Structures, magnetic refrigeration and single molecule-magnet behavior of five rhombus-shaped tetranuclear Ln(iii)-based clusters
Wang, Wen-Min; Huai, Lei; Wang, Xi-Wen; Jiang, Kai-Jun; Shen, Hai-Yun; Gao, Hong-Ling; Fang, Ming; Cui, Jian-Zhong; New Journal of Chemistry 44 (2020) 10266–10274; doi:10.1039/D0NJ01969K

data_7059616
_publ_section_title
;
 Structures, magnetic refrigeration and single molecule-magnet behavior of
 five rhombus-shaped tetranuclear Ln(iii)-based clusters
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10266
_journal_page_last               10274
_journal_paper_doi               10.1039/D0NJ01969K
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C104 H84 Dy4 N12 O16 S6, C2 H3 N'
_chemical_formula_sum            'C106 H87 Dy4 N13 O16 S6'
_chemical_formula_weight         2641.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-12 deposited with the CCDC.	2020-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.649(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.194(3)
_cell_length_b                   12.779(2)
_cell_length_c                   28.304(5)
_cell_measurement_reflns_used    14573
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5362.2(17)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113.15
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53324
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         3.122
_exptl_absorpt_coefficient_mu    2.941
_exptl_absorpt_correction_T_max  0.7192
_exptl_absorpt_correction_T_min  0.5908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2604
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         12167
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0446P)^2^+7.7295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10683
_reflns_number_total             12167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01969k2.cif
_cod_data_source_block           4
_cod_depositor_comments
;Adding full bibliography for 7059614--7059618.cif.

 Adding full bibliography for 7059614--7059618.cif.
;
_cod_original_cell_volume        5362.3(15)
_cod_database_code               7059616
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.591
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C24 = N4-C24'
 1.3 with sigma of 0.01
 C24-C25 = C24'-C25'
 1.45 with sigma of 0.01
 C26'-C27'
 1.42 with sigma of 0.01
 C25'-C26' = C27'-C28'
 1.36 with sigma of 0.01
 S2'-C25' = S2'-C28'
 1.72 with sigma of 0.01
 O8-H8
 0.82 with sigma of 0.02
3. Restrained planarity
 C24', C25', C26', C27', C28', S2'
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(C24') \\sim Ueq,
Uanis(C25') \\sim Ueq, Uanis(C26') \\sim Ueq, Uanis(C27') \\sim Ueq,
Uanis(C28') \\sim Ueq, Uanis(S2') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N7) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C25') = Uanis(C26') = Uanis(C27') = Uanis(C28') = Uanis(S2') = Uanis(C25)
= Uanis(S2) = Uanis(C28) = Uanis(C27) = Uanis(C26)
5. Others
 Sof(S2')=Sof(C24')=Sof(H24')=Sof(C25')=Sof(C26')=Sof(H26')=Sof(C27')=
 Sof(H27')=Sof(C28')=Sof(H28')=1-FVAR(1)
 Sof(S2)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=
 Sof(C28)=Sof(H28)=FVAR(1)
 Fixed Sof: N7(0.5) C53(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C24(H24), C26(H26),
  C27(H27), C28(H28), C24'(H24'), C26'(H26'), C27'(H27'), C28'(H28'), C29(H29),
 C30(H30), C31(H31), C34(H34), C35(H35), C38(H38), C40(H40), C41(H41), C42(H42),
  C45(H45), C50(H50)
6.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,H52B,
 H52C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              41898
_olex2_submission_special_instructions 'No special instructions were received'