3β-(1-Allyl-1-pyrrolidinio)-16-(2-pyridylmethylene)androst-5-en-17β-ol bromide hemihydrate
Vasuki, G.; Thamotharan, S.; Parthasarathi, V.; Ramamurthi, K.; Dubey, S.; Jindal, D. P.; Acta Crystallographica Section C 58 (2002) o598–o599; doi:10.1107/S0108270102013434

data_2012969
_publ_section_title
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 3\b-(1-Allyl-1-pyrrolidinio)-16-(2-pyridylmethylene)androst-5-en-17\b-ol
 bromide hemihydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o598
_journal_page_last               o599
_journal_paper_doi               10.1107/S0108270102013434
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C32 H45 Br N2 O , 0.5H2 O'
_chemical_formula_moiety         'C32 H45 Br N2 O , 0.5H2 O'
_chemical_formula_sum            'C32 H46 Br N2 O1.5'
_chemical_formula_weight         562.61
_chemical_name_systematic
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3\b-(1-Allyl-1-pyrrolidinio)-16-(2-pyridylmethylene)androst-5-ene-17\b-ol
bromide hemihydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 106.15(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.054(4)
_cell_length_b                   9.3083(18)
_cell_length_c                   15.551(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2927.4(11)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2835
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.23
_refine_ls_abs_structure_details 'Flack (1983) How many Friedels?'
_refine_ls_abs_structure_Flack   -0.002(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         2751
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.062
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
' w = 1/[\s^2^(Fo^2^)+(0.0413P)^2^+2.1207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.072
_refine_ls_wR_factor_ref         0.089
_reflns_number_gt                2100
_reflns_number_total             2751
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            de1189.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2012969
_cod_database_fobs_code          2012969