#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312981.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_4312981
loop_
_publ_author_name
'Anastassiya V. Makarycheva-Mikhailova'
'Nadezhda A. Bokach'
'Vadim Yu. Kukushkin'
'Paul F. Kelly'
'Liam M. Gilby'
'Maxim L. Kuznetsov'
'Kathryn E. Holmes'
'Matti Haukka'
'Jonathan Parr'
'Julia M. Stonehouse'
'Mark R. J. Elsegood'
'Armando J. L. Pombeiro'
_publ_section_title
;
 Platinum(IV)-Mediated Nitrile-Sulfimide Coupling: A Route to
 Heterodiazadienes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              301
_journal_page_last               311
_journal_paper_doi               10.1021/ic025960w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C20 H18 Cl2 N2 Pt S2'
_chemical_formula_weight         616.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'geom except NH coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.347(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4631(5)
_cell_length_b                   17.7135(9)
_cell_length_c                   12.4772(7)
_cell_measurement_reflns_used    6122
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.47
_cell_volume                     2057.47(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14800
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.291
_exptl_absorpt_correction_T_max  0.669
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.990
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0134P)²+4.1194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0505
_reflns_number_gt                2973
_reflns_number_total             3618
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic025960w-2_s2_4.cif
_cod_data_source_block           structure_8
_cod_database_code               4312981
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.00253(2) 0.240735(10) 0.678819(15) 0.02406(7) Uani 1 1 d . . .
Cl1 Cl -0.17360(14) 0.17329(7) 0.56353(11) 0.0325(3) Uani 1 1 d . . .
Cl2 Cl 0.02857(15) 0.14705(9) 0.80609(13) 0.0504(4) Uani 1 1 d . . .
S1 S 0.25739(13) 0.25804(7) 0.51476(9) 0.0270(3) Uani 1 1 d . . .
C1 C 0.2774(5) 0.1656(3) 0.4630(4) 0.0262(11) Uani 1 1 d . . .
C2 C 0.1724(5) 0.1109(3) 0.4669(4) 0.0327(13) Uani 1 1 d . . .
H2 H 0.0875 0.1234 0.4937 0.039 Uiso 1 1 calc R . .
C3 C 0.1925(6) 0.0388(3) 0.4316(4) 0.0368(13) Uani 1 1 d . . .
H3 H 0.1201 0.0018 0.4327 0.044 Uiso 1 1 calc R . .
C4 C 0.3173(6) 0.0196(3) 0.3945(4) 0.0390(14) Uani 1 1 d . . .
H4 H 0.3307 -0.0304 0.3707 0.047 Uiso 1 1 calc R . .
C5 C 0.4218(6) 0.0736(3) 0.3925(4) 0.0396(14) Uani 1 1 d . . .
H5 H 0.5083 0.0603 0.3685 0.048 Uiso 1 1 calc R . .
C6 C 0.4018(6) 0.1468(3) 0.4250(4) 0.0347(13) Uani 1 1 d . . .
H6 H 0.4730 0.1841 0.4214 0.042 Uiso 1 1 calc R . .
S2 S -0.00758(13) 0.34293(6) 0.58112(9) 0.0217(3) Uani 1 1 d . . .
C7 C 0.1206(5) 0.2956(3) 0.4131(4) 0.0239(11) Uani 1 1 d . . .
C8 C 0.1280(6) 0.2895(3) 0.3029(4) 0.0305(12) Uani 1 1 d . . .
H8 H 0.2052 0.2625 0.2816 0.037 Uiso 1 1 calc R . .
C9 C 0.0255(5) 0.3218(3) 0.2245(4) 0.0321(13) Uani 1 1 d . . .
H9 H 0.0334 0.3175 0.1499 0.039 Uiso 1 1 calc R . .
C10 C -0.0891(6) 0.3607(3) 0.2530(4) 0.0301(12) Uani 1 1 d . . .
H10 H -0.1603 0.3821 0.1981 0.036 Uiso 1 1 calc R . .
C11 C -0.0997(5) 0.3682(3) 0.3613(4) 0.0252(11) Uani 1 1 d . . .
H11 H -0.1775 0.3952 0.3817 0.030 Uiso 1 1 calc R . .
C12 C 0.0050(5) 0.3358(2) 0.4402(4) 0.0215(11) Uani 1 1 d . . .
C13 C -0.1668(5) 0.3962(3) 0.5858(4) 0.0219(11) Uani 1 1 d . . .
C14 C -0.1561(6) 0.4730(3) 0.5977(4) 0.0331(13) Uani 1 1 d . . .
H14 H -0.0682 0.4984 0.5959 0.040 Uiso 1 1 calc R . .
C15 C -0.2774(6) 0.5125(3) 0.6123(5) 0.0403(14) Uani 1 1 d . . .
H15 H -0.2731 0.5657 0.6211 0.048 Uiso 1 1 calc R . .
C16 C -0.4049(6) 0.4749(3) 0.6144(4) 0.0344(13) Uani 1 1 d . . .
H16 H -0.4871 0.5023 0.6260 0.041 Uiso 1 1 calc R . .
C17 C -0.4128(6) 0.3982(3) 0.5998(4) 0.0339(13) Uani 1 1 d . . .
H17 H -0.5015 0.3729 0.5991 0.041 Uiso 1 1 calc R . .
C18 C -0.2939(5) 0.3576(3) 0.5861(4) 0.0283(12) Uani 1 1 d . . .
H18 H -0.2987 0.3044 0.5771 0.034 Uiso 1 1 calc R . .
N2 N 0.1266(4) 0.3963(2) 0.6360(3) 0.0252(9) Uani 1 1 d . . .
C19 C 0.1935(5) 0.3662(3) 0.7308(4) 0.0267(12) Uani 1 1 d . . .
C20 C 0.3143(6) 0.4133(3) 0.7927(4) 0.0401(14) Uani 1 1 d . . .
H20A H 0.3085 0.4132 0.8704 0.048 Uiso 1 1 calc R . .
H20B H 0.3060 0.4652 0.7652 0.048 Uiso 1 1 calc R . .
H20C H 0.4067 0.3920 0.7828 0.048 Uiso 1 1 calc R . .
N1 N 0.1586(4) 0.3015(3) 0.7672(3) 0.0277(10) Uani 1 1 d . . .
H1A H 0.200(6) 0.289(3) 0.823(4) 0.042 Uiso 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'
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'
Pt Pt -1.7033 8.3905 '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
N1 Pt1 S2 79.28(13) . . ?
N1 Pt1 Cl2 91.80(13) . . ?
S2 Pt1 Cl2 170.00(5) . . ?
N1 Pt1 Cl1 175.51(12) . . ?
S2 Pt1 Cl1 97.26(4) . . ?
Cl2 Pt1 Cl1 91.87(5) . . ?
C7 S1 C1 101.4(2) . . ?
C6 C1 C2 120.0(5) . . ?
C6 C1 S1 119.8(4) . . ?
C2 C1 S1 120.2(4) . . ?
C3 C2 C1 119.6(5) . . ?
C2 C3 C4 120.7(5) . . ?
C5 C4 C3 119.6(5) . . ?
C4 C5 C6 120.6(5) . . ?
C5 C6 C1 119.7(5) . . ?
N2 S2 C13 106.1(2) . . ?
N2 S2 C12 105.6(2) . . ?
C13 S2 C12 106.0(2) . . ?
N2 S2 Pt1 107.12(15) . . ?
C13 S2 Pt1 111.96(16) . . ?
C12 S2 Pt1 119.21(15) . . ?
C8 C7 C12 117.3(4) . . ?
C8 C7 S1 121.2(4) . . ?
C12 C7 S1 121.4(3) . . ?
C9 C8 C7 121.1(5) . . ?
C8 C9 C10 120.7(5) . . ?
C11 C10 C9 119.9(5) . . ?
C10 C11 C12 119.1(5) . . ?
C11 C12 C7 121.9(4) . . ?
C11 C12 S2 120.2(4) . . ?
C7 C12 S2 117.9(3) . . ?
C14 C13 C18 122.5(5) . . ?
C14 C13 S2 118.8(4) . . ?
C18 C13 S2 118.5(4) . . ?
C13 C14 C15 118.0(5) . . ?
C16 C15 C14 120.5(5) . . ?
C17 C16 C15 120.1(5) . . ?
C18 C17 C16 120.6(5) . . ?
C17 C18 C13 118.4(5) . . ?
C19 N2 S2 110.3(3) . . ?
N1 C19 N2 123.2(4) . . ?
N1 C19 C20 121.7(5) . . ?
N2 C19 C20 115.1(4) . . ?
C19 N1 Pt1 119.6(3) . . ?
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
Pt1 N1 1.993(4) . ?
Pt1 S2 2.1748(12) . ?
Pt1 Cl2 2.2794(13) . ?
Pt1 Cl1 2.3267(13) . ?
S1 C7 1.771(5) . ?
S1 C1 1.783(5) . ?
C1 C6 1.386(7) . ?
C1 C2 1.395(7) . ?
C2 C3 1.375(7) . ?
C3 C4 1.386(7) . ?
C4 C5 1.379(8) . ?
C5 C6 1.382(7) . ?
S2 N2 1.632(4) . ?
S2 C13 1.788(5) . ?
S2 C12 1.788(5) . ?
C7 C8 1.394(6) . ?
C7 C12 1.397(6) . ?
C8 C9 1.373(7) . ?
C9 C10 1.384(7) . ?
C10 C11 1.379(6) . ?
C11 C12 1.390(6) . ?
C13 C14 1.370(7) . ?
C13 C18 1.385(7) . ?
C14 C15 1.384(7) . ?
C15 C16 1.381(7) . ?
C16 C17 1.373(7) . ?
C17 C18 1.370(7) . ?
N2 C19 1.347(6) . ?
C19 N1 1.297(6) . ?
C19 C20 1.510(7) . ?
