Monoanionic Molybdenum and Tungsten Tris(dithiolene) Complexes: A Multifrequency EPR Study
Stephen Sproules; Priyabrata Banerjee; Thomas Weyhermüller; Yong Yan; James P. Donahue; Karl Wieghardt; Inorganic Chemistry 50 (2011) 7106–7122; doi:10.1021/ic2006265

data_4325780
_publ_section_title
;
 Monoanionic Molybdenum and Tungsten Tris(dithiolene) Complexes: A
 Multifrequency EPR Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7106
_journal_page_last               7122
_journal_paper_doi               10.1021/ic2006265
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C42 H30 S6 W, C24 H20 P, C H2 Cl2'
_chemical_formula_sum            'C67 H52 Cl2 P S6 W'
_chemical_formula_weight         1335.17
_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                 116.597(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1851(6)
_cell_length_b                   31.0048(12)
_cell_length_c                   14.8110(6)
_cell_measurement_temperature    100(2)
_cell_volume                     5824.6(4)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
'2592 images at 0.5 deg. stepwise rotation in omega and phi, 15 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 40 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            115582
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    2.360
_exptl_absorpt_correction_T_max  0.5283
_exptl_absorpt_correction_T_min  0.3910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_refine_diff_density_max         6.362
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         16917
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+25.1729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                15858
_reflns_number_total             16917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2006265_si_002_5.cif
_cod_data_source_block           5
_cod_database_code               4325780