Very thermostable energetic materials based on a fused-triazole: 3,6-diamino-1H-[1,2,4]triazolo[4,3-b][1,2,4]triazole
Tang, Yongxing; An, Ziwei; Chinnam, Ajay Kumar; Staples, Richard J.; Shreeve, Jean'ne M.; New Journal of Chemistry 45 (2021) 85–91; doi:10.1039/D0NJ05152G

data_7060098
_publ_section_title
;
 Very thermostable energetic materials based on a fused-triazole:
 3,6-diamino-1H-[1,2,4]triazolo[4,3-b][1,2,4]triazole
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              85
_journal_page_last               91
_journal_paper_doi               10.1039/D0NJ05152G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C3 H5 N7'
_chemical_formula_sum            'C3 H5 N7'
_chemical_formula_weight         139.14
_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             2020-10-08
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2020-10-09 deposited with the CCDC.	2020-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.468(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5503(4)
_cell_length_b                   3.56337(11)
_cell_length_c                   14.3130(5)
_cell_measurement_reflns_used    3273
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      76.3800
_cell_measurement_theta_min      4.6650
_cell_volume                     523.29(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (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 0.976
_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    119.00 177.00   0.50    0.05    --  107.11  37.00 150.00  116
  2  \w    150.00 177.00   0.50    0.05    --  107.11  37.00  90.00   54
  3  \w    118.00 144.00   0.50    0.05    --  107.11  37.00  90.00   52
  4  \w    127.00 177.00   0.50    0.05    --  107.11  77.00  30.00  100
  5  \w    134.00 160.00   0.50    0.05    --  107.11  57.00-180.00   52
  6  \w    -27.00   5.00   0.50    0.05    --  -47.45  19.00 120.00   64
  7  \w    -22.00  15.00   0.50    0.05    --  -47.45  19.00 -30.00   74
  8  \w    -61.00 -29.00   0.50    0.05    --  -47.45  57.00-120.00   64
  9  \w    -21.00  15.00   0.50    0.05    --  -47.45  57.00-120.00   72
 10  \w    -43.00 -18.00   0.50    0.05    --  -86.25  37.00 -30.00   50
 11  \w    -69.00 -30.00   0.50    0.05    --  -47.45 125.00   0.00   78
 12  \w    -17.00  12.00   0.50    0.05    --  -47.45 102.00  -5.00   58
 13  \w    -73.00 -22.00   0.50    0.05    --  -47.45 102.00  -5.00  102
 14  \w    -77.00 -40.00   0.50    0.05    --  -86.25 102.00  -5.00   74
 15  \w    -43.00 -17.00   0.50    0.05    --  -86.25  37.00  30.00   52
 16  \w   -151.00-116.00   0.50    0.05    --  -86.25 -37.00 150.00   70
 17  \w   -159.00-116.00   0.50    0.05    --  -86.25 -37.00 120.00   86
 18  \w   -157.00-131.00   0.50    0.05    --  -86.25 -37.00  90.00   52
 19  \w   -157.00-128.00   0.50    0.05    --  -86.25 -77.00   0.00   58
 20  \w   -158.00-114.00   0.50    0.05    --  -86.25 -37.00   0.00   88
 21  \w   -159.00-120.00   0.50    0.05    --  -86.25 -37.00 -90.00   78
 22  \w   -159.00-134.00   0.50    0.05    --  -86.25 -57.00 -90.00   50
 23  \w   -124.00 -99.00   0.50    0.05    --  -86.25-102.00-108.00   50
 24  \w     37.00  65.00   0.50    0.05    --  107.11 -57.00 150.00   56
 25  \w     42.00  86.00   0.50    0.05    --  107.11 -77.00  90.00   88
 26  \w     38.00  63.00   0.50    0.05    --  107.11 -57.00  90.00   50
 27  \w     35.00  60.00   0.50    0.05    --  107.11 -57.00  30.00   50
 28  \w    109.00 162.00   0.50    0.05    --  107.11 102.00  -5.00  106
 29  \w     39.00  65.00   0.50    0.05    --  107.11 -57.00 -30.00   52
 30  \w     39.00  64.00   0.50    0.05    --  107.11 -57.00 -60.00   50
 31  \w     -4.00  22.00   0.50    0.05    --   47.45 -19.00-120.00   52
 32  \w     39.00  64.00   0.50    0.05    --  107.11 -99.00 -30.00   50
 33  \w     77.00 108.00   0.50    0.05    --  107.11-125.00  90.00   62
 34  \w     38.00  69.00   0.50    0.05    --  107.11-125.00  90.00   62
 35  \w     24.00  51.00   0.50    0.05    --   47.45-102.00-108.00   54
 36  \w     75.00 102.00   0.50    0.05    --  107.11-125.00-150.00   54
 37  \w     75.00 108.00   0.50    0.05    --  107.11-125.00-180.00   66
 38  \w     49.00  74.00   0.50    0.05    --  107.11-125.00-180.00   50
 39  \w     41.00  66.00   0.50    0.05    --  107.11-125.00-150.00   50
 40  \w     61.00 100.00   0.50    0.05    --  107.11-102.00-108.00   78
 41  \w     79.00 104.00   0.50    0.05    --  107.11 -99.00 -30.00   50
 42  \w     36.00 100.00   0.50    0.05    --  107.11 -99.00 -60.00  128
;
_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      -0.1281967000
_diffrn_orient_matrix_UB_12      0.2244061000
_diffrn_orient_matrix_UB_13      -0.0266138000
_diffrn_orient_matrix_UB_21      -0.0708549000
_diffrn_orient_matrix_UB_22      -0.3482088000
_diffrn_orient_matrix_UB_23      -0.0507580000
_diffrn_orient_matrix_UB_31      -0.0331330000
_diffrn_orient_matrix_UB_32      -0.1236954000
_diffrn_orient_matrix_UB_33      0.0946644000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4889
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.646
_diffrn_reflns_theta_min         4.721
_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    1.134
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.766
_exptl_crystal_description       needle
_exptl_crystal_F_000             288
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0191(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0439P)^2^+0.2307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1009
_reflns_number_total             1079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05152g2.cif
_cod_data_source_block           js1020f
_cod_depositor_comments
'Adding full bibliography for 7060097--7060098.cif.'
_cod_database_code               7060098
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C3H5N7
_chemical_oxdiff_usercomment     YT1
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.863
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_shelx_res_checksum              62257
_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 YT1
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.802