Asymmetric Transamination of α-Keto Acids Catalyzed by Chiral Pyridoxamines.
Lan, Xiaoyu; Tao, Chuangan; Liu, Xuliang; Zhang, Aina; Zhao, Baoguo; Organic letters 18 (2016) 3658–3661; doi:10.1021/acs.orglett.6b01714

data_1555640
_publ_section_title
;
 Asymmetric Transamination of \a-Keto Acids Catalyzed by Chiral
 Pyridoxamines.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3658
_journal_page_last               3661
_journal_paper_doi               10.1021/acs.orglett.6b01714
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C22 H29 N2 O4.5 S'
_chemical_formula_weight         425.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.916(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0776(15)
_cell_length_b                   24.432(5)
_cell_length_c                   11.904(2)
_cell_measurement_reflns_used    4227
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      49.842
_cell_measurement_theta_min      4.920
_cell_volume                     2222.4(7)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15414
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.667
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
; 
 Flack x determined using 2995 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_coef       0.007(2)
_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   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         8126
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+1.9991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1903
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                7180
_reflns_number_total             8126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01714_si_002.cif
_cod_data_source_block           mo_dm15350_0m
_cod_depositor_comments
;

2022-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C44 H58 N4 O9 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     851.06
_cod_database_code               1555640
_shelxl_version_number           2013-4
_shelx_res_checksum              60065
_shelx_hkl_checksum              64620