Identification code | cu_B0490_0m |
Empirical formula | C28H64Li5N3O8 |
Formula weight | 605.52 |
Temperature/K | 99.99 |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 18.2841(8) |
b/Å | 9.1092(4) |
c/Å | 24.3776(10) |
α/° | 90 |
β/° | 111.387(2) |
γ/° | 90 |
Volume/Å3 | 3780.6(3) |
Z | 4 |
ρcalcg/cm3 | 1.064 |
μ/mm‑1 | 0.586 |
F(000) | 1328.0 |
Crystal size/mm3 | 0.35 × 0.2 × 0.19 |
Radiation | CuKα (λ = 1.54178) |
2Θ range for data collection/° | 5.19 to 135.984 |
Index ranges | -21 ≤ h ≤ 21, -10 ≤ k ≤ 10, -29 ≤ l ≤ 29 |
Reflections collected | 63345 |
Independent reflections | 6869 [Rint = 0.1315, Rsigma = 0.0627] |
Data/restraints/parameters | 6869/6/431 |
Goodness-of-fit on F2 | 1.032 |
Final R indexes [I>=2σ (I)] | R1 = 0.0792, wR2 = 0.2108 |
Final R indexes [all data] | R1 = 0.1013, wR2 = 0.2261 |
Largest diff. peak/hole / e Å-3 | 0.74/-0.36 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
C1 | 708.4(19) | 7087(4) | 2546.3(13) | 57.9(8) |
C2 | 544(2) | 5842(4) | 2110.8(14) | 61.1(8) |
C3 | 1036(3) | 4514(5) | 1489(2) | 92.2(14) |
C4 | 2117.4(19) | 7526(4) | 2966.7(14) | 57.0(8) |
C5 | 2878.0(19) | 6883(4) | 3370.2(15) | 62.3(9) |
C6 | 3096(3) | 4759(5) | 2883(2) | 89.2(14) |
C7 | 1366.1(18) | 7473(3) | 3615.4(13) | 47.7(7) |
C8 | 1164.9(16) | 6290(3) | 3989.3(12) | 44.0(6) |
C9 | 1199.8(19) | 7017(3) | 4561.9(13) | 53.6(7) |
C10 | 340.5(17) | 5667(4) | 3669.3(14) | 54.7(8) |
C11 | 1548(2) | 2418(4) | 3142.7(14) | 56.0(8) |
C12 | 2334.7(18) | 1038(3) | 4838.0(13) | 47.5(7) |
C13 | 1622.2(19) | 1299(3) | 4989.8(13) | 52.3(8) |
C14 | 327(2) | 2255(5) | 4600(2) | 79.4(11) |
C15 | 3236.3(18) | 2144(3) | 4459.2(12) | 46.2(7) |
C16 | 3972.1(18) | 1358(3) | 4851.2(13) | 49.6(7) |
C17 | 4927.6(18) | 1432(3) | 5822.6(13) | 52.3(7) |
C19 | 2917(2) | 7466(3) | 6676.0(14) | 58.4(8) |
C20 | 2141(2) | 6922(4) | 6257.0(15) | 64.0(9) |
C21 | 1865(3) | 4774(5) | 6720(2) | 91.0(14) |
C22 | 4308.4(19) | 6840(3) | 7099.5(13) | 53.6(8) |
C23 | 4414.8(19) | 5540(3) | 7503.6(13) | 50.0(7) |
C24 | 3810(2) | 4219(4) | 8045.6(15) | 65.8(9) |
C25 | 3687(2) | 7393(3) | 6039.2(12) | 48.3(7) |
C26 | 3857.3(17) | 6217(3) | 5650.0(12) | 41.4(6) |
C27 | 4669.7(17) | 5528(3) | 5955.4(13) | 49.0(7) |
C28 | 3837(2) | 6968(3) | 5081.6(13) | 53.2(8) |
Li1 | 1855(3) | 4702(6) | 3377(2) | 52.4(12) |
Li2 | 1585(3) | 3027(5) | 4029(2) | 47.5(11) |
Li3 | 2519(3) | 4618(5) | 4792.7(19) | 41.7(10) |
Li4 | 3419(3) | 3039(5) | 5571.2(19) | 40.6(10) |
Li5 | 3093(3) | 4640(5) | 6221(2) | 46.3(11) |
N1 | 1436.1(14) | 6881(3) | 3071.8(10) | 48.2(6) |
N2 | 2648.2(14) | 2417(2) | 4719.2(9) | 39.6(5) |
N3 | 3585.4(14) | 6768(2) | 6569.2(10) | 45.4(6) |
O1 | 1116.3(15) | 5797(3) | 1842.3(10) | 68.3(7) |
O2 | 2889.6(14) | 5326(3) | 3343.0(11) | 66.7(6) |
O3 | 1720.2(11) | 5156(2) | 4107.0(8) | 41.6(4) |
O4 | 1014.8(13) | 1921(2) | 4487.6(9) | 57.5(6) |
O5 | 4284.0(11) | 2143(2) | 5393.6(8) | 45.8(5) |
O6 | 2091.1(14) | 5355(3) | 6269.4(11) | 66.2(6) |
O7 | 3838.3(13) | 5565(2) | 7767.1(9) | 56.9(6) |
O8 | 3271.3(10) | 5139.8(18) | 5516.0(7) | 36.8(4) |
C18 | 3352(2) | 2335(3) | 6413.4(14) | 51.6(7) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
C1 | 53.3(19) | 64(2) | 52.0(17) | 11.2(15) | 14.2(15) | 0.3(15) |
C2 | 56(2) | 69(2) | 53.7(17) | 3.5(15) | 14.1(15) | -13.7(16) |
C3 | 123(4) | 81(3) | 84(3) | -23(2) | 52(3) | -35(3) |
C4 | 62(2) | 61(2) | 50.8(16) | 8.2(14) | 24.2(15) | -14.5(15) |
C5 | 46.5(18) | 87(3) | 56.0(18) | 13.9(17) | 21.4(15) | -10.8(17) |
C6 | 96(3) | 81(3) | 122(4) | 34(2) | 76(3) | 27(2) |
C7 | 46.7(17) | 41.6(15) | 53.6(16) | 6.6(12) | 16.7(14) | 3.3(12) |
C8 | 44.3(16) | 41.8(15) | 47.7(15) | 2.5(12) | 18.7(13) | 4.9(12) |
C9 | 60.1(19) | 50.5(17) | 56.4(17) | 3.3(14) | 28.6(15) | 7.3(14) |
C10 | 40.6(17) | 61.0(19) | 63.5(18) | 9.3(15) | 20.3(14) | 1.5(14) |
C11 | 54(2) | 66(2) | 47.4(16) | 0.1(15) | 18.4(15) | -5.2(16) |
C12 | 63.2(19) | 31.2(14) | 50.3(15) | -5.8(11) | 23.4(14) | -6.2(13) |
C13 | 67(2) | 43.9(16) | 51.1(16) | 0.9(13) | 27.1(15) | -13.3(14) |
C14 | 66(2) | 88(3) | 100(3) | 17(2) | 49(2) | -6(2) |
C15 | 57.4(18) | 47.1(16) | 39.1(13) | -4.5(12) | 23.6(13) | 1.9(13) |
C16 | 62.0(19) | 40.4(15) | 53.7(16) | -8.7(12) | 29.9(15) | 5.1(13) |
C17 | 50.2(18) | 50.9(17) | 57.1(17) | 8.4(14) | 20.9(14) | 10.6(14) |
C19 | 80(2) | 47.5(18) | 51.9(17) | -11.1(13) | 29.5(17) | 12.9(16) |
C20 | 64(2) | 74(2) | 57.9(18) | -8.3(16) | 27.0(17) | 22.0(18) |
C21 | 76(3) | 102(3) | 117(3) | -34(3) | 62(3) | -22(2) |
C22 | 63(2) | 48.1(17) | 50.6(16) | -12.3(13) | 21.4(15) | -11.0(14) |
C23 | 55.3(18) | 47.3(17) | 49.4(16) | -5.1(12) | 21.4(14) | -0.9(13) |
C24 | 68(2) | 67(2) | 65(2) | 4.8(17) | 27.4(18) | -6.7(18) |
C25 | 68(2) | 29.8(14) | 50.4(15) | -4.0(11) | 25.3(15) | -6.3(13) |
C26 | 55.1(17) | 28.5(13) | 45.5(14) | -2.6(11) | 24.2(13) | -7.5(11) |
C27 | 49.7(17) | 46.3(16) | 53.7(16) | -3.0(13) | 22.3(14) | -8.5(13) |
C28 | 76(2) | 38.8(15) | 53.2(16) | 1.9(13) | 33.9(16) | -7.4(14) |
Li1 | 53(3) | 58(3) | 52(3) | 2(2) | 26(2) | -3(2) |
Li2 | 49(3) | 51(3) | 44(2) | -3(2) | 19(2) | -8(2) |
Li3 | 45(3) | 35(2) | 46(2) | 0.6(18) | 18(2) | 3.0(18) |
Li4 | 49(3) | 35(2) | 43(2) | -2.5(18) | 23(2) | 2.8(19) |
Li5 | 57(3) | 40(2) | 53(3) | -5(2) | 33(2) | -1(2) |
N1 | 45.2(14) | 54.2(15) | 44.0(12) | 5.9(10) | 14.6(11) | -4.4(11) |
N2 | 50.6(14) | 30.6(11) | 42.6(11) | -3.5(9) | 23.1(10) | -1.2(9) |
N3 | 57.0(15) | 37.1(12) | 44.8(12) | -9(1) | 21.8(11) | -1.4(10) |
O1 | 82.2(17) | 69.4(15) | 59.7(13) | -9.4(11) | 33.5(12) | -26.8(13) |
O2 | 60.1(14) | 77.6(17) | 73.2(15) | 14.7(12) | 37.4(12) | 1.3(12) |
O3 | 42.2(11) | 40.2(10) | 44.1(10) | 3.8(8) | 17.8(8) | 2.7(8) |
O4 | 55.1(13) | 64.7(14) | 60.3(12) | 4.7(10) | 30.0(11) | -10.1(11) |
O5 | 54.6(12) | 37.9(10) | 46.3(10) | -0.6(8) | 20.1(9) | 10.4(9) |
O6 | 63.5(15) | 74.7(16) | 73.5(15) | -11.8(12) | 40.3(12) | 2.3(12) |
O7 | 65.4(14) | 56.6(13) | 54.8(12) | 1.7(10) | 29.2(11) | 5.1(10) |
O8 | 45.3(10) | 27.5(9) | 40.7(9) | -3.2(7) | 19.4(8) | -1.8(7) |
C18 | 62(2) | 48.2(17) | 50.5(16) | -5.1(13) | 28.0(16) | -4.2(15) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
C1 | C2 | 1.507(5) | C24 | O7 | 1.411(4) | |
C1 | N1 | 1.484(4) | C25 | C26 | 1.536(4) | |
C2 | O1 | 1.422(4) | C25 | N3 | 1.484(4) | |
C3 | O1 | 1.427(5) | C26 | C27 | 1.532(4) | |
C4 | C5 | 1.499(5) | C26 | C28 | 1.534(4) | |
C4 | N1 | 1.481(4) | C26 | O8 | 1.401(3) | |
C5 | O2 | 1.420(4) | Li1 | Li2 | 2.383(7) | |
C6 | O2 | 1.405(5) | Li1 | Li3 | 3.215(7) | |
C7 | C8 | 1.540(4) | Li1 | N1 | 2.160(6) | |
C7 | N1 | 1.479(4) | Li1 | O2 | 2.005(6) | |
C8 | C9 | 1.525(4) | Li1 | O3 | 1.929(5) | |
C8 | C10 | 1.531(4) | Li2 | Li3 | 2.483(6) | |
C8 | O3 | 1.403(3) | Li2 | N2 | 2.129(5) | |
C11 | Li1 | 2.176(6) | Li2 | O3 | 1.955(5) | |
C11 | Li2 | 2.208(6) | Li2 | O4 | 2.049(5) | |
C12 | C13 | 1.497(4) | Li3 | Li4 | 2.471(6) | |
C12 | N2 | 1.453(3) | Li3 | Li5 | 3.249(6) | |
C13 | O4 | 1.436(4) | Li3 | N2 | 2.035(5) | |
C14 | O4 | 1.415(4) | Li3 | O3 | 1.840(5) | |
C15 | C16 | 1.516(4) | Li3 | O8 | 1.859(5) | |
C15 | N2 | 1.455(3) | Li4 | Li5 | 2.383(6) | |
C16 | O5 | 1.426(3) | Li4 | N2 | 2.118(5) | |
C17 | O5 | 1.414(3) | Li4 | O5 | 1.963(5) | |
C19 | C20 | 1.498(5) | Li4 | O8 | 1.931(5) | |
C19 | N3 | 1.483(4) | Li4 | C18 | 2.197(5) | |
C20 | O6 | 1.431(4) | Li5 | N3 | 2.176(5) | |
C21 | O6 | 1.411(5) | Li5 | O6 | 1.988(5) | |
C22 | C23 | 1.507(4) | Li5 | O7 | 3.610(5) | |
C22 | N3 | 1.475(4) | Li5 | O8 | 1.916(5) | |
C23 | O7 | 1.421(4) | Li5 | C18 | 2.166(6) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
N1 | C1 | C2 | 113.5(3) | O5 | Li4 | Li5 | 144.9(3) | |
O1 | C2 | C1 | 110.8(3) | O5 | Li4 | N2 | 88.52(18) | |
N1 | C4 | C5 | 111.7(2) | O5 | Li4 | C18 | 114.1(2) | |
O2 | C5 | C4 | 112.7(3) | O8 | Li4 | Li3 | 48.08(15) | |
N1 | C7 | C8 | 113.1(2) | O8 | Li4 | Li5 | 51.46(16) | |
C9 | C8 | C7 | 107.4(2) | O8 | Li4 | N2 | 99.8(2) | |
C9 | C8 | C10 | 109.4(2) | O8 | Li4 | O5 | 120.1(2) | |
C10 | C8 | C7 | 111.2(2) | O8 | Li4 | C18 | 107.5(2) | |
O3 | C8 | C7 | 109.0(2) | C18 | Li4 | Li3 | 129.7(2) | |
O3 | C8 | C9 | 110.3(2) | C18 | Li4 | Li5 | 56.27(17) | |
O3 | C8 | C10 | 109.6(2) | Li3 | Li5 | O7 | 166.36(18) | |
Li1 | C11 | Li2 | 65.8(2) | Li4 | Li5 | Li3 | 49.14(16) | |
N2 | C12 | C13 | 110.7(2) | Li4 | Li5 | O7 | 138.2(2) | |
O4 | C13 | C12 | 108.9(2) | N3 | Li5 | Li3 | 110.5(2) | |
N2 | C15 | C16 | 115.7(2) | N3 | Li5 | Li4 | 129.5(2) | |
O5 | C16 | C15 | 108.1(2) | N3 | Li5 | O7 | 55.89(12) | |
N3 | C19 | C20 | 112.0(2) | O6 | Li5 | Li3 | 97.0(2) | |
O6 | C20 | C19 | 111.6(3) | O6 | Li5 | Li4 | 134.4(3) | |
N3 | C22 | C23 | 113.5(2) | O6 | Li5 | N3 | 86.78(19) | |
O7 | C23 | C22 | 110.1(3) | O6 | Li5 | O7 | 82.31(16) | |
N3 | C25 | C26 | 112.8(2) | O6 | Li5 | C18 | 116.0(2) | |
C27 | C26 | C25 | 111.4(2) | O8 | Li5 | Li3 | 30.14(13) | |
C27 | C26 | C28 | 108.7(2) | O8 | Li5 | Li4 | 51.99(15) | |
C28 | C26 | C25 | 107.7(2) | O8 | Li5 | N3 | 87.5(2) | |
O8 | C26 | C25 | 108.8(2) | O8 | Li5 | O6 | 116.0(3) | |
O8 | C26 | C27 | 110.5(2) | O8 | Li5 | O7 | 139.3(2) | |
O8 | C26 | C28 | 109.7(2) | O8 | Li5 | C18 | 109.2(2) | |
C11 | Li1 | Li2 | 57.74(19) | C18 | Li5 | Li3 | 100.74(19) | |
C11 | Li1 | Li3 | 102.7(2) | C18 | Li5 | Li4 | 57.52(17) | |
Li2 | Li1 | Li3 | 49.99(17) | C18 | Li5 | N3 | 138.8(3) | |
N1 | Li1 | C11 | 139.7(3) | C18 | Li5 | O7 | 91.72(18) | |
N1 | Li1 | Li2 | 133.2(3) | C1 | N1 | Li1 | 120.5(2) | |
N1 | Li1 | Li3 | 109.8(2) | C4 | N1 | C1 | 110.3(2) | |
O2 | Li1 | C11 | 114.7(3) | C4 | N1 | Li1 | 102.0(2) | |
O2 | Li1 | Li2 | 129.6(3) | C7 | N1 | C1 | 112.6(2) | |
O2 | Li1 | Li3 | 93.4(2) | C7 | N1 | C4 | 111.3(2) | |
O2 | Li1 | N1 | 87.0(2) | C7 | N1 | Li1 | 99.3(2) | |
O3 | Li1 | C11 | 109.8(2) | C12 | N2 | C15 | 110.3(2) | |
O3 | Li1 | Li2 | 52.67(17) | C12 | N2 | Li2 | 94.0(2) | |
O3 | Li1 | Li3 | 30.64(13) | C12 | N2 | Li3 | 140.1(2) | |
O3 | Li1 | N1 | 88.4(2) | C12 | N2 | Li4 | 101.9(2) | |
O3 | Li1 | O2 | 114.7(3) | C15 | N2 | Li2 | 107.9(2) | |
C11 | Li2 | Li1 | 56.44(19) | C15 | N2 | Li3 | 109.6(2) | |
C11 | Li2 | Li3 | 130.3(3) | C15 | N2 | Li4 | 98.0(2) | |
Li1 | Li2 | Li3 | 82.7(2) | Li3 | N2 | Li2 | 73.16(19) | |
N2 | Li2 | C11 | 113.6(2) | Li3 | N2 | Li4 | 72.98(18) | |
N2 | Li2 | Li1 | 110.0(2) | Li4 | N2 | Li2 | 142.6(2) | |
N2 | Li2 | Li3 | 51.67(15) | C19 | N3 | C25 | 111.2(2) | |
O3 | Li2 | C11 | 107.5(2) | C19 | N3 | Li5 | 101.5(2) | |
O3 | Li2 | Li1 | 51.66(18) | C22 | N3 | C19 | 111.1(2) | |
O3 | Li2 | Li3 | 47.17(15) | C22 | N3 | C25 | 112.9(2) | |
O3 | Li2 | N2 | 97.8(2) | C22 | N3 | Li5 | 119.5(2) | |
O3 | Li2 | O4 | 120.4(3) | C25 | N3 | Li5 | 99.61(19) | |
O4 | Li2 | C11 | 124.7(3) | C2 | O1 | C3 | 111.7(3) | |
O4 | Li2 | Li1 | 161.7(3) | C5 | O2 | Li1 | 104.5(2) | |
O4 | Li2 | Li3 | 103.1(2) | C6 | O2 | C5 | 114.6(3) | |
O4 | Li2 | N2 | 86.6(2) | C6 | O2 | Li1 | 117.4(3) | |
Li1 | Li3 | Li5 | 176.5(2) | C8 | O3 | Li1 | 107.2(2) | |
Li2 | Li3 | Li1 | 47.31(16) | C8 | O3 | Li2 | 130.8(2) | |
Li2 | Li3 | Li5 | 132.2(2) | C8 | O3 | Li3 | 131.1(2) | |
Li4 | Li3 | Li1 | 136.3(2) | Li1 | O3 | Li2 | 75.7(2) | |
Li4 | Li3 | Li2 | 108.6(2) | Li3 | O3 | Li1 | 117.1(2) | |
Li4 | Li3 | Li5 | 46.85(15) | Li3 | O3 | Li2 | 81.6(2) | |
N2 | Li3 | Li1 | 86.53(18) | C13 | O4 | Li2 | 105.7(2) | |
N2 | Li3 | Li2 | 55.17(18) | C14 | O4 | C13 | 112.7(3) | |
N2 | Li3 | Li4 | 55.07(16) | C14 | O4 | Li2 | 131.6(3) | |
N2 | Li3 | Li5 | 95.61(18) | C16 | O5 | Li4 | 109.3(2) | |
O3 | Li3 | Li1 | 32.29(14) | C17 | O5 | C16 | 113.6(2) | |
O3 | Li3 | Li2 | 51.19(17) | C17 | O5 | Li4 | 123.2(2) | |
O3 | Li3 | Li4 | 159.8(3) | C20 | O6 | Li5 | 105.0(2) | |
O3 | Li3 | Li5 | 144.2(2) | C21 | O6 | C20 | 115.5(3) | |
O3 | Li3 | N2 | 105.2(2) | C21 | O6 | Li5 | 117.5(3) | |
O3 | Li3 | O8 | 149.4(3) | C23 | O7 | Li5 | 65.42(16) | |
O8 | Li3 | Li1 | 150.6(2) | C24 | O7 | C23 | 111.5(2) | |
O8 | Li3 | Li2 | 158.2(3) | C24 | O7 | Li5 | 103.5(2) | |
O8 | Li3 | Li4 | 50.58(15) | C26 | O8 | Li3 | 129.7(2) | |
O8 | Li3 | Li5 | 31.16(13) | C26 | O8 | Li4 | 127.0(2) | |
O8 | Li3 | N2 | 105.4(2) | C26 | O8 | Li5 | 108.9(2) | |
Li5 | Li4 | Li3 | 84.0(2) | Li3 | O8 | Li4 | 81.3(2) | |
N2 | Li4 | Li3 | 51.95(15) | Li3 | O8 | Li5 | 118.7(2) | |
N2 | Li4 | Li5 | 125.2(2) | Li5 | O8 | Li4 | 76.56(19) | |
N2 | Li4 | C18 | 126.5(2) | Li5 | C18 | Li4 | 66.22(19) | |
O5 | Li4 | Li3 | 115.9(2) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
C1 | C2 | O1 | C3 | 172.0(3) | C27 | C26 | O8 | Li4 | -9.8(3) | |
C2 | C1 | N1 | C4 | 90.2(3) | C27 | C26 | O8 | Li5 | 77.4(3) | |
C2 | C1 | N1 | C7 | -144.9(3) | C28 | C26 | O8 | Li3 | -2.3(4) | |
C2 | C1 | N1 | Li1 | -28.2(4) | C28 | C26 | O8 | Li4 | 110.1(3) | |
C4 | C5 | O2 | C6 | 84.1(4) | C28 | C26 | O8 | Li5 | -162.8(2) | |
C4 | C5 | O2 | Li1 | -45.8(3) | Li1 | Li3 | O3 | C8 | -152.4(4) | |
C5 | C4 | N1 | C1 | -158.8(3) | Li1 | Li3 | O3 | Li2 | 69.1(3) | |
C5 | C4 | N1 | C7 | 75.5(3) | Li1 | Li3 | O8 | C26 | 15.0(6) | |
C5 | C4 | N1 | Li1 | -29.7(3) | Li1 | Li3 | O8 | Li4 | -116.7(5) | |
C7 | C8 | O3 | Li1 | -45.7(3) | Li1 | Li3 | O8 | Li5 | 173.9(4) | |
C7 | C8 | O3 | Li2 | -131.4(3) | Li2 | Li3 | O3 | C8 | 138.5(3) | |
C7 | C8 | O3 | Li3 | 108.7(3) | Li2 | Li3 | O3 | Li1 | -69.1(3) | |
C8 | C7 | N1 | C1 | 97.8(3) | Li2 | Li3 | O8 | C26 | 151.0(6) | |
C8 | C7 | N1 | C4 | -137.8(3) | Li2 | Li3 | O8 | Li4 | 19.3(7) | |
C8 | C7 | N1 | Li1 | -30.8(3) | Li2 | Li3 | O8 | Li5 | -50.1(8) | |
C9 | C8 | O3 | Li1 | -163.3(2) | Li4 | Li3 | O3 | C8 | 139.9(7) | |
C9 | C8 | O3 | Li2 | 111.0(3) | Li4 | Li3 | O3 | Li1 | -67.7(8) | |
C9 | C8 | O3 | Li3 | -8.9(4) | Li4 | Li3 | O3 | Li2 | 1.5(8) | |
C10 | C8 | O3 | Li1 | 76.1(3) | Li4 | Li3 | O8 | C26 | 131.7(3) | |
C10 | C8 | O3 | Li2 | -9.5(4) | Li4 | Li3 | O8 | Li5 | -69.4(2) | |
C10 | C8 | O3 | Li3 | -129.4(3) | Li5 | Li3 | O3 | C8 | 27.4(5) | |
C12 | C13 | O4 | C14 | -177.8(3) | Li5 | Li3 | O3 | Li1 | 179.8(3) | |
C12 | C13 | O4 | Li2 | -27.8(3) | Li5 | Li3 | O3 | Li2 | -111.0(4) | |
C13 | C12 | N2 | C15 | -168.6(2) | Li5 | Li3 | O8 | C26 | -158.9(4) | |
C13 | C12 | N2 | Li2 | -57.8(3) | Li5 | Li3 | O8 | Li4 | 69.4(2) | |
C13 | C12 | N2 | Li3 | 10.6(4) | N1 | C1 | C2 | O1 | -67.7(3) | |
C13 | C12 | N2 | Li4 | 88.2(3) | N1 | C4 | C5 | O2 | 54.2(4) | |
C15 | C16 | O5 | C17 | 173.7(2) | N1 | C7 | C8 | C9 | 173.9(2) | |
C15 | C16 | O5 | Li4 | 31.9(3) | N1 | C7 | C8 | C10 | -66.5(3) | |
C16 | C15 | N2 | C12 | -64.8(3) | N1 | C7 | C8 | O3 | 54.5(3) | |
C16 | C15 | N2 | Li2 | -166.2(2) | N2 | C12 | C13 | O4 | 64.0(3) | |
C16 | C15 | N2 | Li3 | 115.8(3) | N2 | C15 | C16 | O5 | -53.1(3) | |
C16 | C15 | N2 | Li4 | 41.1(3) | N2 | Li3 | O3 | C8 | 150.7(2) | |
C19 | C20 | O6 | C21 | 83.7(4) | N2 | Li3 | O3 | Li1 | -56.9(3) | |
C19 | C20 | O6 | Li5 | -47.3(3) | N2 | Li3 | O3 | Li2 | 12.2(2) | |
C20 | C19 | N3 | C22 | -157.7(3) | N2 | Li3 | O8 | C26 | 126.2(2) | |
C20 | C19 | N3 | C25 | 75.6(3) | N2 | Li3 | O8 | Li4 | -5.5(2) | |
C20 | C19 | N3 | Li5 | -29.5(3) | N2 | Li3 | O8 | Li5 | -75.0(3) | |
C22 | C23 | O7 | C24 | 167.3(3) | N3 | C19 | C20 | O6 | 54.7(4) | |
C22 | C23 | O7 | Li5 | 71.8(2) | N3 | C22 | C23 | O7 | -68.5(3) | |
C23 | C22 | N3 | C19 | 89.8(3) | N3 | C25 | C26 | C27 | -68.4(3) | |
C23 | C22 | N3 | C25 | -144.5(2) | N3 | C25 | C26 | C28 | 172.4(3) | |
C23 | C22 | N3 | Li5 | -27.9(3) | N3 | C25 | C26 | O8 | 53.6(3) | |
C25 | C26 | O8 | Li3 | 115.3(3) | O3 | Li3 | O8 | C26 | -52.5(6) | |
C25 | C26 | O8 | Li4 | -132.3(2) | O3 | Li3 | O8 | Li4 | 175.8(6) | |
C25 | C26 | O8 | Li5 | -45.2(3) | O3 | Li3 | O8 | Li5 | 106.4(5) | |
C26 | C25 | N3 | C19 | -137.5(3) | O8 | Li3 | O3 | C8 | -30.6(7) | |
C26 | C25 | N3 | C22 | 96.9(3) | O8 | Li3 | O3 | Li1 | 121.8(5) | |
C26 | C25 | N3 | Li5 | -31.0(3) | O8 | Li3 | O3 | Li2 | -169.1(6) | |
C27 | C26 | O8 | Li3 | -122.1(3) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H1A | 753 | 8010 | 2346 | 69 |
H1B | 258 | 7191 | 2677 | 69 |
H2A | 550 | 4901 | 2315 | 73 |
H2B | 16 | 5969 | 1804 | 73 |
H3A | 510 | 4491 | 1183 | 138 |
H3B | 1113 | 3639 | 1738 | 138 |
H3C | 1431 | 4530 | 1305 | 138 |
H4A | 2124 | 8601 | 3028 | 68 |
H4B | 2062 | 7346 | 2553 | 68 |
H5A | 3313 | 7281 | 3264 | 75 |
H5B | 2969 | 7187 | 3780 | 75 |
H6A | 2731 | 5134 | 2505 | 134 |
H6B | 3068 | 3685 | 2885 | 134 |
H6C | 3632 | 5064 | 2938 | 134 |
H7A | 952 | 8236 | 3507 | 57 |
H7B | 1868 | 7947 | 3856 | 57 |
H9A | 1061 | 6298 | 4807 | 80 |
H9B | 828 | 7838 | 4472 | 80 |
H9C | 1733 | 7382 | 4775 | 80 |
H10A | 335 | 5092 | 3328 | 82 |
H10B | -37 | 6476 | 3536 | 82 |
H10C | 195 | 5035 | 3939 | 82 |
H11A | 2059(16) | 2160(40) | 3075(15) | 67(10) |
H11B | 1200(20) | 2470(50) | 2713(12) | 103(14) |
H11C | 1450(40) | 1400(40) | 3280(30) | 190(30) |
H12A | 2741 | 530 | 5169 | 57 |
H12B | 2195 | 397 | 4487 | 57 |
H13A | 1440 | 360 | 5100 | 63 |
H13B | 1752 | 1978 | 5329 | 63 |
H14A | 122 | 1358 | 4714 | 119 |
H14B | -70 | 2664 | 4243 | 119 |
H14C | 451 | 2974 | 4920 | 119 |
H15A | 3392 | 3097 | 4340 | 55 |
H15B | 2991 | 1554 | 4097 | 55 |
H16A | 3844 | 338 | 4925 | 59 |
H16B | 4363 | 1323 | 4658 | 59 |
H17A | 4771 | 442 | 5893 | 79 |
H17B | 5093 | 1995 | 6190 | 79 |
H17C | 5365 | 1367 | 5682 | 79 |
H19A | 2945 | 8543 | 6634 | 70 |
H19B | 2958 | 7258 | 7085 | 70 |
H20A | 1714 | 7356 | 6363 | 77 |
H20B | 2069 | 7244 | 5853 | 77 |
H21A | 2260 | 5029 | 7105 | 136 |
H21B | 1822 | 3703 | 6681 | 136 |
H21C | 1356 | 5185 | 6688 | 136 |
H22A | 4297 | 7746 | 7320 | 64 |
H22B | 4767 | 6904 | 6976 | 64 |
H23A | 4367 | 4620 | 7277 | 60 |
H23B | 4946 | 5569 | 7814 | 60 |
H24A | 3694 | 3422 | 7756 | 99 |
H24B | 3398 | 4263 | 8213 | 99 |
H24C | 4318 | 4038 | 8361 | 99 |
H25A | 4125 | 8107 | 6165 | 58 |
H25B | 3203 | 7930 | 5804 | 58 |
H27A | 4673 | 4962 | 6298 | 73 |
H27B | 5067 | 6305 | 6084 | 73 |
H27C | 4789 | 4876 | 5679 | 73 |
H28A | 3940 | 6240 | 4823 | 80 |
H28B | 4240 | 7736 | 5178 | 80 |
H28C | 3318 | 7407 | 4881 | 80 |
H18A | 2890(20) | 2070(50) | 6540(17) | 94(13) |
H18B | 3250(30) | 1310(40) | 6240(20) | 141(19) |
H18C | 3870(20) | 2140(70) | 6740(20) | 160(20) |
Experimental
Single crystals of C28H64Li5N3O8 [cu_B0490_0m] were []. A suitable crystal was selected and [] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 99.99 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 ShelXL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [cu_B0490_0m]
Crystal Data for C28H64Li5N3O8 (M =605.52 g/mol): monoclinic, space group P21/c (no. 14), a = 18.2841(8) Å, b = 9.1092(4) Å, c = 24.3776(10) Å, β = 111.387(2)°, V = 3780.6(3) Å3, Z = 4, T = 99.99 K, μ(CuKα) = 0.586 mm-1, Dcalc = 1.064 g/cm3, 63345 reflections measured (5.19° ≤ 2Θ ≤ 135.984°), 6869 unique (Rint = 0.1315, Rsigma = 0.0627) which were used in all calculations. The final R1 was 0.0792 (I > 2σ(I)) and wR2 was 0.2261 (all data).
Refinement model description
Number of restraints - 6, 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. Restrained distances
C18-H18A ≈ C18-H18B ≈ C18-H18C
with sigma of 0.02
C11-H11A ≈ C11-H11B ≈ C11-H11C
with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C12(H12A,
H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C19(H19A,H19B),
C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B)
3.b Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C24(H24A,H24B,
H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
This report has been created with Olex2, compiled on 2016.11.07 svn.r3352 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.