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_4068513
_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            'C37 H52 F3 N P2 Ti'
_chemical_formula_weight         677.64
_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                 115.027(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.321(4)
_cell_length_b                   10.832(2)
_cell_length_c                   21.141(4)
_cell_measurement_reflns_used    1414
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.2
_cell_volume                     3801.6(13)
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
'0.30 degree frames measured for 150 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  0.1687
_diffrn_reflns_av_sigmaI/netI    0.2248
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18262
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.9496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.784
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6552
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.2357
_refine_ls_R_factor_gt           0.1096
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1895P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2767
_refine_ls_wR_factor_ref         0.3595
_reflns_number_gt                2533
_reflns_number_total             6552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800910q_si_002.cif
_cod_data_source_block           07126
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068513