#------------------------------------------------------------------------------ #$Date: 2024-06-15 01:13:38 +0300 (Sat, 15 Jun 2024) $ #$Revision: 292406 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571902.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_1571902 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 Semiconductor ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC00954A _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_moiety '0.5(I12 Pb4), C7 H12 N2' _chemical_formula_sum 'C7 H12 I6 N2 Pb2' _chemical_formula_weight 1299.97 _space_group_crystal_system orthorhombic _space_group_IT_number 21 _space_group_name_Hall 'C 2 2' _space_group_name_H-M_alt 'C 2 2 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-09-09 _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 2 _cell_length_a 9.4743(7) _cell_length_b 17.7301(12) _cell_length_c 6.5088(4) _cell_measurement_reflns_used 2570 _cell_measurement_temperature 425.00(10) _cell_measurement_theta_max 30.9050 _cell_measurement_theta_min 2.4210 _cell_volume 1093.35(13) _computing_cell_refinement 'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)' _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 air _diffrn_ambient_temperature 425.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.886 _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 -17.00 33.00 0.50 1.10 -- 4.67 -99.00-150.00 100 2 \w -64.00 -4.00 0.50 1.10 -- -5.45 -38.00-150.00 120 3 \w -78.00 -3.00 0.50 1.10 -- -5.45 -57.00 0.00 150 4 \w -75.00 7.00 0.50 1.10 -- -5.45 -38.00 90.00 164 5 \w 9.00 41.00 0.50 1.10 -- 4.67 38.00 30.00 64 6 \w 52.00 78.00 0.50 1.10 -- 4.67 38.00 30.00 52 ; _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 -0.0148587000 _diffrn_orient_matrix_UB_12 -0.0065014000 _diffrn_orient_matrix_UB_13 0.0394836000 _diffrn_orient_matrix_UB_21 0.0960230000 _diffrn_orient_matrix_UB_22 -0.0348889000 _diffrn_orient_matrix_UB_23 0.0032046000 _diffrn_orient_matrix_UB_31 0.0493288000 _diffrn_orient_matrix_UB_32 0.0659247000 _diffrn_orient_matrix_UB_33 0.0055952000 _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 0.0729 _diffrn_reflns_av_unetI/netI 0.0503 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.886 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 6242 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.851 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.565 _diffrn_reflns_theta_min 2.297 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 23.836 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.09991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 3.949 _exptl_crystal_description block _exptl_crystal_F_000 1100 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.819 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.254 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.52(5) _refine_ls_extinction_coef 0.0019(2) _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 1.107 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 94 _refine_ls_number_reflns 1443 _refine_ls_number_restraints 114 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0414 _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^)+(0.0429P)^2^+6.0408P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1052 _refine_ls_wR_factor_ref 0.1096 _reflns_Friedel_coverage 0.651 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.803 _reflns_number_gt 1136 _reflns_number_total 1443 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc00954a2.cif _cod_data_source_block 3S-425K _cod_database_code 1571902 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H N I Pb' _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 0.199 _shelx_estimated_absorpt_t_min 0.199 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.47887 0.52113 2. Uiso/Uaniso restraints and constraints Uanis(C1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3. Rigid body (RIGU) restrains N1, N2, C1, C2, C3, C4, C5, C6, C7 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Fixed Sof: N1(0.25) H1A(0.25) H1B(0.25) H1C(0.25) C1(0.25) H1D(0.25) H1E(0.25) H1F(0.25) C2(0.25) H2(0.25) C7(0.25) H7(0.25) C3(0.25) C4(0.25) H4(0.25) C5(0.25) H5(0.25) C6(0.25) H6(0.25) N2(0.25) H2A(0.25) 5.a Ternary CH refined with riding coordinates: C2(H2) 5.b Aromatic/amide H refined with riding coordinates: C7(H7), C4(H4), C5(H5), C6(H6), N2(H2A) 5.c Fitted hexagon refined as free rotating group: C7(C3,C4,C5,C6,N2) 5.d Idealised Me refined as rotating group: N1(H1A,H1B,H1C), C1(H1D,H1E,H1F) ; _shelx_res_file ; TITL s-3aepi-425-3_auto_c.res in C222 s-3aepi-425-3_auto.res created by SHELXL-2018/3 at 12:31:36 on 08-Sep-2023 REM Old TITL s-3aepi-425-3_auto_a.res in Cmmm REM SHELXT solution in C222: R1 0.157, Rweak 0.008, Alpha 0.025 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = 0.473 ( 0.009 ) from 364 Parsons' quotients REM Formula found by SHELXT: N I6 Pb2 CELL 0.71073 9.4743 17.7301 6.5088 90 90 90 ZERR 2 0.0007 0.0012 0.0004 0 0 0 LATT -7 SYMM -X,-Y,+Z SYMM -X,+Y,-Z SYMM +X,-Y,-Z SFAC C H I N Pb UNIT 14 24 12 4 4 RIGU N1 N2 C1 C2 C3 > C6 C7 ISOR 0.01 0.02 C1 C7 C3 N2 C4 C2 C6 C5 N1 L.S. 80 PLAN 30 SIZE 0.1 0.1 0.1 TEMP 152 CONF FREE C1 C3 FREE C1 N1 FREE N1 C3 LIST 6 MORE -1 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.042900 6.040800 EXTI 0.001932 BASF 0.52113 FVAR 0.16526 PB1 5 0.500000 0.630094 -0.500000 10.50000 0.05052 0.04158 = 0.05437 0.00000 0.00066 0.00000 I1 3 0.265657 0.500000 -0.500000 10.50000 0.05189 0.04780 = 0.05744 -0.00454 0.00000 0.00000 I2 3 0.500000 0.630965 -1.000000 10.50000 0.14887 0.11106 = 0.04001 0.00000 -0.02857 0.00000 I3 3 0.750000 0.750000 -0.499448 10.50000 0.08882 0.06868 = 0.19405 0.00000 0.00000 -0.04093 PART -1 N1 4 0.974420 0.376227 -1.207529 10.25000 0.03389 0.05130 = 0.04686 -0.01349 0.01625 -0.00403 AFIX 137 H1A 2 0.993461 0.407108 -1.311705 10.25000 -1.20000 H1B 2 0.881584 0.374675 -1.187072 10.25000 -1.20000 H1C 2 1.005746 0.330150 -1.236923 10.25000 -1.20000 AFIX 0 C1 1 0.939295 0.359815 -0.876520 10.25000 0.05711 0.04887 = 0.05299 -0.00081 0.02084 0.00254 AFIX 137 H1D 2 0.937553 0.387751 -0.750200 10.25000 -1.50000 H1E 2 0.974941 0.309995 -0.851129 10.25000 -1.50000 H1F 2 0.845399 0.356490 -0.931213 10.25000 -1.50000 AFIX 0 C2 1 1.038477 0.401490 -1.036911 10.25000 0.04240 0.04773 = 0.04560 -0.00385 0.00778 -0.00007 AFIX 13 H2 2 1.137438 0.385812 -1.027125 10.25000 -1.20000 AFIX 66 C7 1 0.879009 0.518750 -0.992813 10.25000 0.05476 0.04225 = 0.04460 -0.00387 -0.00077 0.00204 AFIX 43 H7 2 0.804051 0.484888 -0.994349 10.25000 -1.20000 AFIX 65 C3 1 1.016844 0.492436 -1.007451 10.25000 0.05137 0.04579 = 0.04368 -0.00178 -0.00228 0.00093 C4 1 1.128878 0.543046 -1.005153 10.25000 0.05418 0.04673 = 0.04816 -0.00517 -0.00172 -0.00105 AFIX 43 H4 2 1.221098 0.525440 -1.014947 10.25000 -1.20000 AFIX 65 C5 1 1.103078 0.619971 -0.988217 10.25000 0.03911 0.04557 = 0.04050 -0.00104 0.00204 0.00019 AFIX 43 H5 2 1.178037 0.653833 -0.986680 10.25000 -1.20000 AFIX 65 C6 1 0.965244 0.646286 -0.973580 10.25000 0.03895 0.03747 = 0.01837 0.00682 -0.00091 0.00166 AFIX 43 H6 2 0.947984 0.697755 -0.962249 10.25000 -1.20000 AFIX 65 N2 4 0.853209 0.595677 -0.975877 10.25000 0.04414 0.04244 = 0.05101 -0.00260 -0.00249 -0.00221 AFIX 43 H2A 2 0.767930 0.611959 -0.966820 10.25000 -1.20000 AFIX 0 HKLF 4 REM s-3aepi-425-3_auto_c.res in C222 REM wR2 = 0.1096, GooF = S = 1.107, Restrained GooF = 1.067 for all data REM R1 = 0.0414 for 1136 Fo > 4sig(Fo) and 0.0566 for all 1443 data REM 94 parameters refined using 114 restraints END WGHT 0.0436 5.7973 REM Highest difference peak 1.819, deepest hole -1.738, 1-sigma level 0.254 Q1 1 0.5010 0.6308 -0.3638 11.00000 0.05 1.82 Q2 1 0.5682 0.6543 -1.0009 11.00000 0.05 1.70 Q3 1 0.7500 0.7500 -0.4071 10.50000 0.05 1.64 Q4 1 0.7500 0.7500 -0.5888 10.50000 0.05 1.59 Q5 1 0.5000 0.6911 -0.5000 10.50000 0.05 1.40 Q6 1 0.5000 0.6068 -1.0000 10.50000 0.05 1.23 Q7 1 0.2682 0.5001 -0.3882 11.00000 0.05 1.04 Q8 1 0.5000 0.5730 -0.5000 10.50000 0.05 1.01 Q9 1 0.2574 0.4477 -0.4981 11.00000 0.05 0.97 Q10 1 0.5001 0.5766 -0.3587 11.00000 0.05 0.94 Q11 1 0.5000 0.5000 -1.0000 10.25000 0.05 0.93 Q12 1 0.4982 0.6358 -1.1279 11.00000 0.05 0.89 Q13 1 0.4998 0.6783 -0.3635 11.00000 0.05 0.81 Q14 1 1.0000 0.3420 -1.5000 10.50000 0.05 0.78 Q15 1 0.7366 0.8260 -0.4996 11.00000 0.05 0.76 Q16 1 0.9967 0.3767 -1.3674 11.00000 0.05 0.74 Q17 1 0.7449 0.7961 -0.5007 11.00000 0.05 0.66 Q18 1 0.5000 0.5510 -1.0000 10.50000 0.05 0.66 Q19 1 1.2482 0.5593 -1.0028 11.00000 0.05 0.63 Q20 1 0.2691 0.4504 -0.3847 11.00000 0.05 0.62 Q21 1 1.0000 0.6877 -1.0000 10.50000 0.05 0.62 Q22 1 0.9997 0.2434 -1.4409 11.00000 0.05 0.61 Q23 1 0.2690 0.4503 -0.6250 11.00000 0.05 0.61 Q24 1 1.0005 0.7675 -0.9293 11.00000 0.05 0.61 Q25 1 1.0000 0.4384 -1.0000 10.50000 0.05 0.60 Q26 1 1.0845 0.4185 -0.9976 11.00000 0.05 0.56 Q27 1 1.2554 0.4994 -1.2462 11.00000 0.05 0.56 Q28 1 1.0000 0.4186 -1.5000 10.50000 0.05 0.55 Q29 1 0.5013 0.6862 -0.8823 11.00000 0.05 0.54 Q30 1 0.4996 0.6799 -1.2361 11.00000 0.05 0.51 ; _shelx_res_checksum 29831 _shelx_hkl_file ; 0 -22 0 84.95 16.92 0 -22 0 43.72 6.06 0 -20 0 -0.31 3.22 0 -20 0 4.70 13.91 0 -18 0 33.63 4.67 0 -18 0 19.78 14.19 0 -4 0 412.33 30.09 0 -2 0 1.99 3.20 0 2 0 6.77 4.78 0 2 0 0.49 0.47 0 4 0 447.34 29.29 0 4 0 415.00 32.45 0 6 0 273.99 18.39 0 6 0 258.50 23.65 0 8 0 6764.47 450.54 0 8 0 6843.31 445.02 0 10 0 138.04 10.11 0 10 0 114.45 20.04 0 12 0 29.89 3.80 0 12 0 6.83 19.39 0 14 0 239.97 17.37 0 14 0 242.36 32.93 0 16 0 1135.53 76.79 0 16 0 1291.10 89.61 0 18 0 41.82 5.55 0 18 0 35.60 22.30 0 20 0 5.86 8.55 0 22 0 40.69 11.23 0 24 0 64.07 12.47 1 -21 0 -8.08 13.89 1 -21 0 8.44 3.68 1 -19 0 116.57 9.91 1 -19 0 129.39 18.82 1 -17 0 17.98 3.39 1 -17 0 16.60 14.24 1 -15 0 531.35 37.02 1 -15 0 640.67 45.39 1 -13 0 90.71 17.49 -1 -13 0 116.30 17.73 1 -13 0 86.14 7.27 1 -11 0 1044.84 73.44 -1 -11 0 999.96 73.18 -1 -9 0 373.29 30.34 1 -9 0 361.41 30.26 -1 -7 0 2251.39 146.11 -1 -7 0 2151.12 149.60 -1 -5 0 992.00 75.10 -1 -5 0 1123.23 72.32 -1 -3 0 2131.97 164.75 -1 -3 0 2583.17 163.16 1 -1 0 1714.61 110.82 -1 -1 0 1636.67 111.62 -1 1 0 1604.55 101.54 -1 1 0 1488.06 101.65 -1 3 0 2317.13 151.10 -1 3 0 2196.06 152.36 1 3 0 2360.80 151.25 -1 5 0 1112.87 78.13 1 5 0 1156.36 75.36 1 7 0 2058.75 154.76 -1 7 0 2315.55 153.28 1 7 0 2309.24 149.32 -1 9 0 438.29 32.44 -1 9 0 360.35 25.30 1 9 0 366.60 34.82 1 9 0 384.60 25.50 -1 11 0 992.87 67.18 1 11 0 1121.02 78.47 -1 11 0 1081.27 74.97 1 13 0 89.47 8.95 -1 13 0 101.11 21.67 1 13 0 119.92 27.34 -1 13 0 146.82 9.39 1 15 0 531.18 41.63 1 15 0 603.45 40.22 1 15 0 639.80 55.38 -1 15 0 598.13 40.12 -1 15 0 626.87 51.62 -1 17 0 6.46 20.04 -1 17 0 19.05 4.07 1 17 0 20.09 3.99 1 17 0 18.00 7.18 1 19 0 127.82 13.59 1 21 0 5.71 7.94 -1 21 0 -3.43 9.85 -1 23 0 62.91 13.29 1 23 0 48.56 10.70 1 25 0 -4.87 8.83 2 -22 0 13.26 4.18 -2 -20 0 332.55 29.28 2 -20 0 306.54 27.87 2 -20 0 245.79 19.17 2 -18 0 109.84 9.43 -2 -18 0 136.29 19.56 2 -18 0 107.14 17.83 -2 -16 0 -1.09 12.62 2 -16 0 -5.99 12.08 2 -16 0 8.37 2.89 2 -14 0 79.81 6.94 -2 -14 0 106.08 17.86 2 -14 0 91.94 15.78 2 -12 0 2895.23 189.26 2 -12 0 2772.78 183.93 -2 -12 0 2955.27 189.60 2 -10 0 228.00 15.54 -2 -10 0 254.39 22.22 -2 -10 0 214.43 15.76 2 -10 0 216.14 21.22 2 -8 0 131.40 8.94 -2 -8 0 133.45 15.15 -2 -8 0 114.46 9.13 2 -8 0 121.82 13.76 2 -6 0 145.53 9.72 -2 -6 0 138.89 10.12 2 -6 0 159.39 13.42 -2 -6 0 148.26 14.65 2 -6 0 139.21 9.84 2 -4 0 9597.47 624.94 2 -4 0 9512.46 623.73 -2 -4 0 9808.00 624.07 -2 -4 0 9389.09 626.34 -2 -2 0 27.25 5.81 2 -2 0 28.30 2.32 -2 0 0 529.61 35.49 -2 0 0 547.24 36.13 -2 2 0 25.37 2.64 -2 2 0 30.95 3.28 2 4 0 9110.19 566.85 -2 4 0 9526.58 568.42 -2 4 0 8313.82 566.84 -2 4 0 8475.56 567.01 -2 6 0 150.50 10.05 -2 6 0 148.59 13.91 2 6 0 134.63 10.25 2 8 0 111.00 8.88 -2 8 0 133.41 14.86 2 10 0 239.03 16.34 -2 10 0 227.73 22.53 2 10 0 215.04 16.72 2 12 0 2867.48 179.33 -2 12 0 2854.17 185.51 -2 12 0 2739.98 179.05 2 12 0 2527.46 179.75 -2 14 0 79.55 19.72 -2 14 0 100.68 7.69 2 14 0 85.66 7.71 2 14 0 62.86 8.72 -2 16 0 19.12 16.49 2 16 0 13.17 3.53 -2 16 0 6.63 3.17 2 16 0 8.41 5.57 -2 18 0 120.40 22.35 -2 18 0 102.57 8.91 2 18 0 81.25 10.43 2 20 0 222.93 18.98 -2 22 0 28.53 12.75 2 22 0 17.58 7.70 2 24 0 5.31 7.35 3 -21 0 4.35 2.84 -3 -21 0 -4.60 13.98 -3 -21 0 0.70 3.73 -3 -19 0 262.04 25.06 3 -19 0 210.07 15.47 3 -17 0 14.29 3.18 3 -17 0 13.40 3.77 3 -17 0 28.72 12.73 -3 -17 0 20.55 13.61 3 -15 0 194.02 19.29 -3 -15 0 169.29 20.15 3 -15 0 155.69 11.94 3 -15 0 157.60 12.36 3 -13 0 100.28 7.21 3 -13 0 93.13 7.53 -3 -13 0 125.75 17.17 -3 -13 0 79.60 7.80 3 -13 0 95.91 8.02 3 -13 0 109.77 15.44 3 -11 0 1261.99 87.78 -3 -11 0 1182.87 84.32 3 -11 0 1318.83 83.73 3 -11 0 1271.28 84.30 -3 -11 0 1416.67 89.64 3 -9 0 259.42 17.47 -3 -9 0 289.93 23.75 -3 -9 0 259.80 18.13 3 -9 0 257.99 18.05 3 -9 0 238.96 20.94 -3 -7 0 765.86 50.18 3 -7 0 738.62 49.55 3 -7 0 782.30 51.83 -3 -7 0 834.76 54.06 -3 -5 0 1095.25 82.30 -3 -5 0 1132.49 84.78 -3 -3 0 2576.22 166.52 -3 -3 0 2465.13 168.53 3 -3 0 2548.53 166.73 3 -1 0 1435.11 86.81 -3 -1 0 1194.77 86.85 -3 1 0 1348.21 89.02 -3 3 0 2822.76 172.30 -3 3 0 2505.89 172.10 3 3 0 2533.64 174.96 -3 5 0 1168.08 77.47 3 5 0 1152.85 82.95 -3 5 0 1201.20 78.89 3 5 0 1209.22 77.06 -3 5 0 1140.33 77.24 -3 7 0 803.34 52.18 3 7 0 898.23 61.97 -3 7 0 870.47 55.38 3 7 0 757.15 52.11 -3 9 0 286.30 18.03 3 9 0 223.75 18.08 3 9 0 325.10 32.75 -3 9 0 286.42 23.05 -3 11 0 1309.29 83.66 3 11 0 1119.81 78.33 -3 13 0 121.56 18.48 3 13 0 88.39 8.61 -3 15 0 163.42 12.51 -3 15 0 219.15 23.26 3 15 0 148.71 13.17 3 15 0 233.97 34.30 -3 17 0 16.08 16.41 3 17 0 15.58 5.41 -3 17 0 9.28 3.65 3 17 0 24.24 28.55 3 19 0 199.94 16.52 3 21 0 -2.65 5.65 -4 -20 0 -2.15 13.52 4 -20 0 2.48 2.54 -4 -18 0 55.62 15.37 4 -18 0 29.78 3.73 4 -16 0 664.44 45.54 4 -16 0 649.70 44.50 4 -14 0 113.04 9.20 4 -14 0 107.73 8.08 -4 -14 0 115.72 16.46 -4 -14 0 101.09 8.86 4 -12 0 17.59 3.52 -4 -12 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22.87 2.82 -6 0 -6 50.43 7.72 -6 0 -6 54.81 5.17 -6 0 6 67.67 5.01 -6 2 -6 17.46 6.30 -6 2 6 22.61 8.53 6 4 6 174.32 17.05 -6 4 -6 163.91 16.14 6 6 6 -1.43 6.21 -6 6 6 8.30 6.20 6 6 -6 -0.87 5.40 -6 6 -6 4.77 6.56 6 8 6 28.41 6.78 -6 8 6 47.48 7.37 -6 8 -6 24.96 7.96 6 10 -6 17.85 8.48 -6 10 -6 14.55 8.10 -6 10 6 21.73 6.12 6 12 -6 48.72 10.43 6 14 -6 -0.64 8.19 7 -11 6 39.54 6.36 -7 -9 -6 7.45 8.97 7 -9 6 1.24 4.66 7 -9 -6 6.78 12.94 7 -7 6 16.98 5.90 -7 -7 -6 11.53 8.67 -7 -7 6 28.70 12.36 7 -7 -6 10.95 11.27 -7 -5 6 30.92 5.29 -7 -5 -6 38.72 8.96 7 -5 -6 44.58 12.27 -7 -5 6 64.42 12.84 -7 -5 -6 56.40 5.06 -7 -3 -6 53.85 7.65 -7 -3 6 58.32 6.10 -7 -3 -6 76.04 5.95 -7 -1 -6 6.75 5.52 -7 -1 -6 14.10 2.76 -7 -1 6 10.85 2.33 -7 -1 6 15.52 10.51 -7 1 -6 8.18 5.46 -7 1 -6 15.51 2.87 -7 1 6 10.98 1.86 -7 1 6 14.08 8.84 -7 3 -6 65.14 8.34 7 3 -6 36.98 6.76 7 5 -6 33.71 7.20 -7 5 -6 43.77 8.33 7 7 -6 13.13 6.86 -7 7 6 17.66 6.72 -7 7 -6 18.70 7.51 -7 9 -6 -4.89 7.36 -8 -6 -6 4.93 7.17 -8 -4 -6 8.10 6.83 8 -4 -6 9.27 9.93 -8 -4 6 21.53 10.77 -8 -2 6 0.93 10.48 -8 0 6 130.98 14.61 -8 0 -6 64.98 8.61 -8 2 -6 3.32 5.50 -8 2 6 14.15 9.10 -8 4 6 28.21 8.43 -8 4 -6 12.65 6.64 -8 6 -6 5.74 6.76 -8 8 -6 28.70 8.43 -9 -5 -6 -0.56 6.88 -9 -3 -6 -2.63 6.42 -9 3 -6 2.52 5.60 -9 5 -6 0.48 6.09 -10 -2 -6 -6.23 5.83 0 -16 7 20.64 4.14 0 -14 7 17.85 3.67 0 -14 7 15.19 4.11 0 -12 -7 10.94 14.18 0 -12 7 2.29 3.48 0 -12 7 3.58 2.59 0 -10 -7 9.13 12.76 0 -10 7 9.59 2.59 0 -10 7 6.79 3.55 0 -8 7 30.19 4.81 0 -8 7 36.92 3.85 0 -6 7 18.07 2.59 0 -6 7 26.81 10.02 0 -4 7 0.49 6.18 0 -4 7 6.78 2.23 0 -2 7 20.78 4.78 0 0 -7 37.70 9.41 0 0 7 35.77 4.48 0 2 7 21.66 2.95 0 2 7 18.71 3.10 0 4 -7 7.51 7.99 0 4 7 3.22 2.17 0 6 -7 26.26 8.38 0 6 7 24.82 3.42 0 8 -7 43.50 9.12 0 8 7 33.88 4.15 1 -15 7 6.74 3.42 -1 -15 7 12.30 4.59 -1 -15 7 12.33 3.57 1 -13 7 0.65 2.93 1 -13 7 0.23 2.95 -1 -13 7 2.77 2.78 -1 -13 7 0.70 4.01 1 -11 7 8.67 2.84 -1 -11 -7 5.67 11.86 1 -11 -7 21.41 13.44 1 -11 7 2.89 2.85 -1 -11 7 3.37 4.13 -1 -11 7 9.78 2.68 -1 -9 -7 12.88 11.49 1 -9 -7 -5.73 12.58 1 -9 7 3.93 2.94 -1 -9 7 6.59 3.90 1 -9 7 -0.39 2.89 -1 -9 7 4.92 2.08 -1 -7 7 10.48 2.08 1 -7 7 10.80 2.53 -1 -7 7 7.44 10.56 1 -7 7 4.21 9.27 1 -7 7 7.45 2.97 -1 -5 7 1.50 1.62 -1 -5 7 9.03 8.89 1 -5 7 -1.22 5.59 1 -5 7 0.74 2.41 -1 -3 7 2.89 7.26 1 -3 7 4.04 3.26 -1 -1 -7 13.85 7.79 -1 -1 7 16.10 5.21 1 -1 7 2.48 1.90 1 1 7 7.49 1.75 -1 1 -7 3.10 7.48 1 1 -7 5.38 7.78 1 1 7 6.25 1.96 -1 1 7 6.96 3.45 -1 3 -7 7.01 7.18 1 3 -7 -0.69 8.01 1 3 7 2.92 1.80 -1 3 7 3.82 2.97 -1 5 7 4.67 2.72 -1 5 -7 0.63 7.52 1 5 -7 7.80 8.51 -1 5 7 4.11 2.69 1 5 7 0.59 1.87 -1 7 -7 5.64 7.07 -1 7 7 8.72 2.93 1 7 7 8.60 2.37 -1 9 -7 3.84 7.16 -1 11 -7 5.43 7.67 1 11 -7 2.09 8.17 -2 -14 7 4.32 4.77 2 -14 7 -0.79 3.47 2 -12 -7 20.27 15.63 -2 -12 7 24.61 5.26 2 -12 7 34.82 4.97 2 -10 -7 3.51 13.37 2 -10 7 13.90 3.30 -2 -10 7 11.30 4.73 2 -8 7 2.11 2.55 -2 -8 7 4.49 1.93 -2 -8 7 -2.06 11.54 2 -8 7 -3.24 8.74 2 -8 -7 -1.14 12.91 2 -8 7 3.60 2.16 -2 -6 7 13.27 10.58 2 -6 7 14.04 5.16 2 -6 7 18.23 2.68 -2 -6 7 16.61 2.12 2 -6 7 15.46 3.38 2 -4 7 38.79 3.75 2 -4 7 50.91 5.68 -2 -4 7 35.85 3.09 -2 -4 7 37.90 10.47 2 -4 7 39.44 3.83 -2 -2 -7 43.23 8.39 2 -2 7 25.09 2.40 -2 -2 7 43.93 8.96 -2 0 -7 13.47 7.87 2 0 7 6.95 1.54 -2 0 7 9.50 5.43 -2 2 -7 22.98 8.34 2 2 -7 18.22 8.88 2 2 7 25.69 2.70 -2 2 7 28.03 5.38 2 2 7 26.22 11.50 -2 4 -7 38.77 8.33 -2 4 7 39.03 5.18 2 4 7 27.54 11.13 -2 6 -7 25.00 7.75 -2 6 7 19.26 3.57 2 6 7 11.63 10.02 -2 6 7 13.39 3.71 -2 8 -7 -0.62 7.06 2 8 -7 12.04 8.53 -2 10 -7 23.60 8.48 2 10 -7 22.61 9.42 2 10 7 15.77 3.23 3 -13 7 -0.81 3.68 3 -13 -7 15.37 15.67 -3 -13 7 6.38 4.77 3 -11 7 13.82 3.54 3 -11 -7 1.22 14.75 -3 -11 7 13.71 5.01 3 -9 7 0.51 2.86 -3 -9 -7 -10.82 10.37 3 -9 -7 3.44 13.80 3 -7 -7 2.29 13.65 -3 -7 7 -5.17 11.59 3 -7 7 7.44 3.52 3 -7 7 4.18 3.24 -3 -5 7 8.96 1.57 3 -5 7 5.43 3.91 -3 -5 7 9.15 10.66 -3 -3 -7 10.82 7.30 -3 -3 7 17.03 9.70 -3 -1 -7 5.99 6.85 -3 -1 7 -1.32 7.87 -3 1 -7 1.14 6.98 -3 1 7 -0.51 5.77 -3 3 -7 18.73 7.48 3 3 7 9.20 1.74 -3 3 7 9.39 5.14 3 3 7 20.15 10.21 -3 5 -7 8.53 6.92 3 5 -7 8.13 8.60 3 5 7 6.79 1.91 -3 5 7 11.80 4.58 3 5 7 -0.81 9.53 -3 7 -7 -3.63 6.74 3 7 -7 8.23 8.76 3 7 7 5.68 2.15 3 7 7 0.77 9.51 -3 7 7 4.76 3.86 -3 9 -7 1.26 6.83 3 9 -7 3.06 8.65 3 9 7 2.03 2.44 3 9 7 0.75 9.75 3 11 7 13.55 3.14 3 11 7 11.72 8.82 4 -12 7 2.10 3.39 -4 -12 7 3.46 4.86 4 -10 -7 1.15 13.90 4 -10 7 2.38 3.35 -4 -8 -7 22.55 10.88 -4 -8 7 29.11 13.91 4 -8 -7 41.37 15.39 4 -8 7 32.24 5.16 4 -6 7 18.75 5.10 -4 -6 7 20.02 11.85 -4 -4 -7 1.39 6.13 -4 -4 7 -7.04 10.03 -4 -2 -7 21.51 7.18 -4 -2 7 25.05 10.06 -4 0 -7 43.59 8.63 -4 0 7 57.36 10.04 -4 2 -7 9.67 7.51 -4 2 7 18.96 6.67 4 2 7 17.66 9.73 -4 4 -7 -0.54 6.16 4 4 7 1.63 1.66 -4 4 7 2.29 5.35 4 4 7 -0.75 9.36 -4 6 -7 17.40 7.75 4 6 -7 21.12 9.32 4 6 7 17.46 2.65 4 6 7 4.37 8.68 -4 6 7 18.57 5.60 -4 8 -7 34.93 8.14 4 8 -7 29.68 10.46 4 8 7 34.28 9.62 -4 8 7 33.30 5.93 4 10 -7 3.03 9.37 5 -13 -7 -1.28 16.93 5 -11 -7 -6.86 14.52 5 -11 7 1.42 4.12 -5 -9 7 7.76 12.86 5 -9 -7 -3.23 14.38 5 -9 7 11.64 4.90 -5 -7 -7 17.39 10.13 5 -7 7 16.58 5.38 5 -7 -7 8.54 13.14 -5 -7 7 15.03 12.29 -5 -5 7 5.82 12.14 -5 -3 -7 6.30 5.97 -5 -3 7 0.89 10.23 -5 -1 -7 8.48 6.57 -5 -1 7 8.30 9.70 -5 1 -7 5.55 6.47 -5 1 7 24.36 8.42 -5 3 -7 3.60 6.35 -5 3 7 4.57 7.15 5 3 7 6.54 9.25 -5 5 -7 1.11 6.34 5 5 7 0.66 8.35 -5 5 7 3.93 5.85 -5 7 -7 2.32 6.95 5 7 7 16.69 8.46 -5 7 7 18.78 6.00 -5 9 7 9.32 5.34 6 -10 -7 1.05 14.12 6 -10 7 5.35 5.22 6 -8 7 -2.46 5.68 6 -8 -7 -1.01 13.41 6 -6 -7 15.01 13.84 -6 -6 7 -1.03 11.52 -6 -4 -7 17.35 6.01 -6 -4 7 41.99 11.61 -6 -2 -7 11.91 6.40 -6 -2 7 30.23 12.13 -6 0 -7 -5.17 6.36 -6 0 7 9.51 9.16 -6 2 -7 4.39 6.29 -6 2 7 16.25 8.45 -6 4 -7 29.71 7.64 -6 4 7 37.44 8.69 6 4 7 38.25 9.86 -6 6 -7 0.56 6.91 -6 6 7 1.61 6.39 7 -5 -7 11.83 13.08 -7 -1 -7 -3.95 6.20 -7 1 -7 -1.37 6.09 -7 3 -7 14.39 6.58 -7 5 -7 -0.53 6.45 -8 4 -7 1.48 6.26 0 -8 8 89.71 13.94 0 -8 8 71.59 7.42 0 -6 8 28.52 8.48 0 -4 8 41.98 6.81 0 -2 8 5.98 3.81 0 0 8 182.24 13.29 0 0 8 182.34 13.20 0 0 -8 183.79 18.04 0 2 8 7.88 2.52 0 2 -8 9.25 7.86 0 2 8 8.31 2.69 0 4 -8 39.27 10.38 0 4 8 42.80 4.48 0 6 8 21.95 3.55 -1 -11 8 27.80 14.53 -1 -9 8 6.03 12.16 -1 -9 8 5.67 4.28 -1 -7 8 56.92 12.17 -1 -5 8 27.87 9.57 1 -5 8 22.65 3.88 1 -3 8 52.93 4.91 -1 -3 8 49.35 8.15 -1 -1 -8 59.36 10.10 1 -1 8 44.68 3.93 -1 -1 8 46.33 6.43 -1 1 -8 46.54 9.79 1 1 -8 37.19 10.41 1 1 8 43.64 4.03 -1 1 8 36.45 5.18 -1 3 -8 52.62 10.72 1 3 -8 71.39 11.77 -1 3 8 60.44 5.69 -1 3 8 49.34 5.34 1 3 8 49.08 4.80 -2 -12 8 31.08 6.07 -2 -10 8 4.40 13.31 -2 -10 8 8.44 4.85 -2 -8 8 24.50 12.89 -2 -6 8 4.07 10.07 -2 -4 8 148.04 16.43 -2 -2 -8 7.92 7.85 -2 -2 8 9.40 6.74 -2 0 -8 43.98 10.19 -2 0 8 53.35 7.49 -2 2 -8 4.64 7.89 -2 2 8 14.10 4.89 -2 4 8 127.91 10.68 -2 4 -8 121.40 14.39 -2 6 8 3.64 3.76 -3 -11 8 21.76 13.83 -3 -11 8 18.68 5.60 -3 -9 8 1.10 12.78 3 -7 -8 16.34 15.02 -3 -7 8 30.14 12.73 -3 -5 8 33.50 11.63 -3 -3 8 67.16 12.07 -3 -1 -8 19.02 8.46 -3 -1 8 31.99 8.23 -3 1 -8 32.94 8.65 -3 1 8 25.29 6.97 -3 3 -8 43.21 9.64 -3 3 8 62.24 7.52 -3 5 8 25.62 5.41 -3 7 8 26.44 5.40 4 -8 -8 31.92 15.87 -4 -8 8 38.61 13.96 -4 -6 8 13.99 11.05 -4 -4 8 37.64 11.87 -4 -2 -8 10.84 7.58 -4 -2 8 -5.87 9.39 -4 0 8 124.66 12.86 -4 0 -8 84.94 11.93 -4 2 -8 6.83 7.54 -4 2 8 6.11 6.44 -4 4 8 37.05 7.29 -4 6 8 14.91 5.42 -4 8 8 54.65 7.45 5 -7 -8 21.31 15.67 -5 -5 8 0.93 10.87 -5 -3 -8 15.57 7.10 -5 -3 8 11.48 10.95 -5 -1 -8 25.86 8.02 -5 -1 8 46.47 10.65 -5 1 -8 37.36 8.93 -5 1 8 26.58 8.70 -5 3 8 16.94 7.15 -5 5 8 3.41 5.93 -6 0 -8 8.85 7.14 0 0 0 0.00 0.00 TITL S-3AEPI-425-3_auto in Amm2 REM Amm2 (#38, found as Cm2m in cab setting) CELL 0.71073 6.508806 9.474260 17.730090 90.0000 90.0000 90.0000 ZERR 16.00 0.000433 0.000682 0.001170 0.0000 0.0000 0.0000 LATT -5 SYMM -x,-y, z SYMM x,-y, z SYMM -x, y, z SFAC C H N I Pb UNIT 16.00 16.00 16.00 16.00 16.00 REM CrysAlisPro recorded range (K): Min=425.0; max=425.0; aver:425.0 TEMP 152 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 38663 _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 5.399 _oxdiff_exptl_absorpt_empirical_full_min 0.221 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' '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 Pb1 Pb 0.500000 0.63009(3) -0.500000 0.0488(3) Uani 1 2 d S T P . . I1 I 0.26566(13) 0.500000 -0.500000 0.0524(4) Uani 1 2 d S T P . . I2 I 0.500000 0.63097(10) -1.000000 0.1000(8) Uani 1 2 d S T P . . I3 I 0.750000 0.750000 -0.499(2) 0.1172(8) Uani 1 2 d S T P . . N1 N 0.974(5) 0.376(3) -1.208(8) 0.044(11) Uani 0.25 1 d . U P A -1 H1A H 0.993461 0.407108 -1.311705 0.053 Uiso 0.25 1 calc R U P A -1 H1B H 0.881584 0.374675 -1.187072 0.053 Uiso 0.25 1 calc R U P A -1 H1C H 1.005746 0.330150 -1.236923 0.053 Uiso 0.25 1 calc R U P A -1 C1 C 0.939(9) 0.360(4) -0.877(13) 0.053(14) Uani 0.25 1 d . U P A -1 H1D H 0.937553 0.387751 -0.750200 0.079 Uiso 0.25 1 calc R U P A -1 H1E H 0.974941 0.309995 -0.851129 0.079 Uiso 0.25 1 calc R U P A -1 H1F H 0.845399 0.356490 -0.931213 0.079 Uiso 0.25 1 calc R U P A -1 C2 C 1.038(5) 0.401(3) -1.037(9) 0.045(9) Uani 0.25 1 d . U P A -1 H2 H 1.137438 0.385812 -1.027125 0.054 Uiso 0.25 1 calc R U P A -1 C7 C 0.879(3) 0.5188(13) -0.993(18) 0.047(8) Uani 0.25 1 d G U P A -1 H7 H 0.804051 0.484888 -0.994349 0.057 Uiso 0.25 1 calc R U P A -1 C3 C 1.017(3) 0.4924(14) -1.01(2) 0.047(7) Uani 0.25 1 d G U P A -1 C4 C 1.129(3) 0.5430(18) -1.005(19) 0.050(8) Uani 0.25 1 d G U P A -1 H4 H 1.221098 0.525440 -1.014947 0.060 Uiso 0.25 1 calc R U P A -1 C5 C 1.103(2) 0.6200(16) -0.988(12) 0.042(9) Uani 0.25 1 d G U P A -1 H5 H 1.178037 0.653833 -0.986680 0.050 Uiso 0.25 1 calc R U P A -1 C6 C 0.965(2) 0.6463(12) -0.974(7) 0.032(10) Uani 0.25 1 d G U P A -1 H6 H 0.947984 0.697755 -0.962249 0.038 Uiso 0.25 1 calc R U P A -1 N2 N 0.853(2) 0.5957(14) -0.976(10) 0.046(9) Uani 0.25 1 d G U P A -1 H2A H 0.767930 0.611959 -0.966820 0.055 Uiso 0.25 1 calc R U P A -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0505(4) 0.0416(4) 0.0544(5) 0.000 0.0007(8) 0.000 I1 0.0519(7) 0.0478(7) 0.0574(7) -0.005(3) 0.000 0.000 I2 0.149(2) 0.1111(14) 0.0400(7) 0.000 -0.029(2) 0.000 I3 0.0888(12) 0.0687(11) 0.194(2) 0.000 0.000 -0.0409(9) N1 0.03(2) 0.051(19) 0.047(14) -0.013(13) 0.016(13) -0.004(16) C1 0.06(2) 0.049(19) 0.05(2) -0.001(17) 0.021(18) 0.003(18) C2 0.042(14) 0.048(10) 0.046(14) -0.004(10) 0.008(10) 0.000(9) C7 0.055(10) 0.042(11) 0.045(14) -0.004(12) -0.001(12) 0.002(8) C3 0.051(10) 0.046(8) 0.044(13) -0.002(11) -0.002(11) 0.001(8) C4 0.054(10) 0.047(10) 0.048(14) -0.005(11) -0.002(12) -0.001(8) C5 0.039(11) 0.046(10) 0.040(15) -0.001(12) 0.002(11) 0.000(9) C6 0.039(12) 0.037(11) 0.018(16) 0.007(10) -0.001(10) 0.002(7) N2 0.044(11) 0.042(10) 0.051(16) -0.003(11) -0.002(11) -0.002(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 I1 Pb1 I1 87.81(3) . 2_665 ? I1 Pb1 I2 90.20(2) 2_665 . ? I1 Pb1 I2 90.20(2) 2_665 1_556 ? I1 Pb1 I2 90.20(2) . . ? I1 Pb1 I2 90.20(2) . 1_556 ? I2 Pb1 I2 179.46(6) 1_556 . ? I3 Pb1 I1 175.82(2) 3_654 2_665 ? I3 Pb1 I1 175.82(2) . . ? I3 Pb1 I1 88.003(17) . 2_665 ? I3 Pb1 I1 88.003(17) 3_654 . ? I3 Pb1 I2 89.8(3) . 1_556 ? I3 Pb1 I2 89.9(3) 3_654 1_556 ? I3 Pb1 I2 89.8(3) 3_654 . ? I3 Pb1 I2 89.9(3) . . ? I3 Pb1 I3 96.180(17) . 3_654 ? Pb1 I1 Pb1 92.19(3) 2_665 . ? Pb1 I2 Pb1 179.46(6) . 1_554 ? Pb1 I3 Pb1 179.9(5) . 6_665 ? H1A N1 H1B 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1D C1 H1E 109.5 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? C2 C1 H1D 109.5 . . ? C2 C1 H1E 109.5 . . ? C2 C1 H1F 109.5 . . ? N1 C2 C1 97(6) . . ? N1 C2 H2 113.1 . . ? N1 C2 C3 112(6) . . ? C1 C2 H2 113.1 . . ? C1 C2 C3 108(5) . . ? C3 C2 H2 113.1 . . ? C3 C7 H7 120.0 . . ? C3 C7 N2 120.0 . . ? N2 C7 H7 120.0 . . ? C7 C3 C2 117(2) . . ? C4 C3 C2 123(2) . . ? C4 C3 C7 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 120.0 . . ? C4 C5 C6 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 H6 120.0 . . ? C5 C6 N2 120.0 . . ? N2 C6 H6 120.0 . . ? C7 N2 H2A 120.0 . . ? C6 N2 C7 120.0 . . ? C6 N2 H2A 120.0 . . ? 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 I1 3.2015(9) . ? Pb1 I1 3.2015(9) 2_665 ? Pb1 I2 3.25444(19) 1_556 ? Pb1 I2 3.25444(19) . ? Pb1 I3 3.1827(4) . ? Pb1 I3 3.1827(4) 3_654 ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N1 C2 1.34(7) . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C1 H1F 0.9600 . ? C1 C2 1.59(9) . ? C2 H2 0.9800 . ? C2 C3 1.64(6) . ? C7 H7 0.9300 . ? C7 C3 1.3900 . ? C7 N2 1.3900 . ? C3 C4 1.3900 . ? C4 H4 0.9300 . ? C4 C5 1.3900 . ? C5 H5 0.9300 . ? C5 C6 1.3900 . ? C6 H6 0.9300 . ? C6 N2 1.3900 . ? N2 H2A 0.8600 . ? 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 N1 C2 C3 C7 59(7) . . . . ? N1 C2 C3 C4 -118(6) . . . . ? C1 C2 C3 C7 -46(8) . . . . ? C1 C2 C3 C4 136(7) . . . . ? C2 C3 C4 C5 177(10) . . . . ? C7 C3 C4 C5 0.0 . . . . ? C3 C7 N2 C6 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 N2 0.0 . . . . ? C5 C6 N2 C7 0.0 . . . . ? N2 C7 C3 C2 -177(9) . . . . ? N2 C7 C3 C4 0.0 . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.47887 2 0.52113