An <i>ent</i>-kaurane diterpenoid from <i>Isodon japonica</i> var. glaucocalyx
Bai, Su-Ping; Luo, Guo-Sheng; Zhang, Xiao-Yi; Liu, Wei; Acta Crystallographica Section E 65 (2009) o1898–; doi:10.1107/S1600536809027159

data_2222668
_publ_section_title
;
 An <i>ent</i>-kaurane diterpenoid from <i>Isodon japonica</i> var.
 glaucocalyx
;
_journal_coeditor_code           EZ2171
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1898
_journal_paper_doi               10.1107/S1600536809027159
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C22 H30 O5'
_chemical_formula_moiety         'C22 H30 O5'
_chemical_formula_sum            'C22 H30 O5'
_chemical_formula_weight         374.46
_chemical_melting_point          463
_chemical_name_common            'glaucocalyxin B'
_chemical_name_systematic
;
14\b-acetoxy-7\a-hydroxy-<i>ent</i>-kaur-16-ene-3,15-dione
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.039(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.485(4)
_cell_length_b                   23.786(10)
_cell_length_c                   9.930(4)
_cell_measurement_reflns_used    12776
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.13
_cell_volume                     2003.8(15)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2004)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19620
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.13
_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_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.199
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         4669
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0896P)^2^+0.022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                2856
_reflns_number_total             4669
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ez2171.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2222668
_cod_database_fobs_code          2222668