Molybdenum(VI) Dioxo and Oxo-Imido Complexes of Fluorinated β-Ketiminato Ligands and Their Use in OAT Reactions
Manuel Volpe; Nadia C. Mösch-Zanetti; Inorganic Chemistry 51 (2012) 1440–1449; doi:10.1021/ic201681u

data_4328125
_publ_section_title
;
 Molybdenum(VI) Dioxo and Oxo-Imido Complexes of Fluorinated \b-Ketiminato
 Ligands and Their Use in OAT Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1440
_journal_page_last               1449
_journal_paper_doi               10.1021/ic201681u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C25 H27 F6 Mo N2 O3 P, C7 H8'
_chemical_formula_sum            'C32 H35 F6 Mo N2 O3 P'
_chemical_formula_weight         736.53
_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                 95.499(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9011(8)
_cell_length_b                   20.1516(13)
_cell_length_c                   13.5855(10)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.89
_cell_measurement_theta_min      2.65
_cell_volume                     3243.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            96367
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         38.27
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         15579
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+2.4538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                13189
_reflns_number_total             15579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201681u_si_002_2.cif
_cod_data_source_block           moanip
_cod_database_code               4328125