Synthesis of Nitrate Ester and Nitramine Derivatives of Polyfluoro Alkyl Compounds for High Energy Materials
Dharavath, Srinivas; Ghule, Vikas; RSC Adv.  (2016) –; doi:10.1039/C5RA24615F

data_7223860
_publ_section_title
;
 Synthesis of Nitrate Ester and Nitramine Derivatives of Polyfluoro Alkyl
 Compounds for High Energy Materials
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA24615F
_journal_year                    2016
_chemical_formula_moiety         '0.09(C6 H6 F4 N4 O8)'
_chemical_formula_sum            'C6 H6 F4 N4 O8'
_chemical_formula_weight         338
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_date             2015-01-30
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_audit_update_record
;
2015-11-19 deposited with the CCDC.
2016-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 130.54(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4164(17)
_cell_length_b                   13.6481(9)
_cell_length_c                   4.9679(8)
_cell_measurement_reflns_used    705
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.5040
_cell_measurement_theta_min      3.2510
_cell_volume                     588.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3291
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.7395
_diffrn_measured_fraction_theta_max 0.7495
_diffrn_measurement_details
;
  1 omega  -56.00  -23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000  -60.0000 33

  2 omega  -99.00  -59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000  -60.0000 40

  3 omega   -4.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5136  -99.0000  -30.0000 54

  4 omega   54.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5136   57.0000   30.0000 26

  5 omega    2.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5136  -99.0000  120.0000 25

  6 omega   41.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5136  -99.0000  120.0000 25

  7 omega   65.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       35.5136   37.0000 -150.0000 26

  8 omega   39.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 51

  9 omega  138.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 37

 10 omega   44.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 45

 11 omega  107.00  133.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 26

 12 omega   39.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 32

 13 omega   55.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0462132000
_diffrn_orient_matrix_UB_12      -0.1019895000
_diffrn_orient_matrix_UB_13      0.1742862000
_diffrn_orient_matrix_UB_21      -0.1708916000
_diffrn_orient_matrix_UB_22      -0.0304863000
_diffrn_orient_matrix_UB_23      -0.2485846000
_diffrn_orient_matrix_UB_31      0.0127200000
_diffrn_orient_matrix_UB_32      -0.0375963000
_diffrn_orient_matrix_UB_33      -0.2727125000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0079
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            1137
_diffrn_reflns_theta_full        70.79
_diffrn_reflns_theta_max         71.79
_diffrn_reflns_theta_min         6.04
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             509
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.033
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2222
_reflns_number_gt                824
_reflns_number_total             862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra24615f2.cif
_cod_data_source_block           srinu
_cod_original_cell_volume        588.28(13)
_cod_database_code               7223860
_chemical_oxdiff_formula         'C6 H6 F4 N4 O8'
_chemical_oxdiff_usercomment     SRINIVAS
_reflns_odcompleteness_completeness 77.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97