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_7715268
_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         'C7 H7 N11 O8'
_chemical_formula_sum            'C7 H7 N11 O8'
_chemical_formula_weight         373.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-24
_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                 96.3532(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.67654(7)
_cell_length_b                   15.58666(16)
_cell_length_c                   10.82025(11)
_cell_measurement_reflns_used    14190
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.2920
_cell_measurement_theta_min      4.9940
_cell_volume                     1286.71(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.102a 64-bit (release 15-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.92a (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      99.99(10)
_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 0.995
_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   -117.00 -70.00   0.50    0.40    --  -46.46-131.00  58.00   94
  2  \w   -119.00 -64.00   0.50    0.40    --  -46.46-139.00-116.00  110
  3  \w     42.00 103.00   0.50    0.40    --   46.46-139.00-116.00  122
  4  \w     38.00  97.00   0.50    0.40    --   46.46-131.00  58.00  118
  5  \w   -158.00 -64.00   0.50    1.60    --  -91.75-139.00-116.00  188
  6  \w    -91.00 -21.00   0.50    1.60    --  -91.75 131.00 129.00  140
  7  \w     42.00 122.00   0.50    1.60    --  113.25-139.00-116.00  160
  8  \w     42.00 116.00   0.50    1.60    --  113.25-131.00  58.00  148
  9  \w     91.00 178.00   0.50    1.60    --  113.25 131.00 129.00  174
 10  \w    -27.00  29.00   0.50    0.40    --  -46.46  19.00 -30.00  112
 11  \w    -27.00  29.00   0.50    0.40    --  -46.46  19.00  90.00  112
 12  \w    -90.00 -16.00   0.50    0.40    --  -46.46 131.00 129.00  148
 13  \w    -29.00  27.00   0.50    0.40    --   46.46 -19.00 -60.00  112
 14  \w    -51.00 -19.00   0.50    1.60    --  -91.75  45.00 -60.00   64
 15  \w     41.00 105.00   0.50    1.60    --  113.25 -77.00  30.00  128
 16  \w     41.00 105.00   0.50    1.60    --  113.25 -77.00-150.00  128
 17  \w     41.00  71.00   0.50    1.60    --  113.25 -61.00  90.00   60
 18  \w     41.00 106.00   0.50    1.60    --  113.25 -95.00  90.00  130
 19  \w     43.00 111.00   0.50    1.60    --  113.25-125.00 -60.00  136
 20  \w    115.00 169.00   0.50    1.60    --  113.25  30.00  60.00  108
 21  \w     52.00  78.00   0.50    1.60    --  113.25 -77.00  60.00   52
 22  \w     80.00 106.00   0.50    1.60    --  113.25-125.00-180.00   52
 23  \w    102.00 133.00   0.50    1.60    --  113.25 125.00-150.00   62
 24  \w     99.00 158.00   0.50    1.60    --  113.25  30.00 120.00  118
 25  \w     45.00  94.00   0.50    1.60    --  113.25 -95.00 150.00   98
 26  \w     56.00  82.00   0.50    1.60    --  113.25-125.00   0.00   52
 27  \w     97.00 175.00   0.50    1.60    --  113.25  61.00-150.00  156
 28  \w     99.00 178.00   0.50    1.60    --  113.25  30.00 150.00  158
 29  \w    101.00 126.00   0.50    1.60    --  113.25  45.00 150.00   50
 30  \w     42.00 106.00   0.50    1.60    --  113.25 -95.00 -30.00  128
 31  \w     73.00  99.00   0.50    1.60    --  113.25-125.00  30.00   52
 32  \w     41.00  66.00   0.50    1.60    --  113.25 -61.00-150.00   50
 33  \w     41.00  69.00   0.50    1.60    --  113.25 -61.00 -90.00   56
 34  \w     73.00 105.00   0.50    1.60    --  113.25 -95.00  30.00   64
 35  \w     95.00 133.00   0.50    1.60    --  113.25  68.00 101.61   76
 36  \w    141.00 178.00   0.50    1.60    --  113.25  68.00 101.61   74
 37  \w     43.00  69.00   0.50    1.60    --  113.25 -79.00 159.96   52
 38  \w     93.00 119.00   0.50    1.60    --  113.25 -79.00 159.96   52
 39  \w     81.00 106.00   0.50    1.60    --  113.25 -95.00 -60.00   50
 40  \w    152.00 178.00   0.50    1.60    --  113.25 125.00-150.00   52
 41  \w     99.00 146.00   0.50    1.60    --  113.25  30.00-150.00   94
 42  \w    114.00 140.00   0.50    1.60    --  113.25  30.00  90.00   52
 43  \w    114.00 144.00   0.50    1.60    --  113.25  15.00  60.00   60
 44  \w     41.00  66.00   0.50    1.60    --  113.25 -61.00  30.00   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      -0.0748704000
_diffrn_orient_matrix_UB_12      -0.0069357000
_diffrn_orient_matrix_UB_13      -0.1377015000
_diffrn_orient_matrix_UB_21      0.0009857000
_diffrn_orient_matrix_UB_22      0.0985717000
_diffrn_orient_matrix_UB_23      -0.0108114000
_diffrn_orient_matrix_UB_31      0.1874897000
_diffrn_orient_matrix_UB_32      -0.0034234000
_diffrn_orient_matrix_UB_33      -0.0378912000
_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  0.0220
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17390
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.670
_diffrn_reflns_theta_min         4.996
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.675
_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            colorless
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0384P)^2^+0.7717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2660
_reflns_number_total             2779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04203k2.cif
_cod_data_source_block           5-PGV-2062
_cod_depositor_comments
'Adding full bibliography for 7715268--7715271.cif.'
_cod_database_code               7715268
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12H12N6O12
_chemical_oxdiff_usercomment     PGV-2062
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.801
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.50
_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(H6A)
;
_shelx_res_checksum              26823
_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 1.163
_oxdiff_exptl_absorpt_empirical_full_min 0.865