3β-Chloro-6-[2-(2-cyanoacetyl)hydrazin-1-ylidene]-5α-cholestane
Yusufzai, Samina Khan; Osman, Hasnah; Abdul Rahim, Aisyah Saad; Arshad, Suhana; Razak, Ibrahim Abdul; Acta Crystallographica Section E 68 (2012) o1056–o1057; doi:10.1107/S1600536812009336

data_2234218
_publ_section_title
;
 3\b-Chloro-6-[2-(2-cyanoacetyl)hydrazin-1-ylidene]-5\a-cholestane
;
_journal_coeditor_code           HB6661
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1056
_journal_page_last               o1057
_journal_paper_doi               10.1107/S1600536812009336
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C30 H48 Cl N3 O'
_chemical_formula_moiety         'C30 H48 Cl N3 O'
_chemical_formula_sum            'C30 H48 Cl N3 O'
_chemical_formula_weight         502.16
_chemical_name_systematic
;
3\b-Chloro-6-[2-(2-cyanoacetyl)hydrazin-1-ylidene]-5\a-cholestane
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.1623(2)
_cell_length_b                   19.7586(3)
_cell_length_c                   26.4077(4)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.20
_cell_volume                     5824.26(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51504
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.9759
_exptl_absorpt_correction_T_min  0.9513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.517
_refine_ls_abs_structure_details 'Flack (1983), 5882 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(11)
_refine_ls_extinction_coef       0.00130(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         13243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.1035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+25.2717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2214
_reflns_number_gt                12103
_reflns_number_total             13243
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6661.cif
_cod_data_source_block           I
_cod_database_code               2234218
_cod_database_fobs_code          2234218