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_4328128
_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         'C34 H35 F6 Mo N3 O3'
_chemical_formula_sum            'C34 H35 F6 Mo N3 O3'
_chemical_formula_weight         743.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.261(3)
_cell_angle_beta                 97.153(3)
_cell_angle_gamma                109.447(3)
_cell_formula_units_Z            4
_cell_length_a                   12.1333(9)
_cell_length_b                   14.5487(11)
_cell_length_c                   20.2490(14)
_cell_measurement_reflns_used    4129
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.72
_cell_volume                     3310.2(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    'SIR-92 (Giacovazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            123716
_diffrn_reflns_theta_full        26.27
_diffrn_reflns_theta_max         26.27
_diffrn_reflns_theta_min         1.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         13091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0577P)^2^+2.7058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                10295
_reflns_number_total             13091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201681u_si_002_5.cif
_cod_data_source_block           mofluo
_cod_database_code               4328128