3β-Acetoxy-6-hydroxyiminocholestane
Ketuly, Kamal Aziz; Hadi, A. Hamid A.; Ng, Seik Weng; Tiekink, Edward R. T.; Acta Crystallographica Section E 67 (2011) o773–o774; doi:10.1107/S1600536811007306

data_2229664
_publ_section_title
;
 3\b-Acetoxy-6-hydroxyiminocholestane
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o773
_journal_page_last               o774
_journal_paper_doi               10.1107/S1600536811007306
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C29 H49 N O3'
_chemical_formula_moiety         'C29 H49 N O3'
_chemical_formula_sum            'C29 H49 N O3'
_chemical_formula_weight         459.69
_chemical_name_common
;
3\b-Acetoxy-6-hydroxyiminocholestane
;
_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-[(1<i>R</i>)-1,5-dimethylhexyl]-6-hydroxyimino-10,13-dimethyl-
2,3,4,7,8,9,10,11,12,13,14,15,16,17-tetradecahydro-1<i>H</i>-
cyclopenta[<i>a</i>]phenanthren-3-yl acetate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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
_cell_angle_beta                 93.466(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3934(13)
_cell_length_b                   9.6588(11)
_cell_length_c                   25.018(3)
_cell_measurement_reflns_used    2461
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      2.3
_cell_volume                     2748.1(6)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_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
_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  0.086
_diffrn_reflns_av_sigmaI/netI    0.086
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26531
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.23
_refine_ls_abs_structure_details nd
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         6690
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.99
_refine_ls_R_factor_all          0.092
_refine_ls_R_factor_gt           0.050
_refine_ls_shift/su_max_lt       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^)+(0.0489P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.096
_refine_ls_wR_factor_ref         0.114
_reflns_number_gt                4553
_reflns_number_total             6690
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5806.cif
_cod_data_source_block           I
_cod_original_cell_volume        2748.1(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2229664
_cod_database_fobs_code          2229664