#------------------------------------------------------------------------------
#$Date: 2022-07-23 03:08:42 +0300 (Sat, 23 Jul 2022) $
#$Revision: 276835 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/07/7710724.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7710724
loop_
_publ_author_name
'Bauer, Josh'
'Benz, Maximilian'
'Klapötke, Thomas M'
'Stierstorfer, Jörg'
_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         'C H6 N7, Br'
_chemical_formula_sum            'C H6 Br N7'
_chemical_formula_weight         196.04
_chemical_name_common            1,3,5-triaminotetrazolium_bromide
_chemical_name_systematic        1,3,5-triaminotetrazolium_bromide
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2022-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.817(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2609(7)
_cell_length_b                   11.5021(13)
_cell_length_c                   9.3564(12)
_cell_measurement_reflns_used    968
_cell_measurement_temperature    101
_cell_measurement_theta_max      30.7820
_cell_measurement_theta_min      2.9180
_cell_volume                     648.28(14)
_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  'Encifer 1.5.1, CCDC 2014'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      101
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00   7.00   1.00   10.00    --  -19.40 -77.00 150.00   28
  2  ω      5.00  86.00   1.00   10.00    --   20.49  57.00  30.00   81
  3  ω    -36.00  44.00   1.00   10.00    --   20.49 -77.00 -90.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      -0.0352345000
_diffrn_orient_matrix_UB_12      -0.0253616000
_diffrn_orient_matrix_UB_13      -0.0718181000
_diffrn_orient_matrix_UB_21      -0.0210561000
_diffrn_orient_matrix_UB_22      0.0560782000
_diffrn_orient_matrix_UB_23      -0.0321687000
_diffrn_orient_matrix_UB_31      0.1103251000
_diffrn_orient_matrix_UB_32      0.0024926000
_diffrn_orient_matrix_UB_33      -0.0060500000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2374
_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         26.371
_diffrn_reflns_theta_min         2.873
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09106
_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            'light orange'
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0377
_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/[σ²(Fo²)+(0.0449P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1045
_reflns_number_total             1328
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01480g2.cif
_cod_data_source_block           qx395
_cod_database_code               7710724
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.146
_shelx_estimated_absorpt_t_max   0.303
_shelx_res_file
;
TITL v1_a.res in P2(1)/c
    v1.res
    created by SHELXL-2018/3 at 17:08:03 on 10-Nov-2021
REM Old TITL v1 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.084, Rweak 0.003, Alpha 0.032
REM <I/s> 0.968 for 75 systematic absences, Orientation as input
REM Formula found by SHELXT: C7 N Br
CELL 0.71073 6.2609 11.5021 9.3564 90 105.817 90
ZERR 4 0.0007 0.0013 0.0012 0 0.012 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N
UNIT 4 24 4 28

L.S. 22
PLAN  20
SIZE 0.5 0.4 0.25
TEMP -172.15
BOND
list 4
HTAB
fmap 2 53
acta
SHEL 1000 0.8
REM <olex2.extras>
REM <HklSrc "%.\\v1.hkl">
REM </olex2.extras>

WGHT    0.044900
FVAR       0.69774
BR1   3    0.143250    0.375611    0.771768    11.00000    0.01375    0.01540 =
         0.01263    0.00295    0.00201    0.00127
N3    4    0.678155    0.264548    0.455400    11.00000    0.01146    0.00902 =
         0.00972   -0.00068   -0.00126    0.00005
N2    4    0.672738    0.308947    0.327390    11.00000    0.01015    0.01528 =
         0.00773   -0.00142   -0.00185   -0.00210
N1    4    0.490126    0.378473    0.304136    11.00000    0.01316    0.01108 =
         0.00980    0.00029    0.00148   -0.00098
N4    4    0.522188    0.296994    0.521202    11.00000    0.01497    0.01263 =
         0.01223    0.00009    0.00491    0.00021
N6    4    0.824299    0.176665    0.518517    11.00000    0.01801    0.01874 =
         0.01266    0.00091   -0.00179    0.01042
N7    4    0.226926    0.431501    0.433117    11.00000    0.01735    0.02024 =
         0.01207    0.00571    0.00138    0.00696
N5    4    0.399407    0.441094    0.174095    11.00000    0.02118    0.01833 =
         0.00920    0.00418    0.00427    0.00009
C1    1    0.401859    0.371685    0.420543    11.00000    0.01208    0.01180 =
         0.00763   -0.00188    0.00001   -0.00488
H7A   2    0.150493    0.465001    0.370191    11.00000    0.01006
H5A   2    0.486571    0.492524    0.165920    11.00000    0.00152
H5B   2    0.386560    0.392184    0.106841    11.00000    0.03132
H7B   2    0.182689    0.419888    0.519965    11.00000    0.04329
H6A   2    0.903603    0.155156    0.440093    11.00000    0.03714
H6B   2    0.890132    0.210287    0.609379    11.00000    0.04804
HKLF 4




REM  v1_a.res in P2(1)/c
REM wR2 = 0.0890, GooF = S = 1.035, Restrained GooF = 1.035 for all data
REM R1 = 0.0377 for 1045 Fo > 4sig(Fo) and 0.0559 for all 1328 data
REM 106 parameters refined using 0 restraints

END

WGHT      0.0449      0.0000

REM Instructions for potential hydrogen bonds
EQIV $1 -x, -y+1, -z+1
HTAB N7 Br1_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB N5 Br1_$2
EQIV $3 x, y, z-1
HTAB N5 Br1_$3
EQIV $4 x, -y+1/2, z-1/2
HTAB N5 N4_$4
HTAB N7 Br1
EQIV $5 x+1, -y+1/2, z-1/2
HTAB N6 Br1_$5
EQIV $6 x+1, y, z
HTAB N6 Br1_$6

REM Highest difference peak  1.210,  deepest hole -0.834,  1-sigma level  0.159
Q1    1   0.0105  0.3762  0.8059  11.00000  0.05    1.21
Q2    1   0.1805  0.3803  0.6679  11.00000  0.05    0.98
Q3    1   0.2737  0.3662  0.7402  11.00000  0.05    0.91
Q4    1   0.0976  0.3784  0.8838  11.00000  0.05    0.75
Q5    1   0.0546  0.3163  0.6965  11.00000  0.05    0.63
Q6    1   0.3633  0.2166  0.4121  11.00000  0.05    0.60
Q7    1   0.0902  0.3122  0.5974  11.00000  0.05    0.55
Q8    1   0.2333  0.3165  0.8489  11.00000  0.05    0.55
Q9    1   0.0791  0.4577  0.7104  11.00000  0.05    0.51
Q10   1  -0.0215  0.3807  0.6822  11.00000  0.05    0.50
Q11   1   1.1852  0.1834  0.4585  11.00000  0.05    0.46
Q12   1   0.8005  0.2999  0.2985  11.00000  0.05    0.45
Q13   1   0.8953  0.1073  0.4639  11.00000  0.05    0.45
Q14   1   0.7505  0.1350  0.3928  11.00000  0.05    0.44
Q15   1   0.3535  0.2993  0.7873  11.00000  0.05    0.44
Q16   1   0.3023  0.2438  0.4943  11.00000  0.05    0.43
Q17   1   0.6759  0.4022  0.1252  11.00000  0.05    0.43
Q18   1   0.1194  0.2809  0.7365  11.00000  0.05    0.43
Q19   1   0.0837  0.5344  0.2270  11.00000  0.05    0.42
Q20   1   0.7167  0.1414  0.5601  11.00000  0.05    0.42
;
_shelx_res_checksum              14672
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.14325(6) 0.37561(4) 0.77177(5) 0.01424(17) Uani 1 1 d . . . . .
N3 N 0.6782(5) 0.2645(3) 0.4554(4) 0.0109(8) Uani 1 1 d . . . . .
N2 N 0.6727(5) 0.3089(3) 0.3274(4) 0.0119(8) Uani 1 1 d . . . . .
N1 N 0.4901(5) 0.3785(3) 0.3041(4) 0.0117(8) Uani 1 1 d . . . . .
N4 N 0.5222(6) 0.2970(3) 0.5212(4) 0.0130(8) Uani 1 1 d . . . . .
N6 N 0.8243(6) 0.1767(4) 0.5185(5) 0.0176(9) Uani 1 1 d . . . . .
N7 N 0.2269(7) 0.4315(4) 0.4331(5) 0.0171(9) Uani 1 1 d . . . . .
N5 N 0.3994(7) 0.4411(4) 0.1741(5) 0.0162(9) Uani 1 1 d . . . . .
C1 C 0.4019(7) 0.3717(4) 0.4205(5) 0.0110(9) Uani 1 1 d . . . . .
H7A H 0.150(7) 0.465(4) 0.370(6) 0.010(14) Uiso 1 1 d . . . . .
H5A H 0.487(6) 0.493(4) 0.166(5) 0.002(11) Uiso 1 1 d . . . . .
H5B H 0.387(9) 0.392(4) 0.107(7) 0.031(17) Uiso 1 1 d . . . . .
H7B H 0.183(9) 0.420(5) 0.520(7) 0.043(17) Uiso 1 1 d . . . . .
H6A H 0.904(8) 0.155(4) 0.440(6) 0.037(16) Uiso 1 1 d . . . . .
H6B H 0.890(9) 0.210(5) 0.609(7) 0.048(19) Uiso 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0138(2) 0.0154(3) 0.0126(3) 0.0029(2) 0.00201(17) 0.00127(19)
N3 0.0115(17) 0.0090(18) 0.010(2) -0.0007(16) -0.0013(15) 0.0001(15)
N2 0.0102(16) 0.0153(19) 0.0077(19) -0.0014(18) -0.0018(14) -0.0021(16)
N1 0.0132(17) 0.0111(18) 0.010(2) 0.0003(17) 0.0015(15) -0.0010(16)
N4 0.0150(17) 0.0126(19) 0.012(2) 0.0001(17) 0.0049(15) 0.0002(17)
N6 0.0180(19) 0.019(2) 0.013(2) 0.0009(19) -0.0018(17) 0.0104(18)
N7 0.017(2) 0.020(2) 0.012(2) 0.006(2) 0.0014(18) 0.0070(19)
N5 0.021(2) 0.018(2) 0.009(2) 0.0042(19) 0.0043(18) 0.0001(19)
C1 0.0121(19) 0.012(2) 0.008(2) -0.002(2) 0.0000(16) -0.0049(19)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N3 N4 118.4(3) . . ?
N2 N3 N6 122.1(3) . . ?
N4 N3 N6 119.1(4) . . ?
N3 N2 N1 100.9(3) . . ?
N2 N1 N5 124.5(3) . . ?
C1 N1 N2 110.3(3) . . ?
C1 N1 N5 125.0(3) . . ?
N3 N4 C1 101.3(3) . . ?
N4 C1 N1 109.1(4) . . ?
N7 C1 N1 124.8(4) . . ?
N7 C1 N4 126.1(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N3 N2 1.294(5) . ?
N3 N4 1.341(5) . ?
N3 N6 1.383(5) . ?
N2 N1 1.363(5) . ?
N1 N5 1.395(5) . ?
N1 C1 1.351(5) . ?
N4 C1 1.344(6) . ?
N7 C1 1.326(6) . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
? ? ? ? ? ? ? ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
