Acyl migrations sensitive to supramolecular encapsulation
Lagerna, Oleksandra; Shivanyuk, Alexander; Kienko, Tetyana; Shishkina, Svitlana V.; Lukin, Oleg; Fetyukhin, Volodymyr; Chemical Communications 61 (2025) 8500–8503; doi:10.1039/D5CC01417D

data_7134457
_publ_section_title
;
 Acyl migrations sensitive to supramolecular encapsulation
;
_journal_issue                   47
_journal_name_full               'Chemical Communications'
_journal_page_first              8500
_journal_page_last               8503
_journal_paper_doi               10.1039/D5CC01417D
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C H2 Cl2, C92 H80 O12'
_chemical_formula_sum            'C93 H82 Cl2 O12'
_chemical_formula_weight         1462.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-23
_audit_creation_method
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Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                82.547(2)
_cell_angle_beta                 78.9260(10)
_cell_angle_gamma                81.9300(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0383(4)
_cell_length_b                   15.1570(5)
_cell_length_c                   20.5626(7)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.23
_cell_volume                     3926.3(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44774
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.612
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         13759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0581P)^2^+4.0985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9085
_reflns_number_total             13759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01417d2.cif
_cod_data_source_block           6b_ch2cl2
_cod_depositor_comments          'Adding full bibliography for 7134457.cif.'
_cod_database_code               7134457
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C29(H29A,H29B), C30(H30A,H30B), C37(H37A,H37B), C38(H38A,
 H38B), C45(H45A,H45B), C46(H46A,H46B), C53(H53A,H53B), C54(H54A,H54B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C13(H13), C17(H17), C20(H20), C24(H24), C27(H27),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C40(H40), C41(H41), C42(H42),
  C43(H43), C44(H44), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C63(H63), C64(H64), C65(H65),
  C66(H66), C67(H67), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
 C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C87(H87), C88(H88), C89(H89),
  C90(H90), C91(H91)
2.d Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C76(H76A,H76B,H76C), C84(H84A,H84B,H84C), C92(H92A,H92B,
 H92C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40002
_shelx_hkl_checksum              53578
_shelx_fab_checksum              11336
_olex2_submission_special_instructions 'No special instructions were received'