mo_B0334_0m

Table 1 Crystal data and structure refinement for mo_B0334_0m.
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

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0334_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O12806.8(7)4085.5(7)8062.6(7)19.3(3)
O22492.7(8)3612.9(8)5565.2(7)21.9(3)
N12596.8(10)4981.4(10)9976.3(10)27.6(3)
C13245.7(11)5070.0(11)8144.8(12)23.0(4)
C43393.9(12)5362.6(13)9272.5(13)28.3(4)
C34321.5(13)5079.2(13)7657.2(14)33.3(4)
C61612.6(14)5511.5(15)9844.0(15)39.7(5)
C22600.7(14)5873.1(12)7566.8(13)33.0(4)
C82793.8(17)4174.6(18)3839.3(14)49.1(5)
C52955.8(17)5137.6(17)11014.6(14)46.6(5)
C72549.6(17)4439.3(14)4912.5(14)42.7(5)
Li23484.4(19)2526.1(19)5609.5(19)23.9(5)
Li12043.9(19)3766.9(19)6910.7(19)22.7(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0334_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
O121.1(5)17.3(5)19.6(5)-2.1(4)-2.0(4)-1.7(4)
O225.9(6)20.5(5)19.3(5)4.7(4)-0.8(4)-2.3(4)
N128.6(7)31.0(7)23.1(7)-9.3(6)-3.2(5)4.2(5)
C123.8(8)17.7(7)27.4(8)-2.2(6)-2.1(6)-0.6(5)
C425.8(8)25.3(8)33.9(9)-7.6(7)-5.0(7)-1.1(6)
C328.0(9)29.3(9)42.7(10)-2.4(7)5.1(7)-5.6(7)
C634.0(9)41.3(10)43.9(10)-5.3(8)5.1(8)10.5(8)
C239.3(10)22.0(8)37.7(9)1.7(7)-6.9(8)2.3(7)
C857.5(13)62.6(13)27.2(9)17.3(9)2.1(9)-3.6(10)
C554.6(12)56.0(12)29.4(10)-16.5(9)-8.5(9)-2.1(9)
C771.6(14)25.9(9)30.6(9)9.2(7)2.9(9)-5.8(8)
Li223.8(12)26.0(13)22.0(12)0.3(10)2.7(10)-2(1)
Li123.5(12)22.8(12)21.7(12)-0.1(10)-2.9(10)-1.2(9)

 

Table 4 Bond Lengths for mo_B0334_0m.
AtomAtomLength/Å AtomAtomLength/Å
O1C11.4053(17) C8C71.492(3)
O1Li211.967(3) Li2O121.967(3)
O1Li121.927(3) Li2O231.952(3)
O1Li11.862(3) Li2N122.100(3)
O2C71.379(2) Li2C422.723(3)
O2Li21.913(3) Li2Li232.560(5)
O2Li231.952(3) Li2Li13.009(4)
O2Li11.880(3) Li2Li132.499(3)
N1C41.477(2) Li2Li123.341(4)
N1C61.463(2) Li1O111.927(3)
N1C51.462(2) Li1Li213.341(4)
N1Li212.100(3) Li1Li232.499(3)
C1C41.548(2) Li1Li122.924(4)
C1C31.539(2) Li1Li133.500(5)
C1C21.541(2) Li1Li112.923(4)
C4Li212.723(3)    

11/2-Y,+X,3/2-Z; 2+Y,1/2-X,3/2-Z; 31/2-X,1/2-Y,+Z

 

Table 5 Bond Angles for mo_B0334_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1O1Li21112.47(11) N12Li2Li23157.56(9)
C1O1Li12115.43(11) N12Li2Li13117.16(13)
C1O1Li1118.81(11) N12Li2Li1145.84(12)
Li12O1Li2179.84(11) N12Li2Li12105.76(11)
Li1O1Li21121.47(12) C42Li2Li1139.51(11)
Li1O1Li12100.98(13) C42Li2Li1285.35(8)
C7O2Li2123.92(13) Li23Li2C42152.20(16)
C7O2Li23130.14(13) Li23Li2Li152.57(9)
C7O2Li1121.59(13) Li23Li2Li1296.56(6)
Li2O2Li2382.96(12) Li13Li2C4284.94(10)
Li1O2Li2105.00(11) Li13Li2Li2372.99(10)
Li1O2Li2381.40(11) Li1Li2Li1254.52(7)
C4N1Li2197.62(11) Li13Li2Li1257.96(8)
C6N1C4112.34(13) Li13Li2Li178.30(12)
C6N1Li21109.02(13) O1Li1O11122.33(13)
C5N1C4108.61(14) O1Li1O2129.04(14)
C5N1C6108.99(14) O1Li1Li23149.00(14)
C5N1Li21119.88(14) O11Li1Li2350.79(9)
O1C1C4110.39(12) O1Li1Li2130.15(7)
O1C1C3110.09(12) O11Li1Li2192.20(10)
O1C1C2110.96(12) O1Li1Li2104.70(12)
C3C1C4106.68(13) O11Li1Li297.90(10)
C3C1C2106.38(13) O11Li1Li1138.70(8)
C2C1C4112.16(13) O11Li1Li1369.44(9)
N1C4C1115.78(12) O1Li1Li1391.66(9)
N1C4Li2149.85(9) O11Li1Li12109.90(9)
C1C4Li2177.30(10) O1Li1Li1185.87(12)
O2C7C8115.15(16) O1Li1Li1240.33(10)
O12Li2N1286.75(11) O2Li1O11100.65(12)
O12Li2C4259.76(8) O2Li1Li237.89(7)
O12Li2Li23113.03(8) O2Li1Li2350.54(9)
O12Li2Li181.75(10) O2Li1Li21149.53(12)
O12Li2Li1228.38(6) O2Li1Li11122.21(13)
O12Li2Li1349.38(9) O2Li1Li1378.15(8)
O2Li2O12117.21(13) O2Li1Li12103.10(12)
O23Li2O1296.79(11) Li23Li1Li21130.19(12)
O2Li2O2396.93(12) Li23Li1Li254.44(11)
O23Li2N12122.30(13) Li2Li1Li21113.34(10)
O2Li2N12132.01(14) Li23Li1Li1175.61(10)
O23Li2C42104.60(11) Li21Li1Li1380.79(6)
O2Li2C42158.45(13) Li23Li1Li12109.50(10)
O2Li2Li2349.16(9) Li23Li1Li1357.34(8)
O23Li2Li2347.88(9) Li2Li1Li1344.36(7)
O23Li2Li191.07(10) Li11Li1Li296.74(8)
O2Li2Li13109.41(12) Li12Li1Li268.52(9)
O23Li2Li12103.17(10) Li11Li1Li2156.96(9)
O2Li2Li1288.88(10) Li12Li1Li2146.44(9)
O2Li2Li137.11(7) Li12Li1Li1353.23(4)
O23Li2Li1348.05(8) Li11Li1Li1353.23(4)
N12Li2C4232.52(6) Li11Li1Li1273.55(8)

11/2-Y,+X,3/2-Z; 2+Y,1/2-X,3/2-Z; 31/2-X,1/2-Y,+Z

 

Table 6 Torsion Angles for mo_B0334_0m.
ABCDAngle/˚ ABCDAngle/˚
O1C1C4N1-34.79(17) Li21O1Li1Li13-84.72(16)
O1C1C4Li21-2.23(11) Li21O1Li1Li12-68.37(14)
C1O1Li1O11-149.79(14) Li2O2C7C846.0(2)
C1O1Li1O267.6(2) Li22O2C7C8-66.0(2)
C1O1Li1Li21-147.99(18) Li2O2Li1O159.3(2)
C1O1Li1Li22143.7(2) Li22O2Li1O1139.63(19)
C1O1Li1Li2100.69(13) Li2O2Li1O11-89.20(12)
C1O1Li1Li13127.29(12) Li22O2Li1O11-8.92(11)
C1O1Li1Li12143.64(10) Li22O2Li1Li21104.4(3)
C1O1Li1Li11-163.42(10) Li2O2Li1Li2124.2(3)
C3C1C4N1-154.39(13) Li22O2Li1Li280.28(12)
C3C1C4Li21-121.83(12) Li2O2Li1Li22-80.28(12)
C6N1C4C1-70.86(17) Li22O2Li1Li13104.62(11)
C6N1C4Li21-114.23(15) Li2O2Li1Li1324.34(13)
C2C1C4N189.51(16) Li22O2Li1Li1125.98(14)
C2C1C4Li21122.07(13) Li2O2Li1Li11-54.30(16)
C5N1C4C1168.50(14) Li2O2Li1Li12-23.07(11)
C5N1C4Li21125.13(16) Li22O2Li1Li1257.21(10)
C7O2Li1O11123.34(15) Li21N1C4C143.38(15)
C7O2Li1O1-88.1(2) Li1O1C1C4153.97(13)
C7O2Li1Li22132.25(16) Li13O1C1C4-85.89(14)
C7O2Li1Li2-147.46(18) Li13O1C1C331.63(17)
C7O2Li1Li21-123.3(2) Li1O1C1C3-88.51(16)
C7O2Li1Li11158.24(14) Li1O1C1C228.99(18)
C7O2Li1Li13-123.13(13) Li13O1C1C2149.13(13)
C7O2Li1Li12-170.53(13) Li13O1Li1O1182.92(8)
Li21O1C1C43.26(16) Li13O1Li1O2-59.7(2)
Li21O1C1C3120.78(14) Li13O1Li1Li2-26.60(13)
Li21O1C1C2-121.72(14) Li13O1Li1Li2184.72(16)
Li21O1Li1O11-1.8(2) Li13O1Li1Li2216.5(3)
Li21O1Li1O2-144.43(15) Li13O1Li1Li1169.30(8)
Li21O1Li1Li2-111.32(15) Li13O1Li1Li1216.35(9)
Li21O1Li1Li22-68.3(3) Li1O2C7C8-172.76(16)
Li21O1Li1Li11-15.42(14)      

11/2-Y,+X,3/2-Z; 21/2-X,1/2-Y,+Z; 3+Y,1/2-X,3/2-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0334_0m.
AtomxyzU(eq)
H3A47604571799550
H3B46275765773050
H3C42634908693650
H6A17216257988360
H6B113652981037960
H6C13225335918160
H2A25965703684349
H2B29026557766349
H2C18945870782749
H8A28274806343574
H8B22563724356874
H8C34593820381074
H5A361847891110870
H5B245148531148970
H5C303958751114370
H7A30824919516651
H7B18834808492851
H4A3460(15)6142(16)9361(14)40(5)
H4B4059(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.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
  2. Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R. (2007). J. Appl. Cryst. 40, 609-613.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [mo_B0334_0m]

Crystal Data for C8H19Li2NO2 (=175.12 g/mol): tetragonal, space group P42/n (no. 86), a = 12.998(4) Å, c = 13.199(4) Å, = 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)

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