Isoinversion Behavior in the Enantioselective Oxidations of Pyridylmethylthiobenzimidazoles to Chiral Proton Pump Inhibitors on Titanium Salalen Complexes
Talsi, Evgenii P.; Rybalova, Tatyana V.; Bryliakov, Konstantin P.; ACS Catalysis 5 (2015) 4673–; doi:10.1021/acscatal.5b01212

data_4513383
_publ_section_title
;
 Isoinversion Behavior in the Enantioselective Oxidations of
 Pyridylmethylthiobenzimidazoles to Chiral Proton Pump Inhibitors on
 Titanium Salalen Complexes
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              4673
_journal_paper_doi               10.1021/acscatal.5b01212
_journal_volume                  5
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C72 H78 N4 O11 Ti2'
_chemical_formula_sum            'C72 H78 N4 O11 Ti2'
_chemical_formula_weight         1271.18
_chemical_name_common            (R,R,SN-R,R,SN)-2A
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                   12.3687(5)
_cell_length_b                   12.3687(5)
_cell_length_c                   44.436(2)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.33
_cell_volume                     6798.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            40609
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BIPYRAMID
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.41
_platon_squeeze_details
;
;
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7374
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0634P)^2^+1.5249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                6774
_reflns_number_total             7374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs5b01212_si_004.cif
_cod_data_source_block           Ti-2A_brycl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4513383--4513387.cif.
;
_cod_original_sg_symbol_H-M      'P4(3)2(1)2 '
_cod_database_code               4513383