‘Windmill’-shaped LnIII4 (LnIII = Gd and Dy) clusters: magnetocaloric effect and single-molecule-magnet behavior
Wang, Wen-Min; Wang, Mei-Jiao; Hao, Sha-Sha; Shen, Qin-Yu; Wang, Mei-Ling; Liu, Qiao-Ling; Guan, Xiao-Fen; Zhang, Xiu-Tang; Wu, Zhi-Lei; New Journal of Chemistry 44 (2020) 4631–4638; doi:10.1039/C9NJ05317D

data_7059324
_publ_section_title
;
 &#x2018;Windmill&#x2019;-shaped LnIII4 (LnIII = Gd and Dy) clusters:
 magnetocaloric effect and single-molecule-magnet behavior
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4631
_journal_page_last               4638
_journal_paper_doi               10.1039/C9NJ05317D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C76 H88 Dy4 N16 O16, 4(C2 H5 O), 4(C H4 O)'
_chemical_formula_sum            'C88 H124 Dy4 N16 O24'
_chemical_formula_weight         2440.02
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-09-07 deposited with the CCDC.	2020-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.9020(14)
_cell_length_b                   26.9020(14)
_cell_length_c                   13.9514(9)
_cell_measurement_reflns_used    5933
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.70
_cell_volume                     10096.9(10)
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1143
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44363
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_min         2.700
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.002
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0770 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.7769.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.990
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1627
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1280P)^2^+167.1380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2116
_refine_ls_wR_factor_ref         0.2783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2784
_reflns_number_total             5175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05317d2.cif
_cod_data_source_block           mo_0111_1_0m
_cod_depositor_comments
;Adding full bibliography for 7059323--7059324.cif.

 Adding full bibliography for 7059323--7059324.cif.
;
_cod_original_cell_volume        10096.9(12)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7059324
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.476
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C16-C15
 1.52 with sigma of 0.02
3. Rigid bond restraints
 O5, C20, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C15, C16, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C22A, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C22B, O6, C22A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O4, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C17, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22A) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22A) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C22B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22A) = Uanis(C22B)
5. Others
 Sof(H6B)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(H6A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C17(H17A,H17B), C15(H15A,H15B)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C4(H4), C3(H3), C10(H10), C11(H11), C13(H13), C20(H20)
6.c Fitted hexagon refined as free rotating group:
 N1(C6,C5,C4,C3,C2), C14(C9,C10,C11,C12,C13)
6.d Tetrahedral OH refined with riding coordinates:
 O6(H6A), O6(H6B)
6.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C16(H16A,H16B,
 H16C), C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F)
6.f Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              19926
_olex2_submission_special_instructions 'No special instructions were received'