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_7058358
_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 Dy4 N12 O16'
_chemical_formula_sum            'C136 H104 Dy4 N12 O16'
_chemical_formula_weight         2812.31
_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
_audit_creation_date             2018-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-07 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                87.098(2)
_cell_angle_beta                 89.370(3)
_cell_angle_gamma                86.006(2)
_cell_formula_units_Z            1
_cell_length_a                   13.7157(6)
_cell_length_b                   16.2542(8)
_cell_length_c                   17.1198(7)
_cell_measurement_reflns_used    8678
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.27
_cell_volume                     3802.4(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)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.1160
_diffrn_reflns_av_unetI/netI     0.0946
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56611
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.372
_diffrn_reflns_theta_min         2.186
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.998
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0750 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.7984.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_refine_diff_density_max         1.659
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         13934
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8690
_reflns_number_total             13934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj05109g2.cif
_cod_data_source_block           mo_1115_2_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7058356--7058358.cif.'
_cod_database_code               7058358
_shelx_shelxl_version_number     2016/6
_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
 H8-O8
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C67(H67), C61(H61), C30(H30), C68(H68), C42(H42), C64(H64), C48(H48),
 C25(H25), C15(H15), C41(H41), C51(H51), C26(H26), C39(H39), C32(H32), C14(H14),
  C46(H46), C65(H65), C16(H16), C37(H37), C10(H10), C66(H66), C34(H34),
 C31(H31), C36(H36), C17(H17), C23(H23), C0AA(H0AA), C7(H7), C57(H57), C21(H21),
  C58(H58), C47(H47), C33(H33), C5(H5), C20(H20), C35(H35), C54(H54), C4(H4),
 C19(H19), C3(H3), C56(H56), C55(H55), C18(H18), C1(H1), C2(H2)
4.b Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              3954
_shelx_fab_checksum              21362
_olex2_submission_special_instructions 'No special instructions were received'