Single molecule magnet behavior and magnetic refrigeration of four tetranuclear lanthanide (Ln = GdIII, TbIII, DyIII) clusters
Yu, Hong; Cao, Jia-Miao; Zhang, Jun-Rui; Li, Rui-Cong; Cheng, Yan; Yang, Chen; Hou, Yin-Ling; Fang, Ming; New Journal of Chemistry 43 (2019) 19429–19436; doi:10.1039/C9NJ04260A

data_7059063
_publ_section_title
;
 Single molecule magnet behavior and magnetic refrigeration of four
 tetranuclear lanthanide (Ln = GdIII, TbIII, DyIII) clusters
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19429
_journal_page_last               19436
_journal_paper_doi               10.1039/C9NJ04260A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C152 H168 N12 O16 Tb4, 4(C2 N)'
_chemical_formula_sum            'C160 H168 N16 O16 Tb4'
_chemical_formula_weight         3206.77
_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   mixed
_audit_creation_date             2019-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-14 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.213(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.876(2)
_cell_length_b                   24.925(3)
_cell_length_c                   19.267(2)
_cell_measurement_reflns_used    15501
_cell_measurement_temperature    386(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     7949.7(16)
_computing_data_collection       'Bruker XSCANS'
_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      386.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            66243
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.034
_exptl_absorpt_coefficient_mu    1.821
_exptl_absorpt_correction_T_max  0.7846
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.162
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         13972
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+48.8227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10398
_reflns_number_total             13972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04260a2.cif
_cod_data_source_block           2
_cod_database_code               7059063
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.659
_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
 O8-H8
 0.85 with sigma of 0.02
 C17-C18
 1.45 with sigma of 0.02
 H15-H18C
 2.2 with sigma of 0.02
 N8-C79
 1.05 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim C10 \\sim C11 \\sim C16 \\sim C15 \\sim C14 \\sim C13 \\sim C12 \\sim
C18 \\sim C17: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C78) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C69) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq,
Uanis(C73) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(N8)
\\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C35(H35A,H35B), C53(H53A,H53B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8A), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28),
  C33(H33), C34(H34), C30(H30), C31(H31), C39(H39), C40(H40), C43(H43),
 C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51), C52(H52), C60(H60),
  C71(H71)
4.c Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16), C32(C33,C34,C29,C30,C31)
4.d Idealised Me refined as rotating group:
 C18(H18B,H18A,H18C), C36(H36A,H36B,H36C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,
 H76C)
;
_shelx_res_checksum              12738
_shelx_fab_checksum              89039
_olex2_submission_special_instructions 'No special instructions were received'