Identification code | mo_B0378_0m |
Empirical formula | C14H31Li2NO3 |
Formula weight | 275.28 |
Temperature/K | 99.99 |
Crystal system | triclinic |
Space group | P-1 |
a/Å | 9.9122(8) |
b/Å | 13.2804(10) |
c/Å | 14.5570(12) |
α/° | 81.866(3) |
β/° | 88.357(3) |
γ/° | 68.748(3) |
Volume/Å3 | 1767.4(2) |
Z | 4 |
ρcalcg/cm3 | 1.035 |
μ/mm‑1 | 0.068 |
F(000) | 608.0 |
Crystal size/mm3 | 1.32 × 0.96 × 0.27 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.41 to 58 |
Index ranges | -13 ≤ h ≤ 13, -18 ≤ k ≤ 18, -19 ≤ l ≤ 19 |
Reflections collected | 86037 |
Independent reflections | 9360 [Rint = 0.0680, Rsigma = 0.0339] |
Data/restraints/parameters | 9360/0/455 |
Goodness-of-fit on F2 | 1.022 |
Final R indexes [I>=2σ (I)] | R1 = 0.0461, wR2 = 0.1228 |
Final R indexes [all data] | R1 = 0.0538, wR2 = 0.1291 |
Largest diff. peak/hole / e Å-3 | 0.50/-0.24 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
O6 | 3987.2(7) | 8065.8(5) | 6898.2(5) | 16.55(15) |
O3 | 6607.1(8) | 8025.3(6) | 7767.8(5) | 17.35(15) |
O4 | 3846.3(8) | 5703.4(6) | 6576.6(5) | 20.27(16) |
O1 | 8200.4(8) | 5746.3(6) | 9139.5(5) | 20.33(16) |
O5 | 1280.1(9) | 8273.8(7) | 3157.7(6) | 30.7(2) |
O2 | 8986.6(11) | 7139.8(7) | 11308.8(6) | 31.5(2) |
N1 | 8722.6(10) | 7718.6(7) | 9191.0(6) | 18.55(18) |
N2 | 1966.6(9) | 7728.1(7) | 5687.0(6) | 16.70(17) |
C18 | 2755.3(11) | 8956.5(8) | 6540.5(7) | 17.20(19) |
C25 | 6643.3(12) | 6643.0(9) | 5566.9(7) | 21.2(2) |
C7 | 8730.9(11) | 8299.7(9) | 8240.5(7) | 20.2(2) |
C21 | 4617.6(11) | 7462.2(8) | 9565.6(7) | 17.86(19) |
C2 | 9524.0(12) | 5831.7(9) | 8788.5(8) | 21.6(2) |
C8 | 7204.6(11) | 8837.3(8) | 7787.3(7) | 18.3(2) |
C12 | 2358.0(12) | 6045.4(9) | 6813.2(8) | 23.4(2) |
C17 | 1550.3(11) | 8530.5(8) | 6357.3(7) | 18.5(2) |
C11 | 1479.9(11) | 6809.2(9) | 5993.9(8) | 22.2(2) |
C1 | 9874.2(11) | 6617.5(9) | 9310.2(7) | 21.5(2) |
C4 | 8928.1(12) | 8361.0(9) | 9894.5(7) | 23.3(2) |
C14 | 1297.1(11) | 8268.1(9) | 4767.3(7) | 22.0(2) |
C13 | 4743.4(15) | 4836.2(10) | 7233.4(9) | 31.8(3) |
C19 | 3138.9(13) | 9557.3(9) | 5652.4(8) | 25.1(2) |
C24 | 3500.9(13) | 6987.1(10) | 9325.0(8) | 27.6(2) |
C15 | 2077.1(13) | 7691.2(10) | 3974.7(7) | 27.2(2) |
C20 | 2182.5(13) | 9760.5(9) | 7245.7(8) | 27.4(2) |
C23 | 3772.6(14) | 8587.1(10) | 9837.9(8) | 27.9(2) |
C22 | 5412.7(14) | 6740.0(11) | 10446.9(8) | 28.3(2) |
C9 | 7366.6(13) | 9362.3(10) | 6802.4(7) | 26.0(2) |
C5 | 8260.2(13) | 8198.9(9) | 10823.6(8) | 26.0(2) |
C10 | 6224.3(13) | 9734.1(9) | 8322.9(8) | 24.4(2) |
C3 | 7699.7(13) | 5084.3(9) | 8648.2(8) | 26.9(2) |
C28 | 6219.8(14) | 5985.7(12) | 4930.3(9) | 32.6(3) |
C16 | 1890.0(16) | 7823.6(12) | 2352.4(9) | 38.7(3) |
C6 | 8480.3(19) | 7031.1(12) | 12229.6(9) | 41.6(3) |
C27 | 8099.5(14) | 5893.3(14) | 6009.4(9) | 41.3(3) |
C26 | 6915(2) | 7565.3(13) | 4935.4(12) | 51.6(5) |
Li1 | 6834.9(19) | 7279.0(15) | 9045.2(12) | 20.1(3) |
Li2 | 4695.0(19) | 8071.6(15) | 8084.6(12) | 19.7(3) |
Li3 | 5996.7(19) | 7741.2(15) | 6641.2(12) | 20.1(3) |
Li4 | 4352.2(19) | 6978.4(14) | 6087.7(12) | 19.6(3) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
O6 | 16.7(3) | 15.4(3) | 13.9(3) | -2.5(2) | -1.7(2) | -1.2(3) |
O3 | 20.7(3) | 20.8(3) | 14.0(3) | -3.2(3) | 2.0(3) | -11.4(3) |
O4 | 23.3(4) | 16.4(3) | 18.9(3) | 1.5(3) | -1.9(3) | -5.9(3) |
O1 | 20.8(4) | 20.7(3) | 21.3(4) | -6.0(3) | 0.1(3) | -8.4(3) |
O5 | 30.1(4) | 34.5(5) | 17.8(4) | -4.4(3) | -6.3(3) | 0.7(4) |
O2 | 46.1(5) | 25.6(4) | 19.6(4) | -5.4(3) | 3.0(4) | -8.5(4) |
N1 | 21.3(4) | 20.7(4) | 14.8(4) | -3.7(3) | -0.3(3) | -8.4(3) |
N2 | 17.6(4) | 16.6(4) | 14.6(4) | -1.8(3) | -1.3(3) | -4.7(3) |
C18 | 18.3(4) | 14.2(4) | 16.1(4) | -1.8(3) | -1.9(3) | -2.3(4) |
C25 | 25.4(5) | 22.1(5) | 19.3(5) | -9.4(4) | 6.6(4) | -10.4(4) |
C7 | 21.0(5) | 25.4(5) | 17.9(5) | -3.0(4) | 3.1(4) | -12.9(4) |
C21 | 20.8(5) | 20.6(4) | 12.9(4) | -2.0(3) | 1.9(3) | -8.6(4) |
C2 | 19.6(5) | 23.6(5) | 21.2(5) | -6.9(4) | 1.4(4) | -6.3(4) |
C8 | 22.2(5) | 20.5(5) | 15.1(4) | -2.1(3) | 2.5(4) | -11.4(4) |
C12 | 28.0(5) | 22.5(5) | 21.2(5) | -1.6(4) | 6.5(4) | -11.9(4) |
C17 | 16.1(4) | 18.4(4) | 18.0(4) | -4.1(4) | 1.4(3) | -2.3(4) |
C11 | 19.7(5) | 23.4(5) | 25.8(5) | -4.2(4) | 1.3(4) | -10.4(4) |
C1 | 17.9(5) | 25.3(5) | 21.9(5) | -5.9(4) | -1.3(4) | -7.2(4) |
C4 | 28.6(5) | 23.6(5) | 21.2(5) | -6.2(4) | -2.1(4) | -12.3(4) |
C14 | 20.4(5) | 22.1(5) | 18.5(5) | -2.7(4) | -4.6(4) | -1.6(4) |
C13 | 41.8(7) | 22.3(5) | 26.8(6) | 4.3(4) | -11.4(5) | -8.4(5) |
C19 | 28.1(5) | 20.8(5) | 24.1(5) | 5.9(4) | -4.0(4) | -9.1(4) |
C24 | 29.3(6) | 34.5(6) | 24.8(5) | -2.9(5) | 2.2(4) | -18.8(5) |
C15 | 29.2(6) | 26.7(5) | 17.4(5) | -2.3(4) | -3.3(4) | -0.1(4) |
C20 | 27.6(5) | 20.4(5) | 28.1(6) | -11.0(4) | -4.8(4) | 1.8(4) |
C23 | 36.4(6) | 25.5(5) | 20.4(5) | -6.4(4) | 9.8(5) | -8.8(5) |
C22 | 31.0(6) | 34.0(6) | 17.2(5) | 3.3(4) | -0.5(4) | -11.0(5) |
C9 | 31.5(6) | 31.1(6) | 18.1(5) | 2.8(4) | 1.7(4) | -17.0(5) |
C5 | 32.0(6) | 24.3(5) | 20.9(5) | -8.4(4) | -0.3(4) | -7.3(4) |
C10 | 28.4(5) | 20.4(5) | 24.9(5) | -5.3(4) | 2.6(4) | -8.9(4) |
C3 | 29.6(6) | 26.0(5) | 28.4(6) | -7.6(4) | -5.6(4) | -12.2(5) |
C28 | 29.6(6) | 41.3(7) | 31.3(6) | -20.8(5) | 2.9(5) | -12.4(5) |
C16 | 44.9(8) | 45.4(7) | 19.0(5) | -8.6(5) | -1.9(5) | -6.8(6) |
C6 | 65.6(10) | 38.2(7) | 21.7(6) | -6.6(5) | 9.2(6) | -19.4(7) |
C27 | 24.6(6) | 69.2(10) | 28.8(6) | -13.4(6) | 4.2(5) | -13.3(6) |
C26 | 87.2(13) | 36.9(7) | 41.6(8) | -17.5(6) | 38.7(9) | -33.6(8) |
Li1 | 20.4(8) | 21.7(8) | 17.4(8) | -1.4(6) | 0.5(6) | -7.3(7) |
Li2 | 20.7(8) | 24.3(8) | 14.1(7) | -4.0(6) | 1.9(6) | -7.7(7) |
Li3 | 22.7(8) | 22.4(8) | 15.9(8) | -5.6(6) | 3.4(6) | -8.1(7) |
Li4 | 21.8(8) | 18.7(8) | 18.3(8) | -4.1(6) | 1.0(6) | -6.9(7) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O6 | C18 | 1.4059(11) | C18 | C17 | 1.5390(14) | |
O6 | Li2 | 1.8848(19) | C18 | C19 | 1.5337(14) | |
O6 | Li3 | 1.9167(19) | C18 | C20 | 1.5341(14) | |
O6 | Li4 | 1.9201(18) | C25 | C28 | 1.5210(15) | |
O3 | C8 | 1.4096(12) | C25 | C27 | 1.5230(18) | |
O3 | Li1 | 1.9574(19) | C25 | C26 | 1.5244(17) | |
O3 | Li2 | 1.9189(19) | C25 | Li3 | 2.2122(19) | |
O3 | Li3 | 1.8962(19) | C25 | Li4 | 2.279(2) | |
O4 | C12 | 1.4249(13) | C7 | C8 | 1.5410(15) | |
O4 | C13 | 1.4234(13) | C21 | C24 | 1.5287(15) | |
O4 | Li4 | 1.9695(19) | C21 | C23 | 1.5270(15) | |
O1 | C2 | 1.4311(13) | C21 | C22 | 1.5325(15) | |
O1 | C3 | 1.4302(12) | C21 | Li1 | 2.243(2) | |
O1 | Li1 | 1.9819(19) | C21 | Li2 | 2.202(2) | |
O5 | C15 | 1.4097(13) | C2 | C1 | 1.5127(14) | |
O5 | C16 | 1.4116(15) | C8 | C9 | 1.5338(14) | |
O2 | C5 | 1.4176(14) | C8 | C10 | 1.5332(14) | |
O2 | C6 | 1.4243(15) | C12 | C11 | 1.5120(15) | |
N1 | C7 | 1.4873(13) | C4 | C5 | 1.5111(16) | |
N1 | C1 | 1.4836(14) | C14 | C15 | 1.5118(15) | |
N1 | C4 | 1.4844(13) | Li1 | Li2 | 2.387(3) | |
N1 | Li1 | 2.176(2) | Li1 | Li3 | 3.536(2) | |
N2 | C17 | 1.4867(12) | Li2 | Li3 | 2.443(2) | |
N2 | C11 | 1.4771(13) | Li2 | Li4 | 3.504(2) | |
N2 | C14 | 1.4769(13) | Li3 | Li4 | 2.416(3) | |
N2 | Li4 | 2.265(2) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C18 | O6 | Li2 | 117.70(8) | N2 | C17 | C18 | 113.04(8) | |
C18 | O6 | Li3 | 130.50(8) | N2 | C11 | C12 | 112.86(9) | |
C18 | O6 | Li4 | 107.16(8) | N1 | C1 | C2 | 112.40(8) | |
Li2 | O6 | Li3 | 79.97(8) | N1 | C4 | C5 | 115.52(9) | |
Li2 | O6 | Li4 | 134.16(8) | N2 | C14 | C15 | 113.43(8) | |
Li3 | O6 | Li4 | 78.05(8) | O5 | C15 | C14 | 106.55(9) | |
C8 | O3 | Li1 | 104.60(8) | O2 | C5 | C4 | 111.54(9) | |
C8 | O3 | Li2 | 128.77(8) | O3 | Li1 | O1 | 111.85(9) | |
C8 | O3 | Li3 | 121.82(8) | O3 | Li1 | N1 | 87.83(7) | |
Li2 | O3 | Li1 | 76.01(8) | O3 | Li1 | C21 | 107.58(9) | |
Li3 | O3 | Li1 | 133.14(8) | O3 | Li1 | Li2 | 51.27(6) | |
Li3 | O3 | Li2 | 79.62(8) | O3 | Li1 | Li3 | 23.04(5) | |
C12 | O4 | Li4 | 110.15(8) | O1 | Li1 | N1 | 86.74(7) | |
C13 | O4 | C12 | 112.30(9) | O1 | Li1 | C21 | 114.14(9) | |
C13 | O4 | Li4 | 122.53(9) | O1 | Li1 | Li2 | 125.75(10) | |
C2 | O1 | Li1 | 104.23(8) | O1 | Li1 | Li3 | 98.70(7) | |
C3 | O1 | C2 | 112.75(8) | N1 | Li1 | C21 | 145.27(9) | |
C3 | O1 | Li1 | 113.13(8) | N1 | Li1 | Li2 | 133.22(10) | |
C15 | O5 | C16 | 112.85(9) | N1 | Li1 | Li3 | 106.32(7) | |
C5 | O2 | C6 | 111.59(10) | C21 | Li1 | Li2 | 56.70(6) | |
C7 | N1 | Li1 | 99.46(7) | C21 | Li1 | Li3 | 97.90(7) | |
C1 | N1 | C7 | 110.82(8) | Li2 | Li1 | Li3 | 43.56(6) | |
C1 | N1 | C4 | 109.88(8) | O6 | Li2 | O3 | 99.41(8) | |
C1 | N1 | Li1 | 99.90(8) | O6 | Li2 | C21 | 142.69(10) | |
C4 | N1 | C7 | 110.15(8) | O6 | Li2 | Li1 | 141.29(10) | |
C4 | N1 | Li1 | 125.69(8) | O6 | Li2 | Li3 | 50.59(6) | |
C17 | N2 | Li4 | 96.74(7) | O6 | Li2 | Li4 | 23.14(5) | |
C11 | N2 | C17 | 111.06(8) | O3 | Li2 | C21 | 110.67(9) | |
C11 | N2 | Li4 | 101.70(7) | O3 | Li2 | Li1 | 52.72(6) | |
C14 | N2 | C17 | 109.63(8) | O3 | Li2 | Li3 | 49.78(6) | |
C14 | N2 | C11 | 108.67(8) | O3 | Li2 | Li4 | 92.03(7) | |
C14 | N2 | Li4 | 128.10(8) | C21 | Li2 | Li1 | 58.36(7) | |
O6 | C18 | C17 | 108.61(8) | C21 | Li2 | Li3 | 145.78(10) | |
O6 | C18 | C19 | 109.70(8) | C21 | Li2 | Li4 | 130.87(8) | |
O6 | C18 | C20 | 110.96(8) | Li1 | Li2 | Li3 | 94.12(9) | |
C19 | C18 | C17 | 111.61(8) | Li1 | Li2 | Li4 | 120.84(8) | |
C19 | C18 | C20 | 108.73(9) | Li3 | Li2 | Li4 | 43.53(6) | |
C20 | C18 | C17 | 107.21(9) | O6 | Li3 | C25 | 109.47(9) | |
C28 | C25 | C27 | 105.88(10) | O6 | Li3 | Li1 | 90.40(7) | |
C28 | C25 | C26 | 106.15(11) | O6 | Li3 | Li2 | 49.44(6) | |
C28 | C25 | Li3 | 148.16(9) | O6 | Li3 | Li4 | 51.04(6) | |
C28 | C25 | Li4 | 83.18(8) | O3 | Li3 | O6 | 99.09(8) | |
C27 | C25 | C26 | 106.81(13) | O3 | Li3 | C25 | 143.65(10) | |
C27 | C25 | Li3 | 96.99(9) | O3 | Li3 | Li1 | 23.83(5) | |
C27 | C25 | Li4 | 130.56(9) | O3 | Li3 | Li2 | 50.60(6) | |
C26 | C25 | Li3 | 87.55(9) | O3 | Li3 | Li4 | 139.90(10) | |
C26 | C25 | Li4 | 117.20(11) | C25 | Li3 | Li1 | 131.53(8) | |
Li3 | C25 | Li4 | 65.06(7) | C25 | Li3 | Li2 | 144.57(10) | |
N1 | C7 | C8 | 112.53(8) | C25 | Li3 | Li4 | 58.81(7) | |
C24 | C21 | C22 | 105.53(9) | Li2 | Li3 | Li1 | 42.32(6) | |
C24 | C21 | Li1 | 132.96(9) | Li4 | Li3 | Li1 | 118.75(8) | |
C24 | C21 | Li2 | 89.37(8) | Li4 | Li3 | Li2 | 92.32(8) | |
C23 | C21 | C24 | 106.82(9) | O6 | Li4 | O4 | 115.47(9) | |
C23 | C21 | C22 | 106.66(9) | O6 | Li4 | N2 | 87.24(7) | |
C23 | C21 | Li1 | 113.60(9) | O6 | Li4 | C25 | 106.69(9) | |
C23 | C21 | Li2 | 94.63(8) | O6 | Li4 | Li2 | 22.70(5) | |
C22 | C21 | Li1 | 85.29(8) | O6 | Li4 | Li3 | 50.91(6) | |
C22 | C21 | Li2 | 148.68(9) | O4 | Li4 | N2 | 82.85(7) | |
Li2 | C21 | Li1 | 64.94(7) | O4 | Li4 | C25 | 117.07(9) | |
O1 | C2 | C1 | 107.65(8) | O4 | Li4 | Li2 | 103.55(7) | |
O3 | C8 | C7 | 108.60(8) | O4 | Li4 | Li3 | 132.48(10) | |
O3 | C8 | C9 | 111.11(8) | N2 | Li4 | C25 | 144.95(9) | |
O3 | C8 | C10 | 110.11(8) | N2 | Li4 | Li2 | 105.26(7) | |
C9 | C8 | C7 | 107.45(8) | N2 | Li4 | Li3 | 131.81(9) | |
C10 | C8 | C7 | 111.18(8) | C25 | Li4 | Li2 | 97.89(7) | |
C10 | C8 | C9 | 108.37(9) | C25 | Li4 | Li3 | 56.13(6) | |
O4 | C12 | C11 | 107.92(8) | Li3 | Li4 | Li2 | 44.14(6) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
O6 | C18 | C17 | N2 | -59.48(10) | Li1 | O3 | Li3 | O6 | 69.84(13) | |
O4 | C12 | C11 | N2 | -54.11(11) | Li1 | O3 | Li3 | C25 | -72.1(2) | |
O1 | C2 | C1 | N1 | -59.89(11) | Li1 | O3 | Li3 | Li2 | 59.45(12) | |
N1 | C7 | C8 | O3 | -57.30(10) | Li1 | O3 | Li3 | Li4 | 32.8(2) | |
N1 | C7 | C8 | C9 | -177.58(8) | Li1 | O1 | C2 | C1 | 52.52(10) | |
N1 | C7 | C8 | C10 | 64.00(11) | Li1 | N1 | C7 | C8 | 28.76(10) | |
N1 | C4 | C5 | O2 | 68.85(13) | Li1 | N1 | C1 | C2 | 31.60(10) | |
N2 | C14 | C15 | O5 | 177.60(9) | Li1 | N1 | C4 | C5 | 33.22(14) | |
C18 | O6 | Li2 | O3 | -120.24(9) | Li2 | O6 | C18 | C17 | -120.16(9) | |
C18 | O6 | Li2 | C21 | 95.87(17) | Li2 | O6 | C18 | C19 | 117.60(10) | |
C18 | O6 | Li2 | Li1 | -159.45(14) | Li2 | O6 | C18 | C20 | -2.56(12) | |
C18 | O6 | Li2 | Li3 | -130.69(9) | Li2 | O3 | C8 | C7 | 135.15(10) | |
C18 | O6 | Li2 | Li4 | 167.02(15) | Li2 | O3 | C8 | C9 | -106.87(11) | |
C7 | N1 | C1 | C2 | -72.58(11) | Li2 | O3 | C8 | C10 | 13.19(13) | |
C7 | N1 | C4 | C5 | 151.85(9) | Li2 | O3 | Li3 | O6 | 10.39(8) | |
C8 | O3 | Li3 | O6 | -119.07(9) | Li2 | O3 | Li3 | C25 | -131.51(17) | |
C8 | O3 | Li3 | C25 | 99.02(17) | Li2 | O3 | Li3 | Li1 | -59.45(12) | |
C8 | O3 | Li3 | Li1 | 171.09(16) | Li2 | O3 | Li3 | Li4 | -26.62(15) | |
C8 | O3 | Li3 | Li2 | -129.46(10) | Li3 | O6 | C18 | C17 | 138.91(10) | |
C8 | O3 | Li3 | Li4 | -156.08(13) | Li3 | O6 | C18 | C19 | 16.67(13) | |
C17 | N2 | C11 | C12 | -72.68(11) | Li3 | O6 | C18 | C20 | -103.49(11) | |
C17 | N2 | C14 | C15 | 157.32(9) | Li3 | O6 | Li2 | O3 | 10.45(8) | |
C11 | N2 | C17 | C18 | 138.13(9) | Li3 | O6 | Li2 | C21 | -133.43(17) | |
C11 | N2 | C14 | C15 | -81.13(11) | Li3 | O6 | Li2 | Li1 | -28.76(16) | |
C1 | N1 | C7 | C8 | 133.23(9) | Li3 | O6 | Li2 | Li4 | -62.29(12) | |
C1 | N1 | C4 | C5 | -85.79(11) | Li3 | O3 | C8 | C7 | -121.76(9) | |
C4 | N1 | C7 | C8 | -104.97(10) | Li3 | O3 | C8 | C9 | -3.78(13) | |
C4 | N1 | C1 | C2 | 165.46(9) | Li3 | O3 | C8 | C10 | 116.28(10) | |
C14 | N2 | C17 | C18 | -101.77(9) | Li4 | O6 | C18 | C17 | 50.13(10) | |
C14 | N2 | C11 | C12 | 166.65(9) | Li4 | O6 | C18 | C19 | -72.10(10) | |
C13 | O4 | C12 | C11 | -169.63(9) | Li4 | O6 | C18 | C20 | 167.73(9) | |
C19 | C18 | C17 | N2 | 61.59(11) | Li4 | O6 | Li2 | O3 | 72.74(13) | |
C20 | C18 | C17 | N2 | -179.44(8) | Li4 | O6 | Li2 | C21 | -71.1(2) | |
C3 | O1 | C2 | C1 | 175.60(8) | Li4 | O6 | Li2 | Li1 | 33.5(2) | |
C16 | O5 | C15 | C14 | 179.92(11) | Li4 | O6 | Li2 | Li3 | 62.29(12) | |
C6 | O2 | C5 | C4 | 172.58(10) | Li4 | O4 | C12 | C11 | 50.04(11) | |
Li1 | O3 | C8 | C7 | 51.53(10) | Li4 | N2 | C17 | C18 | 32.80(9) | |
Li1 | O3 | C8 | C9 | 169.51(9) | Li4 | N2 | C11 | C12 | 29.34(10) | |
Li1 | O3 | C8 | C10 | -70.42(10) | Li4 | N2 | C14 | C15 | 41.34(14) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H7A | 9360 | 7775 | 7847 | 24 |
H7B | 9148 | 8868 | 8272 | 24 |
H17A | 1301 | 8183 | 6952 | 22 |
H17B | 675 | 9156 | 6114 | 22 |
H11A | 1549 | 6392 | 5471 | 27 |
H11B | 450 | 7103 | 6165 | 27 |
H1A | 10007 | 6323 | 9979 | 26 |
H1B | 10798 | 6679 | 9087 | 26 |
H4A | 8513 | 9145 | 9638 | 28 |
H4B | 9980 | 8170 | 9996 | 28 |
H14A | 1282 | 9025 | 4670 | 26 |
H14B | 281 | 8306 | 4760 | 26 |
H13A | 4616 | 5063 | 7852 | 48 |
H13B | 5759 | 4653 | 7061 | 48 |
H13C | 4473 | 4195 | 7240 | 48 |
H19A | 3884 | 9838 | 5797 | 38 |
H19B | 2272 | 10166 | 5396 | 38 |
H19C | 3506 | 9051 | 5196 | 38 |
H15A | 3078 | 7688 | 3941 | 33 |
H15B | 2121 | 6927 | 4062 | 33 |
H20A | 1916 | 9389 | 7812 | 41 |
H20B | 1329 | 10375 | 6980 | 41 |
H20C | 2936 | 10031 | 7395 | 41 |
H9A | 7990 | 8799 | 6449 | 39 |
H9B | 7802 | 9912 | 6835 | 39 |
H9C | 6411 | 9711 | 6494 | 39 |
H10A | 5281 | 10090 | 8001 | 37 |
H10B | 6673 | 10275 | 8359 | 37 |
H10C | 6093 | 9410 | 8951 | 37 |
H3A | 7454 | 5432 | 8004 | 40 |
H3B | 6839 | 5003 | 8947 | 40 |
H3C | 8463 | 4364 | 8657 | 40 |
H16A | 1319 | 8275 | 1805 | 58 |
H16B | 1887 | 7081 | 2394 | 58 |
H16C | 2888 | 7802 | 2300 | 58 |
H6A | 7445 | 7152 | 12208 | 62 |
H6B | 8632 | 7571 | 12567 | 62 |
H6C | 9015 | 6296 | 12548 | 62 |
H27A | 7993 | 5245 | 6369 | 62 |
H27B | 8436 | 6282 | 6421 | 62 |
H27C | 8806 | 5671 | 5523 | 62 |
H5A | 7231(17) | 8310(12) | 10744(10) | 30(4) |
H12A | 2058(16) | 5417(12) | 6943(10) | 29(4) |
H2A | 9397(15) | 6091(11) | 8137(10) | 23(3) |
H24A | 2807(18) | 6981(13) | 9852(12) | 40(4) |
H22A | 6161(19) | 6998(14) | 10719(12) | 44(4) |
H23A | 3030(19) | 8558(14) | 10348(12) | 43(4) |
H22B | 4701(18) | 6747(13) | 10981(12) | 38(4) |
H24B | 2830(20) | 7429(15) | 8756(13) | 51(5) |
H23B | 4430(17) | 8920(13) | 10077(11) | 37(4) |
H23C | 3175(18) | 9124(14) | 9302(12) | 39(4) |
H28A | 6990(20) | 5746(14) | 4443(13) | 48(5) |
H26A | 7770(20) | 7257(17) | 4518(15) | 64(6) |
H26B | 5870(30) | 8020(20) | 4458(17) | 85(7) |
H2B | 10325(16) | 5117(12) | 8892(10) | 28(3) |
H22C | 5934(18) | 5975(14) | 10349(12) | 40(4) |
H28B | 5330(20) | 6465(15) | 4557(13) | 48(5) |
H24C | 3964(17) | 6195(13) | 9187(11) | 37(4) |
H12B | 2231(16) | 6378(12) | 7408(10) | 29(4) |
H5B | 8333(17) | 8766(13) | 11173(11) | 37(4) |
H26C | 7240(20) | 8016(18) | 5274(15) | 69(6) |
H28C | 6070(20) | 5294(17) | 5291(14) | 61(6) |
Experimental
Single crystals of C14H31Li2NO3 [mo_B0378_0m] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 99.99 K during data collection. Using Olex2 [1], the structure was solved with the XT [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0378_0m]
Crystal Data for C14H31Li2NO3 (M =275.28 g/mol): triclinic, space group P-1 (no. 2), a = 9.9122(8) Å, b = 13.2804(10) Å, c = 14.5570(12) Å, α = 81.866(3)°, β = 88.357(3)°, γ = 68.748(3)°, V = 1767.4(2) Å3, Z = 4, T = 99.99 K, μ(MoKα) = 0.068 mm-1, Dcalc = 1.035 g/cm3, 86037 reflections measured (4.41° ≤ 2Θ ≤ 58°), 9360 unique (Rint = 0.0680, Rsigma = 0.0339) which were used in all calculations. The final R1 was 0.0461 (I > 2σ(I)) and wR2 was 0.1291 (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:
C7(H7A,H7B), C17(H17A,H17B), C11(H11A,H11B), C1(H1A,H1B), C4(H4A,H4B),
C14(H14A,H14B), C15(H15A,H15B)
2.b Idealised Me refined as rotating group:
C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C9(H9A,H9B,
H9C), C10(H10A,H10B,H10C), C3(H3A,H3B,H3C), C16(H16A,H16B,H16C), C6(H6A,H6B,
H6C), C27(H27A,H27B,H27C)
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.