Ancillary Ligand Effects upon Dithiolene Redox Noninnocence in Tungsten Bis(dithiolene) Complexes
Yong Yan; Christopher Keating; Perumalreddy Chandrasekaran; Upul Jayarathne; Joel T. Mague; Serena DeBeer; Kyle M. Lancaster; Stephen Sproules; Igor V. Rubtsov; James P. Donahue; Inorganic Chemistry 52 (2013) 6743–6751; doi:10.1021/ic4009174

data_4335149
_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
;
 Ancillary Ligand Effects upon Dithiolene Redox Noninnocence in Tungsten
 Bis(dithiolene) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6743
_journal_page_last               6751
_journal_paper_doi               10.1021/ic4009174
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C12 H18 S6 W, C8 H20 N, 0.5(C6 H6)'
_chemical_formula_sum            'C23 H41 N S6 W'
_chemical_formula_weight         707.78
_chemical_name_systematic
; 
 Tetraethylammonium tris(butane-2,3-dithiolato)tungstate(V) 
 hemibenzene solvate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.042(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5750(11)
_cell_length_b                   24.536(3)
_cell_length_c                   12.7760(15)
_cell_measurement_reflns_used    9087
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.35
_cell_volume                     2884.6(6)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009a)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009a)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEx 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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24096
_diffrn_reflns_theta_full        27.20
_diffrn_reflns_theta_max         27.20
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    4.451
_exptl_absorpt_correction_T_max  0.9162
_exptl_absorpt_correction_T_min  0.6586
_exptl_absorpt_correction_type   'integration numerical gaussian'
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.104
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         6417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+2.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                4479
_reflns_number_total             6417
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic4009174_si_002_14.cif
_cod_data_source_block           jpd379b1_0m
_cod_database_code               4335149