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_2022616
_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 H4 O2, H2 O'
_chemical_formula_moiety         '2(C20 H27 Cl O2), C2 H4 O2, H2 O'
_chemical_formula_sum            'C42 H60 Cl2 O7'
_chemical_formula_weight         747.80
_chemical_name_common            'Turinabol acetic acid solvate hydrate'
_chemical_name_systematic
;
4-Chloro-17\b-hydroxy-17\a-methylandrosta-1,4-dien-3-one
acetic acid hemisolvate hemihydrate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_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            8
_cell_length_a                   10.70311(10)
_cell_length_b                   10.70311(10)
_cell_length_c                   68.7275(8)
_cell_measurement_reflns_used    32928
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.275
_cell_measurement_theta_min      4.180
_cell_volume                     7873.19(14)
_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)
;
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;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
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;
SHELXL2016 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Rigaku OD SuperNova Dual source diffractometer with an Eos detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -84
_diffrn_reflns_number            116676
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.275
_diffrn_reflns_theta_min         4.180
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.872
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       needle
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.251
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2580 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.006(4)
_refine_ls_extinction_coef       0.00061(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7557
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0382P)^2^+2.5992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                7057
_reflns_number_total             7557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vp3023sup1.cif
_cod_data_source_block           TBOL3
_cod_original_cell_volume        7873.20(18)
_cod_database_code               2022616
_shelx_hkl_checksum              31829
_shelx_res_checksum              61219
_cod_database_fobs_code 2022616