9ddb19ce-4412-4989-9420-7bd7014865292020-06-24T09:08:23.023328SUCCESS9ddb19ce-4412-4989-9420-7bd701486529.htmlTable 1 Crystallographic data for Sc complexes0C14H26Cl13N2O5Sb2ScFormula[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNC12H24Cl6FeO6ScFormula[ScCl2(18-crown-6)][FeCl4]C12H30Cl3O9ScFormula[ScCl3(H2O)3]·18-crown-6C16H48N5NaO32Sc2Formula[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3C8H30N4O24Sc2Formula[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4C16H36N3O19ScFormula[Sc(NO3)3(H2O)2]·(12-crown-4)21051.68M[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN577.82M[ScCl2(18-crown-6)][FeCl4]469.67M[ScCl3(H2O)3]·18-crown-6935.50M[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3656.28M[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4619.44M[Sc(NO3)3(H2O)2]·(12-crown-4)2OrthorhombicCrystal system[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNOrthorhombicCrystal system[ScCl2(18-crown-6)][FeCl4]OrthorhombicCrystal system[ScCl3(H2O)3]·18-crown-6TriclinicCrystal system[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3TriclinicCrystal system[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4OrthorhombicCrystal system[Sc(NO3)3(H2O)2]·(12-crown-4)2Pbca (no. 61)Space group[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNPna21 (no. 33)Space group[ScCl2(18-crown-6)][FeCl4]Pbcn (no. 60)Space group[ScCl3(H2O)3]·18-crown-6P1̄ (no. 2)Space group[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3P1̄ (no. 2)Space group[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4P21212 (no. 18)Space group[Sc(NO3)3(H2O)2]·(12-crown-4)221.209(2)a/Å[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN19.2026(15)a/Å[ScCl2(18-crown-6)][FeCl4]10.7210(10)a/Å[ScCl3(H2O)3]·18-crown-68.7342(10)a/Å[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)37.5712(15)a/Å[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-411.6362(15)a/Å[Sc(NO3)3(H2O)2]·(12-crown-4)213.4224(10)b/Å[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN11.2156(10)b/Å[ScCl2(18-crown-6)][FeCl4]14.8569(15)b/Å[ScCl3(H2O)3]·18-crown-613.4735(15)b/Å[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)39.2350(15)b/Å[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-413.432(3)b/Å[Sc(NO3)3(H2O)2]·(12-crown-4)224.800(2)c/Å[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN21.0990(15)c/Å[ScCl2(18-crown-6)][FeCl4]13.2776(15)c/Å[ScCl3(H2O)3]·18-crown-616.842(3)c/Å[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)39.862(3)c/Å[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-48.7311(10)c/Å[Sc(NO3)3(H2O)2]·(12-crown-4)290.0α/°[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN90.0α/°[ScCl2(18-crown-6)][FeCl4]90.0α/°[ScCl3(H2O)3]·18-crown-6100.341(4)α/°[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)385.497(7)α/°[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-490.0α/°[Sc(NO3)3(H2O)2]·(12-crown-4)290.0β/°[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN90.0β/°[ScCl2(18-crown-6)][FeCl4]90.0β/°[ScCl3(H2O)3]·18-crown-698.989(4)β/°[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)384.869(8)β/°[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-490.0β/°[Sc(NO3)3(H2O)2]·(12-crown-4)290.0γ/°[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN90.0γ/°[ScCl2(18-crown-6)][FeCl4]90.0γ/°[ScCl3(H2O)3]·18-crown-693.665(7)γ/°[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)369.545(15)γ/°[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-490.0γ/°[Sc(NO3)3(H2O)2]·(12-crown-4)27060.0(10)U/Å3[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN4544.1(6)U/Å3[ScCl2(18-crown-6)][FeCl4]2114.9(4)U/Å3[ScCl3(H2O)3]·18-crown-61917.2(4)U/Å3[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3642.7(2)U/Å3[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-41364.7(3)U/Å3[Sc(NO3)3(H2O)2]·(12-crown-4)21.979Dcalc/g cm−3[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN1.689Dcalc/g cm−3[ScCl2(18-crown-6)][FeCl4]1.475Dcalc/g cm−3[ScCl3(H2O)3]·18-crown-61.621Dcalc/g cm−3[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)31.696Dcalc/g cm−3[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-41.507Dcalc/g cm−3[Sc(NO3)3(H2O)2]·(12-crown-4)28Z[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN8Z[ScCl2(18-crown-6)][FeCl4]4Z[ScCl3(H2O)3]·18-crown-62Z[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)31Z[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-42Z[Sc(NO3)3(H2O)2]·(12-crown-4)24064F(000)[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN2344F(000)[ScCl2(18-crown-6)][FeCl4]984F(000)[ScCl3(H2O)3]·18-crown-6976F(000)[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3340F(000)[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4652F(000)[Sc(NO3)3(H2O)2]·(12-crown-4)20.36 × 0.24 × 0.16Crystal size/mm[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN0.26 × 0.26 × 0.20Crystal size/mm[ScCl2(18-crown-6)][FeCl4]0.30 × 0.26 × 0.20Crystal size/mm[ScCl3(H2O)3]·18-crown-60.32 × 0.30 × 0.26Crystal size/mm[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)30.26 × 0.20 × 0.10Crystal size/mm[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-40.28 × 0.20 × 0.18Crystal size/mm[Sc(NO3)3(H2O)2]·(12-crown-4)238521No. reflections measured[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN33479No. reflections measured[ScCl2(18-crown-6)][FeCl4]17374No. reflections measured[ScCl3(H2O)3]·18-crown-626054No. reflections measured[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)38198No. reflections measured[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-49719No. reflections measured[Sc(NO3)3(H2O)2]·(12-crown-4)28017 (0.107)No. unique reflns (Rint)[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN10116 (0.060)No. unique reflns (Rint)[ScCl2(18-crown-6)][FeCl4]2415(0.073)No. unique reflns (Rint)[ScCl3(H2O)3]·18-crown-66636 (0.058)No. unique reflns (Rint)[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)32801 (0.085)No. unique reflns (Rint)[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-43109 (0.050)No. unique reflns (Rint)[Sc(NO3)3(H2O)2]·(12-crown-4)255.02θ(max)/°[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN55.02θ(max)/°[ScCl2(18-crown-6)][FeCl4]54.92θ(max)/°[ScCl3(H2O)3]·18-crown-650.02θ(max)/°[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)354.92θ(max)/°[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-454.92θ(max)/°[Sc(NO3)3(H2O)2]·(12-crown-4)20.8822, 0.7992Max., min. transmission[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN0.8875, 0.8157Max., min. transmission[ScCl2(18-crown-6)][FeCl4]0.9492, 0.7854Max., min. transmission[ScCl3(H2O)3]·18-crown-60.8954, 0.8798Max., min. transmission[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)30.9230, 0.8746Max., min. transmission[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-40.8857, 0.8521Max., min. transmission[Sc(NO3)3(H2O)2]·(12-crown-4)28017No. of data in refinement[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN10116No. of data in refinement[ScCl2(18-crown-6)][FeCl4]2415No. of data in refinement[ScCl3(H2O)3]·18-crown-66636No. of data in refinement[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)32801No. of data in refinement[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-43109No. of data in refinement[Sc(NO3)3(H2O)2]·(12-crown-4)2335/0No. params/restraints[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN470/1No. params/restraints[ScCl2(18-crown-6)][FeCl4]125/3No. params/restraints[ScCl3(H2O)3]·18-crown-6493/3No. params/restraints[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3191/6No. params/restraints[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4185/2No. params/restraints[Sc(NO3)3(H2O)2]·(12-crown-4)2n.a.Flack parameter[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN0.09(1)Flack parameter[ScCl2(18-crown-6)][FeCl4]n.a.Flack parameter[ScCl3(H2O)3]·18-crown-6n.a.Flack parameter[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3n.a.Flack parameter[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-40.00(3)Flack parameter[Sc(NO3)3(H2O)2]·(12-crown-4)227.19μ/cm−1[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN16.67μ/cm−1[ScCl2(18-crown-6)][FeCl4]7.65μ/cm−1[ScCl3(H2O)3]·18-crown-64.79μ/cm−1[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)36.36μ/cm−1[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-43.58μ/cm−1[Sc(NO3)3(H2O)2]·(12-crown-4)20.952S[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN0.992S[ScCl2(18-crown-6)][FeCl4]1.036S[ScCl3(H2O)3]·18-crown-61.019S[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)31.027S[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-41.015S[Sc(NO3)3(H2O)2]·(12-crown-4)20.003Max. shift/e.s.d.[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN0.001Max. shift/e.s.d.[ScCl2(18-crown-6)][FeCl4]0.001Max. shift/e.s.d.[ScCl3(H2O)3]·18-crown-60.001Max. shift/e.s.d.[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)30.000Max. shift/e.s.d.[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-40.000Max. shift/e.s.d.[Sc(NO3)3(H2O)2]·(12-crown-4)2−0.97 to +0.94Residual e-density/e Å−3[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN−0.56 to +0.44Residual e-density/e Å−3[ScCl2(18-crown-6)][FeCl4]–0.39 to +0.37Residual e-density/e Å−3[ScCl3(H2O)3]·18-crown-6−0.56 to +1.01Residual e-density/e Å−3[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3−0.47 to +0.34Residual e-density/e Å−3[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4−0.37 to +0.22Residual e-density/e Å−3[Sc(NO3)3(H2O)2]·(12-crown-4)20.042 ( 4920 refs)R (I > 2σ(I))[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN0.039 (7859 refs)R (I > 2σ(I))[ScCl2(18-crown-6)][FeCl4]0.038 (1767 refs)R (I > 2σ(I))[ScCl3(H2O)3]·18-crown-60.050 (4294 refs)R (I > 2σ(I))[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)30.041 (2053 refs)R (I > 2σ(I))[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-40.041 (2506 refs)R (I > 2σ(I))[Sc(NO3)3(H2O)2]·(12-crown-4)20.098R (all data)[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN0.065R (all data)[ScCl2(18-crown-6)][FeCl4]0.062R (all data)[ScCl3(H2O)3]·18-crown-60.090R (all data)[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)30.069R (all data)[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-40.060R (all data)[Sc(NO3)3(H2O)2]·(12-crown-4)20.086wR2 (all data)[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN0.080wR2 (all data)[ScCl2(18-crown-6)][FeCl4]0.092wR2 (all data)[ScCl3(H2O)3]·18-crown-60.145wR2 (all data)[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)30.098wR2 (all data)[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-40.088wR2 (all data)[Sc(NO3)3(H2O)2]·(12-crown-4)2Compound[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN[ScCl2(18-crown-6)][FeCl4][ScCl3(H2O)3]·18-crown-6[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4[Sc(NO3)3(H2O)2]·(12-crown-4)2FormulaC14H26Cl13N2O5Sb2ScC12H24Cl6FeO6ScC12H30Cl3O9ScC16H48N5NaO32Sc2C8H30N4O24Sc2C16H36N3O19ScM1051.68577.82469.67935.50656.28619.44Crystal systemOrthorhombicOrthorhombicOrthorhombicTriclinicTriclinicOrthorhombicSpace groupPbca (no. 61)Pna21 (no. 33)Pbcn (no. 60)P1̄ (no. 2)P1̄ (no. 2)P21212 (no. 18)a/Å21.209(2)19.2026(15)10.7210(10)8.7342(10)7.5712(15)11.6362(15)b/Å13.4224(10)11.2156(10)14.8569(15)13.4735(15)9.2350(15)13.432(3)c/Å24.800(2)21.0990(15)13.2776(15)16.842(3)9.862(3)8.7311(10)α/°90.090.090.0100.341(4)85.497(7)90.0β/°90.090.090.098.989(4)84.869(8)90.0γ/°90.090.090.093.665(7)69.545(15)90.0U/Å37060.0(10)4544.1(6)2114.9(4)1917.2(4)642.7(2)1364.7(3)Dcalc/g cm−31.9791.6891.4751.6211.6961.507Z884212F(000)40642344984976340652Crystal size/mm0.36 × 0.24 × 0.160.26 × 0.26 × 0.200.30 × 0.26 × 0.200.32 × 0.30 × 0.260.26 × 0.20 × 0.100.28 × 0.20 × 0.18No. reflections measured3852133479173742605481989719No. unique reflns (Rint)8017 (0.107)10116 (0.060)2415(0.073)6636 (0.058)2801 (0.085)3109 (0.050)2θ(max)/°55.055.054.950.054.954.9Max., min. transmission0.8822, 0.79920.8875, 0.81570.9492, 0.78540.8954, 0.87980.9230, 0.87460.8857, 0.8521No. of data in refinement8017101162415663628013109No. params/restraints335/0470/1125/3493/3191/6185/2Flack parametern.a.0.09(1)n.a.n.a.n.a.0.00(3)μ/cm−127.1916.677.654.796.363.58S0.9520.9921.0361.0191.0271.015Max. shift/e.s.d.0.0030.0010.0010.0010.0000.000Residual e-density/e Å−3−0.97 to +0.94−0.56 to +0.44–0.39 to +0.37−0.56 to +1.01−0.47 to +0.34−0.37 to +0.22R (I > 2σ(I))0.042 ( 4920 refs)0.039 (7859 refs)0.038 (1767 refs)0.050 (4294 refs)0.041 (2053 refs)0.041 (2506 refs)R (all data)0.0980.0650.0620.0900.0690.060wR2 (all data)0.0860.0800.0920.1450.0980.088Table 2 Selected bond lengths (Å) and angles (°) for [ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN02.135(3)Sc(1)–O(1)2.361(2)Sc(1)–O(4)Sc(1)–O(1)Sc(1)–N(1)2.154(3)Sc(1)–O(1)2.272(4)2.155(3)Sc(1)–O(2)2.361(2)Sc(1)–O(5)Sc(1)–O(2)Sc(1)–N(1)2.176(3)Sc(1)–O(2)2.272(4)2.164(3)Sc(1)–O(3)2.361(2)NoValueSc(1)–O(3)Sc(1)–N(1)NoValueSc(1)–O(3)2.272(4)1.444(6)–1.469(6)C–O2.361(2)C–C (ring)C–OSc(1)–N(1)1.477(7)–1.501(7)C–O2.272(4)2.356(1)–2.382(1)Sb(1)–Cl2.361(2)NoValueSb(1)–ClSc(1)–N(1)NoValueSb(1)–Cl2.272(4)2.356(1)–2.372(1)Sb(2)–Cl2.361(2)NoValueSb(2)–ClSc(1)–N(1)NoValueSb(2)–Cl2.272(4)71.2(1)O(1)–Sc(1)–O(2)2.361(2)O(5)–Sc(1)–O(1)O(1)–Sc(1)–O(2)Sc(1)–N(1)71.7(1)O(1)–Sc(1)–O(2)2.272(4)72.1(1)O(2)–Sc(1)–O(3)2.361(2)N(1)–Sc(1)–Cl(1)O(2)–Sc(1)–O(3)Sc(1)–N(1)178.2(1)O(2)–Sc(1)–O(3)2.272(4)71.5(1)O(3)–Sc(1)–O(4)2.361(2)O(5)–Sc(1)–Cl(1)O(3)–Sc(1)–O(4)Sc(1)–N(1)92.14(9)O(3)–Sc(1)–O(4)2.272(4)72.5(1)O(4)–Sc(1)–O(5)2.361(2)O(4)–Sc(1)–Cl(1)O(4)–Sc(1)–O(5)Sc(1)–N(1)95.7(1)O(4)–Sc(1)–O(5)2.272(4)Sc(1)–Cl(1)2.361(2)Sc(1)–N(1)2.272(4)Sc(1)–O(1)2.135(3)Sc(1)–O(4)2.154(3)Sc(1)–O(2)2.155(3)Sc(1)–O(5)2.176(3)Sc(1)–O(3)2.164(3)C–O1.444(6)–1.469(6)C–C (ring)1.477(7)–1.501(7)Sb(1)–Cl2.356(1)–2.382(1)Sb(2)–Cl2.356(1)–2.372(1)O(1)–Sc(1)–O(2)71.2(1)O(5)–Sc(1)–O(1)71.7(1)O(2)–Sc(1)–O(3)72.1(1)N(1)–Sc(1)–Cl(1)178.2(1)O(3)–Sc(1)–O(4)71.5(1)O(5)–Sc(1)–Cl(1)92.14(9)O(4)–Sc(1)–O(5)72.5(1)O(4)–Sc(1)–Cl(1)95.7(1)Table 3 Selected bond lengths (Å) and angles (°) for [ScCl2(18-crown-6)][FeCl4]02.195(2)Sc(1)–O(1)2.435(1)Sc(1)–O(5)Sc(1)–O(1)Sc(1)–Cl(2)2.243(2)Sc(1)–O(1)2.413(1)2.192(2)Sc(1)–O(2)2.435(1)Sc(1)–O(6)Sc(1)–O(2)Sc(1)–Cl(2)2.210(2)Sc(1)–O(2)2.413(1)2.230(2)Sc(1)–O(3)2.435(1)NoValueSc(1)–O(3)Sc(1)–Cl(2)NoValueSc(1)–O(3)2.413(1)2.425(1)Sc(2)–Cl(3)2.435(1)Sc(2)–Cl(4)Sc(2)–Cl(3)Sc(1)–Cl(2)2.402(1)Sc(2)–Cl(3)2.413(1)2.264(2)Sc(2)–O(7)2.435(1)Sc(2)–O(11)Sc(2)–O(7)Sc(1)–Cl(2)2.213(2)Sc(2)–O(7)2.413(1)2.216(2)Sc(2)–O(9)2.435(1)Sc(2)–O(12)Sc(2)–O(9)Sc(1)–Cl(2)2.202(2)Sc(2)–O(9)2.413(1)2.200(2)Sc(2)–O(10)2.435(1)NoValueSc(2)–O(10)Sc(1)–Cl(2)NoValueSc(2)–O(10)2.413(1)1.417(4)–1.473(4)C–O2.435(1)C–CC–OSc(1)–Cl(2)1.483(5)–1.503(5)C–O2.413(1)2.179(1)–2.202(1)Fe(1)–Cl2.435(1)NoValueFe(1)–ClSc(1)–Cl(2)NoValueFe(1)–Cl2.413(1)2.184(1)–2.202(1)Fe(2)–Cl2.435(1)NoValueFe(2)–ClSc(1)–Cl(2)NoValueFe(2)–Cl2.413(1)70.76(9)O(1)–Sc(1)–O(2)2.435(1)O(6)–Sc(1)–O(1)O(1)–Sc(1)–O(2)Sc(1)–Cl(2)69.60(9)O(1)–Sc(1)–O(2)2.413(1)71.68(8)O(2)–Sc(1)–O(3)2.435(1)Cl(1)–Sc(1)–Cl(2)O(2)–Sc(1)–O(3)Sc(1)–Cl(2)177.96(5)O(2)–Sc(1)–O(3)2.413(1)77.50(9)O(3)–Sc(1)–O(5)2.435(1)O(1)–Sc(1)–Cl(1)O(3)–Sc(1)–O(5)Sc(1)–Cl(2)85.58(7)O(3)–Sc(1)–O(5)2.413(1)71.72(8)O(5)–Sc(1)–O(6)2.435(1)O(3)–Sc(1)–Cl(1)O(5)–Sc(1)–O(6)Sc(1)–Cl(2)95.50(7)O(5)–Sc(1)–O(6)2.413(1)77.85(9)O(7)–Sc(2)–O(9)2.435(1)O(12)–Sc(2)-O(7)O(7)–Sc(2)–O(9)Sc(1)–Cl(2)72.28(9)O(7)–Sc(2)–O(9)2.413(1)70.66(8)O(9)–Sc(2)–O(10)2.435(1)Cl(3)–Sc(2)–Cl(4)O(9)–Sc(2)–O(10)Sc(1)–Cl(2)176.35(4)O(9)–Sc(2)–O(10)2.413(1)71.11(9)O(10)–Sc(2)–O(11)2.435(1)O(11)–Sc(2)–Cl(3)O(10)–Sc(2)–O(11)Sc(1)–Cl(2)86.47(7)O(10)–Sc(2)–O(11)2.413(1)68.96(9)O(11)–Sc(2)–O(12)2.435(1)O(9)–Sc(2)–Cl(3)O(11)–Sc(2)–O(12)Sc(1)–Cl(2)95.12(7)O(11)–Sc(2)–O(12)2.413(1)Sc(1)–Cl(1)2.435(1)Sc(1)–Cl(2)2.413(1)Sc(1)–O(1)2.195(2)Sc(1)–O(5)2.243(2)Sc(1)–O(2)2.192(2)Sc(1)–O(6)2.210(2)Sc(1)–O(3)2.230(2)Sc(2)–Cl(3)2.425(1)Sc(2)–Cl(4)2.402(1)Sc(2)–O(7)2.264(2)Sc(2)–O(11)2.213(2)Sc(2)–O(9)2.216(2)Sc(2)–O(12)2.202(2)Sc(2)–O(10)2.200(2)C–O1.417(4)–1.473(4)C–C1.483(5)–1.503(5)Fe(1)–Cl2.179(1)–2.202(1)Fe(2)–Cl2.184(1)–2.202(1)O(1)–Sc(1)–O(2)70.76(9)O(6)–Sc(1)–O(1)69.60(9)O(2)–Sc(1)–O(3)71.68(8)Cl(1)–Sc(1)–Cl(2)177.96(5)O(3)–Sc(1)–O(5)77.50(9)O(1)–Sc(1)–Cl(1)85.58(7)O(5)–Sc(1)–O(6)71.72(8)O(3)–Sc(1)–Cl(1)95.50(7)O(7)–Sc(2)–O(9)77.85(9)O(12)–Sc(2)-O(7)72.28(9)O(9)–Sc(2)–O(10)70.66(8)Cl(3)–Sc(2)–Cl(4)176.35(4)O(10)–Sc(2)–O(11)71.11(9)O(11)–Sc(2)–Cl(3)86.47(7)O(11)–Sc(2)–O(12)68.96(9)O(9)–Sc(2)–Cl(3)95.12(7)Table 4 Selected bond lengths (Å) and angles (°) for [ScCl3(H2O)3]·18-crown-602.142(1)Sc(1)–O(5)2.177(2)Sc(1)–Cl(2)Sc(1)–O(5)Sc(1)–Cl(1)2.4267(8)Sc(1)–O(5)2.4403(6)1.419(3)–1.446(3)C–O2.177(2)C–CC–OSc(1)–Cl(1)1.441(3)–1.484(4)C–O2.4403(6)81.89(4)O(4)–Sc(1)–O(5)2.177(2)O(4)–Sc(1)–Cl(1)O(4)–Sc(1)–O(5)Sc(1)–Cl(1)88.14(2)O(4)–Sc(1)–O(5)2.4403(6)163.78(8)O(5)–Sc(1)–O(5i)2.177(2)O(4)–Sc(1)–Cl(2)O(5)–Sc(1)–O(5i)Sc(1)–Cl(1)180.00O(5)–Sc(1)–O(5i)2.4403(6)91.86(2)Cl(1)–Sc(1)–Cl(2)2.177(2)O(5)–Sc(1)–Cl(1)Cl(1)–Sc(1)–Cl(2)Sc(1)–Cl(1)89.79(5)Cl(1)–Sc(1)–Cl(2)2.4403(6)176.27(3)Cl(1)–Sc(1)–Cl(1i)2.177(2)O(5)–Sc(1)–Cl(2)Cl(1)–Sc(1)–Cl(1i)Sc(1)–Cl(1)98.11(4)Cl(1)–Sc(1)–Cl(1i)2.4403(6)Sc(1)–O(4)2.177(2)Sc(1)–Cl(1)2.4403(6)Sc(1)–O(5)2.142(1)Sc(1)–Cl(2)2.4267(8)C–O1.419(3)–1.446(3)C–C1.441(3)–1.484(4)O(4)–Sc(1)–O(5)81.89(4)O(4)–Sc(1)–Cl(1)88.14(2)O(5)–Sc(1)–O(5i)163.78(8)O(4)–Sc(1)–Cl(2)180.00Cl(1)–Sc(1)–Cl(2)91.86(2)O(5)–Sc(1)–Cl(1)89.79(5)Cl(1)–Sc(1)–Cl(1i)176.27(3)O(5)–Sc(1)–Cl(2)98.11(4)Table 5 Selected bond lengths (Å) and angles (°) for [Sc(NO3)3(H2O)2]·(12-crown-4)202.268(1)Sc(1)–O(3)2.252(2)Sc(1)–O(6)Sc(1)–O(3)Sc(1)–O(4)2.105(2)Sc(1)–O(3)2.201(2)1.417(3)–1.444(3)C–O2.252(2)C–CC–OSc(1)–O(4)1.492(3)–1.505(4)C–O2.201(2)56.98(7)O(1)–Sc(1)–O(1i)2.252(2)O(3)–Sc(1)–O(4)O(1)–Sc(1)–O(1i)Sc(1)–O(4)57.58(5)O(1)–Sc(1)–O(1i)2.201(2)Sc(1)–O(1)2.252(2)Sc(1)–O(4)2.201(2)Sc(1)–O(3)2.268(1)Sc(1)–O(6)2.105(2)C–O1.417(3)–1.444(3)C–C1.492(3)–1.505(4)O(1)–Sc(1)–O(1i)56.98(7)O(3)–Sc(1)–O(4)57.58(5)O(6)–Sc(1)–O(6i)153.64(9)Table 6 Selected bond lengths (Å) and angles (°) for [Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-402.366(2)Sc(1)–O(2)2.261(2)Sc(1)–O(7)Sc(1)–O(2)Sc(1)–O(6)2.050(2)Sc(1)–O(2)2.101(2)2.128(2)Sc(1)–O(4)2.261(2)Sc(1)–O(7i)Sc(1)–O(4)Sc(1)–O(6)2.064(2)Sc(1)–O(4)2.101(2)2.186(2)Sc(1)–O(5)2.261(2)Sc(1)⋯Sc(1i)Sc(1)–O(5)Sc(1)–O(6)3.296(1)Sc(1)–O(5)2.101(2)1.511(4)C(1)–C(2)2.261(2)C(3)–C(4)C(1)–C(2)Sc(1)–O(6)1.488(4)C(1)–C(2)2.101(2)1.431(3)–1.435(3)C–O2.261(2)NoValueC–OSc(1)–O(6)NoValueC–O2.101(2)55.23(6)O(1)–Sc(1)–O(2)2.261(2)O(7)–Sc(1)–O(7i)O(1)–Sc(1)–O(2)Sc(1)–O(6)73.54(7)O(1)–Sc(1)–O(2)2.101(2)Sc(1)–O(1)2.261(2)Sc(1)–O(6)2.101(2)Sc(1)–O(2)2.366(2)Sc(1)–O(7)2.050(2)Sc(1)–O(4)2.128(2)Sc(1)–O(7i)2.064(2)Sc(1)–O(5)2.186(2)Sc(1)⋯Sc(1i)3.296(1)C(1)–C(2)1.511(4)C(3)–C(4)1.488(4)C–O1.431(3)–1.435(3)O(1)–Sc(1)–O(2)55.23(6)O(7)–Sc(1)–O(7i)73.54(7)Sc(1)–O(7)–Sc(1i)106.46(7)Table 7 Selected bond lengths (Å) and angles (°) for [Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)302.345(2)Sc(1)–O(2)2.346(2)Sc(2)–O(10)Sc(1)–O(2)Sc(2)–O(9)2.033(2)Sc(1)–O(2)2.089(2)2.298(3)Sc(1)–O(4)2.346(2)Sc(2)–O(11)Sc(1)–O(4)Sc(2)–O(9)2.155(3)Sc(1)–O(4)2.089(2)2.337(2)Sc(1)–O(5)2.346(2)Sc(2)–O(12)Sc(1)–O(5)Sc(2)–O(9)2.174(2)Sc(1)–O(5)2.089(2)2.170(2)Sc(1)–O(7)2.346(2)Sc(2)–O(13)Sc(1)–O(7)Sc(2)–O(9)2.352(2)Sc(1)–O(7)2.089(2)2.153(3)Sc(1)–O(8)2.346(2)Sc(2)–O(14)Sc(1)–O(8)Sc(2)–O(9)2.291(2)Sc(1)–O(8)2.089(2)2.039(2)Sc(1)–O(9)2.346(2)Sc(2)–O(16)Sc(1)–O(9)Sc(2)–O(9)2.341(2)Sc(1)–O(9)2.089(2)2.087(2)Sc(1)–O(10)2.346(2)Sc(2)–O(17)Sc(1)–O(10)Sc(2)–O(9)2.355(2)Sc(1)–O(10)2.089(2)3.324(1)Sc(1)⋯Sc(2)2.346(2)NoValueSc(1)⋯Sc(2)Sc(2)–O(9)NoValueSc(1)⋯Sc(2)2.089(2)2.465(3)Na(1)–O(19)2.346(2)Na(1)–O(23)Na(1)–O(19)Sc(2)–O(9)2.499(3)Na(1)–O(19)2.089(2)2.490(3)Na(1)–O(20)2.346(2)Na(1)–O(24)Na(1)–O(20)Sc(2)–O(9)2.449(3)Na(1)–O(20)2.089(2)2.503(3)Na(1)–O(21)2.346(2)Na(1)–O(25)Na(1)–O(21)Sc(2)–O(9)2.449(3)Na(1)–O(21)2.089(2)2.431(3)Na(1)–O(22)2.346(2)Na(1)–O(26)Na(1)–O(22)Sc(2)–O(9)2.475(3)Na(1)–O(22)2.089(2)1.416(4)–1.436(4)C–O2.346(2)C–CC–OSc(2)–O(9)1.502(5)–1.518(5)C–O2.089(2)54.38(9)O(1)–Sc(1)–O(2)2.346(2)O(13)–Sc(2)–O(14)O(1)–Sc(1)–O(2)Sc(2)–O(9)54.89(9)O(1)–Sc(1)–O(2)2.089(2)55.02(9)O(4)–Sc(1)–O(5)2.346(2)O(16)–Sc(2)–O(17)O(4)–Sc(1)–O(5)Sc(2)–O(9)54.28(9)O(4)–Sc(1)–O(5)2.089(2)72.52(9)O(9)–Sc(1)–O(10)2.346(2)O(9)–Sc(2)–O(10)O(9)–Sc(1)–O(10)Sc(2)–O(9)72.61(9)O(9)–Sc(1)–O(10)2.089(2)107.3(1)Sc(1)–O(9)–Sc(2)2.346(2)Sc(1)–O(10)–Sc(2)Sc(1)–O(9)–Sc(2)Sc(2)–O(9)107.6(1)Sc(1)–O(9)–Sc(2)2.089(2)Sc(1)–O(1)2.346(2)Sc(2)–O(9)2.089(2)Sc(1)–O(2)2.345(2)Sc(2)–O(10)2.033(2)Sc(1)–O(4)2.298(3)Sc(2)–O(11)2.155(3)Sc(1)–O(5)2.337(2)Sc(2)–O(12)2.174(2)Sc(1)–O(7)2.170(2)Sc(2)–O(13)2.352(2)Sc(1)–O(8)2.153(3)Sc(2)–O(14)2.291(2)Sc(1)–O(9)2.039(2)Sc(2)–O(16)2.341(2)Sc(1)–O(10)2.087(2)Sc(2)–O(17)2.355(2)Sc(1)⋯Sc(2)3.324(1)Na(1)–O(19)2.465(3)Na(1)–O(23)2.499(3)Na(1)–O(20)2.490(3)Na(1)–O(24)2.449(3)Na(1)–O(21)2.503(3)Na(1)–O(25)2.449(3)Na(1)–O(22)2.431(3)Na(1)–O(26)2.475(3)C–O1.416(4)–1.436(4)C–C1.502(5)–1.518(5)O(1)–Sc(1)–O(2)54.38(9)O(13)–Sc(2)–O(14)54.89(9)O(4)–Sc(1)–O(5)55.02(9)O(16)–Sc(2)–O(17)54.28(9)O(9)–Sc(1)–O(10)72.52(9)O(9)–Sc(2)–O(10)72.61(9)Sc(1)–O(9)–Sc(2)107.3(1)Sc(1)–O(10)–Sc(2)107.6(1)http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/Articleimage/2003/DT/b210458j/b210458j-f1.gifThe structure of the cation in [ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN showing the atom labelling scheme. Displacement ellipsoids are drawn at the 40% probability level and the H atoms are omitted for clarity.http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/Articleimage/2003/DT/b210458j/b210458j-f2.gifThe structure of the cation involving Sc(1) in [ScCl2(18-crown-6][FeCl4] showing the atom labelling scheme. The Sc(2) species is similar, differing in the conformation at C(7) and O(4). Displacement ellipsoids are drawn at the 50% probability level and the H atoms are omitted for clarity.http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/Articleimage/2003/DT/b210458j/b210458j-f3.gifThe structure of [ScCl3(H2O)3]·18-crown-6 (a) shows the Sc(1) group with the atom labelling scheme and the 2-fold symmetry lying along O(4), Sc(1) and Cl(2). Displacement ellipsoids are drawn at the 50% probability level; (b) view down the a direction showing the chain of O–H⋯O bonds between the Sc groups and the crown parallel to the c direction. The H-bonding is indicated by single lines and the H atoms are omitted for clarity.http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/Articleimage/2003/DT/b210458j/b210458j-f4.gifThe structure of [Sc(NO3)2(H2O)4](NO3)·15-crown-5 showing the O–H⋯O H-bonded chain between the Sc cation and the crown (H-bonds as dotted lines) lying parallel to the b direction. A partial atom labelling scheme is shown with O(10)–O(13) being coordinated water molecules. O(17A) (not labelled) is in a disordered part of the crown and is not involved in H-bonding. H atoms are omitted for clarity.http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/Articleimage/2003/DT/b210458j/b210458j-f5.gifThe structure of [Sc(NO3)3(H2O)2]·(12-crown-4)2 (a) shows the Sc(1) group with the atom labelling scheme and the 2-fold symmetry in the c direction passing through Sc(1), N(1) and O(2). Displacement ellipsoids are drawn at the 50% probability level; (b) view down the c direction showing the O–H⋯O bonds (thin lines) between O(6i) of the Sc group and the crown. (Symmetry operation: i = 1/2+x, 1/2−y, −z).http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/Articleimage/2003/DT/b210458j/b210458j-f6.gifThe structure of [Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4 (a) shows the centrosymmetric cation with the atom labelling scheme. Displacement ellipsoids are drawn at the 50% probability level; (b) shows part of the 2-dimensional sheet formed by the O–H⋯O H-bonding (indicated by dotted lines).http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/Articleimage/2003/DT/b210458j/b210458j-f7.gifThe structure of [Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3 showing the scandium dimer with the atom labelling scheme. Displacement ellipsoids are drawn at the 50% probability level and the H atoms are omitted for clarity.[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNScCClNSbsystemAutoTableParserOrthorhombic[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNCrystal systemPbca[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNSpace groupFalse8.0[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN8Z[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNCrystal system4064.0[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN4064F(000)1051.68[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN1051.68M[ScCl2(18-crown-6)][FeCl4]ScClFesystemAutoTableParserOrthorhombic[ScCl2(18-crown-6)][FeCl4]Crystal systemPna21[ScCl2(18-crown-6)][FeCl4]Space groupFalse8.0[ScCl2(18-crown-6)][FeCl4]8Z[ScCl2(18-crown-6)][FeCl4]Crystal system2344.0[ScCl2(18-crown-6)][FeCl4]2344F(000)577.82[ScCl2(18-crown-6)][FeCl4]577.82M[ScCl3(H2O)3]·18-crown-6HOScClsystemAutoTableParserOrthorhombic[ScCl3(H2O)3]·18-crown-6Crystal systemPbcn[ScCl3(H2O)3]·18-crown-6Space groupFalse4.0[ScCl3(H2O)3]·18-crown-64Z[ScCl3(H2O)3]·18-crown-6Crystal system984.0[ScCl3(H2O)3]·18-crown-6984F(000)469.67[ScCl3(H2O)3]·18-crown-6469.67M[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3OScHNNasystemAutoTableParserTriclinic[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3Crystal systemP1̄[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3Space groupFalse2.0[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)32Z[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3Crystal system976.0[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3976F(000)935.5[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3935.50M[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4HOScNsystemAutoTableParserTriclinic[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4Crystal systemP1̄[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4Space groupFalse1.0[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-41Z[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4Crystal system340.0[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4340F(000)656.28[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4656.28M[Sc(NO3)3(H2O)2]·(12-crown-4)2HOScNsystemAutoTableParserOrthorhombic[Sc(NO3)3(H2O)2]·(12-crown-4)2Crystal systemP21212[Sc(NO3)3(H2O)2]·(12-crown-4)2Space groupFalse2.0[Sc(NO3)3(H2O)2]·(12-crown-4)22Z[Sc(NO3)3(H2O)2]·(12-crown-4)2Crystal system652.0[Sc(NO3)3(H2O)2]·(12-crown-4)2652F(000)619.44[Sc(NO3)3(H2O)2]·(12-crown-4)2619.44M[ScCl2(18-crown-6)][FeCl4]ScClFeSpace groupAutoTableParserOrthorhombic[ScCl2(18-crown-6)][FeCl4]Crystal systemPna21[ScCl2(18-crown-6)][FeCl4]Space groupFalse8.0[ScCl2(18-crown-6)][FeCl4]8Z[ScCl2(18-crown-6)][FeCl4]Space group2344.0[ScCl2(18-crown-6)][FeCl4]2344F(000)577.82[ScCl2(18-crown-6)][FeCl4]577.82M[ScCl3(H2O)3]·18-crown-6HOScClSpace groupAutoTableParserOrthorhombic[ScCl3(H2O)3]·18-crown-6Crystal systemPbcn[ScCl3(H2O)3]·18-crown-6Space groupFalse4.0[ScCl3(H2O)3]·18-crown-64Z[ScCl3(H2O)3]·18-crown-6Space group984.0[ScCl3(H2O)3]·18-crown-6984F(000)469.67[ScCl3(H2O)3]·18-crown-6469.67M[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3OScHNNaSpace groupAutoTableParserTriclinic[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3Crystal systemP1̄[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3Space groupFalse2.0[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)32Z[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3Space group976.0[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3976F(000)935.5[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3935.50M[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4HOScNSpace groupAutoTableParserTriclinic[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4Crystal systemP1̄[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4Space groupFalse1.0[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-41Z[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4Space group340.0[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4340F(000)656.28[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4656.28M[Sc(NO3)3(H2O)2]·(12-crown-4)2HOScNSpace groupAutoTableParserOrthorhombic[Sc(NO3)3(H2O)2]·(12-crown-4)2Crystal systemP21212[Sc(NO3)3(H2O)2]·(12-crown-4)2Space groupFalse2.0[Sc(NO3)3(H2O)2]·(12-crown-4)22Z[Sc(NO3)3(H2O)2]·(12-crown-4)2Space group652.0[Sc(NO3)3(H2O)2]·(12-crown-4)2652F(000)619.44[Sc(NO3)3(H2O)2]·(12-crown-4)2619.44M[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNScCClNSbSpace groupAutoTableParserOrthorhombic[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNCrystal systemPbca[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNSpace groupFalse8.0[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN8Z[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNSpace group4064.0[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN4064F(000)1051.68[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCN1051.68M10.1039/b210458j12-crown-412-crown-4ScCl2(18-crown-6)][FeCl4crown ether–Ti15-crown-5[ScCl4(MeCN)2]−ScCl3(H2O)3Othioether-scandium(III)crown etherSc(NO3)3·5H2OC12H30N3O18Sc1HLewis acidhydrogenethersd6-acetoneP4O10[ScCl3(H2O)3]·18-crown-6O(4)H2Oligands[ScCl(15-crown-5)(MeCN)][SbCl6]2O(N)FeCl318-crown-61Hhydrogenlanthanidescandium[Sc(12-crown-4)2][SbCl6][Sb2Cl8(MeCN)2]·2MeCNO[Sc(H2O)2(NO3)3]·15-crown-5[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-412-crown-4O–Hcrown[Sc2(OH)2(H2O)6(NO3)2](NO3)2·12-crown-4HHH2Onitrogenscandium[Sc(H2O)2(NO3)3]·(12-crown-4)2MeCNchlorideOCl−crown OMeCNO(4)MeCNScCl3·6H2OScCl3(thf)3ClcrownScCl3(H2O)3MeCN[ScCl3(H2O)3]2·12-crown-4ScCl3·6H2OMe2CO3222br, 1631m, 1300m, 1262w, 1140m, 1101mchlorideNa+NaOHcrowncrown15-crown-5HScCl3·6H2Oscandiumν2(NO3)[15]aneS2O3crown etherscandium[ScCl2(12-crown-4)]+chlorines[ScCl2(18-crown-6)]SbCl6O–Hcrown1H[CuCl4]2−oxygencrownSbCl5SbCl5ScCl2(18-crown-6][FeCl4ScCl2(18-crown-6)][FeCl4C10H32Cl6O11Sc2ethersethers[ScCl3(H2O)3]·18-crown-6scandiumscandium nitrateethanolOHScCl3-R3POethanold6-acetone[ScCl(18-crown-6)]2+1Hhydrogenscandium chloride/crown etherOethanolMe2COMeCNcrownClHMeCN[ScCl(15-crown-5)(MeCN)][SbCl6]2·MeCNether oxygensd6-acetone12-crown-4thia-oxa-crown 1,4-dithia-7,10,13-trioxacyclopentadecanetransition metals15-crown-5crownHSbCl5Sc(NO3)3·5H2Oscandium chlorideMeCN[Sc(H2O)4(NO3)2]NO3·15-crown-5[ScCl2(18-crown-6)]FeCl4O(N)nitratescandium12-crown-4MeCN15-crown-5ethanolscandiumSc(NO3)3(OPPh3)2d6-acetone[ScCl2(15-crown-5)]+nitratecrownoxygennitrateSc(NO3)3·5H2OScCl3(thf)3Sc(NO3)3·5H2OH12-crown-4)·[Sc(NO3)3(H2O)2]·(12-crown-4d(Sc–O)MeCN18-crown-6O(11)crownHd3-MeCNsodiumHC10H28N3O18ScNaOHethersOMeCN[ScCl2(18-crown-6)]FeCl4crowncrown[ScCl2(18-crown-6)]SbCl6MeCN1H15-crown-5HHethers15-crown-512-crown-4EtOHscandium nitrateScCl2O5’scandiumscandium[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3[ScCl4(MeCN)2]−O–HEtOH[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4ethanol[Sc(NO3)3(H2O)2]·(12-crown-4)212-crown-4Sc(NO3)3·5H2OScCl3(thf)3[ScCl3(H2O)3]2·15-crown-5crownScCl3(thf)3scandium-aquo-hydroxo-nitrato[ScCl3(H2O)3]2·15-crown-5[ScCl2([15]aneS2O3)]FeCl4[Sc(H2O)2(NO3)3]·(12-crown-4)2scandiumHHscandium nitrate18-crown-6SbCl5CH2Ohydrogenhydroxy[Sc(H2O)4(NO3)2]NO3·15-crown-5scandium18-crown-618-crown-6ScCl3(thf)3crownH18-crown-6crownscandiumSc(1)crown ethersScCl2([15]aneS2O3)][FeCl4scandiumscandiumscandiumNO3ligandO(17A)ethanolMo[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNSbCl31Hethanolbidentate nitrate1H[Sc(12-crown-4)2]3+ScCl2(18-crown-6)][FeCl415-crown-5FeCl3nitrateHSbCl5[Sc(12-crown-4)2]3+FeCl3[ScCl3(H2O)3]·18-crown-6hydrated scandium nitrate7-coordinate trans pentagonal bipyramidal scandiumScCl3·6H2OO–H[Sc(NO3)3(H2O)2]·(12-crown-4)2HHNC12H30Cl3O9ScO–HHNO3ligandsO(13)ethersO–H12-crown-412-crown-412-crown-412-crown-4thia-oxa-crown [15]aneS2O3oxygenScCl3(thf)3MeCN1H12-crown-4ethanolHnitrogen[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNnitrogencrown etherd6-acetone[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNN(1)Sc(III)CH2SSc–ClScCl3(thf)3MeCNLiClScCl2(18-crown-6)][FeCl4H[ScCl(15-crown-5)(MeCN)]2+scandium-aquo-nitratoOcrownethanolscandium chloride-crownscandiumMeCN[Sc(18-crown-6)]3+EtOHScCl4(MeCN)2O H[Sc(12-crown-4)2]3+cationC12H36Cl6O12Sc2[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4chloride[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3nitrate1HcrownMeCNC10H28N3O18ScethanolTiCl4(18-crown-6)Ocrown1Hcrownscandium nitrateHSc(1)Sc3+18-crown-6[ScCl2(18-crown-6)]SbCl6ethersO(4)MeCNMeCNpentagonal bipyramidalcrownNO3ligandsO(N)ScCl3(thf)3nitrateH[ScCl2(15-crown-5)]+SbCl518-crown-6chlorideOOethanolLewis acidMeCNSbCl5crown ether oxygen18-crown-6hydrogenFeCl3HScCl2(15-crown-5)][SbCl6crown etherHcrown ether9-coordinate lanthanideHydrogend3-MeCNcrown etherH[SbCl6]−HHnitrogen[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4H2OCD2Cl2hydrogen[15]aneS2O3mer-[ScCl3(H2O)3]·18-crown-6DPX400MeCN[ScCl3(H2O)3]·18-crown-6nitrogenOroutine.Methylene hydrogenScCl3(thf)3Sc(1)ethersScCl3·6H2O[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3nitratecrown etherscrownFeCl3scandium nitrateethanolScCl2(18-crown-6)][FeCl4crownHhydrate[ScCl3(H2O)3]2·18-crown-6Sc3+[Sc(H2O)2(NO3)3]·(12-crown-4)2crown OOMeCNSc(NO3)3(H2O)2ScCl3(thf)31HscandiumH1HSc(1)scandium chloridecrownbidentate nitrateO HethanolSc(NO3)3·5H2OethanolC12H24Cl6FeO6ScMeCNMe2COMeCNhydrogen[Sc(NO3)2(H2O)4](NO3)·15-crown-5[Sc(NO3)2(H2O)4](NO3)·15-crown-5[Sc(NO)3(H2O)2]·(12-crown-4)2[Sc(H2O)3(NO3)3]·18-crown-6scandium[ScCl(15-crown-5)(MeCN)][SbCl6]2·MeCNHethanolSbCl5OHSc2(NO3)4(H2O)4(OH)2FeCl3ScCl3(thf)3H[Sb(18-crown-6·SbCl5)(MeCN)x]3+Na/benzophenoneFeCl3crown ether[ScCl3(H2O)3]2·18-crown-6H[ScCl3(thf)3]/18-crown-6/SbCl5/MeCNScandium(III)[Sc2(H2O)6(OH)2(NO3)2](NO3)2·12-crown-4ScCl3(MeCN)3ScCl3·6H2OScCl3/18-crown-6TiCl4(18-crown-6)15-crown-5chlorideScCl3·6H2O12-crown-4Sc(NO3)3·5H2O[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3ScCl2([15]aneS2O3)][FeCl4[Sc(H2O)6]3+scandiumH1Hcrown[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3Hcrown etherO⋯O[Sc(12-crown-4)2][SbCl6]2[Sc(H2O)3(NO3)3]·18-crown-6HHd(O⋯O)O15-crown-5[Sc(H2O)4(NO3)2]NO3·15-crown-5SbCl5nitratecrowncrown[Sc(H2O)2(NO3)3]·(12-crown-4)2scandiumdichloroscandium(III)OHEtOH1H15-crown-5dihydroxy-bridged Sc dimerH2O15-crown-518-crown-6scandiumO(2)[ScCl2(12-crown-4)(MeCN)]SbCl6MeCNthioetherSbCl5OCl(2)graphite12-crown-4HMeCNFeCl3H[ScCl(MeCN)(15-crown-5)][SbCl6]2·MeCNHHH18-crown-6ScCl3·6H2OScCl3(MeCN)3[ScCl(15-crown-5)(MeCN)][SbCl6]2OH(O)crownSbCl5crowncrownscandiumscandiumHbidentate NO3scandium[ScCl3(H2O)3]·18-crown-6OH18-crown-6[ScCl3(H2O)3]·18-crown-6ethanolMeCN[ScCl3(H2O)3]n·(crown)etherslanthanidescandium(III)μ-OOHd6-acetonecrown ether[ScCl2(12-crown-4)(MeCN)]SbCl6crown etherscandiumcrownethanolHSc–OMeCNHMeCNHNaScCl3(H2O)3oxygensethanol18-crown-6Lewis acidsScCl3(thf)3[ScCl3(H2O)3]·18-crown-6C8H28Cl6O10Sc2ethanold6-acetoneSbCl5d6-acetoneScCl3scandium[Sc2(NO3)4(H2O)4(OH)2][Na(12-crown-4)2](NO3)·(H2O)3ClcrownHH18-crown-6[Sc(H2O)4(NO3)2]NO3·15-crown-5scandiumetherspentagonal bipyramidalHHHSc(NO3)3·5H2O(18-crown-6)Cl3Ti–O–TiCl3(18-crown-6)[Sc2(NO3)2(H2O)6(OH)2](NO3)2·12-crown-4MeCNScCl3·6H2OnitrateO HscandiumSbCl51HSbCl5ScCl3(thf)3[Sc2(NO3)4(H2O)4(OH)2]·[Na(12-crown-4)2]NO3·(H2O)3FeCl3[Sc(NO3)3(H2O)3]·18-crown-612-crown-418-crown-6Na+[Sc(NO3)2(H2O)4](NO3)·(C10H20O5)thioetherethanolScCl3(H2O)3O–Sc–OMeCNethanol1HScCl3(thf)3CD2Cl2HMeCN1H[ScCl3(H2O)3]2·12-crown-4[ScCl2(15-crown-5)]+scandiumcrown50Michael D. BrownWilliam LevasonDavid C. MurrayMichael C. PophamGillian ReidMichael WebsterMichael D. BrownWilliam LevasonDavid C. MurrayMichael C. PophamGillian ReidMichael WebsterDalton Transactionshttp://pubs.rsc.org/en/Content/ArticlePDF/2003/DT/B210458Jhttp://pubs.rsc.org/en/Content/ArticleLanding/2003/DT/B210458J865857Royal Society of Chemistry1916monochromatorNN(-LRB-TableNNTablemonochromator2218NMRNNresonanceNN(-LRB-δNNδNMR resonance4845[Sc(NO3)3(OPPh3)2]NN(-LRB-δNNδ[Sc(NO3)3(OPPh3)2]2219°NN(-LRB-TableNNTable°2521-HYPHcoordinateNN(-LRB-TableNNTable- coordinate2003-02-2418-crown-6crown15-crown-5crown0.11 ) 2868 unique reflections ( 1726 withRint