Highly energetic <i>N</i>-cyano-substituted CL-20 analogues: challenging the stability limits of polynitro hexaazaisowurtzitanes.
Parakhin, Vladimir V.; Pokhvisneva, Galina V.; Shlykova, Nina I.; Samigullina, Aida I.; Nikitin, Sergei V.; Smirnov, Gennady A.; Gordeev, Pavel B.; Kon'kova, Tatyana S.; Lempert, David B.; Pivkina, Alla N.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6100–6111; doi:10.1039/d3dt04203k

data_7715269
_publ_section_title
;
 Highly energetic <i>N</i>-cyano-substituted CL-20 analogues: challenging
 the stability limits of polynitro hexaazaisowurtzitanes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6100
_journal_page_last               6111
_journal_paper_doi               10.1039/d3dt04203k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C8 H6 N12 O8'
_chemical_formula_sum            'C8 H6 N12 O8'
_chemical_formula_weight         398.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-06-19
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2023-11-15 deposited with the CCDC.	2024-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7723(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.78897(7)
_cell_length_b                   13.33467(14)
_cell_length_c                   13.43040(12)
_cell_measurement_reflns_used    15518
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      77.4980
_cell_measurement_theta_min      4.6570
_cell_volume                     1391.90(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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   -120.00 -48.00   0.50    0.50    --  -48.70-163.00  55.00  144
  2  \w    -83.00  -7.00   0.50    0.50    --  -48.70 117.00 -67.00  152
  3  \w   -139.00 -48.00   0.50    1.80    --  -86.25-163.00  55.00  182
  4  \w   -154.00 -78.00   0.50    1.80    --  -86.25-117.00-155.00  152
  5  \w     40.00 109.00   0.50    1.80    --  107.75-117.00-155.00  138
  6  \w     54.00 138.00   0.50    1.80    --  107.75-163.00  55.00  168
  7  \w    100.00 176.00   0.50    1.80    --  107.75 117.00 -67.00  152
  8  \w    -26.00  26.00   0.50    0.50    --  -48.70  19.00-120.00  104
  9  \w   -118.00 -73.00   0.50    0.50    --  -48.70-125.00 -90.00   90
 10  \w    -26.00  26.00   0.50    0.50    --  -48.70  19.00 120.00  104
 11  \w     54.00 108.00   0.50    0.50    --   48.70-163.00  55.00  108
 12  \w     34.00  59.00   0.50    0.50    --   48.70-117.00-155.00   50
 13  \w    -24.00  23.00   0.50    0.50    --   48.70 -19.00 -60.00   94
 14  \w    -50.00 -14.00   0.50    1.80    --  -86.25  45.00 150.00   72
 15  \w    147.00 173.00   0.50    1.80    --  107.75  15.00 120.00   52
 16  \w     38.00  92.00   0.50    1.80    --  107.75-103.00-129.42  108
 17  \w     36.00  71.00   0.50    1.80    --  107.75 -61.00   0.00   70
 18  \w     63.00  88.00   0.50    1.80    --  107.75 -77.00   0.00   50
 19  \w     51.00 110.00   0.50    1.80    --  107.75-125.00-120.00  118
 20  \w     45.00  78.00   0.50    1.80    --  107.75 -95.00  60.00   66
 21  \w     96.00 129.00   0.50    1.80    --  107.75 125.00 120.00   66
 22  \w     98.00 160.00   0.50    1.80    --  107.75  45.00  90.00  124
 23  \w     36.00  61.00   0.50    1.80    --  107.75 -61.00 -90.00   50
 24  \w     42.00  69.00   0.50    1.80    --  107.75 -61.00  30.00   54
 25  \w     67.00 105.00   0.50    1.80    --  107.75-125.00 -30.00   76
 26  \w    121.00 176.00   0.50    1.80    --  107.75 125.00 -90.00  110
 27  \w     87.00 163.00   0.50    1.80    --  107.75  77.00 -30.00  152
 28  \w     39.00  74.00   0.50    1.80    --  107.75-106.00-118.49   70
 29  \w     82.00 107.00   0.50    1.80    --  107.75-106.00-118.49   50
 30  \w    114.00 171.00   0.50    1.80    --  107.75  45.00-120.00  114
 31  \w     37.00  76.00   0.50    1.80    --  107.75 -77.00 -60.00   78
 32  \w    128.00 154.00   0.50    1.80    --  107.75  45.00 -90.00   52
 33  \w    105.00 131.00   0.50    1.80    --  107.75  30.00 150.00   52
 34  \w     76.00 102.00   0.50    1.80    --  107.75 -77.00-150.00   52
 35  \w     41.00  67.00   0.50    1.80    --  107.75 -77.00 150.00   52
 36  \w     64.00  90.00   0.50    1.80    --  107.75 -95.00   0.00   52
 37  \w     66.00 103.00   0.50    1.80    --  107.75-125.00  90.00   74
 38  \w    130.00 156.00   0.50    1.80    --  107.75  15.00  90.00   52
 39  \w    137.00 163.00   0.50    1.80    --  107.75  15.00 -90.00   52
 40  \w     97.00 130.00   0.50    1.80    --  107.75  15.00 -90.00   66
 41  \w    114.00 140.00   0.50    1.80    --  107.75  45.00 -60.00   52
 42  \w    130.00 155.00   0.50    1.80    --  107.75 125.00 120.00   50
 43  \w     82.00 108.00   0.50    1.80    --  107.75 -79.00  84.18   52
 44  \w     36.00  94.00   0.50    1.80    --  107.75 -77.00-120.00  116
;
_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      -0.0067641000
_diffrn_orient_matrix_UB_12      -0.0422181000
_diffrn_orient_matrix_UB_13      -0.1069891000
_diffrn_orient_matrix_UB_21      0.0344227000
_diffrn_orient_matrix_UB_22      -0.1060866000
_diffrn_orient_matrix_UB_23      0.0420729000
_diffrn_orient_matrix_UB_31      -0.1950591000
_diffrn_orient_matrix_UB_32      -0.0173562000
_diffrn_orient_matrix_UB_33      0.0034142000
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.708
_diffrn_reflns_theta_min         4.678
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (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            colorless
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0405P)^2^+0.7810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2852
_reflns_number_total             2957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04203k2.cif
_cod_data_source_block           23-VVP2304
_cod_depositor_comments
'Adding full bibliography for 7715268--7715271.cif.'
_cod_database_code               7715269
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C8 H6 N12 O8'
_chemical_oxdiff_usercomment     VVP2304
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.714
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.52
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
;
_shelx_res_checksum              66079
_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 1.102
_oxdiff_exptl_absorpt_empirical_full_min 0.883