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_1559438
_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         'C4 H6 N2 O6'
_chemical_formula_sum            'C4 H6 N2 O6'
_chemical_formula_weight         178.11
_chemical_name_common            N-ethyl-N-nitroglycine
_chemical_name_systematic        N-ethyl-N-nitroglycine
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_audit_creation_date             2018-09-05
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8051(4)
_cell_length_b                   14.4941(7)
_cell_length_c                   5.2206(2)
_cell_measurement_reflns_used    1478
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.7420
_cell_measurement_theta_min      4.7320
_cell_volume                     666.26(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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     -3.00  99.00   1.00   15.00    --   29.79  77.00 -90.00  102
  2  \w     31.00  99.00   1.00   15.00    --   29.79  57.00 120.00   68
  3  \w     59.00  94.00   1.00   15.00    --   29.79 179.00 150.00   35
  4  \w   -104.00  27.00   1.00   15.00    --  -28.70   0.00 -60.00  131
  5  \w     26.00  95.00   1.00   15.00    --   29.79-133.00  39.00   69
  6  \w   -108.00 -60.00   1.00   15.00    --  -28.70-179.00  60.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0586045000
_diffrn_orient_matrix_UB_12      0.0137104000
_diffrn_orient_matrix_UB_13      -0.0850397000
_diffrn_orient_matrix_UB_21      0.0179701000
_diffrn_orient_matrix_UB_22      0.0469922000
_diffrn_orient_matrix_UB_23      0.0231620000
_diffrn_orient_matrix_UB_31      0.0521642000
_diffrn_orient_matrix_UB_32      -0.0007587000
_diffrn_orient_matrix_UB_33      -0.1034720000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4692
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_min         4.149
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0396P)^2^+0.1888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                603
_reflns_number_total             709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef0c02910_si_003.cif
_cod_data_source_block           nx345
_cod_database_code               1559438
_shelx_res_checksum              63636