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_7059596
_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 Nd3 O16, 3(C H4 O), 5[CH4O]'
_chemical_formula_sum            'C111 H109 N6 Nd3 O24'
_chemical_formula_weight         2343.76
_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                 104.600(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3875(18)
_cell_length_b                   17.4829(11)
_cell_length_c                   23.7829(16)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.37
_cell_volume                     10215.1(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      150.0
_diffrn_measured_fraction_theta_full 0.998
_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  0.1091
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            134366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_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    1.571
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.8269.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             4396
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.571
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1200
_refine_ls_number_reflns         20092
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0931P)^2^+30.9517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13838
_reflns_number_total             20092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01172j2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7059596--7059602.cif.

 Adding full bibliography for 7059596--7059602.cif.
;
_cod_database_code               7059596
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.714
_platon_squeeze_special_details
;
A solvent mask was calculated and 364 electrons were
found in a volume of 1410\%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-H17A
 2.2 with sigma of 0.02
 H10I_$1-H10I
 2.2 with sigma of 0.02
 H10I_$2-H10G_$3
 2.15 with sigma of 0.02
3. Rigid bond restraints
 C104, O17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C59, C64, C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C62, C61, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C105, O18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C60 \\sim C61 \\sim C62: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C63 \\sim C64: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C59 \\sim C64 \\sim C63: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C104 \\sim O17: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
O17 \\sim C104: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C105 \\sim O18: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
O18 \\sim C105: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C59) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C15(H15A,H15B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C24(H24), C51(H51), C19(H19), C88(H88), C81(H81), C72(H72),
 C33(H33), C99(H99), C39(H39), C103(H103), C3(H3), C63(H63), C62(H62), C61(H61),
  C60(H60), C59(H59), C73(H73), C100(H100), C71(H71), C66(H66), C55(H55),
 C5(H5A), C102(H102), C96(H96), C10(H10), C69(H69), C85(H85), C77(H77),
 C18(H18), C36(H36), C31(H31), C11(H11), C54(H54), C8(H8), C40(H40), C74(H74),
 C57(H57), C76(H76), C86(H86), C89(H89), C43(H43), C44(H44), C84(H84), C75(H75),
  C32(H32), C13(H13), C70(H70), C26(H26), C93(H93), C27(H27), C22(H22),
 C12(H12), C78(H78), C48(H48), C87(H87), C4(H4), C58(H58), C29(H29), C17(H17),
 C56(H56), C41(H41), C30(H30), C91(H91), C101(H101), C25(H25), C45(H45),
 C46(H46), C47(H47), C42(H42), C92(H92), C90(H90)
5.c Fitted hexagon refined as free rotating group:
 C64(C63,C62,C61,C60,C59)
5.d Tetrahedral OH refined with riding coordinates:
 O18(H18A)
5.e Idealised Me refined as rotating group:
 C106(H10D,H10E,H10F), C105(H10A,H10B,H10C), C104(H10G,H10H,H10I)
5.f Idealised tetrahedral OH refined as rotating group:
 O19(H19A), O17(H17A)
;
_shelx_res_checksum              35878
_shelx_fab_checksum              50130
_olex2_submission_special_instructions 'No special instructions were received'