Shape-adaptive single-molecule magnetism and hysteresis up to 14 K in oxide clusterfullerenes Dy2O@C72 and Dy2O@C74 with fused pentagon pairs and flexible Dy‒(μ2-O)‒Dy angle
Velkos, Georgios; Yang, Wei; Yao, Yang-Rong; Sudarkova, Svetlana M.; Liu, XinYe; Büchner, Bernd; Avdoshenko, Stanislav M.; Chen, Ning; Popov, Alexey A.; Chemical Science 11 (2020) 4766–4772; doi:10.1039/D0SC00624F

data_1557826
_publ_section_title
;
 Shape-adaptive single-molecule magnetism and hysteresis up to 14 K in
 oxide clusterfullerenes Dy2O@C72 and Dy2O@C74 with fused pentagon pairs
 and flexible Dy--(\m2-O)--Dy angle
;
_journal_issue                   18
_journal_name_full               'Chemical Science'
_journal_page_first              4766
_journal_page_last               4772
_journal_paper_doi               10.1039/D0SC00624F
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C72, Dy2 O, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C120 H56 Dy2 N4 Ni O'
_chemical_formula_weight         1953.39
_chemical_name_systematic        Dy2O@Cs(10528)-C72
_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   geom
_audit_creation_date             2018-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-12-27 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                84.837(2)
_cell_angle_beta                 88.064(2)
_cell_angle_gamma                61.889(2)
_cell_formula_units_Z            2
_cell_length_a                   14.3857(7)
_cell_length_b                   14.7255(6)
_cell_length_c                   19.1301(9)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      68.429
_cell_measurement_theta_min      2.319
_cell_volume                     3559.7(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      119.98
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12960
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.429
_diffrn_reflns_theta_min         2.319
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.910
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1082 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.3039.
The \l/2 correction factor is Not present.
;
_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    1.822
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.992
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         12960
_refine_ls_number_restraints     963
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0953
_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^)+(0.1500P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2726
_refine_ls_wR_factor_ref         0.2800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11767
_reflns_number_total             12960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc00624f2.cif
_cod_data_source_block           a_a_tw
_cod_depositor_comments
;Adding full bibliography for 1557826--1557827.cif.

 Adding full bibliography for 1557826--1557827.cif.
;
_cod_database_code               1557826
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.382
_shelx_estimated_absorpt_t_min   0.268
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.686(5)
 0.314(5)
2. 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
3. Restrained distances
 C23-C22
 1.38 with sigma of 0.02
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C1
 with sigma of 0.02
 C1-C3 \\sim C1-C4 \\sim C2-C4 \\sim C2-C5 \\sim C3-C5
 with sigma of 0.02
 C1-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C8 \\sim C8-C1
 with sigma of 0.02
 C1-C6 \\sim C1-C7 \\sim C5-C7 \\sim C5-C8 \\sim C6-C8
 with sigma of 0.02
 C25-C26 \\sim C26-C10 \\sim C10-C9 \\sim C9-C24 \\sim C24-C25
 with sigma of 0.02
 C25-C10 \\sim C25-C9 \\sim C26-C9 \\sim C26-C24 \\sim C10-C24
 with sigma of 0.02
 C15-C32 \\sim C32-C33 \\sim C33-C34 \\sim C34-C16 \\sim C16-C15
 with sigma of 0.02
 C15-C33 \\sim C15-C34 \\sim C32-C34 \\sim C32-C16 \\sim C33-C16
 with sigma of 0.02
 C20-C38 \\sim C38-C39 \\sim C39-C40 \\sim C40-C21 \\sim C21-C20
 with sigma of 0.02
 C20-C39 \\sim C20-C40 \\sim C38-C40 \\sim C38-C21 \\sim C39-C21
 with sigma of 0.02
 C42-C41 \\sim C41-C59 \\sim C59-C60 \\sim C60-C43 \\sim C43-C42
 with sigma of 0.02
 C42-C59 \\sim C42-C60 \\sim C41-C60 \\sim C41-C43 \\sim C59-C43
 with sigma of 0.02
 C46-C45 \\sim C45-C62 \\sim C62-C63 \\sim C63-C47 \\sim C47-C46
 with sigma of 0.02
 C46-C62 \\sim C46-C63 \\sim C45-C63 \\sim C45-C47 \\sim C62-C47
 with sigma of 0.02
 C70-C58 \\sim C58-C57 \\sim C57-C56 \\sim C56-C69 \\sim C69-C70
 with sigma of 0.02
 C70-C57 \\sim C70-C56 \\sim C58-C56 \\sim C58-C69 \\sim C57-C69
 with sigma of 0.02
 C55-C37 \\sim C37-C36 \\sim C36-C35 \\sim C35-C54 \\sim C54-C55
 with sigma of 0.02
 C55-C36 \\sim C55-C35 \\sim C37-C35 \\sim C37-C54 \\sim C36-C54
 with sigma of 0.02
 C13-C12 \\sim C12-C28 \\sim C28-C29 \\sim C29-C30 \\sim C30-C13
 with sigma of 0.02
 C13-C28 \\sim C13-C29 \\sim C12-C29 \\sim C12-C30 \\sim C28-C30
 with sigma of 0.02
 C65-C64 \\sim C64-C72 \\sim C72-C67 \\sim C67-C66 \\sim C66-C65
 with sigma of 0.02
 C65-C72 \\sim C65-C67 \\sim C64-C67 \\sim C64-C66 \\sim C72-C66
 with sigma of 0.02
 C65-C66 \\sim C66-C51 \\sim C51-C50 \\sim C50-C49 \\sim C49-C65
 with sigma of 0.02
 C65-C51 \\sim C65-C50 \\sim C66-C50 \\sim C66-C49 \\sim C51-C49
 with sigma of 0.02
4. Restrained planarity
 C9, C10, C24, C25, C26
 with sigma of 0.1
 C15, C16, C32, C33, C34
 with sigma of 0.1
 C20, C21, C38, C39, C40
 with sigma of 0.1
 C41, C42, C43, C59, C60
 with sigma of 0.1
 C45, C46, C47, C62, C63
 with sigma of 0.1
 C56, C57, C58, C69, C70
 with sigma of 0.1
 C35, C36, C37, C54, C55
 with sigma of 0.1
 C12, C13, C28, C29, C30
 with sigma of 0.1
 C1, C2, C3, C4, C5
 with sigma of 0.1
 C1, C5, C6, C7, C8
 with sigma of 0.1
 C64, C65, C66, C67, C72
 with sigma of 0.1
 C49, C50, C51, C65, C66
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
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: within
2A with sigma of 0.008 and sigma for terminal atoms of 0.016
Dy1B \\sim Dy2B \\sim Dy3B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
6. Others
 Fixed Sof: Dy1A(0.6) Dy1B(0.75) Dy2A(0.3) Dy2B(0.2) Dy3A(0.1) Dy3B(0.05)
7.a Secondary CH2 refined with riding coordinates:
 C3P(H3PA,H3PB), C6P(H6PA,H6PB), C12P(H12A,H12B), C15P(H15A,H15B), C21P(H21A,
 H21B), C24P(H24A,H24B), C30P(H30A,H30B), C33P(H33A,H33B)
7.b Aromatic/amide H refined with riding coordinates:
 C9P(H9P), C18P(H18P), C27P(H27P), C36P(H36P), C1S(H1S), C2S(H2S), C3S(H3S),
 C4S(H4S), C5S(H5S), C6S(H6S), C7S(H7S), C8S(H8S), C9S(H9S), C10S(H10S),
 C11S(H11S), C12S(H12S)
7.c Idealised Me refined as rotating group:
 C4P(H4PA,H4PB,H4PC), C7P(H7PA,H7PB,H7PC), C13P(H13A,H13B,H13C), C16P(H16A,
 H16B,H16C), C22P(H22A,H22B,H22C), C25P(H25A,H25B,H25C), C31P(H31A,H31B,H31C),
 C34P(H34A,H34B,H34C)
;
_olex2_submission_special_instructions 'No special instructions were received'