Coupling Dy3 toroics in macrocycles
Yang, Qianqian; Wu, Jianfeng; Zhao, Chen; Ying, Xu; Zhu, Dong-Mei; Guo, Xuefeng; Liu, Dan; Zhang, Yi-Quan; Tang, Jinkui; Chemical Communications 61 (2025) 8751–8754; doi:10.1039/D4CC06785A

data_7134539
_publ_section_title
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 Coupling Dy3 toroics in macrocycles
;
_journal_issue                   48
_journal_name_full               'Chemical Communications'
_journal_page_first              8751
_journal_page_last               8754
_journal_paper_doi               10.1039/D4CC06785A
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C42 H62 Br2 Dy6 N12 O24, 6(Br), 2[CH3CH2OH], 2[CH3CN], 2[H2O]'
_chemical_formula_sum            'C50 H84 Br8 Dy6 N14 O28'
_chemical_formula_weight         2943.59
_chemical_name_systematic        1
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-12-20 deposited with the CCDC.	2025-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.553(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9070(17)
_cell_length_b                   17.303(2)
_cell_length_c                   20.936(3)
_cell_measurement_reflns_used    6758
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      2.71
_cell_volume                     4276.0(10)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41373
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.122
_diffrn_reflns_theta_max         25.122
_diffrn_reflns_theta_min         2.089
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.990
_exptl_absorpt_correction_T_max  0.151
_exptl_absorpt_correction_T_min  0.122
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.286
_exptl_crystal_description       block
_exptl_crystal_F_000             2764
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.351
_refine_diff_density_min         -1.724
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7561
_refine_ls_number_restraints     341
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+86.9903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5187
_reflns_number_total             7561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06785a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7134539.cif.'
_cod_original_cell_volume        4276.1(10)
_cod_database_code               7134539
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.254
_shelx_estimated_absorpt_t_min   0.212
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H18 of C18, H19 of C19, H14 of C14, H20 of C20, H6 of C6,
   H13 of C13, H5B of C5, H11 of C11, H4 of C4, H9 of C9, All N(H) groups
 At 1.5 times of:
  All O(H) groups, H5 of C1, All O(H,H) groups
2. Restrained distances
 H5-O5
 0.85 with sigma of 0.001
 H5-Dy1
 3 with sigma of 0.01
 H5-Dy2_$1
 3 with sigma of 0.01
 H5-H13
 1.95 with sigma of 0.001
 Dy2-H9A \\sim Dy2-H9B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
4.a Free rotating group:
 O9(H9A,H9B)
4.b Rotating group:
 O6(H6A,H6B), O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B)
4.c Ternary CH refined with riding coordinates:
 O7(H7), O8(H8)
4.d Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C21(H21A,H21B)
4.e Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5A), C4(H4), C5(H5B), C6(H6), C9(H9), C13(H13), C11(H11),
 C14(H14), C18(H18), C19(H19), C20(H20)
4.f Fitted hexagon refined as free rotating group:
 C13(N3,C10,C11,C12,N4)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 236 electrons were 
found in a volume of 1048\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH3CH2OH], 2[CH3CN], 2[H2O] per Asymmetric Unit 
which account for 232 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2694
_shelx_hkl_checksum              91969
_shelx_fab_checksum              25276
_olex2_submission_special_instructions 'No special instructions were received'