Identification code | mo_B1032_0m |
Empirical formula | C28H68Li4O3Si4 |
Formula weight | 592.94 |
Temperature/K | 100.01 |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 9.8606(18) |
b/Å | 19.160(2) |
c/Å | 20.638(3) |
α/° | 90 |
β/° | 91.536(6) |
γ/° | 90 |
Volume/Å3 | 3897.8(10) |
Z | 4 |
ρcalcg/cm3 | 1.010 |
μ/mm‑1 | 0.176 |
F(000) | 1312.0 |
Crystal size/mm3 | 0.34 × 0.25 × 0.15 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.484 to 54 |
Index ranges | -12 ≤ h ≤ 12, -24 ≤ k ≤ 24, -25 ≤ l ≤ 26 |
Reflections collected | 38837 |
Independent reflections | 8504 [Rint = 0.0304, Rsigma = 0.0268] |
Data/restraints/parameters | 8504/0/396 |
Goodness-of-fit on F2 | 1.059 |
Final R indexes [I>=2σ (I)] | R1 = 0.0315, wR2 = 0.0774 |
Final R indexes [all data] | R1 = 0.0403, wR2 = 0.0814 |
Largest diff. peak/hole / e Å-3 | 0.47/-0.29 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Si3 | 1672.5(3) | 8115.3(2) | 1193.9(2) | 12.85(8) |
Si4 | 3773.4(3) | 8948.6(2) | 3592.4(2) | 13.92(8) |
Si2 | 6291.5(3) | 6976.6(2) | 1872.1(2) | 12.86(8) |
Si1 | 1596.0(3) | 5485.7(2) | 3463.7(2) | 13.77(8) |
O1 | 1710.4(8) | 6038.3(4) | 1531.7(4) | 14.54(18) |
O2 | 5343.3(9) | 6459.9(5) | 3911.2(4) | 18.8(2) |
O3 | 95.5(8) | 7882.4(5) | 3536.8(4) | 15.59(19) |
C9 | 1596.7(12) | 7778.5(7) | 2028.4(6) | 14.0(2) |
C8 | 7738.3(13) | 6672.2(7) | 2409.2(7) | 20.4(3) |
C13 | 3771.1(12) | 7997.3(6) | 3467.4(6) | 13.8(2) |
C1 | 1834.1(13) | 6423.6(6) | 3276.7(6) | 14.8(2) |
C10 | 2631.8(14) | 7519.3(7) | 640.6(6) | 19.7(3) |
C4 | 637.8(17) | 5018.4(8) | 2796.6(7) | 28.3(3) |
C28 | -1023.4(12) | 8272.4(7) | 3248.5(6) | 18.2(3) |
C11 | 2559.0(14) | 8984.5(7) | 1179.3(7) | 22.0(3) |
C14 | 4621.2(15) | 9246.0(8) | 4375.3(7) | 25.4(3) |
C7 | 6361.1(14) | 7958.4(7) | 1829.5(7) | 23.5(3) |
C19 | 540.0(14) | 5679.4(7) | 578.4(7) | 22.7(3) |
C17 | 2552.4(13) | 5531.2(7) | 1213.1(7) | 21.3(3) |
C18 | 1609.4(14) | 5132.5(7) | 752.7(7) | 24.1(3) |
C5 | 4642.5(12) | 6699.8(7) | 2176.5(7) | 15.2(3) |
C21 | 6441.5(14) | 5957.2(7) | 3925.7(7) | 22.1(3) |
C12 | -45.7(13) | 8248.0(7) | 786.0(7) | 20.0(3) |
C20 | 384.5(12) | 6055.0(7) | 1217.3(6) | 17.1(3) |
C23 | 6098.1(17) | 6313.5(8) | 5005.5(7) | 29.4(3) |
C6 | 6656.1(14) | 6654.6(9) | 1030.0(7) | 26.5(3) |
C27 | -2203.5(13) | 8171.6(8) | 3701.1(7) | 25.9(3) |
C2 | 3249.5(15) | 5016.4(7) | 3589.8(8) | 26.7(3) |
C22 | 6522.3(14) | 5680.5(7) | 4612.6(7) | 22.2(3) |
C15 | 4632.2(15) | 9414.7(7) | 2914.2(7) | 24.3(3) |
C16 | 2011.8(14) | 9323.2(7) | 3616.2(8) | 27.5(3) |
C26 | -1495.9(14) | 8058.8(8) | 4355.0(7) | 24.9(3) |
C25 | -258.8(15) | 7642.4(8) | 4172.7(7) | 24.7(3) |
C3 | 617.1(16) | 5345.2(8) | 4221.6(7) | 28.2(3) |
C24 | 5012.2(16) | 6640.5(8) | 4571.7(7) | 28.5(3) |
Li3 | 1762(2) | 7606.0(11) | 3114.5(10) | 15.3(4) |
Li1 | 2338(2) | 6631.4(11) | 2250.1(10) | 15.9(4) |
Li2 | 4044(2) | 6761.4(11) | 3219.5(11) | 17.6(4) |
Li4 | 3733(2) | 7743.9(11) | 2410.5(11) | 16.4(4) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Si3 | 13.67(16) | 13.29(16) | 11.53(17) | 2.44(13) | -0.68(13) | -1.96(12) |
Si4 | 13.19(16) | 12.21(16) | 16.25(18) | -3.43(13) | -1.87(13) | -0.35(12) |
Si2 | 10.41(16) | 16.45(17) | 11.80(17) | -0.73(13) | 2.23(12) | -0.47(12) |
Si1 | 17.32(17) | 11.94(16) | 12.09(17) | -0.41(13) | 0.83(13) | -0.59(12) |
O1 | 12.0(4) | 16.7(4) | 14.7(4) | -3.8(4) | -2.6(3) | 0.7(3) |
O2 | 21.4(5) | 21.3(5) | 13.7(5) | 0.1(4) | -2.2(4) | 10.1(4) |
O3 | 13.1(4) | 19.2(4) | 14.6(4) | 4.6(4) | 3.0(3) | 5.0(3) |
C9 | 15.2(6) | 14.7(6) | 12.1(6) | 1.7(5) | 1.2(5) | 0.2(5) |
C8 | 14.7(6) | 25.9(7) | 20.4(7) | -0.1(6) | 0.5(5) | 1.4(5) |
C13 | 11.4(6) | 13.5(6) | 16.5(6) | -1.0(5) | -0.8(5) | 1.0(5) |
C1 | 15.5(6) | 12.9(6) | 15.9(7) | -2.1(5) | -2.8(5) | 2.1(5) |
C10 | 21.8(7) | 22.1(7) | 15.4(7) | 1.8(5) | 5.0(5) | -1.9(5) |
C4 | 43.6(9) | 20.1(7) | 20.7(7) | 2.7(6) | -6.8(6) | -12.5(6) |
C28 | 12.7(6) | 23.0(7) | 18.8(7) | 0.1(5) | -3.3(5) | 4.5(5) |
C11 | 23.8(7) | 18.5(7) | 23.7(7) | 4.1(6) | -2.4(6) | -4.9(5) |
C14 | 25.7(7) | 28.3(8) | 22.1(7) | -10.4(6) | -2.7(6) | -0.5(6) |
C7 | 22.3(7) | 20.7(7) | 27.4(8) | 5.4(6) | 0.7(6) | -2.6(5) |
C19 | 23.4(7) | 24.8(7) | 19.6(7) | -5.8(6) | -6.9(5) | 0.1(5) |
C17 | 18.5(6) | 20.6(7) | 24.4(7) | -9.1(6) | -4.4(5) | 5.6(5) |
C18 | 25.1(7) | 20.1(7) | 26.9(8) | -9.3(6) | -4.5(6) | 1.7(5) |
C5 | 12.2(6) | 17.0(6) | 16.4(7) | -2.2(5) | 1.9(5) | -1.1(5) |
C21 | 18.0(6) | 27.3(7) | 21.2(7) | 4.8(6) | 3.0(5) | 10.6(5) |
C12 | 19.3(6) | 21.6(7) | 18.8(7) | 3.6(5) | -4.1(5) | -0.9(5) |
C20 | 12.2(6) | 19.1(6) | 19.9(7) | -2.3(5) | -3.7(5) | -0.9(5) |
C23 | 40.6(9) | 29.6(8) | 17.5(7) | -0.1(6) | -8.4(6) | 8.3(7) |
C6 | 21.1(7) | 42.2(9) | 16.5(7) | -5.0(6) | 4.7(5) | -0.3(6) |
C27 | 13.5(6) | 34.2(8) | 30.2(8) | -8.0(6) | 3.5(6) | 2.6(6) |
C2 | 27.0(7) | 16.9(7) | 36.2(9) | 2.8(6) | 0.1(6) | 5.0(5) |
C22 | 21.1(7) | 24.6(7) | 20.9(7) | 6.2(6) | 0.5(5) | 6.8(5) |
C15 | 30.8(8) | 18.6(7) | 23.3(7) | 0.7(6) | -1.6(6) | -6.9(6) |
C16 | 18.2(7) | 17.6(7) | 46.3(10) | -6.1(6) | -4.4(6) | 3.8(5) |
C26 | 24.8(7) | 27.7(7) | 22.8(7) | -1.8(6) | 9.6(6) | 3.5(6) |
C25 | 28.7(7) | 28.4(8) | 17.5(7) | 6.2(6) | 8.5(6) | 7.9(6) |
C3 | 36.4(8) | 24.6(7) | 24.1(8) | 1.1(6) | 11.9(6) | -5.2(6) |
C24 | 38.8(9) | 32.2(8) | 14.3(7) | -3.6(6) | -2.1(6) | 16.9(7) |
Li3 | 12.8(10) | 17.1(10) | 15.9(11) | -0.4(8) | 1.2(8) | 1.0(8) |
Li1 | 14.8(10) | 18.1(11) | 14.6(11) | -2.1(8) | -0.2(8) | -1.8(8) |
Li2 | 16.8(10) | 19.9(11) | 15.9(11) | 1.0(9) | -2.2(8) | 1.0(8) |
Li4 | 16(1) | 16(1) | 17.1(11) | 1.1(8) | 1.5(8) | -2.4(8) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Si3 | C9 | 1.8424(13) | C9 | Li1 | 2.357(2) | |
Si3 | C10 | 1.8869(13) | C9 | Li4 | 2.230(2) | |
Si3 | C11 | 1.8816(13) | C13 | Li3 | 2.223(2) | |
Si3 | C12 | 1.8888(14) | C13 | Li2 | 2.439(3) | |
Si4 | C13 | 1.8408(13) | C13 | Li4 | 2.234(3) | |
Si4 | C14 | 1.8872(14) | C1 | Li3 | 2.291(2) | |
Si4 | C15 | 1.8808(14) | C1 | Li1 | 2.225(3) | |
Si4 | C16 | 1.8814(14) | C1 | Li2 | 2.280(3) | |
Si2 | C8 | 1.8760(14) | C28 | C27 | 1.5238(18) | |
Si2 | C7 | 1.8846(14) | C19 | C18 | 1.5228(19) | |
Si2 | C5 | 1.8370(13) | C19 | C20 | 1.5136(18) | |
Si2 | C6 | 1.8879(14) | C17 | C18 | 1.5178(19) | |
Si2 | Li4 | 3.149(2) | C5 | Li1 | 2.285(2) | |
Si1 | C1 | 1.8543(13) | C5 | Li2 | 2.250(3) | |
Si1 | C4 | 1.8762(15) | C5 | Li4 | 2.250(3) | |
Si1 | C2 | 1.8739(14) | C21 | C22 | 1.5136(19) | |
Si1 | C3 | 1.8793(14) | C23 | C22 | 1.524(2) | |
O1 | C17 | 1.4474(15) | C23 | C24 | 1.513(2) | |
O1 | C20 | 1.4443(15) | C27 | C26 | 1.518(2) | |
O1 | Li1 | 1.955(2) | C26 | C25 | 1.5135(19) | |
O2 | C21 | 1.4490(15) | Li3 | Li1 | 2.654(3) | |
O2 | C24 | 1.4520(16) | Li3 | Li2 | 2.776(3) | |
O2 | Li2 | 1.978(2) | Li3 | Li4 | 2.471(3) | |
O3 | C28 | 1.4473(15) | Li1 | Li2 | 2.591(3) | |
O3 | C25 | 1.4424(16) | Li1 | Li4 | 2.553(3) | |
O3 | Li3 | 1.954(2) | Li2 | Li4 | 2.529(3) | |
C9 | Li3 | 2.267(2) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C9 | Si3 | C10 | 112.78(6) | C9 | Li3 | C1 | 106.84(10) | |
C9 | Si3 | C11 | 110.83(6) | C9 | Li3 | Li1 | 56.57(7) | |
C9 | Si3 | C12 | 113.91(6) | C9 | Li3 | Li2 | 101.47(9) | |
C10 | Si3 | C12 | 105.66(6) | C9 | Li3 | Li4 | 55.95(8) | |
C11 | Si3 | C10 | 106.58(6) | C13 | Li3 | C9 | 108.34(10) | |
C11 | Si3 | C12 | 106.57(6) | C13 | Li3 | C1 | 105.18(10) | |
C13 | Si4 | C14 | 114.69(6) | C13 | Li3 | Li1 | 104.64(9) | |
C13 | Si4 | C15 | 111.39(6) | C13 | Li3 | Li2 | 57.14(7) | |
C13 | Si4 | C16 | 112.56(6) | C13 | Li3 | Li4 | 56.54(8) | |
C15 | Si4 | C14 | 107.21(7) | C1 | Li3 | Li1 | 52.86(7) | |
C15 | Si4 | C16 | 105.82(7) | C1 | Li3 | Li2 | 52.42(7) | |
C16 | Si4 | C14 | 104.51(7) | C1 | Li3 | Li4 | 99.78(9) | |
C8 | Si2 | C7 | 108.05(6) | Li1 | Li3 | Li2 | 56.96(8) | |
C8 | Si2 | C6 | 106.37(6) | Li4 | Li3 | Li1 | 59.62(8) | |
C8 | Si2 | Li4 | 122.73(6) | Li4 | Li3 | Li2 | 57.29(8) | |
C7 | Si2 | C6 | 105.97(7) | O1 | Li1 | C9 | 107.73(10) | |
C7 | Si2 | Li4 | 65.22(6) | O1 | Li1 | C1 | 122.94(11) | |
C5 | Si2 | C8 | 111.98(6) | O1 | Li1 | C5 | 106.14(10) | |
C5 | Si2 | C7 | 109.74(6) | O1 | Li1 | Li3 | 148.14(11) | |
C5 | Si2 | C6 | 114.37(6) | O1 | Li1 | Li2 | 145.79(12) | |
C5 | Si2 | Li4 | 44.69(6) | O1 | Li1 | Li4 | 137.89(12) | |
C6 | Si2 | Li4 | 130.66(6) | C9 | Li1 | Li3 | 53.40(7) | |
C1 | Si1 | C4 | 111.95(6) | C9 | Li1 | Li2 | 104.59(10) | |
C1 | Si1 | C2 | 112.29(6) | C9 | Li1 | Li4 | 53.84(7) | |
C1 | Si1 | C3 | 112.51(6) | C1 | Li1 | C9 | 106.01(9) | |
C4 | Si1 | C3 | 106.42(7) | C1 | Li1 | C5 | 108.75(10) | |
C2 | Si1 | C4 | 106.99(7) | C1 | Li1 | Li3 | 55.16(7) | |
C2 | Si1 | C3 | 106.26(7) | C1 | Li1 | Li2 | 55.88(8) | |
C17 | O1 | Li1 | 124.11(10) | C1 | Li1 | Li4 | 99.16(10) | |
C20 | O1 | C17 | 109.52(9) | C5 | Li1 | C9 | 103.73(9) | |
C20 | O1 | Li1 | 126.31(9) | C5 | Li1 | Li3 | 103.62(9) | |
C21 | O2 | C24 | 109.01(10) | C5 | Li1 | Li2 | 54.52(7) | |
C21 | O2 | Li2 | 132.69(10) | C5 | Li1 | Li4 | 55.09(7) | |
C24 | O2 | Li2 | 116.76(10) | Li2 | Li1 | Li3 | 63.88(8) | |
C28 | O3 | Li3 | 126.70(10) | Li4 | Li1 | Li3 | 56.62(8) | |
C25 | O3 | C28 | 109.76(9) | Li4 | Li1 | Li2 | 58.90(8) | |
C25 | O3 | Li3 | 123.13(10) | O2 | Li2 | C13 | 101.84(10) | |
Si3 | C9 | Li3 | 166.28(9) | O2 | Li2 | C1 | 118.75(11) | |
Si3 | C9 | Li1 | 119.20(8) | O2 | Li2 | C5 | 119.59(11) | |
Si3 | C9 | Li4 | 106.22(8) | O2 | Li2 | Li3 | 137.26(11) | |
Li3 | C9 | Li1 | 70.03(8) | O2 | Li2 | Li1 | 157.43(12) | |
Li4 | C9 | Li3 | 66.66(8) | O2 | Li2 | Li4 | 139.34(12) | |
Li4 | C9 | Li1 | 67.58(8) | C13 | Li2 | Li3 | 49.94(7) | |
Si4 | C13 | Li3 | 112.19(8) | C13 | Li2 | Li1 | 100.50(9) | |
Si4 | C13 | Li2 | 172.28(9) | C13 | Li2 | Li4 | 53.40(7) | |
Si4 | C13 | Li4 | 110.61(8) | C1 | Li2 | C13 | 98.84(9) | |
Li3 | C13 | Li2 | 72.92(8) | C1 | Li2 | Li3 | 52.79(7) | |
Li3 | C13 | Li4 | 67.35(8) | C1 | Li2 | Li1 | 53.90(7) | |
Li4 | C13 | Li2 | 65.37(8) | C1 | Li2 | Li4 | 98.40(10) | |
Si1 | C1 | Li3 | 170.13(9) | C5 | Li2 | C13 | 106.55(10) | |
Si1 | C1 | Li1 | 113.85(8) | C5 | Li2 | C1 | 108.06(10) | |
Si1 | C1 | Li2 | 114.37(8) | C5 | Li2 | Li3 | 100.87(10) | |
Li1 | C1 | Li3 | 71.98(8) | C5 | Li2 | Li1 | 55.79(7) | |
Li1 | C1 | Li2 | 70.22(9) | C5 | Li2 | Li4 | 55.80(8) | |
Li2 | C1 | Li3 | 74.79(8) | Li1 | Li2 | Li3 | 59.16(8) | |
O3 | C28 | C27 | 105.59(11) | Li4 | Li2 | Li3 | 55.29(8) | |
C20 | C19 | C18 | 101.95(11) | Li4 | Li2 | Li1 | 59.80(8) | |
O1 | C17 | C18 | 105.84(10) | C9 | Li4 | Si2 | 130.34(9) | |
C17 | C18 | C19 | 102.14(11) | C9 | Li4 | C13 | 109.27(10) | |
Si2 | C5 | Li1 | 158.46(10) | C9 | Li4 | C5 | 109.19(10) | |
Si2 | C5 | Li2 | 124.68(9) | C9 | Li4 | Li3 | 57.39(8) | |
Si2 | C5 | Li4 | 100.28(8) | C9 | Li4 | Li1 | 58.58(8) | |
Li2 | C5 | Li1 | 69.69(8) | C9 | Li4 | Li2 | 110.64(10) | |
Li2 | C5 | Li4 | 68.40(9) | C13 | Li4 | Si2 | 116.95(9) | |
Li4 | C5 | Li1 | 68.52(8) | C13 | Li4 | C5 | 113.98(10) | |
O2 | C21 | C22 | 105.82(10) | C13 | Li4 | Li3 | 56.10(8) | |
O1 | C20 | C19 | 105.62(10) | C13 | Li4 | Li1 | 107.64(10) | |
C24 | C23 | C22 | 102.40(12) | C13 | Li4 | Li2 | 61.23(8) | |
C26 | C27 | C28 | 102.87(11) | C5 | Li4 | Si2 | 35.03(4) | |
C21 | C22 | C23 | 102.20(11) | C5 | Li4 | Li3 | 110.82(10) | |
C25 | C26 | C27 | 102.03(11) | C5 | Li4 | Li1 | 56.39(7) | |
O3 | C25 | C26 | 105.93(11) | C5 | Li4 | Li2 | 55.80(8) | |
O2 | C24 | C23 | 106.47(11) | Li3 | Li4 | Si2 | 143.87(10) | |
O3 | Li3 | C9 | 111.25(10) | Li3 | Li4 | Li1 | 63.75(8) | |
O3 | Li3 | C13 | 121.02(11) | Li3 | Li4 | Li2 | 67.42(9) | |
O3 | Li3 | C1 | 103.06(10) | Li1 | Li4 | Si2 | 89.90(8) | |
O3 | Li3 | Li1 | 133.48(11) | Li2 | Li4 | Si2 | 78.52(7) | |
O3 | Li3 | Li2 | 144.40(11) | Li2 | Li4 | Li1 | 61.30(8) | |
O3 | Li3 | Li4 | 156.52(12) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H8A | 8592.9 | 6853.81 | 2245.64 | 31 |
H8B | 7765 | 6160.88 | 2411.35 | 31 |
H8C | 7612.92 | 6842.8 | 2851.24 | 31 |
H10A | 3590.41 | 7507.84 | 778.36 | 30 |
H10B | 2551.21 | 7693.19 | 194.68 | 30 |
H10C | 2251.95 | 7047.47 | 661.46 | 30 |
H4A | -248.53 | 5240.71 | 2724.6 | 42 |
H4B | 508.68 | 4529.21 | 2919.14 | 42 |
H4C | 1152.75 | 5041.16 | 2397.52 | 42 |
H28A | -1258.05 | 8092.05 | 2810.2 | 22 |
H28B | -787.51 | 8773.03 | 3213.67 | 22 |
H11A | 2076.96 | 9316.88 | 1451.17 | 33 |
H11B | 2568.7 | 9159.06 | 733.13 | 33 |
H11C | 3492.97 | 8930.44 | 1346.1 | 33 |
H14A | 4144.25 | 9046.4 | 4742.42 | 38 |
H14B | 4591.8 | 9756.5 | 4400.32 | 38 |
H14C | 5567.67 | 9089.44 | 4389.83 | 38 |
H7A | 6283.12 | 8153.22 | 2265.95 | 35 |
H7B | 5610.67 | 8129.51 | 1551.9 | 35 |
H7C | 7225.62 | 8103.14 | 1648.35 | 35 |
H19A | 857.14 | 5999.89 | 238.02 | 27 |
H19B | -322.78 | 5459.91 | 430.31 | 27 |
H17A | 2981.15 | 5211.08 | 1534.65 | 26 |
H17B | 3274.64 | 5767.33 | 971.33 | 26 |
H18A | 1203.26 | 4724.43 | 968.74 | 29 |
H18B | 2089.45 | 4973.24 | 364.28 | 29 |
H21A | 7305.7 | 6183.61 | 3812.04 | 27 |
H21B | 6251.31 | 5573.74 | 3614.85 | 27 |
H12A | -508.72 | 7797.25 | 741.42 | 30 |
H12B | 69.36 | 8453.13 | 356.04 | 30 |
H12C | -589.35 | 8562.35 | 1049.04 | 30 |
H20A | 85.2 | 6542.48 | 1143.94 | 21 |
H20B | -290.12 | 5815.19 | 1485.69 | 21 |
H23A | 5729.7 | 6172.31 | 5427.36 | 35 |
H23B | 6868.48 | 6637.05 | 5082.14 | 35 |
H6A | 7530.11 | 6840.77 | 895.02 | 40 |
H6B | 5937.03 | 6812.56 | 727.43 | 40 |
H6C | 6690.34 | 6143.47 | 1030.3 | 40 |
H27A | -2792.24 | 8589.94 | 3706.22 | 31 |
H27B | -2756.96 | 7760.65 | 3572.8 | 31 |
H2A | 3806.49 | 5079.54 | 3208.03 | 40 |
H2B | 3077.21 | 4517.87 | 3654.83 | 40 |
H2C | 3729.37 | 5206.33 | 3972.6 | 40 |
H22A | 7455.65 | 5530.28 | 4733.81 | 27 |
H22B | 5892.03 | 5284.56 | 4670.38 | 27 |
H15A | 5578.15 | 9260.74 | 2896.1 | 36 |
H15B | 4604.97 | 9919.24 | 2990.88 | 36 |
H15C | 4160.86 | 9307.09 | 2502.16 | 36 |
H16A | 1551.12 | 9256.47 | 3194.07 | 41 |
H16B | 2065.52 | 9822.95 | 3714.79 | 41 |
H16C | 1501.1 | 9085.41 | 3952.04 | 41 |
H26A | -1236.84 | 8507.96 | 4560.47 | 30 |
H26B | -2075.09 | 7792.54 | 4651.68 | 30 |
H25A | 498.2 | 7724.74 | 4488.25 | 30 |
H25B | -467.99 | 7137.04 | 4164.17 | 30 |
H3A | 1096.9 | 5567.48 | 4588.79 | 42 |
H3B | 532.44 | 4843.58 | 4304.18 | 42 |
H3C | -288.41 | 5551.16 | 4166.97 | 42 |
H24A | 4107.04 | 6455.93 | 4677.75 | 34 |
H24B | 5005.04 | 7153.62 | 4627.87 | 34 |
H13A | 3366(17) | 7801(9) | 3849(8) | 31(4) |
H1A | 1995(18) | 6623(9) | 3710(9) | 39(5) |
H9A | 1220(18) | 8192(10) | 2259(9) | 39(5) |
H13B | 4709(18) | 7863(9) | 3514(8) | 34(5) |
H9B | 852(17) | 7440(9) | 2025(8) | 29(4) |
H5A | 4125(18) | 6648(10) | 1782(9) | 41(5) |
H1B | 891(18) | 6584(9) | 3175(9) | 40(5) |
H5B | 4775(19) | 6231(10) | 2316(9) | 44(5) |
Experimental
Single crystals of C28H68Li4O3Si4 [mo_B1032_0m] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 100.01 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_B1032_0m]
Crystal Data for C28H68Li4O3Si4 (M =592.94 g/mol): monoclinic, space group P21/c (no. 14), a = 9.8606(18) Å, b = 19.160(2) Å, c = 20.638(3) Å, β = 91.536(6)°, V = 3897.8(10) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 0.176 mm-1, Dcalc = 1.010 g/cm3, 38837 reflections measured (4.484° ≤ 2Θ ≤ 54°), 8504 unique (Rint = 0.0304, Rsigma = 0.0268) which were used in all calculations. The final R1 was 0.0315 (I > 2σ(I)) and wR2 was 0.0814 (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:
C28(H28A,H28B), C19(H19A,H19B), C17(H17A,H17B), C18(H18A,H18B), C21(H21A,
H21B), C20(H20A,H20B), C23(H23A,H23B), C27(H27A,H27B), C22(H22A,H22B),
C26(H26A,H26B), C25(H25A,H25B), C24(H24A,H24B)
2.b Idealised Me refined as rotating group:
C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C),
C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C6(H6A,H6B,H6C),
C2(H2A,H2B,H2C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C)
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.