Dimethylated β-cyclodextrin inclusion complexes containing the guest steroid hormones progesterone and 17β-estradiol: syntheses, crystal structures, thermal analyses and steroid solubility enhancements
Vicatos, Alexios I.; Hoossen, Zakiena; Edmonds-Smith, Cesarina; Caira, Mino R.; CrystEngComm 28 (2026) 1019–1029; doi:10.1039/D5CE01106J

data_7251689
_publ_section_title
;
 Dimethylated \b-cyclodextrin inclusion complexes containing the guest
 steroid hormones progesterone and 17\b-estradiol: syntheses, crystal
 structures, thermal analyses and steroid solubility enhancements
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1019
_journal_page_last               1029
_journal_paper_doi               10.1039/D5CE01106J
_journal_volume                  28
_journal_year                    2026
_chemical_absolute_configuration syn
_chemical_formula_moiety
;
C56 H98 O35, C56.4 H98.8 O35, 2(C18 H24 O2), 11.6(H2 O)
;
_chemical_formula_sum            'C148.4 H268 O85.6'
_chemical_formula_weight         3422.01
_chemical_name_common
;
Di-methylated beta-CD beta-estradiol clathrate hydrate
;
_chemical_name_systematic
;
heptakis(2,6-di-O-methyl)-beta-cyclodextrin (17beta)-
estra-1,3,5(10)-triene-3,17-diol clathrate hydrate
;
_chemical_temperature_decomposition 600
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2026-01-05 deposited with the CCDC.	2026-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.687(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1388(17)
_cell_length_b                   30.448(4)
_cell_length_c                   21.052(3)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.52
_cell_volume                     8634(2)
_computing_cell_refinement       'Program SAINT, v8.34A, Bruker AXS'
_computing_data_collection       'Bruker 2013, APEX2, v2013.10-0.'
_computing_data_reduction        'Program SAINT, v8.34A, Bruker AXS'
_computing_molecular_graphics
;
POV-Ray in interface X-Seed (LJ Barbour, 1999)
;
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-Version 2019/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean n/a
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II Duo diffractometer'
_diffrn_measurement_method       'phi- and omega-scans of 0.50 deg.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            160651
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.393
_diffrn_reflns_theta_min         1.653
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS-2012/1, Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             3686
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 11542 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2142
_refine_ls_number_reflns         43107
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0979P)^2^+4.2877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                31422
_reflns_number_total             43107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01106j2.cif
_cod_data_source_block           dmbbes5bV
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_chemical_melting_point' was changed to
'_chemical_temperature_decomposition' since the value had been
'decomp at 600 K'. The value 'decomp at 600 K' was changed to '600'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        8634.5(18)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C148.40 H268 O85.60'
_cod_database_code               7251689
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              78280