Crystal structure of (E)-amino(2-(4-(dimethylamino)benzylidene)hydrazineyl)methaniminium nitrate, C10H16N6O3
Liu, Xiao-Jing; Liu, E.; Jin, Ze-Sen; Li, Zhuang-Yu; Jian, Fang-Fang; Liang, Tongling; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 795–796; doi:10.1515/ncrs-2021-0092

data_8104714
_publ_section_title
;
 Crystal structure of
 (E)-amino(2-(4-(dimethylamino)benzylidene)hydrazineyl)methaniminium
 nitrate, C10H16N6O3
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              795
_journal_page_last               796
_journal_paper_doi               10.1515/ncrs-2021-0092
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'N O3, C10 H16 N5'
_chemical_formula_sum            'C10 H16 N6 O3'
_chemical_formula_weight         268.277
_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'
_symmetry_Int_Tables_number      14
_cell_angle_alpha                90
_cell_angle_beta                 104.557(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2312(1)
_cell_length_b                   17.7721(3)
_cell_length_c                   11.0146(2)
_cell_measurement_reflns_used    6565
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      74.4770
_cell_measurement_theta_min      2.4720
_cell_volume                     1370.08(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9564
_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    -50.00 -11.00   0.50    0.05    --  -47.20  77.00  68.00   78
  2  \w    -96.00 -71.00   0.50    0.05    --  -47.20 -77.00 -57.00   50
  3  \w    -24.00  36.00   0.50    0.05    --   47.20 -77.00 -57.00  120
  4  \w     40.00  66.00   0.50    0.05    --   47.20 -77.00 -57.00   52
  5  \w    -78.00 -40.00   0.50    0.05    --  -99.00  77.00  68.00   76
  6  \w   -168.00-105.00   0.50    0.05    --  -99.00 -77.00 -57.00  126
  7  \w     73.00 104.00   0.50    0.05    --  103.25 -77.00 -57.00   62
  8  \w     44.00  70.00   0.50    0.05    --  103.25 -77.00 -57.00   52
  9  \w    -22.00  28.00   0.50    0.05    --  -47.20  19.00  60.00  100
 10  \w   -113.00 -81.00   0.50    0.05    --  -47.20-125.00  60.00   64
 11  \w     28.00 103.00   0.50    0.05    --   47.20  77.00  68.00  150
 12  \w    -63.00 -27.00   0.50    0.05    --  -99.00  61.00  60.00   72
 13  \w    -58.00 -27.00   0.50    0.05    --  -99.00  61.00 -90.00   62
 14  \w   -167.00-115.00   0.50    0.05    --  -99.00 -30.00 150.00  104
 15  \w    -67.00 -27.00   0.50    0.05    --  -99.00  61.00  30.00   80
 16  \w    -67.00 -26.00   0.50    0.05    --  -99.00  61.00-120.00   82
 17  \w   -166.00 -93.00   0.50    0.05    --  -99.00 -45.00   0.00  146
 18  \w     32.00  74.00   0.50    0.05    --  103.25 -61.00  90.00   84
 19  \w     34.00  63.00   0.50    0.05    --  103.25 -94.00 120.00   58
 20  \w     31.00  68.00   0.50    0.05    --  103.25 -61.00 -60.00   74
 21  \w     71.00  96.00   0.50    0.05    --  103.25 -94.00 120.00   50
 22  \w    136.00 165.00   0.50    0.05    --  103.25  15.00-150.00   58
 23  \w     56.00 105.00   0.50    0.05    --  103.25 -94.00-180.00   98
 24  \w     98.00 129.00   0.50    0.05    --  103.25  15.00-150.00   62
 25  \w    131.00 169.00   0.50    0.05    --  103.25  77.00  68.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0897290000
_diffrn_orient_matrix_UB_12      -0.0721825000
_diffrn_orient_matrix_UB_13      -0.0375507000
_diffrn_orient_matrix_UB_21      -0.1660561000
_diffrn_orient_matrix_UB_22      -0.0066434000
_diffrn_orient_matrix_UB_23      -0.1186117000
_diffrn_orient_matrix_UB_31      0.1131831000
_diffrn_orient_matrix_UB_32      0.0475030000
_diffrn_orient_matrix_UB_33      -0.0736010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9564
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9426
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9564
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.05
_diffrn_reflns_theta_min         4.84
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             570.007
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.2929
_refine_diff_density_min         -0.3071
_refine_diff_density_rms         0.0595
_refine_ls_d_res_high            0.7979
_refine_ls_d_res_low             9.1423
_refine_ls_goodness_of_fit_ref   1.0403
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0403
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.0048
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+0.5106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -9
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2450
_reflns_number_total             2698
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_j_ncrs-2021-0092_suppl.cif
_cod_data_source_block           TX4061
_cod_database_code               8104714