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_7249402
_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         'C40 H18 Dy2 F36 N8 O14'
_chemical_formula_sum            'C40 H18 Dy2 F36 N8 O14'
_chemical_formula_weight         1843.62
_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             2024-05-04
_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                88.227(6)
_cell_angle_beta                 86.765(6)
_cell_angle_gamma                74.619(7)
_cell_formula_units_Z            2
_cell_length_a                   12.3888(11)
_cell_length_b                   13.7920(10)
_cell_length_c                   18.7166(14)
_cell_measurement_reflns_used    2472
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.8410
_cell_measurement_theta_min      3.3050
_cell_volume                     3078.2(4)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.1704
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20818
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.324
_exptl_absorpt_coefficient_mu    14.462
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)'
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_description       block
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         10861
_refine_ls_number_restraints     1177
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5356
_reflns_number_total             10861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00748d2.cif
_cod_data_source_block           exp_11542
_cod_depositor_comments
'Adding full bibliography for 7249401--7249403.cif.'
_cod_database_code               7249402
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.391
_shelx_estimated_absorpt_t_min   0.356
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C7-C6 \\sim C7-C6A
 with sigma of 0.02
 F9A-C6A \\sim F9-C6 \\sim F7-C6 \\sim F8-C6 \\sim F8A-C6A \\sim F7A-C6A
 with sigma of 0.02
 C12-C11 \\sim C12-C11A
 with sigma of 0.02
 F18-C11 \\sim F17-C11 \\sim F16-C11 \\sim F18A-C11A \\sim F17A-C11A \\sim
F16A-C11A
 with sigma of 0.02
 F1-C1 \\sim F1A-C1A
 with sigma of 0.02
 F2-C1 \\sim F2A-C1A
 with sigma of 0.02
 F3-C1 \\sim F3A-C1A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2
 with sigma of 0.02
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F1-F3 \\sim F1A-F3A
 with sigma of 0.04
 F1-C2 \\sim F1A-C2
 with sigma of 0.04
 F2-F3 \\sim F2A-F3A
 with sigma of 0.04
 F2-C2 \\sim F2A-C2
 with sigma of 0.04
 F3-C2 \\sim F3A-C2
 with sigma of 0.04
 C2-C1 \\sim C2-C1A
 with sigma of 0.02
 F1-C1 \\sim F2-C1 \\sim F3-C1 \\sim F3A-C1A \\sim F2A-C1A \\sim F1A-C1A
 with sigma of 0.02
 F4-C5 \\sim F4A-C5
 with sigma of 0.02
 F5-C5 \\sim F5A-C5
 with sigma of 0.02
 F6-C5 \\sim F6A-C5
 with sigma of 0.02
 F5A-C5 \\sim F5-C5 \\sim F6A-C5 \\sim F6-C5 \\sim F4A-C5 \\sim F4-C5
 with sigma of 0.02
 F31-C36 \\sim F31A-C36 \\sim F32A-C36 \\sim F32-C36 \\sim F33A-C36 \\sim
F33-C36
 with sigma of 0.02
 F34-C40 \\sim F34A-C40 \\sim F36-C40 \\sim F36A-C40 \\sim F35-C40 \\sim
F35A-C40
 with sigma of 0.02
 C9-C10A \\sim C9-C10
 with sigma of 0.02
 F11-C10 \\sim F11A-C10A \\sim F12-C10 \\sim F10-C10 \\sim F10A-C10A \\sim
F12A-C10A
 with sigma of 0.02
 F26A-C31 \\sim F27-C31 \\sim F27A-C31 \\sim F25-C31 \\sim F25A-C31 \\sim
F26-C31
 with sigma of 0.02
 F12A-F10A \\sim F12A-F11A \\sim F11A-F10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim C6 \\sim C6A \\sim F8A \\sim F7A \\sim F9A \\sim C7:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F16 \\sim F17 \\sim F18 \\sim C11 \\sim C11A \\sim F18A \\sim F16A \\sim F17A
\\sim C12: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
F1 \\sim F2 \\sim F3 \\sim C1 \\sim C1A \\sim F1A \\sim F2A \\sim F3A \\sim C2:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F4 \\sim F5 \\sim F6 \\sim C5 \\sim F4A \\sim F6A \\sim F5A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F31 \\sim F32 \\sim F33 \\sim C36 \\sim F33A \\sim F31A \\sim F32A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F34 \\sim F35 \\sim F36 \\sim C40 \\sim F36A \\sim F34A \\sim F35A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F10 \\sim F11 \\sim F12 \\sim C10 \\sim F10A \\sim C10A \\sim F11A \\sim F12A
\\sim C9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
F25 \\sim F26 \\sim F27 \\sim C31 \\sim F27A \\sim F25A \\sim F26A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C7, C6A, F8A, F7A, F9A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C7, F9, C6, F7, F8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C12, C11, F17, F16, F18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C12, C11A, F16A, F18A, F17A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1, F1, F2, F3, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C2, C1A, F1A, F2A, F3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C10, F11, F10, F12, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C10A, C9, F11A, F10A, F12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C6A)=Sof(F8A)=Sof(F7A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C6)=FVAR(1)
 Sof(C11A)=Sof(F18A)=Sof(F16A)=Sof(F17A)=1-FVAR(2)
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(C11)=FVAR(2)
 Sof(C1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C1)=FVAR(3)
 Sof(F4A)=Sof(F6A)=Sof(F5A)=1-FVAR(4)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(4)
 Sof(F33A)=Sof(F31A)=Sof(F32A)=1-FVAR(5)
 Sof(F31)=Sof(F32)=Sof(F33)=FVAR(5)
 Sof(F36A)=Sof(F34A)=Sof(F35A)=1-FVAR(6)
 Sof(F34)=Sof(F35)=Sof(F36)=FVAR(6)
 Sof(F10A)=Sof(C10A)=Sof(F11A)=Sof(F12A)=1-FVAR(7)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C10)=FVAR(7)
 Sof(F27A)=Sof(F25A)=Sof(F26A)=1-FVAR(8)
 Sof(F25)=Sof(F26)=Sof(F27)=FVAR(8)
6.a Riding coordinates:
 O13(H13A,H13B), O14(H14A,H14B)
6.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N8(H8), C3(H3), C8(H8A), C13(H13), C16(H16), C17(H17), C18(H18),
 C23(H23), C24(H24), C25(H25), C28(H28), C33(H33), C38(H38)
;
_shelx_res_checksum              97799
_shelx_hkl_checksum              92644
_olex2_submission_special_instructions 'No special instructions were received'