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_4068518
_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_moiety         'C31 H50 Br N P2 Ti, 0.5(C5 H12)'
_chemical_formula_sum            'C33.5 H56 Br N P2 Ti'
_chemical_formula_weight         662.54
_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                 90.487(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.7142(7)
_cell_length_b                   41.7972(16)
_cell_length_c                   14.6885(7)
_cell_measurement_reflns_used    8258
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.3
_cell_measurement_theta_min      2.4
_cell_volume                     7191.5(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003), XTEL (loc. libr.)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'XS (Sheldrick, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
'0.5 degree frames measured for 1 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49595
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            78118
_diffrn_reflns_theta_full        19.31
_diffrn_reflns_theta_max         19.31
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_correction_T_min  0.9547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.974
_refine_diff_density_min         -2.245
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         17753
_refine_ls_number_restraints     354
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+17.9822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1972
_reflns_number_gt                14652
_reflns_number_total             17753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800910q_si_002.cif
_cod_data_source_block           07511
_cod_depositor_comments
;

2025-11-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C67 H112 Br2 N2 P4 Ti2'
_cod_original_formula_weight         1325.09
_cod_original_formula_moiety         '2(C31 H50 Br N P2 Ti), C5 H12'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068518