Dinuclear lanthanide molecular magnetic materials bridged by tetrazine derivatives containing N6 and N8 atom sites display slow magnetic relaxation behavior
Chen, Ji-Tun; Guo, Rui; Zhang, Yi-Quan; Sun, Wen-Bin; CrystEngComm 26 (2024) 6184–6193; doi:10.1039/D4CE00748D

data_7249403
_publ_section_title
;
 Dinuclear lanthanide molecular magnetic materials bridged by tetrazine
 derivatives containing N6 and N8 atom sites display slow magnetic
 relaxation behavior
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6184
_journal_page_last               6193
_journal_paper_doi               10.1039/D4CE00748D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C29 H15 Dy F9 N4 O6 S3'
_chemical_formula_sum            'C29 H15 Dy F9 N4 O6 S3'
_chemical_formula_weight         945.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-11 deposited with the CCDC.	2024-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.144(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.874(3)
_cell_length_b                   10.4191(12)
_cell_length_c                   19.9901(16)
_cell_measurement_reflns_used    1081
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.2530
_cell_measurement_theta_min      4.2610
_cell_volume                     6793.8(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -69.00  10.00   1.00   10.00    --    0.00 -57.00  90.00   79
  2  \w      5.00  33.00   1.00   10.00    --    0.00 -99.00   0.00   28
  3  \w      2.00  65.00   1.00   10.00    --    0.00  57.00-150.00   63
  4  \w     -2.00  73.00   1.00   30.00    --   54.63 -57.00-150.00   75
  5  \w    -10.00  71.00   1.00   30.00    --   54.63 -57.00  30.00   81
  6  \w     46.00 114.00   1.00   30.00    --   54.63  57.00 150.00   68
  7  \w     11.00  74.00   1.00   30.00    --   54.63 -57.00 -60.00   63
  8  \w     50.00  82.00   1.00   30.00    --  109.26 -92.00-150.00   32
  9  \w     44.00 104.00   1.00   30.00    --  109.26 -63.00-150.00   60
 10  \w     41.00 134.00   1.00   30.00    --  109.26 -37.00  90.00   93
 11  \w     42.00 125.00   1.00   30.00    --  109.26 -50.00 -30.00   83
 12  \w     47.00 135.00   1.00   30.00    --  109.26 -37.00 150.00   88
 13  \w     68.00 105.00   1.00   30.00    --  109.26 -63.00   0.00   37
 14  \w     50.00 159.00   1.00   30.00    --  109.26  12.00-180.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0027396000
_diffrn_orient_matrix_UB_12      0.0369554000
_diffrn_orient_matrix_UB_13      0.0739730000
_diffrn_orient_matrix_UB_21      -0.0432020000
_diffrn_orient_matrix_UB_22      0.0549887000
_diffrn_orient_matrix_UB_23      -0.0205280000
_diffrn_orient_matrix_UB_31      -0.0188108000
_diffrn_orient_matrix_UB_32      -0.1322496000
_diffrn_orient_matrix_UB_33      0.0119926000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1363
_diffrn_reflns_av_unetI/netI     0.2258
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11982
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.984
_diffrn_reflns_theta_max         66.984
_diffrn_reflns_theta_min         2.709
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       block
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         6046
_refine_ls_number_restraints     498
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.2320
_refine_ls_R_factor_gt           0.0964
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1018P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2245
_reflns_number_total             6046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00748d2.cif
_cod_data_source_block           exp_11540
_cod_depositor_comments
'Adding full bibliography for 7249401--7249403.cif.'
_cod_database_code               7249403
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.392
_shelx_estimated_absorpt_t_min   0.357
_olex2_refinement_description
;
1. Restrained distances
 C18-C17
 1.4 with sigma of 0.02
 C17A-C18A
 1.4 with sigma of 0.02
 C20-C18A = C19A-C17A
 2.4 with sigma of 0.02
 F2A-C8 = C8-F2
 1.4 with sigma of 0.02
 F1-C8 = C8-F1A
 1.4 with sigma of 0.02
 F3A-C8 = C8-F3
 1.4 with sigma of 0.02
2. Restrained planarity
 C20, C19A, C18A, C17A, S3A
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
S3 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim S3A \\sim C19A \\sim C18A
\\sim C17A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
S2 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim S2A \\sim C11A \\sim C10A \\sim
C9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F1 \\sim F2 \\sim F3 \\sim C8 \\sim F3A \\sim F2A \\sim F1A \\sim C7: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F7 \\sim F8 \\sim F9 \\sim C24 \\sim F8A \\sim F7A \\sim F9A \\sim C23: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F4 \\sim F5 \\sim F6 \\sim C16 \\sim F6A \\sim F5A \\sim F4A \\sim C15: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C22 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Others
 Sof(S3A)=Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17A)=1-FVAR(1)
 Sof(S3)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=FVAR(1)
 Sof(S2A)=Sof(C11A)=Sof(H11A)=Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(H9A)=1-FVAR(2)
 Sof(S2)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=FVAR(2)
 Sof(F3A)=Sof(F2A)=Sof(F1A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
 Sof(F8A)=Sof(F7A)=Sof(F9A)=1-FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(4)
 Sof(F6A)=Sof(F5A)=Sof(F4A)=1-FVAR(5)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(5)
5.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C1(H1), C2(H2), C3(H3), C6(H6), C9(H9), C10(H10), C11(H11),
 C14(H14), C17(H17), C18(H18), C19(H19), C22(H22), C25(H25), C27(H27),
 C19A(H19A), C18A(H18A), C17A(H17A), C11A(H11A), C10A(H10A), C9A(H9A)
;
_shelx_res_checksum              6370
_shelx_hkl_checksum              45068
_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 3.349
_oxdiff_exptl_absorpt_empirical_full_min 0.587