Improving stability of the metal-free primary energetic cyanuric triazide (CTA) through cocrystallization.
Foroughi, Leila M.; Wiscons, Ren A.; Du Bois, Derek R.; Matzger, Adam J.; Chemical communications (Cambridge, England) 56 (2020) 2111–2114; doi:10.1039/c9cc09465b

data_7125861
_publ_section_title
;
 Improving stability of the metal-free primary energetic cyanuric triazide
 (CTA) through cocrystallization.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2111
_journal_page_last               2114
_journal_paper_doi               10.1039/c9cc09465b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C3 N12, 0.5(C6 N6 O6)'
_chemical_formula_sum            'C6 N15 O3'
_chemical_formula_weight         330.21
_chemical_name_systematic
'2:1 cyanuric triazide/benzotrifuroxan cocrystal'
_chemical_properties_physical    'Heat-sensitive,impact sensitive energetic'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-06
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_audit_update_record
;
2019-12-03 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1063(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6224(3)
_cell_length_b                   11.4096(3)
_cell_length_c                   12.9021(3)
_cell_measurement_reflns_used    8461
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.5920
_cell_measurement_theta_min      4.6680
_cell_volume                     2428.15(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.5a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.5a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.5a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -20.00  64.00   0.50    3.00    --   50.49 -59.00 -71.00  168
  2  \w     34.00 119.00   0.50    4.00    --  105.75 -59.00 -71.00  170
  3  \w     37.00 122.00   0.50    3.00    --   50.49  59.00  68.00  170
  4  \w     92.00 178.00   0.50    4.00    --  105.75  59.00  68.00  172
  5  \w     71.00 122.00   0.50    3.00    --   50.49 125.00 120.00  102
  6  \w     71.00 122.00   0.50    3.00    --   50.49 125.00 150.00  102
  7  \w     71.00 122.00   0.50    3.00    --   50.49 125.00   0.00  102
  8  \w     30.00 118.00   0.50    3.00    --   50.49  77.00 -30.00  176
  9  \w     33.00  69.00   0.50    4.00    --  105.75 -37.00 -60.00   72
 10  \w     33.00  69.00   0.50    4.00    --  105.75 -37.00 -90.00   72
 11  \w     34.00 106.00   0.50    4.00    --  105.75 -57.00-150.00  144
 12  \w     34.00 116.00   0.50    4.00    --  105.75-125.00-120.00  164
 13  \w     33.00  69.00   0.50    4.00    --  105.75 -37.00 -30.00   72
 14  \w     33.00  69.00   0.50    4.00    --  105.75 -37.00  60.00   72
 15  \w     33.00  69.00   0.50    4.00    --  105.75 -37.00  90.00   72
 16  \w     33.00  69.00   0.50    4.00    --  105.75 -37.00 150.00   72
 17  \w    -64.00  22.00   0.50    3.00    --  -50.49  59.00  68.00  172
 18  \w    -76.00 -32.00   0.50    4.00    -- -105.75  19.00 120.00   88
 19  \w   -119.00 -34.00   0.50    4.00    -- -105.75  59.00  68.00  170
 20  \w   -121.00 -37.00   0.50    3.00    --  -50.49 -59.00 -71.00  168
 21  \w   -177.00 -92.00   0.50    4.00    -- -105.75 -59.00 -71.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0607277000
_diffrn_orient_matrix_UB_12      0.0943563000
_diffrn_orient_matrix_UB_13      0.0257134000
_diffrn_orient_matrix_UB_21      -0.0399105000
_diffrn_orient_matrix_UB_22      -0.0017820000
_diffrn_orient_matrix_UB_23      -0.1142817000
_diffrn_orient_matrix_UB_31      -0.0586789000
_diffrn_orient_matrix_UB_32      -0.0965974000
_diffrn_orient_matrix_UB_33      0.0274140000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11321
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         4.713
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.5a (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_description       blade
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method 'slurry w/ 1:1 isooctane:toluene'
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0390P)^2^+0.9230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1964
_reflns_number_total             2132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09465b2.cif
_cod_data_source_block           exp_760_cta-btf
_cod_depositor_comments
'Adding full bibliography for 7125861--7125862.cif.'
_cod_database_code               7125861
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C N O'
_diffrn_oxdiff_ac3_digest_frames
;
015ffa6c562eb7665d82cb57da475979b8026704058
;
_diffrn_oxdiff_ac3_digest_hkl
;
01f69163a5b057b872564bc4e7428f3861ee82
;
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_olex2_refinement_description
;
1. Others
 Fixed Sof: C4(0.5) C5(0.5) C6(0.5) C7(0.5) C8(0.5) C9(0.5) N13(0.5) N17(0.5)
 N15(0.5) N14(0.5) N18(0.5) N16(0.5) O4(0.5) O6(0.5) O2(0.5) O1(0.5) O3(0.5)
 O5(0.5)
;
_olex2_exptl_crystal_mounting_method 'MiTeGen MicroMount w/ mineral oil'
_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 1.488
_oxdiff_exptl_absorpt_empirical_full_min 0.715