Ring closure of polynitroazoles via an N,N′-alkylene bridge: towards high thermally stable energetic compounds
Tang, Yongxing; He, Chunlin; Imler, Gregory H.; Parrish, Damon A.; Shreeve, Jean'ne M.; Journal of Materials Chemistry A 6 (2018) 8382–; doi:10.1039/C8TA02704H

data_7237136
_publ_section_title
;
 Ring closure of polynitroazoles via an N,N&#x2032;-alkylene bridge:
 towards high thermally stable energetic compounds
;
_journal_issue                   18
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              8382
_journal_paper_doi               10.1039/C8TA02704H
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C8 H4 N8 O8, 0.5(C2 H3 N)'
_chemical_formula_sum            'C9 H5.5 N8.5 O8'
_chemical_formula_weight         360.72
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-19 deposited with the CCDC.
2018-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                120.00(3)
_cell_formula_units_Z            6
_cell_length_a                   8.443(2)
_cell_length_b                   8.443(2)
_cell_length_c                   33.962(7)
_cell_measurement_reflns_used    8022
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.061
_cell_measurement_theta_min      3.034
_cell_volume                     2096.6(10)
_computing_cell_refinement       'Bruker APEX3 v2015.5-2 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 v2015.5-2 (Bruker, 2015)'
_computing_data_reduction
;
Bruker SAINT v8.34A (Bruker, 2013), Bruker XPREP v2014/2 (Bruker, 2014)
;
_computing_molecular_graphics    'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_publication_material  'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Photon 100'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'HELIOS multilayer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            11485
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.302
_diffrn_reflns_theta_min         3.905
_diffrn_source                   '1uS microfocus'
_exptl_absorpt_coefficient_mu    1.349
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5 (Bruker, 2008)'
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       plates
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 743 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(14)
_refine_ls_extinction_coef       0.0024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2529
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0260P)^2^+0.7943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.643
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                2190
_reflns_number_total             2529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta02704h2.cif
_cod_data_source_block           shrv593
_cod_original_cell_volume        2096.8(11)
_cod_original_formula_sum        'C9 H5.50 N8.50 O8'
_cod_database_code               7237136
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.966
_shelx_res_checksum              87726