Methyl <i>N</i>'-(17β-hydroxyandrost-1-en-3-ylidene)hydrazinedithiocarboxylate
Li-Ming Zhang; Wei-Xiao Hu; Chun-Nian Xia; Acta Crystallographica Section E 63 (2007) o2467–o2468; doi:10.1107/S1600536807016868

data_2213234
_publ_section_title
;
 Methyl
 <i>N</i>'-(17\b-hydroxyandrost-1-en-3-ylidene)hydrazinedithiocarboxylate
;
_journal_coeditor_code           CI2351
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2467
_journal_page_last               o2468
_journal_paper_doi               10.1107/S1600536807016868
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C21 H32 N2 O S2'
_chemical_formula_moiety         'C21 H32 N2 O S2'
_chemical_formula_sum            'C21 H32 N2 O S2'
_chemical_formula_weight         392.61
_chemical_name_systematic
;
Methyl N'-(17\b-hydroxyandrost-1-en-3-ylidene)hydrazinedithiocarboxylate
;
_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            4
_cell_length_a                   9.8693(10)
_cell_length_b                   11.7844(12)
_cell_length_c                   18.0029(18)
_cell_measurement_reflns_used    5693
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.35
_cell_volume                     2093.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13545
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.9242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.194
_refine_ls_abs_structure_details 'Flack (1983), 2031 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0623P)^2^+0.1604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                4085
_reflns_number_total             4850
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2351.cif
_cod_data_source_block           I
_cod_database_code               2213234
_cod_database_fobs_code          2213234