# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1514 data_italy1 _audit_creation_method SHELXL _chemical_name_systematic ; 'Tris(3-hydroxy-2(1H)-pyridonate)aluminium(III)' ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H9 Al N3 O6' _chemical_formula_weight 354.23 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 9.6840(14) _cell_length_b 9.6840(14) _cell_length_c 29.523(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2397.7(7) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 14.63 _cell_measurement_theta_max 19.72 _exptl_crystal_description 'chunk' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method ? _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 0.165 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.984 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method '\w-scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.57 _diffrn_reflns_number 1888 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 22.50 _reflns_number_total 705 _reflns_number_observed 640 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Rigaku/MSC Control Software' _computing_cell_refinement 'Rigaku/MSC Control Software' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+3.4391P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.49(52) _refine_ls_number_reflns 705 _refine_ls_number_parameters 77 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_obs 0.0413 _refine_ls_wR_factor_all 0.1211 _refine_ls_wR_factor_obs 0.1160 _refine_ls_goodness_of_fit_all 1.149 _refine_ls_goodness_of_fit_obs 1.162 _refine_ls_restrained_S_all 1.148 _refine_ls_restrained_S_obs 1.161 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al 0.6667 0.3333 0.96860(8) 0.0304(6) Uani 1 d S . O1 O 0.8498(3) 0.4336(4) 0.92995(9) 0.0372(9) Uani 1 d . . O2 O 0.7824(3) 0.5185(3) 1.00481(9) 0.0369(8) Uani 1 d . . C1 C 0.9509(5) 0.5734(6) 0.94453(15) 0.0359(12) Uani 1 d . . N2 N 1.0853(6) 0.6692(6) 0.9204(2) 0.0573(14) Uani 1 d . . C3 C 1.1923(8) 0.8072(8) 0.9357(2) 0.079(2) Uani 1 d . . H3 H 1.2859(8) 0.8673(8) 0.9194(2) 0.095 Uiso 1 calc R . C4 C 1.1710(6) 0.8627(6) 0.9733(3) 0.084(2) Uani 1 d . . H4 H 1.2463(6) 0.9658(6) 0.9819(3) 0.100 Uiso 1 calc R . C5 C 1.0266(8) 0.7657(6) 1.0043(2) 0.066(2) Uani 1 d . . H5 H 1.0141(8) 0.8013(6) 1.0324(2) 0.079 Uiso 1 calc R . C6 C 0.9192(5) 0.6228(5) 0.9863(2) 0.0379(12) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0331(7) 0.0331(7) 0.0250(9) 0.000 0.000 0.0166(4) O1 0.034(2) 0.041(2) 0.030(2) -0.008(2) 0.004(2) 0.0135(14) O2 0.042(2) 0.034(2) 0.0320(14) -0.0025(14) 0.005(2) 0.0163(14) C1 0.036(3) 0.049(3) 0.027(3) 0.003(2) 0.002(2) 0.024(2) N2 0.037(2) 0.059(3) 0.060(3) 0.017(2) 0.009(2) 0.012(2) C3 0.072(4) 0.080(4) 0.067(4) 0.000(3) 0.028(3) 0.024(4) C4 0.046(3) 0.025(3) 0.144(6) 0.005(4) 0.000(4) -0.008(2) C5 0.082(4) 0.046(3) 0.063(4) -0.024(3) -0.020(3) 0.027(3) C6 0.041(3) 0.031(3) 0.039(3) 0.000(2) -0.003(2) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.915(3) 3_665 ? Al1 O1 1.915(3) . yes Al1 O1 1.915(3) 2_655 ? Al1 O2 1.899(3) 3_665 ? Al1 O2 1.899(3) . yes Al1 O2 1.899(3) 2_655 ? O1 C1 1.285(6) . yes O2 C6 1.317(6) . yes C1 N2 1.362(6) . yes N2 C3 1.295(9) . yes C3 C4 1.294(11) . yes C3 H3 0.93 . ? C4 C5 1.538(10) . yes C4 H4 0.93 . ? C5 C6 1.355(6) . yes C5 H5 0.93 . ? C6 C1 1.412(5) . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 88.14(14) 3_665 . ? O1 Al1 O1 88.14(14) 3_665 2_655 ? O1 Al1 O1 88.14(14) . 2_655 yes O2 Al1 O2 91.40(15) 3_665 . ? O2 Al1 O2 91.40(15) 3_665 2_655 ? O2 Al1 O2 91.40(15) . 2_655 yes O2 Al1 O1 84.08(9) . . yes O2 Al1 O1 84.08(9) 2_655 2_655 ? O2 Al1 O1 84.08(9) 3_665 3_665 ? O2 Al1 O1 97.08(10) . 2_655 yes O2 Al1 O1 97.08(10) 2_655 3_665 ? O2 Al1 O1 97.09(10) 3_665 . ? O2 Al1 O1 170.47(11) . 3_665 yes O2 Al1 O1 170.47(10) 2_655 . ? O2 Al1 O1 170.47(11) 3_665 2_655 ? C1 O1 Al1 111.1(3) . . yes C6 O2 Al1 112.6(3) . . yes O1 C1 N2 120.5(4) . . ? O1 C1 C6 118.0(4) . . ? N2 C1 C6 121.4(5) . . ? C3 N2 C1 121.3(5) . . ? C4 C3 N2 121.1(6) . . ? C4 C3 H3 119.5(4) . . ? N2 C3 H3 119.5(3) . . ? C3 C4 C5 122.8(5) . . ? C3 C4 H4 118.6(4) . . ? C5 C4 H4 118.6(3) . . ? C6 C5 C4 113.0(5) . . ? C6 C5 H5 123.5(4) . . ? C4 C5 H5 123.5(3) . . ? O2 C6 C5 125.8(5) . . ? O2 C6 C1 114.1(4) . . ? C5 C6 C1 120.1(5) . . ? _refine_diff_density_max 0.268 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.045