Identification code | C2c |
Empirical formula | C20H48K2Li2N2O5 |
Formula weight | 488.68 |
Temperature/K | 100.01 |
Crystal system | monoclinic |
Space group | C2/c |
a/Å | 23.29(2) |
b/Å | 13.532(9) |
c/Å | 21.12(3) |
α/° | 90 |
β/° | 121.01(3) |
γ/° | 90 |
Volume/Å3 | 5705(10) |
Z | 8 |
ρcalcg/cm3 | 1.138 |
μ/mm‑1 | 0.360 |
F(000) | 2128.0 |
Crystal size/mm3 | 0.25 × 0.24 × 0.21 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.902 to 53.998 |
Index ranges | ? ≤ h ≤ ?, ? ≤ k ≤ ?, ? ≤ l ≤ ? |
Reflections collected | 6223 |
Independent reflections | 6223 [Rint = ?, Rsigma = 0.0265] |
Data/restraints/parameters | 6223/0/377 |
Goodness-of-fit on F2 | 1.070 |
Final R indexes [I>=2σ (I)] | R1 = 0.0428, wR2 = 0.0841 |
Final R indexes [all data] | R1 = 0.0622, wR2 = 0.0907 |
Largest diff. peak/hole / e Å-3 | 0.26/-0.27 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
K1 | 3770.9(2) | 3803.0(3) | 7394.3(2) | 20.12(11) |
K2 | 4428.3(2) | 3789.2(3) | 6125.0(2) | 19.62(10) |
O4 | 4317.3(6) | 2275.7(8) | 6943.4(6) | 15.4(3) |
O2 | 4763.2(6) | 5327.0(9) | 8001.6(6) | 14.8(2) |
O1 | 3617.8(6) | 4917.1(9) | 6301.2(7) | 18.3(3) |
N2 | 5143.1(8) | 661.7(10) | 6416.0(8) | 18.5(3) |
C7 | 4434.6(9) | 5800.2(13) | 8309.5(10) | 17.9(4) |
N1 | 3870.8(7) | 6971.2(10) | 6430.5(8) | 15.9(3) |
O3B | 2541(4) | 3582(6) | 7297(5) | 25.9(13) |
O5 | 5454.5(7) | 2675.1(9) | 6452.6(7) | 22.1(3) |
C8 | 4582.8(11) | 5347.3(15) | 9039.2(11) | 23.9(4) |
C2 | 4043.2(11) | 7340.2(15) | 5897.4(11) | 27.8(4) |
C3 | 3185.8(9) | 6574.1(13) | 6071.5(10) | 19.4(4) |
C18 | 5624.1(11) | 2085.4(13) | 6039.2(11) | 24.6(4) |
C1 | 3937.4(10) | 7788.2(13) | 6915.0(11) | 23.8(4) |
C20 | 6320.3(13) | 2348.5(16) | 6183.2(15) | 42.2(6) |
C17 | 5669.6(11) | 987.1(13) | 6276.1(12) | 22.7(4) |
C6 | 2426.1(9) | 5145.3(15) | 5659.8(13) | 35.2(5) |
C15 | 4505.8(11) | 480.6(17) | 5736.5(12) | 36.2(5) |
C13 | 3718.5(10) | 1762.1(14) | 6601.0(12) | 27.6(4) |
C16 | 5345.1(11) | -251.1(14) | 6843.4(12) | 29.6(5) |
C19 | 5133.4(15) | 2239.1(16) | 5209.7(12) | 43.9(6) |
C10 | 2651.8(15) | 5003(2) | 7992.6(17) | 45.0(6) |
C5 | 3066.4(12) | 5438.4(16) | 5032.5(11) | 37.5(5) |
C9 | 2265.6(11) | 4079.5(17) | 7683.8(14) | 38.3(5) |
C4 | 3104.6(9) | 5498.7(13) | 5781(1) | 20.7(4) |
Li1 | 4410.1(14) | 5622(2) | 6961.5(15) | 15.0(6) |
Li2 | 5146.6(15) | 1983(2) | 7006.0(16) | 17.0(6) |
C11B | 2236(3) | 2709(3) | 6966(3) | 32.1(11) |
C12B | 1579(3) | 2863(4) | 6245(3) | 44.1(13) |
C14 | 3226.7(14) | 2160(2) | 5842.7(17) | 56.6(9) |
C12 | 1918(3) | 2522(4) | 6137(3) | 49.5(13) |
C11 | 1859(4) | 2874(4) | 6745(4) | 43.7(13) |
O3 | 2356(4) | 3720(7) | 7110(5) | 45(2) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
K1 | 24.2(2) | 13.18(18) | 30.8(2) | 1.09(16) | 19.67(18) | 0.72(15) |
K2 | 25.9(2) | 13.19(18) | 20.4(2) | 0.38(15) | 12.40(17) | 3.82(15) |
O4 | 11.1(5) | 15.9(6) | 16.4(6) | -2.3(5) | 5.1(5) | -0.8(5) |
O2 | 16.0(6) | 15.4(6) | 16.1(6) | -0.5(5) | 10.6(5) | -1.0(5) |
O1 | 12.9(6) | 12.5(6) | 19.9(6) | 1.2(5) | 1.7(5) | 2.3(5) |
N2 | 25.1(8) | 12.3(7) | 20.0(8) | 0.6(6) | 13.1(7) | 1.9(6) |
C7 | 21.3(9) | 15.8(9) | 20.5(9) | -0.9(7) | 13.4(8) | -0.8(7) |
N1 | 17.2(7) | 12.1(7) | 18.1(8) | -1.8(6) | 8.9(6) | -0.1(6) |
O3B | 38(3) | 15(2) | 35(4) | 5(2) | 26(3) | 2(2) |
O5 | 39.0(8) | 12.3(6) | 29.5(7) | 0.7(5) | 28.0(7) | 3.9(5) |
C8 | 33.0(11) | 22.8(10) | 24(1) | -1.2(8) | 20.5(10) | 1.3(8) |
C2 | 33.5(11) | 24(1) | 31.7(11) | 2.6(8) | 21(1) | 0.1(8) |
C3 | 15.5(8) | 14.0(8) | 22.3(10) | 1.2(7) | 5.3(8) | 3.0(7) |
C18 | 44.8(12) | 14.0(9) | 32.4(11) | 0.9(8) | 32.4(10) | 4.0(8) |
C1 | 26.6(10) | 15.5(9) | 30.2(11) | -6.2(8) | 15.4(9) | -0.3(7) |
C20 | 64.3(16) | 23.2(11) | 74.2(18) | -0.5(11) | 60.7(15) | 0.9(10) |
C17 | 34.6(11) | 14.8(9) | 30.3(11) | 0.1(7) | 24.9(10) | 5.3(8) |
C6 | 14.4(9) | 22.5(10) | 50.1(14) | -2.6(9) | 3.4(9) | -0.9(8) |
C15 | 38.4(12) | 33.2(12) | 30.0(12) | -6.2(9) | 12.6(10) | -5.8(10) |
C13 | 19.1(9) | 17.6(10) | 35.0(12) | -5.8(8) | 6.1(9) | -1.7(7) |
C16 | 41.8(12) | 18.0(9) | 38.8(12) | 8.0(8) | 27.7(10) | 4.4(9) |
C19 | 88(2) | 22.9(11) | 34.5(13) | 7.2(9) | 41.5(14) | 7.2(12) |
C10 | 46.0(16) | 37.2(14) | 53.5(17) | -5.8(12) | 26.8(14) | -5.6(12) |
C5 | 53.8(14) | 23.2(11) | 18.7(10) | -3.0(8) | 6.8(10) | 0.2(10) |
C9 | 32.1(12) | 34.7(12) | 56.4(15) | -0.6(11) | 28.7(12) | 0.1(9) |
C4 | 14.9(8) | 13.9(9) | 20.6(10) | -0.6(7) | 0.0(8) | 1.3(7) |
Li1 | 13.4(14) | 14.8(14) | 15.6(14) | 0.5(11) | 6.7(12) | 0.5(11) |
Li2 | 20.0(14) | 14.9(14) | 18.4(15) | 1.2(11) | 11.5(13) | 2.8(11) |
C11B | 22(2) | 31(3) | 45(3) | -5(2) | 19(3) | -3(2) |
C12B | 35(3) | 58(3) | 33(3) | -10(3) | 13(3) | -12(3) |
C14 | 33.4(14) | 25.1(13) | 55.2(18) | -6.8(12) | -17.1(13) | -2.3(10) |
C12 | 36(3) | 51(3) | 57(4) | 4(3) | 21(3) | -3(2) |
C11 | 31(3) | 46(3) | 54(4) | 7(3) | 22(3) | -5(3) |
O3 | 59(5) | 35(3) | 43(5) | 11(3) | 29(4) | 18(3) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
K1 | K21 | 3.723(3) | N1 | C3 | 1.471(3) | |
K1 | K2 | 3.709(4) | N1 | C1 | 1.459(2) | |
K1 | O4 | 2.8366(19) | N1 | Li1 | 2.172(3) | |
K1 | O2 | 2.861(2) | O3B | C9 | 1.439(10) | |
K1 | O1 | 2.623(3) | O3B | C11B | 1.370(10) | |
K1 | O3B | 2.781(8) | O3B | C11 | 1.702(11) | |
K1 | O51 | 2.643(3) | O5 | K11 | 2.643(3) | |
K1 | Li1 | 3.242(3) | O5 | C18 | 1.382(2) | |
K1 | Li21 | 3.277(3) | O5 | Li2 | 1.903(3) | |
K1 | C11B | 3.529(6) | C8 | K21 | 3.270(3) | |
K1 | O3 | 3.033(10) | C3 | C4 | 1.552(3) | |
K2 | K11 | 3.723(3) | C18 | C20 | 1.530(3) | |
K2 | K21 | 4.988(7) | C18 | C17 | 1.554(3) | |
K2 | O4 | 2.776(2) | C18 | C19 | 1.535(4) | |
K2 | O21 | 2.775(2) | C6 | C4 | 1.541(3) | |
K2 | O1 | 2.5993(19) | C13 | Li21 | 2.778(5) | |
K2 | O5 | 2.600(2) | C13 | C14 | 1.509(4) | |
K2 | C81 | 3.270(3) | C10 | C9 | 1.480(3) | |
K2 | Li1 | 3.058(3) | C5 | C4 | 1.539(4) | |
K2 | Li2 | 3.005(3) | C9 | O3 | 1.418(12) | |
O4 | C13 | 1.383(2) | Li1 | O21 | 1.929(3) | |
O4 | Li2 | 1.909(3) | Li1 | Li11 | 2.507(6) | |
O4 | Li21 | 1.945(4) | Li2 | K11 | 3.277(3) | |
O2 | K21 | 2.7748(19) | Li2 | O41 | 1.945(4) | |
O2 | C7 | 1.390(2) | Li2 | C131 | 2.778(5) | |
O2 | Li11 | 1.929(3) | Li2 | Li21 | 2.508(6) | |
O2 | Li1 | 1.949(4) | C11B | C12B | 1.518(7) | |
O1 | C4 | 1.379(2) | C11B | C12 | 1.529(8) | |
O1 | Li1 | 1.900(3) | C11B | C11 | 0.787(6) | |
N2 | C17 | 1.469(3) | C11B | O3 | 1.399(12) | |
N2 | C15 | 1.459(3) | C12B | C12 | 1.036(7) | |
N2 | C16 | 1.457(2) | C12B | C11 | 0.911(7) | |
N2 | Li2 | 2.176(3) | C12 | C11 | 1.440(8) | |
C7 | C8 | 1.523(3) | C11 | O3 | 1.526(13) | |
N1 | C2 | 1.464(3) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
K2 | K1 | K21 | 84.31(10) | C16 | N2 | C17 | 109.99(15) | |
O4 | K1 | K2 | 47.94(4) | C16 | N2 | C15 | 107.88(17) | |
O4 | K1 | K21 | 76.82(7) | C16 | N2 | Li2 | 115.91(16) | |
O4 | K1 | O2 | 106.08(7) | O2 | C7 | C8 | 113.28(16) | |
O4 | K1 | Li1 | 96.20(8) | C2 | N1 | C3 | 112.50(16) | |
O4 | K1 | Li21 | 36.21(8) | C2 | N1 | Li1 | 111.64(14) | |
O4 | K1 | C11B | 100.29(10) | C3 | N1 | Li1 | 98.30(13) | |
O4 | K1 | O3 | 122.4(2) | C1 | N1 | C2 | 107.96(16) | |
O2 | K1 | K21 | 47.67(4) | C1 | N1 | C3 | 109.48(14) | |
O2 | K1 | K2 | 77.79(7) | C1 | N1 | Li1 | 116.78(15) | |
O2 | K1 | Li1 | 36.57(8) | C9 | O3B | K1 | 130.6(5) | |
O2 | K1 | Li21 | 94.90(9) | C9 | O3B | C11 | 96.9(5) | |
O2 | K1 | C11B | 153.51(8) | C11B | O3B | K1 | 111.9(5) | |
O2 | K1 | O3 | 131.3(2) | C11B | O3B | C9 | 115.3(6) | |
O1 | K1 | K2 | 44.49(6) | C11B | O3B | C11 | 27.0(3) | |
O1 | K1 | K21 | 109.00(7) | C11 | O3B | K1 | 132.4(5) | |
O1 | K1 | O4 | 90.26(8) | K2 | O5 | K11 | 90.46(6) | |
O1 | K1 | O2 | 72.08(7) | C18 | O5 | K11 | 129.31(14) | |
O1 | K1 | O3B | 109.21(14) | C18 | O5 | K2 | 133.58(13) | |
O1 | K1 | O51 | 149.46(6) | C18 | O5 | Li2 | 115.11(15) | |
O1 | K1 | Li1 | 35.87(6) | Li2 | O5 | K11 | 90.75(14) | |
O1 | K1 | Li21 | 120.06(7) | Li2 | O5 | K2 | 82.14(11) | |
O1 | K1 | C11B | 110.79(10) | C7 | C8 | K21 | 87.55(12) | |
O1 | K1 | O3 | 101.88(16) | N1 | C3 | C4 | 115.16(14) | |
O3B | K1 | K21 | 137.20(18) | O5 | C18 | C20 | 111.02(17) | |
O3B | K1 | K2 | 137.67(19) | O5 | C18 | C17 | 110.07(15) | |
O3B | K1 | O4 | 121.35(19) | O5 | C18 | C19 | 110.82(19) | |
O3B | K1 | O2 | 132.4(2) | C20 | C18 | C17 | 105.60(16) | |
O3B | K1 | Li1 | 131.76(15) | C20 | C18 | C19 | 106.58(19) | |
O3B | K1 | Li21 | 120.40(15) | C19 | C18 | C17 | 112.58(17) | |
O3B | K1 | C11B | 21.1(2) | N2 | C17 | C18 | 115.19(15) | |
O3B | K1 | O3 | 7.3(3) | O4 | C13 | Li21 | 40.45(10) | |
O51 | K1 | K21 | 44.30(4) | O4 | C13 | C14 | 112.7(2) | |
O51 | K1 | K2 | 108.82(9) | C14 | C13 | Li21 | 150.86(17) | |
O51 | K1 | O4 | 71.16(9) | O3B | C9 | C10 | 107.3(4) | |
O51 | K1 | O2 | 89.59(7) | O3 | C9 | O3B | 18.0(4) | |
O51 | K1 | O3B | 101.21(15) | O3 | C9 | C10 | 110.0(5) | |
O51 | K1 | Li1 | 120.22(8) | O1 | C4 | C3 | 109.94(15) | |
O51 | K1 | Li21 | 35.49(6) | O1 | C4 | C6 | 110.45(17) | |
O51 | K1 | C11B | 96.58(11) | O1 | C4 | C5 | 110.81(17) | |
O51 | K1 | O3 | 108.51(16) | C6 | C4 | C3 | 105.21(15) | |
Li1 | K1 | K2 | 51.66(6) | C5 | C4 | C3 | 112.72(16) | |
Li1 | K1 | K21 | 76.00(8) | C5 | C4 | C6 | 107.53(17) | |
Li1 | K1 | Li21 | 107.81(9) | K2 | Li1 | K1 | 72.07(9) | |
Li1 | K1 | C11B | 142.91(10) | O2 | Li1 | K1 | 61.02(9) | |
Li21 | K1 | K2 | 75.73(7) | O21 | Li1 | K1 | 115.18(12) | |
Li21 | K1 | K21 | 50.35(6) | O2 | Li1 | K2 | 111.19(13) | |
Li21 | K1 | C11B | 105.06(12) | O21 | Li1 | K2 | 62.92(9) | |
C11B | K1 | K21 | 140.12(10) | O21 | Li1 | O2 | 94.54(14) | |
C11B | K1 | K2 | 123.59(10) | O21 | Li1 | N1 | 119.66(15) | |
O3 | K1 | K21 | 143.7(2) | O2 | Li1 | N1 | 123.37(15) | |
O3 | K1 | K2 | 131.9(2) | O21 | Li1 | Li11 | 50.07(13) | |
O3 | K1 | Li1 | 125.61(17) | O2 | Li1 | Li11 | 49.36(11) | |
O3 | K1 | Li21 | 126.17(18) | O1 | Li1 | K1 | 53.99(10) | |
O3 | K1 | C11B | 23.1(2) | O1 | Li1 | K2 | 57.73(9) | |
K1 | K2 | K11 | 95.69(10) | O1 | Li1 | O2 | 114.25(16) | |
K11 | K2 | K21 | 47.73(4) | O1 | Li1 | O21 | 119.87(17) | |
K1 | K2 | K21 | 47.96(7) | O1 | Li1 | N1 | 87.61(13) | |
O4 | K2 | K1 | 49.34(5) | O1 | Li1 | Li11 | 149.58(10) | |
O4 | K2 | K11 | 84.66(7) | N1 | Li1 | K1 | 123.79(13) | |
O4 | K2 | K21 | 55.98(6) | N1 | Li1 | K2 | 124.06(14) | |
O4 | K2 | C81 | 146.94(5) | N1 | Li1 | Li11 | 122.72(9) | |
O4 | K2 | Li1 | 101.85(10) | Li11 | Li1 | K1 | 101.09(12) | |
O4 | K2 | Li2 | 38.30(7) | Li11 | Li1 | K2 | 100.90(11) | |
O21 | K2 | K1 | 84.69(7) | K2 | Li2 | K11 | 72.54(9) | |
O21 | K2 | K11 | 49.66(4) | O4 | Li2 | K11 | 114.87(13) | |
O21 | K2 | K21 | 56.89(4) | O41 | Li2 | K11 | 59.47(9) | |
O21 | K2 | O4 | 112.86(9) | O41 | Li2 | K2 | 111.46(13) | |
O21 | K2 | C81 | 46.60(7) | O4 | Li2 | K2 | 64.36(9) | |
O21 | K2 | Li1 | 38.23(7) | O4 | Li2 | O41 | 93.95(14) | |
O21 | K2 | Li2 | 103.17(9) | O41 | Li2 | N2 | 129.13(16) | |
O1 | K2 | K1 | 45.00(4) | O4 | Li2 | N2 | 115.19(15) | |
O1 | K2 | K11 | 117.65(8) | O4 | Li2 | C131 | 118.21(16) | |
O1 | K2 | K21 | 79.92(6) | O41 | Li2 | C131 | 27.47(8) | |
O1 | K2 | O4 | 92.10(6) | O4 | Li2 | Li21 | 50.04(11) | |
O1 | K2 | O21 | 76.05(7) | O41 | Li2 | Li21 | 48.78(13) | |
O1 | K2 | O5 | 159.77(5) | N2 | Li2 | K11 | 127.87(13) | |
O1 | K2 | C81 | 103.88(7) | N2 | Li2 | K2 | 118.50(14) | |
O1 | K2 | Li1 | 38.17(6) | N2 | Li2 | C131 | 103.81(13) | |
O1 | K2 | Li2 | 127.08(8) | N2 | Li2 | Li21 | 123.63(10) | |
O5 | K2 | K1 | 118.41(6) | O5 | Li2 | K11 | 53.76(10) | |
O5 | K2 | K11 | 45.23(5) | O5 | Li2 | K2 | 59.01(10) | |
O5 | K2 | K21 | 79.86(4) | O5 | Li2 | O4 | 122.92(16) | |
O5 | K2 | O4 | 76.96(6) | O5 | Li2 | O41 | 112.11(18) | |
O5 | K2 | O21 | 92.39(7) | O5 | Li2 | N2 | 86.82(14) | |
O5 | K2 | C81 | 78.51(8) | O5 | Li2 | C131 | 104.42(16) | |
O5 | K2 | Li1 | 126.94(7) | O5 | Li2 | Li21 | 149.46(11) | |
O5 | K2 | Li2 | 38.85(7) | C131 | Li2 | K11 | 63.16(8) | |
C81 | K2 | K11 | 62.31(7) | C131 | Li2 | K2 | 131.73(12) | |
C81 | K2 | K1 | 130.46(5) | Li21 | Li2 | K11 | 99.42(12) | |
C81 | K2 | K21 | 98.08(6) | Li21 | Li2 | K2 | 102.21(11) | |
Li1 | K2 | K1 | 56.27(7) | Li21 | Li2 | C131 | 68.75(17) | |
Li1 | K2 | K11 | 81.70(7) | O3B | C11B | K1 | 47.0(4) | |
Li1 | K2 | K21 | 59.03(7) | O3B | C11B | C12B | 112.5(5) | |
Li1 | K2 | C81 | 76.02(8) | O3B | C11B | C12 | 123.0(5) | |
Li2 | K2 | K11 | 57.11(7) | O3B | C11B | O3 | 18.6(5) | |
Li2 | K2 | K1 | 82.08(8) | C12B | C11B | K1 | 124.4(3) | |
Li2 | K2 | K21 | 59.08(7) | C12B | C11B | C12 | 39.7(3) | |
Li2 | K2 | C81 | 113.08(9) | C12 | C11B | K1 | 101.2(3) | |
Li2 | K2 | Li1 | 118.11(11) | C11 | C11B | K1 | 135.1(6) | |
K2 | O4 | K1 | 82.71(7) | C11 | C11B | O3B | 100.6(7) | |
C13 | O4 | K1 | 92.04(12) | C11 | C11B | C12B | 28.8(6) | |
C13 | O4 | K2 | 115.95(12) | C11 | C11B | C12 | 68.5(7) | |
C13 | O4 | Li2 | 130.10(15) | C11 | C11B | O3 | 83.6(7) | |
C13 | O4 | Li21 | 112.08(15) | O3 | C11B | K1 | 58.1(4) | |
Li2 | O4 | K1 | 137.83(10) | O3 | C11B | C12B | 94.0(5) | |
Li21 | O4 | K1 | 84.32(12) | O3 | C11B | C12 | 109.6(6) | |
Li21 | O4 | K2 | 130.49(11) | C12 | C12B | C11B | 70.7(5) | |
Li2 | O4 | K2 | 77.34(10) | C11 | C12B | C11B | 24.6(5) | |
Li2 | O4 | Li21 | 81.17(15) | C11 | C12B | C12 | 95.2(7) | |
K21 | O2 | K1 | 82.67(7) | C12B | C12 | C11B | 69.5(5) | |
C7 | O2 | K1 | 91.68(11) | C12B | C12 | C11 | 39.0(4) | |
C7 | O2 | K21 | 112.55(12) | C11 | C12 | C11B | 30.5(3) | |
C7 | O2 | Li1 | 114.73(15) | C11B | C11 | O3B | 52.3(6) | |
C7 | O2 | Li11 | 131.67(14) | C11B | C11 | C12B | 126.6(10) | |
Li1 | O2 | K1 | 82.41(10) | C11B | C11 | C12 | 81.0(7) | |
Li11 | O2 | K1 | 136.61(10) | C11B | C11 | O3 | 65.6(6) | |
Li11 | O2 | K21 | 78.85(11) | C12B | C11 | O3B | 131.4(7) | |
Li1 | O2 | K21 | 130.58(10) | C12B | C11 | C12 | 45.7(5) | |
Li11 | O2 | Li1 | 80.57(14) | C12B | C11 | O3 | 120.1(7) | |
K2 | O1 | K1 | 90.51(7) | C12 | C11 | O3B | 108.2(5) | |
C4 | O1 | K1 | 134.25(12) | C12 | C11 | O3 | 107.6(6) | |
C4 | O1 | K2 | 128.08(13) | O3 | C11 | O3B | 14.7(4) | |
C4 | O1 | Li1 | 114.45(14) | C9 | O3 | K1 | 116.3(5) | |
Li1 | O1 | K1 | 90.14(12) | C9 | O3 | C11 | 106.3(7) | |
Li1 | O1 | K2 | 84.10(12) | C11B | O3 | K1 | 98.8(5) | |
C17 | N2 | Li2 | 96.40(13) | C11B | O3 | C9 | 114.9(8) | |
C15 | N2 | C17 | 112.62(18) | C11B | O3 | C11 | 30.8(3) | |
C15 | N2 | Li2 | 113.76(15) | C11 | O3 | K1 | 126.3(6) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
K1 | O4 | C13 | Li21 | -84.70(13) | C9 | O3B | C11B | O3 | 74(2) | |
K1 | O4 | C13 | C14 | 81.0(2) | C9 | O3B | C11 | C11B | -135.4(8) | |
K1 | O2 | C7 | C8 | 81.33(16) | C9 | O3B | C11 | C12B | 115.7(10) | |
K1 | O1 | C4 | C3 | 91.66(18) | C9 | O3B | C11 | C12 | 162.1(5) | |
K1 | O1 | C4 | C6 | -24.0(2) | C9 | O3B | C11 | O3 | 72(3) | |
K1 | O1 | C4 | C5 | -143.06(14) | C4 | O1 | Li1 | K1 | 140.15(14) | |
K1 | O1 | Li1 | K2 | 90.50(7) | C4 | O1 | Li1 | K2 | -129.35(15) | |
K1 | O1 | Li1 | O21 | 100.90(17) | C4 | O1 | Li1 | O21 | -118.95(19) | |
K1 | O1 | Li1 | O2 | -10.12(14) | C4 | O1 | Li1 | O2 | 130.02(16) | |
K1 | O1 | Li1 | N1 | -135.92(9) | C4 | O1 | Li1 | N1 | 4.22(16) | |
K1 | O1 | Li1 | Li11 | 39.8(4) | C4 | O1 | Li1 | Li11 | 180.0(4) | |
K1 | O3B | C9 | C10 | 18.7(5) | Li11 | O2 | C7 | C8 | -96.6(2) | |
K1 | O3B | C9 | O3 | 120(3) | Li1 | O2 | C7 | C8 | 163.75(15) | |
K1 | O3B | C11B | C12B | -116.8(4) | Li1 | O1 | C4 | C3 | -24.9(2) | |
K1 | O3B | C11B | C12 | -73.1(6) | Li1 | O1 | C4 | C6 | -140.54(17) | |
K1 | O3B | C11B | C11 | -144.2(7) | Li1 | O1 | C4 | C5 | 100.40(18) | |
K1 | O3B | C11B | O3 | -121(3) | Li1 | N1 | C3 | C4 | -35.94(18) | |
K1 | O3B | C11 | C11B | 47.3(8) | Li2 | O4 | C13 | Li21 | 97.2(2) | |
K1 | O3B | C11 | C12B | -61.6(11) | Li2 | O4 | C13 | C14 | -97.1(3) | |
K1 | O3B | C11 | C12 | -15.2(8) | Li21 | O4 | C13 | C14 | 165.7(2) | |
K1 | O3B | C11 | O3 | -105(3) | Li2 | N2 | C17 | C18 | -41.9(2) | |
K11 | O5 | C18 | C20 | -15.7(2) | Li2 | O5 | C18 | C20 | -129.40(18) | |
K11 | O5 | C18 | C17 | 100.89(17) | Li2 | O5 | C18 | C17 | -12.8(2) | |
K11 | O5 | C18 | C19 | -133.92(15) | Li2 | O5 | C18 | C19 | 112.36(19) | |
K1 | C11B | C12B | C12 | 62.8(5) | C11B | O3B | C9 | C10 | -179.3(5) | |
K1 | C11B | C12B | C11 | -122.5(11) | C11B | O3B | C9 | O3 | -78(2) | |
K1 | C11B | C12 | C12B | -131.6(5) | C11B | O3B | C11 | C12B | -108.9(13) | |
K1 | C11B | C12 | C11 | -134.3(6) | C11B | O3B | C11 | C12 | -62.5(7) | |
K1 | C11B | C11 | O3B | -37.3(7) | C11B | O3B | C11 | O3 | -152(3) | |
K1 | C11B | C11 | C12B | 80.6(13) | C11B | C12B | C12 | C11 | 2.2(5) | |
K1 | C11B | C11 | C12 | 84.2(8) | C11B | C12B | C11 | O3B | 68.9(10) | |
K1 | C11B | C11 | O3 | -29.9(8) | C11B | C12B | C11 | C12 | -5.0(12) | |
K1 | C11B | O3 | C9 | -124.5(6) | C11B | C12B | C11 | O3 | 80.6(11) | |
K1 | C11B | O3 | C11 | 155.5(7) | C11B | C12 | C11 | O3B | 45.3(5) | |
K2 | O4 | C13 | Li21 | -167.59(16) | C11B | C12 | C11 | C12B | 176.0(10) | |
K2 | O4 | C13 | C14 | -1.9(2) | C11B | C12 | C11 | O3 | 60.7(6) | |
K21 | O2 | C7 | C8 | -1.43(18) | C11B | C11 | O3 | K1 | 30.5(8) | |
K2 | O1 | C4 | C3 | -127.16(14) | C11B | C11 | O3 | C9 | -111.5(7) | |
K2 | O1 | C4 | C6 | 117.17(16) | C12B | C11B | C12 | C11 | -2.7(6) | |
K2 | O1 | C4 | C5 | -1.9(2) | C12B | C11B | C11 | O3B | -117.9(10) | |
K2 | O1 | Li1 | K1 | -90.50(7) | C12B | C11B | C11 | C12 | 3.6(9) | |
K2 | O1 | Li1 | O21 | 10.40(15) | C12B | C11B | C11 | O3 | -110.5(10) | |
K2 | O1 | Li1 | O2 | -100.62(15) | C12B | C11B | O3 | K1 | -128.6(4) | |
K2 | O1 | Li1 | N1 | 133.58(10) | C12B | C11B | O3 | C9 | 106.9(6) | |
K2 | O1 | Li1 | Li11 | -50.7(4) | C12B | C11B | O3 | C11 | 26.9(6) | |
K2 | O5 | C18 | C20 | 126.87(17) | C12B | C12 | C11 | O3B | -130.7(8) | |
K2 | O5 | C18 | C17 | -116.57(17) | C12B | C12 | C11 | C11B | -176.0(10) | |
K2 | O5 | C18 | C19 | 8.6(2) | C12B | C12 | C11 | O3 | -115.2(8) | |
O2 | C7 | C8 | K21 | 1.12(14) | C12B | C11 | O3 | K1 | -89.1(9) | |
N1 | C3 | C4 | O1 | 44.0(2) | C12B | C11 | O3 | C9 | 128.9(8) | |
N1 | C3 | C4 | C6 | 162.91(16) | C12B | C11 | O3 | C11B | -119.6(11) | |
N1 | C3 | C4 | C5 | -80.2(2) | C12 | C11B | C12B | C11 | 174.8(13) | |
O3B | C9 | O3 | K1 | -42(2) | C12 | C11B | C11 | O3B | -121.5(6) | |
O3B | C9 | O3 | C11B | 73(2) | C12 | C11B | C11 | C12B | -3.6(9) | |
O3B | C9 | O3 | C11 | 104(2) | C12 | C11B | C11 | O3 | -114.1(6) | |
O3B | C11B | C12B | C12 | 115.1(7) | C12 | C11B | O3 | K1 | -91.2(4) | |
O3B | C11B | C12B | C11 | -70.1(11) | C12 | C11B | O3 | C9 | 144.3(5) | |
O3B | C11B | C12 | C12B | -86.2(7) | C12 | C11B | O3 | C11 | 64.4(7) | |
O3B | C11B | C12 | C11 | -88.9(8) | C12 | C12B | C11 | O3B | 73.9(10) | |
O3B | C11B | C11 | C12B | 117.9(10) | C12 | C12B | C11 | C11B | 5.0(12) | |
O3B | C11B | C11 | C12 | 121.5(6) | C12 | C12B | C11 | O3 | 85.6(9) | |
O3B | C11B | C11 | O3 | 7.4(8) | C12 | C11 | O3 | K1 | -40.6(8) | |
O3B | C11B | O3 | K1 | 48(2) | C12 | C11 | O3 | C9 | 177.4(5) | |
O3B | C11B | O3 | C9 | -77(2) | C12 | C11 | O3 | C11B | -71.1(7) | |
O3B | C11B | O3 | C11 | -157(3) | C11 | O3B | C9 | C10 | -158.7(3) | |
O3B | C11 | O3 | K1 | 54(3) | C11 | O3B | C9 | O3 | -57(2) | |
O3B | C11 | O3 | C9 | -88(3) | C11 | O3B | C11B | K1 | 144.2(7) | |
O3B | C11 | O3 | C11B | 24(3) | C11 | O3B | C11B | C12B | 27.5(6) | |
O5 | C18 | C17 | N2 | 41.2(2) | C11 | O3B | C11B | C12 | 71.1(7) | |
C2 | N1 | C3 | C4 | 81.69(19) | C11 | O3B | C11B | O3 | 24(3) | |
C1 | N1 | C3 | C4 | -158.27(16) | C11 | C11B | C12B | C12 | -174.8(13) | |
C20 | C18 | C17 | N2 | 161.06(17) | C11 | C11B | C12 | C12B | 2.7(6) | |
C15 | N2 | C17 | C18 | 77.2(2) | C11 | C11B | O3 | K1 | -155.5(7) | |
C16 | N2 | C17 | C18 | -162.48(17) | C11 | C11B | O3 | C9 | 80.0(8) | |
C19 | C18 | C17 | N2 | -83.0(2) | C11 | C12B | C12 | C11B | -2.2(5) | |
C10 | C9 | O3 | K1 | 42.5(5) | O3 | C11B | C12B | C12 | 116.3(7) | |
C10 | C9 | O3 | C11B | 157.2(5) | O3 | C11B | C12B | C11 | -68.9(11) | |
C10 | C9 | O3 | C11 | -171.1(4) | O3 | C11B | C12 | C12B | -71.7(7) | |
C9 | O3B | C11B | K1 | -165.3(7) | O3 | C11B | C12 | C11 | -74.4(7) | |
C9 | O3B | C11B | C12B | 77.9(7) | O3 | C11B | C11 | O3B | -7.4(8) | |
C9 | O3B | C11B | C12 | 121.6(6) | O3 | C11B | C11 | C12B | 110.5(10) | |
C9 | O3B | C11B | C11 | 50.5(9) | O3 | C11B | C11 | C12 | 114.1(6) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H2A | 4055 | 6788 | 5604 | 42 |
H2B | 4484 | 7658 | 6162 | 42 |
H2C | 3706 | 7822 | 5569 | 42 |
H3A | 2888 | 7009 | 5651 | 23 |
H3B | 3032 | 6601 | 6429 | 23 |
H1A | 4398 | 8037 | 7168 | 36 |
H1B | 3830 | 7556 | 7282 | 36 |
H1C | 3628 | 8320 | 6621 | 36 |
H20A | 6320 | 3032 | 6029 | 63 |
H20B | 6437 | 1902 | 5901 | 63 |
H20C | 6650 | 2280 | 6712 | 63 |
H6A | 2337 | 4471 | 5462 | 53 |
H6B | 2070 | 5586 | 5309 | 53 |
H6C | 2440 | 5154 | 6132 | 53 |
H15A | 4324 | 1107 | 5476 | 54 |
H15B | 4190 | 185 | 5857 | 54 |
H15C | 4576 | 28 | 5420 | 54 |
H16A | 5419 | -766 | 6567 | 44 |
H16B | 4992 | -463 | 6935 | 44 |
H16C | 5760 | -138 | 7316 | 44 |
H19A | 4674 | 2136 | 5099 | 66 |
H19B | 5233 | 1766 | 4928 | 66 |
H19C | 5179 | 2914 | 5072 | 66 |
H10A | 2573(15) | 5410(20) | 7562(17) | 68 |
H5A | 3507 | 5589 | 5102 | 56 |
H5B | 2737 | 5917 | 4689 | 56 |
H5C | 2931 | 4771 | 4830 | 56 |
H9AA | 2303 | 3655 | 8086 | 46 |
H9AB | 1787 | 4232 | 7340 | 46 |
H9BC | 2418 | 3576 | 8079 | 46 |
H9BD | 1784 | 4208 | 7487 | 46 |
H11A | 2152 | 2323 | 7308 | 39 |
H11B | 2542 | 2319 | 6868 | 39 |
H12A | 1655 | 3279 | 5915 | 66 |
H12B | 1258 | 3188 | 6346 | 66 |
H12C | 1400 | 2222 | 6010 | 66 |
H8A | 5067(11) | 5405(16) | 9406(12) | 26(5) |
H8B | 4335(11) | 5698(16) | 9231(11) | 28(6) |
H7A | 4569(10) | 6504(16) | 8418(11) | 20(5) |
H7B | 3933(10) | 5795(14) | 7964(10) | 18(5) |
H8C | 4460(11) | 4628(18) | 8965(12) | 35(6) |
H13A | 3754(10) | 1027(15) | 6530(11) | 22(5) |
H13B | 3483(12) | 1753(18) | 6915(13) | 43(7) |
H14A | 2799(16) | 1780(20) | 5621(17) | 72(9) |
H14B | 3145(14) | 2830(20) | 5877(15) | 56(8) |
H14C | 3402(19) | 2060(30) | 5510(20) | 104(15) |
H12D | 1833 | 3068 | 5795 | 74 |
H12E | 1589 | 1996 | 5877 | 74 |
H12F | 2370 | 2264 | 6325 | 74 |
H11C | 1961 | 2335 | 7105 | 52 |
H11D | 1397 | 3109 | 6564 | 52 |
H17A | 5688(11) | 537(17) | 5927(12) | 31(6) |
H17B | 6097(11) | 913(15) | 6760(12) | 24(5) |
H10B | 3114(16) | 4860(20) | 8309(16) | 63(9) |
H10C | 2516(16) | 5320(30) | 8316(18) | 81(10) |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
O3B | 0.5 | H9AA | 0.5 | H9AB | 0.5 | ||
H9BC | 0.5 | H9BD | 0.5 | C11B | 0.5 | ||
H11A | 0.5 | H11B | 0.5 | C12B | 0.5 | ||
H12A | 0.5 | H12B | 0.5 | H12C | 0.5 | ||
C12 | 0.5 | H12D | 0.5 | H12E | 0.5 | ||
H12F | 0.5 | C11 | 0.5 | H11C | 0.5 | ||
H11D | 0.5 | O3 | 0.5 |
Experimental
Single crystals of C20H48K2Li2N2O5 [C2c] 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 SIR2004 [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [C2c]
Crystal Data for C20H48K2Li2N2O5 (M =488.68 g/mol): monoclinic, space group C2/c (no. 15), a = 23.29(2) Å, b = 13.532(9) Å, c = 21.12(3) Å, β = 121.01(3)°, V = 5705(10) Å3, Z = 8, T = 100.01 K, μ(MoKα) = 0.360 mm-1, Dcalc = 1.138 g/cm3, 6223 reflections measured (4.902° ≤ 2Θ ≤ 53.998°), 6223 unique (Rint = ?, Rsigma = 0.0265) which were used in all calculations. The final R1 was 0.0428 (I > 2σ(I)) and wR2 was 0.0907 (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, All C(H,H,H,H) groups
At 1.5 times of:
All C(H) groups, All C(H,H,H) groups
2. Others
Fixed Sof: O3B(0.5) H9AA(0.5) H9AB(0.5) H9BC(0.5) H9BD(0.5) C11B(0.5)
H11A(0.5) H11B(0.5) C12B(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C12(0.5) H12D(0.5)
H12E(0.5) H12F(0.5) C11(0.5) H11C(0.5) H11D(0.5) O3(0.5)
3.a Secondary CH2 refined with riding coordinates:
C3(H3A,H3B), C9(H9AA,H9AB), C9(H9BC,H9BD), C11B(H11A,H11B), C11(H11C,H11D)
3.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C6(H6A,H6B,H6C),
C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C5(H5A,H5B,H5C),
C12B(H12A,H12B,H12C), C12(H12D,H12E,H12F)
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.