Mechanistic Insight into Fragmentation Reactions of Titanapinacolate Complexes
Jesudoss V. Kingston; Oleg V. Ozerov; Sean Parkin; Carolyn P. Brock; Folami T. Ladipo; Journal of the American Chemical Society 124 (2002) 12217–12224; doi:10.1021/ja0271577

data_4115197
_publ_section_title
;
 Mechanistic Insight into Fragmentation Reactions of Titanapinacolate
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12217
_journal_page_last               12224
_journal_paper_doi               10.1021/ja0271577
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source
;
Synthesized in the laboratory of F. Ladipo
;
_chemical_formula_moiety         'C67 H82 O5 Si Ti, C5 H12'
_chemical_formula_sum            'C72 H94 O5 Si Ti'
_chemical_formula_weight         1115.46
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2000-03-15
_audit_creation_method
'SHELXL-97, macros written locally, and C. P. Brock'
_cell_angle_alpha                90.
_cell_angle_beta                 97.94(1)
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   13.986(1)
_cell_length_b                   11.690(1)
_cell_length_c                   19.815(2)
_cell_measurement_reflns_used    24566
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     3208.6(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT software (Nonius, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL PC (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR92 (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla,
Polidori & Camalli, 1994) in maXus (Mackay, Gilmore,
Edwards, Tremayne, Stewart & Shankland, 1998)
;
_diffrn_ambient_temperature      173(1)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa-CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans with 2.0\% steps'
_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  0.045
_diffrn_reflns_av_sigmaI/netI    0.047
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17997
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        <1.
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description
;
Thin lozenges.
;
_exptl_crystal_F_000             1204
_exptl_crystal_preparation
;
Crystals were grown by slow evaporation of pentane solutions at -15 C.
;
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.25
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         5651
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.053
_refine_ls_R_factor_gt           0.047
_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^)+(0.050P)^2^+1.9P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.109
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                5242
_reflns_number_total             5651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0271577_s2_1.cif
_cod_data_source_block           k99108
_cod_database_code               4115197