Unusual zig-zag-shaped Ln-radical coordination networks derived from a nitronyl nitroxide with two imidazole groups: single-crystal-to-single-crystal transformations and magnetic properties.
Jin, Chao-Yi; Zhang, Qiuxue; Tang, Jinkui; Cheng, Peng; Li, Licun; Dalton transactions (Cambridge, England : 2003) 54 (2025) 7718–7725; doi:10.1039/d4dt03488k

data_7718495
_publ_section_title
;
 Unusual zig-zag-shaped Ln-radical coordination networks derived from a
 nitronyl nitroxide with two imidazole groups:
 single-crystal-to-single-crystal transformations and magnetic properties.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7718
_journal_page_last               7725
_journal_paper_doi               10.1039/d4dt03488k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C83 H51 F54 Gd3 N12 O22, 2.25[C6H14]'
_chemical_formula_sum            'C96.5 H82.5 F54 Gd3 N12 O22'
_chemical_formula_weight         3259.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-27 deposited with the CCDC.	2025-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.288(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0907(8)
_cell_length_b                   23.0966(6)
_cell_length_c                   23.9398(10)
_cell_measurement_reflns_used    15364
_cell_measurement_temperature    300
_cell_measurement_theta_max      61.8470
_cell_measurement_theta_min      3.8340
_cell_volume                     13774.5(9)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -25.00  94.00   0.50    9.00    --    5.00  57.00-120.00  238
  2  \w    -82.00  40.00   0.50    9.00    --  -49.00  71.00  11.66  244
  3  \w   -138.00 -16.00   0.50    9.00    --  -49.00 -70.00  98.36  244
  4  \w    -79.00  40.00   0.50    9.00    --  -49.00  57.00   0.00  238
  5  \w   -138.00 -19.00   0.50    9.00    --  -49.00 -57.00 150.00  238
  6  \w   -138.00 -18.00   0.50    9.00    --  -49.00 -45.00  25.62  240
  7  \w   -199.00 -77.00   0.50    5.00    -- -110.00 -68.00 -19.54  244
  8  \w   -103.00 -77.00   0.50    5.00    -- -110.00 -71.00  -8.35   52
  9  \w   -199.00 -78.00   0.50    5.00    -- -110.00 -71.00 -72.12  242
 10  \w   -199.00 -77.00   0.50    5.00    -- -110.00 -72.00-168.26  244
 11  \w    -90.00 -63.00   0.50    5.00    -- -110.00  72.00 -60.00   54
 12  \w   -191.00-111.00   0.50    5.00    -- -110.00 -72.00 -37.08  160
 13  \w   -105.00 -80.00   0.50    5.00    -- -110.00 -57.00-120.00   50
 14  \w   -192.00 -81.00   0.50    5.00    -- -110.00 -63.00 -90.69  222
 15  \w   -157.00-118.00   0.50    5.00    -- -110.00 -57.00-120.00   78
 16  \w   -170.00-143.00   0.50    5.00    -- -110.00 -71.00  -8.35   54
 17  \w   -107.00 -35.00   0.50    5.00    -- -110.00  72.00   0.00  144
 18  \w   -139.00 -32.00   0.50    5.00    -- -110.00  72.00-150.00  214
 19  \w   -107.00 -82.00   0.50    5.00    -- -110.00  72.00 120.00   50
 20  \w   -142.00-117.00   0.50    5.00    -- -110.00 -72.00  30.00   50
 21  \w   -101.00 -76.00   0.50    5.00    -- -110.00 -72.00  30.00   50
 22  \w   -102.00 -70.00   0.50    5.00    -- -110.00  72.00 -30.00   64
 23  \w   -179.00 -77.00   0.50    5.00    -- -110.00 -71.00 -45.12  204
 24  \w    -96.00 -42.00   0.50    5.00    -- -110.00  72.00 -90.00  108
 25  \w   -100.00 -73.00   0.50    5.00    -- -110.00  72.00  90.00   54
 26  \w   -199.00 -81.00   0.50    5.00    -- -110.00 -57.00-150.00  236
 27  \w   -183.00 -77.00   0.50    5.00    -- -110.00 -71.00  14.09  212
 28  \w    -74.00 -21.00   0.50    5.00    -- -110.00  72.00-180.00  106
 29  \w   -137.00 -79.00   0.50    5.00    -- -110.00  72.00-180.00  116
 30  \w   -112.00 -46.00   0.50    5.00    -- -110.00  72.00  30.00  132
 31  \w   -104.00 -77.00   0.50    5.00    -- -110.00 -69.00 -23.37   54
 32  \w   -102.00 -76.00   0.50    5.00    -- -110.00 -72.00   0.00   52
 33  \w   -103.00 -77.00   0.50    5.00    -- -110.00 -71.00  21.94   52
 34  \w   -104.00 -76.00   0.50    5.00    -- -110.00 -72.00 -37.08   56
 35  \w   -103.00 -77.00   0.50    5.00    -- -110.00 -70.00  24.03   52
 36  \w   -102.00 -76.00   0.50    5.00    -- -110.00 -72.00 -30.00   52
 37  \w   -198.00 -77.00   0.50    5.00    -- -110.00 -68.00  -0.09  242
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0172212000
_diffrn_orient_matrix_UB_12      -0.0635565000
_diffrn_orient_matrix_UB_13      0.0142777000
_diffrn_orient_matrix_UB_21      -0.0225171000
_diffrn_orient_matrix_UB_22      -0.0163510000
_diffrn_orient_matrix_UB_23      -0.0598566000
_diffrn_orient_matrix_UB_31      0.0611922000
_diffrn_orient_matrix_UB_32      0.0119956000
_diffrn_orient_matrix_UB_33      -0.0057520000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1634
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            113504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        46.093
_diffrn_reflns_theta_max         46.093
_diffrn_reflns_theta_min         3.548
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24590
_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 bluish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       plate
_exptl_crystal_F_000             6398
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2216
_refine_ls_number_reflns         11776
_refine_ls_number_restraints     4250
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1674P)^2^+8.2281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2194
_refine_ls_wR_factor_ref         0.2424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8425
_reflns_number_total             11776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03488k2.cif
_cod_data_source_block           Gd-300K
_cod_depositor_comments
'Adding full bibliography for 7718494--7718497.cif.'
_cod_original_cell_volume        13774.5(8)
_cod_original_formula_sum        'C96.50 H82.50 F54 Gd3 N12 O22'
_cod_database_code               7718495
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.452
_shelx_estimated_absorpt_t_min   0.254
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2A-O2B
 0.5 with sigma of 0.01
 C69B-C69A
 0.3 with sigma of 0.001
 C9-N4
 1.4 with sigma of 0.01
 C9-N8
 1.2 with sigma of 0.005
 N10A-C19
 1.5 with sigma of 0.01
 Gd3B_$1-N12
 2.5 with sigma of 0.01
 O2B-C69B \\sim O1-C58 \\sim O2A-C69B
 with sigma of 0.01
 O4B-C7B \\sim O4A-C7A \\sim O3B-C5B \\sim O3A-C5A
 with sigma of 0.02
 C7A-C8A \\sim C8B-C7B \\sim C4A-C5B \\sim C9B-C10B \\sim C9A-C10A \\sim
C3B-C69B \\sim C58-C51 \\sim C13A-
 C12B \\sim C13B-C12A
 with sigma of 0.01
 C68-C69B \\sim C68-C58
 with sigma of 0.02
 N10-C19 \\sim N10A-C19
 with sigma of 0.02
 N10-O16 \\sim N10A-O16A
 with sigma of 0.02
 N10-C43 \\sim N10A-C43
 with sigma of 0.02
 C19-O16 \\sim C19-O16A
 with sigma of 0.04
 O16-C43 \\sim O16A-C43
 with sigma of 0.04
 F43B-F45B \\sim F44B-F45B \\sim F44B-F43B \\sim F43A-F45A \\sim F44A-F45A
\\sim F43A-F44A \\sim F51B-
 F50B \\sim F50B-F49B \\sim F51B-F49B \\sim F51A-F49A \\sim F50A-F49A \\sim
F48B-F46B \\sim F47B-F46B ~
 F47B-F48B \\sim F54A-F53A \\sim F52A-F53A \\sim F52A-F54A \\sim F52B-F53B
\\sim F54B-F53B \\sim F52B-
 F54B \\sim F40B-F42B \\sim F40B-F41B \\sim F42B-F41B
 with sigma of 0.01
 O3A-C5B \\sim O3A-C5A
 with sigma of 0.02
 F42B-C13B \\sim F40B-C13B \\sim F41B-C13B \\sim F39A-C13A \\sim F37A-C13A
\\sim F38A-C13A \\sim F43A-
 C8A \\sim F44A-C8A \\sim F45A-C8A \\sim F44B-C8B \\sim F45B-C8B \\sim F43B-C8B
\\sim F47B-C4B \\sim F48B-
 C4B \\sim F46B-C4B \\sim F47A-C4A \\sim F48A-C4A \\sim F46A-C4A \\sim F50B-C3B
\\sim F51B-C3B \\sim F49B-
 C3B \\sim F49A-C3A \\sim F50A-C3A \\sim F51A-C3A \\sim F54B-C51 \\sim F52B-C51
\\sim F53B-C51 \\sim F19B-
 C1C \\sim F21B-C1C \\sim F20B-C1C \\sim F38B-C9B \\sim F13A-C49 \\sim F7B-C66
\\sim F17A-C65 \\sim F39B-C9B
 with sigma of 0.02
 C5B-C6A \\sim C5A-C6A
 with sigma of 0.02
 C5B-C4A \\sim C5A-C4A
 with sigma of 0.02
 C5B-O3B \\sim C5A-O3B
 with sigma of 0.02
 C5B-C6B \\sim C5A-C6B
 with sigma of 0.02
 C5B-F48B \\sim C5A-F48B
 with sigma of 0.02
 C5B-C4A \\sim C5B-C4B
 with sigma of 0.02
 C4A-C5A \\sim C4B-C5A
 with sigma of 0.02
 F48A-C4A \\sim F48A-C4B
 with sigma of 0.02
 C5A-C4A \\sim C4B-C5B \\sim C5A-C6A \\sim C6B-C7B \\sim C6B-C5B \\sim C6A-C7A
\\sim C7A-C8A \\sim C8B-C7B
 with sigma of 0.02
 F46A-C4A \\sim F46A-C4B
 with sigma of 0.02
 F47A-C4A \\sim F47A-C4B
 with sigma of 0.02
 C4A-F47B \\sim C4B-F47B
 with sigma of 0.02
 C4A-F46B \\sim C4B-F46B
 with sigma of 0.02
 C1C-C57 \\sim C1B-C57 \\sim C54-C2A \\sim C2B-C54
 with sigma of 0.02
 F21A-C23 \\sim F23B-C23
 with sigma of 0.02
 F20A-C23 \\sim F22B-C23
 with sigma of 0.02
 F19A-C23 \\sim F24B-C23
 with sigma of 0.02
 F14A-C49 \\sim F14B-C49 \\sim F15B-C49 \\sim F15A-C49 \\sim F13B-C49 \\sim
F13A-C49 \\sim F8B-C66 ~
 F9B-C66 \\sim F9A-C66 \\sim F7A-C66 \\sim F7B-C66 \\sim F8A-C66 \\sim F11B-C33
\\sim F10A-C33 \\sim F10B-
 C33 \\sim F11A-C33 \\sim F12A-C33 \\sim F12B-C33
 with sigma of 0.02
 F8B-F7B \\sim F9B-F8B \\sim F9B-F7B
 with sigma of 0.01
 F36B-C28 \\sim F35A-C28 \\sim F35B-C28 \\sim F34A-C28 \\sim F34B-C28 \\sim
F36A-C28
 with sigma of 0.01
 C13A-C12A \\sim C13B-C12B \\sim C9A-C10A \\sim C9B-C10B \\sim C5A-C4A \\sim
C5B-C4B \\sim C8B-C7B ~
 C8A-C7A \\sim C58-C51 \\sim C69B-C3A \\sim C69A-C3B
 with sigma of 0.01
 O5A-C10A \\sim O5B-C10B \\sim O6A-C12A \\sim O6B-C12B
 with sigma of 0.02
3. Rigid bond restraints
 C12B, C13B, C11B, C10B, C9B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(O4B) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C12B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2B) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(F53B) \\sim Ueq, Uanis(F54B)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Sof(F31B)=Sof(F33B)=Sof(F32B)=1-FVAR(1)
 Sof(F32A)=Sof(F33A)=Sof(F31A)=FVAR(1)
 Sof(F34B)=Sof(F35B)=Sof(F36B)=1-FVAR(2)
 Sof(F35A)=Sof(F34A)=Sof(F36A)=FVAR(2)
 Sof(F25B)=Sof(F26B)=Sof(F27B)=1-FVAR(3)
 Sof(F30A)=Sof(F29A)=Sof(F28A)=FVAR(3)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=1-FVAR(4)
 Sof(F8A)=Sof(F7A)=Sof(F9A)=FVAR(4)
 Sof(F10B)=Sof(F12B)=Sof(F11B)=1-FVAR(5)
 Sof(F11A)=Sof(F10A)=Sof(F12A)=FVAR(5)
 Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(6)
 Sof(F14A)=Sof(F15A)=Sof(F13A)=FVAR(6)
 Sof(F17B)=Sof(F16B)=Sof(F18B)=1-FVAR(7)
 Sof(F16A)=Sof(F18A)=Sof(F17A)=FVAR(7)
 Sof(C1C)=Sof(F20B)=Sof(F19B)=Sof(F21B)=Sof(C2B)=Sof(F28B)=Sof(F29B)=Sof(F30B)=
 1-FVAR(8)
 Sof(F25A)=Sof(F23A)=Sof(F27A)=Sof(C2A)=Sof(F22A)=Sof(F24A)=Sof(F26A)=Sof(C1B)=
 FVAR(8)
 Sof(F53B)=Sof(F54B)=Sof(F52B)=Sof(C5B)=Sof(Gd3B)=Sof(O6B)=Sof(O5B)=Sof(O4B)=
 Sof(O3B)=Sof(F41B)=Sof(F47B)=Sof(F42B)=Sof(F38B)=Sof(F39B)=Sof(C10B)=Sof(F45B)=
 Sof(F44B)=Sof(F37B)=Sof(C13B)=Sof(F43B)=Sof(F40B)=Sof(F46B)=Sof(C8B)=Sof(F49B)=
 Sof(C11B)=Sof(H11B)=Sof(F50B)=Sof(C7B)=Sof(C6B)=Sof(H6B)=Sof(F48B)=Sof(F51B)=
 Sof(C9B)=Sof(C3B)=Sof(C4B)=1-FVAR(9)
 Sof(Gd3A)=Sof(O6A)=Sof(O5A)=Sof(O4A)=Sof(O3A)=Sof(F38A)=Sof(F48A)=Sof(F39A)=
 Sof(F40A)=Sof(F42A)=Sof(C10A)=Sof(F45A)=Sof(F44A)=Sof(F41A)=Sof(C13A)=
 Sof(F43A)=Sof(F37A)=Sof(F46A)=Sof(C8A)=Sof(F49A)=Sof(C11A)=Sof(H11A)=Sof(F50A)=
 Sof(C7A)=Sof(C6A)=Sof(H6A)=Sof(F47A)=Sof(F51A)=Sof(C9A)=Sof(C3A)=Sof(C4A)=
 Sof(F53A)=Sof(F54A)=Sof(F52A)=Sof(C5A)=FVAR(9)
 Sof(F24B)=Sof(F23B)=Sof(F22B)=1-FVAR(10)
 Sof(F21A)=Sof(F20A)=Sof(F19A)=FVAR(10)
 Fixed Sof: N10(0.9) O2B(0.5) O16(0.9) C12B(0.3) C12A(0.7) H68(0.5) H68A(0.5)
 C69B(0.5) O16A(0.1) N10A(0.1) O2A(0.5) C69A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C11(H11), C12(H12), C15(H15), C17(H17),
 C18(H18), C21(H21), C22(H22), C26(H26), C34(H34), C36(H36), C37(H37), C38(H38),
  C41(H41), C42(H42), C45(H45), C47(H47), C50(H50), C53(H53), C56(H56),
 C61(H61), C11A(H11A), C6A(H6A), C11B(H11B), C68(H68), C68(H68A), C6B(H6B)
6.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C1A(H1AA,H1AB,H1AC), C52(H52A,H52B,H52C), C55(H55A,H55B,
 H55C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 452 electrons were 
found in a volume of 3302\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.25[C6H14] per formula unit 
which account for 450 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13874
_shelx_hkl_checksum              57452
_shelx_fab_checksum              49109
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.958
_oxdiff_exptl_absorpt_empirical_full_min 0.337