Two LnIII4 (LnIII = Gd and Dy) clusters constructed by 8-hydroxyquinoline schiff base and β-diketonate coligand: Magnetic refrigeration property and single-molecule magnet behavior
Hou, Yin-Ling; Han, Xue; Hu, Xin-Yan; Shen, Jie-Xuan; Wang, Jie; Shi, Ying; Ji, Jia; Hua, Yu-Peng; Wang, Wen-Min; Inorganica Chimica Acta 502 (2020) 119290–; doi:10.1016/j.ica.2019.119290

data_1565469
_publ_section_title
;
 Two LnIII4 (LnIII&#x00A0;=&#x00A0;Gd and Dy) clusters constructed by
 8-hydroxyquinoline schiff base and \b-diketonate coligand: Magnetic
 refrigeration property and single-molecule magnet behavior
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119290
_journal_paper_doi               10.1016/j.ica.2019.119290
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C164 H120 Dy4 N12 O16, 2(C2 H3 N)'
_chemical_formula_sum            'C168 H126 Dy4 N14 O16'
_chemical_formula_weight         3246.82
_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
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 100.2563(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4736(5)
_cell_length_b                   19.6747(7)
_cell_length_c                   24.6633(8)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      2.25
_cell_volume                     6911.0(4)
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0660
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            101908
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.410
_diffrn_reflns_theta_min         2.234
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.211
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0849 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.8669.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.932
_refine_diff_density_min         -2.054
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         14173
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0930P)^2^+37.3910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1834
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10185
_reflns_number_total             14173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119290.cif
_cod_data_source_block           2
_cod_database_code               1565469
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.538
_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
 H53-H38
 2.2 with sigma of 0.02
 H63-H39
 2.2 with sigma of 0.02
 H1-H15
 2.2 with sigma of 0.02
 O9-H9
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C73) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C78)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C66(H66), C56(H56), C62(H62), C72(H72), C18(H18), C12(H12), C71(H71),
 C13(H13), C17(H17), C70(H70), C65(H65), C61(H61), C23(H23), C10(H10), C1(H1),
 C15(H15), C4(H4), C55(H55), C22(H22), C28(H28), C52(H52), C14(H14), C60(H60),
 C11(H11), C25(H25), C24(H24), C39(H39), C63(H63), C2(H2), C75(H75), C53(H53),
 C49(H49), C80(H80), C50(H50), C38(H38), C26(H26), C37(H37), C36(H36), C34(H34),
  C51(H51), C35(H35), C42(H42), C48(H48), C3(H3), C40(H40), C27(H27), C41(H41)
4.b Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C77(H77A,H77B,H77C), C82(H82A,H82B,H82C), C78(H78A,H78B,
 H78C), C83(H83A,H83B,H83C)
;