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_7707966
_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 Gd2 N3 O12), 2[CH4O]'
_chemical_formula_sum            'C116 H106 Gd4 N6 O26'
_chemical_formula_weight         2629.14
_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                89.078(2)
_cell_angle_beta                 89.403(2)
_cell_angle_gamma                68.0660(18)
_cell_formula_units_Z            2
_cell_length_a                   14.0128(6)
_cell_length_b                   17.0735(7)
_cell_length_c                   23.9952(10)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.30
_cell_volume                     5324.5(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 0.998
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            91026
_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         26.458
_diffrn_reflns_theta_min         2.305
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.534
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0861 before and 0.0573 after correction.
The Ratio of minimum to maximum transmission is 0.7684.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.898
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1353
_refine_ls_number_reflns         21943
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+15.0293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16616
_reflns_number_total             21943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01344k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7707966--7707970.cif.'
_cod_database_code               7707966
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.559
_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
 O23-H23
 0.87 with sigma of 0.01
 O24-H24
 0.87 with sigma of 0.01
 H13C_$1-H4_$2
 2.2 with sigma of 0.02
 C139-H12
 1.924117 with sigma of 0.02
 Gd8-H12
 2.938819 with sigma of 0.02
 C56-H11
 1.917717 with sigma of 0.02
 Gd4-H11
 3.050301 with sigma of 0.02
 C148-H23
 1.919149 with sigma of 0.02
 Gd2-H23
 2.9992 with sigma of 0.02
 C112-H24
 1.915551 with sigma of 0.02
 Gd6-H24
 2.916442 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C63(H63), C7(H7), C68(H68), C43(H43), C18(H18), C42(H42), C101(H101),
 C92(H92), C93(H93), C74(H74), C77(H77), C80(H80), C109(H109), C48(H48),
 C71(H71), C26(H26), C97(H97), C5(H5), C96(H96), C104(H104), C107(H107),
 C98(H98), C45(H45), C67(H67), C61(H61), C3(H3), C79(H79), C108(H108), C21(H21),
  C33(H33), C59(H59), C25(H25), C89(H89), C70(H70), C4(H4A), C95(H95),
 C110(H110), C15(H15), C44(H44), C111(H111), C78(H78), C11(H11D), C30(H30),
 C81(H81), C69(H69), C41(H41), C99(H99), C51(H51), C12(H12A), C100(H100),
 C60(H60), C94(H94), C55(H55), C54(H54), C53(H53), C22(H22), C86(H86), C36(H36),
  C52(H52), C23(H23A), C82(H82), C24(H24A), C13(H13), C14(H14), C85(H85),
 C40(H40), C37(H37), C38(H38), C29(H29), C39(H39), C27(H27), C83(H83), C28(H28),
  C84(H84)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C112(H11A,H11B,H11C), C66(H66A,H66B,H66C), C139(H13A,
 H13B,H13C), C148(H14A,H14B,H14C), C56(H56A,H56B,H56C)
4.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O16(H16)
;
_shelx_res_checksum              98549
_shelx_fab_checksum              3489
_olex2_submission_special_instructions 'No special instructions were received'