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_7059618
_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         'C144 H100 N12 O16 S6 Tb4'
_chemical_formula_sum            'C144 H100 N12 O16 S6 Tb4'
_chemical_formula_weight         3082.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-14 deposited with the CCDC.	2020-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                75.940(17)
_cell_angle_beta                 85.756(19)
_cell_angle_gamma                67.311(15)
_cell_formula_units_Z            1
_cell_length_a                   14.923(3)
_cell_length_b                   15.285(2)
_cell_length_c                   16.316(4)
_cell_measurement_reflns_used    5392
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     3330.0(12)
_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      113.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.969
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41677
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.998
_exptl_absorpt_coefficient_mu    2.260
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.007
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         14821
_refine_ls_number_restraints     736
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9544
_reflns_number_total             14821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01969k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;Adding full bibliography for 7059614--7059618.cif.

 Adding full bibliography for 7059614--7059618.cif.
;
_cod_original_cell_volume        3329.8(12)
_cod_database_code               7059618
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.661
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N4-C25' = N4-C25
 2.4 with sigma of 0.01
 C26-C27 = C26'-C27' = C41-C40
 1.48 with sigma of 0.01
 S2-C25 = S2-C28 = S2'-C25' = S2'-C28' = S3-C39 = S3-C42
 1.72 with sigma of 0.01
 C25-C26 = C27-C28 = C25'-C26' = C27'-C28' = C39-C40 = C41-C42
 1.34 with sigma of 0.01
 C48-C49 = C48'-C49 = C66-C67 = C66-C67' = C24-C25 = C24-C25'
 1.5 with sigma of 0.01
 O8-H8
 0.82 with sigma of 0.02
3. Restrained planarity
 C66, C67', C68', C69', C70', C71', C72'
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C67' \\sim C68'
\\sim C69' \\sim C70' \\sim C71' \\sim C72': within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C43' \\sim C44'
\\sim C45' \\sim C46' \\sim C47' \\sim C48': within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
S2 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim S2' \\sim C25' \\sim C26'
\\sim C27' \\sim C28': within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C42 \\sim C41 \\sim C40: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C67') \\sim Ueq,
Uanis(C68') \\sim Ueq, Uanis(C69') \\sim Ueq, Uanis(C70') \\sim Ueq,
Uanis(C71') \\sim Ueq, Uanis(C72') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C43') \\sim Ueq,
Uanis(C44') \\sim Ueq, Uanis(C45') \\sim Ueq, Uanis(C46') \\sim Ueq,
Uanis(C47') \\sim Ueq, Uanis(C48') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(S2) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(S2') \\sim Ueq, Uanis(C25') \\sim Ueq,
Uanis(C26') \\sim Ueq, Uanis(C27') \\sim Ueq, Uanis(C28') \\sim Ueq, Uanis(S1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(H24A)=Sof(S2')=Sof(C25')=Sof(C26')=Sof(H26')=Sof(C27')=Sof(H27')=
 Sof(C28')=Sof(H28')=1-FVAR(1)
 Sof(H24)=Sof(S2)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=
 Sof(H28)=FVAR(1)
 Sof(C47')=Sof(H47')=Sof(C46')=Sof(H46')=Sof(C45')=Sof(H45')=Sof(C44')=
 Sof(H44')=Sof(C43')=Sof(H43')=Sof(C48')=1-FVAR(2)
 Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 Sof(C47)=Sof(H47)=Sof(C48)=FVAR(2)
 Sof(C67')=Sof(C72')=Sof(H72')=Sof(C71')=Sof(H71')=Sof(C70')=Sof(H70')=
 Sof(C69')=Sof(H69')=Sof(C68')=Sof(H68')=1-FVAR(3)
 Sof(C67)=Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70)=Sof(C71)=
 Sof(H71)=Sof(C72)=Sof(H72)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C69'(H69')
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8A), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24),
 C24(H24A), C26(H26), C27(H27), C28(H28), C26'(H26'), C27'(H27'), C28'(H28'),
 C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C47'(H47'),
 C46'(H46'), C45'(H45'), C44'(H44'), C43'(H43'), C50(H50), C53(H53), C54(H54),
 C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
  C65(H65), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C72'(H72'),
 C71'(H71'), C70'(H70'), C68'(H68')
6.c Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,C48), C47'(C46',C45',C44',C43',C48'), C67(C68,C69,C70,C71,
 C72), C67'(C72',C71',C70',C69',C68')
;
_shelx_res_checksum              45775
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20