5,22-Stigmastadien-3β-yl <i>p</i>-toluenesulfonate
Ketuly, Kamal Aziz; Hadi, A. Hamid A.; Khaledi, Hamid; Tiekink, Edward R. T.; Acta Crystallographica Section E 66 (2010) o1336–; doi:10.1107/S1600536810016661

data_2226137
_publ_section_title
;
 5,22-Stigmastadien-3\b-yl <i>p</i>-toluenesulfonate
;
_journal_coeditor_code           HB5438
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1336
_journal_paper_doi               10.1107/S1600536810016661
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C36 H54 O3 S'
_chemical_formula_moiety         'C36 H54 O3 S'
_chemical_formula_sum            'C36 H54 O3 S'
_chemical_formula_weight         566.86
_chemical_name_common
;
5,22-Stigmastadien-3\b-yl <i>p</i>-toluenesulfonate
;
_chemical_name_systematic
;
(3<i>S</i>,8<i>S</i>,9<i>S</i>,10<i>R</i>,13<i>R</i>,14<i>S</i>,17<i>R</i>)-
17-[(<i>E</i>,2<i>R</i>,5<i>S</i>)-5-ethyl-6-methylhept-3-en-2-yl]-10,13-
dimethyl-2,3,4,7,8,9,11,12,14,15,16,17-dodecahydro-1<i>H</i>-
cyclopenta[<i>a</i>]phenanthren-3-yl <i>p</i>-toluenesulfonate
;
_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                90.7770(10)
_cell_angle_beta                 96.1660(10)
_cell_angle_gamma                101.1530(10)
_cell_formula_units_Z            2
_cell_length_a                   7.03610(10)
_cell_length_b                   11.23500(10)
_cell_length_c                   21.1550(2)
_cell_measurement_reflns_used    8182
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.6
_cell_volume                     1630.23(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997), DIAMOND (Brandenburg, 2006) and
Qmol (Gans & Shalloway, 2001)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_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  0.018
_diffrn_reflns_av_sigmaI/netI    0.037
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15647
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.37
_refine_ls_abs_structure_details 'Flack (1983), 5643 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         13115
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.035
_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^)+(0.0490P)^2^+0.2642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.087
_refine_ls_wR_factor_ref         0.089
_reflns_number_gt                12382
_reflns_number_total             13115
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5438.cif
_cod_data_source_block           I
_cod_database_code               2226137
_cod_database_fobs_code          2226137