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_7062176
_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         'C91 H67 Cl6 Dy4 N6 O27, 6(C H4 O), C2 H3 N'
_chemical_formula_sum            'C99 H94 Cl6 Dy4 N7 O33'
_chemical_formula_weight         2772.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 100.539(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.0219(7)
_cell_length_b                   19.1466(5)
_cell_length_c                   19.2115(5)
_cell_measurement_reflns_used    21768
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      28.8080
_cell_measurement_theta_min      3.4650
_cell_volume                     10495.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -11.00  45.00   1.00   20.00    --   18.63  77.00  60.00   56
  2  \w     20.00  61.00   1.00   20.00    --   18.63 -99.00-150.00   41
  3  \w    -50.00  34.00   1.00   20.00    --   18.63 -57.00  90.00   84
  4  \w     -3.00  89.00   1.00   20.00    --   18.63  77.00 -60.00   92
  5  \w    -25.00  91.00   1.00   20.00    --   18.63  19.00 -90.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027047000
_diffrn_orient_matrix_UB_12      0.0165535000
_diffrn_orient_matrix_UB_13      0.0335603000
_diffrn_orient_matrix_UB_21      0.0017752000
_diffrn_orient_matrix_UB_22      0.0328351000
_diffrn_orient_matrix_UB_23      -0.0163423000
_diffrn_orient_matrix_UB_31      -0.0246523000
_diffrn_orient_matrix_UB_32      0.0041852000
_diffrn_orient_matrix_UB_33      -0.0044383000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70408
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.335
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.052
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             5468
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.362
_refine_diff_density_min         -3.470
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1366
_refine_ls_number_reflns         20583
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0772
_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^)+(0.0001P)^2^+305.9250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15423
_reflns_number_total             20583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04701b2.cif
_cod_data_source_block           ts20181019_sq
_cod_depositor_comments
'Adding full bibliography for 7062176--7062177.cif.'
_cod_database_code               7062176
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cl1 Dy1'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C55) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C33) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O26(H26), O28(H28A), O32(H32), O33(H33)
3.b Rotating group:
 O25(H25A,H25B), O27(H27A,H27B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C19(H19),
 C20(H20), C21(H21), C23(H23), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35),
  C36(H36), C38(H38), C42(H42), C43(H43), C44(H44), C49(H49), C50(H50),
 C51(H51), C53(H53), C57(H57), C58(H58), C59(H59), C64(H64), C65(H65), C66(H66),
  C68(H68), C72(H72), C73(H73), C74(H74), C79(H79), C80(H80), C81(H81),
 C83(H83), C87(H87), C88(H88), C89(H89)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C60(H60A,H60B,
 H60C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C96(H96A,H96B,H96C), C95(H95A,
 H95B,H95C), C94(H94A,H94B,H94C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C),
 C99(H99A,H99B,H99C), C93(H93A,H93B,H93C)
3.e Idealised tetrahedral OH refined as rotating group:
 O12(H12A), O29(H29A), O31(H31)
;
_shelx_res_checksum              1240
_shelx_fab_checksum              61179
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.505
_oxdiff_exptl_absorpt_empirical_full_min 0.487