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

data_7713698
_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         'C4 H2 N5 O6, H4 N, H2 O'
_chemical_formula_sum            'C4 H8 N6 O7'
_chemical_formula_weight         252.16
_chemical_melting_point          506
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 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                 96.6790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.26070(10)
_cell_length_b                   9.13530(10)
_cell_length_c                   12.5011(2)
_cell_measurement_reflns_used    3564
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.4620
_cell_measurement_theta_min      5.9930
_cell_volume                     936.98(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.80a (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      100.00(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 0.981
_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    -53.00 -20.00   0.50    0.19    --  -91.75  45.00 120.00   66
  2  \w    -39.00  28.00   0.50    0.05    --  -47.10  19.00  30.00  134
  3  \w    -78.00  12.00   0.50    0.05    --  -47.10 102.00 -71.00  180
  4  \w    -79.00 -21.00   0.50    0.19    --  -91.75 102.00 -71.00  116
  5  \w    -39.00  28.00   0.50    0.05    --  -47.10  19.00 -90.00  134
  6  \w   -120.00 -35.00   0.50    0.05    --  -47.10 -37.00 -90.00  170
  7  \w   -120.00 -35.00   0.50    0.05    --  -47.10 -37.00  90.00  170
  8  \w   -120.00 -35.00   0.50    0.05    --  -47.10 -37.00   0.00  170
  9  \w   -120.00 -35.00   0.50    0.05    --  -47.10 -37.00-180.00  170
 10  \w   -120.00 -83.00   0.50    0.05    --  -47.10 -37.00-120.00   74
 11  \w   -162.00 -87.00   0.50    0.19    --  -91.75-102.00-174.00  150
 12  \w     42.00  94.00   0.50    0.19    --  113.25 -77.00  60.00  104
 13  \w     42.00  94.00   0.50    0.19    --  113.25 -77.00 120.00  104
 14  \w     42.00  69.00   0.50    0.19    --  113.25 -61.00  30.00   54
 15  \w     42.00  94.00   0.50    0.19    --  113.25 -77.00 -30.00  104
 16  \w     42.00  69.00   0.50    0.19    --  113.25 -61.00   0.00   54
 17  \w     42.00  69.00   0.50    0.19    --  113.25 -61.00 -60.00   54
 18  \w     42.00  69.00   0.50    0.19    --  113.25 -61.00 -30.00   54
 19  \w     42.00  69.00   0.50    0.19    --  113.25 -61.00-120.00   54
 20  \w     42.00  69.00   0.50    0.19    --  113.25 -61.00-180.00   54
 21  \w     42.00  94.00   0.50    0.19    --  113.25 -77.00-150.00  104
 22  \w     42.00 104.00   0.50    0.19    --  113.25 -94.00-120.00  124
 23  \w     10.00  81.00   0.50    0.05    --   47.10-102.00-174.00  142
 24  \w     43.00 104.00   0.50    0.19    --  113.25-102.00-174.00  122
 25  \w     44.00 108.00   0.50    0.19    --  113.25-125.00 -60.00  128
 26  \w     44.00 108.00   0.50    0.19    --  113.25-125.00 -30.00  128
 27  \w    100.00 178.00   0.50    0.19    --  113.25  15.00  30.00  156
 28  \w    106.00 178.00   0.50    0.19    --  113.25  61.00 -30.00  144
 29  \w    108.00 178.00   0.50    0.19    --  113.25 102.00 -71.00  140
;
_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      0.0443529000
_diffrn_orient_matrix_UB_12      -0.0882175000
_diffrn_orient_matrix_UB_13      0.1043171000
_diffrn_orient_matrix_UB_21      -0.0857940000
_diffrn_orient_matrix_UB_22      -0.1354804000
_diffrn_orient_matrix_UB_23      -0.0535380000
_diffrn_orient_matrix_UB_31      0.1610708000
_diffrn_orient_matrix_UB_32      -0.0479712000
_diffrn_orient_matrix_UB_33      -0.0404820000
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5189
_diffrn_reflns_point_group_measured_fraction_full 0.766
_diffrn_reflns_point_group_measured_fraction_max 0.713
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.141
_diffrn_reflns_theta_min         6.014
_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    1.507
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (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    1.788
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.6(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         1465
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0512P)^2^+0.1483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.450
_reflns_Friedel_fraction_full    0.531
_reflns_Friedel_fraction_max     0.444
_reflns_number_gt                1424
_reflns_number_total             1465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02232c2.cif
_cod_data_source_block           js623b
_cod_database_code               7713698
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C5H8N8O10
_chemical_oxdiff_usercomment     SOHAN-626
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4(4)
 0.6(4)
;
_shelx_res_checksum              3766
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id SOHAN-626
_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 1.196
_oxdiff_exptl_absorpt_empirical_full_min 0.853