Synthesis, X-ray characterization and study of new ionic complexes of 2-pyridone, obtained by oxidation with I2
Antoniadis, Constantinos D.; Hadjikakou, Sotiris K.; Hadjiliadis, Nick; Kubicki, Maciej; Butler, Ian S.; New Journal of Chemistry 29 (2005) 714–; doi:10.1039/b417828a

data_7050069
_publ_section_title
;
 Synthesis, X-ray characterization and study of new ionic complexes of
 2-pyridone, obtained by oxidation with I2
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              714
_journal_paper_doi               10.1039/b417828a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C10 H11 N2 O2, 2(C5 H5 N O), I3'
_chemical_formula_sum            'C20 H21 I3 N4 O4'
_chemical_formula_weight         762.11
_chemical_name_common
'tris(2-hydroxypyridine)-2-hydroxypyridinium triiodide'
_chemical_name_systematic
;
tris(2-hydroxypyridine)-2-hydroxypyridinium triiodide
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.635(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0652(11)
_cell_length_b                   15.6176(14)
_cell_length_c                   11.5015(11)
_cell_measurement_reflns_used    2983
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     2490.8(4)
_computing_cell_refinement
'CrysAlisCCD v.169 (Oxford Diffraction, 2002a)'
_computing_data_collection
'CrysAlisCCD v.169 (Oxford Diffraction, 2002a)'
_computing_data_reduction
'CrysAlisRed v.169 (Oxford Diffraction, 2002b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'KUMA KM4CCD four-circle diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8005
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    3.797
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1989)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.178
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                2150
_reflns_number_total             3130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b417828a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050069