Synthesis, Structure, and Characterization of Molybdenum(VI) Imido Complexes with N-Salicylidene-2-aminophenol
Martin Minelli; Frances Namuswe; Daniel Jeffrey; Amy L. Morrow; Ilia A. Guzei; Dale Swenson; Eberhard Bothe; Thomas Weyhermüller; Inorganic Chemistry 45 (2006) 5455–5464; doi:10.1021/ic060370+

data_4327295
_publ_section_title
;
 Synthesis, Structure, and Characterization of Molybdenum(VI) Imido
 Complexes with N-Salicylidene-2-aminophenol
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5455
_journal_page_last               5464
_journal_paper_doi               10.1021/ic060370+
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C31 H32 Mo N4 O3'
_chemical_formula_weight         604.55
_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                 99.995(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8469(5)
_cell_length_b                   12.7485(7)
_cell_length_c                   25.1199(14)
_cell_measurement_temperature    100(2)
_cell_volume                     2790.1(3)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'1706 images at 0.5 deg. stepwise rotation in omega and phi, 35 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            21653
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7440
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0797P)^2^+0.7451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                5638
_reflns_number_total             7440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0603702Bsi20060306_025323_8.cif
_cod_data_source_block           9
_cod_database_code               4327295