mo_B1036_0m

Table 1 Crystal data and structure refinement for mo_B1036_0m.
Identification code mo_B1036_0m
Empirical formula C24H54Li2O4Si2
Formula weight 476.73
Temperature/K 100.0
Crystal system triclinic
Space group P-1
a/Å 8.996(2)
b/Å 17.382(4)
c/Å 20.982(6)
α/° 112.633(6)
β/° 93.252(9)
γ/° 93.891(14)
Volume/Å3 3009.2(14)
Z 4
ρcalcg/cm3 1.052
μ/mm‑1 0.141
F(000) 1056.0
Crystal size/mm3 1.34 × 1.2 × 0.98
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.556 to 51.998
Index ranges -11 ≤ h ≤ 11, -21 ≤ k ≤ 21, -25 ≤ l ≤ 25
Reflections collected 58894
Independent reflections 11800 [Rint = 0.0535, Rsigma = 0.0435]
Data/restraints/parameters 11800/0/650
Goodness-of-fit on F2 1.028
Final R indexes [I>=2σ (I)] R1 = 0.0482, wR2 = 0.1107
Final R indexes [all data] R1 = 0.0618, wR2 = 0.1173
Largest diff. peak/hole / e Å-3 0.63/-0.56

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B1036_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Si32227.0(6)5864.9(3)6479.0(2)15.94(11)
Si4-2105.2(6)8859.1(3)8295.0(3)19.81(12)
Si17192.2(6)8249.7(3)3993.3(2)16.00(11)
Si23117.5(6)6422.1(4)890.8(3)23.51(13)
O8-1356.2(15)7100.1(8)6142.6(7)22.8(3)
O51966.0(16)7994.0(8)8903.0(7)27.4(3)
O71730.8(15)8171.9(8)6503.0(7)23.2(3)
O13270.3(15)7087.7(8)3448.5(7)22.0(3)
O46747.0(15)7996.9(8)1522.7(7)22.9(3)
O22757.2(15)8607.9(8)3143.4(7)23.5(3)
O6-753.9(16)6773.9(8)8384.6(7)27.5(3)
O37313.7(15)6373.8(8)1816.6(7)25.3(3)
C272273(2)6101.2(12)5678.5(9)22.5(4)
C16503(2)8246.5(11)3159.9(9)18.1(4)
C48-2050(2)6255.0(12)5881.3(11)25.7(4)
C47-3395(2)6231.1(12)5405.3(10)24.6(4)
C64741(2)6286.5(14)345.4(10)28.7(5)
C132978(2)9402.5(12)3725.7(10)25.6(4)
C122053(2)7317.5(12)3870(1)22.5(4)
C40-1735(2)6093.9(12)7901.0(11)29.4(5)
C45837(2)8662.5(13)4670.3(10)25.0(4)
C251695(2)6729.7(11)7223.4(9)18.1(4)
C176805(2)5558.9(12)1790.1(12)31.9(5)
C53649(2)6740.2(12)1813.7(9)18.3(4)
C45-2370(2)7626.7(12)5992.9(11)25.3(4)
C37-925(2)6773.6(13)9054.7(10)27.9(4)
C31-3669(2)7994.7(14)7912.6(11)31.7(5)
C112168(2)6856.5(13)4351.6(11)29.8(5)
C264134(2)5515.9(13)6605.0(11)28.3(4)
C188160(3)5073.9(13)1692.2(11)33.0(5)
C46-3859(2)7110.1(12)5741.4(11)26.7(4)
C208914(2)6483.6(15)1921.0(14)38.0(6)
C30-1741(2)9050.2(13)9238.5(10)27.0(4)
C39031(2)8884.7(13)4402.9(10)26.7(4)
C93385(2)6223.3(11)3314(1)24.8(4)
C218122(2)7969.8(14)1213.7(11)30.2(5)
C29-437(2)8585.3(11)7840.7(10)18.9(4)
C441283(2)8589.1(14)6072.8(12)33.3(5)
C27521(2)7161.3(12)3913.5(10)25.2(4)
C142032(3)9988.7(13)3543.8(11)32.8(5)
C333094(2)7497.7(12)9019.3(10)26.2(4)
C413022(3)8637.5(16)6937.1(12)40.6(6)
C246136(3)8767.7(15)1628.7(13)42.8(6)
C344218(3)8094.2(14)9591.7(11)35.0(5)
C199406(2)5750.6(13)2069.1(11)30.0(5)
C103155(2)6153.3(13)3997.7(11)28.7(5)
C15933(2)9418.1(13)2947.5(11)29.0(5)
C82009(3)7215.5(18)732.4(12)43.6(6)
C161830(3)8686.9(14)2606.1(12)37.9(6)
C28869(2)4915.5(12)6253.4(10)25.7(4)
C36A2627(9)8842(4)9229(4)28.0(15)
C39-2950(3)5904.9(15)8310.7(12)38.8(5)
C38-2562(3)6563.8(15)9038.5(13)42.5(6)
C32-2979(3)9813.5(15)8290.1(13)41.3(6)
C42A3850(9)9055(5)6538(5)33.4(13)
C237153(3)9229.0(16)1338.5(17)57.9(8)
C71945(3)5381.5(17)460.8(12)49.0(7)
C228115(3)8618(2)912.7(17)60.1(8)
C35B3806(6)8997(3)9611(4)27.3(15)
C432662(3)9090.1(18)6014.0(14)50.3(7)
Li14148(3)7700.1(19)2911.2(16)19.7(6)
Li25975(4)7305.6(19)2031.0(16)20.7(6)
Li3467(4)7559.4(19)8082.0(16)21.7(7)
Li4356(3)7522.4(18)6878.5(16)19.5(6)
C35A3492(8)8844(4)9875(4)38.9(18)
C36B2156(9)8843(4)9436(4)29.1(15)
C42B3470(40)9272(19)6655(14)52(6)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B1036_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Si318.5(3)15.2(2)14.9(2)6.02(19)2.84(19)5.01(19)
Si422.8(3)21.0(3)18.4(3)9.1(2)5.3(2)9.1(2)
Si117.3(3)15.5(2)14.0(2)4.55(19)-0.15(19)2.32(19)
Si216.2(3)37.8(3)13.6(2)7.4(2)1.2(2)-1.2(2)
O822.2(7)15.8(6)27.4(7)6.5(6)-6.1(6)0.6(5)
O532.7(8)17.4(7)25.7(7)2.6(6)-7.7(6)4.1(6)
O724.1(7)22.7(7)26.7(7)15.1(6)-1.1(6)-1.6(5)
O129.7(8)18.0(6)21.7(7)9.3(5)11.1(6)7.8(5)
O425.8(7)22.0(7)24.9(7)11.6(6)10.9(6)6.6(5)
O228.7(8)17.9(7)20.6(7)3.5(5)-2.5(6)9.3(6)
O637.6(8)26.7(7)16.9(7)9.2(6)1.9(6)-8.4(6)
O321.9(7)21.9(7)34.2(8)12.0(6)6.6(6)6.9(6)
C2725(1)24.4(10)18.3(9)8.3(8)3.3(8)3.3(8)
C120(1)17.1(9)17.0(9)6.5(7)1.4(8)1.0(7)
C4824.4(11)16.4(9)33.7(11)7.8(8)-0.7(9)0.0(8)
C4723.9(10)21.1(10)24(1)4.1(8)1.0(8)-0.8(8)
C625.4(11)38.1(12)17(1)4.1(9)6.6(8)2.0(9)
C1327.0(11)19(1)26.4(10)4.0(8)-0.9(8)5.7(8)
C1219.6(10)24.9(10)24.3(10)10.4(8)4.1(8)4.3(8)
C4037.1(12)20.9(10)26.2(11)5.7(9)1.0(9)-1.7(9)
C425.1(11)30.1(11)16.9(9)5.3(8)1.6(8)7.4(8)
C2522.8(10)16.5(9)16.8(9)7.7(8)3.9(8)5.2(8)
C1733.2(12)20.9(10)41.1(13)11.6(9)3.1(10)2.4(9)
C516.1(9)22.4(10)14.9(9)5.2(7)2.9(7)3.3(7)
C4526.6(11)19.7(10)30.2(11)11.5(8)-6.6(9)2.3(8)
C3737.1(12)30.1(11)18.2(10)10.7(9)7.1(9)3.6(9)
C3124.0(11)42.6(13)27.8(11)13.6(10)1.4(9)1.0(9)
C1134.7(12)26.9(11)35.4(12)18.3(9)15.5(10)6.5(9)
C2627.7(11)29.4(11)26.4(11)7.7(9)2.1(9)12.1(9)
C1846.1(14)24.8(11)29.7(11)10.8(9)4.5(10)13.3(10)
C4622.6(11)26.2(11)28.5(11)8.1(9)-2.7(8)3.9(8)
C2022.7(11)39.7(13)66.4(16)34.1(12)14.7(11)11.0(9)
C3035.1(12)25.7(10)18.3(10)5.2(8)3.9(8)8.1(9)
C323.5(11)27.0(11)27.2(11)9.5(9)-5.3(8)-0.7(8)
C932.5(11)15.5(9)24.9(10)6.0(8)2.9(9)3.8(8)
C2123.6(11)40.4(12)31.8(11)18.8(10)6.7(9)4.5(9)
C2923(1)16.3(9)16.6(9)5.2(8)3.5(8)3.9(8)
C4430.2(12)40.5(13)44.0(13)31.6(11)5.9(10)8.8(10)
C229.7(11)21.6(10)26.1(10)10.9(8)2.6(9)5.4(8)
C1438.9(13)26.2(11)30.6(11)6.2(9)0.8(10)16.6(9)
C3332.3(12)24.7(10)22.5(10)9.7(8)0.3(9)7.8(9)
C4133.7(13)52.7(15)37.8(13)24.9(12)-7.4(10)-14.7(11)
C2459.0(17)37.5(13)48.9(14)28.9(12)27.2(13)27.2(12)
C3432.0(12)41.4(13)31.2(12)15(1)-4.9(10)2.3(10)
C1928.9(11)33.9(12)35.3(12)19.9(10)9.2(9)12.8(9)
C1030.3(12)28.4(11)34.4(12)18.8(9)6.7(9)6.1(9)
C1525.0(11)32.3(11)36.1(12)19.5(10)1.1(9)9.5(9)
C835.6(13)80.2(19)28.7(12)32.0(13)10(1)26.2(13)
C1648.1(15)26.4(11)34.3(12)7.7(10)-12.9(11)10.7(10)
C2830.3(11)19.1(10)29.2(11)10.2(8)6.1(9)3.5(8)
C36A34(4)15(2)32(4)5(2)5(3)8(2)
C3934.3(13)38.0(13)40.6(13)13.4(11)2.8(10)-8.1(10)
C3843.9(15)39.7(13)42.8(14)12.7(11)21.0(11)4.6(11)
C3250.2(15)40.8(13)49.7(15)29.6(12)23.4(12)28.3(12)
C42A25(3)29(3)49(3)17(2)11.6(19)4.0(18)
C2362.7(19)31.0(13)90(2)33.5(15)17.3(16)2.3(12)
C743.9(15)63.0(17)23.7(12)3.7(11)0.5(11)-22.7(13)
C2246.7(16)89(2)86(2)74(2)28.2(15)19.9(15)
C35B29(3)20(2)26(3)2(2)2(2)0.8(19)
C4352.0(16)56.1(17)54.0(16)38.0(14)-0.6(13)-15.9(13)
Li119.1(16)19.7(15)19.7(15)6.5(13)2.9(12)3.8(12)
Li221.4(16)18.7(15)22.3(16)7.6(13)4.8(13)3.4(12)
Li326.3(17)19.1(15)18.3(15)5.6(13)2.9(13)3.7(13)
Li422.6(16)17.7(15)19.2(15)8.4(13)-0.1(13)2.8(12)
C35A45(4)26(3)36(4)5(2)-14(3)-2(2)
C36B29(4)25(3)22(3)-4(2)3(2)4(2)
C42B57(14)46(11)57(11)33(9)-9(9)-29(9)

 

Table 4 Bond Lengths for mo_B1036_0m.
AtomAtomLength/Å AtomAtomLength/Å
Si3C271.8782(19) C1Li22.301(4)
Si3C251.8175(19) C48C471.512(3)
Si3C261.896(2) C47C461.516(3)
Si3C281.870(2) C13C141.513(3)
Si4C311.881(2) C12C111.516(3)
Si4C301.882(2) C40C391.522(3)
Si4C291.816(2) C25Li32.234(4)
Si4C321.887(2) C25Li42.183(3)
Si1C11.8196(19) C17C181.508(3)
Si1C41.884(2) C5Li12.261(4)
Si1C31.885(2) C5Li22.195(4)
Si1C21.8794(19) C45C461.507(3)
Si2C61.878(2) C37C381.488(3)
Si2C51.8219(19) C11C101.535(3)
Si2C81.873(2) C18C191.506(3)
Si2C71.891(2) C20C191.511(3)
O8C481.437(2) C9C101.510(3)
O8C451.439(2) C21C221.489(3)
O8Li42.000(3) C29Li32.223(4)
O5C331.444(2) C29Li42.339(4)
O5C36A1.433(6) C44C431.505(3)
O5Li31.988(4) C14C151.516(3)
O5C36B1.460(6) C33C341.517(3)
O7C441.416(2) C41C42A1.499(9)
O7C411.421(3) C41C42B1.48(2)
O7Li42.008(3) C24C231.480(3)
O1C121.427(2) C34C35B1.622(7)
O1C91.430(2) C34C35A1.429(6)
O1Li11.985(3) C15C161.511(3)
O4C211.424(2) C36AC35B1.241(8)
O4C241.425(2) C36AC35A1.522(11)
O4Li22.005(3) C36AC36B0.623(6)
O2C131.441(2) C39C381.518(3)
O2C161.419(2) C42AC431.511(10)
O2Li12.010(3) C42AC42B0.53(4)
O6C401.428(2) C23C221.469(4)
O6C371.423(2) C35BC35A0.759(6)
O6Li32.004(3) C35BC36B1.490(10)
O3C171.438(2) C43C42B1.40(2)
O3C201.432(3) Li1Li22.470(4)
O3Li22.011(3) Li3Li42.497(4)
C1Li12.209(4) C35AC36B1.471(9)

 

Table 5 Bond Angles for mo_B1036_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C27Si3C26105.30(9) C33C34C35B101.8(2)
C25Si3C27113.14(9) C35AC34C33104.2(3)
C25Si3C26114.84(9) C35AC34C35B27.9(3)
C25Si3C28110.73(9) C18C19C20102.38(18)
C28Si3C27106.57(9) C9C10C11103.75(16)
C28Si3C26105.63(10) C16C15C14101.58(16)
C31Si4C30107.48(10) O2C16C15106.68(17)
C31Si4C32103.53(11) O5C36AC35A102.5(5)
C30Si4C32105.02(10) C35BC36AO5119.1(5)
C29Si4C31111.10(10) C35BC36AC35A29.7(3)
C29Si4C30111.33(9) C36BC36AO580.0(11)
C29Si4C32117.64(10) C36BC36AC35B100.8(15)
C1Si1C4112.06(9) C36BC36AC35A73.4(13)
C1Si1C3116.84(9) C38C39C40103.52(18)
C1Si1C2110.71(9) C37C38C39102.84(18)
C4Si1C3104.81(9) C41C42AC43103.8(5)
C2Si1C4107.79(9) C42BC42AC4178(3)
C2Si1C3103.96(9) C42BC42AC4368(3)
C6Si2C7102.89(11) C22C23C24106.2(2)
C5Si2C6114.23(9) C23C22C21104.4(2)
C5Si2C8110.66(10) C36AC35BC34104.9(4)
C5Si2C7115.32(10) C36AC35BC36B24.3(4)
C8Si2C6106.76(10) C35AC35BC3461.7(7)
C8Si2C7106.23(13) C35AC35BC36A96.1(9)
C48O8C45109.18(14) C35AC35BC36B73.8(8)
C48O8Li4123.14(14) C36BC35BC34101.6(5)
C45O8Li4124.16(14) C44C43C42A106.3(4)
C33O5Li3122.60(14) C42BC43C44101.3(10)
C33O5C36B110.9(3) C42BC43C42A20.3(16)
C36AO5C33104.8(3) O1Li1O297.64(14)
C36AO5Li3125.2(3) O1Li1C1120.15(16)
C36AO5C36B24.9(2) O1Li1C5101.32(14)
C36BO5Li3126.4(3) O1Li1Li2130.98(16)
C44O7C41108.28(16) O2Li1C1110.58(15)
C44O7Li4125.69(15) O2Li1C5112.33(15)
C41O7Li4117.42(15) O2Li1Li2130.11(16)
C12O1C9105.50(14) C1Li1C5113.63(15)
C12O1Li1126.31(14) C1Li1Li258.60(12)
C9O1Li1125.37(14) C5Li1Li255.07(11)
C21O4C24110.16(16) O4Li2O3104.61(15)
C21O4Li2128.46(15) O4Li2C1100.43(14)
C24O4Li2118.80(15) O4Li2C5120.47(16)
C13O2Li1126.01(14) O4Li2Li1126.27(16)
C16O2C13109.18(14) O3Li2C1110.41(15)
C16O2Li1119.73(15) O3Li2C5107.80(15)
C40O6Li3121.45(14) O3Li2Li1127.97(16)
C37O6C40107.21(15) C1Li2Li155.03(11)
C37O6Li3131.25(15) C5Li2C1112.61(15)
C17O3Li2122.33(15) C5Li2Li157.62(11)
C20O3C17108.78(15) O5Li3O696.61(14)
C20O3Li2125.21(15) O5Li3C25104.57(15)
Si1C1Li1109.20(12) O5Li3C29112.05(15)
Si1C1Li2138.59(12) O5Li3Li4135.52(18)
Li1C1Li266.37(12) O6Li3C25104.75(15)
O8C48C47105.89(15) O6Li3C29124.29(17)
C48C47C46102.21(15) O6Li3Li4125.20(17)
O2C13C14106.66(16) C25Li3Li454.63(11)
O1C12C11105.36(15) C29Li3C25112.09(15)
O6C40C39106.47(17) C29Li3Li459.06(11)
Si3C25Li3164.28(14) O8Li4O7102.22(14)
Si3C25Li4110.08(12) O8Li4C25124.79(16)
Li4C25Li368.84(13) O8Li4C29107.88(15)
O3C17C18106.28(17) O8Li4Li3128.48(17)
Si2C5Li1153.31(13) O7Li4C25107.81(15)
Si2C5Li2108.14(12) O7Li4C29102.02(14)
Li2C5Li167.32(12) O7Li4Li3127.56(17)
O8C45C46106.59(15) C25Li4C29109.62(14)
O6C37C38103.38(17) C25Li4Li356.53(11)
C12C11C10104.38(16) C29Li4Li354.62(11)
C19C18C17102.37(17) C34C35AC36A101.3(6)
C45C46C47102.05(16) C34C35AC36B112.7(5)
O3C20C19107.05(17) C35BC35AC3490.4(9)
O1C9C10104.50(15) C35BC35AC36A54.2(7)
O4C21C22105.53(18) C35BC35AC36B76.5(9)
Si4C29Li3107.79(12) C36BC35AC36A24.0(2)
Si4C29Li4139.89(13) O5C36BC35B102.9(5)
Li3C29Li466.32(12) O5C36BC35A103.7(5)
O7C44C43106.45(18) C36AC36BO575.2(10)
C13C14C15104.71(16) C36AC36BC35B54.9(12)
O5C33C34106.74(16) C36AC36BC35A82.6(14)
O7C41C42A106.8(4) C35AC36BC35B29.7(3)
O7C41C42B104.5(9) C42AC42BC4182(3)
C42BC41C42A20.3(15) C42AC42BC4391(4)
O4C24C23106.43(19) C43C42BC41110.4(13)

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B1036_0m.
AtomxyzU(eq)
H27A1265.776194.895538.4934
H27B2621.265627.195303.3834
H27C2955.716604.785775.8834
H48A-2363.326104.416266.5231
H48B-1347.315857.585623.231
H47A-4200.015806.465392.3530
H47B-3122.086111.634928.1930
H6A5332.416827.34473.5143
H6B4368.196074.47-145.2543
H6C5370.635886.76423.4543
H13A40469622.933809.2331
H13B2663.019340.64149.3931
H12A1086.27146.723580.5227
H12B2137.567930.384137.8927
H40A-1183.255597.067684.6835
H40B-2179.2562517530.9735
H4A5709.439246.864749.8737
H4B6228.128629.875103.8137
H4C4869.548325.474509.337
H17A6030.255275.681398.6938
H17B6375.175606.192226.1138
H45A-2004.287807.565631.3830
H45B-2461.728130.886415.0930
H37A-592.577330.049422.1333
H37B-350.66347.579133.7733
H31A-3416.647508.048008.9747
H31B-3811.0578377410.247
H31C-4593.368188.738119.5347
H11A1168.126623.284402.4136
H11B2636.637234.174815.5836
H26A43585074.916171.6442
H26B4133.315298.836972.3942
H26C4895.775993.516736.1642
H18A8072.864651.891901.1940
H18B8312.974790.541194.9740
H46A-4426.27271.65401.5732
H46B-4470.877164.796131.4132
H20A9252.37016.342316.3146
H20B9344.636497.311501.2946
H30A-2678.549147.759460.5241
H30B-1015.819542.529466.1441
H30C-1339.018559.849280.0541
H3A9807.38688.764084.340
H3B9308.618818.484836.1740
H3C8933.649476.754501.2840
H9A4382.176060.533164.8330
H9B2607.865861.382949.1430
H21A8186.567409.18847.3136
H21B8982.388097.431566.0336
H44A505.188962.836280.6540
H44B872.238178.585609.5340
H2A6557.166825.983836.9738
H2B8064.137187.914340.7938
H2C8111.786902.44352138
H14A2657.8610374.893401.1139
H14B1498.8310322.783943.9839
H33A3589.087221.678590.7331
H33B2636.357060.369160.7331
H41A3659.778260.867056.149
H41B2730.759061.477371.8249
H41C3829.838270.926915.8449
H41D2786.318909.397424.3449
H24A6077.589094.522129.4451
H24B5117.278661.781388.8551
H34C5258.297995.749475.2142
H34D4081.688044.3710039.5942
H34A4446.67866.659948.3442
H34B5159.638198.699402.7642
H19A10376.795590.051884.1936
H19B9489.165878.092572.8336
H10A4121.446237.644277.4634
H10B2645.575599.183924.9934
H15A15.889242.883115.8735
H15B655.39690.582627.2235
H8A2600.087762.21918.4265
H8B1083.447255.54963.165
H8C1764.157043.91232.8765
H16A1155.838167.792360.845
H16B2447.048791.872266.4845
H28A-149.665063.676202.5339
H28B950.564703.466623.1939
H28C1096.224482.055816.4539
H36A1852.169240.639352.1934
H36B3303.038985.118926.634
H39A-3953.495957.948121.6947
H39B-2923.835333.618304.547
H38A-3115.327061.029115.9751
H38B-2787.26336.479392.2751
H32A-3237.059746.467810.3162
H32B-226810311.298521.962
H32C-3887.049878.58535.6562
H42A4658.28723.586305.240
H42B4289.389624.756846.6540
H23A6574.199462.771051.6370
H23B7763.049694.821715.6770
H7A1684.485273.21-2874
H7B1027.465397.08694.4374
H7C2514.014934.86493.2774
H22A9139.348884.2942.1472
H22B7702.448370.14421.1872
H35A4069.779445.1910077.0133
H35B4316.89147.399263.7833
H43A2460.039676.816116.2760
H43B2988.738846.15540.2160
H43C3219.488756.785623.260
H43D2412.359607.185956.6860
H29A370(30)9010(15)8108(13)42(7)
H25A2550(30)7123(15)7418(12)38(7)
H1A7340(30)8168(15)2893(12)40(7)
H5A2740(30)6877(14)2029(11)32(6)
H1B6250(20)8802(15)3233(11)32(6)
H29B-580(30)8662(15)7429(13)40(7)
H5B3890(30)6234(15)1879(12)38(6)
H25B1550(20)6503(13)7570(11)30(6)
H35C4224.679343.8610088.2647
H35D2812.58818.3410222.6447
H36C1626.028876.739845.5935
H36D1785.249249.589254.9635
H42C3276.819833.96985.6962
H42D4553.419277.346597.0662

 

Table 7 Atomic Occupancy for mo_B1036_0m.
AtomOccupancy AtomOccupancy AtomOccupancy
H41A0.75 H41B0.75 H41C0.25
H41D0.25 H34C0.492(12) H34D0.492(12)
H34A0.508(12) H34B0.508(12) C36A0.508(12)
H36A0.508(12) H36B0.508(12) C42A0.71(3)
H42A0.71(3) H42B0.71(3) C35B0.492(12)
H35A0.492(12) H35B0.492(12) H43A0.75
H43B0.75 H43C0.25 H43D0.25
C35A0.508(12) H35C0.508(12) H35D0.508(12)
C36B0.492(12) H36C0.492(12) H36D0.492(12)
C42B0.29(3) H42C0.29(3) H42D0.29(3)

Experimental

Single crystals of C24H54Li2O4Si2 [mo_B1036_0m] 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 XT [2] structure solution program using Intrinsic Phasing 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. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [mo_B1036_0m]

Crystal Data for C24H54Li2O4Si2 (=476.73 g/mol): triclinic, space group P-1 (no. 2), a = 8.996(2) Å, b = 17.382(4) Å, c = 20.982(6) Å, α = 112.633(6)°, β = 93.252(9)°, γ = 93.891(14)°, = 3009.2(14) Å3, Z = 4, T = 100.0 K, μ(MoKα) = 0.141 mm-1, Dcalc = 1.052 g/cm3, 58894 reflections measured (4.556° ≤ 2Θ ≤ 51.998°), 11800 unique (Rint = 0.0535, Rsigma = 0.0435) which were used in all calculations. The final R1 was 0.0482 (I > 2σ(I)) and wR2 was 0.1173 (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, All C(H,H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Sof(C42A)=Sof(H42A)=Sof(H42B)=1-FVAR(1)
Sof(C42B)=Sof(H42C)=Sof(H42D)=FVAR(1)
Sof(H34A)=Sof(H34B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C35A)=Sof(H35C)=
Sof(H35D)=1-FVAR(2)
Sof(H34C)=Sof(H34D)=Sof(C35B)=Sof(H35A)=Sof(H35B)=Sof(C36B)=Sof(H36C)=
Sof(H36D)=FVAR(2)
Fixed Sof: H41A(0.75) H41B(0.75) H41C(0.25) H41D(0.25) H43A(0.75) H43B(0.75)
H43C(0.25) H43D(0.25)
3.a Secondary CH2 refined with riding coordinates:
C48(H48A,H48B), C47(H47A,H47B), C13(H13A,H13B), C12(H12A,H12B), C40(H40A,
H40B), C17(H17A,H17B), C45(H45A,H45B), C37(H37A,H37B), C11(H11A,H11B),
C18(H18A,H18B), C46(H46A,H46B), C20(H20A,H20B), C9(H9A,H9B), C21(H21A,H21B),
C44(H44A,H44B), C14(H14A,H14B), C33(H33A,H33B), C41(H41A,H41B), C41(H41C,H41D),
C24(H24A,H24B), C34(H34C,H34D), C34(H34A,H34B), C19(H19A,H19B), C10(H10A,
H10B), C15(H15A,H15B), C16(H16A,H16B), C36A(H36A,H36B), C39(H39A,H39B),
C38(H38A,H38B), C42A(H42A,H42B), C23(H23A,H23B), C22(H22A,H22B), C35B(H35A,
H35B), C43(H43A,H43B), C43(H43C,H43D), C35A(H35C,H35D), C36B(H36C,H36D),
C42B(H42C,H42D)
3.b Idealised Me refined as rotating group:
C27(H27A,H27B,H27C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C31(H31A,H31B,H31C),
C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C),
C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C7(H7A,H7B,H7C)

This report has been created with Olex2, compiled on 2017.08.10 svn.r3458 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.