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_7059064
_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         '2(C76 H84 Dy2 N6 O8), C2 H3 N'
_chemical_formula_sum            'C154 H171 Dy4 N13 O16'
_chemical_formula_weight         3110.03
_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             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                98.158(3)
_cell_angle_beta                 93.186(3)
_cell_angle_gamma                110.613(4)
_cell_formula_units_Z            2
_cell_length_a                   17.010(3)
_cell_length_b                   20.099(4)
_cell_length_c                   24.220(3)
_cell_measurement_reflns_used    17527
_cell_measurement_temperature    386(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.0
_cell_volume                     7622(2)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0599
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77624
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.999
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.763
_refine_diff_density_min         -4.005
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1722
_refine_ls_number_reflns         26235
_refine_ls_number_restraints     398
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0788
_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^)+(0.1379P)^2^+70.1336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2298
_refine_ls_wR_factor_ref         0.2397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20275
_reflns_number_total             26235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04260a2.cif
_cod_data_source_block           3
_cod_database_code               7059064
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.595
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H16C,H16D,H16E} of C164, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  {H13A,H13B,H13C} of C130, {H13D,H13E,H13F} of C131, {H13G,H13H,H13I} of
  C132, {H13J,H13K,H13L} of C133, {H13M,H13N,H13O} of C139, {H14A,H14B,H14C} of
  C140, {H14D,H14E,H14F} of C141, {H66A,H66B,H66C} of C66, {H54A,H54B,H54C} of
  C54, {H65A,H65B,H65C} of C65, {H36A,H36B,H36C} of C36, {H57A,H57B,H57C} of
  C57, {H64A,H64B,H64C} of C64, {H67A,H67B,H67C} of C67, {H68A,H68B,H68C} of
  C68, {H74A,H74B,H74C} of C74, {H56A,H56B,H56C} of C56, {H55A,H55B,H55C} of
  C55, {H63A,H63B,H63C} of C63, {H18A,H18B,H18C} of C18, {H15I,H15J,H15K} of
  C152, {H14G,H14H,H14I} of C142, {H14J,H14K,H14L} of C143, {H14M,H14N,H14O} of
  C144, {H15C,H15D,H15E} of C150, {H15F,H15G,H15H} of C151, {H11C,H11D,H11E} of
  C112, {H94A,H94B,H94C} of C94, {H76A,H76B,H76C} of C76, {H75A,H75B,H75C} of
  C75
2. Restrained distances
 C152-C149
 1.54 with sigma of 0.02
 C149-C150
 1.54 with sigma of 0.02
 C149-C151
 1.54 with sigma of 0.02
 C151-C152
 2.54 with sigma of 0.02
 C151-C150
 2.54 with sigma of 0.02
 C150-C152
 2.54 with sigma of 0.02
 H136-H14F
 2.2 with sigma of 0.02
3. Rigid bond restraints
 N6, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C149 \\sim C150 \\sim C151 \\sim C152: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C16A \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15A: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C140 \\sim C138 \\sim C141 \\sim C139: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89)
\\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(C93) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C145) \\sim Ueq, Uanis(C151) \\sim Ueq, Uanis(C149) \\sim Ueq,
Uanis(C150) \\sim Ueq, Uanis(C152) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(C141)
\\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C81) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C110) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C164) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C133) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C135) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15A) \\sim Ueq,
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C139) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C163) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C76) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C131) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=1-FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 O8(H8), O16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C35(H35A,H35B), C53(H53A,H53B), C93(H93A,H93B), C111(H11A,
 H11B), C129(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8A), C9(H9), C10(H10), C12(H12), C13(H13),
 C15A(H15A), C16A(H16A), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
 C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C39(H39), C40(H40), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51), C52(H52),
 C60(H60), C71(H71), C79(H79), C80(H80), C83(H83), C84(H84), C85(H85), C86(H86),
  C88(H88), C89(H89), C91(H91), C92(H92), C97(H97), C98(H98), C101(H101),
 C102(H102), C103(H103), C104(H104), C106(H106), C107(H107), C109(H109),
 C110(H110), C115(H115), C116(H116), C119(H119), C120(H120), C121(H121),
 C122(H122), C124(H124), C125(H125), C127(H127), C128(H128), C136(H136),
 C147(H147), C15B(H15B), C16B(H16B)
6.d Fitted hexagon refined as free rotating group:
 C29(C30,C31,C32,C33,C34)
6.e Idealised Me refined as rotating group:
 C18(H18A,H18B,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), C94(H94A,H94B,H94C), C112(H11C,H11D,H11E), C130(H13A,H13B,H13C),
 C131(H13D,H13E,H13F), C132(H13G,H13H,H13I), C133(H13J,H13K,H13L), C139(H13M,
 H13N,H13O), C140(H14A,H14B,H14C), C141(H14D,H14E,H14F), C142(H14G,H14H,H14I),
 C143(H14J,H14K,H14L), C144(H14M,H14N,H14O), C150(H15C,H15D,H15E), C151(H15F,
 H15G,H15H), C164(H16C,H16D,H16E), C152(H15I,H15J,H15K)
;
_shelx_res_checksum              33479
_shelx_fab_checksum              62158
_olex2_submission_special_instructions 'No special instructions were received'