Four tetra-nuclear lanthanide complexes based on 8-hydroxyquinolin derivatives: magnetic refrigeration and single-molecule magnet behaviour
Fang, Ming; Shao, Li-Jun; Shi, Tian-Xing; Chen, Ying-Ying; Yu, Hong; Li, Peng-Fei; Wang, Wen-Min; Zhao, Bin; New Journal of Chemistry 42 (2018) 11847–; doi:10.1039/C8NJ02161A

data_7057496
_publ_section_title
;
 Four tetra-nuclear lanthanide complexes based on 8-hydroxyquinolin
 derivatives: magnetic refrigeration and single-molecule magnet behaviour
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11847
_journal_paper_doi               10.1039/C8NJ02161A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C134 H136 Ho4 N18 O16'
_chemical_formula_sum            'C134 H138 Ho4 N18 O16'
_chemical_formula_weight         2916.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-03-17 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.520(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.1765(13)
_cell_length_b                   17.1770(11)
_cell_length_c                   22.4477(14)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.294
_cell_measurement_theta_min      2.359
_cell_volume                     6727.3(8)
_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      149.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0742
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            82176
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.175
_exptl_absorpt_coefficient_mu    2.393
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1505 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.8300.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.104
_refine_diff_density_min         -1.508
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         11852
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.007
_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^+79.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9818
_reflns_number_total             11852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02161a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7057494--7057497.cif.'
_cod_database_code               7057496
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.515
_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
 H3AA_$1-H2AA_$2
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C13, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C27, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C0AA \\sim C1AA \\sim C3AA: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C2AA \\sim N5AA \\sim C4AA: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C59) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq,
Uanis(C4AA) \\sim Ueq, Uanis(N5AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1AA) = Uanis(C4AA) = Uanis(C3AA)
Uanis(C3AA) = Uanis(C2AA) = Uanis(C1AA) = Uanis(C4AA)
5.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C37(H37), C18(H18), C23(H23), C3(H3), C7(H7), C8(H8A), C31(H31),
 C2(H2), C38(H38), C32(H32), C1(H1), C22(H22), C17(H17), C25(H25), C62(H62),
 C33(H33), C51(H51), C10(H10), C30(H30), C40(H40), C28(H28), C15(H15), C12(H12),
  C13(H13), C14(H14), C29(H29), C1AA(H1AA), C4AA(H4AA), C2AA(H2AA), C3AA(H3AA)
5.b Fitted hexagon refined as free rotating group:
 C15(C11,C12,C13,N3,C14)
5.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C66(H66A,H66B,
 H66C), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C), C46(H46A,H46B,H46C), C58(H58A,
 H58B,H58C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C48(H48A,H48B,H48C),
 C59(H59A,H59B,H59C)
;
_shelx_res_checksum              41929
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20