#------------------------------------------------------------------------------
#$Date: 2019-11-23 04:55:52 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232174 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/71/4347118.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_4347118
loop_
_publ_author_name
'Travis, Will'
'Knapp, Caroline E.'
'Savory, Christopher N.'
'Ganose, Alex M.'
'Kafourou, Panagiota'
'Song, Xingchi'
'Sharif, Zainab'
'Cockcroft, Jeremy K.'
'Scanlon, David O.'
'Bronstein, Hugo'
'Palgrave, Robert G.'
_publ_section_title
;
 Hybrid Organic-Inorganic Coordination Complexes as Tunable Optical
 Response Materials.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3393
_journal_page_last               3400
_journal_paper_doi               10.1021/acs.inorgchem.5b02749
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C44 H24 I2 N8 Pb'
_chemical_formula_sum            'C44 H24 I2 N8 Pb'
_chemical_formula_weight         1125.70
_chemical_name_systematic        PbI2dppn
_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             2015-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.8576(14)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   26.1924(4)
_cell_length_b                   12.5713(2)
_cell_length_c                   33.1849(5)
_cell_measurement_reflns_used    12392
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.5830
_cell_measurement_theta_min      4.7050
_cell_volume                     10921.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -116.00  -48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6216  -57.0000 -180.0000 68

#__ type_ start__ end____ width___ exp.time_
  2 omega  -79.00   26.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6216   19.0000 -180.0000 105

#__ type_ start__ end____ width___ exp.time_
  3 omega  109.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3614  125.0000  -60.0000 69

#__ type_ start__ end____ width___ exp.time_
  4 omega   78.00  172.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3614   30.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega   84.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3614   30.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
  6 omega   29.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3614  -94.0000 -120.0000 80

#__ type_ start__ end____ width___ exp.time_
  7 omega  -95.00   -7.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.8716  125.0000    0.0000 88

#__ type_ start__ end____ width___ exp.time_
  8 omega  -47.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.8716   38.0000  -90.0000 57

#__ type_ start__ end____ width___ exp.time_
  9 omega   42.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8716 -121.0000  176.0000 43

#__ type_ start__ end____ width___ exp.time_
 10 omega    1.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8716  -99.0000  -30.0000 59

#__ type_ start__ end____ width___ exp.time_
 11 omega   39.00   65.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 12 omega   85.00  111.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 13 omega   37.00   91.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 54

#__ type_ start__ end____ width___ exp.time_
 14 omega   84.00  115.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   60.0000 31

#__ type_ start__ end____ width___ exp.time_
 15 omega   46.00  140.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
 16 omega  120.00  177.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   60.0000 57

#__ type_ start__ end____ width___ exp.time_
 17 omega   36.00   85.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  120.0000 49

#__ type_ start__ end____ width___ exp.time_
 18 omega  100.00  126.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega  130.00  170.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -60.0000 40

#__ type_ start__ end____ width___ exp.time_
 20 omega   37.00   63.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 21 omega   86.00  100.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000    0.0000 14
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0293394000
_diffrn_orient_matrix_UB_12      -0.0413700000
_diffrn_orient_matrix_UB_13      -0.0363240000
_diffrn_orient_matrix_UB_21      -0.0450067000
_diffrn_orient_matrix_UB_22      0.0322431000
_diffrn_orient_matrix_UB_23      -0.0284597000
_diffrn_orient_matrix_UB_31      0.0240210000
_diffrn_orient_matrix_UB_32      0.1107586000
_diffrn_orient_matrix_UB_33      -0.0052629000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            38672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.356
_diffrn_reflns_theta_min         3.377
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.696
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       plate
_exptl_crystal_F_000             6384
_exptl_crystal_preparation
'dppn and lead (II) iodide were separately dissolved in minimum amounts of NMP and layered.'
_exptl_crystal_recrystallization_method 'Layered in NMP'
_exptl_crystal_size_max          0.0658
_exptl_crystal_size_mid          0.0323
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         11082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0404
_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/[σ²(Fo²)+(0.0418P)²+71.0727P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8882
_reflns_number_total             11082
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02749_si_002.cif
_cod_data_source_block           xstr0409
_cod_database_code               4347118
_chemical_oxdiff_formula         'Pb I2 C44 N8 H24'
_chemical_oxdiff_usercomment     'Very thin crystal'
_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.
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(I1D) = Uanis(I2D)
Uanis(I1D) = Uanis(I3D)
3. Others
 Sof(I1D)=Sof(I2D)=Sof(Pb1D)=Sof(I3D)=1-FVAR(1)
 Sof(Pb2D)=0.5*(1-FVAR(2))
 Sof(Pb2)=0.5*FVAR(2)
 Sof(I1)=Sof(I2)=Sof(Pb1)=Sof(I3)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C1A(H1A), C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C8A(H8A),
 C8B(H8B), C9A(H9A), C9B(H9B), C10A(H10A), C10B(H10B), C14A(H14A), C14B(H14B),
 C17A(H17A), C17B(H17B), C19A(H19A), C19B(H19B), C20A(H20A), C20B(H20B),
 C21A(H21A), C21B(H21B), C22A(H22A), C22B(H22B), C1C(H1C), C2C(H2C), C3C(H3C),
 C8C(H8C), C9C(H9C), C10C(H10C), C14C(H14C), C17C(H17C), C19C(H19C), C20C(H20C),
  C21C(H21C), C22C(H22C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-03-30
_olex2_exptl_crystal_mounting_method 'Mounted on a nylon loop'
_olex2_submission_original_sample_id XSTR0409
_olex2_submission_special_instructions 'No special instructions were received'
_usercomment
'Ligands are labelled with the subsection A B and C to indicate the three different ligand environments in the asymmetric unit'
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
C1B C 0.2204(3) 0.2777(6) 0.3015(2) 0.0483(16) Uani 1 1 d . . . . .
H1B H 0.2075 0.2408 0.2791 0.058 Uiso 1 1 calc R . . . .
C1A C 0.4427(3) 0.2918(6) 0.1905(2) 0.0456(15) Uani 1 1 d . . . . .
H1A H 0.4564 0.2511 0.2116 0.055 Uiso 1 1 calc R . . . .
C2A C 0.4713(3) 0.3053(6) 0.1561(2) 0.0501(17) Uani 1 1 d . . . . .
H2A H 0.5033 0.2740 0.1543 0.060 Uiso 1 1 calc R . . . .
C2B C 0.1898(3) 0.2892(6) 0.3343(2) 0.0527(18) Uani 1 1 d . . . . .
H2B H 0.1572 0.2601 0.3340 0.063 Uiso 1 1 calc R . . . .
C3A C 0.4513(3) 0.3655(6) 0.1251(2) 0.0458(16) Uani 1 1 d . . . . .
H3A H 0.4694 0.3747 0.1018 0.055 Uiso 1 1 calc R . . . .
C3B C 0.2087(3) 0.3447(6) 0.3677(2) 0.0510(18) Uani 1 1 d . . . . .
H3B H 0.1892 0.3516 0.3905 0.061 Uiso 1 1 calc R . . . .
C4A C 0.4036(3) 0.4129(5) 0.12864(18) 0.0386(14) Uani 1 1 d . . . . .
C4B C 0.2574(3) 0.3903(5) 0.36665(19) 0.0409(14) Uani 1 1 d . . . . .
C5A C 0.3773(2) 0.3953(5) 0.16459(18) 0.0356(13) Uani 1 1 d . . . . .
C5B C 0.2858(2) 0.3729(5) 0.33176(19) 0.0386(14) Uani 1 1 d . . . . .
C6A C 0.3275(2) 0.4454(5) 0.16950(18) 0.0358(13) Uani 1 1 d . . . . .
C6B C 0.3363(2) 0.4220(5) 0.32935(18) 0.0388(14) Uani 1 1 d . . . . .
C7A C 0.3061(2) 0.5130(5) 0.13998(17) 0.0363(13) Uani 1 1 d . . . . .
C7B C 0.3562(2) 0.4874(5) 0.36022(18) 0.0395(14) Uani 1 1 d . . . . .
C8A C 0.2580(3) 0.5552(6) 0.1456(2) 0.0429(15) Uani 1 1 d . . . . .
H8A H 0.2433 0.6007 0.1264 0.052 Uiso 1 1 calc R . . . .
C8B C 0.4039(3) 0.5322(6) 0.35586(19) 0.0430(15) Uani 1 1 d . . . . .
H8B H 0.4175 0.5769 0.3758 0.052 Uiso 1 1 calc R . . . .
C9A C 0.2319(3) 0.5293(6) 0.1801(2) 0.0435(15) Uani 1 1 d . . . . .
H9A H 0.1995 0.5565 0.1844 0.052 Uiso 1 1 calc R . . . .
C9B C 0.4312(3) 0.5106(6) 0.3220(2) 0.0447(15) Uani 1 1 d . . . . .
H9B H 0.4632 0.5406 0.3186 0.054 Uiso 1 1 calc R . . . .
C10A C 0.2559(3) 0.4605(5) 0.2081(2) 0.0425(15) Uani 1 1 d . . . . .
H10A H 0.2384 0.4421 0.2310 0.051 Uiso 1 1 calc R . . . .
C10B C 0.4094(3) 0.4425(5) 0.29292(18) 0.0407(14) Uani 1 1 d . . . . .
H10B H 0.4282 0.4258 0.2705 0.049 Uiso 1 1 calc R . . . .
C11A C 0.3339(2) 0.5355(5) 0.10339(18) 0.0370(13) Uani 1 1 d . . . . .
C11B C 0.3257(3) 0.5083(5) 0.39581(18) 0.0404(14) Uani 1 1 d . . . . .
C12A C 0.3812(2) 0.4817(5) 0.09709(18) 0.0392(14) Uani 1 1 d . . . . .
C12B C 0.2775(3) 0.4554(6) 0.39945(19) 0.0439(15) Uani 1 1 d . . . . .
C13A C 0.3466(3) 0.7088(6) -0.0227(2) 0.0482(17) Uani 1 1 d . . . . .
C13B C 0.3056(3) 0.6715(6) 0.5222(2) 0.054(2) Uani 1 1 d . . . . .
C14A C 0.3215(3) 0.6925(6) 0.0136(2) 0.0463(16) Uani 1 1 d . . . . .
H14A H 0.2921 0.7311 0.0187 0.056 Uiso 1 1 calc R . . . .
C14B C 0.3335(3) 0.6590(7) 0.4869(2) 0.0554(19) Uani 1 1 d . . . . .
H14B H 0.3634 0.6975 0.4834 0.067 Uiso 1 1 calc R . . . .
C15A C 0.3400(3) 0.6190(6) 0.04237(19) 0.0416(14) Uani 1 1 d . . . . .
C15B C 0.3158(3) 0.5880(6) 0.45692(19) 0.0479(17) Uani 1 1 d . . . . .
C16A C 0.3858(3) 0.5607(5) 0.03510(19) 0.0409(15) Uani 1 1 d . . . . .
C16B C 0.2691(3) 0.5302(6) 0.4615(2) 0.0469(16) Uani 1 1 d . . . . .
C17A C 0.4107(3) 0.5777(6) -0.0013(2) 0.0453(16) Uani 1 1 d . . . . .
H17A H 0.4402 0.5397 -0.0063 0.054 Uiso 1 1 calc R . . . .
C17B C 0.2421(3) 0.5439(7) 0.4970(2) 0.059(2) Uani 1 1 d . . . . .
H17B H 0.2119 0.5064 0.5006 0.071 Uiso 1 1 calc R . . . .
C18A C 0.3920(3) 0.6499(6) -0.02981(19) 0.0452(16) Uani 1 1 d . . . . .
C18B C 0.2599(3) 0.6127(7) 0.5268(2) 0.060(2) Uani 1 1 d . . . . .
C19A C 0.4176(3) 0.6679(7) -0.0668(2) 0.0545(19) Uani 1 1 d . . . . .
H19A H 0.4469 0.6294 -0.0723 0.065 Uiso 1 1 calc R . . . .
C19B C 0.2334(4) 0.6262(8) 0.5641(2) 0.071(3) Uani 1 1 d . . . . .
H19B H 0.2039 0.5872 0.5684 0.086 Uiso 1 1 calc R . . . .
C20A C 0.3997(3) 0.7403(7) -0.0939(2) 0.055(2) Uani 1 1 d . . . . .
H20A H 0.4169 0.7517 -0.1175 0.066 Uiso 1 1 calc R . . . .
C20B C 0.2510(4) 0.6948(8) 0.5928(2) 0.071(3) Uani 1 1 d . . . . .
H20B H 0.2333 0.7026 0.6164 0.085 Uiso 1 1 calc R . . . .
C21A C 0.3551(3) 0.7986(8) -0.0866(2) 0.061(2) Uani 1 1 d . . . . .
H21A H 0.3433 0.8481 -0.1056 0.074 Uiso 1 1 calc R . . . .
C21B C 0.2953(4) 0.7538(8) 0.5875(2) 0.068(3) Uani 1 1 d . . . . .
H21B H 0.3062 0.8015 0.6074 0.082 Uiso 1 1 calc R . . . .
C22A C 0.3288(3) 0.7838(7) -0.0521(2) 0.057(2) Uani 1 1 d . . . . .
H22A H 0.2993 0.8227 -0.0479 0.068 Uiso 1 1 calc R . . . .
C22B C 0.3232(4) 0.7428(8) 0.5533(2) 0.068(2) Uani 1 1 d . . . . .
H22B H 0.3532 0.7813 0.5505 0.082 Uiso 1 1 calc R . . . .
N1A N 0.3966(2) 0.3349(5) 0.19434(16) 0.0407(12) Uani 1 1 d . . . . .
N1B N 0.2679(2) 0.3173(5) 0.30049(16) 0.0409(12) Uani 1 1 d . . . . .
N2A N 0.3022(2) 0.4205(4) 0.20363(15) 0.0378(11) Uani 1 1 d . . . . .
N2B N 0.3630(2) 0.4003(4) 0.29592(15) 0.0368(11) Uani 1 1 d . . . . .
N3A N 0.4065(2) 0.4922(4) 0.06286(16) 0.0416(12) Uani 1 1 d . . . . .
N3B N 0.2498(2) 0.4660(5) 0.43201(18) 0.0516(15) Uani 1 1 d . . . . .
N4A N 0.3139(2) 0.6034(5) 0.07684(15) 0.0414(12) Uani 1 1 d . . . . .
N4B N 0.3446(2) 0.5734(5) 0.42336(16) 0.0447(13) Uani 1 1 d . . . . .
I1 I 0.23931(3) 0.15070(7) 0.19502(2) 0.0361(2) Uani 0.793(5) 1 d . . . A 1
I2 I 0.41837(5) 0.12305(9) 0.29551(5) 0.0435(2) Uani 0.793(5) 1 d . . . A 1
Pb1 Pb 0.33213(5) 0.25834(8) 0.24607(4) 0.02884(16) Uani 0.793(5) 1 d . . . A 1
C1C C 0.4066(3) 0.0224(7) 0.6927(3) 0.058(2) Uani 1 1 d . . . . .
H1C H 0.3888 0.0405 0.7156 0.069 Uiso 1 1 calc R . . . .
C2C C 0.3834(3) -0.0473(6) 0.6657(3) 0.0553(19) Uani 1 1 d . . . . .
H2C H 0.3509 -0.0742 0.6696 0.066 Uiso 1 1 calc R . . . .
C3C C 0.4111(3) -0.0751(6) 0.6324(3) 0.0547(19) Uani 1 1 d . . . . .
H3C H 0.3976 -0.1233 0.6137 0.066 Uiso 1 1 calc R . . . .
C4C C 0.4593(3) -0.0312(5) 0.6268(2) 0.0466(16) Uani 1 1 d . . . . .
C5C C 0.4787(3) 0.0394(5) 0.6549(2) 0.0469(17) Uani 1 1 d . . . . .
C6C C 0.5278(3) 0.0925(5) 0.6494(2) 0.0461(16) Uani 1 1 d . . . . .
C7C C 0.5545(3) 0.0742(6) 0.6144(2) 0.0514(18) Uani 1 1 d . . . . .
C8C C 0.5996(3) 0.1303(6) 0.6090(3) 0.061(2) Uani 1 1 d . . . . .
H8C H 0.6171 0.1226 0.5853 0.073 Uiso 1 1 calc R . . . .
C9C C 0.6182(3) 0.1969(7) 0.6388(3) 0.066(2) Uani 1 1 d . . . . .
H9C H 0.6487 0.2335 0.6359 0.079 Uiso 1 1 calc R . . . .
C10C C 0.5896(3) 0.2085(7) 0.6743(3) 0.062(2) Uani 1 1 d . . . . .
H10C H 0.6023 0.2520 0.6949 0.075 Uiso 1 1 calc R . . . .
C11C C 0.5347(3) 0.0003(6) 0.5842(2) 0.0470(16) Uani 1 1 d . . . . .
C12C C 0.4885(3) -0.0575(6) 0.5905(2) 0.0479(17) Uani 1 1 d . . . . .
C13C C 0.5494(3) -0.1770(6) 0.4602(2) 0.0473(16) Uani 1 1 d . . . . .
C14C C 0.5674(3) -0.1016(6) 0.4878(2) 0.0517(19) Uani 1 1 d . . . . .
H14C H 0.5963 -0.0617 0.4824 0.062 Uiso 1 1 calc R . . . .
C15C C 0.5419(3) -0.0858(6) 0.5239(2) 0.0469(16) Uani 1 1 d . . . . .
C16C C 0.4970(3) -0.1459(6) 0.5312(2) 0.0472(17) Uani 1 1 d . . . . .
C17C C 0.4792(3) -0.2213(6) 0.5035(2) 0.0514(17) Uani 1 1 d . . . . .
H17C H 0.4501 -0.2606 0.5087 0.062 Uiso 1 1 calc R . . . .
C18C C 0.5051(3) -0.2384(6) 0.4675(2) 0.0507(17) Uani 1 1 d . . . . .
C19C C 0.4882(3) -0.3149(7) 0.4383(2) 0.0556(19) Uani 1 1 d . . . . .
H19C H 0.4594 -0.3559 0.4429 0.067 Uiso 1 1 calc R . . . .
C20C C 0.5142(3) -0.3281(8) 0.4037(2) 0.059(2) Uani 1 1 d . . . . .
H20C H 0.5027 -0.3780 0.3848 0.071 Uiso 1 1 calc R . . . .
C21C C 0.5582(3) -0.2672(7) 0.3961(2) 0.058(2) Uani 1 1 d . . . . .
H21C H 0.5754 -0.2774 0.3723 0.069 Uiso 1 1 calc R . . . .
C22C C 0.5756(3) -0.1945(7) 0.4230(2) 0.0533(19) Uani 1 1 d . . . . .
H22C H 0.6046 -0.1552 0.4177 0.064 Uiso 1 1 calc R . . . .
N1C N 0.4528(3) 0.0659(5) 0.68858(19) 0.0527(15) Uani 1 1 d . . . . .
N2C N 0.5454(3) 0.1594(5) 0.6789(2) 0.0551(16) Uani 1 1 d . . . . .
N3C N 0.4702(2) -0.1289(5) 0.56548(18) 0.0479(14) Uani 1 1 d . . . . .
N4C N 0.5608(2) -0.0141(5) 0.55089(19) 0.0484(14) Uani 1 1 d . . . . .
I3 I 0.42776(3) 0.35074(8) 0.71818(3) 0.0489(3) Uani 0.793(5) 1 d . . . A 1
Pb2 Pb 0.5000 0.17488(13) 0.7500 0.0420(3) Uani 0.793(5) 2 d S T P A 1
I1D I 0.2495(3) 0.1372(5) 0.2045(2) 0.0876(13) Uani 0.207(5) 1 d . . . A 2
I2D I 0.4148(4) 0.1380(8) 0.2933(3) 0.0876(13) Uani 0.207(5) 1 d . . . A 2
Pb1D Pb 0.3324(3) 0.2762(6) 0.2500(2) 0.0658(19) Uani 0.207(5) 1 d . . . A 2
I3D I 0.4184(3) 0.3672(4) 0.7027(2) 0.0876(13) Uani 0.207(5) 1 d . . . A 2
Pb2D Pb 0.5000 0.2301(6) 0.7500 0.0601(11) Uani 0.207(5) 2 d S T P A 2
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'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 1 -1 0.0161 -0.0000 1.0000 -1.0000 -0.0050 0.0607 0.1160
0 -1 1 0.0161 0.0000 -1.0000 1.0000 0.0050 -0.0607 -0.1160
15 1 8 0.0403 15.2977 1.1844 8.2323 0.1008 -0.8846 0.4553
-15 -1 -8 0.0198 -15.2857 -0.8992 -8.4951 -0.1027 0.9007 -0.4221
3 -3 -19 0.0040 3.3929 -3.4961 -19.1090 0.9383 0.2784 -0.2052
-3 3 19 0.0040 -3.3929 3.4961 19.1090 -0.9383 -0.2784 0.2052
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
N1B C1B C2B 122.8(7) . .
N1A C1A C2A 122.7(7) . .
C3A C2A C1A 118.7(7) . .
C1B C2B C3B 118.9(7) . .
C2A C3A C4A 119.8(7) . .
C2B C3B C4B 119.1(7) . .
C3A C4A C5A 117.9(6) . .
C3A C4A C12A 122.2(6) . .
C5A C4A C12A 119.9(6) . .
C3B C4B C5B 117.5(7) . .
C3B C4B C12B 121.4(6) . .
C5B C4B C12B 121.1(6) . .
C4A C5A C6A 119.2(6) . .
N1A C5A C4A 122.0(6) . .
N1A C5A C6A 118.8(6) . .
C4B C5B C6B 118.7(6) . .
N1B C5B C4B 122.7(6) . .
N1B C5B C6B 118.6(6) . .
C7A C6A C5A 121.5(6) . .
N2A C6A C5A 116.8(6) . .
N2A C6A C7A 121.7(6) . .
C7B C6B C5B 121.5(6) . .
N2B C6B C5B 116.8(6) . .
N2B C6B C7B 121.7(6) . .
C6A C7A C11A 119.9(6) . .
C8A C7A C6A 119.0(6) . .
C8A C7A C11A 121.1(6) . .
C6B C7B C11B 119.6(6) . .
C8B C7B C6B 118.6(6) . .
C8B C7B C11B 121.8(6) . .
C7A C8A C9A 119.6(6) . .
C9B C8B C7B 120.0(6) . .
C8A C9A C10A 117.9(6) . .
C8B C9B C10B 118.2(6) . .
N2A C10A C9A 123.5(6) . .
N2B C10B C9B 123.0(6) . .
C12A C11A C7A 119.1(6) . .
N4A C11A C7A 118.8(6) . .
N4A C11A C12A 122.1(6) . .
C12B C11B C7B 119.1(6) . .
N4B C11B C7B 118.0(6) . .
N4B C11B C12B 122.9(6) . .
C11A C12A C4A 120.2(6) . .
N3A C12A C4A 117.7(6) . .
N3A C12A C11A 122.1(6) . .
C11B C12B C4B 119.8(6) . .
N3B C12B C4B 118.4(7) . .
N3B C12B C11B 121.8(7) . .
C14A C13A C18A 118.9(7) . .
C14A C13A C22A 122.1(8) . .
C18A C13A C22A 119.0(7) . .
C14B C13B C18B 119.6(8) . .
C14B C13B C22B 120.4(9) . .
C18B C13B C22B 120.0(8) . .
C15A C14A C13A 121.0(7) . .
C15B C14B C13B 119.4(9) . .
C14A C15A C16A 119.7(6) . .
N4A C15A C14A 119.5(6) . .
N4A C15A C16A 120.8(6) . .
C14B C15B C16B 120.8(7) . .
N4B C15B C14B 118.7(8) . .
N4B C15B C16B 120.6(7) . .
C17A C16A C15A 118.7(7) . .
N3A C16A C15A 121.8(6) . .
N3A C16A C17A 119.4(7) . .
C17B C16B C15B 118.7(7) . .
N3B C16B C15B 121.8(6) . .
N3B C16B C17B 119.5(8) . .
C18A C17A C16A 121.4(7) . .
C18B C17B C16B 120.5(9) . .
C13A C18A C19A 118.4(7) . .
C17A C18A C13A 120.2(6) . .
C17A C18A C19A 121.4(7) . .
C13B C18B C19B 117.5(9) . .
C17B C18B C13B 121.0(7) . .
C17B C18B C19B 121.6(10) . .
C20A C19A C18A 120.7(8) . .
C20B C19B C18B 120.9(10) . .
C19A C20A C21A 120.7(7) . .
C19B C20B C21B 121.1(8) . .
C22A C21A C20A 121.1(8) . .
C22B C21B C20B 121.2(9) . .
C21A C22A C13A 120.1(9) . .
C21B C22B C13B 119.4(10) . .
C1A N1A Pb1 121.1(5) . .
C1A N1A Pb1D 123.5(5) . .
C5A N1A C1A 118.9(6) . .
C5A N1A Pb1 117.2(4) . .
C5A N1A Pb1D 116.3(4) . .
C1B N1B Pb1 122.0(5) . .
C1B N1B Pb1D 126.4(5) . .
C5B N1B C1B 118.9(6) . .
C5B N1B Pb1 118.0(4) . .
C5B N1B Pb1D 114.1(5) . .
C6A N2A Pb1 119.1(4) . .
C6A N2A Pb1D 121.8(4) . .
C10A N2A C6A 118.4(6) . .
C10A N2A Pb1 120.0(4) . .
C10A N2A Pb1D 118.7(5) . .
C6B N2B Pb1 120.6(4) . .
C6B N2B Pb1D 119.9(5) . .
C10B N2B C6B 118.5(6) . .
C10B N2B Pb1 120.1(4) . .
C10B N2B Pb1D 121.2(5) . .
C12A N3A C16A 116.0(6) . .
C12B N3B C16B 116.6(7) . .
C11A N4A C15A 117.0(6) . .
C11B N4B C15B 116.2(7) . .
N1A Pb1 I1 107.47(12) . .
N1A Pb1 I2 94.08(13) . .
N1B Pb1 N1A 142.05(18) . .
N1B Pb1 I1 89.47(13) . .
N1B Pb1 I2 104.68(13) . .
N2A Pb1 N1A 62.94(17) . .
N2A Pb1 N1B 87.85(17) . .
N2A Pb1 I1 80.46(12) . .
N2A Pb1 I2 152.37(13) . .
N2B Pb1 N1A 88.31(17) . .
N2B Pb1 N1B 63.33(17) . .
N2B Pb1 N2A 83.44(17) . .
N2B Pb1 I1 148.83(13) . .
N2B Pb1 I2 80.61(12) . .
I1 Pb1 I2 123.36(4) . .
N1C C1C C2C 124.9(7) . .
C1C C2C C3C 116.5(8) . .
C2C C3C C4C 120.4(8) . .
C3C C4C C12C 120.8(7) . .
C5C C4C C3C 118.8(7) . .
C5C C4C C12C 120.3(7) . .
C4C C5C C6C 121.2(7) . .
N1C C5C C4C 122.0(7) . .
N1C C5C C6C 116.8(7) . .
C7C C6C C5C 119.6(7) . .
N2C C6C C5C 118.0(7) . .
N2C C6C C7C 122.3(7) . .
C6C C7C C11C 120.3(7) . .
C8C C7C C6C 118.3(8) . .
C8C C7C C11C 121.4(7) . .
C9C C8C C7C 119.9(8) . .
C8C C9C C10C 118.3(8) . .
N2C C10C C9C 122.3(9) . .
C12C C11C C7C 120.6(7) . .
N4C C11C C7C 118.7(7) . .
N4C C11C C12C 120.7(7) . .
C11C C12C C4C 117.7(7) . .
N3C C12C C4C 118.8(7) . .
N3C C12C C11C 123.4(7) . .
C14C C13C C18C 121.2(7) . .
C14C C13C C22C 120.5(7) . .
C18C C13C C22C 118.3(7) . .
C13C C14C C15C 120.0(7) . .
C14C C15C C16C 119.1(7) . .
N4C C15C C14C 119.1(7) . .
N4C C15C C16C 121.8(7) . .
C17C C16C C15C 120.7(7) . .
N3C C16C C15C 120.4(7) . .
N3C C16C C17C 119.0(7) . .
C16C C17C C18C 120.3(7) . .
C13C C18C C19C 119.3(7) . .
C17C C18C C13C 118.6(8) . .
C17C C18C C19C 122.1(7) . .
C20C C19C C18C 120.1(8) . .
C19C C20C C21C 121.1(9) . .
C22C C21C C20C 120.6(8) . .
C21C C22C C13C 120.7(8) . .
C1C N1C C5C 117.3(7) . .
C1C N1C Pb2 121.2(5) . .
C1C N1C Pb2D 122.8(5) . .
C5C N1C Pb2 120.6(5) . .
C5C N1C Pb2D 119.8(5) . .
C6C N2C Pb2 121.9(5) . .
C6C N2C Pb2D 131.0(5) . .
C10C N2C C6C 118.7(7) . .
C10C N2C Pb2 118.8(6) . .
C10C N2C Pb2D 110.1(6) . .
C12C N3C C16C 116.6(7) . .
C11C N4C C15C 117.0(6) . .
N1C Pb2 N1C 119.5(3) 2_656 .
N1C Pb2 I3 81.08(13) . .
N1C Pb2 I3 81.08(13) 2_656 2_656
N1C Pb2 I3 151.56(14) 2_656 .
N1C Pb2 I3 151.56(14) . 2_656
N2C Pb2 N1C 114.8(2) . 2_656
N2C Pb2 N1C 114.8(2) 2_656 .
N2C Pb2 N1C 60.5(2) . .
N2C Pb2 N1C 60.5(2) 2_656 2_656
N2C Pb2 N2C 171.7(3) 2_656 .
N2C Pb2 I3 92.03(14) . .
N2C Pb2 I3 92.03(14) 2_656 2_656
N2C Pb2 I3 93.96(15) . 2_656
N2C Pb2 I3 93.96(15) 2_656 .
I3 Pb2 I3 88.05(5) . 2_656
N1A Pb1D I1D 105.4(3) . .
N1A Pb1D I2D 91.8(3) . .
N1B Pb1D N1A 151.6(4) . .
N1B Pb1D N2A 93.2(3) . .
N1B Pb1D I1D 88.0(3) . .
N1B Pb1D I2D 106.5(3) . .
N2A Pb1D N1A 64.0(2) . .
N2A Pb1D I1D 84.7(3) . .
N2A Pb1D I2D 154.2(4) . .
N2B Pb1D N1A 93.3(3) . .
N2B Pb1D N1B 69.0(3) . .
N2B Pb1D N2A 90.7(3) . .
N2B Pb1D I1D 156.3(4) . .
N2B Pb1D I2D 81.4(3) . .
I2D Pb1D I1D 111.9(4) . .
N1C Pb2D N1C 97.4(3) 2_656 .
N1C Pb2D I3D 77.72(17) . .
N1C Pb2D I3D 160.05(17) 2_656 .
N1C Pb2D I3D 77.72(17) 2_656 2_656
N1C Pb2D I3D 160.05(17) . 2_656
N2C Pb2D N1C 54.2(2) . .
N2C Pb2D N1C 54.2(2) 2_656 2_656
N2C Pb2D N1C 99.7(3) . 2_656
N2C Pb2D N1C 99.7(3) 2_656 .
N2C Pb2D N2C 143.2(4) 2_656 .
N2C Pb2D I3D 93.06(17) . .
N2C Pb2D I3D 107.11(19) 2_656 .
N2C Pb2D I3D 107.11(19) . 2_656
N2C Pb2D I3D 93.06(17) 2_656 2_656
I3D Pb2D I3D 113.1(4) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1B C2B 1.381(10) .
C1B N1B 1.341(9) .
C1A C2A 1.396(10) .
C1A N1A 1.334(9) .
C2A C3A 1.367(11) .
C2B C3B 1.386(11) .
C3A C4A 1.391(10) .
C3B C4B 1.402(10) .
C4A C5A 1.415(9) .
C4A C12A 1.467(10) .
C4B C5B 1.414(9) .
C4B C12B 1.446(10) .
C5A C6A 1.461(9) .
C5A N1A 1.332(9) .
C5B C6B 1.463(9) .
C5B N1B 1.325(9) .
C6A C7A 1.401(9) .
C6A N2A 1.367(8) .
C6B C7B 1.400(9) .
C6B N2B 1.359(8) .
C7A C8A 1.384(9) .
C7A C11A 1.464(8) .
C7B C8B 1.383(10) .
C7B C11B 1.470(9) .
C8A C9A 1.390(9) .
C8B C9B 1.379(9) .
C9A C10A 1.404(10) .
C9B C10B 1.398(10) .
C10A N2A 1.326(9) .
C10B N2B 1.333(8) .
C11A C12A 1.433(9) .
C11A N4A 1.322(9) .
C11B C12B 1.437(10) .
C11B N4B 1.312(9) .
C12A N3A 1.341(8) .
C12B N3B 1.327(9) .
C13A C14A 1.407(9) .
C13A C18A 1.426(11) .
C13A C22A 1.426(11) .
C13B C14B 1.410(10) .
C13B C18B 1.420(13) .
C13B C22B 1.433(12) .
C14A C15A 1.404(10) .
C14B C15B 1.403(11) .
C15A C16A 1.432(10) .
C15A N4A 1.366(8) .
C15B C16B 1.434(11) .
C15B N4B 1.378(9) .
C16A C17A 1.406(9) .
C16A N3A 1.361(9) .
C16B C17B 1.408(10) .
C16B N3B 1.353(10) .
C17A C18A 1.390(11) .
C17B C18B 1.384(13) .
C18A C19A 1.438(9) .
C18B C19B 1.448(11) .
C19A C20A 1.352(12) .
C19B C20B 1.354(14) .
C20A C21A 1.406(13) .
C20B C21B 1.393(15) .
C21A C22A 1.368(11) .
C21B C22B 1.374(12) .
N1A Pb1 2.628(6) .
N1A Pb1D 2.642(9) .
N1B Pb1 2.615(6) .
N1B Pb1D 2.473(9) .
N2A Pb1 2.584(6) .
N2A Pb1D 2.490(9) .
N2B Pb1 2.547(5) .
N2B Pb1D 2.306(10) .
I1 Pb1 3.2163(15) .
I2 Pb1 3.2320(16) .
C1C C2C 1.381(12) .
C1C N1C 1.339(10) .
C2C C3C 1.385(11) .
C3C C4C 1.394(11) .
C4C C5C 1.373(11) .
C4C C12C 1.484(10) .
C5C C6C 1.465(10) .
C5C N1C 1.367(9) .
C6C C7C 1.394(10) .
C6C N2C 1.359(10) .
C7C C8C 1.393(11) .
C7C C11C 1.450(12) .
C8C C9C 1.372(13) .
C9C C10C 1.422(12) .
C10C N2C 1.325(11) .
C11C C12C 1.433(10) .
C11C N4C 1.331(9) .
C12C N3C 1.304(10) .
C13C C14C 1.390(12) .
C13C C18C 1.422(11) .
C13C C22C 1.446(10) .
C14C C15C 1.404(10) .
C15C C16C 1.425(10) .
C15C N4C 1.352(10) .
C16C C17C 1.391(11) .
C16C N3C 1.373(9) .
C17C C18C 1.409(10) .
C18C C19C 1.424(12) .
C19C C20C 1.365(11) .
C20C C21C 1.415(12) .
C21C C22C 1.345(12) .
N1C Pb2 2.719(7) .
N1C Pb2D 3.127(9) .
N2C Pb2 2.682(7) .
N2C Pb2D 2.819(7) .
I3 Pb2 3.0746(9) .
Pb2 N1C 2.719(7) 2_656
Pb2 N2C 2.682(7) 2_656
Pb2 I3 3.0747(10) 2_656
I1D Pb1D 3.135(9) .
I2D Pb1D 3.089(12) .
I3D Pb2D 3.128(6) .
Pb2D N1C 3.127(9) 2_656
Pb2D N2C 2.819(7) 2_656
Pb2D I3D 3.128(6) 2_656
