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_7713188
_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 F12 Mn N6 O6, C H2 Cl2'
_chemical_formula_sum            'C23 H19 Cl2 F12 Mn N6 O6'
_chemical_formula_weight         829.28
_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             2023-01-30
_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                68.5020(10)
_cell_angle_beta                 74.357(2)
_cell_angle_gamma                69.152(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5400(4)
_cell_length_b                   12.2077(5)
_cell_length_c                   16.3666(6)
_cell_measurement_reflns_used    6831
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.71
_cell_volume                     1635.98(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 0.992
_diffrn_measured_fraction_theta_max 0.991
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15752
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.314
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7445
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0779P)^2^+1.9143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6003
_reflns_number_total             7445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01277h2.cif
_cod_data_source_block           1_CCDC5
_cod_database_code               7713188
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.973
_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. Restrained distances
 Cl3-C23 \\sim Cl2-C23 \\sim Cl4-C23 \\sim Cl1-C23
 with sigma of 0.02
3. Rigid bond restraints
 F2, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Cl4 \\sim Cl1: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Cl2 \\sim Cl3: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Cl1 \\sim Cl4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(F5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(Cl3) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Sof(F3A)=Sof(F2A)=Sof(F1A)=Sof(H23c)=Sof(H23d)=Sof(Cl3)=Sof(Cl4)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(Cl1)=Sof(Cl2)=Sof(H23a)=Sof(H23b)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C23(H23a,H23b), C23(H23c,H23d)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C15(H15), C10(H10), C11(H11), C12(H12)
6.c 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              17945
_olex2_submission_special_instructions 'No special instructions were received'