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_7707968
_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         'C106 H110 Dy8 N30 O46, 6(C H4 O)'
_chemical_formula_sum            'C112 H134 Dy8 N30 O52'
_chemical_formula_weight         4032.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 93.5526(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4129(12)
_cell_length_b                   16.7883(14)
_cell_length_c                   43.787(3)
_cell_measurement_reflns_used    9773
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.38
_cell_volume                     10574.7(14)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0419
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            71080
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.224
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0925 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.7254.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.003
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.168
_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     916
_refine_ls_number_reflns         19282
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0589P)^2^+180.6571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15611
_reflns_number_total             19282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01344k2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7707966--7707970.cif.'
_cod_original_cell_volume        10574.7(15)
_cod_database_code               7707968
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O21-H21
 0.85 with sigma of 0.01
 O23-H23
 0.85 with sigma of 0.01
 O22-H22
 0.85 with sigma of 0.01
 H25A-H22
 2.2 with sigma of 0.02
 H8-H30B
 2.2 with sigma of 0.02
 C54-H24A
 1.89 with sigma of 0.02
 C54-O24
 1.45 with sigma of 0.02
 C51-H21
 1.919016 with sigma of 0.02
 Dy1-H21
 3.036668 with sigma of 0.02
 C53-H23
 1.856467 with sigma of 0.02
 Dy4-H23
 3.035946 with sigma of 0.02
 C52-H22
 1.861505 with sigma of 0.02
 Dy4-H22
 2.984452 with sigma of 0.02
3. Rigid bond restraints
 C52, O22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 N8(H8), C45(H45), C23(H23A), C43(H43), N2(H2), C24(H24), C47(H47), C25(H25),
 C44(H44), N5(H5), C3(H3), C33(H33), C14(H14), C37(H37), C27(H27), C17(H17),
 C2(H2A), C7(H7), C12(H12A), C34(H34), C35(H35), C13(H13), C4(H4A)
5.b Tetrahedral OH refined with riding coordinates:
 O12(H12), O16(H16)
5.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C30(H30A,H30B,H30C), C51(H51A,H51B,H51C), C40(H40A,H40B,
 H40C), C53(H53A,H53B,H53C), C20(H20A,H20B,H20C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C10(H10A,H10B,H10C), C52(H52A,H52B,H52C)
5.d Idealised tetrahedral OH refined as rotating group:
 O20(H20), O4(H4), O24(H24A), O8(H8A), O25(H25A)
;
_shelx_res_checksum              58835
_shelx_fab_checksum              63614
_olex2_submission_special_instructions 'No special instructions were received'