3β-Acetoxy-5α-cholestan-6-one 2-cyanoacetylhydrazone
Yusufzai, Samina Khan; Osman, Hasnah; Sulaiman, Othman; Arshad, Suhana; Razak, Ibrahim Abdul; Acta Crystallographica Section E 68 (2012) o473–o474; doi:10.1107/S1600536812001432

data_2233519
_publ_section_title
;
 3\b-Acetoxy-5\a-cholestan-6-one 2-cyanoacetylhydrazone
;
_journal_coeditor_code           IS5021
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o473
_journal_page_last               o474
_journal_paper_doi               10.1107/S1600536812001432
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C32 H51 N3 O3'
_chemical_formula_moiety         'C32 H51 N3 O3'
_chemical_formula_sum            'C32 H51 N3 O3'
_chemical_formula_weight         525.76
_chemical_name_common
;
3\b-Acetoxy-5\a-cholestan-6-one 2-cyanoacetylhydrazone
;
_chemical_name_systematic
;
6-[2-(2-Cyanoacetyl)hydrazin-1-ylidene]-5\a-cholestan-3\b-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                90.00
_cell_angle_beta                 109.1710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1691(2)
_cell_length_b                   9.66940(10)
_cell_length_c                   19.1447(3)
_cell_measurement_reflns_used    5129
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.87
_cell_volume                     3002.05(7)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Bruker SMART APEXII CCD area-detector
;
_diffrn_measurement_method       '\f and \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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40102
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_correction_T_min  0.9765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         9291
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0539P)^2^+0.0496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                6778
_reflns_number_total             9291
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is5021.cif
_cod_data_source_block           I
_cod_original_cell_volume        3002.04(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2233519
_cod_database_fobs_code          2233519