(25<i>R</i>)-5β-Hydroxyspirost-2-en-6-one
Angel Dago Morales; Ramón Pomés Hernández; Francisco Coll Manchado; María Teresa Hechavarría Fonseca; Graciela Punte; Gustavo Echeverría; Acta Crystallographica Section C 53 (1997) 1705–1706; doi:10.1107/S0108270197006501

data_2006660
_publ_section_title
;
 (25<i>R</i>)-5\b-Hydroxyspirost-2-en-6-one
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1705
_journal_page_last               1706
_journal_paper_doi               10.1107/S0108270197006501
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C27 H40 O4'
_chemical_formula_structural     'C27 H40 O4'
_chemical_formula_sum            'C27 H40 O4'
_chemical_formula_weight         428.59
_chemical_melting_point          166.80(10)
_chemical_name_systematic
;
 (25R)-5\b-hydroxy-spirost-2-en-6-one
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.61(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.667(2)
_cell_length_b                   7.182(4)
_cell_length_c                   14.337(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     1190.8(7)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1993)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    SHELXTL/Plus
_computing_publication_material  SHELXL93
_computing_structure_refinement  SHELXL93
_computing_structure_solution    SHELXTL/Plus
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w-2\q scan technique'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.1224
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4172
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        3.1
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type
'empirical, via \y scan (SHELXTL/Plus; Sheldrick, 1990)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.252
_refine_ls_abs_structure_details
;this X-ray analysis does not determine the absolute stereochemistry, which
 was
known from chemical studies. 16 Friedel pairs were used in the
 refinement
(Flack, 1983)
;
_refine_ls_abs_structure_Flack   -2(5)
_refine_ls_extinction_coef       0.008(4)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.986
_refine_ls_goodness_of_fit_obs   0.901
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.990
_refine_ls_restrained_S_obs      0.900
_refine_ls_R_factor_all          0.2286
_refine_ls_R_factor_obs          .0703
_refine_ls_shift/esd_max         0.031
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1344P)^2^+2.2491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3332
_refine_ls_wR_factor_obs         .1754
_reflns_number_observed          1432
_reflns_number_total             4026
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1242.cif
_cod_data_source_block           C27H40O4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '166.7-166.9' was changed to
'166.80(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '166.7-166.9' was changed to
'166.80(10)' - the average value was taken and precision was
estimated.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.1344P)^2^+2.2491P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.1344P)^2^+2.2491P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2006660