Synthesis of Unsymmetrical Diolate, Oxametallacyclopentene, Amido-Alkoxide and Thiolato-Alkoxide Complexes Using Dialkyl and Diaryl Titanium Aminotroponiminate Complexes: A Route to Unsymmetrical Vicinal Diols
Dietrich P. Steinhuebel; Stephen J. Lippard; Journal of the American Chemical Society 121 (1999) 11762–11772; doi:10.1021/ja992662y

data_4116650
_publ_section_title
;
 Synthesis of Unsymmetrical Diolate, Oxametallacyclopentene,
 Amido-Alkoxide and Thiolato-Alkoxide Complexes Using Dialkyl and Diaryl
 Titanium Aminotroponiminate Complexes: A Route to Unsymmetrical Vicinal
 Diols
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11762
_journal_page_last               11772
_journal_paper_doi               10.1021/ja992662y
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C51 H51 N5 O3 S Ti'
_chemical_formula_weight         861.93
_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                60.514(15)
_cell_angle_beta                 88.656(16)
_cell_angle_gamma                87.332(17)
_cell_formula_units_Z            2
_cell_length_a                   13.233(4)
_cell_length_b                   13.823(4)
_cell_length_c                   13.863(3)
_cell_measurement_temperature    188(2)
_cell_volume                     2205.0(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.1056
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13993
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.765334
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         9759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0595
_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^)+(0.1038P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1840
_reflns_number_gt                5559
_reflns_number_total             9759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992662y_4.cif
_cod_data_source_block           14
_cod_original_cell_volume        2205.0(10)
_cod_database_code               4116650