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_7714833
_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 H9 N7 O8'
_chemical_formula_sum            'C6 H9 N7 O8'
_chemical_formula_weight         307.20
_chemical_melting_point          401
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-21
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.2321(2)
_cell_length_b                   10.9604(3)
_cell_length_c                   35.1593(9)
_cell_measurement_reflns_used    3856
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.4960
_cell_measurement_theta_min      5.0170
_cell_volume                     2401.60(12)
_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
;
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 2018/2 (Sheldrick, 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.918
_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   -118.00 -40.00   0.50    1.44    --  -47.62 -30.00-173.00  156
  2  \w    -87.00 -28.00   0.50    5.76    --  -91.75 145.00  12.00  118
  3  \w   -159.00 -84.00   0.50    5.76    --  -91.75 -30.00-173.00  150
  4  \w    138.00 165.00   0.50    5.76    --  107.19  92.00 131.00   54
  5  \w    -79.00 -50.00   0.50    1.44    --  -47.62 125.00 120.00   58
  6  \w    -24.00   2.00   0.50    1.44    --  -47.62  19.00 150.00   52
  7  \w    -67.00 -40.00   0.50    1.44    --  -47.62 125.00 -90.00   54
  8  \w   -162.00-133.00   0.50    5.76    --  -91.75 -77.00 -90.00   58
  9  \w   -153.00-127.00   0.50    5.76    --  -91.75 -57.00 120.00   52
 10  \w   -153.00-126.00   0.50    5.76    --  -91.75 -77.00 -30.00   54
 11  \w   -161.00-135.00   0.50    5.76    --  -91.75 -77.00 120.00   52
 12  \w     80.00 106.00   0.50    5.76    --  107.19-125.00  90.00   52
 13  \w     40.00  66.00   0.50    5.76    --  107.19-125.00  90.00   52
 14  \w     39.00  64.00   0.50    5.76    --  107.19 -57.00  90.00   50
 15  \w     35.00  60.00   0.50    5.76    --  107.19 -57.00   0.00   50
;
_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      -0.2399408000
_diffrn_orient_matrix_UB_12      0.0035684000
_diffrn_orient_matrix_UB_13      0.0104440000
_diffrn_orient_matrix_UB_21      0.0565783000
_diffrn_orient_matrix_UB_22      0.0554811000
_diffrn_orient_matrix_UB_23      0.0389910000
_diffrn_orient_matrix_UB_31      -0.0176628000
_diffrn_orient_matrix_UB_32      0.1291003000
_diffrn_orient_matrix_UB_33      -0.0170608000
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            8297
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.295
_diffrn_reflns_theta_min         2.513
_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    1.395
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.872
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+1.7068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2042
_reflns_number_total             2332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03954d2.cif
_cod_data_source_block           js222b
_cod_depositor_comments
'Adding full bibliography for 7714833--7714836.cif.'
_cod_database_code               7714833
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C6H9N7O8
_chemical_oxdiff_usercomment     'Colorless Blocks'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.846
_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              55443
_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-143
_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 1.185
_oxdiff_exptl_absorpt_empirical_full_min 0.828