#------------------------------------------------------------------------------
#$Date: 2022-05-20 11:28:26 +0300 (Fri, 20 May 2022) $
#$Revision: 275570 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/53/8105314.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_8105314
loop_
_publ_author_name
'Li, Zhuang-yu'
'Liu, E'
'Liu, Xiao-jing'
'Jian, Fang-fang'
_publ_section_title
;
 Crystal structure of bis(2,3-diphenyltetrazolidine-5-thione-κ1
 S)-(nitrato-κ1 O)-(nitrato-κ2 O,O′)lead(II), C26H20N10O6S2Pb
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              869
_journal_page_last               871
_journal_paper_doi               10.1515/ncrs-2020-0068
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C26 H20 N9 O3 Pb S2, N O3'
_chemical_formula_sum            'C26 H20 N10 O6 Pb S2'
_chemical_formula_weight         839.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_cell_angle_alpha                113.14(3)
_cell_angle_beta                 92.05(3)
_cell_angle_gamma                102.75(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3480(19)
_cell_length_b                   12.985(3)
_cell_length_c                   14.278(3)
_cell_measurement_reflns_used    3347
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.17
_cell_volume                     1539.8(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.9916
_diffrn_measured_fraction_theta_max 0.9916
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7057
_diffrn_reflns_theta_full        26.9702
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    5.673
_exptl_absorpt_correction_T_max  0.9138
_exptl_absorpt_correction_T_min  0.9024
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.8113
_exptl_crystal_description       block
_exptl_crystal_F_000             810.5406
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.5048
_refine_diff_density_min         -1.4503
_refine_diff_density_rms         0.2061
_refine_ls_d_res_high            0.7836
_refine_ls_d_res_low             13.0063
_refine_ls_goodness_of_fit_ref   1.0419
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.0404
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0452P)²+0.8999P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              14
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5294
_reflns_number_total             6644
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2020-0068_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105314
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -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_refinement_flags_posn
_atom_site_refinement_flags_adp
Pb1 Pb -0.01253(2) 0.326147(17) 0.430355(16) 0.04009(8) Uani 1.000000 . .
S1 S 0.11310(16) 0.15207(12) 0.43936(11) 0.0466(3) Uani 1.000000 . .
S2 S 0.25732(15) 0.46339(15) 0.42217(12) 0.0551(4) Uani 1.000000 . .
O4 O -0.1892(5) 0.1555(5) 0.2602(4) 0.0797(15) Uani 1.000000 . .
O5 O 0.0331(4) 0.2365(4) 0.2505(3) 0.0549(10) Uani 1.000000 . .
N1 N -0.1399(5) 0.1214(4) 0.5245(3) 0.0402(10) Uani 1.000000 . .
N2 N -0.1735(4) 0.1297(3) 0.6148(3) 0.0356(9) Uani 1.000000 . .
N3 N -0.0498(4) 0.1547(3) 0.6790(3) 0.0352(9) Uani 1.000000 . .
N4 N 0.0665(4) 0.1623(4) 0.6301(3) 0.0364(9) Uani 1.000000 . .
N5 N 0.3587(5) 0.4374(4) 0.5908(3) 0.0456(10) Uani 1.000000 . .
N6 N 0.4173(5) 0.5088(4) 0.6853(3) 0.0424(10) Uani 1.000000 . .
N7 N 0.4325(5) 0.6182(4) 0.6993(4) 0.0434(10) Uani 1.000000 . .
N8 N 0.3860(5) 0.6231(4) 0.6135(4) 0.0443(10) Uani 1.000000 . .
C1 C -0.4145(6) 0.1636(6) 0.6064(5) 0.0588(16) Uani 1.000000 . .
H1 H -0.3802(6) 0.2120(6) 0.5739(5) 0.071(2) Uiso 1.000000 R .
C2 C -0.5631(7) 0.1399(7) 0.6251(6) 0.076(2) Uani 1.000000 . .
H2 H -0.6292(7) 0.1735(7) 0.6046(6) 0.091(3) Uiso 1.000000 R .
C3 C -0.6108(7) 0.0685(7) 0.6729(6) 0.076(2) Uani 1.000000 . .
H3 H -0.7092(7) 0.0542(7) 0.6841(6) 0.092(3) Uiso 1.000000 R .
C4 C -0.5173(7) 0.0174(7) 0.7046(6) 0.072(2) Uani 1.000000 . .
H4 H -0.5514(7) -0.0309(7) 0.7373(6) 0.087(2) Uiso 1.000000 R .
C5 C -0.3687(6) 0.0392(5) 0.6870(5) 0.0558(15) Uani 1.000000 . .
H5 H -0.3027(6) 0.0055(5) 0.7075(5) 0.0670(18) Uiso 1.000000 R .
C6 C -0.3239(5) 0.1107(5) 0.6393(4) 0.0434(12) Uani 1.000000 . .
C7 C -0.0769(7) 0.2877(5) 0.8486(5) 0.0508(14) Uani 1.000000 . .
H7 H -0.1118(7) 0.3312(5) 0.8190(5) 0.0610(16) Uiso 1.000000 R .
C8 C -0.0597(8) 0.3221(5) 0.9546(5) 0.0581(15) Uani 1.000000 . .
H8 H -0.0835(8) 0.3896(5) 0.9973(5) 0.0697(18) Uiso 1.000000 R .
C9 C -0.0072(7) 0.2557(6) 0.9959(5) 0.0578(15) Uani 1.000000 . .
H9 H 0.0052(7) 0.2793(6) 1.0668(5) 0.0694(19) Uiso 1.000000 R .
C10 C 0.0272(8) 0.1550(6) 0.9339(5) 0.0630(17) Uani 1.000000 . .
H10 H 0.0607(8) 0.1106(6) 0.9632(5) 0.076(2) Uiso 1.000000 R .
C11 C 0.0122(6) 0.1194(5) 0.8287(5) 0.0508(14) Uani 1.000000 . .
H11 H 0.0369(6) 0.0522(5) 0.7863(5) 0.0610(17) Uiso 1.000000 R .
C12 C -0.0404(5) 0.1865(4) 0.7887(4) 0.0359(10) Uani 1.000000 . .
C13 C 0.0100(5) 0.1431(4) 0.5349(4) 0.0352(11) Uani 1.000000 . .
C14 C 0.3501(8) 0.3996(5) 0.7889(5) 0.0622(17) Uani 1.000000 . .
H14 H 0.2516(8) 0.3801(5) 0.7605(5) 0.075(2) Uiso 1.000000 R .
C15 C 0.3918(10) 0.3586(6) 0.8595(6) 0.077(2) Uani 1.000000 . .
H15 H 0.3210(10) 0.3107(6) 0.8786(6) 0.093(3) Uiso 1.000000 R .
C16 C 0.5360(11) 0.3886(7) 0.9004(6) 0.079(2) Uani 1.000000 . .
H16 H 0.5632(11) 0.3596(7) 0.9466(6) 0.095(3) Uiso 1.000000 R .
C17 C 0.6433(8) 0.4615(6) 0.8748(5) 0.0660(18) Uani 1.000000 . .
H17 H 0.7411(8) 0.4825(6) 0.9050(5) 0.079(2) Uiso 1.000000 R .
C18 C 0.6055(7) 0.5029(6) 0.8045(5) 0.0561(15) Uani 1.000000 . .
H18 H 0.6768(7) 0.5515(6) 0.7863(5) 0.0673(18) Uiso 1.000000 R .
C19 C 0.4596(6) 0.4705(5) 0.7622(4) 0.0444(12) Uani 1.000000 . .
C20 C 0.6245(6) 0.7894(5) 0.8104(5) 0.0589(16) Uani 1.000000 . .
H20 H 0.6819(6) 0.7778(5) 0.7571(5) 0.0707(19) Uiso 1.000000 R .
C21 C 0.6757(8) 0.8802(6) 0.9063(6) 0.0696(19) Uani 1.000000 . .
H21 H 0.7685(8) 0.9307(6) 0.9177(6) 0.084(2) Uiso 1.000000 R .
C22 C 0.5890(9) 0.8956(6) 0.9848(6) 0.073(2) Uani 1.000000 . .
H22 H 0.6247(9) 0.9557(6) 1.0492(6) 0.088(2) Uiso 1.000000 R .
C23 C 0.4503(9) 0.8227(6) 0.9682(6) 0.0707(19) Uani 1.000000 . .
H23 H 0.3929(9) 0.8342(6) 1.0215(6) 0.085(2) Uiso 1.000000 R .
C24 C 0.3948(7) 0.7320(5) 0.8725(5) 0.0539(14) Uani 1.000000 . .
H24 H 0.3003(7) 0.6834(5) 0.8601(5) 0.0647(17) Uiso 1.000000 R .
C25 C 0.4856(6) 0.7170(5) 0.7966(5) 0.0466(13) Uani 1.000000 . .
C26 C 0.3386(5) 0.5097(5) 0.5465(4) 0.0462(13) Uani 1.000000 . .
N10 N -0.0874(6) 0.1596(4) 0.2068(4) 0.0501(12) Uani 1.000000 . .
O6 O -0.0987(7) 0.0942(4) 0.1173(4) 0.0848(16) Uani 1.000000 . .
N9 N 0.0149(5) 0.4737(4) 0.6998(4) 0.0480(11) Uani 1.000000 . .
O1 O 0.0883(5) 0.5263(5) 0.6522(5) 0.0810(16) Uani 1.000000 . .
O2 O 0.0076(8) 0.5225(5) 0.7900(4) 0.106(2) Uani 1.000000 . .
O3 O -0.0484(7) 0.3706(4) 0.6529(4) 0.0917(18) Uani 1.000000 . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Pb -3.20855 10.15388 31.06170 13.06370 18.44200 5.96960 0.69020 2.35760 8.61800
47.25790 13.4118003845
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
S2 Pb1 S1 93.55(5) . .
O5 Pb1 S1 80.04(11) . .
O5 Pb1 S2 75.14(10) . .
C13 S1 Pb1 90.27(16) . .
C26 S2 Pb1 99.30(19) . .
N10 O5 Pb1 102.9(3) . .
C13 N1 N2 104.5(4) . .
N3 N2 N1 110.1(4) . .
C6 N2 N1 124.0(4) . .
C6 N2 N3 125.9(4) . .
N4 N3 N2 109.5(4) . .
C12 N3 N2 126.0(4) . .
C12 N3 N4 123.9(4) . .
C13 N4 N3 104.5(4) . .
C26 N5 N6 103.2(4) . .
N7 N6 N5 111.1(4) . .
C19 N6 N5 123.2(4) . .
C19 N6 N7 125.7(4) . .
N8 N7 N6 110.3(4) . .
C25 N7 N6 124.5(4) . .
C25 N7 N8 125.2(4) . .
C26 N8 N7 103.5(4) . .
C6 C1 C2 115.9(7) . .
C3 C2 C1 121.0(7) . .
C4 C3 C2 121.6(6) . .
C5 C4 C3 118.8(7) . .
C6 C5 C4 118.4(6) . .
C1 C6 N2 115.9(5) . .
C5 C6 N2 119.7(5) . .
C5 C6 C1 124.3(5) . .
C12 C7 C8 117.8(5) . .
C9 C8 C7 119.6(6) . .
C10 C9 C8 121.1(6) . .
C11 C10 C9 120.5(6) . .
C12 C11 C10 117.7(5) . .
C7 C12 N3 117.6(5) . .
C11 C12 N3 119.0(5) . .
C11 C12 C7 123.3(5) . .
N1 C13 S1 123.5(4) . .
N4 C13 S1 125.1(4) . .
N4 C13 N1 111.4(4) . .
C19 C14 C15 118.1(6) . .
C16 C15 C14 120.0(7) . .
C17 C16 C15 121.2(7) . .
C18 C17 C16 120.2(7) . .
C19 C18 C17 118.2(6) . .
C14 C19 N6 118.1(5) . .
C18 C19 N6 119.5(5) . .
C18 C19 C14 122.3(6) . .
C25 C20 C21 117.9(6) . .
C22 C21 C20 120.2(6) . .
C23 C22 C21 120.4(6) . .
C24 C23 C22 120.8(7) . .
C25 C24 C23 117.4(6) . .
C20 C25 N7 119.2(5) . .
C24 C25 N7 117.6(5) . .
C24 C25 C20 123.3(6) . .
N5 C26 S2 124.1(4) . .
N8 C26 S2 124.0(4) . .
N8 C26 N5 111.9(5) . .
O5 N10 O4 117.2(5) . .
O6 N10 O4 123.0(6) . .
O6 N10 O5 119.9(5) . .
O2 N9 O1 121.1(6) . .
O3 N9 O1 119.0(6) . .
O3 N9 O2 119.9(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 S1 2.8097(15) .
Pb1 S2 2.7845(17) .
Pb1 O5 2.466(4) .
S1 C13 1.724(5) .
S2 C26 1.718(6) .
O4 N10 1.246(7) .
O5 N10 1.272(6) .
N1 N2 1.307(6) .
N1 C13 1.357(6) .
N2 N3 1.344(5) .
N2 C6 1.453(6) .
N3 N4 1.320(5) .
N3 C12 1.448(6) .
N4 C13 1.346(7) .
N5 N6 1.310(6) .
N5 C26 1.361(7) .
N6 N7 1.329(6) .
N6 C19 1.447(7) .
N7 N8 1.314(6) .
N7 C25 1.446(7) .
N8 C26 1.362(7) .
C1 C2 1.413(9) .
C1 C6 1.375(8) .
C2 C3 1.363(11) .
C3 C4 1.370(11) .
C4 C5 1.407(8) .
C5 C6 1.360(8) .
C7 C8 1.391(8) .
C7 C12 1.381(7) .
C8 C9 1.379(8) .
C9 C10 1.375(9) .
C10 C11 1.378(9) .
C11 C12 1.374(7) .
C14 C15 1.391(10) .
C14 C19 1.389(9) .
C15 C16 1.358(11) .
C16 C17 1.384(11) .
C17 C18 1.379(9) .
C18 C19 1.376(8) .
C20 C21 1.389(9) .
C20 C25 1.380(8) .
C21 C22 1.383(11) .
C22 C23 1.376(11) .
C23 C24 1.392(9) .
C24 C25 1.380(8) .
N10 O6 1.210(7) .
N9 O1 1.261(6) .
N9 O2 1.204(7) .
N9 O3 1.228(7) .
loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
Pb1 S1 0.0100
Pb1 S2 0.0100
Pb1 O5 0.0100
