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_7059062
_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
'C176 H168 Gd4 N12 O16, 2(C H2 Cl2), 8(C2 H3 N)'
_chemical_formula_sum            'C194 H196 Cl4 Gd4 N20 O16'
_chemical_formula_weight         3834.50
_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   mixed
_atom_sites_solution_primary     iterative
_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                117.432(2)
_cell_angle_beta                 90.789(2)
_cell_angle_gamma                104.152(2)
_cell_formula_units_Z            1
_cell_length_a                   16.9504(9)
_cell_length_b                   17.2420(9)
_cell_length_c                   17.9310(9)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.28
_cell_volume                     4461.2(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker XSCANS'
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73617
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.463
_diffrn_reflns_theta_min         2.277
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.595
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0771 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.7715.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.260
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         18364
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0527
_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^)+(0.1049P)^2^+3.7566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13261
_reflns_number_total             18364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04260a2.cif
_cod_data_source_block           4
_cod_database_code               7059062
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.655
_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. Rigid bond restraints
 C63, C65
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C63, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C2AA, C65, C63, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C64 \\sim C65 \\sim C63 \\sim C2AA: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C65) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C88(H88A,H88B)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C38(H38), C81(H81), C37(H37), C33(H33), C35(H35), C9(H9), C87(H87),
 C20(H20), C44(H44), C74(H74), C8(H8A), C61(H61), C80(H80), C3(H3), C42(H42),
 C34(H34), C43(H43), C86(H86), C2(H2), C15(H15), C21(H21), C23(H23), C25(H25),
 C73(H73), C66(H66), C85(H85), C13(H13), C24(H24), C5(H5), C78(H78), C27(H27),
 C12(H12), C30(H30), C11(H11), C26(H26), C70(H70), C76(H76), C31(H31), C22(H22),
  C6(H6), C67(H67), C50(H50), C1(H1), C77(H77), C69(H69), C68(H68)
4.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C54(H54A,H54B,H54C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C89(H89A,H89B,H89C), C57(H57A,H57B,H57C), C95(H95A,H95B,H95C), C45(H45A,
 H45B,H45C), C56(H56A,H56B,H56C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C),
 C65(H65A,H65B,H65C), C63(H63A,H63B,H63C), C93(H93A,H93B,H93C), C91(H91A,H91B,
 H91C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              334
_olex2_submission_special_instructions 'No special instructions were received'