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_7713185
_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         'C26 H38 Mn N12 O6, 2(Cl O4), C H4 O'
_chemical_formula_sum            'C27 H42 Cl2 Mn N12 O15'
_chemical_formula_weight         900.56
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-21
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-26 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                92.069(2)
_cell_angle_beta                 100.953(2)
_cell_angle_gamma                108.176(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1394(9)
_cell_length_b                   12.6882(11)
_cell_length_c                   14.9298(13)
_cell_measurement_reflns_used    8428
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.42
_cell_volume                     1958.0(3)
_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 0.985
_diffrn_measured_fraction_theta_max 0.986
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16264
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_min         2.086
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.555
_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    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8897
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0589P)^2^+1.3648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7391
_reflns_number_total             8897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01277h2.cif
_cod_data_source_block           1_CCDC2
_cod_database_code               7713185
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.978
_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 C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 Mn1-H4
 2.810075 with sigma of 0.02
 C25-H4
 1.897147 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O16: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O16 \\sim O15: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O16)=Sof(H16)=Sof(H01D)=Sof(H01E)=Sof(H01F)=1-FVAR(1)
 Sof(H01A)=Sof(H01B)=Sof(H01C)=Sof(O15)=Sof(H15)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C22(H22), C23(H23), C24(H24)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C14(H14A,
 H14B,H14C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C01L(H01D,H01E,H01F), C01L(H01A,H01B,
 H01C)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O16(H16), O15(H15)
;
_shelx_res_checksum              52006
_olex2_submission_special_instructions 'No special instructions were received'