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_4325776
_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, C H2 Cl2'
_chemical_formula_sum            'C43 H32 Cl2 Mo S6'
_chemical_formula_weight         907.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.470(4)
_cell_angle_beta                 100.012(4)
_cell_angle_gamma                97.854(4)
_cell_formula_units_Z            4
_cell_length_a                   11.9102(6)
_cell_length_b                   16.7887(9)
_cell_length_c                   22.286(2)
_cell_measurement_temperature    100(2)
_cell_volume                     4073.7(5)
_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 KappaCCD'
_diffrn_measurement_method
'2308 images at 0.5 deg. stepwise rotation in omega and phi, 10 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            96279
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2006/1'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.36
_refine_diff_density_max         2.124
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         29361
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+4.1510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                26718
_reflns_number_total             29361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2006265_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4325776