Non-natural 14-hydroxy steroids. III. (±)-Methyl 17β-benzoyloxy-14β-hydroxy-3β-isopropenyl-1,7-dioxo-5β-androstan-19-oate
Michel, A. G.; Drouin, M.; Acta Crystallographica Section C 49 (1993) 1683–1685; doi:10.1107/S0108270193002744

data_2001411
_publ_section_title
;
 Non-natural 14-hydroxy steroids. III. (+-)-Methyl
 17\b-benzoyloxy-14\b-hydroxy-3\b-isopropenyl-1,7-dioxo-5\b-androstan-19-oate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1683
_journal_page_last               1685
_journal_paper_doi               10.1107/S0108270193002744
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety         'C30 H36 O7'
_chemical_formula_sum            'C30 H36 O7'
_chemical_formula_weight         508.61
_chemical_melting_point          429.5(5)
_chemical_name_systematic
;
Methyl 17\b-benzoyloxy-14\b-hydroxy-3\b-methylethynyl-1,7-dioxo-
5\b-androstan-19-oate
;
_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'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4939(3)
_cell_length_b                   11.8032(3)
_cell_length_c                   35.0205(15)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    293
_cell_measurement_theta_max      36.00
_cell_measurement_theta_min      30.00
_cell_volume                     2684.28(18)
_computing_cell_refinement       nrccad_TRUANG
_computing_data_collection       'NRCCAD DATCOL (Le Page, White & Gabe, 1986)'
_computing_data_reduction
'nrcvax DATRD2 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics    'ORTEP, PLUTO'
_computing_publication_material  'PLATON92 (Spek, 1990)'
_computing_structure_refinement  'nrcvax LSTSQ'
_computing_structure_solution    'nrcvax SOLVER'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       Nonius
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .70930
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3441
_diffrn_reflns_theta_max         44.8
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .83
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       'irregular prism-like'
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.32
_refine_diff_density_max         .410
_refine_diff_density_min         -.220
_refine_ls_extinction_coef       .60(10)
_refine_ls_extinction_method     'Zachariasen (1963) & Larson (1967)'
_refine_ls_goodness_of_fit_obs   2.59
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         1456
_refine_ls_R_factor_all          .103
_refine_ls_R_factor_obs          .072
_refine_ls_shift/esd_max         .077
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'Weighting scheme: counting statistics'
_refine_ls_wR_factor_all         .066
_refine_ls_wR_factor_obs         .064
_reflns_number_observed          1456
_reflns_number_total             2054
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            cd1040.cif
_cod_data_source_block           cd1040_structure_1_of_1
_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.

'_refine_ls_matrix_type' value 'Full' changed to 'full'
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:

'_chemical_melting_point' value '429-430 K' was changed to '429.5(5)'
- 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 '429-430 K' was changed to '429.5(5)'
- the average value was taken and precision was
estimated.

'_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.

'_refine_ls_matrix_type' value 'Full' changed to 'full'
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 

  Adding the _atom_site_type_symbol data item to prevent confusion
  between hydrogen and holmium.

  Andrius Merkys
  2013-10-21
;
_cod_database_code               2001411