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_7058860
_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 Gd6 N10 O30'
_chemical_formula_sum            'C72 H102 Gd6 N10 O30'
_chemical_formula_weight         2531.13
_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                93.079(2)
_cell_angle_beta                 106.093(2)
_cell_angle_gamma                106.8576(19)
_cell_formula_units_Z            1
_cell_length_a                   11.9049(6)
_cell_length_b                   14.4988(6)
_cell_length_c                   15.2214(7)
_cell_measurement_reflns_used    8935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.64
_cell_volume                     2390.1(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      149.98
_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  0.0957
_diffrn_reflns_av_unetI/netI     0.0735
_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            42084
_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         2.189
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.178
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.7636.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.224
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         9421
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0457P)^2^+3.1371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6767
_reflns_number_total             9421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj03921j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7058860--7058861.cif.'
_cod_original_cell_volume        2390.06(19)
_cod_database_code               7058860
_shelx_shelxl_version_number     2018/3
_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-H9_$1
 2.2 with sigma of 0.02
3. Rigid bond restraints
 O4, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O3, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C35, O15
 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
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\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(C36B) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C34B) \\sim Ueq,
Uanis(C34A) \\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(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=1-FVAR(1)
 Sof(C36B)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C34B)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), N4(H4A,H4B), C30(H30A,H30B), C15(H15A,H15B), C29(H29A,H29B),
 C33(H33A,H33B), C28(H28A,H28B), C32(H32A,H32B), C26(H26A,H26B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C11(H11), C23(H23), C4(H4), C8(H8), C18(H18), C5(H5), C12(H12),
 C3(H3), C13(H13)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C21(H21A,H21B,
 H21C), C25(H25A,H25B,H25C), C36B(H36A,H36B,H36C), C34B(H34A,H34B,H34C),
 C36A(H36D,H36E,H36F), C34A(H34D,H34E,H34F)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12A)
;
_shelx_res_checksum              61051
_shelx_fab_checksum              47880
_olex2_submission_special_instructions 'No special instructions were received'