Bases, solvates and salts: new benzimidazole- and pyridine-scaffolded ligands
Bocian, Aleksandra; Gorczyński, Adam; Marcinkowski, Dawid; Dutkiewicz, Grzegorz; Patroniak, Violetta; Kubicki, Maciej; Acta Crystallographica Section C 76 (2020) 367–374; doi:10.1107/S2053229620004131

data_2022109
_publ_section_title
;
 Bases, solvates and salts: new benzimidazole- and pyridine-scaffolded
 ligands
;
_journal_coeditor_code           EF3005
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              367
_journal_page_last               374
_journal_paper_doi               10.1107/S2053229620004131
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C13 H14 N6, 1.25H2 O'
_chemical_formula_moiety         'C13 H14 N6, 5/4(H2 O)'
_chemical_formula_sum            'C13 H16.5 N6 O1.25'
_chemical_formula_weight         276.82
_chemical_name_systematic
'2-{(2<i>E</i>)-1-Methyl-2-[(1-methyl-1<i>H</i>-imidazol-2-yl)methylidene]hydrazinyl}-1<i>H</i>-benzimidazole hydrate'
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                106.760(2)
_cell_angle_beta                 97.854(2)
_cell_angle_gamma                103.408(2)
_cell_formula_units_Z            8
_cell_length_a                   9.1836(3)
_cell_length_b                   16.5814(4)
_cell_length_c                   20.8041(6)
_cell_measurement_reflns_used    24014
_cell_measurement_temperature    130.0(10)
_cell_measurement_theta_max      75.9440
_cell_measurement_theta_min      2.8920
_cell_volume                     2879.43(15)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      130.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku SuperNova diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51173
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         77.159
_diffrn_reflns_theta_min         2.273
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2019)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.271
_refine_ls_extinction_coef       0.00062(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         11893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.6386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                9917
_reflns_number_total             11893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3005sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;

2022-12-20
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '4(C13 H14 N6), 5(H2 O)'
_cod_original_formula_iupac      '4C13 H14 N6, 5H2 O'
_cod_original_formula_sum        'C52 H66 N24 O5'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1107.28
_cod_database_code               2022109
_cod_database_fobs_code          2022109
_shelx_hkl_checksum              70650
_shelx_res_checksum              77306
_shelx_fab_checksum              37667