Nitroiminotriazole (NIT) based potential solid propellants: synthesis, characterization, and applications.
Lal, Sohan; Staples, Richard J.; Shreeve, Jean'ne M.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 903–907; doi:10.1039/d3dt03954d

data_7714835
_publ_section_title
;
 Nitroiminotriazole (NIT) based potential solid propellants: synthesis,
 characterization, and applications.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              903
_journal_page_last               907
_journal_paper_doi               10.1039/d3dt03954d
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C2 H2 K N5 O2'
_chemical_formula_sum            'C2 H2 K N5 O2'
_chemical_formula_weight         167.19
_chemical_melting_point          533
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2041(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.07223(5)
_cell_length_b                   10.00743(14)
_cell_length_c                   6.99455(9)
_cell_measurement_reflns_used    4771
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.3940
_cell_measurement_theta_min      6.5190
_cell_volume                     276.331(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.99a (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(2)
_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 0.991
_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     66.00  92.00   0.50    0.05    --  113.25 -94.00-120.00   52
  2  \w     44.00 108.00   0.50    0.05    --  113.25-125.00  90.00  128
  3  \w     64.00 108.00   0.50    0.05    --  113.25-125.00 120.00   88
  4  \w     42.00 104.00   0.50    0.05    --  113.25 -94.00   0.00  124
  5  \w     42.00  94.00   0.50    0.05    --  113.25 -77.00   0.00  104
  6  \w     50.00  94.00   0.50    0.05    --  113.25 -77.00  90.00   88
  7  \w     42.00  69.00   0.50    0.05    --  113.25 -61.00 -90.00   54
  8  \w     42.00  69.00   0.50    0.05    --  113.25 -61.00-150.00   54
  9  \w     42.00  69.00   0.50    0.05    --  113.25 -61.00-180.00   54
 10  \w     42.00  94.00   0.50    0.05    --  113.25 -77.00-120.00  104
 11  \w     43.00  68.00   0.50    0.05    --  113.25 -61.00 -60.00   50
 12  \w     42.00  69.00   0.50    0.05    --  113.25 -61.00 150.00   54
 13  \w    -27.00  40.00   0.50    0.05    --   47.11 -27.00 142.00  134
 14  \w    110.00 178.00   0.50    0.05    --  113.25  77.00  30.00  136
 15  \w    101.00 178.00   0.50    0.05    --  113.25  45.00   0.00  154
 16  \w    126.00 170.00   0.50    0.05    --  113.25  77.00 -60.00   88
 17  \w    117.00 156.00   0.50    0.05    --  113.25  61.00   0.00   78
 18  \w    106.00 178.00   0.50    0.05    --  113.25  61.00  60.00  144
 19  \w    110.00 178.00   0.50    0.05    --  113.25  77.00 120.00  136
 20  \w    108.00 133.00   0.50    0.05    --  113.25  45.00 120.00   50
 21  \w    101.00 178.00   0.50    0.05    --  113.25  45.00  90.00  154
 22  \w    101.00 178.00   0.50    0.05    --  113.25  45.00  60.00  154
 23  \w    101.00 178.00   0.50    0.05    --  113.25  27.00 -54.00  154
 24  \w    101.00 178.00   0.50    0.05    --  113.25  45.00-180.00  154
 25  \w     35.00 121.00   0.50    0.05    --   47.11  27.00 -54.00  172
 26  \w     35.00 120.00   0.50    0.05    --   47.11  37.00   0.00  170
 27  \w     35.00 119.00   0.50    0.05    --   47.11  46.00  75.38  168
 28  \w     35.00 120.00   0.50    0.05    --   47.11  37.00 150.00  170
 29  \w    -41.00  28.00   0.50    0.05    --  -47.11  27.00 -54.00  138
 30  \w    -47.00  26.00   0.50    0.05    --  -47.11  37.00   0.00  146
 31  \w    -53.00 -20.00   0.50    0.05    --  -91.75  45.00 -60.00   66
 32  \w   -119.00 -34.00   0.50    0.05    --  -47.11 -45.00 -23.31  170
 33  \w   -120.00 -35.00   0.50    0.05    --  -47.11 -37.00  30.00  170
 34  \w   -121.00 -35.00   0.50    0.05    --  -47.11 -27.00 142.00  172
 35  \w   -163.00 -88.00   0.50    0.05    --  -91.75 -48.00  60.46  150
 36  \w   -163.00 -79.00   0.50    0.05    --  -91.75 -45.00  90.00  168
 37  \w   -163.00 -82.00   0.50    0.05    --  -91.75 -47.00 -18.07  162
 38  \w   -163.00 -79.00   0.50    0.05    --  -91.75 -45.00 -30.00  168
 39  \w   -163.00 -79.00   0.50    0.05    --  -91.75 -45.00   0.00  168
 40  \w   -163.00 -79.00   0.50    0.05    --  -91.75 -45.00  30.00  168
 41  \w   -163.00 -79.00   0.50    0.05    --  -91.75 -45.00  60.00  168
 42  \w   -166.00 -79.00   0.50    0.05    --  -91.75 -27.00 142.00  174
 43  \w   -166.00 -79.00   0.50    0.05    --  -91.75 -30.00  60.00  174
 44  \w   -161.00 -94.00   0.50    0.05    --  -91.75-125.00 -60.00  134
;
_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      -0.3771276000
_diffrn_orient_matrix_UB_12      -0.0385878000
_diffrn_orient_matrix_UB_13      -0.0669066000
_diffrn_orient_matrix_UB_21      0.0474629000
_diffrn_orient_matrix_UB_22      -0.0374214000
_diffrn_orient_matrix_UB_23      -0.2051914000
_diffrn_orient_matrix_UB_31      0.0886027000
_diffrn_orient_matrix_UB_32      -0.1441950000
_diffrn_orient_matrix_UB_33      0.0712213000
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5570
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.665
_diffrn_reflns_theta_min         6.528
_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    8.001
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.99a (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    2.009
_exptl_crystal_description       irregular
_exptl_crystal_F_000             168
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 479 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(9)
_refine_ls_extinction_coef       0.014(3)
_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   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1123
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0493P)^2^+0.0668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.927
_reflns_Friedel_fraction_max     0.856
_reflns_number_gt                1117
_reflns_number_total             1123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03954d2.cif
_cod_data_source_block           js923b
_cod_depositor_comments
'Adding full bibliography for 7714833--7714836.cif.'
_cod_database_code               7714835
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C4H4K3N10O4
_chemical_oxdiff_usercomment     SOHAN-800-K
_shelx_estimated_absorpt_t_max   0.526
_shelx_estimated_absorpt_t_min   0.354
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2)
;
_shelx_res_checksum              46870
_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-800-K
_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 1.305
_oxdiff_exptl_absorpt_empirical_full_min 0.823