Solid forms and β-cyclodextrin complexation of turinabol
Turza, Alexandru; Ulici, Adelina; Muresan-Pop, Marieta; Borodi, Gheorghe; Acta Crystallographica Section C 78 (2022) 305–313; doi:10.1107/S2053229622004004

data_2022617
_publ_section_title
;
 Solid forms and \b-cyclodextrin complexation of turinabol
;
_journal_coeditor_code           VP3023
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              305
_journal_page_last               313
_journal_paper_doi               10.1107/S2053229622004004
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_iupac          '2C20 H27 Cl O2, C2 H3 F3 O'
_chemical_formula_moiety         '2(C20 H27 Cl O2), C2 H3 F3 O'
_chemical_formula_sum            'C42 H57 Cl2 F3 O5'
_chemical_formula_weight         769.77
_chemical_name_common            Turinabol_2,2,2_trifluoroethanol_solvate
_chemical_name_systematic
;
4-Chloro-17\b-hydroxy-17\a-methylandrosta-1,4-dien-3-one
2,2,2_trifluoroethanol hemisolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3088(3)
_cell_length_b                   12.9337(3)
_cell_length_c                   29.6661(7)
_cell_measurement_reflns_used    7938
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.8210
_cell_measurement_theta_min      3.7160
_cell_volume                     3955.41(17)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.4335
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku OD SuperNova Dual source diffractometer with an Eos detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            27841
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.898
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.952
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2018)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.287
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2168 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7527
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0595P)^2^+0.6178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                6093
_reflns_number_total             7527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vp3023sup1.cif
_cod_data_source_block           TBOL4
_cod_original_cell_volume        3955.44(17)
_cod_database_code               2022617
_shelx_hkl_checksum              75499
_shelx_res_checksum              89211
_cod_database_fobs_code 2022617