Crystal structure of 2-isopropyl-5,7'-dimethyl-1',3',3a',6',8a',8b'-hexahydrospiro[cyclohexane-1,6'-furo[3,4-<i>d</i>]imidazo[1,5-<i>b</i>]isoxazol]-8'(7'<i>H</i>)-one
Abda, Heithem; Ezzayani, Khaireddine; Aouadi, Kaiss; Guerfel, Taha; Vidal, Sebastien; Msaddek, Moncef; Acta Crystallographica Section E 72 (2016) 1150–1152; doi:10.1107/S2056989016010641

data_2241772
_publ_section_title
;
 Crystal structure of
 2-isopropyl-5,7'-dimethyl-1',3',3a',6',8a',8b'-hexahydrospiro[cyclohexane-1,6'-furo[3,4-<i>d</i>]imidazo[1,5-<i>b</i>]isoxazol]-8'(7'<i>H</i>)-one
;
_journal_coeditor_code           ZS2363
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1150
_journal_page_last               1152
_journal_paper_doi               10.1107/S2056989016010641
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C17 H28 N2 O3'
_chemical_formula_moiety         'C17 H28 N2 O3'
_chemical_formula_sum            'C17 H28 N2 O3'
_chemical_formula_weight         308.42
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7474(6)
_cell_length_b                   11.1404(8)
_cell_length_c                   19.208(2)
_cell_measurement_reflns_used    5548
_cell_measurement_temperature    150
_cell_measurement_theta_max      66.6890
_cell_measurement_theta_min      4.5360
_cell_volume                     1657.8(2)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
CAMERON (Watkin <i>et al.</i>, 1996)
;
_computing_publication_material
;
CRYSTALS (Betteridge <i>et al.</i>, 2003)
;
_computing_structure_refinement
;
CRYSTALS (Betteridge <i>et al.</i>, 2003)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.4678
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur (Atlas, Gemini Ultra)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10374
_diffrn_reflns_theta_full        66.778
_diffrn_reflns_theta_max         66.778
_diffrn_reflns_theta_min         11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2013) based on expressions derived by Clark &
Reid
(1995); changes in illuminated volume were kept to a minimum, and were
taken
into account (G\"orbitz, 1999)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.428
_exptl_crystal_size_min          0.252
_refine_diff_density_max         0.16
_refine_diff_density_min         -0.17
_refine_ls_abs_structure_details
;
Flack (1983), 1261 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.6(3)
_refine_ls_extinction_coef       74(4)
_refine_ls_extinction_method
;
Larson (1970), Equation 22
;
_refine_ls_goodness_of_fit_ref   1.0287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2866
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994: Prince,
1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:  0.124E+04 0.195E+04 0.105E+04 304.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0957
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                2680
_reflns_number_total             2879
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            zs2363sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               2241772
_cod_database_fobs_code          2241772