Crystal structure of (±)-(5<i>SR</i>,6<i>SR</i>)-6-ethenyl-1-[(<i>RS</i>)-1-phenylethoxy]-1-azaspiro[4.5]decan-2-one
Oishi, Takeshi; Yamamoto, Shio; Yokoyama, Takashi; Kobayashi, Akihiro; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 71 (2015) 1528–1530; doi:10.1107/S2056989015021209

data_2241356
_publ_section_title
;
 Crystal structure of
 (+-)-(5<i>SR</i>,6<i>SR</i>)-6-ethenyl-1-[(<i>RS</i>)-1-phenylethoxy]-1-azaspiro[4.5]decan-2-one
;
_journal_coeditor_code           IS5431
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1528
_journal_page_last               1530
_journal_paper_doi               10.1107/S2056989015021209
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C19 H25 N O2'
_chemical_formula_moiety         'C19 H25 N O2'
_chemical_formula_sum            'C19 H25 N O2'
_chemical_formula_weight         299.41
_chemical_melting_point          357.8
_chemical_name_systematic
(+-)-(5<i>SR</i>,6<i>SR</i>)-6-Ethenyl-1-[(<i>RS</i>)-1-phenylethoxy]-1-azaspiro[4.5]decan-2-one
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                93.306(2)
_cell_angle_beta                 108.710(2)
_cell_angle_gamma                114.929(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9032(5)
_cell_length_b                   9.6307(5)
_cell_length_c                   11.3401(6)
_cell_measurement_reflns_used    5086
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      25.0619
_cell_measurement_theta_min      2.6639
_cell_volume                     813.83(8)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2014)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010) and <i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS2013</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      90.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayered confocal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14217
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.2546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                2304
_reflns_number_total             2861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5431sup1.cif
_cod_data_source_block           I
_cod_database_code               2241356
_cod_database_fobs_code          2241356
_shelx_res_checksum              8032