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_7712851
_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 Ho N5 O14, 1[CHCl3;]'
_chemical_formula_sum            'C51 H37 Cl3 Cu F30 Ho N5 O14'
_chemical_formula_weight         1848.67
_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                78.907(3)
_cell_angle_beta                 81.807(3)
_cell_angle_gamma                75.538(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3457(3)
_cell_length_b                   12.5536(4)
_cell_length_c                   23.3498(8)
_cell_measurement_reflns_used    18129
_cell_measurement_temperature    113.00
_cell_measurement_theta_max      32.5650
_cell_measurement_theta_min      1.6940
_cell_volume                     3421.65(19)
_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 0.996
_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   10.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00   10.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00   10.00    --  -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      0.0099994000
_diffrn_orient_matrix_UB_12      -0.0517765000
_diffrn_orient_matrix_UB_13      0.0192513000
_diffrn_orient_matrix_UB_21      0.0114419000
_diffrn_orient_matrix_UB_22      -0.0285834000
_diffrn_orient_matrix_UB_23      -0.0243810000
_diffrn_orient_matrix_UB_31      0.0576603000
_diffrn_orient_matrix_UB_32      0.0006508000
_diffrn_orient_matrix_UB_33      -0.0016998000
_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  0.0586
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_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       -30
_diffrn_reflns_number            41759
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.698
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74238
_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 0.13206 before and 0.05115 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    1.794
_exptl_crystal_description       block
_exptl_crystal_F_000             1814
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         16457
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0479P)^2^+1.0479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12730
_reflns_number_total             16457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00752a2.cif
_cod_data_source_block           HoCu
_cod_original_cell_volume        3421.6(2)
_cod_database_code               7712851
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.626
_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 2.3A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2.3A
F24A \\sim F22A \\sim F23A \\sim F23B \\sim F24B \\sim F22B \\sim F28A \\sim
F30A \\sim F29A \\sim F28B \\sim F30B \\sim F29B: within 2.5A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2.5A
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F24A) \\sim Ueq, Uanis(F30A) \\sim Ueq, Uanis(F23B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
2. Others
 Sof(F23B)=Sof(F22B)=Sof(F24B)=Sof(F28B)=Sof(F30B)=Sof(F29B)=1-FVAR(1)
 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 86 electrons were 
found in a volume of 456\%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              26156
_shelx_fab_checksum              72810
_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 1.628
_oxdiff_exptl_absorpt_empirical_full_min 0.783