C-H Bond Activation of Arenes by a Transient η2-Cyclopropene Niobium Complex
Pascal Oulié; Cédric Boulho; Laure Vendier; Yannick Coppel; Michel Etienne; Journal of the American Chemical Society 128 (2006) 15962–15963; doi:10.1021/ja066985n

data_4111226
_publ_contact_author
;
Michel Etienne
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       etienne@lcc-toulouse.fr
_publ_section_title
;
 C-H Bond Activation of Arenes by a Transient \h2-Cyclopropene Niobium
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15962
_journal_page_last               15963
_journal_paper_doi               10.1021/ja066985n
_journal_volume                  128
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H42 B1 N6 Nb'
_chemical_formula_sum            'C33 H42 B N6 Nb'
_chemical_formula_weight         626.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90
_cell_angle_beta                 97.966(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5725(9)
_cell_length_b                   18.7234(15)
_cell_length_c                   15.1039(12)
_cell_measurement_reflns_used    3351
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.17
_cell_measurement_theta_min      2.55
_cell_measurement_wavelength     0.71073
_cell_volume                     3241.1(4)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_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  0.0618
_diffrn_reflns_av_unetI/netI     0.0909
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24339
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1491
_reflns_number_gt                3913
_reflns_number_total             6622
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja066985nsi20060928_123022.cif
_cod_data_source_block           global
_cod_database_code               4111226