Crystal structure of (E)-amino(2-(thiazol-2-ylmethylene)hydrazineyl)methaniminium nitrate, C10H16N12O6S2
Jin, Ze-Sen; Liu, E.; Liu, Xiao-jing; Li, Zhuang-yu; Jian, Fang-fang; Liang, Tongling; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 357–359; doi:10.1515/ncrs-2022-0007

data_8105696
_publ_section_title
;
 Crystal structure of
 (E)-amino(2-(thiazol-2-ylmethylene)hydrazineyl)methaniminium nitrate,
 C10H16N12O6S2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              357
_journal_page_last               359
_journal_paper_doi               10.1515/ncrs-2022-0007
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C5 H8 N5 S, N O3'
_chemical_formula_sum            'C5 H8 N6 O3 S'
_chemical_formula_weight         232.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                67.973(2)
_cell_angle_beta                 87.916(2)
_cell_angle_gamma                88.347(2)
_cell_formula_units_Z            4
_cell_length_a                   7.6977(2)
_cell_length_b                   11.5353(3)
_cell_length_c                   11.7533(3)
_cell_measurement_reflns_used    10835
_cell_measurement_temperature    170.01(10)
_cell_measurement_theta_max      31.2170
_cell_measurement_theta_min      1.8360
_cell_volume                     966.69(5)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.846
_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    -40.00 -15.00   0.50    2.00    --    5.00  45.00 120.00   50
  2  \w    -23.00  71.00   0.50    2.00    --  -11.40  45.00  30.00  188
  3  \w   -100.00  78.00   0.50    2.00    --  -11.40  45.00 150.00  356
  4  \w   -100.00  23.00   0.50    2.00    --  -11.40  45.00  90.00  246
  5  \w     52.00  78.00   0.50    2.00    --  -11.40  45.00  90.00   52
  6  \w      9.00  35.00   0.50    2.00    --  -11.40  45.00   0.00   52
  7  \w    -79.00 -40.00   0.50    2.00    --  -11.40  45.00  30.00   78
;
_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      -0.0137048000
_diffrn_orient_matrix_UB_12      -0.0496114000
_diffrn_orient_matrix_UB_13      0.0574576000
_diffrn_orient_matrix_UB_21      0.0193478000
_diffrn_orient_matrix_UB_22      -0.0440345000
_diffrn_orient_matrix_UB_23      -0.0277636000
_diffrn_orient_matrix_UB_31      0.0891178000
_diffrn_orient_matrix_UB_32      0.0008030000
_diffrn_orient_matrix_UB_33      0.0130065000
_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  0.0140
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14660
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.860
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82974
_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    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.2850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4688
_reflns_number_total             5143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0007_suppl.cif
_cod_data_source_block           mx9127
_cod_depositor_comments
;

2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C10 H16 N12 O6 S2'
_cod_original_formula_weight         464.47
_cod_original_formula_moiety         '2(C5 H8 N5 S), 2(N O3)'
_cod_original_formula_units_Z            2
_cod_database_code               8105696
_chemical_oxdiff_formula         CHNO
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C4(H4), N3A(H3A), C1A(H1A), C2A(H2A), C4A(H4AC)
2.b X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), N4A(H4AA,H4AB), N5A(H5AA,H5AB)
;
_shelx_res_checksum              91288
_shelx_hkl_checksum              31954
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.621