Convenient synthesis of energetic polynitro materials including (NO2)3CCH2CH2NH3-salts via Michael addition of trinitromethane.
Axthammer, Quirin J.; Klapötke, Thomas M; Krumm, Burkhard; Scharf, Regina; Unger, Cornelia C.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18909–18920; doi:10.1039/c6dt03779h

data_7041098
_publ_section_title
;
 Convenient synthesis of energetic polynitro materials including
 (NO2)3CCH2CH2NH3-salts via Michael addition of trinitromethane.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18909
_journal_page_last               18920
_journal_paper_doi               10.1039/c6dt03779h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C4 H6 N4 O7'
_chemical_formula_sum            'C4 H6 N4 O7'
_chemical_formula_weight         222.11
_chemical_name_common            4,4,4-trinitrobutanamide
_chemical_name_systematic        4,4,4-trinitrobutanamide
_space_group_IT_number           2
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Thu Jun 20 15:18:27 2013'
;
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-09-26 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                80.728(7)
_cell_angle_beta                 87.505(7)
_cell_angle_gamma                88.355(6)
_cell_formula_units_Z            2
_cell_length_a                   6.1081(5)
_cell_length_b                   7.5366(6)
_cell_length_c                   8.8543(7)
_cell_measurement_reflns_used    1595
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2010
_cell_measurement_theta_min      4.7930
_cell_volume                     401.80(6)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
;
_computing_publication_material
;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   -9.00   41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994   57.0000  -90.0000 50

  2 omega -100.00  -75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -77.0000    0.0000 25

  3 omega  -97.00  -19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.6994  -57.0000  120.0000 78

  4 omega   -3.00  102.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932   77.0000    0.0000 105

  5 omega  -24.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000   90.0000 98

  6 omega  -16.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.7932  -99.0000 -120.0000 80

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       omega-scan
_diffrn_orient_matrix_UB_11      -0.0459895000
_diffrn_orient_matrix_UB_12      -0.0833300000
_diffrn_orient_matrix_UB_13      0.0331760000
_diffrn_orient_matrix_UB_21      0.0550389000
_diffrn_orient_matrix_UB_22      -0.0422974000
_diffrn_orient_matrix_UB_23      -0.0572952000
_diffrn_orient_matrix_UB_31      0.0915024000
_diffrn_orient_matrix_UB_32      -0.0191055000
_diffrn_orient_matrix_UB_33      0.0470663000
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3448
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         4.27
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.0521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                1685
_reflns_number_total             1971
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6dt03779h2.cif
_cod_data_source_block           manuscript
_cod_depositor_comments
'Adding full bibliography for 7041098--7041104.cif.'
_cod_database_code               7041098
loop_