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_7132474
_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         'C5 H3 N9 O6'
_chemical_formula_sum            'C5 H3 N9 O6'
_chemical_formula_weight         285.16
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-03
_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                 98.440(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8502(4)
_cell_length_b                   7.3093(4)
_cell_length_c                   16.7588(7)
_cell_measurement_reflns_used    2277
_cell_measurement_temperature    298.35
_cell_measurement_theta_max      21.7870
_cell_measurement_theta_min      2.4320
_cell_volume                     1072.37(9)
_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      298.35
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.944
_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     12.00  40.00   0.50    7.00    --   16.22  45.00 -30.00   56
  2  \w     43.00  83.00   0.50    7.00    --   16.22  45.00 -30.00   80
  3  \w     69.00  94.00   0.50    7.00    --   16.22  14.00  -7.00   50
  4  \w     11.00  40.00   0.50    7.00    --   16.22-125.00  60.00   58
  5  \w     45.00  71.00   0.50    7.00    --   16.22-125.00  60.00   52
  6  \w    -88.00  52.00   0.50    7.00    --  -14.97  14.00  -7.00  280
  7  \w    -52.00  41.00   0.50    7.00    --   16.22 -61.00 -90.00  186
  8  \w    -19.00  13.00   0.50    7.00    --  -14.97 -94.00-120.00   64
  9  \w     20.00  46.00   0.50    7.00    --   16.22 -77.00-180.00   52
 10  \w     10.00  71.00   0.50    7.00    --   16.22-125.00-180.00  122
 11  \w    -63.00  90.00   0.50    7.00    --   16.22 -14.00-178.00  306
 12  \w    -51.00 -10.00   0.50    7.00    --   16.22 -77.00-180.00   82
 13  \w    -94.00  59.00   0.50    7.00    --  -14.97 -14.00-178.00  306
 14  \w    -69.00 -38.00   0.50    7.00    --  -14.97 125.00 -90.00   62
 15  \w    -88.00 -63.00   0.50    7.00    --  -14.97 -30.00   0.00   50
;
_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      0.0538453000
_diffrn_orient_matrix_UB_12      -0.0001950000
_diffrn_orient_matrix_UB_13      -0.0274515000
_diffrn_orient_matrix_UB_21      -0.0592368000
_diffrn_orient_matrix_UB_22      0.0197700000
_diffrn_orient_matrix_UB_23      -0.0321378000
_diffrn_orient_matrix_UB_31      0.0124166000
_diffrn_orient_matrix_UB_32      0.0950308000
_diffrn_orient_matrix_UB_33      0.0066226000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11964
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.928
_diffrn_reflns_theta_min         2.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38931
_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    1.766
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1216P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.2247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1129
_reflns_number_total             2204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05116a3.cif
_cod_data_source_block           aks180
_cod_depositor_comments
'Adding full bibliography for 7132470--7132475.cif.'
_cod_database_code               7132474
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.897
_reflns_odcompleteness_completeness 98.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Rotating group:
 N9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2)
;
_shelx_res_checksum              54980
_shelx_hkl_checksum              57439
_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 1.642
_oxdiff_exptl_absorpt_empirical_full_min 0.445