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_2020814
_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_moiety         'C14 H21 N O4'
_chemical_formula_sum            'C14 H21 N O4'
_chemical_formula_weight         267.32
_chemical_name_systematic
(5<i>S</i>,8<i>R</i>)-8-<i>tert</i>-Butyl-7-methoxy-8-methyl-9-oxa-6-azaspiro[4.5]decane-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                 100.243(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7007(3)
_cell_length_b                   6.3466(2)
_cell_length_c                   13.3458(4)
_cell_measurement_reflns_used    2829
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5367
_cell_measurement_theta_min      3.0625
_cell_volume                     725.21(4)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.952
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.537
_diffrn_reflns_theta_min         3.062
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.80028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.15
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 774 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.5(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3396
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0485P)^2^+0.0692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                2235
_reflns_number_total             3396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3237sup1.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2020814
_cod_database_fobs_code          2020814
_shelx_estimated_absorpt_t_min   0.97
_shelx_estimated_absorpt_t_max   0.991
_shelx_hkl_checksum              5568
_shelx_res_checksum              19052
_shelxl_version_number           .2013