Crystal structure of tert-butyl (R)-(1-(benzylamino)-3-methoxy-1-oxopropan-2-yl)carbamate, C16H24N2O4
Sun, Wei; Zhu, Zhi-Ling; Zuo, Li-Min; Zhao, Ting; Zhu, Ming-Hui; Shan, Guang-Zhi; Zeitschrift für Kristallographie - New Crystal Structures 234 (2018) 119–120; doi:10.1515/ncrs-2018-0219

data_8105561
_publ_section_title
;
 Crystal structure of tert-butyl
 (R)-(1-(benzylamino)-3-methoxy-1-oxopropan-2-yl)carbamate, C16H24N2O4
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              119
_journal_page_last               120
_journal_paper_doi               10.1515/ncrs-2018-0219
_journal_volume                  234
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C16 H24 N2 O4'
_chemical_formula_sum            'C16 H24 N2 O4'
_chemical_formula_weight         308.37
_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   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 94.2278(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7872(2)
_cell_length_b                   5.02626(11)
_cell_length_c                   15.5479(3)
_cell_measurement_reflns_used    8805
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.5610
_cell_measurement_theta_min      4.1150
_cell_volume                     840.70(3)
_computing_cell_refinement
;
CrysAlisPro 1.171.39.32a (Rigaku OD, 2017) [2]
;
_computing_data_collection
;
CrysAlisPro 1.171.39.32a (Rigaku OD, 2017) [2]
;
_computing_data_reduction
;
CrysAlisPro 1.171.39.32a (Rigaku OD, 2017) [2]
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [5]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [4]'
_computing_structure_solution    'Superflip [3]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4674
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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   -129.00 -53.00   1.00    1.00    --  -41.95 178.00  90.00   76
  2  \w     17.00 116.00   1.00    1.00    --   41.95  38.00 -30.00   99
  3  \w     35.00 131.00   1.00    1.00    --   41.95 178.00-180.00   96
  4  \w      1.00 122.00   1.00    1.00    --   41.95  19.00  90.00  121
  5  \w     67.00 166.00   1.00    1.10    --   92.50  45.00-150.00   99
  6  \w      9.00 129.00   1.00    1.10    --   92.50 -89.00 -68.52  120
  7  \w     10.00  84.00   1.00    1.10    --   92.50 -95.00 -90.00   74
  8  \w     20.00 122.00   1.00    1.10    --   92.50 -61.00  60.00  102
  9  \w      9.00 131.00   1.00    1.10    --   92.50 -92.00 136.49  122
 10  \w     63.00 165.00   1.00    1.10    --   92.50  61.00-120.00  102
 11  \w     20.00 122.00   1.00    1.10    --   92.50 -61.00 -60.00  102
 12  \w     10.00  84.00   1.00    1.10    --   92.50 -95.00-180.00   74
 13  \w      9.00 130.00   1.00    1.10    --   92.50 -90.00-146.34  121
 14  \w     11.00 145.00   1.00    1.10    --   92.50 -15.00-120.00  134
 15  \w     10.00  84.00   1.00    1.10    --   92.50 -95.00  30.00   74
 16  \w     16.00 125.00   1.00    1.10    --   92.50 -77.00-180.00  109
 17  \w     40.00 174.00   1.00    1.10    --   92.50  15.00-180.00  134
 18  \w     63.00 165.00   1.00    1.10    --   92.50  61.00   0.00  102
 19  \w     10.00  84.00   1.00    1.10    --   92.50 -95.00  60.00   74
 20  \w     73.00 166.00   1.00    1.10    --   92.50 125.00-120.00   93
 21  \w     67.00 166.00   1.00    1.10    --   92.50  45.00-180.00   99
 22  \w     73.00 166.00   1.00    1.10    --   92.50 125.00 -30.00   93
 23  \w      9.00 118.00   1.00    1.00    --   41.95  77.00 150.00  109
 24  \w     23.00 133.00   1.00    1.00    --   56.00  78.00-153.20  110
 25  \w     31.00 141.00   1.00    1.00    --   64.00  78.00  77.45  110
 26  \w     32.00 140.00   1.00    1.00    --   64.00  76.00 -47.90  108
 27  \w     35.00 145.00   1.00    1.10    --   68.00  79.00 142.39  110
 28  \w     35.00 145.00   1.00    1.10    --   68.00  78.00-112.94  110
 29  \w     39.00 149.00   1.00    1.10    --   72.00  78.00 -25.88  110
 30  \w     39.00 149.00   1.00    1.10    --   72.00  79.00  36.08  110
 31  \w     46.00 149.00   1.00    1.10    --   76.00  66.00 114.97  103
 32  \w     63.00 165.00   1.00    1.10    --   92.50  61.00 120.00  102
 33  \w     63.00 165.00   1.00    1.10    --   92.50  61.00 -90.00  102
 34  \w     63.00 165.00   1.00    1.10    --   92.50  61.00 -60.00  102
 35  \w     63.00 165.00   1.00    1.10    --   92.50  61.00  60.00  102
 36  \w     60.00 169.00   1.00    1.10    --   92.50  77.00-180.00  109
 37  \w     60.00 150.00   1.00    1.10    --   92.50  77.00  60.00   90
 38  \w     63.00 165.00   1.00    1.10    --   92.50  61.00 150.00  102
 39  \w     63.00 165.00   1.00    1.10    --   92.50  61.00 -30.00  102
 40  \w     60.00 169.00   1.00    1.10    --   92.50  77.00   0.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1409832000
_diffrn_orient_matrix_UB_12      -0.0367978000
_diffrn_orient_matrix_UB_13      0.0050659000
_diffrn_orient_matrix_UB_21      -0.0103656000
_diffrn_orient_matrix_UB_22      -0.1108649000
_diffrn_orient_matrix_UB_23      -0.0926538000
_diffrn_orient_matrix_UB_31      0.0224741000
_diffrn_orient_matrix_UB_32      -0.2834360000
_diffrn_orient_matrix_UB_33      0.0355773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24014
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.887
_diffrn_reflns_theta_max         66.887
_diffrn_reflns_theta_min         4.109
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.110
_refine_diff_density_min         -0.131
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 1037 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.12(9)
_refine_ls_extinction_coef       0.0053(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2949
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.1216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                2650
_reflns_number_total             2949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0219_suppl.cif
_cod_data_source_block           exp_567
_cod_database_code               8105561