<i>tert</i>-Butyl (2<i>S</i>)-2-{3-[(<i>R</i>)-bis(<i>tert</i>-butoxycarbonyl)amino]-2-oxopiperidin-1-yl}-3-methylbutanoate
Kangas, Michael J.; Fronczek, Frank R.; Watkins, Steven F.; Acta Crystallographica Section E 67 (2011) o3057–; doi:10.1107/S1600536811043212

data_2232431
_publ_section_title
;
 <i>tert</i>-Butyl
 (2<i>S</i>)-2-{3-[(<i>R</i>)-bis(<i>tert</i>-butoxycarbonyl)amino]-2-oxopiperidin-1-yl}-3-methylbutanoate
;
_journal_coeditor_code           PV2462
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3057
_journal_paper_doi               10.1107/S1600536811043212
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C24 H42 N2 O7'
_chemical_formula_moiety         'C24 H42 N2 O7'
_chemical_formula_sum            'C24 H42 N2 O7'
_chemical_formula_weight         470.6
_chemical_name_systematic
;
<i>tert</i>-Butyl (2<i>S</i>)-2-{3-[(<i>R</i>)-bis(<i>tert</i>-
butoxycarbonyl)amino]-2-oxopiperidin-1-yl}-3-methylbutanoate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 110.7290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.282(3)
_cell_length_b                   9.4315(10)
_cell_length_c                   11.5884(10)
_cell_measurement_pressure       101.3
_cell_measurement_reflns_used    8306
_cell_measurement_temperature    86.0(5)
_cell_measurement_theta_max      67.83
_cell_measurement_theta_min      3.46
_cell_volume                     2788.8(5)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      86.0(5)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10823
_diffrn_reflns_theta_full        67.0
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.8779
_exptl_absorpt_correction_T_min  0.7998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.121
_refine_ls_abs_structure_details 'Flack (1983), 2174 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(10)
_refine_ls_extinction_coef       0.00066(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXS97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.6036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                4782
_reflns_number_total             4844
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2462.cif
_cod_data_source_block           I
_cod_original_cell_volume        2788.7(5)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2232431
_cod_database_fobs_code          2232431