Structure elucidation of cyasterone stereoisomers isolated from Cyathula officinalis.
Okuzumi, Keiko; Hara, Noriyuki; Uekusa, Hidehiro; Fujimoto, Yoshinori; Organic & biomolecular chemistry 3 (2005) 1227–1232; doi:10.1039/b416868b

data_7150054
_publ_section_title
;
 Structure elucidation of cyasterone stereoisomers isolated from
 Cyathula officinalis.
;
_journal_issue                   7
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1227
_journal_page_last               1232
_journal_paper_doi               10.1039/b416868b
_journal_volume                  3
_journal_year                    2005
_chemical_formula_sum            'C32 H56 O11'
_chemical_formula_weight         616.77
_chemical_name_common            'cyasterone 1'
_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                 100.215(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6542(11)
_cell_length_b                   7.7755(4)
_cell_length_c                   15.7636(12)
_cell_measurement_reflns_used    10590
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.195
_cell_measurement_theta_min      3.29
_cell_volume                     1647.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'RIGAKU UX-18 Rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18438
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.9279
_exptl_absorpt_correction_T_min  0.7509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCORE, Rigaku'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_coef       0.0201(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5428
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0854P)^2^+1.7591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1693
_reflns_number_gt                5250
_reflns_number_total             5428
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b416868b.txt
_cod_data_source_block           cyasterone1
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7150054