Syntheses, structures, and magnetic properties of the lanthanide complexes of imidazole-substituted nitronyl nitroxide biradicals
Xia, Cheng-Cai; Ji, Wen-Jie; Zhang, Xin-Yu; Miao, Hao; Zhang, Yi-Quan; Wang, Xin-Yi; Dalton Transactions  (2022) –; doi:10.1039/D2DT01652D

data_7710864
_publ_section_title
;
 Syntheses, structures, and magnetic properties of the lanthanide
 complexes of imidazole-substituted nitronyl nitroxide biradicals
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01652D
_journal_year                    2022
_chemical_formula_moiety         'C22 H32 Gd N11 O13, C H4 O'
_chemical_formula_sum            'C23 H36 Gd N11 O14'
_chemical_formula_weight         847.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-22
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.02.18 svn.raf6880d7 for OlexSys, GUI svn.r6471)
;
_audit_update_record
;
2022-05-21 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6136(4)
_cell_length_b                   17.0969(6)
_cell_length_c                   17.6798(6)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.54
_cell_volume                     3208.2(2)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30441
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.536
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.152
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 3095 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7303
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0173
_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^)+(0.0249P)^2^+0.1664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0465
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                7117
_reflns_number_total             7303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01652d2.cif
_cod_data_source_block           1_CCDC2
_cod_database_code               7710864
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.919
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C12(H12a,H12b)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C13(H13), C14(H14)
3.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C17(H17a,
 H17b,H17c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C22(H22a,H22b,H22c),
 C23(H23a,H23b,H23c)
3.d Idealised tetrahedral OH refined as rotating group:
 O14(H14a)
;
_shelx_res_checksum              46089
_shelx_hkl_checksum              91611
_olex2_submission_special_instructions 'No special instructions were received'