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 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Si3 | 2227.0(6) | 5864.9(3) | 6479.0(2) | 15.94(11) |
Si4 | -2105.2(6) | 8859.1(3) | 8295.0(3) | 19.81(12) |
Si1 | 7192.2(6) | 8249.7(3) | 3993.3(2) | 16.00(11) |
Si2 | 3117.5(6) | 6422.1(4) | 890.8(3) | 23.51(13) |
O8 | -1356.2(15) | 7100.1(8) | 6142.6(7) | 22.8(3) |
O5 | 1966.0(16) | 7994.0(8) | 8903.0(7) | 27.4(3) |
O7 | 1730.8(15) | 8171.9(8) | 6503.0(7) | 23.2(3) |
O1 | 3270.3(15) | 7087.7(8) | 3448.5(7) | 22.0(3) |
O4 | 6747.0(15) | 7996.9(8) | 1522.7(7) | 22.9(3) |
O2 | 2757.2(15) | 8607.9(8) | 3143.4(7) | 23.5(3) |
O6 | -753.9(16) | 6773.9(8) | 8384.6(7) | 27.5(3) |
O3 | 7313.7(15) | 6373.8(8) | 1816.6(7) | 25.3(3) |
C27 | 2273(2) | 6101.2(12) | 5678.5(9) | 22.5(4) |
C1 | 6503(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) |
C6 | 4741(2) | 6286.5(14) | 345.4(10) | 28.7(5) |
C13 | 2978(2) | 9402.5(12) | 3725.7(10) | 25.6(4) |
C12 | 2053(2) | 7317.5(12) | 3870(1) | 22.5(4) |
C40 | -1735(2) | 6093.9(12) | 7901.0(11) | 29.4(5) |
C4 | 5837(2) | 8662.5(13) | 4670.3(10) | 25.0(4) |
C25 | 1695(2) | 6729.7(11) | 7223.4(9) | 18.1(4) |
C17 | 6805(2) | 5558.9(12) | 1790.1(12) | 31.9(5) |
C5 | 3649(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) |
C11 | 2168(2) | 6856.5(13) | 4351.6(11) | 29.8(5) |
C26 | 4134(2) | 5515.9(13) | 6605.0(11) | 28.3(4) |
C18 | 8160(3) | 5073.9(13) | 1692.2(11) | 33.0(5) |
C46 | -3859(2) | 7110.1(12) | 5741.4(11) | 26.7(4) |
C20 | 8914(2) | 6483.6(15) | 1921.0(14) | 38.0(6) |
C30 | -1741(2) | 9050.2(13) | 9238.5(10) | 27.0(4) |
C3 | 9031(2) | 8884.7(13) | 4402.9(10) | 26.7(4) |
C9 | 3385(2) | 6223.3(11) | 3314(1) | 24.8(4) |
C21 | 8122(2) | 7969.8(14) | 1213.7(11) | 30.2(5) |
C29 | -437(2) | 8585.3(11) | 7840.7(10) | 18.9(4) |
C44 | 1283(2) | 8589.1(14) | 6072.8(12) | 33.3(5) |
C2 | 7521(2) | 7161.3(12) | 3913.5(10) | 25.2(4) |
C14 | 2032(3) | 9988.7(13) | 3543.8(11) | 32.8(5) |
C33 | 3094(2) | 7497.7(12) | 9019.3(10) | 26.2(4) |
C41 | 3022(3) | 8637.5(16) | 6937.1(12) | 40.6(6) |
C24 | 6136(3) | 8767.7(15) | 1628.7(13) | 42.8(6) |
C34 | 4218(3) | 8094.2(14) | 9591.7(11) | 35.0(5) |
C19 | 9406(2) | 5750.6(13) | 2069.1(11) | 30.0(5) |
C10 | 3155(2) | 6153.3(13) | 3997.7(11) | 28.7(5) |
C15 | 933(2) | 9418.1(13) | 2947.5(11) | 29.0(5) |
C8 | 2009(3) | 7215.5(18) | 732.4(12) | 43.6(6) |
C16 | 1830(3) | 8686.9(14) | 2606.1(12) | 37.9(6) |
C28 | 869(2) | 4915.5(12) | 6253.4(10) | 25.7(4) |
C36A | 2627(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) |
C42A | 3850(9) | 9055(5) | 6538(5) | 33.4(13) |
C23 | 7153(3) | 9229.0(16) | 1338.5(17) | 57.9(8) |
C7 | 1945(3) | 5381.5(17) | 460.8(12) | 49.0(7) |
C22 | 8115(3) | 8618(2) | 912.7(17) | 60.1(8) |
C35B | 3806(6) | 8997(3) | 9611(4) | 27.3(15) |
C43 | 2662(3) | 9090.1(18) | 6014.0(14) | 50.3(7) |
Li1 | 4148(3) | 7700.1(19) | 2911.2(16) | 19.7(6) |
Li2 | 5975(4) | 7305.6(19) | 2031.0(16) | 20.7(6) |
Li3 | 467(4) | 7559.4(19) | 8082.0(16) | 21.7(7) |
Li4 | 356(3) | 7522.4(18) | 6878.5(16) | 19.5(6) |
C35A | 3492(8) | 8844(4) | 9875(4) | 38.9(18) |
C36B | 2156(9) | 8843(4) | 9436(4) | 29.1(15) |
C42B | 3470(40) | 9272(19) | 6655(14) | 52(6) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Si3 | 18.5(3) | 15.2(2) | 14.9(2) | 6.02(19) | 2.84(19) | 5.01(19) |
Si4 | 22.8(3) | 21.0(3) | 18.4(3) | 9.1(2) | 5.3(2) | 9.1(2) |
Si1 | 17.3(3) | 15.5(2) | 14.0(2) | 4.55(19) | -0.15(19) | 2.32(19) |
Si2 | 16.2(3) | 37.8(3) | 13.6(2) | 7.4(2) | 1.2(2) | -1.2(2) |
O8 | 22.2(7) | 15.8(6) | 27.4(7) | 6.5(6) | -6.1(6) | 0.6(5) |
O5 | 32.7(8) | 17.4(7) | 25.7(7) | 2.6(6) | -7.7(6) | 4.1(6) |
O7 | 24.1(7) | 22.7(7) | 26.7(7) | 15.1(6) | -1.1(6) | -1.6(5) |
O1 | 29.7(8) | 18.0(6) | 21.7(7) | 9.3(5) | 11.1(6) | 7.8(5) |
O4 | 25.8(7) | 22.0(7) | 24.9(7) | 11.6(6) | 10.9(6) | 6.6(5) |
O2 | 28.7(8) | 17.9(7) | 20.6(7) | 3.5(5) | -2.5(6) | 9.3(6) |
O6 | 37.6(8) | 26.7(7) | 16.9(7) | 9.2(6) | 1.9(6) | -8.4(6) |
O3 | 21.9(7) | 21.9(7) | 34.2(8) | 12.0(6) | 6.6(6) | 6.9(6) |
C27 | 25(1) | 24.4(10) | 18.3(9) | 8.3(8) | 3.3(8) | 3.3(8) |
C1 | 20(1) | 17.1(9) | 17.0(9) | 6.5(7) | 1.4(8) | 1.0(7) |
C48 | 24.4(11) | 16.4(9) | 33.7(11) | 7.8(8) | -0.7(9) | 0.0(8) |
C47 | 23.9(10) | 21.1(10) | 24(1) | 4.1(8) | 1.0(8) | -0.8(8) |
C6 | 25.4(11) | 38.1(12) | 17(1) | 4.1(9) | 6.6(8) | 2.0(9) |
C13 | 27.0(11) | 19(1) | 26.4(10) | 4.0(8) | -0.9(8) | 5.7(8) |
C12 | 19.6(10) | 24.9(10) | 24.3(10) | 10.4(8) | 4.1(8) | 4.3(8) |
C40 | 37.1(12) | 20.9(10) | 26.2(11) | 5.7(9) | 1.0(9) | -1.7(9) |
C4 | 25.1(11) | 30.1(11) | 16.9(9) | 5.3(8) | 1.6(8) | 7.4(8) |
C25 | 22.8(10) | 16.5(9) | 16.8(9) | 7.7(8) | 3.9(8) | 5.2(8) |
C17 | 33.2(12) | 20.9(10) | 41.1(13) | 11.6(9) | 3.1(10) | 2.4(9) |
C5 | 16.1(9) | 22.4(10) | 14.9(9) | 5.2(7) | 2.9(7) | 3.3(7) |
C45 | 26.6(11) | 19.7(10) | 30.2(11) | 11.5(8) | -6.6(9) | 2.3(8) |
C37 | 37.1(12) | 30.1(11) | 18.2(10) | 10.7(9) | 7.1(9) | 3.6(9) |
C31 | 24.0(11) | 42.6(13) | 27.8(11) | 13.6(10) | 1.4(9) | 1.0(9) |
C11 | 34.7(12) | 26.9(11) | 35.4(12) | 18.3(9) | 15.5(10) | 6.5(9) |
C26 | 27.7(11) | 29.4(11) | 26.4(11) | 7.7(9) | 2.1(9) | 12.1(9) |
C18 | 46.1(14) | 24.8(11) | 29.7(11) | 10.8(9) | 4.5(10) | 13.3(10) |
C46 | 22.6(11) | 26.2(11) | 28.5(11) | 8.1(9) | -2.7(8) | 3.9(8) |
C20 | 22.7(11) | 39.7(13) | 66.4(16) | 34.1(12) | 14.7(11) | 11.0(9) |
C30 | 35.1(12) | 25.7(10) | 18.3(10) | 5.2(8) | 3.9(8) | 8.1(9) |
C3 | 23.5(11) | 27.0(11) | 27.2(11) | 9.5(9) | -5.3(8) | -0.7(8) |
C9 | 32.5(11) | 15.5(9) | 24.9(10) | 6.0(8) | 2.9(9) | 3.8(8) |
C21 | 23.6(11) | 40.4(12) | 31.8(11) | 18.8(10) | 6.7(9) | 4.5(9) |
C29 | 23(1) | 16.3(9) | 16.6(9) | 5.2(8) | 3.5(8) | 3.9(8) |
C44 | 30.2(12) | 40.5(13) | 44.0(13) | 31.6(11) | 5.9(10) | 8.8(10) |
C2 | 29.7(11) | 21.6(10) | 26.1(10) | 10.9(8) | 2.6(9) | 5.4(8) |
C14 | 38.9(13) | 26.2(11) | 30.6(11) | 6.2(9) | 0.8(10) | 16.6(9) |
C33 | 32.3(12) | 24.7(10) | 22.5(10) | 9.7(8) | 0.3(9) | 7.8(9) |
C41 | 33.7(13) | 52.7(15) | 37.8(13) | 24.9(12) | -7.4(10) | -14.7(11) |
C24 | 59.0(17) | 37.5(13) | 48.9(14) | 28.9(12) | 27.2(13) | 27.2(12) |
C34 | 32.0(12) | 41.4(13) | 31.2(12) | 15(1) | -4.9(10) | 2.3(10) |
C19 | 28.9(11) | 33.9(12) | 35.3(12) | 19.9(10) | 9.2(9) | 12.8(9) |
C10 | 30.3(12) | 28.4(11) | 34.4(12) | 18.8(9) | 6.7(9) | 6.1(9) |
C15 | 25.0(11) | 32.3(11) | 36.1(12) | 19.5(10) | 1.1(9) | 9.5(9) |
C8 | 35.6(13) | 80.2(19) | 28.7(12) | 32.0(13) | 10(1) | 26.2(13) |
C16 | 48.1(15) | 26.4(11) | 34.3(12) | 7.7(10) | -12.9(11) | 10.7(10) |
C28 | 30.3(11) | 19.1(10) | 29.2(11) | 10.2(8) | 6.1(9) | 3.5(8) |
C36A | 34(4) | 15(2) | 32(4) | 5(2) | 5(3) | 8(2) |
C39 | 34.3(13) | 38.0(13) | 40.6(13) | 13.4(11) | 2.8(10) | -8.1(10) |
C38 | 43.9(15) | 39.7(13) | 42.8(14) | 12.7(11) | 21.0(11) | 4.6(11) |
C32 | 50.2(15) | 40.8(13) | 49.7(15) | 29.6(12) | 23.4(12) | 28.3(12) |
C42A | 25(3) | 29(3) | 49(3) | 17(2) | 11.6(19) | 4.0(18) |
C23 | 62.7(19) | 31.0(13) | 90(2) | 33.5(15) | 17.3(16) | 2.3(12) |
C7 | 43.9(15) | 63.0(17) | 23.7(12) | 3.7(11) | 0.5(11) | -22.7(13) |
C22 | 46.7(16) | 89(2) | 86(2) | 74(2) | 28.2(15) | 19.9(15) |
C35B | 29(3) | 20(2) | 26(3) | 2(2) | 2(2) | 0.8(19) |
C43 | 52.0(16) | 56.1(17) | 54.0(16) | 38.0(14) | -0.6(13) | -15.9(13) |
Li1 | 19.1(16) | 19.7(15) | 19.7(15) | 6.5(13) | 2.9(12) | 3.8(12) |
Li2 | 21.4(16) | 18.7(15) | 22.3(16) | 7.6(13) | 4.8(13) | 3.4(12) |
Li3 | 26.3(17) | 19.1(15) | 18.3(15) | 5.6(13) | 2.9(13) | 3.7(13) |
Li4 | 22.6(16) | 17.7(15) | 19.2(15) | 8.4(13) | -0.1(13) | 2.8(12) |
C35A | 45(4) | 26(3) | 36(4) | 5(2) | -14(3) | -2(2) |
C36B | 29(4) | 25(3) | 22(3) | -4(2) | 3(2) | 4(2) |
C42B | 57(14) | 46(11) | 57(11) | 33(9) | -9(9) | -29(9) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Si3 | C27 | 1.8782(19) | C1 | Li2 | 2.301(4) | |
Si3 | C25 | 1.8175(19) | C48 | C47 | 1.512(3) | |
Si3 | C26 | 1.896(2) | C47 | C46 | 1.516(3) | |
Si3 | C28 | 1.870(2) | C13 | C14 | 1.513(3) | |
Si4 | C31 | 1.881(2) | C12 | C11 | 1.516(3) | |
Si4 | C30 | 1.882(2) | C40 | C39 | 1.522(3) | |
Si4 | C29 | 1.816(2) | C25 | Li3 | 2.234(4) | |
Si4 | C32 | 1.887(2) | C25 | Li4 | 2.183(3) | |
Si1 | C1 | 1.8196(19) | C17 | C18 | 1.508(3) | |
Si1 | C4 | 1.884(2) | C5 | Li1 | 2.261(4) | |
Si1 | C3 | 1.885(2) | C5 | Li2 | 2.195(4) | |
Si1 | C2 | 1.8794(19) | C45 | C46 | 1.507(3) | |
Si2 | C6 | 1.878(2) | C37 | C38 | 1.488(3) | |
Si2 | C5 | 1.8219(19) | C11 | C10 | 1.535(3) | |
Si2 | C8 | 1.873(2) | C18 | C19 | 1.506(3) | |
Si2 | C7 | 1.891(2) | C20 | C19 | 1.511(3) | |
O8 | C48 | 1.437(2) | C9 | C10 | 1.510(3) | |
O8 | C45 | 1.439(2) | C21 | C22 | 1.489(3) | |
O8 | Li4 | 2.000(3) | C29 | Li3 | 2.223(4) | |
O5 | C33 | 1.444(2) | C29 | Li4 | 2.339(4) | |
O5 | C36A | 1.433(6) | C44 | C43 | 1.505(3) | |
O5 | Li3 | 1.988(4) | C14 | C15 | 1.516(3) | |
O5 | C36B | 1.460(6) | C33 | C34 | 1.517(3) | |
O7 | C44 | 1.416(2) | C41 | C42A | 1.499(9) | |
O7 | C41 | 1.421(3) | C41 | C42B | 1.48(2) | |
O7 | Li4 | 2.008(3) | C24 | C23 | 1.480(3) | |
O1 | C12 | 1.427(2) | C34 | C35B | 1.622(7) | |
O1 | C9 | 1.430(2) | C34 | C35A | 1.429(6) | |
O1 | Li1 | 1.985(3) | C15 | C16 | 1.511(3) | |
O4 | C21 | 1.424(2) | C36A | C35B | 1.241(8) | |
O4 | C24 | 1.425(2) | C36A | C35A | 1.522(11) | |
O4 | Li2 | 2.005(3) | C36A | C36B | 0.623(6) | |
O2 | C13 | 1.441(2) | C39 | C38 | 1.518(3) | |
O2 | C16 | 1.419(2) | C42A | C43 | 1.511(10) | |
O2 | Li1 | 2.010(3) | C42A | C42B | 0.53(4) | |
O6 | C40 | 1.428(2) | C23 | C22 | 1.469(4) | |
O6 | C37 | 1.423(2) | C35B | C35A | 0.759(6) | |
O6 | Li3 | 2.004(3) | C35B | C36B | 1.490(10) | |
O3 | C17 | 1.438(2) | C43 | C42B | 1.40(2) | |
O3 | C20 | 1.432(3) | Li1 | Li2 | 2.470(4) | |
O3 | Li2 | 2.011(3) | Li3 | Li4 | 2.497(4) | |
C1 | Li1 | 2.209(4) | C35A | C36B | 1.471(9) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C27 | Si3 | C26 | 105.30(9) | C33 | C34 | C35B | 101.8(2) | |
C25 | Si3 | C27 | 113.14(9) | C35A | C34 | C33 | 104.2(3) | |
C25 | Si3 | C26 | 114.84(9) | C35A | C34 | C35B | 27.9(3) | |
C25 | Si3 | C28 | 110.73(9) | C18 | C19 | C20 | 102.38(18) | |
C28 | Si3 | C27 | 106.57(9) | C9 | C10 | C11 | 103.75(16) | |
C28 | Si3 | C26 | 105.63(10) | C16 | C15 | C14 | 101.58(16) | |
C31 | Si4 | C30 | 107.48(10) | O2 | C16 | C15 | 106.68(17) | |
C31 | Si4 | C32 | 103.53(11) | O5 | C36A | C35A | 102.5(5) | |
C30 | Si4 | C32 | 105.02(10) | C35B | C36A | O5 | 119.1(5) | |
C29 | Si4 | C31 | 111.10(10) | C35B | C36A | C35A | 29.7(3) | |
C29 | Si4 | C30 | 111.33(9) | C36B | C36A | O5 | 80.0(11) | |
C29 | Si4 | C32 | 117.64(10) | C36B | C36A | C35B | 100.8(15) | |
C1 | Si1 | C4 | 112.06(9) | C36B | C36A | C35A | 73.4(13) | |
C1 | Si1 | C3 | 116.84(9) | C38 | C39 | C40 | 103.52(18) | |
C1 | Si1 | C2 | 110.71(9) | C37 | C38 | C39 | 102.84(18) | |
C4 | Si1 | C3 | 104.81(9) | C41 | C42A | C43 | 103.8(5) | |
C2 | Si1 | C4 | 107.79(9) | C42B | C42A | C41 | 78(3) | |
C2 | Si1 | C3 | 103.96(9) | C42B | C42A | C43 | 68(3) | |
C6 | Si2 | C7 | 102.89(11) | C22 | C23 | C24 | 106.2(2) | |
C5 | Si2 | C6 | 114.23(9) | C23 | C22 | C21 | 104.4(2) | |
C5 | Si2 | C8 | 110.66(10) | C36A | C35B | C34 | 104.9(4) | |
C5 | Si2 | C7 | 115.32(10) | C36A | C35B | C36B | 24.3(4) | |
C8 | Si2 | C6 | 106.76(10) | C35A | C35B | C34 | 61.7(7) | |
C8 | Si2 | C7 | 106.23(13) | C35A | C35B | C36A | 96.1(9) | |
C48 | O8 | C45 | 109.18(14) | C35A | C35B | C36B | 73.8(8) | |
C48 | O8 | Li4 | 123.14(14) | C36B | C35B | C34 | 101.6(5) | |
C45 | O8 | Li4 | 124.16(14) | C44 | C43 | C42A | 106.3(4) | |
C33 | O5 | Li3 | 122.60(14) | C42B | C43 | C44 | 101.3(10) | |
C33 | O5 | C36B | 110.9(3) | C42B | C43 | C42A | 20.3(16) | |
C36A | O5 | C33 | 104.8(3) | O1 | Li1 | O2 | 97.64(14) | |
C36A | O5 | Li3 | 125.2(3) | O1 | Li1 | C1 | 120.15(16) | |
C36A | O5 | C36B | 24.9(2) | O1 | Li1 | C5 | 101.32(14) | |
C36B | O5 | Li3 | 126.4(3) | O1 | Li1 | Li2 | 130.98(16) | |
C44 | O7 | C41 | 108.28(16) | O2 | Li1 | C1 | 110.58(15) | |
C44 | O7 | Li4 | 125.69(15) | O2 | Li1 | C5 | 112.33(15) | |
C41 | O7 | Li4 | 117.42(15) | O2 | Li1 | Li2 | 130.11(16) | |
C12 | O1 | C9 | 105.50(14) | C1 | Li1 | C5 | 113.63(15) | |
C12 | O1 | Li1 | 126.31(14) | C1 | Li1 | Li2 | 58.60(12) | |
C9 | O1 | Li1 | 125.37(14) | C5 | Li1 | Li2 | 55.07(11) | |
C21 | O4 | C24 | 110.16(16) | O4 | Li2 | O3 | 104.61(15) | |
C21 | O4 | Li2 | 128.46(15) | O4 | Li2 | C1 | 100.43(14) | |
C24 | O4 | Li2 | 118.80(15) | O4 | Li2 | C5 | 120.47(16) | |
C13 | O2 | Li1 | 126.01(14) | O4 | Li2 | Li1 | 126.27(16) | |
C16 | O2 | C13 | 109.18(14) | O3 | Li2 | C1 | 110.41(15) | |
C16 | O2 | Li1 | 119.73(15) | O3 | Li2 | C5 | 107.80(15) | |
C40 | O6 | Li3 | 121.45(14) | O3 | Li2 | Li1 | 127.97(16) | |
C37 | O6 | C40 | 107.21(15) | C1 | Li2 | Li1 | 55.03(11) | |
C37 | O6 | Li3 | 131.25(15) | C5 | Li2 | C1 | 112.61(15) | |
C17 | O3 | Li2 | 122.33(15) | C5 | Li2 | Li1 | 57.62(11) | |
C20 | O3 | C17 | 108.78(15) | O5 | Li3 | O6 | 96.61(14) | |
C20 | O3 | Li2 | 125.21(15) | O5 | Li3 | C25 | 104.57(15) | |
Si1 | C1 | Li1 | 109.20(12) | O5 | Li3 | C29 | 112.05(15) | |
Si1 | C1 | Li2 | 138.59(12) | O5 | Li3 | Li4 | 135.52(18) | |
Li1 | C1 | Li2 | 66.37(12) | O6 | Li3 | C25 | 104.75(15) | |
O8 | C48 | C47 | 105.89(15) | O6 | Li3 | C29 | 124.29(17) | |
C48 | C47 | C46 | 102.21(15) | O6 | Li3 | Li4 | 125.20(17) | |
O2 | C13 | C14 | 106.66(16) | C25 | Li3 | Li4 | 54.63(11) | |
O1 | C12 | C11 | 105.36(15) | C29 | Li3 | C25 | 112.09(15) | |
O6 | C40 | C39 | 106.47(17) | C29 | Li3 | Li4 | 59.06(11) | |
Si3 | C25 | Li3 | 164.28(14) | O8 | Li4 | O7 | 102.22(14) | |
Si3 | C25 | Li4 | 110.08(12) | O8 | Li4 | C25 | 124.79(16) | |
Li4 | C25 | Li3 | 68.84(13) | O8 | Li4 | C29 | 107.88(15) | |
O3 | C17 | C18 | 106.28(17) | O8 | Li4 | Li3 | 128.48(17) | |
Si2 | C5 | Li1 | 153.31(13) | O7 | Li4 | C25 | 107.81(15) | |
Si2 | C5 | Li2 | 108.14(12) | O7 | Li4 | C29 | 102.02(14) | |
Li2 | C5 | Li1 | 67.32(12) | O7 | Li4 | Li3 | 127.56(17) | |
O8 | C45 | C46 | 106.59(15) | C25 | Li4 | C29 | 109.62(14) | |
O6 | C37 | C38 | 103.38(17) | C25 | Li4 | Li3 | 56.53(11) | |
C12 | C11 | C10 | 104.38(16) | C29 | Li4 | Li3 | 54.62(11) | |
C19 | C18 | C17 | 102.37(17) | C34 | C35A | C36A | 101.3(6) | |
C45 | C46 | C47 | 102.05(16) | C34 | C35A | C36B | 112.7(5) | |
O3 | C20 | C19 | 107.05(17) | C35B | C35A | C34 | 90.4(9) | |
O1 | C9 | C10 | 104.50(15) | C35B | C35A | C36A | 54.2(7) | |
O4 | C21 | C22 | 105.53(18) | C35B | C35A | C36B | 76.5(9) | |
Si4 | C29 | Li3 | 107.79(12) | C36B | C35A | C36A | 24.0(2) | |
Si4 | C29 | Li4 | 139.89(13) | O5 | C36B | C35B | 102.9(5) | |
Li3 | C29 | Li4 | 66.32(12) | O5 | C36B | C35A | 103.7(5) | |
O7 | C44 | C43 | 106.45(18) | C36A | C36B | O5 | 75.2(10) | |
C13 | C14 | C15 | 104.71(16) | C36A | C36B | C35B | 54.9(12) | |
O5 | C33 | C34 | 106.74(16) | C36A | C36B | C35A | 82.6(14) | |
O7 | C41 | C42A | 106.8(4) | C35A | C36B | C35B | 29.7(3) | |
O7 | C41 | C42B | 104.5(9) | C42A | C42B | C41 | 82(3) | |
C42B | C41 | C42A | 20.3(15) | C42A | C42B | C43 | 91(4) | |
O4 | C24 | C23 | 106.43(19) | C43 | C42B | C41 | 110.4(13) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H27A | 1265.77 | 6194.89 | 5538.49 | 34 |
H27B | 2621.26 | 5627.19 | 5303.38 | 34 |
H27C | 2955.71 | 6604.78 | 5775.88 | 34 |
H48A | -2363.32 | 6104.41 | 6266.52 | 31 |
H48B | -1347.31 | 5857.58 | 5623.2 | 31 |
H47A | -4200.01 | 5806.46 | 5392.35 | 30 |
H47B | -3122.08 | 6111.63 | 4928.19 | 30 |
H6A | 5332.41 | 6827.34 | 473.51 | 43 |
H6B | 4368.19 | 6074.47 | -145.25 | 43 |
H6C | 5370.63 | 5886.76 | 423.45 | 43 |
H13A | 4046 | 9622.93 | 3809.23 | 31 |
H13B | 2663.01 | 9340.6 | 4149.39 | 31 |
H12A | 1086.2 | 7146.72 | 3580.52 | 27 |
H12B | 2137.56 | 7930.38 | 4137.89 | 27 |
H40A | -1183.25 | 5597.06 | 7684.68 | 35 |
H40B | -2179.25 | 6251 | 7530.97 | 35 |
H4A | 5709.43 | 9246.86 | 4749.87 | 37 |
H4B | 6228.12 | 8629.87 | 5103.81 | 37 |
H4C | 4869.54 | 8325.47 | 4509.3 | 37 |
H17A | 6030.25 | 5275.68 | 1398.69 | 38 |
H17B | 6375.17 | 5606.19 | 2226.11 | 38 |
H45A | -2004.28 | 7807.56 | 5631.38 | 30 |
H45B | -2461.72 | 8130.88 | 6415.09 | 30 |
H37A | -592.57 | 7330.04 | 9422.13 | 33 |
H37B | -350.6 | 6347.57 | 9133.77 | 33 |
H31A | -3416.64 | 7508.04 | 8008.97 | 47 |
H31B | -3811.05 | 7837 | 7410.2 | 47 |
H31C | -4593.36 | 8188.73 | 8119.53 | 47 |
H11A | 1168.12 | 6623.28 | 4402.41 | 36 |
H11B | 2636.63 | 7234.17 | 4815.58 | 36 |
H26A | 4358 | 5074.91 | 6171.64 | 42 |
H26B | 4133.31 | 5298.83 | 6972.39 | 42 |
H26C | 4895.77 | 5993.51 | 6736.16 | 42 |
H18A | 8072.86 | 4651.89 | 1901.19 | 40 |
H18B | 8312.97 | 4790.54 | 1194.97 | 40 |
H46A | -4426.2 | 7271.6 | 5401.57 | 32 |
H46B | -4470.87 | 7164.79 | 6131.41 | 32 |
H20A | 9252.3 | 7016.34 | 2316.31 | 46 |
H20B | 9344.63 | 6497.31 | 1501.29 | 46 |
H30A | -2678.54 | 9147.75 | 9460.52 | 41 |
H30B | -1015.81 | 9542.52 | 9466.14 | 41 |
H30C | -1339.01 | 8559.84 | 9280.05 | 41 |
H3A | 9807.3 | 8688.76 | 4084.3 | 40 |
H3B | 9308.61 | 8818.48 | 4836.17 | 40 |
H3C | 8933.64 | 9476.75 | 4501.28 | 40 |
H9A | 4382.17 | 6060.53 | 3164.83 | 30 |
H9B | 2607.86 | 5861.38 | 2949.14 | 30 |
H21A | 8186.56 | 7409.18 | 847.31 | 36 |
H21B | 8982.38 | 8097.43 | 1566.03 | 36 |
H44A | 505.18 | 8962.83 | 6280.65 | 40 |
H44B | 872.23 | 8178.58 | 5609.53 | 40 |
H2A | 6557.16 | 6825.98 | 3836.97 | 38 |
H2B | 8064.13 | 7187.91 | 4340.79 | 38 |
H2C | 8111.78 | 6902.44 | 3521 | 38 |
H14A | 2657.86 | 10374.89 | 3401.11 | 39 |
H14B | 1498.83 | 10322.78 | 3943.98 | 39 |
H33A | 3589.08 | 7221.67 | 8590.73 | 31 |
H33B | 2636.35 | 7060.36 | 9160.73 | 31 |
H41A | 3659.77 | 8260.86 | 7056.1 | 49 |
H41B | 2730.75 | 9061.47 | 7371.82 | 49 |
H41C | 3829.83 | 8270.92 | 6915.84 | 49 |
H41D | 2786.31 | 8909.39 | 7424.34 | 49 |
H24A | 6077.58 | 9094.52 | 2129.44 | 51 |
H24B | 5117.27 | 8661.78 | 1388.85 | 51 |
H34C | 5258.29 | 7995.74 | 9475.21 | 42 |
H34D | 4081.68 | 8044.37 | 10039.59 | 42 |
H34A | 4446.6 | 7866.65 | 9948.34 | 42 |
H34B | 5159.63 | 8198.69 | 9402.76 | 42 |
H19A | 10376.79 | 5590.05 | 1884.19 | 36 |
H19B | 9489.16 | 5878.09 | 2572.83 | 36 |
H10A | 4121.44 | 6237.64 | 4277.46 | 34 |
H10B | 2645.57 | 5599.18 | 3924.99 | 34 |
H15A | 15.88 | 9242.88 | 3115.87 | 35 |
H15B | 655.3 | 9690.58 | 2627.22 | 35 |
H8A | 2600.08 | 7762.21 | 918.42 | 65 |
H8B | 1083.44 | 7255.54 | 963.1 | 65 |
H8C | 1764.15 | 7043.91 | 232.87 | 65 |
H16A | 1155.83 | 8167.79 | 2360.8 | 45 |
H16B | 2447.04 | 8791.87 | 2266.48 | 45 |
H28A | -149.66 | 5063.67 | 6202.53 | 39 |
H28B | 950.56 | 4703.46 | 6623.19 | 39 |
H28C | 1096.22 | 4482.05 | 5816.45 | 39 |
H36A | 1852.16 | 9240.63 | 9352.19 | 34 |
H36B | 3303.03 | 8985.11 | 8926.6 | 34 |
H39A | -3953.49 | 5957.94 | 8121.69 | 47 |
H39B | -2923.83 | 5333.61 | 8304.5 | 47 |
H38A | -3115.32 | 7061.02 | 9115.97 | 51 |
H38B | -2787.2 | 6336.47 | 9392.27 | 51 |
H32A | -3237.05 | 9746.46 | 7810.31 | 62 |
H32B | -2268 | 10311.29 | 8521.9 | 62 |
H32C | -3887.04 | 9878.5 | 8535.65 | 62 |
H42A | 4658.2 | 8723.58 | 6305.2 | 40 |
H42B | 4289.38 | 9624.75 | 6846.65 | 40 |
H23A | 6574.19 | 9462.77 | 1051.63 | 70 |
H23B | 7763.04 | 9694.82 | 1715.67 | 70 |
H7A | 1684.48 | 5273.21 | -28 | 74 |
H7B | 1027.46 | 5397.08 | 694.43 | 74 |
H7C | 2514.01 | 4934.86 | 493.27 | 74 |
H22A | 9139.34 | 8884.2 | 942.14 | 72 |
H22B | 7702.44 | 8370.14 | 421.18 | 72 |
H35A | 4069.77 | 9445.19 | 10077.01 | 33 |
H35B | 4316.8 | 9147.39 | 9263.78 | 33 |
H43A | 2460.03 | 9676.81 | 6116.27 | 60 |
H43B | 2988.73 | 8846.1 | 5540.21 | 60 |
H43C | 3219.48 | 8756.78 | 5623.2 | 60 |
H43D | 2412.35 | 9607.18 | 5956.68 | 60 |
H29A | 370(30) | 9010(15) | 8108(13) | 42(7) |
H25A | 2550(30) | 7123(15) | 7418(12) | 38(7) |
H1A | 7340(30) | 8168(15) | 2893(12) | 40(7) |
H5A | 2740(30) | 6877(14) | 2029(11) | 32(6) |
H1B | 6250(20) | 8802(15) | 3233(11) | 32(6) |
H29B | -580(30) | 8662(15) | 7429(13) | 40(7) |
H5B | 3890(30) | 6234(15) | 1879(12) | 38(6) |
H25B | 1550(20) | 6503(13) | 7570(11) | 30(6) |
H35C | 4224.67 | 9343.86 | 10088.26 | 47 |
H35D | 2812.5 | 8818.34 | 10222.64 | 47 |
H36C | 1626.02 | 8876.73 | 9845.59 | 35 |
H36D | 1785.24 | 9249.58 | 9254.96 | 35 |
H42C | 3276.81 | 9833.9 | 6985.69 | 62 |
H42D | 4553.41 | 9277.34 | 6597.06 | 62 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
H41A | 0.75 | H41B | 0.75 | H41C | 0.25 | ||
H41D | 0.25 | H34C | 0.492(12) | H34D | 0.492(12) | ||
H34A | 0.508(12) | H34B | 0.508(12) | C36A | 0.508(12) | ||
H36A | 0.508(12) | H36B | 0.508(12) | C42A | 0.71(3) | ||
H42A | 0.71(3) | H42B | 0.71(3) | C35B | 0.492(12) | ||
H35A | 0.492(12) | H35B | 0.492(12) | H43A | 0.75 | ||
H43B | 0.75 | H43C | 0.25 | H43D | 0.25 | ||
C35A | 0.508(12) | H35C | 0.508(12) | H35D | 0.508(12) | ||
C36B | 0.492(12) | H36C | 0.492(12) | H36D | 0.492(12) | ||
C42B | 0.29(3) | H42C | 0.29(3) | H42D | 0.29(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.
Crystal structure determination of [mo_B1036_0m]
Crystal Data for C24H54Li2O4Si2 (M =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)°, V = 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.