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_4115198
_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_formula_sum            'C81 H100 O5 Si3 Ti'
_chemical_formula_weight         1285.78
_chemical_name_systematic
; 
 ? 
;
_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                79.350(10)
_cell_angle_beta                 84.900(10)
_cell_angle_gamma                76.400(10)
_cell_formula_units_Z            2
_cell_length_a                   11.242(2)
_cell_length_b                   13.483(3)
_cell_length_c                   25.368(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3668.8(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18975
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.215
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_F_000             1380
_refine_diff_density_max         .860
_refine_diff_density_min         -.417
_refine_diff_density_rms         .089
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         9593
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+42.6988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2522
_refine_ls_wR_factor_ref         0.2558
_reflns_number_gt                8368
_reflns_number_total             9593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0271577_s2_2.cif
_cod_data_source_block           k00034xx
_cod_database_code               4115198