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_7713189
_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         '2(C26 H38 Co N12 O6), 4(Cl O4), 4(C H4 O)'
_chemical_formula_sum            'C56 H92 Cl4 Co2 N24 O32'
_chemical_formula_weight         1873.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-06
_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                90
_cell_angle_beta                 106.946(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.7524(10)
_cell_length_b                   18.2753(10)
_cell_length_c                   12.4972(6)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     4096.9(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38308
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.075
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.632
_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    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         9400
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0599P)^2^+3.8609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7736
_reflns_number_total             9400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01277h2.cif
_cod_data_source_block           1_CCDC6
_cod_database_code               7713189
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.975
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
O8 \\sim O01K: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
C14 \\sim C13: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O01K) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(O01K)=Sof(H01K)=Sof(C13)=Sof(H13a)=Sof(H13b)=Sof(H13c)=1-FVAR(1)
 Sof(O8)=Sof(H8)=Sof(C14)=Sof(H14a)=Sof(H14b)=Sof(H14c)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C26(H26), C11(H11), C24(H24), C25(H25)
4.b Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C2(H2a,H2b,H2c), C5(H5a,H5b,H5c), C1(H1a,H1b,H1c),
 C01F(H01d,H01e,H01f), C19(H19a,H19b,H19c), C15(H15a,H15b,H15c), C18(H18a,H18b,
 H18c), C4(H4a,H4b,H4c), C01L(H01a,H01b,H01c), C01O(H01g,H01h,H01i), C13(H13a,
 H13b,H13c), C14(H14a,H14b,H14c)
4.c Idealised tetrahedral OH refined as rotating group:
 O11(H11a), O3(H3), O01K(H01K), O12(H12a), O8(H8)
;
_shelx_res_checksum              90045
_olex2_submission_special_instructions 'No special instructions were received'