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_4325777
_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 Mo S6, C24 H20 P, C H2 Cl2'
_chemical_formula_sum            'C67 H52 Cl2 Mo P S6'
_chemical_formula_weight         1247.26
_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                 116.543(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.101(2)
_cell_length_b                   30.901(4)
_cell_length_c                   14.709(2)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      2.51
_cell_volume                     5733.7(14)
_computing_cell_refinement       'Bruker SAINT 7.34a'
_computing_data_collection       'Bruker SAINT 7.34a'
_computing_data_reduction        'Bruker SAINT 7.34a'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX2, INCOTEC Multi-Layer-Optics'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            112508
_diffrn_reflns_theta_full        26.74
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Vers. 2006/1 Bruker AXS (2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             2564
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         12019
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0447P)^2^+8.5984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                9949
_reflns_number_total             12019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2006265_si_002_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        5733.7(13)
_cod_database_code               4325777