Identification code | mo_B0314_0m |
Empirical formula | C34H76Li5N3O8 |
Formula weight | 689.67 |
Temperature/K | 99.98 |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 13.137(6) |
b/Å | 17.220(8) |
c/Å | 19.039(9) |
α/° | 90 |
β/° | 96.585(12) |
γ/° | 90 |
Volume/Å3 | 4279(4) |
Z | 4 |
ρcalcg/cm3 | 1.071 |
μ/mm‑1 | 0.072 |
F(000) | 1520.0 |
Crystal size/mm3 | 0.414 × 0.22 × 0.14 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.914 to 51.998 |
Index ranges | -16 ≤ h ≤ 16, -21 ≤ k ≤ 20, -23 ≤ l ≤ 21 |
Reflections collected | 41663 |
Independent reflections | 8397 [Rint = 0.0417, Rsigma = 0.0388] |
Data/restraints/parameters | 8397/0/521 |
Goodness-of-fit on F2 | 1.031 |
Final R indexes [I>=2σ (I)] | R1 = 0.0449, wR2 = 0.1106 |
Final R indexes [all data] | R1 = 0.0629, wR2 = 0.1212 |
Largest diff. peak/hole / e Å-3 | 0.34/-0.29 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
O3 | 7273.7(7) | 7560.4(6) | 2977.8(5) | 18.1(2) |
O8 | 5010.1(7) | 6454.1(6) | 2550.2(5) | 18.7(2) |
O5 | 5338.3(8) | 5635.5(6) | 4209.3(6) | 23.5(2) |
O6 | 3216.9(8) | 7791.9(6) | 1941.9(6) | 22.7(2) |
O2 | 9020.5(9) | 6137.6(6) | 3184.8(6) | 28.9(3) |
O7 | 1209.6(8) | 5265.3(7) | 749.2(6) | 30.4(3) |
O4 | 6614.2(8) | 8693.7(6) | 4436.5(6) | 25.6(2) |
O1 | 11393.5(8) | 8842.1(7) | 3388.8(6) | 31.2(3) |
N3 | 3548.4(9) | 6377.4(7) | 1300.3(6) | 19.4(3) |
N2 | 5639.1(9) | 7254.0(7) | 3989.3(6) | 18.9(3) |
N1 | 9319.2(9) | 7580.5(7) | 2577.6(7) | 19.9(3) |
C32 | 5116.4(11) | 5873.3(8) | 2046.8(8) | 20.0(3) |
C7 | 8395.9(11) | 7779.1(9) | 2088.7(8) | 20.0(3) |
C10 | 7801.3(12) | 8876.6(8) | 2842.9(8) | 22.1(3) |
C31 | 4649.6(11) | 6168.4(9) | 1323.0(8) | 20.4(3) |
C28 | 2890.6(11) | 5747.6(9) | 983.2(8) | 21.7(3) |
C26 | 3665.7(12) | 7813.3(9) | 1295.5(8) | 22.8(3) |
C34 | 4592.0(12) | 5128.0(9) | 2256.6(8) | 23.6(3) |
C8 | 7516.8(11) | 8103.7(8) | 2473.7(8) | 18.0(3) |
C18 | 5698.8(13) | 6900.1(9) | 4681.0(8) | 23.1(3) |
C25 | 3320.2(12) | 7093.1(9) | 885.5(8) | 21.9(3) |
C29 | 1818.7(12) | 5775.1(9) | 1203.7(8) | 23.7(3) |
C1 | 10071.6(11) | 8221.0(9) | 2646.6(8) | 23.0(3) |
C19 | 6081.9(12) | 6075.9(9) | 4655.1(8) | 24.0(3) |
C20 | 5629.3(14) | 4843.7(9) | 4173.8(9) | 29.8(4) |
C15 | 5097.8(12) | 7992.3(9) | 3985.5(9) | 24.6(3) |
C27 | 3297.5(13) | 8514.1(9) | 2307.8(9) | 27.8(4) |
C9 | 6600.8(11) | 8232.0(9) | 1914.9(8) | 23.7(3) |
C4 | 9831.7(12) | 6873.8(9) | 2353.6(9) | 26.0(4) |
C33 | 6252.1(12) | 5703.7(10) | 2001.1(9) | 28.3(4) |
C2 | 10662.6(11) | 8231.7(9) | 3372.8(8) | 24.4(3) |
C16 | 5556.9(13) | 8582.0(9) | 4521.1(9) | 28.6(4) |
C6 | 8740.9(14) | 5393.1(10) | 3416.6(11) | 37.7(4) |
C5 | 9252.5(13) | 6136.6(9) | 2476.7(9) | 29.1(4) |
C17 | 7164.8(15) | 9049.3(10) | 5037.2(9) | 33.7(4) |
C21 | 2917.1(13) | 6624.1(11) | 3390.8(10) | 30.9(4) |
C11 | 8630.3(12) | 7451.3(11) | 4569.4(9) | 28.3(4) |
C30 | 203.4(13) | 5192.5(12) | 938.2(10) | 39.2(4) |
C12 | 9548.6(13) | 6917(1) | 4758.0(9) | 28.2(4) |
C13 | 10222.7(13) | 7073.5(12) | 5448.0(9) | 37.1(4) |
C3 | 12018.2(13) | 8864.2(12) | 4045.4(10) | 38.5(4) |
C24 | 1612.0(16) | 4793.4(12) | 4113.1(12) | 48.6(5) |
C14 | 11109.3(15) | 6513.0(13) | 5602.3(12) | 50.7(6) |
C22 | 2086.6(19) | 6033.1(15) | 3489.0(12) | 22.9(7) |
C23 | 2484.9(18) | 5358.6(15) | 3946.5(14) | 27.2(7) |
Li5 | 3584.0(19) | 6761.2(14) | 2407.5(14) | 22.5(5) |
Li4 | 4602.3(19) | 6386.3(15) | 3497.2(13) | 23.4(5) |
Li1 | 8544.8(19) | 7177.8(15) | 3456.8(14) | 23.9(5) |
Li2 | 7145.1(19) | 7745.3(15) | 3977.2(13) | 23.7(5) |
Li3 | 6054.1(19) | 7042.9(15) | 3023.5(13) | 21.9(5) |
C22A | 2619(7) | 5732(5) | 3617(5) | 42(2) |
C23A | 1741(7) | 5616(5) | 3970(6) | 68(3) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
O3 | 19.3(5) | 16.8(5) | 18.7(5) | 0.9(4) | 3.7(4) | -0.6(4) |
O8 | 21.6(5) | 15.9(5) | 18.5(5) | -3.5(4) | 2.4(4) | -0.6(4) |
O5 | 30.6(6) | 15.3(5) | 24.0(6) | 0.9(4) | 0.4(4) | 0.9(4) |
O6 | 28.8(6) | 13.6(5) | 25.8(6) | -0.4(4) | 4.2(4) | -1.1(4) |
O2 | 34.1(6) | 15.5(5) | 37.6(7) | 1.6(5) | 6.7(5) | 1.8(5) |
O7 | 28.1(6) | 34.8(7) | 28.4(6) | -9.3(5) | 3.5(5) | -13.1(5) |
O4 | 33.6(6) | 21.5(6) | 22.8(6) | -6.3(5) | 7.2(5) | -4.6(5) |
O1 | 24.4(6) | 36.0(7) | 33.3(6) | -7.8(5) | 3.9(5) | -9.8(5) |
N3 | 22.3(6) | 14.8(6) | 20.3(6) | 0.9(5) | -1.2(5) | -2.5(5) |
N2 | 22.8(6) | 14.9(6) | 19.5(6) | -0.1(5) | 4.7(5) | 1.5(5) |
N1 | 17.5(6) | 17.8(6) | 24.5(7) | -2.8(5) | 3.3(5) | 0.6(5) |
C32 | 22.7(7) | 17.2(7) | 20.3(7) | -3.3(6) | 2.7(6) | 0.6(6) |
C7 | 22.8(7) | 19.7(8) | 17.9(7) | -0.9(6) | 3.8(6) | -0.7(6) |
C10 | 24.0(7) | 17.0(8) | 25.7(8) | -0.5(6) | 5.3(6) | 0.8(6) |
C31 | 24.0(7) | 16.9(7) | 20.6(8) | -3.0(6) | 4.1(6) | -1.4(6) |
C28 | 27.0(8) | 16.9(8) | 20.0(8) | -1.0(6) | -2.2(6) | -2.6(6) |
C26 | 25.8(8) | 17.9(8) | 24.5(8) | 3.0(6) | 2.2(6) | -1.8(6) |
C34 | 31.7(8) | 15.4(8) | 23.0(8) | 0.4(6) | -0.2(6) | 1.5(6) |
C8 | 19.3(7) | 16.0(7) | 19.0(7) | 0.7(6) | 3.5(6) | 0.1(6) |
C18 | 28.7(8) | 23.2(8) | 17.9(8) | -1.6(6) | 5.1(6) | -3.2(6) |
C25 | 26.5(8) | 18.6(8) | 19.9(8) | 3.8(6) | -0.9(6) | -1.9(6) |
C29 | 28.4(8) | 18.1(8) | 23.6(8) | -2.0(6) | -0.7(6) | -4.5(6) |
C1 | 19.2(7) | 23.3(8) | 27.2(8) | 0.8(7) | 6.0(6) | -2.3(6) |
C19 | 26.9(8) | 24.8(8) | 19.8(8) | 3.6(7) | -0.1(6) | -0.6(6) |
C20 | 41.8(10) | 18.0(8) | 30.1(9) | 3.9(7) | 6.5(7) | 3.9(7) |
C15 | 24.5(8) | 20.7(8) | 29.3(9) | -0.6(7) | 6.9(7) | 2.5(6) |
C27 | 34.2(9) | 16.4(8) | 32.3(9) | -4.4(7) | 2.0(7) | 0.0(6) |
C9 | 23.1(7) | 24.1(8) | 23.7(8) | 2.5(7) | 1.8(6) | 0.0(6) |
C4 | 25.0(8) | 23.7(8) | 30.1(9) | -3.8(7) | 6.2(7) | 5.6(6) |
C33 | 26.2(8) | 28.8(9) | 29.9(9) | -5.5(7) | 3.3(7) | 4.2(7) |
C2 | 19.2(7) | 25.7(8) | 28.5(8) | -3.1(7) | 3.8(6) | -0.6(6) |
C16 | 35.2(9) | 20.3(8) | 32.8(9) | -3.6(7) | 14.2(7) | 2.3(7) |
C6 | 37.4(10) | 21.1(9) | 52.0(12) | 9.1(8) | -5.9(8) | -3.0(7) |
C5 | 33.5(9) | 20.5(8) | 33.0(9) | -5.6(7) | 3.0(7) | 6.0(7) |
C17 | 50.8(11) | 24.2(9) | 25.4(9) | -6.5(7) | 2.2(8) | -6.3(8) |
C21 | 27.5(8) | 33.6(10) | 32.6(10) | 8.3(8) | 7.4(7) | -2.2(7) |
C11 | 25.7(8) | 36.2(10) | 23.0(8) | 0.0(7) | 2.3(7) | -0.9(7) |
C30 | 31.9(9) | 47.4(11) | 39(1) | -9.7(9) | 6.9(8) | -16.1(8) |
C12 | 28.1(8) | 29.6(9) | 25.5(9) | 5.4(7) | -2.8(7) | -5.1(7) |
C13 | 29.3(9) | 54.1(12) | 26.6(9) | 3.4(8) | -3.2(7) | -6.8(8) |
C3 | 27.3(9) | 49.7(12) | 37.5(10) | -15.5(9) | -0.3(8) | -3.1(8) |
C24 | 50.9(12) | 38.8(11) | 54.1(13) | 15.4(10) | -2.9(10) | -13.6(9) |
C14 | 42.4(11) | 50.3(13) | 53.6(13) | 20.0(11) | -19.5(10) | -9.0(9) |
C22 | 21.2(12) | 24.0(13) | 23.6(12) | 2.5(10) | 2.8(9) | 3(1) |
C23 | 25.3(14) | 24.9(14) | 31.4(13) | 6.3(11) | 3.6(10) | -0.6(10) |
Li5 | 22.6(12) | 17.0(12) | 27.9(14) | 0.9(11) | 2.9(10) | 0(1) |
Li4 | 26.2(13) | 20.7(13) | 23.4(13) | 2.0(11) | 3.6(10) | -0.9(10) |
Li1 | 24.7(13) | 23.1(13) | 23.9(13) | 0.9(11) | 3.1(10) | 3.7(10) |
Li2 | 25.3(13) | 24.4(13) | 21.6(13) | -4.3(11) | 3.1(10) | -1.2(10) |
Li3 | 22.7(12) | 21.6(13) | 21.6(13) | -1.8(10) | 3.2(10) | -2.7(10) |
C22A | 39(5) | 27(4) | 64(6) | 12(4) | 21(4) | 11(4) |
C23A | 45(5) | 60(6) | 109(8) | 48(6) | 45(5) | 16(4) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O3 | C8 | 1.4030(18) | N1 | C7 | 1.482(2) | |
O3 | Li1 | 1.925(3) | N1 | C1 | 1.4767(19) | |
O3 | Li2 | 1.956(3) | N1 | C4 | 1.4771(19) | |
O3 | Li3 | 1.844(3) | N1 | Li1 | 2.170(3) | |
O8 | C32 | 1.4033(18) | C32 | C31 | 1.529(2) | |
O8 | Li5 | 1.936(3) | C32 | C34 | 1.531(2) | |
O8 | Li4 | 1.942(3) | C32 | C33 | 1.532(2) | |
O8 | Li3 | 1.854(3) | C7 | C8 | 1.542(2) | |
O5 | C19 | 1.4352(19) | C10 | C8 | 1.531(2) | |
O5 | C20 | 1.4197(19) | C28 | C29 | 1.516(2) | |
O5 | Li4 | 2.036(3) | C26 | C25 | 1.507(2) | |
O6 | C26 | 1.4248(19) | C8 | C9 | 1.528(2) | |
O6 | C27 | 1.4235(19) | C18 | C19 | 1.509(2) | |
O6 | Li5 | 2.018(3) | C1 | C2 | 1.506(2) | |
O2 | C6 | 1.418(2) | C15 | C16 | 1.514(2) | |
O2 | C5 | 1.416(2) | C4 | C5 | 1.512(2) | |
O2 | Li1 | 1.985(3) | C21 | C22 | 1.519(3) | |
O7 | C29 | 1.4145(19) | C21 | Li5 | 2.169(3) | |
O7 | C30 | 1.415(2) | C21 | Li4 | 2.238(3) | |
O4 | C16 | 1.429(2) | C21 | C22A | 1.654(9) | |
O4 | C17 | 1.420(2) | C11 | C12 | 1.527(2) | |
O4 | Li2 | 2.014(3) | C11 | Li1 | 2.160(3) | |
O1 | C2 | 1.4217(19) | C11 | Li2 | 2.198(3) | |
O1 | C3 | 1.415(2) | C12 | C13 | 1.522(2) | |
N3 | C31 | 1.487(2) | C13 | C14 | 1.515(3) | |
N3 | C28 | 1.4723(19) | C24 | C23 | 1.564(3) | |
N3 | C25 | 1.4758(19) | C24 | C23A | 1.455(9) | |
N3 | Li5 | 2.204(3) | C22 | C23 | 1.509(4) | |
N2 | C18 | 1.445(2) | Li5 | Li4 | 2.424(4) | |
N2 | C15 | 1.456(2) | Li4 | Li3 | 2.475(4) | |
N2 | Li4 | 2.162(3) | Li1 | Li2 | 2.395(4) | |
N2 | Li2 | 2.154(3) | Li2 | Li3 | 2.493(4) | |
N2 | Li3 | 2.010(3) | C22A | C23A | 1.414(12) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C8 | O3 | Li1 | 107.41(11) | C22 | C21 | Li5 | 123.10(15) | |
C8 | O3 | Li2 | 127.50(12) | C22 | C21 | Li4 | 125.69(17) | |
C8 | O3 | Li3 | 128.44(12) | Li5 | C21 | Li4 | 66.71(11) | |
Li1 | O3 | Li2 | 76.22(11) | C22A | C21 | Li5 | 117.2(3) | |
Li3 | O3 | Li1 | 121.57(13) | C22A | C21 | Li4 | 93.9(4) | |
Li3 | O3 | Li2 | 81.97(11) | C12 | C11 | Li1 | 92.87(12) | |
C32 | O8 | Li5 | 105.63(11) | C12 | C11 | Li2 | 152.93(14) | |
C32 | O8 | Li4 | 130.60(12) | Li1 | C11 | Li2 | 66.67(11) | |
C32 | O8 | Li3 | 126.56(12) | C13 | C12 | C11 | 117.53(15) | |
Li5 | O8 | Li4 | 77.36(11) | C14 | C13 | C12 | 114.39(17) | |
Li3 | O8 | Li5 | 124.68(12) | C23 | C22 | C21 | 112.3(2) | |
Li3 | O8 | Li4 | 81.32(12) | C22 | C23 | C24 | 112.47(19) | |
C19 | O5 | Li4 | 107.30(11) | O8 | Li5 | O6 | 118.73(13) | |
C20 | O5 | C19 | 111.52(12) | O8 | Li5 | N3 | 88.07(11) | |
C20 | O5 | Li4 | 133.49(12) | O8 | Li5 | C21 | 109.23(13) | |
C26 | O6 | Li5 | 107.49(11) | O8 | Li5 | Li4 | 51.44(9) | |
C27 | O6 | C26 | 112.65(12) | O6 | Li5 | N3 | 82.29(10) | |
C27 | O6 | Li5 | 123.57(12) | O6 | Li5 | C21 | 112.03(13) | |
C6 | O2 | Li1 | 129.35(14) | O6 | Li5 | Li4 | 133.72(14) | |
C5 | O2 | C6 | 112.76(13) | N3 | Li5 | Li4 | 133.46(13) | |
C5 | O2 | Li1 | 110.98(12) | C21 | Li5 | N3 | 145.72(14) | |
C29 | O7 | C30 | 112.27(13) | C21 | Li5 | Li4 | 58.00(10) | |
C16 | O4 | Li2 | 109.22(11) | O8 | Li4 | O5 | 119.73(13) | |
C17 | O4 | C16 | 112.28(12) | O8 | Li4 | N2 | 97.68(12) | |
C17 | O4 | Li2 | 121.97(13) | O8 | Li4 | C21 | 106.28(13) | |
C3 | O1 | C2 | 111.14(13) | O8 | Li4 | Li5 | 51.19(9) | |
C31 | N3 | Li5 | 97.52(10) | O8 | Li4 | Li3 | 47.79(8) | |
C28 | N3 | C31 | 110.91(12) | O5 | Li4 | N2 | 85.57(11) | |
C28 | N3 | C25 | 108.78(12) | O5 | Li4 | C21 | 124.46(13) | |
C28 | N3 | Li5 | 124.06(11) | O5 | Li4 | Li5 | 155.87(15) | |
C25 | N3 | C31 | 110.79(11) | O5 | Li4 | Li3 | 101.88(12) | |
C25 | N3 | Li5 | 104.02(11) | N2 | Li4 | C21 | 118.71(13) | |
C18 | N2 | C15 | 110.37(12) | N2 | Li4 | Li5 | 116.45(13) | |
C18 | N2 | Li4 | 93.96(11) | N2 | Li4 | Li3 | 50.84(9) | |
C18 | N2 | Li2 | 102.79(12) | C21 | Li4 | Li5 | 55.29(10) | |
C18 | N2 | Li3 | 139.94(12) | C21 | Li4 | Li3 | 132.79(14) | |
C15 | N2 | Li4 | 108.56(12) | Li5 | Li4 | Li3 | 86.51(12) | |
C15 | N2 | Li2 | 96.06(12) | O3 | Li1 | O2 | 117.85(14) | |
C15 | N2 | Li3 | 109.68(12) | O3 | Li1 | N1 | 89.03(11) | |
Li2 | N2 | Li4 | 143.19(11) | O3 | Li1 | C11 | 109.55(13) | |
Li3 | N2 | Li4 | 72.66(11) | O3 | Li1 | Li2 | 52.47(9) | |
Li3 | N2 | Li2 | 73.47(11) | O2 | Li1 | N1 | 84.13(11) | |
C7 | N1 | Li1 | 97.81(11) | O2 | Li1 | C11 | 118.03(14) | |
C1 | N1 | C7 | 112.02(12) | O2 | Li1 | Li2 | 139.08(15) | |
C1 | N1 | C4 | 108.57(12) | N1 | Li1 | Li2 | 129.71(14) | |
C1 | N1 | Li1 | 122.57(12) | C11 | Li1 | N1 | 135.27(14) | |
C4 | N1 | C7 | 112.10(12) | C11 | Li1 | Li2 | 57.41(10) | |
C4 | N1 | Li1 | 103.23(12) | O3 | Li2 | O4 | 128.84(14) | |
O8 | C32 | C31 | 108.51(12) | O3 | Li2 | N2 | 97.37(12) | |
O8 | C32 | C34 | 109.65(12) | O3 | Li2 | C11 | 106.92(12) | |
O8 | C32 | C33 | 110.39(12) | O3 | Li2 | Li1 | 51.31(9) | |
C31 | C32 | C34 | 111.57(12) | O3 | Li2 | Li3 | 47.08(9) | |
C31 | C32 | C33 | 107.73(12) | O4 | Li2 | N2 | 87.11(11) | |
C34 | C32 | C33 | 108.98(13) | O4 | Li2 | C11 | 107.18(13) | |
N1 | C7 | C8 | 112.88(12) | O4 | Li2 | Li1 | 146.19(15) | |
N3 | C31 | C32 | 113.26(12) | O4 | Li2 | Li3 | 120.71(13) | |
N3 | C28 | C29 | 112.56(12) | N2 | Li2 | C11 | 131.80(14) | |
O6 | C26 | C25 | 107.23(12) | N2 | Li2 | Li1 | 126.43(14) | |
O3 | C8 | C7 | 108.97(12) | N2 | Li2 | Li3 | 50.61(9) | |
O3 | C8 | C10 | 109.17(12) | C11 | Li2 | Li1 | 55.92(10) | |
O3 | C8 | C9 | 110.48(12) | C11 | Li2 | Li3 | 131.62(14) | |
C10 | C8 | C7 | 112.12(12) | Li1 | Li2 | Li3 | 84.57(12) | |
C9 | C8 | C7 | 107.11(12) | O3 | Li3 | O8 | 147.09(15) | |
C9 | C8 | C10 | 108.97(12) | O3 | Li3 | N2 | 106.50(13) | |
N2 | C18 | C19 | 110.51(13) | O3 | Li3 | Li4 | 161.46(15) | |
N3 | C25 | C26 | 112.29(12) | O3 | Li3 | Li2 | 50.95(9) | |
O7 | C29 | C28 | 106.82(12) | O8 | Li3 | N2 | 106.28(13) | |
N1 | C1 | C2 | 111.10(12) | O8 | Li3 | Li4 | 50.89(9) | |
O5 | C19 | C18 | 108.02(13) | O8 | Li3 | Li2 | 161.91(15) | |
N2 | C15 | C16 | 115.18(14) | N2 | Li3 | Li4 | 56.50(9) | |
N1 | C4 | C5 | 113.13(13) | N2 | Li3 | Li2 | 55.92(9) | |
O1 | C2 | C1 | 107.73(13) | Li4 | Li3 | Li2 | 111.04(13) | |
O4 | C16 | C15 | 109.35(12) | C23A | C22A | C21 | 119.0(7) | |
O2 | C5 | C4 | 108.28(13) | C22A | C23A | C24 | 110.3(7) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
O8 | C32 | C31 | N3 | -58.83(15) | Li5 | O8 | Li3 | Li2 | 65.7(5) | |
O6 | C26 | C25 | N3 | -54.16(16) | Li5 | O6 | C26 | C25 | 53.44(15) | |
N3 | C28 | C29 | O7 | 166.97(12) | Li5 | N3 | C31 | C32 | 31.58(14) | |
N2 | C18 | C19 | O5 | -64.27(16) | Li5 | N3 | C28 | C29 | 41.78(18) | |
N2 | C15 | C16 | O4 | 53.89(18) | Li5 | N3 | C25 | C26 | 26.16(15) | |
N1 | C7 | C8 | O3 | -56.90(15) | Li5 | C21 | C22 | C23 | 107.0(2) | |
N1 | C7 | C8 | C10 | 64.07(16) | Li5 | C21 | C22A | C23A | -144.9(8) | |
N1 | C7 | C8 | C9 | -176.44(12) | Li4 | O8 | C32 | C31 | 136.81(14) | |
N1 | C1 | C2 | O1 | 177.83(11) | Li4 | O8 | C32 | C34 | 14.73(19) | |
N1 | C4 | C5 | O2 | -50.61(17) | Li4 | O8 | C32 | C33 | -105.35(16) | |
C32 | O8 | Li3 | O3 | 38.2(3) | Li4 | O8 | Li3 | O3 | 173.1(3) | |
C32 | O8 | Li3 | N2 | -146.83(12) | Li4 | O8 | Li3 | N2 | -11.89(13) | |
C32 | O8 | Li3 | Li4 | -134.94(15) | Li4 | O8 | Li3 | Li2 | -2.2(5) | |
C32 | O8 | Li3 | Li2 | -137.2(4) | Li4 | O5 | C19 | C18 | 27.88(15) | |
C7 | N1 | C1 | C2 | 148.51(12) | Li4 | N2 | C18 | C19 | 58.18(14) | |
C7 | N1 | C4 | C5 | -73.15(17) | Li4 | N2 | C15 | C16 | 159.26(13) | |
C31 | N3 | C28 | C29 | 157.08(12) | Li4 | C21 | C22 | C23 | 23.5(3) | |
C31 | N3 | C25 | C26 | -77.67(15) | Li4 | C21 | C22A | C23A | 149.3(9) | |
C28 | N3 | C31 | C32 | -99.36(14) | Li1 | O3 | C8 | C7 | 43.69(15) | |
C28 | N3 | C25 | C26 | 160.15(12) | Li1 | O3 | C8 | C10 | -79.06(14) | |
C34 | C32 | C31 | N3 | 62.07(16) | Li1 | O3 | C8 | C9 | 161.12(12) | |
C8 | O3 | Li3 | O8 | 49.6(3) | Li1 | O3 | Li3 | O8 | -109.8(3) | |
C8 | O3 | Li3 | N2 | -125.43(14) | Li1 | O3 | Li3 | N2 | 75.20(17) | |
C8 | O3 | Li3 | Li4 | -147.5(4) | Li1 | O3 | Li3 | Li4 | 53.2(5) | |
C8 | O3 | Li3 | Li2 | -132.30(15) | Li1 | O3 | Li3 | Li2 | 68.34(14) | |
C18 | N2 | C15 | C16 | 57.58(17) | Li1 | O2 | C5 | C4 | 42.82(17) | |
C25 | N3 | C31 | C32 | 139.72(13) | Li1 | N1 | C7 | C8 | 35.11(14) | |
C25 | N3 | C28 | C29 | -80.82(15) | Li1 | N1 | C1 | C2 | 32.90(18) | |
C1 | N1 | C7 | C8 | -94.79(14) | Li1 | N1 | C4 | C5 | 31.09(16) | |
C1 | N1 | C4 | C5 | 162.57(13) | Li1 | C11 | C12 | C13 | 158.07(15) | |
C20 | O5 | C19 | C18 | -178.28(12) | Li2 | O3 | C8 | C7 | 129.44(14) | |
C15 | N2 | C18 | C19 | 169.65(13) | Li2 | O3 | C8 | C10 | 6.69(18) | |
C27 | O6 | C26 | C25 | -167.12(12) | Li2 | O3 | C8 | C9 | -113.13(15) | |
C4 | N1 | C7 | C8 | 142.87(12) | Li2 | O3 | Li3 | O8 | -178.1(3) | |
C4 | N1 | C1 | C2 | -87.17(15) | Li2 | O3 | Li3 | N2 | 6.86(13) | |
C33 | C32 | C31 | N3 | -178.35(12) | Li2 | O3 | Li3 | Li4 | -15.2(5) | |
C6 | O2 | C5 | C4 | -163.36(13) | Li2 | O4 | C16 | C15 | -24.00(17) | |
C17 | O4 | C16 | C15 | -162.47(13) | Li2 | N2 | C18 | C19 | -88.82(14) | |
C21 | C22 | C23 | C24 | 174.08(18) | Li2 | N2 | C15 | C16 | -48.50(15) | |
C21 | C22A | C23A | C24 | 179.4(6) | Li2 | C11 | C12 | C13 | -162.6(3) | |
C11 | C12 | C13 | C14 | 179.27(16) | Li3 | O3 | C8 | C7 | -117.96(15) | |
C30 | O7 | C29 | C28 | 175.33(14) | Li3 | O3 | C8 | C10 | 119.28(15) | |
C3 | O1 | C2 | C1 | -176.94(13) | Li3 | O3 | C8 | C9 | -0.54(19) | |
Li5 | O8 | C32 | C31 | 50.21(14) | Li3 | O8 | C32 | C31 | -110.36(15) | |
Li5 | O8 | C32 | C34 | -71.86(14) | Li3 | O8 | C32 | C34 | 127.57(14) | |
Li5 | O8 | C32 | C33 | 168.06(13) | Li3 | O8 | C32 | C33 | 7.49(19) | |
Li5 | O8 | Li3 | O3 | -118.9(3) | Li3 | N2 | C18 | C19 | -9.4(2) | |
Li5 | O8 | Li3 | N2 | 56.10(18) | Li3 | N2 | C15 | C16 | -123.08(14) | |
Li5 | O8 | Li3 | Li4 | 67.99(14) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H7A | 8153 | 7308 | 1822 | 24 |
H7B | 8583 | 8169 | 1744 | 24 |
H10A | 7212 | 9075 | 3060 | 33 |
H10B | 7995 | 9253 | 2495 | 33 |
H10C | 8379 | 8797 | 3210 | 33 |
H31A | 5037 | 6631 | 1195 | 24 |
H31B | 4724 | 5762 | 965 | 24 |
H28A | 3208 | 5242 | 1126 | 26 |
H28B | 2847 | 5785 | 462 | 26 |
H26A | 4422 | 7823 | 1392 | 27 |
H26B | 3439 | 8284 | 1022 | 27 |
H34A | 4938 | 4936 | 2707 | 35 |
H34B | 4630 | 4734 | 1889 | 35 |
H34C | 3872 | 5237 | 2308 | 35 |
H25A | 2573 | 7125 | 742 | 26 |
H25B | 3666 | 7069 | 451 | 26 |
H29A | 1827 | 5607 | 1702 | 28 |
H29B | 1542 | 6310 | 1158 | 28 |
H1A | 9710 | 8722 | 2558 | 28 |
H1B | 10554 | 8159 | 2287 | 28 |
H19A | 6751 | 6065 | 4463 | 29 |
H19B | 6174 | 5851 | 5137 | 29 |
H20A | 6268 | 4805 | 3956 | 45 |
H20B | 5088 | 4554 | 3889 | 45 |
H20C | 5733 | 4626 | 4652 | 45 |
H27A | 4020 | 8665 | 2398 | 42 |
H27B | 3010 | 8462 | 2758 | 42 |
H27C | 2918 | 8913 | 2019 | 42 |
H9A | 6403 | 7737 | 1684 | 36 |
H9B | 6788 | 8603 | 1561 | 36 |
H9C | 6024 | 8438 | 2141 | 36 |
H4A | 10526 | 6841 | 2616 | 31 |
H4B | 9911 | 6916 | 1844 | 31 |
H33A | 6593 | 6178 | 1866 | 42 |
H33B | 6314 | 5300 | 1646 | 42 |
H33C | 6575 | 5525 | 2462 | 42 |
H2A | 10192 | 8321 | 3735 | 29 |
H2B | 11014 | 7728 | 3472 | 29 |
H16A | 5185 | 9081 | 4451 | 34 |
H16B | 5491 | 8395 | 5006 | 34 |
H6A | 8171 | 5190 | 3092 | 57 |
H6B | 8531 | 5434 | 3893 | 57 |
H6C | 9328 | 5041 | 3426 | 57 |
H5A | 8613 | 6113 | 2148 | 35 |
H5B | 9676 | 5678 | 2392 | 35 |
H17A | 6808 | 9522 | 5157 | 51 |
H17B | 7856 | 9182 | 4931 | 51 |
H17C | 7210 | 8689 | 5438 | 51 |
H30A | -191 | 4839 | 608 | 59 |
H30B | -127 | 5703 | 918 | 59 |
H30C | 232 | 4985 | 1419 | 59 |
H13A | 10500 | 7607 | 5434 | 45 |
H13B | 9792 | 7050 | 5842 | 45 |
H3A | 12518 | 9286 | 4041 | 58 |
H3B | 12380 | 8369 | 4124 | 58 |
H3C | 11589 | 8953 | 4426 | 58 |
H24A | 1907 | 4367 | 4410 | 73 |
H24B | 1116 | 5076 | 4363 | 73 |
H24C | 1266 | 4583 | 3670 | 73 |
H24D | 1002 | 4720 | 4358 | 73 |
H24E | 1530 | 4505 | 3666 | 73 |
H24F | 2217 | 4601 | 4412 | 73 |
H14A | 11579 | 6569 | 5241 | 76 |
H14B | 10847 | 5980 | 5597 | 76 |
H14C | 11475 | 6628 | 6069 | 76 |
H22A | 1528 | 6292 | 3708 | 27 |
H22B | 1796 | 5835 | 3020 | 27 |
H23A | 2841 | 5560 | 4396 | 33 |
H23B | 2991 | 5067 | 3703 | 33 |
H15A | 4369(14) | 7930(10) | 4073(9) | 29(5) |
H21A | 3160(16) | 6812(12) | 3898(12) | 52(6) |
H21B | 2528(19) | 7085(15) | 3158(13) | 72(7) |
H18A | 6173(12) | 7160(9) | 5050(9) | 21(4) |
H15B | 5069(12) | 8226(10) | 3504(9) | 25(4) |
H18B | 5008(12) | 6895(9) | 4876(8) | 20(4) |
H12A | 10055(15) | 6918(11) | 4394(10) | 37(5) |
H12B | 9307(14) | 6349(12) | 4784(10) | 39(5) |
H11A | 8193(15) | 7393(11) | 4947(10) | 38(5) |
H11B | 8896(15) | 8019(12) | 4632(11) | 48(6) |
H22C | 2535 | 5415 | 3180 | 51 |
H22D | 3215 | 5519 | 3922 | 51 |
H23C | 1128 | 5813 | 3673 | 82 |
H23D | 1815 | 5909 | 4420 | 82 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
H24A | 0.732(5) | H24B | 0.732(5) | H24C | 0.732(5) | ||
H24D | 0.268(5) | H24E | 0.268(5) | H24F | 0.268(5) | ||
C22 | 0.732(5) | H22A | 0.732(5) | H22B | 0.732(5) | ||
C23 | 0.732(5) | H23A | 0.732(5) | H23B | 0.732(5) | ||
C22A | 0.268(5) | H22C | 0.268(5) | H22D | 0.268(5) | ||
C23A | 0.268(5) | H23C | 0.268(5) | H23D | 0.268(5) |
Experimental
Single crystals of C34H76Li5N3O8 [mo_B0314_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_B0314_0m]
Crystal Data for C34H76Li5N3O8 (M =689.67 g/mol): monoclinic, space group P21/c (no. 14), a = 13.137(6) Å, b = 17.220(8) Å, c = 19.039(9) Å, β = 96.585(12)°, V = 4279(4) Å3, Z = 4, T = 99.98 K, μ(MoKα) = 0.072 mm-1, Dcalc = 1.071 g/cm3, 41663 reflections measured (4.914° ≤ 2Θ ≤ 51.998°), 8397 unique (Rint = 0.0417, Rsigma = 0.0388) which were used in all calculations. The final R1 was 0.0449 (I > 2σ(I)) and wR2 was 0.1212 (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, All C(H,H,H,H,H,H) groups
2. Others
Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=
Sof(H23C)=Sof(H23D)=1-FVAR(1)
Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=
Sof(H23B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C7(H7A,H7B), C31(H31A,H31B), C28(H28A,H28B), C26(H26A,H26B), C25(H25A,H25B),
C29(H29A,H29B), C1(H1A,H1B), C19(H19A,H19B), C4(H4A,H4B), C2(H2A,H2B),
C16(H16A,H16B), C5(H5A,H5B), C13(H13A,H13B), C22(H22A,H22B), C23(H23A,H23B),
C22A(H22C,H22D), C23A(H23C,H23D)
3.b Me refined with riding coordinates:
C24(H24A,H24B,H24C), C24(H24D,H24E,H24F)
3.c Idealised Me refined as rotating group:
C10(H10A,H10B,H10C), C34(H34A,H34B,H34C), C20(H20A,H20B,H20C), C27(H27A,H27B,
H27C), C9(H9A,H9B,H9C), C33(H33A,H33B,H33C), C6(H6A,H6B,H6C), C17(H17A,H17B,
H17C), C30(H30A,H30B,H30C), C3(H3A,H3B,H3C), C14(H14A,H14B,H14C)
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.