#------------------------------------------------------------------------------
#$Date: 2022-02-04 21:23:32 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272624 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243735.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_7243735
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         'C12 H14 N12 Pb2 S2, 2(N O3)'
_chemical_formula_sum            'C12 H14 N14 O6 Pb2 S2'
_chemical_formula_weight         928.87
_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   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                89.660(4)
_cell_angle_beta                 76.812(4)
_cell_angle_gamma                71.301(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1834(8)
_cell_length_b                   7.7618(8)
_cell_length_c                   10.8730(12)
_cell_measurement_reflns_used    9273
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.65
_cell_measurement_theta_min      2.78
_cell_volume                     557.61(11)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0564
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            55573
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.502
_diffrn_reflns_theta_min         2.778
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    15.330
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.766
_exptl_crystal_description       prism
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0144
_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)+(0.0028P)²+0.8722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0280
_refine_ls_wR_factor_ref         0.0289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3190
_reflns_number_total             3395
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01251g1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7243734--7243737.cif.'
_cod_database_code               7243735
_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   0.339
_shelx_estimated_absorpt_t_max   0.579
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
Pb Pb -0.11886(2) 0.82493(2) -0.07072(2) 0.00920(3) Uani 1 1 d . . . . .
S1 S 0.16495(8) 1.00353(8) -0.16693(5) 0.00937(10) Uani 1 1 d . . . . .
N1 N 0.2250(3) 1.0531(3) 0.27632(18) 0.0103(4) Uani 1 1 d . . . . .
N2 N 0.3671(3) 0.8701(3) 0.04371(18) 0.0092(4) Uani 1 1 d . . . . .
N3 N 0.4687(3) 0.7691(3) -0.07241(18) 0.0106(4) Uani 1 1 d . . . . .
N4 N 0.4681(3) 0.7128(3) -0.2779(2) 0.0126(4) Uani 1 1 d . . . . .
H4A H 0.577(5) 0.619(4) -0.287(3) 0.015 Uiso 1 1 d . U . . .
H4B H 0.431(5) 0.744(4) -0.340(3) 0.015 Uiso 1 1 d . U . . .
N5 N 0.6034(3) 0.6366(3) 0.1169(2) 0.0123(4) Uani 1 1 d . . . . .
H5A H 0.643(4) 0.570(4) 0.047(3) 0.015 Uiso 1 1 d . U . . .
H5B H 0.661(4) 0.604(4) 0.171(3) 0.015 Uiso 1 1 d . U . . .
N6 N 0.3438(3) 0.8901(3) 0.48713(19) 0.0143(4) Uani 1 1 d . . . . .
C1 C 0.1482(4) 1.1393(3) 0.3919(2) 0.0130(4) Uani 1 1 d . . . . .
H1 H 0.049130 1.262172 0.394505 0.016 Uiso 1 1 d R U . . .
C2 C 0.2082(4) 1.0581(3) 0.4968(2) 0.0140(5) Uani 1 1 d . . . . .
H2 H 0.154676 1.123051 0.581800 0.017 Uiso 1 1 d R U . . .
C4 C 0.4214(4) 0.8056(3) 0.3712(2) 0.0127(4) Uani 1 1 d . . . . .
H4 H 0.529027 0.685221 0.365537 0.015 Uiso 1 1 d R U . . .
C5 C 0.3641(3) 0.8857(3) 0.2647(2) 0.0093(4) Uani 1 1 d . . . . .
C6 C 0.4478(3) 0.7937(3) 0.1360(2) 0.0094(4) Uani 1 1 d . . . . .
C7 C 0.3831(3) 0.8154(3) -0.1676(2) 0.0091(4) Uani 1 1 d . . . . .
N7 N 0.0456(3) 0.5663(3) 0.2287(2) 0.0129(4) Uani 1 1 d . . . . .
O1 O 0.0953(3) 0.5824(2) 0.11198(17) 0.0183(4) Uani 1 1 d . . . . .
O2 O -0.1013(3) 0.5092(3) 0.27212(18) 0.0203(4) Uani 1 1 d . . . . .
O3 O 0.1413(3) 0.6028(3) 0.30191(19) 0.0216(4) 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 65.25(6) 2_575 2_575 ?
N2 Pb S1 69.03(5) 2_575 2_575 ?
N1 Pb S1 132.78(4) 2_575 2_575 ?
N2 Pb S1 84.63(5) 2_575 . ?
N1 Pb S1 78.28(4) 2_575 . ?
S1 Pb S1 86.508(17) 2_575 . ?
N2 Pb Pb 71.97(5) 2_575 2_575 ?
N1 Pb Pb 108.99(4) 2_575 2_575 ?
S1 Pb Pb 43.368(12) 2_575 2_575 ?
S1 Pb Pb 43.140(12) . 2_575 ?
C7 S1 Pb 98.74(8) . 2_575 ?
C7 S1 Pb 96.36(8) . . ?
Pb S1 Pb 93.492(17) 2_575 . ?
C7 S1 S1 101.05(8) . 2_575 ?
Pb S1 S1 46.875(13) 2_575 2_575 ?
Pb S1 S1 46.617(13) . 2_575 ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Pb 125.62(15) . 2_575 ?
C5 N1 Pb 116.43(15) . 2_575 ?
C6 N2 N3 111.05(18) . . ?
C6 N2 Pb 122.46(15) . 2_575 ?
N3 N2 Pb 125.50(13) . 2_575 ?
C7 N3 N2 116.52(19) . . ?
C7 N4 H4A 122(2) . . ?
C7 N4 H4B 121(2) . . ?
H4A N4 H4B 116(3) . . ?
C6 N5 H5A 122(2) . . ?
C6 N5 H5B 119(2) . . ?
H5A N5 H5B 119(3) . . ?
C4 N6 C2 116.8(2) . . ?
N1 C1 C2 121.1(2) . . ?
N1 C1 H1 114.4 . . ?
C2 C1 H1 124.6 . . ?
N6 C2 C1 121.7(2) . . ?
N6 C2 H2 117.1 . . ?
C1 C2 H2 121.2 . . ?
N6 C4 C5 122.2(2) . . ?
N6 C4 H4 115.3 . . ?
C5 C4 H4 122.4 . . ?
N1 C5 C4 120.3(2) . . ?
N1 C5 C6 116.9(2) . . ?
C4 C5 C6 122.8(2) . . ?
N2 C6 N5 122.4(2) . . ?
N2 C6 C5 118.4(2) . . ?
N5 C6 C5 119.2(2) . . ?
N3 C7 N4 118.1(2) . . ?
N3 C7 S1 126.34(18) . . ?
N4 C7 S1 115.52(17) . . ?
O3 N7 O1 120.9(2) . . ?
O3 N7 O2 119.8(2) . . ?
O1 N7 O2 119.3(2) . . ?
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 2.4354(19) 2_575 ?
Pb N1 2.6009(19) 2_575 ?
Pb S1 2.8155(6) 2_575 ?
Pb S1 2.8274(6) . ?
Pb Pb 4.1099(3) 2_575 ?
S1 C7 1.765(2) . ?
S1 S1 3.8667(12) 2_575 ?
N1 C1 1.337(3) . ?
N1 C5 1.347(3) . ?
N2 C6 1.317(3) . ?
N2 N3 1.402(3) . ?
N3 C7 1.312(3) . ?
N4 C7 1.346(3) . ?
N4 H4A 0.87(3) . ?
N4 H4B 0.79(3) . ?
N5 C6 1.342(3) . ?
N5 H5A 0.86(3) . ?
N5 H5B 0.79(3) . ?
N6 C4 1.336(3) . ?
N6 C2 1.342(3) . ?
C1 C2 1.387(3) . ?
C1 H1 0.9863 . ?
C2 H2 0.9877 . ?
C4 C5 1.393(3) . ?
C4 H4 0.9952 . ?
C5 C6 1.477(3) . ?
N7 O3 1.251(3) . ?
N7 O1 1.254(3) . ?
N7 O2 1.266(3) . ?
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
_geom_hbond_publ_flag
N4 H4A O3 0.87(3) 2.17(3) 3.034(3) 175(3) 2_665 yes
N4 H4B N6 0.79(3) 2.29(3) 3.071(3) 167(3) 1_554 yes
N5 H5A O1 0.86(3) 2.25(3) 3.000(3) 147(3) 2_665 yes
N5 H5B O2 0.79(3) 2.17(3) 2.932(3) 162(3) 1_655 yes
C1 H1 O2 0.99 2.43 3.298(3) 146.3 1_565 yes
C2 H2 S1 0.99 2.89 3.632(2) 132.7 1_556 yes
C2 H2 O3 0.99 2.56 3.368(3) 139.0 2_576 yes
C4 H4 O2 1.00 2.53 3.390(3) 144.3 1_655 yes
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 169.7(2) . . . . ?
Pb N2 N3 C7 -21.5(3) 2_575 . . . ?
C5 N1 C1 C2 -0.7(3) . . . . ?
Pb N1 C1 C2 176.71(17) 2_575 . . . ?
C4 N6 C2 C1 1.2(4) . . . . ?
N1 C1 C2 N6 -0.5(4) . . . . ?
C2 N6 C4 C5 -0.7(4) . . . . ?
C1 N1 C5 C4 1.2(3) . . . . ?
Pb N1 C5 C4 -176.46(17) 2_575 . . . ?
C1 N1 C5 C6 -179.6(2) . . . . ?
Pb N1 C5 C6 2.8(3) 2_575 . . . ?
N6 C4 C5 N1 -0.5(4) . . . . ?
N6 C4 C5 C6 -179.7(2) . . . . ?
N3 N2 C6 N5 -1.8(3) . . . . ?
Pb N2 C6 N5 -170.95(17) 2_575 . . . ?
N3 N2 C6 C5 177.85(19) . . . . ?
Pb N2 C6 C5 8.7(3) 2_575 . . . ?
N1 C5 C6 N2 -7.4(3) . . . . ?
C4 C5 C6 N2 171.8(2) . . . . ?
N1 C5 C6 N5 172.3(2) . . . . ?
C4 C5 C6 N5 -8.5(3) . . . . ?
N2 N3 C7 N4 -175.0(2) . . . . ?
N2 N3 C7 S1 5.6(3) . . . . ?
Pb S1 C7 N3 8.2(2) 2_575 . . . ?
Pb S1 C7 N3 -86.4(2) . . . . ?
S1 S1 C7 N3 -39.4(2) 2_575 . . . ?
Pb S1 C7 N4 -171.18(17) 2_575 . . . ?
Pb S1 C7 N4 94.28(17) . . . . ?
S1 S1 C7 N4 141.25(17) 2_575 . . . ?
