Oxidatively Induced α-Hydrogen Abstraction. A Mild Protocol to Generate Terminal Titanium Alkylidenes Containing a β-Hydrogen
Bailey, Brad C.; Basuli, Falguni; Huffman, John C.; Mindiola, Daniel J.; Organometallics 25 (2006) 3963–; doi:10.1021/om060308k

data_4075469
_publ_section_title
;
 Oxidatively Induced \a-Hydrogen Abstraction. A Mild Protocol to Generate
 Terminal Titanium Alkylidenes Containing a \b-Hydrogen
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3963
_journal_paper_doi               10.1021/om060308k
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C40 H60 F3 N2 O3 S Ti'
_chemical_formula_weight         753.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.912(9)
_cell_length_b                   18.992(16)
_cell_length_c                   19.841(17)
_cell_measurement_reflns_used    625
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      22.32
_cell_measurement_theta_min      2.32
_cell_volume                     4112(6)
_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      125(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
'   0.30 degree frames measured for 60.17 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  0.3258
_diffrn_reflns_av_sigmaI/netI    0.3952
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19325
_diffrn_reflns_theta_full        23.37
_diffrn_reflns_theta_max         23.37
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange/brown
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.60(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.641
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         5908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.641
_refine_ls_R_factor_all          0.2319
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0024P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                1536
_reflns_number_total             5908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060308ksi20060405_114140.cif
_cod_data_source_block           05438
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P2(1)2(1)2(1) '
_cod_database_code               4075469