Co<sup>II</sup>-catalysed synthesis of <i>N</i>-(4-meth-oxy-phen-yl)-5-(pyridin-4-yl)-1,3,4-oxa-diazol-2-amine hemi-hydro-chloride monohydrate.
Gautam, Ram N.; Sonkar, Sankatha P.; Yadav, Shailendra; Nath, Paras; Bharty, Manoj K.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 351–354; doi:10.1107/S2056989024002044

data_2023048
_publ_section_title
;
 Co<sup>II</sup>-catalysed synthesis of
 <i>N</i>-(4-meth-oxy-phen-yl)-5-(pyridin-4-yl)-1,3,4-oxa-diazol-2-amine
 hemi-hydro-chloride monohydrate.
;
_journal_coeditor_code           HB8088
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              351
_journal_page_last               354
_journal_paper_doi               10.1107/S2056989024002044
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C28 H25 N8 O4 +, Cl -, 2H2 O'
_chemical_formula_moiety         'C28 H25 N8 O4 +, Cl -, 2(H2 O)'
_chemical_formula_sum            'C28 H29 Cl N8 O6'
_chemical_formula_weight         609.04
_chemical_name_common
;
<i>N</i>-(4-methoxyphenyl)-5-(pyridin-4-yl)-1,3,4-oxadiazol-2-amine
hemihydrochloride monohydrate
;
_chemical_name_systematic
;
<i>N</i>-(4-Methoxyphenyl)-5-(pyridin-4-yl)-1,3,4-oxadiazol-2-amine
4-{5-[(4-methoxyphenyl)amino]-1,3,4-oxadiazol-2-yl}pyridin-1-ium
chloride dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 107.006(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5406(9)
_cell_length_b                   13.7457(5)
_cell_length_c                   10.5650(3)
_cell_measurement_reflns_used    8519
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1520
_cell_measurement_theta_min      2.4650
_cell_volume                     2852.54(19)
_computing_cell_refinement
;
FRAMBO (Bruker, 2004)
;
_computing_data_collection
;
FRAMBO (Bruker, 2004)
;
_computing_data_reduction
;
FRAMBO (Bruker, 2004)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16772
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.472
_diffrn_source                   'sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56472
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pinkish
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0602P)^2^+1.1461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                2026
_reflns_number_total             3121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8088.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023048.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2023048
_shelx_hkl_checksum              39548
_shelx_res_checksum              68288