(17<i>S</i>)-2α,3α,18β,23,24-Pentahydroxy-19(18→ 17)-<i>abeo</i>-28-norolean-12-en-21-one from the rhizome of <i>Phlomis umbrosa</i>
Pu Liu; Wei Qiao; Wei Jia; Jie Teng; Hong-Quan Duan; Acta Crystallographica Section E 62 (2006) o919–o921; doi:10.1107/S1600536806003151

data_2208229
_publ_section_title
;
 (17<i>S</i>)-2\a,3\a,18\b,23,24-Pentahydroxy-19(18\\rightarrow
 17)-<i>abeo</i>-28-norolean-12-en-21-one from the rhizome of
 <i>Phlomis umbrosa</i>
;
_journal_coeditor_code           AC6229
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o919
_journal_page_last               o921
_journal_paper_doi               10.1107/S1600536806003151
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C29 H46 O6'
_chemical_formula_moiety         'C29 H46 O6'
_chemical_formula_sum            'C29 H46 O6'
_chemical_formula_weight         490.66
_chemical_melting_point          563
_chemical_name_systematic
;
(17S)-2\a,3\a,18\b,23,24-pentahydroxy-19(18\\rightarrow17)-abeo-28-
norolean-12-en-21-one
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0637(10)
_cell_length_b                   11.6334(17)
_cell_length_c                   31.080(4)
_cell_measurement_reflns_used    2980
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.18
_cell_measurement_theta_min      2.63
_cell_volume                     2554.0(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            14539
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.244
_refine_ls_abs_structure_details 'None, Friedel Pairs merged'
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                2090
_reflns_number_total             3012
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ac6229.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'P 2ab 2ab'
_cod_database_code               2208229
_cod_database_fobs_code          2208229