Obtaining superior high-density fused-ring energetic materials <i>via</i> the introduction of carbonyl, <i>o</i>-NH<sub>2</sub>-NO<sub>2</sub> and nitroamino groups.
Guo, Xiaoyu; Feng, Yizhen; Zhi, Shengjie; Fu, Yajie; Liu, Yingle; Liu, Qiangqiang; Gao, Haixiang; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4035–4040; doi:10.1039/d3dt04237e

data_7715065
_publ_section_title
;
 Obtaining superior high-density fused-ring energetic materials <i>via</i>
 the introduction of carbonyl, <i>o</i>-NH<sub>2</sub>-NO<sub>2</sub> and
 nitroamino groups.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4035
_journal_page_last               4040
_journal_paper_doi               10.1039/d3dt04237e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C6 H4 N8 O7, H2 O'
_chemical_formula_sum            'C6 H6 N8 O8'
_chemical_formula_weight         318.19
_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
_audit_creation_date             2022-06-29
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-11-07 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.635(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7948(4)
_cell_length_b                   9.4387(5)
_cell_length_c                   16.5829(12)
_cell_measurement_reflns_used    1792
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.6770
_cell_measurement_theta_min      5.3960
_cell_volume                     1062.40(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_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    -44.00  12.00   0.50    0.50    --   42.30 -57.00  30.00  112
  2  \w     84.00 131.00   0.50    0.50    --   42.30  77.00 -60.00   94
  3  \w     35.00  60.00   0.50    0.50    --   42.30 -57.00  90.00   50
  4  \w    -43.00   9.00   0.50    0.50    --   42.30 -57.00  90.00  104
  5  \w     15.00  73.00   0.50    0.50    --   42.30 -57.00  30.00  116
  6  \w    105.00 130.00   0.50    0.50    --   42.30  77.00 -30.00   50
  7  \w    151.00 183.00   0.50    0.80    --  101.60  82.00 -60.00   64
  8  \w     13.00  65.00   0.50    0.80    --  101.60 -63.00  30.00  104
  9  \w    134.00 170.00   0.50    0.80    --  101.60  38.00 -30.00   72
 10  \w     69.00 127.00   0.50    0.80    --  101.60  38.00 -30.00  116
 11  \w     69.00 109.00   0.50    0.80    --  101.60 -63.00  30.00   80
 12  \w     12.00 118.00   0.50    0.80    --  101.60 -50.00-150.00  212
 13  \w     12.00 143.00   0.50    0.80    --  101.60 -82.00  30.00  262
 14  \w     52.00 172.00   0.50    0.80    --  101.60 -25.00   0.00  240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1470794000
_diffrn_orient_matrix_UB_12      -0.0012000000
_diffrn_orient_matrix_UB_13      0.0680013000
_diffrn_orient_matrix_UB_21      0.0483467000
_diffrn_orient_matrix_UB_22      -0.1570010000
_diffrn_orient_matrix_UB_23      0.0168752000
_diffrn_orient_matrix_UB_31      0.1659626000
_diffrn_orient_matrix_UB_32      0.0446841000
_diffrn_orient_matrix_UB_33      0.0611338000
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4736
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.404
_diffrn_reflns_theta_min         5.341
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.641
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0527P)^2^+0.7146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1682
_reflns_number_total             2027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04237e2.cif
_cod_data_source_block           20220607
_cod_depositor_comments
'Adding full bibliography for 7715064--7715066.cif.'
_cod_database_code               7715065
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Free rotating group:
 O8(H8A)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N8(H8)
2.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_shelx_res_checksum              71315
_shelx_hkl_checksum              28252
_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 1.561
_oxdiff_exptl_absorpt_empirical_full_min 0.612