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_7715270
_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         'C9 H8 N14 O14'
_chemical_formula_sum            'C9 H8 N14 O14'
_chemical_formula_weight         536.29
_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             2023-10-24
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2023-11-16 deposited with the CCDC.	2024-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.891(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5629(4)
_cell_length_b                   8.4701(3)
_cell_length_c                   17.2484(5)
_cell_measurement_reflns_used    14217
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.6700
_cell_measurement_theta_min      3.4870
_cell_volume                     1863.27(11)
_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      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 1.000
_diffrn_measured_fraction_theta_max 0.966
_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    -69.00  26.00   0.50    2.00    --  -46.59  74.00 103.00  190
  2  \w   -119.00 -24.00   0.50    2.00    --  -46.59 -74.00 -25.00  190
  3  \w     24.00 120.00   0.50    2.00    --   46.59  74.00 103.00  192
  4  \w    -25.00  69.00   0.50    2.00    --   46.59 -74.00 -25.00  188
  5  \w   -164.00 -69.00   0.50    8.00    --  -91.75 -74.00 -25.00  190
  6  \w    -96.00 -19.00   0.50    8.00    --  -91.75  74.00 103.00  154
  7  \w     91.00 178.00   0.50    8.00    --  113.25  74.00 103.00  174
  8  \w     41.00  96.00   0.50    8.00    --  113.25 -74.00 -25.00  110
  9  \w    -27.00  29.00   0.50    2.00    --  -46.59  19.00 -90.00  112
 10  \w     34.00  93.00   0.50    2.00    --   46.59-125.00 150.00  118
 11  \w    -51.00 -19.00   0.50    8.00    --  -91.75  45.00 -90.00   64
 12  \w     43.00 111.00   0.50    8.00    --  113.25-125.00 -30.00  136
 13  \w     95.00 178.00   0.50    8.00    --  113.25 125.00  30.00  166
 14  \w     41.00 106.00   0.50    8.00    --  113.25 -95.00 -30.00  130
 15  \w     95.00 178.00   0.50    8.00    --  113.25 125.00-180.00  166
 16  \w    106.00 147.00   0.50    8.00    --  113.25 125.00 150.00   82
 17  \w    153.00 178.00   0.50    8.00    --  113.25 125.00 150.00   50
 18  \w    111.00 169.00   0.50    8.00    --  113.25 107.00  62.01  116
 19  \w     44.00  75.00   0.50    8.00    --  113.25-143.00 -62.34   62
 20  \w     90.00 116.00   0.50    8.00    --  113.25-143.00 -62.34   52
 21  \w     42.00  71.00   0.50    8.00    --  113.25 -61.00  30.00   58
 22  \w     85.00 117.00   0.50    8.00    --  113.25-141.00 165.22   64
 23  \w    111.00 149.00   0.50    8.00    --  113.25  30.00  30.00   76
 24  \w     57.00  83.00   0.50    8.00    --  113.25   0.00-180.00   52
 25  \w     96.00 143.00   0.50    8.00    --  113.25  61.00  90.00   94
 26  \w     57.00 142.00   0.50    8.00    --  113.25 -88.00  28.48  170
 27  \w     61.00  96.00   0.50    8.00    --  113.25-125.00   0.00   70
 28  \w     90.00 115.00   0.50    8.00    --  113.25  77.00-180.00   50
 29  \w    131.00 177.00   0.50    8.00    --  113.25  77.00-180.00   92
 30  \w     48.00  74.00   0.50    8.00    --  113.25 -80.00 -37.61   52
 31  \w     45.00  70.00   0.50    8.00    --  113.25 -61.00 -30.00   50
 32  \w     66.00 117.00   0.50    8.00    --  113.25-139.00-143.94  102
 33  \w     98.00 151.00   0.50    8.00    --  113.25 125.00-120.00  106
 34  \w    130.00 177.00   0.50    8.00    --  113.25  77.00 -30.00   94
 35  \w     48.00  74.00   0.50    8.00    --  113.25 -95.00  30.00   52
 36  \w    100.00 143.00   0.50    8.00    --  113.25  45.00 -90.00   86
 37  \w    130.00 169.00   0.50    8.00    --  113.25  30.00-150.00   78
 38  \w    116.00 142.00   0.50    8.00    --  113.25  36.00  33.17   52
 39  \w     41.00  73.00   0.50    8.00    --  113.25 -95.00 -60.00   64
 40  \w    133.00 159.00   0.50    8.00    --  113.25  30.00  60.00   52
 41  \w    127.00 176.00   0.50    8.00    --  113.25   0.00-180.00   98
 42  \w     55.00 106.00   0.50    8.00    --  113.25 -95.00-150.00  102
;
_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      -0.0923291000
_diffrn_orient_matrix_UB_12      -0.1156865000
_diffrn_orient_matrix_UB_13      -0.0148993000
_diffrn_orient_matrix_UB_21      0.0635963000
_diffrn_orient_matrix_UB_22      -0.0938577000
_diffrn_orient_matrix_UB_23      0.0773086000
_diffrn_orient_matrix_UB_31      -0.0451295000
_diffrn_orient_matrix_UB_32      0.1044198000
_diffrn_orient_matrix_UB_33      0.0530001000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23475
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         83.954
_diffrn_reflns_theta_min         3.465
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.672
_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    1.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1088
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0340P)^2^+2.2312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3523
_reflns_number_total             4051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04203k2.cif
_cod_data_source_block           15-PGV2061
_cod_depositor_comments
'Adding full bibliography for 7715268--7715271.cif.'
_cod_database_code               7715270
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C9H8N14O14
_chemical_oxdiff_usercomment     PGV2061
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.843
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
;
_shelx_res_checksum              73495
_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 1.787
_oxdiff_exptl_absorpt_empirical_full_min 0.788