Stereoselective Synthesis of Quaternary Pyrrolidine-2,3-diones and β-Amino Acids.
Shymanska, Nataliia V.; Pierce, Joshua G.; Organic letters 19 (2017) 2961–2964; doi:10.1021/acs.orglett.7b01185

data_1546106
_publ_section_title
;
 Stereoselective Synthesis of Quaternary Pyrrolidine-2,3-diones and
 \b-Amino Acids.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2961
_journal_page_last               2964
_journal_paper_doi               10.1021/acs.orglett.7b01185
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C17 H24 N O2, 1.5(H2 O)'
_chemical_formula_sum            'C17 H27 N O3.5'
_chemical_formula_weight         301.39
_chemical_name_common            NB-078-023
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2016(13)
_cell_length_b                   21.2016(13)
_cell_length_c                   7.9468(5)
_cell_measurement_reflns_used    212
_cell_measurement_temperature    210.(2)
_cell_measurement_theta_max      19.9820
_cell_measurement_theta_min      1.9242
_cell_volume                     3572.1(4)
_computing_cell_refinement       'APEX2 v2014.9-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      210.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10069
_diffrn_reflns_theta_full        21.96
_diffrn_reflns_theta_max         21.96
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.370
_refine_ls_abs_structure_details
;
Flack x determined using 681 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
_refine_ls_abs_structure_Flack          -1.8(10)
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2189
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0701P)^2^+1.7731P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                1803
_reflns_number_total             2189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b01185_si_003.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1546106.cif.'
_cod_original_cell_volume        3572.1(5)
_cod_original_formula_sum        'C17 H27 N O3.50'
_cod_database_code               1546106
_shelx_res_checksum              52793
_shelx_hkl_checksum              26067