17-β-Estradiol—β-Cyclodextrin Complex as Solid: Synthesis, Structural and Physicochemical Characterization
Mazurek, Anna Helena; Szeleszczuk, Łukasz; Bethanis, Kostas; Christoforides, Elias; Dudek, Marta Katarzyna; Zielińska-Pisklak, Monika; Pisklak, Dariusz Maciej; Molecules 28 (2023) 3747–; doi:10.3390/molecules28093747

data_1569084
_publ_section_title
;
 17-\b-Estradiol---\b-Cyclodextrin Complex as Solid: Synthesis, Structural
 and Physicochemical Characterization
;
_journal_issue                   9
_journal_name_full               Molecules
_journal_page_first              3747
_journal_paper_doi               10.3390/molecules28093747
_journal_volume                  28
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_compound_source        'as described'
_chemical_formula_moiety         'C51 H82 O46.5'
_chemical_formula_sum            'C51 H82 O46.5'
_chemical_formula_weight         1439.16
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-02T17:00:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.500(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1245(15)
_cell_length_b                   24.4180(18)
_cell_length_c                   15.6004(11)
_cell_measurement_reflns_used    9073
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.25
_cell_measurement_theta_min      3.05
_cell_measurement_wavelength     1.54184
_cell_volume                     6867.2(9)
_computing_cell_refinement       'SAINT V8.40B integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      -0.023623
_diffrn_orient_matrix_UB_12      0.009032
_diffrn_orient_matrix_UB_13      -0.065915
_diffrn_orient_matrix_UB_21      0.042056
_diffrn_orient_matrix_UB_22      -0.018115
_diffrn_orient_matrix_UB_23      -0.013502
_diffrn_orient_matrix_UB_31      -0.027391
_diffrn_orient_matrix_UB_32      -0.035602
_diffrn_orient_matrix_UB_33      -0.009852
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            105516
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 4239 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     950
_refine_ls_number_reflns         11945
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.104
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1769P)^2^+15.8528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2591
_refine_ls_wR_factor_ref         0.2688
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                10450
_reflns_number_total             11945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            estradiol_beta-CD.cif
_cod_data_source_block           cu_2022kbperst_0m
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C51 H82 O46.50'
_cod_database_code               1569084
_shelx_estimated_absorpt_t_min   0.669
_shelx_estimated_absorpt_t_max   0.871
_shelx_res_checksum              78854
_shelx_hkl_checksum              84867