Molybdenum Chalcogenobenzimidato Complexes: Radical Synthesis and Nitrile Extrusion via β-EPh (E = S, Se, and Te) Elimination
Arjun Mendiratta; Christopher C. Cummins; Olga P. Kryatova; Elena V. Rybak-Akimova; James E. McDonough; Carl D. Hoff; Inorganic Chemistry 42 (2003) 8621–8623; doi:10.1021/ic035077d

data_4312836
_publ_section_title
;
 Molybdenum Chalcogenobenzimidato Complexes: Radical Synthesis and Nitrile
 Extrusion via \b-EPh (E = S, Se, and Te) Elimination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8621
_journal_page_last               8623
_journal_paper_doi               10.1021/ic035077d
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C53 H74 Mo N4 O S'
_chemical_formula_weight         911.16
_chemical_name_common            2_S
_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                 111.261(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.534(2)
_cell_length_b                   24.450(2)
_cell_length_c                   21.635(2)
_cell_measurement_reflns_used    13221
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.09
_cell_volume                     10122.7(16)
_computing_cell_refinement       'Brucker SMART'
_computing_data_collection       'Brucker SMART'
_computing_data_reduction        'Brucker SHELXTL'
_computing_molecular_graphics    'Brucker SHELXTL'
_computing_publication_material  'Brucker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37898
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.4332
_exptl_absorpt_correction_T_min  0.3526
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         13221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.227
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+13.7733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                10678
_reflns_number_total             13221
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic035077dsi20030915_124914_1.cif
_cod_data_source_block           002228m
_cod_original_cell_volume        10122.5(18)
_cod_database_code               4312836