Solvent control of optical resolution of 2-amino-1-phenylethanol using dehydroabietic acid
Taniguchi, Kayoko; Aruga, Marie; Yasutake, Mikio; Hirose, Takuji; Organic & Biomolecular Chemistry 6 (2008) 458–463; doi:10.1039/b717071h

data_7150841
_publ_section_title
;
 Solvent control of optical resolution of 2-amino-1-phenylethanol using
 dehydroabietic acid
;
_journal_issue                   3
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              458
_journal_page_last               463
_journal_paper_doi               10.1039/b717071h
_journal_volume                  6
_journal_year                    2008
_chemical_absolute_configuration syn
_chemical_formula_moiety         ' C20 H27 O2, C8 H12 N O, C2 H6 O'
_chemical_formula_sum            'C30 H45 N O4'
_chemical_formula_weight         483.67
_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                 106.42(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.595(3)
_cell_length_b                   6.1165(12)
_cell_length_c                   18.862(4)
_cell_measurement_temperature    123(2)
_cell_volume                     1393.8(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    Ortep3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELS-97
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7017
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.9970
_exptl_absorpt_correction_T_min  0.9692
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'see text'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3349
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                2396
_reflns_number_total             3349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717071h.txt
_cod_data_source_block           R-APE/DAA
_cod_original_cell_volume        1393.8(5)
_cod_original_sg_symbol_Hall     P2yb
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7150841