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_4110484
_publ_contact_author
;
    Masood Parvez
    Department of Chemistry
    University of Calgary
    2500 University Drive N.W.
    Calgary, Alberta, Canada T2N 1N4  
;
_publ_contact_author_email       ' parvez@ucalgary.ca '
_publ_contact_author_fax         ' (403)289-9488 '
_publ_contact_author_phone       ' (403)220-5348 '
_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 Cl F20 N O2 P Ti'
_chemical_formula_weight         1334.24
_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                71.616(15)
_cell_angle_beta                 77.542(12)
_cell_angle_gamma                84.788(8)
_cell_formula_units_Z            2
_cell_length_a                   12.165(2)
_cell_length_b                   14.823(3)
_cell_length_c                   17.749(3)
_cell_measurement_reflns_used    24213
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.1
_cell_volume                     2964.8(10)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0588
_diffrn_reflns_av_sigmaI/netI    0.1096
_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            24213
_diffrn_reflns_theta_full        27.36
_diffrn_reflns_theta_max         27.36
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_correction_T_min  0.9500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         13325
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.0539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                6951
_reflns_number_total             13325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0583618si20051220_050743.cif
_cod_data_source_block           Compound_I
_cod_original_cell_volume        2964.8(9)
_cod_database_code               4110484