Tenulin 0.25-hydrate, a sesquiterpene lactone isolated from <i>Helenium amarum</i>
Knight, Kyle S.; Smith, Cole T.; Waddell, Thomas G.; Noll, Bruce; Acta Crystallographica Section E 69 (2013) o1237–o1238; doi:10.1107/S1600536813018369

data_2238329
_publ_section_title
;
 Tenulin 0.25-hydrate, a sesquiterpene lactone isolated from <i>Helenium
 amarum</i>
;
_journal_coeditor_code           CV5419
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1237
_journal_page_last               o1238
_journal_paper_doi               10.1107/S1600536813018369
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C17 H22 O5, 0.25H2 O'
_chemical_formula_moiety         'C17 H22 O5, 0.25(H2 O)'
_chemical_formula_sum            'C17 H22.5 O5.25'
_chemical_formula_weight         310.86
_chemical_name_common
;
Tenulin 0.25-hydrate
;
_chemical_name_systematic
;
2-Hydroxy-2,2a,6,9a-tetramethyl-2a,4a,5,6,6a,9a,9b,9c-octahydro-2<i>H</i>-
1,4-dioxadicyclopent[<i>cd</i>,<i>f</i>]azulene-3,9-dione 0.25-hydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.5508(16)
_cell_length_b                   28.371(4)
_cell_length_c                   10.5228(14)
_cell_measurement_reflns_used    6528
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.41
_cell_volume                     3149.9(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i> 2009)'
_computing_publication_material  'OLEX2 (Dolomanov <i>et al.</i> 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19558
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         2.406
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0607P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                4678
_reflns_number_total             5543
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv5419.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C17 H22.50 O5.25'
_cod_database_code               2238329
_cod_database_fobs_code          2238329
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           .2013