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_7710865
_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         'C54 H42 F36 Gd2 N8 O16, 2(C7 H8)'
_chemical_formula_sum            'C68 H58 F36 Gd2 N8 O16'
_chemical_formula_weight         2241.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-02
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.03.08 svn.r54f81f84 for OlexSys, GUI svn.r6487)
;
_audit_update_record
;
2022-05-21 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.609(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.0794(16)
_cell_length_b                   10.7816(4)
_cell_length_c                   22.2970(8)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.35
_cell_volume                     9003.8(6)
_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    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42158
_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         27.506
_diffrn_reflns_theta_min         2.098
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.597
_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    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.663
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         10326
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.265
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+33.1417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9257
_reflns_number_total             10326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01652d2.cif
_cod_data_source_block           1_sq
_cod_database_code               7710865
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.939
_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
 F3-C2 \\sim F1-C2 \\sim F2-C2
 with sigma of 0.02
 F4-C2 \\sim F1-C2 \\sim F2-C2
 with sigma of 0.02
 F1-F2 \\sim F2-F4 \\sim F4-F1
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F1
 with sigma of 0.02
 F3-C2 \\sim F2-C2 \\sim F1-C2
 with sigma of 0.02
3. Rigid bond restraints
 F2, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(F4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F3)=1-FVAR(1)
 Sof(F4)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C01F(H01g,H01h), C01H(H01j,H01k)
6.b Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00X(H00X), C010(H010), C017(H017), C01A(H01r), C01G(H01i),
 C01K(H01s), C01L(H01t), C01R(H01u), C01S(H01v)
6.c Idealised Me refined as rotating group:
 C01C(H01a,H01b,H01c), C01D(H01d,H01e,H01f), C01M(H01l,H01m,H01n), C01V(H01w,
 H01x,H01y)
;
_shelx_res_checksum              85243
_shelx_hkl_checksum              98966
_shelx_fab_checksum              50385
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'