(+)-Methyl 3β-acetoxy-13-carboxy-19-hydroxy-11-oxo-<i>C</i>-norolean-18-en-30-oate γ-lactone
Gaware, Rawindra; Czollner, Laszlo; Jordis, Ulrich; Mereiter, Kurt; Acta Crystallographica Section E 66 (2010) o2597–o2598; doi:10.1107/S1600536810036901

data_2227232
_publ_section_title
;
 (+)-Methyl
 3\b-acetoxy-13-carboxy-19-hydroxy-11-oxo-<i>C</i>-norolean-18-en-30-oate
 \g-lactone
;
_journal_coeditor_code           BT5349
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2597
_journal_page_last               o2598
_journal_paper_doi               10.1107/S1600536810036901
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C33 H46 O7'
_chemical_formula_moiety         'C33 H46 O7'
_chemical_formula_sum            'C33 H46 O7'
_chemical_formula_weight         554.70
_chemical_melting_point          565
_chemical_name_systematic
;
(+)-Methyl
3\b-acetoxy-13-carboxy-19-hydroxy-11-oxo-<i>C</i>-norolean-18-en-30-oate
\g-lactone
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6310(4)
_cell_length_b                   16.7922(9)
_cell_length_c                   22.3822(13)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.59
_cell_volume                     2868.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT, SADABS and XPREP (Bruker, 2008)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
PLATON (Spek, 2009) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41398
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+0.3708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                4540
_reflns_number_total             4654
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5349.cif
_cod_data_source_block           I
_cod_database_code               2227232
_cod_database_fobs_code          2227232