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_7707970
_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 Ho2 N3 O12), 2[CH4O]'
_chemical_formula_sum            'C116 H106 Ho4 N6 O26'
_chemical_formula_weight         2659.86
_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                88.946(2)
_cell_angle_beta                 89.287(2)
_cell_angle_gamma                67.992(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0531(7)
_cell_length_b                   17.0946(8)
_cell_length_c                   24.0090(11)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.31
_cell_volume                     5346.4(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      150.0
_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  0.0716
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            85156
_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         26.021
_diffrn_reflns_theta_min         2.300
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0865 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.7943.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1353
_refine_ls_number_reflns         21016
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+10.7926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15503
_reflns_number_total             21016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01344k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7707966--7707970.cif.'
_cod_original_cell_volume        5346.5(4)
_cod_database_code               7707970
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.447
_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
 O23-H23A
 0.87 with sigma of 0.01
 O24-H24A
 0.87 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O11-H11
 0.87 with sigma of 0.01
 C113-H23A
 1.921856 with sigma of 0.02
 Ho3-H23A
 3.053637 with sigma of 0.02
 C114-H24A
 1.924774 with sigma of 0.02
 Ho4-H24A
 2.955226 with sigma of 0.02
 C57-H12
 1.921453 with sigma of 0.02
 Ho1-H12
 3.025658 with sigma of 0.02
 C56-H11
 1.903633 with sigma of 0.02
 Ho2-H11
 2.951144 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C25 \\sim C20 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C23 \\sim C22 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C99) \\sim Ueq, Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C64(H64), C44(H44), C85(H85), C7(H7), C45(H45), C75(H75), C68(H68), C3(H3),
 C14(H14), C62(H62), C90(H90), C15(H15), C86(H86), C41(H41), C27(H27), C83(H83),
  C48(H48), C105(H105), C40(H40), C28(H28), C11(H11A), C26(H26), C30(H30),
 C51(H51), C82(H82), C36(H36), C29(H29), C102(H102), C33(H33), C4(H4A),
 C72(H72), C13(H13), C60(H60), C5(H5), C87(H87), C39(H39), C21(H21), C61(H61),
 C71(H71), C37(H37), C43(H43), C69(H69), C84(H84), C97(H97), C54(H54), C42(H42),
  C52(H52), C55(H55), C38(H38), C112(H112), C18(H18), C95(H95), C93(H93),
 C70(H70), C94(H94), C108(H108), C53(H53), C12(H12A), C98(H98), C96(H96),
 C78(H78), C109(H109), C101(H101), C81(H81), C79(H79), C110(H110), C22(H22),
 C80(H80), C25(H25), C111(H111), C100(H100), C99(H99), C23(H23), C24(H24)
4.b Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C10(H10A,H10B,H10C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C113(H11B,H11C,H11D), C114(H11E,H11F,H11G)
4.c Idealised tetrahedral OH refined as rotating group:
 O22(H22A), O4(H4)
;
_shelx_res_checksum              69736
_shelx_fab_checksum              71596
_olex2_submission_special_instructions 'No special instructions were received'