Assembly of dysprosium(III) cubanes in metal–organic framework with ecu topology and slow magnetic relaxation
Shao, Dong; Wan, Yi; Yang, Jiong; Zhu, Junlun; Ruan, Zhijun; Shi, Le; Dalton Transactions  (2023) –; doi:10.1039/D3DT03137C

data_7714459
_publ_section_title
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 Assembly of dysprosium(III) cubanes in metal--organic framework with ecu
 topology and slow magnetic relaxation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03137C
_journal_year                    2023
_chemical_formula_moiety         'C32 H20 Dy4 O32, 8.5[C3H7NO]'
_chemical_formula_sum            'C57.5 H79.5 Dy4 N8.5 O40.5'
_chemical_formula_weight         2187.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
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2023-11-07 deposited with the CCDC.	2023-11-13 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 108.984(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.442(4)
_cell_length_b                   21.256(6)
_cell_length_c                   17.195(5)
_cell_measurement_reflns_used    9288
_cell_measurement_temperature    281.00
_cell_measurement_theta_max      26.480
_cell_measurement_theta_min      2.497
_cell_volume                     4646(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      281.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.947
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34784
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.589
_diffrn_reflns_theta_min         1.916
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.263
_exptl_absorpt_correction_T_max  0.0453
_exptl_absorpt_correction_T_min  0.0199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1520 before and 0.1153 after correction.
The Ratio of minimum to maximum transmission is 0.4393.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         9459
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0634P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7113
_reflns_number_total             9459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03137c2.cif
_cod_data_source_block           Dy4MOF
_cod_original_formula_sum        'C57.50 H79.50 Dy4 N8.50 O40.50'
_cod_database_code               7714459
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.640
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O18) \\sim Ueq,
Uanis(O17) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O21)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C15)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) = Uanis(C2) = Uanis(O13) = Uanis(O5)
2. Others
 Sof(H15)=Sof(O13)=Sof(H13A)=1-FVAR(1)
 Sof(H2)=Sof(O5)=Sof(H5)=FVAR(1)
 Fixed Sof: H8(0.5) H9(0.5) H11(0.5) H7(0.5) O2(0.5) H2A(0.5) O17(0.5)
 H17(0.5) O9(0.5) H9A(0.5) O19(0.5) H19(0.5)
3.a Rotating group:
 O3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C13(H13), C7(H7), C15(H15), C2(H2)
3.c Idealised tetrahedral OH refined as rotating group:
 O13(H13A), O7(H7A), O2(H2A), O17(H17), O9(H9A), O19(H19), O5(H5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30347
_shelx_fab_checksum              85291
_olex2_submission_special_instructions 'No special instructions were received'