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_2022615
_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          'C20 H27 Cl O2'
_chemical_formula_moiety         'C20 H27 Cl O2'
_chemical_formula_sum            'C20 H27 Cl O2'
_chemical_formula_weight         334.86
_chemical_name_common            Turinabol
_chemical_name_systematic
;
4-Chloro-17\b-hydroxy-17\a-methylandrosta-1,4-dien-3-one
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.759(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8409(3)
_cell_length_b                   10.2250(2)
_cell_length_c                   16.4751(5)
_cell_measurement_reflns_used    11218
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.9430
_cell_measurement_theta_min      4.0920
_cell_volume                     1822.31(8)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_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
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.4335
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26247
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.803
_diffrn_reflns_theta_min         4.087
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.208
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2594 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6891
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.0816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                6235
_reflns_number_total             6891
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           TBOL2
_cod_database_code               2022615
_shelx_hkl_checksum              89722
_shelx_res_checksum              78616
_cod_database_fobs_code 2022615