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_1565468
_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 Gd4 N12 O16, 2(C2 H3 N)'
_chemical_formula_sum            'C168 H126 Gd4 N14 O16'
_chemical_formula_weight         3225.82
_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                 100.2417(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4655(5)
_cell_length_b                   19.6990(9)
_cell_length_c                   24.7036(10)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.39
_cell_volume                     6927.3(5)
_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      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1171
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            110008
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.231
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.8369.
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             3232
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.385
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         13646
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0860P)^2^+27.7150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1784
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8963
_reflns_number_total             13646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119290.cif
_cod_data_source_block           1
_cod_database_code               1565468
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.572
_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
 O8-H8
 0.82 with sigma of 0.02
 H1-H15
 2.2 with sigma of 0.02
 H15-H1
 2.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C66(H66), C42(H42), C47(H47), C37(H37), C36(H36), C18(H18),
 C46(H46), C39(H39), C72(H72), C41(H41), C24(H24), C65(H65), C80(H80), C70(H70),
  C62(H62), C38(H38), C71(H71), C14(H14), C25(H25), C17(H17), C34(H34),
 C48(H48), C75(H75), C22(H22), C3(H3), C15(H15), C49(H49), C63(H63), C35(H35),
 C50(H50), C52(H52), C26(H26), C1(H1), C4(H4), C58(H58), C51(H51), C28(H28),
 C11(H11), C27(H27), C61(H61), C60(H60), C10(H10), C59(H59), C13(H13), C2(H2),
 C12(H12)
4.b Idealised Me refined as rotating group:
 C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C77(H77A,H77B,H77C), C83(H83A,H83B,
 H83C), C73(H73A,H73B,H73C)
;