Molecular assemblies from linear-shaped Ln<sub>4</sub> clusters to Ln<sub>8</sub> clusters using different β-diketonates: disparate magnetocaloric effects and single-molecule magnet behaviours.
Wang, Wen-Min; Wu, Zhi-Lei; Cui, Jian-Zhong; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12931–12943; doi:10.1039/d1dt01344k

data_7707967
_publ_section_title
;
 Molecular assemblies from linear-shaped Ln<sub>4</sub> clusters to
 Ln<sub>8</sub> clusters using different \b-diketonates: disparate
 magnetocaloric effects and single-molecule magnet behaviours.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12931
_journal_page_last               12943
_journal_paper_doi               10.1039/d1dt01344k
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C57 H49 Dy2 N3 O12), 2[CH4O]'
_chemical_formula_sum            'C116 H106 Dy4 N6 O26'
_chemical_formula_weight         2650.14
_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             2021-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-10 deposited with the CCDC.	2021-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                89.0348(17)
_cell_angle_beta                 89.3377(19)
_cell_angle_gamma                68.0886(18)
_cell_formula_units_Z            2
_cell_length_a                   14.0115(7)
_cell_length_b                   17.0605(7)
_cell_length_c                   23.9794(10)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.32
_cell_volume                     5317.2(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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0630
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            88457
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.854
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0849 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.7855.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.565
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1353
_refine_ls_number_reflns         20932
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+18.9854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15870
_reflns_number_total             20932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01344k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7707966--7707970.cif.'
_cod_database_code               7707967
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.524
_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, All O(H) groups
2. Restrained distances
 O12-H12
 0.87 with sigma of 0.01
 O11-H11
 0.87 with sigma of 0.01
 O24-H24
 0.87 with sigma of 0.01
 O23-H23A
 0.87 with sigma of 0.01
 H22_$1-H11G_$2
 2.2 with sigma of 0.02
 C57-H12
 1.923272 with sigma of 0.02
 Dy1-H12
 3.042226 with sigma of 0.02
 C56-H11
 1.920063 with sigma of 0.02
 Dy8-H11
 2.939982 with sigma of 0.02
 C114-H24
 1.913154 with sigma of 0.02
 Dy3-H24
 3.002584 with sigma of 0.02
 C113-H23A
 1.900674 with sigma of 0.02
 Dy6-H23A
 2.925666 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C87) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C16)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C71(H71), C52(H52), C49(H49), C77(H77), C8(H8), C109(H109), C65(H65),
 C98(H98), C76(H76), C38(H38), C72(H72), C62(H62), C58(H58), C102(H102),
 C90(H90), C105(H105), C33(H33), C35(H35), C5(H5), C92(H92), C68(H68), C47(H47),
  C60(H60), C106(H106), C91(H91), C32(H32), C101(H101), C89(H89), C14(H14),
 C1(H1), C59(H59), C73(H73), C31(H31), C34(H34), C23(H23), C61(H61), C95(H95),
 C48(H48), C83(H83), C20(H20), C75(H75), C107(H107), C15(H15), C100(H100),
 C80(H80), C99(H99), C69(H69), C88(H88), C2(H2), C13(H13), C41(H41), C43(H43),
 C70(H70), C45(H45), C42(H42), C74(H74), C4(H4), C11(H11A), C44(H44), C3(H3),
 C16(H16), C26(H26), C27(H27), C12(H12A), C87(H87), C19(H19), C84(H84),
 C30(H30), C28(H28), C29(H29), C17(H17), C18(H18), C85(H85), C86(H86)
4.b Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C112(H11B,H11C,H11D), C113(H11E,H11F,H11G), C114(H11H,
 H11I,H11J), C57(H57A,H57B,H57C), C56(H56A,H56B,H56C)
4.c Idealised tetrahedral OH refined as rotating group:
 O10(H10), O22(H22)
;
_shelx_res_checksum              82344
_shelx_fab_checksum              5968
_olex2_submission_special_instructions 'No special instructions were received'