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_7714836
_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_formula_moiety         'C6 H12 N4 O2'
_chemical_formula_sum            'C6 H12 N4 O2'
_chemical_formula_weight         172.20
_chemical_melting_point          423
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-31
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2689(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.80690(8)
_cell_length_b                   5.75687(6)
_cell_length_c                   17.86698(18)
_cell_measurement_reflns_used    5130
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.8210
_cell_measurement_theta_min      4.9530
_cell_volume                     800.773(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.950
_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    -17.00  13.00   0.50    0.05    --   47.62 -19.00  30.00   60
  2  \w    -25.00  23.00   0.50    0.05    --   47.62 -19.00 -30.00   96
  3  \w    -23.00   2.00   0.50    0.05    --   47.62 -19.00-180.00   50
  4  \w    114.00 178.00   0.50    0.08    --  107.19  37.00-180.00  128
  5  \w    132.00 157.00   0.50    0.08    --  107.19  57.00 -30.00   50
  6  \w     37.00  62.00   0.50    0.08    --  107.19 -57.00 -60.00   50
  7  \w     65.00 104.00   0.50    0.08    --  107.19 -99.00-120.00   78
  8  \w     76.00 101.00   0.50    0.08    --  107.19-125.00  30.00   50
  9  \w     43.00  71.00   0.50    0.08    --  107.19-125.00  30.00   56
 10  \w     71.00 104.00   0.50    0.08    --  107.19 -99.00 -60.00   66
 11  \w     64.00 104.00   0.50    0.08    --  107.19 -99.00-180.00   80
 12  \w     74.00 100.00   0.50    0.08    --  107.19 -99.00 120.00   52
 13  \w     77.00 105.00   0.50    0.08    --  107.19 -77.00 150.00   56
 14  \w     36.00  62.00   0.50    0.08    --  107.19 -77.00 150.00   52
 15  \w     35.00  85.00   0.50    0.08    --  107.19 -99.00 150.00  100
 16  \w     50.00 104.00   0.50    0.08    --  107.19 -99.00  60.00  108
 17  \w     43.00  90.00   0.50    0.08    --  107.19 -99.00  30.00   94
 18  \w    -24.00  16.00   0.50    0.05    --  -47.62  19.00-180.00   80
 19  \w    -69.00   0.00   0.50    0.05    --  -47.62  77.00-180.00  138
 20  \w    -61.00  -9.00   0.50    0.05    --  -47.62  57.00  60.00  104
 21  \w    -43.00  26.00   0.50    0.05    --  -47.62  37.00 120.00  138
 22  \w    -67.00 -26.00   0.50    0.08    --  -91.75  57.00 -30.00   82
 23  \w    -67.00 -32.00   0.50    0.08    --  -91.75  57.00 -60.00   70
 24  \w    -65.00 -25.00   0.50    0.08    --  -91.75  57.00-120.00   80
 25  \w    -46.00 -20.00   0.50    0.08    --  -91.75  57.00-180.00   52
 26  \w   -148.00-123.00   0.50    0.08    --  -91.75 -37.00 -60.00   50
 27  \w   -156.00-131.00   0.50    0.08    --  -91.75 -57.00-120.00   50
 28  \w   -162.00-127.00   0.50    0.08    --  -91.75 -57.00-150.00   70
 29  \w   -163.00-128.00   0.50    0.08    --  -91.75 -57.00-180.00   70
 30  \w   -159.00-131.00   0.50    0.08    --  -91.75 -57.00 -90.00   56
 31  \w   -163.00-130.00   0.50    0.08    --  -91.75 -57.00 -60.00   66
 32  \w   -160.00-131.00   0.50    0.08    --  -91.75 -57.00 -30.00   58
 33  \w   -163.00-138.00   0.50    0.08    --  -91.75 -77.00 120.00   50
 34  \w   -150.00-114.00   0.50    0.08    --  -91.75-125.00 120.00   72
 35  \w   -163.00-137.00   0.50    0.08    --  -91.75 -99.00 -30.00   52
;
_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      0.0015288000
_diffrn_orient_matrix_UB_12      0.0340815000
_diffrn_orient_matrix_UB_13      -0.0854679000
_diffrn_orient_matrix_UB_21      -0.1233101000
_diffrn_orient_matrix_UB_22      0.2077335000
_diffrn_orient_matrix_UB_23      0.0041367000
_diffrn_orient_matrix_UB_31      0.1547804000
_diffrn_orient_matrix_UB_32      0.1652005000
_diffrn_orient_matrix_UB_33      0.0123958000
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7110
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.992
_diffrn_reflns_theta_min         4.964
_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    0.923
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0402P)^2^+0.3186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1532
_reflns_number_total             1607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03954d2.cif
_cod_data_source_block           js122f
_cod_depositor_comments
'Adding full bibliography for 7714833--7714836.cif.'
_cod_database_code               7714836
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C6H12N4O2
_chemical_oxdiff_usercomment     SOHAN-45
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.812
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_shelx_res_checksum              89967
_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-45
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.863