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#$Date: 2024-04-05 02:09:01 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290896 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/81/7248133.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_7248133
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         'C20  H15  N5  Pb1  S2'
_chemical_formula_sum            'C20 H15 N5 Pb S2'
_chemical_formula_weight         596.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 98.331(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6513(12)
_cell_length_b                   19.384(4)
_cell_length_c                   18.237(4)
_cell_measurement_reflns_used    4457
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.38
_cell_volume                     1976.7(7)
_computing_cell_refinement       'APEX3 Software (Bruker, 2019)'
_computing_data_collection       'APEX3 Software (Bruker, 2019)'
_computing_data_reduction        'APEX3 Software (Bruker, 2019)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.986
_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  0.1483
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29693
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.340
_diffrn_reflns_theta_min         2.385
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    8.762
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
_refine_diff_density_max         6.893
_refine_diff_density_min         -6.925
_refine_diff_density_rms         0.504
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3558
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.1221
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1014P)²+198.1175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2664
_refine_ls_wR_factor_ref         0.2754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3040
_reflns_number_total             3558
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01207g1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7248133--7248135.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7248133
_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   0.344
_shelx_estimated_absorpt_t_max   0.851
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.76023(16) 0.41811(5) 0.46935(5) 0.0154(3) Uani 1 1 d . . . . .
S1 S 0.2833(11) 0.4533(3) 0.4303(3) 0.0169(12) Uani 1 1 d . U . . .
S2 S 0.5940(12) 0.3367(4) 0.5886(3) 0.0210(13) Uani 1 1 d . . . . .
N1 N 0.920(4) 0.3075(11) 0.4090(11) 0.0191(15) Uani 1 1 d . . . . .
N2 N 0.587(4) 0.3899(11) 0.3343(11) 0.0167(15) Uani 1 1 d . . . . .
N3 N 0.427(4) 0.4346(11) 0.2946(11) 0.0171(16) Uani 1 1 d . . . . .
N4 N 0.132(4) 0.5138(10) 0.3029(11) 0.0134(19) Uani 1 1 d . U . . .
H4A H 0.044567 0.533439 0.333282 0.016 Uiso 1 1 calc R U . . .
N5 N 0.218(4) 0.4281(13) 0.6000(12) 0.027(4) Uani 1 1 d . . . . .
C1 C 0.375(4) 0.3904(13) 0.5958(13) 0.015(3) Uani 1 1 d . U . . .
C2 C 1.105(5) 0.2736(14) 0.4466(14) 0.021(2) Uani 1 1 d . . . . .
H2 H 1.134676 0.278224 0.499015 0.025 Uiso 1 1 d R U . . .
C3 C 1.253(5) 0.2320(14) 0.4141(14) 0.021(3) Uani 1 1 d . . . . .
H3 H 1.390017 0.211693 0.441951 0.025 Uiso 1 1 d R U . . .
C4 C 1.197(5) 0.2203(14) 0.3364(13) 0.019(3) Uani 1 1 d . . . . .
H4 H 1.281910 0.186982 0.312271 0.022 Uiso 1 1 d R U . . .
C5 C 1.015(4) 0.2582(12) 0.2981(12) 0.013(2) Uani 1 1 d . . . . .
H5 H 0.982732 0.253958 0.245711 0.016 Uiso 1 1 d R U . . .
C6 C 0.879(5) 0.3027(13) 0.3345(13) 0.0168(18) Uani 1 1 d . . . . .
C7 C 0.698(5) 0.3474(14) 0.2954(13) 0.0174(11) Uani 1 1 d . . . . .
C8 C 0.295(4) 0.4660(13) 0.3338(13) 0.0146(17) Uani 1 1 d . . . . .
C9 C 0.087(4) 0.5354(12) 0.2286(13) 0.0121(19) Uani 1 1 d . U . . .
C10 C -0.126(4) 0.5708(13) 0.2076(13) 0.016(3) Uani 1 1 d . . . . .
H10 H -0.226302 0.579287 0.244094 0.019 Uiso 1 1 d R U . . .
C11 C -0.199(5) 0.5943(13) 0.1366(13) 0.017(3) Uani 1 1 d . . . . .
H11 H -0.336639 0.622560 0.125635 0.021 Uiso 1 1 d R U . . .
C12 C -0.061(5) 0.5755(14) 0.0811(13) 0.020(3) Uani 1 1 d . . . . .
H12 H -0.113546 0.586305 0.030516 0.024 Uiso 1 1 d R U . . .
C13 C 0.151(5) 0.5402(14) 0.1022(13) 0.018(3) Uani 1 1 d . . . . .
H13 H 0.250184 0.529749 0.065949 0.022 Uiso 1 1 d R U . . .
C14 C 0.221(4) 0.5204(12) 0.1747(12) 0.012(3) Uani 1 1 d . . . . .
H14 H 0.366657 0.495552 0.186907 0.015 Uiso 1 1 d R U . . .
C15 C 0.652(5) 0.3485(13) 0.2128(13) 0.0174(11) Uani 1 1 d . . . . .
C16 C 0.819(5) 0.3802(14) 0.1759(13) 0.018(3) Uani 1 1 d . . . . .
H16 H 0.965537 0.396606 0.202455 0.022 Uiso 1 1 d R U . . .
C17 C 0.771(5) 0.3887(13) 0.0996(13) 0.015(3) Uani 1 1 d . . . . .
H17 H 0.885083 0.411547 0.074620 0.018 Uiso 1 1 d R U . . .
C18 C 0.565(5) 0.3645(13) 0.0602(14) 0.018(3) Uani 1 1 d . . . . .
H18 H 0.532123 0.372121 0.008234 0.021 Uiso 1 1 d R U . . .
C19 C 0.402(5) 0.3291(15) 0.0965(14) 0.022(3) Uani 1 1 d . . . . .
H19 H 0.261895 0.309262 0.069716 0.026 Uiso 1 1 d R U . . .
C20 C 0.451(5) 0.3232(14) 0.1744(13) 0.020(3) Uani 1 1 d . . . . .
H20 H 0.337950 0.300771 0.200038 0.024 Uiso 1 1 d 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'
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 62.1(7) . . ?
N2 Pb S1 65.5(5) . . ?
N1 Pb S1 118.3(5) . . ?
N2 Pb S2 118.3(5) . . ?
N1 Pb S2 92.2(5) . . ?
S1 Pb S2 85.36(19) . . ?
N2 Pb S1 132.7(5) . 3_666 ?
N1 Pb S1 163.2(5) . 3_666 ?
S1 Pb S1 78.34(19) . 3_666 ?
S2 Pb S1 86.24(18) . 3_666 ?
N2 Pb S1 93.9(5) . 1_655 ?
N1 Pb S1 72.4(5) . 1_655 ?
S1 Pb S1 141.5(2) . 1_655 ?
S2 Pb S1 132.74(17) . 1_655 ?
S1 Pb S1 96.52(16) 3_666 1_655 ?
N2 Pb Pb 123.6(5) . 3_766 ?
N1 Pb Pb 118.6(5) . 3_766 ?
S1 Pb Pb 116.52(14) . 3_766 ?
S2 Pb Pb 117.92(14) . 3_766 ?
S1 Pb Pb 49.16(12) 3_666 3_766 ?
S1 Pb Pb 47.36(11) 1_655 3_766 ?
N2 Pb Pb 102.3(5) . 3_666 ?
N1 Pb Pb 160.1(5) . 3_666 ?
S1 Pb Pb 41.96(13) . 3_666 ?
S2 Pb Pb 84.62(13) . 3_666 ?
S1 Pb Pb 36.38(12) 3_666 3_666 ?
S1 Pb Pb 123.48(12) 1_655 3_666 ?
Pb Pb Pb 79.87(4) 3_766 3_666 ?
C8 S1 Pb 96.5(8) . . ?
C8 S1 Pb 118.9(8) . 3_666 ?
Pb S1 Pb 101.66(19) . 3_666 ?
C1 S2 Pb 92.6(9) . . ?
C2 N1 C6 119(2) . . ?
C2 N1 Pb 118.5(16) . . ?
C6 N1 Pb 117.3(17) . . ?
C7 N2 N3 116(2) . . ?
C7 N2 Pb 120.4(16) . . ?
N3 N2 Pb 119.9(14) . . ?
C8 N3 N2 114(2) . . ?
C8 N4 C9 128(2) . . ?
C8 N4 H4A 116.0 . . ?
C9 N4 H4A 116.0 . . ?
N5 C1 S2 179(2) . . ?
N1 C2 C3 123(2) . . ?
N1 C2 H2 118.6 . . ?
C3 C2 H2 117.9 . . ?
C2 C3 C4 118(2) . . ?
C2 C3 H3 121.2 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 118(2) . . ?
C5 C4 H4 121.3 . . ?
C3 C4 H4 121.1 . . ?
C4 C5 C6 121(2) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.6 . . ?
N1 C6 C5 120(2) . . ?
N1 C6 C7 118(2) . . ?
C5 C6 C7 123(2) . . ?
N2 C7 C6 118(2) . . ?
N2 C7 C15 121(2) . . ?
C6 C7 C15 121(2) . . ?
N3 C8 N4 121(2) . . ?
N3 C8 S1 127(2) . . ?
N4 C8 S1 112.3(17) . . ?
C14 C9 C10 117(2) . . ?
C14 C9 N4 126(2) . . ?
C10 C9 N4 116(2) . . ?
C11 C10 C9 123(2) . . ?
C11 C10 H10 118.4 . . ?
C9 C10 H10 118.2 . . ?
C10 C11 C12 118(2) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 121.3 . . ?
C13 C12 C11 118(2) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C14 C13 C12 122(2) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C9 C14 C13 121(2) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 H14 119.2 . . ?
C20 C15 C16 120(2) . . ?
C20 C15 C7 122(2) . . ?
C16 C15 C7 118(2) . . ?
C15 C16 C17 120(2) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 121(2) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 120(2) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.4 . . ?
C18 C19 C20 118(2) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 H19 120.8 . . ?
C15 C20 C19 122(2) . . ?
C15 C20 H20 119.4 . . ?
C19 C20 H20 118.9 . . ?
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 2.57(2) . ?
Pb N1 2.63(2) . ?
Pb S1 2.771(7) . ?
Pb S2 2.949(7) . ?
Pb S1 3.123(6) 3_666 ?
Pb S1 3.212(6) 1_655 ?
Pb Pb 4.219(2) 3_766 ?
Pb Pb 4.575(2) 3_666 ?
S1 C8 1.79(2) . ?
S2 C1 1.64(2) . ?
N1 C2 1.34(3) . ?
N1 C6 1.35(3) . ?
N2 C7 1.31(3) . ?
N2 N3 1.38(3) . ?
N3 C8 1.26(3) . ?
N4 C8 1.37(3) . ?
N4 C9 1.41(3) . ?
N4 H4A 0.8800 . ?
N5 C1 1.16(3) . ?
C2 C3 1.36(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.42(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.37(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.39(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.45(4) . ?
C7 C15 1.49(3) . ?
C9 C14 1.36(3) . ?
C9 C10 1.39(3) . ?
C10 C11 1.38(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.41(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.38(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.38(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.34(4) . ?
C15 C16 1.38(4) . ?
C16 C17 1.39(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.36(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.39(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.41(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
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
C7 N2 N3 C8 168(2) . . . . ?
Pb N2 N3 C8 -32(3) . . . . ?
C6 N1 C2 C3 -2(4) . . . . ?
Pb N1 C2 C3 -157(2) . . . . ?
N1 C2 C3 C4 -4(4) . . . . ?
C2 C3 C4 C5 8(4) . . . . ?
C3 C4 C5 C6 -5(4) . . . . ?
C2 N1 C6 C5 6(4) . . . . ?
Pb N1 C6 C5 160.6(18) . . . . ?
C2 N1 C6 C7 -172(2) . . . . ?
Pb N1 C6 C7 -17(3) . . . . ?
C4 C5 C6 N1 -2(4) . . . . ?
C4 C5 C6 C7 175(2) . . . . ?
N3 N2 C7 C6 176(2) . . . . ?
Pb N2 C7 C6 17(3) . . . . ?
N3 N2 C7 C15 0(4) . . . . ?
Pb N2 C7 C15 -158.9(18) . . . . ?
N1 C6 C7 N2 0(4) . . . . ?
C5 C6 C7 N2 -177(2) . . . . ?
N1 C6 C7 C15 176(2) . . . . ?
C5 C6 C7 C15 -1(4) . . . . ?
N2 N3 C8 N4 178(2) . . . . ?
N2 N3 C8 S1 -5(3) . . . . ?
C9 N4 C8 N3 -1(4) . . . . ?
C9 N4 C8 S1 -178.2(18) . . . . ?
Pb S1 C8 N3 32(2) . . . . ?
Pb S1 C8 N3 139(2) 3_666 . . . ?
Pb S1 C8 N4 -150.6(16) . . . . ?
Pb S1 C8 N4 -43(2) 3_666 . . . ?
C8 N4 C9 C14 -11(4) . . . . ?
C8 N4 C9 C10 164(2) . . . . ?
C14 C9 C10 C11 -4(4) . . . . ?
N4 C9 C10 C11 -179(2) . . . . ?
C9 C10 C11 C12 6(4) . . . . ?
C10 C11 C12 C13 -6(4) . . . . ?
C11 C12 C13 C14 3(4) . . . . ?
C10 C9 C14 C13 1(4) . . . . ?
N4 C9 C14 C13 175(2) . . . . ?
C12 C13 C14 C9 -1(4) . . . . ?
N2 C7 C15 C20 -74(4) . . . . ?
C6 C7 C15 C20 110(3) . . . . ?
N2 C7 C15 C16 102(3) . . . . ?
C6 C7 C15 C16 -73(3) . . . . ?
C20 C15 C16 C17 3(4) . . . . ?
C7 C15 C16 C17 -173(2) . . . . ?
C15 C16 C17 C18 -2(4) . . . . ?
C16 C17 C18 C19 -2(4) . . . . ?
C17 C18 C19 C20 4(4) . . . . ?
C16 C15 C20 C19 -1(4) . . . . ?
C7 C15 C20 C19 175(3) . . . . ?
C18 C19 C20 C15 -2(4) . . . . ?
