Enantioselective Addition of Diethylzinc to Aldehydes Catalyzed by Titanium(IV) Complexes of Diol Derivatives ofd-Mannitol and the Spectroscopic Study of the Catalytic System
You, Jing-Song; Shao, Ming-Yuan; Gau, Han-Mou; Organometallics 19 (2000) 3368–; doi:10.1021/om000265m

data_4077513
_publ_section_title
;
 Enantioselective Addition of Diethylzinc to Aldehydes Catalyzed by
 Titanium(IV) Complexes of Diol Derivatives ofd-Mannitol and the
 Spectroscopic Study of the Catalytic System
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3368
_journal_paper_doi               10.1021/om000265m
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C36 H68 O16 Ti2'
_chemical_formula_weight         852.70
_chemical_melting_point          108.5(5)
_chemical_name_systematic
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 bis[(m-1,2:5,6-di-O-isopropylidene-D-mannitolate)bis(2-propoxo)titanium(IV)]

;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 90.724(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6698(13)
_cell_length_b                   24.129(3)
_cell_length_c                   10.2718(14)
_cell_measurement_reflns_used    3983
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.055
_cell_measurement_theta_min      2.155
_cell_volume                     2396.5(5)
_computing_data_collection       'Smart-1000 (Bruker)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Smart-1000
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12169
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.713892
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal plate'
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6586
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          1.043
_refine_ls_shift/su_mean         0.122
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                4442
_reflns_number_total             6586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000265m.cif
_cod_data_source_block           complex_4(OM000265M)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '108-109' was changed to '108.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4077513