Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 Table 1. Crystal data and structure refinement for shelxs1419. Identification code shelxs1419 Empirical formula C8 H14 Li N O Si Formula weight 175.23 Temperature 293(2) K Wavelength 0.71073 A Crystal system orthorhombic Space group Pbca Unit cell dimensions a = 20.838(4) A alpha = 90 deg. b = 15.254(3) A beta = 90 deg. c = 26.986(5) A gamma = 90 deg. Volume 8578(3) A^3 Z 32 Density (calculated) 1.086 Mg/m^3 Absorption coefficient 0.174 mm^-1 F(000) 3008 Crystal size .5 x .5 x .5 mm Theta range for data collection 1.80 to 24.11 deg. Index ranges -23<=h<=23, -16<=k<=15, -30<=l<=30 Reflections collected 50537 Independent reflections 6446 [R(int) = 0.0622] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 6446 / 0 / 445 Goodness-of-fit on F^2 0.945 Final R indices [I>2sigma(I)] R1 = 0.0430, wR2 = 0.1010 R indices (all data) R1 = 0.0673, wR2 = 0.1159 Largest diff. peak and hole 0.230 and -0.173 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for shelxs1419. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Si(1) 2476(1) 4747(1) 2815(1) 46(1) Si(2) 4629(1) 2643(1) 2130(1) 52(1) Si(3) 4647(1) 3755(1) 3971(1) 52(1) Si(4) 1906(1) 3274(1) 4496(1) 46(1) N(1) 2901(1) 3791(1) 2887(1) 36(1) N(2) 4352(1) 3553(1) 2424(1) 44(1) N(3) 3915(1) 3283(1) 3835(1) 42(1) N(4) 2517(1) 3915(1) 4290(1) 41(1) O(1) 2858(1) 3057(1) 1918(1) 55(1) O(2) 3826(1) 4829(1) 1791(1) 62(1) O(3) 3665(1) 2397(1) 4743(1) 56(1) O(4) 3359(1) 4445(2) 5047(1) 69(1) C(11) 2396(1) 2795(2) 2255(1) 41(1) C(12) 1910(1) 2439(2) 2005(1) 60(1) C(13) 2058(1) 2483(2) 1491(1) 66(1) C(14) 2623(1) 2858(2) 1454(1) 62(1) C(15) 2553(1) 2964(2) 2787(1) 44(1) C(21) 4482(1) 4836(2) 1868(1) 52(1) C(22) 4758(2) 5266(2) 1496(1) 71(1) C(23) 4262(2) 5549(2) 1169(1) 78(1) C(24) 3713(2) 5273(2) 1355(1) 72(1) C(25) 4692(1) 4377(2) 2328(1) 58(1) C(31) 3971(1) 1937(2) 4370(1) 46(1) C(32) 4283(2) 1270(2) 4573(1) 67(1) C(33) 4183(2) 1301(2) 5093(1) 73(1) C(34) 3816(2) 1981(2) 5179(1) 66(1) C(35) 3887(1) 2316(2) 3861(1) 51(1) C(41) 2812(1) 4937(2) 4966(1) 55(1) C(42) 2676(2) 5378(2) 5378(1) 77(1) C(43) 3152(2) 5166(3) 5737(1) 93(1) C(44) 3550(2) 4600(3) 5530(1) 88(1) C(45) 2528(1) 4825(2) 4464(1) 54(1) C(16) 1728(1) 4817(2) 3195(1) 76(1) C(17) 2209(2) 4979(2) 2163(1) 66(1) C(18) 3041(2) 5628(2) 3010(1) 74(1) C(26) 5511(2) 2475(4) 2175(2) 133(2) C(27) 4452(2) 2602(3) 1451(1) 83(1) C(28) 4224(2) 1674(3) 2415(2) 112(1) C(36) 4914(2) 3673(2) 4633(1) 77(1) C(37) 5317(1) 3293(3) 3594(1) 92(1) C(38) 4565(2) 4937(2) 3838(1) 89(1) C(46) 1924(2) 2221(2) 4150(1) 85(1) C(47) 1961(2) 2985(2) 5171(1) 79(1) C(48) 1086(1) 3771(3) 4427(2) 91(1) Li(1) 3461(2) 3861(3) 2232(1) 47(1) Li(2) 3871(2) 3511(3) 3058(1) 47(1) Li(3) 2980(2) 3730(3) 3662(1) 47(1) Li(4) 3395(2) 3546(3) 4500(1) 49(1) ________________________________________________________________ Table 3. Selected bond lengths [A] and angles [deg] for shelxs1419. _____________________________________________________________ _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 4. Bond lengths [A] and angles [deg] for shelxs1419. _____________________________________________________________ Si(1)-N(1) 1.718(2) Si(1)-C(18) 1.862(3) Si(1)-C(16) 1.868(3) Si(1)-C(17) 1.879(2) Si(1)-Li(1) 2.919(4) Si(1)-Li(3) 2.954(4) Si(2)-N(2) 1.699(2) Si(2)-C(26) 1.860(3) Si(2)-C(28) 1.867(4) Si(2)-C(27) 1.870(3) Si(2)-Li(1) 3.073(4) Si(3)-N(3) 1.725(2) Si(3)-C(38) 1.846(4) Si(3)-C(37) 1.865(3) Si(3)-C(36) 1.876(3) Si(3)-Li(2) 2.971(4) Si(3)-Li(4) 2.991(4) Si(4)-N(4) 1.699(2) Si(4)-C(46) 1.859(3) Si(4)-C(47) 1.877(3) Si(4)-C(48) 1.877(3) Si(4)-Li(4) 3.130(4) N(1)-C(15) 1.480(3) N(1)-Li(3) 2.098(4) N(1)-Li(2) 2.115(4) N(1)-Li(1) 2.122(4) N(2)-C(25) 1.467(3) N(2)-Li(2) 1.982(4) N(2)-Li(1) 1.983(4) N(3)-C(35) 1.479(3) N(3)-Li(3) 2.118(4) N(3)-Li(2) 2.128(4) N(3)-Li(4) 2.135(4) N(4)-C(45) 1.466(3) N(4)-Li(3) 1.970(4) N(4)-Li(4) 1.995(4) O(1)-C(14) 1.380(3) O(1)-C(11) 1.382(3) O(1)-Li(1) 1.950(4) O(2)-C(24) 1.378(3) O(2)-C(21) 1.381(3) O(2)-Li(1) 2.042(4) O(3)-C(34) 1.374(3) O(3)-C(31) 1.382(3) O(3)-Li(4) 1.955(5) O(4)-C(41) 1.382(3) O(4)-C(44) 1.383(3) O(4)-Li(4) 2.015(4) C(11)-C(12) 1.334(3) C(11)-C(15) 1.493(3) C(11)-Li(1) 2.752(5) C(12)-C(13) 1.422(4) C(13)-C(14) 1.313(4) C(15)-Li(1) 2.774(4) C(15)-Li(3) 2.780(4) C(21)-C(22) 1.329(4) C(21)-C(25) 1.491(4) C(21)-Li(1) 2.774(5) C(22)-C(23) 1.426(4) C(23)-C(24) 1.320(4) C(25)-Li(1) 2.695(5) C(31)-C(32) 1.327(4) C(31)-C(35) 1.499(3) C(31)-Li(4) 2.755(5) C(32)-C(33) 1.418(4) C(33)-C(34) 1.310(4) C(35)-Li(4) 2.748(5) C(41)-C(42) 1.329(4) C(41)-C(45) 1.490(3) C(41)-Li(4) 2.749(5) C(42)-C(43) 1.424(5) C(43)-C(44) 1.320(5) C(45)-Li(4) 2.660(5) Li(1)-Li(2) 2.446(5) Li(2)-Li(3) 2.493(5) Li(3)-Li(4) 2.438(5) N(1)-Si(1)-C(18) 104.72(12) N(1)-Si(1)-C(16) 114.69(12) C(18)-Si(1)-C(16) 109.35(16) N(1)-Si(1)-C(17) 114.75(11) C(18)-Si(1)-C(17) 108.33(15) C(16)-Si(1)-C(17) 104.85(13) N(1)-Si(1)-Li(1) 45.98(10) C(18)-Si(1)-Li(1) 92.35(13) C(16)-Si(1)-Li(1) 155.43(15) C(17)-Si(1)-Li(1) 77.87(12) N(1)-Si(1)-Li(3) 44.21(9) C(18)-Si(1)-Li(3) 86.33(13) C(16)-Si(1)-Li(3) 84.44(12) C(17)-Si(1)-Li(3) 158.17(13) Li(1)-Si(1)-Li(3) 85.64(11) N(2)-Si(2)-C(26) 114.72(16) N(2)-Si(2)-C(28) 107.53(14) C(26)-Si(2)-C(28) 108.0(2) N(2)-Si(2)-C(27) 114.71(13) C(26)-Si(2)-C(27) 104.66(18) C(28)-Si(2)-C(27) 106.75(19) N(2)-Si(2)-Li(1) 36.47(10) C(26)-Si(2)-Li(1) 149.31(18) C(28)-Si(2)-Li(1) 94.88(16) C(27)-Si(2)-Li(1) 87.26(12) N(3)-Si(3)-C(38) 106.53(13) N(3)-Si(3)-C(37) 112.87(13) C(38)-Si(3)-C(37) 109.37(19) N(3)-Si(3)-C(36) 115.90(12) C(38)-Si(3)-C(36) 106.11(16) C(37)-Si(3)-C(36) 105.78(16) N(3)-Si(3)-Li(2) 44.80(10) C(38)-Si(3)-Li(2) 84.88(14) C(37)-Si(3)-Li(2) 84.76(13) C(36)-Si(3)-Li(2) 160.61(13) N(3)-Si(3)-Li(4) 44.46(10) C(38)-Si(3)-Li(4) 96.68(15) C(37)-Si(3)-Li(4) 150.82(16) C(36)-Si(3)-Li(4) 78.27(12) Li(2)-Si(3)-Li(4) 84.71(11) N(4)-Si(4)-C(46) 108.46(13) N(4)-Si(4)-C(47) 114.04(13) C(46)-Si(4)-C(47) 106.48(16) N(4)-Si(4)-C(48) 114.64(13) C(46)-Si(4)-C(48) 108.49(18) C(47)-Si(4)-C(48) 104.32(17) N(4)-Si(4)-Li(4) 35.09(10) C(46)-Si(4)-Li(4) 95.52(14) C(47)-Si(4)-Li(4) 88.14(13) C(48)-Si(4)-Li(4) 148.01(14) C(15)-N(1)-Si(1) 116.73(15) C(15)-N(1)-Li(3) 100.56(17) Si(1)-N(1)-Li(3) 100.98(14) C(15)-N(1)-Li(2) 109.59(18) Si(1)-N(1)-Li(2) 133.57(16) Li(3)-N(1)-Li(2) 72.57(15) C(15)-N(1)-Li(1) 99.18(17) Si(1)-N(1)-Li(1) 98.42(14) Li(3)-N(1)-Li(1) 142.17(17) Li(2)-N(1)-Li(1) 70.50(15) C(25)-N(2)-Si(2) 116.94(16) C(25)-N(2)-Li(2) 115.1(2) Si(2)-N(2)-Li(2) 123.20(17) C(25)-N(2)-Li(1) 101.69(19) Si(2)-N(2)-Li(1) 112.92(16) Li(2)-N(2)-Li(1) 76.15(17) C(35)-N(3)-Si(3) 116.19(16) C(35)-N(3)-Li(3) 107.16(19) Si(3)-N(3)-Li(3) 136.58(17) C(35)-N(3)-Li(2) 101.99(17) Si(3)-N(3)-Li(2) 100.38(14) Li(3)-N(3)-Li(2) 71.91(15) C(35)-N(3)-Li(4) 97.32(18) Si(3)-N(3)-Li(4) 101.07(14) Li(3)-N(3)-Li(4) 69.96(15) Li(2)-N(3)-Li(4) 140.86(18) C(45)-N(4)-Si(4) 116.77(15) C(45)-N(4)-Li(3) 113.80(19) Si(4)-N(4)-Li(3) 124.54(16) C(45)-N(4)-Li(4) 99.31(19) Si(4)-N(4)-Li(4) 115.60(16) Li(3)-N(4)-Li(4) 75.87(17) C(14)-O(1)-C(11) 106.68(19) C(14)-O(1)-Li(1) 139.6(2) C(11)-O(1)-Li(1) 110.19(17) C(24)-O(2)-C(21) 107.1(2) C(24)-O(2)-Li(1) 142.1(2) C(21)-O(2)-Li(1) 106.66(18) C(34)-O(3)-C(31) 106.5(2) C(34)-O(3)-Li(4) 140.1(2) C(31)-O(3)-Li(4) 110.13(18) C(41)-O(4)-C(44) 106.9(2) C(41)-O(4)-Li(4) 106.56(18) C(44)-O(4)-Li(4) 142.7(2) C(12)-C(11)-O(1) 108.21(19) C(12)-C(11)-C(15) 136.3(2) O(1)-C(11)-C(15) 115.44(19) C(12)-C(11)-Li(1) 147.30(19) O(1)-C(11)-Li(1) 41.68(13) C(15)-C(11)-Li(1) 75.16(15) C(11)-C(12)-C(13) 108.1(2) C(14)-C(13)-C(12) 106.8(2) C(13)-C(14)-O(1) 110.2(2) N(1)-C(15)-C(11) 115.48(18) N(1)-C(15)-Li(1) 49.04(13) C(11)-C(15)-Li(1) 73.49(15) N(1)-C(15)-Li(3) 47.88(12) C(11)-C(15)-Li(3) 163.32(19) Li(1)-C(15)-Li(3) 91.89(14) C(22)-C(21)-O(2) 108.6(2) C(22)-C(21)-C(25) 137.1(3) O(2)-C(21)-C(25) 114.3(2) C(22)-C(21)-Li(1) 149.7(2) O(2)-C(21)-Li(1) 44.85(13) C(25)-C(21)-Li(1) 71.28(16) C(21)-C(22)-C(23) 107.7(3) C(24)-C(23)-C(22) 107.2(3) C(23)-C(24)-O(2) 109.5(3) N(2)-C(25)-C(21) 114.0(2) N(2)-C(25)-Li(1) 46.11(14) C(21)-C(25)-Li(1) 77.11(16) C(32)-C(31)-O(3) 108.2(2) C(32)-C(31)-C(35) 137.1(2) O(3)-C(31)-C(35) 114.7(2) C(32)-C(31)-Li(4) 147.5(2) O(3)-C(31)-Li(4) 41.77(13) C(35)-C(31)-Li(4) 73.90(16) C(31)-C(32)-C(33) 108.2(3) C(34)-C(33)-C(32) 106.7(3) C(33)-C(34)-O(3) 110.3(2) N(3)-C(35)-C(31) 115.0(2) N(3)-C(35)-Li(4) 50.41(14) C(31)-C(35)-Li(4) 74.48(16) C(42)-C(41)-O(4) 108.7(3) C(42)-C(41)-C(45) 137.2(3) O(4)-C(41)-C(45) 114.1(2) C(42)-C(41)-Li(4) 150.2(3) O(4)-C(41)-Li(4) 44.64(13) C(45)-C(41)-Li(4) 70.75(16) C(41)-C(42)-C(43) 107.7(3) C(44)-C(43)-C(42) 107.3(3) C(43)-C(44)-O(4) 109.3(3) N(4)-C(45)-C(41) 114.0(2) N(4)-C(45)-Li(4) 47.75(14) C(41)-C(45)-Li(4) 77.33(17) O(1)-Li(1)-N(2) 124.6(2) O(1)-Li(1)-O(2) 116.25(19) N(2)-Li(1)-O(2) 88.59(17) O(1)-Li(1)-N(1) 88.58(17) N(2)-Li(1)-N(1) 106.50(18) O(2)-Li(1)-N(1) 136.6(2) O(1)-Li(1)-Li(2) 118.9(2) N(2)-Li(1)-Li(2) 51.91(13) O(2)-Li(1)-Li(2) 124.0(2) N(1)-Li(1)-Li(2) 54.62(13) O(1)-Li(1)-C(25) 147.1(2) N(2)-Li(1)-C(25) 32.20(11) O(2)-Li(1)-C(25) 59.39(12) N(1)-Li(1)-C(25) 117.23(17) Li(2)-Li(1)-C(25) 69.15(14) O(1)-Li(1)-C(11) 28.13(8) N(2)-Li(1)-C(11) 127.4(2) O(2)-Li(1)-C(11) 137.80(18) N(1)-Li(1)-C(11) 60.49(12) Li(2)-Li(1)-C(11) 97.52(16) C(25)-Li(1)-C(11) 159.65(19) O(1)-Li(1)-C(21) 132.68(18) N(2)-Li(1)-C(21) 60.19(13) O(2)-Li(1)-C(21) 28.49(9) N(1)-Li(1)-C(21) 138.1(2) Li(2)-Li(1)-C(21) 99.93(17) C(25)-Li(1)-C(21) 31.61(9) C(11)-Li(1)-C(21) 160.55(17) O(1)-Li(1)-C(15) 58.93(12) N(2)-Li(1)-C(15) 112.29(18) O(2)-Li(1)-C(15) 157.7(2) N(1)-Li(1)-C(15) 31.78(9) Li(2)-Li(1)-C(15) 68.77(14) C(25)-Li(1)-C(15) 137.80(16) C(11)-Li(1)-C(15) 31.35(8) C(21)-Li(1)-C(15) 168.03(17) O(1)-Li(1)-Si(1) 94.09(15) N(2)-Li(1)-Si(1) 128.80(18) O(2)-Li(1)-Si(1) 104.01(18) N(1)-Li(1)-Si(1) 35.60(8) Li(2)-Li(1)-Si(1) 81.66(14) C(25)-Li(1)-Si(1) 118.85(16) C(11)-Li(1)-Si(1) 72.16(10) C(21)-Li(1)-Si(1) 118.84(17) C(15)-Li(1)-Si(1) 57.13(9) O(1)-Li(1)-Si(2) 95.24(17) N(2)-Li(1)-Si(2) 30.61(9) O(2)-Li(1)-Si(2) 95.17(14) N(1)-Li(1)-Si(2) 118.60(16) Li(2)-Li(1)-Si(2) 70.89(14) C(25)-Li(1)-Si(2) 55.38(10) C(11)-Li(1)-Si(2) 106.44(15) C(21)-Li(1)-Si(2) 71.69(11) C(15)-Li(1)-Si(2) 106.82(14) Si(1)-Li(1)-Si(2) 152.20(14) N(2)-Li(2)-N(1) 106.79(18) N(2)-Li(2)-N(3) 146.4(2) N(1)-Li(2)-N(3) 106.78(17) N(2)-Li(2)-Li(1) 51.94(13) N(1)-Li(2)-Li(1) 54.88(13) N(3)-Li(2)-Li(1) 161.6(2) N(2)-Li(2)-Li(3) 159.4(2) N(1)-Li(2)-Li(3) 53.39(13) N(3)-Li(2)-Li(3) 53.84(13) Li(1)-Li(2)-Li(3) 107.85(19) N(2)-Li(2)-Si(3) 115.85(17) N(1)-Li(2)-Si(3) 132.42(17) N(3)-Li(2)-Si(3) 34.82(8) Li(1)-Li(2)-Si(3) 156.7(2) Li(3)-Li(2)-Si(3) 81.15(13) N(4)-Li(3)-N(1) 144.3(2) N(4)-Li(3)-N(3) 107.83(18) N(1)-Li(3)-N(3) 107.82(18) N(4)-Li(3)-Li(4) 52.52(14) N(1)-Li(3)-Li(4) 163.1(2) N(3)-Li(3)-Li(4) 55.35(14) N(4)-Li(3)-Li(2) 161.1(2) N(1)-Li(3)-Li(2) 54.04(13) N(3)-Li(3)-Li(2) 54.25(13) Li(4)-Li(3)-Li(2) 109.1(2) N(4)-Li(3)-C(15) 129.4(2) N(1)-Li(3)-C(15) 31.56(9) N(3)-Li(3)-C(15) 110.28(17) Li(4)-Li(3)-C(15) 148.5(2) Li(2)-Li(3)-C(15) 68.06(14) N(4)-Li(3)-Si(1) 114.59(18) N(1)-Li(3)-Si(1) 34.82(8) N(3)-Li(3)-Si(1) 131.86(17) Li(4)-Li(3)-Si(1) 154.7(2) Li(2)-Li(3)-Si(1) 80.20(13) C(15)-Li(3)-Si(1) 56.67(9) O(3)-Li(4)-N(4) 127.7(2) O(3)-Li(4)-O(4) 112.1(2) N(4)-Li(4)-O(4) 89.03(18) O(3)-Li(4)-N(3) 88.07(17) N(4)-Li(4)-N(3) 106.25(18) O(4)-Li(4)-N(3) 139.6(2) O(3)-Li(4)-Li(3) 121.1(2) N(4)-Li(4)-Li(3) 51.60(14) O(4)-Li(4)-Li(3) 126.0(2) N(3)-Li(4)-Li(3) 54.69(13) O(3)-Li(4)-C(45) 150.0(2) N(4)-Li(4)-C(45) 32.94(10) O(4)-Li(4)-C(45) 60.21(13) N(3)-Li(4)-C(45) 116.88(18) Li(3)-Li(4)-C(45) 68.95(15) O(3)-Li(4)-C(35) 59.31(12) N(4)-Li(4)-C(35) 110.87(18) O(4)-Li(4)-C(35) 159.7(2) N(3)-Li(4)-C(35) 32.27(10) Li(3)-Li(4)-C(35) 68.20(14) C(45)-Li(4)-C(35) 137.01(17) O(3)-Li(4)-C(41) 131.78(19) N(4)-Li(4)-C(41) 60.55(13) O(4)-Li(4)-C(41) 28.80(10) N(3)-Li(4)-C(41) 139.0(2) Li(3)-Li(4)-C(41) 100.35(18) C(45)-Li(4)-C(41) 31.93(9) C(35)-Li(4)-C(41) 168.35(18) O(3)-Li(4)-C(31) 28.10(9) N(4)-Li(4)-C(31) 127.9(2) O(4)-Li(4)-C(31) 135.68(19) N(3)-Li(4)-C(31) 60.25(12) Li(3)-Li(4)-C(31) 97.96(17) C(45)-Li(4)-C(31) 160.82(19) C(35)-Li(4)-C(31) 31.62(8) C(41)-Li(4)-C(31) 159.78(18) O(3)-Li(4)-Si(3) 90.22(15) N(4)-Li(4)-Si(3) 129.33(18) O(4)-Li(4)-Si(3) 107.99(18) N(3)-Li(4)-Si(3) 34.46(8) Li(3)-Li(4)-Si(3) 81.62(14) C(45)-Li(4)-Si(3) 119.80(16) C(35)-Li(4)-Si(3) 56.45(9) C(41)-Li(4)-Si(3) 121.43(17) C(31)-Li(4)-Si(3) 69.73(11) O(3)-Li(4)-Si(4) 99.66(17) N(4)-Li(4)-Si(4) 29.31(9) O(4)-Li(4)-Si(4) 93.22(15) N(3)-Li(4)-Si(4) 118.44(16) Li(3)-Li(4)-Si(4) 70.18(14) C(45)-Li(4)-Si(4) 54.82(10) C(35)-Li(4)-Si(4) 106.12(15) C(41)-Li(4)-Si(4) 70.50(11) C(31)-Li(4)-Si(4) 108.28(15) Si(3)-Li(4)-Si(4) 151.31(14) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 5. Anisotropic displacement parameters (A^2 x 10^3) for shelxs1419. The anisotropic displacement factor exponent takes the form: -2 pi^2 [ h^2 a*^2 U11 + ... + 2 h k a* b* U12 ] _______________________________________________________________________ U11 U22 U33 U23 U13 U12 _______________________________________________________________________ Si(1) 52(1) 50(1) 36(1) 5(1) 1(1) 12(1) Si(2) 46(1) 69(1) 42(1) 1(1) 0(1) 10(1) Si(3) 46(1) 68(1) 42(1) 1(1) -5(1) -3(1) Si(4) 54(1) 47(1) 38(1) 0(1) 5(1) 2(1) N(1) 39(1) 39(1) 31(1) 1(1) 0(1) 0(1) N(2) 38(1) 58(2) 37(1) 6(1) 3(1) -4(1) N(3) 42(1) 51(2) 32(1) 1(1) -2(1) 3(1) N(4) 48(1) 43(1) 33(1) -3(1) 4(1) 6(1) O(1) 46(1) 87(2) 31(1) -3(1) 2(1) -10(1) O(2) 51(1) 74(2) 60(1) 24(1) 4(1) -2(1) O(3) 66(1) 69(1) 34(1) 5(1) 3(1) 14(1) O(4) 69(1) 89(2) 50(1) -29(1) -9(1) 10(1) C(11) 43(1) 45(2) 35(1) 0(1) 2(1) 0(1) C(12) 48(2) 84(2) 48(2) -7(1) 0(1) -12(1) C(13) 59(2) 95(3) 43(1) -17(1) -10(1) -2(2) C(14) 59(2) 97(2) 30(1) -11(1) 1(1) 5(2) C(15) 49(1) 47(2) 35(1) 2(1) 1(1) -4(1) C(21) 50(2) 53(2) 53(2) 3(1) 7(1) -10(1) C(22) 64(2) 80(2) 69(2) 25(2) 10(2) -15(2) C(23) 82(2) 85(3) 67(2) 34(2) 15(2) -3(2) C(24) 72(2) 77(2) 67(2) 34(2) 0(2) 8(2) C(25) 49(2) 77(2) 47(1) 5(1) -2(1) -13(1) C(31) 49(1) 52(2) 38(1) -3(1) 4(1) 1(1) C(32) 75(2) 60(2) 65(2) 11(1) 5(2) 17(2) C(33) 75(2) 86(3) 57(2) 30(2) 3(2) 15(2) C(34) 73(2) 88(3) 36(1) 16(1) 3(1) 3(2) C(35) 60(2) 56(2) 37(1) -6(1) 0(1) 5(1) C(41) 61(2) 50(2) 55(2) -13(1) 9(1) -2(1) C(42) 86(2) 80(3) 65(2) -32(2) 12(2) 1(2) C(43) 107(3) 117(3) 55(2) -42(2) 7(2) -14(2) C(44) 81(2) 125(3) 57(2) -33(2) -15(2) -2(2) C(45) 63(2) 51(2) 47(1) -2(1) 4(1) 4(1) C(16) 65(2) 102(3) 60(2) 15(2) 11(1) 36(2) C(17) 76(2) 76(2) 47(2) 13(1) -2(1) 25(2) C(18) 99(2) 46(2) 76(2) -2(1) -10(2) 5(2) C(26) 65(2) 197(5) 136(4) -75(3) -24(2) 51(3) C(27) 93(2) 107(3) 48(2) -16(2) -2(2) 25(2) C(28) 169(4) 66(3) 100(3) 12(2) 34(3) 6(3) C(36) 68(2) 106(3) 57(2) 0(2) -19(1) -17(2) C(37) 49(2) 145(4) 82(2) -20(2) 3(2) 2(2) C(38) 92(3) 77(3) 99(3) 12(2) -22(2) -18(2) C(46) 118(3) 63(2) 74(2) -15(2) 22(2) -23(2) C(47) 97(2) 93(3) 46(2) 12(2) 10(2) -16(2) C(48) 55(2) 95(3) 123(3) 29(2) 10(2) 2(2) Li(1) 42(2) 59(3) 39(2) 8(2) 2(2) -2(2) Li(2) 47(2) 60(3) 32(2) 4(2) 2(2) 2(2) Li(3) 50(2) 60(3) 29(2) -3(2) 2(2) 4(2) Li(4) 57(2) 51(3) 38(2) -6(2) 0(2) 10(2) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for shelxs1419. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(12) 1539 2203 2142 72 H(13) 1803 2285 1231 79 H(14) 2834 2973 1157 74 H(15A) 2156 2968 2974 52 H(15B) 2811 2480 2909 52 H(22) 5195 5365 1457 85 H(23) 4316 5868 878 94 H(24) 3311 5365 1214 87 H(25A) 5148 4255 2304 70 H(25B) 4629 4766 2608 70 H(32) 4526 854 4405 80 H(33) 4346 913 5327 87 H(34) 3677 2157 5491 79 H(35A) 4218 2077 3647 61 H(35B) 3476 2125 3731 61 H(42) 2331 5757 5423 92 H(43) 3178 5384 6058 112 H(44) 3903 4347 5684 105 H(45A) 2092 5047 4468 64 H(45B) 2770 5175 4230 64 H(16A) 1434 4367 3093 113 H(16B) 1533 5381 3148 113 H(16C) 1832 4739 3538 113 H(17A) 2571 4940 1944 99 H(17B) 2030 5558 2146 99 H(17C) 1891 4558 2066 99 H(18A) 3164 5537 3349 110 H(18B) 2834 6187 2978 110 H(18C) 3415 5613 2803 110 H(26A) 5729 2993 2063 199 H(26B) 5634 1987 1972 199 H(26C) 5625 2358 2513 199 H(27A) 3997 2570 1401 124 H(27B) 4653 2094 1309 124 H(27C) 4617 3120 1295 124 H(28A) 4396 1575 2741 168 H(28B) 4298 1166 2213 168 H(28C) 3772 1782 2438 168 H(36A) 4590 3918 4845 115 H(36B) 5307 3991 4676 115 H(36C) 4980 3069 4718 115 H(37A) 5349 2674 3653 138 H(37B) 5713 3571 3688 138 H(37C) 5236 3397 3249 138 H(38A) 4435 5015 3499 134 H(38B) 4970 5222 3891 134 H(38C) 4248 5187 4054 134 H(46A) 1837 2329 3806 127 H(46B) 1604 1832 4282 127 H(46C) 2340 1957 4183 127 H(47A) 2367 2712 5236 118 H(47B) 1621 2588 5256 118 H(47C) 1923 3508 5367 118 H(48A) 1065 4308 4612 137 H(48B) 769 3369 4550 137 H(48C) 1005 3891 4083 137 ________________________________________________________________