Identification code | mo_B0517_0m |
Empirical formula | C22H50Li4N2O6 |
Formula weight | 466.40 |
Temperature/K | 100.01 |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 15.696(3) |
b/Å | 9.3886(17) |
c/Å | 19.721(4) |
α/° | 90 |
β/° | 92.353(7) |
γ/° | 90 |
Volume/Å3 | 2903.8(10) |
Z | 4 |
ρcalcg/cm3 | 1.067 |
μ/mm‑1 | 0.073 |
F(000) | 1024.0 |
Crystal size/mm3 | 0.35 × 0.23 × 0.14 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 5.056 to 52 |
Index ranges | -19 ≤ h ≤ 19, -11 ≤ k ≤ 11, -24 ≤ l ≤ 24 |
Reflections collected | 76371 |
Independent reflections | 5705 [Rint = 0.0453, Rsigma = 0.0203] |
Data/restraints/parameters | 5705/0/340 |
Goodness-of-fit on F2 | 1.058 |
Final R indexes [I>=2σ (I)] | R1 = 0.0358, wR2 = 0.0855 |
Final R indexes [all data] | R1 = 0.0457, wR2 = 0.0915 |
Largest diff. peak/hole / e Å-3 | 0.28/-0.19 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
C1 | 2563.8(8) | 352.0(14) | 4781.9(7) | 26.2(3) |
C2 | 3253.2(8) | 1131.3(15) | 5188.7(6) | 28.9(3) |
C3 | 3975.1(9) | 3335.5(19) | 5262.0(8) | 40.8(4) |
C4 | 1195.1(8) | 807.5(13) | 4202.6(6) | 19.5(3) |
C5 | 1426.8(8) | 1749.6(13) | 3614.5(6) | 20.7(3) |
C6 | 1436.2(9) | 4179.0(14) | 3315.4(6) | 27.2(3) |
C7 | 1324.8(8) | 912.6(12) | 5449.2(6) | 19.2(3) |
C8 | 1019.8(7) | 2330.5(12) | 5752.2(5) | 16.8(2) |
C9 | 774.1(8) | 2015.0(14) | 6483.6(6) | 24.6(3) |
C10 | 238.8(8) | 2925.6(14) | 5357.4(6) | 22.9(3) |
C11 | 3798.9(7) | 8432.0(13) | 6864.1(6) | 18.7(2) |
C12 | 3958.9(8) | 7511.4(13) | 6250.1(6) | 19.8(3) |
C13 | 5027.9(8) | 5866.4(15) | 6634.8(7) | 30.0(3) |
C14 | 3159.1(8) | 8243.3(13) | 7964.1(6) | 19.3(3) |
C15 | 3820.2(8) | 7350.9(13) | 8345.5(6) | 21.0(3) |
C16 | 4247.0(8) | 5006.0(15) | 8556.2(7) | 28.3(3) |
C17 | 2258.8(7) | 8182.1(12) | 6917.5(6) | 17.1(2) |
C18 | 1670.4(7) | 6872.4(12) | 6862.4(6) | 16.1(2) |
C19 | 1353.6(8) | 6430.0(14) | 7557.9(6) | 22.8(3) |
C20 | 900.9(8) | 7285.6(14) | 6400.6(7) | 24.7(3) |
C21 | 2414.6(11) | 5816.6(16) | 4724.3(6) | 31.1(3) |
C22 | 3297.1(9) | 3031.2(14) | 7183.1(6) | 22.3(3) |
Li1 | 2113.8(13) | 3415(2) | 4819.4(10) | 21.9(4) |
Li2 | 1863.8(14) | 5276(2) | 5657.6(10) | 23.7(4) |
Li3 | 2200.3(13) | 3759(2) | 6604.2(10) | 21.7(4) |
Li4 | 3200.7(13) | 5482(2) | 7107.4(10) | 20.6(4) |
N1 | 1748.8(6) | 1111.6(11) | 4802.8(5) | 17.9(2) |
N2 | 3095.0(6) | 7845(1) | 7242.9(5) | 15.8(2) |
O1 | 3348.9(6) | 2503.1(11) | 4893.9(4) | 28.3(2) |
O2 | 1414.1(6) | 3179.4(9) | 3856.3(4) | 21.6(2) |
O3 | 1690.1(5) | 3305.8(8) | 5748.3(4) | 17.42(18) |
O4 | 4153.6(5) | 6083.7(9) | 6453.4(4) | 20.46(19) |
O5 | 3638.4(5) | 5891.2(9) | 8211.5(4) | 21.8(2) |
O6 | 2121.2(5) | 5752.6(8) | 6578.6(4) | 16.50(18) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
C1 | 28.9(7) | 24.4(7) | 25.3(6) | -3.9(5) | 0.9(5) | 7.5(5) |
C2 | 25.2(7) | 37.9(8) | 23.6(6) | -3.1(6) | -1.0(5) | 9.1(6) |
C3 | 26.7(7) | 60.9(11) | 34.7(8) | -10.3(7) | -1.8(6) | -13.9(7) |
C4 | 24.1(6) | 18.1(6) | 16.3(5) | -3.4(5) | 0.9(5) | -5.1(5) |
C5 | 25.3(6) | 21.6(6) | 15.2(5) | -4.2(5) | 0.8(5) | -4.7(5) |
C6 | 37.3(7) | 26.8(7) | 17.3(6) | 6.4(5) | -0.9(5) | -7.5(6) |
C7 | 25.4(6) | 15.7(6) | 16.3(5) | 2.8(4) | 1.0(5) | -3.6(5) |
C8 | 19.7(6) | 17.4(6) | 13.4(5) | 0.6(4) | 1.4(4) | -4.4(5) |
C9 | 29.6(7) | 27.3(7) | 17.1(6) | 1.3(5) | 5.0(5) | -6.5(5) |
C10 | 21.3(6) | 25.5(6) | 21.7(6) | -0.8(5) | 0.1(5) | -0.6(5) |
C11 | 18.2(6) | 16.8(6) | 21.0(6) | -0.6(5) | 0.0(5) | -2.3(5) |
C12 | 19.7(6) | 20.9(6) | 18.9(6) | 1.2(5) | 1.4(4) | -1.2(5) |
C13 | 19.3(6) | 31.6(7) | 39.1(7) | 0.0(6) | 0.4(5) | 3.6(6) |
C14 | 20.6(6) | 19.3(6) | 17.9(6) | -5.5(5) | -0.9(4) | 2.0(5) |
C15 | 20.4(6) | 24.3(6) | 17.8(6) | -4.8(5) | -2.2(5) | 0.8(5) |
C16 | 26.8(7) | 31.5(7) | 26.2(6) | 5.3(6) | -2.4(5) | 10.2(6) |
C17 | 18.5(6) | 14.7(6) | 17.8(5) | 0.2(4) | -0.8(4) | 3.3(5) |
C18 | 15.6(5) | 15.7(6) | 16.8(5) | 0.2(4) | -0.3(4) | 2.3(4) |
C19 | 22.2(6) | 24.8(6) | 21.9(6) | 1.1(5) | 6.1(5) | -1.2(5) |
C20 | 19.6(6) | 23.5(6) | 30.3(7) | 1.5(5) | -6.5(5) | 1.4(5) |
C21 | 51.7(9) | 26.2(7) | 15.4(6) | -0.3(5) | 2.0(6) | -15.8(7) |
C22 | 26.6(7) | 19.6(6) | 20.4(6) | 0.3(5) | -3.8(5) | 3.0(5) |
Li1 | 27.1(11) | 22.7(10) | 16.1(9) | 0.0(8) | 3.1(8) | -6.4(9) |
Li2 | 34.1(12) | 19.4(10) | 17.3(9) | 0.3(8) | -0.7(8) | -3.8(9) |
Li3 | 28.1(11) | 19(1) | 17.8(9) | -0.2(8) | -2.5(8) | -1.4(8) |
Li4 | 19.4(10) | 20(1) | 22.1(10) | -1.1(8) | -1.6(8) | 0.3(8) |
N1 | 21.0(5) | 18.1(5) | 14.5(5) | -1.7(4) | 1.3(4) | -0.4(4) |
N2 | 15.4(5) | 17.2(5) | 14.9(5) | -1.7(4) | -0.3(4) | 0.2(4) |
O1 | 22.1(5) | 39.5(6) | 23.2(4) | -5.4(4) | -0.3(4) | -5.6(4) |
O2 | 32.8(5) | 18.7(4) | 13.3(4) | 1.3(3) | 0.2(3) | -6.6(4) |
O3 | 21.6(4) | 16.8(4) | 13.9(4) | -0.6(3) | 0.3(3) | -5.9(3) |
O4 | 17.8(4) | 19.7(4) | 23.9(4) | -2.8(3) | 1.0(3) | 1.5(3) |
O5 | 23.2(4) | 20.7(4) | 21.2(4) | 0.5(3) | -3.6(3) | 4.7(4) |
O6 | 18.6(4) | 15.1(4) | 15.7(4) | -2.8(3) | -1.2(3) | 1.4(3) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
C1 | C2 | 1.5095(18) | C18 | C19 | 1.5354(16) | |
C1 | N1 | 1.4667(16) | C18 | C20 | 1.5324(16) | |
C2 | O1 | 1.4235(17) | C18 | Li4 | 2.759(2) | |
C3 | O1 | 1.4302(16) | C18 | O6 | 1.3970(14) | |
C4 | C5 | 1.5146(16) | C21 | Li1 | 2.313(3) | |
C4 | N1 | 1.4675(14) | C21 | Li2 | 2.127(2) | |
C5 | O2 | 1.4250(15) | C22 | Li3 | 2.139(2) | |
C6 | O2 | 1.4223(14) | C22 | Li4 | 2.311(2) | |
C7 | C8 | 1.5433(16) | Li1 | Li2 | 2.448(3) | |
C7 | N1 | 1.4740(14) | Li1 | Li3 | 3.532(3) | |
C8 | C9 | 1.5371(16) | Li1 | N1 | 2.237(2) | |
C8 | C10 | 1.5306(16) | Li1 | O1 | 2.119(2) | |
C8 | Li1 | 2.762(2) | Li1 | O2 | 2.166(2) | |
C8 | O3 | 1.3951(14) | Li1 | O3 | 1.977(2) | |
C9 | Li3 | 2.776(2) | Li2 | Li3 | 2.390(3) | |
C11 | C12 | 1.5169(16) | Li2 | Li4 | 3.482(3) | |
C11 | N2 | 1.4664(15) | Li2 | O3 | 1.879(2) | |
C12 | O4 | 1.4286(15) | Li2 | O6 | 1.898(2) | |
C13 | O4 | 1.4186(15) | Li3 | Li4 | 2.437(3) | |
C14 | C15 | 1.5101(16) | Li3 | O3 | 1.887(2) | |
C14 | N2 | 1.4701(14) | Li3 | O6 | 1.876(2) | |
C15 | O5 | 1.4224(15) | Li4 | N2 | 2.241(2) | |
C16 | O5 | 1.4185(14) | Li4 | O4 | 2.092(2) | |
C17 | C18 | 1.5390(16) | Li4 | O5 | 2.289(2) | |
C17 | N2 | 1.4715(15) | Li4 | O6 | 1.969(2) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
N1 | C1 | C2 | 110.89(10) | Li2 | Li3 | C9 | 97.64(9) | |
O1 | C2 | C1 | 107.87(10) | Li2 | Li3 | Li1 | 43.76(7) | |
N1 | C4 | C5 | 110.55(9) | Li2 | Li3 | Li4 | 92.33(10) | |
O2 | C5 | C4 | 106.67(9) | Li4 | Li3 | C9 | 158.48(10) | |
N1 | C7 | C8 | 112.57(9) | Li4 | Li3 | Li1 | 117.67(9) | |
C7 | C8 | Li1 | 81.31(8) | O3 | Li3 | C9 | 58.61(6) | |
C9 | C8 | C7 | 106.91(9) | O3 | Li3 | C22 | 135.09(12) | |
C9 | C8 | Li1 | 151.98(9) | O3 | Li3 | Li1 | 24.54(5) | |
C10 | C8 | C7 | 111.88(9) | O3 | Li3 | Li2 | 50.48(7) | |
C10 | C8 | C9 | 108.73(10) | O3 | Li3 | Li4 | 139.18(12) | |
C10 | C8 | Li1 | 91.92(8) | O6 | Li3 | C9 | 122.27(10) | |
O3 | C8 | C7 | 108.54(9) | O6 | Li3 | C22 | 112.59(11) | |
O3 | C8 | C9 | 110.48(9) | O6 | Li3 | Li1 | 93.71(8) | |
O3 | C8 | C10 | 110.25(9) | O6 | Li3 | Li2 | 51.12(7) | |
O3 | C8 | Li1 | 42.67(6) | O6 | Li3 | Li4 | 52.38(7) | |
C8 | C9 | Li3 | 74.59(8) | O6 | Li3 | O3 | 100.13(10) | |
N2 | C11 | C12 | 110.21(9) | C18 | Li4 | Li2 | 52.52(5) | |
O4 | C12 | C11 | 110.55(9) | C22 | Li4 | C18 | 122.46(9) | |
N2 | C14 | C15 | 111.05(9) | C22 | Li4 | Li2 | 91.91(8) | |
O5 | C15 | C14 | 108.27(9) | C22 | Li4 | Li3 | 53.46(7) | |
N2 | C17 | C18 | 112.39(9) | Li3 | Li4 | C18 | 72.60(8) | |
C17 | C18 | Li4 | 81.36(8) | Li3 | Li4 | Li2 | 43.29(7) | |
C19 | C18 | C17 | 111.62(9) | N2 | Li4 | C18 | 58.97(6) | |
C19 | C18 | Li4 | 91.56(8) | N2 | Li4 | C22 | 169.41(11) | |
C20 | C18 | C17 | 107.21(9) | N2 | Li4 | Li2 | 96.20(8) | |
C20 | C18 | C19 | 108.85(10) | N2 | Li4 | Li3 | 130.99(10) | |
C20 | C18 | Li4 | 152.02(9) | N2 | Li4 | O5 | 75.01(7) | |
O6 | C18 | C17 | 108.49(9) | O4 | Li4 | C18 | 113.81(9) | |
O6 | C18 | C19 | 110.01(9) | O4 | Li4 | C22 | 105.19(9) | |
O6 | C18 | C20 | 110.62(9) | O4 | Li4 | Li2 | 86.04(8) | |
O6 | C18 | Li4 | 42.48(6) | O4 | Li4 | Li3 | 113.14(10) | |
Li2 | C21 | Li1 | 66.77(8) | O4 | Li4 | N2 | 82.23(8) | |
Li3 | C22 | Li4 | 66.29(8) | O4 | Li4 | O5 | 110.30(9) | |
C8 | Li1 | Li3 | 50.91(5) | O5 | Li4 | C18 | 108.21(8) | |
C21 | Li1 | C8 | 123.23(9) | O5 | Li4 | C22 | 95.12(8) | |
C21 | Li1 | Li2 | 52.98(7) | O5 | Li4 | Li2 | 159.69(9) | |
C21 | Li1 | Li3 | 89.54(7) | O5 | Li4 | Li3 | 131.45(10) | |
Li2 | Li1 | C8 | 72.07(7) | O6 | Li4 | C18 | 28.63(4) | |
Li2 | Li1 | Li3 | 42.47(7) | O6 | Li4 | C22 | 102.42(9) | |
N1 | Li1 | C8 | 59.17(6) | O6 | Li4 | Li2 | 25.29(5) | |
N1 | Li1 | C21 | 173.84(11) | O6 | Li4 | Li3 | 48.99(7) | |
N1 | Li1 | Li2 | 130.68(10) | O6 | Li4 | N2 | 82.49(8) | |
N1 | Li1 | Li3 | 95.88(7) | O6 | Li4 | O4 | 105.08(10) | |
O1 | Li1 | C8 | 113.39(9) | O6 | Li4 | O5 | 134.46(10) | |
O1 | Li1 | C21 | 102.14(10) | C1 | N1 | C4 | 111.78(9) | |
O1 | Li1 | Li2 | 114.41(10) | C1 | N1 | C7 | 112.82(9) | |
O1 | Li1 | Li3 | 88.30(7) | C1 | N1 | Li1 | 104.32(9) | |
O1 | Li1 | N1 | 80.99(8) | C4 | N1 | C7 | 113.55(9) | |
O1 | Li1 | O2 | 116.68(10) | C4 | N1 | Li1 | 110.05(9) | |
O2 | Li1 | C8 | 103.86(8) | C7 | N1 | Li1 | 103.55(8) | |
O2 | Li1 | C21 | 97.25(9) | C11 | N2 | C14 | 111.97(9) | |
O2 | Li1 | Li2 | 125.13(11) | C11 | N2 | C17 | 111.98(9) | |
O2 | Li1 | Li3 | 151.72(9) | C11 | N2 | Li4 | 104.49(8) | |
O2 | Li1 | N1 | 76.59(7) | C14 | N2 | C17 | 113.05(9) | |
O3 | Li1 | C8 | 28.57(4) | C14 | N2 | Li4 | 111.39(9) | |
O3 | Li1 | C21 | 101.73(9) | C17 | N2 | Li4 | 103.30(8) | |
O3 | Li1 | Li2 | 48.85(7) | C2 | O1 | C3 | 111.64(11) | |
O3 | Li1 | Li3 | 23.35(5) | C2 | O1 | Li1 | 106.40(9) | |
O3 | Li1 | N1 | 82.40(8) | C3 | O1 | Li1 | 114.97(11) | |
O3 | Li1 | O1 | 104.86(10) | C5 | O2 | Li1 | 112.09(9) | |
O3 | Li1 | O2 | 129.01(11) | C6 | O2 | C5 | 111.69(9) | |
C21 | Li2 | Li1 | 60.25(8) | C6 | O2 | Li1 | 124.27(9) | |
C21 | Li2 | Li3 | 137.18(13) | C8 | O3 | Li1 | 108.76(9) | |
C21 | Li2 | Li4 | 116.40(10) | C8 | O3 | Li2 | 139.37(10) | |
Li1 | Li2 | Li4 | 119.10(10) | C8 | O3 | Li3 | 115.83(9) | |
Li3 | Li2 | Li1 | 93.77(10) | Li2 | O3 | Li1 | 78.76(9) | |
Li3 | Li2 | Li4 | 44.38(7) | Li2 | O3 | Li3 | 78.76(9) | |
O3 | Li2 | C21 | 112.52(11) | Li3 | O3 | Li1 | 132.11(10) | |
O3 | Li2 | Li1 | 52.39(7) | C12 | O4 | Li4 | 106.03(9) | |
O3 | Li2 | Li3 | 50.76(7) | C13 | O4 | C12 | 113.53(9) | |
O3 | Li2 | Li4 | 93.53(8) | C13 | O4 | Li4 | 120.96(9) | |
O3 | Li2 | O6 | 99.62(10) | C15 | O5 | Li4 | 112.86(8) | |
O6 | Li2 | C21 | 133.93(12) | C16 | O5 | C15 | 110.45(9) | |
O6 | Li2 | Li1 | 141.33(12) | C16 | O5 | Li4 | 121.85(9) | |
O6 | Li2 | Li3 | 50.31(7) | C18 | O6 | Li2 | 117.99(9) | |
O6 | Li2 | Li4 | 26.31(6) | C18 | O6 | Li3 | 140.71(10) | |
C9 | Li3 | Li1 | 82.11(6) | C18 | O6 | Li4 | 108.89(9) | |
C22 | Li3 | C9 | 119.07(10) | Li2 | O6 | Li4 | 128.40(10) | |
C22 | Li3 | Li1 | 120.00(9) | Li3 | O6 | Li2 | 78.56(9) | |
C22 | Li3 | Li2 | 139.01(12) | Li3 | O6 | Li4 | 78.62(9) | |
C22 | Li3 | Li4 | 60.25(8) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
C1 | C2 | O1 | C3 | 178.22(11) | C22 | Li3 | O6 | C18 | -103.78(15) | |
C1 | C2 | O1 | Li1 | 52.05(12) | C22 | Li3 | O6 | Li2 | 135.62(12) | |
C2 | C1 | N1 | C4 | 153.82(10) | C22 | Li3 | O6 | Li4 | 2.22(11) | |
C2 | C1 | N1 | C7 | -76.76(13) | Li1 | C8 | C9 | Li3 | 9.2(2) | |
C2 | C1 | N1 | Li1 | 34.94(12) | Li1 | C8 | O3 | Li2 | 94.58(15) | |
C4 | C5 | O2 | C6 | -167.07(10) | Li1 | C8 | O3 | Li3 | -162.03(13) | |
C4 | C5 | O2 | Li1 | 48.29(12) | Li1 | Li2 | O3 | C8 | -105.78(14) | |
C5 | C4 | N1 | C1 | -83.07(12) | Li1 | Li2 | O3 | Li3 | 137.43(10) | |
C5 | C4 | N1 | C7 | 147.89(10) | Li1 | Li2 | O6 | C18 | -167.70(16) | |
C5 | C4 | N1 | Li1 | 32.36(12) | Li1 | Li2 | O6 | Li3 | -25.81(19) | |
C7 | C8 | C9 | Li3 | 112.80(9) | Li1 | Li2 | O6 | Li4 | 39.5(2) | |
C7 | C8 | O3 | Li1 | 53.20(11) | Li1 | Li3 | O3 | C8 | 156.81(17) | |
C7 | C8 | O3 | Li2 | 147.78(13) | Li1 | Li3 | O3 | Li2 | -63.42(13) | |
C7 | C8 | O3 | Li3 | -108.83(11) | Li1 | Li3 | O6 | C18 | 131.49(13) | |
C8 | C7 | N1 | C1 | 131.70(10) | Li1 | Li3 | O6 | Li2 | 10.89(8) | |
C8 | C7 | N1 | C4 | -99.79(11) | Li1 | Li3 | O6 | Li4 | -122.51(8) | |
C8 | C7 | N1 | Li1 | 19.53(12) | Li2 | Li3 | O3 | C8 | -139.77(11) | |
C9 | C8 | O3 | Li1 | 170.12(10) | Li2 | Li3 | O3 | Li1 | 63.42(13) | |
C9 | C8 | O3 | Li2 | -95.30(15) | Li2 | Li3 | O6 | C18 | 120.60(15) | |
C9 | C8 | O3 | Li3 | 8.09(14) | Li2 | Li3 | O6 | Li4 | -133.40(10) | |
C9 | Li3 | O3 | C8 | -4.91(8) | Li3 | Li2 | O3 | C8 | 116.79(14) | |
C9 | Li3 | O3 | Li1 | -161.72(12) | Li3 | Li2 | O3 | Li1 | -137.43(10) | |
C9 | Li3 | O3 | Li2 | 134.86(9) | Li3 | Li2 | O6 | C18 | -141.89(11) | |
C9 | Li3 | O6 | C18 | 48.48(19) | Li3 | Li2 | O6 | Li4 | 65.34(12) | |
C9 | Li3 | O6 | Li2 | -72.12(11) | Li4 | C18 | O6 | Li2 | -157.73(13) | |
C9 | Li3 | O6 | Li4 | 154.48(12) | Li4 | C18 | O6 | Li3 | 95.10(16) | |
C10 | C8 | C9 | Li3 | -126.25(10) | Li4 | Li2 | O3 | C8 | 129.64(12) | |
C10 | C8 | O3 | Li1 | -69.66(12) | Li4 | Li2 | O3 | Li1 | -124.58(9) | |
C10 | C8 | O3 | Li2 | 24.91(17) | Li4 | Li2 | O3 | Li3 | 12.85(8) | |
C10 | C8 | O3 | Li3 | 128.31(11) | Li4 | Li2 | O6 | C18 | 152.77(15) | |
C11 | C12 | O4 | C13 | -85.37(12) | Li4 | Li2 | O6 | Li3 | -65.34(12) | |
C11 | C12 | O4 | Li4 | 49.77(11) | Li4 | Li3 | O3 | C8 | -168.79(15) | |
C12 | C11 | N2 | C14 | 153.81(9) | Li4 | Li3 | O3 | Li1 | 34.4(2) | |
C12 | C11 | N2 | C17 | -78.01(12) | Li4 | Li3 | O3 | Li2 | -29.03(18) | |
C12 | C11 | N2 | Li4 | 33.12(11) | Li4 | Li3 | O6 | C18 | -105.99(15) | |
C14 | C15 | O5 | C16 | 179.63(9) | Li4 | Li3 | O6 | Li2 | 133.40(10) | |
C14 | C15 | O5 | Li4 | 39.42(12) | N1 | C1 | C2 | O1 | -61.00(13) | |
C15 | C14 | N2 | C11 | -77.40(12) | N1 | C4 | C5 | O2 | -53.15(12) | |
C15 | C14 | N2 | C17 | 154.99(10) | N1 | C7 | C8 | C9 | -167.93(9) | |
C15 | C14 | N2 | Li4 | 39.20(12) | N1 | C7 | C8 | C10 | 73.13(12) | |
C17 | C18 | O6 | Li2 | -104.57(11) | N1 | C7 | C8 | Li1 | -15.44(9) | |
C17 | C18 | O6 | Li3 | 148.26(13) | N1 | C7 | C8 | O3 | -48.74(12) | |
C17 | C18 | O6 | Li4 | 53.15(11) | N2 | C11 | C12 | O4 | -58.44(12) | |
C18 | C17 | N2 | C11 | 132.96(10) | N2 | C14 | C15 | O5 | -52.24(13) | |
C18 | C17 | N2 | C14 | -99.44(11) | N2 | C17 | C18 | C19 | 71.53(12) | |
C18 | C17 | N2 | Li4 | 21.08(11) | N2 | C17 | C18 | C20 | -169.35(9) | |
C19 | C18 | O6 | Li2 | 133.06(11) | N2 | C17 | C18 | Li4 | -16.72(9) | |
C19 | C18 | O6 | Li3 | 25.89(18) | N2 | C17 | C18 | O6 | -49.85(12) | |
C19 | C18 | O6 | Li4 | -69.21(11) | O3 | C8 | C9 | Li3 | -5.13(9) | |
C20 | C18 | O6 | Li2 | 12.76(14) | O3 | Li2 | O6 | C18 | -128.87(10) | |
C20 | C18 | O6 | Li3 | -94.41(16) | O3 | Li2 | O6 | Li3 | 13.01(10) | |
C20 | C18 | O6 | Li4 | 170.49(10) | O3 | Li2 | O6 | Li4 | 78.36(14) | |
C21 | Li2 | O3 | C8 | -109.85(15) | O3 | Li3 | O6 | C18 | 107.62(14) | |
C21 | Li2 | O3 | Li1 | -4.07(11) | O3 | Li3 | O6 | Li2 | -12.98(10) | |
C21 | Li2 | O3 | Li3 | 133.37(13) | O3 | Li3 | O6 | Li4 | -146.39(11) | |
C21 | Li2 | O6 | C18 | 96.50(18) | O6 | Li2 | O3 | C8 | 103.86(14) | |
C21 | Li2 | O6 | Li3 | -121.61(18) | O6 | Li2 | O3 | Li1 | -150.36(11) | |
C21 | Li2 | O6 | Li4 | -56.3(2) | O6 | Li2 | O3 | Li3 | -12.93(10) | |
C22 | Li3 | O3 | C8 | 96.28(17) | O6 | Li3 | O3 | C8 | -126.66(10) | |
C22 | Li3 | O3 | Li1 | -60.5(2) | O6 | Li3 | O3 | Li1 | 76.53(15) | |
C22 | Li3 | O3 | Li2 | -123.96(17) | O6 | Li3 | O3 | Li2 | 13.10(10) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H1A | 2731 | 263 | 4305 | 31 |
H1B | 2498 | -619 | 4968 | 31 |
H2A | 3093 | 1225 | 5667 | 35 |
H2B | 3797 | 598 | 5179 | 35 |
H3A | 3823 | 3406 | 5738 | 61 |
H3B | 3997 | 4291 | 5064 | 61 |
H3C | 4534 | 2879 | 5237 | 61 |
H4A | 593 | 974 | 4311 | 23 |
H4B | 1256 | -205 | 4073 | 23 |
H5A | 2001 | 1503 | 3461 | 25 |
H5B | 1009 | 1627 | 3229 | 25 |
H6A | 1949 | 4019 | 3058 | 41 |
H6B | 1447 | 5148 | 3501 | 41 |
H6C | 929 | 4059 | 3015 | 41 |
H7A | 1727 | 445 | 5779 | 23 |
H7B | 829 | 273 | 5374 | 23 |
H9A | 1273 | 1653 | 6744 | 37 |
H9B | 320 | 1299 | 6479 | 37 |
H9C | 573 | 2892 | 6694 | 37 |
H10A | 39 | 3785 | 5584 | 34 |
H10B | -216 | 2209 | 5341 | 34 |
H10C | 393 | 3164 | 4894 | 34 |
H11A | 4322 | 8473 | 7162 | 22 |
H11B | 3657 | 9413 | 6715 | 22 |
H12A | 3446 | 7514 | 5940 | 24 |
H12B | 4440 | 7910 | 6002 | 24 |
H13A | 5373 | 6075 | 6244 | 45 |
H13B | 5117 | 4874 | 6774 | 45 |
H13C | 5197 | 6500 | 7011 | 45 |
H14A | 2598 | 8110 | 8167 | 23 |
H14B | 3315 | 9262 | 8006 | 23 |
H15A | 4397 | 7591 | 8195 | 25 |
H15B | 3803 | 7541 | 8839 | 25 |
H16A | 4817 | 5219 | 8398 | 42 |
H16B | 4109 | 4005 | 8463 | 42 |
H16C | 4235 | 5182 | 9046 | 42 |
H17A | 2343 | 8565 | 6457 | 20 |
H17B | 1980 | 8931 | 7184 | 20 |
H19A | 948 | 5642 | 7500 | 34 |
H19B | 1072 | 7241 | 7767 | 34 |
H19C | 1839 | 6124 | 7851 | 34 |
H20A | 1095 | 7547 | 5951 | 37 |
H20B | 607 | 8098 | 6598 | 37 |
H20C | 508 | 6476 | 6357 | 37 |
H21A | 2880(12) | 6400(20) | 4949(9) | 58(5) |
H21B | 2710(11) | 5319(19) | 4350(9) | 48(5) |
H21C | 2016(13) | 6480(20) | 4492(10) | 66(6) |
H22A | 3228(11) | 2750(19) | 7662(10) | 51(5) |
H22B | 3217(13) | 2140(20) | 6928(10) | 65(6) |
H22C | 3922(11) | 3225(18) | 7153(8) | 45(5) |
Experimental
Single crystals of C22H50Li4N2O6 [mo_B0517_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 ShelXT [2] structure solution program using Intrinsic Phasing and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0517_0m]
Crystal Data for C22H50Li4N2O6 (M =466.40 g/mol): monoclinic, space group P21/c (no. 14), a = 15.696(3) Å, b = 9.3886(17) Å, c = 19.721(4) Å, β = 92.353(7)°, V = 2903.8(10) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 0.073 mm-1, Dcalc = 1.067 g/cm3, 76371 reflections measured (5.056° ≤ 2Θ ≤ 52°), 5705 unique (Rint = 0.0453, Rsigma = 0.0203) which were used in all calculations. The final R1 was 0.0358 (I > 2σ(I)) and wR2 was 0.0915 (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:
C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C11(H11A,
H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B)
2.b Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C20(H20A,H20B,
H20C)
This report has been created with Olex2, compiled on 2016.09.09 svn.r3337 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.