‘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_7059323
_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 Gd4 N16 O16, 4(C H4 O)'
_chemical_formula_sum            'C80 H104 Gd4 N16 O20'
_chemical_formula_weight         2238.79
_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
_audit_creation_date             2018-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_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                   26.8502(16)
_cell_length_b                   26.8502(16)
_cell_length_c                   16.7797(12)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.65
_cell_volume                     12097.0(13)
_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)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1102
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50215
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.387
_diffrn_reflns_theta_min         2.086
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.220
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0967 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.7061.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.863
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0930P)^2^+91.4390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3694
_reflns_number_total             6153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05317d2.cif
_cod_data_source_block           mo_0428_3_0m_sq
_cod_depositor_comments
;Adding full bibliography for 7059323--7059324.cif.

 Adding full bibliography for 7059323--7059324.cif.
;
_cod_original_cell_volume        12097.0(17)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7059323
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.575
_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
2. Restrained distances
 C16-C15
 1.5 with sigma of 0.02
 N4-C16
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16 \\sim C15 \\sim N4: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C17(H17A,H17B), C15(H15A,H15B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C13(H13), C11(H11), C10(H10), C4(H4)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C16(H16A,H16B,
 H16C)
4.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              26135
_shelx_fab_checksum              74590
_olex2_submission_special_instructions 'No special instructions were received'