Single molecule magnet behavior and magnetic refrigeration of carbonyl oxygen-bridged tetranuclear lanthanide complexes
Yang, Chen; Wei, Yu-Heng; Xu, Shuang; Zhang, Hao-Yu; Yang, Yue-Qi; Zhang, Bo; Fang, Ming; New Journal of Chemistry 45 (2021) 14103–14110; doi:10.1039/D1NJ01833G

data_7060796
_publ_section_title
;
 Single molecule magnet behavior and magnetic refrigeration of carbonyl
 oxygen-bridged tetranuclear lanthanide complexes
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14103
_journal_page_last               14110
_journal_paper_doi               10.1039/D1NJ01833G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C64 H64 Gd4 N12 O16, 4(C H4 O)'
_chemical_formula_sum            'C68 H80 Gd4 N12 O20'
_chemical_formula_weight         2014.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-01 deposited with the CCDC.	2021-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.3149(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.8296(8)
_cell_length_b                   8.3601(3)
_cell_length_c                   30.9973(11)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.54
_cell_volume                     7205.6(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_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      150.0
_diffrn_measured_fraction_theta_full 0.998
_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  0.0871
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            50891
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.399
_diffrn_reflns_theta_min         2.249
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.715
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0813 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.7882.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       block
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.856
_refine_diff_density_min         -1.661
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         7389
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5459
_reflns_number_total             7389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01833g2.cif
_cod_data_source_block           mo_1214_9_0m
_cod_depositor_comments
'Adding full bibliography for 7060795--7060797.cif.'
_cod_database_code               7060796
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.383
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C29(H29), C18(H18), C8(H8), C3(H3), C27(H27), C23(H23),
 C14(H14), C12(H12), C26(H26), C5(H5A), C11(H11), C20(H20), C4(H4), C19(H19)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C15(H15A,H15B,H15C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
3.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O8(H8A)
;
_shelx_res_checksum              82128
_olex2_submission_special_instructions 'No special instructions were received'