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_7703158
_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, H2 O, 2(C H6 N3)'
_chemical_formula_sum            'C5 H15 N17 O7'
_chemical_formula_weight         425.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-29 deposited with the CCDC.	2019-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                85.471(3)
_cell_angle_beta                 80.793(4)
_cell_angle_gamma                82.300(3)
_cell_formula_units_Z            4
_cell_length_a                   6.7723(3)
_cell_length_b                   13.1291(5)
_cell_length_c                   18.8628(8)
_cell_measurement_reflns_used    2443
_cell_measurement_temperature    189.7(10)
_cell_measurement_theta_max      72.8960
_cell_measurement_theta_min      4.7450
_cell_volume                     1637.80(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      189.7(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -67.00  21.00   1.00    1.00    --  -40.08  57.00 120.00   88
  2  \w   -115.00  -8.00   1.00    1.00    --  -40.08 -77.00 -30.00  107
  3  \w    -67.00  33.00   1.00    1.00    --  -40.08  57.00-120.00  100
  4  \w    107.00 171.00   1.00    1.00    --  105.48 125.00 -60.00   64
  5  \w     55.00 178.00   1.00    1.00    --  105.48  15.00   0.00  123
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1027915000
_diffrn_orient_matrix_UB_12      0.0074388000
_diffrn_orient_matrix_UB_13      0.0662738000
_diffrn_orient_matrix_UB_21      -0.1437086000
_diffrn_orient_matrix_UB_22      -0.0705642000
_diffrn_orient_matrix_UB_23      0.0447444000
_diffrn_orient_matrix_UB_31      0.1505264000
_diffrn_orient_matrix_UB_32      -0.0950393000
_diffrn_orient_matrix_UB_33      -0.0218868000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9467
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         3.403
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         5733
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.4072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5006
_reflns_number_total             5733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03829a2.cif
_cod_data_source_block           1
_cod_database_code               7703158
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     C4A-A2G-ACE3
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.803
_reflns_odcompleteness_completeness 59.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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(O2WA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) = Uanis(O2WA)
3. Others
 Sof(O2WA)=Sof(H2WC)=Sof(H2WD)=1-FVAR(1)
 Sof(O2W)=Sof(H2WA)=Sof(H2WB)=FVAR(1)
4.a Riding coordinates:
 O2W(H2WA,H2WB), O2WA(H2WC,H2WD)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N13(H13)
4.c X=CH2 refined with riding coordinates:
 N26(H26A,H26B), N27(H27A,H27B), N28(H28B,H28A), N29(H29A,H29B), N30(H30A,
 H30B), N31(H31B,H31A), N32(H32A,H32B), N33(H33A,H33B), N34(H34A,H34B),
 N23(H23B,H23A), N24(H24A,H24B), N25(H25B,H25A)
;
_shelx_res_checksum              78242
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.674
_oxdiff_exptl_absorpt_empirical_full_min 0.509