#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:47:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179306 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/03/4320343.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_4320343
loop_
_publ_author_name
'José Ruiz'
'Venancio Rodríguez'
'Consuelo Vicente'
'José M. Martí'
'Gregorio López'
'José Pérez'
_publ_section_title
;
 Synthesis and Reactivity of Bridging and Terminal Hydrosulfido Palladium
 and Platinum Complexes. Crystal Structures of
 [NBu4]2[{Pt(C6F5)2(μ-SH)}2], [Pt(C6F5)2(PPh3){S(H)AgPPh3}], and
 [Pt(C6F5)2(PPh3){S(AuPPh3)2}]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5354
_journal_page_last               5360
_journal_paper_doi               10.1021/ic0013633
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C56 H74 F20 N2 Pt2 S2'
_chemical_formula_weight         1609.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.706(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7811(9)
_cell_length_b                   12.4547(8)
_cell_length_c                   19.5582(16)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.18
_cell_measurement_theta_min      10.28
_cell_volume                     3024.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7056
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    4.789
_exptl_absorpt_correction_T_max  0.8048
_exptl_absorpt_correction_T_min  0.6226
_exptl_absorpt_correction_type   PSI
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5295
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          2.239
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0590P)²+7.9899P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                4583
_reflns_number_total             5295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0013633_1.cif
_cod_data_source_block           complex3
_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.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320343
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.375218(15) 0.550664(17) 0.006355(11) 0.02731(9) Uani 1 1 d . . .
F16 F 0.2131(3) 0.5485(3) -0.1471(2) 0.0451(9) Uani 1 1 d . . .
F13 F 0.2052(4) 0.9446(3) -0.0332(2) 0.0552(11) Uani 1 1 d . . .
C11 C 0.2755(4) 0.6624(4) -0.0476(3) 0.0257(11) Uani 1 1 d . . .
F25 F 0.2449(3) 0.5864(3) 0.24714(19) 0.0469(9) Uani 1 1 d . . .
F23 F 0.0118(3) 0.4021(3) 0.0629(2) 0.0468(9) Uani 1 1 d . . .
F26 F 0.3866(3) 0.6124(3) 0.16770(18) 0.0406(8) Uani 1 1 d . . .
F14 F 0.0883(3) 0.9039(3) -0.1654(2) 0.0528(10) Uani 1 1 d . . .
C26 C 0.2931(4) 0.5607(4) 0.1384(3) 0.0290(12) Uani 1 1 d . . .
F24 F 0.0556(3) 0.4816(3) 0.1957(2) 0.0488(10) Uani 1 1 d . . .
F15 F 0.0927(3) 0.7042(3) -0.22106(19) 0.0551(10) Uani 1 1 d . . .
C25 C 0.2216(5) 0.5481(5) 0.1809(3) 0.0325(13) Uani 1 1 d . . .
F12 F 0.3227(3) 0.7905(3) 0.04344(18) 0.0438(9) Uani 1 1 d . . .
C15 C 0.1507(4) 0.7241(5) -0.1553(3) 0.0357(14) Uani 1 1 d . . .
C12 C 0.2673(4) 0.7650(5) -0.0235(3) 0.0315(12) Uani 1 1 d . . .
C14 C 0.1486(5) 0.8253(5) -0.1276(3) 0.0358(14) Uani 1 1 d . . .
C16 C 0.2132(4) 0.6463(4) -0.1160(3) 0.0294(12) Uani 1 1 d . . .
C23 C 0.1046(5) 0.4563(5) 0.0885(3) 0.0334(13) Uani 1 1 d . . .
C24 C 0.1264(5) 0.4953(5) 0.1553(3) 0.0348(13) Uani 1 1 d . . .
C13 C 0.2069(5) 0.8452(5) -0.0614(3) 0.0368(13) Uani 1 1 d . . .
C21 C 0.2740(4) 0.5263(4) 0.0696(3) 0.0259(11) Uani 1 1 d . . .
C22 C 0.1774(4) 0.4710(4) 0.0471(3) 0.0279(12) Uani 1 1 d . . .
S1 S 0.50204(12) 0.42401(14) 0.06528(9) 0.0385(4) Uani 1 1 d . . .
H1 H 0.541(3) 0.485(4) 0.098(2) 0.000(10) Uiso 1 1 d . . .
F22 F 0.1493(3) 0.4313(3) -0.01898(18) 0.0410(8) Uani 1 1 d . . .
N1 N 0.2810(4) 0.2276(4) -0.1633(3) 0.0406(12) Uani 1 1 d . B .
C69 C 0.2507(5) 0.3203(5) -0.2140(3) 0.0397(14) Uani 1 1 d . . .
H69A H 0.3167 0.3619 -0.2139 0.048 Uiso 1 1 calc R . .
H69B H 0.2013 0.3681 -0.1961 0.048 Uiso 1 1 calc R . .
C79 C 0.1815(5) 0.1655(5) -0.1564(3) 0.0399(14) Uani 1 1 d . . .
H79A H 0.1485 0.1331 -0.2027 0.048 Uiso 1 1 calc R . .
H79B H 0.2050 0.1059 -0.1228 0.048 Uiso 1 1 calc R . .
C68 C 0.1975(5) 0.2909(5) -0.2895(3) 0.0417(14) Uani 1 1 d . . .
H68A H 0.2456 0.2432 -0.3086 0.050 Uiso 1 1 calc R . .
H68B H 0.1295 0.2519 -0.2911 0.050 Uiso 1 1 calc R . .
C66 C 0.1188(7) 0.3655(7) -0.4101(4) 0.067(2) Uani 1 1 d . . .
H66A H 0.1051 0.4323 -0.4372 0.101 Uiso 1 1 calc R . .
H66B H 0.0503 0.3289 -0.4118 0.101 Uiso 1 1 calc R . .
H66C H 0.1653 0.3188 -0.4303 0.101 Uiso 1 1 calc R . .
C89 C 0.3538(5) 0.1492(5) -0.1889(4) 0.0426(15) Uani 1 1 d . . .
H89A H 0.3693 0.0889 -0.1550 0.051 Uiso 1 1 calc R . .
H89B H 0.3134 0.1194 -0.2344 0.051 Uiso 1 1 calc R . .
C88 C 0.4589(5) 0.1917(5) -0.1987(4) 0.0470(16) Uani 1 1 d . . .
H88A H 0.5034 0.2162 -0.1528 0.056 Uiso 1 1 calc R . .
H88B H 0.4454 0.2543 -0.2308 0.056 Uiso 1 1 calc R . .
C77 C 0.0120(5) 0.1512(5) -0.1166(4) 0.0454(15) Uani 1 1 d . . .
H77A H -0.0176 0.1072 -0.1589 0.055 Uiso 1 1 calc R . .
H77B H 0.0474 0.1022 -0.0782 0.055 Uiso 1 1 calc R . .
C78 C 0.0953(6) 0.2286(5) -0.1324(4) 0.0448(16) Uani 1 1 d . . .
H78A H 0.0603 0.2795 -0.1697 0.054 Uiso 1 1 calc R . .
H78B H 0.1283 0.2704 -0.0897 0.054 Uiso 1 1 calc R . .
C67 C 0.1745(7) 0.3912(6) -0.3334(4) 0.0567(19) Uani 1 1 d . . .
H67A H 0.2429 0.4295 -0.3319 0.068 Uiso 1 1 calc R . .
H67B H 0.1278 0.4393 -0.3133 0.068 Uiso 1 1 calc R . .
C86 C 0.6272(6) 0.1443(7) -0.2381(4) 0.062(2) Uani 1 1 d . . .
H86A H 0.6624 0.0861 -0.2579 0.093 Uiso 1 1 calc R . .
H86B H 0.6724 0.1654 -0.1923 0.093 Uiso 1 1 calc R . .
H86C H 0.6170 0.2060 -0.2701 0.093 Uiso 1 1 calc R . .
C76 C -0.0791(6) 0.2089(6) -0.0953(4) 0.059(2) Uani 1 1 d . . .
H76A H -0.1305 0.1561 -0.0854 0.089 Uiso 1 1 calc R . .
H76B H -0.1156 0.2562 -0.1336 0.089 Uiso 1 1 calc R . .
H76C H -0.0504 0.2517 -0.0529 0.089 Uiso 1 1 calc R . .
C87 C 0.5195(6) 0.1064(6) -0.2290(4) 0.0542(18) Uani 1 1 d . . .
H87A H 0.5305 0.0431 -0.1975 0.065 Uiso 1 1 calc R . .
H87B H 0.4751 0.0834 -0.2753 0.065 Uiso 1 1 calc R . .
C99 C 0.3356(7) 0.2797(6) -0.0922(3) 0.062(2) Uani 1 1 d D . .
H99A H 0.2970 0.3473 -0.0876 0.074 Uiso 1 1 calc R A 1
H99B H 0.4102 0.2991 -0.0935 0.074 Uiso 1 1 calc R A 1
C98 C 0.3403(11) 0.2098(10) -0.0240(7) 0.042(4) Uani 0.60(2) 1 d PD B 1
H98A H 0.3342 0.2578 0.0153 0.050 Uiso 0.60(2) 1 calc PR B 1
H98B H 0.2782 0.1600 -0.0328 0.050 Uiso 0.60(2) 1 calc PR B 1
C97 C 0.4415(13) 0.1469(15) -0.0029(8) 0.073(6) Uani 0.60(2) 1 d P B 1
H97A H 0.5026 0.1929 -0.0076 0.087 Uiso 0.60(2) 1 calc PR B 1
H97B H 0.4378 0.0855 -0.0355 0.087 Uiso 0.60(2) 1 calc PR B 1
C96 C 0.463(2) 0.105(2) 0.0718(10) 0.090(7) Uani 0.60(2) 1 d P B 1
H96A H 0.5303 0.0638 0.0823 0.134 Uiso 0.60(2) 1 calc PR B 1
H96B H 0.4034 0.0581 0.0767 0.134 Uiso 0.60(2) 1 calc PR B 1
H96C H 0.4689 0.1652 0.1046 0.134 Uiso 0.60(2) 1 calc PR B 1
C98' C 0.4034(16) 0.1983(16) -0.0396(9) 0.052(6) Uani 0.40(2) 1 d PD B 2
H98C H 0.4072 0.1280 -0.0625 0.062 Uiso 0.40(2) 1 calc PR B 2
H98D H 0.4775 0.2255 -0.0209 0.062 Uiso 0.40(2) 1 calc PR B 2
C97' C 0.3427(14) 0.1889(18) 0.0191(11) 0.054(6) Uani 0.40(2) 1 d PD B 2
H97C H 0.3292 0.2614 0.0359 0.064 Uiso 0.40(2) 1 calc PR B 2
H97D H 0.2723 0.1536 0.0005 0.064 Uiso 0.40(2) 1 calc PR B 2
C96' C 0.408(3) 0.124(3) 0.0793(14) 0.074(8) Uani 0.40(2) 1 d PD B 2
H96D H 0.3687 0.1184 0.1165 0.111 Uiso 0.40(2) 1 calc PR B 2
H96E H 0.4772 0.1599 0.0980 0.111 Uiso 0.40(2) 1 calc PR B 2
H96F H 0.4206 0.0522 0.0626 0.111 Uiso 0.40(2) 1 calc PR B 2
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'
F F 0.0171 0.0103 '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'
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
C11 Pt1 C21 90.4(2) . . ?
C11 Pt1 S1 91.37(15) . 3_665 ?
C21 Pt1 S1 178.22(15) . 3_665 ?
C11 Pt1 S1 175.72(15) . . ?
C21 Pt1 S1 93.82(15) . . ?
S1 Pt1 S1 84.43(6) 3_665 . ?
C16 C11 C12 112.9(5) . . ?
C16 C11 Pt1 123.3(4) . . ?
C12 C11 Pt1 123.6(4) . . ?
F26 C26 C21 119.6(5) . . ?
F26 C26 C25 116.2(5) . . ?
C21 C26 C25 124.2(5) . . ?
F25 C25 C24 119.8(5) . . ?
F25 C25 C26 120.7(5) . . ?
C24 C25 C26 119.4(5) . . ?
F15 C15 C16 121.5(6) . . ?
F15 C15 C14 119.1(5) . . ?
C16 C15 C14 119.4(5) . . ?
F12 C12 C13 116.5(5) . . ?
F12 C12 C11 118.6(5) . . ?
C13 C12 C11 124.8(6) . . ?
F14 C14 C13 120.3(6) . . ?
F14 C14 C15 120.6(6) . . ?
C13 C14 C15 119.1(5) . . ?
F16 C16 C15 116.3(5) . . ?
F16 C16 C11 119.7(5) . . ?
C15 C16 C11 123.9(5) . . ?
F23 C23 C24 119.7(5) . . ?
F23 C23 C22 120.1(5) . . ?
C24 C23 C22 120.1(6) . . ?
F24 C24 C23 120.4(6) . . ?
F24 C24 C25 120.6(6) . . ?
C23 C24 C25 119.1(5) . . ?
C14 C13 F13 119.8(5) . . ?
C14 C13 C12 119.8(6) . . ?
F13 C13 C12 120.4(6) . . ?
C26 C21 C22 113.7(5) . . ?
C26 C21 Pt1 124.2(4) . . ?
C22 C21 Pt1 122.1(4) . . ?
F22 C22 C21 119.9(5) . . ?
F22 C22 C23 116.7(5) . . ?
C21 C22 C23 123.4(5) . . ?
Pt1 S1 Pt1 95.57(6) 3_665 . ?
C69 N1 C89 111.0(5) . . ?
C69 N1 C79 110.9(5) . . ?
C89 N1 C79 107.1(5) . . ?
C69 N1 C99 105.1(5) . . ?
C89 N1 C99 112.8(5) . . ?
C79 N1 C99 110.1(5) . . ?
N1 C69 C68 116.1(5) . . ?
C78 C79 N1 116.6(5) . . ?
C67 C68 C69 109.7(5) . . ?
C88 C89 N1 117.0(5) . . ?
C89 C88 C87 111.0(6) . . ?
C76 C77 C78 112.3(6) . . ?
C79 C78 C77 109.3(5) . . ?
C68 C67 C66 111.5(6) . . ?
C86 C87 C88 113.1(6) . . ?
N1 C99 C98' 112.6(8) . . ?
N1 C99 C98 116.6(6) . . ?
C98' C99 C98 34.8(7) . . ?
C97 C98 C99 112.4(12) . . ?
C98 C97 C96 113.4(16) . . ?
C97' C98' C99 104.1(13) . . ?
C96' C97' C98' 110.0(18) . . ?
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 C11 2.009(5) . ?
Pt1 C21 2.014(5) . ?
Pt1 S1 2.3591(15) 3_665 ?
Pt1 S1 2.3577(15) . ?
F16 C16 1.361(6) . ?
F13 C13 1.357(7) . ?
C11 C16 1.400(8) . ?
C11 C12 1.375(8) . ?
F25 C25 1.346(7) . ?
F23 C23 1.354(7) . ?
F26 C26 1.359(6) . ?
F14 C14 1.353(6) . ?
C26 C21 1.379(8) . ?
C26 C25 1.381(8) . ?
F24 C24 1.348(7) . ?
F15 C15 1.347(7) . ?
C25 C24 1.368(9) . ?
F12 C12 1.370(7) . ?
C15 C16 1.370(8) . ?
C15 C14 1.376(9) . ?
C12 C13 1.369(8) . ?
C14 C13 1.354(9) . ?
C23 C24 1.358(9) . ?
C23 C22 1.383(8) . ?
C21 C22 1.390(8) . ?
C22 F22 1.350(7) . ?
S1 Pt1 2.3591(15) 3_665 ?
N1 C69 1.511(8) . ?
N1 C89 1.513(8) . ?
N1 C79 1.521(8) . ?
N1 C99 1.543(8) . ?
C69 C68 1.517(9) . ?
C79 C78 1.515(9) . ?
C68 C67 1.505(9) . ?
C66 C67 1.534(11) . ?
C89 C88 1.498(9) . ?
C88 C87 1.516(10) . ?
C77 C76 1.508(9) . ?
C77 C78 1.522(10) . ?
C86 C87 1.505(10) . ?
C99 C98' 1.554(16) . ?
C99 C98 1.583(13) . ?
C98 C97 1.48(2) . ?
C97 C96 1.51(3) . ?
C98' C97' 1.53(3) . ?
C97' C96' 1.505(18) . ?
