#------------------------------------------------------------------------------ #$Date: 2021-05-19 01:24:15 +0300 (Wed, 19 May 2021) $ #$Revision: 265319 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/39/4003947.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_4003947 loop_ _publ_author_name 'Zhang, Wenhao' 'Zhang, Weihua' 'Wang, Kai' 'Chu, Yanmeng' 'Du, Jiankang' 'Mei, Anyi' 'Rong, Yaoguang' 'Hu, Yue' 'Han, Hongwei' _publ_section_title ; Revealing the Role of Bifunctional Molecules in Crystallizing Methylammonium Lead Iodide through Geometric Isomers ; _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/acs.chemmater.1c00391 _journal_year 2021 _chemical_formula_moiety '2(C7 H14 N O2), 0.5(I8 Pb2)' _chemical_formula_sum 'C14 H28 I4 N2 O4 Pb' _chemical_formula_weight 1003.17 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2020-11-11 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 102.027(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 35.9280(17) _cell_length_b 9.1976(4) _cell_length_c 8.6505(4) _cell_measurement_reflns_used 5308 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 73.3960 _cell_measurement_theta_min 4.9620 _cell_volume 2795.8(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_unetI/netI 0.0345 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 9044 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.025 _diffrn_reflns_theta_min 2.515 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 46.561 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.21023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'pale red' _exptl_crystal_density_diffrn 2.383 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description platy _exptl_crystal_F_000 1808 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.857 _refine_diff_density_min -1.541 _refine_diff_density_rms 0.156 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 117 _refine_ls_number_reflns 2771 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.120 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0363 _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^)+(0.0571P)^2^+3.4744P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1010 _refine_ls_wR_factor_ref 0.1034 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2319 _reflns_number_total 2771 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cm1c00391_si_002.cif _cod_data_source_block 1111_sq _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_crystal_density_meas' value 'none' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 4003947 _shelx_shelxl_version_number 2018/3 _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. ; _oxdiff_exptl_absorpt_empirical_full_min 0.546 _oxdiff_exptl_absorpt_empirical_full_max 3.020 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H,H) groups At 1.5 times of: All O(H) groups 2.a Ternary CH refined with riding coordinates: C1(H1), C6(H6) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B) 2.c Idealised Me refined as rotating group: N1(H1A,H1B,H1C) 2.d Idealised tetrahedral OH refined as rotating group: O1(H1D) ; _shelx_res_file ; TITL 1111_a.res in C2/c 1111_sq.res created by SHELXL-2018/3 at 09:28:07 on 11-Nov-2020 REM Old TITL 1111 in C2/c REM SHELXT solution in C2/c: R1 0.106, Rweak 0.005, Alpha 0.017 REM 0.376 for 177 systematic absences, Orientation as input REM Formula found by SHELXT: C14 N2 O4 I4 Pb CELL 1.54178 35.928 9.1976 8.6505 90 102.027 90 ZERR 4 0.0017 0.0004 0.0004 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O I Pb UNIT 56 112 8 16 16 4 L.S. 10 0 5 PLAN 20 BOND list 4 ABIN fmap 2 acta REM REM REM WGHT 0.057100 3.474400 FVAR 0.11083 C1 1 0.640981 0.700992 0.388451 11.00000 0.06468 0.06138 = 0.05526 -0.00548 0.00557 0.00298 AFIX 13 H1 2 0.641947 0.649464 0.290205 11.00000 -1.20000 AFIX 0 C2 1 0.644286 0.858508 0.359670 11.00000 0.06157 0.08093 = 0.07564 0.01126 -0.00025 0.00127 AFIX 23 H2A 2 0.667295 0.876798 0.320759 11.00000 -1.20000 H2B 2 0.646210 0.910939 0.458314 11.00000 -1.20000 AFIX 0 C3 1 0.604873 0.658348 0.437748 11.00000 0.05912 0.08310 = 0.08869 0.03512 0.00824 0.00251 AFIX 23 H3A 2 0.604319 0.700391 0.540081 11.00000 -1.20000 H3B 2 0.603679 0.553414 0.446826 11.00000 -1.20000 AFIX 0 C4 1 0.610279 0.913376 0.240706 11.00000 0.06000 0.06446 = 0.08043 0.01833 0.00154 0.00607 AFIX 23 H4A 2 0.610954 0.873760 0.137407 11.00000 -1.20000 H4B 2 0.611629 1.018452 0.234005 11.00000 -1.20000 AFIX 0 C5 1 0.570821 0.712570 0.314970 11.00000 0.05180 0.10505 = 0.10663 0.03977 0.00665 0.00308 AFIX 23 H5A 2 0.569757 0.660523 0.216619 11.00000 -1.20000 H5B 2 0.547603 0.691659 0.351307 11.00000 -1.20000 AFIX 0 C6 1 0.572919 0.870574 0.285624 11.00000 0.06375 0.08501 = 0.06947 0.00869 0.00921 0.01278 AFIX 13 H6 2 0.572181 0.919876 0.385371 11.00000 -1.20000 AFIX 0 C7 1 0.540001 0.928262 0.163759 11.00000 0.06453 0.10179 = 0.06867 0.01395 0.00470 0.00711 N1 3 0.674960 0.652858 0.513718 11.00000 0.06028 0.05982 = 0.06038 -0.00009 -0.00247 0.00743 AFIX 137 H1A 2 0.696365 0.677750 0.484027 11.00000 -1.20000 H1B 2 0.674292 0.556814 0.525372 11.00000 -1.20000 H1C 2 0.674124 0.695818 0.605120 11.00000 -1.20000 AFIX 0 O1 4 0.537158 1.065561 0.156874 11.00000 0.09581 0.09549 = 0.12543 0.01579 -0.02733 0.02457 AFIX 147 H1D 2 0.517013 1.088117 0.098039 11.00000 -1.50000 AFIX 0 O2 4 0.519310 0.846519 0.074292 11.00000 0.10003 0.10890 = 0.11387 0.01745 -0.02893 0.01167 I1 5 0.752729 0.443756 0.813181 11.00000 0.06919 0.04665 = 0.04800 -0.01243 0.00840 0.00640 I2 5 0.660215 0.279313 0.414181 11.00000 0.06259 0.06199 = 0.06810 -0.00109 0.01216 -0.00699 PB1 6 0.750000 0.250000 0.500000 10.50000 0.05725 0.04054 = 0.04385 0.00005 0.00797 0.00132 HKLF 4 REM 1111_a.res in C2/c REM wR2 = 0.1034, GooF = S = 1.120, Restrained GooF = 1.120 for all data REM R1 = 0.0363 for 2319 Fo > 4sig(Fo) and 0.0426 for all 2771 data REM 117 parameters refined using 0 restraints END WGHT 0.0571 3.4750 REM Highest difference peak 0.857, deepest hole -1.541, 1-sigma level 0.156 Q1 1 0.7633 0.3220 0.4248 11.00000 0.05 0.86 Q2 1 0.6662 0.3579 0.3439 11.00000 0.05 0.79 Q3 1 0.7615 0.1717 0.4191 11.00000 0.05 0.79 Q4 1 0.7506 0.2881 0.7767 11.00000 0.05 0.74 Q5 1 0.7382 0.1408 0.4064 11.00000 0.05 0.71 Q6 1 0.7430 0.2377 0.3408 11.00000 0.05 0.65 Q7 1 0.7688 0.4852 0.7720 11.00000 0.05 0.62 Q8 1 0.6782 0.2433 0.3212 11.00000 0.05 0.61 Q9 1 0.7396 0.5155 0.8831 11.00000 0.05 0.61 Q10 1 0.6492 0.3649 0.4869 11.00000 0.05 0.58 Q11 1 0.6429 0.2143 0.4963 11.00000 0.05 0.57 Q12 1 0.7401 0.3926 0.4600 11.00000 0.05 0.55 Q13 1 0.6669 0.4018 0.4750 11.00000 0.05 0.55 Q14 1 0.6415 0.7768 0.4578 11.00000 0.05 0.55 Q15 1 0.7616 0.4581 0.9707 11.00000 0.05 0.54 Q16 1 0.6280 0.3003 0.4485 11.00000 0.05 0.52 Q17 1 0.7428 0.0961 0.4661 11.00000 0.05 0.52 Q18 1 0.7595 0.2933 0.8562 11.00000 0.05 0.52 Q19 1 0.7607 0.3732 0.7305 11.00000 0.05 0.50 Q20 1 0.7092 0.4442 0.4911 11.00000 0.05 0.50 ; _shelx_res_checksum 71749 _shelx_hkl_file ; -2 0 0 4728.32 167.91 4 0 0 1159.91 45.10 -4 0 0 1351.19 45.21 -6 0 0 732.57 28.60 6 0 0 795.25 28.45 8 0 0 3613.45 127.46 -8 0 0 3467.46 127.74 10 0 0 9631.04 349.14 -10 0 0 9999.00 349.84 12 0 0 7583.29 278.87 -12 0 0 8084.41 280.13 -14 0 0 3598.26 127.24 14 0 0 3328.87 124.83 -16 0 0 422.30 20.88 16 0 0 357.84 17.06 -18 0 0 746.98 35.87 18 0 0 692.36 30.49 18 0 0 791.75 27.63 18 0 0 700.65 27.67 20 0 0 1703.67 69.92 -20 0 0 1858.91 78.73 20 0 0 1935.80 66.69 20 0 0 1776.79 66.91 22 0 0 3033.33 109.92 -22 0 0 3319.41 126.80 24 0 0 1277.77 47.20 26 0 0 278.70 12.20 28 0 0 239.85 11.05 30 0 0 202.28 9.85 32 0 0 365.18 15.41 34 0 0 475.21 19.23 36 0 0 108.71 6.19 38 0 0 22.94 2.95 40 0 0 8.85 1.97 -42 0 0 29.71 2.69 -1 -1 0 154.50 7.83 1 1 0 195.84 8.31 3 1 0 331.48 11.52 -3 -1 0 313.53 11.55 -5 -1 0 3.10 1.63 5 1 0 2.71 1.28 7 1 0 76.98 4.10 -7 -1 0 76.93 4.43 -7 1 0 71.05 4.62 7 1 0 82.21 3.69 9 1 0 151.59 6.14 -9 1 0 143.97 7.62 -11 -1 0 215.59 8.27 -11 -1 0 207.45 11.24 -11 1 0 232.28 11.44 11 -1 0 215.15 8.23 -13 -1 0 6.51 4.06 -13 1 0 8.46 4.69 13 1 0 9.14 1.71 13 -1 0 9.79 3.28 -15 -1 0 33.79 5.73 -15 1 0 31.49 6.71 15 1 0 30.12 2.54 15 -1 0 26.74 4.32 17 1 0 13.87 2.89 -17 -1 0 12.74 5.27 -17 1 0 18.08 7.21 17 -1 0 17.62 2.00 17 1 0 14.56 2.00 17 -1 0 15.69 4.21 17 -1 0 19.79 2.78 17 1 0 14.41 2.06 19 1 0 127.13 7.27 -19 1 0 152.37 7.29 19 -1 0 149.83 10.20 19 -1 0 152.17 7.16 19 1 0 148.77 6.45 19 1 0 130.75 6.36 19 -1 0 155.71 6.45 19 1 0 161.16 8.77 -19 -1 0 152.98 12.93 19 1 0 137.13 7.03 -21 1 0 73.61 5.43 21 1 0 68.75 5.82 21 1 0 74.63 5.75 21 1 0 66.93 4.17 21 1 0 68.64 4.19 21 -1 0 76.50 4.25 21 -1 0 70.01 4.93 23 1 0 31.95 3.54 23 1 0 31.34 3.19 -23 1 0 37.05 4.97 23 -1 0 36.52 3.23 23 -1 0 26.50 4.08 25 -1 0 33.27 3.39 -25 1 0 36.74 5.69 25 1 0 27.45 3.08 25 1 0 30.69 3.65 25 -1 0 20.46 4.19 -27 1 0 11.02 5.21 27 1 0 6.88 2.93 27 -1 0 2.71 3.17 27 -1 0 12.33 4.25 27 1 0 5.51 3.43 29 -1 0 47.85 5.17 29 1 0 35.63 3.95 29 1 0 44.51 4.64 29 -1 0 46.38 4.36 31 -1 0 50.63 4.60 31 1 0 53.71 4.97 31 1 0 41.30 4.12 31 -1 0 54.93 5.25 33 -1 0 12.28 4.36 33 1 0 16.75 4.62 33 -1 0 18.53 3.82 33 1 0 15.52 3.21 35 -1 0 9.66 3.47 35 -1 0 6.08 3.82 35 1 0 5.92 2.65 35 1 0 8.55 4.45 37 1 0 3.02 3.71 37 -1 0 1.41 3.15 37 1 0 2.50 2.24 37 -1 0 5.92 3.26 39 -1 0 10.59 2.84 39 1 0 17.12 3.80 -41 1 0 10.13 2.28 41 -1 0 4.97 2.02 -43 1 0 4.04 1.58 43 -1 0 4.77 1.71 -43 -1 0 5.03 1.65 0 2 0 2217.53 80.62 2 2 0 361.01 15.56 -2 2 0 356.13 14.06 -4 -2 0 892.84 32.34 4 2 0 995.60 34.83 -6 -2 0 1148.17 47.31 6 2 0 1275.32 48.16 -6 -2 0 1292.96 45.66 -8 2 0 53.34 3.93 -8 -2 0 58.42 4.30 8 2 0 55.14 6.25 -8 -2 0 53.84 5.47 8 2 0 58.60 3.43 -10 2 0 668.40 24.94 -10 -2 0 602.25 24.78 10 2 0 672.81 24.09 10 2 0 638.26 27.02 -12 2 0 1181.54 43.08 12 2 0 1077.66 41.21 14 2 0 42.51 3.34 -14 -2 0 35.22 2.45 14 -2 0 33.40 2.41 -14 2 0 45.81 5.38 16 -2 0 280.17 9.42 -16 2 0 253.46 10.11 -16 -2 0 231.50 9.03 16 2 0 255.32 9.51 -16 -2 0 230.87 14.15 16 2 0 262.81 11.02 18 2 0 132.90 6.38 18 2 0 144.54 7.75 -18 2 0 136.09 7.16 18 2 0 128.67 7.12 18 2 0 130.52 5.92 18 -2 0 145.53 11.05 18 -2 0 152.80 6.25 -18 -2 0 140.91 11.52 20 2 0 42.21 3.47 20 -2 0 58.79 5.21 20 2 0 45.23 4.23 20 2 0 51.63 3.10 -20 2 0 54.56 4.56 20 -2 0 51.15 3.43 20 2 0 43.92 4.75 22 2 0 426.83 17.60 22 -2 0 422.62 17.62 22 -2 0 437.45 16.17 22 2 0 386.30 15.82 -22 2 0 417.65 17.30 22 2 0 396.89 16.45 -24 2 0 79.99 6.10 24 -2 0 82.23 4.80 24 -2 0 71.64 6.64 24 2 0 69.55 5.27 24 2 0 64.95 4.17 -26 2 0 4.17 4.21 26 -2 0 2.50 2.82 26 2 0 4.06 2.39 26 -2 0 1.93 5.21 26 2 0 2.76 3.67 28 2 0 60.24 5.64 28 -2 0 61.57 6.60 28 -2 0 69.47 4.93 -28 2 0 67.38 5.95 28 2 0 54.82 4.10 30 2 0 1.26 4.08 30 -2 0 3.36 3.23 -30 2 0 1.24 3.69 30 2 0 2.11 2.32 30 -2 0 4.80 4.84 32 2 0 67.93 6.12 32 -2 0 71.10 4.95 32 2 0 51.02 4.01 32 -2 0 61.72 6.64 34 -2 0 90.41 7.16 34 2 0 107.36 7.18 34 -2 0 109.01 6.05 36 2 0 15.43 4.43 36 -2 0 7.86 4.43 38 2 0 6.79 3.56 38 -2 0 2.13 3.52 -38 2 0 4.88 2.86 40 -2 0 2.78 2.71 -40 2 0 4.84 2.24 40 -2 0 1.89 2.19 40 2 0 5.90 2.95 -40 2 0 4.34 2.19 -42 2 0 1.11 1.48 42 -2 0 2.82 1.56 42 -2 0 2.50 1.87 -42 2 0 0.65 1.56 -1 3 0 209.01 9.31 1 3 0 210.75 9.87 3 3 0 801.02 30.51 -3 3 0 763.37 28.76 -5 3 0 22.20 2.13 5 3 0 27.58 4.38 -5 -3 0 20.75 2.82 -7 -3 0 54.36 3.88 7 3 0 56.97 5.79 -9 -3 0 232.08 13.19 9 3 0 238.74 13.26 -9 -3 0 222.92 11.26 -9 -3 0 227.65 10.31 -9 3 0 261.44 9.79 -11 -3 0 3.10 3.10 -11 -3 0 4.60 4.25 11 3 0 3.19 4.06 -11 3 0 2.52 1.63 -13 3 0 124.87 6.60 -13 -3 0 129.89 9.92 -15 -3 0 255.93 11.57 -15 -3 0 267.95 15.43 -15 3 0 281.13 11.24 15 -3 0 252.68 9.83 -15 3 0 250.61 10.85 15 -3 0 229.04 11.29 15 3 0 236.27 10.16 17 -3 0 13.28 2.04 17 -3 0 11.33 5.79 -17 -3 0 14.50 5.32 -17 3 0 12.72 3.13 17 3 0 12.17 2.63 19 -3 0 52.13 6.34 19 -3 0 58.31 3.47 -19 3 0 49.59 4.60 19 3 0 49.44 3.97 19 3 0 47.90 3.95 21 3 0 1.43 2.95 21 -3 0 1.26 2.26 -21 3 0 2.28 3.49 21 3 0 -0.54 3.21 -23 3 0 31.71 4.47 23 -3 0 29.91 3.26 23 3 0 29.10 4.04 -25 3 0 104.28 6.84 25 3 0 100.09 6.66 25 -3 0 107.47 5.84 27 -3 0 24.11 3.56 -27 3 0 18.60 4.12 27 3 0 21.01 4.62 -29 3 0 0.50 3.23 29 -3 0 -0.43 6.94 29 -3 0 1.95 3.02 29 3 0 0.80 4.17 -31 3 0 10.85 3.84 31 3 0 7.16 4.28 31 -3 0 6.27 6.12 -33 3 0 8.44 3.52 33 -3 0 6.29 6.10 33 3 0 1.91 4.15 -35 3 0 26.09 3.86 35 3 0 21.38 4.43 -35 3 0 27.11 3.84 35 -3 0 17.58 5.60 37 -3 0 12.02 4.62 37 3 0 19.08 3.52 -37 3 0 17.14 3.28 37 -3 0 20.44 2.80 -37 3 0 18.90 3.23 39 -3 0 -0.82 3.39 -39 3 0 -0.39 2.24 -39 3 0 0.28 2.13 39 -3 0 1.87 1.95 39 3 0 2.95 2.54 41 -3 0 0.87 2.24 -41 3 0 0.07 1.45 41 -3 0 -0.41 1.24 -41 3 0 0.28 1.54 0 4 0 1611.16 59.22 -2 4 0 1761.44 63.93 2 4 0 1750.44 64.85 -4 4 0 348.23 13.04 4 4 0 334.51 14.89 -4 -4 0 302.76 14.06 -6 -4 0 95.55 5.97 -6 4 0 104.60 5.06 -6 4 0 98.31 4.12 6 4 0 115.41 5.25 6 4 0 118.17 7.27 -8 4 0 478.07 18.23 -8 -4 0 447.13 19.79 -8 4 0 497.02 18.34 8 4 0 515.53 21.44 -8 -4 0 435.52 19.75 8 4 0 491.94 18.21 -8 4 0 458.82 18.25 -10 -4 0 1474.63 58.49 10 4 0 1609.96 56.36 10 4 0 1565.32 56.08 10 4 0 1726.16 60.66 -10 4 0 1532.18 56.21 -10 4 0 1563.06 56.19 -10 4 0 1464.84 56.29 -10 -4 0 1509.27 57.58 -12 4 0 1351.27 48.76 12 4 0 1418.36 48.74 -12 4 0 1285.69 48.96 -12 4 0 1409.22 48.81 12 4 0 1251.14 48.31 12 4 0 1341.55 48.83 -12 4 0 1318.40 48.66 -14 4 0 374.90 14.43 14 4 0 336.68 14.02 -14 4 0 378.16 14.43 16 4 0 51.41 3.82 -16 4 0 57.99 4.82 -16 4 0 64.93 4.12 -16 4 0 71.14 4.32 -18 4 0 87.72 5.12 18 4 0 62.85 4.56 -18 4 0 82.51 5.06 18 -4 0 84.05 7.88 -18 4 0 75.76 5.43 -20 4 0 382.09 16.34 20 -4 0 403.14 18.53 -20 4 0 424.17 15.99 20 4 0 361.99 15.65 22 -4 0 624.50 26.41 -22 4 0 598.35 24.13 -22 4 0 647.98 23.85 22 4 0 574.45 23.57 24 -4 0 399.99 19.25 24 4 0 389.42 16.47 -24 4 0 378.72 16.71 -24 4 0 425.32 16.58 26 4 0 52.84 4.93 -26 4 0 64.11 5.25 26 -4 0 69.06 9.09 -26 4 0 61.16 5.10 -26 4 0 67.08 5.43 -28 4 0 4.69 3.73 28 4 0 2.50 3.43 28 -4 0 5.71 7.86 -28 4 0 5.77 3.65 30 -4 0 37.33 3.73 -30 4 0 36.70 4.51 -30 4 0 35.74 4.62 30 4 0 37.02 4.30 32 4 0 168.82 8.07 -32 4 0 142.06 8.07 32 -4 0 161.01 7.60 -32 4 0 156.02 8.20 -34 4 0 109.92 6.71 34 4 0 135.70 6.66 -34 4 0 127.78 6.90 34 -4 0 122.46 6.19 -36 4 0 39.30 3.78 36 4 0 42.95 3.41 36 -4 0 39.48 3.13 -36 4 0 34.64 3.58 38 -4 0 1.24 1.45 -38 4 0 1.24 2.02 38 4 0 4.04 1.78 -38 4 0 0.95 2.15 38 -4 0 3.28 3.43 40 -4 0 0.63 2.21 -1 5 0 282.78 11.26 1 5 0 321.75 12.78 1 5 0 248.51 11.55 -1 5 0 326.59 12.28 1 5 0 275.29 11.26 3 5 0 438.14 16.99 -3 -5 0 416.18 16.69 3 5 0 382.37 15.00 -3 5 0 378.61 15.23 3 5 0 362.49 15.19 -5 5 0 6.66 2.58 5 5 0 6.32 2.45 5 5 0 7.03 2.63 5 5 0 4.43 2.47 -5 -5 0 5.99 2.24 -7 5 0 145.60 6.84 -7 5 0 140.52 6.99 7 5 0 141.48 6.88 7 5 0 146.45 6.92 -9 5 0 260.75 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19 -1 1 312.53 13.46 19 -1 1 313.49 17.14 19 1 1 363.81 13.22 19 1 1 305.63 13.65 19 -1 1 337.92 13.06 19 1 1 323.49 15.58 19 -1 1 365.33 14.19 17 -1 1 11.50 4.12 17 1 1 12.44 2.97 17 1 1 11.13 2.69 17 -1 1 12.17 1.89 17 1 1 9.57 1.09 17 -1 1 9.38 2.21 15 -1 1 184.03 7.60 15 1 1 186.25 10.68 15 1 1 204.11 9.68 15 1 1 167.50 7.66 15 1 1 180.21 7.10 13 1 1 499.80 22.68 13 1 1 554.07 21.42 13 1 1 528.31 19.16 -13 -1 -1 519.07 19.21 11 1 1 1739.83 66.49 11 1 1 1742.00 62.83 11 1 1 1912.08 64.85 9 -1 1 2605.98 92.45 9 1 1 2549.09 95.47 9 1 1 2567.11 93.25 9 -1 1 2572.66 92.99 7 -1 1 185.99 7.66 7 1 1 174.01 7.92 7 -1 1 199.61 7.90 7 1 1 198.96 11.33 5 -1 1 186.68 8.09 5 -1 1 225.90 8.36 3 -1 1 88.63 4.23 -1 1 -1 2186.17 78.19 1 -1 1 2173.54 78.13 1 -1 -1 1589.78 57.58 -1 1 1 1636.70 57.64 3 -1 -1 2006.59 72.38 -3 -1 1 2020.74 72.29 -5 -1 1 356.69 14.06 5 1 -1 392.85 13.95 5 -1 -1 361.64 14.28 -5 -1 1 363.79 13.91 7 1 -1 206.08 8.33 7 1 -1 191.72 8.44 -7 -1 1 200.77 7.88 -7 -1 1 185.42 8.83 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-0.20 0.00 -5 9 6 -1.01 0.00 5 9 6 -0.91 0.00 7 9 6 -0.85 0.00 9 9 6 -0.50 0.00 11 9 6 -0.08 0.00 13 9 6 0.21 0.00 -12 10 6 0.16 0.00 -10 10 6 0.23 0.00 -8 10 6 0.02 0.00 -6 10 6 -0.38 0.00 -4 10 6 -0.63 0.00 -2 10 6 -0.45 0.00 0 10 6 0.09 0.00 2 10 6 0.54 0.00 -41 1 7 0.00 0.00 27 1 7 -0.93 0.00 29 1 7 -0.57 0.00 -40 2 7 0.13 0.00 -38 2 7 -0.09 0.00 28 2 7 -0.45 0.00 -39 3 7 0.17 0.00 25 3 7 0.26 0.00 27 3 7 0.24 0.00 -38 4 7 0.29 0.00 -36 4 7 0.91 0.00 24 4 7 0.02 0.00 26 4 7 0.09 0.00 -35 5 7 0.55 0.00 -33 5 7 0.43 0.00 23 5 7 -0.13 0.00 -32 6 7 -0.61 0.00 -30 6 7 -1.06 0.00 20 6 7 0.16 0.00 -29 7 7 -0.51 0.00 -27 7 7 -0.13 0.00 -25 7 7 0.20 0.00 15 7 7 0.13 0.00 17 7 7 0.22 0.00 -24 8 7 -0.19 0.00 -22 8 7 -0.17 0.00 -20 8 7 0.11 0.00 6 8 7 -0.94 0.00 8 8 7 -0.54 0.00 10 8 7 -0.25 0.00 12 8 7 -0.13 0.00 -15 9 7 0.59 0.00 -13 9 7 0.26 0.00 -11 9 7 -0.08 0.00 -9 9 7 -0.19 0.00 -7 9 7 -0.11 0.00 -5 9 7 -0.05 0.00 -3 9 7 -0.24 0.00 -1 9 7 -0.68 0.00 1 9 7 -1.11 0.00 3 9 7 -1.27 0.00 -38 0 8 0.48 0.00 -36 0 8 1.29 0.00 16 0 8 -0.44 0.00 22 0 8 -0.34 0.00 24 0 8 0.19 0.00 -39 1 8 0.02 0.00 -37 1 8 0.39 0.00 23 1 8 -0.25 0.00 25 1 8 -0.06 0.00 -38 2 8 -0.20 0.00 -36 2 8 -0.66 0.00 22 2 8 -0.04 0.00 24 2 8 -0.38 0.00 -37 3 8 -0.58 0.00 -35 3 8 -1.11 0.00 21 3 8 0.18 0.00 23 3 8 0.05 0.00 -34 4 8 -0.27 0.00 18 4 8 -0.76 0.00 20 4 8 -0.37 0.00 -33 5 8 0.61 0.00 -31 5 8 0.51 0.00 -29 5 8 -0.20 0.00 17 5 8 -0.72 0.00 19 5 8 -0.54 0.00 -28 6 8 -0.84 0.00 -26 6 8 -0.72 0.00 10 6 8 0.13 0.00 12 6 8 -0.24 0.00 14 6 8 -0.30 0.00 16 6 8 -0.26 0.00 -25 7 8 0.30 0.00 -23 7 8 0.45 0.00 -21 7 8 0.09 0.00 -19 7 8 -0.36 0.00 -17 7 8 -0.41 0.00 7 7 8 0.47 0.00 9 7 8 0.14 0.00 11 7 8 0.04 0.00 -16 8 8 0.06 0.00 -14 8 8 0.32 0.00 -12 8 8 0.36 0.00 -10 8 8 0.17 0.00 -8 8 8 -0.03 0.00 -6 8 8 0.02 0.00 -4 8 8 0.35 0.00 -2 8 8 0.77 0.00 0 8 8 1.03 0.00 2 8 8 1.03 0.00 4 8 8 0.81 0.00 -35 1 9 0.53 0.00 -33 1 9 -0.18 0.00 -31 1 9 -1.11 0.00 17 1 9 -1.23 0.00 19 1 9 -0.94 0.00 -34 2 9 0.22 0.00 -32 2 9 -0.49 0.00 -30 2 9 -1.13 0.00 16 2 9 -0.36 0.00 18 2 9 -0.62 0.00 -33 3 9 -0.32 0.00 -31 3 9 -0.30 0.00 -29 3 9 -0.07 0.00 13 3 9 0.67 0.00 15 3 9 0.73 0.00 17 3 9 0.40 0.00 -30 4 9 0.24 0.00 -28 4 9 0.59 0.00 12 4 9 0.77 0.00 14 4 9 0.40 0.00 -27 5 9 0.14 0.00 -25 5 9 -0.15 0.00 -23 5 9 -0.14 0.00 -19 5 9 0.51 0.00 7 5 9 0.72 0.00 9 5 9 0.97 0.00 11 5 9 0.61 0.00 -22 6 9 0.57 0.00 -20 6 9 0.84 0.00 -18 6 9 0.76 0.00 -16 6 9 0.49 0.00 -2 6 9 -1.23 0.00 0 6 9 -1.22 0.00 2 6 9 -0.63 0.00 4 6 9 0.09 0.00 6 6 9 0.51 0.00 -15 7 9 0.38 0.00 -13 7 9 0.40 0.00 -11 7 9 0.43 0.00 -9 7 9 0.34 0.00 -7 7 9 0.05 0.00 -5 7 9 -0.34 0.00 -3 7 9 -0.61 0.00 -1 7 9 -0.63 0.00 -30 0 10 0.82 0.00 -28 0 10 0.30 0.00 -26 0 10 -0.23 0.00 -20 0 10 -0.11 0.00 2 0 10 -1.56 0.00 4 0 10 -2.25 0.00 6 0 10 -2.18 0.00 8 0 10 -1.40 0.00 10 0 10 -0.38 0.00 12 0 10 0.41 0.00 -29 1 10 0.00 0.00 -27 1 10 -0.21 0.00 -25 1 10 -0.31 0.00 5 1 10 -1.67 0.00 7 1 10 -1.05 0.00 9 1 10 -0.52 0.00 11 1 10 -0.26 0.00 -28 2 10 -0.55 0.00 -26 2 10 -0.24 0.00 -24 2 10 -0.01 0.00 -22 2 10 0.17 0.00 6 2 10 -0.27 0.00 8 2 10 -0.17 0.00 10 2 10 -0.42 0.00 -25 3 10 0.31 0.00 -23 3 10 0.44 0.00 -21 3 10 0.36 0.00 3 3 10 0.32 0.00 5 3 10 -0.04 0.00 7 3 10 -0.47 0.00 9 3 10 -0.57 0.00 -22 4 10 0.60 0.00 -20 4 10 0.31 0.00 -18 4 10 -0.15 0.00 -16 4 10 -0.60 0.00 -14 4 10 -0.94 0.00 -2 4 10 -0.23 0.00 0 4 10 0.48 0.00 2 4 10 0.59 0.00 4 4 10 0.10 0.00 6 4 10 -0.49 0.00 -17 5 10 -0.46 0.00 -15 5 10 -1.11 0.00 -13 5 10 -1.45 0.00 -11 5 10 -1.39 0.00 -9 5 10 -1.04 0.00 -7 5 10 -0.65 0.00 -5 5 10 -0.37 0.00 -3 5 10 -0.25 0.00 -1 5 10 -0.21 0.00 1 5 10 -0.18 0.00 -19 1 11 -0.34 0.00 -17 1 11 -0.42 0.00 -15 1 11 -0.11 0.00 -13 1 11 0.36 0.00 -11 1 11 0.59 0.00 -9 1 11 0.48 0.00 -7 1 11 0.30 0.00 -5 1 11 0.36 0.00 -3 1 11 0.56 0.00 -1 1 11 0.54 0.00 -16 2 11 -0.26 0.00 -14 2 11 -0.02 0.00 -12 2 11 0.38 0.00 -10 2 11 0.76 0.00 -8 2 11 0.93 0.00 -6 2 11 0.83 0.00 -4 2 11 0.48 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 91117) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.009 196 17 ' ' 2 0.500 0.500 0.001 196 17 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta -1 3 1 15.473 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL 1111_a.res in C2/c CELL 35.9280 9.1976 8.6505 90.00 102.03 90.00 SPGR C2/c # Solvent Accessible Volume = 390 # Electrons Found in S.A.V. = 34 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others Q101 0.337 0.370 0.142 ! 0.85 eA-3 Q102 0.265 0.177 0.933 ! 0.78 eA-3 Q103 0.265 0.318 0.909 ! 0.77 eA-3 Q104 0.264 0.125 0.100 ! 0.76 eA-3 Q105 0.242 0.248 0.845 ! 0.73 eA-3 Q106 0.142 0.271 0.461 ! 0.66 eA-3 Q107 0.252 0.210 0.274 ! 0.66 eA-3 Q108 0.752 0.273 0.788 ! 0.66 eA-3 Q109 0.175 0.243 0.824 ! 0.64 eA-3 Q110 0.345 0.367 0.033 ! 0.63 eA-3 Q111 0.755 0.221 0.776 ! 0.63 eA-3 Q112 0.549 0.315 0.304 ! 0.61 eA-3 Q113 0.234 0.492 0.251 ! 0.59 eA-3 Q114 0.672 0.405 0.465 ! 0.58 eA-3 Q115 0.561 0.316 0.277 ! 0.58 eA-3 Q116 0.757 0.281 0.854 ! 0.57 eA-3 Q117 0.642 0.214 0.497 ! 0.57 eA-3 Q118 0.743 0.093 0.467 ! 0.57 eA-3 Q119 0.251 0.035 0.464 ! 0.56 eA-3 Q120 0.649 0.187 0.308 ! 0.56 eA-3 Q121 0.845 0.254 0.188 ! 0.55 eA-3 Q122 0.649 0.344 0.510 ! 0.55 eA-3 Q123 0.773 0.309 0.866 ! 0.55 eA-3 Q124 0.627 0.311 0.427 ! 0.54 eA-3 Q125 0.242 0.386 0.741 ! 0.54 eA-3 Q126 0.834 0.323 0.656 ! 0.53 eA-3 Q127 0.714 0.024 0.215 ! 0.52 eA-3 Q128 0.960 0.510 0.432 ! 0.52 eA-3 Q129 0.337 0.241 0.941 ! 0.52 eA-3 Q130 0.708 0.433 0.514 ! 0.51 eA-3 C131 0.556 0.361 0.246 ! 0.51 eA-3 Q132 0.741 0.474 0.390 ! 0.50 eA-3 ) ; _shelx_fab_checksum 21043 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6410(2) 0.7010(10) 0.3885(10) 0.061(2) Uani 1 1 d . . . . . H1 H 0.641947 0.649464 0.290205 0.074 Uiso 1 1 calc R . . . . C2 C 0.6443(3) 0.8585(11) 0.3597(12) 0.075(3) Uani 1 1 d . . . . . H2A H 0.667295 0.876798 0.320759 0.090 Uiso 1 1 calc R . . . . H2B H 0.646210 0.910939 0.458314 0.090 Uiso 1 1 calc R . . . . C3 C 0.6049(3) 0.6583(12) 0.4377(13) 0.078(3) Uani 1 1 d . . . . . H3A H 0.604319 0.700391 0.540081 0.094 Uiso 1 1 calc R . . . . H3B H 0.603679 0.553414 0.446826 0.094 Uiso 1 1 calc R . . . . C4 C 0.6103(2) 0.9134(11) 0.2407(12) 0.070(2) Uani 1 1 d . . . . . H4A H 0.610954 0.873760 0.137407 0.084 Uiso 1 1 calc R . . . . H4B H 0.611629 1.018452 0.234005 0.084 Uiso 1 1 calc R . . . . C5 C 0.5708(3) 0.7126(13) 0.3150(15) 0.089(3) Uani 1 1 d . . . . . H5A H 0.569757 0.660523 0.216619 0.107 Uiso 1 1 calc R . . . . H5B H 0.547603 0.691659 0.351307 0.107 Uiso 1 1 calc R . . . . C6 C 0.5729(3) 0.8706(12) 0.2856(12) 0.073(2) Uani 1 1 d . . . . . H6 H 0.572181 0.919876 0.385371 0.088 Uiso 1 1 calc R . . . . C7 C 0.5400(3) 0.9283(14) 0.1638(13) 0.080(3) Uani 1 1 d . . . . . N1 N 0.67496(19) 0.6529(8) 0.5137(8) 0.0623(17) Uani 1 1 d . . . . . H1A H 0.696365 0.677750 0.484027 0.075 Uiso 1 1 calc GR . . . . H1B H 0.674292 0.556814 0.525372 0.075 Uiso 1 1 calc GR . . . . H1C H 0.674124 0.695818 0.605120 0.075 Uiso 1 1 calc GR . . . . O1 O 0.5372(2) 1.0656(10) 0.1569(12) 0.113(3) Uani 1 1 d . . . . . H1D H 0.517013 1.088117 0.098039 0.169 Uiso 1 1 calc GR . . . . O2 O 0.5193(2) 0.8465(11) 0.0743(11) 0.115(3) Uani 1 1 d . . . . . I1 I 0.75273(2) 0.44376(5) 0.81318(5) 0.05517(17) Uani 1 1 d . . . . . I2 I 0.66021(2) 0.27931(6) 0.41418(7) 0.06444(18) Uani 1 1 d . . . . . Pb1 Pb 0.750000 0.250000 0.500000 0.04759(14) Uani 1 2 d S T P . . 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 C1 0.065(5) 0.061(5) 0.055(4) -0.005(4) 0.006(4) 0.003(4) C2 0.062(5) 0.081(6) 0.076(6) 0.011(5) 0.000(4) 0.001(5) C3 0.059(5) 0.083(7) 0.089(6) 0.035(5) 0.008(4) 0.003(5) C4 0.060(5) 0.064(5) 0.080(6) 0.018(5) 0.002(4) 0.006(4) C5 0.052(5) 0.105(8) 0.107(8) 0.040(7) 0.007(5) 0.003(5) C6 0.064(5) 0.085(7) 0.069(5) 0.009(5) 0.009(4) 0.013(5) C7 0.065(6) 0.102(8) 0.069(6) 0.014(6) 0.005(5) 0.007(6) N1 0.060(4) 0.060(4) 0.060(4) 0.000(3) -0.002(3) 0.007(3) O1 0.096(6) 0.095(6) 0.125(7) 0.016(5) -0.027(5) 0.025(5) O2 0.100(6) 0.109(6) 0.114(6) 0.017(5) -0.029(5) 0.012(5) I1 0.0692(3) 0.0467(3) 0.0480(3) -0.01243(19) 0.0084(2) 0.0064(2) I2 0.0626(3) 0.0620(3) 0.0681(3) -0.0011(2) 0.0122(3) -0.0070(2) Pb1 0.0572(2) 0.0405(2) 0.0439(2) 0.00005(14) 0.00797(17) 0.00132(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -4.0753 8.5060 '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 C2 C1 C3 114.1(8) . . ? C2 C1 N1 108.9(7) . . ? C3 C1 N1 109.6(7) . . ? C1 C2 C4 111.1(8) . . ? C1 C3 C5 109.4(8) . . ? C2 C4 C6 111.7(8) . . ? C6 C5 C3 112.2(9) . . ? C5 C6 C4 112.1(8) . . ? C5 C6 C7 113.9(9) . . ? C7 C6 C4 109.6(8) . . ? O1 C7 C6 115.3(10) . . ? O2 C7 C6 120.9(11) . . ? O2 C7 O1 123.6(10) . . ? Pb1 I1 Pb1 153.479(17) . 4_656 ? I1 Pb1 I1 86.573(5) . 6_565 ? I1 Pb1 I1 93.427(5) 7_656 6_565 ? I1 Pb1 I1 93.427(5) . 4_646 ? I1 Pb1 I1 180.0 7_656 . ? I1 Pb1 I1 86.573(5) 7_656 4_646 ? I1 Pb1 I1 180.0 4_646 6_565 ? I2 Pb1 I1 86.826(14) 7_656 4_646 ? I2 Pb1 I1 93.174(14) 7_656 6_565 ? I2 Pb1 I1 93.174(14) . 4_646 ? I2 Pb1 I1 90.061(14) . . ? I2 Pb1 I1 90.062(14) 7_656 7_656 ? I2 Pb1 I1 89.938(14) . 7_656 ? I2 Pb1 I1 86.826(14) . 6_565 ? I2 Pb1 I1 89.939(14) 7_656 . ? I2 Pb1 I2 180.00(2) . 7_656 ? 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 C1 C2 1.479(13) . ? C1 C3 1.500(13) . ? C1 N1 1.520(10) . ? C2 C4 1.511(12) . ? C3 C5 1.527(13) . ? C4 C6 1.525(13) . ? C5 C6 1.480(15) . ? C6 C7 1.507(13) . ? C7 O1 1.267(14) . ? C7 O2 1.215(14) . ? I1 Pb1 3.2590(4) 4_656 ? I1 Pb1 3.2271(4) . ? I2 Pb1 3.1673(6) . ?