Androstane-3β,5α,6β,17β-tetrol trihydrate
Andrade, L. C. R.; de Almeida, M. J. B. M.; Paixão, J. A.; Carvalho, J. F. S.; Sá e Melo, M. L.; Acta Crystallographica Section E 67 (2011) o1643–o1644; doi:10.1107/S1600536811021349

data_2230583
_publ_section_title
;
 Androstane-3\b,5\a,6\b,17\b-tetrol trihydrate
;
_journal_coeditor_code           BT5554
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1643
_journal_page_last               o1644
_journal_paper_doi               10.1107/S1600536811021349
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C19 H32 O4, 3H2 O'
_chemical_formula_moiety         'C19 H32 O4, 3(H2 O)'
_chemical_formula_sum            'C19 H38 O7'
_chemical_formula_weight         378.49
_chemical_melting_point          547
_chemical_name_systematic
;
Androstane-3\b,5\a,6\b,17\b-tetrol trihydrate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.5600(10)
_cell_angle_beta                 83.0910(10)
_cell_angle_gamma                68.9300(10)
_cell_formula_units_Z            1
_cell_length_a                   5.8420(2)
_cell_length_b                   7.3366(2)
_cell_length_c                   12.7922(3)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.937
_cell_measurement_theta_min      3.066
_cell_volume                     492.97(2)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14489
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         2222
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0531P)^2^+0.0525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                2132
_reflns_number_total             2222
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5554.cif
_cod_data_source_block           I
_cod_database_code               2230583
_cod_database_fobs_code          2230583