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_7714834
_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         'C2 H3 N5 O2, H2 O'
_chemical_formula_sum            'C2 H5 N5 O3'
_chemical_formula_weight         147.11
_chemical_melting_point          478
_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             2023-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.652(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.16088(12)
_cell_length_b                   8.67413(16)
_cell_length_c                   6.54739(15)
_cell_measurement_reflns_used    2140
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.5270
_cell_measurement_theta_min      7.0460
_cell_volume                     280.810(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.91a 64-bit (release 29-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.92a (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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_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    -62.00 -21.00   0.50    0.06    --  -91.75  61.00  60.00   82
  2  \w    -48.00 -20.00   0.50    0.06    --  -91.75  45.00   0.00   56
  3  \w    -14.00  22.00   0.50    0.05    --  -47.12  87.00-135.00   72
  4  \w    -72.00 -33.00   0.50    0.05    --  -47.12  87.00-135.00   78
  5  \w    -42.00 -17.00   0.50    0.06    --  -91.75  15.00-180.00   50
  6  \w    -77.00 -51.00   0.50    0.06    --  -91.75  87.00-135.00   52
  7  \w     21.00  48.00   0.50    0.05    --   47.12 -87.00 107.00   54
  8  \w    -17.00  12.00   0.50    0.05    --   47.12 -87.00 107.00   58
  9  \w     48.00  92.00   0.50    0.06    --  113.25 -77.00 150.00   88
 10  \w     42.00  67.00   0.50    0.06    --  113.25 -61.00 150.00   50
 11  \w     72.00 104.00   0.50    0.06    --  113.25 -87.00 107.00   64
 12  \w     44.00  69.00   0.50    0.06    --  113.25 -61.00  90.00   50
 13  \w     49.00  91.00   0.50    0.06    --  113.25 -77.00   0.00   84
 14  \w     44.00  69.00   0.50    0.06    --  113.25 -61.00  30.00   50
 15  \w     42.00  67.00   0.50    0.06    --  113.25 -61.00 120.00   50
 16  \w     42.00  67.00   0.50    0.06    --  113.25 -61.00   0.00   50
 17  \w     42.00  89.00   0.50    0.06    --  113.25 -77.00 -60.00   94
 18  \w    -24.00  28.00   0.50    0.05    --   47.12 -19.00-180.00  104
 19  \w     42.00  67.00   0.50    0.06    --  113.25 -61.00-150.00   50
 20  \w     44.00  69.00   0.50    0.06    --  113.25 -61.00-180.00   50
 21  \w    106.00 141.00   0.50    0.06    --  113.25  87.00-135.00   70
 22  \w    150.00 178.00   0.50    0.06    --  113.25  87.00-135.00   56
 23  \w    110.00 171.00   0.50    0.06    --  113.25  61.00-180.00  122
 24  \w    128.00 159.00   0.50    0.06    --  113.25  45.00 150.00   62
 25  \w    -79.00 -38.00   0.50    0.05    --  -47.12 -37.00 120.00   82
 26  \w   -118.00 -89.00   0.50    0.05    --  -47.12 -37.00 120.00   58
 27  \w   -142.00-116.00   0.50    0.06    --  -91.75 -87.00 107.00   52
 28  \w    -51.00 -25.00   0.50    0.06    --  -91.75  87.00-135.00   52
 29  \w   -101.00 -43.00   0.50    0.05    --  -47.12 -37.00  60.00  116
 30  \w    -22.00  38.00   0.50    0.05    --   47.12 -19.00  90.00  120
 31  \w   -136.00 -82.00   0.50    0.06    --  -91.75 -30.00   0.00  108
 32  \w    151.00 176.00   0.50    0.06    --  113.25  30.00   0.00   50
 33  \w    134.00 176.00   0.50    0.06    --  113.25  45.00 -60.00   84
 34  \w     64.00 106.00   0.50    0.06    --  113.25-125.00 120.00   84
 35  \w    103.00 128.00   0.50    0.06    --  113.25  45.00 -60.00   50
 36  \w    127.00 175.00   0.50    0.06    --  113.25  61.00 -90.00   96
 37  \w    119.00 176.00   0.50    0.06    --  113.25  61.00 -30.00  114
 38  \w    107.00 136.00   0.50    0.06    --  113.25  61.00 150.00   58
 39  \w     55.00 107.00   0.50    0.06    --  113.25-125.00 -60.00  104
 40  \w    101.00 127.00   0.50    0.06    --  113.25  30.00   0.00   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      0.0764190000
_diffrn_orient_matrix_UB_12      -0.1550865000
_diffrn_orient_matrix_UB_13      -0.0818034000
_diffrn_orient_matrix_UB_21      0.3020399000
_diffrn_orient_matrix_UB_22      0.0379397000
_diffrn_orient_matrix_UB_23      0.0967009000
_diffrn_orient_matrix_UB_31      -0.0049155000
_diffrn_orient_matrix_UB_32      -0.0777515000
_diffrn_orient_matrix_UB_33      0.2104139000
_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     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2882
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.067
_diffrn_reflns_theta_min         7.059
_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    1.396
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.92a (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    1.740
_exptl_crystal_description       irregular
_exptl_crystal_F_000             152
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.035
_exptl_crystal_size_rad          0.040
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 517 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.17(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1171
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0442P)^2^+0.0492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                1153
_reflns_number_total             1171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03954d2.cif
_cod_data_source_block           js10123d
_cod_depositor_comments
;
Adding full bibliography for 7714833--7714836.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C4 H10 N10 O6'
_cod_original_formula_weight         294.22
_cod_original_formula_moiety         '2(C2 H3 N5 O2), 2(H2 O)'
_cod_original_formula_units_Z            1
_cod_database_code               7714834
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C2H9N7O4
_chemical_oxdiff_usercomment     JMS-SOHAN-800-HA
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.818
_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              41412
_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 'JMS-SOHAN-800 HA'
_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 1.124
_oxdiff_exptl_absorpt_empirical_full_min 0.858