#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/35/4313504.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_4313504
loop_
_publ_author_name
'José S. Casas'
'Eduardo E. Castellano'
'J. Ellena'
'María S. García Tasende'
'Agustín Sánchez'
'José Sordo'
'María J. Vidarte'
_publ_section_title
;
 Compositional and Structural Variety of Diphenyllead(IV) Complexes
 Obtained by Reaction of Diphenyllead Dichloride with Thiosemicarbazones
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2584
_journal_page_last               2595
_journal_paper_doi               10.1021/ic026219r
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C13 H12 N4 S'
_chemical_formula_weight         256.33
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.3340(2)
_cell_length_b                   11.6570(2)
_cell_length_c                   17.3750(4)
_cell_measurement_reflns_used    2878
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      0.998
_cell_volume                     2497.97(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'φ scans and ω scans winth κ offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0126
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5389
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.9344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0892P)²+1.2163P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                2509
_reflns_number_total             2835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026219r_1.cif
_cod_data_source_block           HBPyTSC
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multiscan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313504
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.12606(3) -0.35811(3) -0.02518(2) 0.02370(18) Uani 1 1 d . . .
N1 N -0.04454(12) -0.37563(12) 0.06735(9) 0.0251(3) Uani 1 1 d . . .
H1A H -0.0904 -0.3455 0.1001 0.030 Uiso 1 1 calc R . .
H1B H -0.0503 -0.4483 0.0543 0.030 Uiso 1 1 calc R . .
N2 N 0.03608(11) -0.19931(11) 0.06104(8) 0.0205(3) Uani 1 1 d . . .
H2 H 0.0888 -0.1529 0.0474 0.025 Uiso 1 1 calc R . .
N3 N -0.04670(10) -0.16262(12) 0.10667(8) 0.0199(3) Uani 1 1 d . . .
N4 N 0.10572(11) 0.01443(11) 0.06258(8) 0.0198(3) Uani 1 1 d . . .
C1 C 0.03342(12) -0.31120(14) 0.03750(9) 0.0205(3) Uani 1 1 d . . .
C2 C -0.05355(12) -0.05633(14) 0.12809(9) 0.0191(3) Uani 1 1 d . . .
C3 C 0.02434(12) 0.03790(13) 0.11191(8) 0.0186(3) Uani 1 1 d . . .
C4 C 0.01619(10) 0.14373(10) 0.14902(7) 0.0233(4) Uani 1 1 d . . .
H4 H -0.0422 0.1586 0.1828 0.028 Uiso 1 1 calc R . .
C5 C 0.09437(10) 0.22684(10) 0.13604(7) 0.0274(4) Uani 1 1 d R . .
H5 H 0.0904 0.2994 0.1608 0.033 Uiso 1 1 calc R . .
C6 C 0.17846(13) 0.20233(15) 0.08641(10) 0.0251(4) Uani 1 1 d . . .
H6 H 0.2337 0.2572 0.0770 0.030 Uiso 1 1 calc R . .
C7 C 0.18017(13) 0.09570(14) 0.05069(9) 0.0224(3) Uani 1 1 d . . .
H7 H 0.2372 0.0797 0.0160 0.027 Uiso 1 1 calc R . .
C8 C -0.15079(13) -0.03416(14) 0.17639(9) 0.0218(4) Uani 1 1 d . . .
C9 C -0.22549(15) 0.05100(17) 0.15773(11) 0.0297(4) Uani 1 1 d . . .
H9 H -0.2131 0.1005 0.1153 0.036 Uiso 1 1 calc R . .
C10 C -0.31869(16) 0.0635(2) 0.20153(12) 0.0385(5) Uani 1 1 d . . .
H10 H -0.3699 0.1214 0.1885 0.046 Uiso 1 1 calc R . .
C11 C -0.33739(16) -0.0077(2) 0.26396(12) 0.0403(5) Uani 1 1 d . . .
H11 H -0.4010 0.0017 0.2936 0.048 Uiso 1 1 calc R . .
C12 C -0.26323(16) -0.09239(19) 0.28294(10) 0.0356(5) Uani 1 1 d . . .
H12 H -0.2757 -0.1411 0.3258 0.043 Uiso 1 1 calc R . .
C13 C -0.17024(14) -0.10615(16) 0.23914(9) 0.0272(4) Uani 1 1 d . . .
H13 H -0.1197 -0.1648 0.2520 0.033 Uiso 1 1 calc R . .
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'
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
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C1 N2 N3 117.12(13) . . ?
C1 N2 H2 121.4 . . ?
N3 N2 H2 121.4 . . ?
C2 N3 N2 121.09(13) . . ?
C7 N4 C3 118.01(14) . . ?
N1 C1 N2 115.92(14) . . ?
N1 C1 S1 124.71(13) . . ?
N2 C1 S1 119.37(12) . . ?
N3 C2 C3 127.36(14) . . ?
N3 C2 C8 112.44(13) . . ?
C3 C2 C8 120.16(14) . . ?
N4 C3 C4 121.89(13) . . ?
N4 C3 C2 117.05(14) . . ?
C4 C3 C2 121.00(13) . . ?
C5 C4 C3 119.23(8) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 118.92(8) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 118.52(14) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
N4 C7 C6 123.43(15) . . ?
N4 C7 H7 118.3 . . ?
C6 C7 H7 118.3 . . ?
C9 C8 C13 119.41(16) . . ?
C9 C8 C2 121.78(15) . . ?
C13 C8 C2 118.68(15) . . ?
C8 C9 C10 119.73(19) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 120.7(2) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 119.87(17) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 119.89(19) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C8 120.42(18) . . ?
C12 C13 H13 119.8 . . ?
C8 C13 H13 119.8 . . ?
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
S1 C1 1.6790(16) . ?
N1 C1 1.330(2) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
N2 C1 1.367(2) . ?
N2 N3 1.3684(18) . ?
N2 H2 0.8800 . ?
N3 C2 1.297(2) . ?
N4 C7 1.337(2) . ?
N4 C3 1.355(2) . ?
C2 C3 1.488(2) . ?
C2 C8 1.494(2) . ?
C3 C4 1.3961(19) . ?
C4 C5 1.3872 . ?
C4 H4 0.9500 . ?
C5 C6 1.386(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.390(2) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.390(3) . ?
C8 C13 1.399(2) . ?
C9 C10 1.393(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(2) . ?
C12 H12 0.9500 . ?
C13 H13 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
C1 N2 N3 C2 -176.23(14) . . . . ?
N3 N2 C1 N1 -5.9(2) . . . . ?
N3 N2 C1 S1 174.32(11) . . . . ?
N2 N3 C2 C3 -3.2(2) . . . . ?
N2 N3 C2 C8 178.99(13) . . . . ?
C7 N4 C3 C4 0.8(2) . . . . ?
C7 N4 C3 C2 -176.20(13) . . . . ?
N3 C2 C3 N4 7.7(2) . . . . ?
C8 C2 C3 N4 -174.67(13) . . . . ?
N3 C2 C3 C4 -169.35(15) . . . . ?
C8 C2 C3 C4 8.3(2) . . . . ?
N4 C3 C4 C5 -0.97(17) . . . . ?
C2 C3 C4 C5 175.94(10) . . . . ?
C3 C4 C5 C6 0.07(11) . . . . ?
C4 C5 C6 C7 0.91(18) . . . . ?
C3 N4 C7 C6 0.2(2) . . . . ?
C5 C6 C7 N4 -1.1(2) . . . . ?
N3 C2 C8 C9 -125.78(17) . . . . ?
C3 C2 C8 C9 56.3(2) . . . . ?
N3 C2 C8 C13 50.1(2) . . . . ?
C3 C2 C8 C13 -127.88(16) . . . . ?
C13 C8 C9 C10 -0.1(3) . . . . ?
C2 C8 C9 C10 175.71(16) . . . . ?
C8 C9 C10 C11 0.5(3) . . . . ?
C9 C10 C11 C12 -0.3(3) . . . . ?
C10 C11 C12 C13 -0.2(3) . . . . ?
C11 C12 C13 C8 0.6(3) . . . . ?
C9 C8 C13 C12 -0.4(3) . . . . ?
C2 C8 C13 C12 -176.35(15) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 4735768
