High temperature quantum tunnelling of magnetization and thousand kelvin anisotropy barrier in a Dy<sub>2</sub> single-molecule magnet.
Wu, Haipeng; Li, Min; Xia, Zhengqiang; Montigaud, Vincent; Cador, Olivier; Le Guennic, Boris; Ke, Hongshan; Wang, Wenyuan; Xie, Gang; Chen, Sanping; Gao, Shengli; Chemical communications (Cambridge, England) 57 (2021) 371–374; doi:10.1039/d0cc06993k

data_7127474
_publ_section_title
;
 High temperature quantum tunnelling of magnetization and thousand kelvin
 anisotropy barrier in a Dy<sub>2</sub> single-molecule magnet.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              371
_journal_page_last               374
_journal_paper_doi               10.1039/d0cc06993k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C72 H132 Dy2 I6 O4 P4, 3(C7 H8)'
_chemical_formula_sum            'C100 H164 Dy2 I6 O4 P4'
_chemical_formula_weight         2640.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-17 deposited with the CCDC.	2020-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.442(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6886(10)
_cell_length_b                   28.4973(18)
_cell_length_c                   23.6204(14)
_cell_measurement_reflns_used    9485
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      68.288
_cell_measurement_theta_min      3.624
_cell_volume                     10541.2(11)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      152.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            225120
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.310
_diffrn_reflns_theta_min         3.101
_exptl_absorpt_coefficient_mu    22.215
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.2519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1318 before and 0.0761 after correction. The Ratio of minimum to maximum transmission is 0.3345. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       block
_exptl_crystal_F_000             5224
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.626
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         19267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+13.7872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18271
_reflns_number_total             19267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06993k2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7127474.cif.'
_cod_database_code               7127474
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.176
_shelx_estimated_absorpt_t_min   0.125
_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.a Ternary CH refined with riding coordinates:
 C25(H25), C37(H37), C67(H67), C43(H43), C13(H13), C55(H55), C61(H61),
 C49(H49), C31(H31), C19(H19), C7(H7), C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C72(H72A,H72B), C56(H56A,H56B), C60(H60A,H60B), C68(H68A,
 H68B), C50(H50A,H50B), C41(H41A,H41B), C24(H24A,H24B), C36(H36A,H36B),
 C42(H42A,H42B), C30(H30A,H30B), C48(H48A,H48B), C66(H66A,H66B), C71(H71A,H71B),
  C54(H54A,H54B), C70(H70A,H70B), C3(H3A,H3B), C47(H47A,H47B), C40(H40A,H40B),
 C2(H2A,H2B), C69(H69A,H69B), C18(H18A,H18B), C38(H38A,H38B), C14(H14A,H14B),
 C51(H51A,H51B), C65(H65A,H65B), C6(H6A,H6B), C26(H26A,H26B), C11(H11A,H11B),
 C12(H12A,H12B), C15(H15A,H15B), C59(H59A,H59B), C4(H4A,H4B), C57(H57A,H57B),
 C63(H63A,H63B), C20(H20A,H20B), C44(H44A,H44B), C32(H32A,H32B), C45(H45A,H45B),
  C17(H17A,H17B), C8(H8A,H8B), C5(H5A,H5B), C10(H10A,H10B), C29(H29A,H29B),
 C9(H9A,H9B), C39(H39A,H39B), C58(H58A,H58B), C46(H46A,H46B), C33(H33A,H33B),
 C64(H64A,H64B), C16(H16A,H16B), C23(H23A,H23B), C53(H53A,H53B), C28(H28A,H28B),
  C35(H35A,H35B), C52(H52A,H52B), C27(H27A,H27B), C21(H21A,H21B), C34(H34A,
 H34B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C86(H86), C82(H82), C83(H83), C84(H84), C85(H85), C89(H89), C93(H93),
 C75(H75), C90(H90), C92(H92), C91(H91), C79(H79), C76(H76), C78(H78), C77(H77)
2.d Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C87(H87A,H87B,H87C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              49389
_shelx_fab_checksum              64969
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20