#------------------------------------------------------------------------------ #$Date: 2019-11-22 23:20:33 +0200 (Fri, 22 Nov 2019) $ #$Revision: 231550 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/33/4003376.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_4003376 loop_ _publ_author_name 'Fateev, Sergey A.' 'Petrov, Andrey A.' 'Khrustalev, Victor N.' 'Dorovatovskii, Pavel V.' 'Zubavichus, Yan V.' 'Goodilin, Eugene A.' 'Tarasov, Alexey B.' _publ_section_title ; Solution Processing of Methylammonium Lead Iodide Perovskite from \g-Butyrolactone: Crystallization Mediated by Solvation Equilibrium ; _journal_issue 15 _journal_name_full 'Chemistry of Materials' _journal_page_first 5237 _journal_paper_doi 10.1021/acs.chemmater.8b01906 _journal_volume 30 _journal_year 2018 _chemical_formula_moiety 'I8 Pb3, C4 H6 O2, 2(C H6 N)' _chemical_formula_sum 'C6 H18 I8 N2 O2 Pb3' _chemical_formula_weight 1787.02 _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_Hall '-C 2y' _space_group_name_H-M_alt 'C 1 2/m 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 101.80(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 21.822(4) _cell_length_b 4.5979(9) _cell_length_c 16.653(3) _cell_measurement_reflns_used 600 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 32.0 _cell_measurement_theta_min 2.0 _cell_volume 1635.6(6) _computing_cell_refinement 'iMosflm (Battye et al., 2011)' _computing_data_collection 'Marccd (Doyle, 2011)' _computing_data_reduction iMosflm _computing_molecular_graphics 'SHELXTL (Sheldrick, 2015)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_device_type 'Rayonix SX165 CCD' _diffrn_measurement_method '/f scan' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.96990 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_unetI/netI 0.1958 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 7812 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_theta_full 35.587 _diffrn_reflns_theta_max 38.348 _diffrn_reflns_theta_min 1.705 _exptl_absorpt_coefficient_mu 25.955 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_correction_T_min 0.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Scala (Evans, 2006)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 3.629 _exptl_crystal_description needle _exptl_crystal_F_000 1508 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _refine_diff_density_max 4.890 _refine_diff_density_min -3.734 _refine_diff_density_rms 0.559 _refine_ls_extinction_coef 0.00026(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 68 _refine_ls_number_reflns 1923 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 0.885 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0862 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+100P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1989 _refine_ls_wR_factor_ref 0.2224 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1273 _reflns_number_total 1923 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cm8b01906_si_002.cif _cod_data_source_block igla1 _cod_original_sg_symbol_H-M 'C 2/m' _cod_database_code 4003376 _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_min 0.072 _shelx_estimated_absorpt_t_max 0.779 _shelxl_version_number 2014/6 _shelx_res_file ; TITL igla1 in C2/m CELL 0.96990 21.8216 4.5979 16.6531 90.000 101.799 90.000 ZERR 2.00 0.0044 0.0009 0.0033 0.000 0.030 0.000 LATT 7 SYMM -X, +Y, -Z SFAC C H N O I Pb DISP C 0.007 0.003 25.571 DISP H -0 0 0.636 DISP N 0.013 0.007 47.42 DISP O 0.021 0.012 81.964 DISP I -0.034 3.136 18629.286 DISP Pb -9.900 4.074 21889.318 UNIT 12 36 4 4 16 6 TEMP -173.0 SIZE 0.01 0.02 0.21 OMIT 7 3 12 OMIT -10 0 20 OMIT -25 1 2 OMIT -2 0 1 OMIT 13 5 2 OMIT -24 0 9 OMIT 9 5 7 OMIT -6 0 4 OMIT 14 4 8 OMIT -8 4 15 OMIT 14 4 7 OMIT -7 1 18 OMIT -24 0 13 OMIT -6 0 3 OMIT -18 0 18 OMIT -12 0 20 OMIT -6 4 15 OMIT 9 3 14 OMIT -5 1 1 OMIT -9 5 9 OMIT -2 0 3 OMIT 13 5 1 OMIT 11 5 3 OMIT -16 0 18 OMIT -16 4 10 OMIT 6 0 1 OMIT -6 2 4 OMIT -20 4 2 OMIT 11 5 2 OMIT -16 0 19 OMIT -13 5 2 OMIT -24 0 12 OMIT 18 4 3 OMIT -26 0 4 OMIT -14 4 13 OMIT 22 0 9 OMIT -2 0 6 OMIT 11 3 11 OMIT 5 1 7 OMIT 10 4 10 OMIT 2 2 3 OMIT -15 1 7 OMIT -7 5 8 OMIT -8 2 4 OMIT -15 3 2 OMIT -11 1 4 OMIT 3 1 0 OMIT -11 1 2 OMIT -6 0 8 OMIT -21 1 7 OMIT -3 1 2 OMIT -11 1 8 OMIT -11 1 5 OMIT 6 4 10 OMIT -1 5 11 OMIT 4 0 4 OMIT -8 0 5 OMIT -13 5 3 L.S. 124 BOND $H ACTA CONF FLAT 0.001 O1 O2 C2 C3 C5 DFIX 1.210 0.001 C2 O2 DFIX 1.360 0.001 O1 C2 DFIX 1.440 0.001 O1 C5 DFIX 1.500 0.001 C2 C3 DFIX 1.520 0.001 C3 C4 C4 C5 DFIX 2.220 0.001 O1 O2 DFIX 2.460 0.001 O2 C3 DFIX 2.360 0.001 O1 C4 DFIX 2.370 0.001 C2 C4 DFIX 2.300 0.001 C2 C5 DFIX 2.345 0.001 O1 C3 DFIX 2.375 0.001 C3 C5 DFIX 1.475 0.001 N1 C1 EADP N1 C1 EADP O1 O2 C2 C3 C4 C5 WGHT 0.000000 100.000000 EXTI 0.000259 FVAR 0.10563 PB1 6 0.586558 0.500000 0.749392 10.50000 0.03803 0.03085 = 0.02880 0.00000 0.00162 0.00000 PB2 6 0.500000 1.000000 0.500000 10.25000 0.02669 0.02775 = 0.02595 0.00000 -0.00005 0.00000 I1 5 0.688378 0.000000 0.798549 10.50000 0.03211 0.03557 = 0.05440 0.00000 -0.00778 0.00000 I2 5 0.544681 0.500000 0.912369 10.50000 0.08357 0.05443 = 0.03340 0.00000 0.01460 0.00000 I3 5 0.478030 1.000000 0.686191 10.50000 0.02602 0.03701 = 0.02588 0.00000 0.00199 0.00000 I4 5 0.394069 0.500000 0.453975 10.50000 0.02513 0.03174 = 0.03288 0.00000 0.00070 0.00000 PART 1 N1 3 0.892338 0.500000 0.907541 10.50000 0.06641 0.04111 = 0.25164 0.00000 -0.07276 0.00000 AFIX 3 H1A 2 0.924748 0.500000 0.951671 10.50000 -1.50000 H1B 2 0.894738 0.339730 0.876271 11.00000 -1.50000 AFIX 0 C1 1 0.832302 0.500000 0.935220 10.50000 0.06641 0.04111 = 0.25164 0.00000 -0.07276 0.00000 AFIX 3 H1C 2 0.797142 0.500000 0.887980 10.50000 -1.50000 H1D 2 0.829912 0.672580 0.968980 11.00000 -1.50000 AFIX 0 PART 2 O1 4 0.824932 0.559095 0.735379 10.25000 0.03705 0.09182 = 0.07877 -0.02903 0.01977 -0.02597 O2 4 0.863624 0.958785 0.801821 10.25000 0.03705 0.09182 = 0.07877 -0.02903 0.01977 -0.02597 C2 1 0.841032 0.845068 0.737115 10.25000 0.03705 0.09182 = 0.07877 -0.02903 0.01977 -0.02597 C3 1 0.826299 0.968933 0.652039 10.25000 0.03705 0.09182 = 0.07877 -0.02903 0.01977 -0.02597 AFIX 3 H3A 2 0.864549 1.000253 0.629359 10.25000 -1.20000 H3B 2 0.805029 1.159443 0.651159 10.25000 -1.20000 AFIX 0 C4 1 0.781485 0.747288 0.604197 10.25000 0.03705 0.09182 = 0.07877 -0.02903 0.01977 -0.02597 AFIX 3 H4A 2 0.788045 0.729068 0.547317 10.25000 -1.20000 H4B 2 0.737055 0.795448 0.602727 10.25000 -1.20000 AFIX 0 C5 1 0.799048 0.468791 0.652578 10.25000 0.03705 0.09182 = 0.07877 -0.02903 0.01977 -0.02597 AFIX 3 H5A 2 0.762399 0.340341 0.650948 10.25000 -1.20000 H5B 2 0.831029 0.361631 0.629908 10.25000 -1.20000 PART 0 AFIX 0 HKLF 4 REM igla1 in C2/m REM R1 = 0.0862 for 1273 Fo > 4sig(Fo) and 0.1100 for all 1923 data REM 68 parameters refined using 16 restraints END WGHT 0.0560 0.0000 REM Highest difference peak 4.890, deepest hole -3.734, 1-sigma level 0.559 Q1 1 0.5810 0.5000 0.9279 10.50000 0.05 4.19 Q2 1 0.5069 1.0000 0.6418 10.50000 0.05 2.47 Q3 1 0.5514 0.5000 0.7871 10.50000 0.05 2.39 Q4 1 0.7271 0.0000 0.7682 10.50000 0.05 2.33 Q5 1 0.6203 0.6298 0.7235 11.00000 0.05 2.15 Q6 1 0.5395 0.9214 0.4686 11.00000 0.05 2.13 Q7 1 0.5476 1.0000 0.4725 10.50000 0.05 2.12 Q8 1 0.4728 0.5000 0.6955 10.50000 0.05 2.10 Q9 1 0.7112 1.0000 0.6096 10.50000 0.05 2.03 Q10 1 0.8352 0.5000 0.8313 10.50000 0.05 1.86 Q11 1 0.8377 0.5000 1.0189 10.50000 0.05 1.86 Q12 1 0.6188 0.5000 0.7009 10.50000 0.05 1.78 Q13 1 0.4420 1.0000 0.7298 10.50000 0.05 1.73 Q14 1 0.5000 0.5000 0.5000 10.25000 0.05 1.72 Q15 1 0.5206 0.5000 0.8285 10.50000 0.05 1.65 Q16 1 0.7602 1.0000 0.5962 10.50000 0.05 1.65 Q17 1 0.5600 0.7321 0.7105 11.00000 0.05 1.63 Q18 1 0.4376 0.4067 0.4310 11.00000 0.05 1.63 Q19 1 0.4176 0.5000 0.3968 10.50000 0.05 1.61 Q20 1 0.3601 0.5000 0.4878 10.50000 0.05 1.61 ; _shelx_res_checksum 42093 _shelx_hkl_file ; 27 1 -1 0.37 7.76 27 1 -2 7.38 9.13 27 1 -3 116.02 39.05 27 1 -4 101.71 34.74 27 1 -5 47.70 19.30 27 1 -6 21.57 12.07 -27 -1 6 0.23 13.61 27 1 -7 272.34 76.14 -27 -1 7 8.28 85.41 26 0 -1 2.95 20.36 26 0 -1 5.67 5.30 26 0 -2 9.11 25.60 26 0 -2 1.37 4.77 26 0 -3 3.95 22.51 26 0 -3 -1.81 4.67 -26 0 4 2.09 22.04 26 0 -4 20.54 22.11 26 0 -4 0.44 5.53 26 0 -5 10.74 24.27 26 0 -5 -0.22 5.19 -26 0 6 2.83 22.13 26 0 -6 8.42 19.06 26 0 -6 0.47 5.28 -26 0 7 11.30 22.70 26 0 -7 2.41 16.16 26 0 -7 1.62 7.58 -26 0 8 0.23 23.63 26 0 -8 1.32 7.62 -26 0 9 -6.83 26.68 26 0 -9 10.05 17.80 26 0 -9 -0.58 7.71 -26 0 10 -3.34 24.78 26 0 -10 -6.21 19.22 -26 0 11 1.74 25.12 26 0 -11 -0.41 19.15 26 2 -2 12.69 9.34 26 2 -3 5.29 7.98 26 2 -4 33.34 14.47 26 2 -5 7.93 9.58 -26 -2 5 0.42 14.06 26 2 -6 8.55 8.40 -26 -2 6 1.85 29.17 25 -1 -1 -3.04 14.08 25 -1 -1 1.65 4.24 25 1 -1 2.66 4.43 -25 -1 1 -3.28 15.08 -25 1 2 11.41 53.88 25 -1 -2 4.31 56.24 25 -1 -2 -1.14 45.78 -25 -1 2 1.51 50.49 25 -1 -3 381.85 76.46 25 -1 -3 -1.15 59.66 25 1 -3 367.70 60.64 -25 -1 3 4.04 67.68 25 -1 -4 11.86 22.55 25 -1 -4 1.46 5.40 25 1 -4 8.23 6.69 -25 -1 4 2.95 13.62 25 -1 -5 12.88 27.30 25 -1 -5 1.36 6.30 25 1 -5 12.33 6.46 -25 -1 5 2.49 13.76 25 -1 -6 266.18 50.26 25 -1 -6 -0.35 38.57 25 1 -6 195.83 39.22 -25 1 7 -1.38 22.55 25 -1 -7 110.98 26.69 25 -1 -7 -2.30 19.22 25 1 -7 108.27 20.48 -25 -1 7 38.47 26.14 -25 1 8 -0.54 23.68 25 -1 -8 41.20 27.60 25 -1 -8 0.02 9.19 25 1 -8 24.84 8.02 -25 -1 8 -7.42 24.45 -25 1 9 0.48 38.36 25 -1 -9 18.74 22.63 25 -1 -9 1.68 8.67 25 1 -9 6.12 5.88 -25 -1 9 -8.56 26.55 25 -1 -10 0.00 19.34 25 1 -10 11.61 9.80 -25 -1 10 -3.84 26.39 25 -1 -11 8.72 21.91 25 1 -11 0.30 19.84 -25 -1 11 0.00 28.24 25 -1 -12 0.86 23.16 25 1 -12 0.16 21.74 -25 -1 12 0.72 30.58 -24 0 1 7.97 27.58 24 0 -1 2.03 17.28 24 0 -1 9.02 5.44 -24 0 2 -8.19 26.30 24 0 -2 12.91 17.10 24 0 -2 11.14 6.76 -24 0 3 -8.78 22.47 24 0 -3 5.90 17.94 24 0 -3 1.85 5.26 -24 0 4 1.48 22.40 24 0 -4 2.08 4.43 -24 0 5 2.27 18.55 24 0 -5 31.46 17.28 24 0 -5 32.64 11.85 -24 0 6 5.01 25.72 24 0 -6 160.84 37.08 24 0 -6 81.80 29.36 -24 0 7 7.13 8.07 24 0 -7 18.52 17.58 24 0 -7 17.65 9.86 -24 0 8 2.05 149.73 24 0 -8 472.52 154.96 24 0 -8 432.17 122.22 -24 0 9 -9.76 13.86 24 0 -9 0.60 13.01 -24 0 10 -4.22 15.01 24 0 -10 5.32 12.37 24 0 -10 0.75 6.35 -24 0 11 11.65 25.34 24 0 -11 7.95 16.81 24 0 -11 -1.01 7.20 -24 0 12 1.42 34.15 24 0 -12 104.68 20.46 24 0 -12 2.30 11.18 -24 0 13 -8.21 30.46 24 0 -13 24.40 19.13 24 0 -13 -1.66 7.21 -24 0 14 2.05 35.03 24 0 -14 -5.47 21.36 24 2 -1 6.36 5.38 -24 -2 1 1.54 13.12 24 -2 -2 -1.03 15.67 24 -2 -2 1.10 6.46 24 2 -2 10.31 5.35 -24 -2 2 4.42 16.66 24 -2 -3 8.60 24.24 24 -2 -3 -0.05 6.74 24 2 -3 1.42 4.79 24 -2 -4 5.52 27.22 24 2 -4 2.49 5.22 -24 -2 4 -4.62 22.62 24 2 -5 28.77 10.52 -24 -2 5 -0.80 27.41 24 -2 -6 56.42 27.92 24 2 -6 58.57 18.74 -24 -2 6 6.21 31.09 24 -2 -7 10.26 25.25 24 2 -7 12.46 7.19 -24 -2 7 1.25 29.53 24 -2 -8 260.79 97.28 24 2 -8 296.58 79.16 -24 -2 8 -9.47 97.17 24 -2 -9 108.30 49.62 24 2 -9 151.12 41.76 -24 -2 9 5.41 43.10 24 2 -10 0.78 8.57 -24 -2 10 0.05 19.51 24 -2 -11 5.47 22.23 24 2 -11 -2.27 8.06 -24 -2 11 6.28 20.60 -23 1 1 -3.06 43.67 23 -1 -1 129.95 47.75 23 -1 -1 -0.18 38.43 23 1 -1 281.85 39.37 -23 -1 1 1.88 42.33 23 -1 -2 288.97 93.59 23 1 -2 277.42 75.76 -23 -1 2 12.33 91.18 23 -1 -3 86.48 24.91 23 -1 -3 0.02 13.74 23 1 -3 69.54 15.07 -23 -1 3 4.23 26.45 23 -1 -4 14.82 18.91 23 -1 -4 0.68 5.28 23 1 -4 6.10 6.32 -23 -1 4 3.27 26.24 23 -1 -5 14.66 18.48 23 -1 -5 1.65 5.65 23 1 -5 8.56 5.79 -23 -1 5 5.35 22.99 -23 1 6 -12.71 25.48 23 -1 -6 5.98 19.44 23 -1 -6 1.87 5.45 23 1 -6 0.91 5.78 -23 -1 6 -1.37 20.12 23 -1 -7 7.76 14.69 23 -1 -7 0.94 5.61 23 1 -7 -2.69 5.69 -23 -1 7 -6.45 21.16 23 -1 -8 17.12 13.32 23 -1 -8 -1.80 8.32 23 1 -8 18.99 6.84 -23 -1 8 10.71 20.47 -23 1 9 2.66 33.28 23 -1 -9 2.00 14.82 23 -1 -9 0.51 7.05 23 1 -9 0.01 6.06 -23 -1 9 1.84 23.52 -23 1 10 -24.33 42.68 23 -1 -10 6.46 13.91 23 -1 -10 3.68 7.51 23 1 -10 12.10 7.20 -23 -1 10 15.77 24.19 23 -1 -11 -0.02 21.81 23 -1 -11 -1.55 7.07 23 1 -11 4.56 6.49 -23 -1 11 2.21 26.18 23 -1 -12 36.20 24.78 23 1 -12 16.25 24.23 23 1 -12 71.62 20.45 -23 -1 12 35.07 28.15 23 -1 -13 4.32 20.00 23 1 -13 -1.20 18.74 23 1 -13 22.02 9.47 -23 -1 13 12.65 26.61 23 -1 -14 24.08 26.63 23 1 -14 10.04 25.28 23 1 -14 90.73 23.29 -23 -1 14 -7.18 31.04 23 3 -1 155.18 41.04 -23 -3 1 -0.74 43.19 23 3 -2 164.32 44.18 -23 -3 2 19.25 48.59 23 3 -3 31.03 12.37 -23 -3 3 3.54 15.23 23 3 -4 6.38 8.12 -23 -3 4 7.31 17.23 23 3 -5 7.00 9.64 -23 -3 5 5.03 21.65 23 3 -6 1.63 7.35 -23 -3 6 -0.86 23.36 23 3 -7 0.93 9.02 -23 -3 7 -2.35 24.14 23 3 -8 1.12 7.44 -23 -3 8 -1.25 24.87 -22 0 1 10.65 22.51 22 0 -1 15.05 7.74 -22 0 2 10.26 19.07 22 0 -2 2.45 5.54 -22 0 3 141.65 125.21 22 0 -3 355.69 100.43 -22 0 4 202.41 194.00 22 0 -4 544.93 151.85 -22 0 5 -3.67 21.54 22 0 -5 -0.55 5.45 -22 0 6 14.48 22.89 22 0 -6 57.51 20.00 22 0 -6 49.60 17.28 -22 0 7 496.59 255.79 22 0 -7 756.85 257.45 22 0 -7 620.84 197.61 -22 0 8 131.91 178.65 22 0 -8 518.57 182.21 22 0 -8 495.50 142.00 -22 0 9 -2.85 10.80 22 0 -9 55.26 19.97 22 0 -9 46.19 15.96 -22 0 10 3.96 9.90 22 0 -10 11.55 15.09 22 0 -10 12.86 7.22 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2.15 10.84 -21 1 0 1.71 20.16 21 -1 0 9.21 12.00 21 -1 0 7.67 5.25 21 1 1 3.85 4.31 -21 1 -1 2.80 13.64 21 -1 1 3.02 4.10 21 1 2 149.51 35.81 -21 -1 -2 0.78 38.91 -21 1 -2 3.00 34.80 21 -1 2 4.02 41.31 21 -1 2 141.67 35.78 21 1 3 580.68 151.91 -21 -1 -3 3.54 193.70 21 -1 3 512.15 151.85 21 1 4 173.72 55.59 21 -1 4 171.01 55.63 21 1 5 107.33 30.45 -21 -1 -5 3.77 32.51 21 -1 5 95.16 30.39 21 1 6 123.85 34.53 -21 -1 -6 -2.41 34.79 -21 1 -6 108.19 34.41 21 -1 6 101.44 34.46 21 1 7 632.93 173.61 -21 1 -7 533.43 173.36 21 -1 7 499.82 173.51 21 1 8 61.08 14.06 -21 1 -8 44.93 14.01 21 -1 8 -0.77 13.39 21 1 9 0.91 4.96 -21 -1 -9 2.89 5.10 -21 1 -9 2.02 4.74 21 -1 9 0.88 4.42 -21 -1 -10 21.28 10.22 21 3 0 5.66 6.15 -21 -3 0 0.65 11.88 21 3 1 2.42 4.34 -21 -3 -1 1.38 14.64 21 3 2 72.82 19.92 -21 -3 -2 -2.23 19.39 21 3 3 338.10 82.71 -21 -3 -3 1.88 100.21 21 3 4 60.13 21.60 22 0 0 52.83 16.04 -22 0 0 3.70 19.46 22 0 1 25.92 9.28 -22 0 -1 -4.56 17.44 22 0 2 16.14 7.02 -22 0 -2 1.01 8.99 22 0 3 70.60 20.89 -22 0 -3 -0.96 18.82 22 0 4 12.40 6.62 -22 0 -4 7.21 18.64 22 0 5 27.07 11.37 22 0 6 27.39 11.14 22 0 7 0.07 4.82 22 0 8 52.97 19.96 -22 0 -8 58.59 19.79 22 0 9 46.77 16.76 -22 0 -9 43.86 16.54 22 2 0 42.69 9.20 22 -2 0 18.27 21.01 22 -2 0 -2.02 9.13 22 2 1 15.26 6.15 -22 -2 -1 0.96 16.64 22 -2 1 15.41 24.05 22 -2 1 -1.27 6.15 22 2 2 11.01 4.92 -22 -2 -2 -2.63 17.42 -22 2 -2 6.76 7.02 22 -2 2 0.03 6.26 22 2 3 50.35 10.56 -22 2 -3 22.92 11.03 22 -2 3 -0.80 10.40 22 2 4 3.30 4.50 -22 2 -4 0.03 6.58 22 -2 4 1.98 5.89 22 2 5 22.64 8.40 -22 2 -5 10.57 7.64 22 -2 5 1.72 6.88 22 2 6 25.86 11.18 22 2 7 1.62 4.93 23 1 0 66.85 12.19 -23 -1 0 9.55 14.75 23 -1 0 2.50 23.13 23 -1 0 1.45 10.97 23 1 1 26.32 6.31 -23 -1 -1 0.57 20.48 23 -1 1 -6.26 25.81 23 -1 1 -0.37 6.26 23 1 2 669.27 95.05 -23 -1 -2 1.77 115.64 23 -1 2 1.21 94.10 23 1 3 231.72 37.97 23 -1 3 -0.97 37.09 23 1 4 2.26 5.29 -23 -1 -4 1.91 21.40 23 -1 4 1.69 5.14 23 1 5 2.08 4.22 -23 1 -5 -0.74 4.96 23 -1 5 -1.16 5.22 23 1 6 143.46 24.83 23 -1 6 -0.67 23.66 23 1 7 -0.43 4.54 23 3 0 24.89 11.52 -23 -3 0 -4.01 14.29 24 0 0 24.68 9.42 -24 0 0 5.22 21.40 24 0 1 10.14 27.61 24 0 1 41.14 12.49 -24 0 -1 -0.47 20.68 24 0 2 -3.99 21.34 24 0 2 4.72 4.45 -24 0 -2 -11.08 23.48 24 0 3 27.90 11.36 24 0 4 37.72 14.63 24 0 5 20.11 9.39 24 0 6 33.60 13.30 24 2 0 17.58 8.03 -24 -2 0 1.30 11.67 24 2 1 34.77 13.19 -24 -2 -1 3.94 16.20 24 2 2 3.36 6.39 24 2 3 15.16 8.58 24 2 4 21.89 11.07 25 1 0 18.45 6.01 -25 -1 0 -3.08 14.08 25 -1 0 0.64 5.63 25 1 1 148.51 23.57 -25 -1 -1 1.26 20.83 25 -1 1 -0.53 22.84 25 1 2 48.33 11.93 25 -1 2 0.06 10.37 25 1 3 -0.19 6.62 25 -1 3 2.20 5.49 25 1 4 17.57 9.11 26 0 0 13.20 7.42 26 0 1 15.68 9.28 26 0 2 19.97 9.83 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 58075 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, 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 0.58656(5) 0.5000 0.74939(6) 0.0333(4) Uani 1 2 d S T P . . Pb2 Pb 0.5000 1.0000 0.5000 0.0276(5) Uani 1 4 d S T P . . I1 I 0.68838(7) 0.0000 0.79855(10) 0.0431(5) Uani 1 2 d S T P . . I2 I 0.54468(10) 0.5000 0.91237(9) 0.0568(7) Uani 1 2 d S T P . . I3 I 0.47803(6) 1.0000 0.68619(8) 0.0301(5) Uani 1 2 d S T P . . I4 I 0.39407(6) 0.5000 0.45398(8) 0.0307(5) Uani 1 2 d S T P . . N1 N 0.8923(9) 0.5000 0.908(2) 0.135(15) Uani 1 2 d DS T P A 1 H1A H 0.9247 0.5000 0.9517 0.202 Uiso 1 2 d R U P A 1 H1B H 0.8947 0.3397 0.8763 0.202 Uiso 1 1 d R U . A 1 C1 C 0.8323(10) 0.5000 0.935(2) 0.135(15) Uani 1 2 d DS T P A 1 H1C H 0.7971 0.5000 0.8880 0.202 Uiso 1 2 d R U P A 1 H1D H 0.8299 0.6726 0.9690 0.202 Uiso 1 1 d R U . A 1 O1 O 0.8249(6) 0.559(2) 0.7354(7) 0.068(8) Uani 0.25 1 d D . P B 2 O2 O 0.8636(5) 0.959(3) 0.8018(7) 0.068(8) Uani 0.25 1 d D . P B 2 C2 C 0.8410(3) 0.845(2) 0.7371(6) 0.068(8) Uani 0.25 1 d D . P B 2 C3 C 0.8263(8) 0.969(3) 0.6520(7) 0.068(8) Uani 0.25 1 d D . P B 2 H3A H 0.8645 1.0003 0.6294 0.082 Uiso 0.25 1 d R U P B 2 H3B H 0.8050 1.1594 0.6512 0.082 Uiso 0.25 1 d R U P B 2 C4 C 0.7815(8) 0.747(3) 0.6042(7) 0.068(8) Uani 0.25 1 d D . P B 2 H4A H 0.7880 0.7291 0.5473 0.082 Uiso 0.25 1 d R U P B 2 H4B H 0.7371 0.7954 0.6027 0.082 Uiso 0.25 1 d R U P B 2 C5 C 0.7990(7) 0.469(3) 0.6526(9) 0.068(8) Uani 0.25 1 d D . P B 2 H5A H 0.7624 0.3403 0.6509 0.082 Uiso 0.25 1 d R U P B 2 H5B H 0.8310 0.3616 0.6299 0.082 Uiso 0.25 1 d R U P B 2 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 0.0380(7) 0.0308(8) 0.0288(6) 0.000 0.0016(4) 0.000 Pb2 0.0267(8) 0.0277(9) 0.0259(7) 0.000 0.0000(5) 0.000 I1 0.0321(9) 0.0356(10) 0.0544(10) 0.000 -0.0078(7) 0.000 I2 0.0836(14) 0.0544(13) 0.0334(9) 0.000 0.0146(8) 0.000 I3 0.0260(8) 0.0370(10) 0.0259(7) 0.000 0.0020(5) 0.000 I4 0.0251(8) 0.0317(10) 0.0329(8) 0.000 0.0007(6) 0.000 N1 0.066(14) 0.041(13) 0.25(4) 0.000 -0.07(2) 0.000 C1 0.066(14) 0.041(13) 0.25(4) 0.000 -0.07(2) 0.000 O1 0.037(12) 0.09(2) 0.079(15) -0.03(2) 0.020(11) -0.026(18) O2 0.037(12) 0.09(2) 0.079(15) -0.03(2) 0.020(11) -0.026(18) C2 0.037(12) 0.09(2) 0.079(15) -0.03(2) 0.020(11) -0.026(18) C3 0.037(12) 0.09(2) 0.079(15) -0.03(2) 0.020(11) -0.026(18) C4 0.037(12) 0.09(2) 0.079(15) -0.03(2) 0.020(11) -0.026(18) C5 0.037(12) 0.09(2) 0.079(15) -0.03(2) 0.020(11) -0.026(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0070 0.0030 '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 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0210 0.0120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.0340 3.1360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -9.9000 4.0740 '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 I2 Pb1 I1 95.27(5) . . I1 Pb1 I1 92.38(5) 1_565 . I2 Pb1 I3 87.58(5) . . I1 Pb1 I3 89.80(3) 1_565 . I1 Pb1 I3 176.23(4) . . I1 Pb1 I3 176.23(4) 1_565 1_545 I1 Pb1 I3 89.80(3) . 1_545 I3 Pb1 I3 87.85(4) . 1_545 I3 Pb2 I4 89.33(4) . . I4 Pb2 I4 89.57(4) 5_666 . Pb1 I1 Pb1 92.38(5) 1_545 . Pb2 I3 Pb1 93.91(4) . . Pb1 I3 Pb1 87.85(4) . 1_565 C1 N1 H1A 111.0 . . C1 N1 H1B 109.7 . . H1A N1 H1B 109.6 . . N1 C1 H1C 110.4 . . N1 C1 H1D 109.5 . . H1C C1 H1D 109.6 . . C2 O1 C5 110.38(6) . . O2 C2 O1 119.60(10) . . O2 C2 C3 130.37(10) . . O1 C2 C3 110.04(6) . . C2 C3 C4 103.37(8) . . C2 C3 H3A 112.3 . . C4 C3 H3A 113.5 . . C2 C3 H3B 111.1 . . C4 C3 H3B 109.6 . . H3A C3 H3B 107.1 . . C5 C4 C3 102.80(9) . . C5 C4 H4A 111.5 . . C3 C4 H4A 110.8 . . C5 C4 H4B 109.9 . . C3 C4 H4B 112.6 . . H4A C4 H4B 109.1 . . O1 C5 C4 105.76(8) . . O1 C5 H5A 110.8 . . C4 C5 H5A 111.9 . . O1 C5 H5B 109.9 . . C4 C5 H5B 109.8 . . H5A C5 H5B 108.7 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pb1 I2 3.036(2) . Pb1 I1 3.1856(13) . Pb1 I3 3.3139(12) . Pb1 I3 3.3140(13) 1_545 Pb2 I3 3.2329(14) 5_676 Pb2 I3 3.2329(14) . Pb2 I4 3.2390(10) 5_676 Pb2 I4 3.2390(10) 5_666 Pb2 I4 3.2390(10) 1_565 Pb2 I4 3.2391(10) . I1 Pb1 3.1856(13) 1_545 I3 Pb1 3.3140(12) 1_565 I4 Pb2 3.2391(10) 1_545 N1 C1 1.4750(11) . N1 H1A 0.9100 . N1 H1B 0.9100 . C1 H1C 0.9800 . C1 H1D 0.9800 . O1 C2 1.3598(9) . O1 C5 1.4402(10) . O2 C2 1.2084(8) . C2 C3 1.4996(9) . C3 C4 1.5202(11) . C3 H3A 0.9900 . C3 H3B 0.9900 . C4 C5 1.5197(10) . C4 H4A 0.9900 . C4 H4B 0.9900 . C5 H5A 0.9900 . C5 H5B 0.9900 . 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 O2 C2 C3 C4 -163.0(2) O1 C2 C3 C4 16.9(2) C2 C3 C4 C5 -25.8(3) C2 O1 C5 C4 -17.2(2) C3 C4 C5 O1 26.5(4)