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_4119859
_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         'C33 H48 N3 Nb'
_chemical_formula_sum            'C33 H48 N3 Nb'
_chemical_formula_weight         579.65
_chemical_melting_point          439(1)
_chemical_name_common            'Complex 3'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 111.256(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2011(4)
_cell_length_b                   18.8526(9)
_cell_length_c                   9.5779(4)
_cell_measurement_reflns_used    9386
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.16
_cell_volume                     1548.40(12)
_computing_cell_refinement       'Bruker APEX2 v.2009.1'
_computing_data_collection       'Bruker APEX2 v.2009.1'
_computing_data_reduction        'Bruker APEX2 v.2009.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.871
_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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12610
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.9756
_exptl_absorpt_correction_T_min  0.9183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       rode
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+1.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                4542
_reflns_number_total             4997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4033007_si_002_3.cif
_cod_data_source_block           (3)
_cod_database_code               4119859