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_7059061
_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 Gd4 N12 O16, 2(C2 H3 N)'
_chemical_formula_sum            'C160 H180 Gd4 N16 O16'
_chemical_formula_weight         3212.19
_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                 96.0510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7993(5)
_cell_length_b                   21.8519(7)
_cell_length_c                   21.1006(7)
_cell_measurement_reflns_used    9743
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.383
_cell_measurement_theta_min      2.364
_cell_volume                     7702.8(4)
_computing_data_collection       'Bruker SMART'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57254
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.869
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_T_max  27.383
_exptl_absorpt_correction_T_min  2.364
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.399
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         13538
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0358P)^2^+26.1980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11509
_reflns_number_total             13538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04260a2.cif
_cod_data_source_block           1
_cod_database_code               7059061
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.585
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H8-O8
 0.85 with sigma of 0.02
 C1B-C2 \\sim C2-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C67 \\sim C69 \\sim C68 \\sim C66: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) = Uanis(C1B)
4. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H2AA)=Sof(H2AB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C20(H20A,H20B), C38(H38A,H38B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8A), C9(H9), C11(H11), C12(H12), C16(H16),
 C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C29(H29),
  C30(H30), C34(H34), C35(H35), C36(H36), C40(H40), C41(H41), C43(H43),
 C44(H44), C45(H45), C47(H47), C48(H48), C52(H52), C53(H53), C54(H54), C60(H60),
  C71(H71)
5.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C19(H19A,H19B,H19C), C37(H37A,H37B,H37C), 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), C1B(H1BA,H1BB,H1BC), C79(H79A,H79B,H79C)
;
_shelx_res_checksum              55285
_shelx_fab_checksum              96813
_olex2_submission_special_instructions 'No special instructions were received'