Synthesis of chiral α-substituted α-amino acid and amine derivatives through Ni-catalyzed asymmetric hydrogenation.
Liu, Gongyi; Zhang, Xianghe; Wang, Heng; Cong, Hengjiang; Zhang, Xumu; Dong, Xiu-Qin; Chemical communications (Cambridge, England) 56 (2020) 4934–4937; doi:10.1039/d0cc01220c

data_7126248
_publ_section_title
;
 Synthesis of chiral \a-substituted \a-amino acid and amine derivatives
 through Ni-catalyzed asymmetric hydrogenation.
;
_journal_issue                   36
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4934
_journal_page_last               4937
_journal_paper_doi               10.1039/d0cc01220c
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C9 H11 N O5 S'
_chemical_formula_sum            'C9 H11 N O5 S'
_chemical_formula_weight         245.25
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-20 deposited with the CCDC.	2020-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   7.15760(10)
_cell_length_b                   7.15760(10)
_cell_length_c                   37.3509(3)
_cell_measurement_reflns_used    15515
_cell_measurement_temperature    298.98(13)
_cell_measurement_theta_max      71.4390
_cell_measurement_theta_min      3.5120
_cell_volume                     1657.17(4)
_computing_cell_refinement
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_collection
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_reduction
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.98(13)
_diffrn_detector                 'Hybrid Pixel Counting (HPC) detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HyPix-6000HE'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -35.00  94.00   0.50    0.50    --    5.00  36.00 152.00  258
  2  \w    -35.00  94.00   0.50    0.50    --    5.00  36.00 152.00  258
  3  \w   -131.00  -7.00   0.50    0.50    --  -96.70  62.00 136.00  248
  4  \w    -82.00  42.00   0.50    0.50    --  -47.40  57.00   0.00  248
  5  \w   -137.00  -8.00   0.50    0.50    --  -47.40 -38.00 -90.00  258
  6  \w   -186.00 -62.00   0.50    0.50    --  -96.70 -57.00-120.00  248
  7  \w   -186.00 -57.00   0.50    0.50    --  -96.70 -38.00  30.00  258
  8  \w   -186.00 -57.00   0.50    0.50    --  -96.70 -38.00-180.00  258
  9  \w   -186.00 -62.00   0.50    0.50    --  -96.70 -62.00  -1.00  248
 10  \w   -131.00  -7.00   0.50    0.50    --  -96.70  57.00 150.00  248
 11  \w   -186.00 -56.00   0.50    0.50    --  -96.70 -36.00  -3.00  260
 12  \w   -186.00 -60.00   0.50    0.50    --  -96.70 -45.00 154.00  252
 13  \w   -137.00  -8.00   0.50    0.50    --  -47.40 -75.00-120.00  258
 14  \w   -137.00  -8.00   0.50    0.50    --  -47.40 -75.00  90.00  258
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from \w-scans and \phi-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0890730000
_diffrn_orient_matrix_UB_12      -0.0309717000
_diffrn_orient_matrix_UB_13      0.0356987000
_diffrn_orient_matrix_UB_21      0.1063602000
_diffrn_orient_matrix_UB_22      -0.1108492000
_diffrn_orient_matrix_UB_23      -0.0200435000
_diffrn_orient_matrix_UB_31      0.2062594000
_diffrn_orient_matrix_UB_32      0.2201112000
_diffrn_orient_matrix_UB_33      -0.0050719000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'VariMax VHF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            19791
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.279
_diffrn_reflns_theta_min         3.550
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 785 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0410P)^2^+0.1653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.613
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                2082
_reflns_number_total             2116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01220c2.cif
_cod_data_source_block           dongxq-liugongyi-lgy-5-104-3-rt-20200111
_cod_depositor_comments
'Adding full bibliography for 7126247--7126248.cif.'
_cod_original_cell_volume        1657.17(5)
_cod_database_code               7126248
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'H C N O'
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.812
_reflns_odcompleteness_completeness 98.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
;
_shelx_res_checksum              71356
_shelx_hkl_checksum              84199
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.591
_oxdiff_exptl_absorpt_empirical_full_min 0.741