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_7713186
_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         'C22 H17 Co F12 N6 O6, C H2 Cl2'
_chemical_formula_sum            'C23 H19 Cl2 Co F12 N6 O6'
_chemical_formula_weight         833.27
_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     heavy
_audit_creation_date             2023-02-07
_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                68.656(6)
_cell_angle_beta                 72.820(5)
_cell_angle_gamma                69.263(4)
_cell_formula_units_Z            2
_cell_length_a                   9.5397(14)
_cell_length_b                   12.2112(18)
_cell_length_c                   15.954(3)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    193
_cell_measurement_theta_max      54.20
_cell_measurement_theta_min      4.39
_cell_volume                     1589.0(5)
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17287
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.197
_diffrn_reflns_theta_min         4.392
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.643
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         5652
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0915P)^2^+1.9075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5411
_reflns_number_total             5652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01277h2.cif
_cod_data_source_block           1_CCDC3
_cod_original_cell_volume        1589.0(4)
_cod_database_code               7713186
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 F01C, C015
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl01: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Cl00 \\sim Cl0A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(F01E) \\sim Ueq, Uanis(F01C) \\sim Ueq, Uanis(F012) \\sim Ueq,
Uanis(F013) \\sim Ueq, Uanis(F00X) \\sim Ueq, Uanis(F00S) \\sim Ueq,
Uanis(Cl00) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F01E) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C015) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F01F) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F012) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(Cl00)=Sof(Cl01)=Sof(H01c)=Sof(H01d)=1-FVAR(1)
 Sof(H01a)=Sof(H01b)=Sof(Cl1)=Sof(Cl0A)=FVAR(1)
 Sof(F01D)=Sof(F0)=Sof(F01F)=1-FVAR(2)
 Sof(F012)=Sof(F01C)=Sof(F01E)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C01F(H01c,H01d), C01F(H01a,H01b)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C11(H11), C00W(H00W), C00Y(H00Y)
5.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C2(H2a,H2b,H2c), C5(H5a,H5b,H5c), C1(H1a,H1b,H1c)
;
_shelx_res_checksum              38270
_olex2_submission_special_instructions 'No special instructions were received'