#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:16:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179053 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/15/4301586.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_4301586
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            'C12 H21 O P S4 W'
_chemical_formula_weight         524.35
_chemical_name_systematic
; 
 Bis(but-2-ene-2,3-dithiolato-κ²S,S')(carbonyl)
(trimethylphosphine)tungsten(IV) 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.982(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9220(12)
_cell_length_b                   9.5740(13)
_cell_length_c                   21.246(3)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.33
_cell_volume                     1813.7(4)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2008a)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2008a)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008b)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω 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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0208
_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       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31081
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    6.908
_exptl_absorpt_correction_T_max  0.5225
_exptl_absorpt_correction_T_min  0.4513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008a)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0052P)²+1.8300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0342
_refine_ls_wR_factor_ref         0.0345
_reflns_number_gt                4371
_reflns_number_total             4513
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic802016b_si_001_7.cif
_cod_data_source_block           jpd226_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        1813.8(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301586
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
W1 W 0.698701(8) 0.412654(8) 0.862433(4) 0.00899(3) Uani 1 1 d . . .
S1 S 0.65448(5) 0.38509(5) 0.75304(2) 0.01219(9) Uani 1 1 d . . .
S2 S 0.89806(5) 0.26044(5) 0.84123(2) 0.01357(10) Uani 1 1 d . . .
S3 S 0.60587(6) 0.64242(5) 0.84975(2) 0.01319(10) Uani 1 1 d . . .
S4 S 0.86301(5) 0.53016(6) 0.93330(2) 0.01344(10) Uani 1 1 d . . .
P1 P 0.42460(6) 0.37149(6) 0.86085(3) 0.01159(10) Uani 1 1 d . . .
O1 O 0.68904(19) 0.21896(18) 0.98224(8) 0.0229(3) Uani 1 1 d . . .
C1 C 0.8040(2) 0.2965(2) 0.72151(10) 0.0141(4) Uani 1 1 d . . .
C2 C 0.9090(2) 0.2374(2) 0.76048(10) 0.0141(4) Uani 1 1 d . . .
C3 C 0.7083(2) 0.7565(2) 0.89748(10) 0.0157(4) Uani 1 1 d . . .
C4 C 0.8225(2) 0.7068(2) 0.93466(10) 0.0146(4) Uani 1 1 d . . .
C5 C 0.8075(3) 0.2938(3) 0.65080(10) 0.0202(5) Uani 1 1 d . . .
H5A H 0.8574 0.3782 0.6359 0.030 Uiso 1 1 calc R . .
H5B H 0.7046 0.2904 0.6331 0.030 Uiso 1 1 calc R . .
H5C H 0.8626 0.2111 0.6373 0.030 Uiso 1 1 calc R . .
C6 C 1.0388(2) 0.1517(3) 0.73865(11) 0.0213(5) Uani 1 1 d . . .
H6A H 1.0036 0.0874 0.7054 0.032 Uiso 1 1 calc R . .
H6B H 1.0819 0.0981 0.7742 0.032 Uiso 1 1 calc R . .
H6C H 1.1154 0.2138 0.7221 0.032 Uiso 1 1 calc R . .
C7 C 0.6641(3) 0.9086(2) 0.89442(13) 0.0265(5) Uani 1 1 d . . .
H7A H 0.6279 0.9380 0.9354 0.040 Uiso 1 1 calc R . .
H7B H 0.5844 0.9214 0.8620 0.040 Uiso 1 1 calc R . .
H7C H 0.7514 0.9650 0.8839 0.040 Uiso 1 1 calc R . .
C8 C 0.9172(3) 0.7969(3) 0.97862(11) 0.0229(5) Uani 1 1 d . . .
H8A H 0.9523 0.8789 0.9558 0.034 Uiso 1 1 calc R . .
H8B H 1.0036 0.7431 0.9948 0.034 Uiso 1 1 calc R . .
H8C H 0.8571 0.8273 1.0138 0.034 Uiso 1 1 calc R . .
C9 C 0.6941(2) 0.2898(2) 0.93847(10) 0.0150(4) Uani 1 1 d . . .
C10 C 0.3085(2) 0.4358(2) 0.79521(11) 0.0180(4) Uani 1 1 d . . .
H10A H 0.2026 0.4218 0.8041 0.027 Uiso 1 1 calc R . .
H10B H 0.3326 0.3847 0.7569 0.027 Uiso 1 1 calc R . .
H10C H 0.3278 0.5356 0.7892 0.027 Uiso 1 1 calc R . .
C11 C 0.3733(2) 0.1882(2) 0.86339(12) 0.0207(5) Uani 1 1 d . . .
H11A H 0.4224 0.1441 0.9003 0.031 Uiso 1 1 calc R . .
H11B H 0.4054 0.1417 0.8250 0.031 Uiso 1 1 calc R . .
H11C H 0.2643 0.1798 0.8662 0.031 Uiso 1 1 calc R . .
C12 C 0.3361(2) 0.4429(3) 0.92943(11) 0.0190(4) Uani 1 1 d . . .
H12A H 0.2280 0.4246 0.9263 0.028 Uiso 1 1 calc R . .
H12B H 0.3535 0.5439 0.9314 0.028 Uiso 1 1 calc R . .
H12C H 0.3790 0.3987 0.9676 0.028 Uiso 1 1 calc R . .
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'
P P 0.1023 0.0942 '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 S4 78.12(6) . . ?
C9 W1 S2 80.06(6) . . ?
S4 W1 S2 87.73(2) . . ?
C9 W1 S1 136.27(6) . . ?
S4 W1 S1 139.803(19) . . ?
S2 W1 S1 81.022(18) . . ?
C9 W1 S3 128.52(6) . . ?
S4 W1 S3 80.556(19) . . ?
S2 W1 S3 144.930(19) . . ?
S1 W1 S3 86.890(18) . . ?
C9 W1 P1 82.49(6) . . ?
S4 W1 P1 132.718(18) . . ?
S2 W1 P1 130.619(19) . . ?
S1 W1 P1 80.639(18) . . ?
S3 W1 P1 78.725(18) . . ?
C1 S1 W1 109.30(7) . . ?
C2 S2 W1 109.67(7) . . ?
C3 S3 W1 110.19(8) . . ?
C4 S4 W1 110.64(7) . . ?
C12 P1 C11 102.89(11) . . ?
C12 P1 C10 103.68(11) . . ?
C11 P1 C10 102.30(11) . . ?
C12 P1 W1 112.71(8) . . ?
C11 P1 W1 113.80(8) . . ?
C10 P1 W1 119.56(8) . . ?
C2 C1 C5 124.54(19) . . ?
C2 C1 S1 119.58(16) . . ?
C5 C1 S1 115.88(16) . . ?
C1 C2 C6 124.3(2) . . ?
C1 C2 S2 119.37(16) . . ?
C6 C2 S2 116.36(16) . . ?
C4 C3 C7 123.7(2) . . ?
C4 C3 S3 119.44(17) . . ?
C7 C3 S3 116.86(17) . . ?
C3 C4 C8 123.6(2) . . ?
C3 C4 S4 119.17(16) . . ?
C8 C4 S4 117.17(16) . . ?
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 178.96(18) . . ?
P1 C10 H10A 109.5 . . ?
P1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P1 C11 H11A 109.5 . . ?
P1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P1 C12 H12A 109.5 . . ?
P1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 2.000(2) . ?
W1 S4 2.3514(5) . ?
W1 S2 2.3550(5) . ?
W1 S1 2.3588(6) . ?
W1 S3 2.3626(6) . ?
W1 P1 2.4762(6) . ?
S1 C1 1.735(2) . ?
S2 C2 1.736(2) . ?
S3 C3 1.730(2) . ?
S4 C4 1.730(2) . ?
P1 C12 1.815(2) . ?
P1 C11 1.815(2) . ?
P1 C10 1.816(2) . ?
O1 C9 1.153(3) . ?
C1 C2 1.353(3) . ?
C1 C5 1.504(3) . ?
C2 C6 1.505(3) . ?
C3 C4 1.354(3) . ?
C3 C7 1.509(3) . ?
C4 C8 1.508(3) . ?
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 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
