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_7249401
_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         'C60 H32 Dy2 F18 N6 O12 S6, 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H36 Cl4 Dy2 F18 N6 O12 S6'
_chemical_formula_weight         2058.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-11-04 deposited with the CCDC.	2024-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.4222(5)
_cell_length_b                   22.5632(6)
_cell_length_c                   13.7569(2)
_cell_measurement_reflns_used    5124
_cell_measurement_temperature    297
_cell_measurement_theta_max      29.9617
_cell_measurement_theta_min      2.8639
_cell_volume                     7580.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -8.00   84.00   1.0000   92.7300
omega____ theta____ kappa____ phi______ frames
    -       20.2277   77.0000  -30.0000 92

  2 omega   -8.00   41.00   1.0000   92.7300
omega____ theta____ kappa____ phi______ frames
    -       20.2277   77.0000  -90.0000 49

  3 omega  -40.00  -14.00   1.0000   92.7300
omega____ theta____ kappa____ phi______ frames
    -      -21.3215   77.0000   90.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0256695000
_diffrn_orient_matrix_UB_12      0.0107773000
_diffrn_orient_matrix_UB_13      -0.0163552000
_diffrn_orient_matrix_UB_21      0.0134529000
_diffrn_orient_matrix_UB_22      0.0230371000
_diffrn_orient_matrix_UB_23      -0.0257503000
_diffrn_orient_matrix_UB_31      0.0017697000
_diffrn_orient_matrix_UB_32      -0.0185123000
_diffrn_orient_matrix_UB_33      -0.0415423000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22682
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.870
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.368
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       block
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         7855
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0295P)^2^+8.7182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5243
_reflns_number_total             7855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00748d2.cif
_cod_data_source_block           exp_11491
_cod_depositor_comments
'Adding full bibliography for 7249401--7249403.cif.'
_cod_database_code               7249401
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C11A-C10A
 1.4 with sigma of 0.02
 C9-C10
 1.4 with sigma of 0.02
 C1A-C2A
 1.4 with sigma of 0.02
 C3-C2 = C2-C1
 1.4 with sigma of 0.02
 C4-C3A = C2A-C1A
 1.4 with sigma of 0.02
 C10A-S2A
 2.6 with sigma of 0.02
 C2A-C3A
 1.4 with sigma of 0.02
 C3A-S1A = S1A-C2A
 2.6 with sigma of 0.02
 C9A-C11A
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2A)
\\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(S1A) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(S1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S2, S2A, C9, C9A, C10, C10A, C11, C11A, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, F7A, F8, F8A, F9, F9A, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F1A, F2, F2A, F3, F3A, C7, C7A, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F4A, F5, F5A, F6, F6A, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1, S1A, C1, C1A, C2, C2A, C3, C3A, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(S2A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=1-FVAR(2)
 Sof(S2)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C7A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C8)=FVAR(3)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(4)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(4)
 Sof(S1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=1-FVAR(5)
 Sof(S1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C2(H2), C2A(H2A), C3(H3), C3A(H3A), C6(H6), C9(H9),
 C9A(H9A), C10(H10), C10A(H10A), C11(H11), C11A(H11A), C14(H14), C17(H17),
 C18(H18), C19(H19), C22(H22), C27(H27), C28(H28), C29(H29), C30(H30)
;
_shelx_res_checksum              20882
_shelx_hkl_checksum              75585
_olex2_submission_special_instructions 'No special instructions were received'