Two hexanuclear lanthanide Ln6III clusters featuring remarkable magnetocaloric effect and slow magnetic relaxation behavior
Wang, Wen-Min; Xue, Cai-Long; Jing, Ru-Yi; Ma, Xin; Yang, Lu-Na; Luo, Shu-Chang; Wu, Zhi-Lei; New Journal of Chemistry 44 (2020) 18025–18030; doi:10.1039/D0NJ03442H

data_7060015
_publ_section_title
;
 Two hexanuclear lanthanide Ln6III clusters featuring remarkable
 magnetocaloric effect and slow magnetic relaxation behavior
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18025
_journal_page_last               18030
_journal_paper_doi               10.1039/D0NJ03442H
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C62 H78 Dy6 N8 O32, 3[C2H3N], 2[CH4O]'
_chemical_formula_sum            'C70 H95 Dy6 N11 O34'
_chemical_formula_weight         2609.58
_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             2020-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-21 deposited with the CCDC.	2020-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                91.697(3)
_cell_angle_beta                 114.999(2)
_cell_angle_gamma                116.737(2)
_cell_formula_units_Z            1
_cell_length_a                   14.2565(6)
_cell_length_b                   14.3411(7)
_cell_length_c                   14.4407(7)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.61
_cell_volume                     2300.0(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       '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    'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0506
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38431
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         2.607
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.885
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1014 before and 0.0652 after correction.
The Ratio of minimum to maximum transmission is 0.7030.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_description       block
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.742
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         9035
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0562P)^2^+3.9929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6917
_reflns_number_total             9035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03442h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7060014--7060015.cif.'
_cod_original_cell_volume        2299.99(19)
_cod_database_code               7060015
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.548
_shelx_estimated_absorpt_t_min   0.304
_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
 O13-H13
 0.87 with sigma of 0.01
 O14-O16A
 2 with sigma of 0.02
 H12_$1-O14
 2.2 with sigma of 0.02
 O11-H11
 0.85 with sigma of 0.02
 O9-H11
 2.3 with sigma of 0.02
 C31-H13
 1.91498 with sigma of 0.02
 Dy3-H13
 2.999742 with sigma of 0.02
 O14-N4 \\sim N4-O15
 with sigma of 0.02
 O16B-N4 \\sim N4-O14
 with sigma of 0.02
 O16B-N4 \\sim N4-O15
 with sigma of 0.02
 O16B-N4 \\sim N4-O16A
 with sigma of 0.02
3. Rigid bond restraints
 N4, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O16B, N4, O14, O15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O16B, N4, O14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O14, N4, O16A, O16B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
N4 \\sim O14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N4 \\sim O15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16B) = Uanis(O16A)
5. Others
 Sof(O16B)=1-FVAR(1)
 Sof(O16A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C28(H28), C12(H12A), C11(H11A), C10(H10), C18(H18), C23(H23),
 C8(H8), C5(H5)
6.c Fitted hexagon refined as free rotating group:
 C14(C13,C12,C11,C10,C9)
6.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C25(H25A,H25B,
 H25C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C15(H15A,
 H15B,H15C)
;
_shelx_res_checksum              62116
_shelx_fab_checksum              98030
_olex2_submission_special_instructions 'No special instructions were received'