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_7125862
_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
'2,4,6-triazido-1,3,5-triazine benzenetrifuroxan'
_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             2019-09-19
_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                 97.727(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0625(14)
_cell_length_b                   11.4704(11)
_cell_length_c                   13.0200(10)
_cell_measurement_reflns_used    1338
_cell_measurement_temperature    298.4(4)
_cell_measurement_theta_max      59.1110
_cell_measurement_theta_min      5.2350
_cell_volume                     2525.1(4)
_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      air
_diffrn_ambient_temperature      298.4(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_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     -7.00  19.00   0.50    7.00    --    4.27 -80.00  65.00   52
  2  \w    -24.00  27.00   0.50    7.00    --   -4.27 -99.00 150.00  102
  3  \w    -58.00 -32.00   0.50    7.00    --   -4.27 -80.00  65.00   52
  4  \w    -25.00  24.00   0.50    7.00    --   -4.27 -99.00 -90.00   98
  5  \w    -65.00 -14.00   0.50    7.00    --    4.27 -80.00  65.00  102
  6  \w     54.00  82.00   0.50   55.00    --  105.75 -80.00  65.00   56
  7  \w     80.00 106.00   0.50   55.00    --  105.75 -57.00  90.00   52
  8  \w     42.00 106.00   0.50   55.00    --  105.75 -57.00  60.00  128
  9  \w     33.00  69.00   0.50   55.00    --  105.75 -37.00 -90.00   72
 10  \w     34.00  73.00   0.50   55.00    --  105.75 -19.00-120.00   78
 11  \w     32.00  74.00   0.50   55.00    --  105.75 -19.00-150.00   84
 12  \w     34.00  66.00   0.50   55.00    --  105.75 -37.00-150.00   64
 13  \w     85.00 170.00   0.50   55.00    --  105.75  77.00-150.00  170
 14  \w     86.00 172.00   0.50   55.00    --  105.75  80.00-171.00  172
 15  \w     37.00  67.00   0.50   55.00    --  105.75 -57.00  90.00   60
 16  \w     32.00  76.00   0.50   55.00    --  105.75 -19.00  90.00   88
 17  \w      1.00  28.00   0.50    7.00    --    4.27  80.00-171.00   54
 18  \w    -97.00 -72.00   0.50   55.00    -- -105.75  80.00-171.00   50
 19  \w   -158.00-133.00   0.50   55.00    -- -105.75 -80.00  65.00   50
;
_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      0.0463330000
_diffrn_orient_matrix_UB_12      -0.0695447000
_diffrn_orient_matrix_UB_13      0.0895504000
_diffrn_orient_matrix_UB_21      -0.0218716000
_diffrn_orient_matrix_UB_22      0.0916732000
_diffrn_orient_matrix_UB_23      0.0777536000
_diffrn_orient_matrix_UB_31      -0.0753761000
_diffrn_orient_matrix_UB_32      -0.0694432000
_diffrn_orient_matrix_UB_33      0.0130021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6148
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.502
_diffrn_reflns_theta_max         66.502
_diffrn_reflns_theta_min         5.232
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27287
_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    1.737
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method 'melt fusion'
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1714P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2299
_refine_ls_wR_factor_ref         0.2685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1304
_reflns_number_total             2215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09465b2.cif
_cod_data_source_block           exp_738
_cod_depositor_comments
'Adding full bibliography for 7125861--7125862.cif.'
_cod_database_code               7125862
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C48 N132 O24 '
_diffrn_oxdiff_ac3_digest_frames
;
01fe05fcccae8074aeede7e0687dbf4e8c0158444c0
;
_diffrn_oxdiff_ac3_digest_hkl
;
0182b062edb11e7fc5d7de35256bec2b6707b8
;
_reflns_odcompleteness_completeness 98.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Others
 Fixed Sof: C5(0.5) C9(0.5) C7(0.5) C8(0.5) C6(0.5) C4(0.5) N14(0.5) N16(0.5)
 N18(0.5) N13(0.5) N15(0.5) N17(0.5) O5(0.5) O3(0.5) O1(0.5) O2(0.5) O6(0.5)
 O4(0.5)
2.a Free rotating group:
 C5(C9,C7,C8,C6,C4,N14,N16,N18,N13,N15,N17,O5,O3,O1,O2,O6,O4)
;
_olex2_exptl_crystal_mounting_method 'MiTeGen in 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 2.428
_oxdiff_exptl_absorpt_empirical_full_min 0.472