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#$Date: 2024-07-05 18:24:11 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292956 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/84/7248438.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_7248438
loop_
_publ_author_name
'Mahmoudi, Ghodrat'
'García-Santos, Isabel'
'Fernández-Vázquez, Roi'
'Gomila, Rosa M.'
'Castiñeiras, Alfonso'
'Doustkhah, Esmail'
'Zangrando, Ennio'
'Frontera, Antonio'
_publ_section_title
;
 Structural diversity and tetrel bonding significance in lead(ii)
 complexes with pyrazoylisonicotinoylhydrazone and varied anionic
 co-ligands
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              2526
_journal_page_last               2535
_journal_paper_doi               10.1039/D4CE00325J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C12 H9 N7 O Pb S'
_chemical_formula_sum            'C12 H9 N7 O Pb S'
_chemical_formula_weight         506.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2024-03-12 deposited with the CCDC.	2024-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.905(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4135(7)
_cell_length_b                   16.6666(12)
_cell_length_c                   10.1721(7)
_cell_measurement_reflns_used    8805
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.285
_cell_measurement_theta_min      2.355
_cell_volume                     1418.81(18)
_computing_cell_refinement       'APEX4 Software (Bruker, 2022)'
_computing_data_collection       'APEX4 Software (Bruker, 2022)'
_computing_data_reduction        'APEX4 Software (Bruker, 2022)'
_computing_molecular_graphics    'DIAMOND, Brandenburg,K.(1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0577
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24267
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.355
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    12.051
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.371
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0214
_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)+(0.0083P)²+3.2879P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2807
_reflns_number_total             3231
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00325j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7248436--7248439.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7248438
_shelx_shelxl_version_number     2019/2
_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   0.486
_shelx_estimated_absorpt_t_max   0.714
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Pb1 Pb -0.11215(2) -0.03951(2) 0.71351(2) 0.01081(5) Uani 1 1 d . . . . .
S1 S 0.13839(14) 0.15850(6) 1.01596(11) 0.0225(2) Uani 1 1 d . . . . .
O1 O -0.2712(3) 0.04908(15) 0.5774(2) 0.0132(6) Uani 1 1 d . . . . .
N1 N 0.2056(4) -0.03660(19) 0.7955(3) 0.0114(6) Uani 1 1 d . . . . .
N2 N 0.0407(4) 0.05865(18) 0.6132(3) 0.0093(6) Uani 1 1 d . . . . .
N3 N -0.0403(4) 0.11616(19) 0.5304(3) 0.0113(6) Uani 1 1 d . . . . .
N4 N 0.5394(4) -0.0287(2) 0.8250(3) 0.0160(7) Uani 1 1 d . . . . .
N5 N 0.2529(4) 0.1481(2) 0.6220(4) 0.0142(7) Uani 1 1 d . . . . .
H15A H 0.192(6) 0.179(3) 0.582(4) 0.017 Uiso 1 1 d . U . . .
H15B H 0.325(6) 0.162(3) 0.656(4) 0.017 Uiso 1 1 d . U . . .
N6 N -0.4844(4) 0.2728(2) 0.2816(3) 0.0151(7) Uani 1 1 d . . . . .
N7 N -0.0935(4) 0.0630(2) 0.8763(3) 0.0159(7) Uani 1 1 d . . . . .
C1 C 0.2938(5) -0.0892(2) 0.8705(4) 0.0138(8) Uani 1 1 d . . . . .
H1 H 0.242412 -0.130701 0.914294 0.017 Uiso 1 1 d R U . . .
C2 C 0.4601(5) -0.0842(2) 0.8853(4) 0.0155(8) Uani 1 1 d . . . . .
H2 H 0.518996 -0.122041 0.940773 0.019 Uiso 1 1 d R U . . .
C3 C 0.4499(5) 0.0248(2) 0.7521(4) 0.0139(8) Uani 1 1 d . . . . .
H3 H 0.501413 0.066274 0.708561 0.017 Uiso 1 1 d R U . . .
C4 C 0.2846(5) 0.0214(2) 0.7383(3) 0.0101(8) Uani 1 1 d . . . . .
C5 C 0.1869(5) 0.0803(2) 0.6533(3) 0.0111(8) Uani 1 1 d . . . . .
C6 C -0.1964(4) 0.1044(2) 0.5199(3) 0.0096(7) Uani 1 1 d . . . . .
C7 C -0.2940(5) 0.1635(2) 0.4359(3) 0.0098(8) Uani 1 1 d . . . . .
C8 C -0.2259(5) 0.2259(2) 0.3703(4) 0.0145(8) Uani 1 1 d . . . . .
H8 H -0.113180 0.232483 0.377161 0.017 Uiso 1 1 d R U . . .
C9 C -0.3252(5) 0.2781(2) 0.2948(4) 0.0172(9) Uani 1 1 d . . . . .
H9 H -0.277354 0.320240 0.249634 0.021 Uiso 1 1 d R U . . .
C10 C -0.5485(5) 0.2128(2) 0.3456(4) 0.0154(8) Uani 1 1 d . . . . .
H10 H -0.661641 0.208062 0.337537 0.018 Uiso 1 1 d R U . . .
C11 C -0.4593(5) 0.1572(2) 0.4229(4) 0.0149(8) Uani 1 1 d . . . . .
H11 H -0.510484 0.115423 0.466133 0.018 Uiso 1 1 d R U . . .
C12 C 0.0057(5) 0.1023(2) 0.9337(4) 0.0152(8) 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
O1 Pb1 N7 87.21(10) . . ?
O1 Pb1 N2 67.30(10) . . ?
N7 Pb1 N2 78.70(11) . . ?
O1 Pb1 N1 130.76(9) . . ?
N7 Pb1 N1 77.34(11) . . ?
N2 Pb1 N1 63.93(10) . . ?
O1 Pb1 N3 92.52(8) . 3_556 ?
N7 Pb1 N3 146.26(10) . 3_556 ?
N2 Pb1 N3 70.21(9) . 3_556 ?
N1 Pb1 N3 77.47(8) . 3_556 ?
O1 Pb1 N4 72.03(9) . 1_455 ?
N7 Pb1 N4 73.39(10) . 1_455 ?
N2 Pb1 N4 131.17(9) . 1_455 ?
N1 Pb1 N4 141.70(8) . 1_455 ?
N3 Pb1 N4 138.17(8) 3_556 1_455 ?
O1 Pb1 S1 139.48(7) . 3_557 ?
N7 Pb1 S1 82.01(8) . 3_557 ?
N2 Pb1 S1 145.92(8) . 3_557 ?
N1 Pb1 S1 84.62(7) . 3_557 ?
N3 Pb1 S1 117.40(6) 3_556 3_557 ?
N4 Pb1 S1 67.45(6) 1_455 3_557 ?
O1 Pb1 N2 68.61(8) . 3_556 ?
N7 Pb1 N2 137.11(9) . 3_556 ?
N2 Pb1 N2 59.64(11) . 3_556 ?
N1 Pb1 N2 91.93(8) . 3_556 ?
N3 Pb1 N2 24.02(7) 3_556 3_556 ?
N4 Pb1 N2 126.35(8) 1_455 3_556 ?
S1 Pb1 N2 138.90(5) 3_557 3_556 ?
C6 O1 Pb1 116.2(2) . . ?
C1 N1 C4 116.8(3) . . ?
C1 N1 Pb1 129.4(3) . . ?
C4 N1 Pb1 113.3(2) . . ?
C5 N2 N3 112.4(3) . . ?
C5 N2 Pb1 126.2(2) . . ?
N3 N2 Pb1 118.5(2) . . ?
C6 N3 N2 111.3(3) . . ?
C2 N4 C3 116.0(3) . . ?
C5 N5 H15A 114(3) . . ?
C5 N5 H15B 122(4) . . ?
H15A N5 H15B 120(5) . . ?
C9 N6 C10 116.9(3) . . ?
C12 N7 Pb1 138.1(3) . . ?
N1 C1 C2 121.0(4) . . ?
N1 C1 H1 119.5 . . ?
C2 C1 H1 119.5 . . ?
N4 C2 C1 122.5(4) . . ?
N4 C2 H2 118.7 . . ?
C1 C2 H2 118.7 . . ?
N4 C3 C4 122.1(4) . . ?
N4 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
N1 C4 C3 121.6(3) . . ?
N1 C4 C5 117.2(3) . . ?
C3 C4 C5 121.2(3) . . ?
N2 C5 N5 124.8(4) . . ?
N2 C5 C4 116.3(3) . . ?
N5 C5 C4 118.9(3) . . ?
O1 C6 N3 126.7(3) . . ?
O1 C6 C7 117.7(3) . . ?
N3 C6 C7 115.5(3) . . ?
C11 C7 C8 117.9(3) . . ?
C11 C7 C6 119.5(3) . . ?
C8 C7 C6 122.6(3) . . ?
C9 C8 C7 118.8(4) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
N6 C9 C8 123.7(4) . . ?
N6 C9 H9 118.1 . . ?
C8 C9 H9 118.1 . . ?
N6 C10 C11 123.7(4) . . ?
N6 C10 H10 118.1 . . ?
C11 C10 H10 118.2 . . ?
C10 C11 C7 118.9(4) . . ?
C10 C11 H11 120.5 . . ?
C7 C11 H11 120.6 . . ?
N7 C12 S1 177.9(4) . . ?
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
Pb1 O1 2.346(3) . ?
Pb1 N7 2.374(3) . ?
Pb1 N2 2.375(3) . ?
Pb1 N1 2.717(3) . ?
Pb1 N3 3.176(3) 3_556 ?
Pb1 N4 3.255(3) 1_455 ?
Pb1 S1 3.4175(11) 3_557 ?
Pb1 N2 3.452(3) 3_556 ?
S1 C12 1.623(4) . ?
O1 C6 1.289(4) . ?
N1 C1 1.337(5) . ?
N1 C4 1.340(5) . ?
N2 C5 1.306(5) . ?
N2 N3 1.406(4) . ?
N3 C6 1.321(5) . ?
N4 C2 1.328(5) . ?
N4 C3 1.340(5) . ?
N5 C5 1.312(5) . ?
N5 H15A 0.80(5) . ?
N5 H15B 0.71(5) . ?
N6 C9 1.336(5) . ?
N6 C10 1.336(5) . ?
N7 C12 1.168(5) . ?
C1 C2 1.395(6) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.497(5) . ?
C6 C7 1.493(5) . ?
C7 C11 1.388(5) . ?
C7 C8 1.391(5) . ?
C8 C9 1.384(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.386(5) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
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
N5 H15A S1 0.80(5) 2.82(5) 3.503(4) 145(4) 4_565 yes
N5 H15B N6 0.71(5) 2.22(5) 2.919(5) 167(5) 4_666 yes
C2 H2 S1 0.95 2.93 3.640(4) 132.1 3_657 yes
C3 H3 O1 0.95 2.46 3.113(5) 125.9 1_655 yes
C8 H8 S1 0.95 3.03 3.791(4) 138.5 4_565 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 -163.1(3) . . . . ?
Pb1 N2 N3 C6 -1.1(4) . . . . ?
C4 N1 C1 C2 -1.3(5) . . . . ?
Pb1 N1 C1 C2 169.8(3) . . . . ?
C3 N4 C2 C1 2.4(6) . . . . ?
N1 C1 C2 N4 -1.2(6) . . . . ?
C2 N4 C3 C4 -1.2(6) . . . . ?
C1 N1 C4 C3 2.5(5) . . . . ?
Pb1 N1 C4 C3 -170.1(3) . . . . ?
C1 N1 C4 C5 179.5(3) . . . . ?
Pb1 N1 C4 C5 7.0(4) . . . . ?
N4 C3 C4 N1 -1.2(6) . . . . ?
N4 C3 C4 C5 -178.2(3) . . . . ?
N3 N2 C5 N5 0.6(5) . . . . ?
Pb1 N2 C5 N5 -159.7(3) . . . . ?
N3 N2 C5 C4 -177.9(3) . . . . ?
Pb1 N2 C5 C4 21.8(4) . . . . ?
N1 C4 C5 N2 -17.8(5) . . . . ?
C3 C4 C5 N2 159.3(3) . . . . ?
N1 C4 C5 N5 163.6(3) . . . . ?
C3 C4 C5 N5 -19.3(5) . . . . ?
Pb1 O1 C6 N3 -0.3(5) . . . . ?
Pb1 O1 C6 C7 -178.1(2) . . . . ?
N2 N3 C6 O1 0.9(5) . . . . ?
N2 N3 C6 C7 178.8(3) . . . . ?
O1 C6 C7 C11 0.1(5) . . . . ?
N3 C6 C7 C11 -178.0(3) . . . . ?
O1 C6 C7 C8 179.5(3) . . . . ?
N3 C6 C7 C8 1.4(5) . . . . ?
C11 C7 C8 C9 -0.4(5) . . . . ?
C6 C7 C8 C9 -179.8(3) . . . . ?
C10 N6 C9 C8 -0.3(6) . . . . ?
C7 C8 C9 N6 0.6(6) . . . . ?
C9 N6 C10 C11 -0.1(6) . . . . ?
N6 C10 C11 C7 0.2(6) . . . . ?
C8 C7 C11 C10 0.0(6) . . . . ?
C6 C7 C11 C10 179.4(3) . . . . ?
