Chemistry of 2,5-diaminotetrazole.
Bauer, Josh; Benz, Maximilian; Klapötke, Thomas M; Stierstorfer, Jörg; Dalton transactions (Cambridge, England : 2003)  (2022) –; doi:10.1039/d2dt01480g

data_7710732
_publ_section_title
;
 Chemistry of 2,5-diaminotetrazole.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt01480g
_journal_year                    2022
_chemical_formula_moiety         'C2 N8 O2, 2(C H6 N7)'
_chemical_formula_sum            'C4 H12 N22 O2'
_chemical_formula_weight         400.36
_chemical_name_common
'di(1,3,5-triaminotetrazolium) 5,5-bistetrazole-1N-dioxide'
_chemical_name_systematic
'di(1,3,5-triaminotetrazolium) 5,5-bistetrazole-1N-dioxide'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_audit_creation_date             2022-03-09
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2022-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.757(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5454(12)
_cell_length_b                   5.1159(6)
_cell_length_c                   14.5922(17)
_cell_measurement_reflns_used    561
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      23.2140
_cell_measurement_theta_min      2.0990
_cell_volume                     753.81(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      101(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -96.00 -60.00   0.80   20.00    --  -23.68 178.00 120.00   45
  2  \w    -95.00 -63.00   0.80   20.00    --  -23.68-178.00 -60.00   40
  3  \w    -73.00  -1.00   0.80   20.00    --  -23.68 121.00  87.00   90
  4  \w    -31.00  -3.00   0.80   20.00    --   24.62 128.00  39.64   35
  5  \w     16.00  64.00   0.80   20.00    --   24.62 -99.00 -60.00   60
  6  \w    -44.00  39.20   0.80   20.00    --   24.62 -38.00 -60.00  104
  7  \w    -43.00  93.00   0.80   20.00    --   24.62   0.00 150.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0607923000
_diffrn_orient_matrix_UB_12      0.0444682000
_diffrn_orient_matrix_UB_13      -0.0313834000
_diffrn_orient_matrix_UB_21      0.0333414000
_diffrn_orient_matrix_UB_22      0.0387312000
_diffrn_orient_matrix_UB_23      -0.0336376000
_diffrn_orient_matrix_UB_31      -0.0112637000
_diffrn_orient_matrix_UB_32      -0.1254786000
_diffrn_orient_matrix_UB_33      -0.0214605000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_sigmaI/netI    0.1905
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5990
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       plate
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0287P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                914
_reflns_number_total             1543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01480g2.cif
_cod_data_source_block           rx029
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710732
_shelx_res_checksum              46505