3166

Table 1 Crystal data and structure refinement for 3166.
Identification code 3166
Empirical formula C54H120K6Li8O19Si6
Formula weight 1533.16
Temperature/K 293(2)
Crystal system triclinic
Space group P1
a/Å 13.4104(15)
b/Å 13.4700(15)
c/Å 13.8314(14)
α/° 118.487(11)
β/° 94.653(9)
γ/° 95.912(10)
Volume/Å3 2159.9(5)
Z 1
ρcalcg/cm3 1.179
μ/mm‑1 0.439
F(000) 819.0
Crystal size/mm3 0.28 × 0.27 × 0.25
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.608 to 50
Index ranges -15 ≤ h ≤ 15, -16 ≤ k ≤ 16, -15 ≤ l ≤ 16
Reflections collected 15657
Independent reflections 11650 [Rint = 0.0476, Rsigma = 0.1438]
Data/restraints/parameters 11650/3/862
Goodness-of-fit on F2 0.947
Final R indexes [I>=2σ (I)] R1 = 0.0874, wR2 = 0.2400
Final R indexes [all data] R1 = 0.1841, wR2 = 0.3467
Largest diff. peak/hole / e Å-3 0.92/-0.58
Flack parameter0.5(2)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3166. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
K5-2121(5)-3113(6)341(6)62(2)
K32112(5)-6876(6)-328(6)56.0(19)
K11732(5)-2269(5)2435(6)59(2)
K6-1729(5)-7719(5)-2426(6)57.9(19)
K21157(5)-4184(6)-2111(6)59.5(19)
Si23509(7)-4192(7)1810(8)57(2)
Si4-3507(7)-5797(8)-1804(8)64(3)
Si5-517(7)-6679(8)-4069(7)60(3)
Si3529(7)-3292(9)4079(8)62(3)
Si1-923(8)-2530(9)-1541(10)70(3)
Si6911(8)-7488(8)1541(8)63(3)
O4-2338(16)-5490(17)-1331(16)55(5)
O22320(13)-4524(17)1334(17)51(5)
O18-3280(20)-1422(19)972(16)79(7)
O163223(19)-8580(20)-890(30)119(11)
O3433(16)-3812(17)2759(15)51(5)
O5-486(16)-6110(17)-2749(18)54(6)
O152700(20)-4020(20)-3190(20)87(8)
O17-2750(18)-6010(20)3150(20)80(7)
O12-1574(15)-6962(18)-167(19)64(6)
O81568(15)-3014(16)214(18)50(5)
O91801(13)-5559(17)-1334(19)59(6)
O13-1798(15)-4457(17)1336(16)50(5)
O6644(15)-6537(16)1208(14)49(5)
O1-682(17)-3426(15)-1163(19)60(6)
O71(19)-4950(20)60(20)44(3)
O11-239(14)-2469(13)1505(15)42(5)
O10230(17)-7560(20)-1510(20)73(7)
O142921(16)-280(20)3700(20)100(9)
O19-3110(30)-9740(20)-3593(18)167(17)
C414560(30)-9650(40)-1310(50)118(18)
C48-4400(40)-180(40)1420(40)140(20)
C81050(20)-4260(40)4630(30)91(13)
C13-1010(30)-5700(30)-4510(30)109(15)
C54250(20)-5410(30)1080(30)67(9)
C10-4180(20)-4570(30)-1190(30)80(12)
C424240(30)-8680(30)-470(40)99(14)
C47-4060(30)-1270(40)460(40)93(13)
C2-2120(30)-3080(30)-2630(40)80(11)
C182190(40)-7070(50)2400(50)140(20)
C364320(40)-4110(50)-3550(50)170(30)
C45-4330(30)-5770(30)3720(40)101(13)
C71330(30)-1930(30)4850(20)72(11)
C14-1460(30)-8100(30)-4920(30)99(14)
C3170(30)-2180(40)-2240(40)98(16)
C16-70(30)-7830(20)2230(30)79(10)
C30-2960(30)-3350(40)2390(40)118(17)
C222930(30)-6720(30)-2350(30)75(10)
C44130(30)-3000(30)1610(40)76(12)
C11-4110(30)-6910(40)-1600(40)114(16)
C63820(20)-3720(40)3380(30)79(12)
C12-3650(20)-6250(30)-3240(30)83(11)
C46-3300(30)-5180(30)3820(30)77(10)
C353280(50)-4870(40)-3950(40)140(20)
C25-180(30)-1340(40)2320(60)150(20)
C23270(30)-8600(30)-2270(30)89(13)
C43-3420(40)-7040(30)3000(30)128(17)
C383110(20)-2930(30)-2970(40)96(15)
C171110(30)-8940(30)380(30)97(12)
C1-1100(30)-1160(20)-290(40)107(17)
C27-1900(20)-7990(20)-260(30)57(8)
C192210(40)-2220(40)170(30)150(20)
C9-700(20)-3090(30)4610(30)88(13)
C15760(30)-6950(40)-4500(30)89(12)
C50-3040(40)-400(50)2130(50)130(20)
C392870(20)-9530(20)-2030(30)87(11)
C49-3730(40)40(40)2440(30)150(30)
C403900(30)-9930(30)-2450(40)132(18)
C28-2500(60)-8440(50)-290(60)240(60)
C202770(30)-1790(40)-140(30)81(9)
C29-2690(30)-4350(30)1610(30)67(9)
C212655(18)-5770(30)-1710(30)56(10)
C374170(50)-3080(40)-2580(80)450(70)
C24230(30)-9230(40)-3090(40)220(40)
C26160(60)-560(50)3020(70)360(70)
Li8-1480(30)-5570(40)-130(50)59(13)
Li21550(40)-4580(40)110(40)47(14)
Li4-380(40)-3920(40)1510(40)71(17)
Li6370(30)-6150(40)-1550(40)50(12)
Li7-100(40)-6550(40)-80(40)67(16)
Li1140(30)-3420(40)80(40)58(16)
Li31130(40)-4990(30)1750(30)53(13)
Li5-1100(40)-5040(40)-1710(60)100(30)
C44-4320(30)-7020(30)2950(40)114(15)
K4-1149(6)-5835(6)2081(6)61(2)
C52-3410(30)-11760(40)-4520(40)128(12)
C333370(40)1610(40)4380(40)158(15)
C53-4130(40)-11200(40)-4790(40)156(14)
C324020(40)1310(40)4980(40)160(15)
C51-2890(40)-10670(40)-3480(40)159(15)
C342850(30)680(40)3370(40)139(14)
C54-3500(40)-10110(40)-4520(40)132(13)
C313430(40)170(40)4610(40)177(16)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3166. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
K553(5)54(4)65(5)19(4)4(4)15(4)
K347(4)50(4)65(5)21(4)6(4)20(3)
K160(5)40(4)58(5)12(3)-8(4)2(3)
K646(4)48(4)63(5)16(4)-2(4)4(3)
K264(5)62(4)53(4)28(4)9(4)13(4)
Si245(5)46(5)70(6)25(5)-9(5)-1(4)
Si442(5)60(6)68(7)15(5)1(5)13(5)
Si566(6)61(6)45(6)23(5)-1(5)9(5)
Si354(6)61(6)57(6)18(5)11(5)14(5)
Si170(8)57(6)88(8)42(6)0(6)9(5)
Si681(7)51(6)57(6)24(5)14(5)24(5)
O460(14)50(11)52(12)22(9)7(10)17(10)
O222(9)41(11)60(13)5(10)-4(9)-5(8)
O18120(20)61(13)34(11)1(9)10(12)28(13)
O1650(14)90(20)240(30)90(20)17(17)41(14)
O346(12)55(12)37(10)10(9)5(9)8(10)
O551(12)39(11)59(15)16(10)-9(10)7(9)
O1580(20)88(17)97(18)52(14)14(15)-11(14)
O1778(15)73(17)100(20)43(15)57(14)45(13)
O1245(12)53(13)76(16)20(12)5(11)2(10)
O846(12)33(11)66(14)22(10)5(10)-2(9)
O930(11)57(12)90(16)37(12)7(11)9(10)
O1350(13)53(12)38(12)12(10)21(10)12(10)
O666(12)49(12)29(9)16(8)5(9)15(10)
O157(15)39(10)86(16)36(10)4(12)1(10)
O747(6)30(5)45(8)10(5)10(5)6(4)
O1153(12)15(8)35(10)-3(7)3(9)5(8)
O1047(13)81(17)83(17)34(14)1(12)13(12)
O1467(13)120(18)101(19)68(16)-41(12)-68(13)
O19280(40)55(16)73(12)-43(11)-42(17)78(19)
C4170(20)80(30)180(50)50(30)-40(20)8(18)
C48150(40)120(30)90(30)-10(20)-10(30)70(30)
C854(19)130(40)100(30)60(30)35(19)50(20)
C13210(40)61(17)40(18)28(15)-20(20)-20(20)
C547(18)68(18)100(30)48(18)9(17)14(14)
C1039(17)80(30)70(20)2(19)-1(15)11(17)
C4270(20)60(20)150(40)30(20)10(20)32(16)
C4780(30)90(30)80(30)30(20)-20(20)30(20)
C290(20)50(20)100(30)40(20)0(20)8(19)
C18120(40)150(40)190(50)120(40)-60(40)10(30)
C3670(30)150(50)180(40)-10(40)60(30)-10(30)
C45100(30)120(20)140(30)90(20)70(30)80(20)
C780(20)80(20)18(12)0(12)24(13)8(17)
C14110(30)61(19)100(30)30(20)-50(20)-3(19)
C3110(40)90(30)100(30)70(30)-30(30)-20(30)
C1690(30)52(16)90(20)21(14)41(18)18(16)
C3070(30)230(50)110(30)100(40)60(20)110(30)
C22110(30)49(17)48(18)11(14)-1(16)31(17)
C450(20)50(20)140(30)50(20)0(20)-2(18)
C1130(20)170(40)100(30)50(30)-20(20)-10(20)
C643(17)110(30)70(30)40(20)-17(17)2(18)
C1240(16)68(18)100(20)13(16)-28(15)7(14)
C4680(20)100(30)60(20)40(20)28(16)34(19)
C35180(60)70(20)140(40)20(20)30(40)10(30)
C2526(18)40(20)260(70)0(30)-40(30)-5(17)
C2370(20)70(20)70(20)-13(18)-17(17)33(17)
C43190(50)60(20)100(30)0(20)80(30)10(30)
C3829(13)90(30)160(40)60(30)12(16)0(14)
C17110(30)110(30)90(20)60(20)30(20)20(20)
C1140(30)24(12)180(40)55(19)80(30)39(16)
C2755(15)33(12)80(20)34(13)-4(14)-24(11)
C19220(50)120(40)40(20)20(20)-40(30)-60(40)
C940(20)90(20)100(30)15(18)6(18)19(17)
C1590(20)140(40)50(20)50(20)24(18)30(20)
C50140(40)140(50)110(50)40(40)0(30)100(40)
C3972(18)51(15)76(19)-20(14)1(14)22(13)
C49150(50)140(50)70(20)-30(30)-30(30)100(40)
C40150(30)70(20)220(50)80(30)120(30)40(20)
C28280(110)230(60)250(80)210(60)-90(70)-140(70)
C2074(19)110(20)70(20)63(19)-11(16)-26(18)
C2980(20)68(17)49(17)19(14)18(16)31(16)
C2113(11)90(30)90(20)60(20)2(13)-1(14)
C37280(70)80(30)700(130)20(50)-330(80)40(40)
C24160(40)140(30)120(30)-120(30)-100(30)130(30)
C26290(80)130(40)360(100)-90(50)-220(80)140(40)
Li80(20)20(20)120(40)10(20)10(20)2(17)
Li290(30)40(20)10(20)14(18)-10(20)10(20)
Li4110(40)40(20)40(20)15(18)-20(20)-40(20)
Li640(20)80(30)40(30)30(20)15(17)50(20)
Li790(40)60(30)80(30)60(30)20(30)40(30)
Li131(19)50(30)40(30)-20(20)17(19)-20(18)
Li3110(40)20(20)24(17)-4(15)30(20)20(20)
Li530(30)60(20)180(70)60(30)-10(40)-20(20)
C4460(20)110(30)180(40)60(20)80(20)18(19)
K459(5)61(5)62(5)28(4)18(4)11(4)
C5260(20)120(30)210(30)90(30)0(20)0(20)
C33230(40)50(30)150(40)30(30)-80(30)-10(20)
C53100(30)120(30)200(40)60(30)-20(30)-20(30)
C32180(40)130(40)100(30)10(30)0(30)-30(30)
C51200(40)90(30)160(30)50(30)-30(30)0(30)
C34150(30)140(40)130(30)70(30)40(30)20(30)
C54190(30)110(30)90(30)60(20)0(30)-10(20)
C31180(40)160(40)200(40)100(30)10(30)-60(30)

 

Table 4 Bond Lengths for 3166.
AtomAtomLength/Å AtomAtomLength/Å
K5O42.88(2) O17C431.49(5)
K5O182.73(3) O17K42.75(2)
K5O132.79(2) O12C271.34(3)
K5O12.87(2) O12Li81.84(5)
K5O112.70(2) O12Li71.98(6)
K5Li83.28(5) O12K42.71(2)
K5Li43.30(6) O8C191.32(5)
K5Li13.13(4) O8Li22.04(5)
K5Li53.32(7) O8Li11.90(4)
K3O22.86(2) O9C211.30(3)
K3O162.69(2) O9Li21.88(5)
K3O92.77(2) O9Li61.94(5)
K3O62.922(19) O13C291.29(4)
K3O102.70(2) O13Li81.98(5)
K3Li23.04(5) O13Li41.92(6)
K3Li63.26(4) O13K42.70(2)
K3Li73.06(6) O6Li71.96(5)
K3Li33.28(4) O6Li31.86(5)
K1O22.90(2) O6K42.83(2)
K1O32.80(2) O1Li11.96(6)
K1O82.72(2) O1Li51.93(4)
K1O112.77(2) O7Li82.01(5)
K1O142.64(2) O7Li22.08(6)
K1Li23.20(5) O7Li41.97(6)
K1Li43.16(5) O7Li62.18(5)
K1Li13.31(5) O7Li72.06(5)
K1Li33.31(4) O7Li12.04(6)
K6O42.89(2) O7Li32.70(5)
K6O52.82(2) O11C251.39(5)
K6O122.77(2) O11Li41.95(5)
K6O102.76(2) O11Li11.92(4)
K6O192.78(3) O10C231.30(4)
K6Li83.07(5) O10Li61.91(5)
K6Li63.10(5) O10Li71.92(6)
K6Li73.33(5) O14C341.57(5)
K6Li53.25(4) O14C311.22(5)
K2O52.95(2) O19C511.40(5)
K2O152.70(3) O19C541.18(4)
K2O82.80(2) C41C421.41(6)
K2O92.72(2) C41C401.59(6)
K2O12.93(2) C48C471.58(5)
K2Li23.37(5) C48C502.12(6)
K2Li63.20(5) C48C491.50(5)
K2Li13.17(4) C36C351.54(7)
K2Li53.30(5) C36C371.45(8)
Si2O21.606(19) C45C461.48(5)
Si2C51.90(3) C45C441.50(5)
Si2C41.87(3) C30C291.37(5)
Si2C61.94(4) C22C211.27(4)
Si4O41.58(2) C25C261.05(7)
Si4C101.84(4) C23C241.04(4)
Si4C111.79(5) C43C441.21(6)
Si4C121.77(4) C38C371.55(6)
Si5O51.60(2) C27C280.95(7)
Si5C131.85(4) C19C201.14(5)
Si5C141.94(4) C50C491.15(6)
Si5C151.87(4) C39C401.59(5)
Si3O31.60(2) Li8Li42.50(6)
Si3C81.95(4) Li8Li63.22(6)
Si3C71.79(3) Li8Li72.39(6)
Si3C91.86(3) Li8Li13.31(6)
Si1O11.58(2) Li8Li52.68(9)
Si1C21.92(4) Li8K43.25(6)
Si1C31.96(5) Li2Li43.31(8)
Si1C11.89(4) Li2Li62.53(6)
Si6O61.62(2) Li2Li73.17(7)
Si6C181.88(5) Li2Li12.59(7)
Si6C161.82(3) Li2Li32.66(6)
Si6C171.91(4) Li4Li73.24(7)
O4Li82.00(6) Li4Li12.51(6)
O4Li51.91(6) Li4Li32.68(8)
O2Li21.87(5) Li4K43.14(4)
O2Li31.89(5) Li6Li72.46(6)
O18C471.31(4) Li6Li13.34(6)
O18C501.51(6) Li6Li52.66(7)
O16C421.49(4) Li7Li32.65(7)
O16C391.48(4) Li7K43.17(5)
O3Li41.89(5) Li1Li52.66(7)
O3Li31.93(4) Li3K43.29(5)
O3K42.98(2) C52C531.40(6)
O5Li61.97(4) C52C511.53(6)
O5Li51.81(7) C33C321.37(6)
O15C351.48(6) C33C341.42(6)
O15C381.39(4) C53C541.48(6)
O17C461.40(4) C32C311.48(6)

 

Table 5 Bond Angles for 3166.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O4K5Li837.1(11) Li5Li8K668.5(17)
O4K5Li480.6(8) Li5Li8Li652.6(17)
O4K5Li178.3(9) Li5Li8Li151.4(16)
O4K5Li535.0(8) Li5Li8K4161(2)
O18K5O4136.8(7) K4Li8Li1111.7(17)
O18K5O13127.1(7) K3Li2K1128.9(16)
O18K5O1123.1(7) K3Li2K2116.7(15)
O18K5Li8157.3(10) K3Li2Li4112.7(17)
O18K5Li4138.2(10) K3Li2Li759.1(12)
O18K5Li1139.2(10) K1Li2K2113.1(15)
O18K5Li5146.5(13) K1Li2Li458.2(11)
O13K5O469.7(6) O2Li2K366.3(16)
O13K5O1108.5(6) O2Li2K163.7(14)
O13K5Li837.0(11) O2Li2K2156(2)
O13K5Li435.5(9) O2Li2O8114(2)
O13K5Li178.3(11) O2Li2O7113(3)
O13K5Li584.2(12) O2Li2Li490(2)
O1K5O469.5(6) O2Li2Li6133(3)
O1K5Li878.0(10) O2Li2Li791(2)
O1K5Li482.1(10) O2Li2Li1129(3)
O1K5Li137.8(11) O2Li2Li345.2(17)
O1K5Li535.3(8) O8Li2K3163(3)
O11K5O4108.3(6) O8Li2K157.5(12)
O11K5O18114.9(6) O8Li2K255.9(13)
O11K5O1369.4(6) O8Li2O797(3)
O11K5O171.5(6) O8Li2Li484(2)
O11K5Li877.8(9) O8Li2Li6113(2)
O11K5Li436.3(8) O8Li2Li7137(3)
O11K5Li137.6(9) O8Li2Li146.7(15)
O11K5Li585.1(11) O8Li2Li3123(2)
Li8K5Li444.6(11) O9Li2K363.4(15)
Li8K5Li547.9(14) O9Li2K1158(2)
Li1K5Li862.2(12) O9Li2K253.7(13)
Li1K5Li445.9(13) O9Li2O2120(3)
Li1K5Li548.6(12) O9Li2O8106(2)
Li5K5Li473.6(15) O9Li2O7105(2)
O2K3O668.8(5) O9Li2Li4139(2)
O2K3Li236.8(9) O9Li2Li649.7(14)
O2K3Li682.4(9) O9Li2Li789.7(19)
O2K3Li777.8(10) O9Li2Li1111(2)
O2K3Li334.9(9) O9Li2Li3131(2)
O16K3O2136.9(8) O7Li2K398.5(18)
O16K3O9129.0(9) O7Li2K191.6(19)
O16K3O6121.0(8) O7Li2K290.8(17)
O16K3Li2158.6(12) O7Li2Li434.2(13)
O16K3Li6137.8(11) O7Li2Li655.5(15)
O16K3Li7138.1(10) O7Li2Li739.6(14)
O16K3Li3143.0(11) O7Li2Li150.5(17)
O9K3O270.4(6) O7Li2Li368(2)
O9K3O6108.7(6) Li4Li2K2109.2(17)
O9K3Li237.4(10) Li6Li2K371.1(14)
O9K3Li636.4(10) Li6Li2K1146(2)
O9K3Li778.0(8) Li6Li2K263.9(14)
O9K3Li386.1(9) Li6Li2Li489.7(19)
O6K3Li278.3(11) Li6Li2Li749.5(16)
O6K3Li682.4(9) Li6Li2Li181.6(19)
O6K3Li738.1(9) Li6Li2Li3103(2)
O6K3Li334.3(9) Li7Li2K1112.1(19)
O10K3O2109.2(7) Li7Li2K2111.0(15)
O10K3O16113.7(9) Li7Li2Li460.0(15)
O10K3O970.1(7) Li1Li2K3148(2)
O10K3O671.8(7) Li1Li2K168.8(15)
O10K3Li279.6(10) Li1Li2K262.6(15)
O10K3Li635.8(10) Li1Li2Li448.6(16)
O10K3Li738.1(10) Li1Li2Li790.0(19)
O10K3Li386.8(10) Li1Li2Li3101(2)
Li2K3Li647.1(12) Li3Li2K370.0(14)
Li2K3Li349.6(12) Li3Li2K167.9(14)
Li6K3Li376.4(11) Li3Li2K2159(2)
Li7K3Li262.6(13) Li3Li2Li452.1(16)
Li7K3Li645.5(11) Li3Li2Li753.3(16)
Li7K3Li349.3(13) K5Li4Li2112.0(15)
O2K1Li235.2(10) K1Li4K5114.7(13)
O2K1Li477.2(11) K1Li4Li259.3(12)
O2K1Li180.7(9) K1Li4Li7111(2)
O2K1Li334.6(8) O3Li4K5153(3)
O3K1O270.0(6) O3Li4K161.2(14)
O3K1Li277.9(10) O3Li4O7115(3)
O3K1Li436.4(9) O3Li4O11112(2)
O3K1Li180.9(8) O3Li4Li8132(3)
O3K1Li335.7(9) O3Li4Li289(2)
O8K1O271.1(6) O3Li4Li793(2)
O8K1O3108.3(6) O3Li4Li1129(3)
O8K1O1167.9(6) O3Li4Li346.2(16)
O8K1Li239.3(10) O3Li4K467.4(14)
O8K1Li477.7(9) O13Li4K557.7(16)
O8K1Li135.1(7) O13Li4K1160(3)
O8K1Li386.4(7) O13Li4O3116(2)
O11K1O2107.4(5) O13Li4O7103(2)
O11K1O369.8(6) O13Li4O11108(3)
O11K1Li278.9(10) O13Li4Li851.3(15)
O11K1Li437.7(10) O13Li4Li2140(2)
O11K1Li135.4(7) O13Li4Li788.1(18)
O11K1Li385.8(10) O13Li4Li1115(2)
O14K1O2127.7(8) O13Li4Li3126(2)
O14K1O3136.9(7) O13Li4K458.8(13)
O14K1O8114.6(7) O7Li4K591.6(17)
O14K1O11123.2(7) O7Li4K195(2)
O14K1Li2141.4(11) O7Li4O11102(2)
O14K1Li4154.0(12) O7Li4Li851.9(15)
O14K1Li1135.4(10) O7Li4Li236.4(15)
O14K1Li3148.4(10) O7Li4Li737.3(14)
Li2K1Li146.8(12) O7Li4Li152.6(16)
Li2K1Li348.2(11) O7Li4Li369(2)
Li4K1Li262.6(13) O7Li4K496.3(17)
Li4K1Li145.6(10) O11Li4K554.8(14)
Li4K1Li348.9(13) O11Li4K160.2(13)
Li3K1Li175.2(12) O11Li4Li8116(2)
O4K6Li839.0(11) O11Li4Li289(2)
O4K6Li679.4(9) O11Li4Li7139(2)
O4K6Li781.2(9) O11Li4Li149.0(15)
O4K6Li535.7(12) O11Li4Li3127(3)
O5K6O468.6(6) O11Li4K4160(3)
O5K6Li878.3(10) Li8Li4K567.3(16)
O5K6Li638.4(9) Li8Li4K1146(2)
O5K6Li781.1(9) Li8Li4Li288.2(19)
O5K6Li533.7(13) Li8Li4Li747.1(16)
O12K6O470.9(6) Li8Li4Li183(2)
O12K6O5108.6(6) Li8Li4Li399(2)
O12K6O1068.4(7) Li8Li4K469.3(16)
O12K6Li836.3(11) Li7Li4K5112.1(14)
O12K6Li678.6(9) Li7Li4Li258.0(16)
O12K6Li736.4(11) Li1Li4K563.6(15)
O12K6Li585.7(14) Li1Li4K170.3(15)
O10K6O4108.9(7) Li1Li4Li250.6(17)
O10K6O572.7(7) Li1Li4Li789.9(19)
O10K6Li876.7(10) Li1Li4Li3102(2)
O10K6Li637.5(9) Li1Li4K4148(2)
O10K6Li735.1(11) Li3Li4K5160.5(19)
O10K6Li585.7(12) Li3Li4K168.3(16)
O19K6O4122.7(8) Li3Li4Li251.5(16)
O19K6O5141.5(9) Li3Li4Li752.2(15)
O19K6O12109.9(8) Li3Li4K468.4(14)
O19K6O10124.9(8) K4Li4K5116.2(16)
O19K6Li8135.7(11) K4Li4K1127.3(17)
O19K6Li6157.6(10) K4Li4Li2110.9(18)
O19K6Li7134.4(10) K4Li4Li759.6(12)
O19K6Li5148.8(13) K3Li6Li1109.9(15)
Li8K6Li662.8(11) K6Li6K3116.9(15)
Li8K6Li743.7(12) K6Li6K2126.8(12)
Li8K6Li550.0(17) K6Li6Li858.1(11)
Li6K6Li744.7(12) K6Li6Li1111.1(12)
Li6K6Li549.3(13) K2Li6K3115.3(13)
Li5K6Li773.6(15) K2Li6Li157.9(11)
O5K2Li280.2(9) O5Li6K3160(2)
O5K2Li637.0(8) O5Li6K663.1(13)
O5K2Li176.7(8) O5Li6K264.4(14)
O5K2Li533.0(11) O5Li6O9116(3)
O15K2O5129.7(8) O5Li6O7110.2(19)
O15K2O8116.4(8) O5Li6Li888.5(17)
O15K2O9100.7(8) O5Li6Li2131(3)
O15K2O1151.0(8) O5Li6Li7130(2)
O15K2Li2120.9(12) O5Li6Li187.4(18)
O15K2Li6130.0(9) O5Li6Li542.9(19)
O15K2Li1152.1(9) O9Li6K357.8(11)
O15K2Li5159.4(14) O9Li6K6164(2)
O8K2O5106.8(6) O9Li6K257.9(14)
O8K2O169.8(7) O9Li6O799(2)
O8K2Li237.2(9) O9Li6Li8137(2)
O8K2Li678.6(9) O9Li6Li247.6(17)
O8K2Li136.5(9) O9Li6Li7113(2)
O8K2Li584.1(13) O9Li6Li184.6(18)
O9K2O571.3(6) O9Li6Li5123(2)
O9K2O868.9(7) O7Li6K390.1(15)
O9K2O1107.6(7) O7Li6K696.0(15)
O9K2Li233.8(10) O7Li6K293.7(17)
O9K2Li637.1(7) O7Li6Li838.0(13)
O9K2Li177.5(11) O7Li6Li251.8(18)
O9K2Li584.0(12) O7Li6Li752.2(16)
O1K2O567.5(6) O7Li6Li136.3(13)
O1K2Li282.0(11) O7Li6Li567(2)
O1K2Li678.4(8) O10Li6K355.9(11)
O1K2Li137.2(10) O10Li6K661.6(14)
O1K2Li535.3(10) O10Li6K2161(2)
Li6K2Li245.1(11) O10Li6O5117(3)
Li6K2Li548.1(12) O10Li6O9109.3(19)
Li1K2Li246.5(14) O10Li6O7102(2)
Li1K2Li663.2(11) O10Li6Li886.0(19)
Li1K2Li548.5(14) O10Li6Li2112(2)
Li5K2Li273.6(16) O10Li6Li750.1(17)
O2Si2C5113.4(14) O10Li6Li1139(2)
O2Si2C4111.6(14) O10Li6Li5127(2)
O2Si2C6114.2(13) Li8Li6K3108.9(16)
C5Si2C6105.3(17) Li8Li6K2112.7(15)
C4Si2C5104.6(18) Li8Li6Li160.7(12)
C4Si2C6106.9(17) Li2Li6K361.8(14)
O4Si4C10113.5(13) Li2Li6K6147(2)
O4Si4C11110.8(15) Li2Li6K271.1(16)
O4Si4C12108.7(14) Li2Li6Li889.7(19)
C10Si4C11109(2) Li2Li6Li150.0(17)
C12Si4C10105.4(17) Li2Li6Li5101(2)
C12Si4C11109.4(19) Li7Li6K362.9(15)
O5Si5C13107.7(14) Li7Li6K672.5(17)
O5Si5C14114.2(16) Li7Li6K2145(2)
O5Si5C15112.5(14) Li7Li6Li847.6(16)
C13Si5C14104.1(15) Li7Li6Li279(2)
C13Si5C15110.2(19) Li7Li6Li188.5(18)
C15Si5C14107.8(19) Li7Li6Li5101(2)
O3Si3C8114.7(15) Li5Li6K3157(2)
O3Si3C7113.5(13) Li5Li6K668.2(12)
O3Si3C9113.8(15) Li5Li6K267.9(15)
C7Si3C8105.8(19) Li5Li6Li853.2(19)
C7Si3C9105.8(15) Li5Li6Li151.1(17)
C9Si3C8102.1(18) K3Li7K6116.2(16)
O1Si1C2112.4(14) K3Li7Li258.3(14)
O1Si1C3111.7(17) K3Li7Li4113.9(19)
O1Si1C1109.4(17) K3Li7K4127.9(14)
C2Si1C3105.6(19) O12Li7K3159(2)
C1Si1C2109(2) O12Li7K656.2(13)
C1Si1C3108.6(17) O12Li7O7102(2)
O6Si6C18112.3(16) O12Li7Li848.7(17)
O6Si6C16111.8(15) O12Li7Li2142(2)
O6Si6C17118.0(14) O12Li7Li487(2)
C18Si6C1798(2) O12Li7Li6114(2)
C16Si6C18111(2) O12Li7Li3125(3)
C16Si6C17105.0(15) O12Li7K458.1(15)
K6O4K5155.0(8) O6Li7K367.0(16)
Si4O4K5102.6(10) O6Li7K6154(2)
Si4O4K6101.2(9) O6Li7O12111(3)
Si4O4Li8135.7(18) O6Li7O7113(3)
Si4O4Li5138(3) O6Li7Li8129(3)
Li8O4K582.3(15) O6Li7Li291(2)
Li8O4K675.4(15) O6Li7Li489(2)
Li5O4K585.0(18) O6Li7Li6135(3)
Li5O4K682.6(17) O6Li7Li344.6(15)
Li5O4Li886(3) O6Li7K461.6(15)
K3O2K1155.5(8) O7Li7K398(2)
Si2O2K3103.1(10) O7Li7K692.1(15)
Si2O2K199.8(9) O7Li7Li853.1(16)
Si2O2Li2133(2) O7Li7Li240.2(16)
Si2O2Li3136.3(19) O7Li7Li435.5(14)
Li2O2K376.9(16) O7Li7Li657.0(16)
Li2O2K181.1(17) O7Li7Li368.5(18)
Li3O2K385.0(12) O7Li7K494(2)
Li3O2K184.4(14) O10Li7K360.7(16)
Li3O2Li290(2) O10Li7K656.1(14)
C47O18K5133(2) O10Li7O12106(3)
C47O18C50108(3) O10Li7O6117(3)
C50O18K5119(2) O10Li7O7107(2)
C42O16K3135(2) O10Li7Li8114(2)
C39O16K3112.5(18) O10Li7Li289(2)
C39O16C42110(3) O10Li7Li4142(2)
K1O3K4155.9(7) O10Li7Li650.0(17)
Si3O3K1105.6(10) O10Li7Li3129(3)
Si3O3Li4143(2) O10Li7K4157(2)
Si3O3Li3127.1(18) Li8Li7K3150(2)
Si3O3K498.3(10) Li8Li7K662.4(16)
Li4O3K182.4(15) Li8Li7Li293.2(19)
Li4O3K476.6(14) Li8Li7Li449.9(17)
Li3O3K186.7(15) Li8Li7Li3103(2)
Li3O3Li489(2) Li8Li7K470(2)
Li3O3K481.2(16) Li2Li7K6112.1(15)
K6O5K2155.3(9) Li2Li7Li462.0(16)
Si5O5K6105.3(10) Li2Li7K4113.6(18)
Si5O5K297.3(9) Li4Li7K6110.3(15)
Si5O5Li6134.4(18) Li6Li7K371.5(16)
Si5O5Li5136(3) Li6Li7K662.8(14)
Li6O5K678.5(16) Li6Li7Li883.1(19)
Li6O5K278.6(16) Li6Li7Li251.4(17)
Li5O5K686.2(16) Li6Li7Li492.4(18)
Li5O5K284.4(14) Li6Li7Li3105(2)
Li5O5Li689(3) Li6Li7K4149(2)
C35O15K2133(2) Li3Li7K369.7(16)
C38O15K2117(2) Li3Li7K6160.5(17)
C38O15C35110(3) Li3Li7Li253.5(15)
C46O17C4398(3) Li3Li7Li453.0(16)
C46O17K4131(2) Li3Li7K468.2(15)
C43O17K4130(2) K4Li7K6113.8(17)
C27O12K696.1(17) K4Li7Li458.6(12)
C27O12Li8166(2) K5Li1K1115.2(12)
C27O12Li7117(2) K5Li1K2127.6(17)
C27O12K495.5(18) K5Li1Li861.1(10)
Li8O12K680.7(19) K5Li1Li6112.1(13)
Li8O12Li777.6(19) K1Li1Li6110.9(17)
Li8O12K489.0(19) K2Li1K1115.7(11)
Li7O12K687.4(16) K2Li1Li8110.9(15)
Li7O12K483.6(16) K2Li1Li658.9(11)
K4O12K6167.6(9) O8Li1K5159(2)
K1O8K2168.1(8) O8Li1K155.2(13)
C19O8K1102.3(19) O8Li1K261.0(12)
C19O8K289.4(19) O8Li1O1116(2)
C19O8Li2139(3) O8Li1O7103(3)
C19O8Li1138(3) O8Li1O11107(2)
Li2O8K183.2(15) O8Li1Li8138(3)
Li2O8K286.9(14) O8Li1Li251.4(17)
Li1O8K189.7(16) O8Li1Li4114(3)
Li1O8K282.4(15) O8Li1Li688.9(17)
Li1O8Li282(2) O8Li1Li5127(2)
K2O9K3168.3(9) O1Li1K563.7(13)
C21O9K388.1(18) O1Li1K1156(2)
C21O9K2103.5(19) O1Li1K264.9(14)
C21O9Li2130(2) O1Li1O7115(2)
C21O9Li6145(2) O1Li1Li891.1(17)
Li2O9K379.2(17) O1Li1Li2131(2)
Li2O9K292.5(17) O1Li1Li4130(2)
Li2O9Li683(2) O1Li1Li690.4(16)
Li6O9K385.9(15) O1Li1Li546.2(17)
Li6O9K285.0(15) O7Li1K595.1(14)
C29O13K587.8(18) O7Li1K189(2)
C29O13Li8126(2) O7Li1K297.4(16)
C29O13Li4153(2) O7Li1Li834.9(13)
C29O13K4103.8(17) O7Li1Li251.7(18)
Li8O13K585.0(17) O7Li1Li449.9(17)
Li8O13K486.4(17) O7Li1Li639.2(13)
Li4O13K586.8(16) O7Li1Li568.8(18)
Li4O13Li880(2) O11Li1K558.8(11)
Li4O13K483.8(16) O11Li1K156.8(14)
K4O13K5168.2(8) O11Li1K2161(2)
Si6O6K397.6(10) O11Li1O1114(2)
Si6O6Li7136.0(17) O11Li1O7100(2)
Si6O6Li3135.1(18) O11Li1Li888.2(16)
Si6O6K4106.3(9) O11Li1Li2115(3)
Li7O6K374.9(18) O11Li1Li450.2(16)
Li7O6K480.8(18) O11Li1Li6139(2)
Li3O6K383.5(13) O11Li1Li5126(2)
Li3O6Li788(2) Li8Li1K1109.9(18)
Li3O6K486.6(16) Li8Li1Li657.8(13)
K4O6K3154.1(8) Li2Li1K5146(2)
K5O1K2154.3(8) Li2Li1K164.4(15)
Si1O1K5100.5(12) Li2Li1K270.9(14)
Si1O1K2103.9(11) Li2Li1Li886.5(19)
Si1O1Li1137.4(18) Li2Li1Li648.4(13)
Si1O1Li5136(3) Li2Li1Li599(2)
Li1O1K578.5(12) Li4Li1K570.5(16)
Li1O1K278.0(13) Li4Li1K164.1(15)
Li5O1K585(2) Li4Li1K2147(2)
Li5O1K282.9(19) Li4Li1Li848.4(15)
Li5O1Li186(3) Li4Li1Li281(2)
Li8O7Li2171(3) Li4Li1Li689(2)
Li8O7Li6100(2) Li4Li1Li5100(2)
Li8O7Li772(2) Li5Li1K569.4(16)
Li8O7Li1110(2) Li5Li1K1158(2)
Li8O7Li3113(2) Li5Li1K268.4(17)
Li2O7Li672.7(19) Li5Li1Li851.9(18)
Li2O7Li177.8(19) Li5Li1Li651.0(16)
Li2O7Li366.3(18) K1Li3K3117.4(13)
Li4O7Li878(2) K1Li3K4117.6(13)
Li4O7Li2109(2) O2Li3K360.1(11)
Li4O7Li6178(3) O2Li3K161.0(13)
Li4O7Li7107(2) O2Li3O3118(2)
Li4O7Li177.4(19) O2Li3O6121(2)
Li4O7Li368.1(19) O2Li3O790.2(16)
Li6O7Li3112.0(16) O2Li3Li244.6(15)
Li7O7Li2100(2) O2Li3Li4111(2)
Li7O7Li671(2) O2Li3Li7108.9(19)
Li7O7Li1175(3) O2Li3K4170(2)
Li7O7Li366.3(17) O3Li3K3169(2)
Li1O7Li6105(2) O3Li3K157.6(12)
Li1O7Li3116.1(19) O3Li3O6121(3)
K5O11K1168.3(7) O3Li3O787.8(19)
C25O11K5106.5(18) O3Li3Li2110(2)
C25O11K185.1(18) O3Li3Li445.0(15)
C25O11Li4134(3) O3Li3Li7112(3)
C25O11Li1143(3) O3Li3K463.3(14)
Li4O11K588.8(16) O6Li3K362.1(11)
Li4O11K182.1(17) O6Li3K1172(2)
Li1O11K583.6(14) O6Li3O792.5(18)
Li1O11K187.8(15) O6Li3Li2111.4(18)
Li1O11Li481(2) O6Li3Li4110(2)
K3O10K6166.5(10) O6Li3Li747.5(14)
C23O10K3102.4(19) O6Li3K458.9(14)
C23O10K690.9(19) O7Li3K381.5(10)
C23O10Li6131(3) O7Li3K179.5(12)
C23O10Li7148(3) O7Li3Li245.7(14)
Li6O10K388.3(14) O7Li3Li443.0(13)
Li6O10K681.0(13) O7Li3Li745.2(12)
Li7O10K381.2(18) O7Li3K480.2(14)
Li7O10K688.7(17) Li2Li3K360.4(13)
Li7O10Li679.9(19) Li2Li3K163.8(13)
C34O14K1117(2) Li2Li3Li476.4(19)
C31O14K1134(3) Li2Li3Li773.3(17)
C31O14C34107(3) Li2Li3K4126(2)
C51O19K6117(2) Li4Li3K3124.4(16)
C54O19K6124(3) Li4Li3K162.8(12)
C54O19C51107(3) Li4Li3Li774.8(18)
C42C41C40106(3) Li4Li3K462.3(14)
C47C48C5074(3) Li7Li3K361.1(14)
C49C48C47104(3) Li7Li3K1124.6(17)
C49C48C5031(2) Li7Li3K463.3(16)
C41C42O16109(3) K4Li3K3116.8(13)
O18C47C48103(3) K5Li5K2117.2(13)
C37C36C35104(5) K6Li5K5118.1(17)
C46C45C44106(3) K6Li5K2118.6(18)
O17C46C45107(3) O4Li5K559.9(18)
O15C35C3698(3) O4Li5K661.7(12)
C26C25O11156(5) O4Li5K2174(4)
C24C23O10152(6) O4Li5O1117(3)
C44C43O17117(4) O4Li5Li848.1(19)
O15C38C3791(3) O4Li5Li6113(3)
C28C27O12141(6) O4Li5Li1112(3)
C20C19O8161(5) O5Li5K5175(4)
O18C50C4875(2) O5Li5K660.1(13)
C49C50O18113(4) O5Li5K262.6(16)
C49C50C4843(3) O5Li5O4120(2)
O16C39C40102(3) O5Li5O1122(3)
C50C49C48106(4) O5Li5Li8111(3)
C39C40C41101(3) O5Li5Li647.7(18)
O13C29C30125(3) O5Li5Li1115(3)
C22C21O9130(3) O1Li5K559.3(18)
C36C37C38101(5) O1Li5K6175(4)
K5Li8Li156.7(11) O1Li5K261.8(14)
K5Li8K4113.6(15) O1Li5Li8114(3)
K6Li8K5125.1(19) O1Li5Li6115(3)
K6Li8Li659.1(12) O1Li5Li147.3(18)
K6Li8Li1112.8(17) Li8Li5K565.3(18)
K6Li8K4119.0(15) Li8Li5K661.4(13)
O4Li8K560.6(14) Li8Li5K2126(2)
O4Li8K665.6(15) Li8Li5Li674(2)
O4Li8O13109(2) Li8Li5Li177(3)
O4Li8O7114(3) Li6Li5K5128(3)
O4Li8Li4126(3) Li6Li5K662.4(15)
O4Li8Li692(2) Li6Li5K263.9(16)
O4Li8Li7135(3) Li1Li5K562.0(16)
O4Li8Li188(2) Li1Li5K6128(3)
O4Li8Li545.5(18) Li1Li5K263.1(12)
O4Li8K4153(2) Li1Li5Li678(2)
O12Li8K5157(2) C43C44C45101(4)
O12Li8K662.9(16) O3K4Li880.5(8)
O12Li8O4118(3) O3K4Li436.0(9)
O12Li8O13107(3) O3K4Li777.2(10)
O12Li8O7108(2) O3K4Li335.5(8)
O12Li8Li4116(3) O17K4O3128.2(7)
O12Li8Li691(2) O17K4O6151.6(7)
O12Li8Li753.7(18) O17K4Li8121.4(10)
O12Li8Li1144(2) O17K4Li4129.9(13)
O12Li8Li5130(3) O17K4Li7152.2(12)
O12Li8K456.5(17) O17K4Li3159.3(9)
O13Li8K558.0(13) O12K4O3107.8(6)
O13Li8K6159(2) O12K4O17114.6(8)
O13Li8O799(2) O12K4O671.6(6)
O13Li8Li449.0(18) O12K4Li834.5(10)
O13Li8Li6141(2) O12K4Li478.2(9)
O13Li8Li7116(3) O12K4Li738.3(10)
O13Li8Li186.2(17) O12K4Li386.0(8)
O13Li8Li5123(2) O13K4O369.3(6)
O13Li8K456.0(15) O13K4O1799.2(7)
O7Li8K591.3(17) O13K4O1269.2(7)
O7Li8K6100.9(19) O13K4O6108.6(6)
O7Li8Li450.4(18) O13K4Li837.6(9)
O7Li8Li641.9(14) O13K4Li437.4(12)
O7Li8Li754.8(18) O13K4Li778.0(8)
O7Li8Li135.5(14) O13K4Li385.8(9)
O7Li8Li569(2) O6K4O369.5(6)
O7Li8K492(2) O6K4Li880.2(9)
Li4Li8K568.0(17) O6K4Li478.0(12)
Li4Li8K6151(2) O6K4Li737.6(9)
Li4Li8Li692(2) O6K4Li334.4(8)
Li4Li8Li148.8(15) Li8K4Li374.2(10)
Li4Li8Li5100(2) Li4K4Li846.1(11)
Li4Li8K464.6(16) Li4K4Li761.9(12)
Li6Li8K5111.5(17) Li4K4Li349.2(14)
Li6Li8Li161.5(14) Li7K4Li843.8(11)
Li6Li8K4114.1(16) Li7K4Li348.5(11)
Li7Li8K5145(2) C53C52C5194(4)
Li7Li8K673.9(17) C32C33C34115(4)
Li7Li8Li483(2) C52C53C54102(4)
Li7Li8Li649.3(16) C33C32C3196(4)
Li7Li8Li190.2(19) O19C51C52108(3)
Li7Li8Li5102(2) C33C34O1497(3)
Li7Li8K466.4(18) O19C54C53105(4)
Li5Li8K566.8(16) O14C31C32115(4)

 

Table 6 Torsion Angles for 3166.
ABCDAngle/˚ ABCDAngle/˚
K5O18C47C48172(3) C7Si3O3Li3101(3)
K5O18C50C48-174(2) C7Si3O3K4-173.3(15)
K5O18C50C49-155(5) C14Si5O5K66.1(17)
K5O13C29C30-70(3) C14Si5O5K2176.1(13)
K5O11C25C26177(23) C14Si5O5Li695(3)
K3O2Li2K1169.1(8) C14Si5O5Li5-95(3)
K3O2Li2K2-103(6) C3Si1O1K5163.3(15)
K3O2Li2O8-161(3) C3Si1O1K2-8.2(17)
K3O2Li2O9-35(2) C3Si1O1Li179(3)
K3O2Li2O789(2) C3Si1O1Li5-102(4)
K3O2Li2Li4115.1(12) C16Si6O6K3-165.0(12)
K3O2Li2Li626(3) C16Si6O6Li7-89(3)
K3O2Li2Li755.1(13) C16Si6O6Li3107(3)
K3O2Li2Li1146(3) C16Si6O6K44.8(15)
K3O2Li2Li384.8(13) C4Si2O2K3120.0(16)
K3O2Li3K1-157.9(8) C4Si2O2K1-51.3(18)
K3O2Li3O3-168(2) C4Si2O2Li236(3)
K3O2Li3O613(2) C4Si2O2Li3-143(3)
K3O2Li3O7-80.0(10) C11Si4O4K5-119.4(17)
K3O2Li3Li2-76.8(16) C11Si4O4K652.9(19)
K3O2Li3Li4-118.6(16) C11Si4O4Li8-28(3)
K3O2Li3Li7-38.1(17) C11Si4O4Li5144(3)
K3O16C42C41-160(3) C6Si2O2K3-118.6(15)
K3O16C39C40144(2) C6Si2O2K170.1(17)
K3O9C21C2260(4) C6Si2O2Li2157(3)
K3O9Li2K1130(7) C6Si2O2Li3-22(3)
K3O9Li2K2-171.8(7) C12Si4O4K5120.3(14)
K3O9Li2O236(3) C12Si4O4K6-67.4(15)
K3O9Li2O8166(2) C12Si4O4Li8-148(3)
K3O9Li2O7-92(2) C12Si4O4Li524(3)
K3O9Li2Li4-95(3) C46O17C43C4434(5)
K3O9Li2Li6-87.2(15) C46C45C44C4318(5)
K3O9Li2Li7-55.1(11) C35O15C38C37-54(6)
K3O9Li2Li1-145(2) C35C36C37C38-39(8)
K3O9Li2Li3-18(3) C43O17C46C45-17(4)
K3O6Li3O2-13(2) C38O15C35C3632(5)
K3O6Li3O3168(3) C17Si6O6K3-43.1(18)
K3O6Li3O779.0(11) C17Si6O6Li733(4)
K3O6Li3Li236(2) C17Si6O6Li3-131(3)
K3O6Li3Li4119.1(16) C17Si6O6K4126.6(16)
K3O6Li3Li775.0(17) C1Si1O1K543.0(17)
K3O6Li3K4156.0(7) C1Si1O1K2-128.6(16)
K3O10C23C24-119(10) C1Si1O1Li1-41(3)
K1O2Li2K3-169.1(8) C1Si1O1Li5137(4)
K1O2Li2K288(6) C27O12Li8K538(16)
K1O2Li2O830(2) C27O12Li8K6-79(11)
K1O2Li2O9155(3) C27O12Li8O4-41(12)
K1O2Li2O7-80(2) C27O12Li8O1382(12)
K1O2Li2Li4-54.1(10) C27O12Li8O7-172(10)
K1O2Li2Li6-143(4) C27O12Li8Li4134(10)
K1O2Li2Li7-114.0(15) C27O12Li8Li6-133(11)
K1O2Li2Li1-23(3) C27O12Li8Li7-168(11)
K1O2Li2Li3-84.3(13) C27O12Li8Li1-171(9)
K1O2Li3K3157.9(8) C27O12Li8Li5-94(11)
K1O2Li3O3-10(2) C27O12Li8K4108(11)
K1O2Li3O6171(3) C9Si3O3K1124.8(15)
K1O2Li3O777.9(10) C9Si3O3Li427(4)
K1O2Li3Li281.0(17) C9Si3O3Li3-137(3)
K1O2Li3Li439.3(16) C9Si3O3K4-52.2(17)
K1O2Li3Li7119.8(18) C15Si5O5K6-117.2(16)
K1O3Li4K5-88(4) C15Si5O5K252.8(17)
K1O3Li4O13-158(3) C15Si5O5Li6-28(3)
K1O3Li4O782(2) C15Si5O5Li5142(3)
K1O3Li4O11-34(3) C50O18C47C48-8(5)
K1O3Li4Li8142(4) C50C48C47O186(3)
K1O3Li4Li254.9(11) C39O16C42C411(5)
K1O3Li4Li7112.8(15) C49C48C47O18-5(6)
K1O3Li4Li121(3) C40C41C42O1620(5)
K1O3Li4Li386.8(16) C21O9Li2K3-78(3)
K1O3Li4K4168.0(9) C21O9Li2K151(8)
K1O8C19C20154(17) C21O9Li2K2110(3)
K1O11C25C26-2(24) C21O9Li2O2-42(5)
K1O14C34C33165(3) C21O9Li2O888(4)
K1O14C31C32178(3) C21O9Li2O7-170(3)
K6O5Li5K2157.2(8) C21O9Li2Li4-173(3)
K6O5Li5O4-16(4) C21O9Li2Li6-165(3)
K6O5Li5O1175(4) C21O9Li2Li7-133(3)
K6O5Li5Li836(2) C21O9Li2Li1137(3)
K6O5Li5Li678.5(16) C21O9Li2Li3-97(4)
K6O5Li5Li1121(3) C37C36C35O158(7)
K6O12C27C28-94(8) Li8O12C27C28-17(16)
K6O12Li8K5117(7) Li8O13C29C30-152(3)
K6O12Li8O438(2) Li2O2Li3K376.8(16)
K6O12Li8O13161(2) Li2O2Li3K1-81.0(17)
K6O12Li8O7-93(2) Li2O2Li3O3-91(3)
K6O12Li8Li4-147(3) Li2O2Li3O690(3)
K6O12Li8Li6-54.3(12) Li2O2Li3O7-3.2(19)
K6O12Li8Li7-89.3(17) Li2O2Li3Li4-42(2)
K6O12Li8Li1-92(4) Li2O2Li3Li739(2)
K6O12Li8Li5-16(3) Li2O8C19C2060(18)
K6O12Li8K4-173.0(8) Li2O9C21C22134(4)
K6O10C23C2459(10) Li4O13C29C309(8)
K6O19C51C52-154(3) Li4O11C25C2672(24)
K6O19C54C53177(3) Li6O5Li5K6-78.5(16)
K2O5Li5K6-157.2(8) Li6O5Li5K278.6(16)
K2O5Li5O4-174(4) Li6O5Li5O4-95(4)
K2O5Li5O117(4) Li6O5Li5O196(4)
K2O5Li5Li8-121(2) Li6O5Li5Li8-42(3)
K2O5Li5Li6-78.6(16) Li6O5Li5Li142(3)
K2O5Li5Li1-36(3) Li6O9C21C22-20(7)
K2O15C35C36-143(3) Li6O9Li2K387.2(15)
K2O15C38C37122(4) Li6O9Li2K1-143(7)
K2O8C19C20-25(18) Li6O9Li2K2-84.6(15)
K2O9C21C22-120(4) Li6O9Li2O2124(3)
K2O9Li2K3171.8(7) Li6O9Li2O8-107(3)
K2O9Li2K1-59(7) Li6O9Li2O7-5(2)
K2O9Li2O2-152(3) Li6O9Li2Li4-8(3)
K2O9Li2O8-22(2) Li6O9Li2Li732.1(18)
K2O9Li2O780(2) Li6O9Li2Li1-58(2)
K2O9Li2Li477(3) Li6O9Li2Li369(4)
K2O9Li2Li684.6(15) Li6O10C23C24-20(12)
K2O9Li2Li7116.7(12) Li7O12C27C28176(8)
K2O9Li2Li127(2) Li7O12Li8K5-154(7)
K2O9Li2Li3153(3) Li7O12Li8K689.3(17)
Si2O2Li2K396(2) Li7O12Li8O4127(3)
Si2O2Li2K1-95(2) Li7O12Li8O13-110(3)
Si2O2Li2K2-7(7) Li7O12Li8O7-4(3)
Si2O2Li2O8-65(4) Li7O12Li8Li4-58(3)
Si2O2Li2O960(4) Li7O12Li8Li635.0(18)
Si2O2Li2O7-174.9(17) Li7O12Li8Li1-3(4)
Si2O2Li2Li4-149(2) Li7O12Li8Li574(3)
Si2O2Li2Li6121(3) Li7O12Li8K4-83.7(16)
Si2O2Li2Li7151(2) Li7O6Li3K3-75.0(17)
Si2O2Li2Li1-118(3) Li7O6Li3O2-88(3)
Si2O2Li2Li3-179(3) Li7O6Li3O393(3)
Si2O2Li3K3-104(2) Li7O6Li3O74(2)
Si2O2Li3K198(2) Li7O6Li3Li2-39(3)
Si2O2Li3O389(3) Li7O6Li3Li444(2)
Si2O2Li3O6-91(3) Li7O6Li3K480.9(18)
Si2O2Li3O7176.2(19) Li7O10C23C24148(9)
Si2O2Li3Li2179(3) Li1O8C19C20-103(18)
Si2O2Li3Li4138(2) Li1O11C25C26-81(25)
Si2O2Li3Li7-142(2) Li3O2Li2K3-84.8(13)
Si5O5Li5K6108(2) Li3O2Li2K184.3(13)
Si5O5Li5K2-95(2) Li3O2Li2K2173(6)
Si5O5Li5O492(4) Li3O2Li2O8114(3)
Si5O5Li5O1-77(5) Li3O2Li2O9-120(3)
Si5O5Li5Li8144(2) Li3O2Li2O74(3)
Si5O5Li5Li6-173(3) Li3O2Li2Li430.3(17)
Si5O5Li5Li1-131(3) Li3O2Li2Li6-59(4)
Si3O3Li4K518(7) Li3O2Li2Li7-29.7(19)
Si3O3Li4K1106(3) Li3O2Li2Li161(3)
Si3O3Li4O13-52(4) Li3O3Li4K5-175(5)
Si3O3Li4O7-173(2) Li3O3Li4K1-86.8(16)
Si3O3Li4O1172(4) Li3O3Li4O13115(3)
Si3O3Li4Li8-112(4) Li3O3Li4O7-5(3)
Si3O3Li4Li2161(3) Li3O3Li4O11-121(3)
Si3O3Li4Li7-141(3) Li3O3Li4Li855(4)
Si3O3Li4Li1127(4) Li3O3Li4Li2-31.9(18)
Si3O3Li4Li3-167(3) Li3O3Li4Li726(2)
Si3O3Li4K4-86(3) Li3O3Li4Li1-66(3)
Si6O6Li3K394(2) Li3O3Li4K481.2(16)
Si6O6Li3O281(3) C44C45C46O172(4)
Si6O6Li3O3-98(3) K4O3Li4K5104(5)
Si6O6Li3O7173.2(17) K4O3Li4K1-168.0(9)
Si6O6Li3Li2130(2) K4O3Li4O1334(2)
Si6O6Li3Li4-147(2) K4O3Li4O7-87(2)
Si6O6Li3Li7169(3) K4O3Li4O11158(3)
Si6O6Li3K4-110(2) K4O3Li4Li8-26(3)
O18C50C49C48-28(7) K4O3Li4Li2-113.1(13)
O16C39C40C4131(4) K4O3Li4Li7-55.2(13)
O15C38C37C3656(6) K4O3Li4Li1-147(3)
O17C43C44C45-33(5) K4O3Li4Li3-81.2(16)
C8Si3O3K1-118.1(14) K4O17C46C45152(2)
C8Si3O3Li4144(3) K4O17C43C44-135(4)
C8Si3O3Li3-20(3) K4O12C27C2890(8)
C8Si3O3K464.9(15) K4O12Li8K5-70(7)
C13Si5O5K6121.2(15) K4O12Li8K6173.0(8)
C13Si5O5K2-68.8(15) K4O12Li8O4-149(2)
C13Si5O5Li6-150(3) K4O12Li8O13-26(2)
C13Si5O5Li521(3) K4O12Li8O780(2)
C5Si2O2K32.1(16) K4O12Li8Li426(3)
C5Si2O2K1-169.2(13) K4O12Li8Li6118.7(13)
C5Si2O2Li2-82(3) K4O12Li8Li783.7(16)
C5Si2O2Li399(3) K4O12Li8Li181(4)
C10Si4O4K53.4(18) K4O12Li8Li5157(3)
C10Si4O4K6175.7(15) K4O13C29C30112(3)
C10Si4O4Li895(3) K4O6Li3K3-156.0(7)
C10Si4O4Li5-93(3) K4O6Li3O2-169(2)
C42O16C39C40-21(4) K4O6Li3O312(2)
C42C41C40C39-32(4) K4O6Li3O7-77.0(12)
C47O18C50C486(4) K4O6Li3Li2-120(2)
C47O18C50C4925(7) K4O6Li3Li4-36.8(16)
C47C48C49C5021(7) K4O6Li3Li7-80.9(18)
C2Si1O1K5-78.1(18) C52C53C54O19-54(5)
C2Si1O1K2110.3(17) C33C32C31O1428(6)
C2Si1O1Li1-162(3) C53C52C51O19-22(5)
C2Si1O1Li516(4) C32C33C34O1424(6)
C18Si6O6K369(2) C51O19C54C5337(5)
C18Si6O6Li7145(3) C51C52C53C5440(5)
C18Si6O6Li3-19(3) C34O14C31C32-15(6)
C18Si6O6K4-121(2) C34C33C32C31-31(6)
C7Si3O3K13.7(18) C54O19C51C52-10(5)
C7Si3O3Li4-95(3) C31O14C34C33-4(5)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3166.
AtomxyzU(eq)
H41A4453-10290-1172142
H41B5280-9487-1339142
H8A1775-41104749136
H8B815-50484093136
H8C807-40905318136
H13A-527-5013-4221164
H13B-1637-5510-4223164
H13C-1132-6067-5305164
H5A3979-60501158100
H5B4948-51611404100
H5C4187-5629303100
H10A-4207-4337-425120
H10B-4863-4782-1586120
H10C-3838-3944-1255120
H42A4720-7998-278118
H42B4213-8756186118
H47A-4598-1925141112
H47B-3871-1117-128112
H2A-2660-3387-2383120
H2B-1984-3674-3326120
H2C-2314-2465-2724120
H18A2279-62822968217
H18B2709-71731934217
H18C2249-75412743217
H364919-4270-3853207
H45A-4837-54963406121
H45B-4481-56464437121
H7A1973-19774589108
H7B1426-17115625108
H7C1017-13674751108
H14A-1327-8614-4643149
H14B-1370-8440-5688149
H14C-2138-7948-4845149
H3A803-1948-1752147
H3B37-1573-2384147
H3C214-2849-2929147
H16A109-73573017118
H16B-125-86182030118
H16C-705-76831989118
H30A-3590-32412103177
H30B-2444-27212571177
H30C-3045-34023053177
H22A2935-7178-1991113
H22B3599-6576-2503113
H22C2466-7116-3032113
H4A3865-23172058114
H4B3996-3207845114
H4C4849-28781840114
H11A-3978-6698-824171
H11B-3846-7606-2031171
H11C-4827-7038-1826171
H6A3375-42003553119
H6B3716-29373816119
H6C4508-37773551119
H12A-3224-6819-3595125
H12B-3449-5608-3350125
H12C-4341-6572-3569125
H46A-3339-4608358792
H46B-2974-4795459192
H353078-5632-4504167
H23A921-8681-1981106
H23B-217-9004-2042106
H43A-3305-76922316153
H43B-3202-71723606153
H38A2828-2327-2379115
H38B3079-2834-3620115
H17A1772-8864171145
H17B603-9192-254145
H17C1069-9486637145
H1A-464-799189161
H1B-1585-1332103161
H1C-1341-657-533161
H19A1765-1654386179
H19B2638-1999870179
H9A-1048-38094491132
H9B-1110-28014232132
H9C-582-25525397132
H15A1052-7362-4175134
H15B1188-6235-4256134
H15C684-7398-5298134
H39A2528-9273-2495104
H39B2423-10142-2030104
H49A-35118572929184
H49B-4074-2722850184
H40A4210-9506-2776158
H40B3804-10746-2980158
H27A-2838-8876-1042359
H27B-2933-7962175359
H27C-2324-8960-31359
H20A2635-2158-934122
H20B3448-184291122
H20C2697-997170122
H29A-2858-4909184881
H29B-3147-459293281
H21A2761-5320-208067
H21B3164-5419-105567
H374598-2623-1906538
H24A-402-9280-3508326
H24B268-9954-3127326
H24C781-9041-3406326
H26A-322-313219534
H26B743-2422842534
H26C352-6793631534
H44A-4654-74973219136
H44B-4640-72642200136
H52A-2973-12075-5084154
H52B-3715-12341-4364154
H33A375521434215189
H33B287820014842189
H53A-4668-11076-4331187
H53B-4423-11632-5565187
H32A407718125776191
H32B468712694755191
H51A-3131-10636-2823191
H51B-2161-10656-3397191
H34A31885502741167
H34B21497623225167
H54A-2996-10243-5013159
H54B-3919-9594-4588159
H31A3905-3374613213
H31B29922345157213

Experimental

Single crystals of C54H120K6Li8O19Si6 [3166] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 293(2) K during data collection. Using Olex2 [1], the structure was solved with the SIR2004 [2] structure solution program using Direct Methods and refined with the ShelXL [3] refinement package using Least Squares minimisation.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
  2. Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R. (2007). J. Appl. Cryst. 40, 609-613.
  3. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [3166]

Crystal Data for C54H120K6Li8O19Si6 (=1533.16 g/mol): triclinic, space group P1 (no. 1), a = 13.4104(15) Å, b = 13.4700(15) Å, c = 13.8314(14) Å, α = 118.487(11)°, β = 94.653(9)°, γ = 95.912(10)°, = 2159.9(5) Å3, Z = 1, T = 293(2) K, μ(MoKα) = 0.439 mm-1, Dcalc = 1.179 g/cm3, 15657 reflections measured (4.608° ≤ 2Θ ≤ 50°), 11650 unique (Rint = 0.0476, Rsigma = 0.1438) which were used in all calculations. The final R1 was 0.0874 (I > 2σ(I)) and wR2 was 0.3467 (all data).

Refinement model description

Number of restraints - 3, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C41(H41a,H41b), C48(H48a,H48b), C42(H42a,H42b), C47(H47a,H47b), C36(H36a,
H36b), C45(H45a,H45b), C46(H46a,H46b), C35(H35a,H35b), C43(H43a,H43b),
C38(H38a,H38b), C50(H50a,H50b), C39(H39a,H39b), C49(H49a,H49b), C40(H40a,H40b),
C37(H37a,H37b), C44(H44a,H44b), C52(H52a,H52b), C33(H33a,H33b), C53(H53a,
H53b), C32(H32a,H32b), C51(H51a,H51b), C34(H34a,H34b), C54(H54a,H54b),
C31(H31a,H31b)
2.b Aromatic/amide H refined with riding coordinates:
C29(H29), C27(H27), C25(H25), C21(H21), C23(H23), C19(H19)
2.c X=CH2 refined with riding coordinates:
C28(H28a,H28b), C24(H24a,H24b), C30(H30a,H30b), C22(H22a,H22b), C26(H26a,
H26b), C20(H20a,H20b)
2.d Idealised Me refined as rotating group:
C8(H8a,H8b,H8c), C13(H13a,H13b,H13c), C5(H5a,H5b,H5c), C10(H10a,H10b,H10c),
C2(H2a,H2b,H2c), C18(H18a,H18b,H18c), C7(H7a,H7b,H7c), C14(H14a,H14b,H14c),
C3(H3a,H3b,H3c), C16(H16a,H16b,H16c), C4(H4a,H4b,H4c), C11(H11a,H11b,H11c),
C6(H6a,H6b,H6c), C12(H12a,H12b,H12c), C17(H17a,H17b,H17c), C1(H1a,H1b,H1c),
C9(H9a,H9b,H9c), C15(H15a,H15b,H15c)

This report has been created with Olex2, compiled on 2018.04.03 svn.r3497 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.