Boosting intermolecular interactions of fused cyclic explosives: the way to thermostable and insensitive energetic materials with high density
Chen, Xiang; Guo, Zhaoqi; Zhang, Cong; Zhang, Jianguo; Ma, Haixia; New Journal of Chemistry 45 (2021) 9358–9367; doi:10.1039/D1NJ00924A

data_7060604
_publ_section_title
;
 Boosting intermolecular interactions of fused cyclic explosives: the way
 to thermostable and insensitive energetic materials with high density
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9358
_journal_page_last               9367
_journal_paper_doi               10.1039/D1NJ00924A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C3 H2 N7 O, H2 O, C H6 N3'
_chemical_formula_sum            'C4 H10 N10 O2'
_chemical_formula_weight         230.22
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-31 deposited with the CCDC.	2021-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                105.198(5)
_cell_angle_beta                 100.874(5)
_cell_angle_gamma                92.381(5)
_cell_formula_units_Z            1
_cell_length_a                   3.7934(4)
_cell_length_b                   7.4317(7)
_cell_length_c                   8.7328(8)
_cell_measurement_reflns_used    2196
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.419
_cell_measurement_theta_min      2.470
_cell_volume                     232.24(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3223
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.554
_diffrn_reflns_theta_min         2.470
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1434 before and 0.0572 after correction. The Ratio of minimum to maximum transmission is 0.7650. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             120
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 636 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.8(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1933
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0322P)^2^+0.0613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.884
_reflns_Friedel_fraction_max     0.825
_reflns_number_gt                1670
_reflns_number_total             1933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00924a2.cif
_cod_data_source_block           a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7060601--7060604.cif.'
_cod_database_code               7060604
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2-H2a = O2-H2b
 0.85 with sigma of 0.02
 H2a-H2b
 1.34 with sigma of 0.04
3.a X=CH2 refined with riding coordinates:
 N10(H10a,H10b), N8(H8a,H8b), N9(H9a,H9b), N1(H1a,H1b)
;
_shelx_res_checksum              54346
_olex2_submission_special_instructions 'No special instructions were received'