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_4111227
_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         'C28 H38 B1 N6 Nb1'
_chemical_formula_sum            'C28 H38 B N6 Nb'
_chemical_formula_weight         562.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.789(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7281(7)
_cell_length_b                   11.1998(7)
_cell_length_c                   18.2865(12)
_cell_measurement_reflns_used    6500
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.0523
_cell_measurement_theta_min      2.8795
_cell_measurement_wavelength     0.71073
_cell_volume                     2797.2(3)
_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    'SIR92 (Giacovazzo et al, 1993)'
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18924
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.9698
_exptl_absorpt_correction_T_min  0.8474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.0625
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+5.0304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                4621
_reflns_number_total             5695
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja066985nsi20060928_123059.cif
_cod_data_source_block           global
_cod_database_code               4111227