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_7059601
_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 H78 Gd3 N6 O16, 2(C H4 O), 2[CH4O], 3[CH2Cl2]'
_chemical_formula_sum            'C110 H100 Cl6 Gd3 N6 O20'
_chemical_formula_weight         2510.5
_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
_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                 94.078(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9051(11)
_cell_length_b                   26.5476(18)
_cell_length_c                   24.844(2)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.50
_cell_volume                     11121.5(14)
_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)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.970
_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  0.1256
_diffrn_reflns_av_unetI/netI     0.1158
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            73511
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.085
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0788 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.8343.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.685
_refine_diff_density_min         -1.459
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         21245
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1290P)^2^+10.9735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.2303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11990
_reflns_number_total             21245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01172j2.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 7059596--7059602.cif.

 Adding full bibliography for 7059596--7059602.cif.
;
_cod_original_formula_sum        'C110 H100 Gd3 N6 O20 Cl6'
_cod_database_code               7059601
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.658
_platon_squeeze_special_details
;
A solvent mask was calculated and 636 electrons were
found in a volume of 2847\%A^3 in 1 voids per unit cell.
This is consistent with the presence of 2[CH4O] and 3[CH2Cl2] per Formula Unit
which account for 648 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
3. Uiso/Uaniso restraints and constraints
C100 \\sim C101 \\sim C102: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C99 \\sim C98 \\sim C103: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C103) \\sim Ueq, Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C102) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\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), C96(H96A,H96B), C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N2(H2), C59(H59), C62(H62), C76(H76), C60(H60), C56(H56), C88(H88),
 C55(H55), C77(H77), C63(H63), C87(H87), C58(H58), C54(H54), C31(H31), C40(H40),
  C18(H18), C36(H36), C10(H10), C61(H61), C71(H71), C27(H27), C41(H41),
 C39(H39), C24(H24), C43(H43), C26(H26), C78(H78), C19(H19), C25(H25), C22(H22),
  C30(H30), C57(H57), C84(H84), C72(H72), C66(H66), C69(H69), C81(H81),
 C42(H42), C29(H29), C13(H13), C75(H75), C51(H51), C8(H8), C48(H48), C92(H92),
 C70(H70), C89(H89), C12(H12), C91(H91), C74(H74), C4(H4), C17(H17), C5(H5A),
 C45(H45), C85(H85), C33(H33), C32(H32), C44(H44), C73(H73), C93(H93), C86(H86),
  C11(H11), C90(H90), C3(H3), C46(H46), C47(H47), C102(H102), C101(H101),
 C100(H100), C99(H99), C103(H103)
4.c Fitted hexagon refined as free rotating group:
 C102(C101,C100,C99,C98,C103)
4.d Idealised Me refined as rotating group:
 C105(H10A,H10B,H10C), C104(H10D,H10E,H10F)
4.e Idealised tetrahedral OH refined as rotating group:
 O18(H18A), O17(H17A)
;
_shelx_res_checksum              87719
_shelx_fab_checksum              61435
_olex2_submission_special_instructions 'No special instructions were received'