Identification code | mo_B0334_0m |
Empirical formula | C8H19Li2NO2 |
Formula weight | 175.12 |
Temperature/K | 99.99 |
Crystal system | tetragonal |
Space group | P42/n |
a/Å | 12.998(4) |
b/Å | 12.998(4) |
c/Å | 13.199(4) |
α/° | 90 |
β/° | 90 |
γ/° | 90 |
Volume/Å3 | 2230.1(15) |
Z | 8 |
ρcalcg/cm3 | 1.043 |
μ/mm‑1 | 0.069 |
F(000) | 768.0 |
Crystal size/mm3 | 0.36 × 0.21 × 0.2 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 5.4 to 51.986 |
Index ranges | -16 ≤ h ≤ 15, -12 ≤ k ≤ 16, -16 ≤ l ≤ 15 |
Reflections collected | 7719 |
Independent reflections | 2175 [Rint = 0.0264, Rsigma = 0.0247] |
Data/restraints/parameters | 2175/0/132 |
Goodness-of-fit on F2 | 1.108 |
Final R indexes [I>=2σ (I)] | R1 = 0.0440, wR2 = 0.1132 |
Final R indexes [all data] | R1 = 0.0551, wR2 = 0.1190 |
Largest diff. peak/hole / e Å-3 | 0.23/-0.16 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
O1 | 2806.8(7) | 4085.5(7) | 8062.6(7) | 19.3(3) |
O2 | 2492.7(8) | 3612.9(8) | 5565.2(7) | 21.9(3) |
N1 | 2596.8(10) | 4981.4(10) | 9976.3(10) | 27.6(3) |
C1 | 3245.7(11) | 5070.0(11) | 8144.8(12) | 23.0(4) |
C4 | 3393.9(12) | 5362.6(13) | 9272.5(13) | 28.3(4) |
C3 | 4321.5(13) | 5079.2(13) | 7657.2(14) | 33.3(4) |
C6 | 1612.6(14) | 5511.5(15) | 9844.0(15) | 39.7(5) |
C2 | 2600.7(14) | 5873.1(12) | 7566.8(13) | 33.0(4) |
C8 | 2793.8(17) | 4174.6(18) | 3839.3(14) | 49.1(5) |
C5 | 2955.8(17) | 5137.6(17) | 11014.6(14) | 46.6(5) |
C7 | 2549.6(17) | 4439.3(14) | 4912.5(14) | 42.7(5) |
Li2 | 3484.4(19) | 2526.1(19) | 5609.5(19) | 23.9(5) |
Li1 | 2043.9(19) | 3766.9(19) | 6910.7(19) | 22.7(5) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
O1 | 21.1(5) | 17.3(5) | 19.6(5) | -2.1(4) | -2.0(4) | -1.7(4) |
O2 | 25.9(6) | 20.5(5) | 19.3(5) | 4.7(4) | -0.8(4) | -2.3(4) |
N1 | 28.6(7) | 31.0(7) | 23.1(7) | -9.3(6) | -3.2(5) | 4.2(5) |
C1 | 23.8(8) | 17.7(7) | 27.4(8) | -2.2(6) | -2.1(6) | -0.6(5) |
C4 | 25.8(8) | 25.3(8) | 33.9(9) | -7.6(7) | -5.0(7) | -1.1(6) |
C3 | 28.0(9) | 29.3(9) | 42.7(10) | -2.4(7) | 5.1(7) | -5.6(7) |
C6 | 34.0(9) | 41.3(10) | 43.9(10) | -5.3(8) | 5.1(8) | 10.5(8) |
C2 | 39.3(10) | 22.0(8) | 37.7(9) | 1.7(7) | -6.9(8) | 2.3(7) |
C8 | 57.5(13) | 62.6(13) | 27.2(9) | 17.3(9) | 2.1(9) | -3.6(10) |
C5 | 54.6(12) | 56.0(12) | 29.4(10) | -16.5(9) | -8.5(9) | -2.1(9) |
C7 | 71.6(14) | 25.9(9) | 30.6(9) | 9.2(7) | 2.9(9) | -5.8(8) |
Li2 | 23.8(12) | 26.0(13) | 22.0(12) | 0.3(10) | 2.7(10) | -2(1) |
Li1 | 23.5(12) | 22.8(12) | 21.7(12) | -0.1(10) | -2.9(10) | -1.2(9) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O1 | C1 | 1.4053(17) | C8 | C7 | 1.492(3) | |
O1 | Li21 | 1.967(3) | Li2 | O12 | 1.967(3) | |
O1 | Li12 | 1.927(3) | Li2 | O23 | 1.952(3) | |
O1 | Li1 | 1.862(3) | Li2 | N12 | 2.100(3) | |
O2 | C7 | 1.379(2) | Li2 | C42 | 2.723(3) | |
O2 | Li2 | 1.913(3) | Li2 | Li23 | 2.560(5) | |
O2 | Li23 | 1.952(3) | Li2 | Li1 | 3.009(4) | |
O2 | Li1 | 1.880(3) | Li2 | Li13 | 2.499(3) | |
N1 | C4 | 1.477(2) | Li2 | Li12 | 3.341(4) | |
N1 | C6 | 1.463(2) | Li1 | O11 | 1.927(3) | |
N1 | C5 | 1.462(2) | Li1 | Li21 | 3.341(4) | |
N1 | Li21 | 2.100(3) | Li1 | Li23 | 2.499(3) | |
C1 | C4 | 1.548(2) | Li1 | Li12 | 2.924(4) | |
C1 | C3 | 1.539(2) | Li1 | Li13 | 3.500(5) | |
C1 | C2 | 1.541(2) | Li1 | Li11 | 2.923(4) | |
C4 | Li21 | 2.723(3) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C1 | O1 | Li21 | 112.47(11) | N12 | Li2 | Li23 | 157.56(9) | |
C1 | O1 | Li12 | 115.43(11) | N12 | Li2 | Li13 | 117.16(13) | |
C1 | O1 | Li1 | 118.81(11) | N12 | Li2 | Li1 | 145.84(12) | |
Li12 | O1 | Li21 | 79.84(11) | N12 | Li2 | Li12 | 105.76(11) | |
Li1 | O1 | Li21 | 121.47(12) | C42 | Li2 | Li1 | 139.51(11) | |
Li1 | O1 | Li12 | 100.98(13) | C42 | Li2 | Li12 | 85.35(8) | |
C7 | O2 | Li2 | 123.92(13) | Li23 | Li2 | C42 | 152.20(16) | |
C7 | O2 | Li23 | 130.14(13) | Li23 | Li2 | Li1 | 52.57(9) | |
C7 | O2 | Li1 | 121.59(13) | Li23 | Li2 | Li12 | 96.56(6) | |
Li2 | O2 | Li23 | 82.96(12) | Li13 | Li2 | C42 | 84.94(10) | |
Li1 | O2 | Li2 | 105.00(11) | Li13 | Li2 | Li23 | 72.99(10) | |
Li1 | O2 | Li23 | 81.40(11) | Li1 | Li2 | Li12 | 54.52(7) | |
C4 | N1 | Li21 | 97.62(11) | Li13 | Li2 | Li12 | 57.96(8) | |
C6 | N1 | C4 | 112.34(13) | Li13 | Li2 | Li1 | 78.30(12) | |
C6 | N1 | Li21 | 109.02(13) | O1 | Li1 | O11 | 122.33(13) | |
C5 | N1 | C4 | 108.61(14) | O1 | Li1 | O2 | 129.04(14) | |
C5 | N1 | C6 | 108.99(14) | O1 | Li1 | Li23 | 149.00(14) | |
C5 | N1 | Li21 | 119.88(14) | O11 | Li1 | Li23 | 50.79(9) | |
O1 | C1 | C4 | 110.39(12) | O1 | Li1 | Li21 | 30.15(7) | |
O1 | C1 | C3 | 110.09(12) | O11 | Li1 | Li21 | 92.20(10) | |
O1 | C1 | C2 | 110.96(12) | O1 | Li1 | Li2 | 104.70(12) | |
C3 | C1 | C4 | 106.68(13) | O11 | Li1 | Li2 | 97.90(10) | |
C3 | C1 | C2 | 106.38(13) | O11 | Li1 | Li11 | 38.70(8) | |
C2 | C1 | C4 | 112.16(13) | O11 | Li1 | Li13 | 69.44(9) | |
N1 | C4 | C1 | 115.78(12) | O1 | Li1 | Li13 | 91.66(9) | |
N1 | C4 | Li21 | 49.85(9) | O11 | Li1 | Li12 | 109.90(9) | |
C1 | C4 | Li21 | 77.30(10) | O1 | Li1 | Li11 | 85.87(12) | |
O2 | C7 | C8 | 115.15(16) | O1 | Li1 | Li12 | 40.33(10) | |
O12 | Li2 | N12 | 86.75(11) | O2 | Li1 | O11 | 100.65(12) | |
O12 | Li2 | C42 | 59.76(8) | O2 | Li1 | Li2 | 37.89(7) | |
O12 | Li2 | Li23 | 113.03(8) | O2 | Li1 | Li23 | 50.54(9) | |
O12 | Li2 | Li1 | 81.75(10) | O2 | Li1 | Li21 | 149.53(12) | |
O12 | Li2 | Li12 | 28.38(6) | O2 | Li1 | Li11 | 122.21(13) | |
O12 | Li2 | Li13 | 49.38(9) | O2 | Li1 | Li13 | 78.15(8) | |
O2 | Li2 | O12 | 117.21(13) | O2 | Li1 | Li12 | 103.10(12) | |
O23 | Li2 | O12 | 96.79(11) | Li23 | Li1 | Li21 | 130.19(12) | |
O2 | Li2 | O23 | 96.93(12) | Li23 | Li1 | Li2 | 54.44(11) | |
O23 | Li2 | N12 | 122.30(13) | Li2 | Li1 | Li21 | 113.34(10) | |
O2 | Li2 | N12 | 132.01(14) | Li23 | Li1 | Li11 | 75.61(10) | |
O23 | Li2 | C42 | 104.60(11) | Li21 | Li1 | Li13 | 80.79(6) | |
O2 | Li2 | C42 | 158.45(13) | Li23 | Li1 | Li12 | 109.50(10) | |
O2 | Li2 | Li23 | 49.16(9) | Li23 | Li1 | Li13 | 57.34(8) | |
O23 | Li2 | Li23 | 47.88(9) | Li2 | Li1 | Li13 | 44.36(7) | |
O23 | Li2 | Li1 | 91.07(10) | Li11 | Li1 | Li2 | 96.74(8) | |
O2 | Li2 | Li13 | 109.41(12) | Li12 | Li1 | Li2 | 68.52(9) | |
O23 | Li2 | Li12 | 103.17(10) | Li11 | Li1 | Li21 | 56.96(9) | |
O2 | Li2 | Li12 | 88.88(10) | Li12 | Li1 | Li21 | 46.44(9) | |
O2 | Li2 | Li1 | 37.11(7) | Li12 | Li1 | Li13 | 53.23(4) | |
O23 | Li2 | Li13 | 48.05(8) | Li11 | Li1 | Li13 | 53.23(4) | |
N12 | Li2 | C42 | 32.52(6) | Li11 | Li1 | Li12 | 73.55(8) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
O1 | C1 | C4 | N1 | -34.79(17) | Li21 | O1 | Li1 | Li13 | -84.72(16) | |
O1 | C1 | C4 | Li21 | -2.23(11) | Li21 | O1 | Li1 | Li12 | -68.37(14) | |
C1 | O1 | Li1 | O11 | -149.79(14) | Li2 | O2 | C7 | C8 | 46.0(2) | |
C1 | O1 | Li1 | O2 | 67.6(2) | Li22 | O2 | C7 | C8 | -66.0(2) | |
C1 | O1 | Li1 | Li21 | -147.99(18) | Li2 | O2 | Li1 | O1 | 59.3(2) | |
C1 | O1 | Li1 | Li22 | 143.7(2) | Li22 | O2 | Li1 | O1 | 139.63(19) | |
C1 | O1 | Li1 | Li2 | 100.69(13) | Li2 | O2 | Li1 | O11 | -89.20(12) | |
C1 | O1 | Li1 | Li13 | 127.29(12) | Li22 | O2 | Li1 | O11 | -8.92(11) | |
C1 | O1 | Li1 | Li12 | 143.64(10) | Li22 | O2 | Li1 | Li21 | 104.4(3) | |
C1 | O1 | Li1 | Li11 | -163.42(10) | Li2 | O2 | Li1 | Li21 | 24.2(3) | |
C3 | C1 | C4 | N1 | -154.39(13) | Li22 | O2 | Li1 | Li2 | 80.28(12) | |
C3 | C1 | C4 | Li21 | -121.83(12) | Li2 | O2 | Li1 | Li22 | -80.28(12) | |
C6 | N1 | C4 | C1 | -70.86(17) | Li22 | O2 | Li1 | Li13 | 104.62(11) | |
C6 | N1 | C4 | Li21 | -114.23(15) | Li2 | O2 | Li1 | Li13 | 24.34(13) | |
C2 | C1 | C4 | N1 | 89.51(16) | Li22 | O2 | Li1 | Li11 | 25.98(14) | |
C2 | C1 | C4 | Li21 | 122.07(13) | Li2 | O2 | Li1 | Li11 | -54.30(16) | |
C5 | N1 | C4 | C1 | 168.50(14) | Li2 | O2 | Li1 | Li12 | -23.07(11) | |
C5 | N1 | C4 | Li21 | 125.13(16) | Li22 | O2 | Li1 | Li12 | 57.21(10) | |
C7 | O2 | Li1 | O11 | 123.34(15) | Li21 | N1 | C4 | C1 | 43.38(15) | |
C7 | O2 | Li1 | O1 | -88.1(2) | Li1 | O1 | C1 | C4 | 153.97(13) | |
C7 | O2 | Li1 | Li22 | 132.25(16) | Li13 | O1 | C1 | C4 | -85.89(14) | |
C7 | O2 | Li1 | Li2 | -147.46(18) | Li13 | O1 | C1 | C3 | 31.63(17) | |
C7 | O2 | Li1 | Li21 | -123.3(2) | Li1 | O1 | C1 | C3 | -88.51(16) | |
C7 | O2 | Li1 | Li11 | 158.24(14) | Li1 | O1 | C1 | C2 | 28.99(18) | |
C7 | O2 | Li1 | Li13 | -123.13(13) | Li13 | O1 | C1 | C2 | 149.13(13) | |
C7 | O2 | Li1 | Li12 | -170.53(13) | Li13 | O1 | Li1 | O11 | 82.92(8) | |
Li21 | O1 | C1 | C4 | 3.26(16) | Li13 | O1 | Li1 | O2 | -59.7(2) | |
Li21 | O1 | C1 | C3 | 120.78(14) | Li13 | O1 | Li1 | Li2 | -26.60(13) | |
Li21 | O1 | C1 | C2 | -121.72(14) | Li13 | O1 | Li1 | Li21 | 84.72(16) | |
Li21 | O1 | Li1 | O11 | -1.8(2) | Li13 | O1 | Li1 | Li22 | 16.5(3) | |
Li21 | O1 | Li1 | O2 | -144.43(15) | Li13 | O1 | Li1 | Li11 | 69.30(8) | |
Li21 | O1 | Li1 | Li2 | -111.32(15) | Li13 | O1 | Li1 | Li12 | 16.35(9) | |
Li21 | O1 | Li1 | Li22 | -68.3(3) | Li1 | O2 | C7 | C8 | -172.76(16) | |
Li21 | O1 | Li1 | Li11 | -15.42(14) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H3A | 4760 | 4571 | 7995 | 50 |
H3B | 4627 | 5765 | 7730 | 50 |
H3C | 4263 | 4908 | 6936 | 50 |
H6A | 1721 | 6257 | 9883 | 60 |
H6B | 1136 | 5298 | 10379 | 60 |
H6C | 1322 | 5335 | 9181 | 60 |
H2A | 2596 | 5703 | 6843 | 49 |
H2B | 2902 | 6557 | 7663 | 49 |
H2C | 1894 | 5870 | 7827 | 49 |
H8A | 2827 | 4806 | 3435 | 74 |
H8B | 2256 | 3724 | 3568 | 74 |
H8C | 3459 | 3820 | 3810 | 74 |
H5A | 3618 | 4789 | 11108 | 70 |
H5B | 2451 | 4853 | 11489 | 70 |
H5C | 3039 | 5875 | 11143 | 70 |
H7A | 3082 | 4919 | 5166 | 51 |
H7B | 1883 | 4808 | 4928 | 51 |
H4A | 3460(15) | 6142(16) | 9361(14) | 40(5) |
H4B | 4059(15) | 5024(14) | 9528(13) | 32(5) |
Experimental
Single crystals of C8H19Li2NO2 [mo_B0334_0m] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD 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 XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0334_0m]
Crystal Data for C8H19Li2NO2 (M =175.12 g/mol): tetragonal, space group P42/n (no. 86), a = 12.998(4) Å, c = 13.199(4) Å, V = 2230.1(15) Å3, Z = 8, T = 99.99 K, μ(MoKα) = 0.069 mm-1, Dcalc = 1.043 g/cm3, 7719 reflections measured (5.4° ≤ 2Θ ≤ 51.986°), 2175 unique (Rint = 0.0264, Rsigma = 0.0247) which were used in all calculations. The final R1 was 0.0440 (I > 2σ(I)) and wR2 was 0.1190 (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:
C7(H7A,H7B)
2.b Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C5(H5A,
H5B,H5C)
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.