Crystal structure transformation and step-by-step thermal decomposition behavior of dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate
Jia, Jianhui; Liu, Yu; Huang, Shiliang; Xu, Jinjiang; Li, Shichun; Zhang, Haobin; Cao, Xiong; RSC Adv. 7 (2017) 49105–; doi:10.1039/C7RA08816G

data_7229370
_publ_section_title
;
 Crystal structure transformation and step-by-step thermal decomposition
 behavior of dihydroxylammonium
 5,5&#x2032;-bistetrazole-1,1&#x2032;-diolate
;
_journal_issue                   77
_journal_name_full               'RSC Adv.'
_journal_page_first              49105
_journal_paper_doi               10.1039/C7RA08816G
_journal_volume                  7
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '0.5(C4 N16 O4), 2(H4 N)'
_chemical_formula_sum            'C2 H8 N10 O2'
_chemical_formula_weight         204.18
_chemical_name_systematic        ABTOX
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-08-09 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5982(12)
_cell_length_b                   7.5982(12)
_cell_length_c                   13.294(3)
_cell_measurement_reflns_used    1204
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      3.06
_cell_volume                     767.5(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3930
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.682
_diffrn_reflns_theta_min         3.065
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0865 before and 0.0608 after correction. The Ratio of minimum to maximum transmission is 0.8271. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 405 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -2.0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1189
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0434P)^2^+0.0060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                986
_reflns_number_total             1189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra08816g2.cif
_cod_data_source_block           dm17170
_cod_original_cell_volume        767.5(3)
_cod_database_code               7229370
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Restrained distances
 N9-H9_$1 = N8_$2-H8B_$3 = N8_$2-H8A_$3 = N10_$4-H10_$3
 0.82 with sigma of 0.02
2. Others
 Fixed Sof: N2(0.5) N3(0.5) N4(0.5) C1(0.5) N5(0.5) N6(0.5) N7(0.5) C2(0.5)
;
_shelx_res_checksum              97209
_olex2_submission_special_instructions 'No special instructions were received'