C-H amination reactions inside α-cyclodextrin supramolecular capsule.
Barvík, Ivan; Císařová, Ivana; Dian, Juraj; Holovko-Kamoshenkova, Oksana; Štícha, Martin; Tošner, Zdeněk; Jindřich, Jindřich; Hrdina, Radim; Organic & biomolecular chemistry 23 (2025) 10684–10688; doi:10.1039/d5ob01545f

data_7160873
_publ_section_title
;
 C-H amination reactions inside &#x3b1;-cyclodextrin supramolecular
 capsule.
;
_journal_issue                   47
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              10684
_journal_page_last               10688
_journal_paper_doi               10.1039/d5ob01545f
_journal_volume                  23
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         '4(C36 H54 O30),2(C11 H15 N3 O2),27(O)'
_chemical_formula_sum            'C83 H123 N3 O75.5'
_chemical_formula_weight         2370.84
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-12-18 deposited with the CCDC.	2025-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.205(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.1358(6)
_cell_length_b                   14.0944(6)
_cell_length_c                   24.2566(10)
_cell_measurement_reflns_used    9157
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.0733
_cell_measurement_theta_min      3.3221
_cell_volume                     5515.3(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTONIII CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Cu  multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            81270
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.266
_diffrn_reflns_theta_min         3.258
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       prism
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.211
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 9474 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1487
_refine_ls_number_reflns         21607
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0648
_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^)+(0.1280P)^2^+3.2355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                20991
_reflns_number_total             21607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01545f2.cif
_cod_data_source_block           cu_rhf_19_hrdina
_cod_depositor_comments          'Adding full bibliography for 7160873.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C83 H123 N3 O75.50'
_cod_database_code               7160873
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.733
_shelx_estimated_absorpt_t_max   0.797
_shelx_res_checksum              89388