Investigation of Deuterated FOX-7 – Changes in Structural Behavior and Energetic Characteristics after Deuteration at ambient conditions
Klapoetke, Thomas M.; Krumm, Burkhard; Lechner, Jasmin; Stierstorfer, Joerg; Dalton Transactions  (2022) –; doi:10.1039/D2DT00490A

data_7709779
_publ_section_title
;
 Investigation of Deuterated FOX-7 -- Changes in Structural Behavior and
 Energetic Characteristics after Deuteration at ambient conditions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00490A
_journal_year                    2022
_chemical_formula_moiety         'C2 D4 N4 O4'
_chemical_formula_sum            'C2 D4 N4 O4'
_chemical_formula_weight         152.12
_chemical_name_common            FOX-7-d4
_chemical_name_systematic        d4-diamino-dinitroethene
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_audit_creation_date             2021-11-11
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-02-04 deposited with the CCDC.	2022-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5238(13)
_cell_length_b                   6.9618(8)
_cell_length_c                   11.3592(9)
_cell_measurement_reflns_used    1182
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      28.5740
_cell_measurement_theta_min      3.5540
_cell_volume                     515.91(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      101(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -24.00  44.00   1.00   25.00    --  -19.09  57.00 -30.00   68
  2  \w    -29.00  46.00   1.00   25.00    --  -19.09  57.00-120.00   75
  3  \w    -73.00 -25.00   1.00   25.00    --  -19.09 127.00 136.43   48
  4  \w      4.00  46.00   1.00   25.00    --  -19.09  57.00 150.00   42
  5  \w      4.00  83.00   1.00   25.00    --   20.18  57.00-150.00   79
  6  \w      3.00  83.00   1.00   25.00    --   20.18  57.00  30.00   80
  7  \w      7.00  81.00   1.00   25.00    --   20.18  57.00 -60.00   74
  8  \w      3.00  84.00   1.00   25.00    --   20.18  57.00 120.00   81
  9  \w    -15.00  59.00   1.00   25.00    --   20.18 -99.00 120.00   74
 10  \w    -38.00  31.00   1.00   25.00    --   20.18 -57.00  30.00   69
 11  \w      8.00  59.00   1.00   25.00    --   20.18 -99.00 -30.00   51
 12  \w     -7.00  18.00   1.00   25.00    --   20.18  77.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0726169000
_diffrn_orient_matrix_UB_12      0.0739414000
_diffrn_orient_matrix_UB_13      -0.0103916000
_diffrn_orient_matrix_UB_21      -0.0806563000
_diffrn_orient_matrix_UB_22      0.0680440000
_diffrn_orient_matrix_UB_23      -0.0040287000
_diffrn_orient_matrix_UB_31      0.0069752000
_diffrn_orient_matrix_UB_32      0.0169637000
_diffrn_orient_matrix_UB_33      0.0614095000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8171
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.254
_diffrn_reflns_theta_min         3.432
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            light-orange
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 426 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1279
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0426P)^2^+0.0350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1090
_reflns_number_total             1279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00490a2.cif
_cod_data_source_block           qx396
_cod_database_code               7709779
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              52426
_shelx_hkl_checksum              77171