Bis[14β-hydroxy-3β-<i>O</i>-(<small>L</small>-thevetosyl)-5β-card-20(22)-enolide] methanol solvate monohydrate and 3β-<i>O</i>-(<small>L</small>-2'-<i>o</i>-acetylthevetosyl)-14β-hydroxy-5β-card-20(22)-enolide
Suchada Chantrapromma; Anwar Usman; Hoong-Kun Fun; Surat Laphookhieo; Chatchanok Karalai; Yanisa Rat-a-pa; Kan Chantrapromma; Acta Crystallographica Section C 59 (2003) o68–o70; doi:10.1107/S0108270102023065

data_2013225
_publ_section_title
;Bis[14\b-hydroxy-3\b-<i>O</i>-(<small>L</small>-thevetosyl)-5\b-card-20(22)-enolide]
 methanol solvate monohydrate and
 3\b-<i>O</i>-(<small>L</small>-2'-<i>o</i>-acetylthevetosyl)-14\b-hydroxy-5\b-card-20(22)-enolide
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o68
_journal_page_last               o70
_journal_paper_doi               10.1107/S0108270102023065
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '2C30 H46 O8, C H4 O, H2 O'
_chemical_formula_moiety         '2C30 H46 O8, C H4 O, H2 O'
_chemical_formula_sum            'C61 H98 O18'
_chemical_formula_weight         1119.39
_chemical_name_systematic
;
3\b-o-(L-thevetoyl)-14\b-hydroxy-5\b-card-20(22)-enolide methanol solvate
monohydrate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.4120(10)
_cell_angle_beta                 101.4710(10)
_cell_angle_gamma                109.5990(10)
_cell_formula_units_Z            1
_cell_length_a                   10.4353(5)
_cell_length_b                   10.4491(5)
_cell_length_c                   14.8760(7)
_cell_measurement_reflns_used    7201
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      1.41
_cell_volume                     1487.14(12)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type
;
Siemens SMART CCD area-detector
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_sigmaI/netI    0.1352
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9863
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.700
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         6292
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0841P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                4368
_reflns_number_total             6292
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ta1401.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1487.10(10)
_cod_database_code               2013225
_cod_database_fobs_code          2013225