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_2012547
_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 O9, H2 O'
_chemical_formula_moiety         'C20 H24 O9, H2 O'
_chemical_formula_sum            'C20 H26 O10'
_chemical_formula_weight         426.41
_chemical_melting_point          583
_chemical_name_common            'ginkgolide A monohydrate'
_chemical_name_systematic
;
(1R,3S,3aS,4R,6aR,7aR,7bR,8S,10aS,11aS) 3-
(1,1dimethylethyl)hexahydro-4,7b-dihydroxy-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 monohydrate
;
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.931(2)
_cell_length_b                   12.338(2)
_cell_length_c                   17.779(3)
_cell_measurement_reflns_used    19931
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.2
_cell_measurement_theta_min      2.5
_cell_volume                     1959.1(6)
_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  .017
_diffrn_reflns_av_sigmaI/netI    .026
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19931
_diffrn_reflns_theta_full        33.2
_diffrn_reflns_theta_max         33.2
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .117
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             904
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .37
_exptl_crystal_size_min          .35
_refine_diff_density_max         .29
_refine_diff_density_min         -.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          .036
_refine_ls_R_factor_gt           .032
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.3730P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .080
_refine_ls_wR_factor_ref         .083
_reflns_number_gt                3936
_reflns_number_total             4144
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bk1627.cif
_cod_data_source_block           I
_cod_original_cell_volume        1959.2(6)
_cod_database_code               2012547
_cod_database_fobs_code          2012547