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_4109645
_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_moiety         'C39 H51 N P2 Ti, 0.5(C5 H12) '
_chemical_formula_sum            'C41.5 H57 N P2 Ti'
_chemical_formula_weight         679.72
_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                71.050(2)
_cell_angle_beta                 81.016(2)
_cell_angle_gamma                81.334(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2211(8)
_cell_length_b                   13.1095(11)
_cell_length_c                   15.5962(13)
_cell_measurement_reflns_used    2006
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.53
_cell_volume                     1941.1(3)
_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      128(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
'   0.30 degree frames measured for  10.16 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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18868
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red/orange
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             730
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         8909
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                6417
_reflns_number_total             8909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070989qsi20070211_102452.cif
_cod_data_source_block           05322
_cod_original_sg_symbol_Hall     '-P 1  '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C41.50 H57 N P2 Ti'
_cod_database_code               4109645