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#$Date: 2022-02-04 21:23:32 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272624 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243736.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_7243736
loop_
_publ_author_name
'García-Santos, Isabel'
'Castiñeiras, Alfonso'
'Mahmoudi, Ghodrat'
'Babashkina, Maria G.'
'Zangrando, Ennio'
'Gomila, Rosa M.'
'Frontera, Antonio'
'Safin, Damir A.'
_publ_section_title
;
 Lead(ii) supramolecular structures formed through a cooperative influence
 of the hydrazinecarbothioamide derived and ancillary ligands
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              368
_journal_page_last               378
_journal_paper_doi               10.1039/D1CE01251G
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C16 H22 N10 O Pb2 S2, 2(C N S)'
_chemical_formula_sum            'C18 H22 N12 O Pb2 S4'
_chemical_formula_weight         965.09
_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   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-28 deposited with the CCDC.	2021-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.731(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4190(10)
_cell_length_b                   10.2159(6)
_cell_length_c                   12.8155(7)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.53
_cell_measurement_theta_min      2.23
_cell_volume                     2634.8(2)
_computing_cell_refinement       'APEX3 Software (Bruker, 2019)'
_computing_data_collection       'APEX3 Software (Bruker, 2019)'
_computing_data_reduction        'APEX3 Software (Bruker, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52116
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         2.655
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    13.119
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.433
_exptl_crystal_description       prism
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0186
_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)+(0.0081P)²+7.0717P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0353
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3414
_reflns_number_total             3849
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01251g1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7243734--7243737.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7243736
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.507
_shelx_estimated_absorpt_t_max   0.622
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
Pb Pb 0.04850(2) 0.69303(2) 0.12890(2) 0.01069(3) Uani 1 1 d . . . . .
S1 S -0.08570(3) 0.66393(6) 0.15070(5) 0.01099(13) Uani 1 1 d . . . . .
O1W O 0.000000 0.8929(3) 0.250000 0.0158(6) Uani 1 2 d S T P . .
H1A H 0.025100 0.959653 0.301700 0.024 Uiso 1 1 d R U . . .
N1 N 0.14513(12) 0.5313(2) 0.14349(17) 0.0121(5) Uani 1 1 d . . . . .
N2 N 0.01687(11) 0.4599(2) 0.12282(17) 0.0098(4) Uani 1 1 d . . . . .
N3 N -0.04837(11) 0.4114(2) 0.11227(18) 0.0115(5) Uani 1 1 d . . . . .
N4 N -0.15740(11) 0.4491(2) 0.11392(18) 0.0124(5) Uani 1 1 d . . . . .
H14A H -0.187529 0.503198 0.118950 0.015 Uiso 1 1 d R U . . .
N5 N 0.04416(12) 0.2378(2) 0.11919(19) 0.0150(5) Uani 1 1 d . . . . .
H16A H 0.009413 0.210305 0.125314 0.018 Uiso 1 1 d R U . . .
H16B H 0.076813 0.178705 0.122114 0.018 Uiso 1 1 d R U . . .
C1 C 0.20755(14) 0.5717(3) 0.1514(2) 0.0146(6) Uani 1 1 d . . . . .
H11 H 0.216872 0.661897 0.164359 0.017 Uiso 1 1 d R U . . .
C2 C 0.25994(15) 0.4883(3) 0.1416(2) 0.0177(6) Uani 1 1 d . . . . .
H12 H 0.304067 0.520281 0.147137 0.021 Uiso 1 1 d R U . . .
C3 C 0.24564(15) 0.3575(3) 0.1237(2) 0.0179(6) Uani 1 1 d . . . . .
H13 H 0.280119 0.297730 0.115804 0.022 Uiso 1 1 d R U . . .
C4 C 0.18121(15) 0.3135(3) 0.1171(2) 0.0175(6) Uani 1 1 d . . . . .
H14 H 0.170969 0.223384 0.105409 0.021 Uiso 1 1 d R U . . .
C5 C 0.13129(14) 0.4032(3) 0.1281(2) 0.0117(5) Uani 1 1 d . . . . .
C6 C 0.06078(14) 0.3653(3) 0.1232(2) 0.0117(5) Uani 1 1 d . . . . .
C7 C -0.09424(14) 0.4949(3) 0.1249(2) 0.0108(5) Uani 1 1 d . . . . .
C8 C -0.17339(14) 0.3119(3) 0.0971(2) 0.0152(5) Uani 1 1 d . . . . .
H18A H -0.156797 0.281120 0.034004 0.023 Uiso 1 1 d R U . . .
H18B H -0.152497 0.261420 0.158864 0.023 Uiso 1 1 d R U . . .
H18C H -0.221687 0.300330 0.087064 0.023 Uiso 1 1 d R U . . .
S2 S 0.15514(4) 1.04372(7) 0.61775(6) 0.01655(15) Uani 1 1 d . . . . .
N6 N 0.07446(13) 1.0357(3) 0.4168(2) 0.0230(6) Uani 1 1 d . . . . .
C9 C 0.10801(15) 1.0386(3) 0.5001(2) 0.0160(6) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
S S 0.1246 0.1234 '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
N2 Pb N1 64.71(7) . . ?
N2 Pb S1 87.39(5) . 2 ?
N1 Pb S1 77.54(5) . 2 ?
N2 Pb S1 69.33(5) . . ?
N1 Pb S1 132.57(5) . . ?
S1 Pb S1 89.50(2) 2 . ?
N2 Pb O1W 126.70(6) . . ?
N1 Pb O1W 139.49(5) . . ?
S1 Pb O1W 65.65(3) 2 . ?
S1 Pb O1W 65.61(3) . . ?
N2 Pb Pb 82.04(5) . 2 ?
N1 Pb Pb 115.18(5) . 2 ?
S1 Pb Pb 45.421(14) 2 2 ?
S1 Pb Pb 45.362(14) . 2 ?
O1W Pb Pb 45.92(4) . 2 ?
C7 S1 Pb 107.06(9) . 2 ?
C7 S1 Pb 98.75(9) . . ?
Pb S1 Pb 89.217(19) 2 . ?
C7 S1 S1 99.74(9) . 2 ?
Pb S1 S1 45.277(14) 2 2 ?
Pb S1 S1 45.218(14) . 2 ?
Pb O1W H1A 130.4 . . ?
C1 N1 C5 119.2(2) . . ?
C1 N1 Pb 121.63(19) . . ?
C5 N1 Pb 118.51(18) . . ?
C6 N2 N3 112.0(2) . . ?
C6 N2 Pb 122.26(18) . . ?
N3 N2 Pb 125.61(16) . . ?
C7 N3 N2 116.7(2) . . ?
C7 N4 C8 122.4(2) . . ?
C7 N4 H14A 117.6 . . ?
C8 N4 H14A 120.0 . . ?
C6 N5 H16A 125.0 . . ?
C6 N5 H16B 118.0 . . ?
H16A N5 H16B 115.9 . . ?
N1 C1 C2 123.1(3) . . ?
N1 C1 H11 118.4 . . ?
C2 C1 H11 118.4 . . ?
C3 C2 C1 117.7(3) . . ?
C3 C2 H12 121.2 . . ?
C1 C2 H12 121.1 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H13 120.0 . . ?
C4 C3 H13 120.0 . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 H14 120.5 . . ?
C5 C4 H14 120.5 . . ?
N1 C5 C4 121.0(3) . . ?
N1 C5 C6 116.0(2) . . ?
C4 C5 C6 123.1(3) . . ?
N2 C6 N5 122.9(3) . . ?
N2 C6 C5 117.7(2) . . ?
N5 C6 C5 119.4(2) . . ?
N3 C7 N4 117.0(2) . . ?
N3 C7 S1 128.1(2) . . ?
N4 C7 S1 114.8(2) . . ?
N4 C8 H18A 109.5 . . ?
N4 C8 H18B 109.5 . . ?
H18A C8 H18B 109.5 . . ?
N4 C8 H18C 109.5 . . ?
H18A C8 H18C 109.5 . . ?
H18B C8 H18C 109.5 . . ?
N6 C9 S2 179.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb N2 2.465(2) . ?
Pb N1 2.556(2) . ?
Pb S1 2.8139(7) 2 ?
Pb S1 2.8168(7) . ?
Pb O1W 2.842(2) . ?
Pb Pb 3.9542(3) 2 ?
S1 C7 1.761(3) . ?
S1 S1 3.9642(14) 2 ?
O1W H1A 1.0258 . ?
N1 C1 1.327(4) . ?
N1 C5 1.347(3) . ?
N2 C6 1.318(3) . ?
N2 N3 1.406(3) . ?
N3 C7 1.297(3) . ?
N4 C7 1.356(3) . ?
N4 C8 1.447(3) . ?
N4 H14A 0.8373 . ?
N5 C6 1.345(4) . ?
N5 H16A 0.7792 . ?
N5 H16B 0.8952 . ?
C1 C2 1.390(4) . ?
C1 H11 0.9500 . ?
C2 C3 1.379(4) . ?
C2 H12 0.9499 . ?
C3 C4 1.379(4) . ?
C3 H13 0.9499 . ?
C4 C5 1.395(4) . ?
C4 H14 0.9499 . ?
C5 C6 1.482(4) . ?
C8 H18A 0.9800 . ?
C8 H18B 0.9801 . ?
C8 H18C 0.9800 . ?
S2 C9 1.646(3) . ?
N6 C9 1.167(4) . ?
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
_geom_torsion_publ_flag
C6 N2 N3 C7 171.2(2) . . . . ?
Pb N2 N3 C7 -12.4(3) . . . . ?
C5 N1 C1 C2 1.8(4) . . . . ?
Pb N1 C1 C2 -168.9(2) . . . . ?
N1 C1 C2 C3 -0.5(4) . . . . ?
C1 C2 C3 C4 -0.7(4) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C1 N1 C5 C4 -1.9(4) . . . . ?
Pb N1 C5 C4 169.0(2) . . . . ?
C1 N1 C5 C6 178.3(2) . . . . ?
Pb N1 C5 C6 -10.8(3) . . . . ?
C3 C4 C5 N1 0.8(4) . . . . ?
C3 C4 C5 C6 -179.4(3) . . . . ?
N3 N2 C6 N5 -3.1(4) . . . . ?
Pb N2 C6 N5 -179.53(19) . . . . ?
N3 N2 C6 C5 176.8(2) . . . . ?
Pb N2 C6 C5 0.3(3) . . . . ?
N1 C5 C6 N2 7.1(4) . . . . ?
C4 C5 C6 N2 -172.7(3) . . . . ?
N1 C5 C6 N5 -173.0(2) . . . . ?
C4 C5 C6 N5 7.2(4) . . . . ?
N2 N3 C7 N4 179.4(2) . . . . ?
N2 N3 C7 S1 1.7(4) . . . . ?
C8 N4 C7 N3 4.7(4) . . . . ?
C8 N4 C7 S1 -177.2(2) . . . . ?
Pb S1 C7 N3 -85.1(3) 2 . . . ?
Pb S1 C7 N3 6.8(3) . . . . ?
S1 S1 C7 N3 -39.0(3) 2 . . . ?
Pb S1 C7 N4 97.16(19) 2 . . . ?
Pb S1 C7 N4 -170.97(18) . . . . ?
S1 S1 C7 N4 143.20(18) 2 . . . ?
