Tetranuclear lanthanide complexes showing magnetic refrigeration and single molecule magnet behavior
Yu, Hong; Yang, Jia-Xing; Han, Ju-Qing; Li, Peng-Fei; Hou, Yin-Ling; Wang, Wen-Min; Fang, Ming; New Journal of Chemistry 43 (2019) 8067–; doi:10.1039/C8NJ05109G

data_7058356
_publ_section_title
;
 Tetranuclear lanthanide complexes showing magnetic refrigeration and
 single molecule magnet behavior
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8067
_journal_paper_doi               10.1039/C8NJ05109G
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C136 H104 Gd4 N12 O16, 2(C2 H3 N)'
_chemical_formula_sum            'C140 H110 Gd4 N14 O16'
_chemical_formula_weight         2873.41
_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   mixed
_audit_creation_date             2018-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-07 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                80.276(3)
_cell_angle_beta                 67.618(4)
_cell_angle_gamma                68.757(3)
_cell_formula_units_Z            1
_cell_length_a                   14.9021(8)
_cell_length_b                   15.4352(10)
_cell_length_c                   15.5643(10)
_cell_measurement_reflns_used    8149
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.766
_cell_measurement_theta_min      2.429
_cell_volume                     3083.4(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0711
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35405
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.448
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0876 before and 0.0709 after correction.
The Ratio of minimum to maximum transmission is 0.7851.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.018
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         10790
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0909
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+114.6750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7582
_reflns_number_total             10790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj05109g2.cif
_cod_data_source_block           111_sq
_cod_depositor_comments
'Adding full bibliography for 7058356--7058358.cif.'
_cod_database_code               7058356
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.531
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H8-O8
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C40(H40), C7(H7), C8(H8A), C41(H41), C68(H68), C67(H67), C66(H66), C65(H65),
 C64(H64), C42(H42), C2(H2), C10(H10), C35(H35), C34(H34), C3(H3), C61(H61),
 C54(H54), C56(H56), C58(H58), C25(H25), C1(H1), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C14(H14), C15(H15), C16(H16), C12(H12), C13(H13), C19(H19),
  C18(H18), C26(H26), C39(H39), C57(H57), C48(H48), C47(H47), C46(H46),
 C45(H45), C44(H44), C51(H51), C23(H23), C24(H24), C55(H55)
4.b Fitted hexagon refined as free rotating group:
 C5(C6,C7,C8,C9,C4), C63(C68,C67,C66,C65,C64), C33(C38,C37,C36,C35,C34),
 C27(C28,C29,C30,C31,C32), C14(C15,C16,C11,C12,C13), C17(C22,C21,C20,C19,C18),
 C43(C48,C47,C46,C45,C44)
4.c Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C49(H49A,H49B,H49C), C70(H70A,H70B,H70C)
;
_shelx_res_checksum              39321
_shelx_fab_checksum              24206
_olex2_submission_special_instructions 'No special instructions were received'