Large magnetocaloric effect and remarkable single-molecule-magnet behavior in triangle-assembled LnIII6 clusters
Wang, Wen-Min; Yue, Rong-Xin; Gao, Yu; Wang, Mei-Jiao; Hao, Sha-Sha; Shi, Ying; Kang, Xiao-Min; Wu, Zhi-Lei; New Journal of Chemistry 43 (2019) 16639–; doi:10.1039/C9NJ03921J

data_7058861
_publ_section_title
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 Large magnetocaloric effect and remarkable single-molecule-magnet
 behavior in triangle-assembled LnIII6 clusters
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16639
_journal_paper_doi               10.1039/C9NJ03921J
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C72 H102 Dy6 N10 O30'
_chemical_formula_sum            'C72 H102 Dy6 N10 O30'
_chemical_formula_weight         2562.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-22 deposited with the CCDC.    2019-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                93.0144(19)
_cell_angle_beta                 106.282(2)
_cell_angle_gamma                106.9591(18)
_cell_formula_units_Z            1
_cell_length_a                   11.9121(6)
_cell_length_b                   14.5229(6)
_cell_length_c                   15.2125(8)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.64
_cell_volume                     2390.3(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42796
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.190
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.705
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0903 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.7218.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.851
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         9417
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+6.5898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7508
_reflns_number_total             9417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03921j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7058860--7058861.cif.'
_cod_database_code               7058861
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.559
_shelx_estimated_absorpt_t_min   0.374
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H9_$1-H9_$2
 2.2 with sigma of 0.02
 C36B-C35 \\sim C35-C34B
 with sigma of 0.02
3. Rigid bond restraints
 C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C35 \\sim O15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C35: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C15 \\sim O4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C14 \\sim C15 \\sim O4: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36B) = Uanis(C36A) = Uanis(C34B) = Uanis(C34A)
5. Others
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=1-FVAR(1)
 Sof(C34B)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C36B)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B),
 C33(H33A,H33B), C28(H28A,H28B), C26(H26A,H26B), C15(H15A,H15B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C8(H8), C5(H5), C3(H3), C4(H4), C18(H18), C23(H23), C11(H11),
 C12(H12A), C13(H13)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C), C21(H21A,H21B,H21C), C34B(H34A,H34B,H34C), C36B(H36A,H36B,H36C),
 C34A(H34D,H34E,H34F), C36A(H36D,H36E,H36F)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12)
;
_shelx_res_checksum              90922
_shelx_fab_checksum              85919
_olex2_submission_special_instructions 'No special instructions were received'