Electronic Supplementary Information for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _audit_creation_method maXus _journal_coden_Cambridge 222 _publ_contact_author_name 'Zoltan Szabo' _publ_contact_author_address ; Department of Inorganic Chemistry Royal Institute of Technology (KTH) Teknikringen 30 Stockholm S-10044 SWEDEN ; _publ_contact_author_email ZOLTAN@KTH.SE loop_ _publ_author_name _publ_author_address 'Giuseppe Palladino' ; Inorganic Chemistry Royal Institute of Technology 100 44 Stockholm Sweden ; 'Zoltan Szabo' ; Inorganic Chemistry Royal Institute of Technology 100 44 Stockholm Sweden ; 'Andreas Fischer' ; Inorganic Chemistry Royal Institute of Technology 100 44 Stockholm Sweden ; 'Ingmar Grenthe' ; Inorganic Chemistry Royal Institute of Technology 100 44 Stockholm Sweden ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Structure, Equilibrium and Ligand Exchange Dynamics in the Binary and Ternary Dioxouranium(VI)-Ethylenediamine-N-N'-diacetic acid - Fluoride System; A Potentiometric, NMR and X-Ray study. ; _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Sheldrick, G.M. (1997). SHELXS-97. Program for Crystal Structure Solution. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal Structures. University of Gottingen, Germany. ; data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 611790' _chemical_compound_source 'Local laboratory' _exptl_crystal_description Fragment _exptl_crystal_colour Yellow _cell_measurement_temperature 299 _refine_ls_hydrogen_treatment constr _diffrn_measurement_device 'Bruker-Nonius KappaCCD' _computing_data_collection KappaCCD _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.432 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1100.57 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_cell_setting monoclinic _chemical_formula_moiety 'C18 H32 N6 O16 U2, 2(H2 O)' _chemical_formula_sum 'C18 H36 N6 O18 U2' _chemical_name_systematic ; ? ; _cell_length_a 18.805(2) _cell_length_b 6.3685(3) _cell_length_c 12.865(1) _cell_angle_alpha 90.00 _cell_angle_beta 102.775(7) _cell_angle_gamma 90.00 _cell_volume 1502.6(2) _diffrn_reflns_number 20893 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 4.52 _diffrn_reflns_theta_full 27.50 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _cell_measurement_reflns_used 119 _cell_measurement_theta_min 4.6 _cell_measurement_theta_max 20.4 _diffrn_measurement_method '\f & \w' _computing_cell_refinement 'Dirax/lsq (Duisenberg, 1992)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_T_max 0.853 _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.09 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 10.849 _reflns_number_total 3443 _reflns_number_gt 2673 _reflns_threshold_expression I>2\s(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0091P)^2^+2.5890P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3443 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0403 _refine_ls_wR_factor_gt 0.0362 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 U1 U 0.242849(8) 0.63028(2) 0.415832(11) 0.02090(5) Uani 1 1 d . . . C1 C 0.3920(3) 0.4356(6) 0.3692(3) 0.0310(10) Uani 1 1 d . . . C2 C 0.4189(2) 0.6503(7) 0.4110(3) 0.0343(10) Uani 1 1 d . . . C3 C 0.3914(2) 0.9458(7) 0.5172(4) 0.0362(11) Uani 1 1 d . . . C4 C 0.3353(2) 1.0170(7) 0.5752(3) 0.0341(11) Uani 1 1 d . . . C5 C 0.2032(2) 1.0343(6) 0.5564(3) 0.0280(9) Uani 1 1 d . . . C6 C 0.1316(3) 0.9600(6) 0.4878(3) 0.0307(10) Uani 1 1 d . . . C7 C 0.1054(2) 0.3455(7) 0.2769(3) 0.0297(10) Uani 1 1 d . . . C8 C 0.0962(2) 0.1448(6) 0.2141(3) 0.0270(9) Uani 1 1 d . . . C9 C 0.0319(2) -0.0133(6) 0.0460(3) 0.0289(10) Uani 1 1 d . . . N1 N 0.03273(18) 0.1608(5) 0.1230(2) 0.0226(7) Uani 1 1 d . . . N2 N 0.37566(19) 0.7257(5) 0.4853(3) 0.0273(8) Uani 1 1 d . . . N3 N 0.26254(18) 0.9894(5) 0.5041(2) 0.0250(8) Uani 1 1 d . . . O1 O 0.24597(17) 0.5266(4) 0.5441(2) 0.0325(7) Uani 1 1 d . . . O2 O 0.24303(17) 0.7483(4) 0.2918(2) 0.0346(7) Uani 1 1 d . . . O3 O 0.32909(16) 0.3841(4) 0.3818(2) 0.0357(7) Uani 1 1 d . . . O4 O 0.43085(18) 0.3255(5) 0.3258(3) 0.0455(8) Uani 1 1 d . . . O5 O 0.13676(16) 0.8125(4) 0.4229(2) 0.0305(7) Uani 1 1 d . . . O6 O 0.07386(18) 1.0357(5) 0.4967(3) 0.0476(9) Uani 1 1 d . . . O7 O 0.16494(16) 0.3570(5) 0.3470(2) 0.0372(7) Uani 1 1 d . . . O8 O 0.05735(19) 0.4758(5) 0.2594(3) 0.0514(10) Uani 1 1 d . . . O9 O 0.4306(2) 0.9699(6) 0.1907(3) 0.0575(10) Uani 1 1 d . . . H2A H 0.4699 0.6420 0.4471 0.041 Uiso 1 1 calc R . . H2B H 0.4146 0.7479 0.3520 0.041 Uiso 1 1 calc R . . H3A H 0.3897 1.0326 0.4547 0.043 Uiso 1 1 calc R . . H3B H 0.4396 0.9572 0.5630 0.043 Uiso 1 1 calc R . . H4A H 0.3388 0.9348 0.6396 0.041 Uiso 1 1 calc R . . H4B H 0.3431 1.1635 0.5951 0.041 Uiso 1 1 calc R . . H5A H 0.2008 1.1842 0.5687 0.034 Uiso 1 1 calc R . . H5B H 0.2119 0.9640 0.6249 0.034 Uiso 1 1 calc R . . H8A H 0.1399 0.1170 0.1881 0.032 Uiso 1 1 calc R . . H8B H 0.0891 0.0291 0.2597 0.032 Uiso 1 1 calc R . . H9A H 0.0284 -0.1469 0.0807 0.035 Uiso 1 1 calc R . . H9B H 0.0768 -0.0124 0.0206 0.035 Uiso 1 1 calc R . . H1A H 0.0343 0.2843 0.0896 0.027 Uiso 1 1 calc R . . H1B H -0.0086 0.1574 0.1473 0.027 Uiso 1 1 calc R . . H2 H 0.3907 0.6488 0.5458 0.033 Uiso 1 1 calc R . . H3 H 0.2593 1.0851 0.4508 0.030 Uiso 1 1 calc R . . H9C H 0.4745 0.9233 0.2039 0.069 Uiso 1 1 d R . . H9D H 0.4227 1.0497 0.2264 0.069 Uiso 1 1 d R . . 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 U1 0.02252(8) 0.01739(7) 0.02079(7) -0.00327(7) 0.00045(5) -0.00135(7) C1 0.033(3) 0.027(2) 0.031(2) 0.0012(17) 0.003(2) 0.0053(19) C2 0.030(2) 0.033(2) 0.040(2) 0.002(2) 0.0074(19) -0.001(2) C3 0.028(3) 0.025(2) 0.050(3) -0.0051(19) -0.002(2) -0.0047(18) C4 0.034(3) 0.027(2) 0.035(2) -0.0096(18) -0.005(2) -0.0049(19) C5 0.037(3) 0.021(2) 0.027(2) -0.0032(16) 0.0092(19) 0.0006(18) C6 0.039(3) 0.024(2) 0.031(2) -0.0025(18) 0.010(2) -0.0017(19) C7 0.036(3) 0.031(2) 0.0218(19) -0.0076(18) 0.0070(18) -0.009(2) C8 0.031(2) 0.026(2) 0.0201(18) -0.0018(17) -0.0029(16) -0.0031(19) C9 0.037(3) 0.023(2) 0.023(2) -0.0108(16) -0.0020(18) -0.0026(18) N1 0.0276(19) 0.0192(18) 0.0198(15) -0.0033(13) 0.0023(13) -0.0055(13) N2 0.026(2) 0.0213(18) 0.0328(19) -0.0012(14) 0.0021(16) -0.0011(14) N3 0.027(2) 0.0218(18) 0.0251(17) -0.0012(14) 0.0036(15) -0.0021(14) O1 0.0397(19) 0.0275(16) 0.0274(14) 0.0023(12) 0.0011(13) -0.0096(13) O2 0.047(2) 0.0328(17) 0.0240(14) 0.0020(12) 0.0075(14) 0.0006(14) O3 0.0294(17) 0.0226(15) 0.0548(18) -0.0069(14) 0.0085(14) 0.0008(14) O4 0.041(2) 0.039(2) 0.060(2) -0.0135(16) 0.0170(17) 0.0034(15) O5 0.0259(16) 0.0280(16) 0.0348(16) -0.0090(12) 0.0009(13) 0.0018(12) O6 0.035(2) 0.050(2) 0.061(2) -0.0252(17) 0.0173(17) -0.0004(16) O7 0.0345(17) 0.0346(17) 0.0368(16) -0.0120(14) -0.0047(13) -0.0130(15) O8 0.046(2) 0.052(2) 0.048(2) -0.0299(17) -0.0054(17) 0.0113(18) O9 0.047(2) 0.067(2) 0.054(2) -0.0217(19) 0.0019(18) 0.0070(19) _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 U1 O2 1.764(3) . ? U1 O1 1.766(3) . ? U1 O7 2.321(3) . ? U1 O5 2.328(3) . ? U1 O3 2.366(3) . ? U1 N2 2.534(3) . ? U1 N3 2.544(3) . ? C1 O4 1.232(5) . ? C1 O3 1.273(5) . ? C1 C2 1.515(6) . ? C2 N2 1.466(5) . ? C3 N2 1.472(5) . ? C3 C4 1.491(6) . ? C4 N3 1.479(5) . ? C5 N3 1.453(5) . ? C5 C6 1.513(6) . ? C6 O6 1.218(5) . ? C6 O5 1.274(5) . ? C7 O8 1.211(5) . ? C7 O7 1.275(5) . ? C7 C8 1.502(5) . ? C8 N1 1.481(4) . ? C9 N1 1.485(4) . ? C9 C9 1.498(7) 3 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2 0.9100 . ? N3 H3 0.9100 . ? O9 H9C 0.8573 . ? O9 H9D 0.7221 . ? 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 O2 U1 O1 176.19(13) . . ? O2 U1 O7 95.83(12) . . ? O1 U1 O7 87.95(11) . . ? O2 U1 O5 89.77(12) . . ? O1 U1 O5 90.08(13) . . ? O7 U1 O5 85.09(10) . . ? O2 U1 O3 88.66(12) . . ? O1 U1 O3 92.45(13) . . ? O7 U1 O3 80.40(11) . . ? O5 U1 O3 165.17(9) . . ? O2 U1 N2 91.03(13) . . ? O1 U1 N2 86.19(12) . . ? O7 U1 N2 143.56(11) . . ? O5 U1 N2 130.80(10) . . ? O3 U1 N2 63.99(10) . . ? O2 U1 N3 89.52(12) . . ? O1 U1 N3 86.98(11) . . ? O7 U1 N3 149.52(11) . . ? O5 U1 N3 64.90(10) . . ? O3 U1 N3 129.83(10) . . ? N2 U1 N3 65.92(11) . . ? O4 C1 O3 124.9(4) . . ? O4 C1 C2 119.3(4) . . ? O3 C1 C2 115.8(4) . . ? N2 C2 C1 109.7(4) . . ? N2 C3 C4 108.0(4) . . ? N3 C4 C3 108.4(3) . . ? N3 C5 C6 110.1(3) . . ? O6 C6 O5 123.5(4) . . ? O6 C6 C5 121.2(4) . . ? O5 C6 C5 115.3(4) . . ? O8 C7 O7 126.5(4) . . ? O8 C7 C8 119.4(4) . . ? O7 C7 C8 114.1(4) . . ? N1 C8 C7 110.1(3) . . ? N1 C9 C9 109.3(4) . 3 ? C8 N1 C9 111.4(3) . . ? C2 N2 C3 112.8(4) . . ? C2 N2 U1 109.7(2) . . ? C3 N2 U1 116.6(3) . . ? C5 N3 C4 113.0(3) . . ? C5 N3 U1 109.4(2) . . ? C4 N3 U1 114.0(2) . . ? C1 O3 U1 123.2(3) . . ? C6 O5 U1 125.6(3) . . ? C7 O7 U1 134.0(3) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? N2 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? N3 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? N3 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N3 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N3 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.2 . . ? N1 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? N1 C9 H9A 109.8 . . ? C9 C9 H9A 109.8 3 . ? N1 C9 H9B 109.8 . . ? C9 C9 H9B 109.8 3 . ? H9A C9 H9B 108.3 . . ? C8 N1 H1A 109.4 . . ? C9 N1 H1A 109.4 . . ? C8 N1 H1B 109.4 . . ? C9 N1 H1B 109.4 . . ? H1A N1 H1B 108.0 . . ? C2 N2 H2 105.6 . . ? C3 N2 H2 105.6 . . ? U1 N2 H2 105.6 . . ? C5 N3 H3 106.6 . . ? C4 N3 H3 106.6 . . ? U1 N3 H3 106.6 . . ? H9C O9 H9D 116.2 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.629 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.136