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_4327296
_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            'C14 H13 Mo N O5'
_chemical_formula_weight         371.19
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.878(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4839(6)
_cell_length_b                   6.7543(4)
_cell_length_c                   17.5715(9)
_cell_measurement_temperature    100(2)
_cell_volume                     1361.23(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'1028 images at 1.0 deg. stepwise rotaion in omega and phi, 70 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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32182
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.527
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+1.9086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                3581
_reflns_number_total             4339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0603702Bsi20060306_025323_9.cif
_cod_data_source_block           10
_cod_database_code               4327296