Three ginkgolide hydrates from <i>Ginkgo biloba</i> L.: ginkgolide A monohydrate, ginkgolide C sesquihydrate and ginkgolide J dihydrate, all determined at 120K
Jianping, Zhao; Muhammad, Ilias; Dunbar, D. Chuck; Khan, Ikhlas A.; Fischer, Nikolaus H.; Fronczek, Frank R.; Acta Crystallographica Section C 58 (2002) o195–o198; doi:10.1107/S0108270102000689

data_2012548
_publ_section_title
;
 Three ginkgolide hydrates from <i>Ginkgo biloba</i> L.: ginkgolide A
 monohydrate, ginkgolide C sesquihydrate and ginkgolide J dihydrate,
 all determined at 120K
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o195
_journal_page_last               o198
_journal_paper_doi               10.1107/S0108270102000689
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C20 H24 O11, 1.5H2 O'
_chemical_formula_moiety         'C20 H24 O11, 1.5H2 O'
_chemical_formula_sum            'C20 H27 O12.5'
_chemical_formula_weight         467.42
_chemical_melting_point          558
_chemical_name_common            'ginkgolide C sesquihydrate'
_chemical_name_systematic
;
(1S,2R,3S,3aS,4R,6aR,7aR,7bR,8S,10aS,11S,11aR) 3-(1,1-dimethylethyl)
hexahydro-2,4,7b,11-tetrahydroxy-8-methyl-9H-1,7a-(epoxymethano)-1H,6aH-
cyclopenta[c]furo[2,3b]furo[3',2':3,4]cyclopenta[1,2-d]furan-5,9,12
(4H)-trione sesquihydrate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 91.00(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4945(15)
_cell_length_b                   12.973(3)
_cell_length_c                   20.934(4)
_cell_measurement_reflns_used    5587
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      2.5
_cell_volume                     2035.0(7)
_computing_cell_refinement       'DENZO and SCALEPACK'
_computing_data_collection       'COLLECT (Nonius 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full .992
_diffrn_measured_fraction_theta_max .992
_diffrn_measurement_device
'KappaCCD (with Oxford Cryosystems Cryostream cooler)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .019
_diffrn_reflns_av_sigmaI/netI    .026
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22429
_diffrn_reflns_theta_full        29.6
_diffrn_reflns_theta_max         29.6
_diffrn_reflns_theta_min         2.7
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .128
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             988
_exptl_crystal_size_max          .47
_exptl_crystal_size_mid          .27
_exptl_crystal_size_min          .25
_refine_diff_density_max         .37
_refine_diff_density_min         -.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          .033
_refine_ls_R_factor_gt           .031
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.4304P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .084
_refine_ls_wR_factor_ref         .086
_reflns_number_gt                5752
_reflns_number_total             5921
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bk1627.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C20 H27 O12.50'
_cod_database_code               2012548
_cod_database_fobs_code          2012548