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_7249761
_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 Gd2 N8 O16'
_chemical_formula_sum            'C64 H44 F36 Gd2 N8 O16'
_chemical_formula_weight         2179.57
_chemical_name_systematic        1-Gd
_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     direct
_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                83.050(3)
_cell_angle_beta                 85.811(3)
_cell_angle_gamma                78.097(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3629(4)
_cell_length_b                   17.1060(5)
_cell_length_c                   20.6415(6)
_cell_measurement_reflns_used    20581
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      31.9150
_cell_measurement_theta_min      1.7100
_cell_volume                     4577.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49536
_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         26.372
_diffrn_reflns_theta_min         1.559
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull dark blue'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         18706
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0640P)^2^+0.7038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13062
_reflns_number_total             18706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01184h2.cif
_cod_data_source_block           1-Gd
_cod_depositor_comments
'Adding full bibliography for 7249760--7249762.cif.'
_cod_database_code               7249761
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.859
_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(F26) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.012
Uanis(F23) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C63(H63), C62(H62), C64(H64), C40(H40), C24(H24), C31(H31),
 C3(H3), C8(H8), C29(H29), C61(H61), C45(H45), C25(H25), C35(H35), C30(H30),
 C13(H13), C26(H26), C56(H56), C59(H59), C57(H57)
3.b Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C17(H17A,H17B,H17C), C49(H49A,H49B,H49C), C18(H18A,H18B,
 H18C), C21(H21A,H21B,H21C), C53(H53A,H53B,H53C), C20(H20A,H20B,H20C), C50(H50A,
 H50B,H50C)
;
_shelx_res_checksum              81147
_shelx_hkl_checksum              40716
_shelx_fab_checksum              55478
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id 1-Gd
_olex2_submission_special_instructions 'No special instructions were received'