A Homoleptic Molybdenum(IV) Enolate Complex: Synthesis, Molecular and Electronic Structure, and NCN Group Transfer To Form a Terminal Cyanoimide of Molybdenum(VI)
Han Sen Soo; Joshua S. Figueroa; Christopher C. Cummins; Journal of the American Chemical Society 126 (2004) 11370–11376; doi:10.1021/ja0472533

data_4112940
_publ_section_title
;
 A Homoleptic Molybdenum(IV) Enolate Complex: Synthesis, Molecular and
 Electronic Structure, and NCN Group Transfer To Form a Terminal
 Cyanoimide of Molybdenum(VI)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11370
_journal_page_last               11376
_journal_paper_doi               10.1021/ja0472533
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C93 H129 Mo N O6'
_chemical_formula_weight         1452.91
_chemical_name_common            (tBuNC)Mo(OC[Ad]Mes)4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.402(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7807(11)
_cell_length_b                   22.8234(17)
_cell_length_c                   26.558(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.20
_cell_volume                     8188.2(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT^'
_computing_molecular_graphics    'Bruker SMART'
_computing_publication_material  'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.1648
_diffrn_reflns_av_sigmaI/netI    0.1894
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30887
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       prism
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         10703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1760
_refine_ls_R_factor_gt           0.0862
_refine_ls_shift/su_max          0.247
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.2065
_reflns_number_gt                5561
_reflns_number_total             10703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0472533si20040511_101449_2.cif
_cod_data_source_block           1tBuNC
_cod_database_code               4112940