Intermolecular C-H Bond Activation Reactions Promoted by Transient Titanium Alkylidynes. Synthesis, Reactivity, Kinetic, and Theoretical Studies of the Ti\τbC Linkage
Brad C. Bailey; Hongjun Fan; John C. Huffman; Mu-Hyun Baik; Daniel J. Mindiola; Journal of the American Chemical Society 129 (2007) 8781–8793; doi:10.1021/ja070989q

data_4109646
_publ_section_title
;
 Intermolecular C-H Bond Activation Reactions Promoted by Transient
 Titanium Alkylidynes. Synthesis, Reactivity, Kinetic, and Theoretical
 Studies of the Ti\\tbC Linkage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8781
_journal_page_last               8793
_journal_paper_doi               10.1021/ja070989q
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C37 H54 F N P2 Ti'
_chemical_formula_weight         641.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.050(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.246(4)
_cell_length_b                   10.605(2)
_cell_length_c                   20.861(4)
_cell_measurement_reflns_used    983
_cell_measurement_temperature    119(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.29
_cell_volume                     3656.9(13)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'Reciprocal Net (http://recipnet.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      119(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
'   0.30 degree frames measured for 30.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            52410
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown/orange
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       elongated
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+4.0517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                7568
_reflns_number_total             8424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070989qsi20070211_102513.cif
_cod_data_source_block           05342
_cod_original_cell_volume        3656.7(13)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4109646