#------------------------------------------------------------------------------
#$Date: 2022-06-23 12:30:20 +0300 (Thu, 23 Jun 2022) $
#$Revision: 276188 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/54/8105482.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_8105482
loop_
_publ_author_name
'Li, Ji'
'Miao, Ming-Zhi'
_publ_section_title
;
 The crystal structure of
 aqua{N,N,N′,N′-tetrakis[(1H-benzimidazol-\kN 3)
 methyl]cyclohexane-1,2-diamine}lead(II) diacetate--methanol (1/2),
 C44H54N10O7Pb
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1417
_journal_page_last               1420
_journal_paper_doi               10.1515/ncrs-2020-0343
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C38 H40 N10 O Pb, 2(C2 H3 O2), 2(C H4 O)'
_chemical_formula_sum            'C44 H54 N10 O7 Pb'
_chemical_formula_weight         1042.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                101.163(2)
_cell_angle_beta                 110.634(2)
_cell_angle_gamma                100.698(2)
_cell_formula_units_Z            2
_cell_length_a                   12.096(2)
_cell_length_b                   12.9160(2)
_cell_length_c                   16.5904(7)
_cell_measurement_reflns_used    3344
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.90
_cell_measurement_theta_min      2.38
_cell_volume                     2287.0(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2003) [1]'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2003)'
_computing_molecular_graphics    'Diamond (Brandenburg, 2006)[4]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[5]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [2-3]'
_computing_structure_solution    'ShelXS (Sheldrick, 2015) [2-3]'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7966
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.820
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.748
_exptl_absorpt_correction_T_max  0.7056
_exptl_absorpt_correction_T_min  0.5854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick, 2008)[6]'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.813
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         7966
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0604
_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)+(0.0689P)²+0.0406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7079
_reflns_number_total             7966
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2020-0343_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105482
_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   0.706
_shelx_estimated_absorpt_t_min   0.585
_exptl_absorpt_special_details   'SADABS, (Sheldrick, 2008)[6]'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.748(4)
 0.252(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C43-O6 = C44-O7
 1.42 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C44) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5.a Riding coordinates:
 O1(H1A,H1B)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C6(H6)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C15(H15A,
 H15B), C23(H23A,H23B), C31(H31A,H31B)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C18(H18), C19(H19), C20(H20),
 C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36),
  C37(H37), N4(H4), N6(H6A), N8(H8), N10(H10A)
5.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
5.f Idealised tetrahedral OH refined as rotating group:
 O6(H6B), O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 0.50164(3) 0.75760(2) 0.74428(2) 0.04121(13) Uani 1 1 d . . . . .
C1 C 0.6977(7) 0.9397(6) 0.6758(5) 0.0436(19) Uani 1 1 d . . . . .
H1 H 0.7436 0.8861 0.6683 0.052 Uiso 1 1 calc R U . . .
C2 C 0.7253(9) 1.0225(7) 0.6264(6) 0.062(2) Uani 1 1 d . . . . .
H2A H 0.6773 1.0745 0.6293 0.074 Uiso 1 1 calc R U . . .
H2B H 0.6999 0.9842 0.5637 0.074 Uiso 1 1 calc R U . . .
C3 C 0.8627(9) 1.0862(8) 0.6656(7) 0.070(3) Uani 1 1 d . . . . .
H3A H 0.9110 1.0355 0.6591 0.084 Uiso 1 1 calc R U . . .
H3B H 0.8749 1.1390 0.6331 0.084 Uiso 1 1 calc R U . . .
C4 C 0.9047(10) 1.1453(8) 0.7639(7) 0.072(3) Uani 1 1 d . . . . .
H4A H 0.8601 1.1993 0.7702 0.086 Uiso 1 1 calc R U . . .
H4B H 0.9916 1.1833 0.7889 0.086 Uiso 1 1 calc R U . . .
C5 C 0.8818(8) 1.0631(8) 0.8140(6) 0.057(2) Uani 1 1 d . . . . .
H5A H 0.9081 1.1022 0.8767 0.068 Uiso 1 1 calc R U . . .
H5B H 0.9320 1.0132 0.8110 0.068 Uiso 1 1 calc R U . . .
C6 C 0.7468(7) 0.9953(6) 0.7780(5) 0.0421(18) Uani 1 1 d . . . . .
H6 H 0.6994 1.0476 0.7854 0.050 Uiso 1 1 calc R U . . .
C7 C 0.5352(8) 0.7917(7) 0.5536(5) 0.051(2) Uani 1 1 d . . . . .
H7A H 0.5646 0.8246 0.5145 0.061 Uiso 1 1 calc R U . . .
H7B H 0.4467 0.7622 0.5229 0.061 Uiso 1 1 calc R U . . .
C8 C 0.5912(7) 0.7009(7) 0.5711(6) 0.048(2) Uani 1 1 d . . . . .
C9 C 0.6573(8) 0.5789(7) 0.6327(6) 0.052(2) Uani 1 1 d . . . . .
C10 C 0.6924(10) 0.5133(8) 0.6871(7) 0.074(3) Uani 1 1 d . . . . .
H10 H 0.6848 0.5241 0.7417 0.088 Uiso 1 1 calc R U . . .
C11 C 0.7394(9) 0.4309(8) 0.6585(8) 0.071(3) Uani 1 1 d . . . . .
H11 H 0.7629 0.3848 0.6942 0.085 Uiso 1 1 calc R U . . .
C12 C 0.7520(10) 0.4158(8) 0.5785(9) 0.078(3) Uani 1 1 d . . . . .
H12 H 0.7855 0.3602 0.5619 0.094 Uiso 1 1 calc R U . . .
C13 C 0.7170(9) 0.4800(7) 0.5213(7) 0.066(3) Uani 1 1 d . . . . .
H13 H 0.7247 0.4690 0.4667 0.079 Uiso 1 1 calc R U . . .
C14 C 0.6692(8) 0.5623(7) 0.5518(6) 0.052(2) Uani 1 1 d . . . . .
C15 C 0.4836(8) 0.9483(7) 0.6221(6) 0.050(2) Uani 1 1 d . . . . .
H15A H 0.4818 0.9725 0.5699 0.060 Uiso 1 1 calc R U . . .
H15B H 0.5169 1.0130 0.6733 0.060 Uiso 1 1 calc R U . . .
C16 C 0.3554(8) 0.8945(7) 0.6076(5) 0.049(2) Uani 1 1 d . . . . .
C17 C 0.1921(8) 0.7831(7) 0.5960(6) 0.051(2) Uani 1 1 d . . . . .
C18 C 0.1053(9) 0.6956(9) 0.5954(7) 0.073(3) Uani 1 1 d . . . . .
H18 H 0.1250 0.6313 0.6042 0.088 Uiso 1 1 calc R U . . .
C19 C -0.0090(9) 0.7063(11) 0.5818(8) 0.087(4) Uani 1 1 d . . . . .
H19 H -0.0679 0.6487 0.5818 0.104 Uiso 1 1 calc R U . . .
C20 C -0.0389(10) 0.8001(12) 0.5680(8) 0.088(4) Uani 1 1 d . . . . .
H20 H -0.1181 0.8047 0.5584 0.105 Uiso 1 1 calc R U . . .
C21 C 0.0444(10) 0.8873(11) 0.5677(6) 0.076(3) Uani 1 1 d . . . . .
H21 H 0.0234 0.9509 0.5582 0.091 Uiso 1 1 calc R U . . .
C22 C 0.1621(8) 0.8770(9) 0.5823(6) 0.058(2) Uani 1 1 d . . . . .
C23 C 0.8167(8) 0.8535(7) 0.8471(6) 0.050(2) Uani 1 1 d . . . . .
H23A H 0.8955 0.9031 0.8897 0.060 Uiso 1 1 calc R U . . .
H23B H 0.8254 0.8230 0.7922 0.060 Uiso 1 1 calc R U . . .
C24 C 0.7811(8) 0.7625(7) 0.8849(6) 0.049(2) Uani 1 1 d . . . . .
C25 C 0.6839(10) 0.6344(7) 0.9187(7) 0.060(3) Uani 1 1 d . . . . .
C26 C 0.5933(12) 0.5558(9) 0.9257(8) 0.083(3) Uani 1 1 d . . . . .
H26 H 0.5099 0.5485 0.8967 0.100 Uiso 1 1 calc R U . . .
C27 C 0.6359(16) 0.4915(12) 0.9775(11) 0.120(5) Uani 1 1 d . . . . .
H27 H 0.5796 0.4378 0.9842 0.144 Uiso 1 1 calc R U . . .
C28 C 0.7586(18) 0.5019(13) 1.0206(11) 0.129(6) Uani 1 1 d . . . . .
H28 H 0.7820 0.4552 1.0556 0.155 Uiso 1 1 calc R U . . .
C29 C 0.8480(13) 0.5773(11) 1.0148(9) 0.101(4) Uani 1 1 d . . . . .
H29 H 0.9311 0.5837 1.0447 0.121 Uiso 1 1 calc R U . . .
C30 C 0.8072(10) 0.6436(8) 0.9614(7) 0.063(3) Uani 1 1 d . . . . .
C31 C 0.7242(8) 0.9769(7) 0.9138(5) 0.047(2) Uani 1 1 d . . . . .
H31A H 0.7886 1.0456 0.9386 0.056 Uiso 1 1 calc R U . . .
H31B H 0.7416 0.9343 0.9566 0.056 Uiso 1 1 calc R U . . .
C32 C 0.6036(8) 0.9996(7) 0.8993(5) 0.047(2) Uani 1 1 d . . . . .
C33 C 0.4076(8) 0.9840(7) 0.8525(5) 0.046(2) Uani 1 1 d . . . . .
C34 C 0.2828(9) 0.9501(8) 0.8117(6) 0.058(2) Uani 1 1 d . . . . .
H34 H 0.2417 0.8827 0.7685 0.070 Uiso 1 1 calc R U . . .
C35 C 0.2193(10) 1.0204(10) 0.8372(7) 0.068(3) Uani 1 1 d . . . . .
H35 H 0.1338 0.9994 0.8110 0.082 Uiso 1 1 calc R U . . .
C36 C 0.2802(10) 1.1202(9) 0.9004(7) 0.065(3) Uani 1 1 d . . . . .
H36 H 0.2351 1.1669 0.9136 0.078 Uiso 1 1 calc R U . . .
C37 C 0.4036(10) 1.1525(8) 0.9437(6) 0.061(3) Uani 1 1 d . . . . .
H37 H 0.4438 1.2186 0.9886 0.073 Uiso 1 1 calc R U . . .
C38 C 0.4691(8) 1.0830(7) 0.9189(6) 0.051(2) Uani 1 1 d . . . . .
C39 C 0.0339(12) 0.6633(12) 0.8160(9) 0.120(5) Uani 1 1 d . U . . .
H39A H 0.0625 0.6660 0.7691 0.180 Uiso 1 1 calc R U . . .
H39B H -0.0376 0.6899 0.8040 0.180 Uiso 1 1 calc R U . . .
H39C H 0.0134 0.5888 0.8185 0.180 Uiso 1 1 calc R U . . .
C40 C 0.1337(10) 0.7341(8) 0.9047(6) 0.063(3) Uani 1 1 d . . . . .
C41 C 0.2713(19) 0.2104(15) 0.7107(11) 0.156(7) Uani 1 1 d . U . . .
H41A H 0.1883 0.2149 0.6940 0.233 Uiso 1 1 calc R U . . .
H41B H 0.3227 0.2625 0.7679 0.233 Uiso 1 1 calc R U . . .
H41C H 0.2741 0.1376 0.7146 0.233 Uiso 1 1 calc R U . . .
C42 C 0.3174(12) 0.2360(12) 0.6399(8) 0.085(4) Uani 1 1 d . . . . .
C43 C 0.0862(15) 0.4072(15) 0.6648(13) 0.154(7) Uani 1 1 d D . . . .
H43A H 0.0836 0.3875 0.7172 0.232 Uiso 1 1 calc R U . . .
H43B H 0.0594 0.3420 0.6160 0.232 Uiso 1 1 calc R U . . .
H43C H 0.0329 0.4533 0.6489 0.232 Uiso 1 1 calc R U . . .
C44 C 0.652(2) 0.2835(19) 0.8205(13) 0.217(11) Uani 1 1 d D U . . .
H44A H 0.7213 0.2626 0.8556 0.326 Uiso 1 1 calc R U . . .
H44B H 0.5899 0.2731 0.8442 0.326 Uiso 1 1 calc R U . . .
H44C H 0.6768 0.3594 0.8227 0.326 Uiso 1 1 calc R U . . .
N1 N 0.5656(6) 0.8770(5) 0.6377(4) 0.0403(15) Uani 1 1 d . . . . .
N2 N 0.7238(6) 0.9153(5) 0.8281(4) 0.0410(15) Uani 1 1 d . . . . .
N3 N 0.6086(7) 0.6685(6) 0.6434(5) 0.058(2) Uani 1 1 d . . . . .
N4 N 0.6261(6) 0.6406(6) 0.5132(5) 0.0543(19) Uani 1 1 d . . . . .
H4 H 0.6223 0.6492 0.4622 0.065 Uiso 1 1 calc R U . . .
N5 N 0.3168(7) 0.7960(6) 0.6127(5) 0.0516(18) Uani 1 1 d . . . . .
N6 N 0.2671(7) 0.9475(6) 0.5883(5) 0.0548(19) Uani 1 1 d . . . . .
H6A H 0.2749 1.0123 0.5812 0.066 Uiso 1 1 calc R U . . .
N7 N 0.6698(7) 0.7119(6) 0.8705(5) 0.0511(17) Uani 1 1 d . . . . .
N8 N 0.8676(7) 0.7266(6) 0.9390(5) 0.060(2) Uani 1 1 d . . . . .
H8 H 0.9458 0.7510 0.9564 0.072 Uiso 1 1 calc R U . . .
N9 N 0.4966(6) 0.9321(5) 0.8415(4) 0.0469(17) Uani 1 1 d . . . . .
N10 N 0.5929(6) 1.0917(5) 0.9470(4) 0.0465(17) Uani 1 1 d . . . . .
H10A H 0.6521 1.1455 0.9872 0.056 Uiso 1 1 calc R U . . .
O1 O 0.3451(7) 0.6623(6) 0.8067(6) 0.097(3) Uani 1 1 d . . . . .
H1A H 0.3190 0.5961 0.7824 0.145 Uiso 1 1 d R U . . .
H1B H 0.3257 0.6792 0.8491 0.145 Uiso 1 1 d R U . . .
O2 O 0.1001(6) 0.7763(6) 0.9625(5) 0.076(2) Uani 1 1 d . . . . .
O3 O 0.2405(6) 0.7435(5) 0.9145(4) 0.0689(18) Uani 1 1 d . . . . .
O4 O 0.3303(8) 0.1593(7) 0.5906(6) 0.094(3) Uani 1 1 d . . . . .
O5 O 0.3330(8) 0.3312(6) 0.6334(5) 0.089(2) Uani 1 1 d . . . . .
O6 O 0.2079(11) 0.4646(8) 0.6832(9) 0.137(4) Uani 1 1 d D . . . .
H6B H 0.2532 0.4250 0.6962 0.205 Uiso 1 1 calc R U . . .
O7 O 0.6026(19) 0.2172(18) 0.7294(12) 0.245(8) Uani 1 1 d D U . . .
H7 H 0.5398 0.2315 0.7003 0.367 Uiso 1 1 calc R U . . .
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'
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
N2 Pb1 N1 64.47(18) . .
N3 Pb1 N1 63.1(2) . .
N3 Pb1 N2 83.7(2) . .
N3 Pb1 N5 98.4(2) . .
N3 Pb1 O1 130.3(2) . .
N5 Pb1 N1 62.5(2) . .
N5 Pb1 N2 118.3(2) . .
N7 Pb1 N1 120.5(2) . .
N7 Pb1 N2 64.8(2) . .
N7 Pb1 N3 82.6(2) . .
N7 Pb1 N5 176.8(2) . .
N7 Pb1 O1 85.3(2) . .
N9 Pb1 N1 89.3(2) . .
N9 Pb1 N2 66.0(2) . .
N9 Pb1 N3 146.1(3) . .
N9 Pb1 N5 84.2(2) . .
N9 Pb1 N7 96.7(2) . .
N9 Pb1 O1 83.1(2) . .
O1 Pb1 N1 153.9(2) . .
O1 Pb1 N2 132.3(2) . .
O1 Pb1 N5 91.8(2) . .
C2 C1 H1 106.7 . .
C2 C1 C6 111.1(7) . .
C6 C1 H1 106.7 . .
N1 C1 H1 106.7 . .
N1 C1 C2 113.2(7) . .
N1 C1 C6 111.8(6) . .
C1 C2 H2A 109.0 . .
C1 C2 H2B 109.0 . .
C1 C2 C3 112.9(8) . .
H2A C2 H2B 107.8 . .
C3 C2 H2A 109.0 . .
C3 C2 H2B 109.0 . .
C2 C3 H3A 109.7 . .
C2 C3 H3B 109.7 . .
H3A C3 H3B 108.2 . .
C4 C3 C2 109.8(8) . .
C4 C3 H3A 109.7 . .
C4 C3 H3B 109.7 . .
C3 C4 H4A 109.8 . .
C3 C4 H4B 109.8 . .
C3 C4 C5 109.6(8) . .
H4A C4 H4B 108.2 . .
C5 C4 H4A 109.8 . .
C5 C4 H4B 109.8 . .
C4 C5 H5A 108.7 . .
C4 C5 H5B 108.7 . .
C4 C5 C6 114.3(8) . .
H5A C5 H5B 107.6 . .
C6 C5 H5A 108.7 . .
C6 C5 H5B 108.7 . .
C1 C6 H6 106.6 . .
C5 C6 C1 110.2(7) . .
C5 C6 H6 106.6 . .
N2 C6 C1 112.1(6) . .
N2 C6 C5 114.3(7) . .
N2 C6 H6 106.6 . .
H7A C7 H7B 107.9 . .
C8 C7 H7A 109.3 . .
C8 C7 H7B 109.3 . .
N1 C7 H7A 109.3 . .
N1 C7 H7B 109.3 . .
N1 C7 C8 111.7(7) . .
N3 C8 C7 123.3(7) . .
N3 C8 N4 112.6(8) . .
N4 C8 C7 124.0(8) . .
C10 C9 C14 120.5(8) . .
C10 C9 N3 131.3(9) . .
C14 C9 N3 108.2(8) . .
C9 C10 H10 121.0 . .
C9 C10 C11 118.1(10) . .
C11 C10 H10 121.0 . .
C10 C11 H11 119.5 . .
C12 C11 C10 121.0(11) . .
C12 C11 H11 119.5 . .
C11 C12 H12 118.7 . .
C11 C12 C13 122.6(10) . .
C13 C12 H12 118.7 . .
C12 C13 H13 122.5 . .
C12 C13 C14 114.9(9) . .
C14 C13 H13 122.5 . .
C9 C14 C13 122.8(9) . .
C9 C14 N4 106.6(7) . .
N4 C14 C13 130.6(9) . .
H15A C15 H15B 107.7 . .
C16 C15 H15A 108.8 . .
C16 C15 H15B 108.8 . .
N1 C15 H15A 108.8 . .
N1 C15 H15B 108.8 . .
N1 C15 C16 113.8(7) . .
N5 C16 C15 125.4(8) . .
N5 C16 N6 113.5(8) . .
N6 C16 C15 121.1(8) . .
C18 C17 N5 130.1(9) . .
C22 C17 C18 120.4(9) . .
C22 C17 N5 109.4(8) . .
C17 C18 H18 120.8 . .
C19 C18 C17 118.4(11) . .
C19 C18 H18 120.8 . .
C18 C19 H19 119.4 . .
C18 C19 C20 121.1(12) . .
C20 C19 H19 119.4 . .
C19 C20 H20 119.1 . .
C19 C20 C21 121.7(11) . .
C21 C20 H20 119.1 . .
C20 C21 H21 121.3 . .
C20 C21 C22 117.4(11) . .
C22 C21 H21 121.3 . .
C17 C22 C21 120.9(10) . .
C17 C22 N6 106.3(8) . .
N6 C22 C21 132.8(10) . .
H23A C23 H23B 108.0 . .
C24 C23 H23A 109.4 . .
C24 C23 H23B 109.4 . .
N2 C23 H23A 109.4 . .
N2 C23 H23B 109.4 . .
N2 C23 C24 111.3(7) . .
N7 C24 C23 125.8(8) . .
N7 C24 N8 113.9(8) . .
N8 C24 C23 120.3(8) . .
C30 C25 C26 121.8(10) . .
C30 C25 N7 109.2(9) . .
N7 C25 C26 129.0(10) . .
C25 C26 H26 122.4 . .
C27 C26 C25 115.2(12) . .
C27 C26 H26 122.4 . .
C26 C27 H27 118.6 . .
C26 C27 C28 122.7(13) . .
C28 C27 H27 118.6 . .
C27 C28 H28 118.4 . .
C29 C28 C27 123.1(12) . .
C29 C28 H28 118.4 . .
C28 C29 H29 122.2 . .
C28 C29 C30 115.5(12) . .
C30 C29 H29 122.2 . .
C25 C30 C29 121.6(11) . .
N8 C30 C25 105.8(8) . .
N8 C30 C29 132.6(11) . .
H31A C31 H31B 108.1 . .
C32 C31 H31A 109.5 . .
C32 C31 H31B 109.5 . .
N2 C31 H31A 109.5 . .
N2 C31 H31B 109.5 . .
N2 C31 C32 110.9(6) . .
N9 C32 C31 124.4(7) . .
N9 C32 N10 112.9(7) . .
N10 C32 C31 122.7(8) . .
C34 C33 C38 121.5(8) . .
C34 C33 N9 130.6(8) . .
C38 C33 N9 107.9(8) . .
C33 C34 H34 121.4 . .
C33 C34 C35 117.2(9) . .
C35 C34 H34 121.4 . .
C34 C35 H35 119.4 . .
C36 C35 C34 121.3(10) . .
C36 C35 H35 119.4 . .
C35 C36 H36 119.1 . .
C37 C36 C35 121.8(9) . .
C37 C36 H36 119.1 . .
C36 C37 H37 121.2 . .
C36 C37 C38 117.7(9) . .
C38 C37 H37 121.2 . .
C33 C38 C37 120.4(9) . .
N10 C38 C33 106.9(7) . .
N10 C38 C37 132.6(9) . .
H39A C39 H39B 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
C40 C39 H39A 109.5 . .
C40 C39 H39B 109.5 . .
C40 C39 H39C 109.5 . .
O2 C40 C39 116.8(10) . .
O3 C40 C39 117.8(10) . .
O3 C40 O2 125.3(9) . .
H41A C41 H41B 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C42 C41 H41A 109.5 . .
C42 C41 H41B 109.5 . .
C42 C41 H41C 109.5 . .
O4 C42 C41 117.4(13) . .
O4 C42 O5 124.6(11) . .
O5 C42 C41 117.8(12) . .
H43A C43 H43B 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
O6 C43 H43A 109.5 . .
O6 C43 H43B 109.5 . .
O6 C43 H43C 109.5 . .
H44A C44 H44B 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
O7 C44 H44A 109.5 . .
O7 C44 H44B 109.5 . .
O7 C44 H44C 109.5 . .
C1 N1 Pb1 114.4(4) . .
C7 N1 Pb1 103.2(4) . .
C7 N1 C1 110.1(6) . .
C15 N1 Pb1 105.8(4) . .
C15 N1 C1 112.5(6) . .
C15 N1 C7 110.4(6) . .
C6 N2 Pb1 115.7(4) . .
C23 N2 Pb1 104.9(5) . .
C23 N2 C6 112.5(6) . .
C23 N2 C31 109.6(6) . .
C31 N2 Pb1 105.5(5) . .
C31 N2 C6 108.3(6) . .
C8 N3 Pb1 113.7(5) . .
C8 N3 C9 106.0(7) . .
C9 N3 Pb1 138.6(6) . .
C8 N4 C14 106.7(7) . .
C8 N4 H4 126.7 . .
C14 N4 H4 126.7 . .
C16 N5 Pb1 108.0(6) . .
C16 N5 C17 104.5(7) . .
C17 N5 Pb1 131.7(6) . .
C16 N6 C22 106.3(8) . .
C16 N6 H6A 126.9 . .
C22 N6 H6A 126.9 . .
C24 N7 Pb1 113.6(6) . .
C24 N7 C25 104.5(7) . .
C25 N7 Pb1 140.5(6) . .
C24 N8 C30 106.7(8) . .
C24 N8 H8 126.7 . .
C30 N8 H8 126.7 . .
C32 N9 Pb1 116.7(5) . .
C32 N9 C33 105.4(7) . .
C33 N9 Pb1 137.9(6) . .
C32 N10 C38 106.9(7) . .
C32 N10 H10A 126.6 . .
C38 N10 H10A 126.6 . .
Pb1 O1 H1A 110.9 . .
Pb1 O1 H1B 137.0 . .
H1A O1 H1B 111.1 . .
C43 O6 H6B 109.5 . .
C44 O7 H7 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 N1 2.772(6) .
Pb1 N2 2.746(7) .
Pb1 N3 2.670(7) .
Pb1 N5 2.720(7) .
Pb1 N7 2.606(7) .
Pb1 N9 2.530(6) .
Pb1 O1 2.680(7) .
C1 H1 0.9800 .
C1 C2 1.526(11) .
C1 C6 1.551(11) .
C1 N1 1.489(10) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 C3 1.544(13) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3 C4 1.513(13) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C5 1.514(13) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5 C6 1.540(11) .
C6 H6 0.9800 .
C6 N2 1.489(10) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C8 1.485(11) .
C7 N1 1.480(9) .
C8 N3 1.308(11) .
C8 N4 1.351(10) .
C9 C10 1.367(14) .
C9 C14 1.379(12) .
C9 N3 1.402(10) .
C10 H10 0.9300 .
C10 C11 1.379(13) .
C11 H11 0.9300 .
C11 C12 1.371(15) .
C12 H12 0.9300 .
C12 C13 1.385(15) .
C13 H13 0.9300 .
C13 C14 1.396(11) .
C14 N4 1.385(11) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 C16 1.489(12) .
C15 N1 1.466(10) .
C16 N5 1.301(11) .
C16 N6 1.352(10) .
C17 C18 1.388(14) .
C17 C22 1.367(13) .
C17 N5 1.405(11) .
C18 H18 0.9300 .
C18 C19 1.358(14) .
C19 H19 0.9300 .
C19 C20 1.365(17) .
C20 H20 0.9300 .
C20 C21 1.366(16) .
C21 H21 0.9300 .
C21 C22 1.394(13) .
C22 N6 1.377(12) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C23 C24 1.499(12) .
C23 N2 1.477(9) .
C24 N7 1.297(11) .
C24 N8 1.340(11) .
C25 C26 1.403(14) .
C25 C30 1.378(14) .
C25 N7 1.396(11) .
C26 H26 0.9300 .
C26 C27 1.347(16) .
C27 H27 0.9300 .
C27 C28 1.37(2) .
C28 H28 0.9300 .
C28 C29 1.358(19) .
C29 H29 0.9300 .
C29 C30 1.380(14) .
C30 N8 1.369(12) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C31 C32 1.487(11) .
C31 N2 1.486(9) .
C32 N9 1.318(11) .
C32 N10 1.350(9) .
C33 C34 1.359(12) .
C33 C38 1.387(12) .
C33 N9 1.415(10) .
C34 H34 0.9300 .
C34 C35 1.392(13) .
C35 H35 0.9300 .
C35 C36 1.372(15) .
C36 H36 0.9300 .
C36 C37 1.347(14) .
C37 H37 0.9300 .
C37 C38 1.397(11) .
C38 N10 1.378(10) .
C39 H39A 0.9600 .
C39 H39B 0.9600 .
C39 H39C 0.9600 .
C39 C40 1.509(15) .
C40 O2 1.240(11) .
C40 O3 1.223(11) .
C41 H41A 0.9600 .
C41 H41B 0.9600 .
C41 H41C 0.9600 .
C41 C42 1.530(18) .
C42 O4 1.229(14) .
C42 O5 1.240(14) .
C43 H43A 0.9600 .
C43 H43B 0.9600 .
C43 H43C 0.9600 .
C43 O6 1.415(14) .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .
C44 O7 1.431(15) .
N4 H4 0.8600 .
N6 H6A 0.8600 .
N8 H8 0.8600 .
N10 H10A 0.8600 .
O1 H1A 0.8189 .
O1 H1B 0.8203 .
O6 H6B 0.8200 .
O7 H7 0.8200 .
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
N4 H4 O5 0.86 1.89 2.723(10) 161.8 2_666
N6 H6A O4 0.86 1.85 2.689(11) 165.2 1_565
N8 H8 O2 0.86 1.80 2.634(11) 163.9 1_655
N10 H10A O3 0.86 1.82 2.668(9) 168.7 2_677
O1 H1A O6 0.82 1.98 2.734(13) 153.5 .
O1 H1B O3 0.82 1.92 2.694(10) 157.0 .
O6 H6B O5 0.82 2.03 2.691(13) 136.8 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C1 C2 C3 C4 -57.8(11) . . . .
C1 C6 N2 Pb1 -38.9(7) . . . .
C1 C6 N2 C23 81.7(8) . . . .
C1 C6 N2 C31 -157.0(6) . . . .
C2 C1 C6 C5 -50.0(9) . . . .
C2 C1 C6 N2 -178.5(6) . . . .
C2 C1 N1 Pb1 -168.0(5) . . . .
C2 C1 N1 C7 76.3(8) . . . .
C2 C1 N1 C15 -47.3(9) . . . .
C2 C3 C4 C5 57.6(11) . . . .
C3 C4 C5 C6 -57.7(11) . . . .
C4 C5 C6 C1 53.4(10) . . . .
C4 C5 C6 N2 -179.3(8) . . . .
C5 C6 N2 Pb1 -165.2(5) . . . .
C5 C6 N2 C23 -44.6(9) . . . .
C5 C6 N2 C31 76.7(8) . . . .
C6 C1 C2 C3 53.9(10) . . . .
C6 C1 N1 Pb1 -41.6(7) . . . .
C6 C1 N1 C7 -157.3(6) . . . .
C6 C1 N1 C15 79.1(8) . . . .
C7 C8 N3 Pb1 9.4(11) . . . .
C7 C8 N3 C9 177.2(8) . . . .
C7 C8 N4 C14 -177.7(8) . . . .
C8 C7 N1 Pb1 -51.6(7) . . . .
C8 C7 N1 C1 70.9(8) . . . .
C8 C7 N1 C15 -164.2(7) . . . .
C9 C10 C11 C12 0.8(16) . . . .
C9 C14 N4 C8 0.4(9) . . . .
C10 C9 C14 C13 -0.3(14) . . . .
C10 C9 C14 N4 179.9(9) . . . .
C10 C9 N3 Pb1 -16.8(17) . . . .
C10 C9 N3 C8 -179.9(11) . . . .
C10 C11 C12 C13 -1.2(17) . . . .
C11 C12 C13 C14 0.8(15) . . . .
C12 C13 C14 C9 -0.1(14) . . . .
C12 C13 C14 N4 179.7(9) . . . .
C13 C14 N4 C8 -179.5(9) . . . .
C14 C9 C10 C11 -0.1(15) . . . .
C14 C9 N3 Pb1 164.0(6) . . . .
C14 C9 N3 C8 1.0(10) . . . .
C15 C16 N5 Pb1 35.0(10) . . . .
C15 C16 N5 C17 178.8(8) . . . .
C15 C16 N6 C22 -177.9(8) . . . .
C16 C15 N1 Pb1 -39.0(7) . . . .
C16 C15 N1 C1 -164.5(6) . . . .
C16 C15 N1 C7 72.0(8) . . . .
C17 C18 C19 C20 0.7(18) . . . .
C17 C22 N6 C16 -1.6(10) . . . .
C18 C17 C22 C21 0.1(14) . . . .
C18 C17 C22 N6 179.0(8) . . . .
C18 C17 N5 Pb1 -46.7(13) . . . .
C18 C17 N5 C16 -177.9(10) . . . .
C18 C19 C20 C21 -0.4(19) . . . .
C19 C20 C21 C22 -0.1(17) . . . .
C20 C21 C22 C17 0.2(15) . . . .
C20 C21 C22 N6 -178.4(10) . . . .
C21 C22 N6 C16 177.1(10) . . . .
C22 C17 C18 C19 -0.5(15) . . . .
C22 C17 N5 Pb1 130.5(7) . . . .
C22 C17 N5 C16 -0.7(10) . . . .
C23 C24 N7 Pb1 10.3(11) . . . .
C23 C24 N7 C25 179.4(8) . . . .
C23 C24 N8 C30 -179.4(8) . . . .
C24 C23 N2 Pb1 -44.8(7) . . . .
C24 C23 N2 C6 -171.4(7) . . . .
C24 C23 N2 C31 68.0(9) . . . .
C25 C26 C27 C28 0(2) . . . .
C25 C30 N8 C24 -0.5(10) . . . .
C26 C25 C30 C29 -1.3(17) . . . .
C26 C25 C30 N8 179.3(9) . . . .
C26 C25 N7 Pb1 -14.6(16) . . . .
C26 C25 N7 C24 -178.7(10) . . . .
C26 C27 C28 C29 0(3) . . . .
C27 C28 C29 C30 0(2) . . . .
C28 C29 C30 C25 1.2(19) . . . .
C28 C29 C30 N8 -179.7(12) . . . .
C29 C30 N8 C24 -179.7(12) . . . .
C30 C25 C26 C27 0.6(17) . . . .
C30 C25 N7 Pb1 164.7(7) . . . .
C30 C25 N7 C24 0.5(10) . . . .
C31 C32 N9 Pb1 -3.3(10) . . . .
C31 C32 N9 C33 177.7(7) . . . .
C31 C32 N10 C38 -177.3(7) . . . .
C32 C31 N2 Pb1 -43.2(7) . . . .
C32 C31 N2 C6 81.2(8) . . . .
C32 C31 N2 C23 -155.7(7) . . . .
C33 C34 C35 C36 0.6(14) . . . .
C33 C38 N10 C32 -0.9(9) . . . .
C34 C33 C38 C37 -2.0(13) . . . .
C34 C33 C38 N10 179.0(7) . . . .
C34 C33 N9 Pb1 3.1(14) . . . .
C34 C33 N9 C32 -178.3(9) . . . .
C34 C35 C36 C37 -3.4(15) . . . .
C35 C36 C37 C38 3.3(14) . . . .
C36 C37 C38 C33 -0.6(13) . . . .
C36 C37 C38 N10 178.0(9) . . . .
C37 C38 N10 C32 -179.7(9) . . . .
C38 C33 C34 C35 2.0(13) . . . .
C38 C33 N9 Pb1 -178.8(6) . . . .
C38 C33 N9 C32 -0.2(9) . . . .
N1 C1 C2 C3 -179.3(7) . . . .
N1 C1 C6 C5 -177.6(7) . . . .
N1 C1 C6 N2 53.9(8) . . . .
N1 C7 C8 N3 32.4(12) . . . .
N1 C7 C8 N4 -149.8(8) . . . .
N1 C15 C16 N5 3.8(12) . . . .
N1 C15 C16 N6 -177.0(7) . . . .
N2 C23 C24 N7 27.1(12) . . . .
N2 C23 C24 N8 -152.7(8) . . . .
N2 C31 C32 N9 35.6(11) . . . .
N2 C31 C32 N10 -146.5(7) . . . .
N3 C8 N4 C14 0.3(10) . . . .
N3 C9 C10 C11 -179.2(9) . . . .
N3 C9 C14 C13 179.0(8) . . . .
N3 C9 C14 N4 -0.8(10) . . . .
N4 C8 N3 Pb1 -168.6(5) . . . .
N4 C8 N3 C9 -0.8(10) . . . .
N5 C16 N6 C22 1.3(10) . . . .
N5 C17 C18 C19 176.5(10) . . . .
N5 C17 C22 C21 -177.4(8) . . . .
N5 C17 C22 N6 1.4(10) . . . .
N6 C16 N5 Pb1 -144.2(6) . . . .
N6 C16 N5 C17 -0.4(10) . . . .
N7 C24 N8 C30 0.9(11) . . . .
N7 C25 C26 C27 179.7(11) . . . .
N7 C25 C30 C29 179.4(10) . . . .
N7 C25 C30 N8 0.0(11) . . . .
N8 C24 N7 Pb1 -169.9(6) . . . .
N8 C24 N7 C25 -0.8(10) . . . .
N9 C32 N10 C38 0.8(9) . . . .
N9 C33 C34 C35 179.9(8) . . . .
N9 C33 C38 C37 179.7(7) . . . .
N9 C33 C38 N10 0.7(9) . . . .
N10 C32 N9 Pb1 178.6(5) . . . .
N10 C32 N9 C33 -0.4(9) . . . .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.748(4)
2 0.252(4)
