(–)-(3a'<i>S</i>,4'<i>S</i>,9b'<i>S</i>,1<i>R</i>,2<i>S</i>,5<i>R</i>)-4'-Ethyl-3a',4',5',7',8',9b'-hexahydro-2-isopropyl-5-methyl-2'-phenylspiro[cyclohexane-1,7'-dioxino[3,2-<i>e</i>]isoindole]-1',3',9'-trione
Schollmeyer, Dieter; Hoffmann, Ralf; Mattay, Jochen; Acta Crystallographica Section E 61 (2005) o290–o291; doi:10.1107/S1600536805000140

data_2204996
_publ_section_title
(--)-(3a'<i>S</i>,4'<i>S</i>,9b'<i>S</i>,1<i>R</i>,2<i>S</i>,5<i>R</i>)-4'-Ethyl-3a',4',5',7',8',9b'-hexahydro-2-isopropyl-5-methyl-2'-phenylspiro[cyclohexane-1,7'-dioxino[3,2-<i>e</i>]isoindole]-1',3',9'-trione
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o290
_journal_page_last               o291
_journal_paper_doi               10.1107/S1600536805000140
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C27 H33 N O5'
_chemical_formula_moiety         'C27 H33 N O5'
_chemical_formula_sum            'C27 H33 N O5'
_chemical_formula_weight         451.54
_chemical_melting_point          164
_chemical_name_systematic
;
(-)-(3a'S,4'S,9b'S,1R,2S,5R)-4'-Ethyl-3a',4',5',7',8',9b'-hexahydro-2-
isopropyl-5-methyl-2'-phenylspiro[cyclohexane-1,7'-dioxino[3,2-e]isoindole]-
1',3',9'-trione
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.007(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3100(10)
_cell_length_b                   13.1112(5)
_cell_length_c                   26.642(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      36
_cell_volume                     4998.6(5)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'CORINC (Dr\"ager & Gattow, 1971)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \q/2\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22636
_diffrn_reflns_theta_full        75.06
_diffrn_reflns_theta_max         75.06
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   '(CORINC; Dr\"ager, 1971)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      1.237
_exptl_crystal_density_method    floatation
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.194
_refine_ls_abs_structure_details 'Flack (1983), 9618 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         20376
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.2501P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1370
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                16110
_reflns_number_total             20376
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6574.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2204996
_cod_database_fobs_code          2204996