Synthesis, Structures, and Properties of Mixed Dithiolene-Carbonyl and Dithiolene-Phosphine Complexes of Tungsten
P. Chandrasekaran; Kuppuswamy Arumugam; Upul Jayarathne; Lisa M. Pérez; Joel T. Mague; James P. Donahue; Inorganic Chemistry 48 (2009) 2103–2113; doi:10.1021/ic802016b

data_4301585
_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_moiety         'C12 H24 O2 P2 S2 W'
_chemical_formula_sum            'C12 H24 O2 P2 S2 W'
_chemical_formula_weight         510.22
_chemical_name_systematic
; 
 But-2-ene-2,3-dithiolatodicarbonylbis(trimethyl 
phosphine)tungsten(II) 
;
_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                 105.522(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.633(4)
_cell_length_b                   10.553(3)
_cell_length_c                   13.062(4)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.48
_cell_volume                     1810.7(9)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w 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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30894
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    6.783
_exptl_absorpt_correction_T_max  0.5446
_exptl_absorpt_correction_T_min  0.3732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0145
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0088P)^2^+1.2117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0355
_reflns_number_gt                4350
_reflns_number_total             4497
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic802016b_si_001_6.cif
_cod_data_source_block           jpd221
_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        1810.6(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301585