#------------------------------------------------------------------------------
#$Date: 2024-04-05 02:09:01 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290896 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/81/7248135.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_7248135
loop_
_publ_author_name
'Eftekhari-Sis, Bagher'
'García-Santos, Isabel'
'Castiñeiras, Alfonso'
'Mahmoudi, Ghodrat'
'Zangrando, Ennio'
'Frontera, Antonio'
'Safin, Damir A.'
_publ_section_title
;
 On the pivotal role of tetrel bonding in the supramolecular architectures
 of PbII--NCS complexes with chelating thiosemicarbazide derivatives
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1637
_journal_page_last               1646
_journal_paper_doi               10.1039/D3CE01207G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C7 H7 N7 Pb S2'
_chemical_formula_sum            'C7 H7 N7 Pb S2'
_chemical_formula_weight         460.51
_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
;
2023-11-29 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                97.201(3)
_cell_angle_beta                 93.084(2)
_cell_angle_gamma                107.496(2)
_cell_formula_units_Z            2
_cell_length_a                   6.9411(4)
_cell_length_b                   8.1607(5)
_cell_length_c                   10.8395(7)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.97
_cell_measurement_theta_min      2.64
_cell_volume                     578.25(6)
_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 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  0.0740
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69028
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.195
_diffrn_reflns_theta_min         2.646
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    14.937
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.645
_exptl_crystal_description       prism
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.035
_refine_diff_density_min         -1.568
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0206
_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)+1.2805P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0313
_refine_ls_wR_factor_ref         0.0337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4004
_reflns_number_total             4430
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01207g1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7248133--7248135.cif.'
_cod_database_code               7248135
_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   0.663
_shelx_estimated_absorpt_t_max   0.754
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 0.14409(2) 0.33240(2) 0.41962(2) 0.00874(2) Uani 1 1 d . . . . .
S1 S 0.16175(9) 0.51275(8) 0.65931(6) 0.01002(11) Uani 1 1 d . . . . .
S2 S -0.01743(11) 0.04167(10) 0.81336(7) 0.01859(14) Uani 1 1 d . . . . .
N7 N -0.1230(3) 0.1211(3) 0.5784(2) 0.0159(5) Uani 1 1 d . . . . .
N1 N 0.2603(3) 0.4630(3) 0.2088(2) 0.0107(4) Uani 1 1 d . . . . .
N2 N 0.3892(3) 0.6301(3) 0.4440(2) 0.0091(4) Uani 1 1 d . . . . .
N3 N 0.4818(3) 0.7260(3) 0.5600(2) 0.0103(4) Uani 1 1 d . . . . .
N4 N 0.4585(3) 0.7904(3) 0.7678(2) 0.0129(4) Uani 1 1 d . . . . .
H14A H 0.583315 0.871135 0.768187 0.015 Uiso 1 1 d R U . . .
H14B H 0.421947 0.753723 0.830201 0.015 Uiso 1 1 d R U . . .
N6 N 0.6022(3) 0.8695(3) 0.3683(2) 0.0126(4) Uani 1 1 d . . . . .
H15A H 0.649990 0.922239 0.442036 0.015 Uiso 1 1 d R U . . .
H15B H 0.665291 0.901035 0.311032 0.015 Uiso 1 1 d R U . . .
N5 N 0.3439(4) 0.6400(3) 0.0044(2) 0.0144(4) Uani 1 1 d . . . . .
C7 C -0.0792(4) 0.0909(3) 0.6767(3) 0.0133(5) Uani 1 1 d . . . . .
C1 C 0.1828(4) 0.3870(3) 0.0931(2) 0.0127(5) Uani 1 1 d . . . . .
H11 H 0.098036 0.272644 0.080286 0.015 Uiso 1 1 d R U . . .
C2 C 0.2259(4) 0.4751(4) -0.0086(2) 0.0137(5) Uani 1 1 d . . . . .
H12 H 0.171061 0.417505 -0.088168 0.016 Uiso 1 1 d R U . . .
C3 C 0.4208(4) 0.7157(4) 0.1208(2) 0.0137(5) Uani 1 1 d . . . . .
H14 H 0.503398 0.830727 0.133467 0.016 Uiso 1 1 d R U . . .
C4 C 0.3816(4) 0.6281(3) 0.2235(2) 0.0091(4) Uani 1 1 d . . . . .
C5 C 0.4637(4) 0.7120(3) 0.3524(2) 0.0098(5) Uani 1 1 d . . . . .
C6 C 0.3826(4) 0.6874(3) 0.6569(2) 0.0090(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'
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 62.68(7) . . ?
N2 Pb N3 76.97(6) . 2_666 ?
N1 Pb N3 86.11(6) . 2_666 ?
N2 Pb S1 68.48(5) . . ?
N1 Pb S1 128.33(5) . . ?
N3 Pb S1 98.81(5) 2_666 . ?
N2 Pb S1 86.35(5) . 2_566 ?
N1 Pb S1 73.68(5) . 2_566 ?
N3 Pb S1 158.20(5) 2_666 2_566 ?
S1 Pb S1 87.768(19) . 2_566 ?
N2 Pb N7 136.32(7) . . ?
N1 Pb N7 157.25(7) . . ?
N3 Pb N7 108.67(6) 2_666 . ?
S1 Pb N7 67.85(5) . . ?
S1 Pb N7 93.08(5) 2_566 . ?
N2 Pb Pb 72.89(5) . 2_566 ?
N1 Pb Pb 102.83(5) . 2_566 ?
N3 Pb Pb 139.61(4) 2_666 2_566 ?
S1 Pb Pb 45.054(13) . 2_566 ?
S1 Pb Pb 42.714(13) 2_566 2_566 ?
N7 Pb Pb 77.41(5) . 2_566 ?
N2 Pb Pb 38.54(5) . 2_666 ?
N1 Pb Pb 82.49(5) . 2_666 ?
N3 Pb Pb 42.34(4) 2_666 2_666 ?
S1 Pb Pb 69.108(13) . 2_666 ?
S1 Pb Pb 124.474(13) 2_566 2_666 ?
N7 Pb Pb 120.14(5) . 2_666 ?
Pb Pb Pb 99.139(6) 2_566 2_666 ?
C6 S1 Pb 99.54(8) . . ?
C6 S1 Pb 99.87(8) . 2_566 ?
Pb S1 Pb 92.231(19) . 2_566 ?
C7 N7 Pb 127.51(19) . . ?
C1 N1 C4 117.5(2) . . ?
C1 N1 Pb 125.10(17) . . ?
C4 N1 Pb 116.51(16) . . ?
C5 N2 N3 110.8(2) . . ?
C5 N2 Pb 125.40(17) . . ?
N3 N2 Pb 123.51(15) . . ?
C6 N3 N2 116.2(2) . . ?
C6 N3 Pb 111.42(16) . 2_666 ?
N2 N3 Pb 103.70(13) . 2_666 ?
C6 N4 H14A 115.5 . . ?
C6 N4 H14B 118.1 . . ?
H14A N4 H14B 120.8 . . ?
C5 N6 H15A 120.1 . . ?
C5 N6 H15B 119.2 . . ?
H15A N6 H15B 118.0 . . ?
C2 N5 C3 116.4(2) . . ?
N7 C7 S2 178.1(2) . . ?
N1 C1 C2 121.4(2) . . ?
N1 C1 H11 119.3 . . ?
C2 C1 H11 119.3 . . ?
N5 C2 C1 121.9(2) . . ?
N5 C2 H12 119.0 . . ?
C1 C2 H12 119.1 . . ?
N5 C3 C4 122.3(2) . . ?
N5 C3 H14 118.8 . . ?
C4 C3 H14 118.9 . . ?
N1 C4 C3 120.4(2) . . ?
N1 C4 C5 117.0(2) . . ?
C3 C4 C5 122.5(2) . . ?
N2 C5 N6 124.2(2) . . ?
N2 C5 C4 117.6(2) . . ?
N6 C5 C4 118.1(2) . . ?
N3 C6 N4 117.2(2) . . ?
N3 C6 S1 126.6(2) . . ?
N4 C6 S1 116.18(18) . . ?
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 2.484(2) . ?
Pb N1 2.702(2) . ?
Pb N3 2.780(2) 2_666 ?
Pb S1 2.7982(7) . ?
Pb S1 2.9196(6) 2_566 ?
Pb N7 2.922(2) . ?
Pb Pb 4.1219(3) 2_566 ?
Pb Pb 4.9682(3) 2_666 ?
S1 C6 1.756(3) . ?
S2 C7 1.650(3) . ?
N7 C7 1.169(4) . ?
N1 C1 1.334(3) . ?
N1 C4 1.342(3) . ?
N2 C5 1.309(3) . ?
N2 N3 1.404(3) . ?
N3 C6 1.306(3) . ?
N4 C6 1.357(3) . ?
N4 H14A 0.9165 . ?
N4 H14B 0.7968 . ?
N6 C5 1.338(3) . ?
N6 H15A 0.8562 . ?
N6 H15B 0.8031 . ?
N5 C2 1.334(3) . ?
N5 C3 1.339(3) . ?
C1 C2 1.388(4) . ?
C1 H11 0.9300 . ?
C2 H12 0.9300 . ?
C3 C4 1.392(4) . ?
C3 H14 0.9300 . ?
C4 C5 1.479(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 H14A S2 0.92 2.69 3.570(2) 162.1 1_665 yes
N4 H14B N5 0.80 2.23 3.023(3) 174.5 1_556 yes
N6 H15B S2 0.80 2.80 3.524(2) 151.2 2_666 yes
C1 H11 S2 0.93 2.86 3.631(3) 141.3 2_556 yes
C2 H12 S1 0.93 2.94 3.666(3) 135.9 1_554 yes
C2 H12 S2 0.93 2.98 3.665(3) 131.8 1_554 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
C5 N2 N3 C6 159.9(2) . . . . ?
Pb N2 N3 C6 -25.9(3) . . . . ?
C5 N2 N3 Pb -77.46(19) . . . 2_666 ?
Pb N2 N3 Pb 96.72(14) . . . 2_666 ?
C4 N1 C1 C2 0.1(4) . . . . ?
Pb N1 C1 C2 169.06(19) . . . . ?
C3 N5 C2 C1 0.8(4) . . . . ?
N1 C1 C2 N5 -1.0(4) . . . . ?
C2 N5 C3 C4 0.3(4) . . . . ?
C1 N1 C4 C3 1.0(4) . . . . ?
Pb N1 C4 C3 -168.94(19) . . . . ?
C1 N1 C4 C5 178.9(2) . . . . ?
Pb N1 C4 C5 9.0(3) . . . . ?
N5 C3 C4 N1 -1.2(4) . . . . ?
N5 C3 C4 C5 -179.0(2) . . . . ?
N3 N2 C5 N6 -3.0(3) . . . . ?
Pb N2 C5 N6 -177.01(18) . . . . ?
N3 N2 C5 C4 -179.9(2) . . . . ?
Pb N2 C5 C4 6.1(3) . . . . ?
N1 C4 C5 N2 -10.1(3) . . . . ?
C3 C4 C5 N2 167.8(2) . . . . ?
N1 C4 C5 N6 172.8(2) . . . . ?
C3 C4 C5 N6 -9.3(4) . . . . ?
N2 N3 C6 N4 -173.2(2) . . . . ?
Pb N3 C6 N4 68.3(2) 2_666 . . . ?
N2 N3 C6 S1 7.9(3) . . . . ?
Pb N3 C6 S1 -110.61(19) 2_666 . . . ?
Pb S1 C6 N3 9.2(2) . . . . ?
Pb S1 C6 N3 -84.8(2) 2_566 . . . ?
Pb S1 C6 N4 -169.67(18) . . . . ?
Pb S1 C6 N4 96.35(19) 2_566 . . . ?
