Trinitromethyl-Triazolone (TNMTO): A Highly Dense Oxidizer
Lal, Sohan; Staples, Richard J.; Shreeve, Jean'ne M.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02232C

data_7713697
_publ_section_title
;
 Trinitromethyl-Triazolone (TNMTO): A Highly Dense Oxidizer
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02232C
_journal_year                    2023
_chemical_formula_moiety         'C3 H2 N6 O7'
_chemical_formula_sum            'C3 H2 N6 O7'
_chemical_formula_weight         234.11
_chemical_melting_point          353
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-07 deposited with the CCDC.	2023-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.573(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4982(2)
_cell_length_b                   7.1276(2)
_cell_length_c                   13.8819(4)
_cell_measurement_reflns_used    4363
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.4490
_cell_measurement_theta_min      6.5470
_cell_volume                     817.37(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (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      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 0.982
_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    -76.00  26.00   0.50    0.50    --  -46.85  91.00 112.00  204
  2  \w    -18.00  76.00   0.50    0.50    --   46.85 -91.00  -1.00  188
  3  \w    -78.00 -19.00   0.50    2.00    --  -91.75  91.00 112.00  118
  4  \w     42.00 104.00   0.50    2.00    --  113.25 -91.00  -1.00  124
  5  \w    103.00 178.00   0.50    2.00    --  113.25  91.00 112.00  150
  6  \w    -39.00  29.00   0.50    0.50    --  -46.85  19.00-120.00  136
  7  \w    -27.00  38.00   0.50    0.50    --   46.85 -19.00 -90.00  130
  8  \w    -27.00  38.00   0.50    0.50    --   46.85 -19.00 -30.00  130
  9  \w    -53.00 -20.00   0.50    2.00    --  -91.75  45.00 -60.00   66
 10  \w   -163.00 -81.00   0.50    2.00    --  -91.75 -91.00  -1.00  164
 11  \w     44.00 108.00   0.50    2.00    --  113.25-125.00 -30.00  128
 12  \w     42.00  94.00   0.50    2.00    --  113.25 -77.00 150.00  104
 13  \w     42.00  94.00   0.50    2.00    --  113.25 -77.00-150.00  104
 14  \w     42.00  94.00   0.50    2.00    --  113.25 -77.00  30.00  104
 15  \w     42.00  69.00   0.50    2.00    --  113.25 -61.00  90.00   54
 16  \w    110.00 178.00   0.50    2.00    --  113.25  77.00 150.00  136
 17  \w     42.00  94.00   0.50    2.00    --  113.25 -77.00-180.00  104
 18  \w     42.00  69.00   0.50    2.00    --  113.25 -61.00  30.00   54
 19  \w     42.00  69.00   0.50    2.00    --  113.25 -61.00-120.00   54
 20  \w    101.00 178.00   0.50    2.00    --  113.25  45.00 150.00  154
 21  \w     42.00  94.00   0.50    2.00    --  113.25 -77.00  60.00  104
 22  \w     42.00  69.00   0.50    2.00    --  113.25 -61.00  60.00   54
 23  \w    106.00 178.00   0.50    2.00    --  113.25  61.00   0.00  144
 24  \w     42.00  94.00   0.50    2.00    --  113.25 -77.00   0.00  104
 25  \w     42.00  94.00   0.50    2.00    --  113.25 -77.00  90.00  104
 26  \w     42.00  69.00   0.50    2.00    --  113.25 -61.00 150.00   54
 27  \w   -120.00 -34.00   0.50    0.50    --  -46.85 -37.00  60.00  172
 28  \w     35.00 110.00   0.50    0.50    --   46.85  37.00 -90.00  150
;
_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      -0.0229542000
_diffrn_orient_matrix_UB_12      -0.1126704000
_diffrn_orient_matrix_UB_13      -0.0969821000
_diffrn_orient_matrix_UB_21      -0.0740625000
_diffrn_orient_matrix_UB_22      -0.1629770000
_diffrn_orient_matrix_UB_23      0.0474217000
_diffrn_orient_matrix_UB_31      -0.1696200000
_diffrn_orient_matrix_UB_32      0.0864799000
_diffrn_orient_matrix_UB_33      -0.0370703000
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8681
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.393
_diffrn_reflns_theta_min         5.585
_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    1.682
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.91a (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    1.902
_exptl_crystal_description       needle
_exptl_crystal_F_000             472
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0793P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1461
_reflns_number_total             1751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02232c2.cif
_cod_data_source_block           js623a
_cod_database_code               7713697
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C3H2N6O7
_chemical_oxdiff_usercomment     SOHAN-630
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
;
_shelx_res_checksum              96331
_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-630
_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 1.419
_oxdiff_exptl_absorpt_empirical_full_min 0.772