Construction of a family of Ln3 clusters using multidentate Schiff base and β-diketonate ligands: fluorescence properties, magnetocaloric effect and slow magnetic relaxation
Wang, Wen-Min; Gao, Yu; Yue, Rong-Xin; Qiao, Na; Wang, Dan-Tong; Shi, Ying; Zhang, Huan; Cui, Jian-Zhong; New Journal of Chemistry 44 (2020) 9230–9237; doi:10.1039/D0NJ01172J

data_7059600
_publ_section_title
;
 Construction of a family of Ln3 clusters using multidentate Schiff base
 and \b-diketonate ligands: fluorescence properties, magnetocaloric effect
 and slow magnetic relaxation
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9230
_journal_page_last               9237
_journal_paper_doi               10.1039/D0NJ01172J
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C103 H77 N6 O16 Tb3, 3(C H4 O), 5[CH4O]'
_chemical_formula_sum            'C111 H109 N6 O24 Tb3'
_chemical_formula_weight         2387.89
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-06 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.714(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1172(19)
_cell_length_b                   17.8025(12)
_cell_length_c                   23.5489(14)
_cell_measurement_reflns_used    9028
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.33
_cell_volume                     10310.6(12)
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0993
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            168853
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.098
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             4456
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.724
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1213
_refine_ls_number_reflns         20227
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0950P)^2^+51.1760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14133
_reflns_number_total             20227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01172j2.cif
_cod_data_source_block           4
_cod_depositor_comments
;Adding full bibliography for 7059596--7059602.cif.

 Adding full bibliography for 7059596--7059602.cif.
;
_cod_database_code               7059600
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.590
_platon_squeeze_special_details
;
A solvent mask was calculated and 356 electrons were
found in a volume of 1464\%A^3 in 2 voids per unit cell.
This is consistent with the presence of 5[CH4O] per Formula Unit
which account for 360 electrons per unit cell.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H5-H19A
 2.2 with sigma of 0.02
 H19A-H18A
 2.2 with sigma of 0.02
 O1-H17A
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C91(H91), N5(H5), C29(H29), C19(H19), C44(H44), C24(H24), C63(H63),
 C66(H66), C58(H58), C84(H84), C103(H103), C39(H39), C46(H46), C69(H69),
 C40(H40), C11(H11), C85(H85), C96(H96), C48(H48), C59(H59), C27(H27), C92(H92),
  C93(H93), C5(H5A), C51(H51), C74(H74), C78(H78), C60(H60), C36(H36), C56(H56),
  C81(H81), C8(H8), C26(H26), C3(H3), C10(H10), C87(H87), C90(H90), C33(H33),
 C25(H25), C47(H47), C45(H45), C102(H102), C89(H89), C17(H17), C75(H75),
 C30(H30), C62(H62), C73(H73), C70(H70), C4(H4), C101(H101), C12(H12), C43(H43),
  C99(H99), C32(H32), C71(H71), C86(H86), C88(H88), C100(H100), C22(H22),
 C76(H76), C41(H41), C13(H13), C61(H61), C72(H72), C77(H77), C31(H31), C55(H55),
  C42(H42), C18(H18), C57(H57), C54(H54)
4.c Idealised Me refined as rotating group:
 C105(H10A,H10B,H10C), C106(H10D,H10E,H10F), C104(H10G,H10H,H10I)
4.d Idealised tetrahedral OH refined as rotating group:
 O18(H18A), O19(H19A), O17(H17A)
;
_shelx_res_checksum              33460
_shelx_fab_checksum              21218
_olex2_submission_special_instructions 'No special instructions were received'