Magnetic relaxation in unique nitronyl nitroxide biradical-Ln-Cu chains with Ln-bis(NIT)-Cu-bis(NIT)-Ln units
Han, Jing; Jin, Chaoyi; Wang, Xiao-Tong; Huang, Xiaohui; Song, Hong-Wei; Xie, Junfang; Li, Licun; Dalton Transactions  (2023) –; doi:10.1039/D3DT00752A

data_7712849
_publ_section_title
;
 Magnetic relaxation in unique nitronyl nitroxide biradical-Ln-Cu chains
 with Ln-bis(NIT)-Cu-bis(NIT)-Ln units
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00752A
_journal_year                    2023
_chemical_formula_moiety         'C50 H36 Cu F30 N5 O14 Tb, 1[CHCl3]'
_chemical_formula_sum            'C51 H37 Cl3 Cu F30 N5 O14 Tb'
_chemical_formula_weight         1842.66
_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   geom
_audit_creation_date             2023-04-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-14 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                78.95(3)
_cell_angle_beta                 81.23(3)
_cell_angle_gamma                75.61(3)
_cell_formula_units_Z            2
_cell_length_a                   12.488(3)
_cell_length_b                   12.660(3)
_cell_length_c                   23.659(5)
_cell_measurement_reflns_used    7870
_cell_measurement_temperature    113.0
_cell_measurement_theta_max      27.8545
_cell_measurement_theta_min      1.6826
_cell_volume                     3534.2(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.00
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -115.0000 - 65.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.3829
	          2theta: -24.7171
scan:
	Number of images: 180
	           Slice: -115.0000 - 65.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.3829
	          2theta: -24.7171
scan:
	Number of images: 180
	           Slice: -115.0000 - 65.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.3829
	          2theta: -24.7171
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.1406
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27473
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.682
_exptl_absorpt_coefficient_mu    1.546
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5437
_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 bluish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       block
_exptl_crystal_F_000             1810
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.014
_refine_diff_density_min         -2.177
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         11833
_refine_ls_number_restraints     1125
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.1616
_refine_ls_R_factor_gt           0.1384
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3661
_refine_ls_wR_factor_ref         0.3889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8358
_reflns_number_total             11833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00752a2.cif
_cod_data_source_block           TbCu
_cod_database_code               7712849
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.747
_shelx_estimated_absorpt_t_min   0.654
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H22A-H19C
 2 with sigma of 0.01
 F28A-F30A \\sim F28A-F29A \\sim F30A-F29A \\sim F28B-F30B \\sim F28B-F29B
\\sim F30B-F29B
 with sigma of 0.04
 C39-F28A \\sim C39-C38 \\sim C39-F30A \\sim C39-F29A \\sim C39-F28B \\sim
C39-F30B \\sim C39-F29B
 with sigma of 0.02
3. Rigid bond restraints
 F23, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 F24, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C50 \\sim C29 \\sim C26 \\sim C49 \\sim C39 \\sim C28 \\sim C27 \\sim C25 \\sim
C5 \\sim C14 \\sim C18 \\sim C33 \\sim C6 \\sim C34 \\sim C47 \\sim C7 \\sim
C17 \\sim C44 \\sim C16 \\sim C4 \\sim C13 \\sim C3 \\sim C9 \\sim C38 \\sim
C43 \\sim C42 \\sim C41 \\sim C2 \\sim C12 \\sim C40 \\sim C24 \\sim C30 \\sim
C45 \\sim C36 \\sim C48 \\sim C37 \\sim C46 \\sim C11 \\sim C10 \\sim C8 \\sim
C32 \\sim C22 \\sim C1 \\sim C15 \\sim C23 \\sim C31 \\sim C20 \\sim C19 \\sim
C21 \\sim C35: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
F16 \\sim F18 \\sim F17 \\sim F28A \\sim F30A \\sim F29A \\sim F28B \\sim F30B
\\sim F29B \\sim F24 \\sim F22 \\sim F23 \\sim F22A \\sim F24A \\sim F23A \\sim
F2 \\sim F1: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
Uanis(C34) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C18) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(F16) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F28A)
\\sim Ueq, Uanis(F30A) \\sim Ueq, Uanis(F29A) \\sim Ueq, Uanis(F28B) \\sim Ueq,
Uanis(F30B) \\sim Ueq, Uanis(F29B) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F22A) \\sim Ueq, Uanis(F24A) \\sim Ueq,
Uanis(F23A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(F28B)=Sof(F30B)=Sof(F29B)=1-FVAR(1)
 Sof(F28A)=Sof(F30A)=Sof(F29A)=FVAR(1)
 Sof(F22A)=Sof(F24A)=Sof(F23A)=1-FVAR(2)
 Sof(F24)=Sof(F22)=Sof(F23)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C46(H46), C40(H40), C48(H48), C50(H50), C41(H41), C3(H3), C44(H44),
 C8(H8), C37(H37), C27(H27), C32(H32)
6.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C18(H18A,
 H18B,H18C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 42 electrons were 
found in a volume of 504\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
1[CHCl3] per Asymmetric Unit 
which account for 116 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26745
_shelx_fab_checksum              40957
_olex2_submission_special_instructions 'No special instructions were received'