(±)-2'-Phenylcyclohexanespiro-4'-(azepano[1,2-<i>b</i>]isoxazolidine)
Crimmins, Daryl; Choi, Ka Wai; Boyd, Peter D. W.; Brimble, Margaret A.; Acta Crystallographica Section E 64 (2008) o1535–; doi:10.1107/S1600536808021867

data_2218888
_publ_section_title
;
 (+-)-2'-Phenylcyclohexanespiro-4'-(azepano[1,2-<i>b</i>]isoxazolidine)
;
_journal_coeditor_code           BI2294
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1535
_journal_paper_doi               10.1107/S1600536808021867
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C19 H27 N O'
_chemical_formula_moiety         'C19 H27 N O'
_chemical_formula_sum            'C19 H27 N O'
_chemical_formula_weight         285.42
_chemical_melting_point          338.8(7)
_chemical_name_common
8-Aza-14-phenylisoxazolo[2,3-<i>g</i>]spiro[5.6]dodecane
_chemical_name_systematic
;
(+-)-2'-Phenylcyclohexanespiro-4'-(azepano[1,2-b]isoxazolidine)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.0580(10)
_cell_angle_beta                 92.8330(10)
_cell_angle_gamma                96.5270(10)
_cell_formula_units_Z            4
_cell_length_a                   9.85160(10)
_cell_length_b                   10.45600(10)
_cell_length_c                   16.09570(10)
_cell_measurement_reflns_used    6437
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      1.29
_cell_volume                     1612.34(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       \w
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15138
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.9845
_exptl_absorpt_correction_T_min  0.9775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0839
_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^)+(0.0475P)^2^+4.1372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1942
_reflns_number_gt                4959
_reflns_number_total             6437
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2294.cif
_cod_data_source_block           I
_cod_original_cell_volume        1612.34(2)
_cod_database_code               2218888
_cod_database_fobs_code          2218888