Isolation of 1,4,5,8-tetraazanaphthalene radicals.
Deshapriya, Saroshan; Demir, Selvan; Chemical communications (Cambridge, England) 61 (2025) 12301–12304; doi:10.1039/d5cc03096j

data_7134848
_publ_section_title
;
 Isolation of 1,4,5,8-tetraazanaphthalene radicals.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12301
_journal_page_last               12304
_journal_paper_doi               10.1039/d5cc03096j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C18 H28 K N4 O6'
_chemical_formula_sum            'C18 H28 K N4 O6'
_chemical_formula_weight         435.54
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-27
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.22 svn.r631f81ec for OlexSys, GUI svn.r7248)
;
_audit_update_record
;
2025-05-30 deposited with the CCDC.	2025-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                74.121(3)
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'CrysAlisPro system (CCD 43.144a 64-bit (release 23-01-2025))'
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_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -31.00  22.00   0.50    0.05    --  -47.65  19.00-180.00  106
  2  \w    -29.00  27.00   0.50    0.05    --  -47.65  19.00-120.00  112
  3  \w    -52.00 -22.00   0.50    0.05    --  -91.75  45.00   0.00   60
  4  \w    -28.00  17.00   0.50    0.05    --  -47.65  19.00 120.00   90
  5  \w     44.00 101.00   0.50    0.05    --   47.65-139.00  64.00  114
  6  \w     42.00  67.00   0.50    0.05    --  113.25 -94.00  90.00   50
  7  \w     90.00 118.00   0.50    0.05    --  113.25-139.00  64.00   56
  8  \w     76.00 102.00   0.50    0.05    --  113.25 -94.00 150.00   52
  9  \w     45.00  71.00   0.50    0.05    --  113.25 -94.00 150.00   52
 10  \w     79.00 104.00   0.50    0.05    --  113.25 -94.00  60.00   50
 11  \w     56.00  81.00   0.50    0.05    --  113.25-125.00   0.00   50
 12  \w     77.00 102.00   0.50    0.05    --  113.25 -94.00  90.00   50
 13  \w     54.00  92.00   0.50    0.05    --   47.65-130.00-121.00   76
 14  \w     79.00 104.00   0.50    0.05    --  113.25 -94.00-180.00   50
 15  \w     77.00 102.00   0.50    0.05    --  113.25-130.00-121.00   50
 16  \w     74.00 101.00   0.50    0.05    --  113.25 -94.00-150.00   54
 17  \w     77.00 103.00   0.50    0.05    --  113.25 -94.00-120.00   52
 18  \w     48.00 102.00   0.50    0.05    --  113.25 -94.00 -60.00  108
 19  \w     65.00 102.00   0.50    0.05    --  113.25 -94.00 120.00   74
 20  \w     45.00 102.00   0.50    0.05    --  113.25 -94.00  30.00  114
 21  \w     79.00 104.00   0.50    0.05    --  113.25 -94.00 -30.00   50
 22  \w     42.00  95.00   0.50    0.05    --  113.25 -94.00 -90.00  106
 23  \w     46.00  72.00   0.50    0.05    --  113.25 -77.00-120.00   52
 24  \w     43.00  69.00   0.50    0.05    --  113.25 -61.00-180.00   52
 25  \w     43.00  69.00   0.50    0.05    --  113.25 -61.00 -30.00   52
 26  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00 150.00   50
 27  \w     43.00  68.00   0.50    0.05    --  113.25 -61.00 120.00   50
 28  \w     43.00  68.00   0.50    0.05    --  113.25 -61.00  60.00   50
 29  \w     42.00  69.00   0.50    0.05    --  113.25 -61.00-120.00   54
 30  \w     -4.00  27.00   0.50    0.05    --   47.65 -19.00-150.00   62
 31  \w    112.00 137.00   0.50    0.05    --  113.25 130.00 -49.00   50
 32  \w    -16.00  22.00   0.50    0.05    --   47.65 -19.00 -60.00   76
 33  \w    105.00 130.00   0.50    0.05    --  113.25 139.00 124.00   50
 34  \w    150.00 177.00   0.50    0.05    --  113.25  15.00 150.00   54
 35  \w    103.00 177.00   0.50    0.05    --  113.25  45.00  60.00  148
 36  \w    110.00 176.00   0.50    0.05    --  113.25  77.00   0.00  132
 37  \w    104.00 145.00   0.50    0.05    --  113.25  30.00  60.00   82
 38  \w    101.00 141.00   0.50    0.05    --  113.25  45.00 -30.00   80
 39  \w    102.00 159.00   0.50    0.05    --  113.25  45.00-180.00  114
 40  \w    142.00 175.00   0.50    0.05    --  113.25  77.00-120.00   66
 41  \w    124.00 174.00   0.50    0.05    --  113.25  77.00 -90.00  100
 42  \w    105.00 135.00   0.50    0.05    --  113.25  15.00 150.00   60
 43  \w   -122.00 -82.00   0.50    0.05    --  -91.75 -15.00 -90.00   80
 44  \w   -104.00 -67.00   0.50    0.05    --  -47.65-139.00  64.00   74
 45  \w   -134.00-109.00   0.50    0.05    --  -91.75-139.00  64.00   50
 46  \w   -108.00 -75.00   0.50    0.05    --  -47.65-130.00-121.00   66
 47  \w   -123.00 -92.00   0.50    0.05    --  -91.75-130.00-121.00   62
 48  \w   -161.00-126.00   0.50    0.05    --  -91.75 -15.00 -90.00   70
 49  \w    -54.00 -29.00   0.50    0.05    --  -47.65 130.00 -49.00   50
 50  \w    -66.00 -41.00   0.50    0.05    --  -47.65 139.00 124.00   50
 51  \w    -57.00 -32.00   0.50    0.05    --  -91.75 139.00 124.00   50
;
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'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1980520000
_diffrn_orient_matrix_UB_12      0.0828688000
_diffrn_orient_matrix_UB_13      -0.0147767000
_diffrn_orient_matrix_UB_21      -0.0907609000
_diffrn_orient_matrix_UB_22      -0.0251568000
_diffrn_orient_matrix_UB_23      0.1874758000
_diffrn_orient_matrix_UB_31      -0.0009980000
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_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6458
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.118
_diffrn_reflns_theta_min         5.403
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.573
_exptl_absorpt_correction_T_max  1.000
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_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.107a (Rigaku Oxford Diffraction, 2025)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent dark blue'
_exptl_crystal_density_diffrn    1.373
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_exptl_crystal_F_000             231
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.1459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
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_reflns_number_gt                2232
_reflns_number_total             2245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03096j2.cif
_cod_data_source_block           '[K(18-crown-6)]TAN'
_cod_depositor_comments
'Adding full bibliography for 7134847--7134849.cif.'
_cod_original_cell_volume        526.70(5)
_cod_database_code               7134848
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         KC18H28O6N4
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.359
_diffrn_oxdiff_digest_hkl
;
430b067b6c3d620011eef50feec914521b2508
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_diffrn_oxdiff_digest_od_ed
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_olex2_refinement_description
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_shelx_res_checksum              69309
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_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.420
_oxdiff_exptl_absorpt_empirical_full_min 0.716