An Eight-Coordinate Vanadium Thiolate Complex with Charge Delocalization between V(V)-Thiolate and V(IV)-Thiyl Radical Forms
Ya-Ho Chang; Chia-Ling Su; Ru-Rong Wu; Ju-Hsiou Liao; Yi-Hung Liu; Hua-Fen Hsu; Journal of the American Chemical Society 133 (2011) 5708–5711; doi:10.1021/ja2004208

data_4105975
_publ_section_title
;
 An Eight-Coordinate Vanadium Thiolate Complex with Charge Delocalization
 between V(V)-Thiolate and V(IV)-Thiyl Radical Forms
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5708
_journal_page_last               5711
_journal_paper_doi               10.1021/ja2004208
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C52 H59 O2 P2 S3 Si3 V'
_chemical_formula_weight         1009.32
_chemical_name_common            '[PPh4][VO(OMe)(PS3")]'
_chemical_name_systematic
; 
 ? 
;
_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                 91.043(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6229(12)
_cell_length_b                   14.6619(12)
_cell_length_c                   25.248(2)
_cell_measurement_temperature    298(2)
_cell_volume                     5412.3(8)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    Ortep-3
_computing_publication_material  'Wingx publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       'phi-omega scan'
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38764
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  0.9845
_exptl_absorpt_correction_T_min  0.9773
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       needle
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                6092
_reflns_number_total             9533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2004208_si_002_1.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        5412.2(8)
_cod_database_code               4105975