Nitrogen-rich Energetic Salts of 1H,1′H-5,5′-Bistetrazole-1,1′-diolate: Synthesis, Characterization, and Thermal Behaviors
Shang, Yu; Jin, Bo; Peng, Ru-Fang; Guo, Zhicheng; Liu, Qiangqiang; Zhao, Jun; Zhang, Qingchun; RSC Adv.  (2016) –; doi:10.1039/C6RA10108A

data_7225139
_publ_section_title
;
 Nitrogen-rich Energetic Salts of
 1H,1&#x2032;H-5,5&#x2032;-Bistetrazole-1,1&#x2032;-diolate: Synthesis,
 Characterization, and Thermal Behaviors
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA10108A
_journal_year                    2016
_chemical_formula_moiety         'C N4 O, C2 H4 N3'
_chemical_formula_sum            'C3 H5 N7 O'
_chemical_formula_weight         155.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-06 deposited with the CCDC.
2016-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.767(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.2410(12)
_cell_length_b                   10.5185(8)
_cell_length_c                   7.7546(7)
_cell_measurement_reflns_used    1399
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.3750
_cell_measurement_theta_min      5.1560
_cell_volume                     1221.27(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671 -125.0000 -120.0000 67

  2 omega    7.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671   19.0000 -150.0000 101

  3 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -99.0000  -90.0000 74

  4 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671 -125.0000    0.0000 67

  5 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671 -125.0000  120.0000 67

  6 omega   39.00  109.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -60.0000 70

  7 omega   90.00  175.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  150.0000 85

  8 omega   38.00   91.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

  9 omega   38.00   91.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

 10 omega   39.00  109.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 70

 11 omega   38.00   91.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

 12 omega   39.00  109.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 70

 13 omega   91.00  176.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -120.0000 85

 14 omega   41.00  126.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000    0.0000 85

 15 omega   39.00  109.00   1.0000    1.3800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 70

 16 omega   19.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671   57.0000  -90.0000 84

 17 omega    9.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671   77.0000    0.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0903685000
_diffrn_orient_matrix_UB_12      -0.0689587000
_diffrn_orient_matrix_UB_13      0.0487491000
_diffrn_orient_matrix_UB_21      -0.0366472000
_diffrn_orient_matrix_UB_22      -0.1109085000
_diffrn_orient_matrix_UB_23      -0.1222947000
_diffrn_orient_matrix_UB_31      0.0326820000
_diffrn_orient_matrix_UB_32      0.0664330000
_diffrn_orient_matrix_UB_33      -0.1534703000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3333
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.061
_diffrn_reflns_theta_max         67.061
_diffrn_reflns_theta_min         5.139
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0910P)^2^+0.0810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                947
_reflns_number_total             1093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra10108a2.cif
_cod_data_source_block           xnkd-01
_cod_original_cell_volume        1221.26(18)
_cod_database_code               7225139
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B)
;
_shelx_res_checksum              81121
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-08-17
_olex2_submission_special_instructions 'No special instructions were received'