3167tri

Table 1 Crystal data and structure refinement for 3167tri.
Identification code 3167tri
Empirical formula C40H104K4Li4O12Si8
Formula weight 1186.11
Temperature/K 173.15
Crystal system orthorhombic
Space group Pbca
a/Å 13.9966(5)
b/Å 22.8582(8)
c/Å 44.793(2)
α/° 90
β/° 90
γ/° 90
Volume/Å3 14330.9(10)
Z 8
ρcalcg/cm3 1.099
μ/mm‑1 0.424
F(000) 5120.0
Crystal size/mm3 0.35 × 0.29 × 0.24
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.368 to 51.998
Index ranges -17 ≤ h ≤ 17, -28 ≤ k ≤ 28, -55 ≤ l ≤ 55
Reflections collected 189441
Independent reflections 14062 [Rint = 0.1146, Rsigma = 0.0569]
Data/restraints/parameters 14062/470/821
Goodness-of-fit on F2 1.131
Final R indexes [I>=2σ (I)] R1 = 0.0796, wR2 = 0.1756
Final R indexes [all data] R1 = 0.1202, wR2 = 0.1933
Largest diff. peak/hole / e Å-3 0.47/-0.56

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3167tri. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
K111499.8(8)1430.2(5)1021.3(3)44.2(3)
K211267.1(8)61.2(5)1558.1(3)45.5(3)
K37823.8(8)1359.4(5)1543.4(3)45.4(3)
K47969.8(7)303.7(4)841.2(3)40.0(3)
Si112518.6(11)1403.5(8)1768.0(4)56.0(4)
Si212659.7(10)-24.4(7)875.8(4)51.2(4)
Si39863.6(10)1103.2(7)404.6(3)46.2(4)
Si49765.1(12)2465.5(6)1402.3(4)54.5(4)
Si59626.3(10)-880.2(6)1085.8(3)43.2(3)
Si69313.5(13)521.6(8)2089.9(4)64.0(5)
Si76831.3(10)1746.1(6)810.0(4)45.4(4)
Si86582.3(10)-54.6(7)1509.8(4)56.6(4)
O111550(2)1227.1(15)1605.1(8)46.7(9)
O211680(2)268.3(14)980.3(7)42.3(8)
O39781(2)926.0(13)747.2(7)36.4(7)
O49695(2)1793.3(13)1317.1(7)39.6(8)
O59647(2)-208.2(13)1179.2(7)39.6(8)
O69500(2)659.7(14)1747.3(7)42.6(8)
O77764(2)1456.8(13)945.3(8)39.9(8)
O87602(2)216.2(13)1430.9(8)43.1(8)
C112332(5)1914(3)2088.8(16)82(2)
C213392(5)1768(4)1506.9(18)108(3)
C313162(4)751(3)1918.6(15)77(2)
C413561(4)530(3)757.5(17)84(2)
C512519(5)-545(3)556.8(15)80(2)
C613232(4)-461(3)1181.2(16)73.2(19)
C710956(5)804(4)231.9(15)87(2)
C89886(5)1914(3)370.3(15)76(2)
C98842(5)838(3)182.8(14)71.6(18)
C108801(5)2891(3)1221.0(17)88(2)
C1110937(6)2785(3)1293(2)101(3)
C129666(6)2556(3)1812.0(17)93(2)
C138525(4)-1241(2)1223.0(15)62.3(16)
C1410647(4)-1304(3)1237.6(15)65.0(17)
C159657(4)-949(3)672.1(13)64.3(16)
C168114(6)795(4)2218.2(17)109(3)
C1710261(7)770(5)2332.0(17)142(4)
C189194(7)-280(4)2145(2)127(4)
C195998(4)2008(3)1110.1(15)69.7(18)
C206129(4)1223(3)573.5(16)74(2)
C217069(4)2395(3)567.6(15)65.7(17)
C225751(5)498(3)1669(2)114(3)
C236613(5)-652(3)1788.1(16)78(2)
C245969(4)-358(3)1170.9(17)84(2)
Li110244(6)1286(4)1602(2)45(2)
Li210388(5)275(3)923.1(18)36.5(18)
Li38885(5)138(3)1478.0(19)42.0(19)
Li49073(6)1486(3)978.3(19)40.5(19)
O9B12430(30)2244(12)662(8)78(7)
O10B6890(30)-398(19)453(12)68(11)
O11B6830(110)2190(70)1900(40)72(8)
O12B11810(20)-793(14)1968(6)84(5)
C25B12632(19)2061(13)323(5)112(10)
C26B13594(18)2267(11)279(6)93(7)
C27B13580(40)2808(18)436(11)190(30)
C28B12960(20)2637(13)715(6)116(11)
C29B6970(50)-1020(20)494(17)130(20)
C30B6040(60)-1240(30)289(17)150(30)
C31B5540(30)-710(20)175(13)83(11)
C32B6200(40)-269(19)273(12)79(12)
C33B6280(40)2045(17)2152(10)77(8)
C34B5820(40)2630(30)2213(14)90(8)
C35B5560(40)2760(20)1966(11)93(8)
C36B6640(40)2750(30)1864(12)82(8)
C37B12553(19)-1179(11)1914(5)142(10)
C38B13145(16)-1336(10)2180(6)124(8)
C39B12290(20)-1312(12)2391(5)125(8)
C40B11691(15)-787(11)2284(4)143(10)
O9A12510(20)2073(10)624(6)69(5)
O10A7141(13)-472(8)426(4)47(3)
O11A6810(40)2100(20)1911(13)65(4)
O12A12030(40)-740(20)1967(13)130(15)
C25A12228(13)2594(16)444(9)210(20)
C26A13092(14)2709(13)260(4)107(8)
C27A13851(15)2568(14)480(8)109(11)
C28A13470(14)2222(13)685(5)132(11)
C29A6959(16)-1092(9)448(5)63(4)
C30A5925(16)-1161(11)402(5)87(5)
C31A5753(16)-683(13)181(6)112(9)
C32A6564(15)-298(8)172(4)62(4)
C33A5932(10)1930(6)2045(4)79(4)
C34A5478(13)2444(6)2188(5)88(4)
C35A5968(12)2952(5)2015(4)88(4)
C36A6949(11)2715(8)1953(5)84(4)
C37A13000(20)-858(18)2033(9)166(15)
C38A12720(40)-1300(30)2271(15)220(30)
C39A11750(30)-1484(19)2320(10)197(19)
C40A11410(20)-1309(15)2055(7)149(13)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3167tri. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
K140.9(6)46.7(6)44.8(6)6.5(5)-2.3(5)-12.3(5)
K241.2(6)50.0(6)45.2(6)7.8(5)-2.9(5)3.8(5)
K345.1(6)38.9(6)52.2(7)-4.0(5)7.7(5)3.7(5)
K432.2(5)34.5(5)53.1(7)-1.4(5)-1.9(5)-2.0(4)
Si137.1(8)81.6(12)49.2(9)-3.2(8)-8.4(7)-7.0(8)
Si226.6(7)64.1(10)63.0(10)-4.7(8)1.7(7)-0.8(7)
Si343.5(8)54.5(9)40.6(8)3.8(7)-0.6(7)-2.0(7)
Si457.5(10)35.1(8)70.9(11)-7.4(7)-10.2(8)0.6(7)
Si537.4(7)37.0(7)55.1(9)-2.8(7)1.0(7)-1.4(6)
Si672.5(11)71.8(11)47.6(10)12.7(8)15.1(9)16.4(9)
Si733.8(7)39.6(7)62.8(10)-0.7(7)-4.2(7)4.3(6)
Si834.8(8)51.9(9)82.9(12)3.1(8)18.5(8)-3.4(7)
O135.5(18)57(2)48(2)2.3(17)-5.4(16)-4.0(16)
O228.6(16)51(2)48(2)3.2(16)-1.0(15)0.2(15)
O334.8(17)38.7(17)35.7(18)0.4(14)1.2(14)4.2(14)
O438.4(18)33.8(17)47(2)0.7(15)-5.1(15)-1.1(14)
O534.6(17)34.8(17)49(2)1.3(15)6.6(15)-1.3(14)
O646.7(19)42.2(19)39(2)0.3(15)4.6(15)-7.2(15)
O731.9(17)33.0(17)55(2)1.1(15)-2.1(15)1.2(14)
O833.2(17)38.0(18)58(2)0.8(16)9.6(16)-1.1(14)
C167(4)87(5)91(5)-27(4)-18(4)-8(4)
C260(4)173(9)92(6)4(6)-5(4)-52(5)
C353(4)113(6)65(4)-21(4)-17(3)22(4)
C445(4)104(5)102(6)4(4)20(4)-13(4)
C556(4)103(5)82(5)-26(4)7(4)14(4)
C638(3)82(4)100(5)-3(4)-15(3)13(3)
C773(5)133(7)55(4)-1(4)6(3)28(4)
C872(4)76(4)78(5)28(4)-16(4)-11(4)
C974(4)89(5)51(4)-2(3)-6(3)-24(4)
C10103(6)49(4)111(6)-11(4)-30(5)23(4)
C11116(6)49(4)138(8)0(4)-4(6)-28(4)
C12103(6)81(5)94(6)-29(4)-26(5)16(4)
C1354(3)39(3)94(5)1(3)10(3)-7(3)
C1460(4)52(3)83(5)-1(3)-1(3)2(3)
C1562(4)65(4)67(4)-13(3)-6(3)5(3)
C16117(7)146(8)63(5)4(5)20(5)21(6)
C17154(9)225(12)49(5)1(6)-18(5)-98(8)
C18135(8)122(8)122(8)55(6)4(6)-24(6)
C1946(3)78(4)85(5)6(4)1(3)15(3)
C2051(4)63(4)108(6)-12(4)-24(4)4(3)
C2156(4)57(4)84(5)16(3)-10(3)9(3)
C2268(5)87(5)187(9)-8(6)65(6)3(4)
C2375(4)70(4)90(5)2(4)23(4)-26(4)
C2438(3)106(6)107(6)16(5)-10(3)-18(3)
Li137(4)48(5)49(5)3(4)-2(4)-9(4)
Li225(4)34(4)50(5)2(4)3(3)0(3)
Li333(4)40(4)53(5)2(4)7(4)-2(3)
Li437(4)32(4)52(5)3(4)1(4)3(3)
O9B110(14)51(14)73(11)18(9)19(8)-39(11)
O10B42(18)41(10)120(20)-23(11)-23(14)4(11)
O11B87(16)51(13)79(15)-1(14)25(12)12(12)
O12B91(10)96(13)65(8)22(7)-22(7)14(7)
C25B124(17)132(19)80(12)-12(11)30(12)-75(15)
C26B80(12)96(14)102(15)16(11)24(11)0(11)
C27B300(50)120(20)140(30)-20(20)100(30)-160(30)
C28B120(20)120(19)109(16)-29(14)38(15)-78(16)
C29B120(30)40(13)220(60)10(20)-100(30)-40(19)
C30B230(50)77(14)160(50)-10(30)-140(40)-50(30)
C31B29(13)120(20)100(30)-29(18)2(11)0(12)
C32B100(30)68(12)60(30)-15(17)-29(19)4(17)
C33B106(17)55(13)70(15)11(11)28(13)12(12)
C34B97(17)72(16)102(13)-4(13)31(12)28(13)
C35B101(15)68(15)111(15)-1(14)0(15)30(13)
C36B107(16)56(11)82(16)21(13)16(13)12(14)
C37B180(20)150(20)98(11)27(13)5(11)87(18)
C38B128(14)70(11)173(18)-27(12)-60(11)33(11)
C39B200(20)98(15)74(10)29(10)-54(10)3(16)
C40B155(16)200(20)76(9)45(13)9(11)82(14)
O9A77(7)53(11)77(10)8(7)2(7)-31(8)
O10A40(7)42(5)58(5)3(4)-11(5)-3(5)
O11A85(8)45(7)66(6)-4(6)16(6)8(5)
O12A130(20)90(20)160(30)41(15)-50(20)21(16)
C25A69(8)240(30)320(40)210(30)6(13)-20(14)
C26A107(12)129(18)85(12)44(11)-10(8)-48(13)
C27A64(8)140(30)125(19)50(17)-15(9)-52(10)
C28A82(11)170(20)141(18)87(16)-16(11)-54(12)
C29A76(8)43(6)71(8)-3(6)-11(7)5(7)
C30A96(8)84(11)80(11)-1(8)-30(9)-49(7)
C31A82(12)121(15)132(17)29(11)-71(13)-25(9)
C32A91(12)53(6)42(8)-2(5)-14(6)0(6)
C33A76(7)55(5)107(10)-14(6)17(6)-2(5)
C34A88(9)62(8)113(9)-9(7)26(7)7(6)
C35A94(9)42(5)127(10)-2(6)27(8)11(5)
C36A80(8)53(6)118(12)-18(8)15(7)6(6)
C37A146(19)170(30)180(30)60(20)-100(20)4(18)
C38A210(30)210(50)230(60)120(40)-90(40)20(40)
C39A260(40)160(30)180(30)80(20)-120(30)-70(30)
C40A180(20)150(20)110(20)50(20)-36(19)-26(19)

 

Table 4 Bond Lengths for 3167tri.
AtomAtomLength/Å AtomAtomLength/Å
K1K23.9601(15) Si7C191.878(6)
K1O12.657(4) Si7C201.877(6)
K1O22.674(3) Si7C211.868(6)
K1O32.936(3) Si8O81.595(3)
K1O42.971(3) Si8C221.859(7)
K1Li13.155(9) Si8C231.850(7)
K1Li23.096(7) Si8C241.877(7)
K1Li43.404(8) O1Li11.833(9)
K1O9B2.78(3) O2Li21.826(8)
K1O9A2.71(3) O3Li21.885(8)
K2O12.702(4) O3Li41.922(8)
K2O22.694(3) O4Li11.887(9)
K2O52.898(3) O4Li41.884(9)
K2O62.950(3) O5Li21.901(8)
K2Li13.151(9) O5Li31.886(9)
K2Li23.138(8) O6Li11.887(9)
K2Li33.358(8) O6Li31.902(9)
K2O12B2.79(3) O7Li41.840(8)
K2O12A2.79(5) O8Li31.817(8)
K3K43.9699(15) Li1Li33.288(11)
K3O42.978(3) Li1Li43.270(12)
K3O62.983(4) Li2Li33.271(11)
K3O72.690(4) Li2Li43.333(10)
K3O82.680(3) O9BC25B1.60(4)
K3Li13.402(8) O9BC28B1.19(4)
K3Li33.175(8) O10BC29B1.43(6)
K3Li43.090(8) O10BC32B1.28(6)
K3O11B2.85(16) O11BC33B1.39(16)
K3O11A2.76(5) O11BC36B1.33(18)
K4O32.937(3) O12BC37B1.38(4)
K4O53.029(3) O12BC40B1.43(4)
K4O72.692(3) C25BC26B1.44(3)
K4O82.699(4) C26BC27B1.42(5)
K4Li23.404(7) C27BC28B1.57(4)
K4Li33.149(9) C29BC30B1.67(9)
K4Li43.174(8) C30BC31B1.49(10)
K4O10B2.81(5) C31BC32B1.43(5)
K4O10A2.821(19) C33BC34B1.51(6)
Si1O11.591(3) C34BC35B1.20(8)
Si1C11.870(7) C35BC36B1.59(7)
Si1C21.885(7) C37BC38B1.49(3)
Si1C31.868(7) C38BC39B1.52(4)
Si2O21.596(3) C39BC40B1.54(3)
Si2C41.866(6) O9AC25A1.49(4)
Si2C51.870(7) O9AC28A1.41(3)
Si2C61.873(6) O10AC29A1.44(2)
Si3O31.592(3) O10AC32A1.45(2)
Si3C71.845(6) O11AC33A1.43(5)
Si3C81.861(6) O11AC36A1.42(5)
Si3C91.843(6) O12AC37A1.41(5)
Si4O41.586(3) O12AC40A1.62(6)
Si4C101.851(6) C25AC26A1.49(3)
Si4C111.861(8) C26AC27A1.48(4)
Si4C121.852(8) C27AC28A1.32(3)
Si5O51.592(3) C29AC30A1.47(3)
Si5C131.853(5) C30AC31A1.49(4)
Si5C141.855(6) C31AC32A1.44(2)
Si5C151.860(6) C33AC34A1.481(18)
Si6O61.588(4) C34AC35A1.55(2)
Si6C161.882(8) C35AC36A1.501(18)
Si6C171.805(8) C37AC38A1.52(6)
Si6C181.857(9) C38AC39A1.43(6)
Si7O71.584(3) C39AC40A1.34(4)

 

Table 5 Bond Angles for 3167tri.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O1K1K242.81(8) Li1O1K187.3(3)
O1K1O283.77(11) Li1O1K285.7(3)
O1K1O3111.38(10) K1O2K295.07(11)
O1K1O468.44(10) Si2O2K1121.14(17)
O1K1Li135.47(17) Si2O2K2113.10(17)
O1K1Li290.23(17) Si2O2Li2144.4(3)
O1K1Li495.09(16) Li2O2K184.7(3)
O1K1O9B132.3(8) Li2O2K285.6(3)
O1K1O9A136.7(6) K1O3K4146.85(12)
O2K1K242.65(7) Si3O3K1104.12(15)
O2K1O370.03(9) Si3O3K4108.90(15)
O2K1O4112.83(9) Si3O3Li2124.8(3)
O2K1Li190.30(17) Si3O3Li4112.8(3)
O2K1Li235.98(15) Li2O3K176.5(2)
O2K1Li497.33(15) Li2O3K486.9(2)
O2K1O9B125.5(7) Li2O3Li4122.2(4)
O2K1O9A116.4(5) Li4O3K186.3(3)
O3K1K282.89(7) Li4O3K478.5(2)
O3K1O466.39(9) K1O4K3143.76(11)
O3K1Li181.21(16) Si4O4K1108.96(16)
O3K1Li236.29(15) Si4O4K3107.18(16)
O3K1Li434.30(15) Si4O4Li1114.0(3)
O4K1K283.11(7) Si4O4Li4125.7(3)
O4K1Li135.72(17) Li1O4K177.5(3)
O4K1Li282.75(15) Li1O4K385.6(3)
O4K1Li433.51(15) Li4O4K186.0(3)
Li1K1K251.05(16) Li4O4K375.2(3)
Li1K1Li459.7(2) Li4O4Li1120.2(4)
Li2K1K251.03(15) K2O5K4144.79(12)
Li2K1Li175.4(2) Si5O5K2111.91(16)
Li2K1Li461.48(18) Si5O5K4103.13(15)
Li4K1K288.97(13) Si5O5Li2114.4(3)
O9BK1K2156.6(9) Si5O5Li3125.5(3)
O9BK1O3113.9(9) Li2O5K278.7(3)
O9BK1O4118.0(8) Li2O5K484.0(2)
O9BK1Li1143.8(7) Li3O5K286.4(3)
O9BK1Li2136.3(7) Li3O5K475.8(3)
O9BK1Li4114.2(9) Li3O5Li2119.5(4)
O9AK1K2150.6(6) K2O6K3145.08(12)
O9AK1O3111.5(6) Si6O6K2108.86(17)
O9AK1O4125.9(6) Si6O6K3105.84(16)
O9AK1Li1152.9(5) Si6O6Li1125.1(3)
O9AK1Li2129.2(5) Si6O6Li3114.4(3)
O9AK1Li4117.7(7) Li1O6K277.9(3)
O1K2K141.92(8) Li1O6K385.5(3)
O1K2O5111.70(10) Li1O6Li3120.4(4)
O1K2O669.10(9) Li3O6K284.7(3)
O1K2Li135.46(16) Li3O6K377.6(3)
O1K2Li288.52(16) K3O7K495.06(10)
O1K2Li395.86(15) Si7O7K3116.21(17)
O1K2O12B126.8(6) Si7O7K4115.52(16)
O1K2O12A122.4(12) Si7O7Li4146.7(3)
O2K2K142.27(7) Li4O7K383.8(3)
O2K2O182.53(11) Li4O7K486.7(3)
O2K2O569.04(9) K3O8K495.15(10)
O2K2O6111.97(10) Si8O8K3116.14(16)
O2K2Li190.04(17) Si8O8K4114.62(18)
O2K2Li235.48(15) Si8O8Li3145.1(3)
O2K2Li395.79(16) Li3O8K387.7(3)
O2K2O12B134.2(7) Li3O8K486.1(3)
O2K2O12A131.5(14) K1Li1K3119.1(3)
O5K2K182.91(7) K1Li1Li3105.5(3)
O5K2O667.11(9) K1Li1Li464.0(2)
O5K2Li182.50(16) K2Li1K177.8(2)
O5K2Li236.43(14) K2Li1K3119.4(2)
O5K2Li334.09(16) K2Li1Li362.8(2)
O6K2K182.93(7) K2Li1Li4107.4(3)
O6K2Li135.83(16) O1Li1K157.3(3)
O6K2Li281.90(15) O1Li1K258.8(3)
O6K2Li334.33(16) O1Li1K3175.8(4)
Li1K2K151.15(16) O1Li1O4117.2(5)
Li1K2Li360.6(2) O1Li1O6119.4(5)
Li2K2K150.09(13) O1Li1Li3121.3(4)
Li2K2Li174.9(2) O1Li1Li4121.1(4)
Li2K2Li360.35(19) O4Li1K166.8(3)
Li3K2K188.59(14) O4Li1K2133.6(4)
O12BK2K1158.6(6) O4Li1K360.8(2)
O12BK2O5116.8(6) O4Li1Li398.1(3)
O12BK2O6111.4(6) O4Li1Li429.9(2)
O12BK2Li1134.9(7) O6Li1K1132.2(4)
O12BK2Li2144.5(7) O6Li1K266.3(3)
O12BK2Li3112.3(6) O6Li1K361.0(2)
O12AK2K1151.8(12) O6Li1O4118.4(4)
O12AK2O5123.0(11) O6Li1Li329.9(2)
O12AK2O6115.7(13) O6Li1Li497.2(3)
O12AK2Li1135.4(14) Li3Li1K356.65(19)
O12AK2Li2147.7(13) Li4Li1K355.15(19)
O12AK2Li3118.9(12) Li4Li1Li371.2(3)
O4K3K483.53(7) K1Li2K278.88(18)
O4K3O665.87(9) K1Li2K4119.9(2)
O4K3Li133.58(15) K1Li2Li3107.3(3)
O4K3Li381.38(15) K1Li2Li463.8(2)
O4K3Li436.12(16) K2Li2K4119.4(2)
O6K3K482.88(7) K2Li2Li363.2(2)
O6K3Li133.57(15) K2Li2Li4106.2(3)
O6K3Li335.81(16) O2Li2K159.3(2)
O6K3Li481.72(16) O2Li2K258.9(2)
O7K3K442.50(7) O2Li2K4178.0(4)
O7K3O470.17(9) O2Li2O3120.8(4)
O7K3O6111.96(10) O2Li2O5116.7(4)
O7K3Li196.41(16) O2Li2Li3122.0(4)
O7K3Li389.74(17) O2Li2Li4122.9(4)
O7K3Li436.30(16) O3Li2K167.2(2)
O7K3O11B119(4) O3Li2K2132.7(4)
O7K3O11A121.8(13) O3Li2K459.5(2)
O8K3K442.61(8) O3Li2O5117.8(4)
O8K3O4111.27(9) O3Li2Li396.0(3)
O8K3O668.04(9) O3Li2Li429.2(2)
O8K3O783.66(10) O5Li2K1133.2(4)
O8K3Li194.70(16) O5Li2K264.9(2)
O8K3Li334.87(16) O5Li2K462.2(2)
O8K3Li490.18(16) O5Li2Li330.1(2)
O8K3O11B134(3) O5Li2Li497.9(3)
O8K3O11A130.9(10) Li3Li2K456.26(19)
Li1K3K488.83(15) Li3Li2Li470.6(2)
Li3K3K450.83(16) Li4Li2K456.19(18)
Li3K3Li159.9(2) K3Li3K2120.0(2)
Li4K3K451.61(15) K3Li3Li163.5(2)
Li4K3Li160.3(2) K3Li3Li2106.7(3)
Li4K3Li375.1(2) K4Li3K2120.5(2)
O11BK3K4151(4) K4Li3K377.76(19)
O11BK3O4114(3) K4Li3Li1107.0(3)
O11BK3O6125(4) K4Li3Li264.0(2)
O11BK3Li1119(3) O5Li3K259.5(2)
O11BK3Li3150(4) O5Li3K3134.4(4)
O11BK3Li4133(3) O5Li3K468.8(3)
O11AK3K4151.0(12) O5Li3O6117.2(4)
O11AK3O4116.6(10) O5Li3Li197.3(3)
O11AK3O6123.5(13) O5Li3Li230.4(2)
O11AK3Li1119.7(11) O6Li3K261.0(2)
O11AK3Li3146.9(12) O6Li3K366.6(2)
O11AK3Li4136.1(11) O6Li3K4133.1(4)
O3K4K382.16(7) O6Li3Li129.7(2)
O3K4O565.78(8) O6Li3Li297.5(3)
O3K4Li233.56(14) O8Li3K2177.3(4)
O3K4Li380.62(15) O8Li3K357.5(2)
O3K4Li436.41(15) O8Li3K458.7(3)
O5K4K383.03(7) O8Li3O5121.2(5)
O5K4Li233.73(14) O8Li3O6117.4(4)
O5K4Li335.48(15) O8Li3Li1120.9(4)
O5K4Li481.67(15) O8Li3Li2122.5(4)
O7K4K342.44(7) Li1Li3K256.6(2)
O7K4O369.10(9) Li2Li3K256.48(18)
O7K4O5112.01(9) Li2Li3Li171.3(3)
O7K4O883.26(10) K3Li4K1121.0(3)
O7K4Li296.11(14) K3Li4K478.64(18)
O7K4Li390.24(16) K3Li4Li164.6(2)
O7K4Li435.37(15) K3Li4Li2107.2(3)
O7K4O10B127.4(9) K4Li4K1117.7(2)
O7K4O10A133.3(3) K4Li4Li1106.8(3)
O8K4K342.24(7) K4Li4Li263.04(19)
O8K4O3109.94(10) O3Li4K159.4(2)
O8K4O568.29(9) O3Li4K3132.1(4)
O8K4Li294.76(16) O3Li4K465.1(2)
O8K4Li335.14(15) O3Li4Li196.2(3)
O8K4Li488.09(17) O3Li4Li228.6(2)
O8K4O10B117.4(10) O4Li4K160.5(2)
O8K4O10A121.4(3) O4Li4K368.7(3)
Li2K4K388.70(14) O4Li4K4134.2(4)
Li3K4K351.42(15) O4Li4O3116.3(4)
Li3K4Li259.73(19) O4Li4Li129.9(2)
Li3K4Li474.3(2) O4Li4Li296.6(3)
Li4K4K349.75(15) O7Li4K1175.5(4)
Li4K4Li260.76(18) O7Li4K359.9(2)
O10BK4K3144.0(10) O7Li4K457.9(2)
O10BK4O3130.8(10) O7Li4O3116.5(4)
O10BK4O5120.5(9) O7Li4O4122.6(5)
O10BK4Li2126.4(10) O7Li4Li1124.2(4)
O10BK4Li3135.4(10) O7Li4Li2120.9(4)
O10BK4Li4150.3(10) Li1Li4K156.4(2)
O10AK4K3152.1(4) Li1Li4Li270.8(3)
O10AK4O3124.4(4) Li2Li4K154.70(17)
O10AK4O5113.9(3) C25BO9BK1117.1(17)
O10AK4Li2117.9(4) C28BO9BK1133(3)
O10AK4Li3133.6(3) C28BO9BC25B106(2)
O10AK4Li4149.7(4) C29BO10BK4116(4)
O1Si1C1113.1(3) C32BO10BK4131(3)
O1Si1C2112.3(3) C32BO10BC29B112(4)
O1Si1C3111.9(3) C33BO11BK3125(9)
C1Si1C2106.9(4) C36BO11BK3132(10)
C3Si1C1106.7(3) C36BO11BC33B103(10)
C3Si1C2105.3(4) C37BO12BK2122.5(17)
O2Si2C4112.3(3) C37BO12BC40B105.7(19)
O2Si2C5113.6(2) C40BO12BK2127.9(19)
O2Si2C6112.1(2) C26BC25BO9B102(2)
C4Si2C5106.7(3) C27BC26BC25B102(3)
C4Si2C6106.3(3) C26BC27BC28B100(2)
C5Si2C6105.3(3) O9BC28BC27B112(3)
O3Si3C7111.7(3) O10BC29BC30B99(5)
O3Si3C8109.5(3) C31BC30BC29B108(4)
O3Si3C9112.3(2) C32BC31BC30B99(4)
C7Si3C8108.7(4) O10BC32BC31B121(5)
C9Si3C7107.1(3) O11BC33BC34B100(7)
C9Si3C8107.3(3) C35BC34BC33B100(4)
O4Si4C10111.0(3) C34BC35BC36B88(4)
O4Si4C11111.8(3) O11BC36BC35B99(8)
O4Si4C12110.0(3) O12BC37BC38B115(2)
C10Si4C11108.7(4) C37BC38BC39B93.0(16)
C10Si4C12108.7(3) C40BC39BC38B105.2(16)
C12Si4C11106.4(4) O12BC40BC39B103.7(19)
O5Si5C13111.0(2) C25AO9AK1130.5(19)
O5Si5C14113.1(2) C28AO9AK1120.0(17)
O5Si5C15110.0(2) C28AO9AC25A99.5(17)
C13Si5C14106.6(3) C29AO10AK4130.0(12)
C13Si5C15108.2(3) C29AO10AC32A103.1(16)
C14Si5C15107.7(3) C32AO10AK4125.0(11)
O6Si6C16112.1(3) C33AO11AK3121(3)
O6Si6C17113.4(3) C36AO11AK3128(3)
O6Si6C18109.8(3) C36AO11AC33A109(4)
C17Si6C16111.5(5) C37AO12AK2129(3)
C17Si6C18107.3(5) C37AO12AC40A107(3)
C18Si6C16102.0(4) C40AO12AK2119(3)
O7Si7C19111.8(2) C26AC25AO9A103(2)
O7Si7C20112.4(2) C25AC26AC27A100.2(19)
O7Si7C21114.0(2) C28AC27AC26A107.5(17)
C20Si7C19106.4(3) C27AC28AO9A113.1(19)
C21Si7C19105.9(3) O10AC29AC30A105.6(18)
C21Si7C20105.8(3) C29AC30AC31A100.0(16)
O8Si8C22112.4(3) C32AC31AC30A109.8(14)
O8Si8C23114.5(3) C31AC32AO10A104.5(14)
O8Si8C24111.9(3) O11AC33AC34A109(2)
C22Si8C24106.0(4) C33AC34AC35A100.8(12)
C23Si8C22104.9(4) C36AC35AC34A103.0(13)
C23Si8C24106.4(3) O11AC36AC35A105(3)
K1O1K295.27(11) O12AC37AC38A92(4)
Si1O1K1115.44(18) C39AC38AC37A123(4)
Si1O1K2114.23(18) C40AC39AC38A96(4)
Si1O1Li1146.6(4) C39AC40AO12A106(3)

 

Table 6 Torsion Angles for 3167tri.
ABCDAngle/˚ ABCDAngle/˚
K1O1Li1K295.50(11) Si7O7Li4O3-104.7(6)
K1O1Li1O4-31.0(5) Si7O7Li4O4100.4(7)
K1O1Li1O6123.6(5) Si7O7Li4Li1136.3(5)
K1O1Li1Li388.9(4) Si7O7Li4Li2-137.0(5)
K1O1Li1Li43.0(4) Si8O8Li3K3-135.4(6)
K1O2Li2K2-95.52(10) Si8O8Li3K4129.3(6)
K1O2Li2O328.8(5) Si8O8Li3O598.9(7)
K1O2Li2O5-126.3(4) Si8O8Li3O6-104.9(6)
K1O2Li2Li3-92.1(4) Si8O8Li3Li1-138.7(5)
K1O2Li2Li4-5.7(4) Si8O8Li3Li2134.8(5)
K1O3Li2K247.7(4) C1Si1O1K1124.9(3)
K1O3Li2K4151.07(12) C1Si1O1K2-126.1(3)
K1O3Li2O2-26.7(4) C1Si1O1Li1-3.8(7)
K1O3Li2O5128.2(5) C2Si1O1K13.7(4)
K1O3Li2Li3106.3(2) C2Si1O1K2112.8(4)
K1O3Li2Li476.7(4) C2Si1O1Li1-125.0(7)
K1O4Li1K2-43.5(4) C3Si1O1K1-114.5(3)
K1O4Li1K3-147.74(12) C3Si1O1K2-5.5(3)
K1O4Li1O128.1(4) C3Si1O1Li1116.8(7)
K1O4Li1O6-126.8(5) C4Si2O2K1-5.4(4)
K1O4Li1Li3-103.4(3) C4Si2O2K2-117.1(3)
K1O4Li1Li4-77.7(4) C4Si2O2Li2125.8(6)
K1O4Li4K3148.77(12) C5Si2O2K1-126.6(3)
K1O4Li4K4101.2(4) C5Si2O2K2121.7(3)
K1O4Li4O321.2(4) C5Si2O2Li24.6(7)
K1O4Li4O7176.2(5) C6Si2O2K1114.2(3)
K1O4Li4Li173.0(4) C6Si2O2K22.4(3)
K1O4Li4Li242.9(2) C6Si2O2Li2-114.6(6)
K1O9BC25BC26B-137(2) C7Si3O3K160.2(3)
K1O9BC28BC27B158(3) C7Si3O3K4-122.8(3)
K1O9AC25AC26A-176.8(17) C7Si3O3Li2-23.0(5)
K1O9AC28AC27A-176(3) C7Si3O3Li4152.1(4)
K2O1Li1K1-95.50(11) C8Si3O3K1-60.3(3)
K2O1Li1O4-126.5(5) C8Si3O3K4116.7(2)
K2O1Li1O628.1(5) C8Si3O3Li2-143.5(4)
K2O1Li1Li3-6.6(4) C8Si3O3Li431.6(4)
K2O1Li1Li4-92.5(4) C9Si3O3K1-179.4(3)
K2O2Li2K195.52(10) C9Si3O3K4-2.4(3)
K2O2Li2O3124.3(5) C9Si3O3Li297.4(4)
K2O2Li2O5-30.8(4) C9Si3O3Li4-87.5(4)
K2O2Li2Li33.4(4) C10Si4O4K1121.0(3)
K2O2Li2Li489.8(4) C10Si4O4K3-61.7(3)
K2O5Li3K3103.7(5) C10Si4O4Li1-154.6(4)
K2O5Li3K4149.36(12) C10Si4O4Li422.1(5)
K2O5Li3O620.7(4) C11Si4O4K1-0.6(3)
K2O5Li3O8177.0(5) C11Si4O4K3176.7(3)
K2O5Li3Li143.9(2) C11Si4O4Li183.8(4)
K2O5Li3Li274.8(3) C11Si4O4Li4-99.5(5)
K2O6Li1K144.8(4) C12Si4O4K1-118.6(3)
K2O6Li1K3149.12(12) C12Si4O4K358.6(3)
K2O6Li1O1-26.1(5) C12Si4O4Li1-34.3(4)
K2O6Li1O4128.2(5) C12Si4O4Li4142.5(4)
K2O6Li1Li376.3(4) C13Si5O5K2118.8(3)
K2O6Li1Li4105.9(3) C13Si5O5K4-64.7(3)
K2O12BC37BC38B144(2) C13Si5O5Li2-154.1(4)
K2O12BC40BC39B-169.8(19) C13Si5O5Li317.0(5)
K2O12AC37AC38A178(5) C14Si5O5K2-1.0(3)
K2O12AC40AC39A-158(4) C14Si5O5K4175.4(2)
K3O4Li1K1147.74(12) C14Si5O5Li286.1(4)
K3O4Li1K2104.2(4) C14Si5O5Li3-102.9(4)
K3O4Li1O1175.9(5) C15Si5O5K2-121.5(2)
K3O4Li1O620.9(5) C15Si5O5K455.0(2)
K3O4Li1Li344.3(2) C15Si5O5Li2-34.4(4)
K3O4Li1Li470.1(4) C15Si5O5Li3136.7(4)
K3O4Li4K1-148.77(12) C16Si6O6K2-171.9(3)
K3O4Li4K4-47.6(4) C16Si6O6K34.1(4)
K3O4Li4O3-127.6(4) C16Si6O6Li199.8(5)
K3O4Li4O727.4(4) C16Si6O6Li3-79.2(5)
K3O4Li4Li1-75.8(4) C17Si6O6K260.7(5)
K3O4Li4Li2-105.9(2) C17Si6O6K3-123.3(4)
K3O6Li1K1-104.3(5) C17Si6O6Li1-27.6(6)
K3O6Li1K2-149.12(12) C17Si6O6Li3153.4(5)
K3O6Li1O1-175.3(5) C18Si6O6K2-59.4(4)
K3O6Li1O4-20.9(5) C18Si6O6K3116.7(3)
K3O6Li1Li3-72.8(4) C18Si6O6Li1-147.6(5)
K3O6Li1Li4-43.2(2) C18Si6O6Li333.4(5)
K3O7Li4K495.45(10) C19Si7O7K34.1(3)
K3O7Li4O3125.2(4) C19Si7O7K4114.2(3)
K3O7Li4O4-29.7(4) C19Si7O7Li4-118.0(6)
K3O7Li4Li16.2(4) C20Si7O7K3-115.5(3)
K3O7Li4Li292.9(4) C20Si7O7K4-5.4(3)
K3O8Li3K4-95.32(10) C20Si7O7Li4122.4(6)
K3O8Li3O5-125.7(5) C21Si7O7K3124.1(3)
K3O8Li3O630.5(4) C21Si7O7K4-125.8(3)
K3O8Li3Li1-3.3(4) C21Si7O7Li42.0(7)
K3O8Li3Li2-89.8(4) C22Si8O8K3-0.3(4)
K3O11BC33BC34B-171(9) C22Si8O8K4-109.9(4)
K3O11BC36BC35B136(11) C22Si8O8Li3128.3(7)
K3O11AC33AC34A-171(2) C23Si8O8K3-120.0(3)
K3O11AC36AC35A148(3) C23Si8O8K4130.5(3)
K4O3Li2K1-151.07(12) C23Si8O8Li38.7(7)
K4O3Li2K2-103.4(4) C24Si8O8K3118.8(3)
K4O3Li2O2-177.7(5) C24Si8O8K49.3(3)
K4O3Li2O5-22.9(4) C24Si8O8Li3-112.6(7)
K4O3Li2Li3-44.8(2) Li1O4Li4K1-73.0(4)
K4O3Li2Li4-74.4(3) Li1O4Li4K375.8(4)
K4O5Li3K2-149.36(12) Li1O4Li4K428.2(7)
K4O5Li3K3-45.7(4) Li1O4Li4O3-51.8(6)
K4O5Li3O6-128.6(5) Li1O4Li4O7103.2(5)
K4O5Li3O827.6(4) Li1O4Li4Li2-30.1(5)
K4O5Li3Li1-105.4(3) Li2O5Li3K2-74.8(3)
K4O5Li3Li2-74.5(4) Li2O5Li3K328.8(7)
K4O7Li4K3-95.45(10) Li2O5Li3K474.5(4)
K4O7Li4O329.8(4) Li2O5Li3O6-54.1(6)
K4O7Li4O4-125.2(5) Li2O5Li3O8102.2(5)
K4O7Li4Li1-89.2(4) Li2O5Li3Li1-30.9(5)
K4O7Li4Li2-2.5(4) Li3O6Li1K1-31.5(7)
K4O8Li3K395.32(10) Li3O6Li1K2-76.3(4)
K4O8Li3O5-30.4(5) Li3O6Li1K372.8(4)
K4O8Li3O6125.9(4) Li3O6Li1O1-102.5(6)
K4O8Li3Li192.0(4) Li3O6Li1O451.9(7)
K4O8Li3Li25.5(4) Li3O6Li1Li429.6(5)
K4O10BC29BC30B167(5) Li4O3Li2K1-76.7(4)
K4O10BC32BC31B-158(4) Li4O3Li2K2-29.0(6)
K4O10AC29AC30A122(2) Li4O3Li2K474.4(3)
K4O10AC32AC31A-133.7(17) Li4O3Li2O2-103.4(5)
Si1O1Li1K1135.1(6) Li4O3Li2O551.5(6)
Si1O1Li1K2-129.4(6) Li4O3Li2Li329.6(5)
Si1O1Li1O4104.1(7) Li4O4Li1K177.7(4)
Si1O1Li1O6-101.2(7) Li4O4Li1K234.2(7)
Si1O1Li1Li3-136.0(5) Li4O4Li1K3-70.1(4)
Si1O1Li1Li4138.2(5) Li4O4Li1O1105.8(5)
Si2O2Li2K1-139.7(5) Li4O4Li1O6-49.1(7)
Si2O2Li2K2124.8(5) Li4O4Li1Li3-25.7(5)
Si2O2Li2O3-111.0(6) O9BC25BC26BC27B-39(4)
Si2O2Li2O594.0(7) O10BC29BC30BC31B-3(8)
Si2O2Li2Li3128.1(5) O11BC33BC34BC35B48(9)
Si2O2Li2Li4-145.4(4) O12BC37BC38BC39B35(3)
Si3O3Li2K197.9(3) C25BO9BC28BC27B2(5)
Si3O3Li2K2145.7(3) C25BC26BC27BC28B39(5)
Si3O3Li2K4-111.0(3) C26BC27BC28BO9B-26(6)
Si3O3Li2O271.3(6) C28BO9BC25BC26B23(4)
Si3O3Li2O5-133.9(4) C29BO10BC32BC31B10(8)
Si3O3Li2Li3-155.8(3) C29BC30BC31BC32B7(6)
Si3O3Li2Li4174.7(5) C30BC31BC32BO10B-11(6)
Si4O4Li1K1-105.4(2) C32BO10BC29BC30B-3(8)
Si4O4Li1K2-148.9(4) C33BO11BC36BC35B-35(11)
Si4O4Li1K3106.9(2) C33BC34BC35BC36B-62(4)
Si4O4Li1O1-77.3(5) C34BC35BC36BO11B65(10)
Si4O4Li1O6127.8(4) C36BO11BC33BC34B0(12)
Si4O4Li1Li3151.2(2) C37BO12BC40BC39B-12(3)
Si4O4Li1Li4176.9(5) C37BC38BC39BC40B-39(2)
Si4O4Li4K1110.5(3) C38BC39BC40BO12B34(3)
Si4O4Li4K3-100.7(3) C40BO12BC37BC38B-16(3)
Si4O4Li4K4-148.3(3) O9AC25AC26AC27A-37(4)
Si4O4Li4O3131.7(4) O10AC29AC30AC31A34(2)
Si4O4Li4O7-73.3(6) O11AC33AC34AC35A22(3)
Si4O4Li4Li1-176.5(6) O12AC37AC38AC39A7(9)
Si4O4Li4Li2153.4(3) C25AO9AC28AC27A-27(3)
Si5O5Li3K2114.5(3) C25AC26AC27AC28A22(5)
Si5O5Li3K3-141.8(4) C26AC27AC28AO9A3(5)
Si5O5Li3K4-96.1(3) C28AO9AC25AC26A39(3)
Si5O5Li3O6135.2(4) C29AO10AC32AC31A32.0(19)
Si5O5Li3O8-68.5(6) C29AC30AC31AC32A-14(3)
Si5O5Li3Li1158.4(3) C30AC31AC32AO10A-11(3)
Si5O5Li3Li2-170.7(6) C32AO10AC29AC30A-42.6(19)
Si6O6Li1K1149.5(3) C33AO11AC36AC35A-21(4)
Si6O6Li1K2104.7(3) C33AC34AC35AC36A-33.3(17)
Si6O6Li1K3-106.2(3) C34AC35AC36AO11A34(3)
Si6O6Li1O178.5(6) C36AO11AC33AC34A-1(5)
Si6O6Li1O4-127.1(4) C37AO12AC40AC39A44(6)
Si6O6Li1Li3-179.0(6) C37AC38AC39AC40A19(9)
Si6O6Li1Li4-149.4(3) C38AC39AC40AO12A-33(6)
Si7O7Li4K3130.1(6) C40AO12AC37AC38A-26(6)
Si7O7Li4K4-134.4(6)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3167tri.
AtomxyzU(eq)
H1A1202822742017122
H1B1295120102179122
H1C1192117272238122
H2A1351415111336162
H2B1399318421613162
H2C1312421391437162
H3A127385352054116
H3B137318792028116
H3C133544961753116
H4A13301764593125
H4B14143331691125
H4C13712787926125
H5A12075-858613120
H5B13142-716507120
H5C12268-335383120
H6A13397-2011347110
H6B13812-6481105110
H6C12785-7611251110
H7A11515926348130
H7B1101395027130
H7C10920376229130
H8A92622074426113
H8B100312023163113
H8C103782074503113
H9A8800411200107
H9B8932947-27107
H9C82521015258107
H10A887728721004131
H10B883633001286131
H10C817927271277131
H11A1145425661389151
H11B1096431951356151
H11C1101127631076151
H12A905523951880139
H12B969829731862139
H12C1019123481910139
H13A8524-1242144293
H13B8505-1645115093
H13C7965-1028115093
H14A11243-1162114897
H14B10562-1719119097
H14C10675-1253145597
H15A9112-73958696
H15B9622-136361796
H15C10253-78159696
H16A811812242223164
H16B79806442419164
H16C76186612080164
H17A108706052265214
H17B101316432537214
H17C1029511982326214
H18A8710-4342008190
H18B9000-3602351190
H18C9809-4702105190
H19A574316711219104
H19B547022271019104
H19C634622641248104
H20A64851137390111
H20B55121398522111
H20C6022859685111
H21A7383270168598
H21B6464254448998
H21C7485228040298
H22A60326671850171
H22B51423101719171
H22C56418091522171
H23A7007-9741712118
H23B5962-7931824118
H23C6885-5061975118
H24A5800-371036125
H24B5388-5651232125
H24C6399-6301068125
H25A125891632296134
H25B121802255185134
H26A140671993365111
H26B13736232665111
H27A132813123318228
H27B142372931495228
H28A133902522882139
H28B125892981781139
H29A6905-1129707152
H29B7588-1167416152
H30A6269-1481120185
H30B5604-1475412185
H31A5479-714-45100
H31B4906-659267100
H32A6498-999295
H32B58244536895
H33A66801912232093
H33B57961742210593
H35A525331471953112
H35B516024541869112
H37A12977-10061761170
H37B12282-15431829170
H38A13640-10402226148
H38B13433-17302165148
H39A11918-16782380149
H39B12507-12532600149
H40A11010-8382338172
H40B11929-4172371172
H1116682507316250
H2120782932574250
H3131253122195129
H413122244984129
H5143902368380131
H6140932931574131
H7135002420881158
H8138541859699158
H97147-124164776
H107320-130929476
H115563-1097589104
H125765-1550319104
H135644-854-19134
H145175-460239134
H15636211519174
H166923-347-1774
H1760521623219695
H1855011767189195
H19562224622404106
H1D477824452158106
H1E562530391827105
H1F599933112138105
H1G722528971772101
H1H738127892124101
H37C13347-5172114199
H37D13349-10331863199
H39C11698-19122349236
H39D11451-12752489236

 

Table 8 Atomic Occupancy for 3167tri.
AtomOccupancy AtomOccupancy AtomOccupancy
O9B0.45(2) O10B0.30(4) O11B0.20(3)
O12B0.58(2) C25B0.45(2) H25A0.45(2)
H25B0.45(2) C26B0.45(2) H26A0.45(2)
H26B0.45(2) C27B0.45(2) H27A0.45(2)
H27B0.45(2) C28B0.45(2) H28A0.45(2)
H28B0.45(2) C29B0.30(4) H29A0.30(4)
H29B0.30(4) C30B0.30(4) H30A0.30(4)
H30B0.30(4) C31B0.30(4) H31A0.30(4)
H31B0.30(4) C32B0.30(4) H32A0.30(4)
H32B0.30(4) C33B0.20(3) H33A0.20(3)
H33B0.20(3) C34B0.20(3) C35B0.20(3)
H35A0.20(3) H35B0.20(3) C36B0.20(3)
C37B0.58(2) H37A0.58(2) H37B0.58(2)
C38B0.58(2) H38A0.58(2) H38B0.58(2)
C39B0.58(2) H39A0.58(2) H39B0.58(2)
C40B0.58(2) H40A0.58(2) H40B0.58(2)
O9A0.55(2) O10A0.70(4) O11A0.80(3)
O12A0.42(2) C25A0.55(2) H10.55(2)
H20.55(2) C26A0.55(2) H30.55(2)
H40.55(2) C27A0.55(2) H50.55(2)
H60.55(2) C28A0.55(2) H70.55(2)
H80.55(2) C29A0.70(4) H90.70(4)
H100.70(4) C30A0.70(4) H110.70(4)
H120.70(4) C31A0.70(4) H130.70(4)
H140.70(4) C32A0.70(4) H150.70(4)
H160.70(4) C33A0.80(3) H170.80(3)
H180.80(3) C34A0.80(3) H190.80(3)
H1D0.80(3) C35A0.80(3) H1E0.80(3)
H1F0.80(3) C36A0.80(3) H1G0.80(3)
H1H0.80(3) C37A0.42(2) H37C0.42(2)
H37D0.42(2) C38A0.42(2) C39A0.42(2)
H39C0.42(2) H39D0.42(2) C40A0.42(2)

Experimental

Single crystals of C40H104K4Li4O12Si8 [3167tri] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 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 [3167tri]

Crystal Data for C40H104K4Li4O12Si8 (=1186.11 g/mol): orthorhombic, space group Pbca (no. 61), a = 13.9966(5) Å, b = 22.8582(8) Å, c = 44.793(2) Å, = 14330.9(10) Å3, Z = 8, T = 173.15 K, μ(MoKα) = 0.424 mm-1, Dcalc = 1.099 g/cm3, 189441 reflections measured (4.368° ≤ 2Θ ≤ 51.998°), 14062 unique (Rint = 0.1146, Rsigma = 0.0569) which were used in all calculations. The final R1 was 0.0796 (I > 2σ(I)) and wR2 was 0.1933 (all data).

Refinement model description

Number of restraints - 470, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Rigid bond restraints
O9B, C25B, C26B, C27B, C28B, O9A, C25A, C26A, C27A, C28A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
O10B, C29B, C30B, C31B, C32B, O10A, C29A, C30A, C31A, C32A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
O12B, C37B, C38B, C39B, C40B, O12A, C37A, C38A, C39A, C40A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
O11B, C33B, C34B, C35B, C36B, O11A, C33A, C34A, C35A, C36A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O11B ≈ C33B ≈ C34B ≈ C35B ≈ C36B ≈ O11A ≈ C33A ≈
C34A ≈ C35A ≈ C36A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O9A) ≈ Ueq, Uanis(C27A) ≈ Ueq, Uanis(C28A) ≈ Ueq, Uanis(C26A)
≈ Ueq, Uanis(C25A) ≈ Ueq, Uanis(C28B) ≈ Ueq, Uanis(C27B) ≈ Ueq,
Uanis(C26B) ≈ Ueq, Uanis(C25B) ≈ Ueq, Uanis(O9B) ≈ Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(O10A) ≈ Ueq, Uanis(C31A) ≈ Ueq, Uanis(C30A) ≈ Ueq,
Uanis(C29A) ≈ Ueq, Uanis(C32A) ≈ Ueq, Uanis(O10B) ≈ Ueq,
Uanis(C29B) ≈ Ueq, Uanis(C30B) ≈ Ueq, Uanis(C31B) ≈ Ueq,
Uanis(C32B) ≈ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O12B) ≈ Ueq, Uanis(C40B) ≈ Ueq, Uanis(C39B) ≈ Ueq,
Uanis(C38B) ≈ Ueq, Uanis(C37B) ≈ Ueq, Uanis(O12A) ≈ Ueq,
Uanis(C37A) ≈ Ueq, Uanis(C38A) ≈ Ueq, Uanis(C39A) ≈ Ueq,
Uanis(C40A) ≈ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O11A) ≈ Ueq, Uanis(C33A) ≈ Ueq, Uanis(C34A) ≈ Ueq,
Uanis(C35A) ≈ Ueq, Uanis(C36A) ≈ Ueq, Uanis(O11B) ≈ Ueq,
Uanis(C36B) ≈ Ueq, Uanis(C35B) ≈ Ueq, Uanis(C34B) ≈ Ueq,
Uanis(C33B) ≈ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
Sof(O9B)=Sof(C25B)=Sof(H25A)=Sof(H25B)=Sof(C26B)=Sof(H26A)=Sof(H26B)=
Sof(C27B)=Sof(H27A)=Sof(H27B)=Sof(C28B)=Sof(H28A)=Sof(H28B)=1-FVAR(1)
Sof(O9A)=Sof(C25A)=Sof(H1)=Sof(H2)=Sof(C26A)=Sof(H3)=Sof(H4)=Sof(C27A)=
Sof(H5)=Sof(H6)=Sof(C28A)=Sof(H7)=Sof(H8)=FVAR(1)
Sof(O11B)=Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(C34B)=Sof(C35B)=Sof(H35A)=
Sof(H35B)=Sof(C36B)=1-FVAR(2)
Sof(O11A)=Sof(C33A)=Sof(H17)=Sof(H18)=Sof(C34A)=Sof(H19)=Sof(H1D)=Sof(C35A)=
Sof(H1E)=Sof(H1F)=Sof(C36A)=Sof(H1G)=Sof(H1H)=FVAR(2)
Sof(O10A)=Sof(C29A)=Sof(H9)=Sof(H10)=Sof(C30A)=Sof(H11)=Sof(H12)=Sof(C31A)=
Sof(H13)=Sof(H14)=Sof(C32A)=Sof(H15)=Sof(H16)=1-FVAR(3)
Sof(O10B)=Sof(C29B)=Sof(H29A)=Sof(H29B)=Sof(C30B)=Sof(H30A)=Sof(H30B)=
Sof(C31B)=Sof(H31A)=Sof(H31B)=Sof(C32B)=Sof(H32A)=Sof(H32B)=FVAR(3)
Sof(O12A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(C39A)=Sof(H39C)=
Sof(H39D)=Sof(C40A)=1-FVAR(4)
Sof(O12B)=Sof(C37B)=Sof(H37A)=Sof(H37B)=Sof(C38B)=Sof(H38A)=Sof(H38B)=
Sof(C39B)=Sof(H39A)=Sof(H39B)=Sof(C40B)=Sof(H40A)=Sof(H40B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
C25B(H25A,H25B), C26B(H26A,H26B), C27B(H27A,H27B), C28B(H28A,H28B), C29B(H29A,
H29B), C30B(H30A,H30B), C31B(H31A,H31B), C32B(H32A,H32B), C33B(H33A,H33B),
C35B(H35A,H35B), C37B(H37A,H37B), C38B(H38A,H38B), C39B(H39A,H39B), C40B(H40A,
H40B), C25A(H1,H2), C26A(H3,H4), C27A(H5,H6), C28A(H7,H8), C29A(H9,H10),
C30A(H11,H12), C31A(H13,H14), C32A(H15,H16), C33A(H17,H18), C34A(H19,H1D),
C35A(H1E,H1F), C36A(H1G,H1H), C37A(H37C,H37D), C39A(H39C,H39D)
5.b Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
H24C)

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