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_7132070
_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 N7 O8'
_chemical_formula_sum            'C3 H N7 O8'
_chemical_formula_weight         263.11
_chemical_melting_point          373
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-03 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.206(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5694(2)
_cell_length_b                   20.2409(5)
_cell_length_c                   6.5938(2)
_cell_measurement_reflns_used    5504
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      79.7330
_cell_measurement_theta_min      6.7410
_cell_volume                     874.42(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(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 0.981
_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    119.00 172.00   0.50    1.20    --  113.25  61.00-150.00  106
  2  \w    114.00 143.00   0.50    1.20    --  113.25  61.00  30.00   58
  3  \w    147.00 173.00   0.50    1.20    --  113.25  61.00  30.00   52
  4  \w    110.00 178.00   0.50    1.20    --  113.25  77.00  60.00  136
  5  \w    104.00 152.00   0.50    1.20    --  113.25  45.00  90.00   96
  6  \w    100.00 158.00   0.50    1.20    --  113.25  56.00 141.00  116
  7  \w     34.00  60.00   0.50    0.30    --   47.10  56.00 141.00   52
  8  \w     78.00 105.00   0.50    0.30    --   47.10  56.00 141.00   54
  9  \w    115.00 174.00   0.50    1.20    --  113.25  15.00 -60.00  118
 10  \w     58.00  84.00   0.50    1.20    --  113.25 -77.00  30.00   52
 11  \w     55.00  94.00   0.50    1.20    --  113.25 -77.00  90.00   78
 12  \w     42.00  68.00   0.50    1.20    --  113.25 -77.00   0.00   52
 13  \w     42.00  87.00   0.50    1.20    --  113.25 -77.00  60.00   90
 14  \w     45.00  86.00   0.50    1.20    --  113.25 -77.00 -60.00   82
 15  \w     52.00  83.00   0.50    1.20    --  113.25 -77.00 -90.00   62
 16  \w     49.00  87.00   0.50    1.20    --  113.25 -77.00-150.00   76
 17  \w     43.00  68.00   0.50    1.20    --  113.25 -77.00-120.00   50
 18  \w     42.00  67.00   0.50    1.20    --  113.25 -61.00 -60.00   50
 19  \w     43.00  68.00   0.50    1.20    --  113.25 -61.00 -30.00   50
 20  \w     42.00  68.00   0.50    1.20    --  113.25 -61.00   0.00   52
 21  \w     42.00  67.00   0.50    1.20    --  113.25 -61.00  30.00   50
 22  \w     42.00  67.00   0.50    1.20    --  113.25 -61.00  90.00   50
 23  \w     43.00  69.00   0.50    1.20    --  113.25 -61.00 120.00   52
 24  \w     42.00  67.00   0.50    1.20    --  113.25 -61.00 150.00   50
 25  \w     -3.00  61.00   0.50    0.30    --   47.10 -56.00  -1.00  128
 26  \w     47.00  79.00   0.50    1.20    --  113.25-125.00 -60.00   64
 27  \w     83.00 108.00   0.50    1.20    --  113.25-125.00 -60.00   50
 28  \w     53.00  79.00   0.50    1.20    --  113.25-125.00   0.00   52
 29  \w     46.00  95.00   0.50    1.20    --  113.25-125.00  30.00   98
 30  \w     82.00 108.00   0.50    1.20    --  113.25-125.00   0.00   52
 31  \w     50.00  88.00   0.50    0.30    --   47.10-125.00-150.00   76
 32  \w    -39.00  -1.00   0.50    0.30    --  -47.10  19.00 -60.00   76
 33  \w    -47.00  25.00   0.50    0.30    --  -47.10  56.00 141.00  144
 34  \w    -58.00 -33.00   0.50    1.20    --  -91.75  56.00 141.00   50
 35  \w   -135.00-108.00   0.50    1.20    --  -91.75 -94.00 120.00   54
 36  \w   -142.00-116.00   0.50    1.20    --  -91.75 -56.00  -1.00   52
 37  \w   -118.00 -32.00   0.50    0.30    --  -47.10 -56.00  -1.00  172
;
_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      -0.0370503914
_diffrn_orient_matrix_UB_12      -0.0175215597
_diffrn_orient_matrix_UB_13      0.2216392098
_diffrn_orient_matrix_UB_21      0.1813860080
_diffrn_orient_matrix_UB_22      -0.0483769306
_diffrn_orient_matrix_UB_23      0.0072028735
_diffrn_orient_matrix_UB_31      0.1450087082
_diffrn_orient_matrix_UB_32      0.0560815522
_diffrn_orient_matrix_UB_33      0.0755007122
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7932
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.468
_diffrn_reflns_theta_min         4.369
_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    1.790
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.86a (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_description       needle
_exptl_crystal_F_000             528
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0468P)^2^+0.1712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7045
_reflns_number_total             7932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03909a2.cif
_cod_data_source_block           js323b2
_cod_database_code               7132070
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C3HN7O8
_chemical_oxdiff_usercomment     SOHAN-480
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.699(5)
 0.301(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
;
_shelx_res_checksum              60549
_shelx_hkl_checksum              54735
_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
_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 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.740