Stemofoline ethyl acetate solvate
Mungkornasawakul, Pitchaya; Pyne, Stephen G.; Ung, Alison T.; Jatisatienr, Araya; Willis, Anthony C.; Acta Crystallographica Section E 65 (2009) o1878–o1879; doi:10.1107/S1600536809026889

data_2222881
_publ_section_title
;
 Stemofoline ethyl acetate solvate
;
_journal_coeditor_code           SJ2635
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1878
_journal_page_last               o1879
_journal_paper_doi               10.1107/S1600536809026889
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C22 H29 N O5, C4 H8 O2'
_chemical_formula_moiety         'C22 H29 N O5, C4 H8 O2'
_chemical_formula_sum            'C26 H37 N O7'
_chemical_formula_weight         475.58
_chemical_name_common
;
Stemofoline ethyl acetate solvate
;
_chemical_name_systematic
;(2<i>R</i>,3<i>R</i>,5<i>R</i>,5a<i>S</i>,
6<i>R</i>,8a<i>R</i>,9<i>S</i>)-(5<i>Z</i>)-5-[3-butyltetrahydro-6-methyl-
2,5-methano-4,3,8a-[1]propanyl[3]ylidenefuro[3,2-f][1,4]oxazepin-7(5<i>H</i>)-
ylidene]-4-methoxy-3-methylfuran-2(5<i>H</i>)-one
 ethyl acetate solvate
;
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.39080(10)
_cell_length_b                   10.6549(2)
_cell_length_c                   22.4143(4)
_cell_measurement_reflns_used    36203
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2481.55(7)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) in TEXSAN (Molecular Structure Corporation,
1997)
;
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41745
_diffrn_reflns_theta_full        27.470
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         2.638
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (Mackay <i>et
al.</i>,  2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details
;
The absolute configuration was not determined in this experiment.
;
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002240
_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:
 38.7 60.5 31.2 8.38
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1190
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                2149
_reflns_number_total             3209
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2635.cif
_cod_data_source_block           I
_cod_database_code               2222881
_cod_database_fobs_code          2222881