Exploring the reactive chemistry of FOX-7: synthesis of cyclic triazinane-based energetic materials featuring the FOX-7 backbone
Yan, Chao; Cheng, Guangbin; Wang, Kangcai; Liu, Tianlin; Jin, Yunhe; Yang, Hongwei; Zhang, Qinghua; New Journal of Chemistry 43 (2019) 10429–; doi:10.1039/C9NJ01932D

data_7058457
_publ_section_title
;
 Exploring the reactive chemistry of FOX-7: synthesis of cyclic
 triazinane-based energetic materials featuring the FOX-7 backbone
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10429
_journal_paper_doi               10.1039/C9NJ01932D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C9 H14 N10 O8, H2 O'
_chemical_formula_sum            'C9 H16 N10 O9'
_chemical_formula_weight         408.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-15 deposited with the CCDC.    2019-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.084(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.038(4)
_cell_length_b                   7.1500(16)
_cell_length_c                   13.854(3)
_cell_measurement_reflns_used    857
_cell_measurement_temperature    173
_cell_measurement_theta_max      21.191
_cell_measurement_theta_min      2.978
_cell_volume                     1666.6(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_unetI/netI     0.1024
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11113
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.436
_diffrn_reflns_theta_min         1.210
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0737 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.8785.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3399
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0602P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1791
_reflns_number_total             3399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01932d2.cif
_cod_data_source_block           mo_20180681-yx-48_0m
_cod_depositor_comments
'Adding full bibliography for 7058456--7058460.cif.'
_cod_original_cell_volume        1666.6(6)
_cod_database_code               7058457
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H9A-H7
 2.2 with sigma of 0.02
 H7-H9B
 2.2 with sigma of 0.02
3.a Free rotating group:
 O9(H9A)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C5(H5A,H5B), C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N4(H4), N7(H7), N3(H3)
;
_shelx_res_checksum              89776
_olex2_submission_special_instructions 'No special instructions were received'