A facile synthesis of energetic salts based on fully nitroamino-functionalized [1,2,4]triazolo[4,3-b][1,2,4]triazole.
Bian, Chengming; Feng, Wenjing; Lei, Qunying; Huang, Haifeng; Li, Xia; Wang, Jianlong; Li, Chuan; Xiao, Zhongliang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 368–374; doi:10.1039/c9dt03829a

data_7703157
_publ_section_title
;
 A facile synthesis of energetic salts based on fully
 nitroamino-functionalized [1,2,4]triazolo[4,3-b][1,2,4]triazole.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              368
_journal_page_last               374
_journal_paper_doi               10.1039/c9dt03829a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C3 H N11 O6, 2(C H7 N4), 0.72(H2 O1)'
_chemical_formula_sum            'C5 H16.44 N19 O6.72'
_chemical_formula_weight         450.36
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-28 deposited with the CCDC.	2019-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.786(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3254(7)
_cell_length_b                   12.5221(13)
_cell_length_c                   19.3440(19)
_cell_measurement_reflns_used    5633
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.69
_cell_volume                     1743.1(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23305
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.409
_diffrn_reflns_theta_min         2.691
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0761 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.4058.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             933
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0560P)^2^+1.5139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2525
_reflns_number_total             3552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03829a2.cif
_cod_data_source_block           mo_1119_1_0m
_cod_database_code               7703157
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C5)
3. Others
 Sof(H17A)=Sof(N20)=Sof(H20A)=Sof(H20B)=Sof(N21)=Sof(H21A)=Sof(H21B)=Sof(C6)=1-
 FVAR(1)
 Sof(O7)=Sof(H7A)=Sof(H7B)=Sof(N19)=Sof(H19A)=Sof(H19B)=Sof(H17)=Sof(N18)=
 Sof(H18A)=Sof(H18B)=Sof(C5)=FVAR(1)
4.a Free rotating group:
 O7(H7A,H7B)
4.b Rotating group:
 N15(H15A,H15B), N16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N14(H14), N17(H17), N17(H17A)
4.d X=CH2 refined with riding coordinates:
 N12(H12A,H12B), N13(H13A,H13B), N19(H19A,H19B), N18(H18A,H18B), N20(H20A,
 H20B), N21(H21A,H21B)
;
_olex2_submission_special_instructions 'No special instructions were received'