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_7712848
_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 Gd N5 O14, 1[CHCl3;]'
_chemical_formula_sum            'C51 H37 Cl3 Cu F30 Gd N5 O14'
_chemical_formula_weight         1840.99
_chemical_name_systematic        GdCu
_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                78.877(3)
_cell_angle_beta                 81.598(3)
_cell_angle_gamma                75.717(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3499(4)
_cell_length_b                   12.5775(5)
_cell_length_c                   23.4654(9)
_cell_measurement_reflns_used    17333
_cell_measurement_temperature    113
_cell_measurement_theta_max      31.9580
_cell_measurement_theta_min      2.0380
_cell_volume                     3447.2(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_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   -115.00  65.00   1.00    1.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00    1.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00    1.00    --  -25.00  45.00 180.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0101679000
_diffrn_orient_matrix_UB_12      -0.0438904000
_diffrn_orient_matrix_UB_13      0.0225799000
_diffrn_orient_matrix_UB_21      -0.0267882000
_diffrn_orient_matrix_UB_22      0.0392469000
_diffrn_orient_matrix_UB_23      0.0185642000
_diffrn_orient_matrix_UB_31      -0.0522439000
_diffrn_orient_matrix_UB_32      0.0035641000
_diffrn_orient_matrix_UB_33      -0.0102522000
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39071
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.711
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75042
_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.
R(int) was 0.15337 before and 0.09543 after correction. 
;
_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    1.774
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         15025
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11828
_reflns_number_total             15025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00752a2.cif
_cod_data_source_block           GdCu
_cod_database_code               7712848
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.658
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
F24A \\sim F22A \\sim F23A \\sim F23B \\sim F22B \\sim F24B \\sim F28A \\sim
F30A \\sim F29A \\sim F28B \\sim F30B \\sim F29B: within 3A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 3A
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F14A) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F30A) \\sim Ueq,
Uanis(F24A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
2. Others
 Sof(F23B)=Sof(F22B)=Sof(F24B)=Sof(F28B)=Sof(F30B)=Sof(F29B)=Sof(F13A)=
 Sof(F14A)=1-FVAR(1)
 Sof(F14)=Sof(F13)=Sof(F28A)=Sof(F30A)=Sof(F29A)=Sof(F24A)=Sof(F22A)=Sof(F23A)=
 FVAR(1)
3.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)
3.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 92 electrons were 
found in a volume of 745\%A^3^ in 5 voids per unit cell. 
This is consistent with the presence of 
1[CHCl3;] per Formula Unit 
which account for 116 electrons 
per unit cell.
;
_shelx_res_checksum              48126
_shelx_fab_checksum              1853
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.703