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_7715064
_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 N6 O5, H2 O'
_chemical_formula_sum            'C6 H6 N6 O6'
_chemical_formula_weight         258.17
_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             2022-10-01
_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                 97.747(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1700(2)
_cell_length_b                   6.5296(2)
_cell_length_c                   15.4974(4)
_cell_measurement_reflns_used    2197
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      72.9240
_cell_measurement_theta_min      5.7550
_cell_volume                     919.46(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_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      8.00  33.00   1.00    1.00    --  -40.73  38.00  30.00   25
  2  \w    -62.00  -7.00   1.00    1.00    --  -40.73  38.00  30.00   55
  3  \w    -61.00  -9.00   1.00    1.00    --  -40.73  77.00  90.00   52
  4  \w     21.00 110.00   1.00    1.00    --   40.73  57.00-180.00   89
  5  \w     34.00  96.00   1.00    1.00    --  106.95 -45.00-120.00   62
  6  \w     91.00 155.00   1.00    1.00    --  106.95  45.00   0.00   64
  7  \w    144.00 171.00   1.00    1.00    --  106.95 125.00   0.00   27
  8  \w     35.00 118.00   1.00    1.00    --  106.95 -45.00 150.00   83
  9  \w     35.00 106.00   1.00    1.00    --  106.95 -95.00 120.00   71
 10  \w     37.00 113.00   1.00    1.00    --  106.95-125.00  60.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0943627000
_diffrn_orient_matrix_UB_12      0.1060854000
_diffrn_orient_matrix_UB_13      -0.0619351000
_diffrn_orient_matrix_UB_21      0.0191479000
_diffrn_orient_matrix_UB_22      -0.2063224000
_diffrn_orient_matrix_UB_23      -0.0454490000
_diffrn_orient_matrix_UB_31      -0.1394905000
_diffrn_orient_matrix_UB_32      0.0432852000
_diffrn_orient_matrix_UB_33      -0.0645198000
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3074
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.046
_diffrn_reflns_theta_min         5.312
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0040(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         1769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0501P)^2^+0.3480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1612
_reflns_number_total             1769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04237e2.cif
_cod_data_source_block           0927-1
_cod_depositor_comments
'Adding full bibliography for 7715064--7715066.cif.'
_cod_database_code               7715064
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1)
;
_shelx_res_checksum              48448
_shelx_hkl_checksum              21540
_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 1.800
_oxdiff_exptl_absorpt_empirical_full_min 0.557