Linear trinuclear and tetranuclear Ln(III) compounds aggregated by multidentate Schiff base ligands: insights into the magnetocaloric effect, slow magnetic relaxation behavior and catalytic CO<sub>2</sub> conversion.
Guan, Xiao-Fen; Qiao, Na; Wu, Zhi-Lei; Wang, Wen-Min; Cui, Jian-Zhong; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12841–12848; doi:10.1039/d5dt01252j

data_7719139
_publ_section_title
;
 Linear trinuclear and tetranuclear Ln(III) compounds aggregated by
 multidentate Schiff base ligands: insights into the magnetocaloric
 effect, slow magnetic relaxation behavior and catalytic CO<sub>2</sub>
 conversion.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12841
_journal_page_last               12848
_journal_paper_doi               10.1039/d5dt01252j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C104 H79 Dy3 N8 O17, C2 Cl2'
_chemical_formula_sum            'C106 H79 Cl2 Dy3 N8 O17'
_chemical_formula_weight         2295.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2025-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.635(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.3707(12)
_cell_length_b                   16.0273(10)
_cell_length_c                   12.6854(8)
_cell_measurement_reflns_used    5534
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.40
_cell_volume                     4636.5(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0719
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38911
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.439
_diffrn_reflns_theta_min         2.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.525
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0930 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.3659.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             2278
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.074
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.206
_refine_ls_abs_structure_details
;
 Flack x determined using 3011 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9506
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                7834
_reflns_number_total             9506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01252j2.cif
_cod_data_source_block           mo_0412_17_0m
_cod_depositor_comments
'Adding full bibliography for 7719138--7719141.cif.'
_cod_database_code               7719139
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.463
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C46 \\sim Cl1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: O9(0.5) C45(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C7BA(H7BA), C0BA(H0BA), C0AA(H0AA), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C4AA(H4AA), C12(H12), C40(H40), C44(H44), C43(H43), C42(H42),
 C41(H41), C54(H54), C19(H19), C18(H18), C17(H17), C16(H16), C15(H15), C3(H3),
 C27(H27), C28(H28), C10(H10), C26(H26), C5(H5), C22(H22), C9AA(H9AA), C37(H37),
  C4(H4), C11(H11), C8(H8), C29(H29), C25(H25)
4.c Fitted hexagon refined as free rotating group:
 C35(C30,C31,C32,C33,C34), C40(C39,C44,C43,C42,C41), C20(C19,C18,C17,C16,C15)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              92396
_shelx_hkl_checksum              97433
_olex2_submission_special_instructions 'No special instructions were received'