C-H Bond Activation of Benzene by Unsaturated η2-Cyclopropene and η2-Benzyne Complexes of Niobium
Cédric Boulho; Pascal Oulié; Laure Vendier; Michel Etienne; Véronique Pimienta; Abel Locati; Fabienne Bessac; Feliu Maseras; Dimitrios A. Pantazis; John E. McGrady; Journal of the American Chemical Society 132 (2010) 14239–14250; doi:10.1021/ja1061505

data_4103225
_publ_contact_author
;
Prof Michel Etienne
;
_publ_contact_author_address
;
CNRS; LCC (Laboratoire de Chimie de Coordination)
205, route de Narbonne
F-31077 Toulouse, France
Universit\'e de Toulouse
UPS, INPT; LCC; 
F-31077 Toulouse,
France
;
_publ_contact_author_email       etienne@lcc-toulouse.fr
_publ_section_title
;
 C-H Bond Activation of Benzene by Unsaturated \h2-Cyclopropene and
 \h2-Benzyne Complexes of Niobium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14239
_journal_page_last               14250
_journal_paper_doi               10.1021/ja1061505
_journal_volume                  132
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H44 B N6 Nb O2'
_chemical_formula_sum            'C28 H44 B N6 Nb O2'
_chemical_formula_weight         600.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.036(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.593(3)
_cell_length_b                   10.0459(6)
_cell_length_c                   27.465(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     8021.8(12)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \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  0.0617
_diffrn_reflns_av_unetI/netI     0.08
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30938
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.809
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         7495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1455
_reflns_number_gt                4222
_reflns_number_total             7495
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1061505_si_003.cif
_cod_data_source_block           cbe120606
_cod_original_cell_volume        8021.8(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4103225