66 3.14 0 12 0 27.90 2.07 0 12 0 25.01 2.55 0 -12 0 21.32 2.24 0 12 -1 0.56 1.62 0 12 -1 1.72 1.21 0 -12 1 1.98 1.46 0 -12 -1 -0.12 1.32 0 12 -2 14.09 2.14 0 -12 -2 12.21 1.84 0 -12 2 14.95 2.10 0 -12 -2 14.44 1.41 0 12 -2 11.85 1.50 0 -12 -3 49.53 3.24 0 -12 -3 57.50 2.76 0 12 -3 53.77 2.22 0 12 -4 3413.08 104.73 0 -12 -4 3206.98 105.79 0 12 -5 18.28 2.56 0 -12 -5 16.94 2.35 0 12 -5 16.70 1.27 0 -12 -5 15.05 1.27 0 12 -6 5.51 0.98 0 -12 -6 5.72 1.07 0 -12 -6 5.15 1.97 0 12 -6 7.90 2.12 0 12 -7 35.71 3.28 0 -12 -7 27.30 1.84 0 12 -7 31.95 1.92 0 12 -8 23.74 3.05 0 -12 -8 20.06 1.74 0 12 -8 25.85 1.88 0 12 -9 22.43 3.08 0 -12 -9 25.76 2.00 0 12 -9 23.16 1.97 0 12 -10 28.63 2.28 0 -12 -10 25.87 2.25 0 12 -11 93.17 5.92 0 -12 -11 99.68 4.48 0 12 -11 93.38 4.58 0 12 -12 1872.00 59.90 0 12 -12 1825.00 58.03 0 -12 -12 1841.24 57.83 0 12 -13 46.77 4.55 0 -12 -13 44.89 3.24 0 12 -13 43.47 3.33 0 12 -14 17.23 2.40 0 -12 -14 12.20 2.37 0 -12 -15 7.28 2.28 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136.98 5.18 2 10 -4 12.05 2.10 -2 10 4 12.29 1.24 -2 10 3 438.90 13.76 2 10 -3 429.89 15.24 -2 -10 -3 400.74 15.27 2 10 -2 2.90 1.72 -2 10 2 0.41 0.55 -2 -10 -2 0.14 1.47 -2 10 1 1144.65 34.30 -2 10 1 1148.74 35.38 -2 -10 -1 1061.98 35.96 2 10 -1 1143.05 36.13 -2 -10 0 43.38 3.09 -2 10 0 49.79 2.77 2 10 0 51.27 3.07 2 -10 -1 1120.93 35.43 -2 -10 1 1151.36 34.64 -2 10 -1 1144.36 35.85 -2 10 -1 1057.07 35.46 2 -10 -1 1089.74 35.81 2 10 1 1131.83 36.04 2 -10 -2 0.28 0.93 -2 -10 2 0.13 0.52 2 10 2 0.35 1.56 2 -10 -2 0.60 1.26 -2 10 -2 1.31 1.12 -2 10 -2 1.49 1.30 -2 10 -3 414.44 14.36 2 -10 -3 425.89 13.73 2 10 3 418.08 14.40 2 -10 -3 412.21 14.12 -2 10 -3 414.36 14.09 -2 -10 3 408.46 13.16 2 -10 -4 9.01 1.20 2 -10 -4 10.64 1.56 -2 10 -4 11.65 1.83 -2 -10 4 10.69 1.25 -2 -10 4 11.12 1.07 -2 -10 5 179.34 6.32 -2 -10 5 180.16 6.21 2 -10 -5 166.76 6.45 -2 10 -5 177.68 7.36 -2 -10 6 136.54 5.01 -2 10 -6 132.55 5.14 2 -10 -6 126.07 5.19 -2 -10 6 128.81 4.96 -2 10 -6 128.69 6.12 -2 -10 7 1954.09 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-7 71.92 3.81 6 4 -6 89.20 4.32 6 4 -6 91.89 4.44 -6 4 6 83.30 4.40 6 4 -5 52.41 3.15 6 4 -5 51.77 3.21 6 4 -4 2610.50 78.85 -6 -4 -4 2419.86 79.29 6 4 -3 52.27 3.23 -6 -4 -3 51.03 3.73 -6 4 3 56.46 2.05 -6 -4 -2 454.33 16.27 -6 -4 -1 9.40 2.18 -6 -4 -1 13.21 1.95 -6 -4 0 282.09 10.41 -6 -4 1 20.08 2.34 6 -4 -1 17.58 2.35 -6 -4 1 14.88 1.88 -6 -4 2 443.13 15.56 6 -4 -2 453.50 16.20 -6 -4 2 465.73 15.92 6 -4 -3 59.44 3.81 -6 -4 3 59.57 3.48 -6 -4 4 2662.86 82.99 6 -4 -4 2662.61 83.44 -6 4 -4 2660.25 83.07 6 4 5 44.00 3.42 -6 4 -5 44.85 3.11 -6 -4 5 44.38 3.02 6 -4 -5 53.42 3.48 6 -4 -6 88.33 4.69 -6 -4 6 87.89 4.38 6 4 6 86.15 4.82 -6 -4 6 84.43 4.30 -6 4 -6 78.45 4.26 6 -4 -7 68.56 4.12 -6 -4 7 59.23 3.64 6 4 7 62.93 4.26 -6 4 -7 71.76 3.88 -6 -4 8 52.36 3.50 6 -4 -8 58.58 3.94 6 -4 -8 59.83 2.40 6 -4 -9 58.39 2.53 -6 -4 9 64.33 3.81 6 4 9 63.13 4.18 6 -4 -10 584.16 18.70 6 4 10 603.74 20.60 -6 -4 10 577.52 20.04 6 -4 -11 13.37 1.36 6 4 11 15.89 2.86 6 -4 -12 1684.49 52.52 -6 -4 12 1720.04 53.98 6 4 12 1659.46 54.35 6 -4 -13 18.07 1.78 -6 -4 13 19.46 2.93 6 4 13 18.93 3.24 6 -4 -14 8.79 1.52 -6 -4 14 8.14 2.65 6 4 14 5.51 2.96 -6 -4 15 22.62 3.35 6 4 15 20.66 3.51 6 -4 -15 19.43 1.99 6 -4 -16 33.24 2.57 -6 4 -17 25.96 4.13 6 -4 -17 25.99 2.40 -6 4 -18 304.57 13.33 6 -4 -18 320.16 11.50 -6 4 -19 2.93 3.53 6 -4 -19 3.89 1.88 -6 4 -20 446.02 17.64 -6 -6 -20 4.05 3.59 -6 -6 -19 340.39 14.09 -6 -6 -18 4.08 3.40 -6 -6 -17 10.17 3.39 -6 -6 -16 35.56 4.04 6 6 -16 24.85 3.30 6 6 -15 241.43 10.08 -6 6 14 58.14 4.37 6 6 -14 58.57 4.08 -6 6 13 60.71 4.44 6 6 -13 68.93 4.34 -6 6 12 2.44 2.38 6 6 -12 2.23 1.89 -6 6 11 796.01 27.17 6 6 -11 836.25 27.26 6 6 -10 22.19 2.59 -6 6 10 22.34 2.73 6 6 -9 51.91 3.51 -6 6 9 51.58 3.51 6 6 -8 63.51 3.60 6 6 -8 61.51 3.81 -6 6 8 57.49 3.64 6 6 -7 287.05 10.40 6 6 -7 280.26 10.67 -6 6 7 273.76 10.37 6 6 -6 144.72 6.35 -6 6 6 153.55 6.46 6 6 -6 160.22 6.69 6 6 -5 269.07 9.94 6 6 -5 247.56 9.52 6 6 -4 25.82 2.31 -6 -6 -4 25.59 2.73 6 6 -3 705.29 22.86 -6 -6 -3 677.87 23.57 -6 6 2 4.50 1.78 -6 -6 -2 7.10 2.15 -6 -6 -1 87.60 4.31 -6 -6 -1 86.02 4.89 -6 6 1 80.24 4.64 -6 -6 0 56.86 4.00 -6 -6 0 59.25 3.35 -6 -6 0 64.01 4.12 -6 6 0 55.44 3.83 -6 -6 1 177.47 7.63 -6 -6 1 172.17 6.87 -6 6 -1 176.54 7.76 -6 -6 1 164.37 7.59 -6 -6 2 9.60 1.60 -6 6 -2 14.90 2.60 6 -6 -2 8.87 2.20 -6 -6 2 14.59 2.23 -6 -6 3 763.77 25.92 -6 6 -3 784.10 26.38 6 -6 -3 782.29 26.18 6 -6 -4 25.63 2.75 -6 -6 4 23.89 2.57 6 -6 -5 259.33 9.99 -6 6 -5 250.11 9.34 6 6 5 234.06 9.99 -6 -6 5 250.05 9.77 6 -6 -6 156.60 7.02 -6 -6 6 151.82 6.70 6 6 6 154.26 7.16 -6 6 -6 150.62 6.34 -6 -6 6 148.41 6.43 6 -6 -7 262.96 10.34 -6 -6 7 255.47 9.75 -6 -6 7 252.19 10.06 6 6 7 263.28 10.52 -6 6 -7 264.32 9.59 6 6 8 62.57 4.42 -6 -6 8 64.45 3.75 6 -6 -8 62.78 4.16 -6 -6 9 91.57 4.67 6 -6 -9 98.61 5.34 6 6 9 98.87 5.46 6 -6 -9 90.73 3.16 -6 -6 10 22.95 2.58 6 -6 -10 20.94 1.23 6 6 10 18.47 3.05 6 -6 -11 903.53 28.17 6 6 11 905.04 30.58 -6 -6 11 894.19 29.79 6 6 12 1.46 2.58 6 -6 -12 1.38 0.97 -6 -6 12 0.95 2.23 6 -6 -13 53.54 2.64 6 6 13 52.79 4.59 -6 -6 13 51.17 4.09 -6 -6 14 58.19 4.37 6 6 14 61.14 4.92 6 -6 -14 56.75 2.91 6 -6 -15 242.48 8.69 6 -6 -16 25.57 2.20 -6 6 -16 29.56 4.04 6 -6 -17 17.11 2.02 -6 6 -17 14.58 3.65 6 -6 -18 1.40 1.51 -6 6 -18 1.26 3.33 -6 6 -19 332.20 14.01 -6 6 -20 5.57 3.54 -6 -8 -19 4.21 3.23 -6 -8 -18 8.06 3.38 -6 -8 -17 9.29 3.39 -6 -8 -16 654.69 23.20 6 8 -15 6.26 2.53 -6 8 14 351.23 13.80 6 8 -14 373.68 14.01 -6 8 13 98.00 5.65 6 8 -13 106.79 5.78 -6 8 12 29.77 3.21 6 8 -12 28.93 3.20 -6 8 11 48.55 3.76 6 8 -11 52.12 3.84 -6 8 10 1.15 1.99 6 8 -10 3.27 2.07 6 8 -9 52.38 3.41 6 8 -9 48.45 3.76 -6 8 9 56.34 3.67 6 8 -8 1834.37 58.73 -6 8 8 1862.58 58.76 6 8 -8 1905.89 59.39 -6 8 7 10.94 2.02 6 8 -7 12.35 1.91 6 8 -7 14.07 2.50 6 8 -6 522.43 17.50 -6 8 6 506.73 17.54 6 8 -6 522.07 18.18 6 8 -5 73.09 3.79 -6 8 5 69.73 3.84 6 8 -5 80.13 4.60 6 8 -4 14.93 1.83 -6 -8 -3 47.97 3.65 -6 8 2 158.70 7.30 -6 -8 -2 168.09 7.60 -6 8 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22.53 4.12 -16 0 1 23.76 3.90 -16 0 -2 74.88 7.53 -16 0 2 58.79 4.86 -16 0 -3 17.48 5.19 -16 0 -4 134.90 9.11 -16 0 -5 25.07 5.66 -16 0 -6 89.43 7.58 -16 -2 -4 14.33 5.63 -16 -2 -3 186.75 10.90 -16 -2 -2 35.22 4.80 -16 -2 -2 43.18 6.33 -16 -2 -1 147.60 8.50 -16 -2 -1 165.08 10.48 -16 -2 0 5.62 3.53 -16 -2 1 142.83 8.15 -16 2 -1 153.57 8.02 -16 2 -1 151.46 9.88 -16 2 -2 39.40 6.24 -16 -2 2 31.06 4.03 -16 2 -3 165.79 10.20 -16 -2 3 151.45 7.97 -16 2 -4 4.94 4.88 -16 -2 4 7.14 3.29 -16 2 -5 118.86 8.60 -16 2 -6 22.19 5.41 -16 2 -7 143.71 9.19 -16 2 -8 1.98 4.72 -16 -4 -3 13.61 4.15 -16 -4 -2 56.08 5.65 -16 -4 -1 10.88 3.86 -16 -4 0 103.57 7.01 -16 -4 0 125.78 9.19 -16 -4 1 18.47 5.83 -16 -4 1 18.68 4.04 -16 -4 2 56.07 5.30 -16 4 -2 61.94 6.76 -16 4 -3 13.99 5.38 -16 -4 3 12.44 3.76 -16 4 -4 425.19 17.64 -16 -4 4 387.95 15.78 -16 -4 5 9.66 3.48 -16 4 -5 16.54 5.13 -16 4 -6 42.20 6.01 -16 4 -7 7.69 4.95 -16 4 -8 57.33 6.23 -16 4 -9 8.99 5.03 -16 -6 -4 -0.71 4.12 -16 -6 -3 122.14 8.21 -16 -6 -2 10.44 4.30 -16 -6 -1 66.11 6.04 -16 -6 0 3.26 3.74 -16 -6 1 70.57 6.14 -16 6 -2 16.61 5.19 -16 -6 2 16.91 3.89 -16 6 -3 148.41 9.32 -16 -6 3 125.89 7.75 -16 6 -4 5.08 4.80 -16 -6 4 -1.36 3.69 -16 6 -5 121.04 8.40 -16 -6 5 108.09 7.08 -16 -6 6 10.56 3.71 -16 6 -6 20.36 5.32 -16 6 -7 57.86 6.29 -16 6 -8 4.31 4.42 -16 6 -9 25.42 5.27 -16 6 -10 15.12 4.95 -16 -8 -3 9.83 4.84 -16 -8 -2 44.00 5.54 -16 -8 -1 5.50 3.84 -16 -8 0 233.51 11.66 -16 -8 1 3.94 3.72 -16 8 -2 38.04 5.95 -16 -8 2 42.46 5.07 -16 8 -3 7.94 4.77 -16 -8 3 5.93 3.91 -16 8 -4 45.84 6.40 -16 -8 4 40.57 5.03 -16 8 -5 7.66 4.90 -16 -8 5 6.08 3.72 -16 8 -6 44.36 5.94 -16 -8 6 37.62 4.85 -16 8 -7 12.86 5.08 -16 -8 7 14.21 4.08 -16 8 -8 176.77 9.99 -16 8 -9 7.47 4.36 -16 10 -3 12.56 4.79 -16 -10 3 16.65 4.53 -16 10 -4 -1.90 4.73 -16 10 -5 28.51 5.55 -16 10 -6 10.88 4.74 -16 10 -7 53.03 6.28 -16 10 -8 4.54 4.31 -16 12 -3 3.44 4.64 -16 12 -4 97.00 7.64 -16 12 -5 1.49 4.67 -17 -1 -3 30.18 4.88 -17 -1 -2 28.29 4.67 -17 -1 -1 5.10 3.48 -17 -3 -3 16.78 4.37 -17 -3 -2 8.39 3.97 -17 -3 -1 31.99 4.73 -17 -3 0 3.03 3.59 -17 -3 1 27.80 4.53 -17 -5 -4 0.70 4.07 -17 -5 -3 -0.66 4.13 -17 -5 -2 51.28 5.71 -17 -5 -1 10.96 4.06 -17 -5 0 2.98 3.62 -17 -5 1 11.65 4.10 -17 -5 2 55.44 5.55 -17 -7 -1 23.05 4.88 -17 -7 0 14.20 4.51 -17 -7 1 16.86 4.48 -17 -7 2 6.54 4.11 -17 -7 3 25.03 4.85 -17 -7 4 6.35 3.83 0 0 0 0.00 0.00 TITL FCC-126-02-1 in C222(1) REM C222(1) (#20 in standard setting) CELL 0.71073 12.987279 18.838738 17.574061 90.0000 90.0000 90.0000 ZERR 60.00 0.000529 0.000710 0.000804 0.0000 0.0000 0.0000 LATT -7 SYMM -x,-y, z+1/2 SYMM -x, y,-z+1/2 SYMM x,-y,-z SFAC C H N I Pb UNIT 60.00 60.00 60.00 60.00 60.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 94434 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.422 _oxdiff_exptl_absorpt_empirical_full_min 0.645 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb2 Pb 0.99615(3) 0.37635(2) 0.38089(2) 0.03443(11) Uani 1 1 d . . . . . Pb1 Pb 0.50657(3) 0.37743(2) 0.37898(2) 0.03136(10) Uani 1 1 d . . . . . I6 I 0.500000 0.50079(5) 0.250000 0.0357(2) Uani 1 2 d S T P . . I5 I 0.53982(10) 0.500000 0.500000 0.0516(3) Uani 1 2 d S T P . . I8 I 0.500000 0.25956(4) 0.250000 0.0319(2) Uani 1 2 d S T P . . I4 I 0.75422(7) 0.35874(3) 0.36219(4) 0.04123(16) Uani 1 1 d . . . . . I9 I 0.25767(7) 0.40511(4) 0.39393(4) 0.04503(18) Uani 1 1 d . . . . . I3 I 1.000000 0.25479(4) 0.250000 0.0360(2) Uani 1 2 d S T P . . I1 I 0.95859(10) 0.500000 0.500000 0.0511(3) Uani 1 2 d S T P . . I7 I 0.48420(8) 0.26406(4) 0.50815(5) 0.0617(3) Uani 1 1 d . . . . . C1 C 0.3416(10) 0.1252(7) 0.1121(6) 0.064(3) Uani 1 1 d . . . . . H1A H 0.353522 0.074933 0.120325 0.095 Uiso 1 1 calc R U . . . H1B H 0.397506 0.152260 0.134343 0.095 Uiso 1 1 calc R U . . . H1C H 0.338071 0.134668 0.057929 0.095 Uiso 1 1 calc R U . . . C4 C 0.2522(10) 0.0735(4) 0.2734(5) 0.0365(18) Uani 1 1 d . . . . . H4 H 0.253356 0.030648 0.245935 0.044 Uiso 1 1 calc R U . . . C5 C 0.2564(11) 0.0723(5) 0.3507(5) 0.043(2) Uani 1 1 d . . . . . H5 H 0.258757 0.028723 0.376695 0.052 Uiso 1 1 calc R U . . . C7 C 0.2545(11) 0.1973(5) 0.3507(6) 0.056(2) Uani 1 1 d . . . . . H7 H 0.257278 0.240735 0.377022 0.067 Uiso 1 1 calc R U . . . N2 N 0.2483(8) 0.1981(3) 0.2758(4) 0.0405(17) Uani 1 1 d . . . . . N1 N 0.1557(8) 0.1025(6) 0.1181(5) 0.070(3) Uani 1 1 d . . . . . H1D H 0.182129 0.062789 0.097448 0.106 Uiso 1 1 calc R U . . . H1E H 0.121823 0.127239 0.082134 0.106 Uiso 1 1 calc R U . . . H1F H 0.111893 0.090823 0.155728 0.106 Uiso 1 1 calc R U . . . C2 C 0.2404(11) 0.1466(5) 0.1494(6) 0.047(2) Uani 1 1 d . . . . . H2 H 0.226321 0.197140 0.137747 0.057 Uiso 1 1 calc R U . . . C3 C 0.2464(8) 0.1375(4) 0.2350(5) 0.0317(16) Uani 1 1 d . . . . . I2 I 1.000000 0.48746(4) 0.250000 0.0337(2) Uani 1 2 d S T P . . C6 C 0.2570(11) 0.1356(6) 0.3913(7) 0.058(3) Uani 1 1 d . . . . . H6 H 0.259183 0.135910 0.444804 0.069 Uiso 1 1 calc R U . . . 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 Pb2 0.0369(2) 0.03791(18) 0.0285(2) 0.00144(12) 0.00062(17) 0.0025(3) Pb1 0.0357(2) 0.03273(17) 0.02561(19) 0.00029(11) 0.00121(16) -0.0004(2) I6 0.0409(6) 0.0348(4) 0.0315(5) 0.000 0.0049(5) 0.000 I5 0.0579(8) 0.0533(6) 0.0437(7) -0.0231(5) 0.000 0.000 I8 0.0328(6) 0.0326(4) 0.0304(4) 0.000 -0.0040(5) 0.000 I4 0.0225(3) 0.0409(3) 0.0604(4) -0.0099(3) 0.0003(4) 0.0008(3) I9 0.0298(4) 0.0500(4) 0.0553(4) 0.0064(3) 0.0039(4) 0.0047(3) I3 0.0312(6) 0.0397(4) 0.0369(5) 0.000 0.0045(5) 0.000 I1 0.0593(9) 0.0563(6) 0.0377(7) -0.0186(5) 0.000 0.000 I7 0.0910(7) 0.0508(5) 0.0434(4) 0.0209(3) 0.0173(4) 0.0118(5) C1 0.060(7) 0.099(10) 0.032(6) -0.003(6) 0.005(5) -0.012(7) C4 0.033(5) 0.028(3) 0.049(4) 0.000(3) -0.004(6) 0.001(4) C5 0.037(6) 0.046(4) 0.045(5) 0.010(4) -0.010(6) -0.008(5) C7 0.050(6) 0.051(5) 0.068(6) -0.023(4) 0.000(7) -0.003(6) N2 0.031(4) 0.034(3) 0.056(4) -0.007(3) 0.007(5) -0.004(4) N1 0.056(6) 0.103(7) 0.052(7) 0.022(6) -0.021(5) -0.024(6) C2 0.054(7) 0.046(5) 0.041(5) 0.016(4) -0.003(6) -0.005(5) C3 0.020(4) 0.037(3) 0.038(4) 0.001(3) -0.001(5) -0.005(4) I2 0.0393(6) 0.0323(4) 0.0295(5) 0.000 0.0019(5) 0.000 C6 0.060(8) 0.076(6) 0.037(5) -0.005(4) -0.006(7) -0.005(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' I I -0.4742 1.8119 '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' 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 I4 Pb2 I3 82.428(14) . . ? I4 Pb2 I7 86.02(2) . 8_556 ? I3 Pb2 I7 81.577(19) . 8_556 ? I1 Pb2 I4 89.59(3) . . ? I1 Pb2 I3 171.42(3) . . ? I1 Pb2 I7 101.082(19) . 8_556 ? I2 Pb2 I4 90.554(15) . . ? I2 Pb2 I3 87.159(18) . . ? I2 Pb2 I1 89.788(14) . . ? I2 Pb2 I7 168.56(2) . 8_556 ? I6 Pb1 I4 92.303(15) . . ? I6 Pb1 I9 85.203(14) . . ? I5 Pb1 I6 87.170(13) . . ? I5 Pb1 I8 173.06(3) . . ? I5 Pb1 I4 90.29(3) . . ? I5 Pb1 I9 87.98(3) . . ? I8 Pb1 I6 90.083(19) . . ? I8 Pb1 I4 83.450(14) . . ? I8 Pb1 I9 98.147(16) . . ? I4 Pb1 I9 177.029(19) . . ? I7 Pb1 I6 172.74(2) . . ? I7 Pb1 I5 91.324(19) . . ? I7 Pb1 I8 92.18(2) . . ? I7 Pb1 I4 94.81(2) . . ? I7 Pb1 I9 87.65(2) . . ? Pb1 I6 Pb1 88.62(2) . 3_655 ? Pb1 I5 Pb1 164.33(5) 4_566 . ? Pb1 I8 Pb1 91.22(2) . 3_655 ? Pb2 I4 Pb1 163.43(2) . . ? Pb2 I3 Pb2 90.27(2) . 3_755 ? Pb2 I1 Pb2 162.29(5) 4_566 . ? Pb1 I7 Pb2 166.91(3) . 8_456 ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? C5 C4 H4 119.9 . . ? C5 C4 C3 120.2(8) . . ? C3 C4 H4 119.9 . . ? C4 C5 H5 120.0 . . ? C4 C5 C6 120.0(9) . . ? C6 C5 H5 120.0 . . ? N2 C7 H7 118.9 . . ? N2 C7 C6 122.2(9) . . ? C6 C7 H7 118.9 . . ? C7 N2 C3 121.5(8) . . ? H1D N1 H1E 109.5 . . ? H1D N1 H1F 109.5 . . ? H1E N1 H1F 109.5 . . ? C2 N1 H1D 109.5 . . ? C2 N1 H1E 109.5 . . ? C2 N1 H1F 109.5 . . ? C1 C2 H2 109.0 . . ? N1 C2 C1 109.3(9) . . ? N1 C2 H2 109.0 . . ? N1 C2 C3 110.0(9) . . ? C3 C2 C1 110.6(11) . . ? C3 C2 H2 109.0 . . ? C4 C3 C2 125.9(8) . . ? N2 C3 C4 118.6(8) . . ? N2 C3 C2 115.6(7) . . ? Pb2 I2 Pb2 95.41(3) 3_755 . ? C5 C6 H6 121.2 . . ? C7 C6 C5 117.5(11) . . ? C7 C6 H6 121.2 . . ? 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 Pb2 I4 3.1765(10) . ? Pb2 I3 3.2462(7) . ? Pb2 I1 3.1695(4) . ? Pb2 I7 3.2900(8) 8_556 ? Pb2 I2 3.1105(7) . ? Pb1 I6 3.2474(7) . ? Pb1 I5 3.1688(4) . ? Pb1 I8 3.1744(7) . ? Pb1 I4 3.2490(10) . ? Pb1 I9 3.2849(10) . ? Pb1 I7 3.1303(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C1 C2 1.523(17) . ? C4 H4 0.9400 . ? C4 C5 1.361(13) . ? C4 C3 1.383(10) . ? C5 H5 0.9400 . ? C5 C6 1.390(14) . ? C7 H7 0.9400 . ? C7 N2 1.320(13) . ? C7 C6 1.364(15) . ? N2 C3 1.349(9) . ? N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? N1 H1F 0.9000 . ? N1 C2 1.484(14) . ? C2 H2 0.9900 . ? C2 C3 1.516(13) . ? C6 H6 0.9400 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -68.7(14) . . . . ? C1 C2 C3 N2 109.8(10) . . . . ? C4 C5 C6 C7 -1(2) . . . . ? C5 C4 C3 N2 2.1(16) . . . . ? C5 C4 C3 C2 -179.4(13) . . . . ? C7 N2 C3 C4 -0.6(16) . . . . ? C7 N2 C3 C2 -179.3(12) . . . . ? N2 C7 C6 C5 2(2) . . . . ? N1 C2 C3 C4 52.1(16) . . . . ? N1 C2 C3 N2 -129.3(10) . . . . ? C3 C4 C5 C6 -1(2) . . . . ? C6 C7 N2 C3 -2(2) . . . . ?