Crystal structure of (E)-(2-((1H-pyrrol-2-yl)methylene)hydrazineyl)(amino)methaniminium nitrate monohydrate, C6H12N6O4
Jin, Ze-Sen; Liu, Xiao-jing; Li, Zhuang-Yu; Liu, E.; Jian, Fang-fang; Liang, Tongling; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 797–798; doi:10.1515/ncrs-2021-0084

data_8104715
_publ_section_title
;
 Crystal structure of
 (E)-(2-((1H-pyrrol-2-yl)methylene)hydrazineyl)(amino)methaniminium
 nitrate monohydrate, C6H12N6O4
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              797
_journal_page_last               798
_journal_paper_doi               10.1515/ncrs-2021-0084
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'N O3, H2 O, C6 H10 N5'
_chemical_formula_sum            'C6 H12 N6 O4'
_chemical_formula_weight         232.200
_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_Int_Tables_number      14
_cell_angle_alpha                90
_cell_angle_beta                 101.525(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3652(3)
_cell_length_b                   16.8683(7)
_cell_length_c                   8.3779(3)
_cell_measurement_reflns_used    5552
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      31.0550
_cell_measurement_theta_min      2.3950
_cell_volume                     1019.87(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_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      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9962
_diffrn_measured_fraction_theta_max 0.8104
_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    -93.00  67.00   0.50    5.00    --  -11.60  45.00 168.96  320
  2  \w     11.00  67.00   0.50    5.00    --  -11.60  45.00 168.96  112
  3  \w    -25.00   1.00   0.50    5.00    --  -11.60  45.00 -16.08   52
  4  \w    -93.00   4.00   0.50    5.00    --  -11.60  45.00 168.96  194
  5  \w   -100.00 -67.00   0.50    5.00    --  -11.60  45.00 -16.08   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0328206000
_diffrn_orient_matrix_UB_12      -0.0230687000
_diffrn_orient_matrix_UB_13      0.0707443000
_diffrn_orient_matrix_UB_21      -0.0922928000
_diffrn_orient_matrix_UB_22      -0.0051273000
_diffrn_orient_matrix_UB_23      0.0109813000
_diffrn_orient_matrix_UB_31      -0.0083055000
_diffrn_orient_matrix_UB_32      -0.0347933000
_diffrn_orient_matrix_UB_33      -0.0483591000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.9962
_diffrn_reflns_Laue_measured_fraction_max 0.8104
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11032
_diffrn_reflns_point_group_measured_fraction_full 0.9962
_diffrn_reflns_point_group_measured_fraction_max 0.8104
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         31.10
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
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    1.512
_exptl_crystal_description       prism
_exptl_crystal_F_000             488.263
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.2757
_refine_diff_density_min         -0.3316
_refine_diff_density_rms         0.0541
_refine_ls_d_res_high            0.6880
_refine_ls_d_res_low             8.4342
_refine_ls_goodness_of_fit_ref   1.0265
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    21
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0265
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.0033
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.2134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -10
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              -5
_reflns_number_gt                2220
_reflns_number_total             2662
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_j_ncrs-2021-0084_suppl.cif
_cod_data_source_block           MX9047
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               8104715