Metallofullerene single-molecule magnet Dy2O@C2v(5)-C80 with a strong antiferromagnetic Dy···Dy coupling
Velkos, Georgios; Yang, Wei; Yao, Yang-Rong; Sudarkova, Svetlana M.; Liu, Fupin; Avdoshenko, Stanislav; Chen, Ning; Popov, Alexey A.; Chemical Communications  (2022) –; doi:10.1039/D1CC07176A

data_7130158
_publ_section_title
;
 Metallofullerene single-molecule magnet Dy2O@C2v(5)-C80 with a strong
 antiferromagnetic Dy&#x00B7;&#x00B7;&#x00B7;Dy coupling
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07176A
_journal_year                    2022
_chemical_formula_moiety         'Dy0.735 O, 1.232(Dy), C80, C36 H44 N4 Ni'
_chemical_formula_sum            'C116 H44 Dy1.97 N4 Ni O'
_chemical_formula_weight         1888.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc27zt35
_audit_creation_date             2021-12-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.35(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.757(4)
_cell_length_b                   16.954(3)
_cell_length_c                   26.591(5)
_cell_measurement_reflns_used    13387
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.027
_cell_measurement_theta_min      1.444
_cell_volume                     7641(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_unetI/netI     0.0950
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22828
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.407
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         1.444
_exptl_absorpt_coefficient_mu    2.216
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             3737
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
TITL aa P -1 R = 0.16 New: P21/c
CELL   17.7570   16.9540   26.5910     90.00    107.35     90.00
SPGR P21/c
C101 0.249 0.425 0.209 !      16.67 eA-3
C102 0.765 0.095 0.299 !      15.15 eA-3
C103 0.670 0.077 0.148 !       7.11 eA-3
C104 0.598 0.936 0.108 !       6.94 eA-3
C105 0.594 0.079 0.117 !       6.89 eA-3
C106 0.673 0.934 0.139 !       6.39 eA-3
C107 0.289 0.999 0.841 !       6.08 eA-3
C108 0.557 0.012 0.099 !       5.71 eA-3
C109 0.243 0.995 0.708 !       5.26 eA-3
C110 0.757 1.005 0.292 !       5.26 eA-3
C111 0.921 0.997 0.502 !       4.95 eA-3
C112 0.022 0.500 0.949 !       4.44 eA-3
C113 0.053 0.518 0.046 !       3.96 eA-3
Q114 0.083 0.973 0.044 !       3.49 eA-3
Q115 0.250 0.919 0.413 !       2.58 eA-3
Q116 0.601 0.080 0.552 !       2.44 eA-3
Q117 0.737 0.736 0.183 !       1.98 eA-3
Q118 0.808 0.590 0.342 !       1.96 eA-3
Q119 0.405 0.077 0.444 !       1.94 eA-3
Q120 0.782 0.482 0.237 !       1.89 eA-3
Q121 0.504 0.995 0.095 !       1.83 eA-3
Q122 0.427 0.950 0.344 !       1.75 eA-3
Q123 0.114 0.093 0.219 !       1.74 eA-3
Q124 0.630 0.081 0.649 !       1.69 eA-3
C125 0.247 0.960 0.669 !       1.68 eA-3
Q126 0.139 0.971 0.178 !       1.66 eA-3
Q127 0.441 0.434 0.129 !       1.65 eA-3
Q128 0.437 0.576 0.138 !       1.56 eA-3
Q129 0.064 0.469 0.549 !       1.53 eA-3
Q130 0.262 0.800 0.344 !       1.48 eA-3
Q131 0.412 0.314 0.711 !       1.47 eA-3
Q132 0.423 0.492 0.201 !       1.46 eA-3
Q133 0.246 0.973 0.142 !       1.44 eA-3
C134 0.763 0.501 0.632 !       1.44 eA-3
Q135 0.685 0.451 0.152 !       1.44 eA-3
Q136 0.482 0.315 0.822 !       1.41 eA-3
Q137 0.480 0.523 0.069 !       1.36 eA-3
Q138 0.309 0.028 0.448 !       1.35 eA-3
C139 0.232 0.500 0.322 !       1.29 eA-3
Q140 0.614 0.281 0.171 !       1.28 eA-3
Q141 0.321 0.096 0.142 !       1.27 eA-3
Q142 0.660 0.715 0.262 !       1.25 eA-3
Q143 0.512 0.323 0.184 !       1.25 eA-3
C144 0.748 0.496 0.837 !       1.25 eA-3
Q145 0.812 0.699 0.286 !       1.24 eA-3
Q146 0.734 0.298 0.263 !       1.22 eA-3
Q147 0.200 0.374 0.867 !       1.20 eA-3
Q148 0.446 0.486 0.826 !       1.20 eA-3
Q149 0.984 1.001 0.320 !       1.18 eA-3
Q150 0.151 0.849 0.239 !       1.18 eA-3
Q151 0.500 0.857 0.601 !       1.16 eA-3
C152 0.123 0.030 0.716 !       1.13 eA-3
Q153 0.587 0.499 0.462 !       1.10 eA-3
Q154 0.527 0.161 0.600 !       1.05 eA-3
Q155 0.343 0.262 0.773 !       1.05 eA-3
C156 0.998 0.504 0.897 !       1.05 eA-3
Q157 0.331 0.815 0.393 !       1.04 eA-3
Q158 0.904 0.265 0.433 !       1.04 eA-3
Q159 0.737 0.078 0.750 !       1.03 eA-3
Q160 0.065 0.014 0.413 !       1.03 eA-3
C161 0.576 0.626 0.595 !       1.02 eA-3
Q162 0.656 0.264 0.237 !       1.02 eA-3
Q163 0.781 1.001 0.103 !       1.02 eA-3
Q164 0.737 0.326 0.732 !       1.01 eA-3
Q165 0.734 0.926 0.088 !       1.01 eA-3
Q166 0.485 0.888 0.216 !       1.01 eA-3
Q167 0.682 0.550 0.360 !       1.00 eA-3
Q168 0.498 0.124 0.605 !       1.00 eA-3
C169 1.002 0.014 0.500 !       0.99 eA-3
Q170 0.753 0.544 0.594 !       0.98 eA-3
C171 0.878 0.016 0.282 !       0.97 eA-3
Q172 0.248 0.548 0.399 !       0.96 eA-3
Q173 0.802 0.454 0.475 !       0.96 eA-3
Q174 0.905 0.457 0.245 !       0.95 eA-3
Q175 0.342 0.014 0.366 !       0.95 eA-3
Q176 0.189 0.519 0.289 !       0.95 eA-3
Q177 0.334 0.401 0.219 !       0.94 eA-3
Q178 0.986 0.949 0.937 !       0.94 eA-3
Q179 0.176 0.549 0.313 !       0.93 eA-3
C180 0.394 0.506 0.368 !       0.92 eA-3
Q181 0.902 0.534 0.202 !       0.92 eA-3
Q182 0.695 0.121 0.172 !       0.92 eA-3
Q183 0.765 0.365 0.312 !       0.91 eA-3
Q184 0.715 0.502 0.266 !       0.91 eA-3
Q185 0.113 0.594 0.454 !       0.90 eA-3
Q186 0.716 0.503 0.922 !       0.90 eA-3
Q187 0.537 0.453 0.723 !       0.90 eA-3
Q188 0.268 0.473 0.155 !       0.89 eA-3
C189 0.026 0.998 0.632 !       0.89 eA-3
Q190 0.404 0.811 0.378 !       0.89 eA-3
Q191 0.855 0.940 0.974 !       0.88 eA-3
Q192 0.217 0.408 0.081 !       0.88 eA-3
Q193 0.997 0.504 0.140 !       0.88 eA-3
Q194 0.795 0.062 0.454 !       0.88 eA-3
Q195 0.662 0.668 0.103 !       0.88 eA-3
Q196 0.983 0.441 0.109 !       0.87 eA-3
Q197 0.967 0.598 0.406 !       0.86 eA-3
Q198 0.474 0.913 0.733 !       0.86 eA-3
Q199 0.044 0.424 0.560 !       0.85 eA-3
;
_refine_diff_density_max         2.811
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1207
_refine_ls_number_reflns         12494
_refine_ls_number_restraints     1438
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.1613
_refine_ls_R_factor_gt           0.1492
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+110.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3365
_refine_ls_wR_factor_ref         0.3428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11016
_reflns_number_total             12494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07176a2.cif
_cod_data_source_block           aa_sq
_cod_database_code               7130158
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C59-C37
 1.38 with sigma of 0.01
 C73-C56 \\sim C56-C55 \\sim C55-C54 \\sim C54-C72 \\sim C72-C73
 with sigma of 0.02
 C73-C55 \\sim C73-C54 \\sim C56-C54 \\sim C56-C72 \\sim C55-C72
 with sigma of 0.02
 C33-C34 \\sim C34-C14 \\sim C14-C13 \\sim C13-C32 \\sim C32-C33
 with sigma of 0.02
 C33-C14 \\sim C33-C13 \\sim C34-C13 \\sim C34-C32 \\sim C14-C32
 with sigma of 0.02
 C3-C4 \\sim C4-C5 \\sim C5-C1 \\sim C1-C2 \\sim C2-C3
 with sigma of 0.02
 C3-C5 \\sim C3-C1 \\sim C4-C1 \\sim C4-C2 \\sim C5-C2
 with sigma of 0.02
 C19-C40 \\sim C40-C41 \\sim C41-C21 \\sim C21-C20 \\sim C20-C19
 with sigma of 0.02
 C19-C41 \\sim C19-C21 \\sim C40-C21 \\sim C40-C20 \\sim C41-C20
 with sigma of 0.02
 C37-C38 \\sim C38-C17 \\sim C17-C16 \\sim C16-C36 \\sim C36-C37
 with sigma of 0.02
 C37-C17 \\sim C37-C16 \\sim C38-C16 \\sim C38-C36 \\sim C17-C36
 with sigma of 0.02
 C52-C53 \\sim C53-C31 \\sim C31-C30 \\sim C30-C29 \\sim C29-C52
 with sigma of 0.02
 C52-C31 \\sim C52-C30 \\sim C53-C30 \\sim C53-C29 \\sim C31-C29
 with sigma of 0.02
 C76-C60 \\sim C60-C59 \\sim C59-C58 \\sim C58-C75 \\sim C75-C76
 with sigma of 0.02
 C76-C59 \\sim C76-C58 \\sim C60-C58 \\sim C60-C75 \\sim C59-C75
 with sigma of 0.02
 C64-C43 \\sim C43-C42 \\sim C42-C62 \\sim C62-C63 \\sim C63-C64
 with sigma of 0.02
 C64-C42 \\sim C64-C62 \\sim C43-C62 \\sim C43-C63 \\sim C42-C63
 with sigma of 0.02
 C66-C67 \\sim C67-C47 \\sim C47-C46 \\sim C46-C45 \\sim C45-C66
 with sigma of 0.02
 C66-C47 \\sim C66-C46 \\sim C67-C46 \\sim C67-C45 \\sim C47-C45
 with sigma of 0.02
 C25-C8 \\sim C8-C7 \\sim C7-C23 \\sim C23-C24 \\sim C24-C25
 with sigma of 0.02
 C25-C7 \\sim C25-C23 \\sim C8-C23 \\sim C8-C24 \\sim C7-C24
 with sigma of 0.02
 C49-C28 \\sim C28-C27 \\sim C27-C26 \\sim C26-C48 \\sim C48-C49
 with sigma of 0.02
 C49-C27 \\sim C49-C26 \\sim C28-C26 \\sim C28-C48 \\sim C27-C48
 with sigma of 0.02
 C78-C80 \\sim C80-C70 \\sim C70-C69 \\sim C69-C79 \\sim C79-C78
 with sigma of 0.02
 C78-C70 \\sim C78-C69 \\sim C80-C69 \\sim C80-C79 \\sim C70-C79
 with sigma of 0.02
 C65-C64 \\sim C65-C79 \\sim C65-C66
 with sigma of 0.02
 C64-C79 \\sim C79-C66 \\sim C66-C64
 with sigma of 0.02
 C44-C43 \\sim C44-C45 \\sim C44-C22
 with sigma of 0.02
 C43-C45 \\sim C45-C22 \\sim C22-C43
 with sigma of 0.02
 C12-C11 \\sim C12-C2 \\sim C12-C13
 with sigma of 0.02
 C11-C2 \\sim C2-C13 \\sim C13-C11
 with sigma of 0.02
 C18-C19 \\sim C18-C4 \\sim C18-C17
 with sigma of 0.02
 C19-C4 \\sim C4-C17 \\sim C17-C19
 with sigma of 0.02
 C68-C67 \\sim C68-C69 \\sim C68-C50
 with sigma of 0.02
 C67-C69 \\sim C69-C50 \\sim C50-C67
 with sigma of 0.02
 C51-C71 \\sim C51-C52 \\sim C51-C50
 with sigma of 0.02
 C71-C52 \\sim C52-C50 \\sim C50-C71
 with sigma of 0.02
 C61-C60 \\sim C61-C62 \\sim C61-C39
 with sigma of 0.02
 C60-C62 \\sim C62-C39 \\sim C39-C60
 with sigma of 0.02
3. Restrained planarity
 C54, C55, C56, C72, C73
 with sigma of 0.1
 C13, C14, C32, C33, C34
 with sigma of 0.1
 C1, C2, C3, C4, C5
 with sigma of 0.1
 C19, C20, C21, C40, C41
 with sigma of 0.1
 C16, C17, C36, C37, C38
 with sigma of 0.1
 C29, C30, C31, C52, C53
 with sigma of 0.1
 C58, C59, C60, C75, C76
 with sigma of 0.1
 C42, C43, C62, C63, C64
 with sigma of 0.1
 C45, C46, C47, C66, C67
 with sigma of 0.1
 C7, C8, C23, C24, C25
 with sigma of 0.1
 C26, C27, C28, C48, C49
 with sigma of 0.1
 C69, C70, C78, C79, C80
 with sigma of 0.1
4. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64,
  C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79, C80
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1A, N2A, C10A, C30A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Dy1 \\sim Dy2 \\sim Dy3 \\sim Dy4 \\sim Dy5 \\sim Dy6 \\sim Dy7 \\sim Dy8 \\sim
Dy9 \\sim Dy10: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
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 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Dy4) \\sim Ueq, Uanis(Dy8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Others
 1*[Sof(Dy1)]+1*[Sof(Dy3)]+1*[Sof(Dy5)]+1*[Sof(Dy4)]+1*[Sof(Dy2)]+1*[Sof(Dy8)]+
 1*[Sof(Dy7)]+1*[Sof(Dy6)]+1*[Sof(Dy9)]+1*[Sof(Dy10)]=0.0001 with esd of 2
7.a Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C8A(H8AA,H8AB), C14A(H14A,H14B), C17A(H17A,H17B), C23A(H23A,
 H23B), C26A(H26A,H26B), C32A(H32A,H32B), C35A(H35A,H35B)
7.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C11A(H11A), C20A(H20A), C29A(H29A)
7.c Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C9A(H9AA,H9AB,H9AC), C15A(H15A,H15B,H15C), C18A(H18A,
 H18B,H18C), C24A(H24A,H24B,H24C), C27A(H27A,H27B,H27C), C33A(H33A,H33B,H33C),
 C36A(H36A,H36B,H36C)
;
_shelx_res_checksum              80915
_shelx_hkl_checksum              49652
_shelx_fab_checksum              77408
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'