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_7059614
_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 Gd4 N12 O16 S6, C2 H3 N'
_chemical_formula_sum            'C106 H87 Gd4 N13 O16 S6'
_chemical_formula_weight         2620.24
_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                 102.116(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.115(5)
_cell_length_b                   12.699(4)
_cell_length_c                   28.477(9)
_cell_measurement_reflns_used    7068
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     5344(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0932
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_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       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            51638
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.595
_diffrn_reflns_theta_min         3.140
_exptl_absorpt_coefficient_mu    2.636
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.428
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         12314
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0763
_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^)+(0.0780P)^2^+22.3270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7934
_reflns_number_total             12314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01969k2.cif
_cod_data_source_block           2
_cod_depositor_comments
;Adding full bibliography for 7059614--7059618.cif.

 Adding full bibliography for 7059614--7059618.cif.
;
_cod_database_code               7059614
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.621
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C40 = C41-C42 = C39'-C40' = C41'-C42'
 1.35 with sigma of 0.01
 S3-C39 = S3-C42 = S3'-C39' = S3'-C42'
 1.72 with sigma of 0.01
 C38-C39 = C38'-C39' = C40-C41 = C40'-C41'
 1.45 with sigma of 0.01
 N6-C38 = N6-C38'
 1.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C38') \\sim Ueq,
Uanis(S3') \\sim Ueq, Uanis(C39') \\sim Ueq, Uanis(C40') \\sim Ueq, Uanis(C41')
\\sim Ueq, Uanis(C42') \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42) = Uanis(S3) = Uanis(C39') =
Uanis(C40') = Uanis(C41') = Uanis(C42') = Uanis(S3')
4. Others
 Sof(C38')=Sof(H38')=Sof(S3')=Sof(C39')=Sof(C40')=Sof(H40')=Sof(C41')=
 Sof(H41')=Sof(C42')=Sof(H42')=1-FVAR(1)
 Sof(C38)=Sof(H38)=Sof(S3)=Sof(C39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=
 Sof(C42)=Sof(H42)=FVAR(1)
 Fixed Sof: N7(0.5) C53(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
5.a Riding coordinates:
 C48(H48A,H48B,H48C)
5.b Ternary CH refined with riding coordinates:
 O8(H8)
5.c 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), C26(H26),
  C27(H27), C28(H28), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C38'(H38'), C40'(H40'), C41'(H41'),
 C42'(H42'), C45(H45), C50(H50)
5.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C52(H52A,H52B,H52C), C54(H54A,H54B,
 H54C)
;
_shelx_res_checksum              21547
_olex2_submission_special_instructions 'No special instructions were received'