Snapshots of an oxidatively induced alpha-hydrogen abstraction reaction to prepare a terminal and four-coordinate titanium imide
Daniel Mindiola; Falguni Basuli; John C. Huffman; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b304633h

data_7103734
_publ_section_title
;
Snapshots of an oxidatively induced alpha-hydrogen
abstraction reaction to prepare a terminal and four-coordinate titanium
imide
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b304633h
_journal_year                    2003
_chemical_formula_structural     Ti(C29H41N2)(NC6H3iPr2)(O3SCF3);C5H12
_chemical_formula_sum            'C47 H70 F3 N3 O3 S Ti'
_chemical_formula_weight         862.02
_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_date             10/27/2002
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.783(7)
_cell_angle_beta                 106.097(9)
_cell_angle_gamma                96.880(9)
_cell_formula_units_Z            2
_cell_length_a                   10.2710(14)
_cell_length_b                   12.9651(17)
_cell_length_c                   18.451(3)
_cell_measurement_reflns_used    7572
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.44
_cell_volume                     2330.9(6)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(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
'   0.30 degree frames measured for  15.14 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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51577
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_correction_T_min  0.9202
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             924
_exptl_crystal_id                MSC02190
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         10763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.505
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                7221
_reflns_number_total             10763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304633h.txt
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7103734