#------------------------------------------------------------------------------
#$Date: 2021-05-19 01:23:48 +0300 (Wed, 19 May 2021) $
#$Revision: 265318 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/39/4003946.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_4003946
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         '4(C7 H14 N O2), I10 Pb3'
_chemical_formula_sum            'C28 H56 I10 N4 O8 Pb3'
_chemical_formula_weight         2467.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.96490(10)
_cell_length_b                   23.28940(10)
_cell_length_c                   14.05910(10)
_cell_measurement_reflns_used    36832
_cell_measurement_temperature    295.53(11)
_cell_measurement_theta_max      73.6500
_cell_measurement_theta_min      3.7940
_cell_volume                     2797.82(4)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.53(11)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -33.00  31.00   0.50    0.50    --    0.00 -82.00  90.00  128
  2  ω      6.00  92.00   0.50    0.50    --   32.00  72.00-152.55  172
  3  ω    -46.00  56.00   0.50    0.50    --   36.00 -55.00 -57.40  204
  4  ω      9.00  75.00   0.50    0.50    --   36.00  72.00  24.32  132
  5  ω     28.00  76.00   0.50    0.50    --   52.00  73.00-119.54   96
  6  ω     31.00  56.00   0.50    0.50    --   56.00  74.00  86.22   50
  7  ω    114.00 144.00   0.50    0.50    --   56.00  75.00  -7.10   60
  8  ω     33.00  69.00   0.50    0.50    --   56.00  75.00  -7.10   72
  9  ω     32.00  57.00   0.50    0.50    --   60.00  74.00 -44.26   50
 10  ω     32.00  65.00   0.50    0.50    --   60.00  75.00 156.78   66
 11  ω     93.00 119.00   0.50    0.50    --   60.00  75.00 156.78   52
 12  ω     32.00  77.00   0.50    0.50    --   60.00  75.00  42.36   90
 13  ω     36.00  63.00   0.50    0.50    --   64.00  75.00-142.17   54
 14  ω     97.00 123.00   0.50    0.50    --   64.00  75.00 -93.52   52
 15  ω     36.00  76.00   0.50    0.50    --   64.00  75.00 -93.52   80
 16  ω     40.00  71.00   0.50    0.50    --   68.00  75.00 102.38   62
 17  ω     44.00  73.00   0.50    0.50    --   72.00  74.00  78.20   58
 18  ω     44.00  86.00   0.50    0.50    --   72.00  74.00  -2.17   84
 19  ω     44.00  86.00   0.50    0.50    --   72.00  75.00 128.29   84
 20  ω     91.00 122.00   0.50    0.50    --   72.00  75.00 128.29   62
 21  ω     44.00  72.00   0.50    0.50    --   72.00  74.00 -60.54   56
 22  ω    110.00 159.00   0.50    0.50    --   72.00  74.00  -2.17   98
 23  ω     48.00 110.00   0.50    0.50    --   76.00  74.00-117.75  124
 24  ω     49.00  81.00   0.50    0.50    --   76.00  73.00 171.03   64
 25  ω    125.00 165.00   0.50    0.50    --   76.00  74.00-117.75   80
 26  ω     60.00 172.00   0.50    0.50    --   84.00  65.00 -74.23  224
 27  ω    126.00 153.00   0.50    0.50    --   94.60  70.00 -30.42   54
 28  ω     67.00 162.00   0.50    0.50    --   94.60  74.00-124.81  190
 29  ω     69.00 113.00   0.50    0.50    --   94.60  70.00 -30.42   88
 30  ω      6.00 117.00   0.50    0.50    --   94.60 -82.00 -30.00  222
 31  ω      6.00 103.00   0.50    0.50    --   94.60 -61.00-150.00  194
 32  ω     71.00 171.00   0.50    0.50    --   94.60  62.00  76.92  200
 33  ω    133.00 175.00   0.50    0.50    --   94.60  71.00 111.70   84
 34  ω     69.00 166.00   0.50    0.50    --   94.60  68.00-136.87  194
 35  ω     30.00 124.00   0.50    0.50    --   94.60 -82.00  90.00  188
 36  ω     67.00 130.00   0.50    0.50    --   94.60  71.00 111.70  126
 37  ω    101.00 126.00   0.50    0.50    --   94.60 -82.00   0.00   50
 38  ω     36.00  76.00   0.50    0.50    --   94.60 -82.00   0.00   80
 39  ω     68.00 174.00   0.50    0.50    --   94.60  69.00 -54.30  212
 40  ω     22.00 119.00   0.50    0.50    --   94.60 -82.00-150.00  194
 41  ω     44.00  78.00   0.50    0.50    --   94.60 -77.00  30.00   68
 42  ω     73.00 123.00   0.50    0.50    --   94.60  54.00 119.39  100
 43  ω    128.00 184.00   0.50    0.50    --   94.60  63.00 162.46  112
 44  ω     74.00 168.00   0.50    0.50    --   94.60  61.00   0.00  188
 45  ω     71.00 104.00   0.50    0.50    --   94.60  61.00-150.00   66
 46  ω     78.00 178.00   0.50    0.50    --   94.60  61.00-180.00  200
 47  ω     70.00 124.00   0.50    0.50    --   94.60  63.00 162.46  108
 48  ω     73.00 162.00   0.50    0.50    --   94.60  61.00  60.00  178
 49  ω     66.00 100.00   0.50    0.50    --   94.60  75.00  21.56   68
 50  ω     34.00 109.00   0.50    0.50    --   94.60 -61.00  90.00  150
 51  ω     68.00 167.00   0.50    0.50    --   94.60  70.00  15.62  198
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1114307000
_diffrn_orient_matrix_UB_12      -0.0004459000
_diffrn_orient_matrix_UB_13      0.1076415000
_diffrn_orient_matrix_UB_21      -0.0339857000
_diffrn_orient_matrix_UB_22      -0.0643001000
_diffrn_orient_matrix_UB_23      0.0087985000
_diffrn_orient_matrix_UB_31      0.1376033000
_diffrn_orient_matrix_UB_32      -0.0155331000
_diffrn_orient_matrix_UB_33      -0.0394020000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            68096
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.934
_diffrn_reflns_theta_min         3.298
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    60.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04495
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.929
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.018
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.026(9)
_refine_ls_extinction_coef       0.000168(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11059
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0290
_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/[σ²(Fo²)+(0.0469P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                10575
_reflns_number_total             11059
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm1c00391_si_001.cif
_cod_data_source_block           20201122_1rt
_cod_database_code               4003946
_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.
;
_shelx_estimated_absorpt_t_max   0.262
_shelx_estimated_absorpt_t_min   0.039
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.974(9)
 0.026(9)
2. 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
3. Rigid body (RIGU) restrains
 O8, C28, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6), C8(H8), C13(H13), C15(H15), C20(H20), C22(H22), C27(H27)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C26(H26A,H26B)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E), N3(H3C,H3D,H3E), N4(H4C,H4D,H4E)
4.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4), O5(H5), O8(H8A)
;
_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 15.372
_oxdiff_exptl_absorpt_empirical_full_min 0.503
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, 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
C1 C -0.3006(14) 0.5285(6) 0.4418(8) 0.048(3) Uani 1 1 d . . . . .
H1 H -0.396010 0.540258 0.456833 0.058 Uiso 1 1 calc R . . . .
C2 C -0.3334(17) 0.4740(6) 0.3785(10) 0.058(3) Uani 1 1 d . . . . .
H2A H -0.236875 0.460063 0.369082 0.070 Uiso 1 1 calc R . . . .
H2B H -0.373664 0.444457 0.412703 0.070 Uiso 1 1 calc R . . . .
C3 C -0.2470(16) 0.5767(5) 0.3880(9) 0.052(3) Uani 1 1 d . . . . .
H3A H -0.149374 0.566176 0.376256 0.063 Uiso 1 1 calc R . . . .
H3B H -0.229046 0.611072 0.428846 0.063 Uiso 1 1 calc R . . . .
C4 C -0.4523(17) 0.4861(8) 0.2771(10) 0.068(4) Uani 1 1 d . . . . .
H4A H -0.466239 0.451749 0.236396 0.082 Uiso 1 1 calc R . . . .
H4B H -0.552346 0.495450 0.286552 0.082 Uiso 1 1 calc R . . . .
C5 C -0.3707(18) 0.5885(6) 0.2892(10) 0.062(4) Uani 1 1 d . . . . .
H5A H -0.335575 0.619290 0.254816 0.075 Uiso 1 1 calc R . . . .
H5B H -0.466645 0.600733 0.301483 0.075 Uiso 1 1 calc R . . . .
C6 C -0.4031(14) 0.5346(7) 0.2231(10) 0.058(4) Uani 1 1 d . . . . .
H6 H -0.493812 0.543617 0.165657 0.070 Uiso 1 1 calc R . . . .
C7 C -0.2735(14) 0.5206(6) 0.1821(9) 0.047(3) Uani 1 1 d . . . . .
N1 N -0.1743(14) 0.5175(6) 0.5368(8) 0.067(3) Uani 1 1 d . . . . .
H1A H -0.089793 0.504273 0.523260 0.080 Uiso 1 1 calc GR . . . .
H1B H -0.206954 0.491540 0.572569 0.080 Uiso 1 1 calc GR . . . .
H1C H -0.150719 0.549983 0.571355 0.080 Uiso 1 1 calc GR . . . .
O1 O -0.2035(11) 0.5569(4) 0.1489(8) 0.066(3) Uani 1 1 d . . . . .
O2 O -0.2395(15) 0.4661(4) 0.1819(8) 0.070(3) Uani 1 1 d . . . . .
H2 H -0.180645 0.461021 0.148000 0.105 Uiso 1 1 calc GR . . . .
C8 C 0.1743(13) 0.7288(5) 0.4340(7) 0.040(2) Uani 1 1 d . . . . .
H8 H 0.072710 0.728003 0.446671 0.048 Uiso 1 1 calc R . . . .
C9 C 0.1925(16) 0.6749(5) 0.3784(10) 0.052(3) Uani 1 1 d . . . . .
H9A H 0.295076 0.674358 0.368646 0.063 Uiso 1 1 calc R . . . .
H9B H 0.183154 0.641331 0.416950 0.063 Uiso 1 1 calc R . . . .
C10 C 0.1854(14) 0.7829(5) 0.3755(8) 0.041(2) Uani 1 1 d . . . . .
H10A H 0.169995 0.816433 0.412258 0.050 Uiso 1 1 calc R . . . .
H10B H 0.288730 0.785364 0.367147 0.050 Uiso 1 1 calc R . . . .
C11 C 0.0673(16) 0.6738(6) 0.2787(10) 0.057(3) Uani 1 1 d . . . . .
H11A H -0.034577 0.672103 0.289396 0.068 Uiso 1 1 calc R . . . .
H11B H 0.079521 0.639400 0.242885 0.068 Uiso 1 1 calc R . . . .
C12 C 0.0629(15) 0.7818(6) 0.2742(9) 0.055(3) Uani 1 1 d . . . . .
H12A H 0.076661 0.814954 0.236055 0.066 Uiso 1 1 calc R . . . .
H12B H -0.040246 0.784208 0.282852 0.066 Uiso 1 1 calc R . . . .
C13 C 0.0736(13) 0.7261(7) 0.2153(8) 0.053(3) Uani 1 1 d . . . . .
H13 H -0.019385 0.724955 0.156568 0.064 Uiso 1 1 calc R . . . .
C14 C 0.2157(15) 0.7290(6) 0.1778(8) 0.048(3) Uani 1 1 d . . . . .
N2 N 0.3010(12) 0.7309(5) 0.5306(7) 0.051(2) Uani 1 1 d . . . . .
H2C H 0.277249 0.707591 0.574091 0.062 Uiso 1 1 calc GR . . . .
H2D H 0.311075 0.766608 0.554049 0.062 Uiso 1 1 calc GR . . . .
H2E H 0.390610 0.719625 0.521514 0.062 Uiso 1 1 calc GR . . . .
O3 O 0.2670(12) 0.7733(5) 0.1570(8) 0.069(3) Uani 1 1 d . . . . .
O4 O 0.2726(13) 0.6783(5) 0.1698(9) 0.071(3) Uani 1 1 d . . . . .
H4 H 0.352598 0.681735 0.153478 0.107 Uiso 1 1 calc GR . . . .
C15 C -0.4493(19) 0.3595(7) 0.0149(12) 0.070(4) Uani 1 1 d . . . . .
H15 H -0.455892 0.396477 0.046650 0.084 Uiso 1 1 calc R . . . .
C16 C -0.395(2) 0.3146(8) 0.0958(11) 0.081(5) Uani 1 1 d . . . . .
H16A H -0.285689 0.321644 0.132315 0.097 Uiso 1 1 calc R . . . .
H16B H -0.454902 0.318316 0.142357 0.097 Uiso 1 1 calc R . . . .
C17 C -0.604(2) 0.3467(7) -0.0571(16) 0.090(6) Uani 1 1 d . . . . .
H17A H -0.622280 0.372372 -0.113767 0.108 Uiso 1 1 calc R . . . .
H17B H -0.684748 0.354221 -0.025430 0.108 Uiso 1 1 calc R . . . .
C18 C -0.4110(17) 0.2549(7) 0.0560(9) 0.063(4) Uani 1 1 d . . . . .
H18A H -0.383013 0.228165 0.111411 0.076 Uiso 1 1 calc R . . . .
H18B H -0.338178 0.249428 0.017871 0.076 Uiso 1 1 calc R . . . .
C19 C -0.6201(18) 0.2839(7) -0.0949(12) 0.072(4) Uani 1 1 d . . . . .
H19A H -0.727621 0.276791 -0.134418 0.087 Uiso 1 1 calc R . . . .
H19B H -0.554208 0.278324 -0.137547 0.087 Uiso 1 1 calc R . . . .
C20 C -0.5737(15) 0.2415(6) -0.0095(9) 0.054(3) Uani 1 1 d . . . . .
H20 H -0.646382 0.245124 0.030088 0.065 Uiso 1 1 calc R . . . .
C21 C -0.5920(15) 0.1835(6) -0.0558(9) 0.050(3) Uani 1 1 d . . . . .
N3 N -0.3316(16) 0.3654(6) -0.0444(10) 0.076(4) Uani 1 1 d . . . . .
H3C H -0.375573 0.384785 -0.100452 0.091 Uiso 1 1 calc GR . . . .
H3D H -0.303654 0.330711 -0.059159 0.091 Uiso 1 1 calc GR . . . .
H3E H -0.247377 0.384281 -0.007789 0.091 Uiso 1 1 calc GR . . . .
O5 O -0.7289(11) 0.1586(4) -0.0660(7) 0.062(2) Uani 1 1 d . . . . .
H5 H -0.731300 0.127288 -0.093174 0.092 Uiso 1 1 calc GR . . . .
O6 O -0.4918(12) 0.1592(5) -0.0833(8) 0.069(3) Uani 1 1 d . . . . .
C22 C -1.0088(16) 0.5828(6) -0.1054(9) 0.050(3) Uani 1 1 d . . . . .
H22 H -0.984120 0.610627 -0.150824 0.060 Uiso 1 1 calc R . . . .
C23 C -0.8772(17) 0.5831(6) -0.0111(12) 0.065(4) Uani 1 1 d . . . . .
H23A H -0.877459 0.619334 0.022919 0.078 Uiso 1 1 calc R . . . .
H23B H -0.779301 0.580477 -0.026867 0.078 Uiso 1 1 calc R . . . .
C24 C -1.030(2) 0.5258(6) -0.1556(10) 0.067(4) Uani 1 1 d . . . . .
H24A H -0.943590 0.519014 -0.181767 0.081 Uiso 1 1 calc R . . . .
H24B H -1.125413 0.526817 -0.211680 0.081 Uiso 1 1 calc R . . . .
C25 C -0.8854(18) 0.5353(7) 0.0572(11) 0.066(4) Uani 1 1 d . . . . .
H25A H -0.974340 0.541402 0.081697 0.079 Uiso 1 1 calc R . . . .
H25B H -0.791611 0.535703 0.114154 0.079 Uiso 1 1 calc R . . . .
C26 C -1.0409(16) 0.4763(5) -0.0883(9) 0.053(3) Uani 1 1 d . . . . .
H26A H -1.045572 0.440501 -0.124222 0.063 Uiso 1 1 calc R . . . .
H26B H -1.136426 0.479785 -0.069828 0.063 Uiso 1 1 calc R . . . .
C27 C -0.9013(14) 0.4751(5) 0.0057(9) 0.047(3) Uani 1 1 d . . . . .
H27 H -0.806682 0.467739 -0.013503 0.056 Uiso 1 1 calc R . . . .
C28 C -0.9152(18) 0.4304(7) 0.0760(10) 0.062(3) Uani 1 1 d . U . . .
N4 N -1.1565(12) 0.6015(4) -0.0877(9) 0.054(3) Uani 1 1 d . . . . .
H4C H -1.235121 0.598459 -0.144019 0.065 Uiso 1 1 calc GR . . . .
H4D H -1.147336 0.637907 -0.067339 0.065 Uiso 1 1 calc GR . . . .
H4E H -1.175411 0.579423 -0.040985 0.065 Uiso 1 1 calc GR . . . .
O7 O -1.0377(14) 0.4176(4) 0.0918(8) 0.071(3) Uani 1 1 d . U . . .
O8 O -0.7820(19) 0.4032(10) 0.1173(14) 0.152(8) Uani 1 1 d . U . . .
H8A H -0.769217 0.399219 0.177218 0.228 Uiso 1 1 calc GR . . . .
I1 I 0.04797(10) 0.24804(4) 0.10437(5) 0.0507(2) Uani 1 1 d . . . . .
I2 I 0.40554(9) 0.32931(3) 0.33722(5) 0.04293(17) Uani 1 1 d . . . . .
I3 I -0.06715(8) 0.33325(3) 0.36738(6) 0.04495(18) Uani 1 1 d . . . . .
I4 I 0.32252(10) 0.24462(4) 0.58413(6) 0.05022(19) Uani 1 1 d . . . . .
I5 I 0.20235(11) 0.50378(4) 0.42873(6) 0.0545(2) Uani 1 1 d . . . . .
I6 I 0.12485(9) 0.42176(3) 0.68022(6) 0.04528(18) Uani 1 1 d . . . . .
I7 I 0.59972(9) 0.42492(3) 0.66234(6) 0.04819(19) Uani 1 1 d . . . . .
I8 I 0.60692(10) 0.62373(3) 0.65332(7) 0.04851(19) Uani 1 1 d . . . . .
I9 I 0.10874(10) 0.63181(4) 0.65796(7) 0.04944(19) Uani 1 1 d . . . . .
I10 I 0.49806(10) 0.51806(4) 0.90546(6) 0.0549(2) Uani 1 1 d . . . . .
Pb1 Pb 0.14957(5) 0.23394(2) 0.33466(3) 0.03707(11) Uani 1 1 d . . . . .
Pb2 Pb 0.26668(5) 0.37502(2) 0.51156(3) 0.04152(11) Uani 1 1 d . . . . .
Pb3 Pb 0.36100(5) 0.52342(2) 0.67390(3) 0.03873(11) Uani 1 1 d . . . . .
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'
I I -0.3257 6.8362 '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'
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
C3 C1 C2 111.1(10) . . ?
N1 C1 C2 109.8(11) . . ?
N1 C1 C3 107.9(10) . . ?
C4 C2 C1 110.4(12) . . ?
C1 C3 C5 109.7(11) . . ?
C6 C4 C2 112.5(11) . . ?
C3 C5 C6 111.0(10) . . ?
C4 C6 C5 109.8(12) . . ?
C7 C6 C4 114.7(13) . . ?
C7 C6 C5 112.8(12) . . ?
O1 C7 C6 123.3(13) . . ?
O1 C7 O2 121.5(12) . . ?
O2 C7 C6 115.2(12) . . ?
C9 C8 C10 111.8(9) . . ?
N2 C8 C9 109.1(10) . . ?
N2 C8 C10 108.1(9) . . ?
C11 C9 C8 109.2(11) . . ?
C12 C10 C8 110.3(10) . . ?
C9 C11 C13 112.4(10) . . ?
C10 C12 C13 111.8(9) . . ?
C11 C13 C12 109.6(10) . . ?
C14 C13 C11 115.0(12) . . ?
C14 C13 C12 109.9(11) . . ?
O3 C14 C13 123.0(13) . . ?
O3 C14 O4 124.6(12) . . ?
O4 C14 C13 112.4(12) . . ?
C16 C15 N3 110.5(13) . . ?
C17 C15 C16 113.4(15) . . ?
C17 C15 N3 107.8(14) . . ?
C18 C16 C15 112.9(12) . . ?
C15 C17 C19 113.2(13) . . ?
C16 C18 C20 113.1(14) . . ?
C20 C19 C17 111.7(14) . . ?
C18 C20 C19 109.4(12) . . ?
C21 C20 C18 114.6(12) . . ?
C21 C20 C19 106.2(11) . . ?
O5 C21 C20 114.9(11) . . ?
O6 C21 C20 124.5(12) . . ?
O6 C21 O5 120.6(12) . . ?
C23 C22 C24 112.5(11) . . ?
C23 C22 N4 110.9(11) . . ?
N4 C22 C24 110.2(12) . . ?
C22 C23 C25 113.1(11) . . ?
C22 C24 C26 114.1(10) . . ?
C23 C25 C27 112.8(12) . . ?
C24 C26 C27 111.6(11) . . ?
C26 C27 C25 108.7(10) . . ?
C28 C27 C25 109.8(11) . . ?
C28 C27 C26 112.6(12) . . ?
O7 C28 C27 124.1(13) . . ?
O7 C28 O8 123.1(14) . . ?
O8 C28 C27 112.7(13) . . ?
Pb1 I2 Pb2 78.33(2) . . ?
Pb1 I3 Pb2 79.414(19) . . ?
Pb2 I4 Pb1 76.155(19) . . ?
Pb2 I5 Pb3 77.26(2) . . ?
Pb3 I6 Pb2 79.42(2) . . ?
Pb3 I7 Pb2 78.16(2) . . ?
Pb3 I8 Pb1 171.06(3) . 2_656 ?
Pb1 I9 Pb3 173.54(3) 2_556 . ?
I1 Pb1 I2 85.47(2) . . ?
I1 Pb1 I3 94.33(2) . . ?
I1 Pb1 I4 165.94(3) . . ?
I1 Pb1 I8 96.61(2) . 2_646 ?
I1 Pb1 I9 96.91(2) . 2_546 ?
I2 Pb1 I4 80.48(2) . . ?
I2 Pb1 I8 94.45(2) . 2_646 ?
I2 Pb1 I9 177.40(2) . 2_546 ?
I3 Pb1 I2 87.73(2) . . ?
I3 Pb1 I4 84.49(2) . . ?
I3 Pb1 I8 168.98(2) . 2_646 ?
I3 Pb1 I9 93.12(2) . 2_546 ?
I8 Pb1 I4 85.21(2) 2_646 . ?
I8 Pb1 I9 84.26(3) 2_646 2_546 ?
I9 Pb1 I4 97.15(2) 2_546 . ?
I2 Pb2 I7 96.96(2) . . ?
I3 Pb2 I2 85.48(2) . . ?
I3 Pb2 I7 176.63(3) . . ?
I4 Pb2 I2 82.56(2) . . ?
I4 Pb2 I3 86.54(2) . . ?
I4 Pb2 I5 177.39(3) . . ?
I4 Pb2 I6 98.37(3) . . ?
I4 Pb2 I7 96.06(2) . . ?
I5 Pb2 I2 95.77(2) . . ?
I5 Pb2 I3 91.33(2) . . ?
I5 Pb2 I7 86.12(2) . . ?
I6 Pb2 I2 178.83(3) . . ?
I6 Pb2 I3 93.86(2) . . ?
I6 Pb2 I5 83.27(2) . . ?
I6 Pb2 I7 83.66(2) . . ?
I5 Pb3 I9 88.05(2) . . ?
I6 Pb3 I5 81.27(2) . . ?
I6 Pb3 I8 175.98(3) . . ?
I6 Pb3 I9 96.93(2) . . ?
I7 Pb3 I5 86.07(2) . . ?
I7 Pb3 I6 85.90(2) . . ?
I7 Pb3 I8 91.64(2) . . ?
I7 Pb3 I9 173.02(3) . . ?
I8 Pb3 I5 95.40(2) . . ?
I8 Pb3 I9 85.17(3) . . ?
I10 Pb3 I5 169.62(3) . . ?
I10 Pb3 I6 89.79(2) . . ?
I10 Pb3 I7 88.03(2) . . ?
I10 Pb3 I8 93.30(2) . . ?
I10 Pb3 I9 98.33(3) . . ?
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 1.527(19) . ?
C1 C3 1.511(18) . ?
C1 N1 1.489(15) . ?
C2 C4 1.53(2) . ?
C3 C5 1.517(17) . ?
C4 C6 1.50(2) . ?
C5 C6 1.537(19) . ?
C6 C7 1.481(18) . ?
C7 O1 1.226(16) . ?
C7 O2 1.305(16) . ?
C8 C9 1.512(16) . ?
C8 C10 1.523(16) . ?
C8 N2 1.484(14) . ?
C9 C11 1.508(19) . ?
C10 C12 1.512(16) . ?
C11 C13 1.52(2) . ?
C12 C13 1.557(19) . ?
C13 C14 1.520(17) . ?
C14 O3 1.202(16) . ?
C14 O4 1.305(16) . ?
C15 C16 1.51(2) . ?
C15 C17 1.48(2) . ?
C15 N3 1.54(2) . ?
C16 C18 1.49(2) . ?
C17 C19 1.55(2) . ?
C18 C20 1.503(18) . ?
C19 C20 1.51(2) . ?
C20 C21 1.486(19) . ?
C21 O5 1.325(15) . ?
C21 O6 1.220(15) . ?
C22 C23 1.485(19) . ?
C22 C24 1.487(18) . ?
C22 N4 1.485(16) . ?
C23 C25 1.49(2) . ?
C24 C26 1.513(19) . ?
C25 C27 1.565(19) . ?
C26 C27 1.520(17) . ?
C27 C28 1.467(17) . ?
C28 O7 1.221(18) . ?
C28 O8 1.321(18) . ?
I1 Pb1 3.1041(8) . ?
I2 Pb1 3.1859(8) . ?
I2 Pb2 3.2461(9) . ?
I3 Pb1 3.1426(8) . ?
I3 Pb2 3.2158(8) . ?
I4 Pb1 3.3878(8) . ?
I4 Pb2 3.1948(9) . ?
I5 Pb2 3.2054(9) . ?
I5 Pb3 3.3386(9) . ?
I6 Pb2 3.2013(9) . ?
I6 Pb3 3.1952(8) . ?
I7 Pb2 3.3059(9) . ?
I7 Pb3 3.1748(8) . ?
I8 Pb1 3.3406(9) 2_656 ?
I8 Pb3 3.2844(9) . ?
I9 Pb1 3.3430(9) 2_556 ?
I9 Pb3 3.3512(9) . ?
I10 Pb3 3.1151(9) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.974(9)
2 0.026(9)
