11β,13-Dihydrolactucin-8-<i>O</i>-acetate hemihydrate
Fronczek, Chris F.; Gomez-Barrios, Marco L.; Fischer, Nikolaus H.; Fronczek, Frank R.; Acta Crystallographica Section E 65 (2009) o2564–o2565; doi:10.1107/S160053680903829X

data_2223532
_publ_section_title
;
 11\b,13-Dihydrolactucin-8-<i>O</i>-acetate hemihydrate
;
_journal_coeditor_code           PV2210
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2564
_journal_page_last               o2565
_journal_paper_doi               10.1107/S160053680903829X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C17 H20 O6, 0.5H2 O'
_chemical_formula_moiety         'C17 H20 O6, 0.5(H2 O)'
_chemical_formula_sum            'C17 H21 O6.5'
_chemical_formula_weight         329.34
_chemical_name_common
;
11\b,13-Dihydrolactucin-8-<i>O</i>-acetate hemihydrate
;
_chemical_name_systematic
;
9-hydroxymethyl-3,6-dimethyl-2,7-dioxo-
3,3a,4,5,9a,9b-hexahydroazuleno[4,5-<i>b</i>]furan-4-yl
acetate hemihydrate
;
_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           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 100.850(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9276(5)
_cell_length_b                   7.4658(5)
_cell_length_c                   19.8571(10)
_cell_measurement_reflns_used    9656
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      68.33
_cell_measurement_theta_min      2.27
_cell_volume                     1591.05(15)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23565
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         69.04
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.9168
_exptl_absorpt_correction_T_min  0.7962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.138
_refine_ls_abs_structure_details 'Flack (1983), 2516 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(10)
_refine_ls_extinction_coef       0.00101(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5642
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0314P)^2^+0.4082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                5513
_reflns_number_total             5642
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2210.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C17 H21 O6.50'
_cod_database_code               2223532
_cod_database_fobs_code          2223532