#------------------------------------------------------------------------------
#$Date: 2020-09-10 01:24:50 +0300 (Thu, 10 Sep 2020) $
#$Revision: 256268 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/36/4003672.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_4003672
loop_
_publ_author_name
'Petrov, Andrey A.'
'Fateev, Sergey A.'
'Khrustalev, Victor N.'
'Li, Yumao'
'Dorovatovskii, Pavel V.'
'Zubavichus, Yan V.'
'Goodilin, Eugene A.'
'Tarasov, Alexey B.'
_publ_section_title
;
 Formamidinium Haloplumbate Intermediates: The Missing Link in a Chain of
 Hybrid Perovskites Crystallization
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c02156
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         '15(C H5 N2), 3(I9 Pb2)'
_chemical_formula_sum            'C15 H75 I27 N30 Pb6'
_chemical_formula_weight         5345.55
_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_Hall           'P -6'
_space_group_name_H-M_alt        'P -6'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   26.770(3)
_cell_length_b                   26.770(3)
_cell_length_c                   14.860(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      3.3
_cell_volume                     9222.4(19)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80246
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79929
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         30.867
_diffrn_reflns_theta_min         3.251
_exptl_absorpt_coefficient_mu    18.942
_exptl_absorpt_correction_T_max  0.555
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.888
_exptl_crystal_description       prism
_exptl_crystal_F_000             6894
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.532
_refine_diff_density_min         -3.757
_refine_diff_density_rms         0.404
_refine_ls_abs_structure_details
;
 Flack x determined using 3773 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.012(6)
_refine_ls_extinction_coef       0.00014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         13829
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.1230
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.01P)²+600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2654
_refine_ls_wR_factor_ref         0.2866
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                10126
_reflns_number_total             13829
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm0c02156_si_003.cif
_cod_data_source_block           FA5Pb2I9
_cod_original_cell_volume        9222(3)
_cod_database_code               4003672
_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   0.251
_shelx_estimated_absorpt_t_max   0.598
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -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 0.32641(17) 0.98844(15) 0.3614(2) 0.0594(8) Uani 1 1 d . . . . .
I1 I 0.4327(3) 1.0402(3) 0.2277(4) 0.0857(8) Uani 1 1 d . . . . .
I2 I 0.2676(3) 0.8813(3) 0.2305(5) 0.0857(8) Uani 1 1 d . . . . .
I3 I 0.2748(3) 1.0524(3) 0.2485(4) 0.0857(8) Uani 1 1 d . . . . .
I4 I 0.2143(4) 0.9362(3) 0.5000 0.0857(8) Uani 1 2 d S T P . .
I5 I 0.3912(4) 1.0992(4) 0.5000 0.0857(8) Uani 1 2 d S T P . .
I6 I 0.3785(4) 0.9290(4) 0.5000 0.0857(8) Uani 1 2 d S T P . .
Pb2 Pb 0.67170(18) 0.01142(14) 0.3622(2) 0.0612(8) Uani 1 1 d . . . . .
I7 I 0.6076(3) 0.0602(3) 0.2473(6) 0.0994(10) Uani 1 1 d . . . . .
I8 I 0.7766(3) 0.0655(3) 0.2336(5) 0.0994(10) Uani 1 1 d . . . . .
I9 I 0.6161(3) -0.1006(3) 0.2473(6) 0.0994(10) Uani 1 1 d . . . . .
I10 I 0.7364(4) -0.0347(4) 0.5000 0.0994(10) Uani 1 2 d S T P . .
I11 I 0.5607(4) -0.0508(4) 0.5000 0.0994(10) Uani 1 2 d S T P . .
I12 I 0.7253(4) 0.1238(4) 0.5000 0.0994(10) Uani 1 2 d S T P . .
Pb3 Pb 0.0000 0.0000 0.1415(5) 0.0601(13) Uani 1 3 d S T P . .
I13 I 0.1117(2) 0.0671(3) 0.2588(5) 0.0900(17) Uani 1 1 d . . . . .
I14 I 0.0493(4) 0.1108(4) 0.0000 0.0900(17) Uani 1 2 d S T P . .
Pb4 Pb 0.6667 0.3333 0.1384(5) 0.0595(16) Uani 1 3 d S T P . .
I15 I 0.5944(3) 0.2220(2) 0.2574(5) 0.0815(14) Uani 1 1 d . . . . .
I16 I 0.7107(4) 0.2668(3) 0.0000 0.0815(14) Uani 1 2 d S T P . .
Pb5 Pb 0.3333 0.6667 0.1401(5) 0.0682(18) Uani 1 3 d S T P . .
I17 I 0.2683(4) 0.7124(5) 0.2565(6) 0.116(3) Uani 1 1 d . . . . .
I18 I 0.2234(5) 0.6016(6) 0.0000 0.116(3) Uani 1 2 d S T P . .
N1 N 0.244(3) 0.449(2) 0.07840(14) 0.102(10) Uani 1 1 d D . . . .
H1A H 0.2274 0.4109 0.0821 0.122 Uiso 1 1 d R U . . .
H1B H 0.2527 0.4696 0.1277 0.122 Uiso 1 1 d R U . . .
C1 C 0.254(5) 0.473(2) 0.0000 0.102(10) Uani 1 2 d DS T P . .
H1 H 0.2704 0.5142 0.0000 0.122 Uiso 1 2 calc R U P . .
N2 N 0.7236(18) 0.201(2) 0.243(5) 0.102(10) Uani 1 1 d D . . . .
H2A H 0.7221 0.2328 0.2409 0.122 Uiso 1 1 d R U . . .
H2B H 0.6921 0.1673 0.2347 0.122 Uiso 1 1 d R U . . .
N3 N 0.8214(18) 0.250(2) 0.279(5) 0.102(10) Uani 1 1 d D . . . .
H3A H 0.8246 0.2845 0.2783 0.122 Uiso 1 1 d R U . . .
H3B H 0.8520 0.2468 0.2893 0.122 Uiso 1 1 d R U . . .
C2 C 0.772(2) 0.2038(15) 0.264(6) 0.102(10) Uani 1 1 d D . . . .
H2 H 0.7716 0.1681 0.2696 0.122 Uiso 1 1 calc R U . . .
N4 N 0.881(3) 0.208(3) 0.0000 0.102(10) Uani 0.5 2 d DS T P A 1
H4A H 0.9153 0.2388 0.0000 0.122 Uiso 0.5 2 d R U P A 1
H4B H 0.8766 0.1734 0.0000 0.122 Uiso 0.5 2 d R U P A 1
N5 N 0.840(4) 0.267(3) 0.0000 0.102(10) Uani 0.5 2 d DS T P A 1
H5A H 0.8726 0.3008 0.0000 0.122 Uiso 0.5 2 d R U P A 1
H5B H 0.8069 0.2667 0.0000 0.122 Uiso 0.5 2 d R U P A 1
C3 C 0.838(3) 0.218(2) 0.0000 0.102(10) Uani 0.5 2 d DS T P A 1
H3 H 0.8001 0.1847 0.0000 0.122 Uiso 0.5 2 calc R U P A 1
N4' N 0.879(5) 0.256(3) 0.0000 0.102(10) Uani 0.5 2 d DS T P B 2
H4C H 0.9123 0.2563 0.0000 0.122 Uiso 0.5 2 d R U P B 2
H4D H 0.8785 0.2883 0.0000 0.122 Uiso 0.5 2 d R U P B 2
N5' N 0.825(6) 0.155(3) 0.0000 0.102(10) Uani 0.5 2 d DS T P B 2
H5C H 0.8557 0.1511 0.0000 0.122 Uiso 0.5 2 d R U P B 2
H5D H 0.7904 0.1248 0.0000 0.122 Uiso 0.5 2 d R U P B 2
C3' C 0.831(4) 0.207(3) 0.0000 0.102(10) Uani 0.5 2 d DS T P B 2
H3' H 0.7966 0.2083 0.0000 0.122 Uiso 0.5 2 calc R U P B 2
N6 N 0.807(3) -0.110(4) 0.292(9) 0.102(10) Uani 0.5 1 d D . P C 1
H6A H 0.8189 -0.0971 0.3467 0.122 Uiso 0.5 1 d R U P C 1
H6B H 0.8286 -0.1180 0.2564 0.122 Uiso 0.5 1 d R U P C 1
N7 N 0.724(3) -0.104(4) 0.308(8) 0.102(10) Uani 0.5 1 d D . P C 1
H7A H 0.7313 -0.0911 0.3639 0.122 Uiso 0.5 1 d R U P C 1
H7B H 0.6913 -0.1108 0.2825 0.122 Uiso 0.5 1 d R U P C 1
C4 C 0.758(3) -0.116(4) 0.264(6) 0.102(10) Uani 0.5 1 d D . P C 1
H4 H 0.7467 -0.1309 0.2051 0.122 Uiso 0.5 1 calc R U P C 1
N6' N 0.749(3) -0.039(3) 0.288(8) 0.102(10) Uani 0.5 1 d D . P D 2
H6C H 0.7124 -0.0667 0.2832 0.122 Uiso 0.5 1 d R U P D 2
H6D H 0.7567 -0.0047 0.3074 0.122 Uiso 0.5 1 d R U P D 2
N7' N 0.783(4) -0.099(3) 0.238(9) 0.102(10) Uani 0.5 1 d D . P D 2
H7C H 0.7482 -0.1295 0.2309 0.122 Uiso 0.5 1 d R U P D 2
H7D H 0.8137 -0.1013 0.2264 0.122 Uiso 0.5 1 d R U P D 2
C4' C 0.789(3) -0.050(2) 0.263(10) 0.102(10) Uani 0.5 1 d D . P D 2
H4' H 0.8271 -0.0179 0.2630 0.122 Uiso 0.5 1 calc R U P D 2
N8 N 0.872(3) 0.111(2) 0.42161(14) 0.102(10) Uani 1 1 d D . . . .
H8A H 0.8626 0.0742 0.4179 0.122 Uiso 1 1 d R U . . .
H8B H 0.8778 0.1311 0.3723 0.122 Uiso 1 1 d R U . . .
C5 C 0.882(5) 0.135(2) 0.5000 0.102(10) Uani 1 2 d DS T P . .
H5 H 0.8969 0.1760 0.5000 0.122 Uiso 1 2 calc R U P . .
N9 N 0.891(2) 0.7820(15) 0.07840(14) 0.056(7) Uani 1 1 d D . . . .
H9A H 0.8727 0.7441 0.0822 0.068 Uiso 1 1 d R U . . .
H9B H 0.9019 0.8030 0.1277 0.068 Uiso 1 1 d R U . . .
C6 C 0.902(3) 0.8068(15) 0.0000 0.056(7) Uani 1 2 d DS T P . .
H6 H 0.9194 0.8477 0.0000 0.068 Uiso 1 2 calc R U P . .
N10 N 0.530(4) 0.100(3) 0.42261(14) 0.056(7) Uani 0.5 1 d D . P . .
H10A H 0.5123 0.1208 0.4203 0.068 Uiso 0.5 1 d R U P . .
H10B H 0.5387 0.0892 0.3725 0.068 Uiso 0.5 1 d R U P . .
C7 C 0.539(5) 0.084(4) 0.5000 0.056(7) Uani 0.5 2 d DS T P . .
H7 H 0.5540 0.0583 0.5000 0.068 Uiso 0.5 2 calc R U P . .
N11 N 0.392(2) 0.858(3) 0.262(7) 0.056(7) Uani 0.5 1 d D . P . .
H11A H 0.3809 0.8810 0.2843 0.068 Uiso 0.5 1 d R U P . .
H11B H 0.3671 0.8256 0.2350 0.068 Uiso 0.5 1 d R U P . .
N12 N 0.489(2) 0.920(2) 0.281(6) 0.056(7) Uani 0.5 1 d D . P . .
H12A H 0.4808 0.9448 0.3050 0.068 Uiso 0.5 1 d R U P . .
H12B H 0.5248 0.9262 0.2842 0.068 Uiso 0.5 1 d R U P . .
C8 C 0.446(2) 0.872(3) 0.251(7) 0.056(7) Uani 0.5 1 d D . P . .
H8 H 0.4541 0.8466 0.2189 0.068 Uiso 0.5 1 calc R U P . .
N13 N 0.595(4) 0.812(3) 0.42261(14) 0.056(7) Uani 0.5 1 d D . P E 1
H13A H 0.6137 0.8497 0.4203 0.068 Uiso 0.5 1 d R U P E 1
H13B H 0.5847 0.7915 0.3725 0.068 Uiso 0.5 1 d R U P E 1
C9 C 0.585(7) 0.786(3) 0.5000 0.056(7) Uani 0.5 2 d DS T P E 1
H9 H 0.5690 0.7452 0.5000 0.068 Uiso 0.5 2 calc R U P E 1
N14 N 0.640(4) 0.038(2) 0.0000 0.056(7) Uani 0.5 2 d DS T P F 3
H14A H 0.6632 0.0233 0.0000 0.068 Uiso 0.5 2 d R U P F 3
H14B H 0.6026 0.0153 0.0000 0.068 Uiso 0.5 2 d R U P F 3
N15 N 0.719(3) 0.130(3) 0.0000 0.056(7) Uani 0.5 2 d DS T P F 3
H15A H 0.7442 0.1178 0.0000 0.068 Uiso 0.5 2 d R U P F 3
H15B H 0.7311 0.1670 0.0000 0.068 Uiso 0.5 2 d R U P F 3
C10 C 0.664(3) 0.094(2) 0.0000 0.056(7) Uani 0.5 2 d DS T P F 3
H10 H 0.6388 0.1097 0.0000 0.068 Uiso 0.5 2 calc R U P F 3
N16 N 0.1428(18) 0.8683(16) 0.0000 0.056(7) Uani 1 2 d DS T P . .
H16A H 0.1315 0.8940 0.0000 0.068 Uiso 1 2 d R U P . .
H16B H 0.1798 0.8796 0.0000 0.068 Uiso 1 2 d R U P . .
N17 N 0.0498(16) 0.7917(19) 0.0000 0.056(7) Uani 1 2 d DS T P . .
H17A H 0.0357 0.8152 0.0000 0.068 Uiso 1 2 d R U P . .
H17B H 0.0264 0.7541 0.0000 0.068 Uiso 1 2 d R U P . .
C11 C 0.1054(17) 0.8134(14) 0.0000 0.110(16) Uani 1 2 d DS T P . .
H11 H 0.1197 0.7873 0.0000 0.132 Uiso 1 2 calc R U P . .
N18 N 0.5572(16) 0.1174(17) 0.07739(14) 0.110(16) Uani 1 1 d D . . . .
H18A H 0.5442 0.0801 0.0796 0.132 Uiso 1 1 d R U . . .
H18B H 0.5641 0.1373 0.1275 0.132 Uiso 1 1 d R U . . .
C12 C 0.564(3) 0.1428(18) 0.0000 0.110(16) Uani 1 2 d DS T P . .
H12 H 0.5755 0.1826 0.0000 0.132 Uiso 1 2 calc R U P . .
N19 N 0.389(4) 0.594(2) 0.5000 0.110(16) Uani 0.5 2 d DS T P G 2
H19A H 0.4133 0.5808 0.5000 0.132 Uiso 0.5 2 d R U P G 2
H19B H 0.3514 0.5692 0.5000 0.132 Uiso 0.5 2 d R U P G 2
N20 N 0.461(3) 0.689(3) 0.5000 0.110(16) Uani 0.5 2 d DS T P G 2
H20A H 0.4879 0.6785 0.5000 0.132 Uiso 0.5 2 d R U P G 2
H20B H 0.4714 0.7253 0.5000 0.132 Uiso 0.5 2 d R U P G 2
C13 C 0.407(2) 0.649(2) 0.5000 0.110(16) Uani 0.5 2 d DS T P G 2
H13 H 0.3792 0.6607 0.5000 0.132 Uiso 0.5 2 calc R U P G 2
N21 N -0.040(2) 0.467(4) 0.0000 0.110(16) Uani 0.5 2 d DS T P H 1
H21A H -0.0599 0.4293 0.0000 0.132 Uiso 0.5 2 d R U P H 1
H21B H -0.0589 0.4867 0.0000 0.132 Uiso 0.5 2 d R U P H 1
N22 N 0.046(2) 0.469(3) 0.0000 0.110(16) Uani 0.5 2 d DS T P H 1
H22A H 0.0294 0.4309 0.0000 0.132 Uiso 0.5 2 d R U P H 1
H22B H 0.0842 0.4898 0.0000 0.132 Uiso 0.5 2 d R U P H 1
C14 C 0.016(2) 0.494(2) 0.0000 0.110(16) Uani 0.5 2 d DS T P H 1
H14 H 0.0355 0.5351 0.0000 0.132 Uiso 0.5 2 calc R U P H 1
N23 N 0.866(3) 0.947(3) 0.5000 0.110(16) Uani 0.5 2 d DS T P . .
H23A H 0.8286 0.9220 0.5000 0.132 Uiso 0.5 2 d R U P . .
H23B H 0.8774 0.9846 0.5000 0.132 Uiso 0.5 2 d R U P . .
N24 N 0.889(3) 0.876(2) 0.5000 0.110(16) Uani 0.5 2 d DS T P . .
H24A H 0.8531 0.8483 0.5000 0.132 Uiso 0.5 2 d R U P . .
H24B H 0.9170 0.8671 0.5000 0.132 Uiso 0.5 2 d R U P . .
C15 C 0.903(2) 0.930(2) 0.5000 0.110(16) Uani 0.5 2 d DS T P . .
H15 H 0.9428 0.9582 0.5000 0.132 Uiso 0.5 2 calc R U P . .
N25 N -0.0112(17) 0.5302(16) 0.0000 0.110(16) Uani 1 2 d DS T P I 2
H25A H 0.0063 0.5097 0.0000 0.132 Uiso 1 2 d R U P I 2
H25B H -0.0491 0.5127 0.0000 0.132 Uiso 1 2 d R U P I 2
N26 N 0.0764(15) 0.6143(18) 0.0000 0.110(16) Uani 1 2 d DS T P I 2
H26A H 0.0963 0.5963 0.0000 0.132 Uiso 1 2 d R U P I 2
H26B H 0.0944 0.6523 0.0000 0.132 Uiso 1 2 d R U P I 2
C16 C 0.0203(15) 0.5861(16) 0.0000 0.110(16) Uani 1 2 d DS T P I 2
H16 H 0.0010 0.6078 0.0000 0.132 Uiso 1 2 calc R U P I 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0050 0.0020 '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 0.0090 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.2582 2.2555 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -7.4040 10.6371 '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
I2 Pb1 I1 86.67(17) . . ?
I2 Pb1 I3 90.60(17) . . ?
I1 Pb1 I3 88.32(19) . . ?
I2 Pb1 I5 178.0(2) . . ?
I1 Pb1 I5 92.54(18) . . ?
I3 Pb1 I5 91.19(19) . . ?
I2 Pb1 I6 94.90(18) . . ?
I1 Pb1 I6 95.64(19) . . ?
I3 Pb1 I6 173.40(19) . . ?
I5 Pb1 I6 83.37(18) . . ?
I2 Pb1 I4 93.70(19) . . ?
I1 Pb1 I4 178.8(2) . . ?
I3 Pb1 I4 90.5(2) . . ?
I5 Pb1 I4 87.12(19) . . ?
I6 Pb1 I4 85.5(2) . . ?
Pb1 I4 Pb1 76.7(2) 4_556 . ?
Pb1 I5 Pb1 77.2(2) 4_556 . ?
Pb1 I6 Pb1 77.0(2) . 4_556 ?
I8 Pb2 I9 89.8(2) . . ?
I8 Pb2 I7 91.5(2) . . ?
I9 Pb2 I7 90.3(2) . . ?
I8 Pb2 I11 177.7(2) . . ?
I9 Pb2 I11 88.8(2) . . ?
I7 Pb2 I11 90.3(2) . . ?
I8 Pb2 I10 92.0(2) . . ?
I9 Pb2 I10 93.9(2) . . ?
I7 Pb2 I10 174.6(2) . . ?
I11 Pb2 I10 86.3(2) . . ?
I8 Pb2 I12 94.42(19) . . ?
I9 Pb2 I12 175.1(2) . . ?
I7 Pb2 I12 92.16(19) . . ?
I11 Pb2 I12 86.96(18) . . ?
I10 Pb2 I12 83.46(18) . . ?
Pb2 I10 Pb2 76.8(2) 4_556 . ?
Pb2 I11 Pb2 76.9(2) 4_556 . ?
Pb2 I12 Pb2 76.3(2) . 4_556 ?
I13 Pb3 I13 92.1(2) 3 2 ?
I13 Pb3 I13 92.1(2) 3 . ?
I13 Pb3 I13 92.1(2) 2 . ?
I13 Pb3 I14 90.06(17) 3 3 ?
I13 Pb3 I14 174.0(2) 2 3 ?
I13 Pb3 I14 93.41(19) . 3 ?
I13 Pb3 I14 174.0(2) 3 . ?
I13 Pb3 I14 93.41(19) 2 . ?
I13 Pb3 I14 90.06(17) . . ?
I14 Pb3 I14 84.2(2) 3 . ?
I13 Pb3 I14 93.41(19) 3 2 ?
I13 Pb3 I14 90.06(17) 2 2 ?
I13 Pb3 I14 174.0(3) . 2 ?
I14 Pb3 I14 84.2(2) 3 2 ?
I14 Pb3 I14 84.2(2) . 2 ?
Pb3 I14 Pb3 78.5(3) 4 . ?
I15 Pb4 I15 91.7(2) 2_655 . ?
I15 Pb4 I15 91.7(2) 2_655 3_665 ?
I15 Pb4 I15 91.7(2) . 3_665 ?
I15 Pb4 I16 89.72(17) 2_655 . ?
I15 Pb4 I16 93.19(14) . . ?
I15 Pb4 I16 174.8(2) 3_665 . ?
I15 Pb4 I16 93.19(14) 2_655 2_655 ?
I15 Pb4 I16 174.8(2) . 2_655 ?
I15 Pb4 I16 89.72(17) 3_665 2_655 ?
I16 Pb4 I16 85.25(18) . 2_655 ?
I15 Pb4 I16 174.8(2) 2_655 3_665 ?
I15 Pb4 I16 89.72(17) . 3_665 ?
I15 Pb4 I16 93.19(14) 3_665 3_665 ?
I16 Pb4 I16 85.25(18) . 3_665 ?
I16 Pb4 I16 85.25(18) 2_655 3_665 ?
Pb4 I16 Pb4 77.1(2) 4 . ?
I17 Pb5 I17 92.0(3) . 3_565 ?
I17 Pb5 I17 92.0(3) . 2_665 ?
I17 Pb5 I17 92.0(3) 3_565 2_665 ?
I17 Pb5 I18 91.5(2) . 3_565 ?
I17 Pb5 I18 91.8(2) 3_565 3_565 ?
I17 Pb5 I18 174.8(3) 2_665 3_565 ?
I17 Pb5 I18 91.8(2) . . ?
I17 Pb5 I18 174.8(3) 3_565 . ?
I17 Pb5 I18 91.5(2) 2_665 . ?
I18 Pb5 I18 84.5(2) 3_565 . ?
I17 Pb5 I18 174.8(3) . 2_665 ?
I17 Pb5 I18 91.5(2) 3_565 2_665 ?
I17 Pb5 I18 91.8(2) 2_665 2_665 ?
I18 Pb5 I18 84.5(2) 3_565 2_665 ?
I18 Pb5 I18 84.5(2) . 2_665 ?
Pb5 I18 Pb5 78.2(3) 4 . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
N1 C1 N1 127.3(7) 4 . ?
N1 C1 H1 116.4 4 . ?
N1 C1 H1 116.4 . . ?
C2 N2 H2A 118.8 . . ?
C2 N2 H2B 121.1 . . ?
H2A N2 H2B 120.0 . . ?
C2 N3 H3A 121.2 . . ?
C2 N3 H3B 118.8 . . ?
H3A N3 H3B 120.0 . . ?
N2 C2 N3 127.2(7) . . ?
N2 C2 H2 116.4 . . ?
N3 C2 H2 116.4 . . ?
C3 N4 H4A 116.2 . . ?
C3 N4 H4B 123.8 . . ?
H4A N4 H4B 120.0 . . ?
C3 N5 H5A 123.9 . . ?
C3 N5 H5B 116.1 . . ?
H5A N5 H5B 120.0 . . ?
N4 C3 N5 127.3(7) . . ?
N4 C3 H3 116.2 . . ?
N5 C3 H3 116.5 . . ?
C3' N4' H4C 119.7 . . ?
C3' N4' H4D 120.3 . . ?
H4C N4' H4D 120.0 . . ?
C3' N5' H5C 120.3 . . ?
C3' N5' H5D 119.7 . . ?
H5C N5' H5D 120.0 . . ?
N4' C3' N5' 127.3(7) . . ?
N4' C3' H3' 116.4 . . ?
N5' C3' H3' 116.3 . . ?
C4 N6 H6A 118.8 . . ?
C4 N6 H6B 121.2 . . ?
H6A N6 H6B 120.0 . . ?
C4 N7 H7A 121.2 . . ?
C4 N7 H7B 118.8 . . ?
H7A N7 H7B 120.0 . . ?
N7 C4 N6 127.3(7) . . ?
N7 C4 H4 116.3 . . ?
N6 C4 H4 116.3 . . ?
C4' N6' H6C 118.4 . . ?
C4' N6' H6D 121.5 . . ?
H6C N6' H6D 120.0 . . ?
C4' N7' H7C 121.3 . . ?
C4' N7' H7D 118.7 . . ?
H7C N7' H7D 120.0 . . ?
N7' C4' N6' 127.3(7) . . ?
N7' C4' H4' 116.4 . . ?
N6' C4' H4' 116.3 . . ?
C5 N8 H8A 119.8 . . ?
C5 N8 H8B 120.1 . . ?
H8A N8 H8B 120.0 . . ?
N8 C5 N8 127.3(7) . 4_556 ?
N8 C5 H5 116.4 . . ?
N8 C5 H5 116.4 4_556 . ?
C6 N9 H9A 119.9 . . ?
C6 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
N9 C6 N9 127.2(7) 4 . ?
N9 C6 H6 116.4 4 . ?
N9 C6 H6 116.4 . . ?
C7 N10 H10A 119.8 . . ?
C7 N10 H10B 120.1 . . ?
H10A N10 H10B 120.0 . . ?
N10 C7 N10 124.4(7) 4_556 . ?
N10 C7 H7 117.8 4_556 . ?
N10 C7 H7 117.8 . . ?
C8 N11 H11A 123.5 . . ?
C8 N11 H11B 115.2 . . ?
H11A N11 H11B 120.0 . . ?
C8 N12 H12A 115.9 . . ?
C8 N12 H12B 123.8 . . ?
H12A N12 H12B 120.0 . . ?
N12 C8 N11 124.4(7) . . ?
N12 C8 H8 117.8 . . ?
N11 C8 H8 117.9 . . ?
C9 N13 H13A 119.7 . . ?
C9 N13 H13B 120.1 . . ?
H13A N13 H13B 120.0 . . ?
N13 C9 N13 124.5(7) 4_556 . ?
N13 C9 H9 117.8 4_556 . ?
N13 C9 H9 117.8 . . ?
C10 N14 H14A 118.3 . . ?
C10 N14 H14B 121.7 . . ?
H14A N14 H14B 120.0 . . ?
C10 N15 H15A 121.7 . . ?
C10 N15 H15B 118.3 . . ?
H15A N15 H15B 120.0 . . ?
N14 C10 N15 124.5(7) . . ?
N14 C10 H10 117.8 . . ?
N15 C10 H10 117.8 . . ?
C11 N16 H16A 120.9 . . ?
C11 N16 H16B 119.1 . . ?
H16A N16 H16B 120.0 . . ?
C11 N17 H17A 119.1 . . ?
C11 N17 H17B 120.9 . . ?
H17A N17 H17B 120.0 . . ?
N17 C11 N16 124.5(7) . . ?
N17 C11 H11 117.7 . . ?
N16 C11 H11 117.8 . . ?
C12 N18 H18A 119.9 . . ?
C12 N18 H18B 120.1 . . ?
H18A N18 H18B 120.0 . . ?
N18 C12 N18 124.3(6) 4 . ?
N18 C12 H12 117.8 4 . ?
N18 C12 H12 117.8 . . ?
C13 N19 H19A 120.7 . . ?
C13 N19 H19B 119.3 . . ?
H19A N19 H19B 120.0 . . ?
C13 N20 H20A 119.3 . . ?
C13 N20 H20B 120.7 . . ?
H20A N20 H20B 120.0 . . ?
N20 C13 N19 124.4(7) . . ?
N20 C13 H13 117.8 . . ?
N19 C13 H13 117.8 . . ?
C14 N21 H21A 119.6 . . ?
C14 N21 H21B 120.4 . . ?
H21A N21 H21B 120.0 . . ?
C14 N22 H22A 120.4 . . ?
C14 N22 H22B 119.6 . . ?
H22A N22 H22B 120.0 . . ?
N21 C14 N22 124.5(7) . . ?
N21 C14 H14 117.8 . . ?
N22 C14 H14 117.8 . . ?
C15 N23 H23A 119.5 . . ?
C15 N23 H23B 120.5 . . ?
H23A N23 H23B 120.0 . . ?
C15 N24 H24A 120.5 . . ?
C15 N24 H24B 119.5 . . ?
H24A N24 H24B 120.0 . . ?
N23 C15 N24 124.4(7) . . ?
N23 C15 H15 117.8 . . ?
N24 C15 H15 117.8 . . ?
C16 N25 H25A 118.5 . . ?
C16 N25 H25B 121.5 . . ?
H25A N25 H25B 120.0 . . ?
C16 N26 H26A 121.5 . . ?
C16 N26 H26B 118.5 . . ?
H26A N26 H26B 120.0 . . ?
N26 C16 N25 124.3(6) . . ?
N26 C16 H16 117.8 . . ?
N25 C16 H16 117.8 . . ?
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
Pb1 I2 3.157(7) . ?
Pb1 I1 3.165(7) . ?
Pb1 I3 3.165(7) . ?
Pb1 I5 3.301(7) . ?
Pb1 I6 3.307(7) . ?
Pb1 I4 3.319(8) . ?
Pb2 I8 3.094(8) . ?
Pb2 I9 3.108(7) . ?
Pb2 I7 3.131(8) . ?
Pb2 I11 3.293(7) . ?
Pb2 I10 3.295(7) . ?
Pb2 I12 3.313(7) . ?
Pb3 I13 3.136(6) 2 ?
Pb3 I13 3.137(6) . ?
Pb3 I14 3.323(8) . ?
Pb4 I15 3.160(6) . ?
Pb4 I16 3.299(7) . ?
Pb5 I17 3.106(7) . ?
Pb5 I18 3.301(10) . ?
N1 C1 1.300(3) . ?
N1 H1A 0.8801 . ?
N1 H1B 0.8802 . ?
C1 N1 1.300(3) 4 ?
C1 H1 0.9500 . ?
N2 C2 1.300(4) . ?
N2 H2A 0.8799 . ?
N2 H2B 0.8800 . ?
N3 C2 1.300(4) . ?
N3 H3A 0.8798 . ?
N3 H3B 0.8802 . ?
C2 H2 0.9500 . ?
N4 C3 1.300(4) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8799 . ?
N5 C3 1.300(4) . ?
N5 H5A 0.8799 . ?
N5 H5B 0.8801 . ?
C3 H3 0.9500 . ?
N4' C3' 1.300(4) . ?
N4' H4C 0.8804 . ?
N4' H4D 0.8798 . ?
N5' C3' 1.300(4) . ?
N5' H5C 0.8799 . ?
N5' H5D 0.8799 . ?
C3' H3' 0.9500 . ?
N6 C4 1.300(4) . ?
N6 H6A 0.8799 . ?
N6 H6B 0.8800 . ?
N7 C4 1.300(4) . ?
N7 H7A 0.8802 . ?
N7 H7B 0.8802 . ?
C4 H4 0.9500 . ?
N6' C4' 1.300(4) . ?
N6' H6C 0.8801 . ?
N6' H6D 0.8799 . ?
N7' C4' 1.300(4) . ?
N7' H7C 0.8802 . ?
N7' H7D 0.8800 . ?
C4' H4' 0.9500 . ?
N8 C5 1.300(3) . ?
N8 H8A 0.8799 . ?
N8 H8B 0.8801 . ?
C5 N8 1.300(3) 4_556 ?
C5 H5 0.9500 . ?
N9 C6 1.301(3) . ?
N9 H9A 0.8800 . ?
N9 H9B 0.8800 . ?
C6 N9 1.301(3) 4 ?
C6 H6 0.9500 . ?
N10 C7 1.300(3) . ?
N10 H10A 0.8802 . ?
N10 H10B 0.8799 . ?
C7 N10 1.300(3) 4_556 ?
C7 H7 0.9500 . ?
N11 C8 1.300(5) . ?
N11 H11A 0.8804 . ?
N11 H11B 0.8798 . ?
N12 C8 1.300(4) . ?
N12 H12A 0.8801 . ?
N12 H12B 0.8800 . ?
C8 H8 0.9500 . ?
N13 C9 1.300(3) . ?
N13 H13A 0.8800 . ?
N13 H13B 0.8801 . ?
C9 N13 1.300(3) 4_556 ?
C9 H9 0.9500 . ?
N14 C10 1.300(4) . ?
N14 H14A 0.8799 . ?
N14 H14B 0.8801 . ?
N15 C10 1.300(4) . ?
N15 H15A 0.8802 . ?
N15 H15B 0.8802 . ?
C10 H10 0.9500 . ?
N16 C11 1.300(4) . ?
N16 H16A 0.8801 . ?
N16 H16B 0.8799 . ?
N17 C11 1.299(4) . ?
N17 H17A 0.8799 . ?
N17 H17B 0.8799 . ?
C11 H11 0.9500 . ?
N18 C12 1.301(3) . ?
N18 H18A 0.8799 . ?
N18 H18B 0.8800 . ?
C12 N18 1.301(3) 4 ?
C12 H12 0.9500 . ?
N19 C13 1.300(4) . ?
N19 H19A 0.8799 . ?
N19 H19B 0.8801 . ?
N20 C13 1.300(4) . ?
N20 H20A 0.8800 . ?
N20 H20B 0.8800 . ?
C13 H13 0.9500 . ?
N21 C14 1.300(4) . ?
N21 H21A 0.8799 . ?
N21 H21B 0.8799 . ?
N22 C14 1.300(4) . ?
N22 H22A 0.8799 . ?
N22 H22B 0.8799 . ?
C14 H14 0.9500 . ?
N23 C15 1.300(4) . ?
N23 H23A 0.8799 . ?
N23 H23B 0.8803 . ?
N24 C15 1.300(4) . ?
N24 H24A 0.8801 . ?
N24 H24B 0.8799 . ?
C15 H15 0.9500 . ?
N25 C16 1.301(4) . ?
N25 H25A 0.8798 . ?
N25 H25B 0.8801 . ?
N26 C16 1.300(4) . ?
N26 H26A 0.8800 . ?
N26 H26B 0.8800 . ?
C16 H16 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1B I17 0.88 2.78 3.64(4) 167.1 2_665
C1 H1 I18 0.95 3.16 3.90(8) 135.9 .
C1 H1 I18 0.95 3.19 3.92(8) 135.5 2_665
N2 H2A I15 0.88 3.27 4.07(5) 153.5 2_655
N2 H2B I7 0.88 2.62 3.48(5) 165.0 .
N3 H3A I15 0.88 3.18 4.00(5) 154.8 2_655
N3 H3B I3 0.88 3.00 3.83(5) 157.6 2_765
C2 H2 I8 0.95 2.87 3.79(4) 164.3 .
N4 H4B N9 0.88 2.27 3.04(8) 145.8 3_665
N4 H4B N9 0.88 2.27 3.04(8) 145.8 6_665
N5 H5B I16 0.88 2.58 3.46(9) 178.6 .
N5' H5C N9 0.88 2.14 2.86(13) 138.4 3_665
N6 H6A N23 0.88 2.59 3.46(12) 173.2 1_545
N7 H7A I10 0.88 2.49 3.32(11) 159.3 .
N7 H7B I9 0.88 2.22 3.06(7) 159.6 .
N6' H6C I9 0.88 2.32 3.13(8) 152.5 .
N6' H6D I8 0.88 2.00 2.64(9) 128.0 .
N8 H8B I3 0.88 2.88 3.69(4) 153.3 2_765
C5 H5 I5 0.95 3.06 3.96(6) 159.8 2_765
N9 H9A N4 0.88 2.39 3.04(8) 131.3 2_655
N9 H9A N5' 0.88 2.12 2.86(13) 140.6 2_655
N9 H9B I13 0.88 2.79 3.65(2) 166.8 3_665
C6 H6 I14 0.95 2.92 3.71(5) 141.0 2_665
N10 H10A I5 0.88 3.22 3.86(8) 132.1 1_545
N10 H10B I7 0.88 2.98 3.81(6) 158.1 .
C7 H7 I11 0.95 3.01 3.93(7) 161.4 .
N11 H11B I17 0.88 2.87 3.64(6) 146.0 .
N12 H12B I9 0.88 2.92 3.73(7) 154.2 1_565
C8 H8 I17 0.95 3.00 3.74(7) 135.8 3_565
N13 H13A I10 0.88 3.41 4.12(7) 140.5 1_565
N13 H13B I2 0.88 2.97 3.74(5) 148.1 3_565
C9 H9 I6 0.95 3.10 4.02(7) 165.4 3_565
N15 H15B I16 0.88 2.98 3.78(9) 152.3 .
C10 H10 N18 0.95 2.57 3.41(7) 148.3 .
N16 H16A I14 0.88 2.94 3.80(6) 163.9 3_565
N18 H18A N21 0.88 1.56 2.14(5) 120.0 3
N18 H18A N25 0.88 2.16 2.90(5) 140.8 3
N18 H18B I15 0.88 2.77 3.63(3) 166.3 .
C12 H12 I16 0.95 3.15 4.04(4) 155.8 3_665
N20 H20A I6 0.88 2.77 3.64(9) 167.0 3_565
N24 H24A I4 0.88 3.04 3.89(8) 161.9 3_565
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.039 0.301 0.000 88 34 ' '
2 0.261 0.961 0.000 88 34 ' '
3 0.667 0.333 0.500 305 100 ' '
4 0.699 0.739 0.000 88 34 ' '
