Benzonitrile Extrusion from Molybdenum(IV) Ketimide Complexes Obtained via Radical C-E (E = O, S, Se) Bond Formation: Toward a New Nitrogen Atom Transfer Reaction
Arjun Mendiratta; Christopher C. Cummins; Olga P. Kryatova; Elena V. Rybak-Akimova; James E. McDonough; Carl D. Hoff; Journal of the American Chemical Society 128 (2006) 4881–4891; doi:10.1021/ja0587796

data_4110529
_publ_section_title
;
 Benzonitrile Extrusion from Molybdenum(IV) Ketimide Complexes Obtained
 via Radical C-E (E = O, S, Se) Bond Formation: Toward a New Nitrogen Atom
 Transfer Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4881
_journal_page_last               4891
_journal_paper_doi               10.1021/ja0587796
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C49 H59 F5 Mo N4 S'
_chemical_formula_weight         927.00
_chemical_name_common            'fluorinated thio ketimide'
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.329(4)
_cell_angle_beta                 74.155(3)
_cell_angle_gamma                76.599(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6395(10)
_cell_length_b                   12.8842(14)
_cell_length_c                   18.843(2)
_cell_measurement_reflns_used    6896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2311.8(4)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47824
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.9129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         11462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+1.3579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                10018
_reflns_number_total             11462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0587796si20060205_113208_3.cif
_cod_data_source_block           05008
_cod_database_code               4110529