Insensitive Energetic 5-Nitroaminotetrazolate Ionic Liquids
Gao, Yi-Fei; Zhang, Lei; He, Ling; Zhao, Ying; Tang, Ning; Yuan, Wen-Li; Tao, Guo-Hong; RSC Adv.  (2015) –; doi:10.1039/C5RA07415K

data_7220784
_publ_section_title
;
 Insensitive Energetic 5-Nitroaminotetrazolate Ionic Liquids
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA07415K
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'N7 H O2, C5 H9 N2'
_chemical_formula_sum            'C5 H10 N9 O2'
_chemical_formula_weight         228.22
_chemical_melting_point          349
_chemical_name_systematic        '[C1mim]NAT'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-17
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_audit_update_record
;
2014-11-01 deposited with the CCDC.
2015-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                89.262(5)
_cell_angle_beta                 85.726(5)
_cell_angle_gamma                79.991(5)
_cell_formula_units_Z            8
_cell_length_a                   7.3986(4)
_cell_length_b                   10.6152(6)
_cell_length_c                   24.7372(14)
_cell_measurement_reflns_used    3603
_cell_measurement_temperature    143.00(10)
_cell_measurement_theta_max      29.1891
_cell_measurement_theta_min      2.9740
_cell_volume                     1907.91(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      143.00(10)
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -18.00   17.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8924  -99.0000   90.0000 35

  2 omega  -13.00   15.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8924  -99.0000  -90.0000 28

  3 omega   42.00   92.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0174 -178.0000 -180.0000 50

  4 omega   -6.00   92.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0174   37.0000  -60.0000 98

  5 omega    5.00   85.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0174   57.0000   30.0000 80

  6 omega  -46.00   44.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0174  -37.0000  120.0000 90

  7 omega   35.00   80.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0174  178.0000   30.0000 45
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0262923000
_diffrn_orient_matrix_UB_12      0.0665167000
_diffrn_orient_matrix_UB_13      -0.0046466000
_diffrn_orient_matrix_UB_21      -0.0145280000
_diffrn_orient_matrix_UB_22      0.0106444000
_diffrn_orient_matrix_UB_23      0.0283611000
_diffrn_orient_matrix_UB_31      0.0928777000
_diffrn_orient_matrix_UB_32      0.0081330000
_diffrn_orient_matrix_UB_33      0.0009025000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15810
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/ethanol'
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         11281
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.630
_refine_ls_shift/su_mean         0.164
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                5365
_reflns_number_total             11281
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;

2018-01-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C10 H20 N18 O4'
_cod_original_formula_weight         456.44
_cod_original_formula_moiety         '2(N7 H O2), 2(C5 H9 N2)'
_cod_original_formula_units_Z            4
_cod_data_source_file            c5ra07415k2.cif
_cod_data_source_block           120919_s2_gyf
_cod_database_code               7220784
_chemical_oxdiff_formula         C20H20N2O3
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32