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_7050070
_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
;
2(C10 H11 N2 O2), 4(C5 H5 N O), 1.5(I7), 0.5(I5)
;
_chemical_formula_sum            'C40 H42 I13 N8 O8'
_chemical_formula_weight         2412.52
_chemical_name_common
;
hexakis(2-hydroxypyridine)-bis(2-hydroxypyridinium) di-
heptaiodide diiodine iodate
;
_chemical_name_systematic
;
hexakis(2-hydroxypyridine)-bis(2-hydroxypyridinium)
di-heptaiodide diiodine iodate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.545(12)
_cell_angle_beta                 76.688(12)
_cell_angle_gamma                86.422(12)
_cell_formula_units_Z            2
_cell_length_a                   11.2119(16)
_cell_length_b                   12.6039(18)
_cell_length_c                   23.715(3)
_cell_measurement_reflns_used    2420
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      3
_cell_volume                     3195.8(8)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0950
_diffrn_reflns_av_sigmaI/netI    0.1829
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26516
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    6.345
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1989)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2182
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.772
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         11040
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.771
_refine_ls_R_factor_all          0.2058
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                3319
_reflns_number_total             11040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b417828a.txt
_cod_data_source_block           2
_cod_original_cell_volume        3195.8(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050070