Crystal structure evolution of an energetic compound dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate induced by solvents
Xu, Xin; Chen, Dong; Li, Hongzhen; Yan, Mi; Xiong, Ying; Zhao, Haixia; Xu, Rong; RSC Advances 10 (2020) 11939–11944; doi:10.1039/D0RA01182G

data_7240221
_publ_section_title
;
 Crystal structure evolution of an energetic compound dihydroxylammonium
 5,5&#x2032;-bistetrazole-1,1&#x2032;-diolate induced by solvents
;
_journal_issue                   20
_journal_name_full               'RSC Advances'
_journal_page_first              11939
_journal_page_last               11944
_journal_paper_doi               10.1039/D0RA01182G
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         '[NH(CH3CCH3)OH+] [C2HO2N4-].H2O'
_chemical_formula_sum            'C5 H11 N9 O4'
_chemical_formula_weight         261.23
_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   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-01-18 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                73.627(2)
_cell_angle_beta                 82.716(2)
_cell_angle_gamma                83.323(2)
_cell_formula_units_Z            2
_cell_length_a                   6.8110(5)
_cell_length_b                   7.3961(5)
_cell_length_c                   11.6431(9)
_cell_measurement_reflns_used    4209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.810
_cell_measurement_theta_min      5.762
_cell_volume                     556.19(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.996
_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       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7339
_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         25.999
_diffrn_reflns_theta_min         2.881
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             272
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: AC/MT'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.037
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2180
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0464P)^2^+0.1891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1758
_reflns_number_total             2180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra01182g2.cif
_cod_data_source_block           mo_d8v19308_0m
_cod_depositor_comments
'Adding full bibliography for 7240219--7240221.cif.'
_cod_database_code               7240221
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2013-4
_shelx_res_checksum              24858