#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/38/4313893.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_4313893
loop_
_publ_author_name
'Bradley W. Smucker'
'Joshua M. Hudson'
'Mohammad A. Omary'
'Kim R. Dunbar'
_publ_contact_author
;
    Prof. Kim R. Dunbar
    Department of Chemistry
    Texas A&M University
    P.O. Box 30012
    College Station, TX
    7842-3012
    USA
;
_publ_contact_author_email       dunbar@mail.chem.tamu.edu
_publ_contact_author_fax         1(979)8457177
_publ_contact_author_phone       1(979)8455235
_publ_section_title
;
 Structural, Magnetic, and Optoelectronic Properties of
 (Diimine)(dithiolato)platinum(II) and -palladium(II) Complexes and Their
 Charge-Transfer Adducts with Nitrile Acceptors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4714
_journal_page_last               4723
_journal_paper_doi               10.1021/ic0259585
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C54 H54 N8 O2 Pt2 S8'
_chemical_formula_weight         1451.71
_chemical_name_systematic
; 
Di-[(4,4(-di-tert-butyl-2,2(-bipyridine)platinum
(1,3-dithiole-2-one-4,5-dithiolate)] Tetracyanoethylene 
;
_space_group_IT_number           66
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.706(2)
_cell_length_b                   25.099(5)
_cell_length_c                   19.033(4)
_cell_measurement_reflns_used    3555
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      1.62
_cell_volume                     5592.1(19)
_computing_cell_refinement       'SAINT v4.05 (Bruker, 1996)'
_computing_data_collection       'SMART v4.05 (Bruker, 1996)'
_computing_data_reduction        'XPREP SHELXTL v5 (Bruker, 1994)'
_computing_molecular_graphics    'XP SHELXTL v5 (Bruker, 1994)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '5.7 pixels mm-1'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type
'Bruker Smart 1K CCD Area Detector Diffractometer'
_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  0.0860
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24616
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    5.345
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.844
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.274
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0483P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                2858
_reflns_number_total             3555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0259585si20030213_080256_5.cif
_cod_data_source_block           final[(dbbpy)Pt(dmid)]2[TCNE].C6H6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        5592.2(19)
_cod_database_code               4313893
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-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 0.044259(19) 0.276743(9) 0.5000 0.01214(8) Uani 1 2 d S . .
S1 S -0.02142(9) 0.33210(5) 0.41600(5) 0.0176(2) Uani 1 1 d . . .
S2 S -0.13651(12) 0.43939(5) 0.42262(6) 0.0296(3) Uani 1 1 d . . .
N1 N 0.1091(3) 0.22225(14) 0.4319(2) 0.0152(7) Uani 1 1 d . . .
O1 O -0.2015(5) 0.5209(2) 0.5000 0.0412(15) Uani 1 2 d S . .
C2 C -0.1652(7) 0.4764(3) 0.5000 0.0305(17) Uani 1 2 d S . .
C1 C -0.0823(4) 0.38317(18) 0.4647(2) 0.0178(9) Uani 1 1 d . . .
C3 C 0.1055(4) 0.22538(18) 0.3611(2) 0.0190(9) Uani 1 1 d . . .
H3A H 0.0715 0.2551 0.3407 0.023 Uiso 1 1 calc R . .
C6 C 0.2049(4) 0.13860(17) 0.4199(2) 0.0144(8) Uani 1 1 d . . .
C7 C 0.1587(3) 0.17832(17) 0.4609(2) 0.0131(9) Uani 1 1 d . . .
C5 C 0.2018(4) 0.14170(17) 0.3467(2) 0.0148(9) Uani 1 1 d . . .
C4 C 0.1491(4) 0.18707(18) 0.3181(2) 0.0188(9) Uani 1 1 d . . .
H4A H 0.1440 0.1910 0.2696 0.023 Uiso 1 1 calc R . .
C11 C 0.1582(4) 0.0777(2) 0.2511(3) 0.0220(10) Uani 1 1 d . . .
C10 C 0.3437(4) 0.1273(2) 0.2518(3) 0.0216(10) Uani 1 1 d . . .
C8 C 0.2530(4) 0.10026(17) 0.2973(2) 0.0165(9) Uani 1 1 d . . .
C12 C -0.2142(6) 0.2291(3) 0.5000 0.0272(16) Uani 1 2 d S . .
C9 C 0.3086(5) 0.0547(2) 0.3382(3) 0.0231(10) Uani 1 1 d . . .
N2 N -0.1538(4) 0.1832(2) 0.3846(3) 0.0465(14) Uani 1 1 d . . .
C13 C -0.1803(4) 0.2033(2) 0.4357(3) 0.0299(12) Uani 1 1 d . . .
C2SA C -0.5000 0.5000 0.427(2) 0.065(18) Uani 0.50 2 d SP . 1
H2SA H -0.5000 0.5000 0.3786 0.078 Uiso 0.50 2 calc SPR . 1
C1SA C -0.525(4) 0.5432(17) 0.459(2) 0.064(14) Uani 0.50 1 d P . 1
H1SA H -0.5435 0.5739 0.4344 0.077 Uiso 0.50 1 calc PR . 1
C2SB C -0.535(3) 0.5482(18) 0.5000 0.069(13) Uani 0.50 2 d SP . 2
H2SC H -0.5606 0.5833 0.5000 0.083 Uiso 0.50 2 calc SPR . 2
C1SB C -0.520(6) 0.527(2) 0.438(3) 0.13(4) Uani 0.50 1 d P . 2
H1SE H -0.5337 0.5461 0.3966 0.156 Uiso 0.50 1 calc PR . 2
H11C H 0.106(5) 0.059(2) 0.282(3) 0.029(15) Uiso 1 1 d . . .
H11B H 0.194(4) 0.0495(18) 0.219(2) 0.008(11) Uiso 1 1 d . . .
H9C H 0.249(4) 0.0361(19) 0.371(3) 0.026(14) Uiso 1 1 d . . .
H9B H 0.367(4) 0.0646(19) 0.366(2) 0.014(12) Uiso 1 1 d . . .
H11A H 0.121(4) 0.101(2) 0.224(3) 0.024(14) Uiso 1 1 d . . .
H9A H 0.341(4) 0.033(2) 0.307(3) 0.026(14) Uiso 1 1 d . . .
H10B H 0.382(4) 0.096(2) 0.225(3) 0.031(15) Uiso 1 1 d . . .
H10A H 0.403(5) 0.141(2) 0.283(3) 0.036(16) Uiso 1 1 d . . .
H6A H 0.237(4) 0.1099(18) 0.440(2) 0.015(12) Uiso 1 1 d . . .
H10C H 0.315(5) 0.149(2) 0.223(3) 0.033(16) 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'
Pt Pt -1.7033 8.3905 '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'
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 N1 79.3(2) . 10_556 ?
N1 Pt1 S1 174.46(10) . 10_556 ?
N1 Pt1 S1 95.14(11) 10_556 10_556 ?
N1 Pt1 S1 95.14(11) . . ?
N1 Pt1 S1 174.46(10) 10_556 . ?
S1 Pt1 S1 90.39(6) 10_556 . ?
C1 S1 Pt1 102.51(15) . . ?
C1 S2 C2 96.4(2) . . ?
C3 N1 C7 117.7(4) . . ?
C3 N1 Pt1 125.9(3) . . ?
C7 N1 Pt1 116.4(3) . . ?
O1 C2 S2 123.8(2) . . ?
O1 C2 S2 123.8(2) . 10_556 ?
S2 C2 S2 112.3(4) . 10_556 ?
C1 C1 S1 122.30(15) 10_556 . ?
C1 C1 S2 117.37(15) 10_556 . ?
S1 C1 S2 120.2(3) . . ?
N1 C3 C4 123.1(4) . . ?
C7 C6 C5 121.0(4) . . ?
N1 C7 C6 121.6(4) . . ?
N1 C7 C7 113.9(2) . 10_556 ?
C6 C7 C7 124.5(2) . 10_556 ?
C6 C5 C4 116.3(4) . . ?
C6 C5 C8 124.6(4) . . ?
C4 C5 C8 119.1(4) . . ?
C3 C4 C5 120.3(4) . . ?
C5 C8 C11 108.8(4) . . ?
C5 C8 C9 111.3(4) . . ?
C11 C8 C9 109.0(4) . . ?
C5 C8 C10 108.6(4) . . ?
C11 C8 C10 110.1(4) . . ?
C9 C8 C10 109.0(4) . . ?
C12 C12 C13 121.6(3) 13_456 . ?
C12 C12 C13 121.6(3) 13_456 10_556 ?
C13 C12 C13 116.3(7) . 10_556 ?
N2 C13 C12 179.5(7) . . ?
C1SA C2SA C1SA 123(5) . 2_465 ?
C2SA C1SA C1SA 118(2) . 10_556 ?
C1SB C2SB C1SB 130(7) . 10_556 ?
C2SB C1SB C1SB 115(3) . 2_465 ?
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 2.032(4) . ?
Pt1 N1 2.032(4) 10_556 ?
Pt1 S1 2.2533(11) 10_556 ?
Pt1 S1 2.2533(11) . ?
S1 C1 1.735(4) . ?
S2 C1 1.742(4) . ?
S2 C2 1.773(4) . ?
N1 C3 1.350(6) . ?
N1 C7 1.363(5) . ?
O1 C2 1.195(8) . ?
C2 S2 1.773(4) 10_556 ?
C1 C1 1.344(9) 10_556 ?
C3 C4 1.362(6) . ?
C6 C7 1.376(6) . ?
C6 C5 1.396(6) . ?
C7 C7 1.490(8) 10_556 ?
C5 C4 1.405(6) . ?
C5 C8 1.524(6) . ?
C11 C8 1.525(6) . ?
C10 C8 1.529(6) . ?
C8 C9 1.527(6) . ?
C12 C12 1.341(14) 13_456 ?
C12 C13 1.441(7) . ?
C12 C13 1.441(7) 10_556 ?
N2 C13 1.139(7) . ?
C2SA C1SA 1.28(6) . ?
C2SA C1SA 1.28(6) 2_465 ?
C1SA C1SA 1.54(9) 10_556 ?
C2SB C1SB 1.31(6) . ?
C2SB C1SB 1.31(6) 10_556 ?
C1SB C1SB 1.45(11) 2_465 ?
