#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:38:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179196 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313509.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_4313509
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            'C20 H19 Cl N4 Pb S'
_chemical_formula_weight         590.09
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.587(3)
_cell_angle_beta                 104.252(3)
_cell_angle_gamma                114.979(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5816(17)
_cell_length_b                   10.0802(18)
_cell_length_c                   12.170(2)
_cell_measurement_reflns_used    953
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.385
_cell_measurement_theta_min      2.475
_cell_volume                     1005.2(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4087
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    8.641
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.3379
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.628
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0164
_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)+(0.0167P)²+0.9599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0410
_reflns_number_gt                3818
_reflns_number_total             4087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026219r_6.cif
_cod_data_source_block           '[PbPh2Cl(AcPyTSC)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.9599P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.9599P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313509
loop_
_symmetry_equiv_pos_as_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.672294(13) 0.571237(12) 0.708578(9) 0.02046(4) Uani 1 d . . .
S S 0.64534(10) 0.63124(9) 0.49214(7) 0.02762(17) Uani 1 d . . .
Cl Cl 0.51966(11) 0.34401(10) 0.81648(7) 0.0380(2) Uani 1 d . . .
N1 N 0.7816(4) 0.8828(3) 0.4291(3) 0.0325(7) Uani 1 d . . .
N2 N 0.9010(3) 0.9002(3) 0.6198(2) 0.0249(6) Uani 1 d . . .
N3 N 0.8997(3) 0.8297(3) 0.7118(2) 0.0212(5) Uani 1 d . . .
N4 N 0.8962(3) 0.6985(3) 0.8968(2) 0.0238(5) Uani 1 d . . .
C1 C 0.7874(3) 0.8175(3) 0.5204(3) 0.0199(6) Uani 1 d . . .
C2 C 1.0096(4) 0.9106(3) 0.8104(3) 0.0212(6) Uani 1 d . . .
C3 C 1.0180(4) 0.8364(3) 0.9094(3) 0.0224(6) Uani 1 d . . .
C4 C 1.1500(4) 0.9021(4) 1.0105(3) 0.0343(8) Uani 1 d . . .
H4 H 1.2328 0.9980 1.0195 0.041 Uiso 1 calc R . .
C5 C 1.1587(5) 0.8254(5) 1.0978(3) 0.0450(9) Uani 1 d . . .
H5 H 1.2480 0.8683 1.1653 0.054 Uiso 1 calc R . .
C6 C 1.0338(5) 0.6850(4) 1.0838(3) 0.0416(9) Uani 1 d . . .
H6 H 1.0371 0.6311 1.1414 0.050 Uiso 1 calc R . .
C7 C 0.9036(5) 0.6255(4) 0.9828(3) 0.0338(8) Uani 1 d . . .
H7 H 0.8178 0.5315 0.9740 0.041 Uiso 1 calc R . .
C8 C 1.1289(4) 1.0714(4) 0.8276(3) 0.0334(8) Uani 1 d . . .
H8A H 1.1081 1.1033 0.7562 0.050 Uiso 1 calc R . .
H8B H 1.2371 1.0819 0.8502 0.050 Uiso 1 calc R . .
H8C H 1.1183 1.1323 0.8876 0.050 Uiso 1 calc R . .
C11 C 0.5442(4) 0.6891(3) 0.7612(3) 0.0251(6) Uani 1 d . . .
C12 C 0.5090(4) 0.6787(4) 0.8645(3) 0.0361(8) Uani 1 d . . .
H12 H 0.5349 0.6185 0.9102 0.043 Uiso 1 calc R . .
C13 C 0.4347(5) 0.7594(5) 0.8989(4) 0.0467(10) Uani 1 d . . .
H13 H 0.4108 0.7540 0.9684 0.056 Uiso 1 calc R . .
C14 C 0.3959(5) 0.8475(5) 0.8306(4) 0.0518(11) Uani 1 d . . .
H14 H 0.3464 0.9018 0.8545 0.062 Uiso 1 calc R . .
C15 C 0.4298(6) 0.8562(5) 0.7273(4) 0.0512(11) Uani 1 d . . .
H15 H 0.4024 0.9153 0.6812 0.061 Uiso 1 calc R . .
C16 C 0.5050(5) 0.7763(4) 0.6921(3) 0.0394(9) Uani 1 d . . .
H16 H 0.5286 0.7818 0.6225 0.047 Uiso 1 calc R . .
C21 C 0.7948(4) 0.4437(4) 0.6638(3) 0.0262(7) Uani 1 d . . .
C22 C 0.7120(5) 0.2896(4) 0.6298(3) 0.0357(8) Uani 1 d . . .
H22 H 0.6042 0.2385 0.6273 0.043 Uiso 1 calc R . .
C23 C 0.7909(6) 0.2112(5) 0.5992(4) 0.0487(10) Uani 1 d . . .
H23 H 0.7365 0.1068 0.5764 0.058 Uiso 1 calc R . .
C24 C 0.9507(6) 0.2889(5) 0.6028(4) 0.0536(11) Uani 1 d . . .
H24 H 1.0039 0.2362 0.5828 0.064 Uiso 1 calc R . .
C25 C 1.0316(6) 0.4427(5) 0.6354(4) 0.0532(11) Uani 1 d . . .
H25 H 1.1388 0.4942 0.6367 0.064 Uiso 1 calc R . .
C26 C 0.9534(5) 0.5216(4) 0.6665(3) 0.0383(8) Uani 1 d . . .
H26 H 1.0076 0.6260 0.6890 0.046 Uiso 1 calc R . .
H1A H 0.721(5) 0.831(4) 0.365(3) 0.033(11) Uiso 1 d . . .
H1B H 0.879(5) 0.962(5) 0.435(4) 0.053(13) Uiso 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
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
C21 Pb C11 176.16(11) . . ?
C21 Pb N4 88.62(11) . . ?
C11 Pb N4 90.47(10) . . ?
C21 Pb N3 95.07(11) . . ?
C11 Pb N3 87.91(10) . . ?
N4 Pb N3 64.86(8) . . ?
C21 Pb S 86.71(8) . . ?
C11 Pb S 96.68(9) . . ?
N4 Pb S 131.33(6) . . ?
N3 Pb S 67.37(6) . . ?
C21 Pb Cl 86.98(9) . . ?
C11 Pb Cl 89.25(9) . . ?
N4 Pb Cl 87.71(6) . . ?
N3 Pb Cl 152.39(6) . . ?
S Pb Cl 140.21(2) . . ?
C21 Pb S 93.18(9) . 2_666 ?
C11 Pb S 86.89(9) . 2_666 ?
N4 Pb S 167.21(6) . 2_666 ?
N3 Pb S 127.47(6) . 2_666 ?
S Pb S 61.45(3) . 2_666 ?
Cl Pb S 79.75(3) . 2_666 ?
C1 S Pb 103.50(10) . . ?
C1 S Pb 133.05(10) . 2_666 ?
Pb S Pb 118.55(3) . 2_666 ?
C1 N2 N3 115.2(2) . . ?
C2 N3 N2 115.8(2) . . ?
C2 N3 Pb 118.48(19) . . ?
N2 N3 Pb 124.98(17) . . ?
C7 N4 C3 119.6(3) . . ?
C7 N4 Pb 120.2(2) . . ?
C3 N4 Pb 120.04(19) . . ?
N2 C1 N1 117.3(3) . . ?
N2 C1 S 127.2(2) . . ?
N1 C1 S 115.5(2) . . ?
N3 C2 C3 117.3(3) . . ?
N3 C2 C8 123.4(3) . . ?
C3 C2 C8 119.2(3) . . ?
N4 C3 C4 120.2(3) . . ?
N4 C3 C2 118.1(3) . . ?
C4 C3 C2 121.7(3) . . ?
C5 C4 C3 120.1(3) . . ?
C6 C5 C4 119.1(3) . . ?
C5 C6 C7 118.8(3) . . ?
N4 C7 C6 122.3(3) . . ?
C16 C11 C12 121.2(3) . . ?
C16 C11 Pb 119.0(2) . . ?
C12 C11 Pb 119.8(2) . . ?
C11 C12 C13 118.9(3) . . ?
C14 C13 C12 120.2(4) . . ?
C13 C14 C15 120.5(4) . . ?
C14 C15 C16 119.8(4) . . ?
C11 C16 C15 119.3(3) . . ?
C22 C21 C26 121.3(3) . . ?
C22 C21 Pb 120.2(3) . . ?
C26 C21 Pb 118.5(2) . . ?
C21 C22 C23 119.2(4) . . ?
C24 C23 C22 119.7(4) . . ?
C25 C24 C23 120.7(4) . . ?
C24 C25 C26 119.8(4) . . ?
C21 C26 C25 119.3(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
Pb C21 2.186(3) . ?
Pb C11 2.191(3) . ?
Pb N4 2.486(2) . ?
Pb N3 2.585(2) . ?
Pb S 2.7345(9) . ?
Pb Cl 2.7949(9) . ?
Pb S 3.0851(9) 2_666 ?
S C1 1.727(3) . ?
S Pb 3.0851(9) 2_666 ?
N1 C1 1.346(4) . ?
N2 C1 1.316(4) . ?
N2 N3 1.383(3) . ?
N3 C2 1.294(4) . ?
N4 C7 1.341(4) . ?
N4 C3 1.348(4) . ?
C2 C3 1.482(4) . ?
C2 C8 1.493(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.380(5) . ?
C5 C6 1.374(6) . ?
C6 C7 1.376(5) . ?
C11 C16 1.374(5) . ?
C11 C12 1.382(4) . ?
C12 C13 1.383(5) . ?
C13 C14 1.374(6) . ?
C14 C15 1.375(6) . ?
C15 C16 1.388(5) . ?
C21 C22 1.373(5) . ?
C21 C26 1.375(5) . ?
C22 C23 1.386(5) . ?
C23 C24 1.381(6) . ?
C24 C25 1.370(6) . ?
C25 C26 1.386(5) . ?
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
N1 H1A Cl 0.81(4) 2.57(4) 3.367(3) 167(4) 2_666
N1 H1B N2 0.92(5) 2.28(5) 3.149(4) 157(4) 2_776
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
C21 Pb S C1 -106.18(14) . . . . ?
C11 Pb S C1 75.63(13) . . . . ?
N4 Pb S C1 -20.92(14) . . . . ?
N3 Pb S C1 -9.29(12) . . . . ?
Cl Pb S C1 172.53(10) . . . . ?
S Pb S C1 158.40(12) 2_666 . . . ?
C21 Pb S Pb 95.43(10) . . . 2_666 ?
C11 Pb S Pb -82.77(9) . . . 2_666 ?
N4 Pb S Pb -179.31(8) . . . 2_666 ?
N3 Pb S Pb -167.69(7) . . . 2_666 ?
Cl Pb S Pb 14.13(6) . . . 2_666 ?
S Pb S Pb 0.0 2_666 . . 2_666 ?
C1 N2 N3 C2 -179.2(3) . . . . ?
C1 N2 N3 Pb -9.3(4) . . . . ?
C21 Pb N3 C2 -94.4(2) . . . . ?
C11 Pb N3 C2 83.2(2) . . . . ?
N4 Pb N3 C2 -8.3(2) . . . . ?
S Pb N3 C2 -178.7(2) . . . . ?
Cl Pb N3 C2 -1.2(3) . . . . ?
S Pb N3 C2 167.66(19) 2_666 . . . ?
C21 Pb N3 N2 96.0(2) . . . . ?
C11 Pb N3 N2 -86.4(2) . . . . ?
N4 Pb N3 N2 -177.9(2) . . . . ?
S Pb N3 N2 11.7(2) . . . . ?
Cl Pb N3 N2 -170.81(16) . . . . ?
S Pb N3 N2 -1.9(3) 2_666 . . . ?
C21 Pb N4 C7 -75.7(3) . . . . ?
C11 Pb N4 C7 100.5(3) . . . . ?
N3 Pb N4 C7 -172.0(3) . . . . ?
S Pb N4 C7 -160.1(2) . . . . ?
Cl Pb N4 C7 11.3(2) . . . . ?
S Pb N4 C7 22.6(5) 2_666 . . . ?
C21 Pb N4 C3 98.7(2) . . . . ?
C11 Pb N4 C3 -85.0(2) . . . . ?
N3 Pb N4 C3 2.4(2) . . . . ?
S Pb N4 C3 14.3(3) . . . . ?
Cl Pb N4 C3 -174.3(2) . . . . ?
S Pb N4 C3 -163.0(2) 2_666 . . . ?
N3 N2 C1 N1 178.4(3) . . . . ?
N3 N2 C1 S -3.0(4) . . . . ?
Pb S C1 N2 11.4(3) . . . . ?
Pb S C1 N2 165.2(2) 2_666 . . . ?
Pb S C1 N1 -170.0(2) . . . . ?
Pb S C1 N1 -16.3(3) 2_666 . . . ?
N2 N3 C2 C3 -176.6(2) . . . . ?
Pb N3 C2 C3 12.9(3) . . . . ?
N2 N3 C2 C8 1.8(4) . . . . ?
Pb N3 C2 C8 -168.8(2) . . . . ?
C7 N4 C3 C4 0.1(5) . . . . ?
Pb N4 C3 C4 -174.4(2) . . . . ?
C7 N4 C3 C2 177.1(3) . . . . ?
Pb N4 C3 C2 2.7(4) . . . . ?
N3 C2 C3 N4 -10.5(4) . . . . ?
C8 C2 C3 N4 171.0(3) . . . . ?
N3 C2 C3 C4 166.5(3) . . . . ?
C8 C2 C3 C4 -12.0(5) . . . . ?
N4 C3 C4 C5 1.3(5) . . . . ?
C2 C3 C4 C5 -175.7(3) . . . . ?
C3 C4 C5 C6 -1.2(6) . . . . ?
C4 C5 C6 C7 -0.1(6) . . . . ?
C3 N4 C7 C6 -1.5(5) . . . . ?
Pb N4 C7 C6 173.0(3) . . . . ?
C5 C6 C7 N4 1.5(6) . . . . ?
C21 Pb C11 C16 -161.0(16) . . . . ?
N4 Pb C11 C16 122.8(3) . . . . ?
N3 Pb C11 C16 58.0(3) . . . . ?
S Pb C11 C16 -8.9(3) . . . . ?
Cl Pb C11 C16 -149.5(3) . . . . ?
S Pb C11 C16 -69.7(3) 2_666 . . . ?
C21 Pb C11 C12 21.1(19) . . . . ?
N4 Pb C11 C12 -55.1(3) . . . . ?
N3 Pb C11 C12 -119.9(3) . . . . ?
S Pb C11 C12 173.2(3) . . . . ?
Cl Pb C11 C12 32.6(3) . . . . ?
S Pb C11 C12 112.4(3) 2_666 . . . ?
C16 C11 C12 C13 -0.8(5) . . . . ?
Pb C11 C12 C13 177.1(3) . . . . ?
C11 C12 C13 C14 0.4(6) . . . . ?
C12 C13 C14 C15 0.3(7) . . . . ?
C13 C14 C15 C16 -0.6(7) . . . . ?
C12 C11 C16 C15 0.5(6) . . . . ?
Pb C11 C16 C15 -177.4(3) . . . . ?
C14 C15 C16 C11 0.2(7) . . . . ?
C11 Pb C21 C22 50.9(18) . . . . ?
N4 Pb C21 C22 127.2(3) . . . . ?
N3 Pb C21 C22 -168.2(3) . . . . ?
S Pb C21 C22 -101.3(3) . . . . ?
Cl Pb C21 C22 39.4(3) . . . . ?
S Pb C21 C22 -40.1(3) 2_666 . . . ?
C11 Pb C21 C26 -131.4(17) . . . . ?
N4 Pb C21 C26 -55.2(3) . . . . ?
N3 Pb C21 C26 9.5(3) . . . . ?
S Pb C21 C26 76.4(3) . . . . ?
Cl Pb C21 C26 -142.9(3) . . . . ?
S Pb C21 C26 137.5(3) 2_666 . . . ?
C26 C21 C22 C23 0.9(5) . . . . ?
Pb C21 C22 C23 178.5(3) . . . . ?
C21 C22 C23 C24 -0.3(6) . . . . ?
C22 C23 C24 C25 -0.5(7) . . . . ?
C23 C24 C25 C26 0.8(7) . . . . ?
C22 C21 C26 C25 -0.7(5) . . . . ?
Pb C21 C26 C25 -178.3(3) . . . . ?
C24 C25 C26 C21 -0.2(6) . . . . ?
