Conformational study of the 3,6-dihydro-2<i>H</i>-1,4-oxazin-2-one fragment in 8-<i>tert</i>-butyl-7-methoxy-8-methyl-9-oxa-6-azaspiro[4.5]decane-2,10-dione stereoisomers
Żesławska, Ewa; Jakubowska, Anna; Nitek, Wojciech; Acta Crystallographica Section C 73 (2017) 556–562; doi:10.1107/S2053229617009068

data_2020813
_publ_section_title
;
 Conformational study of the 3,6-dihydro-2<i>H</i>-1,4-oxazin-2-one
 fragment in
 8-<i>tert</i>-butyl-7-methoxy-8-methyl-9-oxa-6-azaspiro[4.5]decane-2,10-dione
 stereoisomers
;
_journal_coeditor_code           FN3237
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              556
_journal_page_last               562
_journal_paper_doi               10.1107/S2053229617009068
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C14 H21 N O4'
_chemical_formula_moiety         'C14 H21 N O4'
_chemical_formula_sum            'C14 H21 N O4'
_chemical_formula_weight         267.32
_chemical_name_systematic
(5<i>R</i>,8<i>S</i>)-8-<i>tert</i>-Butyl-7-methoxy-8-methyl-9-oxa-6-azaspiro[4.5]decan-2,10-dione
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.220(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7136(2)
_cell_length_b                   6.3606(2)
_cell_length_c                   13.3613(3)
_cell_measurement_reflns_used    7013
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.341
_cell_measurement_theta_min      3.3611
_cell_volume                     728.78(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SIR97 (Altomare <i>et al.</i>,  1999), SHELXL97 (Sheldrick,
2008) and SHELXL2014
(Sheldrick, 2015)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
;
Rigaku Oxford Diffraction SuperNova Dual Source diffractometer with an
Atlas detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9732
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.342
_diffrn_reflns_theta_min         3.361
_exptl_absorpt_coefficient_mu    0.73
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO (Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.139
_refine_diff_density_min         -0.117
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1165 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   0.05(9)
_refine_ls_extinction_coef       0.036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2784
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.087
_reflns_number_gt                2687
_reflns_number_total             2784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3237sup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2020813
_cod_database_fobs_code          2020813
_shelx_estimated_absorpt_t_min   0.811
_shelx_estimated_absorpt_t_max   0.898
_shelx_hkl_checksum              25872
_shelx_res_checksum              52790
_shelxl_version_number           .2013