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_4112941
_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            'C87 H100 Mo N2 O5.5'
_chemical_formula_weight         1357.63
_chemical_name_common            (NCN)Mo(OC[Ad]Mes)4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 99.320(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.554(4)
_cell_length_b                   20.891(2)
_cell_length_c                   24.730(3)
_cell_measurement_reflns_used    112
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.04
_cell_volume                     17616(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35487
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.3052
_exptl_absorpt_correction_T_min  0.2524
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_description       block
_exptl_crystal_F_000             5776
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.555
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         12649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          14.184
_refine_ls_shift/su_mean         0.065
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                8992
_reflns_number_total             12649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0472533si20040511_101449_3.cif
_cod_data_source_block           complex3
_cod_original_formula_sum        'C87 H100 Mo N2 O5.50'
_cod_database_code               4112941