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_7059615
_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 Er4 N12 O16 S6, 2(C2 H3 N)'
_chemical_formula_sum            'C108 H90 Er4 N14 O16 S6'
_chemical_formula_weight         2701.33
_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                 102.961(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.189(2)
_cell_length_b                   12.7422(19)
_cell_length_c                   28.246(4)
_cell_measurement_reflns_used    9042
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5327.5(13)
_computing_data_collection       'Bruker XSCANS'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.977
_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  0.1515
_diffrn_reflns_av_unetI/netI     0.1425
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.977
_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       -36
_diffrn_reflns_number            46259
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.685
_diffrn_reflns_theta_min         3.125
_exptl_absorpt_coefficient_mu    3.307
_exptl_absorpt_correction_T_max  27.5
_exptl_absorpt_correction_T_min  3.1
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.919
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         12173
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9974
_reflns_number_total             12173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01969k2.cif
_cod_data_source_block           5
_cod_depositor_comments
;Adding full bibliography for 7059614--7059618.cif.

 Adding full bibliography for 7059614--7059618.cif.
;
_cod_original_cell_volume        5327.3(14)
_cod_database_code               7059615
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.558
_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'
 1.29 with sigma of 0.01
 H8-O8
 0.82 with sigma of 0.02
 C24-C25 = C24'-C25'
 1.5 with sigma of 0.01
 S2-C25 = S2-C28 = S2'-C25' = S2'-C28'
 1.72 with sigma of 0.01
 C27-C28 = C27'-C28'
 1.44 with sigma of 0.01
 C25'-C26' = C27'-C28' = C25-C26 = C27-C28
 1.37 with sigma of 0.01
 N7-C53
 1.12 with sigma of 0.01
 N7-C54
 2.66 with sigma of 0.01
 C1AA-C0AA
 1.25 with sigma of 0.02
 C53-C54
 1.25 with sigma of 0.02
 C26'-N2AA_$1
 2.2 with sigma of 0.02
 H26'-N2AA_$1
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C54, C53, N7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(S2') \\sim Ueq, Uanis(C25') \\sim Ueq, Uanis(C26') \\sim Ueq, Uanis(C27')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28') \\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
0.001 and sigma for terminal atoms of 0.002
Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(S2) = Uanis(C25') =
Uanis(S2') = Uanis(C28') = Uanis(C27') = Uanis(C26')
Uanis(N2AA) = Uanis(C1AA) = Uanis(C0AA) = Uanis(C54) = Uanis(C53) = Uanis(N7)
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)
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(N2AA)=Sof(C1AA)=1-FVAR(2)
 Sof(N7)=Sof(C53)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
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), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              2037
_olex2_submission_special_instructions 'No special instructions were received'