Dis-assembly of a Benzylic CF3 Group Mediated by a Niobium(III) Imido Complex
Thomas L. Gianetti; Robert G. Bergman; John Arnold; Journal of the American Chemical Society 135 (2013) 8145–8148; doi:10.1021/ja4033007

data_4119858
_publ_section_title
;
 Dis-assembly of a Benzylic CF3 Group Mediated by a Niobium(III) Imido
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8145
_journal_page_last               8148
_journal_paper_doi               10.1021/ja4033007
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C41 H54 F6 N3 Nb'
_chemical_formula_sum            'C41 H54 F6 N3 Nb'
_chemical_formula_weight         795.78
_chemical_name_common            'Complex 2b'
_chemical_temperature_decomposition 476(1)
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.9710(16)
_cell_length_b                   16.6536(13)
_cell_length_c                   22.7371(17)
_cell_measurement_reflns_used    9238
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.30
_cell_volume                     7940.8(11)
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0088
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            194464
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9084
_exptl_absorpt_correction_T_min  0.8835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0232P)^2^+8.3500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                6551
_reflns_number_total             7298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4033007_si_002_2.cif
_cod_data_source_block           (2)
_cod_database_code               4119858