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_7059602
_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 Er3 N6 O16, 4(C H4 O), 4[CH4O]'
_chemical_formula_sum            'C111 H109 Er3 N6 O24'
_chemical_formula_weight         2412.89
_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                 104.4294(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.5411(15)
_cell_length_b                   17.4414(10)
_cell_length_c                   23.8773(13)
_cell_measurement_reflns_used    9767
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.36
_cell_volume                     10301.2(10)
_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      149.98
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_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  0.0900
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_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       -28
_diffrn_reflns_number            130069
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.090
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.491
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0997 before and 0.0677 after correction.
The Ratio of minimum to maximum transmission is 0.7694.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             4564
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.898
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1233
_refine_ls_number_reflns         19336
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0808P)^2^+50.6938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14025
_reflns_number_total             19336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01172j2.cif
_cod_data_source_block           7
_cod_depositor_comments
;Adding full bibliography for 7059596--7059602.cif.

 Adding full bibliography for 7059596--7059602.cif.
;
_cod_original_cell_volume        10301.1(10)
_cod_database_code               7059602
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.586
_platon_squeeze_special_details
;
A solvent mask was calculated and 282 electrons were
found in a volume of 1007\%A^3 per unit cell.
This is consistent with the presence of 4[CH4O] per Formula Unit
which account for 288 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
 H19A-H18A
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C107, O17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances 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), N5(H5), C57(H57), C29(H29), C73(H73), C10(H10), C89(H89), C36(H36),
 C4(H4), C51(H51), C41(H41), C56(H56), C66(H66), C103(H103), C81(H81), C22(H22),
  C30(H30), C40(H40), C72(H72), C42(H42), C69(H69), C43(H43), C71(H71),
 C24(H24), C17(H17), C58(H58), C85(H85), C102(H102), C25(H25), C84(H84),
 C87(H87), C90(H90), C74(H74), C5(H5A), C59(H59), C19(H19), C70(H70), C48(H48),
 C33(H33), C12(H12), C54(H54), C96(H96), C13(H13), C86(H86), C61(H61), C99(H99),
  C47(H47), C44(H44), C55(H55), C18(H18), C39(H39), C88(H88), C3(H3), C26(H26),
 C101(H101), C32(H32), C8(H8), C78(H78), C76(H76), C27(H27), C100(H100),
 C63(H63), C45(H45), C11(H11), C75(H75), C60(H60), C62(H62), C46(H46), C93(H93),
  C91(H91), C92(H92), C31(H31), C77(H77)
4.c Idealised Me refined as rotating group:
 C105(H10A,H10B,H10C), C107(H10G,H10H,H10I), C104(H10J,H10K,H10L), C106(H10D,
 H10E,H10F)
4.d Idealised tetrahedral OH refined as rotating group:
 O19(H19A), O18(H18A), O17(H17A), O20(H20)
;
_shelx_res_checksum              31463
_shelx_fab_checksum              94187
_olex2_submission_special_instructions 'No special instructions were received'