Energetic derivatives substituted with trinitrophenyl: improving the sensitivity of explosives.
Yu, Qiong; Chen, Yu-Cong; Guo, Zihao; Li, Tao; Liu, Zunqi; Yi, Wenbin; Staples, Richard J.; Shreeve, Jean'ne M.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18467–18472; doi:10.1039/d4dt02070g

data_7716950
_publ_section_title
;
 Energetic derivatives substituted with trinitrophenyl: improving the
 sensitivity of explosives.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18467
_journal_page_last               18472
_journal_paper_doi               10.1039/d4dt02070g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C8 H3 N7 O9'
_chemical_formula_sum            'C8 H3 N7 O9'
_chemical_formula_weight         341.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-06
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.05 svn.r0a1fe1be for OlexSys, GUI svn.r6182)
;
_audit_update_record
;
2022-01-07 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0361(2)
_cell_length_b                   9.5416(2)
_cell_length_c                   21.1634(4)
_cell_measurement_reflns_used    4666
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.7370
_cell_measurement_theta_min      4.1450
_cell_volume                     2430.48(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.979
_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    -43.00  22.00   0.50    2.46    --  -47.57  37.00  90.00  130
  2  \w    -40.00 -14.00   0.50    9.83    --  -86.25  37.00  60.00   52
  3  \w    -64.00  19.00   0.50    2.46    --  -47.57  80.00 122.00  166
  4  \w    -18.00   8.00   0.50    2.46    --   47.57 -19.00   0.00   52
  5  \w     50.00  82.00   0.50    9.83    --  107.11 -69.00 113.00   64
  6  \w     39.00  65.00   0.50    9.83    --  107.11 -57.00  30.00   52
  7  \w     35.00  60.00   0.50    9.83    --  107.11 -57.00   0.00   50
  8  \w     37.00  64.00   0.50    9.83    --  107.11 -57.00  60.00   54
  9  \w     96.00 122.00   0.50    9.83    --  107.11  19.00 -30.00   52
 10  \w    148.00 178.00   0.50    9.83    --  107.11  19.00 -30.00   60
 11  \w    128.00 178.00   0.50    9.83    --  107.11  77.00   0.00  100
 12  \w    144.00 177.00   0.50    9.83    --  107.11  80.00 122.00   66
 13  \w    131.00 173.00   0.50    9.83    --  107.11  57.00 150.00   84
 14  \w    104.00 138.00   0.50    9.83    --  107.11  80.00 122.00   68
 15  \w     96.00 178.00   0.50    9.83    --  107.11  19.00 -60.00  164
 16  \w     37.00  64.00   0.50    9.83    --  107.11 -57.00-120.00   54
 17  \w     35.00  60.00   0.50    9.83    --  107.11 -57.00 -90.00   50
 18  \w     37.00  63.00   0.50    9.83    --  107.11 -57.00 150.00   52
 19  \w    -11.00  14.00   0.50    2.46    --  -47.57  19.00-120.00   50
 20  \w   -119.00 -92.00   0.50    9.83    --  -86.25 -73.00-119.00   54
 21  \w   -150.00-125.00   0.50    9.83    --  -86.25 -37.00-150.00   50
 22  \w   -155.00-127.00   0.50    9.83    --  -86.25 -57.00  90.00   56
 23  \w   -129.00 -67.00   0.50    9.83    --  -86.25 -69.00 113.00  124
;
_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      0.0595433000
_diffrn_orient_matrix_UB_12      -0.0674850000
_diffrn_orient_matrix_UB_13      -0.0568189000
_diffrn_orient_matrix_UB_21      -0.0848374000
_diffrn_orient_matrix_UB_22      -0.1207927000
_diffrn_orient_matrix_UB_23      0.0003061000
_diffrn_orient_matrix_UB_31      -0.0750086000
_diffrn_orient_matrix_UB_32      0.0833010000
_diffrn_orient_matrix_UB_33      -0.0455154000
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.144
_diffrn_reflns_theta_min         4.178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0335P)^2^+1.1768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2284
_reflns_number_total             2520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02070g2.cif
_cod_data_source_block           js1020zzb
_cod_depositor_comments
'Adding full bibliography for 7716950--7716951.cif.'
_cod_original_cell_volume        2430.49(9)
_cod_database_code               7716950
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C8H3N7O9
_chemical_oxdiff_usercomment     QY0044
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7)
;
_shelx_res_checksum              48768
_shelx_hkl_checksum              20334
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id QY-0045
_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 1.828
_oxdiff_exptl_absorpt_empirical_full_min 0.673