#------------------------------------------------------------------------------
#$Date: 2020-06-05 11:55:46 +0200 (vie 05 de jun de 2020) $
#$Revision: 252718 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/62/7126248.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7126248
loop_
_publ_author_name
'Liu, Gongyi'
'Zhang, Xianghe'
'Wang, Heng'
'Cong, Hengjiang'
'Zhang, Xumu'
'Dong, Xiu-Qin'
_publ_section_title
;
 Synthesis of chiral α-substituted α-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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  94.00   0.50    0.50    --    5.00  36.00 152.00  258
  2  ω    -35.00  94.00   0.50    0.50    --    5.00  36.00 152.00  258
  3  ω   -131.00  -7.00   0.50    0.50    --  -96.70  62.00 136.00  248
  4  ω    -82.00  42.00   0.50    0.50    --  -47.40  57.00   0.00  248
  5  ω   -137.00  -8.00   0.50    0.50    --  -47.40 -38.00 -90.00  258
  6  ω   -186.00 -62.00   0.50    0.50    --  -96.70 -57.00-120.00  248
  7  ω   -186.00 -57.00   0.50    0.50    --  -96.70 -38.00  30.00  258
  8  ω   -186.00 -57.00   0.50    0.50    --  -96.70 -38.00-180.00  258
  9  ω   -186.00 -62.00   0.50    0.50    --  -96.70 -62.00  -1.00  248
 10  ω   -131.00  -7.00   0.50    0.50    --  -96.70  57.00 150.00  248
 11  ω   -186.00 -56.00   0.50    0.50    --  -96.70 -36.00  -3.00  260
 12  ω   -186.00 -60.00   0.50    0.50    --  -96.70 -45.00 154.00  252
 13  ω   -137.00  -8.00   0.50    0.50    --  -47.40 -75.00-120.00  258
 14  ω   -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 ω-scans and φ-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/[σ²(Fo²)+(0.0410P)²+0.1653P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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
;
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.04377(9) 0.88800(9) 0.39293(2) 0.05074(16) Uani 1 1 d . . . . .
O3 O 0.1738(3) 1.0581(2) 0.38958(4) 0.0624(4) Uani 1 1 d . . . . .
O1 O -0.0712(2) 0.8015(3) 0.43291(3) 0.0556(4) Uani 1 1 d . . . . .
O5 O 0.2176(3) 0.6734(3) 0.31712(4) 0.0626(4) Uani 1 1 d . . . . .
O4 O 0.2195(3) 0.5564(3) 0.52496(4) 0.0743(5) Uani 1 1 d . . . . .
N1 N -0.0740(3) 0.6907(3) 0.36868(4) 0.0509(4) Uani 1 1 d . . . . .
O2 O -0.2157(3) 0.9280(3) 0.38737(4) 0.0781(6) Uani 1 1 d . . . . .
C7 C 0.0673(3) 0.6001(3) 0.37696(5) 0.0467(4) Uani 1 1 d . . . . .
C9 C 0.2702(3) 0.7083(4) 0.35413(5) 0.0514(4) Uani 1 1 d . . . . .
C2 C 0.0760(4) 0.6863(3) 0.47866(5) 0.0519(5) Uani 1 1 d . . . . .
C4 C 0.1148(3) 0.6056(3) 0.41658(5) 0.0459(4) Uani 1 1 d . . . . .
C3 C 0.0452(3) 0.6968(3) 0.44204(5) 0.0466(4) Uani 1 1 d . . . . .
C1 C 0.1824(4) 0.5817(4) 0.49001(5) 0.0565(5) Uani 1 1 d . . . . .
C5 C 0.2257(4) 0.5057(4) 0.42907(6) 0.0576(5) Uani 1 1 d . . . . .
C6 C 0.2607(5) 0.4938(4) 0.46493(6) 0.0666(6) Uani 1 1 d . . . . .
C8 C 0.1290(5) 0.6283(5) 0.55179(6) 0.0692(7) Uani 1 1 d . . . . .
H9A H 0.361(4) 0.647(4) 0.3584(7) 0.059(6) Uiso 1 1 d . . . . .
H9B H 0.358(4) 0.864(4) 0.3599(6) 0.056(6) Uiso 1 1 d . . . . .
H7 H -0.023(4) 0.453(4) 0.3694(5) 0.045(5) Uiso 1 1 d . . . . .
H5A H 0.293(4) 0.455(4) 0.4119(6) 0.066(7) Uiso 1 1 d . . . . .
H5 H 0.173(6) 0.733(6) 0.3114(8) 0.088(11) Uiso 1 1 d . . . . .
H6 H 0.333(5) 0.420(5) 0.4731(6) 0.076(8) Uiso 1 1 d . . . . .
H8A H -0.016(5) 0.570(5) 0.5488(7) 0.073(8) Uiso 1 1 d . . . . .
H8B H 0.170(5) 0.589(5) 0.5771(8) 0.086(9) Uiso 1 1 d . . . . .
H2 H 0.016(4) 0.754(4) 0.4937(5) 0.061(6) Uiso 1 1 d . . . . .
H1 H -0.197(4) 0.609(4) 0.3658(6) 0.056(7) Uiso 1 1 d . . . . .
H8C H 0.182(5) 0.785(5) 0.5483(7) 0.077(8) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 S1 O1 106.53(9) . . ?
O3 S1 N1 108.22(10) . . ?
O1 S1 N1 104.61(9) . . ?
O2 S1 O3 120.36(12) . . ?
O2 S1 O1 105.47(9) . . ?
O2 S1 N1 110.44(11) . . ?
C3 O1 S1 116.27(11) . . ?
C9 O5 H5 111(3) . . ?
C1 O4 C8 118.2(2) . . ?
S1 N1 H1 110.1(18) . . ?
C7 N1 S1 116.61(13) . . ?
C7 N1 H1 117(2) . . ?
N1 C7 C9 110.30(17) . . ?
N1 C7 C4 112.70(16) . . ?
N1 C7 H7 100.6(13) . . ?
C9 C7 H7 110.0(13) . . ?
C4 C7 C9 112.96(16) . . ?
C4 C7 H7 109.6(12) . . ?
O5 C9 C7 110.75(17) . . ?
O5 C9 H9A 105.1(15) . . ?
O5 C9 H9B 111.9(13) . . ?
C7 C9 H9A 111.4(15) . . ?
C7 C9 H9B 110.9(14) . . ?
H9A C9 H9B 106.5(19) . . ?
C3 C2 H2 114.9(13) . . ?
C1 C2 C3 118.50(19) . . ?
C1 C2 H2 126.6(13) . . ?
C3 C4 C7 123.79(18) . . ?
C3 C4 C5 116.55(17) . . ?
C5 C4 C7 119.59(17) . . ?
C2 C3 O1 114.62(17) . . ?
C4 C3 O1 122.19(16) . . ?
C4 C3 C2 123.15(19) . . ?
O4 C1 C2 124.4(2) . . ?
O4 C1 C6 115.8(2) . . ?
C2 C1 C6 119.75(19) . . ?
C4 C5 H5A 119.3(14) . . ?
C6 C5 C4 121.9(2) . . ?
C6 C5 H5A 118.5(14) . . ?
C1 C6 H6 119.1(14) . . ?
C5 C6 C1 120.1(2) . . ?
C5 C6 H6 120.8(14) . . ?
O4 C8 H8A 111.6(17) . . ?
O4 C8 H8B 107.1(16) . . ?
O4 C8 H8C 109.3(17) . . ?
H8A C8 H8B 113(2) . . ?
H8A C8 H8C 102(3) . . ?
H8B C8 H8C 114(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.4236(17) . ?
S1 O1 1.5908(14) . ?
S1 N1 1.5986(18) . ?
S1 O2 1.4114(17) . ?
O1 C3 1.413(2) . ?
O5 C9 1.422(2) . ?
O5 H5 0.68(3) . ?
O4 C1 1.362(2) . ?
O4 C8 1.422(3) . ?
N1 C7 1.482(3) . ?
N1 H1 0.78(3) . ?
C7 C9 1.520(3) . ?
C7 C4 1.515(2) . ?
C7 H7 0.96(2) . ?
C9 H9A 0.96(3) . ?
C9 H9B 0.99(3) . ?
C2 C3 1.393(3) . ?
C2 C1 1.376(3) . ?
C2 H2 0.97(2) . ?
C4 C3 1.380(3) . ?
C4 C5 1.388(3) . ?
C1 C6 1.392(3) . ?
C5 C6 1.373(3) . ?
C5 H5A 0.97(3) . ?
C6 H6 0.96(3) . ?
C8 H8A 0.91(3) . ?
C8 H8B 1.07(3) . ?
C8 H8C 1.00(3) . ?
