B0988

Table 1 Crystal data and structure refinement for B0988.
Identification code B0988
Empirical formula C40H108K2Li8N2O2Si8
Formula weight 1007.72
Temperature/K 100.0
Crystal system monoclinic
Space group P21/c
a/Å 21.4528(12)
b/Å 17.1385(8)
c/Å 20.4255(11)
α/° 90
β/° 115.646(2)
γ/° 90
Volume/Å3 6770.0(6)
Z 4
ρcalcg/cm3 0.989
μ/mm‑1 0.309
F(000) 2208.0
Crystal size/mm3 0.53 × 0.49 × 0.39
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.496 to 62
Index ranges -31 ≤ h ≤ 31, -24 ≤ k ≤ 24, -29 ≤ l ≤ 29
Reflections collected 226422
Independent reflections 21569 [Rint = 0.0402, Rsigma = 0.0201]
Data/restraints/parameters 21569/0/651
Goodness-of-fit on F2 1.044
Final R indexes [I>=2σ (I)] R1 = 0.0421, wR2 = 0.1079
Final R indexes [all data] R1 = 0.0535, wR2 = 0.1162
Largest diff. peak/hole / e Å-3 2.19/-0.59

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for B0988. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
K18067.6(2)3503.2(2)3805.2(2)25.03(6)
K26464.8(2)5892.1(2)2492.9(2)25.67(6)
Si68481.0(2)5332.3(2)4968.7(2)22.27(8)
Si36146.1(2)4105.2(2)1201.7(2)20.83(7)
Si78613.5(2)7057.7(2)2519.1(2)22.31(8)
Si55640.1(2)5701.4(2)3798.5(2)22.25(8)
Si46369.0(2)2418.3(2)3374.1(2)25.62(8)
Si86046.3(2)7777.5(2)1297.9(2)23.72(8)
Si29197.7(2)4273.2(3)2229.2(2)27.98(9)
Si19096.1(2)1525.5(3)4466.5(3)34.13(10)
O27636.4(5)7254.0(5)3867.2(6)25.07(19)
O17825.6(5)2674.8(6)2038.0(5)24.64(19)
N17760.2(7)999.2(8)2074.2(8)33.2(3)
N26983.0(8)8605.8(7)4115.9(8)35.1(3)
C297787.4(7)5331.6(8)4047.2(7)22.4(2)
C136869.9(7)4186.6(7)2108.5(7)20.6(2)
C177011.9(7)2143.2(8)3044.7(8)24.4(3)
C145291.4(7)4550.3(9)1054.0(8)28.3(3)
C98848.5(7)4154.2(9)2898.5(8)26.8(3)
C349423.9(8)6724.7(10)3316.1(9)33.9(3)
C368503.1(8)8130.9(9)2672.6(9)30.7(3)
C266118.4(8)5159.8(8)4677.8(8)29.5(3)
C337878.9(8)6500.6(8)2508.8(8)25.1(3)
C256118.5(8)6567.7(8)3725.4(8)24.8(3)
C358748.0(9)7001.6(10)1666.9(9)34.5(3)
C218026.2(8)7817.0(9)4397.8(9)31.5(3)
C328166.8(9)5844.7(9)5586.8(8)32.2(3)
C308844.7(10)4361.4(10)5406.0(9)37.4(4)
C195580.2(8)2869.5(9)2635.9(10)32.7(3)
C17735.7(9)2230.2(10)1416.6(9)34.3(3)
C275491.8(8)4981.0(9)3045.4(9)31.1(3)
C165941.5(8)3042.2(9)949.9(9)34.2(3)
C59026.1(8)2125.8(9)3689.9(9)31.6(3)
C186734.5(9)3154.8(10)4139.5(9)34.0(3)
C405810.5(8)6756.2(9)918.5(10)34.6(3)
C385258.7(9)8392.7(10)781.6(9)36.2(3)
C396733.5(8)8107.3(9)1019.7(9)30.9(3)
C284741.3(8)5904.1(10)3708.7(10)33.4(3)
C27396.7(9)1443.3(10)1401.9(10)38.5(4)
C376358.3(9)7807.0(11)2290.6(9)34.1(3)
C156408.8(9)4540.8(11)515.5(9)35.2(3)
C119913.4(9)4984.3(12)2389.4(11)43.8(4)
C319241.3(9)5899.5(12)4992.5(11)43.4(4)
C128460.1(9)4538.8(12)1330.0(10)39.9(4)
C109550.6(9)3298.7(12)2118.0(12)43.2(4)
C227690.1(9)8618.3(9)4226.5(10)36.6(3)
C37329.4(10)329.4(10)2078.3(12)47.6(5)
C810004.2(11)1272.3(14)5135.5(13)58.4(6)
C68708.4(11)2048.7(11)5015.7(10)44.3(4)
C48426.9(10)707.9(13)2136.9(12)49.9(5)
C78624.3(11)571.7(10)4168.0(12)47.0(5)
C206044.1(13)1585.1(11)3739.8(14)53.4(5)
C236636.1(12)9343.2(10)3796.5(13)50.4(5)
C246924.2(12)8473.7(12)4801.0(11)47.2(5)
Li37828.5(13)3807.1(15)2085.5(14)26.4(5)
Li17940.7(13)1892.2(15)2843.4(15)27.7(5)
Li28750.6(13)2889.2(16)2780.9(16)30.3(5)
Li46997.9(12)2901.3(14)2195.0(13)24.4(4)
Li56646.3(14)7584.6(15)3458.9(15)28.7(5)
Li67221.9(13)6364.3(14)4157.6(13)25.9(5)
Li87412.4(14)7440.9(14)2835.8(14)28.1(5)
Li78069.5(13)6384.9(15)3634.1(14)27.4(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for B0988. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
K127.36(14)21.56(12)24.47(14)-2.08(10)9.64(11)0.95(10)
K228.66(14)23.81(13)25.51(14)-0.36(10)12.63(12)1.88(10)
Si623.13(17)20.86(16)18.50(17)1.96(13)4.96(14)3.29(13)
Si318.94(16)19.35(15)19.19(17)-1.29(12)3.54(13)2.20(12)
Si721.47(16)22.49(16)22.75(18)2.95(13)9.37(14)0.88(13)
Si522.82(17)20.58(16)22.13(17)-0.72(13)8.57(14)3.07(13)
Si427.74(19)19.15(16)34.9(2)-0.30(14)18.24(17)-1.14(13)
Si825.48(18)22.53(17)21.44(18)5.30(13)8.55(15)4.35(13)
Si218.06(16)33.1(2)33.3(2)-5.46(16)11.58(16)-1.43(14)
Si129.8(2)23.80(19)35.9(2)4.07(16)2.17(18)5.79(15)
O231.0(5)17.5(4)24.6(5)-2.3(3)10.0(4)-1.3(4)
O124.5(5)25.0(4)25.2(5)-6.9(4)11.5(4)1.2(4)
N127.8(6)26.6(6)41.2(8)-12.9(5)11.1(6)4.6(5)
N259.3(9)21.4(5)31.4(7)2.1(5)26.0(7)12.9(6)
C2924.9(6)19.4(5)19.2(6)1.6(4)6.2(5)2.7(5)
C1318.2(5)19.5(5)21.0(6)-2.9(4)5.7(5)-0.7(4)
C1724.2(6)19.2(5)29.3(7)-0.6(5)11.1(5)2.2(5)
C1421.3(6)28.9(7)27.2(7)-1.4(5)3.5(5)4.8(5)
C920.8(6)28.8(6)30.1(7)-4.1(5)10.1(6)-0.6(5)
C3430.0(7)35.2(8)31.3(8)7.1(6)8.3(6)3.8(6)
C3628.5(7)24.2(6)36.3(8)0.9(6)11.2(6)-1.0(5)
C2632.4(7)23.7(6)27.0(7)3.0(5)7.8(6)-0.6(5)
C3326.0(6)21.1(6)29.1(7)1.3(5)12.6(6)-0.4(5)
C2528.2(6)19.9(6)25.9(7)2.2(5)11.3(6)2.7(5)
C3538.1(8)40.1(8)28.8(8)1.0(6)17.8(7)-4.1(7)
C2134.6(8)23.8(6)30.9(8)-5.1(5)9.3(6)-3.4(5)
C3244.0(9)26.5(7)25.0(7)-0.8(5)14.0(6)4.5(6)
C3043.8(9)29.7(7)24.8(7)3.4(6)1.7(7)13.7(6)
C1921.7(6)29.7(7)44.8(9)-8.2(6)12.7(6)-2.3(5)
C136.0(8)38.9(8)30.1(8)-11.1(6)16.4(7)0.8(6)
C2733.2(7)29.8(7)31.1(7)-8.2(6)14.6(6)-2.9(6)
C1628.7(7)24.4(6)32.6(8)-7.9(6)-2.4(6)0.9(5)
C522.9(6)29.3(7)36.7(8)-0.7(6)7.2(6)2.7(5)
C1833.9(8)37.2(8)34.2(8)-5.5(6)17.8(7)2.2(6)
C4028.2(7)26.3(7)39.2(9)1.6(6)5.2(6)-2.3(5)
C3834.1(8)38.7(8)32.2(8)11.9(7)10.9(7)13.1(6)
C3932.6(7)29.6(7)29.3(7)6.5(6)12.3(6)-0.5(6)
C2828.7(7)34.9(8)39.2(8)3.7(6)17.1(7)6.0(6)
C239.1(8)34.9(8)36.3(9)-17.2(7)11.3(7)0.0(7)
C3736.9(8)41.1(8)25.5(7)9.1(6)14.7(6)15.4(7)
C1536.9(8)42.5(9)26.4(7)4.9(6)13.9(6)7.2(7)
C1130.4(8)55.0(11)50.9(11)-10.2(9)22.2(8)-13.3(7)
C3131.5(8)51.3(10)42.1(10)-0.7(8)11.0(7)-9.4(7)
C1231.9(8)50.9(10)34.5(9)-2.1(7)12.3(7)1.2(7)
C1033.5(8)46.9(10)54.5(11)-7.0(8)24.0(8)7.9(7)
C2247.2(9)23.1(6)41.5(9)-6.4(6)21.2(8)-10.7(6)
C344.7(10)28.1(8)60.0(12)-15.5(8)13.2(9)-0.9(7)
C839.1(10)50.5(11)58.6(13)9.3(10)-4.1(9)12.7(9)
C658.3(11)34.8(8)34.7(9)9.1(7)15.4(8)9.3(8)
C436.8(9)50.9(11)57.3(12)-20.8(9)15.9(9)13.9(8)
C748.1(10)26.2(7)53.2(11)3.9(7)9.4(9)0.9(7)
C2068.6(13)33.6(9)82.5(16)9.7(9)55.7(13)-1.9(9)
C2360.4(12)26.5(8)70.6(14)1.6(8)34.1(11)9.5(8)
C2464.7(13)42.2(9)48.9(11)-12.6(8)38.0(10)-10.0(9)
Li323.7(11)27.5(11)28.0(12)-1.2(9)11.2(10)0.6(9)
Li124.3(11)24.4(11)32.2(13)-4.6(10)10.2(10)3.4(9)
Li223.6(11)29.9(12)37.3(14)-2.4(10)13.1(11)2.2(9)
Li421.4(10)22.9(10)25.8(12)-1.6(9)7.5(9)1.6(8)
Li534.3(13)25.1(11)29.5(13)2.5(10)16.5(11)5.4(10)
Li629.7(12)21.3(10)21.8(11)0.7(9)6.5(10)2.7(9)
Li835.7(13)22.6(11)27.5(12)2.4(9)15.0(11)2.3(9)
Li726.4(12)24.9(11)27.9(12)1.6(9)8.9(10)-0.5(9)

 

Table 4 Bond Lengths for B0988.
AtomAtomLength/Å AtomAtomLength/Å
K1Si63.7997(5) Si2C101.8877(18)
K1Si43.8384(5) Si2Li32.933(2)
K1C293.2685(13) Si2Li22.958(3)
K1C133.5037(14) Si1C51.8415(18)
K1C173.1510(15) Si1C81.883(2)
K1C93.1885(15) Si1C61.887(2)
K1C53.2055(16) Si1C71.8800(19)
K1Li33.363(3) O2C211.4215(17)
K1Li13.331(2) O2Li51.999(3)
K1Li23.207(3) O2Li61.981(3)
K1Li43.258(2) O2Li81.974(3)
K2Si33.9041(5) O2Li71.921(3)
K2Si53.7988(5) O1C11.4202(17)
K2Si83.9126(5) O1Li31.943(3)
K2C293.3548(14) O1Li12.053(3)
K2C133.2414(13) O1Li21.941(3)
K2C333.1948(14) O1Li41.975(3)
K2C253.1382(15) N1C21.465(2)
K2C373.3032(18) N1C31.476(2)
K2Li53.434(3) N1C41.467(2)
K2Li63.174(2) N1Li12.106(3)
K2Li83.231(3) N2C221.434(2)
K2Li73.324(3) N2C231.468(2)
Si6C291.8255(14) N2C241.476(2)
Si6C321.8857(16) N2Li52.132(3)
Si6C301.8900(16) C29Li62.212(3)
Si6C311.8812(18) C29Li72.186(3)
Si6Li63.049(2) C13Li32.177(3)
Si6Li73.063(3) C13Li42.218(3)
Si3C131.8363(14) C17Li12.244(3)
Si3C141.8857(14) C17Li42.158(3)
Si3C161.8923(15) C9Li32.180(3)
Si3C151.8770(17) C9Li22.181(3)
Si3Li42.916(2) C33Li82.150(3)
Si7C341.8837(16) C33Li72.162(3)
Si7C361.8978(15) C25Li52.269(3)
Si7C331.8349(14) C25Li62.167(3)
Si7C351.8861(16) C21C221.520(2)
Si7Li82.989(3) C1C21.526(2)
Si5C261.8828(15) C5Li12.255(3)
Si5C251.8472(14) C5Li22.135(3)
Si5C271.8889(15) C2Li12.766(3)
Si5C281.8884(16) C37Li52.224(3)
Si4C171.8386(14) C37Li82.137(3)
Si4C191.8779(17) Li3Li22.444(4)
Si4C181.8951(17) Li3Li42.445(4)
Si4C201.8798(18) Li1Li22.479(4)
Si8C401.8922(16) Li1Li42.553(3)
Si8C381.8805(16) Li2Li43.417(3)
Si8C391.8817(16) Li5Li62.532(3)
Si8C371.8405(17) Li5Li82.489(4)
Si2C91.8324(16) Li6Li83.437(4)
Si2C111.8749(17) Li6Li72.477(4)
Si2C121.8891(18) Li8Li72.435(4)

 

Table 5 Bond Angles for B0988.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Si6K1Si4118.984(11) Li7C29K270.15(8)
C29K1Si628.69(2) Li7C29Li668.55(10)
C29K1Si4106.30(3) K2C13K1102.74(4)
C29K1C1374.03(3) Si3C13K1155.55(6)
C29K1Li393.13(5) Si3C13K296.58(5)
C29K1Li1155.58(5) Si3C13Li3110.48(9)
C13K1Si6102.45(2) Si3C13Li491.52(8)
C13K1Si473.62(2) Li3C13K168.05(8)
C17K1Si6147.35(3) Li3C13K2129.02(8)
C17K1Si428.38(3) Li3C13Li467.62(10)
C17K1C29130.07(4) Li4C13K164.95(7)
C17K1C1372.35(3) Li4C13K2155.99(9)
C17K1C9114.76(4) Si4C17K197.06(6)
C17K1C576.47(4) Si4C17Li1169.31(11)
C17K1Li381.23(5) Si4C17Li4112.85(9)
C17K1Li140.38(5) Li1C17K174.12(7)
C17K1Li282.50(5) Li4C17K173.02(7)
C17K1Li439.30(5) Li4C17Li170.87(10)
C9K1Si692.03(3) Si2C9K1163.62(7)
C9K1Si4136.18(3) Si2C9Li393.54(9)
C9K1C2985.96(4) Si2C9Li294.56(10)
C9K1C1369.71(4) Li3C9K174.96(8)
C9K1C572.54(4) Li3C9Li268.16(11)
C9K1Li338.76(5) Li2C9K170.51(8)
C9K1Li182.93(5) Si7C33K2167.70(7)
C9K1Li239.88(6) Si7C33Li896.85(9)
C9K1Li480.91(5) Si7C33Li7105.61(10)
C5K1Si6132.07(3) Li8C33K271.35(8)
C5K1Si4101.65(3) Li8C33Li768.77(11)
C5K1C29152.00(4) Li7C33K273.90(8)
C5K1C13113.12(4) Si5C25K295.79(5)
C5K1Li381.38(5) Si5C25Li5171.50(11)
C5K1Li140.31(5) Si5C25Li6112.64(9)
C5K1Li238.90(6) Li5C25K277.00(8)
C5K1Li483.49(5) Li6C25K270.81(8)
Li3K1Si6114.47(4) Li6C25Li569.56(10)
Li3K1Si497.76(4) O2C21C22111.95(13)
Li3K1C1336.89(5) O1C1C2111.77(14)
Li1K1Si6171.97(4) Si1C5K199.43(7)
Li1K1Si468.66(4) Si1C5Li1103.50(10)
Li1K1C1381.72(5) Si1C5Li2168.56(11)
Li1K1Li364.90(6) Li1C5K172.83(7)
Li2K1Si6129.04(5) Li2C5K170.59(8)
Li2K1Si4110.36(5) Li2C5Li168.70(11)
Li2K1C29125.39(6) N1C2C1112.63(14)
Li2K1C1379.10(5) N1C2Li148.58(9)
Li2K1Li343.59(7) C1C2Li175.84(10)
Li2K1Li144.52(7) Si8C37K294.76(7)
Li2K1Li463.81(6) Si8C37Li5167.74(13)
Li4K1Si6139.85(4) Si8C37Li8111.37(10)
Li4K1Si455.32(4) Li5C37K273.95(8)
Li4K1C29111.16(5) Li8C37K269.08(8)
Li4K1C1338.07(5) Li8C37Li569.56(11)
Li4K1Li343.31(6) N2C22C21112.76(13)
Li4K1Li145.58(6) Si2Li3K1104.13(7)
Si3K2Si8107.489(11) O1Li3K183.87(9)
Si5K2Si3114.089(11) O1Li3Si2104.98(10)
Si5K2Si8117.271(11) O1Li3C13108.47(12)
C29K2Si3104.11(2) O1Li3C9106.92(12)
C29K2Si576.77(3) O1Li3Li250.98(9)
C29K2Si8134.31(3) O1Li3Li451.96(9)
C29K2Li581.90(5) C13Li3K175.06(8)
C13K2Si327.86(2) C13Li3Si2146.19(12)
C13K2Si5110.34(3) C13Li3C9123.23(13)
C13K2Si8127.36(3) C13Li3Li2135.59(14)
C13K2C2976.43(3) C13Li3Li456.98(9)
C13K2C37151.27(4) C9Li3K166.28(8)
C13K2Li5157.71(5) C9Li3Si238.57(6)
C13K2Li795.40(5) C9Li3Li255.94(9)
C33K2Si398.67(3) C9Li3Li4129.37(14)
C33K2Si5138.56(3) Li2Li3K164.79(9)
C33K2Si872.38(3) Li2Li3Si266.02(9)
C33K2C2970.94(4) Li2Li3Li488.67(12)
C33K2C1386.78(3) Li4Li3K166.04(8)
C33K2C3771.99(4) Li4Li3Si2154.34(12)
C33K2Li581.22(5) O1Li1K183.21(8)
C33K2Li839.09(5) O1Li1N187.57(11)
C33K2Li738.68(5) O1Li1C17102.31(11)
C25K2Si3142.97(3) O1Li1C5102.98(12)
C25K2Si528.93(3) O1Li1C258.65(8)
C25K2Si897.22(3) O1Li1Li249.64(9)
C25K2C2975.13(4) O1Li1Li449.32(8)
C25K2C13135.10(4) N1Li1K1169.82(13)
C25K2C33115.14(4) N1Li1C17112.64(12)
C25K2C3772.92(4) N1Li1C5119.77(12)
C25K2Li540.08(5) N1Li1C231.45(7)
C25K2Li640.15(5) N1Li1Li2111.67(13)
C25K2Li882.43(5) N1Li1Li4104.88(12)
C25K2Li782.92(5) C17Li1K165.50(7)
C37K2Si3135.43(3) C17Li1C5121.97(13)
C37K2Si598.36(3) C17Li1C2104.44(11)
C37K2Si827.96(3) C17Li1Li2125.10(13)
C37K2C29112.78(4) C17Li1Li452.99(8)
C37K2Li538.48(5) C5Li1K166.86(7)
C37K2Li780.20(5) C5Li1C2133.28(12)
Li5K2Si3173.66(5) C5Li1Li253.35(10)
Li5K2Si568.95(4) C5Li1Li4126.92(13)
Li5K2Si866.37(4) C2Li1K1138.38(10)
Li6K2Si3141.49(4) Li2Li1K165.09(8)
Li6K2Si556.48(5) Li2Li1C296.85(12)
Li6K2Si8109.31(4) Li2Li1Li485.52(11)
Li6K2C2939.48(5) Li4Li1K165.70(8)
Li6K2C13115.02(5) Li4Li1C276.21(10)
Li6K2C3382.09(6) K1Li2Li458.82(6)
Li6K2C3781.74(5) Si2Li2K1107.48(8)
Li6K2Li544.84(6) Si2Li2Li4110.53(9)
Li6K2Li864.91(6) O1Li2K188.33(9)
Li6K2Li744.73(7) O1Li2Si2104.14(12)
Li8K2Si3134.49(5) O1Li2C9106.93(13)
Li8K2Si5111.04(5) O1Li2C5111.61(14)
Li8K2Si853.82(5) O1Li2Li351.03(9)
Li8K2C2980.50(5) O1Li2Li153.68(9)
Li8K2C13125.72(5) O1Li2Li429.52(7)
Li8K2C3738.16(6) C9Li2K169.60(8)
Li8K2Li543.72(6) C9Li2Si238.13(6)
Li8K2Li743.59(6) C9Li2Li355.90(9)
Li7K2Si3119.89(5) C9Li2Li1135.69(13)
Li7K2Si5100.68(5) C9Li2Li494.10(10)
Li7K2Si896.66(4) C5Li2K170.52(9)
Li7K2C2938.21(5) C5Li2Si2144.02(13)
Li7K2Li563.71(6) C5Li2C9122.42(14)
C29Si6K159.28(4) C5Li2Li3138.56(14)
C29Si6C32108.81(7) C5Li2Li157.95(10)
C29Si6C30118.18(7) C5Li2Li499.02(11)
C29Si6C31109.74(8) Li3Li2K171.61(9)
C29Si6Li645.97(6) Li3Li2Si264.96(9)
C29Si6Li744.80(6) Li3Li2Li193.70(12)
C32Si6K1138.47(6) Li3Li2Li445.68(8)
C32Si6C30106.72(8) Li1Li2K170.39(9)
C32Si6Li666.69(7) Li1Li2Si2157.25(13)
C32Si6Li7105.83(7) Li1Li2Li448.15(8)
C30Si6K160.40(5) K1Li4Li257.37(6)
C30Si6Li6148.76(8) Si3Li4K1115.71(8)
C30Si6Li7147.16(7) Si3Li4Li2120.74(9)
C31Si6K1114.06(7) O1Li4K186.34(8)
C31Si6C32107.41(9) O1Li4Si3111.27(11)
C31Si6C30105.47(9) O1Li4C13105.74(12)
C31Si6Li6105.58(8) O1Li4C17108.17(12)
C31Si6Li768.37(8) O1Li4Li350.79(9)
Li6Si6K1103.10(5) O1Li4Li152.04(9)
Li6Si6Li747.81(7) O1Li4Li228.97(7)
Li7Si6K191.72(5) C13Li4K176.98(8)
C13Si3K255.57(4) C13Li4Si339.01(5)
C13Si3C14118.02(6) C13Li4Li355.40(9)
C13Si3C16110.04(6) C13Li4Li1139.23(13)
C13Si3C15109.08(7) C13Li4Li296.52(10)
C13Si3Li449.48(6) C17Li4K167.68(7)
C14Si3K270.40(5) C17Li4Si3140.54(11)
C14Si3C16104.52(7) C17Li4C13128.34(13)
C14Si3Li4132.11(7) C17Li4Li3134.33(13)
C16Si3K2153.00(6) C17Li4Li156.13(9)
C16Si3Li460.64(7) C17Li4Li294.85(10)
C15Si3K299.86(6) Li3Li4K170.65(8)
C15Si3C14107.77(7) Li3Li4Si375.47(9)
C15Si3C16106.81(8) Li3Li4Li191.86(11)
C15Si3Li4120.04(7) Li3Li4Li245.65(8)
Li4Si3K2102.19(5) Li1Li4K168.72(8)
C34Si7C36106.58(8) Li1Li4Si3163.23(12)
C34Si7C35109.23(8) Li1Li4Li246.33(8)
C34Si7Li8116.06(8) O2Li5K280.56(8)
C36Si7Li864.55(7) O2Li5N287.75(12)
C33Si7C34108.61(7) O2Li5C25103.45(12)
C33Si7C36109.77(7) O2Li5C37104.34(12)
C33Si7C35115.89(7) O2Li5Li650.18(9)
C33Si7Li845.59(7) O2Li5Li850.76(9)
C35Si7C36106.37(8) N2Li5K2168.00(12)
C35Si7Li8134.56(8) N2Li5C25123.22(13)
C26Si5K2119.01(5) N2Li5C37113.31(13)
C26Si5C27106.55(7) N2Li5Li6111.94(13)
C26Si5C28107.18(7) N2Li5Li8106.51(13)
C25Si5K255.27(5) C25Li5K262.92(7)
C25Si5C26112.39(7) C25Li5Li653.32(9)
C25Si5C27111.30(7) C25Li5Li8123.72(13)
C25Si5C28115.08(7) C37Li5K267.57(8)
C27Si5K256.64(5) C37Li5C25116.95(14)
C28Si5K2133.01(6) C37Li5Li6125.98(13)
C28Si5C27103.65(8) C37Li5Li853.58(9)
C17Si4K154.56(5) Li6Li5K262.12(8)
C17Si4C19111.71(7) Li8Li5K263.79(8)
C17Si4C18111.38(7) Li8Li5Li686.42(11)
C17Si4C20114.61(8) K2Li6Li858.34(6)
C19Si4K1114.89(5) Si6Li6K2110.88(7)
C19Si4C18107.18(7) Si6Li6Li8111.08(9)
C19Si4C20105.76(10) O2Li6K287.90(9)
C18Si4K158.35(5) O2Li6Si6101.67(10)
C20Si4K1139.05(8) O2Li6C29104.38(12)
C20Si4C18105.69(10) O2Li6C25107.88(12)
C40Si8K255.95(5) O2Li6Li550.81(9)
C38Si8K2136.12(6) O2Li6Li829.57(7)
C38Si8C40105.84(8) O2Li6Li749.55(9)
C38Si8C39107.06(7) C29Li6K274.67(8)
C39Si8K2115.99(5) C29Li6Si636.40(5)
C39Si8C40105.06(8) C29Li6Li5139.36(13)
C37Si8K257.28(6) C29Li6Li895.31(10)
C37Si8C40112.45(8) C29Li6Li755.24(9)
C37Si8C38114.36(8) C25Li6K269.04(8)
C37Si8C39111.43(8) C25Li6Si6150.38(12)
C9Si2C11120.70(8) C25Li6C29129.63(13)
C9Si2C12108.14(7) C25Li6Li557.13(9)
C9Si2C10107.83(8) C25Li6Li894.24(10)
C9Si2Li347.89(7) C25Li6Li7134.31(13)
C9Si2Li247.31(7) Li5Li6K273.03(9)
C11Si2C12106.92(9) Li5Li6Si6152.47(12)
C11Si2C10104.79(9) Li5Li6Li846.27(8)
C11Si2Li3154.61(8) Li7Li6K270.86(9)
C11Si2Li2146.18(9) Li7Li6Si666.39(8)
C12Si2Li365.63(8) Li7Li6Li590.86(12)
C12Si2Li2106.88(8) Li7Li6Li845.10(8)
C10Si2C12107.88(9) K2Li8Li656.75(6)
C10Si2Li3100.57(8) Si7Li8K2107.05(8)
C10Si2Li263.22(8) Si7Li8Li6117.31(9)
Li3Si2Li249.01(7) O2Li8K286.43(9)
C5Si1C8115.27(10) O2Li8Si7111.16(11)
C5Si1C6110.73(8) O2Li8C33106.20(12)
C5Si1C7112.00(9) O2Li8C37108.52(13)
C8Si1C6105.18(11) O2Li8Li551.66(9)
C7Si1C8106.12(10) O2Li8Li629.69(7)
C7Si1C6106.98(10) O2Li8Li750.34(9)
C21O2Li5107.09(11) C33Li8K269.55(8)
C21O2Li6119.11(12) C33Li8Si737.56(6)
C21O2Li8119.66(12) C33Li8Li5137.08(13)
C21O2Li7121.82(12) C33Li8Li694.08(10)
Li6O2Li579.01(11) C33Li8Li755.85(10)
Li8O2Li577.58(11) C37Li8K272.76(9)
Li8O2Li6120.74(12) C37Li8Si7140.23(12)
Li7O2Li5131.07(12) C37Li8C33126.01(14)
Li7O2Li678.78(11) C37Li8Li556.86(10)
Li7O2Li877.39(11) C37Li8Li696.21(11)
C1O1Li3125.22(13) C37Li8Li7137.92(14)
C1O1Li1106.75(12) Li5Li8K272.50(9)
C1O1Li2119.84(12) Li5Li8Si7162.67(13)
C1O1Li4117.82(12) Li5Li8Li647.32(8)
Li3O1Li1128.02(11) Li7Li8K270.25(9)
Li3O1Li477.25(11) Li7Li8Si771.23(9)
Li2O1Li377.99(11) Li7Li8Li592.88(12)
Li2O1Li176.68(12) Li7Li8Li646.08(9)
Li2O1Li4121.51(12) Si6Li7K2106.65(7)
Li4O1Li178.64(11) O2Li7K284.58(9)
C2N1C3109.19(14) O2Li7Si6102.71(11)
C2N1C4111.21(16) O2Li7C29107.47(13)
C2N1Li199.97(11) O2Li7C33107.64(12)
C3N1Li1118.33(14) O2Li7Li651.68(9)
C4N1C3108.90(14) O2Li7Li852.26(9)
C4N1Li1108.94(13) C29Li7K271.65(8)
C22N2C23110.82(15) C29Li7Si636.04(5)
C22N2C24111.82(15) C29Li7Li656.22(9)
C22N2Li599.12(11) C29Li7Li8134.05(14)
C23N2C24108.56(15) C33Li7K267.42(8)
C23N2Li5117.28(15) C33Li7Si6148.11(12)
C24N2Li5109.03(13) C33Li7C29121.97(13)
K1C29K2105.49(4) C33Li7Li6128.59(13)
Si6C29K192.02(5) C33Li7Li855.38(9)
Si6C29K2162.49(6) Li6Li7K264.41(8)
Si6C29Li697.62(9) Li6Li7Si665.80(8)
Si6C29Li799.16(9) Li8Li7K266.16(9)
Li6C29K1158.06(9) Li8Li7Si6153.36(12)
Li6C29K265.84(7) Li8Li7Li688.81(12)
Li7C29K1129.31(9)     

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for B0988.
AtomxyzU(eq)
H14A5144.084336.391409.5242
H14B4943.874428.14562.242
H14C5342.155117.551113.4442
H34A9829.146934.833272.3951
H34B9443.946153.343322.8351
H34C9420.366912.683767.5451
H36A8512.028200.383152.8446
H36B8059.678316.022298.3646
H36C8880.488430.462645.8946
H26A5848.694702.964689.4944
H26B6186.65504.655086.0344
H26C6568.984989.864715.5944
H35A91497319.291726.7352
H35B8335.67198.31254.852
H35C8829.386458.011576.4852
H21A8496.467851.494422.1938
H21B8071.787646.064879.4938
H32A7763.315569.045578.7148
H32B8037.876382.325419.648
H32C8535.975848.976083.2548
H30A8466.484021.825378.1156
H30B9167.514443.515916.1356
H30C9088.754115.545150.5456
H19A5249.73008.452830.1949
H19B5365.752495.512237.5449
H19C5713.363339.962454.6549
H1A8191.572143.51415.7941
H1B7444.612527.25973.0541
H27A5257.465243.112574.7247
H27B5203.574550.373073.147
H27C5937.294775.713097.6147
H16A6341.142789.8926.3551
H16B5541.073004.42475.5151
H16C5836.152781.961317.4351
H18A7169.592956.564518.4951
H18B6402.833239.554344.3851
H18C6820.23649.183951.3951
H40A6224.536426.551111.952
H40B5621.196774.19387.6952
H40C5463.796539.051059.652
H38A5125.618347.16259.7154
H38B5362.638939.16930.2854
H38C4877.378212.47885.6954
H39A7128.337749.891221.0946
H39B6884.868635.241204.5946
H39C6545.188108.7488.7146
H28A4450.636097.973218.8150
H28B4764.976297.584066.8550
H28C4541.965421.943793.8350
H2A6912.921530.451322.5946
H2B7386.071132.77988.4846
H15A6521.65093.48627.6453
H15B6026.964491.7329.1653
H15C6815.054264.44531.2953
H11A9757.275513.072425.866
H11B10041.594960.21983.9166
H11C10315.44851.462842.0966
H31A9624.15867.465479.7965
H31B9108.56446.74872.1565
H31C9387.425679.954638.165
H12A8145.34093.41146.0560
H12B8643.694674.64981.0260
H12C8208.784986.171396.4960
H10A9885.423109.642593.5565
H10B9779.193357.151796.5165
H10C9170.532923.411906.2365
H22A7954.968977.654631.6944
H22B7711.838823.513783.7444
H3A6886.83519.222048.0771
H3B7569.6132.132528.4371
H3C7245.75-7.891660.9971
H8A10241.241008.044881.7488
H8B9989.45926.215510.4788
H8C10254.561750.825362.4388
H6A8943.32549.965184.2466
H6B8765.371728.325435.2966
H6C8215.022139.514712.5766
H4A8350.11368.511722.7475
H4B8657.08411.192588.9975
H4C8718.81149.372140.7975
H7A8134.1672.23857.7270
H7B8669.92272.854595.4670
H7C8823.04272.823895.170
H20A6433.951338.424143.0780
H20B5815.881200.713354.1280
H20C57131781.783912.8880
H23A6874.139775.454123.4876
H23B6154.459322.33725.7476
H23C6648.069424.013327.176
H24A7124.797965.475003.0271
H24B6435.618481.954706.1671
H24C71738885.895148.871
H13A6734(10)4137(11)2499(11)33(5)
H25A6116(12)6944(14)4118(13)50(6)
H37A5953(11)7641(12)2287(11)34(5)
H33A7515(11)6576(12)2077(12)39(5)
H17A7366(12)1866(13)3454(13)47(6)
H137117(11)4645(13)2163(11)41(6)
H5A9319(12)2596(14)3919(12)47(6)
H17B6795(12)1755(14)2693(13)52(6)
H255796(13)6767(14)3280(13)53(7)
H37B6461(13)8402(16)2414(14)64(7)
H5B9293(13)1857(15)3487(13)56(7)
H9A9235(12)4041(13)3400(13)49(6)
H29A7398(11)5051(12)4013(11)38(5)
H29B7908(11)5150(13)3701(12)44(6)
H9B8621(11)4654(13)2931(12)43(6)
H33B7988(11)5944(13)2520(12)43(6)

Experimental

Single crystals of C40H108K2Li8N2O2Si8 [B0988] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 100.0 K during data collection. Using Olex2 [1], the structure was solved with the olex2.solve [2] structure solution program using Charge Flipping and refined with the XL [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. Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H. (2015). Acta Cryst. A71, 59-75.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [B0988]

Crystal Data for C40H108K2Li8N2O2Si8 (=1007.72 g/mol): monoclinic, space group P21/c (no. 14), a = 21.4528(12) Å, b = 17.1385(8) Å, c = 20.4255(11) Å, β = 115.646(2)°, = 6770.0(6) Å3, Z = 4, T = 100.0 K, μ(MoKα) = 0.309 mm-1, Dcalc = 0.989 g/cm3, 226422 reflections measured (4.496° ≤ 2Θ ≤ 62°), 21569 unique (Rint = 0.0402, Rsigma = 0.0201) which were used in all calculations. The final R1 was 0.0421 (I > 2σ(I)) and wR2 was 0.1162 (all data).

Refinement model description

Number of restraints - 0, 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.a Secondary CH2 refined with riding coordinates:
C21(H21A,H21B), C1(H1A,H1B), C2(H2A,H2B), C22(H22A,H22B)
2.b Idealised Me refined as rotating group:
C14(H14A,H14B,H14C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C26(H26A,H26B,
H26C), C35(H35A,H35B,H35C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C19(H19A,
H19B,H19C), C27(H27A,H27B,H27C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C28(H28A,H28B,
H28C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C31(H31A,H31B,H31C), C12(H12A,
H12B,H12C), C10(H10A,H10B,H10C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C6(H6A,H6B,
H6C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C20(H20A,H20B,H20C), C23(H23A,H23B,
H23C), C24(H24A,H24B,H24C)

This report has been created with Olex2, compiled on 2018.05.29 svn.r3508 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.