#------------------------------------------------------------------------------
#$Date: 2019-11-26 02:12:25 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242375 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/23/4132396.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_4132396
loop_
_publ_author_name
'Passarelli, James V.'
'Fairfield, Daniel J.'
'Sather, Nicholas A.'
'Hendricks, Mark P.'
'Sai, Hiroaki'
'Stern, Charlotte L.'
'Stupp, Samuel I.'
_publ_section_title
;
 Enhanced Out-of-Plane Conductivity and Photovoltaic Performance in n = 1
 Layered Perovskites through Organic Cation Design.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7313
_journal_page_last               7323
_journal_paper_doi               10.1021/jacs.8b03659
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'I8 Pb2, 4(C12 H14 N O)'
_chemical_formula_sum            'C48 H56 I8 N4 O4 Pb2'
_chemical_formula_weight         2182.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.668(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5228(17)
_cell_length_b                   12.4668(17)
_cell_length_c                   39.555(6)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.356
_cell_measurement_theta_min      2.912
_cell_volume                     6120.1(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            52790
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.392
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.571
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1295 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.6261. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_description       plate
_exptl_crystal_F_000             3968
_exptl_crystal_preparation
'Prepared from 2:1 solution of cation:lead (II) iodide disolved in GBL with vapor diffusion of DCM.'
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.027
_refine_diff_density_max         2.584
_refine_diff_density_min         -4.336
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details
;
 Flack x determined using 4603 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         10978
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0384
_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)+(0.0133P)²+199.3977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10289
_reflns_number_total             10978
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b03659_si_001.cif
_cod_data_source_block           1_napthyl_ethyl
_cod_original_cell_volume        6120.0(15)
_cod_database_code               4132396
_shelx_shelxl_version_number     2016/6
_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   0.782
_shelx_estimated_absorpt_t_min   0.152
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.625(10)
 0.375(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Rigid body (RIGU) restrains
 C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C23(H23A,H23B), C24(H24A,H24B), C35(H35A,
 H35B), C36(H36A,H36B), C47(H47A,H47B), C48(H48A,H48B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28),
  C31(H31), C32(H32), C33(H33), C34(H34), C38(H38), C39(H39), C40(H40),
 C42(H42), C43(H43), C44(H44), C45(H45)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
;
_olex2_exptl_crystal_mounting_method
'Mounted on kapton loop at RT using grease to fixcrystal in place.'
_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'
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
Pb1 Pb 0.50272(7) 0.34781(6) 0.49362(3) 0.03519(16) Uani 1 1 d . .
Pb2 Pb 0.50606(7) -0.15586(6) 0.49169(3) 0.03545(16) Uani 1 1 d . .
I1 I 0.48061(12) 0.37742(13) 0.41329(4) 0.0499(4) Uani 1 1 d . .
I2 I 0.52493(13) 0.32410(14) 0.57476(4) 0.0489(4) Uani 1 1 d . .
I3 I 0.75635(12) 0.29565(11) 0.49672(5) 0.0461(3) Uani 1 1 d . .
I4 I 0.25233(16) 0.39743(13) 0.48818(6) 0.0532(4) Uani 1 1 d . .
I5 I 0.55901(14) 0.59566(10) 0.49704(5) 0.0524(4) Uani 1 1 d . .
I6 I 0.45133(13) 0.09587(10) 0.48921(5) 0.0490(4) Uani 1 1 d . .
I7 I 0.57166(14) -0.14443(13) 0.57183(4) 0.0520(4) Uani 1 1 d . .
I8 I 0.44645(13) -0.16563(14) 0.41066(4) 0.0511(4) Uani 1 1 d . .
O1 O 0.7633(14) 0.6467(14) 0.6257(4) 0.063(4) Uani 1 1 d . .
N1 N 0.7869(16) 0.6589(18) 0.5589(5) 0.059(5) Uani 1 1 d . .
H1A H 0.835636 0.662901 0.544449 0.071 Uiso 1 1 calc GR .
H1B H 0.797881 0.711804 0.574033 0.071 Uiso 1 1 calc GR .
H1C H 0.721149 0.664828 0.547314 0.071 Uiso 1 1 calc GR .
C1 C 0.707(2) 0.6709(18) 0.6525(6) 0.056(6) Uani 1 1 d . .
C2 C 0.735(2) 0.774(2) 0.6673(6) 0.060(5) Uani 1 1 d . U
C3 C 0.812(2) 0.842(2) 0.6551(7) 0.068(6) Uani 1 1 d . U
H3 H 0.848387 0.821715 0.637161 0.082 Uiso 1 1 calc R .
C4 C 0.829(3) 0.940(3) 0.6713(8) 0.089(8) Uani 1 1 d . U
H4 H 0.875388 0.987727 0.663017 0.107 Uiso 1 1 calc R .
C5 C 0.781(3) 0.970(3) 0.6988(9) 0.099(9) Uani 1 1 d . U
H5 H 0.800694 1.034159 0.709596 0.119 Uiso 1 1 calc R .
C6 C 0.707(3) 0.910(3) 0.7106(9) 0.086(7) Uani 1 1 d . U
H6 H 0.671662 0.934743 0.728250 0.103 Uiso 1 1 calc R .
C7 C 0.683(3) 0.804(2) 0.6954(7) 0.072(6) Uani 1 1 d . U
C8 C 0.609(3) 0.735(3) 0.7076(8) 0.088(9) Uani 1 1 d . .
H8 H 0.576316 0.754833 0.726514 0.105 Uiso 1 1 calc R .
C9 C 0.584(3) 0.640(3) 0.6921(8) 0.088(10) Uani 1 1 d . .
H9 H 0.532422 0.595527 0.699834 0.105 Uiso 1 1 calc R .
C10 C 0.635(2) 0.610(3) 0.6646(7) 0.075(9) Uani 1 1 d . .
H10 H 0.617320 0.543605 0.654260 0.090 Uiso 1 1 calc R .
C11 C 0.726(2) 0.558(2) 0.6047(6) 0.060(6) Uani 1 1 d . .
H11A H 0.651537 0.567945 0.595058 0.071 Uiso 1 1 calc R .
H11B H 0.732203 0.491938 0.617803 0.071 Uiso 1 1 calc R .
C12 C 0.797(2) 0.554(2) 0.5769(7) 0.062(7) Uani 1 1 d . .
H12A H 0.871464 0.541289 0.586587 0.075 Uiso 1 1 calc R .
H12B H 0.774590 0.495927 0.561129 0.075 Uiso 1 1 calc R .
O2 O 0.7825(14) 0.1738(14) 0.6240(4) 0.063(4) Uani 1 1 d . .
N2 N 0.7043(18) 0.0983(16) 0.5598(6) 0.059(6) Uani 1 1 d . .
H2A H 0.709232 0.142139 0.542348 0.071 Uiso 1 1 calc GR .
H2B H 0.665966 0.129792 0.574441 0.071 Uiso 1 1 calc GR .
H2C H 0.672084 0.037732 0.552239 0.071 Uiso 1 1 calc GR .
C13 C 0.804(2) 0.2576(19) 0.6464(6) 0.061(6) Uani 1 1 d . .
C14 C 0.890(2) 0.317(3) 0.6489(8) 0.078(8) Uani 1 1 d . .
H14 H 0.943396 0.300743 0.635335 0.093 Uiso 1 1 calc R .
C15 C 0.905(3) 0.403(3) 0.6710(10) 0.103(11) Uani 1 1 d . .
H15 H 0.962110 0.450617 0.670505 0.123 Uiso 1 1 calc R .
C16 C 0.834(4) 0.416(3) 0.6933(9) 0.109(13) Uani 1 1 d . .
H16 H 0.847474 0.469417 0.709661 0.130 Uiso 1 1 calc R .
C17 C 0.742(4) 0.354(3) 0.6936(8) 0.090(12) Uani 1 1 d . .
C18 C 0.663(5) 0.364(4) 0.7147(10) 0.118(18) Uani 1 1 d . .
H18 H 0.673848 0.416370 0.731429 0.141 Uiso 1 1 calc R .
C19 C 0.579(4) 0.312(4) 0.7139(10) 0.13(2) Uani 1 1 d . .
H19 H 0.530403 0.327495 0.728905 0.150 Uiso 1 1 calc R .
C20 C 0.557(3) 0.223(3) 0.6888(10) 0.107(13) Uani 1 1 d . .
H20 H 0.495204 0.181955 0.687663 0.129 Uiso 1 1 calc R .
C21 C 0.632(3) 0.206(2) 0.6676(7) 0.085(11) Uani 1 1 d . .
H21 H 0.619991 0.149957 0.651916 0.102 Uiso 1 1 calc R .
C22 C 0.723(3) 0.266(2) 0.6681(6) 0.069(8) Uani 1 1 d . .
C23 C 0.852(2) 0.160(2) 0.5986(7) 0.065(7) Uani 1 1 d . .
H23A H 0.854816 0.225356 0.585403 0.078 Uiso 1 1 calc R .
H23B H 0.924705 0.143478 0.609234 0.078 Uiso 1 1 calc R .
C24 C 0.812(2) 0.074(2) 0.5770(8) 0.063(8) Uani 1 1 d . .
H24A H 0.809070 0.009626 0.590395 0.076 Uiso 1 1 calc R .
H24B H 0.859534 0.061749 0.560065 0.076 Uiso 1 1 calc R .
O3 O 0.7706(14) 0.5651(14) 0.3611(4) 0.061(4) Uani 1 1 d . .
N3 N 0.7286(15) 0.5185(16) 0.4264(5) 0.054(5) Uani 1 1 d . .
H3A H 0.767078 0.479976 0.413483 0.065 Uiso 1 1 calc GR .
H3B H 0.672168 0.480344 0.430996 0.065 Uiso 1 1 calc GR .
H3C H 0.769434 0.535548 0.445874 0.065 Uiso 1 1 calc GR .
C25 C 0.842(2) 0.573(2) 0.3381(6) 0.060(6) Uani 1 1 d . .
C26 C 0.907(2) 0.659(2) 0.3350(7) 0.070(8) Uani 1 1 d . .
H26 H 0.906880 0.719190 0.349128 0.085 Uiso 1 1 calc R .
C27 C 0.975(3) 0.652(3) 0.3080(11) 0.102(12) Uani 1 1 d . .
H27 H 1.021732 0.708451 0.304924 0.122 Uiso 1 1 calc R .
C28 C 0.974(3) 0.567(4) 0.2877(11) 0.123(18) Uani 1 1 d . .
H28 H 1.018121 0.567252 0.270483 0.147 Uiso 1 1 calc R .
C29 C 0.910(3) 0.480(3) 0.2910(8) 0.088(10) Uani 1 1 d . .
C30 C 0.838(2) 0.480(2) 0.3162(6) 0.066(7) Uani 1 1 d . .
C31 C 0.773(3) 0.390(2) 0.3190(7) 0.077(8) Uani 1 1 d . .
H31 H 0.727148 0.389837 0.335586 0.092 Uiso 1 1 calc R .
C32 C 0.775(3) 0.301(3) 0.2984(11) 0.111(14) Uani 1 1 d . .
H32 H 0.731579 0.241278 0.301028 0.133 Uiso 1 1 calc R .
C33 C 0.847(4) 0.303(3) 0.2721(12) 0.124(19) Uani 1 1 d . .
H33 H 0.850480 0.245610 0.257272 0.149 Uiso 1 1 calc R .
C34 C 0.907(4) 0.390(4) 0.2702(9) 0.116(16) Uani 1 1 d . .
H34 H 0.951105 0.390396 0.253127 0.139 Uiso 1 1 calc R .
C35 C 0.775(2) 0.651(2) 0.3858(7) 0.069(7) Uani 1 1 d . .
H35A H 0.755008 0.719011 0.374881 0.083 Uiso 1 1 calc R .
H35B H 0.845728 0.656913 0.398807 0.083 Uiso 1 1 calc R .
C36 C 0.6913(18) 0.616(2) 0.4085(7) 0.054(6) Uani 1 1 d . .
H36A H 0.681491 0.671864 0.424803 0.065 Uiso 1 1 calc R .
H36B H 0.622601 0.602694 0.394684 0.065 Uiso 1 1 calc R .
O4 O 0.2410(13) 0.5503(14) 0.3606(4) 0.063(4) Uani 1 1 d . .
N4 N 0.292(2) 0.6031(15) 0.4272(6) 0.065(7) Uani 1 1 d . .
H4A H 0.329429 0.562006 0.414522 0.078 Uiso 1 1 calc GR .
H4B H 0.296340 0.575602 0.448108 0.078 Uiso 1 1 calc GR .
H4C H 0.320114 0.668996 0.428426 0.078 Uiso 1 1 calc GR .
C37 C 0.251(2) 0.476(2) 0.3344(6) 0.061(6) Uani 1 1 d . .
C38 C 0.176(3) 0.401(2) 0.3245(8) 0.081(10) Uani 1 1 d . .
H38 H 0.114980 0.391481 0.335476 0.098 Uiso 1 1 calc R .
C39 C 0.195(5) 0.337(3) 0.2967(11) 0.123(18) Uani 1 1 d . .
H39 H 0.145937 0.283267 0.289119 0.148 Uiso 1 1 calc R .
C40 C 0.281(5) 0.351(3) 0.2806(13) 0.12(2) Uani 1 1 d . .
H40 H 0.288167 0.309074 0.261537 0.150 Uiso 1 1 calc R .
C41 C 0.356(4) 0.420(4) 0.2906(8) 0.107(14) Uani 1 1 d . .
C42 C 0.453(3) 0.435(4) 0.2756(11) 0.132(12) Uani 1 1 d . U
H42 H 0.464985 0.392087 0.257245 0.159 Uiso 1 1 calc R .
C43 C 0.528(3) 0.509(4) 0.2875(10) 0.122(10) Uani 1 1 d . U
H43 H 0.589877 0.515510 0.277021 0.146 Uiso 1 1 calc R .
C44 C 0.516(3) 0.577(4) 0.3149(9) 0.119(10) Uani 1 1 d . U
H44 H 0.568627 0.626732 0.322943 0.143 Uiso 1 1 calc R .
C45 C 0.424(2) 0.568(3) 0.3293(8) 0.097(9) Uani 1 1 d . U
H45 H 0.415190 0.613128 0.347495 0.116 Uiso 1 1 calc R .
C46 C 0.344(2) 0.497(3) 0.3188(7) 0.075(7) Uani 1 1 d . U
C47 C 0.164(2) 0.524(3) 0.3826(8) 0.074(8) Uani 1 1 d . .
H47A H 0.177114 0.452077 0.391857 0.089 Uiso 1 1 calc R .
H47B H 0.091554 0.526308 0.370352 0.089 Uiso 1 1 calc R .
C48 C 0.178(3) 0.608(4) 0.4115(11) 0.108(15) Uani 1 1 d . .
H48A H 0.160118 0.678886 0.402367 0.130 Uiso 1 1 calc R .
H48B H 0.130302 0.591562 0.428337 0.130 Uiso 1 1 calc R .
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'
O O 0.0106 0.0060 '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
I1 Pb1 I2 178.62(6) . .
I1 Pb1 I3 90.88(5) . .
I1 Pb1 I4 87.48(6) . .
I1 Pb1 I6 93.98(5) . .
I2 Pb1 I3 89.42(5) . .
I2 Pb1 I6 87.36(5) . .
I4 Pb1 I2 92.23(6) . .
I4 Pb1 I3 178.27(7) . .
I4 Pb1 I6 89.88(5) . .
I5 Pb1 I1 85.33(5) . .
I5 Pb1 I2 93.33(5) . .
I5 Pb1 I3 89.01(5) . .
I5 Pb1 I4 91.43(5) . .
I5 Pb1 I6 178.49(7) . .
I6 Pb1 I3 89.66(5) . .
I4 Pb2 I3 178.40(7) 3_545 3_445
I4 Pb2 I6 89.93(5) 3_545 .
I4 Pb2 I8 93.57(6) 3_545 .
I5 Pb2 I3 90.49(5) 1_545 3_445
I5 Pb2 I4 90.67(5) 1_545 3_545
I5 Pb2 I6 177.88(8) 1_545 .
I5 Pb2 I7 87.32(5) 1_545 .
I5 Pb2 I8 92.78(5) 1_545 .
I6 Pb2 I3 88.87(5) . 3_445
I7 Pb2 I3 94.07(6) . 3_445
I7 Pb2 I4 84.88(6) . 3_545
I7 Pb2 I6 90.71(5) . .
I7 Pb2 I8 178.45(7) . .
I8 Pb2 I3 87.47(6) . 3_445
I8 Pb2 I6 89.21(5) . .
Pb2 I3 Pb1 156.83(5) 3 .
Pb1 I4 Pb2 155.82(6) . 3_455
Pb1 I5 Pb2 155.11(7) . 1_565
Pb1 I6 Pb2 156.25(7) . .
C1 O1 C11 117.2(19) . .
H1A N1 H1B 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C12 N1 H1A 109.5 . .
C12 N1 H1B 109.5 . .
C12 N1 H1C 109.5 . .
O1 C1 C2 113(2) . .
C10 C1 O1 126(3) . .
C10 C1 C2 121(3) . .
C3 C2 C1 122(2) . .
C7 C2 C1 116(3) . .
C7 C2 C3 121(3) . .
C2 C3 H3 122.0 . .
C4 C3 C2 116(3) . .
C4 C3 H3 122.0 . .
C3 C4 H4 118.1 . .
C5 C4 C3 124(4) . .
C5 C4 H4 118.1 . .
C4 C5 H5 118.9 . .
C6 C5 C4 122(3) . .
C6 C5 H5 118.9 . .
C5 C6 H6 120.6 . .
C5 C6 C7 119(4) . .
C7 C6 H6 120.6 . .
C2 C7 C6 118(3) . .
C8 C7 C2 121(3) . .
C8 C7 C6 122(3) . .
C7 C8 H8 119.8 . .
C9 C8 C7 120(3) . .
C9 C8 H8 119.8 . .
C8 C9 H9 120.2 . .
C8 C9 C10 120(3) . .
C10 C9 H9 120.2 . .
C1 C10 C9 122(3) . .
C1 C10 H10 118.9 . .
C9 C10 H10 118.9 . .
O1 C11 H11A 110.5 . .
O1 C11 H11B 110.5 . .
O1 C11 C12 106(2) . .
H11A C11 H11B 108.7 . .
C12 C11 H11A 110.5 . .
C12 C11 H11B 110.5 . .
N1 C12 C11 107.3(19) . .
N1 C12 H12A 110.2 . .
N1 C12 H12B 110.2 . .
C11 C12 H12A 110.2 . .
C11 C12 H12B 110.2 . .
H12A C12 H12B 108.5 . .
C13 O2 C23 117(2) . .
H2A N2 H2B 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
C24 N2 H2A 109.5 . .
C24 N2 H2B 109.5 . .
C24 N2 H2C 109.5 . .
O2 C13 C22 111(2) . .
C14 C13 O2 125(3) . .
C14 C13 C22 124(3) . .
C13 C14 H14 119.0 . .
C13 C14 C15 122(3) . .
C15 C14 H14 119.0 . .
C14 C15 H15 121.2 . .
C16 C15 C14 118(4) . .
C16 C15 H15 121.2 . .
C15 C16 H16 117.8 . .
C15 C16 C17 124(4) . .
C17 C16 H16 117.8 . .
C16 C17 C22 118(3) . .
C18 C17 C16 128(4) . .
C18 C17 C22 114(4) . .
C17 C18 H18 116.0 . .
C19 C18 C17 128(5) . .
C19 C18 H18 116.0 . .
C18 C19 H19 120.3 . .
C18 C19 C20 119(4) . .
C20 C19 H19 120.3 . .
C19 C20 H20 121.5 . .
C21 C20 C19 117(4) . .
C21 C20 H20 121.5 . .
C20 C21 H21 118.5 . .
C20 C21 C22 123(4) . .
C22 C21 H21 118.5 . .
C13 C22 C17 114(3) . .
C21 C22 C13 128(3) . .
C21 C22 C17 118(3) . .
O2 C23 H23A 110.1 . .
O2 C23 H23B 110.1 . .
H23A C23 H23B 108.4 . .
C24 C23 O2 108(2) . .
C24 C23 H23A 110.1 . .
C24 C23 H23B 110.1 . .
N2 C24 H24A 109.4 . .
N2 C24 H24B 109.4 . .
C23 C24 N2 111(2) . .
C23 C24 H24A 109.4 . .
C23 C24 H24B 109.4 . .
H24A C24 H24B 108.0 . .
C25 O3 C35 116(2) . .
H3A N3 H3B 109.5 . .
H3A N3 H3C 109.5 . .
H3B N3 H3C 109.5 . .
C36 N3 H3A 109.5 . .
C36 N3 H3B 109.5 . .
C36 N3 H3C 109.5 . .
O3 C25 C30 111(2) . .
C26 C25 O3 125(2) . .
C26 C25 C30 124(3) . .
C25 C26 H26 122.3 . .
C25 C26 C27 115(3) . .
C27 C26 H26 122.3 . .
C26 C27 H27 118.9 . .
C28 C27 C26 122(4) . .
C28 C27 H27 118.9 . .
C27 C28 H28 118.8 . .
C27 C28 C29 122(3) . .
C29 C28 H28 118.8 . .
C28 C29 C30 120(3) . .
C28 C29 C34 124(4) . .
C34 C29 C30 116(4) . .
C29 C30 C25 116(3) . .
C31 C30 C25 125(3) . .
C31 C30 C29 119(3) . .
C30 C31 H31 118.4 . .
C32 C31 C30 123(4) . .
C32 C31 H31 118.4 . .
C31 C32 H32 121.3 . .
C31 C32 C33 117(4) . .
C33 C32 H32 121.3 . .
C32 C33 H33 121.1 . .
C34 C33 C32 118(4) . .
C34 C33 H33 121.1 . .
C29 C34 H34 116.6 . .
C33 C34 C29 127(4) . .
C33 C34 H34 116.6 . .
O3 C35 H35A 111.2 . .
O3 C35 H35B 111.2 . .
O3 C35 C36 103(2) . .
H35A C35 H35B 109.1 . .
C36 C35 H35A 111.2 . .
C36 C35 H35B 111.2 . .
N3 C36 C35 109.1(19) . .
N3 C36 H36A 109.9 . .
N3 C36 H36B 109.9 . .
C35 C36 H36A 109.9 . .
C35 C36 H36B 109.9 . .
H36A C36 H36B 108.3 . .
C37 O4 C47 115(2) . .
H4A N4 H4B 109.5 . .
H4A N4 H4C 109.5 . .
H4B N4 H4C 109.5 . .
C48 N4 H4A 109.5 . .
C48 N4 H4B 109.5 . .
C48 N4 H4C 109.5 . .
O4 C37 C46 111(2) . .
C38 C37 O4 123(3) . .
C38 C37 C46 126(3) . .
C37 C38 H38 122.1 . .
C37 C38 C39 116(4) . .
C39 C38 H38 122.1 . .
C38 C39 H39 118.9 . .
C40 C39 C38 122(4) . .
C40 C39 H39 118.9 . .
C39 C40 H40 118.6 . .
C41 C40 C39 123(5) . .
C41 C40 H40 118.6 . .
C40 C41 C42 125(5) . .
C40 C41 C46 121(4) . .
C42 C41 C46 114(5) . .
C41 C42 H42 119.0 . .
C43 C42 C41 122(5) . .
C43 C42 H42 119.0 . .
C42 C43 H43 118.7 . .
C42 C43 C44 123(4) . .
C44 C43 H43 118.7 . .
C43 C44 H44 121.2 . .
C45 C44 C43 118(4) . .
C45 C44 H44 121.2 . .
C44 C45 H45 118.0 . .
C44 C45 C46 124(4) . .
C46 C45 H45 118.0 . .
C37 C46 C41 113(3) . .
C45 C46 C37 127(3) . .
C45 C46 C41 120(3) . .
O4 C47 H47A 110.5 . .
O4 C47 H47B 110.5 . .
O4 C47 C48 106(2) . .
H47A C47 H47B 108.7 . .
C48 C47 H47A 110.5 . .
C48 C47 H47B 110.5 . .
N4 C48 C47 107(3) . .
N4 C48 H48A 110.4 . .
N4 C48 H48B 110.4 . .
C47 C48 H48A 110.4 . .
C47 C48 H48B 110.4 . .
H48A C48 H48B 108.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.174(2) .
Pb1 I2 3.198(2) .
Pb1 I3 3.2283(18) .
Pb1 I4 3.175(2) .
Pb1 I5 3.1681(16) .
Pb1 I6 3.2062(16) .
Pb2 I3 3.2171(18) 3_445
Pb2 I4 3.176(2) 3_545
Pb2 I5 3.1691(16) 1_545
Pb2 I6 3.2110(15) .
Pb2 I7 3.170(2) .
Pb2 I8 3.195(2) .
O1 C1 1.38(3) .
O1 C11 1.42(3) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
N1 C12 1.49(3) .
C1 C2 1.43(3) .
C1 C10 1.32(4) .
C2 C3 1.41(4) .
C2 C7 1.41(4) .
C3 H3 0.9300 .
C3 C4 1.38(4) .
C4 H4 0.9300 .
C4 C5 1.36(5) .
C5 H5 0.9300 .
C5 C6 1.31(5) .
C6 H6 0.9300 .
C6 C7 1.47(4) .
C7 C8 1.40(4) .
C8 H8 0.9300 .
C8 C9 1.35(5) .
C9 H9 0.9300 .
C9 C10 1.39(4) .
C10 H10 0.9300 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C11 C12 1.50(4) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
O2 C13 1.37(3) .
O2 C23 1.43(3) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N2 C24 1.45(4) .
C13 C14 1.30(4) .
C13 C22 1.42(4) .
C14 H14 0.9300 .
C14 C15 1.39(4) .
C15 H15 0.9300 .
C15 C16 1.34(5) .
C16 H16 0.9300 .
C16 C17 1.39(5) .
C17 C18 1.39(6) .
C17 C22 1.49(5) .
C18 H18 0.9300 .
C18 C19 1.22(6) .
C19 H19 0.9300 .
C19 C20 1.49(6) .
C20 H20 0.9300 .
C20 C21 1.35(4) .
C21 H21 0.9300 .
C21 C22 1.37(4) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C23 C24 1.42(4) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
O3 C25 1.36(3) .
O3 C35 1.45(3) .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N3 H3C 0.8900 .
N3 C36 1.45(3) .
C25 C26 1.36(4) .
C25 C30 1.45(3) .
C26 H26 0.9300 .
C26 C27 1.46(5) .
C27 H27 0.9300 .
C27 C28 1.33(6) .
C28 H28 0.9300 .
C28 C29 1.37(6) .
C29 C30 1.43(4) .
C29 C34 1.39(5) .
C30 C31 1.40(4) .
C31 H31 0.9300 .
C31 C32 1.38(4) .
C32 H32 0.9300 .
C32 C33 1.47(6) .
C33 H33 0.9300 .
C33 C34 1.32(6) .
C34 H34 0.9300 .
C35 H35A 0.9700 .
C35 H35B 0.9700 .
C35 C36 1.53(4) .
C36 H36A 0.9700 .
C36 H36B 0.9700 .
O4 C37 1.40(3) .
O4 C47 1.42(3) .
N4 H4A 0.8900 .
N4 H4B 0.8900 .
N4 H4C 0.8900 .
N4 C48 1.49(5) .
C37 C38 1.35(4) .
C37 C46 1.42(4) .
C38 H38 0.9300 .
C38 C39 1.41(5) .
C39 H39 0.9300 .
C39 C40 1.34(6) .
C40 H40 0.9300 .
C40 C41 1.30(6) .
C41 C42 1.43(5) .
C41 C46 1.50(5) .
C42 H42 0.9300 .
C42 C43 1.36(6) .
C43 H43 0.9300 .
C43 C44 1.40(6) .
C44 H44 0.9300 .
C44 C45 1.35(4) .
C45 H45 0.9300 .
C45 C46 1.36(4) .
C47 H47A 0.9700 .
C47 H47B 0.9700 .
C47 C48 1.54(5) .
C48 H48A 0.9700 .
C48 H48B 0.9700 .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.625(10)
2 0.375(10)
