Lanthanide–radical complexes derived from a nitronyl nitroxide ligand with chelating and bridging functions: structure and magnetic properties
Zhou, Yan; Xie, Junfang; Huang, Xiaohui; Jin, Chaoyi; Ma, Yue; Li, Licun; CrystEngComm 27 (2025) 1120–1127; doi:10.1039/D4CE01184H

data_7249762
_publ_section_title
;
 Lanthanide--radical complexes derived from a nitronyl nitroxide ligand
 with chelating and bridging functions: structure and magnetic properties
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1120
_journal_page_last               1127
_journal_paper_doi               10.1039/D4CE01184H
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C64 H44 F36 N8 Nd2 O16'
_chemical_formula_sum            'C64 H44 F36 N8 Nd2 O16'
_chemical_formula_weight         2153.55
_chemical_name_systematic        2-Nd
_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             2024-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-23 deposited with the CCDC.	2025-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                83.017(4)
_cell_angle_beta                 85.211(3)
_cell_angle_gamma                78.285(4)
_cell_formula_units_Z            2
_cell_length_a                   13.3092(5)
_cell_length_b                   17.0890(9)
_cell_length_c                   20.6746(9)
_cell_measurement_reflns_used    13831
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      31.0480
_cell_measurement_theta_min      2.2730
_cell_volume                     4561.8(4)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113.1500
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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   -120.00  60.00   0.50    5.00    --  -30.00  45.00   0.00  360
  2  \w   -120.00  60.00   0.50    5.00    --  -30.00  45.00  90.00  360
  3  \w   -120.00  60.00   0.50    5.00    --  -30.00  45.00 180.00  360
;
_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      0.0276056000
_diffrn_orient_matrix_UB_12      -0.0306090000
_diffrn_orient_matrix_UB_13      0.0217470000
_diffrn_orient_matrix_UB_21      0.0150561000
_diffrn_orient_matrix_UB_22      0.0296533000
_diffrn_orient_matrix_UB_23      0.0162160000
_diffrn_orient_matrix_UB_31      -0.0445479000
_diffrn_orient_matrix_UB_32      0.0012317000
_diffrn_orient_matrix_UB_33      0.0215215000
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36262
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.565
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34035
_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 dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.739
_refine_diff_density_min         -2.598
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         16521
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0844
_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^)+(0.1404P)^2^+36.1533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2313
_refine_ls_wR_factor_ref         0.2495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13000
_reflns_number_total             16521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01184h2.cif
_cod_data_source_block           2-Nd
_cod_depositor_comments
'Adding full bibliography for 7249760--7249762.cif.'
_cod_database_code               7249762
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.885
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(F25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C20(H20), C19(H19), C2(H2), C1(H1), C52(H52), C24(H24), C21(H21),
 C5(H5), C62(H62), C18(H18), C10(H10), C8(H8), C57(H57), C47(H47), C7(H7),
 C37(H37), C25(H25), C42(H42), C26(H26)
3.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C34(H34A,H34B,
 H34C), C32(H32A,H32B,H32C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C31(H31A,
 H31B,H31C)
;
_shelx_res_checksum              75826
_shelx_hkl_checksum              29549
_shelx_fab_checksum              87788
_olex2_submission_original_sample_id 2-Nd
_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 1.865
_oxdiff_exptl_absorpt_empirical_full_min 0.511