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_7719138
_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 Gd3 N8 O17, C H2 Cl2'
_chemical_formula_sum            'C105 H81 Cl2 Gd3 N8 O17'
_chemical_formula_weight         2269.42
_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             2022-11-08
_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                 102.6364(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.3656(6)
_cell_length_b                   16.0110(4)
_cell_length_c                   12.7623(3)
_cell_measurement_reflns_used    9265
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.39
_cell_volume                     4658.8(2)
_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    'XS (Sheldrick, 2008)'
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33515
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.392
_diffrn_reflns_theta_min         2.394
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.242
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.3841.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             2258
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 4120 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         9493
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0423P)^2^+1.4707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                9042
_reflns_number_total             9493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01252j2.cif
_cod_data_source_block           mo_1120_1_0m
_cod_depositor_comments
'Adding full bibliography for 7719138--7719141.cif.'
_cod_database_code               7719138
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.675
_shelx_estimated_absorpt_t_min   0.499
_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
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O9(0.5) C53(0.5) H54A(0.5) H54B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C54(H54A,H54B)
4.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C37(H37), C10(H10), C45(H45), C8(H8), C29(H29), C26(H26), C47(H47),
 C49(H49), C22(H22), C4(H4), C25(H25), C46(H46), C34(H34), C5(H5), C44(H44),
 C33(H33), C40(H40), C48(H48), C42(H42), C32(H32), C12(H12), C28(H28), C27(H27),
  C31(H31), C11(H11), C19(H19), C15(H15), C3(H3), C17(H17), C18(H18), C16(H16),
 C30(H30), C41(H41), C43(H43)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              23570
_shelx_hkl_checksum              62068
_olex2_submission_special_instructions 'No special instructions were received'