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

data_7713699
_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 N5 O5, H5 N2'
_chemical_formula_sum            'C3 H7 N7 O5'
_chemical_formula_weight         221.16
_chemical_melting_point          451
_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                 94.177(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.63691(18)
_cell_length_b                   17.1203(9)
_cell_length_c                   12.4539(6)
_cell_measurement_reflns_used    2813
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      79.1950
_cell_measurement_theta_min      6.2450
_cell_volume                     773.38(7)
_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    '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_temperature      100.15
_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 0.975
_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    -63.00  25.00   0.50    0.70    --  -47.10  60.00 168.00  176
  2  \w   -119.00 -31.00   0.50    0.70    --  -47.10 -60.00  29.00  176
  3  \w    -69.00 -20.00   0.50    2.80    --  -91.75  60.00 168.00   98
  4  \w   -163.00 -76.00   0.50    2.80    --  -91.75 -60.00  29.00  174
  5  \w     97.00 178.00   0.50    2.80    --  113.25  60.00 168.00  162
  6  \w     42.00  68.00   0.50    2.80    --  113.25 -60.00  29.00   52
  7  \w    -83.00 -15.00   0.50    0.70    --  -47.10 125.00 -90.00  136
  8  \w     36.00  93.00   0.50    0.70    --   47.10-125.00-120.00  114
  9  \w    -24.00  63.00   0.50    0.70    --   47.10 -60.00  29.00  174
 10  \w    -53.00 -20.00   0.50    2.80    --  -91.75  45.00   0.00   66
 11  \w    106.00 178.00   0.50    2.80    --  113.25  61.00  60.00  144
 12  \w     42.00 104.00   0.50    2.80    --  113.25 -94.00   0.00  124
 13  \w     42.00  69.00   0.50    2.80    --  113.25 -61.00 150.00   54
 14  \w     42.00  69.00   0.50    2.80    --  113.25 -61.00  90.00   54
 15  \w     42.00  69.00   0.50    2.80    --  113.25 -61.00-150.00   54
 16  \w     42.00  69.00   0.50    2.80    --  113.25 -61.00-180.00   54
 17  \w     97.00 178.00   0.50    2.80    --  113.25 125.00 -30.00  162
 18  \w    106.00 178.00   0.50    2.80    --  113.25  61.00  90.00  144
 19  \w     42.00  94.00   0.50    2.80    --  113.25 -77.00 120.00  104
 20  \w     42.00  94.00   0.50    2.80    --  113.25 -77.00  30.00  104
 21  \w     42.00  69.00   0.50    2.80    --  113.25 -61.00 -30.00   54
 22  \w     42.00 104.00   0.50    2.80    --  113.25 -94.00 -60.00  124
 23  \w    106.00 178.00   0.50    2.80    --  113.25  61.00 -90.00  144
 24  \w    100.00 178.00   0.50    2.80    --  113.25  15.00-120.00  156
 25  \w     42.00  69.00   0.50    2.80    --  113.25 -61.00  60.00   54
 26  \w   -120.00 -35.00   0.50    0.70    --  -47.10 -37.00 -90.00  170
 27  \w     35.00  98.00   0.50    0.70    --   47.10  37.00 120.00  126
 28  \w     31.00 119.00   0.50    0.70    --   47.10  60.00 168.00  176
;
_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      0.0423852000
_diffrn_orient_matrix_UB_12      0.0098256000
_diffrn_orient_matrix_UB_13      -0.1214885000
_diffrn_orient_matrix_UB_21      -0.2977554000
_diffrn_orient_matrix_UB_22      -0.0627734000
_diffrn_orient_matrix_UB_23      -0.0244863000
_diffrn_orient_matrix_UB_31      -0.2999407000
_diffrn_orient_matrix_UB_32      0.0636760000
_diffrn_orient_matrix_UB_33      -0.0055336000
_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  0.0797
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8241
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         81.103
_diffrn_reflns_theta_min         4.398
_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    1.554
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.748
_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    1.899
_exptl_crystal_description       needle
_exptl_crystal_F_000             456
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.017
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0376P)^2^+0.8038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1318
_reflns_number_total             1657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02232c2.cif
_cod_data_source_block           js623c
_cod_database_code               7713699
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C3H7N7O5
_chemical_oxdiff_usercomment     SOHAN-619
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.774
_olex2_refinement_description
;
;
_shelx_res_checksum              8625
_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-619
_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 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.753