#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:16:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179053 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/15/4301583.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_4301583
loop_
_publ_author_name
'P. Chandrasekaran'
'Kuppuswamy Arumugam'
'Upul Jayarathne'
'Lisa M. Pérez'
'Joel T. Mague'
'James P. Donahue'
_publ_contact_author             'James P. Donahue'
_publ_contact_author_address
;
   James P. Donahue
   Department of Chemistry
   Tulane University
   Percival Stern Hall, Room 2015
   6400 Freret Street
   New Orleans, Louisiana 70118-5698
;
_publ_contact_author_email       donahue@tulane.edu
_publ_section_title
;
Synthesis, Structures, and Properties of Mixed Dithiolene-Carbonyl and
Dithiolene-Phosphine Complexes of Tungsten
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2103
_journal_page_last               2113
_journal_paper_doi               10.1021/ic802016b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C10 H12 O2 S4 W'
_chemical_formula_weight         476.29
_chemical_name_systematic
; 
 Dicarbonylbis(1,2-dimethylethene-1,2-dithiolato- 
κ²S,S')tungsten 
;
_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                93.5060(10)
_cell_angle_beta                 93.8910(10)
_cell_angle_gamma                95.5160(10)
_cell_formula_units_Z            2
_cell_length_a                   7.0364(3)
_cell_length_b                   7.6373(3)
_cell_length_c                   13.5606(6)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.27
_cell_measurement_theta_min      2.69
_cell_volume                     722.01(5)
_computing_cell_refinement       'Bruker APEX2 (Bruker-AXS, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2006)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2006a)'
_computing_molecular_graphics    'Bruker APEX2 (Bruker-AXS, 2006)'
_computing_publication_material  'Bruker APEX2 (Bruker-AXS, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12457
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    8.564
_exptl_absorpt_correction_T_max  0.7257
_exptl_absorpt_correction_T_min  0.3078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0175
_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)+(0.0195P)²+0.0498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0402
_reflns_number_gt                3216
_reflns_number_total             3434
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic802016b_si_001_4.cif
_cod_data_source_block           jpd138_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4301583
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.723992(15) 0.777725(14) 0.733299(8) 0.01356(4) Uani 1 1 d . . .
S1 S 1.01643(10) 0.93655(9) 0.79810(5) 0.01677(14) Uani 1 1 d . . .
S2 S 0.60060(10) 0.98310(9) 0.84423(5) 0.01662(14) Uani 1 1 d . . .
S3 S 0.85468(10) 0.75578(10) 0.57735(5) 0.01785(14) Uani 1 1 d . . .
S4 S 0.43804(10) 0.77143(10) 0.62963(5) 0.01720(14) Uani 1 1 d . . .
O1 O 0.9961(3) 0.4765(3) 0.76407(17) 0.0280(5) Uani 1 1 d . . .
O2 O 0.4342(3) 0.5239(3) 0.84007(17) 0.0266(5) Uani 1 1 d . . .
C1 C 0.9710(4) 1.1032(4) 0.8818(2) 0.0173(6) Uani 1 1 d . . .
C2 C 0.7864(4) 1.1258(4) 0.9004(2) 0.0155(5) Uani 1 1 d . . .
C3 C 0.6764(4) 0.7623(4) 0.4846(2) 0.0168(6) Uani 1 1 d . . .
C4 C 0.4912(4) 0.7653(4) 0.5072(2) 0.0165(6) Uani 1 1 d . . .
C5 C 1.1406(4) 1.2169(4) 0.9312(2) 0.0204(6) Uani 1 1 d . . .
H5A H 1.1288 1.3404 0.9183 0.031 Uiso 1 1 calc R . .
H5B H 1.2581 1.1804 0.9048 0.031 Uiso 1 1 calc R . .
H5C H 1.1459 1.2041 1.0028 0.031 Uiso 1 1 calc R . .
C6 C 0.7357(4) 1.2695(4) 0.9727(2) 0.0226(6) Uani 1 1 d . . .
H6A H 0.7904 1.2514 1.0392 0.034 Uiso 1 1 calc R . .
H6B H 0.5961 1.2659 0.9730 0.034 Uiso 1 1 calc R . .
H6C H 0.7877 1.3846 0.9526 0.034 Uiso 1 1 calc R . .
C7 C 0.7381(4) 0.7592(4) 0.3799(2) 0.0241(7) Uani 1 1 d . . .
H7A H 0.7189 0.6381 0.3501 0.036 Uiso 1 1 calc R . .
H7B H 0.8738 0.8030 0.3810 0.036 Uiso 1 1 calc R . .
H7C H 0.6615 0.8345 0.3408 0.036 Uiso 1 1 calc R . .
C8 C 0.3247(4) 0.7633(4) 0.4316(2) 0.0230(6) Uani 1 1 d . . .
H8A H 0.3609 0.8388 0.3786 0.035 Uiso 1 1 calc R . .
H8B H 0.2159 0.8074 0.4633 0.035 Uiso 1 1 calc R . .
H8C H 0.2887 0.6424 0.4035 0.035 Uiso 1 1 calc R . .
C9 C 0.8996(4) 0.5866(4) 0.7525(2) 0.0185(6) Uani 1 1 d . . .
C10 C 0.5369(4) 0.6170(4) 0.8013(2) 0.0186(6) Uani 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'
O O 0.0106 0.0060 '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'
W W -0.8490 6.8722 '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
C9 W1 C10 84.16(12) . . ?
C9 W1 S3 78.49(8) . . ?
C10 W1 S3 133.05(8) . . ?
C9 W1 S4 129.32(9) . . ?
C10 W1 S4 77.15(9) . . ?
S3 W1 S4 80.96(2) . . ?
C9 W1 S1 76.77(9) . . ?
C10 W1 S1 129.44(9) . . ?
S3 W1 S1 88.34(3) . . ?
S4 W1 S1 148.03(3) . . ?
C9 W1 S2 133.22(8) . . ?
C10 W1 S2 79.01(8) . . ?
S3 W1 S2 141.56(3) . . ?
S4 W1 S2 88.80(2) . . ?
S1 W1 S2 81.05(2) . . ?
C1 S1 W1 109.73(10) . . ?
C2 S2 W1 109.32(10) . . ?
C3 S3 W1 109.57(10) . . ?
C4 S4 W1 109.68(10) . . ?
C2 C1 C5 123.3(3) . . ?
C2 C1 S1 119.6(2) . . ?
C5 C1 S1 117.1(2) . . ?
C1 C2 C6 122.5(3) . . ?
C1 C2 S2 120.3(2) . . ?
C6 C2 S2 117.2(2) . . ?
C4 C3 C7 123.5(3) . . ?
C4 C3 S3 120.2(2) . . ?
C7 C3 S3 116.3(2) . . ?
C3 C4 C8 124.2(3) . . ?
C3 C4 S4 119.4(2) . . ?
C8 C4 S4 116.3(2) . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C9 W1 178.7(3) . . ?
O2 C10 W1 178.6(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
W1 C9 2.019(3) . ?
W1 C10 2.020(3) . ?
W1 S3 2.3657(7) . ?
W1 S4 2.3699(7) . ?
W1 S1 2.3711(7) . ?
W1 S2 2.3722(7) . ?
S1 C1 1.720(3) . ?
S2 C2 1.722(3) . ?
S3 C3 1.721(3) . ?
S4 C4 1.726(3) . ?
O1 C9 1.142(4) . ?
O2 C10 1.141(3) . ?
C1 C2 1.365(4) . ?
C1 C5 1.499(4) . ?
C2 C6 1.512(4) . ?
C3 C4 1.361(4) . ?
C3 C7 1.513(4) . ?
C4 C8 1.501(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
