Synthetic manifestation of trinitro-pyrazolo-2<i>H</i>-1,2,3-triazoles (TNPT) as insensitive energetic materials.
Balaraju, Muntha; Kommu, Nagarjuna; Vangara, Srinivas; Sahoo, Aswini K.; Thaltiri, Vikranth; Sahoo, Akhila K.; Chemical communications (Cambridge, England) 60 (2024) 827–830; doi:10.1039/d3cc05116a

data_7132473
_publ_section_title
;
 Synthetic manifestation of trinitro-pyrazolo-2<i>H</i>-1,2,3-triazoles
 (TNPT) as insensitive energetic materials.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              827
_journal_page_last               830
_journal_paper_doi               10.1039/d3cc05116a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C6 H4 N8 O6'
_chemical_formula_sum            'C6 H4 N8 O6'
_chemical_formula_weight         284.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-11
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2023-12-09 deposited with the CCDC.	2023-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.884(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1552(5)
_cell_length_b                   8.1515(4)
_cell_length_c                   15.7139(7)
_cell_measurement_reflns_used    7382
_cell_measurement_temperature    297.8
_cell_measurement_theta_max      26.7240
_cell_measurement_theta_min      2.2660
_cell_volume                     1122.16(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.8
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_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    -32.00  -7.00   0.50    3.70    --   16.22 -29.00 -46.00   50
  2  \w    -40.00  -1.00   0.50    3.70    --  -14.97 -29.00 -46.00   78
  3  \w      5.00  41.00   0.50    3.70    --   16.22 -30.00 -90.00   72
  4  \w    -37.00  18.00   0.50    3.70    --  -14.97 -94.00   0.00  110
  5  \w     -6.00  35.00   0.50    3.70    --   16.22 -61.00  60.00   82
  6  \w     -8.00  52.00   0.50    3.70    --  -14.97  29.00 114.00  120
  7  \w     16.00  41.00   0.50    3.70    --   16.22 -30.00 120.00   50
  8  \w      8.00  90.00   0.50    3.70    --   16.22  29.00 114.00  164
  9  \w    -21.00  22.00   0.50    3.70    --  -14.97 -94.00 120.00   86
 10  \w     39.00  64.00   0.50    3.70    --   16.22-125.00 120.00   50
 11  \w    -57.00 -15.00   0.50    3.70    --   16.22 -30.00 120.00   84
 12  \w    -83.00   9.00   0.50    3.70    --  -14.97 -45.00 120.00  184
 13  \w    -61.00 -12.00   0.50    3.70    --  -14.97 125.00 120.00   98
 14  \w    -56.00 -31.00   0.50    3.70    --  -14.97 125.00  90.00   50
 15  \w    -65.00 -21.00   0.50    3.70    --  -14.97 125.00  60.00   88
 16  \w    -88.00 -63.00   0.50    3.70    --  -14.97 -29.00 -46.00   50
 17  \w    -62.00   9.00   0.50    3.70    --  -14.97 -45.00 -30.00  142
 18  \w    -55.00 -11.00   0.50    3.70    --   16.22 -30.00 -90.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0762721000
_diffrn_orient_matrix_UB_12      -0.0269962000
_diffrn_orient_matrix_UB_13      -0.0074310000
_diffrn_orient_matrix_UB_21      0.0155940000
_diffrn_orient_matrix_UB_22      -0.0182505000
_diffrn_orient_matrix_UB_23      0.0459386000
_diffrn_orient_matrix_UB_31      -0.0219729000
_diffrn_orient_matrix_UB_32      0.0807253000
_diffrn_orient_matrix_UB_33      0.0078798000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11455
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.898
_diffrn_reflns_theta_min         2.326
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.219
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.0945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1974
_reflns_number_total             2347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05116a3.cif
_cod_data_source_block           aks181
_cod_depositor_comments
'Adding full bibliography for 7132470--7132475.cif.'
_cod_database_code               7132473
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.959
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              5728
_shelx_hkl_checksum              3461
_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 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.573