A <i>P</i>2~1~2~1~2~1~ polymorph of (+)-clusianone
Vaneesa Nagalingam, Sree; Wong Pik Ching, Janet; Khaled bin Break, Mohammed; Tahir, M. Ibrahim M.; Khoo, Teng-Jin; Acta Crystallographica Section E 69 (2013) o1799–o1800; doi:10.1107/S1600536813031036

data_2238933
_publ_section_title
;
 A <i>P</i>2~1~2~1~2~1~ polymorph of (+)-clusianone
;
_journal_coeditor_code           TK5270
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1799
_journal_page_last               o1800
_journal_paper_doi               10.1107/S1600536813031036
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C33 H42 O4'
_chemical_formula_moiety         'C33 H42 O4'
_chemical_formula_sum            'C33 H42 O4'
_chemical_formula_weight         502.69
_chemical_melting_point          365
_chemical_name_systematic
(1<i>S</i>,5<i>S</i>,7<i>R</i>)-3-Benzoyl-4-hydroxy-8,8-dimethyl-1,5,7-tris(3-methylbut-2-enyl)bicyclo[3.3.1]nona-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   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2035(2)
_cell_length_b                   13.4629(2)
_cell_length_c                   22.9607(5)
_cell_measurement_reflns_used    19011
_cell_measurement_temperature    100
_cell_measurement_theta_max      71
_cell_measurement_theta_min      3
_cell_volume                     2844.96(10)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics
'CAMERON (Watkin <i>et al.</i>, 1996) and Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement
'CRYSTALS (Betteridge <i>et al.</i>, 2003; Cooper <i>et al.</i>, 2010)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Cu Ka'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39826
_diffrn_reflns_theta_full        71.631
_diffrn_reflns_theta_max         71.631
_diffrn_reflns_theta_min         3.806
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.18
_refine_ls_abs_structure_details 'Flack (1983), 2383 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.04(15)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9567
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5498
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.0006844
_refine_ls_shift/su_mean         0.0000520
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.02P]
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0838
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                5269
_reflns_number_total             5498
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            tk5270.cif
_cod_data_source_block           I
_cod_database_code               2238933