17β-Hydroxy-17α-methylandrostano[3,2-c]pyrazole, Stanozolol: The Crystal Structures of Polymorphs 1 and 2 and 10 Solvates
Karpinska, Jolanta; Erxleben, Andrea; McArdle, Patrick; Crystal Growth & Design 11 (2011) 2829–; doi:10.1021/cg101651p

data_4510898
_publ_section_title
;
 17\b-Hydroxy-17\a-methylandrostano[3,2-c]pyrazole, Stanozolol: The
 Crystal Structures of Polymorphs 1 and 2 and 10 Solvates
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2829
_journal_paper_doi               10.1021/cg101651p
_journal_volume                  11
_journal_year                    2011
_chemical_absolute_configuration
;
 absolute configuration not established by anomalous dispersion
 effects in diffraction measurements on the crystal.
;
_chemical_formula_sum            'C25 H42 N2 O2'
_chemical_formula_weight         402.61
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 123.40
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.321(2)
_cell_length_b                   7.421(2)
_cell_length_c                   15.393(2)
_cell_measurement_reflns_used    3930
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.1956
_cell_measurement_theta_min      3.0427
_cell_volume                     2414.8(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
;
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 16.1048
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    1.00   74.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -       19.7341   77.0000  120.0000 73
  2 omega   63.00   90.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -       19.7341   77.0000 -120.0000 27
  3 omega   31.00   79.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -       19.7341   77.0000  -60.0000 48
  4 omega   -3.00   75.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -       19.7341   77.0000   30.0000 78
  5 omega  -94.00  -32.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -      -17.3903  179.0000 -150.0000 62
  6 omega  -47.00   53.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -      -17.3903   77.0000 -150.0000 100
  7 omega  -94.00  -32.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -      -17.3903  179.0000   60.0000 62
  8 omega  -20.00   26.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -       19.7341   97.0000 -111.0000 46
  9 omega  -10.00   90.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -       19.7341   77.0000 -150.0000 100
 10 omega   34.00   96.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -       19.7341  179.0000  150.0000 62
 11 omega   -6.00   60.00   1.0000   25.6400
omega____ theta____ kappa____ phi______ frames
    -       19.7341   37.0000    0.0000 66
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0303195000
_diffrn_orient_matrix_UB_12      -0.0336085000
_diffrn_orient_matrix_UB_13      0.0157998000
_diffrn_orient_matrix_UB_21      -0.0081518000
_diffrn_orient_matrix_UB_22      0.0076230000
_diffrn_orient_matrix_UB_23      -0.0519489000
_diffrn_orient_matrix_UB_31      0.0120556000
_diffrn_orient_matrix_UB_32      0.0888814000
_diffrn_orient_matrix_UB_33      0.0103105000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17882
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.3487
_diffrn_reflns_theta_min         3.0427
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.7(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4402
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0777P)^2^+0.3032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                3388
_reflns_number_total             4402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            5.cif
_cod_data_source_block           stan_proh
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2414.6(7)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4510898