Competitive ArC-H and ArC-X (X = Cl, Br) Activation in Halobenzenes at Cationic Titanium Centers
Kuangbiao Ma; Warren E. Piers; Masood Parvez; Journal of the American Chemical Society 128 (2006) 3303–3312; doi:10.1021/ja0583618

data_4110485
_publ_contact_author
;
    Masood Parvez
    Department of Chemistry
    University of Calgary
    2500 University Drive N.W.
    Calgary, Alberta, Canada T2N 1N4  
;
_publ_section_title
;
 Competitive ArC-H and ArC-X (X = Cl, Br) Activation in Halobenzenes at
 Cationic Titanium Centers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3303
_journal_page_last               3312
_journal_paper_doi               10.1021/ja0583618
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C60 H62 B Br F20 N O2 P Ti'
_chemical_formula_weight         1378.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.772(7)
_cell_angle_beta                 77.525(6)
_cell_angle_gamma                84.712(7)
_cell_formula_units_Z            2
_cell_length_a                   12.244(2)
_cell_length_b                   14.765(2)
_cell_length_c                   17.718(3)
_cell_measurement_reflns_used    25258
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.7
_cell_volume                     2969.5(8)
_computing_cell_refinement       'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \w and \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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25258
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.4
_diffrn_reflns_theta_min         2.7
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.9451
_exptl_absorpt_correction_T_min  0.8784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       prism
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         13405
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+8.1200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2294
_reflns_number_gt                9528
_reflns_number_total             13405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0583618si20051220_050816.cif
_cod_data_source_block           Compound_I
_cod_database_code               4110485