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_4103226
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H32 B1 N6 Nb1 O1'
_chemical_formula_sum            'C26 H32 B N6 Nb O'
_chemical_formula_weight         548.3
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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
_cell_angle_beta                 93.729(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2075(5)
_cell_length_b                   15.1721(9)
_cell_length_c                   10.3794(6)
_cell_measurement_reflns_used    5964
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.0935
_cell_measurement_theta_min      2.4821
_cell_measurement_wavelength     0.71073
_cell_volume                     1289.76(13)
_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, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_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_orient_matrix_UB_11      -0.0152843312
_diffrn_orient_matrix_UB_12      -0.0376511149
_diffrn_orient_matrix_UB_13      -0.0394605606
_diffrn_orient_matrix_UB_21      -0.0256223131
_diffrn_orient_matrix_UB_22      -0.0236720192
_diffrn_orient_matrix_UB_23      0.0539752108
_diffrn_orient_matrix_UB_31      -0.0813131986
_diffrn_orient_matrix_UB_32      0.0145570421
_diffrn_orient_matrix_UB_33      -0.0143054762
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10138
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.06
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5170
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0534
_reflns_number_gt                4196
_reflns_number_total             5170
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1061505_si_004.cif
_cod_data_source_block           cbe161107
_cod_database_code               4103226