Sweet pharmaceutical salts of stanozolol with enhanced solubility and physical stability
Kong, Minmin; Fu, Xue; Li, Jiaoyang; Li, Jianhui; Chen, Minhua; Deng, Zongwu; Zhang, Hailu; CrystEngComm 18 (2016) 8739–; doi:10.1039/C6CE01876A

data_7226789
_publ_section_title
;
 Sweet pharmaceutical salts of stanozolol with enhanced solubility and
 physical stability
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              8739
_journal_paper_doi               10.1039/C6CE01876A
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H33 N2 O, C4 H4 N O4 S'
_chemical_formula_sum            'C25 H37 N3 O5 S'
_chemical_formula_weight         491.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-16 deposited with the CCDC.
2016-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.633(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3761(5)
_cell_length_b                   17.7987(15)
_cell_length_c                   9.5359(9)
_cell_measurement_reflns_used    1872
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      27.1630
_cell_measurement_theta_min      3.4700
_cell_volume                     1237.74(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector_area_resol_mean 10.4471
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   65.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6514  178.0000    0.0000 27

  2 omega   14.00   56.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6514  -99.0000   30.0000 42

  3 omega  -65.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889    0.0000 -180.0000 140

  4 omega  -91.00  -19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889  -37.0000  120.0000 72
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0336647000
_diffrn_orient_matrix_UB_12      -0.0308106000
_diffrn_orient_matrix_UB_13      0.0358509000
_diffrn_orient_matrix_UB_21      0.0164176000
_diffrn_orient_matrix_UB_22      0.0201730000
_diffrn_orient_matrix_UB_23      0.0646978000
_diffrn_orient_matrix_UB_31      -0.0897449000
_diffrn_orient_matrix_UB_32      0.0152314000
_diffrn_orient_matrix_UB_33      -0.0136807000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8262
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.18(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4381
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0462
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                3506
_reflns_number_total             4381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce01876a2.cif
_cod_data_source_block           nami-150528akmm
_cod_depositor_comments
'Adding full bibliography for 7226788--7226789.cif.'
_cod_original_cell_volume        1237.73(18)
_cod_database_code               7226789
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C13(H13), C14(H14), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C22(H22A,H22B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), N1(H1), N2(H2), C2(H2A)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C4(H4A,H4B,H4C)
2.e Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_olex2_date_sample_data_collection 2015-05-28
_olex2_submission_special_instructions 'No special instructions were received'