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_4325779
_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_sum            'C43 H32 Cl2 S6 W'
_chemical_formula_weight         995.80
_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                108.389(4)
_cell_angle_beta                 100.009(3)
_cell_angle_gamma                97.998(3)
_cell_formula_units_Z            4
_cell_length_a                   11.8989(4)
_cell_length_b                   16.7354(6)
_cell_length_c                   22.2817(8)
_cell_measurement_reflns_used    9230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.80
_cell_volume                     4056.1(3)
_computing_cell_refinement       'Bruker SAINT V7.34A'
_computing_data_collection       'Bruker SAINT V7.34A'
_computing_data_reduction        'Bruker SAINT V7.34A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
'rotating anode, 50 kV, 40 mA, Multi-Layer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            97000
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    3.320
_exptl_absorpt_correction_T_max  0.8831
_exptl_absorpt_correction_T_min  0.7928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.885
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         23613
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+4.7636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                19692
_reflns_number_total             23613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2006265_si_002_4.cif
_cod_data_source_block           4
_cod_original_cell_volume        4056.1(2)
_cod_database_code               4325779