Rational Design of anl-Histidine-Derived Minimal Artificial Acylase for the Kinetic Resolution of Racemic Alcohols
Kazuaki Ishihara; Yuji Kosugi; Matsujiro Akakura; Journal of the American Chemical Society 126 (2004) 12212–12213; doi:10.1021/ja045850j

data_4112975
_publ_section_title
;
 Rational Design of anl-Histidine-Derived Minimal Artificial Acylase for
 the Kinetic Resolution of Racemic Alcohols
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12212
_journal_page_last               12213
_journal_paper_doi               10.1021/ja045850j
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C38 H53 N3 O3 S Si'
_chemical_formula_weight         659.98
_chemical_name_systematic
;
(S)-1-tert-Butyldiphenylsilyloxy-3-(3'-methyl-3'H-imidazol-4'-yl)-
2-(2",4",6"-triisopropylbenzenesulfonylamino)propane
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            8
_cell_length_a                   10.1626(9)
_cell_length_b                   21.9774(19)
_cell_length_c                   34.178(3)
_cell_measurement_temperature    173(2)
_cell_volume                     7633.6(12)
_computing_cell_refinement       'Bruker Smart APEX'
_computing_data_collection       'Bruker Smart APEX'
_computing_data_reduction        'Bruker Smart APEX'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  'ORTEP 3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       'omega mode'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            58323
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.9699
_exptl_absorpt_correction_T_min  0.9553
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker Smart APEX'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         20367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                15321
_reflns_number_total             20367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja045850jsi20040716_034726.cif
_cod_data_source_block           1d
_cod_original_cell_volume        7633.6(11)
_cod_database_code               4112975