Redetermination and absolute configuration of (+)-7-epiclusianone
Christian, Omar E.; Fronczek, Frank R.; Ky, Khoa; Pradhan, Shreedu; Manandhar, Anjela; Richmond, Cecilia; Acta Crystallographica Section E 68 (2012) o3222–o3223; doi:10.1107/S1600536812043784

data_2236304
_publ_section_title
;
 Redetermination and absolute configuration of (+)-7-epiclusianone
;
_journal_coeditor_code           HB6978
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3222
_journal_page_last               o3223
_journal_paper_doi               10.1107/S1600536812043784
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C33 H42 O4'
_chemical_formula_moiety         'C33 H42 O4'
_chemical_formula_sum            'C33 H42 O4'
_chemical_formula_weight         502.67
_chemical_name_common            7-epiclusianone
_chemical_name_systematic
;
3-benzoyl-4-hydroxy-6,6-dimethyl-1,5,7-tris(3-methylbut-2-
enyl)bicyclo[3.3.1]non-3-ene-2,9-dione
;
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6177(4)
_cell_length_b                   12.4157(6)
_cell_length_c                   26.8632(13)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      68.69
_cell_measurement_theta_min      6.10
_cell_volume                     2874.2(2)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (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 0.987
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer optics'
_diffrn_radiation_source         'I\mS microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17192
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         69.02
_diffrn_reflns_theta_min         6.10
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.8893
_exptl_absorpt_correction_T_min  0.8241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.135
_refine_ls_abs_structure_details 'Flack (1983), 2200 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0421P)^2^+0.5041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                5131
_reflns_number_total             5171
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6978.cif
_cod_data_source_block           I
_cod_database_code               2236304
_cod_database_fobs_code          2236304