Identification code | 3182 |
Empirical formula | C28H68Li4O8Si4 |
Formula weight | 672.94 |
Temperature/K | 173.15 |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 20.3421(14) |
b/Å | 10.7413(5) |
c/Å | 21.0670(16) |
α/° | 90 |
β/° | 112.664(9) |
γ/° | 90 |
Volume/Å3 | 4247.7(5) |
Z | 4 |
ρcalcg/cm3 | 1.052 |
μ/mm‑1 | 0.176 |
F(000) | 1472.0 |
Crystal size/mm3 | 0.3 × 0.23 × 0.21 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.19 to 50 |
Index ranges | -24 ≤ h ≤ 24, -12 ≤ k ≤ 12, -25 ≤ l ≤ 24 |
Reflections collected | 46058 |
Independent reflections | 7469 [Rint = 0.0673, Rsigma = 0.0436] |
Data/restraints/parameters | 7469/0/409 |
Goodness-of-fit on F2 | 1.134 |
Final R indexes [I>=2σ (I)] | R1 = 0.0710, wR2 = 0.1920 |
Final R indexes [all data] | R1 = 0.0931, wR2 = 0.2057 |
Largest diff. peak/hole / e Å-3 | 0.43/-0.33 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Si3 | 11247.9(6) | 11341.2(10) | 1251.2(6) | 38.9(3) |
Si1 | 13955.3(5) | 11197.5(9) | 3555.2(5) | 29.1(3) |
Si4 | 13114.7(6) | 7435.0(11) | 1759.3(6) | 40.7(3) |
Si2 | 11590.5(6) | 8726.2(11) | 3504.9(6) | 40.9(3) |
O1 | 13230.9(12) | 10562(2) | 3054.8(12) | 28.7(6) |
O4 | 12790.2(12) | 8379(2) | 2141.1(12) | 29.4(6) |
O2 | 12010.6(13) | 9068(2) | 3027.7(12) | 33.4(6) |
O3 | 11875.7(12) | 10591(2) | 1825.4(12) | 32.4(6) |
O5 | 13587.3(15) | 7578(3) | 3815.9(13) | 42.9(7) |
O7 | 13394.5(15) | 11062(3) | 1557.8(15) | 46.6(7) |
O6 | 11867.5(15) | 12274(3) | 3145.1(17) | 54.6(8) |
O8 | 11064.2(15) | 7714(3) | 1443.5(15) | 49.9(8) |
C2 | 13965(2) | 11391(4) | 4450(2) | 44.7(10) |
C9 | 10352(2) | 10930(5) | 1252(2) | 51.8(11) |
C1 | 14757(2) | 10240(4) | 3641(2) | 43.3(10) |
C13 | 13512(3) | 6261(4) | 3691(2) | 54.3(12) |
C3 | 14093(2) | 12777(4) | 3245(2) | 43.8(10) |
C16 | 13929(2) | 7795(4) | 4539(2) | 47.5(11) |
C15 | 14241(3) | 6554(5) | 4853(2) | 60.5(13) |
C21 | 13161(3) | 12290(4) | 1295(2) | 53.8(12) |
C7 | 11219(3) | 11023(5) | 363(2) | 57.7(13) |
C26 | 10567(3) | 6453(5) | 466(3) | 61.7(14) |
C28 | 10734(3) | 6663(5) | 1614(3) | 58.8(13) |
C14 | 13735(3) | 5652(5) | 4388(3) | 66.9(15) |
C6 | 11920(3) | 9654(5) | 4331(2) | 62.5(13) |
C23 | 14164(3) | 11771(5) | 1049(3) | 67.1(15) |
C27 | 10218(2) | 6151(4) | 941(3) | 59.5(13) |
C24 | 14078(3) | 10829(5) | 1537(3) | 59.3(13) |
C11 | 14112(2) | 7337(5) | 2204(3) | 63.9(14) |
C12 | 12917(3) | 7919(6) | 846(2) | 68.4(15) |
C20 | 12292(3) | 13326(5) | 3489(3) | 63.5(14) |
C8 | 11341(3) | 13077(4) | 1383(3) | 66.8(15) |
C22 | 13777(3) | 12871(5) | 1171(3) | 67.4(15) |
C4 | 11697(3) | 7038(5) | 3757(3) | 61.6(13) |
C5 | 10605(2) | 9002(5) | 3059(3) | 59.4(13) |
C19 | 11993(3) | 13668(6) | 4011(3) | 72.9(16) |
C10 | 12754(3) | 5811(4) | 1707(3) | 67.1(15) |
C25 | 10897(3) | 7718(5) | 715(2) | 60.5(13) |
C18 | 11202(3) | 13495(7) | 3602(4) | 88(2) |
C17 | 11156(3) | 12523(6) | 3108(3) | 72.2(16) |
Li4 | 11838(3) | 8820(6) | 2060(3) | 33.3(14) |
Li3 | 12876(3) | 10199(6) | 2070(3) | 31.0(13) |
Li2 | 12216(3) | 10782(6) | 2824(3) | 31.5(13) |
Li1 | 12990(3) | 8805(6) | 3095(3) | 31.1(13) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Si3 | 29.6(6) | 38.1(6) | 36.3(6) | 6.3(5) | -1.5(5) | 1.0(5) |
Si1 | 22.4(5) | 35.2(5) | 23.9(5) | -4.4(4) | 2.4(4) | -3.3(4) |
Si4 | 39.4(6) | 40.2(6) | 42.7(7) | -12.9(5) | 16.3(5) | -0.5(5) |
Si2 | 34.4(6) | 51.5(7) | 38.4(6) | 2.3(5) | 15.8(5) | -3.2(5) |
O1 | 22.6(12) | 33.0(13) | 23.1(12) | -4.9(10) | 0.8(10) | -1.9(10) |
O4 | 29.8(13) | 29.0(13) | 26.1(13) | -2(1) | 7.2(11) | -0.5(10) |
O2 | 27.4(13) | 40.7(15) | 30.3(14) | 1.2(11) | 9.1(11) | -2.1(11) |
O3 | 27.9(13) | 32.9(13) | 27.5(13) | -0.4(11) | 0.9(11) | 0.4(11) |
O5 | 44.2(16) | 41.7(16) | 29.8(14) | 7.9(12) | 0.0(12) | 2.9(13) |
O7 | 49.1(17) | 50.7(17) | 46.7(17) | 2.3(14) | 25.7(14) | -11.7(14) |
O6 | 36.2(16) | 55.1(19) | 69(2) | -26.0(16) | 16.5(15) | 5.4(14) |
O8 | 46.4(17) | 46.8(17) | 39.1(17) | -3.8(13) | -2.9(13) | -16.1(14) |
C2 | 46(2) | 54(3) | 26(2) | -8.0(18) | 4.6(18) | -4(2) |
C9 | 32(2) | 62(3) | 49(3) | -1(2) | 2(2) | -1(2) |
C1 | 31(2) | 51(2) | 43(2) | 5(2) | 8.2(18) | 4.2(18) |
C13 | 62(3) | 42(2) | 46(3) | -1(2) | 7(2) | -5(2) |
C3 | 41(2) | 39(2) | 45(2) | -4.5(19) | 8.6(19) | -5.9(18) |
C16 | 51(3) | 48(3) | 34(2) | 2.1(19) | 7(2) | -4(2) |
C15 | 55(3) | 70(3) | 42(3) | 21(2) | 3(2) | 0(2) |
C21 | 55(3) | 53(3) | 50(3) | 9(2) | 16(2) | -8(2) |
C7 | 49(3) | 74(3) | 36(2) | 10(2) | 1(2) | -5(2) |
C26 | 66(3) | 54(3) | 45(3) | -13(2) | 0(2) | 0(2) |
C28 | 62(3) | 57(3) | 61(3) | -14(2) | 27(3) | -22(2) |
C14 | 73(3) | 50(3) | 59(3) | 14(2) | 4(3) | 1(3) |
C6 | 69(3) | 76(3) | 47(3) | -4(3) | 26(3) | -1(3) |
C23 | 70(3) | 84(4) | 57(3) | 6(3) | 35(3) | -17(3) |
C27 | 40(2) | 46(3) | 79(4) | -17(2) | 8(2) | -14(2) |
C24 | 55(3) | 69(3) | 58(3) | 4(3) | 27(3) | -4(2) |
C11 | 43(3) | 71(3) | 78(4) | -6(3) | 25(3) | 14(2) |
C12 | 77(4) | 92(4) | 40(3) | -22(3) | 27(3) | -18(3) |
C20 | 48(3) | 59(3) | 82(4) | -19(3) | 24(3) | -2(2) |
C8 | 57(3) | 41(3) | 78(4) | 13(2) | -1(3) | 4(2) |
C22 | 85(4) | 61(3) | 67(3) | 11(3) | 40(3) | -18(3) |
C4 | 59(3) | 63(3) | 66(3) | 14(3) | 27(3) | -2(2) |
C5 | 39(2) | 70(3) | 69(3) | -3(3) | 21(2) | -2(2) |
C19 | 70(4) | 70(4) | 73(4) | -30(3) | 21(3) | -3(3) |
C10 | 71(3) | 40(3) | 85(4) | -23(3) | 25(3) | -3(2) |
C25 | 59(3) | 68(3) | 42(3) | 1(2) | 6(2) | -10(3) |
C18 | 55(3) | 102(5) | 110(5) | -56(4) | 35(3) | -15(3) |
C17 | 40(3) | 80(4) | 91(4) | -26(3) | 20(3) | 8(3) |
Li4 | 27(3) | 34(3) | 29(3) | 0(3) | 0(3) | -4(3) |
Li3 | 29(3) | 38(3) | 22(3) | -1(2) | 6(2) | -3(3) |
Li2 | 29(3) | 32(3) | 33(3) | -5(3) | 12(3) | 5(3) |
Li1 | 28(3) | 32(3) | 29(3) | -3(3) | 6(3) | -2(2) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Si3 | O3 | 1.598(3) | O5 | C16 | 1.429(5) | |
Si3 | C9 | 1.877(4) | O5 | Li1 | 2.024(6) | |
Si3 | C7 | 1.881(5) | O7 | C21 | 1.439(5) | |
Si3 | C8 | 1.884(5) | O7 | C24 | 1.431(5) | |
Si1 | O1 | 1.597(2) | O7 | Li3 | 2.003(7) | |
Si1 | C2 | 1.888(4) | O6 | C20 | 1.438(6) | |
Si1 | C1 | 1.877(4) | O6 | C17 | 1.444(5) | |
Si1 | C3 | 1.878(4) | O6 | Li2 | 1.973(6) | |
Si4 | O4 | 1.588(3) | O8 | C28 | 1.429(5) | |
Si4 | C11 | 1.881(5) | O8 | C25 | 1.439(5) | |
Si4 | C12 | 1.881(5) | O8 | Li4 | 1.999(6) | |
Si4 | C10 | 1.880(5) | C13 | C14 | 1.510(6) | |
Si2 | O2 | 1.593(3) | C16 | C15 | 1.515(6) | |
Si2 | C6 | 1.890(5) | C15 | C14 | 1.477(7) | |
Si2 | C4 | 1.878(5) | C21 | C22 | 1.509(7) | |
Si2 | C5 | 1.880(5) | C26 | C27 | 1.470(7) | |
O1 | Li3 | 1.955(6) | C26 | C25 | 1.516(7) | |
O1 | Li2 | 1.945(6) | C28 | C27 | 1.506(6) | |
O1 | Li1 | 1.960(6) | C23 | C24 | 1.500(7) | |
O4 | Li4 | 1.936(7) | C23 | C22 | 1.496(8) | |
O4 | Li3 | 1.973(7) | C20 | C19 | 1.492(7) | |
O4 | Li1 | 1.945(6) | C19 | C18 | 1.517(7) | |
O2 | Li4 | 1.950(7) | C18 | C17 | 1.451(7) | |
O2 | Li2 | 1.971(7) | Li4 | Li3 | 2.573(8) | |
O2 | Li1 | 1.964(6) | Li4 | Li2 | 2.584(8) | |
O3 | Li4 | 1.975(7) | Li4 | Li1 | 2.513(8) | |
O3 | Li3 | 1.944(6) | Li3 | Li2 | 2.523(8) | |
O3 | Li2 | 1.956(6) | Li3 | Li1 | 2.563(8) | |
O5 | C13 | 1.436(5) | Li2 | Li1 | 2.574(8) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
O3 | Si3 | C9 | 111.96(18) | O4 | Li4 | Li2 | 95.6(3) | |
O3 | Si3 | C7 | 111.79(19) | O4 | Li4 | Li1 | 49.8(2) | |
O3 | Si3 | C8 | 112.44(18) | O2 | Li4 | O3 | 96.9(3) | |
C9 | Si3 | C7 | 107.4(2) | O2 | Li4 | O8 | 122.7(3) | |
C9 | Si3 | C8 | 106.0(2) | O2 | Li4 | Li3 | 95.5(3) | |
C7 | Si3 | C8 | 106.8(3) | O2 | Li4 | Li2 | 49.1(2) | |
O1 | Si1 | C2 | 110.99(17) | O2 | Li4 | Li1 | 50.3(2) | |
O1 | Si1 | C1 | 112.06(17) | O3 | Li4 | O8 | 120.5(3) | |
O1 | Si1 | C3 | 112.31(16) | O3 | Li4 | Li3 | 48.4(2) | |
C1 | Si1 | C2 | 106.83(19) | O3 | Li4 | Li2 | 48.6(2) | |
C1 | Si1 | C3 | 106.7(2) | O3 | Li4 | Li1 | 96.3(3) | |
C3 | Si1 | C2 | 107.6(2) | O8 | Li4 | Li3 | 141.8(3) | |
O4 | Si4 | C11 | 111.25(19) | O8 | Li4 | Li2 | 149.3(3) | |
O4 | Si4 | C12 | 112.0(2) | O8 | Li4 | Li1 | 142.9(3) | |
O4 | Si4 | C10 | 113.1(2) | Li3 | Li4 | Li2 | 58.6(2) | |
C12 | Si4 | C11 | 106.8(3) | Li1 | Li4 | Li3 | 60.5(2) | |
C10 | Si4 | C11 | 107.4(2) | Li1 | Li4 | Li2 | 60.7(2) | |
C10 | Si4 | C12 | 105.8(3) | O1 | Li3 | O4 | 97.2(3) | |
O2 | Si2 | C6 | 111.9(2) | O1 | Li3 | O7 | 115.1(3) | |
O2 | Si2 | C4 | 111.7(2) | O1 | Li3 | Li4 | 95.2(3) | |
O2 | Si2 | C5 | 112.06(19) | O1 | Li3 | Li2 | 49.5(2) | |
C4 | Si2 | C6 | 106.7(2) | O1 | Li3 | Li1 | 49.2(2) | |
C4 | Si2 | C5 | 106.1(2) | O4 | Li3 | O7 | 125.4(3) | |
C5 | Si2 | C6 | 108.0(2) | O4 | Li3 | Li4 | 48.2(2) | |
Si1 | O1 | Li3 | 130.9(2) | O4 | Li3 | Li2 | 96.5(3) | |
Si1 | O1 | Li2 | 137.2(2) | O4 | Li3 | Li1 | 48.7(2) | |
Si1 | O1 | Li1 | 124.4(2) | O3 | Li3 | O1 | 99.1(3) | |
Li3 | O1 | Li1 | 81.8(3) | O3 | Li3 | O4 | 96.9(3) | |
Li2 | O1 | Li3 | 80.6(3) | O3 | Li3 | O7 | 118.1(3) | |
Li2 | O1 | Li1 | 82.5(3) | O3 | Li3 | Li4 | 49.5(2) | |
Si4 | O4 | Li4 | 135.1(2) | O3 | Li3 | Li2 | 49.9(2) | |
Si4 | O4 | Li3 | 121.9(2) | O3 | Li3 | Li1 | 95.5(3) | |
Si4 | O4 | Li1 | 135.3(2) | O7 | Li3 | Li4 | 149.6(3) | |
Li4 | O4 | Li3 | 82.3(3) | O7 | Li3 | Li2 | 138.0(3) | |
Li4 | O4 | Li1 | 80.7(3) | O7 | Li3 | Li1 | 146.0(3) | |
Li1 | O4 | Li3 | 81.7(3) | Li2 | Li3 | Li4 | 60.9(2) | |
Si2 | O2 | Li4 | 134.8(2) | Li2 | Li3 | Li1 | 60.8(2) | |
Si2 | O2 | Li2 | 124.2(2) | Li1 | Li3 | Li4 | 58.6(2) | |
Si2 | O2 | Li1 | 134.3(2) | O1 | Li2 | O2 | 97.2(3) | |
Li4 | O2 | Li2 | 82.4(3) | O1 | Li2 | O3 | 99.0(3) | |
Li4 | O2 | Li1 | 79.9(3) | O1 | Li2 | O6 | 120.0(3) | |
Li1 | O2 | Li2 | 81.7(3) | O1 | Li2 | Li4 | 95.1(3) | |
Si3 | O3 | Li4 | 125.3(2) | O1 | Li2 | Li3 | 49.9(2) | |
Si3 | O3 | Li3 | 139.5(2) | O1 | Li2 | Li1 | 49.0(2) | |
Si3 | O3 | Li2 | 127.6(2) | O2 | Li2 | O6 | 123.4(3) | |
Li3 | O3 | Li4 | 82.1(3) | O2 | Li2 | Li4 | 48.4(2) | |
Li3 | O3 | Li2 | 80.6(3) | O2 | Li2 | Li3 | 96.5(3) | |
Li2 | O3 | Li4 | 82.2(3) | O2 | Li2 | Li1 | 49.0(2) | |
C13 | O5 | Li1 | 120.8(3) | O3 | Li2 | O2 | 96.8(3) | |
C16 | O5 | C13 | 109.3(3) | O3 | Li2 | O6 | 115.4(3) | |
C16 | O5 | Li1 | 126.8(3) | O3 | Li2 | Li4 | 49.2(2) | |
C21 | O7 | Li3 | 117.9(3) | O3 | Li2 | Li3 | 49.5(2) | |
C24 | O7 | C21 | 109.2(3) | O3 | Li2 | Li1 | 94.8(3) | |
C24 | O7 | Li3 | 130.9(3) | O6 | Li2 | Li4 | 144.7(3) | |
C20 | O6 | C17 | 106.0(3) | O6 | Li2 | Li3 | 140.0(4) | |
C20 | O6 | Li2 | 125.9(3) | O6 | Li2 | Li1 | 149.8(3) | |
C17 | O6 | Li2 | 128.1(3) | Li3 | Li2 | Li4 | 60.5(2) | |
C28 | O8 | C25 | 109.2(3) | Li3 | Li2 | Li1 | 60.4(2) | |
C28 | O8 | Li4 | 129.4(3) | Li1 | Li2 | Li4 | 58.3(2) | |
C25 | O8 | Li4 | 119.6(3) | O1 | Li1 | O2 | 97.0(3) | |
O5 | C13 | C14 | 106.1(4) | O1 | Li1 | O5 | 124.9(3) | |
O5 | C16 | C15 | 105.8(4) | O1 | Li1 | Li4 | 97.0(3) | |
C14 | C15 | C16 | 102.7(4) | O1 | Li1 | Li3 | 49.0(2) | |
O7 | C21 | C22 | 105.9(4) | O1 | Li1 | Li2 | 48.5(2) | |
C27 | C26 | C25 | 103.1(4) | O4 | Li1 | O1 | 97.9(3) | |
O8 | C28 | C27 | 106.0(4) | O4 | Li1 | O2 | 99.0(3) | |
C15 | C14 | C13 | 103.4(4) | O4 | Li1 | O5 | 116.7(3) | |
C22 | C23 | C24 | 102.0(4) | O4 | Li1 | Li4 | 49.5(2) | |
C26 | C27 | C28 | 102.5(4) | O4 | Li1 | Li3 | 49.6(2) | |
O7 | C24 | C23 | 105.9(4) | O4 | Li1 | Li2 | 95.6(3) | |
O6 | C20 | C19 | 103.3(4) | O2 | Li1 | O5 | 116.5(3) | |
C23 | C22 | C21 | 103.3(4) | O2 | Li1 | Li4 | 49.8(2) | |
C20 | C19 | C18 | 101.3(4) | O2 | Li1 | Li3 | 95.5(3) | |
O8 | C25 | C26 | 105.0(4) | O2 | Li1 | Li2 | 49.3(2) | |
C17 | C18 | C19 | 104.8(4) | O5 | Li1 | Li4 | 138.2(3) | |
O6 | C17 | C18 | 108.0(4) | O5 | Li1 | Li3 | 147.8(3) | |
O4 | Li4 | O2 | 99.8(3) | O5 | Li1 | Li2 | 147.4(3) | |
O4 | Li4 | O3 | 97.1(3) | Li4 | Li1 | Li3 | 60.9(2) | |
O4 | Li4 | O8 | 115.0(3) | Li4 | Li1 | Li2 | 61.0(2) | |
O4 | Li4 | Li3 | 49.5(2) | Li3 | Li1 | Li2 | 58.8(2) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
O5 | C13 | C14 | C15 | -27.3(6) | C11 | Si4 | O4 | Li3 | 74.7(3) | |
O5 | C16 | C15 | C14 | -31.2(5) | C11 | Si4 | O4 | Li1 | -38.1(4) | |
O7 | C21 | C22 | C23 | 26.4(5) | C12 | Si4 | O4 | Li4 | 68.8(4) | |
O6 | C20 | C19 | C18 | -40.3(6) | C12 | Si4 | O4 | Li3 | -44.8(3) | |
O8 | C28 | C27 | C26 | 31.2(5) | C12 | Si4 | O4 | Li1 | -157.6(3) | |
C2 | Si1 | O1 | Li3 | 176.2(3) | C20 | O6 | C17 | C18 | -17.3(7) | |
C2 | Si1 | O1 | Li2 | 48.0(4) | C20 | C19 | C18 | C17 | 29.7(7) | |
C2 | Si1 | O1 | Li1 | -72.4(3) | C8 | Si3 | O3 | Li4 | 159.8(3) | |
C9 | Si3 | O3 | Li4 | 40.5(3) | C8 | Si3 | O3 | Li3 | -75.5(4) | |
C9 | Si3 | O3 | Li3 | 165.3(4) | C8 | Si3 | O3 | Li2 | 50.2(4) | |
C9 | Si3 | O3 | Li2 | -69.0(3) | C22 | C23 | C24 | O7 | 33.7(5) | |
C1 | Si1 | O1 | Li3 | -64.5(3) | C4 | Si2 | O2 | Li4 | 77.6(4) | |
C1 | Si1 | O1 | Li2 | 167.3(3) | C4 | Si2 | O2 | Li2 | -165.7(3) | |
C1 | Si1 | O1 | Li1 | 46.9(3) | C4 | Si2 | O2 | Li1 | -50.8(4) | |
C13 | O5 | C16 | C15 | 14.5(5) | C5 | Si2 | O2 | Li4 | -41.4(4) | |
C3 | Si1 | O1 | Li3 | 55.7(3) | C5 | Si2 | O2 | Li2 | 75.4(3) | |
C3 | Si1 | O1 | Li2 | -72.6(4) | C5 | Si2 | O2 | Li1 | -169.8(3) | |
C3 | Si1 | O1 | Li1 | 167.0(3) | C19 | C18 | C17 | O6 | -8.5(7) | |
C16 | O5 | C13 | C14 | 7.8(5) | C10 | Si4 | O4 | Li4 | -50.6(4) | |
C16 | C15 | C14 | C13 | 35.1(6) | C10 | Si4 | O4 | Li3 | -164.3(3) | |
C21 | O7 | C24 | C23 | -17.9(5) | C10 | Si4 | O4 | Li1 | 82.9(4) | |
C7 | Si3 | O3 | Li4 | -80.1(3) | C25 | O8 | C28 | C27 | -12.0(5) | |
C7 | Si3 | O3 | Li3 | 44.7(4) | C25 | C26 | C27 | C28 | -37.2(5) | |
C7 | Si3 | O3 | Li2 | 170.4(3) | C17 | O6 | C20 | C19 | 36.4(6) | |
C28 | O8 | C25 | C26 | -11.4(5) | Li4 | O8 | C28 | C27 | -176.8(4) | |
C6 | Si2 | O2 | Li4 | -162.8(3) | Li4 | O8 | C25 | C26 | 155.1(4) | |
C6 | Si2 | O2 | Li2 | -46.1(3) | Li3 | O7 | C21 | C22 | 160.4(4) | |
C6 | Si2 | O2 | Li1 | 68.8(4) | Li3 | O7 | C24 | C23 | 178.8(4) | |
C27 | C26 | C25 | O8 | 30.8(5) | Li2 | O6 | C20 | C19 | -141.8(4) | |
C24 | O7 | C21 | C22 | -5.4(5) | Li2 | O6 | C17 | C18 | 160.7(5) | |
C24 | C23 | C22 | C21 | -36.2(5) | Li1 | O5 | C13 | C14 | -153.6(4) | |
C11 | Si4 | O4 | Li4 | -171.6(4) | Li1 | O5 | C16 | C15 | 174.5(4) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H2A | 13574 | 11940 | 4432 | 67 |
H2B | 14420 | 11758 | 4750 | 67 |
H2C | 13907 | 10576 | 4631 | 67 |
H9A | 10257 | 10043 | 1146 | 78 |
H9B | 9984 | 11427 | 904 | 78 |
H9C | 10346 | 11104 | 1706 | 78 |
H1A | 14709 | 9406 | 3808 | 65 |
H1B | 15187 | 10640 | 3968 | 65 |
H1C | 14793 | 10172 | 3192 | 65 |
H13A | 13821 | 5980 | 3452 | 65 |
H13B | 13012 | 6049 | 3402 | 65 |
H3A | 14181 | 12688 | 2821 | 66 |
H3B | 14503 | 13181 | 3598 | 66 |
H3C | 13666 | 13286 | 3153 | 66 |
H16A | 13580 | 8091 | 4728 | 57 |
H16B | 14309 | 8428 | 4635 | 57 |
H15A | 14726 | 6440 | 4858 | 73 |
H15B | 14261 | 6477 | 5329 | 73 |
H21A | 13043 | 12785 | 1633 | 65 |
H21B | 12735 | 12244 | 861 | 65 |
H7A | 11653 | 11344 | 325 | 87 |
H7B | 10802 | 11435 | 22 | 87 |
H7C | 11186 | 10123 | 278 | 87 |
H26A | 10217 | 6495 | -15 | 74 |
H26B | 10937 | 5830 | 496 | 74 |
H28A | 10480 | 6917 | 1910 | 71 |
H28B | 11096 | 6029 | 1861 | 71 |
H14A | 13321 | 5523 | 4517 | 80 |
H14B | 13969 | 4840 | 4396 | 80 |
H6A | 12429 | 9496 | 4583 | 94 |
H6B | 11656 | 9405 | 4614 | 94 |
H6C | 11844 | 10544 | 4224 | 94 |
H23A | 14672 | 11964 | 1161 | 80 |
H23B | 13943 | 11480 | 566 | 80 |
H27A | 10157 | 5240 | 969 | 71 |
H27B | 9748 | 6561 | 800 | 71 |
H24A | 14101 | 9974 | 1372 | 71 |
H24B | 14459 | 10927 | 2000 | 71 |
H11A | 14321 | 8154 | 2194 | 96 |
H11B | 14296 | 6727 | 1968 | 96 |
H11C | 14238 | 7078 | 2683 | 96 |
H12A | 12402 | 7883 | 581 | 103 |
H12B | 13159 | 7355 | 641 | 103 |
H12C | 13086 | 8771 | 840 | 103 |
H20A | 12241 | 14020 | 3164 | 76 |
H20B | 12802 | 13097 | 3712 | 76 |
H8A | 11453 | 13271 | 1868 | 100 |
H8B | 10894 | 13484 | 1097 | 100 |
H8C | 11726 | 13380 | 1253 | 100 |
H22A | 13605 | 13426 | 764 | 81 |
H22B | 14086 | 13353 | 1576 | 81 |
H4A | 11529 | 6521 | 3341 | 92 |
H4B | 11416 | 6854 | 4033 | 92 |
H4C | 12200 | 6860 | 4026 | 92 |
H5A | 10513 | 9899 | 3003 | 89 |
H5B | 10358 | 8649 | 3335 | 89 |
H5C | 10431 | 8603 | 2605 | 89 |
H19A | 12108 | 14540 | 4167 | 87 |
H19B | 12169 | 13106 | 4414 | 87 |
H10A | 12896 | 5467 | 2172 | 101 |
H10B | 12944 | 5287 | 1437 | 101 |
H10C | 12233 | 5831 | 1486 | 101 |
H25A | 11333 | 7835 | 619 | 73 |
H25B | 10556 | 8392 | 486 | 73 |
H18A | 10957 | 13239 | 3906 | 106 |
H18B | 10983 | 14276 | 3364 | 106 |
H17A | 10948 | 11760 | 3218 | 87 |
H17B | 10848 | 12796 | 2638 | 87 |
Experimental
Single crystals of C28H68Li4O8Si4 [3182] 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.
Crystal structure determination of [3182]
Crystal Data for C28H68Li4O8Si4 (M =672.94 g/mol): monoclinic, space group P21/c (no. 14), a = 20.3421(14) Å, b = 10.7413(5) Å, c = 21.0670(16) Å, β = 112.664(9)°, V = 4247.7(5) Å3, Z = 4, T = 173.15 K, μ(MoKα) = 0.176 mm-1, Dcalc = 1.052 g/cm3, 46058 reflections measured (4.19° ≤ 2Θ ≤ 50°), 7469 unique (Rint = 0.0673, Rsigma = 0.0436) which were used in all calculations. The final R1 was 0.0710 (I > 2σ(I)) and wR2 was 0.2057 (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:
C13(H13A,H13B), C16(H16A,H16B), C15(H15A,H15B), C21(H21A,H21B), C26(H26A,
H26B), C28(H28A,H28B), C14(H14A,H14B), C23(H23A,H23B), C27(H27A,H27B),
C24(H24A,H24B), C20(H20A,H20B), C22(H22A,H22B), C19(H19A,H19B), C25(H25A,H25B),
C18(H18A,H18B), C17(H17A,H17B)
2.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C7(H7A,
H7B,H7C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C8(H8A,
H8B,H8C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
This report has been created with Olex2, compiled on 2016.02.19 svn.r3266 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.