Tetranuclear lanthanide complexes showing magnetic refrigeration and single molecule magnet behavior
Yu, Hong; Yang, Jia-Xing; Han, Ju-Qing; Li, Peng-Fei; Hou, Yin-Ling; Wang, Wen-Min; Fang, Ming; New Journal of Chemistry 43 (2019) 8067–; doi:10.1039/C8NJ05109G

data_7058357
_publ_section_title
;
 Tetranuclear lanthanide complexes showing magnetic refrigeration and
 single molecule magnet behavior
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8067
_journal_paper_doi               10.1039/C8NJ05109G
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C136 H104 N12 O16 Tb4, 2(C2 H3 N)'
_chemical_formula_sum            'C140 H110 N14 O16 Tb4'
_chemical_formula_weight         2880.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-07 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                80.272(3)
_cell_angle_beta                 67.467(3)
_cell_angle_gamma                68.699(2)
_cell_formula_units_Z            1
_cell_length_a                   14.9151(7)
_cell_length_b                   15.4503(8)
_cell_length_c                   15.5107(8)
_cell_measurement_reflns_used    8082
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.43
_cell_volume                     3074.1(3)
_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      293(2)
_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  0.0988
_diffrn_reflns_av_unetI/netI     0.0913
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50754
_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         26.418
_diffrn_reflns_theta_min         2.430
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.345
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0751 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.8229.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         12629
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0380P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7995
_reflns_number_total             12629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj05109g2.cif
_cod_data_source_block           mo_1122_2_0m
_cod_depositor_comments
'Adding full bibliography for 7058356--7058358.cif.'
_cod_database_code               7058357
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.521
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H4-O4
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C48(H48), C46(H46), C25(H25), C26(H26), C60(H60), C42(H42), C47(H47),
 C51(H51), C41(H41), C23(H23), C49(H49), C30(H30), C32(H32), C18(H18), C63(H63),
  C56(H56), C15(H15), C17(H17), C31(H31), C34(H34), C52(H52), C21(H21),
 C37(H37), C33(H33), C61(H61), C39(H39), C16(H16), C59(H59), C53(H53), C10(H10),
  C14(H14), C9(H9), C50(H50), C36(H36), C19(H19), C66(H66), C35(H35), C62(H62),
 C1(H1), C4(H4A), C3(H3), C7(H7), C20(H20), C2(H2), C5(H5)
4.b Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              17601
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20