Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 Table 1. Crystal data and structure refinement for shelxs1435. Identification code shelxs1435 Empirical formula C16 H28 Mg N2 O2 Si2 Formula weight 360.89 Temperature 293(2) K Wavelength 0.71073 A Crystal system triclinic Space group P-1 Unit cell dimensions a = 11.326(2) A alpha = 89.43(3) deg. b = 12.571(3) A beta = 76.80(3) deg. c = 14.982(3) A gamma = 89.53(3) deg. Volume 2076.6(7) A^3 Z 4 Density (calculated) 1.154 Mg/m^3 Absorption coefficient 0.210 mm^-1 F(000) 776 Crystal size 0.5 x 0.5 x 0.5 mm Theta range for data collection 1.62 to 22.51 deg. Index ranges -11<=h<=12, -13<=k<=13, 0<=l<=16 Reflections collected 5410 Independent reflections 5410 [R(int) = 0.0000] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 5410 / 0 / 425 Goodness-of-fit on F^2 1.402 Final R indices [I>2sigma(I)] R1 = 0.0693, wR2 = 0.1820 R indices (all data) R1 = 0.1018, wR2 = 0.2055 Largest diff. peak and hole 0.440 and -0.447 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for shelxs1435. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Mg(1) 9114(2) 14736(1) 9460(1) 50(1) Si(1) 10477(2) 12698(1) 10192(1) 61(1) Si(2) 7126(2) 14734(1) 8230(1) 65(1) Mg(2) 5029(2) 9725(1) 5957(1) 49(1) Si(3) 5636(2) 9874(1) 7986(1) 65(1) Si(4) 5357(2) 12295(1) 5355(1) 59(1) O(1) 7685(3) 14392(3) 10618(2) 62(1) C(1) 6894(5) 13560(5) 10912(4) 68(2) C(2) 6389(5) 13667(5) 11783(4) 76(2) C(3) 6874(5) 14611(5) 12075(4) 76(2) C(4) 7649(5) 15033(4) 11367(3) 57(1) C(5) 11643(6) 13969(5) 8811(4) 77(2) N(1) 10699(3) 13955(3) 9693(3) 51(1) C(21) 9871(6) 12870(5) 11449(4) 79(2) C(22) 9361(6) 11866(5) 9741(5) 89(2) C(23) 11887(7) 11874(5) 10012(6) 105(2) O(2) 10404(7) 15005(7) 6661(5) 191(3) C(6) 9975(6) 13999(6) 6886(4) 75(2) C(7) 10496(6) 13371(5) 6223(4) 74(2) C(8) 11201(9) 13915(10) 5573(6) 135(4) C(9) 11212(7) 14903(9) 5754(5) 116(3) C(10) 9130(6) 13550(5) 7716(4) 74(2) N(2) 8516(4) 14367(3) 8366(3) 59(1) C(24) 6600(6) 15904(6) 8975(5) 98(2) C(25) 7085(6) 15139(6) 7029(4) 93(2) C(26) 5974(6) 13654(6) 8527(5) 100(2) O(3) 3113(3) 9742(3) 6541(2) 60(1) C(11) 2595(5) 10704(4) 6355(4) 57(1) C(12) 1615(5) 10871(5) 7009(4) 79(2) C(13) 1457(6) 10001(5) 7629(4) 86(2) C(14) 2372(6) 9356(5) 7340(4) 76(2) C(15) 3230(5) 11221(4) 5492(3) 57(1) N(3) 4588(3) 11120(3) 5300(3) 48(1) C(27) 6838(6) 11942(5) 5599(5) 86(2) C(28) 4504(6) 13227(5) 6234(5) 91(2) C(29) 5660(7) 13058(5) 4252(5) 105(2) O(4) 8642(7) 9366(6) 6209(5) 160(3) C(16) 7941(5) 8501(5) 6494(4) 63(2) C(17) 8660(5) 7675(4) 6372(5) 77(2) C(18) 9771(9) 7966(8) 6054(8) 149(4) C(19) 9877(6) 8996(7) 5911(5) 100(2) C(20) 6626(5) 8342(4) 6819(4) 64(2) N(4) 5865(4) 9307(3) 6931(3) 57(1) C(30) 4604(6) 11037(5) 8019(4) 83(2) C(31) 7069(7) 10375(6) 8295(5) 100(2) C(32) 4893(8) 8925(6) 8943(4) 104(2) ________________________________________________________________ Table 3. Bond lengths [A] and angles [deg] for shelxs1435. _____________________________________________________________ Mg(1)-N(2) 1.971(5) Mg(1)-O(1) 2.129(4) Mg(1)-N(1)#1 2.129(4) Mg(1)-N(1) 2.134(4) Mg(1)-Mg(1)#1 2.934(3) Mg(1)-Si(2) 3.219(2) Si(1)-N(1) 1.738(4) Si(1)-C(23) 1.865(6) Si(1)-C(21) 1.865(6) Si(1)-C(22) 1.890(6) Si(2)-N(2) 1.693(5) Si(2)-C(24) 1.866(6) Si(2)-C(26) 1.870(7) Si(2)-C(25) 1.876(6) Mg(2)-N(4) 1.977(5) Mg(2)-N(3) 2.115(4) Mg(2)-N(3)#2 2.127(4) Mg(2)-O(3) 2.147(4) Mg(2)-C(15)#2 2.841(5) Mg(2)-Mg(2)#2 2.958(3) Si(3)-N(4) 1.705(4) Si(3)-C(30) 1.858(6) Si(3)-C(31) 1.901(7) Si(3)-C(32) 1.902(7) Si(4)-N(3) 1.733(4) Si(4)-C(27) 1.847(7) Si(4)-C(28) 1.862(6) Si(4)-C(29) 1.867(7) O(1)-C(4) 1.381(6) O(1)-C(1) 1.384(6) C(1)-C(2) 1.308(8) C(2)-C(3) 1.425(8) C(3)-C(4) 1.322(7) C(4)-C(5)#1 1.484(7) C(5)-C(4)#1 1.484(7) C(5)-N(1) 1.498(6) N(1)-Mg(1)#1 2.129(4) O(2)-C(6) 1.369(9) O(2)-C(9) 1.460(9) C(6)-C(7) 1.304(7) C(6)-C(10) 1.494(8) C(7)-C(8) 1.302(12) C(8)-C(9) 1.274(12) C(10)-N(2) 1.479(7) O(3)-C(14) 1.381(6) O(3)-C(11) 1.393(6) C(11)-C(12) 1.319(7) C(11)-C(15) 1.476(7) C(12)-C(13) 1.413(8) C(13)-C(14) 1.307(8) C(15)-N(3) 1.503(6) C(15)-Mg(2)#2 2.841(5) N(3)-Mg(2)#2 2.127(4) O(4)-C(16) 1.359(8) O(4)-C(19) 1.443(9) C(16)-C(17) 1.303(7) C(16)-C(20) 1.472(8) C(17)-C(18) 1.294(11) C(18)-C(19) 1.311(10) C(20)-N(4) 1.472(6) N(2)-Mg(1)-O(1) 106.61(17) N(2)-Mg(1)-N(1)#1 141.98(19) O(1)-Mg(1)-N(1)#1 80.31(15) N(2)-Mg(1)-N(1) 119.04(18) O(1)-Mg(1)-N(1) 106.71(16) N(1)#1-Mg(1)-N(1) 93.02(16) N(2)-Mg(1)-Mg(1)#1 157.63(16) O(1)-Mg(1)-Mg(1)#1 94.99(12) N(1)#1-Mg(1)-Mg(1)#1 46.59(12) N(1)-Mg(1)-Mg(1)#1 46.43(12) N(2)-Mg(1)-Si(2) 26.25(13) O(1)-Mg(1)-Si(2) 87.87(11) N(1)#1-Mg(1)-Si(2) 121.94(14) N(1)-Mg(1)-Si(2) 144.27(12) Mg(1)#1-Mg(1)-Si(2) 167.01(10) N(1)-Si(1)-C(23) 113.7(3) N(1)-Si(1)-C(21) 107.9(2) C(23)-Si(1)-C(21) 108.6(3) N(1)-Si(1)-C(22) 113.5(3) C(23)-Si(1)-C(22) 105.0(3) C(21)-Si(1)-C(22) 107.9(3) N(2)-Si(2)-C(24) 108.3(3) N(2)-Si(2)-C(26) 113.4(3) C(24)-Si(2)-C(26) 108.9(4) N(2)-Si(2)-C(25) 114.4(3) C(24)-Si(2)-C(25) 107.0(3) C(26)-Si(2)-C(25) 104.5(3) N(2)-Si(2)-Mg(1) 30.99(14) C(24)-Si(2)-Mg(1) 79.4(2) C(26)-Si(2)-Mg(1) 114.5(2) C(25)-Si(2)-Mg(1) 136.0(2) N(4)-Mg(2)-N(3) 139.15(18) N(4)-Mg(2)-N(3)#2 119.30(17) N(3)-Mg(2)-N(3)#2 91.57(15) N(4)-Mg(2)-O(3) 108.07(17) N(3)-Mg(2)-O(3) 81.99(15) N(3)#2-Mg(2)-O(3) 110.31(16) N(4)-Mg(2)-C(15)#2 95.23(17) N(3)-Mg(2)-C(15)#2 100.80(15) N(3)#2-Mg(2)-C(15)#2 31.21(15) O(3)-Mg(2)-C(15)#2 140.78(17) N(4)-Mg(2)-Mg(2)#2 153.22(16) N(3)-Mg(2)-Mg(2)#2 45.95(11) N(3)#2-Mg(2)-Mg(2)#2 45.62(11) O(3)-Mg(2)-Mg(2)#2 98.63(13) C(15)#2-Mg(2)-Mg(2)#2 61.25(12) N(4)-Si(3)-C(30) 108.6(3) N(4)-Si(3)-C(31) 114.4(3) C(30)-Si(3)-C(31) 107.1(3) N(4)-Si(3)-C(32) 112.4(3) C(30)-Si(3)-C(32) 107.4(3) C(31)-Si(3)-C(32) 106.5(4) N(3)-Si(4)-C(27) 107.5(2) N(3)-Si(4)-C(28) 112.9(3) C(27)-Si(4)-C(28) 110.7(3) N(3)-Si(4)-C(29) 112.6(3) C(27)-Si(4)-C(29) 107.5(3) C(28)-Si(4)-C(29) 105.5(3) C(4)-O(1)-C(1) 107.0(4) C(4)-O(1)-Mg(1) 114.8(3) C(1)-O(1)-Mg(1) 136.7(3) C(2)-C(1)-O(1) 109.8(5) C(1)-C(2)-C(3) 106.7(5) C(4)-C(3)-C(2) 108.6(5) C(3)-C(4)-O(1) 107.9(5) C(3)-C(4)-C(5)#1 135.6(5) O(1)-C(4)-C(5)#1 116.2(4) C(4)#1-C(5)-N(1) 114.4(4) C(5)-N(1)-Si(1) 113.0(3) C(5)-N(1)-Mg(1)#1 111.8(3) Si(1)-N(1)-Mg(1)#1 118.3(2) C(5)-N(1)-Mg(1) 108.0(4) Si(1)-N(1)-Mg(1) 115.8(2) Mg(1)#1-N(1)-Mg(1) 86.98(16) C(6)-O(2)-C(9) 104.9(7) C(7)-C(6)-O(2) 107.6(6) C(7)-C(6)-C(10) 119.8(6) O(2)-C(6)-C(10) 132.5(6) C(8)-C(7)-C(6) 110.1(7) C(9)-C(8)-C(7) 112.7(7) C(8)-C(9)-O(2) 104.7(8) N(2)-C(10)-C(6) 113.7(5) C(10)-N(2)-Si(2) 114.4(4) C(10)-N(2)-Mg(1) 121.4(4) Si(2)-N(2)-Mg(1) 122.8(2) C(14)-O(3)-C(11) 105.9(4) C(14)-O(3)-Mg(2) 135.1(4) C(11)-O(3)-Mg(2) 110.8(3) C(12)-C(11)-O(3) 108.1(5) C(12)-C(11)-C(15) 137.8(5) O(3)-C(11)-C(15) 114.1(4) C(11)-C(12)-C(13) 108.9(5) C(14)-C(13)-C(12) 106.5(5) C(13)-C(14)-O(3) 110.6(6) C(11)-C(15)-N(3) 113.9(4) C(11)-C(15)-Mg(2)#2 126.9(3) N(3)-C(15)-Mg(2)#2 47.2(2) C(15)-N(3)-Si(4) 115.3(3) C(15)-N(3)-Mg(2) 108.4(3) Si(4)-N(3)-Mg(2) 120.6(2) C(15)-N(3)-Mg(2)#2 101.6(3) Si(4)-N(3)-Mg(2)#2 118.2(2) Mg(2)-N(3)-Mg(2)#2 88.43(15) C(16)-O(4)-C(19) 107.3(7) C(17)-C(16)-O(4) 106.9(5) C(17)-C(16)-C(20) 119.2(5) O(4)-C(16)-C(20) 133.8(6) C(18)-C(17)-C(16) 110.4(6) C(17)-C(18)-C(19) 112.9(7) C(18)-C(19)-O(4) 102.5(7) N(4)-C(20)-C(16) 116.3(5) C(20)-N(4)-Si(3) 114.6(4) C(20)-N(4)-Mg(2) 119.5(3) Si(3)-N(4)-Mg(2) 125.4(2) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 -x+2,-y+3,-z+2 #2 -x+1,-y+2,-z+1 Table 4. Anisotropic displacement parameters (A^2 x 10^3) for shelxs1435. 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 _______________________________________________________________________ Mg(1) 54(1) 51(1) 42(1) -3(1) -3(1) -6(1) Si(1) 70(1) 48(1) 63(1) -4(1) -10(1) 0(1) Si(2) 69(1) 69(1) 58(1) -2(1) -20(1) -11(1) Mg(2) 54(1) 47(1) 42(1) -3(1) -3(1) -1(1) Si(3) 78(1) 64(1) 52(1) -2(1) -14(1) -11(1) Si(4) 70(1) 45(1) 62(1) -3(1) -13(1) -5(1) O(1) 67(2) 70(2) 45(2) -2(2) -2(2) -20(2) C(1) 55(3) 77(4) 67(4) 6(3) -5(3) -23(3) C(2) 69(4) 82(4) 64(4) 13(3) 11(3) -22(3) C(3) 75(4) 88(4) 49(3) 2(3) 17(3) -2(3) C(4) 52(3) 64(3) 47(3) -7(3) 2(3) 6(3) C(5) 84(4) 77(4) 60(4) -12(3) 7(3) -17(3) N(1) 52(2) 49(2) 45(2) -4(2) 4(2) -6(2) C(21) 97(5) 68(4) 67(4) 15(3) -8(3) -9(3) C(22) 105(5) 64(4) 98(5) -3(4) -23(4) -20(4) C(23) 105(6) 79(5) 132(7) -13(4) -26(5) 32(4) O(2) 196(8) 214(9) 142(6) -27(6) 6(5) -44(7) C(6) 92(5) 83(4) 51(4) -5(3) -21(3) 9(4) C(7) 117(5) 57(3) 30(3) -6(3) 18(3) 34(3) C(8) 152(9) 174(10) 76(6) -40(7) -19(6) 82(8) C(9) 94(6) 172(9) 62(5) 20(5) 22(4) -6(6) C(10) 84(4) 77(4) 59(4) -15(3) -11(3) -1(3) N(2) 68(3) 58(3) 47(2) -8(2) -5(2) -2(2) C(24) 80(5) 116(6) 106(6) -40(5) -36(4) 24(4) C(25) 105(5) 106(5) 74(4) 9(4) -36(4) -16(4) C(26) 95(5) 110(6) 100(5) 18(4) -35(4) -34(4) O(3) 55(2) 59(2) 60(2) 4(2) 2(2) -2(2) C(11) 52(3) 54(3) 62(3) -7(3) -6(3) -1(3) C(12) 64(4) 67(4) 90(5) -4(3) 17(3) 9(3) C(13) 74(4) 86(5) 77(4) -1(4) 27(3) 4(4) C(14) 77(4) 72(4) 67(4) 11(3) 10(3) -17(3) C(15) 60(3) 58(3) 49(3) 1(2) -6(3) 1(3) N(3) 49(2) 43(2) 47(2) -5(2) -1(2) 1(2) C(27) 74(4) 70(4) 109(5) 2(4) -12(4) -12(3) C(28) 101(5) 63(4) 116(6) -37(4) -37(4) 19(4) C(29) 134(7) 78(5) 106(6) 31(4) -33(5) -47(4) O(4) 149(6) 171(6) 152(6) 33(5) -19(5) 1(5) C(16) 65(4) 69(4) 55(3) 7(3) -11(3) -11(3) C(17) 33(3) 33(3) 144(6) 12(3) 22(3) 9(2) C(18) 127(9) 92(7) 209(11) 4(7) 0(7) 37(6) C(19) 45(4) 137(7) 112(6) 2(5) -3(4) 7(4) C(20) 69(4) 58(3) 62(4) 11(3) -5(3) -5(3) N(4) 60(3) 60(3) 51(3) 1(2) -10(2) 4(2) C(30) 90(5) 75(4) 81(4) -19(3) -10(4) -5(4) C(31) 96(5) 119(6) 95(5) -9(4) -43(4) -27(4) C(32) 155(7) 92(5) 54(4) 5(3) 0(4) -26(5) _______________________________________________________________________ Table 5. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for shelxs1435. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(1) 6745 13007 10545 81 H(2) 5824 13215 12142 91 H(3) 6677 14885 12665 91 H(5A) 12199 13379 8817 93 H(5B) 11248 13857 8309 93 H(21A) 10372 13359 11681 119 H(21B) 9870 12195 11754 119 H(21C) 9057 13144 11558 119 H(22A) 8651 12283 9731 133 H(22B) 9138 11256 10132 133 H(22C) 9729 11635 9131 133 H(23A) 12197 11764 9367 158 H(23B) 11706 11198 10315 158 H(23C) 12482 12234 10260 158 H(7) 10381 12639 6215 89 H(8) 11648 13616 5035 162 H(9) 11640 15440 5390 139 H(10A) 8520 13131 7522 89 H(10B) 9583 13076 8031 89 H(24A) 6580 15718 9602 147 H(24B) 5802 16110 8919 147 H(24C) 7148 16485 8789 147 H(25A) 7681 15677 6816 139 H(25B) 6295 15414 7020 139 H(25C) 7257 14532 6635 139 H(26A) 6225 13057 8132 150 H(26B) 5204 13913 8449 150 H(26C) 5902 13436 9153 150 H(12) 1110 11464 7055 95 H(13) 826 9907 8142 103 H(14) 2505 8724 7631 92 H(15A) 3013 11970 5515 68 H(15B) 2949 10911 4988 68 H(27A) 6711 11538 6160 129 H(27B) 7273 12579 5659 129 H(27C) 7298 11524 5106 129 H(28A) 4053 13723 5950 137 H(28B) 5064 13607 6505 137 H(28C) 3957 12831 6701 137 H(29A) 5959 12583 3753 157 H(29B) 6254 13596 4262 157 H(29C) 4922 13388 4174 157 H(17) 8411 6976 6497 92 H(18) 10425 7496 5938 179 H(19) 10573 9388 5676 120 H(20A) 6358 7878 6392 77 H(20B) 6484 7972 7405 77 H(30A) 4939 11518 7527 125 H(30B) 4515 11394 8594 125 H(30C) 3826 10798 7954 125 ________________________________________________________________