Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ulderico Mazzi' _publ_contact_author_address ; Pharmaceutical Sciences University of Padova via F. Marzolo n\%5 Padova 35131 ITALY ; _publ_contact_author_email ULDERICO.MAZZI@UNIPD.IT _publ_section_title ; Tris(1,2-dimethyl-3-hydroxy-4(1H)-pyridone)OxoTantalum(V): a new water soluble tantalum complex containing the [Ta=O]3+ core. ; loop_ _publ_author_name 'Ulderico Mazzi' 'Davide Camporese' 'Luciano Marchio' 'Mattia Riondato' 'Andrea Tapparo' 'Alberto Zampieri' # Attachment 'tao.cif' data_tao _database_code_depnum_ccdc_archive 'CCDC 289992' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H40 N3 O15 Ta' _chemical_formula_weight 755.51 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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.282(3) _cell_length_b 14.055(5) _cell_length_c 16.987(6) _cell_angle_alpha 65.704(5) _cell_angle_beta 89.155(6) _cell_angle_gamma 75.270(6) _cell_volume 1524.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10881 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 27.96 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 3.675 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.666 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_type 'Bruker Smart 1000 area detector' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 16173 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.96 _reflns_number_total 6663 _reflns_number_gt 5687 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6663 _refine_ls_number_parameters 401 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.1446(7) 0.0790(4) 0.4023(3) 0.0335(10) Uani 1 1 d . . . C12 C 0.1262(7) 0.0942(4) 0.0471(3) 0.0324(10) Uani 1 1 d . . . C13 C 0.3050(7) 0.2605(4) 0.1643(3) 0.0367(11) Uani 1 1 d . . . C21 C 0.2405(7) -0.0223(4) 0.4051(3) 0.0336(10) Uani 1 1 d . . . C22 C 0.2262(7) -0.0104(4) 0.1077(3) 0.0320(10) Uani 1 1 d . . . C23 C 0.1142(7) 0.3234(4) 0.1501(3) 0.0353(11) Uani 1 1 d . . . C31 C 0.3375(7) -0.1073(4) 0.4814(3) 0.0383(11) Uani 1 1 d . . . C32 C 0.3221(7) -0.0895(4) 0.0823(3) 0.0343(10) Uani 1 1 d . . . C33 C 0.0693(8) 0.4360(4) 0.1194(4) 0.0433(12) Uani 1 1 d . . . C41 C 0.2454(8) 0.0090(5) 0.5523(3) 0.0444(13) Uani 1 1 d . . . H41 H 0.2481 0.0184 0.6033 0.053 Uiso 1 1 calc R . . C42 C 0.2232(8) 0.0368(5) -0.0651(3) 0.0431(12) Uani 1 1 d . . . H42 H 0.2238 0.0514 -0.1237 0.052 Uiso 1 1 calc R . . C43 C 0.4003(9) 0.4233(5) 0.1136(4) 0.0542(15) Uani 1 1 d . . . H43 H 0.4961 0.4587 0.1005 0.065 Uiso 1 1 calc R . . C51 C 0.1483(8) 0.0949(5) 0.4783(3) 0.0430(12) Uani 1 1 d . . . H51 H 0.0870 0.1614 0.4787 0.052 Uiso 1 1 calc R . . C52 C 0.1275(7) 0.1174(4) -0.0418(3) 0.0410(12) Uani 1 1 d . . . H52 H 0.0649 0.1859 -0.0838 0.049 Uiso 1 1 calc R . . C53 C 0.4507(8) 0.3146(5) 0.1440(4) 0.0450(13) Uani 1 1 d . . . H53 H 0.5783 0.2758 0.1516 0.054 Uiso 1 1 calc R . . C61 C 0.4308(9) -0.1745(6) 0.6381(4) 0.0566(16) Uani 1 1 d . . . H61A H 0.4270 -0.1458 0.6807 0.085 Uiso 1 1 calc R . . H61B H 0.5612 -0.2042 0.6316 0.085 Uiso 1 1 calc R . . H61C H 0.3660 -0.2305 0.6566 0.085 Uiso 1 1 calc R . . C62 C 0.4254(10) -0.2007(5) 0.1464(4) 0.0553(15) Uani 1 1 d . . . H62A H 0.3580 -0.2513 0.1466 0.083 Uiso 1 1 calc R . . H62B H 0.4329 -0.2019 0.2032 0.083 Uiso 1 1 calc R . . H62C H 0.5519 -0.2205 0.1306 0.083 Uiso 1 1 calc R . . C63 C -0.1311(9) 0.5024(5) 0.1088(4) 0.0588(16) Uani 1 1 d . . . H63A H -0.1387 0.5485 0.1384 0.088 Uiso 1 1 calc R . . H63B H -0.2122 0.4554 0.1331 0.088 Uiso 1 1 calc R . . H63C H -0.1719 0.5462 0.0482 0.088 Uiso 1 1 calc R . . C71 C 0.4434(11) -0.2142(5) 0.4850(4) 0.0643(19) Uani 1 1 d . . . H71A H 0.5709 -0.2341 0.5117 0.096 Uiso 1 1 calc R . . H71B H 0.4481 -0.2100 0.4272 0.096 Uiso 1 1 calc R . . H71C H 0.3798 -0.2677 0.5185 0.096 Uiso 1 1 calc R . . C72 C 0.4082(8) -0.1464(5) -0.0370(4) 0.0484(14) Uani 1 1 d . . . H72A H 0.3350 -0.1980 -0.0243 0.073 Uiso 1 1 calc R . . H72B H 0.5353 -0.1831 -0.0085 0.073 Uiso 1 1 calc R . . H72C H 0.4134 -0.1118 -0.0985 0.073 Uiso 1 1 calc R . . C73 C 0.1808(11) 0.6028(5) 0.0697(5) 0.076(2) Uani 1 1 d . . . H73A H 0.3002 0.6208 0.0668 0.114 Uiso 1 1 calc R . . H73B H 0.1071 0.6261 0.1090 0.114 Uiso 1 1 calc R . . H73C H 0.1116 0.6386 0.0130 0.114 Uiso 1 1 calc R . . N11 N 0.3360(6) -0.0871(4) 0.5543(3) 0.0396(10) Uani 1 1 d . . . N12 N 0.3165(6) -0.0631(4) -0.0053(3) 0.0367(9) Uani 1 1 d . . . N13 N 0.2174(7) 0.4835(3) 0.1011(3) 0.0437(11) Uani 1 1 d . . . O1 O -0.1560(5) 0.0815(3) 0.2296(2) 0.0434(9) Uani 1 1 d . . . O2W O 0.132(3) -0.2217(10) 0.3283(7) 0.315(11) Uani 1 1 d . . . O3W O -0.0289(19) -0.3281(9) 0.2476(6) 0.095(4) Uani 0.50 1 d P . . O1W O -0.3601(7) -0.0703(4) 0.2714(3) 0.0613(11) Uani 1 1 d D . . O5W O -0.457(4) -0.3997(19) 0.3721(18) 0.243(15) Uani 0.50 1 d P . . O6W O 0.1952(14) -0.5402(8) 0.3218(7) 0.169(4) Uani 1 1 d . . . O7W O -0.0950(11) -0.6487(5) 0.3336(4) 0.097(2) Uani 1 1 d D . . O8W O -0.4555(13) -0.5014(8) 0.2696(6) 0.156(3) Uani 1 1 d . . . O9W O -0.227(3) -0.4621(14) 0.5089(10) 0.189(10) Uani 0.50 1 d P . . O11 O 0.0576(5) 0.1517(3) 0.3264(2) 0.0384(8) Uani 1 1 d . . . O10W O -0.250(4) -0.2969(19) 0.3469(13) 0.271(18) Uani 0.50 1 d P . . O12 O 0.0433(5) 0.1607(3) 0.0792(2) 0.0377(8) Uani 1 1 d . . . O13 O 0.3346(5) 0.1572(3) 0.1963(2) 0.0375(8) Uani 1 1 d . . . O21 O 0.2278(5) -0.0297(3) 0.3299(2) 0.0394(8) Uani 1 1 d . . . O22 O 0.2190(5) -0.0250(3) 0.1900(2) 0.0378(8) Uani 1 1 d . . . O23 O -0.0233(5) 0.2711(3) 0.1675(2) 0.0377(8) Uani 1 1 d . . . Ta Ta 0.07320(3) 0.102301(16) 0.219611(13) 0.03042(7) Uani 1 1 d . . . O4W O -0.048(2) -0.6572(11) 0.5056(7) 0.217(5) Uani 1 1 d . . . H1W H -0.288(8) -0.019(4) 0.262(5) 0.07(2) Uiso 1 1 d D . . H2W H -0.493(3) -0.034(5) 0.264(7) 0.14(4) Uiso 1 1 d D . . H13W H -0.071(11) -0.699(6) 0.306(5) 0.12(3) Uiso 1 1 d D . . H14W H 0.029(7) -0.634(8) 0.336(7) 0.14(5) Uiso 1 1 d 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 C11 0.034(2) 0.040(3) 0.031(2) -0.017(2) 0.0042(19) -0.014(2) C12 0.033(2) 0.037(3) 0.030(2) -0.014(2) 0.0053(19) -0.014(2) C13 0.041(3) 0.045(3) 0.024(2) -0.015(2) 0.0010(19) -0.011(2) C21 0.035(2) 0.041(3) 0.027(2) -0.016(2) 0.0052(19) -0.013(2) C22 0.033(2) 0.041(3) 0.027(2) -0.017(2) 0.0033(18) -0.015(2) C23 0.051(3) 0.034(3) 0.024(2) -0.011(2) 0.007(2) -0.018(2) C31 0.039(3) 0.046(3) 0.029(2) -0.013(2) 0.003(2) -0.016(2) C32 0.037(3) 0.040(3) 0.032(2) -0.018(2) 0.004(2) -0.014(2) C33 0.046(3) 0.041(3) 0.041(3) -0.018(2) 0.000(2) -0.007(2) C41 0.046(3) 0.066(4) 0.032(3) -0.028(3) 0.009(2) -0.018(3) C42 0.051(3) 0.053(3) 0.029(3) -0.018(2) 0.005(2) -0.018(3) C43 0.053(4) 0.050(3) 0.054(4) -0.013(3) 0.000(3) -0.022(3) C51 0.048(3) 0.050(3) 0.039(3) -0.025(3) 0.010(2) -0.015(2) C52 0.043(3) 0.044(3) 0.029(3) -0.010(2) 0.001(2) -0.009(2) C53 0.040(3) 0.050(3) 0.043(3) -0.018(3) 0.000(2) -0.011(2) C61 0.061(4) 0.071(4) 0.029(3) -0.012(3) -0.005(3) -0.016(3) C62 0.075(4) 0.040(3) 0.048(3) -0.021(3) -0.001(3) -0.004(3) C63 0.056(4) 0.041(3) 0.060(4) -0.009(3) 0.002(3) -0.002(3) C71 0.094(5) 0.044(3) 0.042(3) -0.016(3) -0.008(3) 0.002(3) C72 0.055(3) 0.061(4) 0.047(3) -0.038(3) 0.016(3) -0.020(3) C73 0.089(5) 0.034(3) 0.095(6) -0.012(4) -0.001(4) -0.027(3) N11 0.041(2) 0.055(3) 0.023(2) -0.0146(19) 0.0031(17) -0.015(2) N12 0.039(2) 0.048(2) 0.035(2) -0.026(2) 0.0090(18) -0.0175(19) N13 0.050(3) 0.030(2) 0.049(3) -0.010(2) -0.003(2) -0.017(2) O1 0.045(2) 0.051(2) 0.040(2) -0.0207(18) 0.0067(16) -0.0203(17) O2W 0.69(3) 0.178(11) 0.130(8) -0.020(8) 0.012(13) -0.289(17) O3W 0.151(11) 0.067(7) 0.039(5) -0.008(5) -0.020(6) -0.007(7) O1W 0.053(3) 0.055(3) 0.074(3) -0.025(2) 0.006(2) -0.015(2) O5W 0.28(3) 0.18(2) 0.27(3) -0.18(2) -0.16(2) 0.085(19) O6W 0.158(8) 0.172(9) 0.191(10) -0.094(8) 0.018(7) -0.038(7) O7W 0.134(6) 0.065(4) 0.096(5) -0.045(3) 0.016(4) -0.012(4) O8W 0.142(7) 0.151(8) 0.161(8) -0.073(7) 0.005(6) -0.006(6) O9W 0.27(2) 0.133(14) 0.092(10) -0.054(10) -0.022(12) 0.082(15) O11 0.044(2) 0.0379(19) 0.0327(18) -0.0154(16) 0.0040(15) -0.0086(15) O10W 0.32(3) 0.17(2) 0.119(15) 0.001(14) 0.010(18) 0.16(2) O12 0.045(2) 0.0349(18) 0.0288(17) -0.0121(15) 0.0028(14) -0.0052(15) O13 0.0388(19) 0.0359(19) 0.0360(19) -0.0130(16) 0.0039(15) -0.0107(15) O21 0.056(2) 0.0378(19) 0.0263(17) -0.0182(15) 0.0021(15) -0.0086(16) O22 0.052(2) 0.0346(18) 0.0229(16) -0.0109(14) 0.0016(14) -0.0070(15) O23 0.0370(18) 0.0373(18) 0.0345(18) -0.0136(15) 0.0019(14) -0.0055(15) Ta 0.03371(11) 0.03105(11) 0.02632(11) -0.01176(8) 0.00336(7) -0.00912(7) O4W 0.290(15) 0.213(12) 0.142(9) -0.070(9) 0.024(9) -0.067(11) _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 C11 O11 1.311(6) . ? C11 C21 1.399(7) . ? C11 C51 1.399(7) . ? C12 O12 1.288(6) . ? C12 C52 1.408(7) . ? C12 C22 1.409(7) . ? C13 O13 1.282(6) . ? C13 C23 1.408(7) . ? C13 C53 1.417(8) . ? C21 O21 1.330(6) . ? C21 C31 1.389(7) . ? C22 O22 1.329(5) . ? C22 C32 1.378(7) . ? C23 O23 1.348(6) . ? C23 C33 1.394(7) . ? C31 N11 1.378(6) . ? C31 C71 1.481(8) . ? C32 N12 1.376(6) . ? C32 C62 1.490(7) . ? C33 N13 1.376(7) . ? C33 C63 1.487(8) . ? C41 N11 1.331(7) . ? C41 C51 1.371(8) . ? C42 N12 1.352(7) . ? C42 C52 1.373(8) . ? C43 C53 1.344(8) . ? C43 N13 1.350(8) . ? C61 N11 1.474(7) . ? C72 N12 1.489(6) . ? C73 N13 1.486(7) . ? O1 Ta 1.761(4) . ? O11 Ta 2.186(3) . ? O12 Ta 2.174(3) . ? O13 Ta 2.202(4) . ? O21 Ta 2.088(3) . ? O22 Ta 2.083(3) . ? O23 Ta 2.086(4) . ? 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 O11 C11 C21 115.3(4) . . ? O11 C11 C51 125.7(5) . . ? C21 C11 C51 118.9(5) . . ? O12 C12 C52 126.0(5) . . ? O12 C12 C22 115.8(4) . . ? C52 C12 C22 118.1(4) . . ? O13 C13 C23 117.1(5) . . ? O13 C13 C53 124.5(5) . . ? C23 C13 C53 118.3(5) . . ? O21 C21 C31 123.9(5) . . ? O21 C21 C11 114.5(4) . . ? C31 C21 C11 121.6(4) . . ? O22 C22 C32 123.9(4) . . ? O22 C22 C12 114.1(4) . . ? C32 C22 C12 122.0(4) . . ? O23 C23 C33 121.2(5) . . ? O23 C23 C13 117.7(4) . . ? C33 C23 C13 121.1(5) . . ? N11 C31 C21 117.0(5) . . ? N11 C31 C71 120.7(5) . . ? C21 C31 C71 122.3(5) . . ? N12 C32 C22 117.6(4) . . ? N12 C32 C62 120.4(4) . . ? C22 C32 C62 122.0(5) . . ? N13 C33 C23 117.7(5) . . ? N13 C33 C63 120.9(5) . . ? C23 C33 C63 121.3(5) . . ? N11 C41 C51 122.9(5) . . ? N12 C42 C52 121.8(5) . . ? C53 C43 N13 123.2(6) . . ? C41 C51 C11 117.7(5) . . ? C42 C52 C12 118.6(5) . . ? C43 C53 C13 118.5(5) . . ? C41 N11 C31 121.9(4) . . ? C41 N11 C61 118.2(5) . . ? C31 N11 C61 119.9(5) . . ? C42 N12 C32 121.8(4) . . ? C42 N12 C72 117.7(4) . . ? C32 N12 C72 120.4(4) . . ? C43 N13 C33 121.2(5) . . ? C43 N13 C73 118.0(5) . . ? C33 N13 C73 120.8(5) . . ? C11 O11 Ta 117.4(3) . . ? C12 O12 Ta 117.5(3) . . ? C13 O13 Ta 114.3(3) . . ? C21 O21 Ta 120.7(3) . . ? C22 O22 Ta 120.1(3) . . ? C23 O23 Ta 115.5(3) . . ? O1 Ta O22 101.05(16) . . ? O1 Ta O23 95.23(16) . . ? O22 Ta O23 142.22(13) . . ? O1 Ta O21 101.17(16) . . ? O22 Ta O21 68.61(12) . . ? O23 Ta O21 140.73(13) . . ? O1 Ta O12 93.17(15) . . ? O22 Ta O12 72.37(12) . . ? O23 Ta O12 72.89(13) . . ? O21 Ta O12 140.27(13) . . ? O1 Ta O11 93.08(15) . . ? O22 Ta O11 139.96(13) . . ? O23 Ta O11 71.72(13) . . ? O21 Ta O11 71.98(13) . . ? O12 Ta O11 144.46(13) . . ? O1 Ta O13 170.48(15) . . ? O22 Ta O13 86.32(14) . . ? O23 Ta O13 75.29(13) . . ? O21 Ta O13 87.07(14) . . ? O12 Ta O13 83.26(13) . . ? O11 Ta O13 84.88(13) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 1.583 _refine_diff_density_min -1.174 _refine_diff_density_rms 0.119