Unprecedented one-dimensional chain and two-dimensional network dysprosium(iii) single-molecule toroics with white-light emission.
Zhong, Li; Chen, Wen-Bin; OuYang, Zhi-Jian; Yang, Meng; Zhang, Yi-Quan; Gao, Song; Schulze, Michael; Wernsdorfer, Wolfgang; Dong, Wen; Chemical communications (Cambridge, England) 56 (2020) 2590–2593; doi:10.1039/c9cc08852k

data_7125874
_publ_section_title
;
 Unprecedented one-dimensional chain and two-dimensional network
 dysprosium(iii) single-molecule toroics with white-light emission.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2590
_journal_page_last               2593
_journal_paper_doi               10.1039/c9cc08852k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C48 H56 Dy6 O36'
_chemical_formula_sum            'C48 H56 Dy6 O36'
_chemical_formula_weight         2183.92
_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
_audit_creation_date             2019-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                66.985(3)
_cell_angle_beta                 74.839(3)
_cell_angle_gamma                78.055(3)
_cell_formula_units_Z            2
_cell_length_a                   15.0529(5)
_cell_length_b                   16.5502(5)
_cell_length_c                   19.5506(5)
_cell_measurement_reflns_used    12148
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      73.9820
_cell_measurement_theta_min      2.8710
_cell_volume                     4296.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.950
_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    -40.00  23.00   0.50    7.00    --  -46.37  39.00  14.00  126
  2  \w    -21.00  28.00   0.50    7.00    --  -46.37  19.00 150.00   98
  3  \w    -55.00 -29.00   0.50   37.00    -- -102.00 125.00  30.00   52
  4  \w    -70.00 -26.00   0.50    7.00    --  -46.37  77.00  60.00   88
  5  \w    -77.00 -34.00   0.50   37.00    -- -102.00  77.00 120.00   86
  6  \w    -55.00 -29.00   0.50   37.00    -- -102.00  61.00  90.00   52
  7  \w   -110.00 -84.00   0.50   37.00    -- -102.00 125.00  30.00   52
  8  \w   -116.00 -48.00   0.50   37.00    -- -102.00 125.00 -60.00  136
  9  \w    -62.00 -36.00   0.50   37.00    -- -102.00  61.00-120.00   52
 10  \w    -14.00  17.00   0.50    7.00    --  -46.37  19.00-180.00   62
 11  \w    -60.00 -30.00   0.50   37.00    -- -102.00 125.00-150.00   60
 12  \w   -103.00 -54.00   0.50   37.00    -- -102.00  77.00-180.00   98
 13  \w   -116.00 -82.00   0.50   37.00    -- -102.00 125.00-150.00   68
 14  \w   -174.00 -85.00   0.50   37.00    -- -102.00 -15.00 -60.00  178
 15  \w   -119.00 -33.00   0.50    7.00    --  -46.37 -39.00-139.00  172
 16  \w    -21.00  46.00   0.50    7.00    --   46.37 -39.00-139.00  134
 17  \w     90.00 116.00   0.50    7.00    --   46.37  37.00-150.00   52
 18  \w    127.00 172.00   0.50   37.00    --  106.69  77.00 -60.00   90
 19  \w    137.00 168.00   0.50   37.00    --  106.69 125.00   0.00   62
 20  \w     92.00 169.00   0.50   37.00    --  106.69  39.00  14.00  154
 21  \w    120.00 153.00   0.50   37.00    --  106.69  45.00 150.00   66
 22  \w     91.00 178.00   0.50   37.00    --  106.69  15.00 120.00  174
 23  \w     72.00 108.00   0.50   37.00    --  106.69 -94.00 -90.00   72
 24  \w     38.00 113.00   0.50   37.00    --  106.69-125.00-120.00  150
 25  \w     34.00  69.00   0.50   37.00    --  106.69 -94.00 -90.00   70
 26  \w     40.00  72.00   0.50   37.00    --  106.69 -61.00 -90.00   64
 27  \w     37.00  71.00   0.50   37.00    --  106.69 -61.00-150.00   68
 28  \w     38.00  88.00   0.50   37.00    --  106.69 -77.00 -90.00  100
 29  \w     41.00  73.00   0.50   37.00    --  106.69 -61.00   0.00   64
 30  \w     37.00  72.00   0.50   37.00    --  106.69 -61.00  30.00   70
 31  \w     47.00 105.00   0.50   37.00    --  106.69 -94.00  90.00  116
 32  \w     77.00 115.00   0.50   37.00    --  106.69-125.00  90.00   76
 33  \w     79.00 114.00   0.50   37.00    --  106.69-125.00  60.00   70
 34  \w     47.00 116.00   0.50   37.00    --  106.69-125.00  30.00  138
 35  \w     34.00  73.00   0.50   37.00    --  106.69-125.00  60.00   78
 36  \w     37.00  73.00   0.50   37.00    --  106.69-125.00  90.00   72
 37  \w     36.00  73.00   0.50   37.00    --  106.69 -61.00 120.00   74
 38  \w     29.00  85.00   0.50    7.00    --   46.37-125.00  90.00  112
 39  \w     37.00 117.00   0.50    7.00    --   46.37  39.00  14.00  160
 40  \w     77.00 114.00   0.50   37.00    --  106.69 125.00   0.00   74
 41  \w     32.00  75.00   0.50    7.00    --   46.37  37.00-150.00   86
 42  \w   -113.00 -87.00   0.50   37.00    -- -102.00 -45.00 120.00   52
 43  \w   -167.00-126.00   0.50   37.00    -- -102.00 -45.00 120.00   82
 44  \w   -175.00 -95.00   0.50   37.00    -- -102.00 -39.00-139.00  160
 45  \w   -117.00 -37.00   0.50   37.00    -- -102.00 125.00 150.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0944401000
_diffrn_orient_matrix_UB_12      0.0522019000
_diffrn_orient_matrix_UB_13      0.0191252000
_diffrn_orient_matrix_UB_21      0.0448731000
_diffrn_orient_matrix_UB_22      0.0867230000
_diffrn_orient_matrix_UB_23      -0.0382425000
_diffrn_orient_matrix_UB_31      -0.0216581000
_diffrn_orient_matrix_UB_32      0.0112397000
_diffrn_orient_matrix_UB_33      -0.0762141000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1211
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56977
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.241
_diffrn_reflns_theta_min         2.506
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    27.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.074
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         17289
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0962
_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^)+(0.1969P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2565
_refine_ls_wR_factor_ref         0.2846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10953
_reflns_number_total             17289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08852k2.cif
_cod_data_source_block           exp_159_sq
_cod_depositor_comments
'Adding full bibliography for 7125873--7125874.cif.'
_cod_original_cell_volume        4296.7(3)
_cod_database_code               7125874
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Dy C H N O'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C36-H40B
 2.72 with sigma of 0.02
 H40A-C36
 2.72 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O19) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of 0.001
4.a Riding coordinates:
 O13(H13), O14(H14), O18(H18A,H18B), O31(H31), O32(H32)
4.b Rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O33(H33A,H33B), O34(H34A,
 H34B), O35(H35A,H35B), O36(H36A,H36B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C12(H12), C13(H13A), C14(H14A), C20(H20), C21(H21),
 C22(H22), C28(H28), C29(H29), C30(H30), C36(H36), C37(H37), C38(H38), C44(H44),
  C45(H45), C46(H46)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16C,H16D,H16E), C24(H24A,H24B,H24C), C32(H32A,H32B,
 H32C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              43657
_shelx_fab_checksum              51276
_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 3.466
_oxdiff_exptl_absorpt_empirical_full_min 0.414