Crystal structure of (1<i>R</i>,4<i>R</i>)-<i>tert</i>-butyl 3-oxo-2-oxa-5-azabicyclo[2.2.2]octane-5-carboxylate
Krishnamurthy, Suvratha; Jalli, Venkataprasad; Vagvala, Tarun Chand; Moriguchi, Tetsuji; Tsuge, Akihiko; Acta Crystallographica Section E 71 (2015) o449–o450; doi:10.1107/S2056989015010476

data_2240810
_publ_section_title
;
 Crystal structure of (1<i>R</i>,4<i>R</i>)-<i>tert</i>-butyl
 3-oxo-2-oxa-5-azabicyclo[2.2.2]octane-5-carboxylate
;
_journal_coeditor_code           ZS2333
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o449
_journal_page_last               o450
_journal_paper_doi               10.1107/S2056989015010476
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C11 H17 N O4'
_chemical_formula_moiety         'C11 H17 N O4'
_chemical_formula_sum            'C11 H17 N O4'
_chemical_formula_weight         227.26
_chemical_name_common
;
(1<i>R</i>,4<i>R</i>)-<i>tert</i>-butyl
3-oxo-2-oxa-5-azabicyclo[2.2.2]octane-5-carboxylate
;
_chemical_name_systematic
;
(1<i>R</i>,4<i>R</i>)-<i>tert</i>-butyl
3-oxo-2-oxa-5-azabicyclo[2.2.2]octane-5-carboxylate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2010.1-2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6472(4)
_cell_length_b                   9.7084(4)
_cell_length_c                   12.2323(5)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.6762
_cell_measurement_theta_min      2.6783
_cell_volume                     1145.66(8)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker,2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 16.6666
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX2 KY CCD'
_diffrn_measurement_method       ' \f and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13518
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker, 2009)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.267
_refine_ls_abs_structure_details
;
Flack (1983), 2933 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.1(7)
_refine_ls_extinction_coef       0.0015
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.1302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                2728
_reflns_number_total             2791
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2333sup1.cif
_cod_data_source_block           I
_cod_database_code               2240810
_cod_database_fobs_code          2240810