Tautomeric and conformational switching in a new versatile N-rich heterocyclic ligand.
Parisi, Emmanuele; Capasso, Domenica; Capobianco, Amedeo; Peluso, Andrea; Di Gaetano, Sonia; Fusco, Sandra; Manfredi, Carla; Mozzillo, Rosaria; Pinto, Gabriella; Centore, Roberto; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14452–14462; doi:10.1039/d0dt02572k

data_7705602
_publ_section_title
;
 Tautomeric and conformational switching in a new versatile N-rich
 heterocyclic ligand.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14452
_journal_page_last               14462
_journal_paper_doi               10.1039/d0dt02572k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '(C8 H8 N7)+, (Cl)-'
_chemical_formula_sum            'C8 H8 Cl N7'
_chemical_formula_weight         237.66
_chemical_name_systematic
'4-Methyl-7-(2-pyrazinyl)-2<i>H</i>-3<i>H</i>[1,2,4]triazolo[3,2-<i>c</i>][1,2,4]-triazolium chloride'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-07-15 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.96(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.290(2)
_cell_length_b                   16.438(4)
_cell_length_c                   12.291(4)
_cell_measurement_reflns_used    185
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.461
_cell_measurement_theta_min      4.427
_cell_volume                     1016.7(6)
_computing_cell_refinement
;
Dirax/lsq (Duisenberg <i>et al.</i>, 2000)
;
_computing_data_collection       '<i>Collect</i> (Nonius, 1999)'
_computing_data_reduction
;
EvalCCD (Duisenberg <i>et al.</i>, 2003)
;
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 2012) and 
Mercury (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_detector_type
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
CCD rotation images, thick slices
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10090
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         3.030
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 <i>SADABS</i> (Bruker, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_recrystallization_method
'Slow cooling to room temperature of a solution containing water and few drops of HCl 1M.'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0303P)^2^+0.5709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1472
_reflns_number_total             2313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02572k2.cif
_cod_data_source_block           shelx_CCDC5
_cod_depositor_comments
'Adding full bibliography for 7705597--7705603.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7705602
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              48825