Design and synthesis of energetic materials towards high density and positive oxygen balance by N-dinitromethyl functionalization of nitroazoles
Zhao, X. X.; Li, S. H.; Wang, Y.; Li, Y. C.; Zhao, F. Q.; Pang, S. P.; Journal of Materials Chemistry A 4 (2016) 5495–; doi:10.1039/C6TA01501H

data_7236301
_publ_section_title
;
 Design and synthesis of energetic materials towards high density and
 positive oxygen balance by N-dinitromethyl functionalization of
 nitroazoles
;
_journal_issue                   15
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              5495
_journal_paper_doi               10.1039/C6TA01501H
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         'C4 H2 N5 O6, N H3.5352 O0.5352'
_chemical_formula_sum            'C4 H5.54 N6 O6.54'
_chemical_formula_weight         242.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-03
_audit_creation_method
;

  Olex2 1.1

  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)

;
_audit_update_record
;
2015-12-14 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.073(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.9109(4)
_cell_length_b                   27.172(2)
_cell_length_c                   6.9470(6)
_cell_measurement_reflns_used    1238
_cell_measurement_temperature    101.7
_cell_measurement_theta_max      29.2632
_cell_measurement_theta_min      3.0454
_cell_volume                     890.76(13)
_computing_cell_refinement
;

CrysAlisPro, Agilent Technologies,

Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)

(compiled May 16 2011,17:55:39)

;
_computing_data_collection
;

CrysAlisPro, Agilent Technologies,

Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)

(compiled May 16 2011,17:55:39)

;
_computing_data_reduction
;

CrysAlisPro, Agilent Technologies,

Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)

(compiled May 16 2011,17:55:39)

;
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      101.7
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;

  1 omega  -33.00   30.00   1.0000    1.8000

omega____ theta____ kappa____ phi______ frames

    -      -13.4210   37.0000  -90.0000 63

 

  2 omega   -7.00   51.00   1.0000    1.8000

omega____ theta____ kappa____ phi______ frames

    -       18.7335   77.0000 -180.0000 58

 

  3 omega  -45.00   45.00   1.0000    1.8000

omega____ theta____ kappa____ phi______ frames

    -       18.7335  -77.0000    0.0000 90

;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1248293000
_diffrn_orient_matrix_UB_12      0.0120034000
_diffrn_orient_matrix_UB_13      0.0076540000
_diffrn_orient_matrix_UB_21      0.0732619000
_diffrn_orient_matrix_UB_22      0.0227865000
_diffrn_orient_matrix_UB_23      0.0154217000
_diffrn_orient_matrix_UB_31      -0.0405003000
_diffrn_orient_matrix_UB_32      0.0042166000
_diffrn_orient_matrix_UB_33      -0.1048828000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3676
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

CrysAlisPro, Agilent Technologies,

Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)

(compiled May 16 2011,17:55:39)

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             495
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.2661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                1459
_reflns_number_total             1736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ta01501h2.cif
_cod_data_source_block           exp_3285
_cod_original_cell_volume        890.77(13)
_cod_database_code               7236301
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32