Dehydrofluorination of Hydrofluorocarbons by Titanium Alkylidynes via Sequential C−H/C−F Bond Activation Reactions. A Synthetic, Structural, and Mechanistic Study of 1,2-CH Bond Addition and β-Fluoride Elimination
Fout, Alison R.; Scott, Jennifer; Miller, Deanna L.; Bailey, Brad C.; Pink, Maren; Mindiola, Daniel J.; Organometallics 28 (2009) 331–; doi:10.1021/om800910q

data_4068516
_publ_section_title
;
 Dehydrofluorination of Hydrofluorocarbons by Titanium Alkylidynes via
 Sequential C&#x2212;H/C&#x2212;F Bond Activation Reactions. A Synthetic,
 Structural, and Mechanistic Study of 1,2-CH Bond Addition and \b-Fluoride
 Elimination
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              331
_journal_paper_doi               10.1021/om800910q
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C36 H53 F2 N P2 Si Ti'
_chemical_formula_weight         675.72
_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                99.512(4)
_cell_angle_beta                 91.907(4)
_cell_angle_gamma                99.270(4)
_cell_formula_units_Z            2
_cell_length_a                   10.027(2)
_cell_length_b                   11.267(3)
_cell_length_c                   16.941(4)
_cell_measurement_reflns_used    1065
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      3.5
_cell_volume                     1859.4(8)
_computing_cell_refinement       'APEX II v.2.2 (Bruker, 2007)'
_computing_data_collection       'APEX II v.2.2 (Bruker, 2007)'
_computing_data_reduction        'APEX II v.2.2 (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2007)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker SMART APEXII'
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details
'0.30 degree frames measured for 180 seconds each'
_diffrn_measurement_device       'APEX II Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22315
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.9700
_exptl_absorpt_correction_T_min  0.9448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6071
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.7685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                4358
_reflns_number_total             6071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800910q_si_002.cif
_cod_data_source_block           07140
_cod_original_cell_volume        1859.5(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068516