Electron Distribution in the Nonclassical Bis(dithiolene) Electron Transfer Series [M(CO)2(S2C2Me2)2]0/1-/2- (M = Mo, W): Assessment by Structural, Spectroscopic, and Density Functional Theory Results
Dmitry V. Fomitchev; Booyong S. Lim; R. H. Holm; Inorganic Chemistry 40 (2001) 645–654; doi:10.1021/ic001046w

data_4319264
_publ_contact_author
;
       R.H. Holm
       Department of Chemistry and Chemical Biology
       Harvard University
       Cambridge, MA 02138
       USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_fax         '+1 (617) 496-9289'
_publ_contact_author_phone       '+1 (617) 495-0853'
_publ_section_title
;
 Electron Distribution in the Nonclassical Bis(dithiolene) Electron
 Transfer Series [M(CO)2(S2C2Me2)2]0/1-/2- (M = Mo, W): Assessment by
 Structural, Spectroscopic, and Density Functional Theory Results
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              645
_journal_page_last               654
_journal_paper_doi               10.1021/ic001046w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C28 H58 N2 S6 W'
_chemical_formula_weight         798.97
_chemical_name_systematic
; 
 ? 
;
_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                 104.037(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7642(17)
_cell_length_b                   12.6922(13)
_cell_length_c                   18.4816(19)
_cell_measurement_temperature    233(2)
_cell_volume                     3587.4(6)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.594
_diffrn_measured_fraction_theta_max 0.594
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       'rotation around \o axis, 0.3 deg/frame'
_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  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14290
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    3.589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.002
_refine_diff_density_min         -2.043
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.00011(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+3.6237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                4159
_reflns_number_total             5277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001046w_7.cif
_cod_data_source_block           '[Et4N]2[12]'
_cod_database_code               4319264