A New Class of Flexible Energetic Salts: The Crystal Structures of the Ammonium, Lithium, Potassium, and Cesium Salts of Dinitramide
Richard Gilardi; J. Flippen-Anderson; Clifford George; Ray J. Butcher; Journal of the American Chemical Society 119 (1997) 9411–9416; doi:10.1021/ja9709280

data_4117033
_publ_contact_author
;
    Richard Gilardi
    Laboratory for the Structure of Matter
    Naval Research Laboratory
    Washington DC 20375-5341
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_publ_contact_author_email       gilardi@roentgen.nrl.navy.mil
_publ_contact_author_fax         '202 767 6874'
_publ_contact_author_phone       '202 767 3463'
_publ_section_title
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 A New Class of Flexible Energetic Salts: The Crystal Structures of the
 Ammonium, Lithium, Potassium, and Cesium Salts of Dinitramide
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9411
_journal_page_last               9416
_journal_paper_doi               10.1021/ja9709280
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'K N3 O4'
_chemical_formula_weight         145.13
_chemical_name_systematic
; 
     Potassium dinitramide 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.58(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.614(1)
_cell_length_b                   9.280(2)
_cell_length_c                   7.198(1)
_cell_measurement_reflns_used    13
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      44.9
_cell_measurement_theta_min      8.5
_cell_volume                     437.94(13)
_computing_cell_refinement       'Siemens P3 software'
_computing_data_collection       'Siemens P3 software'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3/mv'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            673
_diffrn_reflns_theta_max         57.18
_diffrn_reflns_theta_min         7.83
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.170
_exptl_absorpt_correction_T_max  0.5088
_exptl_absorpt_correction_T_min  0.2362
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_description       chunk
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0073(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.089
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.318
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_obs          0.0281
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.1765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0966
_refine_ls_wR_factor_obs         0.0798
_reflns_number_observed          574
_reflns_number_total             593
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9709280_3.cif
_cod_data_source_block           sri22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.1765P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.1765P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        437.9(1)
_cod_database_code               4117033