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_4510896
_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            'C23.5 H34.5 N2.5 O'
_chemical_formula_weight         368.04
_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                   7.233(2)
_cell_length_b                   11.850(2)
_cell_length_c                   48.672(2)
_cell_measurement_reflns_used    5551
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.8887
_cell_measurement_theta_min      2.9237
_cell_volume                     4171.7(14)
_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  -23.00    3.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -        0.7812   77.0000  -60.0000 52
  2 omega   19.00   57.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.2830   77.0000   60.0000 76
  3 omega  -74.00  -48.50   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.2830   77.0000   60.0000 51
  4 omega   86.00  112.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8455   77.0000  -90.0000 52
  5 omega  -16.00   50.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8455   77.0000  -90.0000 132
  6 omega   25.00   67.00   0.5000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8455   77.0000  150.0000 84
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0873977000
_diffrn_orient_matrix_UB_12      -0.0172566000
_diffrn_orient_matrix_UB_13      0.0051003000
_diffrn_orient_matrix_UB_21      -0.0279918000
_diffrn_orient_matrix_UB_22      0.0145455000
_diffrn_orient_matrix_UB_23      0.0135075000
_diffrn_orient_matrix_UB_31      -0.0345493000
_diffrn_orient_matrix_UB_32      -0.0554495000
_diffrn_orient_matrix_UB_33      0.0019640000
_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  0.0251
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            12520
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.3487
_diffrn_reflns_theta_min         2.9237
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79858
_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    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0274P)^2^+2.3003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                4847
_reflns_number_total             6556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            11.cif
_cod_data_source_block           stan_py
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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        4171.8(14)
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C23.50 H34.50 N2.50 O'
_cod_database_code               4510896