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_7060014
_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 Gd6 N8 O32, 3[C2H3N], 2[CH4O]'
_chemical_formula_sum            'C70 H95 Gd6 N11 O34'
_chemical_formula_weight         2578.08
_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             2020-09-16
_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                90
_cell_angle_beta                 90.532(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4727(6)
_cell_length_b                   19.6943(9)
_cell_length_c                   16.4655(7)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.377
_cell_measurement_theta_min      2.502
_cell_volume                     4693.0(4)
_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      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58285
_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         26.414
_diffrn_reflns_theta_min         2.410
_exptl_absorpt_coefficient_mu    4.251
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1194 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.6684.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       block
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.295
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         9621
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0489P)^2^+17.4626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7596
_reflns_number_total             9621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03442h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7060014--7060015.cif.'
_cod_database_code               7060014
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.404
_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
 O11-H11
 0.85 with sigma of 0.02
 C31-H13
 1.922476 with sigma of 0.02
 Gd1-H13
 2.967842 with sigma of 0.02
3. Rigid bond restraints
 O16, N4, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N4, O14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
O16 \\sim N4 \\sim O14: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C3(H3), C12(H12A), C5(H5), C28(H28), C23(H23), C11(H11A),
 C18(H18), C4(H4)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C16(H16A,H16B,
 H16C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C25(H25A,H25B,H25C), C20(H20A,
 H20B,H20C)
;
_shelx_res_checksum              73745
_shelx_fab_checksum              7072
_olex2_submission_special_instructions 'No special instructions were received'