Reversible single-crystal to single-crystal transformation between triangular single-molecule toroics
Feng, Lixi; Yang, Yue; Wang, Yu-Xia; Zhao, Yizhen; Liu, Zhong-Yi; Cong, Junzhuang; Zhang, Yi-Quan; Cheng, Peng; Dalton Transactions  (2023) –; doi:10.1039/D3DT03191H

data_7714396
_publ_section_title
;
 Reversible single-crystal to single-crystal transformation between
 triangular single-molecule toroics
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03191H
_journal_year                    2023
_chemical_formula_moiety         'C20 H43 Dy3 N8 O20, C3 H6 O'
_chemical_formula_sum            'C23 H49 Dy3 N8 O21'
_chemical_formula_weight         1261.20
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2gw47r
_audit_creation_date             2022-10-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-23 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                102.276(5)
_cell_angle_beta                 107.969(5)
_cell_angle_gamma                100.557(6)
_cell_formula_units_Z            2
_cell_length_a                   11.8703(8)
_cell_length_b                   11.8756(9)
_cell_length_c                   15.4895(7)
_cell_measurement_reflns_used    8658
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.7780
_cell_measurement_theta_min      3.4930
_cell_volume                     1955.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00  11.00   1.00    7.50    --   18.47 -57.00 -30.00   61
  2  \w     62.00  92.00   1.00    7.50    --   18.47-178.00 150.00   30
  3  \w    -10.00  26.00   1.00    7.50    --   18.47  77.00 -60.00   36
  4  \w     -8.00  67.00   1.00    7.50    --   18.47  77.00-180.00   75
  5  \w     -2.00  24.00   1.00    7.50    --   18.47  57.00 150.00   26
  6  \w    -85.00 -36.00   1.00    7.50    --  -19.41 138.00 -99.30   49
  7  \w    -83.00  54.00   1.00    7.50    --  -19.41   0.00 -30.00  137
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0603998000
_diffrn_orient_matrix_UB_12      -0.0288000000
_diffrn_orient_matrix_UB_13      -0.0047804000
_diffrn_orient_matrix_UB_21      -0.0018634000
_diffrn_orient_matrix_UB_22      0.0520969000
_diffrn_orient_matrix_UB_23      0.0313734000
_diffrn_orient_matrix_UB_31      -0.0244915000
_diffrn_orient_matrix_UB_32      0.0219089000
_diffrn_orient_matrix_UB_33      -0.0389853000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13473
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.816
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic whiteish colourless'
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_description       block
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.616
_refine_diff_density_min         -2.525
_refine_diff_density_rms         0.332
_refine_ls_extinction_coef       0.00076(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         6740
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0153P)^2^+114.1045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6131
_reflns_number_total             6740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03191h2.cif
_cod_data_source_block           Dy3
_cod_database_code               7714396
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'Dy C H O N'
_chemical_oxdiff_usercomment     dY3-BINGTONG
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 O7-H7
 0.85 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 Dy2-H6
 3.037961 with sigma of 0.02
 C4-H6
 1.891647 with sigma of 0.02
 Dy3-H7
 2.988873 with sigma of 0.02
 C16-H7
 1.909807 with sigma of 0.02
 C00T-H8
 1.895128 with sigma of 0.02
 Dy3-H8
 2.884535 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C10) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O3)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C6) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(C00T)
\\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C00S) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C00T(H00C,H00D), C14(H14A,H14B), C10(H10A,H10B), C010(H01A,
 H01B), C4(H4A,H4B), C15(H15A,H15B), C5(H5A,H5B), C3(H3A,H3B), C11(H11A,H11B),
 C13(H13A,H13B), C2(H2A,H2B), C9(H9A,H9B), C12(H12A,H12B), C6(H6A,H6B),
 C16(H16A,H16B), C01D(H01C,H01D), C1(H1A,H1B), C8(H8A,H8B), C7(H7A,H7B)
4.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              61761
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.970
_oxdiff_exptl_absorpt_empirical_full_min 0.645