Identification code | cu_b0089_0m |
Empirical formula | C16H39Li4N3O3 |
Formula weight | 349.26 |
Temperature/K | 100.0 |
Crystal system | monoclinic |
Space group | P21/n |
a/Å | 10.8656(4) |
b/Å | 10.9386(5) |
c/Å | 19.3571(8) |
α/° | 90 |
β/° | 102.672(2) |
γ/° | 90 |
Volume/Å3 | 2244.64(16) |
Z | 4 |
ρcalcg/cm3 | 1.034 |
μ/mm‑1 | 0.520 |
F(000) | 768.0 |
Crystal size/mm3 | 0.35 × 0.22 × 0.22 |
Radiation | CuKα (λ = 1.54178) |
2Θ range for data collection/° | 8.624 to 137.996 |
Index ranges | -13 ≤ h ≤ 11, -13 ≤ k ≤ 13, -23 ≤ l ≤ 23 |
Reflections collected | 35901 |
Independent reflections | 4026 [Rint = 0.0521, Rsigma = 0.0235] |
Data/restraints/parameters | 4026/0/280 |
Goodness-of-fit on F2 | 1.995 |
Final R indexes [I>=2σ (I)] | R1 = 0.1116, wR2 = 0.3920 |
Final R indexes [all data] | R1 = 0.1182, wR2 = 0.4055 |
Largest diff. peak/hole / e Å-3 | 1.23/-0.48 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
O1 | 5058.5(19) | 4235.3(18) | 6009.5(10) | 27.0(6) |
O2 | 5367.0(19) | 6745.2(16) | 5483.4(11) | 27.8(6) |
O3 | 3014.8(17) | 5254.3(17) | 4876.3(11) | 25.9(6) |
N1 | 2944(2) | 2571(2) | 5880.9(15) | 30.9(7) |
N2 | 3693(2) | 7008(2) | 6434.2(14) | 32.8(7) |
N3 | 1830(2) | 4586(2) | 3452.4(13) | 29.8(7) |
C1 | 6941(3) | 1546(3) | 5831(2) | 32.9(8) |
C2 | 8281(3) | 1096(3) | 5857.7(19) | 34.3(8) |
C3 | 8608(3) | -179(3) | 6158(3) | 48.5(11) |
C4 | 9957(3) | -594(3) | 6181(3) | 50.7(11) |
C5 | 4867(3) | 3598(3) | 6614.7(16) | 34.0(8) |
C6 | 3493(3) | 3264(3) | 6555.9(19) | 40.4(9) |
C7 | 3489(4) | 1353(4) | 5947(2) | 52.4(11) |
C8 | 1583(3) | 2525(4) | 5803(2) | 51.4(11) |
C9 | 5393(3) | 7833(3) | 5886(2) | 37.3(8) |
C13 | 1697(3) | 5411(3) | 4636.0(17) | 31.3(8) |
C14 | 1159(3) | 4520(3) | 4050(2) | 39.2(8) |
C15 | 1592(4) | 5733(4) | 3092(2) | 55.1(11) |
C16 | 1428(4) | 3554(4) | 2974(2) | 54.2(11) |
Li1 | 6073(4) | 3225(4) | 5427(3) | 23.7(10) |
Li2 | 6355(5) | 5351(4) | 5939(3) | 29.0(11) |
Li3 | 6273(5) | 6345(4) | 4786(3) | 30.4(11) |
Li4 | 4060(5) | 5713(5) | 5736(3) | 30.1(11) |
C10A | 4154(6) | 8049(4) | 6115(3) | 35.4(13) |
C11A | 2402(6) | 7129(6) | 6491(4) | 54.8(18) |
C12A | 4452(7) | 6778(6) | 7178(3) | 45.6(16) |
C10B | 4882(13) | 7736(12) | 6469(7) | 48(3) |
C11B | 3413(19) | 6820(13) | 7091(7) | 67(5) |
C12B | 2643(12) | 7782(11) | 5951(7) | 49(3) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
O1 | 33.3(12) | 27.6(11) | 21.8(11) | 6.1(8) | 9.9(8) | 8.6(8) |
O2 | 28.0(12) | 16.8(10) | 36.4(12) | -1.9(8) | 1.9(9) | -0.4(7) |
O3 | 18.3(11) | 24.7(11) | 35.1(12) | 6.5(8) | 6.4(9) | 4.4(7) |
N1 | 23.5(14) | 28.9(13) | 43.5(15) | 11.7(11) | 14.2(11) | -3.4(9) |
N2 | 33.3(15) | 38.0(15) | 30.3(14) | -10.9(10) | 13.8(11) | 4.5(10) |
N3 | 24.8(14) | 33.4(14) | 26.7(13) | -3.0(10) | -4.5(10) | -1.3(9) |
C1 | 30.3(17) | 26.3(15) | 44.4(19) | 13.1(13) | 13.1(14) | 9.7(11) |
C2 | 28.1(16) | 24.9(15) | 52(2) | 9.7(13) | 14.8(14) | 4.2(11) |
C3 | 35.0(19) | 33.0(18) | 81(3) | 20.9(17) | 20.7(18) | 11.7(13) |
C4 | 35(2) | 31.2(17) | 88(3) | 9.6(18) | 17.6(19) | 9.3(14) |
C5 | 38.1(18) | 38.5(17) | 27.3(16) | 8.9(12) | 11.4(13) | 3.7(12) |
C6 | 45(2) | 41.9(19) | 39.9(18) | 8.9(14) | 20.4(16) | 2.1(14) |
C7 | 55(2) | 40(2) | 65(3) | 8.7(17) | 20(2) | -1.3(15) |
C8 | 30.3(19) | 58(2) | 70(3) | 13.9(19) | 18.9(18) | -2.5(15) |
C9 | 36.0(18) | 27.3(15) | 50(2) | -11.7(13) | 12.2(15) | -4.3(12) |
C13 | 25.2(16) | 34.8(16) | 36.1(17) | 1.8(12) | 11.2(13) | 3.9(11) |
C14 | 28.0(17) | 41.4(17) | 45.6(19) | 0.1(14) | 2.3(14) | -3.4(13) |
C15 | 58(3) | 56(2) | 47(2) | 11.0(18) | 3.7(18) | 10.7(18) |
C16 | 57(2) | 57(2) | 43(2) | -14.1(17) | -0.6(17) | -10.8(18) |
Li1 | 23(2) | 20(2) | 28(2) | 4.0(17) | 4.4(18) | 2.4(16) |
Li2 | 23(2) | 29(2) | 34(3) | 2.7(19) | 4(2) | -3.6(17) |
Li3 | 30(3) | 29(2) | 36(3) | 3(2) | 17(2) | 0.3(19) |
Li4 | 38(3) | 29(2) | 23(2) | -1.9(18) | 4(2) | 4.1(19) |
C10A | 39(3) | 31(2) | 34(3) | -5.2(19) | 3(2) | 6.6(19) |
C11A | 43(3) | 60(4) | 68(4) | -17(3) | 25(3) | 10(3) |
C12A | 58(4) | 47(3) | 30(3) | -7(2) | 6(3) | -2(3) |
C10B | 52(8) | 46(6) | 48(7) | -29(6) | 14(6) | -10(5) |
C11B | 114(16) | 55(8) | 42(7) | -9(5) | 40(9) | 18(8) |
C12B | 56(7) | 41(6) | 55(7) | -9(5) | 23(6) | 9(5) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O1 | C5 | 1.417(3) | N2 | C11B | 1.386(12) | |
O1 | Li1 | 2.062(5) | N2 | C12B | 1.557(13) | |
O1 | Li2 | 1.891(5) | N3 | C14 | 1.498(4) | |
O1 | Li31 | 1.972(6) | N3 | C15 | 1.431(5) | |
O1 | Li4 | 1.953(5) | N3 | C16 | 1.465(5) | |
O2 | C9 | 1.419(4) | N3 | Li21 | 2.065(6) | |
O2 | Li11 | 2.085(5) | C1 | C2 | 1.527(4) | |
O2 | Li2 | 1.960(5) | C1 | Li1 | 2.133(5) | |
O2 | Li3 | 1.888(5) | C2 | C3 | 1.523(4) | |
O2 | Li4 | 1.959(6) | C3 | C4 | 1.526(5) | |
O3 | C13 | 1.416(4) | C5 | C6 | 1.517(5) | |
O3 | Li11 | 2.086(5) | C6 | Li31 | 2.700(6) | |
O3 | Li21 | 1.968(5) | C9 | C10A | 1.525(6) | |
O3 | Li31 | 1.965(5) | C9 | C10B | 1.367(12) | |
O3 | Li4 | 1.867(6) | C13 | C14 | 1.512(5) | |
N1 | C6 | 1.515(5) | Li1 | Li2 | 2.520(7) | |
N1 | C7 | 1.452(5) | Li1 | Li31 | 2.536(7) | |
N1 | C8 | 1.454(4) | Li1 | Li41 | 2.511(7) | |
N1 | Li31 | 2.069(5) | Li2 | Li3 | 2.466(7) | |
N2 | Li4 | 2.056(5) | Li2 | Li31 | 3.436(7) | |
N2 | C10A | 1.437(6) | Li2 | Li41 | 3.381(7) | |
N2 | C11A | 1.437(6) | Li2 | Li4 | 2.469(7) | |
N2 | C12A | 1.515(6) | Li3 | Li4 | 3.403(7) | |
N2 | C10B | 1.507(12) | Li3 | Li41 | 2.461(7) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C5 | O1 | Li1 | 112.4(2) | O31 | Li2 | Li41 | 27.34(13) | |
C5 | O1 | Li2 | 128.6(3) | N31 | Li2 | C131 | 60.89(16) | |
C5 | O1 | Li31 | 105.8(2) | N31 | Li2 | C141 | 33.40(13) | |
C5 | O1 | Li4 | 117.2(2) | N31 | Li2 | Li1 | 105.9(2) | |
Li2 | O1 | Li1 | 79.1(2) | N31 | Li2 | Li3 | 110.0(2) | |
Li2 | O1 | Li31 | 125.6(2) | N31 | Li2 | Li31 | 148.8(2) | |
Li2 | O1 | Li4 | 79.9(2) | N31 | Li2 | Li41 | 117.9(2) | |
Li31 | O1 | Li1 | 77.8(2) | N31 | Li2 | Li4 | 152.9(3) | |
Li4 | O1 | Li1 | 128.9(2) | C131 | Li2 | Li31 | 108.52(19) | |
Li4 | O1 | Li31 | 77.7(2) | C131 | Li2 | Li41 | 57.04(15) | |
C9 | O2 | Li11 | 111.8(2) | C141 | Li2 | C131 | 32.33(11) | |
C9 | O2 | Li2 | 117.6(3) | C141 | Li2 | Li31 | 140.5(2) | |
C9 | O2 | Li3 | 129.5(2) | C141 | Li2 | Li41 | 87.03(18) | |
C9 | O2 | Li4 | 105.9(2) | Li1 | Li2 | C131 | 66.17(17) | |
Li2 | O2 | Li11 | 128.9(2) | Li1 | Li2 | C141 | 94.9(2) | |
Li3 | O2 | Li11 | 79.1(2) | Li1 | Li2 | Li31 | 47.37(15) | |
Li3 | O2 | Li2 | 79.7(2) | Li1 | Li2 | Li41 | 47.65(16) | |
Li3 | O2 | Li4 | 124.4(2) | Li3 | Li2 | C131 | 69.08(18) | |
Li4 | O2 | Li11 | 76.7(2) | Li3 | Li2 | C141 | 79.72(19) | |
Li4 | O2 | Li2 | 78.1(2) | Li3 | Li2 | Li1 | 94.2(2) | |
C13 | O3 | Li11 | 108.6(2) | Li3 | Li2 | Li31 | 90.4(2) | |
C13 | O3 | Li21 | 106.4(2) | Li3 | Li2 | Li41 | 46.61(17) | |
C13 | O3 | Li31 | 120.9(2) | Li3 | Li2 | Li4 | 87.2(2) | |
C13 | O3 | Li4 | 129.4(2) | Li4 | Li2 | C131 | 146.2(3) | |
Li21 | O3 | Li11 | 76.82(19) | Li4 | Li2 | C141 | 165.1(3) | |
Li31 | O3 | Li11 | 128.8(2) | Li4 | Li2 | Li1 | 93.1(2) | |
Li31 | O3 | Li21 | 77.6(2) | Li41 | Li2 | Li31 | 59.87(15) | |
Li4 | O3 | Li11 | 78.7(2) | Li4 | Li2 | Li31 | 45.72(16) | |
Li4 | O3 | Li21 | 123.7(2) | Li4 | Li2 | Li41 | 89.1(2) | |
Li4 | O3 | Li31 | 79.9(2) | O11 | Li3 | N11 | 91.6(2) | |
C6 | N1 | Li31 | 96.5(2) | O11 | Li3 | C51 | 30.05(12) | |
C7 | N1 | C6 | 107.9(3) | O11 | Li3 | Li11 | 52.66(17) | |
C7 | N1 | C8 | 111.3(3) | O11 | Li3 | Li2 | 116.1(2) | |
C7 | N1 | Li31 | 111.4(2) | O11 | Li3 | Li21 | 26.60(12) | |
C8 | N1 | C6 | 107.8(3) | O11 | Li3 | Li4 | 82.69(18) | |
C8 | N1 | Li31 | 120.2(3) | O11 | Li3 | Li41 | 50.82(18) | |
C10A | N2 | Li4 | 97.3(3) | O2 | Li3 | O11 | 103.0(2) | |
C10A | N2 | C11A | 113.4(4) | O2 | Li3 | O31 | 101.4(2) | |
C10A | N2 | C12A | 111.8(4) | O2 | Li3 | N11 | 131.6(3) | |
C11A | N2 | Li4 | 116.6(3) | O2 | Li3 | C51 | 120.8(2) | |
C11A | N2 | C12A | 106.2(4) | O2 | Li3 | Li11 | 53.87(17) | |
C12A | N2 | Li4 | 111.5(3) | O2 | Li3 | Li2 | 51.44(18) | |
C10B | N2 | Li4 | 96.1(4) | O2 | Li3 | Li21 | 84.30(19) | |
C10B | N2 | C12B | 104.3(8) | O2 | Li3 | Li41 | 117.0(3) | |
C11B | N2 | Li4 | 127.9(6) | O2 | Li3 | Li4 | 28.36(13) | |
C11B | N2 | C10B | 113.3(10) | O31 | Li3 | O11 | 98.1(2) | |
C11B | N2 | C12B | 110.6(9) | O31 | Li3 | N11 | 122.1(2) | |
C12B | N2 | Li4 | 101.7(5) | O31 | Li3 | C51 | 114.3(2) | |
C14 | N3 | Li21 | 97.3(2) | O31 | Li3 | Li11 | 121.9(2) | |
C15 | N3 | C14 | 110.7(3) | O31 | Li3 | Li2 | 51.23(17) | |
C15 | N3 | C16 | 111.7(3) | O31 | Li3 | Li21 | 83.49(19) | |
C15 | N3 | Li21 | 107.3(3) | O31 | Li3 | Li41 | 48.29(17) | |
C16 | N3 | C14 | 108.9(3) | O31 | Li3 | Li4 | 85.01(17) | |
C16 | N3 | Li21 | 120.1(3) | N11 | Li3 | C51 | 61.62(17) | |
C2 | C1 | Li1 | 129.2(2) | N11 | Li3 | Li11 | 109.1(2) | |
C3 | C2 | C1 | 116.6(3) | N11 | Li3 | Li21 | 118.2(2) | |
C2 | C3 | C4 | 115.2(3) | N11 | Li3 | Li2 | 151.6(3) | |
O1 | C5 | C6 | 112.2(3) | N11 | Li3 | Li41 | 108.1(2) | |
N1 | C6 | C5 | 112.3(2) | N11 | Li3 | Li4 | 152.9(2) | |
N1 | C6 | Li31 | 49.59(16) | C51 | Li3 | Li21 | 56.63(15) | |
C5 | C6 | Li31 | 74.64(19) | C51 | Li3 | Li4 | 108.79(19) | |
O2 | C9 | C10A | 112.1(3) | Li11 | Li3 | C51 | 67.17(18) | |
C10B | C9 | O2 | 115.2(5) | Li11 | Li3 | Li21 | 47.00(16) | |
O3 | C13 | C14 | 111.4(2) | Li11 | Li3 | Li4 | 47.29(15) | |
N3 | C14 | C13 | 112.0(3) | Li2 | Li3 | C51 | 146.0(2) | |
O1 | Li1 | O21 | 93.5(2) | Li2 | Li3 | Li11 | 93.7(2) | |
O1 | Li1 | O31 | 94.04(19) | Li2 | Li3 | Li21 | 89.6(2) | |
O1 | Li1 | C1 | 120.5(2) | Li2 | Li3 | Li4 | 46.45(16) | |
O1 | Li1 | Li2 | 47.47(15) | Li41 | Li3 | C51 | 67.53(19) | |
O1 | Li1 | Li31 | 49.50(17) | Li41 | Li3 | Li11 | 92.9(2) | |
O1 | Li1 | Li41 | 108.0(2) | Li41 | Li3 | Li21 | 45.91(17) | |
O21 | Li1 | O31 | 93.7(2) | Li4 | Li3 | Li21 | 59.26(14) | |
O21 | Li1 | C1 | 120.8(2) | Li41 | Li3 | Li2 | 86.7(2) | |
O21 | Li1 | Li2 | 108.8(2) | Li41 | Li3 | Li4 | 88.78(19) | |
O21 | Li1 | Li31 | 46.99(16) | O1 | Li4 | O2 | 98.9(2) | |
O21 | Li1 | Li41 | 49.39(17) | O1 | Li4 | N2 | 124.6(3) | |
O31 | Li1 | C1 | 126.2(2) | O1 | Li4 | Li11 | 123.0(2) | |
O31 | Li1 | Li2 | 49.49(15) | O1 | Li4 | Li21 | 85.65(19) | |
O31 | Li1 | Li31 | 109.2(2) | O1 | Li4 | Li2 | 48.95(17) | |
O31 | Li1 | Li41 | 46.79(16) | O1 | Li4 | Li31 | 51.52(18) | |
C1 | Li1 | Li2 | 130.2(3) | O1 | Li4 | Li3 | 84.16(19) | |
C1 | Li1 | Li31 | 124.6(2) | O2 | Li4 | N2 | 91.3(2) | |
C1 | Li1 | Li41 | 131.4(2) | O2 | Li4 | Li11 | 53.92(17) | |
Li2 | Li1 | Li31 | 85.6(2) | O2 | Li4 | Li2 | 50.95(17) | |
Li41 | Li1 | Li2 | 84.5(2) | O2 | Li4 | Li21 | 84.85(19) | |
Li41 | Li1 | Li31 | 84.8(2) | O2 | Li4 | Li3 | 27.24(13) | |
O1 | Li2 | O2 | 101.0(2) | O2 | Li4 | Li31 | 118.3(2) | |
O1 | Li2 | O31 | 103.7(2) | O3 | Li4 | O1 | 102.3(2) | |
O1 | Li2 | N31 | 127.9(3) | O3 | Li4 | O2 | 105.3(2) | |
O1 | Li2 | C131 | 119.3(2) | O3 | Li4 | N2 | 127.1(3) | |
O1 | Li2 | C141 | 142.4(3) | O3 | Li4 | Li11 | 54.54(18) | |
O1 | Li2 | Li1 | 53.45(17) | O3 | Li4 | Li21 | 28.96(13) | |
O1 | Li2 | Li3 | 118.0(3) | O3 | Li4 | Li2 | 119.6(3) | |
O1 | Li2 | Li31 | 27.84(14) | O3 | Li4 | Li31 | 51.82(18) | |
O1 | Li2 | Li41 | 84.4(2) | O3 | Li4 | Li3 | 86.36(19) | |
O1 | Li2 | Li4 | 51.15(18) | N2 | Li4 | Li11 | 106.8(2) | |
O2 | Li2 | O31 | 98.8(2) | N2 | Li4 | Li21 | 149.6(2) | |
O2 | Li2 | N31 | 126.3(3) | N2 | Li4 | Li2 | 109.9(3) | |
O2 | Li2 | C131 | 116.8(2) | N2 | Li4 | Li31 | 150.2(3) | |
O2 | Li2 | C141 | 114.3(2) | N2 | Li4 | Li3 | 118.5(2) | |
O2 | Li2 | Li1 | 122.3(3) | Li11 | Li4 | Li21 | 47.89(16) | |
O2 | Li2 | Li31 | 84.95(19) | Li11 | Li4 | Li3 | 47.91(16) | |
O2 | Li2 | Li3 | 48.87(17) | Li2 | Li4 | Li11 | 94.3(2) | |
O2 | Li2 | Li41 | 83.76(19) | Li2 | Li4 | Li21 | 90.9(2) | |
O2 | Li2 | Li4 | 50.92(17) | Li21 | Li4 | Li3 | 60.86(14) | |
O31 | Li2 | N31 | 90.7(2) | Li2 | Li4 | Li3 | 46.36(17) | |
O31 | Li2 | C131 | 29.85(12) | Li31 | Li4 | Li11 | 94.6(2) | |
O31 | Li2 | C141 | 60.02(16) | Li31 | Li4 | Li21 | 46.71(16) | |
O31 | Li2 | Li1 | 53.69(17) | Li31 | Li4 | Li2 | 88.4(2) | |
O31 | Li2 | Li3 | 51.13(17) | Li31 | Li4 | Li3 | 91.22(19) | |
O31 | Li2 | Li31 | 83.95(18) | N2 | C10A | C9 | 114.5(4) | |
O31 | Li2 | Li4 | 116.3(3) | C9 | C10B | N2 | 120.2(8) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
O1 | C5 | C6 | N1 | 53.6(4) | Li2 | O1 | C5 | C6 | 154.1(3) | |
O1 | C5 | C6 | Li31 | 20.7(2) | Li2 | O2 | C9 | C10A | -107.5(4) | |
O2 | C9 | C10A | N2 | 49.1(5) | Li2 | O2 | C9 | C10B | -64.3(8) | |
O2 | C9 | C10B | N2 | -40.4(14) | Li2 | O2 | Li3 | O11 | 113.2(2) | |
O3 | C13 | C14 | N3 | -54.1(3) | Li2 | O2 | Li3 | O31 | 11.9(2) | |
C1 | C2 | C3 | C4 | -179.7(4) | Li2 | O2 | Li3 | N11 | -142.8(4) | |
C5 | O1 | Li2 | O2 | -127.8(3) | Li2 | O2 | Li3 | C51 | 139.4(3) | |
C5 | O1 | Li2 | O31 | 130.2(3) | Li2 | O2 | Li3 | Li11 | 133.2(2) | |
C5 | O1 | Li2 | N31 | 28.4(5) | Li2 | O2 | Li3 | Li21 | 94.11(19) | |
C5 | O1 | Li2 | C131 | 102.7(3) | Li2 | O2 | Li3 | Li41 | 60.8(3) | |
C5 | O1 | Li2 | C141 | 72.0(5) | Li2 | O2 | Li3 | Li4 | 67.8(3) | |
C5 | O1 | Li2 | Li1 | 110.0(3) | Li21 | O3 | C13 | C14 | 29.7(3) | |
C5 | O1 | Li2 | Li3 | -176.8(3) | Li21 | O3 | Li4 | O1 | -56.4(3) | |
C5 | O1 | Li2 | Li31 | 176.4(4) | Li21 | O3 | Li4 | O2 | 46.5(3) | |
C5 | O1 | Li2 | Li41 | 149.7(3) | Li21 | O3 | Li4 | N2 | 150.2(3) | |
C5 | O1 | Li2 | Li4 | -116.9(3) | Li21 | O3 | Li4 | Li11 | 65.6(3) | |
C7 | N1 | C6 | C5 | 71.6(3) | Li21 | O3 | Li4 | Li2 | -6.9(5) | |
C7 | N1 | C6 | Li31 | 115.0(3) | Li21 | O3 | Li4 | Li31 | -67.6(3) | |
C8 | N1 | C6 | C5 | -168.1(3) | Li21 | O3 | Li4 | Li3 | 26.8(3) | |
C8 | N1 | C6 | Li31 | -124.7(3) | Li21 | N3 | C14 | C13 | 44.1(3) | |
C9 | O2 | Li3 | O11 | -129.5(3) | Li31 | O1 | C5 | C6 | -29.0(3) | |
C9 | O2 | Li3 | O31 | 129.3(3) | Li31 | O1 | Li2 | O2 | 55.9(3) | |
C9 | O2 | Li3 | N11 | -25.4(6) | Li31 | O1 | Li2 | O31 | -46.2(3) | |
C9 | O2 | Li3 | C51 | -103.2(4) | Li31 | O1 | Li2 | N31 | -148.0(3) | |
C9 | O2 | Li3 | Li11 | -109.4(3) | Li31 | O1 | Li2 | C131 | -73.7(3) | |
C9 | O2 | Li3 | Li2 | 117.3(3) | Li31 | O1 | Li2 | C141 | -104.3(4) | |
C9 | O2 | Li3 | Li21 | -148.5(3) | Li31 | O1 | Li2 | Li1 | -66.3(3) | |
C9 | O2 | Li3 | Li41 | 178.1(3) | Li31 | O1 | Li2 | Li3 | 6.8(5) | |
C9 | O2 | Li3 | Li4 | -174.9(5) | Li31 | O1 | Li2 | Li4 | 66.8(3) | |
C13 | O3 | Li4 | O1 | 133.1(3) | Li31 | O1 | Li2 | Li41 | -26.6(3) | |
C13 | O3 | Li4 | O2 | -124.0(3) | Li3 | O2 | C9 | C10A | 152.8(4) | |
C13 | O3 | Li4 | N2 | -20.3(5) | Li3 | O2 | C9 | C10B | -164.0(8) | |
C13 | O3 | Li4 | Li11 | -104.9(3) | Li31 | O3 | C13 | C14 | -55.5(3) | |
C13 | O3 | Li4 | Li21 | -170.5(4) | Li31 | O3 | Li4 | O1 | 11.2(2) | |
C13 | O3 | Li4 | Li2 | -177.4(3) | Li31 | O3 | Li4 | O2 | 114.2(3) | |
C13 | O3 | Li4 | Li31 | 121.9(3) | Li31 | O3 | Li4 | N2 | -142.1(4) | |
C13 | O3 | Li4 | Li3 | -143.7(2) | Li31 | O3 | Li4 | Li11 | 133.2(2) | |
C15 | N3 | C14 | C13 | -67.5(4) | Li31 | O3 | Li4 | Li2 | 60.7(3) | |
C16 | N3 | C14 | C13 | 169.4(3) | Li31 | O3 | Li4 | Li21 | 67.6(3) | |
Li1 | O1 | C5 | C6 | -112.1(3) | Li31 | O3 | Li4 | Li3 | 94.42(17) | |
Li1 | O1 | Li2 | O2 | 122.2(3) | Li31 | N1 | C6 | C5 | -43.5(3) | |
Li1 | O1 | Li2 | O31 | 20.1(2) | Li4 | O1 | C5 | C6 | 55.0(4) | |
Li1 | O1 | Li2 | N31 | -81.6(3) | Li4 | O1 | Li2 | O2 | -10.9(2) | |
Li1 | O1 | Li2 | C131 | -7.4(3) | Li4 | O1 | Li2 | O31 | -113.0(3) | |
Li1 | O1 | Li2 | C141 | -38.0(4) | Li4 | O1 | Li2 | N31 | 145.3(4) | |
Li1 | O1 | Li2 | Li3 | 73.1(3) | Li4 | O1 | Li2 | C131 | -140.5(3) | |
Li1 | O1 | Li2 | Li31 | 66.3(3) | Li4 | O1 | Li2 | C141 | -171.1(5) | |
Li1 | O1 | Li2 | Li41 | 39.67(17) | Li4 | O1 | Li2 | Li1 | -133.1(2) | |
Li1 | O1 | Li2 | Li4 | 133.1(2) | Li4 | O1 | Li2 | Li3 | -60.0(3) | |
Li11 | O2 | C9 | C10A | 59.0(4) | Li4 | O1 | Li2 | Li31 | -66.8(3) | |
Li11 | O2 | C9 | C10B | 102.1(8) | Li4 | O1 | Li2 | Li41 | -93.43(18) | |
Li11 | O2 | Li3 | O11 | -20.1(2) | Li4 | O2 | C9 | C10A | -22.8(4) | |
Li11 | O2 | Li3 | O31 | -121.3(2) | Li4 | O2 | C9 | C10B | 20.4(8) | |
Li11 | O2 | Li3 | N11 | 84.0(4) | Li4 | O2 | Li3 | O11 | 45.4(4) | |
Li11 | O2 | Li3 | C51 | 6.2(2) | Li4 | O2 | Li3 | O31 | -55.8(4) | |
Li11 | O2 | Li3 | Li21 | -39.13(16) | Li4 | O2 | Li3 | N11 | 149.5(3) | |
Li11 | O2 | Li3 | Li2 | -133.2(2) | Li4 | O2 | Li3 | C51 | 71.7(4) | |
Li11 | O2 | Li3 | Li4 | -65.5(3) | Li4 | O2 | Li3 | Li11 | 65.5(3) | |
Li11 | O2 | Li3 | Li41 | -72.5(3) | Li4 | O2 | Li3 | Li21 | 26.3(3) | |
Li11 | O3 | C13 | C14 | 110.9(3) | Li4 | O2 | Li3 | Li2 | -67.8(3) | |
Li11 | O3 | Li4 | O1 | -122.0(2) | Li4 | O2 | Li3 | Li41 | -7.0(5) | |
Li11 | O3 | Li4 | O2 | -19.1(2) | Li4 | O3 | C13 | C14 | -158.6(3) | |
Li11 | O3 | Li4 | N2 | 84.6(3) | Li4 | N2 | C10A | C9 | -42.8(5) | |
Li11 | O3 | Li4 | Li21 | -65.6(3) | Li4 | N2 | C10B | C9 | 33.7(12) | |
Li11 | O3 | Li4 | Li2 | -72.5(3) | C11A | N2 | C10A | C9 | -166.0(4) | |
Li11 | O3 | Li4 | Li31 | -133.2(2) | C12A | N2 | C10A | C9 | 73.9(5) | |
Li11 | O3 | Li4 | Li3 | -38.81(16) | C11B | N2 | C10B | C9 | 169.6(11) | |
Li1 | C1 | C2 | C3 | -177.9(3) | C12B | N2 | C10B | C9 | -70.0(13) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H2A | 8427.35 | 1115.89 | 5370.68 | 41 |
H2B | 8876.15 | 1683.25 | 6144.02 | 41 |
H3A | 8021.51 | -770.77 | 5870.54 | 58 |
H3B | 8462.64 | -203.61 | 6645.52 | 58 |
H4A | 10095.07 | -635.02 | 5698.25 | 76 |
H4B | 10091.76 | -1404.17 | 6401.12 | 76 |
H4C | 10549.57 | -10.05 | 6459.08 | 76 |
H5A | 5156.93 | 4114.01 | 7039.44 | 41 |
H5B | 5381.13 | 2842.82 | 6676.27 | 41 |
H6A | 3418.39 | 2756.64 | 6968.08 | 49 |
H6B | 2998.4 | 4020.74 | 6569.33 | 49 |
H7A | 3137.12 | 881.4 | 5518.52 | 79 |
H7B | 3291.52 | 943.37 | 6359.2 | 79 |
H7C | 4406.28 | 1413.62 | 6006.39 | 79 |
H8A | 1249.15 | 3358.52 | 5793.08 | 77 |
H8B | 1381.99 | 2078.74 | 6203.39 | 77 |
H8C | 1200.41 | 2106.26 | 5360.44 | 77 |
H9AA | 5563.89 | 8537.11 | 5599.27 | 45 |
H9AB | 6088.89 | 7781.77 | 6311.19 | 45 |
H9BC | 6280.51 | 8102.52 | 6041.03 | 45 |
H9BD | 4932.96 | 8478.6 | 5573.97 | 45 |
H13A | 1520.82 | 6256.91 | 4460.43 | 38 |
H13B | 1278.67 | 5287.7 | 5036.47 | 38 |
H14A | 1227.71 | 3679.37 | 4244.41 | 47 |
H14B | 252.96 | 4700.86 | 3867.83 | 47 |
H15A | 1888.14 | 5697.26 | 2648.91 | 83 |
H15B | 2040.13 | 6383.81 | 3392.93 | 83 |
H15C | 683.98 | 5901.85 | 2985.66 | 83 |
H16A | 1603.55 | 2786.45 | 3237.89 | 81 |
H16B | 1891.71 | 3568.27 | 2592.64 | 81 |
H16C | 521.73 | 3617.48 | 2770.08 | 81 |
H10A | 4271.19 | 8735.05 | 6456.62 | 42 |
H10B | 3505.28 | 8299.44 | 5695.51 | 42 |
H11A | 2333.27 | 7793.65 | 6820.16 | 82 |
H11B | 2119.84 | 6362.54 | 6668.1 | 82 |
H11C | 1872.83 | 7313.77 | 6024.29 | 82 |
H12A | 5328.66 | 6596.98 | 7162.02 | 68 |
H12B | 4092.23 | 6081.86 | 7384.28 | 68 |
H12C | 4426.1 | 7506.53 | 7469.22 | 68 |
H10C | 4718.39 | 8575.94 | 6616.43 | 58 |
H10D | 5538.73 | 7383.03 | 6854.37 | 58 |
H11D | 4083.84 | 6332.58 | 7387.56 | 100 |
H11E | 2609.2 | 6383.21 | 7031.38 | 100 |
H11F | 3349.23 | 7610.1 | 7318.89 | 100 |
H12D | 2362.7 | 8426.06 | 6233.36 | 74 |
H12E | 1928.2 | 7253.38 | 5746.57 | 74 |
H12F | 2978.8 | 8154.04 | 5570.28 | 74 |
H1A | 6340(50) | 720(50) | 5600(30) | 71(15) |
H1B | 6900(40) | 1720(40) | 6230(30) | 51(13) |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
H9AA | 0.663(9) | H9AB | 0.663(9) | H9BC | 0.337(9) | ||
H9BD | 0.337(9) | C10A | 0.663(9) | H10A | 0.663(9) | ||
H10B | 0.663(9) | C11A | 0.663(9) | H11A | 0.663(9) | ||
H11B | 0.663(9) | H11C | 0.663(9) | C12A | 0.663(9) | ||
H12A | 0.663(9) | H12B | 0.663(9) | H12C | 0.663(9) | ||
C10B | 0.337(9) | H10C | 0.337(9) | H10D | 0.337(9) | ||
C11B | 0.337(9) | H11D | 0.337(9) | H11E | 0.337(9) | ||
H11F | 0.337(9) | C12B | 0.337(9) | H12D | 0.337(9) | ||
H12E | 0.337(9) | H12F | 0.337(9) |
Experimental
Single crystals of C16H39Li4N3O3 [cu_b0089_0m] were []. A suitable crystal was selected and [] on a diffractometer. The crystal was kept at 100.0 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 [cu_b0089_0m]
Crystal Data for C16H39Li4N3O3 (M =349.26 g/mol): monoclinic, space group P21/n (no. 14), a = 10.8656(4) Å, b = 10.9386(5) Å, c = 19.3571(8) Å, β = 102.672(2)°, V = 2244.64(16) Å3, Z = 4, T = 100.0 K, μ(CuKα) = 0.520 mm-1, Dcalc = 1.034 g/cm3, 35901 reflections measured (8.624° ≤ 2Θ ≤ 137.996°), 4026 unique (Rint = 0.0521, Rsigma = 0.0235) which were used in all calculations. The final R1 was 0.1116 (I > 2σ(I)) and wR2 was 0.4055 (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,H,H) groups
2. Others
Sof(H9BC)=Sof(H9BD)=Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11D)=
Sof(H11E)=Sof(H11F)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C11A)=Sof(H11A)=
Sof(H11B)=Sof(H11C)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C9(H9AA,H9AB), C9(H9BC,
H9BD), C13(H13A,H13B), C14(H14A,H14B), C10A(H10A,H10B), C10B(H10C,H10D)
3.b Idealised Me refined as rotating group:
C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C),
C16(H16A,H16B,H16C), C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12C), C11B(H11D,
H11E,H11F), C12B(H12D,H12E,H12F)
This report has been created with Olex2, compiled on 2018.05.29 svn.r3508 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.