Double butterfly-shaped octanuclear dysprosium clusters: structure, magnetism and assembly mechanism
Li, Yun-Lan; Huang, Zhong-Ming; Wang, Hai-Ling; Zhu, Zhong-Hong; Liang, Fu-Pei; Zou, Hua-Hong; CrystEngComm 25 (2023) 225–232; doi:10.1039/D2CE01506D

data_7245923
_publ_section_title
;
 Double butterfly-shaped octanuclear dysprosium clusters: structure,
 magnetism and assembly mechanism
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              225
_journal_page_last               232
_journal_paper_doi               10.1039/D2CE01506D
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C84 H122 Dy8 N16 O40, 12(C H4 O)'
_chemical_formula_sum            'C92 H158.39 Dy8 N18 O52'
_chemical_formula_weight         3648.75
_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     iterative
_audit_creation_date             2022-11-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-11-04 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                82.531(2)
_cell_angle_beta                 75.268(2)
_cell_angle_gamma                82.046(2)
_cell_formula_units_Z            1
_cell_length_a                   14.1647(4)
_cell_length_b                   14.3993(3)
_cell_length_c                   16.7338(4)
_cell_measurement_reflns_used    25165
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.4940
_cell_measurement_theta_min      2.7360
_cell_volume                     3253.05(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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   -122.00 -16.00   0.50    4.50    --  -43.05 -23.00 -85.00  212
  2  \w    -29.00  37.00   0.50    4.50    --  -43.05  23.00  79.00  132
  3  \w     16.00 124.00   0.50    4.50    --   43.05  23.00  79.00  216
  4  \w   -171.00 -63.00   0.50   11.00    --  -90.25 -23.00 -85.00  216
  5  \w     82.00 178.00   0.50   11.00    --  109.26  23.00  79.00  192
  6  \w    -60.00 -21.00   0.50    4.50    --  -43.05  57.00  30.00   78
  7  \w    -41.00  33.00   0.50    4.50    --  -43.05  37.00 150.00  148
  8  \w    -19.00  28.00   0.50    4.50    --  -43.05  57.00  30.00   94
  9  \w    -27.00  37.00   0.50    4.50    --  -43.05  19.00 -90.00  128
 10  \w    -86.00 -41.00   0.50    4.50    --  -43.05 125.00-180.00   90
 11  \w     44.00  96.00   0.50    4.50    --   43.05-125.00-180.00  104
 12  \w    -28.00  -2.00   0.50    4.50    --   43.05 -23.00 -85.00   52
 13  \w    -49.00 -18.00   0.50   11.00    --  -90.25  45.00  60.00   62
 14  \w    -57.00 -23.00   0.50   11.00    --  -90.25  61.00 -90.00   68
 15  \w    -55.00 -16.00   0.50   11.00    --  -90.25  77.00-150.00   78
 16  \w   -106.00 -64.00   0.50   11.00    --  -90.25  77.00-150.00   84
 17  \w    -59.00 -27.00   0.50   11.00    --  -90.25  61.00  90.00   64
 18  \w    -65.00 -23.00   0.50   11.00    --  -90.25  61.00 -60.00   84
 19  \w     36.00  69.00   0.50   11.00    --  109.26-125.00 150.00   66
 20  \w     58.00  86.00   0.50   11.00    --  109.26-156.00 -48.11   56
 21  \w     40.00 104.00   0.50   11.00    --  109.26 -94.00  30.00  128
 22  \w     37.00  70.00   0.50   11.00    --  109.26 -61.00-180.00   66
 23  \w     75.00 167.00   0.50   11.00    --  109.26   0.00-120.00  184
 24  \w     33.00  64.00   0.50   11.00    --  109.26   0.00-120.00   62
 25  \w     57.00 100.00   0.50   11.00    --  109.26 -94.00 -60.00   86
 26  \w     87.00 159.00   0.50   11.00    --  109.26  45.00-180.00  144
 27  \w     71.00  99.00   0.50   11.00    --  109.26 -94.00 150.00   56
 28  \w     35.00  60.00   0.50   11.00    --  109.26 -61.00-120.00   50
 29  \w     35.00  60.00   0.50   11.00    --  109.26 -61.00  90.00   50
 30  \w     87.00 178.00   0.50   11.00    --  109.26  45.00 150.00  182
 31  \w     34.00 107.00   0.50   11.00    --  109.26-106.00  23.38  146
 32  \w     45.00  73.00   0.50   11.00    --  109.26 -94.00  60.00   56
 33  \w    115.00 143.00   0.50   11.00    --  109.26  77.00 -60.00   56
 34  \w     81.00 107.00   0.50   11.00    --  109.26-105.00-105.08   52
 35  \w     37.00 108.00   0.50   11.00    --  109.26-125.00 -30.00  142
 36  \w     37.00  84.00   0.50   11.00    --  109.26-125.00  30.00   94
 37  \w     43.00  69.00   0.50   11.00    --  109.26 -61.00 150.00   52
 38  \w     84.00 111.00   0.50   11.00    --  109.26  77.00 -60.00   54
 39  \w     97.00 177.00   0.50   11.00    --  109.26 125.00-150.00  160
 40  \w     41.00 104.00   0.50   11.00    --  109.26 -77.00 120.00  126
 41  \w     70.00 109.00   0.50   11.00    --  109.26-114.00-109.34   78
 42  \w     82.00 111.00   0.50   11.00    --  109.26-125.00 150.00   58
 43  \w     39.00  77.00   0.50   11.00    --  109.26-105.00-105.08   76
 44  \w     47.00  75.00   0.50   11.00    --  109.26-109.00 -15.62   56
 45  \w     77.00 107.00   0.50   11.00    --  109.26-109.00 -15.62   60
 46  \w     36.00  58.00   0.50   11.00    --  109.26 -61.00  60.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1109783000
_diffrn_orient_matrix_UB_12      -0.0301949000
_diffrn_orient_matrix_UB_13      -0.0289944000
_diffrn_orient_matrix_UB_21      0.0210489000
_diffrn_orient_matrix_UB_22      0.1019069000
_diffrn_orient_matrix_UB_23      0.0010977000
_diffrn_orient_matrix_UB_31      0.0064727000
_diffrn_orient_matrix_UB_32      -0.0221068000
_diffrn_orient_matrix_UB_33      0.0911555000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39484
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.960
_diffrn_reflns_theta_min         2.744
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.866
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_refine_diff_density_max         8.593
_refine_diff_density_min         -11.699
_refine_diff_density_rms         0.432
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         13042
_refine_ls_number_restraints     3166
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.1024
_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^)+(0.1783P)^2^+106.7234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2773
_refine_ls_wR_factor_ref         0.2811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11961
_reflns_number_total             13042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01506d2.cif
_cod_data_source_block           20221027-lfp-lyl-711-6-4_auto
_cod_depositor_comments
'Adding full bibliography for 7245922--7245923.cif.'
_cod_database_code               7245923
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Dy'
_reflns_odcompleteness_completeness 99.84
_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 C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O12-H12
 0.87 with sigma of 0.01
 O9-H9
 0.87 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 H25-H60
 2.1 with sigma of 0.1
 C83-H9
 1.914743 with sigma of 0.02
 C23-H12
 1.917792 with sigma of 0.02
 Dy3-H12
 2.855657 with sigma of 0.02
 Dy1-H9
 2.926511 with sigma of 0.02
 C25-H13
 1.895994 with sigma of 0.02
 Dy3-H13
 2.94855 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O60 \\sim O25 \\sim O24 \\sim O23 \\sim O21 \\sim O22: within 6.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 6.8A
O8 \\sim O11 \\sim O6 \\sim O4 \\sim O10 \\sim O3 \\sim O1 \\sim O12 \\sim O20
\\sim O5 \\sim O14 \\sim O7 \\sim O2 \\sim O9 \\sim O13 \\sim O18 \\sim O17
\\sim O15 \\sim O25 \\sim O19 \\sim O60 \\sim O22 \\sim O16 \\sim O21 \\sim O23
\\sim O24: within 6.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 6.8A
C35 \\sim C75 \\sim C41 \\sim C37 \\sim C84 \\sim C71 \\sim C53 \\sim C39 \\sim
C27 \\sim C19 \\sim C9 \\sim C73 \\sim C5 \\sim C77 \\sim C81 \\sim C12 \\sim
C20 \\sim C14 \\sim C36 \\sim C16 \\sim C26 \\sim C28 \\sim C32 \\sim C24 \\sim
C34 \\sim C30 \\sim C18 \\sim C38 \\sim C22 \\sim C40 \\sim C42 \\sim C51 \\sim
C83 \\sim C45 \\sim C13 \\sim C21 \\sim C80 \\sim C3 \\sim C76 \\sim C49 \\sim
C82 \\sim C25 \\sim C43 \\sim C11 \\sim C23 \\sim C74 \\sim C8 \\sim C1: within
6.1A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 6.1A
Uanis(C35) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C77) \\sim Ueq,
Uanis(C81) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C74)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Dy1) \\sim Ueq, Uanis(Dy2) \\sim Ueq, Uanis(Dy4) \\sim Ueq, Uanis(Dy3)
\\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of 0.00002
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(N4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq: with sigma of 0.0068 and sigma for terminal atoms of 0.0136
Uanis(C1) \\sim Ueq, Uanis(O24) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O12) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O24) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(N5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Rotating group:
 O10(H10A,H10B)
4.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C24(H24A,H24B), C22(H22A,H22B), C13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C35(H35), C75(H75), C84(H84), C27(H27), C5(H5), C77(H77),
 C81(H81), C20(H20), C14(H14), C36(H36), C16(H16), C32(H32), C30(H30), C40(H40),
  C51(H51), C45(H45)
4.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C83(H83A,H83B,H83C), C21(H21A,H21B,
 H21C), C80(H80A,H80B,H80C), C3(H3A,H3B,H3C), C76(H76A,H76B,H76C), C49(H49A,
 H49B,H49C), C82(H82A,H82B,H82C), C25(H25A,H25B,H25C), C43(H43A,H43B,H43C),
 C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C74(H74A,H74B,H74C), C8(H8A,H8B,H8C),
  C1(H1A,H1B,H1C)
4.e Idealised tetrahedral OH refined as rotating group:
 O25(H25), O60(H60), O22(H22), O21(H21), O23(H23), O24(H24)
;
_shelx_res_checksum              13272
_shelx_hkl_checksum              79527
_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 3.167
_oxdiff_exptl_absorpt_empirical_full_min 0.416