Redetermination and absolute configuration of berkeleydione
Stierle, Andrea; Stierle, Donald; Decato, Daniel; Acta Crystallographica Section E 71 (2015) o248–; doi:10.1107/S2056989015003965

data_2240512
_publ_section_title
;
 Redetermination and absolute configuration of berkeleydione
;
_journal_coeditor_code           SU5086
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o248
_journal_paper_doi               10.1107/S2056989015003965
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C26 H32 O7'
_chemical_formula_moiety         'C26 H32 O7'
_chemical_formula_sum            'C26 H32 O7'
_chemical_formula_weight         456.51
_chemical_name_common            Berkeleydione
_chemical_name_systematic
;(5a<i>S</i>,7<i>R</i>,9<i>S</i>,11<i>R</i>,11a<i>S</i>)-Methyl
9-hydroxy-1,1,5,7,9,11a-hexamethyl-14-methylidene-3,8,10-trioxo-1,3,4,5a,6,7,8,9,10,11,11a,12-dodecahydro-7,11-methanocycloocta[4,5]cyclohepta[1,2-<i>c</i>]pyran-11-carboxylate
;
_space_group_crystal_system      orthorhombic
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_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
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;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1832(6)
_cell_length_b                   14.5805(9)
_cell_length_c                   17.5148(11)
_cell_measurement_reflns_used    9233
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.69
_cell_measurement_theta_min      3.94
_cell_volume                     2345.2(3)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
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APEX2 (Bruker, 2009)
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_computing_data_reduction
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SAINT (Bruker, 2009)
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_computing_molecular_graphics
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OLEX2 (Dolomanov <i>et al.</i>,  2009)
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OLEX2 (Dolomanov <i>et al.</i>,  2009)
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SHELXL2014 (Sheldrick, 2015)
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SHELXS97 (Sheldrick, 2008)
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_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
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_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_theta_max         74.768
_diffrn_reflns_theta_min         3.945
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.190
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1914 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
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_refine_ls_number_reflns         4814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0569P)^2^+0.2309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0907
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_reflns_threshold_expression     I>2\s(I)
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