Revisiting the Reactive Chemistry of FOX-7: Cyclization of FOX-7 Affords Fused-Ring Polynitro Compounds
Yan, Chao; Qi, Xiujuan; Wang, Kangcai; Jin, Yunhe; Cheng, Guangbin; Liu, Tianlin; Yang, Hongwei; Zhang, Qinghua; Chemical Communications  (2019) –; doi:10.1039/C8CC10178G

data_7123056
_publ_section_title
;
 Revisiting the Reactive Chemistry of FOX-7: Cyclization of FOX-7 Affords
 Fused-Ring Polynitro Compounds
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10178G
_journal_year                    2019
_chemical_formula_moiety         'C6 H8 N8 O8'
_chemical_formula_sum            'C6 H8 N8 O8'
_chemical_formula_weight         320.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_audit_update_record
;
2018-12-19 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                94.152(4)
_cell_angle_beta                 104.263(4)
_cell_angle_gamma                104.096(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6754(11)
_cell_length_b                   8.1836(13)
_cell_length_c                   11.2567(17)
_cell_measurement_reflns_used    891
_cell_measurement_temperature    173
_cell_measurement_theta_max      22.537
_cell_measurement_theta_min      2.592
_cell_volume                     572.28(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.976
_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  0.0357
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5180
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.885
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0580 before and 0.0444 after correction.
The Ratio of minimum to maximum transmission is 0.9044.
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    1.858
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0609
_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^)+(0.1009P)^2^+0.2197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1830
_reflns_number_total             2558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc10178g3.cif
_cod_data_source_block           1
_cod_database_code               7123056
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C6(H6A,H6B), C2(H2A,H2B)
;
_shelx_res_checksum              429
_shelx_hkl_checksum              3034
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'