Identification code | mo_B0321_0m |
Empirical formula | C24H56Li4N4O4 |
Formula weight | 492.48 |
Temperature/K | 99.98 |
Crystal system | monoclinic |
Space group | P21/n |
a/Å | 18.0767(15) |
b/Å | 10.0888(9) |
c/Å | 18.548(2) |
α/° | 90 |
β/° | 108.538(4) |
γ/° | 90 |
Volume/Å3 | 3207.1(5) |
Z | 4 |
ρcalcg/cm3 | 1.020 |
μ/mm‑1 | 0.066 |
F(000) | 1088.0 |
Crystal size/mm3 | 0.41 × 0.33 × 0.32 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.686 to 56 |
Index ranges | -23 ≤ h ≤ 23, -13 ≤ k ≤ 13, -24 ≤ l ≤ 24 |
Reflections collected | 70347 |
Independent reflections | 7736 [Rint = 0.0243, Rsigma = 0.0142] |
Data/restraints/parameters | 7736/0/342 |
Goodness-of-fit on F2 | 1.027 |
Final R indexes [I>=2σ (I)] | R1 = 0.0348, wR2 = 0.0916 |
Final R indexes [all data] | R1 = 0.0388, wR2 = 0.0944 |
Largest diff. peak/hole / e Å-3 | 0.34/-0.17 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
O4 | 2052.2(3) | 2246.6(6) | 5371.1(3) | 14.31(13) |
O2 | 1723.9(3) | 4524.8(6) | 4362.7(3) | 13.38(12) |
O1 | 3093.0(3) | 4524.9(6) | 5751.2(3) | 13.92(12) |
O3 | 3074.9(3) | 2908.6(6) | 4463.7(3) | 13.21(12) |
N4 | 1208.4(4) | 1102.3(7) | 3906.8(4) | 15.83(15) |
N3 | 4091.9(4) | 1383.7(8) | 5704.7(4) | 19.46(16) |
N1 | 1847.0(4) | 5420.9(8) | 6287.3(4) | 19.65(16) |
N2 | 2745.3(4) | 6421.8(7) | 4009.2(4) | 17.56(15) |
C19 | 1462.3(5) | 1340.2(9) | 5335.4(5) | 17.61(17) |
C21 | 1686.7(7) | 448.0(12) | 6041.7(6) | 34.0(3) |
C22 | 1348.4(5) | 412.9(8) | 4642.7(5) | 17.86(17) |
C16 | 4071.4(5) | 1256.5(9) | 4901.5(5) | 19.62(18) |
C13 | 3788.2(5) | 2498.7(9) | 4404.9(5) | 15.67(16) |
C9 | 1512.0(5) | 4406.0(9) | 3018.4(5) | 21.25(18) |
C2 | 3413.0(5) | 3901.5(10) | 7059.0(5) | 21.16(18) |
C4 | 2638.9(5) | 6009.1(9) | 6531.5(5) | 19.68(18) |
C1 | 3288.4(5) | 5044.7(9) | 6484.3(5) | 15.79(16) |
C10 | 1883.9(5) | 6567.1(8) | 3765.5(5) | 18.48(17) |
C15 | 4380.5(5) | 3642.2(10) | 4628.3(6) | 25.6(2) |
C18 | 4856.4(6) | 1841.5(12) | 6195.8(6) | 31.0(2) |
C8 | 572.8(5) | 5583.2(10) | 3530.9(6) | 26.9(2) |
C7 | 1438.2(5) | 5239.2(8) | 3689.0(5) | 15.63(16) |
C20 | 710.4(6) | 2092.9(12) | 5305.7(6) | 31.6(2) |
C24 | 376.1(5) | 1330.8(12) | 3523.3(6) | 30.3(2) |
C12 | 3035.6(6) | 6424.6(11) | 3354.2(6) | 28.0(2) |
C3 | 4046.9(5) | 5856.1(10) | 6672.1(5) | 25.3(2) |
C5 | 1639.0(6) | 4907.0(12) | 6938.9(6) | 29.1(2) |
C11 | 3123.3(6) | 7502.6(10) | 4521.3(6) | 28.2(2) |
C14 | 3699.9(6) | 2097.5(11) | 3581.9(5) | 28.1(2) |
C6 | 1261.0(6) | 6410.8(11) | 5898.9(6) | 31.6(2) |
C17 | 3927.3(7) | 96.0(11) | 5988.9(7) | 33.3(2) |
C23 | 1506.8(7) | 316.0(11) | 3395.7(6) | 33.5(2) |
Li2 | 2872.7(8) | 4704.9(14) | 4694.9(8) | 15.4(3) |
Li3 | 3115.0(8) | 2658.9(14) | 5534.5(8) | 15.9(3) |
Li1 | 1954.0(8) | 4151.7(15) | 5411.8(8) | 16.6(3) |
Li4 | 1995.2(8) | 2693.7(14) | 4320.4(8) | 15.2(3) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
O4 | 12.4(3) | 16.5(3) | 13.4(3) | 1.9(2) | 3.2(2) | -3.0(2) |
O2 | 11.8(3) | 15.3(3) | 12.2(3) | 3.5(2) | 2.6(2) | 1.4(2) |
O1 | 13.2(3) | 17.2(3) | 10.5(3) | -3.6(2) | 2.6(2) | 0.0(2) |
O3 | 9.5(3) | 16.5(3) | 13.9(3) | -2.2(2) | 4.2(2) | 1.5(2) |
N4 | 14.9(3) | 16.7(3) | 14.1(3) | 0.5(3) | 2.0(3) | -2.0(3) |
N3 | 17.1(3) | 20.2(4) | 18.0(3) | -0.7(3) | 1.1(3) | 5.1(3) |
N1 | 16.3(3) | 25.6(4) | 17.4(3) | -1.9(3) | 5.9(3) | 6.2(3) |
N2 | 16.5(3) | 17.2(3) | 17.7(3) | 1.4(3) | 3.7(3) | -4.3(3) |
C19 | 16.9(4) | 21.2(4) | 15.0(4) | 2.5(3) | 5.3(3) | -5.4(3) |
C21 | 45.1(6) | 35.3(6) | 18.9(5) | 9.5(4) | 6.1(4) | -16.4(5) |
C22 | 18.9(4) | 15.3(4) | 17.3(4) | 3.3(3) | 2.7(3) | -3.7(3) |
C16 | 17.7(4) | 19.1(4) | 20.5(4) | -5.3(3) | 3.8(3) | 5.4(3) |
C13 | 11.6(3) | 20.0(4) | 15.9(4) | -3.9(3) | 5.2(3) | 1.4(3) |
C9 | 25.6(4) | 22.3(4) | 13.0(4) | 1.8(3) | 2.1(3) | -6.5(3) |
C2 | 21.6(4) | 27.0(5) | 13.0(4) | -0.3(3) | 2.8(3) | 5.8(3) |
C4 | 20.8(4) | 20.2(4) | 17.7(4) | -6.1(3) | 5.5(3) | 2.3(3) |
C1 | 14.3(4) | 19.5(4) | 12.3(4) | -4.3(3) | 2.5(3) | 0.4(3) |
C10 | 17.5(4) | 15.1(4) | 20.5(4) | 4.3(3) | 2.7(3) | 1.0(3) |
C15 | 14.0(4) | 27.9(5) | 34.4(5) | 0.9(4) | 7.0(4) | -3.6(3) |
C18 | 17.7(4) | 45.4(6) | 22.7(5) | -5.3(4) | -3.8(4) | 6.9(4) |
C8 | 13.8(4) | 29.7(5) | 33.3(5) | 11.8(4) | 1.8(4) | 4.0(4) |
C7 | 12.3(4) | 17.0(4) | 15.2(4) | 4.6(3) | 1.1(3) | -0.1(3) |
C20 | 18.9(4) | 42.9(6) | 37.3(6) | -10.7(5) | 15.0(4) | -6.5(4) |
C24 | 16.3(4) | 41.9(6) | 25.7(5) | 9.2(4) | -3.3(4) | -5.6(4) |
C12 | 24.4(5) | 37.6(6) | 23.4(5) | 6.5(4) | 9.6(4) | -7.5(4) |
C3 | 19.7(4) | 29.9(5) | 23.8(4) | -10.5(4) | 3.3(3) | -6.7(4) |
C5 | 23.4(5) | 44.9(6) | 22.7(5) | -1.6(4) | 12.5(4) | 3.4(4) |
C11 | 25.6(5) | 19.6(4) | 32.2(5) | -1.7(4) | -0.9(4) | -5.7(4) |
C14 | 25.2(5) | 41.8(6) | 19.3(4) | -6.4(4) | 10.0(4) | 8.1(4) |
C6 | 25.5(5) | 35.1(6) | 32.1(5) | -0.5(4) | 6.1(4) | 15.1(4) |
C17 | 43.4(6) | 24.3(5) | 34.3(6) | 6.8(4) | 15.2(5) | 8.8(4) |
C23 | 52.0(7) | 27.0(5) | 25.5(5) | -2.4(4) | 17.7(5) | 5.0(5) |
Li2 | 14.4(6) | 16.5(7) | 15.4(6) | -0.1(5) | 4.8(5) | -0.1(5) |
Li3 | 13.9(6) | 17.9(7) | 14.5(6) | -0.4(5) | 2.5(5) | 1.5(5) |
Li1 | 14.8(6) | 19.9(7) | 15.5(6) | -0.8(5) | 5.6(5) | 1.1(5) |
Li4 | 13.5(6) | 16.5(7) | 14.4(6) | -0.3(5) | 3.0(5) | -1.5(5) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O4 | C19 | 1.3902(10) | N1 | C5 | 1.4697(12) | |
O4 | Li3 | 1.8936(15) | N1 | C6 | 1.4674(12) | |
O4 | Li1 | 1.9339(16) | N1 | Li1 | 2.1246(16) | |
O4 | Li4 | 1.9708(15) | N2 | C10 | 1.4843(11) | |
O2 | C7 | 1.3917(10) | N2 | C12 | 1.4686(12) | |
O2 | Li2 | 1.9777(15) | N2 | C11 | 1.4647(12) | |
O2 | Li1 | 1.8938(15) | N2 | Li2 | 2.1176(16) | |
O2 | Li4 | 1.9194(16) | C19 | C21 | 1.5340(12) | |
O1 | C1 | 1.3940(9) | C19 | C22 | 1.5493(12) | |
O1 | Li2 | 1.8799(15) | C19 | C20 | 1.5424(13) | |
O1 | Li3 | 1.9281(16) | C16 | C13 | 1.5431(12) | |
O1 | Li1 | 1.9883(15) | C13 | C15 | 1.5385(12) | |
O3 | C13 | 1.3909(9) | C13 | C14 | 1.5377(12) | |
O3 | Li2 | 1.9239(15) | C9 | C7 | 1.5418(12) | |
O3 | Li3 | 1.9802(15) | C2 | C1 | 1.5377(12) | |
O3 | Li4 | 1.8966(15) | C4 | C1 | 1.5485(12) | |
N4 | C22 | 1.4802(11) | C1 | C3 | 1.5388(12) | |
N4 | C24 | 1.4637(11) | C10 | C7 | 1.5464(12) | |
N4 | C23 | 1.4644(12) | C8 | C7 | 1.5369(12) | |
N4 | Li4 | 2.1202(16) | Li2 | Li3 | 2.538(2) | |
N3 | C16 | 1.4839(11) | Li2 | Li1 | 2.498(2) | |
N3 | C18 | 1.4671(12) | Li2 | Li4 | 2.533(2) | |
N3 | C17 | 1.4676(13) | Li3 | Li1 | 2.534(2) | |
N3 | Li3 | 2.1258(16) | Li3 | Li4 | 2.504(2) | |
N1 | C4 | 1.4813(12) | Li1 | Li4 | 2.522(2) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C19 | O4 | Li3 | 151.16(7) | O1 | Li2 | O2 | 99.75(7) | |
C19 | O4 | Li1 | 125.24(7) | O1 | Li2 | O3 | 98.57(7) | |
C19 | O4 | Li4 | 107.78(6) | O1 | Li2 | N2 | 130.65(8) | |
Li3 | O4 | Li1 | 82.90(6) | O1 | Li2 | Li3 | 49.01(5) | |
Li3 | O4 | Li4 | 80.76(6) | O1 | Li2 | Li1 | 51.70(5) | |
Li1 | O4 | Li4 | 80.48(6) | O1 | Li2 | Li4 | 96.61(7) | |
C7 | O2 | Li2 | 106.57(6) | O3 | Li2 | O2 | 95.69(7) | |
C7 | O2 | Li1 | 157.37(7) | O3 | Li2 | N2 | 128.96(8) | |
C7 | O2 | Li4 | 119.24(7) | O3 | Li2 | Li3 | 50.41(5) | |
Li1 | O2 | Li2 | 80.34(6) | O3 | Li2 | Li1 | 96.53(7) | |
Li1 | O2 | Li4 | 82.83(6) | O3 | Li2 | Li4 | 48.02(5) | |
Li4 | O2 | Li2 | 81.05(6) | N2 | Li2 | Li3 | 176.49(8) | |
C1 | O1 | Li2 | 152.16(7) | N2 | Li2 | Li1 | 122.59(7) | |
C1 | O1 | Li3 | 123.71(7) | N2 | Li2 | Li4 | 123.47(7) | |
C1 | O1 | Li1 | 107.20(6) | Li1 | Li2 | Li3 | 60.40(6) | |
Li2 | O1 | Li3 | 83.60(6) | Li1 | Li2 | Li4 | 60.18(6) | |
Li2 | O1 | Li1 | 80.40(6) | Li4 | Li2 | Li3 | 59.18(6) | |
Li3 | O1 | Li1 | 80.62(6) | O4 | Li3 | O1 | 99.25(7) | |
C13 | O3 | Li2 | 122.96(6) | O4 | Li3 | O3 | 98.96(7) | |
C13 | O3 | Li3 | 107.55(6) | O4 | Li3 | N3 | 130.05(8) | |
C13 | O3 | Li4 | 153.29(7) | O4 | Li3 | Li2 | 96.43(7) | |
Li2 | O3 | Li3 | 81.10(6) | O4 | Li3 | Li1 | 49.23(5) | |
Li4 | O3 | Li2 | 83.04(6) | O4 | Li3 | Li4 | 50.97(5) | |
Li4 | O3 | Li3 | 80.44(6) | O1 | Li3 | O3 | 95.07(7) | |
C22 | N4 | Li4 | 97.11(6) | O1 | Li3 | N3 | 129.14(8) | |
C24 | N4 | C22 | 111.73(7) | O1 | Li3 | Li2 | 47.39(5) | |
C24 | N4 | C23 | 107.70(8) | O1 | Li3 | Li1 | 50.73(5) | |
C24 | N4 | Li4 | 121.62(7) | O1 | Li3 | Li4 | 96.28(7) | |
C23 | N4 | C22 | 110.62(7) | O3 | Li3 | N3 | 89.41(6) | |
C23 | N4 | Li4 | 107.55(7) | O3 | Li3 | Li2 | 48.48(5) | |
C16 | N3 | Li3 | 98.56(6) | O3 | Li3 | Li1 | 93.97(6) | |
C18 | N3 | C16 | 111.62(7) | O3 | Li3 | Li4 | 48.32(5) | |
C18 | N3 | C17 | 108.31(8) | N3 | Li3 | Li2 | 123.81(7) | |
C18 | N3 | Li3 | 118.40(7) | N3 | Li3 | Li1 | 176.62(8) | |
C17 | N3 | C16 | 109.92(8) | N3 | Li3 | Li4 | 122.54(7) | |
C17 | N3 | Li3 | 109.60(7) | Li1 | Li3 | Li2 | 59.01(6) | |
C4 | N1 | Li1 | 99.28(6) | Li4 | Li3 | Li2 | 60.30(6) | |
C5 | N1 | C4 | 111.41(7) | Li4 | Li3 | Li1 | 60.08(6) | |
C5 | N1 | Li1 | 121.68(8) | O4 | Li1 | O1 | 95.85(7) | |
C6 | N1 | C4 | 110.74(8) | O4 | Li1 | N1 | 131.35(8) | |
C6 | N1 | C5 | 108.07(8) | O4 | Li1 | Li2 | 96.69(7) | |
C6 | N1 | Li1 | 105.19(7) | O4 | Li1 | Li3 | 47.87(5) | |
C10 | N2 | Li2 | 99.61(6) | O4 | Li1 | Li4 | 50.40(5) | |
C12 | N2 | C10 | 111.36(7) | O2 | Li1 | O4 | 98.65(7) | |
C12 | N2 | Li2 | 119.94(7) | O2 | Li1 | O1 | 98.91(7) | |
C11 | N2 | C10 | 110.60(7) | O2 | Li1 | N1 | 128.45(8) | |
C11 | N2 | C12 | 108.62(8) | O2 | Li1 | Li2 | 51.30(5) | |
C11 | N2 | Li2 | 106.28(7) | O2 | Li1 | Li3 | 96.64(7) | |
O4 | C19 | C21 | 110.78(7) | O2 | Li1 | Li4 | 49.02(5) | |
O4 | C19 | C22 | 109.53(7) | O1 | Li1 | N1 | 88.89(6) | |
O4 | C19 | C20 | 109.37(8) | O1 | Li1 | Li2 | 47.90(5) | |
C21 | C19 | C22 | 106.45(8) | O1 | Li1 | Li3 | 48.65(5) | |
C21 | C19 | C20 | 108.07(8) | O1 | Li1 | Li4 | 94.17(6) | |
C20 | C19 | C22 | 112.61(7) | N1 | Li1 | Li2 | 120.64(8) | |
N4 | C22 | C19 | 114.81(7) | N1 | Li1 | Li3 | 124.31(7) | |
N3 | C16 | C13 | 115.25(7) | N1 | Li1 | Li4 | 176.31(8) | |
O3 | C13 | C16 | 109.55(7) | Li2 | Li1 | Li3 | 60.59(6) | |
O3 | C13 | C15 | 109.82(7) | Li2 | Li1 | Li4 | 60.59(6) | |
O3 | C13 | C14 | 110.48(7) | Li4 | Li1 | Li3 | 59.37(6) | |
C15 | C13 | C16 | 112.20(7) | O4 | Li4 | N4 | 90.15(6) | |
C14 | C13 | C16 | 106.78(7) | O4 | Li4 | Li2 | 94.64(6) | |
C14 | C13 | C15 | 107.97(8) | O4 | Li4 | Li3 | 48.28(5) | |
N1 | C4 | C1 | 114.04(7) | O4 | Li4 | Li1 | 49.12(5) | |
O1 | C1 | C2 | 109.26(7) | O2 | Li4 | O4 | 96.52(7) | |
O1 | C1 | C4 | 109.27(6) | O2 | Li4 | N4 | 126.36(7) | |
O1 | C1 | C3 | 110.61(7) | O2 | Li4 | Li2 | 50.48(5) | |
C2 | C1 | C4 | 112.25(7) | O2 | Li4 | Li3 | 96.94(7) | |
C2 | C1 | C3 | 108.57(7) | O2 | Li4 | Li1 | 48.15(5) | |
C3 | C1 | C4 | 106.86(7) | O3 | Li4 | O4 | 99.18(7) | |
N2 | C10 | C7 | 114.07(7) | O3 | Li4 | O2 | 98.58(7) | |
O2 | C7 | C9 | 109.84(7) | O3 | Li4 | N4 | 132.79(8) | |
O2 | C7 | C10 | 109.42(7) | O3 | Li4 | Li2 | 48.94(5) | |
O2 | C7 | C8 | 110.66(7) | O3 | Li4 | Li3 | 51.24(5) | |
C9 | C7 | C10 | 111.72(7) | O3 | Li4 | Li1 | 96.46(7) | |
C8 | C7 | C9 | 108.25(7) | N4 | Li4 | Li2 | 174.53(8) | |
C8 | C7 | C10 | 106.91(7) | N4 | Li4 | Li3 | 124.91(7) | |
O2 | Li2 | N2 | 89.15(6) | N4 | Li4 | Li1 | 122.98(7) | |
O2 | Li2 | Li3 | 94.34(6) | Li3 | Li4 | Li2 | 60.52(6) | |
O2 | Li2 | Li1 | 48.36(5) | Li3 | Li4 | Li1 | 60.54(6) | |
O2 | Li2 | Li4 | 48.47(5) | Li1 | Li4 | Li2 | 59.23(6) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
O4 | C19 | C22 | N4 | -54.09(9) | Li2 | O3 | Li4 | Li1 | -38.62(7) | |
N3 | C16 | C13 | O3 | -52.46(9) | Li2 | N2 | C10 | C7 | -31.50(9) | |
N3 | C16 | C13 | C15 | 69.77(9) | Li3 | O4 | C19 | C21 | 48.67(17) | |
N3 | C16 | C13 | C14 | -172.13(7) | Li3 | O4 | C19 | C22 | -68.46(15) | |
N1 | C4 | C1 | O1 | 54.23(10) | Li3 | O4 | C19 | C20 | 167.68(12) | |
N1 | C4 | C1 | C2 | -67.14(9) | Li3 | O1 | C1 | C2 | -7.18(10) | |
N1 | C4 | C1 | C3 | 173.94(7) | Li3 | O1 | C1 | C4 | -130.35(8) | |
N2 | C10 | C7 | O2 | 53.35(9) | Li3 | O1 | C1 | C3 | 112.29(9) | |
N2 | C10 | C7 | C9 | -68.51(9) | Li3 | O1 | Li2 | O2 | 87.27(7) | |
N2 | C10 | C7 | C8 | 173.23(7) | Li3 | O1 | Li2 | O3 | -10.06(6) | |
C19 | O4 | Li3 | O1 | -159.16(11) | Li3 | O1 | Li2 | N2 | -175.39(10) | |
C19 | O4 | Li3 | O3 | 104.17(13) | Li3 | O1 | Li2 | Li1 | 81.52(6) | |
C19 | O4 | Li3 | N3 | 7.3(2) | Li3 | O1 | Li2 | Li4 | 38.37(6) | |
C19 | O4 | Li3 | Li2 | 153.06(12) | Li3 | O3 | C13 | C16 | 38.60(8) | |
C19 | O4 | Li3 | Li1 | -168.32(15) | Li3 | O3 | C13 | C15 | -85.05(8) | |
C19 | O4 | Li3 | Li4 | 110.23(14) | Li3 | O3 | C13 | C14 | 155.96(8) | |
C21 | C19 | C22 | N4 | -173.91(7) | Li3 | O3 | Li4 | O4 | -6.06(6) | |
C13 | O3 | Li4 | O4 | 104.16(14) | Li3 | O3 | Li4 | O2 | 92.03(7) | |
C13 | O3 | Li4 | O2 | -157.74(12) | Li3 | O3 | Li4 | N4 | -104.88(11) | |
C13 | O3 | Li4 | N4 | 5.3(2) | Li3 | O3 | Li4 | Li2 | 82.10(6) | |
C13 | O3 | Li4 | Li2 | -167.68(16) | Li3 | O3 | Li4 | Li1 | 43.48(7) | |
C13 | O3 | Li4 | Li3 | 110.23(15) | Li3 | N3 | C16 | C13 | 33.48(9) | |
C13 | O3 | Li4 | Li1 | 153.71(13) | Li1 | O4 | C19 | C21 | -117.09(9) | |
C1 | O1 | Li2 | O2 | -103.05(14) | Li1 | O4 | C19 | C22 | 125.78(8) | |
C1 | O1 | Li2 | O3 | 159.62(11) | Li1 | O4 | C19 | C20 | 1.92(11) | |
C1 | O1 | Li2 | N2 | -5.7(2) | Li1 | O4 | Li3 | O1 | 9.16(7) | |
C1 | O1 | Li2 | Li3 | 169.68(15) | Li1 | O4 | Li3 | O3 | -87.51(7) | |
C1 | O1 | Li2 | Li1 | -108.80(14) | Li1 | O4 | Li3 | N3 | 175.66(10) | |
C1 | O1 | Li2 | Li4 | -151.95(12) | Li1 | O4 | Li3 | Li2 | -38.62(6) | |
C18 | N3 | C16 | C13 | -91.77(9) | Li1 | O4 | Li3 | Li4 | -81.45(6) | |
C7 | O2 | Li1 | O4 | 158.23(14) | Li1 | O2 | C7 | C9 | -174.38(15) | |
C7 | O2 | Li1 | O1 | -104.40(17) | Li1 | O2 | C7 | C10 | 62.63(19) | |
C7 | O2 | Li1 | N1 | -8.7(2) | Li1 | O2 | C7 | C8 | -54.92(19) | |
C7 | O2 | Li1 | Li2 | -110.10(17) | Li1 | O1 | C1 | C2 | 82.90(8) | |
C7 | O2 | Li1 | Li3 | -153.49(15) | Li1 | O1 | C1 | C4 | -40.27(9) | |
C7 | O2 | Li1 | Li4 | 167.80(18) | Li1 | O1 | C1 | C3 | -157.63(7) | |
C20 | C19 | C22 | N4 | 67.84(10) | Li1 | O1 | Li2 | O2 | 5.75(6) | |
C24 | N4 | C22 | C19 | -89.84(9) | Li1 | O1 | Li2 | O3 | -91.58(7) | |
C12 | N2 | C10 | C7 | 96.08(9) | Li1 | O1 | Li2 | N2 | 103.09(10) | |
C5 | N1 | C4 | C1 | 94.93(9) | Li1 | O1 | Li2 | Li3 | -81.52(6) | |
C11 | N2 | C10 | C7 | -143.05(8) | Li1 | O1 | Li2 | Li4 | -43.15(6) | |
C6 | N1 | C4 | C1 | -144.76(8) | Li1 | N1 | C4 | C1 | -34.54(9) | |
C17 | N3 | C16 | C13 | 148.02(8) | Li4 | O4 | C19 | C21 | 152.12(8) | |
C23 | N4 | C22 | C19 | 150.19(8) | Li4 | O4 | C19 | C22 | 34.99(9) | |
Li2 | O2 | C7 | C9 | 80.61(8) | Li4 | O4 | C19 | C20 | -88.87(8) | |
Li2 | O2 | C7 | C10 | -42.37(8) | Li4 | O4 | Li3 | O1 | 90.61(7) | |
Li2 | O2 | C7 | C8 | -159.92(7) | Li4 | O4 | Li3 | O3 | -6.06(6) | |
Li2 | O2 | Li1 | O4 | -91.67(7) | Li4 | O4 | Li3 | N3 | -102.89(10) | |
Li2 | O2 | Li1 | O1 | 5.70(6) | Li4 | O4 | Li3 | Li2 | 42.83(6) | |
Li2 | O2 | Li1 | N1 | 101.40(10) | Li4 | O4 | Li3 | Li1 | 81.45(6) | |
Li2 | O2 | Li1 | Li3 | -43.39(6) | Li4 | O2 | C7 | C9 | -8.28(9) | |
Li2 | O2 | Li1 | Li4 | -82.09(6) | Li4 | O2 | C7 | C10 | -131.26(7) | |
Li2 | O1 | C1 | C2 | -174.82(12) | Li4 | O2 | C7 | C8 | 111.19(8) | |
Li2 | O1 | C1 | C4 | 62.01(16) | Li4 | O2 | Li1 | O4 | -9.58(6) | |
Li2 | O1 | C1 | C3 | -55.35(16) | Li4 | O2 | Li1 | O1 | 87.79(7) | |
Li2 | O3 | C13 | C16 | 129.27(8) | Li4 | O2 | Li1 | N1 | -176.51(10) | |
Li2 | O3 | C13 | C15 | 5.62(10) | Li4 | O2 | Li1 | Li2 | 82.09(6) | |
Li2 | O3 | C13 | C14 | -113.36(9) | Li4 | O2 | Li1 | Li3 | 38.71(6) | |
Li2 | O3 | Li4 | O4 | -88.16(7) | Li4 | O3 | C13 | C16 | -65.35(16) | |
Li2 | O3 | Li4 | O2 | 9.93(6) | Li4 | O3 | C13 | C15 | 171.00(13) | |
Li2 | O3 | Li4 | N4 | 173.03(11) | Li4 | O3 | C13 | C14 | 52.01(18) | |
Li2 | O3 | Li4 | Li3 | -82.10(6) | Li4 | N4 | C22 | C19 | 38.36(8) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H21A | 2157 | -57 | 6065 | 51 |
H21B | 1258 | -166 | 6012 | 51 |
H21C | 1789 | 997 | 6499 | 51 |
H22A | 1819 | -149 | 4738 | 21 |
H22B | 901 | -181 | 4602 | 21 |
H16A | 3726 | 506 | 4668 | 24 |
H16B | 4603 | 1034 | 4895 | 24 |
H9A | 2053 | 4108 | 3130 | 32 |
H9B | 1363 | 4947 | 2555 | 32 |
H9C | 1167 | 3634 | 2943 | 32 |
H2A | 2953 | 3325 | 6916 | 32 |
H2B | 3493 | 4263 | 7568 | 32 |
H2C | 3873 | 3388 | 7058 | 32 |
H4A | 2762 | 6321 | 7063 | 24 |
H4B | 2639 | 6792 | 6210 | 24 |
H10A | 1710 | 7030 | 3269 | 22 |
H10B | 1744 | 7132 | 4139 | 22 |
H15A | 4222 | 4349 | 4248 | 38 |
H15B | 4898 | 3316 | 4653 | 38 |
H15C | 4398 | 3990 | 5127 | 38 |
H18A | 5262 | 1228 | 6155 | 47 |
H18B | 4858 | 1873 | 6724 | 47 |
H18C | 4960 | 2729 | 6036 | 47 |
H8A | 270 | 4764 | 3486 | 40 |
H8B | 383 | 6086 | 3056 | 40 |
H8C | 514 | 6118 | 3950 | 40 |
H20A | 779 | 2519 | 5798 | 47 |
H20B | 273 | 1468 | 5194 | 47 |
H20C | 601 | 2770 | 4907 | 47 |
H24A | 99 | 481 | 3439 | 45 |
H24B | 305 | 1766 | 3033 | 45 |
H24C | 167 | 1899 | 3841 | 45 |
H12A | 2785 | 5708 | 3005 | 42 |
H12B | 3602 | 6291 | 3531 | 42 |
H12C | 2913 | 7277 | 3089 | 42 |
H3A | 4471 | 5287 | 6631 | 38 |
H3B | 4179 | 6203 | 7191 | 38 |
H3C | 3974 | 6595 | 6313 | 38 |
H5A | 2030 | 4257 | 7214 | 44 |
H5B | 1125 | 4482 | 6757 | 44 |
H5C | 1623 | 5640 | 7280 | 44 |
H11A | 2993 | 8351 | 4253 | 42 |
H11B | 3690 | 7375 | 4689 | 42 |
H11C | 2939 | 7505 | 4965 | 42 |
H14A | 3327 | 1364 | 3428 | 42 |
H14B | 4207 | 1816 | 3550 | 42 |
H14C | 3509 | 2856 | 3244 | 42 |
H6A | 1269 | 7144 | 6248 | 47 |
H6B | 743 | 6000 | 5737 | 47 |
H6C | 1380 | 6749 | 5453 | 47 |
H17A | 3409 | -209 | 5680 | 50 |
H17B | 3943 | 187 | 6520 | 50 |
H17C | 4320 | -550 | 5957 | 50 |
H23A | 2067 | 165 | 3634 | 50 |
H23B | 1418 | 795 | 2916 | 50 |
H23C | 1235 | -538 | 3295 | 50 |
Experimental
Single crystals of C24H56Li4N4O4 [mo_B0321_0m] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 99.98 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 XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0321_0m]
Crystal Data for C24H56Li4N4O4 (M =492.48 g/mol): monoclinic, space group P21/n (no. 14), a = 18.0767(15) Å, b = 10.0888(9) Å, c = 18.548(2) Å, β = 108.538(4)°, V = 3207.1(5) Å3, Z = 4, T = 99.98 K, μ(MoKα) = 0.066 mm-1, Dcalc = 1.020 g/cm3, 70347 reflections measured (4.686° ≤ 2Θ ≤ 56°), 7736 unique (Rint = 0.0243, Rsigma = 0.0142) which were used in all calculations. The final R1 was 0.0348 (I > 2σ(I)) and wR2 was 0.0944 (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:
C22(H22A,H22B), C16(H16A,H16B), C4(H4A,H4B), C10(H10A,H10B)
2.b Idealised Me refined as rotating group:
C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C2(H2A,H2B,H2C), C15(H15A,H15B,H15C),
C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C),
C12(H12A,H12B,H12C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C),
C14(H14A,H14B,H14C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C)
This report has been created with Olex2, compiled on 2015.09.30 svn.r3233 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.