Syntheses and magnetic properties of a bis-bidentate nitronyl nitroxide radical based on triazolopyrimidine and its metal complexes
Xia, Cheng-Cai; Zhang, Xinyu; Zhang, Chengcheng; Li, Gang; Wei, Haiyan; Wang, Xin-Yi; Dalton Transactions  (2023) –; doi:10.1039/D3DT01277H

data_7713187
_publ_section_title
;
 Syntheses and magnetic properties of a bis-bidentate nitronyl nitroxide
 radical based on triazolopyrimidine and its metal complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01277H
_journal_year                    2023
_chemical_formula_moiety         'C32 H19 Co2 F24 N6 O10'
_chemical_formula_sum            'C32 H19 Co2 F24 N6 O10'
_chemical_formula_weight         1221.39
_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     dual
_audit_creation_date             2023-02-05
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_audit_update_record
;
2023-04-26 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                88.8480(10)
_cell_angle_beta                 73.7910(10)
_cell_angle_gamma                75.9650(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2502(3)
_cell_length_b                   13.4340(4)
_cell_length_c                   14.5990(5)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.65
_cell_volume                     2235.25(12)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20599
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.064
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         10000
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0626P)^2^+2.0821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8406
_reflns_number_total             10000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01277h2.cif
_cod_data_source_block           1_CCDC4
_cod_database_code               7713187
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.965
_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. Restrained distances
 F27-C19 = F26-C19 = F25-C19
 1.32 with sigma of 0.01
 F4-C20 \\sim F6-C20 \\sim F5-C20
 with sigma of 0.02
 F4-F6 \\sim F6-F5 \\sim F5-F4
 with sigma of 0.02
 F27-C19 \\sim F25-C19 \\sim F26-C19
 with sigma of 0.02
 F25-F27 \\sim F27-F26 \\sim F26-F25
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F1
 with sigma of 0.02
 F1-C19 \\sim F3-C19 \\sim F2-C19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F5 \\sim F6: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 2A
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F25) \\sim Ueq, Uanis(F27) \\sim Ueq, Uanis(F26) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(F25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C19) \\sim Ueq, Uanis(F26) \\sim Ueq, Uanis(F25) \\sim Ueq, Uanis(F27)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F4A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F3)=Sof(F2)=Sof(F1)=1-FVAR(2)
 Sof(F25)=Sof(F26)=Sof(F27)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C15(H15), C10(H10), C11(H11), C12(H12), C25(H25), C30(H30)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              75133
_olex2_submission_special_instructions 'No special instructions were received'