(25<i>R</i>)-6α-Hydroxy-5α-spirostan-3β-yl tosylate
Fernández-Herrera, María A.; Sandoval-Ramírez, Jesús; Bernès, Sylvain; Rodríguez-Acosta, Maricela; Hernández Linares, María-Guadalupe; Acta Crystallographica Section E 68 (2012) o3413–o3414; doi:10.1107/S1600536812046600

data_2236815
_publ_section_title
;
 (25<i>R</i>)-6\a-Hydroxy-5\a-spirostan-3\b-yl tosylate
;
_journal_coeditor_code           BQ2379
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3413
_journal_page_last               o3414
_journal_paper_doi               10.1107/S1600536812046600
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C34 H50 O6 S'
_chemical_formula_moiety         'C34 H50 O6 S'
_chemical_formula_sum            'C34 H50 O6 S'
_chemical_formula_weight         586.80
_chemical_melting_point          422
_chemical_name_systematic
;
(25<i>R</i>)-6\a-Hydroxy-5\a-spirostan-3\b-yl tosylate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7653(8)
_cell_length_b                   12.2856(11)
_cell_length_c                   37.943(4)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      4.60
_cell_volume                     3153.7(6)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            9218
_diffrn_reflns_theta_full        26.25
_diffrn_reflns_theta_max         26.25
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.157
_refine_ls_abs_structure_details 'Flack (1983), 2504  Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(7)
_refine_ls_extinction_coef       0.0058(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.5535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                5274
_reflns_number_total             6167
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bq2379.cif
_cod_data_source_block           I
_cod_original_cell_volume        3153.6(6)
_cod_database_code               2236815
_cod_database_fobs_code          2236815