Oxygen-Rich Bis(trinitroethyl esters): Suitable Oxidizers as Potential Ammonium Perchlorate Replacements
Unger, Cornelia C.; Holler, Marcel; Krumm, Burkhard; Klapötke, Thomas M.; Energy & Fuels  (2020) –; doi:10.1021/acs.energyfuels.0c02910

data_1559439
_publ_section_title
;
 Oxygen-Rich Bis(trinitroethyl esters): Suitable Oxidizers as Potential
 Ammonium Perchlorate Replacements
;
_journal_name_full               'Energy &amp; Fuels'
_journal_paper_doi               10.1021/acs.energyfuels.0c02910
_journal_year                    2020
_chemical_formula_moiety         'C8 H8 N8 O18'
_chemical_formula_sum            'C8 H8 N8 O18'
_chemical_formula_weight         504.22
_chemical_name_common
'nitraminodiacetic acid bis(2,2,2-trinitroethylester)'
_chemical_name_systematic
'nitraminodiacetic acid bis(2,2,2-trinitroethylester)'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_date             2019-05-16
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                88.360(9)
_cell_angle_beta                 86.992(10)
_cell_angle_gamma                84.906(10)
_cell_formula_units_Z            4
_cell_length_a                   5.8695(7)
_cell_length_b                   17.401(2)
_cell_length_c                   18.116(2)
_cell_measurement_reflns_used    943
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      20.5320
_cell_measurement_theta_min      3.5120
_cell_volume                     1839.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Microsoft Word 2016'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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 -36.00   1.00   17.00    --  -28.70-178.00   0.00   60
  2  \w    -84.00 -44.00   1.00   17.00    --  -28.70-178.00 -60.00   40
  3  \w   -111.00 -67.00   1.00   17.00    --  -28.70 178.00  60.00   44
  4  \w   -104.00  35.00   1.00   17.00    --  -28.70 -19.00 120.00  139
  5  \w      1.00  95.00   1.00   17.00    --   29.79  77.00 -90.00   94
  6  \w     13.00  92.00   1.00   17.00    --   29.79-129.00  34.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0507895000
_diffrn_orient_matrix_UB_12      -0.0360986000
_diffrn_orient_matrix_UB_13      0.0128293000
_diffrn_orient_matrix_UB_21      -0.0284730000
_diffrn_orient_matrix_UB_22      0.0107983000
_diffrn_orient_matrix_UB_23      0.0370291000
_diffrn_orient_matrix_UB_31      -0.1066126000
_diffrn_orient_matrix_UB_32      -0.0160024000
_diffrn_orient_matrix_UB_33      -0.0015367000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_sigmaI/netI    0.2902
_diffrn_reflns_av_unetI/netI     0.2196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.379
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00039(11)
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         7532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.2014
_refine_ls_R_factor_gt           0.0715
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2872
_reflns_number_total             7532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef0c02910_si_005.cif
_cod_data_source_block           ox166
_cod_database_code               1559439
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              31706