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_7125873
_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         'C32 H33 Dy3 O21'
_chemical_formula_sum            'C34 H34 Dy3 O22'
_chemical_formula_weight         1282.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-05-04
_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                90
_cell_angle_beta                 105.5380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.2940(2)
_cell_length_b                   18.1452(2)
_cell_length_c                   22.5707(2)
_cell_measurement_reflns_used    19867
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2310
_cell_measurement_theta_min      3.0730
_cell_volume                     9585.98(16)
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.958
_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    -23.00  28.00   0.50    4.00    --  -46.62  19.00 -60.00  102
  2  \w    -24.00  29.00   0.50    4.00    --  -46.62  19.00-150.00  106
  3  \w    -92.00 -47.00   0.50    4.00    --  -46.62 118.00 -79.00   90
  4  \w    -95.00 -70.00   0.50   12.00    -- -102.00 118.00 -79.00   50
  5  \w    -96.00 -70.00   0.50    4.00    --  -46.62 158.00  74.00   52
  6  \w   -138.00-112.00   0.50   12.00    -- -102.00 158.00  74.00   52
  7  \w    -62.00 -29.00   0.50   12.00    -- -102.00  61.00 150.00   66
  8  \w    -68.00 -29.00   0.50   12.00    -- -102.00  61.00 120.00   78
  9  \w   -119.00 -71.00   0.50    4.00    --  -46.62-125.00 -60.00   96
 10  \w   -105.00 -49.00   0.50    4.00    --  -46.62-158.00  40.00  112
 11  \w     55.00 102.00   0.50    4.00    --   46.62 158.00  74.00   94
 12  \w     95.00 173.00   0.50   12.00    --  106.69 118.00 -79.00  156
 13  \w    141.00 167.00   0.50   12.00    --  106.69  45.00   0.00   52
 14  \w    130.00 177.00   0.50   12.00    --  106.69  30.00 -90.00   94
 15  \w    104.00 129.00   0.50   12.00    --  106.69  45.00   0.00   50
 16  \w     92.00 118.00   0.50   12.00    --  106.69  30.00 -90.00   52
 17  \w     71.00  96.00   0.50   12.00    --  106.69 -77.00-180.00   50
 18  \w     53.00 108.00   0.50   12.00    --  106.69 -94.00-150.00  110
 19  \w     49.00  74.00   0.50   12.00    --  106.69-118.00-166.00   50
 20  \w     35.00  65.00   0.50   12.00    --  106.69 -77.00-180.00   60
 21  \w     37.00  73.00   0.50   12.00    --  106.69 -61.00-120.00   72
 22  \w     39.00  73.00   0.50   12.00    --  106.69 -61.00 -30.00   68
 23  \w     45.00 102.00   0.50   12.00    --  106.69 -77.00  30.00  114
 24  \w     37.00 135.00   0.50   12.00    --  106.69-158.00  40.00  196
 25  \w   -119.00 -94.00   0.50    4.00    --  -46.62-125.00-120.00   50
 26  \w   -150.00-125.00   0.50   12.00    -- -102.00-118.00-166.00   50
 27  \w   -171.00 -87.00   0.50   12.00    -- -102.00 -30.00  30.00  168
;
_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      -0.0392863000
_diffrn_orient_matrix_UB_12      -0.0456486000
_diffrn_orient_matrix_UB_13      -0.0520274000
_diffrn_orient_matrix_UB_21      0.0322024000
_diffrn_orient_matrix_UB_22      -0.0706436000
_diffrn_orient_matrix_UB_23      0.0270335000
_diffrn_orient_matrix_UB_31      -0.0418588000
_diffrn_orient_matrix_UB_32      -0.0115334000
_diffrn_orient_matrix_UB_33      0.0397712000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35482
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.928
_diffrn_reflns_theta_min         3.082
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29451
_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    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.754
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         9712
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0955P)^2^+56.7583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8480
_reflns_number_total             9712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08852k2.cif
_cod_data_source_block           exp_146_sq
_cod_depositor_comments
'Adding full bibliography for 7125873--7125874.cif.'
_cod_original_cell_volume        9585.97(16)
_cod_database_code               7125873
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Dy C H O'
_shelx_estimated_absorpt_t_max   0.312
_shelx_estimated_absorpt_t_min   0.167
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H18 of O18, H17 of O17
 At 1.5 times of:
  All C(H,H,H) groups, H15 of O15, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O17(H17), O18(H18)
3.b Rotating group:
 O19(H19A,H19B), O20(H20A,H20B), O21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C20(H20), C21(H21),
 C22(H22), C28(H28), C29(H29), C30(H30)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C)
3.e Idealised tetrahedral OH refined as rotating group:
 O15(H15)
;
_shelx_res_checksum              16541
_shelx_fab_checksum              68536
_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 2.646
_oxdiff_exptl_absorpt_empirical_full_min 0.286