New thermally stable and friction-insensitive nitrogen-rich salts: a synergy of 1,2,4-triazole, furoxan and hydroxytetrazole motifs
Stebletsova, Irina; Larin, Alexander; Vinogradov, Dmitry B.; Pivkina, Alla N.; Leonov, Nikita E.; Gazieva, Galina A.; Fershtat, Leonid L.; CrystEngComm  (2025) –; doi:10.1039/D5CE01047K

data_7251339
_publ_section_title
;
 New thermally stable and friction-insensitive nitrogen-rich salts: a
 synergy of 1,2,4-triazole, furoxan and hydroxytetrazole motifs
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE01047K
_journal_year                    2025
_chemical_formula_moiety         'C5 H3 N9 O3'
_chemical_formula_sum            'C5 H3 N9 O3'
_chemical_formula_weight         237.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-10-01 deposited with the CCDC.	2025-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.355(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3967(3)
_cell_length_b                   7.17590(10)
_cell_length_c                   13.5983(2)
_cell_measurement_reflns_used    6280
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.9880
_cell_measurement_theta_min      3.4300
_cell_volume                     1683.05(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.136a 64-bit (release 23-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -64.00  28.40   0.55    0.50    --  -44.86  60.00 169.00  168
  2  \w    -64.00  28.40   0.55    0.50    --  -44.86  60.00 169.00  168
  3  \w   -117.00 -26.80   0.55    0.50    --  -44.86 -60.00  30.00  164
  4  \w    -70.00 -21.05   0.55    2.00    --  -93.75  60.00 169.00   89
  5  \w   -167.00 -74.60   0.55    2.00    --  -93.75 -60.00  30.00  168
  6  \w     96.00 177.40   0.55    2.00    --  115.25  60.00 169.00  148
  7  \w     43.00  68.85   0.55    2.00    --  115.25 -60.00  30.00   47
  8  \w    -27.00  63.20   0.55    0.50    --   44.86 -60.00  30.00  164
  9  \w     34.00  92.85   0.55    0.50    --   44.86-125.00-120.00  107
 10  \w     34.00  92.85   0.55    0.50    --   44.86-125.00   0.00  107
 11  \w    -51.00 -20.75   0.55    2.00    --  -93.75  45.00   0.00   55
 12  \w     97.00 177.30   0.55    2.00    --  115.25  45.00 120.00  146
 13  \w     97.00 177.30   0.55    2.00    --  115.25  45.00 120.00  146
 14  \w     97.00 177.30   0.55    2.00    --  115.25  45.00  90.00  146
 15  \w     43.00 103.50   0.55    2.00    --  115.25 -77.00  30.00  110
 16  \w     43.00  69.95   0.55    2.00    --  115.25 -61.00 -30.00   49
 17  \w     43.00  69.95   0.55    2.00    --  115.25 -61.00 120.00   49
 18  \w     99.00 157.30   0.55    2.00    --  115.25  61.00-120.00  106
 19  \w     99.00 157.30   0.55    2.00    --  115.25  61.00-120.00  106
 20  \w     43.00 104.05   0.55    2.00    --  115.25 -95.00  30.00  111
 21  \w     52.00  88.30   0.55    2.00    --  115.25-125.00 -30.00   66
 22  \w     44.00  92.40   0.55    2.00    --  115.25 -77.00  90.00   88
 23  \w     73.00 100.50   0.55    2.00    --  115.25 -77.00 -30.00   50
 24  \w     58.00 105.30   0.55    2.00    --  115.25-125.00-120.00   86
 25  \w    125.00 173.40   0.55    2.00    --  115.25  61.00 -90.00   88
 26  \w     44.00  68.75   0.55    2.00    --  115.25 -61.00 150.00   45
 27  \w     97.00 162.45   0.55    2.00    --  115.25  45.00 -30.00  119
 28  \w    119.00 145.40   0.55    2.00    --  115.25  45.00  60.00   48
 29  \w    147.00 172.30   0.55    2.00    --  115.25  45.00  60.00   46
 30  \w     45.00  71.40   0.55    2.00    --  115.25 -77.00 -30.00   48
 31  \w     57.00 100.45   0.55    2.00    --  115.25 -77.00-120.00   79
 32  \w     50.00  76.40   0.55    2.00    --  115.25 -95.00  90.00   48
 33  \w     70.00 107.40   0.55    2.00    --  115.25-125.00-180.00   68
 34  \w    122.00 147.30   0.55    2.00    --  115.25  45.00-150.00   46
 35  \w    113.00 163.05   0.55    2.00    --  115.25  45.00 -90.00   91
 36  \w    101.00 127.40   0.55    2.00    --  115.25  77.00 -30.00   48
 37  \w     43.00  67.75   0.55    2.00    --  115.25 -61.00 -60.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0860089000
_diffrn_orient_matrix_UB_12      0.0258762000
_diffrn_orient_matrix_UB_13      -0.0678403000
_diffrn_orient_matrix_UB_21      -0.0228094000
_diffrn_orient_matrix_UB_22      -0.1493121000
_diffrn_orient_matrix_UB_23      0.0653586000
_diffrn_orient_matrix_UB_31      -0.0077950000
_diffrn_orient_matrix_UB_32      0.1520925000
_diffrn_orient_matrix_UB_33      0.0756623000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9651
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.832
_diffrn_reflns_theta_min         5.129
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.388
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0471P)^2^+1.6156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1690
_reflns_number_total             1837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01047k2.cif
_cod_data_source_block           Ris570c
_cod_database_code               7251339
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C5 H3 N9 O3'
_chemical_oxdiff_usercomment     Ris570.C
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
;
_shelx_res_checksum              98787
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.870