Table 1. Crystal data and structure refinement for 1. Identification code s92 Empirical formula C22 H44 Si4 Zr Formula weight 512.15 Temperature 293(2) K Wavelength 0.71069 A Crystal system Monoclinic Space group P21/n Unit cell dimensions a = 12.075(6) A alpha = 90 deg. b = 15.420(2) A beta = 99.36(2) deg. c = 15.571(4) A gamma = 90 deg. Volume 2861(2) A^3 Z 4 Density (calculated) 1.189 Mg/m^3 Absorption coefficient 0.558 mm^-1 F(000) 1088 Crystal size ? x ? x ? mm Theta range for data collection 2.33 to 30.07 deg. Index ranges -16<=h<=16, -21<=k<=20, -21<=l<=14 Reflections collected 13237 Independent reflections 7124 [R(int) = 0.0576] Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 7120 / 0 / 257 Goodness-of-fit on F^2 0.487 Final R indices [I>2sigma(I)] R1 = 0.0539, wR2 = 0.1190 R indices (all data) R1 = 0.1298, wR2 = 0.1967 Extinction coefficient 0.002(1) Largest diff. peak and hole 0.978 and -0.870 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 1. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ Zr(1) 887(1) 699(1) 689(1) 44(1) Si(1) 2289(2) 2636(1) -642(2) 66(1) Si(2) 4024(1) -35(1) 1738(1) 51(1) Si(3) 222(2) -39(1) 3031(1) 53(1) Si(4) -1477(2) 2595(1) 463(1) 51(1) C(1) 1764(8) 3563(4) -63(6) 92(3) C(2) 1503(9) 2611(5) -1759(6) 108(4) C(3) 3803(8) 2783(7) -659(10) 162(7) C(4) 2203(5) 1559(4) -101(4) 51(2) C(5) 2052(5) 748(4) -520(4) 47(1) C(6) 2489(5) 101(3) 47(4) 42(1) C(7) 2995(5) 471(4) 856(4) 43(1) C(8) 2800(5) 1377(4) 749(4) 48(1) C(9) 5431(6) 225(6) 1486(7) 101(3) C(10) 3889(7) -1237(4) 1742(6) 78(2) C(11) 3901(7) 423(6) 2806(5) 84(3) C(12) 837(8) -1109(4) 2813(6) 84(3) C(13) 1030(7) 408(5) 4053(4) 71(2) C(14) -1263(6) -211(5) 3169(5) 74(2) C(15) 220(5) 797(4) 2167(4) 46(1) C(16) -688(5) 1070(4) 1544(4) 45(1) C(17) -454(5) 1856(4) 1139(4) 45(1) C(18) 658(5) 2084(4) 1533(4) 48(1) C(19) 1062(5) 1443(4) 2142(4) 52(2) C(20) -2911(5) 2339(5) 671(5) 69(2) C(21) -1143(7) 3730(4) 849(6) 87(3) C(22) -1432(7) 2519(5) -720(5) 77(2) ________________________________________________________________ Table 3. Selected bond lengths [A] and angles [deg] for 1. _____________________________________________________________ _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 4. Bond lengths [A] and angles [deg] for 1. _____________________________________________________________ Zr(1)-C(6) 2.494(6) Zr(1)-C(19) 2.515(6) Zr(1)-C(8) 2.523(6) Zr(1)-C(5) 2.528(6) Zr(1)-C(4) 2.537(7) Zr(1)-C(7) 2.541(6) Zr(1)-C(18) 2.546(5) Zr(1)-C(16) 2.557(6) Zr(1)-C(15) 2.563(6) Zr(1)-C(17) 2.580(6) Zr(1)-Zr(1)#1 3.5143(14) Si(1)-C(2) 1.842(9) Si(1)-C(3) 1.846(9) Si(1)-C(1) 1.856(9) Si(1)-C(4) 1.872(6) Si(2)-C(11) 1.836(8) Si(2)-C(9) 1.849(8) Si(2)-C(10) 1.860(7) Si(2)-C(7) 1.867(6) Si(3)-C(14) 1.860(7) Si(3)-C(13) 1.860(7) Si(3)-C(15) 1.862(6) Si(3)-C(12) 1.863(7) Si(4)-C(20) 1.854(7) Si(4)-C(22) 1.856(8) Si(4)-C(21) 1.872(7) Si(4)-C(17) 1.874(6) C(1)-H(1A) 0.96 C(1)-H(1B) 0.96 C(1)-H(1C) 0.96 C(2)-H(2A) 0.96 C(2)-H(2B) 0.96 C(2)-H(2C) 0.96 C(3)-H(3A) 0.96 C(3)-H(3B) 0.96 C(3)-H(3C) 0.96 C(4)-C(5) 1.410(8) C(4)-C(8) 1.428(8) C(5)-C(6) 1.378(7) C(5)-H(5) 0.93 C(6)-C(7) 1.427(7) C(6)-H(6) 0.93 C(7)-C(8) 1.422(7) C(8)-H(8) 0.93 C(9)-H(9A) 0.96 C(9)-H(9B) 0.96 C(9)-H(9C) 0.96 C(10)-H(10A) 0.96 C(10)-H(10B) 0.96 C(10)-H(10C) 0.96 C(11)-H(11A) 0.96 C(11)-H(11B) 0.96 C(11)-H(11C) 0.96 C(12)-H(12A) 0.96 C(12)-H(12B) 0.96 C(12)-H(12C) 0.96 C(13)-H(13A) 0.96 C(13)-H(13B) 0.96 C(13)-H(13C) 0.96 C(14)-H(14A) 0.96 C(14)-H(14B) 0.96 C(14)-H(14C) 0.96 C(15)-C(16) 1.405(8) C(15)-C(19) 1.428(8) C(16)-C(17) 1.415(8) C(16)-H(16) 0.93 C(17)-C(18) 1.427(8) C(18)-C(19) 1.401(8) C(18)-H(18) 0.93 C(19)-H(19) 0.93 C(20)-H(20A) 0.96 C(20)-H(20B) 0.96 C(20)-H(20C) 0.96 C(21)-H(21A) 0.96 C(21)-H(21B) 0.96 C(21)-H(21C) 0.96 C(22)-H(22A) 0.96 C(22)-H(22B) 0.96 C(22)-H(22C) 0.96 C(6)-Zr(1)-C(19) 124.9(2) C(6)-Zr(1)-C(8) 53.4(2) C(19)-Zr(1)-C(8) 80.5(2) C(6)-Zr(1)-C(5) 31.8(2) C(19)-Zr(1)-C(5) 132.9(2) C(8)-Zr(1)-C(5) 53.0(2) C(6)-Zr(1)-C(4) 53.9(2) C(19)-Zr(1)-C(4) 103.3(2) C(8)-Zr(1)-C(4) 32.8(2) C(5)-Zr(1)-C(4) 32.3(2) C(6)-Zr(1)-C(7) 32.9(2) C(19)-Zr(1)-C(7) 92.0(2) C(8)-Zr(1)-C(7) 32.6(2) C(5)-Zr(1)-C(7) 53.9(2) C(4)-Zr(1)-C(7) 54.9(2) C(6)-Zr(1)-C(18) 132.3(2) C(19)-Zr(1)-C(18) 32.1(2) C(8)-Zr(1)-C(18) 79.0(2) C(5)-Zr(1)-C(18) 118.7(2) C(4)-Zr(1)-C(18) 86.6(2) C(7)-Zr(1)-C(18) 104.7(2) C(6)-Zr(1)-C(16) 169.2(2) C(19)-Zr(1)-C(16) 52.4(2) C(8)-Zr(1)-C(16) 129.9(2) C(5)-Zr(1)-C(16) 158.8(2) C(4)-Zr(1)-C(16) 135.5(2) C(7)-Zr(1)-C(16) 142.7(2) C(18)-Zr(1)-C(16) 52.5(2) C(6)-Zr(1)-C(15) 139.4(2) C(19)-Zr(1)-C(15) 32.7(2) C(8)-Zr(1)-C(15) 111.2(2) C(5)-Zr(1)-C(15) 163.9(2) C(4)-Zr(1)-C(15) 135.9(2) C(7)-Zr(1)-C(15) 111.8(2) C(18)-Zr(1)-C(15) 53.9(2) C(16)-Zr(1)-C(15) 31.9(2) C(6)-Zr(1)-C(17) 157.8(2) C(19)-Zr(1)-C(17) 53.5(2) C(8)-Zr(1)-C(17) 108.3(2) C(5)-Zr(1)-C(17) 129.2(2) C(4)-Zr(1)-C(17) 103.9(2) C(7)-Zr(1)-C(17) 136.9(2) C(18)-Zr(1)-C(17) 32.3(2) C(16)-Zr(1)-C(17) 32.0(2) C(15)-Zr(1)-C(17) 54.1(2) C(6)-Zr(1)-Zr(1)#1 87.92(13) C(19)-Zr(1)-Zr(1)#1 141.5(2) C(8)-Zr(1)-Zr(1)#1 137.8(2) C(5)-Zr(1)-Zr(1)#1 85.48(13) C(4)-Zr(1)-Zr(1)#1 113.1(2) C(7)-Zr(1)-Zr(1)#1 118.60(13) C(18)-Zr(1)-Zr(1)#1 136.33(13) C(16)-Zr(1)-Zr(1)#1 91.38(14) C(15)-Zr(1)-Zr(1)#1 109.57(13) C(17)-Zr(1)-Zr(1)#1 104.04(13) C(2)-Si(1)-C(3) 110.4(6) C(2)-Si(1)-C(1) 108.1(4) C(3)-Si(1)-C(1) 109.3(5) C(2)-Si(1)-C(4) 110.4(3) C(3)-Si(1)-C(4) 104.0(4) C(1)-Si(1)-C(4) 114.6(4) C(11)-Si(2)-C(9) 108.7(4) C(11)-Si(2)-C(10) 111.1(4) C(9)-Si(2)-C(10) 107.5(4) C(11)-Si(2)-C(7) 111.3(3) C(9)-Si(2)-C(7) 106.1(4) C(10)-Si(2)-C(7) 111.8(3) C(14)-Si(3)-C(13) 109.6(4) C(14)-Si(3)-C(15) 107.1(3) C(13)-Si(3)-C(15) 107.5(3) C(14)-Si(3)-C(12) 108.4(4) C(13)-Si(3)-C(12) 108.3(4) C(15)-Si(3)-C(12) 115.8(3) C(20)-Si(4)-C(22) 109.8(4) C(20)-Si(4)-C(21) 107.6(4) C(22)-Si(4)-C(21) 109.8(4) C(20)-Si(4)-C(17) 108.8(3) C(22)-Si(4)-C(17) 113.3(3) C(21)-Si(4)-C(17) 107.5(3) Si(1)-C(1)-H(1A) 109.5(3) Si(1)-C(1)-H(1B) 109.5(3) H(1A)-C(1)-H(1B) 109.5 Si(1)-C(1)-H(1C) 109.5(3) H(1A)-C(1)-H(1C) 109.5 H(1B)-C(1)-H(1C) 109.5 Si(1)-C(2)-H(2A) 109.5(3) Si(1)-C(2)-H(2B) 109.5(4) H(2A)-C(2)-H(2B) 109.5 Si(1)-C(2)-H(2C) 109.5(3) H(2A)-C(2)-H(2C) 109.5 H(2B)-C(2)-H(2C) 109.5 Si(1)-C(3)-H(3A) 109.5(4) Si(1)-C(3)-H(3B) 109.5(5) H(3A)-C(3)-H(3B) 109.5 Si(1)-C(3)-H(3C) 109.5(3) H(3A)-C(3)-H(3C) 109.5 H(3B)-C(3)-H(3C) 109.5 C(5)-C(4)-C(8) 105.2(5) C(5)-C(4)-Si(1) 126.3(5) C(8)-C(4)-Si(1) 122.3(4) C(5)-C(4)-Zr(1) 73.5(3) C(8)-C(4)-Zr(1) 73.1(4) Si(1)-C(4)-Zr(1) 140.0(3) C(6)-C(5)-C(4) 109.8(5) C(6)-C(5)-Zr(1) 72.7(3) C(4)-C(5)-Zr(1) 74.2(4) C(6)-C(5)-H(5) 125.1(3) C(4)-C(5)-H(5) 125.1(4) Zr(1)-C(5)-H(5) 119.67(14) C(5)-C(6)-C(7) 109.9(5) C(5)-C(6)-Zr(1) 75.4(3) C(7)-C(6)-Zr(1) 75.4(3) C(5)-C(6)-H(6) 125.0(3) C(7)-C(6)-H(6) 125.0(3) Zr(1)-C(6)-H(6) 116.05(13) C(8)-C(7)-C(6) 104.5(5) C(8)-C(7)-Si(2) 125.1(4) C(6)-C(7)-Si(2) 128.4(4) C(8)-C(7)-Zr(1) 73.0(3) C(6)-C(7)-Zr(1) 71.7(3) Si(2)-C(7)-Zr(1) 132.0(3) C(7)-C(8)-C(4) 110.5(5) C(7)-C(8)-Zr(1) 74.4(3) C(4)-C(8)-Zr(1) 74.1(3) C(7)-C(8)-H(8) 124.7(4) C(4)-C(8)-H(8) 124.7(3) Zr(1)-C(8)-H(8) 118.5(2) Si(2)-C(9)-H(9A) 109.5(3) Si(2)-C(9)-H(9B) 109.5(3) H(9A)-C(9)-H(9B) 109.5 Si(2)-C(9)-H(9C) 109.5(3) H(9A)-C(9)-H(9C) 109.5 H(9B)-C(9)-H(9C) 109.5 Si(2)-C(10)-H(10A) 109.5(3) Si(2)-C(10)-H(10B) 109.5(2) H(10A)-C(10)-H(10B) 109.5 Si(2)-C(10)-H(10C) 109.5(3) H(10A)-C(10)-H(10C) 109.5 H(10B)-C(10)-H(10C) 109.5 Si(2)-C(11)-H(11A) 109.5(2) Si(2)-C(11)-H(11B) 109.5(3) H(11A)-C(11)-H(11B) 109.5 Si(2)-C(11)-H(11C) 109.5(3) H(11A)-C(11)-H(11C) 109.5 H(11B)-C(11)-H(11C) 109.5 Si(3)-C(12)-H(12A) 109.5(3) Si(3)-C(12)-H(12B) 109.5(3) H(12A)-C(12)-H(12B) 109.5 Si(3)-C(12)-H(12C) 109.5(3) H(12A)-C(12)-H(12C) 109.5 H(12B)-C(12)-H(12C) 109.5 Si(3)-C(13)-H(13A) 109.5(3) Si(3)-C(13)-H(13B) 109.5(3) H(13A)-C(13)-H(13B) 109.5 Si(3)-C(13)-H(13C) 109.5(2) H(13A)-C(13)-H(13C) 109.5 H(13B)-C(13)-H(13C) 109.5 Si(3)-C(14)-H(14A) 109.5(3) Si(3)-C(14)-H(14B) 109.5(3) H(14A)-C(14)-H(14B) 109.5 Si(3)-C(14)-H(14C) 109.5(3) H(14A)-C(14)-H(14C) 109.5 H(14B)-C(14)-H(14C) 109.5 C(16)-C(15)-C(19) 104.5(5) C(16)-C(15)-Si(3) 128.0(5) C(19)-C(15)-Si(3) 125.8(5) C(16)-C(15)-Zr(1) 73.8(3) C(19)-C(15)-Zr(1) 71.8(4) Si(3)-C(15)-Zr(1) 130.1(3) C(15)-C(16)-C(17) 112.0(5) C(15)-C(16)-Zr(1) 74.3(3) C(17)-C(16)-Zr(1) 74.9(3) C(15)-C(16)-H(16) 124.0(4) C(17)-C(16)-H(16) 124.0(3) Zr(1)-C(16)-H(16) 118.33(13) C(16)-C(17)-C(18) 105.2(5) C(16)-C(17)-Si(4) 127.6(5) C(18)-C(17)-Si(4) 125.4(4) C(16)-C(17)-Zr(1) 73.1(3) C(18)-C(17)-Zr(1) 72.5(3) Si(4)-C(17)-Zr(1) 130.8(3) C(19)-C(18)-C(17) 108.4(5) C(19)-C(18)-Zr(1) 72.7(3) C(17)-C(18)-Zr(1) 75.2(3) C(19)-C(18)-H(18) 125.8(3) C(17)-C(18)-H(18) 125.8(3) Zr(1)-C(18)-H(18) 118.2(2) C(18)-C(19)-C(15) 109.9(5) C(18)-C(19)-Zr(1) 75.1(3) C(15)-C(19)-Zr(1) 75.5(3) C(18)-C(19)-H(19) 125.1(3) C(15)-C(19)-H(19) 125.1(3) Zr(1)-C(19)-H(19) 116.15(14) Si(4)-C(20)-H(20A) 109.5(2) Si(4)-C(20)-H(20B) 109.5(3) H(20A)-C(20)-H(20B) 109.5 Si(4)-C(20)-H(20C) 109.5(2) H(20A)-C(20)-H(20C) 109.5 H(20B)-C(20)-H(20C) 109.5 Si(4)-C(21)-H(21A) 109.5(3) Si(4)-C(21)-H(21B) 109.5(3) H(21A)-C(21)-H(21B) 109.5 Si(4)-C(21)-H(21C) 109.5(3) H(21A)-C(21)-H(21C) 109.5 H(21B)-C(21)-H(21C) 109.5 Si(4)-C(22)-H(22A) 109.5(2) Si(4)-C(22)-H(22B) 109.5(3) H(22A)-C(22)-H(22B) 109.5 Si(4)-C(22)-H(22C) 109.5(3) H(22A)-C(22)-H(22C) 109.5 H(22B)-C(22)-H(22C) 109.5 _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: #1 -x,-y,-z Table 5. Anisotropic displacement parameters (A^2 x 10^3) for 1. 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 _______________________________________________________________________ Zr(1) 41(1) 44(1) 46(1) -11(1) 9(1) -3(1) Si(1) 63(1) 48(1) 84(2) 20(1) 9(1) -7(1) Si(2) 41(1) 59(1) 51(1) 1(1) 1(1) 3(1) Si(3) 58(1) 56(1) 45(1) 0(1) 6(1) 8(1) Si(4) 52(1) 47(1) 51(1) 1(1) 4(1) 6(1) C(1) 108(7) 51(4) 112(8) 10(5) 1(6) -13(4) C(2) 166(10) 82(6) 74(6) 23(5) 12(7) -23(6) C(3) 79(6) 108(8) 307(20) 94(10) 59(10) 3(6) C(4) 49(3) 45(3) 57(4) -1(3) -3(3) -3(3) C(5) 48(3) 50(3) 42(3) 3(3) 7(3) -10(3) C(6) 47(3) 39(3) 38(3) 3(2) 4(2) 7(2) C(7) 43(3) 45(3) 42(3) -2(2) 7(3) -1(2) C(8) 42(3) 41(3) 58(4) -4(3) 3(3) -5(3) C(9) 54(4) 149(9) 101(8) 17(7) 18(5) -6(5) C(10) 85(5) 64(4) 78(6) 12(4) -12(5) 13(4) C(11) 73(5) 119(7) 55(5) -10(5) -9(4) 25(5) C(12) 112(7) 60(4) 79(6) 9(4) 12(5) 21(5) C(13) 80(5) 88(5) 43(4) -7(4) 2(4) -1(4) C(14) 74(5) 89(5) 63(5) 4(4) 20(4) -14(4) C(15) 43(3) 51(3) 43(3) -10(3) 5(3) 3(3) C(16) 46(3) 48(3) 42(3) -6(3) 8(3) 2(3) C(17) 50(3) 44(3) 39(3) -4(2) 1(3) 4(3) C(18) 48(3) 40(3) 55(4) -14(3) 5(3) -3(3) C(19) 51(3) 51(3) 51(4) -9(3) -2(3) 7(3) C(20) 60(4) 78(5) 71(5) 5(4) 18(4) 16(4) C(21) 88(6) 50(4) 120(8) -6(5) 3(6) 15(4) C(22) 82(5) 87(5) 62(5) 24(4) 5(4) -4(5) _______________________________________________________________________ Table 6. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 1. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(1A) 966(11) 3513(23) -94(36) 138 H(1B) 1936(48) 4097(5) -330(27) 138 H(1C) 2118(40) 3559(24) 536(12) 138 H(2A) 1593(52) 3154(19) -2041(17) 162 H(2B) 722(12) 2514(46) -1741(6) 162 H(2C) 1785(41) 2150(31) -2078(15) 162 H(3A) 4024(22) 3356(28) -462(70) 242 H(3B) 3949(16) 2704(71) -1242(17) 242 H(3C) 4221(9) 2363(50) -282(58) 242 H(5) 1709(5) 661(4) -1093(4) 56 H(6) 2457(5) -489(3) -79(4) 50 H(8) 3029(5) 1793(4) 1173(4) 57 H(9A) 5505(22) -13(39) 928(21) 151 H(9B) 5995(6) -20(39) 1925(25) 151 H(9C) 5523(23) 843(6) 1474(45) 151 H(10A) 3190(24) -1393(4) 1919(36) 118 H(10B) 4499(29) -1480(5) 2141(29) 118 H(10C) 3907(49) -1457(5) 1168(10) 118 H(11A) 4498(28) 206(29) 3235(8) 127 H(11B) 3192(21) 260(30) 2962(17) 127 H(11C) 3948(46) 1044(6) 2781(11) 127 H(12A) 712(44) -1514(11) 3255(23) 126 H(12B) 1629(12) -1045(9) 2818(39) 126 H(12C) 487(37) -1318(19) 2254(18) 126 H(13A) 1819(7) 356(32) 4038(15) 107 H(13B) 848(34) 91(23) 4542(5) 107 H(13C) 842(34) 1008(11) 4107(18) 107 H(14A) -1291(7) -612(28) 3637(23) 112 H(14B) -1679(12) -442(33) 2640(13) 112 H(14C) -1587(15) 332(8) 3300(35) 112 H(16) -1362(5) 771(4) 1414(4) 54 H(18) 1049(5) 2575(4) 1407(4) 57 H(19) 1771(5) 1439(4) 2480(4) 63 H(20A) -3444(7) 2706(24) 319(25) 103 H(20B) -2949(13) 2434(32) 1274(9) 103 H(20C) -3081(17) 1743(11) 526(32) 103 H(21A) -1631(37) 4128(5) 496(27) 131 H(21B) -377(18) 3860(15) 805(39) 131 H(21C) -1250(50) 3782(12) 1444(14) 131 H(22A) -1444(44) 1921(5) -890(8) 116 H(22B) -758(22) 2787(30) -843(7) 116 H(22C) -2073(24) 2811(29) -1039(5) 116 ________________________________________________________________