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_7710866
_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 N8 O16 Tb2, 2(C7 H8)'
_chemical_formula_sum            'C68 H58 F36 N8 O16 Tb2'
_chemical_formula_weight         2245.06
_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   geom
_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                 119.7990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.1578(17)
_cell_length_b                   10.7660(5)
_cell_length_c                   22.3304(11)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.36
_cell_volume                     9003.6(7)
_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 0.987
_diffrn_measured_fraction_theta_max 0.988
_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  0.0550
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38396
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         2.100
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.695
_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    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         10208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0845P)^2^+23.6614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8352
_reflns_number_total             10208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01652d2.cif
_cod_data_source_block           1_sq_CCDC1
_cod_database_code               7710866
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.935
_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. Others
 Sof(F3)=1-FVAR(1)
 Sof(F4)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C01B(H01a,H01b), C01C(H01c,H01d)
3.b Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00X(H00X), C00Z(H00Z), C019(H019), C01H(H01r), C01L(H01L),
 C01P(H01s), C01R(H01t), C01S(H01u), C01T(H01v)
3.c Idealised Me refined as rotating group:
 C01G(H01e,H01f,H01g), C01J(H01h,H01i,H01j), C01M(H01k,H01m,H01n), C01N(H01o,
 H01p,H01q), C01W(H01w,H01x,H01y)
;
_shelx_res_checksum              72664
_shelx_hkl_checksum              75755
_shelx_fab_checksum              31819
_olex2_submission_special_instructions 'No special instructions were received'