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_7707969
_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 Gd8 N30 O46, 6(C H4 O)'
_chemical_formula_sum            'C112 H134 Gd8 N30 O52'
_chemical_formula_weight         3990.47
_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                 94.068(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5068(8)
_cell_length_b                   17.0170(11)
_cell_length_c                   44.979(3)
_cell_measurement_reflns_used    9288
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.646
_cell_measurement_theta_min      2.561
_cell_volume                     11075.6(12)
_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 0.980
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.981
_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       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            88240
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.235
_exptl_absorpt_coefficient_mu    2.419
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0835 before and 0.0579 after correction.
The Ratio of minimum to maximum transmission is 0.8471.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.117
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         21409
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0870P)^2^+4.1868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13734
_reflns_number_total             21409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01344k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7707966--7707970.cif.'
_cod_original_cell_volume        11075.7(12)
_cod_database_code               7707969
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.728
_shelx_estimated_absorpt_t_min   0.572
_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
 O23-H23
 0.87 with sigma of 0.01
 O22-H22
 0.87 with sigma of 0.01
 H24A-H20
 2.2 with sigma of 0.02
 N12-O16
 1.4 with sigma of 0.02
 O21-H21
 0.87 with sigma of 0.01
 C53-H23
 1.901033 with sigma of 0.02
 Gd4-H23
 3.07179 with sigma of 0.02
 C52-H22
 1.921384 with sigma of 0.02
 Gd1-H22
 3.052046 with sigma of 0.02
 C51-H21
 1.971345 with sigma of 0.02
 Gd1-H21
 2.913531 with sigma of 0.02
3. Rigid bond restraints
 O16, N12, C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C55, O25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C39 \\sim N12 \\sim O16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C40 \\sim C39 \\sim N12 \\sim O16 \\sim C38: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O16 \\sim N12 \\sim C39: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O21 \\sim C51: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(N12) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N14(H14), C43(H43), C17(H17), C13(H13), C2(H2A), C33(H33), C47(H47),
 C3(H3), C45(H45), C27(H27), C44(H44), C23(H23A), C35(H35), C7(H7), C15(H15),
 C24(H24), N5(H5), C14(H14A), C37(H37), C34(H34), C4(H4A), C25(H25)
5.b Tetrahedral OH refined with riding coordinates:
 O16(H16)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C), C30(H30A,H30B,
 H30C), C40(H40A,H40B,H40C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C), C51(H51A,
 H51B,H51C), C10(H10A,H10B,H10C), C55(H55A,H55B,H55C)
5.d Idealised tetrahedral OH refined as rotating group:
 O12(H12), O8(H8), O20(H20), O25(H25A), O4(H4), O24(H24A)
;
_shelx_res_checksum              33115
_shelx_fab_checksum              70278
_olex2_submission_special_instructions 'No special instructions were received'