Asymmetric {Dy4} metallogrid and double-layered {Dy8} cage clusters from carboxylic decorated o-vanillin Schiff bases: syntheses, topological variation, and single molecule magnet behaviors
Wang, Yi-Han; Qin, Yu; Tang, Shen; Teng, Qing-Hu; Zhu, Meng-Meng; Peng, Song; Wang, Kai; Liang, Fu-Pei; New Journal of Chemistry 47 (2023) 2052–2059; doi:10.1039/D2NJ04701B

data_7062177
_publ_section_title
;
 Asymmetric {Dy4} metallogrid and double-layered {Dy8} cage clusters from
 carboxylic decorated o-vanillin Schiff bases: syntheses, topological
 variation, and single molecule magnet behaviors
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2052
_journal_page_last               2059
_journal_paper_doi               10.1039/D2NJ04701B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C134 H100 Cl10 Dy8 N10 O44'
_chemical_formula_sum            'C134 H100 Cl10 Dy8 N10 O44'
_chemical_formula_weight         4208.73
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-23 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                67.554(3)
_cell_angle_beta                 89.584(3)
_cell_angle_gamma                74.827(3)
_cell_formula_units_Z            1
_cell_length_a                   15.3953(5)
_cell_length_b                   16.5545(5)
_cell_length_c                   17.4986(6)
_cell_measurement_reflns_used    8744
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5640
_cell_measurement_theta_min      3.7250
_cell_volume                     3956.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega    4.00   80.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6266   57.0000   90.0000 76

  2 omega  -22.00   89.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6266   19.0000   30.0000 111

  3 omega   24.00   61.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6266  -99.0000  -30.0000 37

  4 omega  -45.00   38.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6266  -57.0000 -150.0000 83

  5 omega  -11.00   34.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6266   77.0000 -180.0000 45

  6 omega  -32.00   -7.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048  -38.0000 -150.0000 25

  7 omega  -32.00   11.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7048  -77.0000  120.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0118137000
_diffrn_orient_matrix_UB_12      -0.0208012000
_diffrn_orient_matrix_UB_13      0.0436344000
_diffrn_orient_matrix_UB_21      0.0464350000
_diffrn_orient_matrix_UB_22      -0.0112350000
_diffrn_orient_matrix_UB_23      -0.0063633000
_diffrn_orient_matrix_UB_31      0.0028021000
_diffrn_orient_matrix_UB_32      0.0421104000
_diffrn_orient_matrix_UB_33      -0.0000505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28554
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.544
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         13900
_refine_ls_number_restraints     1854
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0813P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9960
_reflns_number_total             13900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04701b2.cif
_cod_data_source_block           f-dy-04_sq
_cod_depositor_comments
'Adding full bibliography for 7062176--7062177.cif.'
_cod_original_cell_volume        3956.7(3)
_cod_database_code               7062177
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cl1 Dy1'
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.742
_olex2_refinement_description
;
1. Rigid bond restraints
 C10, C11, C11, C12, C49, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O15, C53, O16, C54, C55, C56, C57, C58, C59, Cl5, N5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.001
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C55 \\sim C54 \\sim C59 \\sim C58
\\sim C57 \\sim C56 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3.8A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 3.8A
O15 \\sim C53 \\sim O16 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim
C59 \\sim Cl5 \\sim N5: within 0A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 0A
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(N5) \\sim Ueq,
Uanis(Cl5) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Dy3) = Uanis(O15)
3.a Riding coordinates:
 C15(H15A,H15B,H15C)
3.b Ternary CH refined with riding coordinates:
 O20(H20), O21(H21), O22(H22)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C12(H12), C18(H18),
 C20(H20A), C21(H21A), C23(H23), C25(H25), C26(H26), C27(H27), C33(H33),
 C35(H35), C36(H36), C38(H38), C40(H40), C41(H41), C42(H42), C49(H49), C50(H50),
  C52(H52), C59(H59), C57(H57), C56(H56), C60(H60), C62(H62), C63(H63), C64(H64)
3.d Fitted hexagon refined as free rotating group:
 C55(C54,C59,C58,C57,C56)
3.e X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B)
3.f Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C67(H67A,H67B,H67C)
;
_shelx_res_checksum              9149
_shelx_fab_checksum              77249
_olex2_submission_special_instructions 'No special instructions were received'