Energetic Performance of Trinitromethyl Nitrotriazole (TNMNT) and Its Energetic Salts†
Lal, Sohan; Staples, Richard J.; Shreeve, Jean'ne M.; Chemical Communications  (2023) –; doi:10.1039/D3CC03909A

data_7132071
_publ_section_title
;
 Energetic Performance of Trinitromethyl Nitrotriazole (TNMNT) and Its
 Energetic Salts&#x2020;
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03909A
_journal_year                    2023
_chemical_formula_moiety         'C3 H N6 O6, H5 N2'
_chemical_formula_sum            'C3 H6 N8 O6'
_chemical_formula_weight         250.16
_chemical_melting_point          401
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-31
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-10 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.0185(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.46056(13)
_cell_length_b                   14.9402(3)
_cell_length_c                   9.66552(18)
_cell_measurement_reflns_used    4582
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      79.8740
_cell_measurement_theta_min      5.4810
_cell_volume                     918.71(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_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 0.969
_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     47.00  73.00   0.50    0.24    --   47.10  37.00 -60.00   52
  2  \w     88.00 118.00   0.50    0.24    --   47.10  37.00 -60.00   60
  3  \w    106.00 167.00   0.50    0.96    --  113.25  61.00 -30.00  122
  4  \w    110.00 172.00   0.50    0.96    --  113.25  61.00   0.00  124
  5  \w    146.00 174.00   0.50    0.96    --  113.25  15.00  90.00   56
  6  \w    100.00 130.00   0.50    0.96    --  113.25  15.00  90.00   60
  7  \w     42.00  67.00   0.50    0.96    --  113.25 -61.00  30.00   50
  8  \w     64.00  89.00   0.50    0.96    --  113.25 -77.00  90.00   50
  9  \w     45.00  90.00   0.50    0.96    --  113.25 -77.00  60.00   90
 10  \w     42.00  67.00   0.50    0.96    --  113.25 -61.00  60.00   50
 11  \w     42.00  67.00   0.50    0.96    --  113.25 -61.00 -30.00   50
 12  \w     42.00  67.00   0.50    0.96    --  113.25 -61.00   0.00   50
 13  \w     42.00  67.00   0.50    0.96    --  113.25 -61.00 150.00   50
 14  \w     95.00 141.00   0.50    0.96    --  113.25 130.00  91.00   92
 15  \w    123.00 150.00   0.50    0.96    --  113.25 139.00 -94.00   54
 16  \w     54.00  91.00   0.50    0.96    --  113.25 -77.00 -90.00   74
 17  \w     42.00  67.00   0.50    0.96    --  113.25 -94.00-150.00   50
 18  \w     92.00 118.00   0.50    0.96    --  113.25-139.00-155.00   52
 19  \w     45.00 100.00   0.50    0.24    --   47.10-139.00-155.00  110
 20  \w     44.00  70.00   0.50    0.96    --  113.25-125.00 -60.00   52
 21  \w     77.00 106.00   0.50    0.96    --  113.25-125.00 -60.00   58
 22  \w     72.00 104.00   0.50    0.96    --  113.25 -94.00-150.00   64
 23  \w     74.00 104.00   0.50    0.96    --  113.25 -97.00 -29.86   60
 24  \w     54.00  79.00   0.50    0.96    --  113.25-130.00  19.00   50
 25  \w     58.00  84.00   0.50    0.96    --  113.25-125.00  60.00   52
 26  \w     43.00  68.00   0.50    0.24    --   47.10-130.00  19.00   50
 27  \w    -36.00  28.00   0.50    0.24    --  -47.10  19.00-120.00  128
 28  \w    -83.00 -48.00   0.50    0.24    --  -47.10 139.00 -94.00   70
 29  \w    -73.00 -36.00   0.50    0.24    --  -47.10 -37.00 -90.00   74
 30  \w   -120.00 -90.00   0.50    0.24    --  -47.10 -37.00 -90.00   60
 31  \w   -162.00-114.00   0.50    0.96    --  -91.75 -77.00 120.00   96
 32  \w   -134.00-104.00   0.50    0.96    --  -91.75-130.00  19.00   60
 33  \w   -109.00 -84.00   0.50    0.24    --  -47.10-130.00  19.00   50
 34  \w   -117.00 -92.00   0.50    0.24    --  -47.10-139.00-155.00   50
;
_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      0.1587341000
_diffrn_orient_matrix_UB_12      -0.0582838000
_diffrn_orient_matrix_UB_13      -0.0612020000
_diffrn_orient_matrix_UB_21      -0.1149385000
_diffrn_orient_matrix_UB_22      -0.0850250000
_diffrn_orient_matrix_UB_23      0.0362241000
_diffrn_orient_matrix_UB_31      -0.1423573000
_diffrn_orient_matrix_UB_32      0.0035675000
_diffrn_orient_matrix_UB_33      -0.1452751000
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6794
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.244
_diffrn_reflns_theta_min         5.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.88a (Rigaku Oxford Diffraction, 2023)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         1949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0502P)^2^+0.2707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1760
_reflns_number_total             1949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03909a2.cif
_cod_data_source_block           js323e
_cod_database_code               7132071
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C2N2H3O2
_chemical_oxdiff_usercomment     SOHAN-480-Hz
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.833
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_shelx_res_checksum              55712
_shelx_hkl_checksum              77628
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id SOHAN-480-HZ
_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 1.573
_oxdiff_exptl_absorpt_empirical_full_min 0.770