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_4110528
_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            'C45 H64 Mo N3 O2.5'
_chemical_formula_weight         782.93
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.669(2)
_cell_angle_beta                 81.701(2)
_cell_angle_gamma                75.221(2)
_cell_formula_units_Z            4
_cell_length_a                   10.8341(11)
_cell_length_b                   19.982(2)
_cell_length_c                   20.569(2)
_cell_measurement_reflns_used    3242
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.59
_cell_volume                     4258.3(7)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega 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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29816
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.9530
_exptl_absorpt_correction_T_min  0.8482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       rod
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         20113
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.9498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                16638
_reflns_number_total             20113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0587796si20060205_113208_2.cif
_cod_data_source_block           04077
_cod_original_cell_volume        4258.2(7)
_cod_original_formula_sum        'C45 H64 Mo N3 O2.50'
_cod_database_code               4110528