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_7712850
_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 Dy F30 N5 O14, 1[CHCl3]'
_chemical_formula_sum            'C51 H37 Cl3 Cu Dy F30 N5 O14'
_chemical_formula_weight         1846.24
_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
_atom_sites_solution_primary     dual
_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                78.869(2)
_cell_angle_beta                 81.766(2)
_cell_angle_gamma                75.581(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3381(3)
_cell_length_b                   12.5691(3)
_cell_length_c                   23.3482(6)
_cell_measurement_reflns_used    24262
_cell_measurement_temperature    113.00
_cell_measurement_theta_max      32.8630
_cell_measurement_theta_min      1.7420
_cell_volume                     3423.50(15)
_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      113.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    2.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00    2.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00    2.00    --  -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      0.0208319000
_diffrn_orient_matrix_UB_12      -0.0540482000
_diffrn_orient_matrix_UB_13      0.0154873000
_diffrn_orient_matrix_UB_21      -0.0263217000
_diffrn_orient_matrix_UB_22      0.0176833000
_diffrn_orient_matrix_UB_23      0.0267016000
_diffrn_orient_matrix_UB_31      -0.0493179000
_diffrn_orient_matrix_UB_32      -0.0159796000
_diffrn_orient_matrix_UB_33      -0.0039412000
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.713
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73563
_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 0.17429 before and 0.09295 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    1.791
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.782
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         15659
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+2.1015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13407
_reflns_number_total             15659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00752a2.cif
_cod_data_source_block           DyCu
_cod_database_code               7712850
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.637
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 C20-C18 = C20-C18A = C20-C19 = C20-C19A
 1.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F16B \\sim F18A \\sim F18B \\sim F17A \\sim F17B \\sim F16A \\sim F26B \\sim
F27B \\sim C18 \\sim C18A \\sim C19 \\sim C19A \\sim F19A \\sim F19B \\sim F20A
\\sim F20B \\sim F21A \\sim F21B \\sim C18A \\sim C18: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uanis(F18A) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F19B) \\sim Ueq,
Uanis(C18A) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 Sof(F19B)=Sof(F20B)=Sof(F21B)=1-FVAR(1)
 Sof(F19A)=Sof(F21A)=Sof(F20A)=FVAR(1)
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C18A)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=1-FVAR(2)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 FVAR(2)
 Sof(F18B)=Sof(F16B)=Sof(F17B)=1-FVAR(3)
 Sof(F16A)=Sof(F18A)=Sof(F17A)=FVAR(3)
 Sof(F27B)=Sof(F26B)=1-FVAR(4)
 Sof(F26A)=Sof(F27A)=FVAR(4)
4.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C50(H50), C46(H46), C48(H48), C44(H44), C40(H40), C3(H3), C8(H8),
 C41(H41), C27(H27), C32(H32), C37(H37)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C19A(H19D,H19E,H19F), C18A(H18D,H18E,H18F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 86 electrons were 
found in a volume of 500\%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.
;
_shelx_res_checksum              8147
_shelx_fab_checksum              90801
_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 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.643