(+)-Hexacyclinol
Pinkerton, David M.; Banwell, Martin G.; Willis, Anthony C.; Acta Crystallographica Section E 66 (2010) o342–o343; doi:10.1107/S1600536810000620

data_2225003
_publ_section_title
;
 (+)-Hexacyclinol
;
_journal_coeditor_code           HG2629
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o342
_journal_page_last               o343
_journal_paper_doi               10.1107/S1600536810000620
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C23 H28 O7'
_chemical_formula_moiety         'C23 H28 O7'
_chemical_formula_sum            'C23 H28 O7'
_chemical_formula_weight         416.47
_chemical_name_common
;
(+)-Hexacyclinol
;
_chemical_name_systematic
;(1a<i>S</i>,2a<i>S</i>,3<i>S</i>,5a<i>S</i>,6a<i>S</i>,7<i>R</i>,7a<i>S</i>,
7b<i>S</i>,8<i>R</i>,8a<i>S</i>,10<i>R</i>)-7-hydroxy-3-(1-methoxy-1-
methylethyl)-10-(2-methyl-1-propenyl)-1a,5a,6a,7,7a,7b,8,8a-octahydro-
2<i>H</i>-8,2a-(epoxymethano)phenanthro[2,3-<i>b</i>:6,7-<i>b'</i>]bisoxirene-
2,5(3<i>H</i>)-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
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   10.82700(10)
_cell_length_b                   20.0530(2)
_cell_length_c                   28.0247(3)
_cell_measurement_reflns_used    119334
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     6084.55(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) in <i>TEXSAN</i> (Molecular Structure
Corporation,
1997)
;
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans with CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80486
_diffrn_reflns_theta_full        27.473
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.585
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
[<i>via</i> Gaussian method (Coppens, 1970) implemented in <i>maXus</i>
(Mackay <i>et al.</i>, 2000)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details
;
The enantiomer has been assigned by reference to an unchanging
centre of chirality in the starting material.
;
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8313
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         7619
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000742
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick
 w=1/[\s^2^(F^2^) + (0.03P)^2^ + 0.00P],
 where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0790
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                5571
_reflns_number_total             7619
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2629.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2225003
_cod_database_fobs_code          2225003