Crystal structure of hydrocortisone 17-butyrate
Zhu, Yu; Shen, Wei; Wang, Hai-li; Acta Crystallographica Section E 70 (2014) o1239–o1240; doi:10.1107/S1600536814023903

data_2240165
_publ_section_title
;
 Crystal structure of hydrocortisone 17-butyrate
;
_journal_coeditor_code           RZ5136
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1239
_journal_page_last               o1240
_journal_paper_doi               10.1107/S1600536814023903
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C25 H36 O6'
_chemical_formula_moiety         'C25 H36 O6'
_chemical_formula_sum            'C25 H36 O6'
_chemical_formula_weight         432.54
_chemical_name_common
;
Hydrocortisone 17-butyrate
;
_chemical_name_systematic
'(8<i>S</i>,9<i>S</i>,10<i>R</i>,11<i>S</i>,13<i>S</i>,14<i>S</i>,17<i>R</i>)-11-Hydroxy-17-(2-hydroxyacetyl)-10,13-dimethyl-3-oxo-2,6,7,8,9,11,12,14,15,16-decahydro-1<i>H</i>-cyclopenta[<i>a</i>]phenanthren-17-yl butanoate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.05738(8)
_cell_length_b                   11.87633(9)
_cell_length_c                   21.13465(15)
_cell_measurement_reflns_used    14007
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      72.3870
_cell_measurement_theta_min      4.1770
_cell_volume                     2273.42(3)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2011)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Agilent Xcalibur Eos Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23353
_diffrn_reflns_theta_full        72.25
_diffrn_reflns_theta_max         72.25
_diffrn_reflns_theta_min         4.18
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO (Agilent, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.280
_refine_ls_abs_structure_details
;
Flack (1983), 1932 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.02(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4496
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.3126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                4389
_reflns_number_total             4496
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz5136sup1.cif
_cod_data_source_block           I
_cod_database_code               2240165
_cod_database_fobs_code          2240165