Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' #============================================================= # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ingmar Persson' _publ_contact_author_address ; Department of Chemistry Swedish University of Agricultural Sciences P.O.Box 7015 SE-75007 Uppsala Sweden ; _publ_contact_author_phone +46-18-671547 _publ_contact_author_fax +46-18-673476 _publ_contact_author_email Ingmar.Persson@kemi.slu.se #===================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The Hydration of the Scandium(III) Ion in Aqueous Solution and Crystalline Hydrates Studied by XAFS Spectroscopy, Large Angle X-Ray Scattering and Crystallography ; loop_ _publ_author_name _publ_author_address 'Patric Lindqvist-Reis' ; Institut fuer Nukleare Entsorgung Forschungszentrum Karlsruhe P.O. Box 3640 76021 Karlsruhe Germany ; 'Ingmar Persson ' ; Department of Chemistry Swedish University of Agricultural Sciences P.O.Box 7015 SE-75007 Uppsala Sweden ; 'Magnus Sandstrom' ; Department of Physical, Inorganic and Structural Chemistry Stockholm University SE-106 91 Stockholm Sweden ; #====================================================================== # 4. DATA data_scoms _database_code_depnum_ccdc_archive 'CCDC 602519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H18 O18 S6 Sc, H12 O6 Sc' _chemical_formula_sum 'C6 H30 O24 S6 Sc2' _chemical_formula_weight 768.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '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' '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' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-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' '-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' _cell_length_a 14.019(2) _cell_length_b 14.019(2) _cell_length_c 25.380(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4319.7(12) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 21 _cell_measurement_theta_max 32 _exptl_crystal_description hexagonal _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Syntex P21 4-circle diffractometer' _diffrn_measurement_method '\q-2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1398 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 20.05 _reflns_number_total 883 _reflns_number_gt 688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Syntex software' _computing_cell_refinement 'Syntex software' _computing_data_reduction 'SHELXTL PLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXL97 #========================================================================= # 8. Refinement Data _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fi t 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^)+(0.0385P)^2^+44.8017P] 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 883 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #========================================================================= # 9. Atomic Coordinates and Displacement Parameters 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.0000 0.0000 0.0000 0.0224(9) Uani 1 d S . . O1 O -0.1342(5) -0.0253(6) -0.0458(2) 0.0346(15) Uani 1 d . . . H1A H -0.195(7) -0.074(7) -0.044(3) 0.04(3) Uiso 1 d . . . H1B H -0.137(8) 0.010(7) -0.065(3) 0.06(4) Uiso 1 d . . . Sc2 Sc 0.0000 0.0000 0.5000 0.0223(9) Uani 1 d S . . O2 O -0.1322(5) -0.1082(5) 0.4530(3) 0.0343(15) Uani 1 d . . . H2A H -0.129(7) -0.132(7) 0.429(3) 0.05(4) Uiso 1 d . . . H2B H -0.199(9) -0.123(9) 0.459(4) 0.11(4) Uiso 1 d . . . Sc3 Sc 0.0000 0.0000 0.23106(8) 0.0209(7) Uani 1 d S . . O3 O -0.1356(4) -0.0862(4) 0.18120(17) 0.0310(12) Uani 1 d . . . O4 O -0.3283(4) -0.1725(4) 0.20020(19) 0.0438(14) Uani 1 d . . . O5 O -0.2644(4) -0.1493(4) 0.11042(18) 0.0450(15) Uani 1 d . . . S1 S -0.24325(14) -0.10499(15) 0.16309(7) 0.0277(6) Uani 1 d . . . C1 C -0.2324(7) 0.0243(6) 0.1604(3) 0.050(2) Uani 1 d . . . H11 H -0.2201 0.0550 0.1953 0.060 Uiso 1 calc R . . H12 H -0.2993 0.0172 0.1465 0.060 Uiso 1 calc R . . H13 H -0.1717 0.0720 0.1381 0.060 Uiso 1 calc R . . O6 O -0.0435(4) -0.1398(4) 0.27498(18) 0.0419(14) Uani 1 d . . . O7 O -0.1795(4) -0.3251(4) 0.2937(2) 0.0451(14) Uani 1 d . . . O8 O -0.1400(4) -0.1818(4) 0.35664(18) 0.0502(15) Uani 1 d . . . S2 S -0.09742(15) -0.22202(14) 0.31627(6) 0.0261(6) Uani 1 d . . . C2 C 0.0065(7) -0.2403(7) 0.3433(3) 0.056(2) Uani 1 d . . . H21 H 0.0642 -0.1712 0.3565 0.067 Uiso 1 calc R . . H22 H 0.0357 -0.2673 0.3167 0.067 Uiso 1 calc R . . H23 H -0.0231 -0.2925 0.3717 0.067 Uiso 1 calc 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 Sc1 0.0188(12) 0.0188(12) 0.029(2) 0.000 0.000 0.0094(6) O1 0.020(4) 0.034(4) 0.042(4) 0.005(3) -0.006(3) 0.008(3) Sc2 0.0236(12) 0.0236(12) 0.0198(19) 0.000 0.000 0.0118(6) O2 0.026(4) 0.044(4) 0.031(4) -0.014(3) -0.004(3) 0.016(3) Sc3 0.0187(9) 0.0187(9) 0.0252(14) 0.000 0.000 0.0094(4) O3 0.021(3) 0.030(3) 0.039(3) -0.009(2) -0.008(2) 0.011(2) O4 0.027(3) 0.053(4) 0.050(3) 0.006(3) 0.012(3) 0.019(3) O5 0.036(3) 0.060(4) 0.036(3) -0.019(3) -0.008(2) 0.021(3) S1 0.0198(12) 0.0323(12) 0.0283(11) -0.0032(9) -0.0001(9) 0.0111(9) C1 0.065(6) 0.045(5) 0.051(5) -0.003(4) -0.005(5) 0.036(5) O6 0.055(4) 0.032(3) 0.037(3) 0.016(3) 0.010(3) 0.020(3) O7 0.043(3) 0.027(3) 0.059(3) -0.007(3) -0.009(3) 0.013(3) O8 0.063(4) 0.067(4) 0.030(3) -0.007(3) 0.005(3) 0.040(3) S2 0.0318(11) 0.0209(11) 0.0259(11) 0.0014(9) 0.0027(9) 0.0134(10) C2 0.056(6) 0.050(6) 0.066(6) 0.003(5) -0.016(5) 0.030(5) #========================================================================= # 10. Molecular Geometry _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 s ymmetry. 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 Sc1 O1 2.085(6) 10 ? Sc1 O1 2.085(6) . ? Sc1 O1 2.085(6) 2 ? Sc1 O1 2.085(6) 12 ? Sc1 O1 2.085(6) 3 ? Sc1 O1 2.085(6) 11 ? O1 H1A 0.78(8) . ? O1 H1B 0.71(8) . ? Sc2 O2 2.086(5) . ? Sc2 O2 2.086(5) 10_556 ? Sc2 O2 2.086(5) 2 ? Sc2 O2 2.086(5) 3 ? Sc2 O2 2.086(5) 12_556 ? Sc2 O2 2.086(5) 11_556 ? O2 H2A 0.69(8) . ? O2 H2B 0.87(11) . ? Sc3 O6 2.064(5) 2 ? Sc3 O6 2.064(4) . ? Sc3 O6 2.064(4) 3 ? Sc3 O3 2.092(4) . ? Sc3 O3 2.092(4) 2 ? Sc3 O3 2.092(4) 3 ? O3 S1 1.470(5) . ? O4 S1 1.441(5) . ? O5 S1 1.441(5) . ? S1 C1 1.743(7) . ? C1 H11 0.9600 . ? C1 H12 0.9600 . ? C1 H13 0.9600 . ? O6 S2 1.458(5) . ? O7 S2 1.442(5) . ? O8 S2 1.436(5) . ? S2 C2 1.741(7) . ? C2 H21 0.9600 . ? C2 H22 0.9600 . ? C2 H23 0.9600 . ? 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 Sc1 O1 180.0 10 . ? O1 Sc1 O1 88.1(2) 10 2 ? O1 Sc1 O1 91.9(2) . 2 ? O1 Sc1 O1 91.9(2) 10 12 ? O1 Sc1 O1 88.1(2) . 12 ? O1 Sc1 O1 88.1(2) 2 12 ? O1 Sc1 O1 88.1(2) 10 3 ? O1 Sc1 O1 91.9(2) . 3 ? O1 Sc1 O1 91.9(2) 2 3 ? O1 Sc1 O1 180.0 12 3 ? O1 Sc1 O1 91.9(2) 10 11 ? O1 Sc1 O1 88.1(2) . 11 ? O1 Sc1 O1 180.0 2 11 ? O1 Sc1 O1 91.9(2) 12 11 ? O1 Sc1 O1 88.1(2) 3 11 ? Sc1 O1 H1A 129(6) . . ? Sc1 O1 H1B 128(8) . . ? H1A O1 H1B 103(9) . . ? O2 Sc2 O2 180.0 . 10_556 ? O2 Sc2 O2 90.5(3) . 2 ? O2 Sc2 O2 89.5(3) 10_556 2 ? O2 Sc2 O2 90.5(3) . 3 ? O2 Sc2 O2 89.5(3) 10_556 3 ? O2 Sc2 O2 90.5(3) 2 3 ? O2 Sc2 O2 89.5(3) . 12_556 ? O2 Sc2 O2 90.5(3) 10_556 12_556 ? O2 Sc2 O2 89.5(3) 2 12_556 ? O2 Sc2 O2 180.0 3 12_556 ? O2 Sc2 O2 89.5(3) . 11_556 ? O2 Sc2 O2 90.5(3) 10_556 11_556 ? O2 Sc2 O2 180.0 2 11_556 ? O2 Sc2 O2 89.5(3) 3 11_556 ? O2 Sc2 O2 90.5(3) 12_556 11_556 ? Sc2 O2 H2A 126(8) . . ? Sc2 O2 H2B 123(7) . . ? H2A O2 H2B 110(10) . . ? O6 Sc3 O6 93.58(19) 2 . ? O6 Sc3 O6 93.58(19) 2 3 ? O6 Sc3 O6 93.58(19) . 3 ? O6 Sc3 O3 174.7(2) 2 . ? O6 Sc3 O3 91.49(19) . . ? O6 Sc3 O3 87.60(18) 3 . ? O6 Sc3 O3 91.49(19) 2 2 ? O6 Sc3 O3 87.60(18) . 2 ? O6 Sc3 O3 174.7(2) 3 2 ? O3 Sc3 O3 87.21(19) . 2 ? O6 Sc3 O3 87.60(18) 2 3 ? O6 Sc3 O3 174.7(2) . 3 ? O6 Sc3 O3 91.49(19) 3 3 ? O3 Sc3 O3 87.21(19) . 3 ? O3 Sc3 O3 87.21(18) 2 3 ? S1 O3 Sc3 147.9(3) . . ? O5 S1 O4 113.5(3) . . ? O5 S1 O3 109.8(3) . . ? O4 S1 O3 110.6(3) . . ? O5 S1 C1 107.7(4) . . ? O4 S1 C1 108.7(4) . . ? O3 S1 C1 106.1(3) . . ? S1 C1 H11 109.5 . . ? S1 C1 H12 109.5 . . ? H11 C1 H12 109.5 . . ? S1 C1 H13 109.5 . . ? H11 C1 H13 109.5 . . ? H12 C1 H13 109.5 . . ? S2 O6 Sc3 158.3(3) . . ? O8 S2 O7 113.4(3) . . ? O8 S2 O6 110.8(3) . . ? O7 S2 O6 110.2(3) . . ? O8 S2 C2 108.6(4) . . ? O7 S2 C2 108.5(4) . . ? O6 S2 C2 105.0(4) . . ? S2 C2 H21 109.5 . . ? S2 C2 H22 109.5 . . ? H21 C2 H22 109.5 . . ? S2 C2 H23 109.5 . . ? H21 C2 H23 109.5 . . ? H22 C2 H23 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O7 0.78(8) 1.87(8) 2.654(8) 179(7) 8_444 O1 H1B O5 0.71(8) 1.94(9) 2.651(9) 173(10) 11 O2 H2A O8 0.69(8) 1.96(9) 2.635(8) 166(10) . O2 H2B O4 0.87(11) 1.76(11) 2.623(8) 176(10) 16_445 _diffrn_measured_fraction_theta_max 0.323 _diffrn_reflns_theta_full 20.05 _diffrn_measured_fraction_theta_full 0.323 _refine_diff_density_max 0.322 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.083