Intermolecular Activation of C-X (X = H, O, F) Bonds by a Ti\τbCtBu Linkage
Brad C. Bailey; John C. Huffman; Daniel J. Mindiola; Journal of the American Chemical Society 129 (2007) 5302–5303; doi:10.1021/ja0684646

data_4109343
_publ_section_title
;
 Intermolecular Activation of C-X (X = H, O, F) Bonds by a Ti\\tbCtBu
 Linkage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5302
_journal_page_last               5303
_journal_paper_doi               10.1021/ja0684646
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C39.5 H55 F6 N P2 Ti'
_chemical_formula_weight         767.69
_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                75.355(2)
_cell_angle_beta                 80.673(2)
_cell_angle_gamma                78.610(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9914(11)
_cell_length_b                   12.9183(12)
_cell_length_c                   14.0469(13)
_cell_measurement_reflns_used    1813
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      2.56
_cell_volume                     2049.4(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local program)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
'   0.30 degree frames measured for 10.17 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  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37771
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       irregular
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                5794
_reflns_number_total             9442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0684646si20061126_122910.cif
_cod_data_source_block           06143
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C39.50 H55 F6 N P2 Ti'
_cod_database_code               4109343