JG_209_auto

b"\n \n \n "

Table 1 Crystal data and structure refinement for JG_209_auto.
Identification code JG_209_auto
Empirical formula C8H4Li4O4
Formula weight 191.87
Temperature/K 100.01(10)
Crystal system monoclinic
Space group P21/n
a/Å 8.4602(5)
b/Å 5.1400(2)
c/Å 16.5862(9)
α/° 90
β/° 99.445(6)
γ/° 90
Volume/Å3 711.48(6)
Z 4
ρcalcg/cm3 1.791
μ/mm‑1 1.102
F(000) 384.0
Crystal size/mm3 0.09 × 0.06 × 0.02
Radiation Cu Kα (λ = 1.54184)
2Θ range for data collection/° 10.814 to 153.122
Index ranges -10 ≤ h ≤ 10, -5 ≤ k ≤ 6, -20 ≤ l ≤ 20
Reflections collected 8592
Independent reflections 1491 [Rint = 0.0949, Rsigma = 0.0602]
Data/restraints/parameters 1491/0/161
Goodness-of-fit on F2 1.109
Final R indexes [I>=2σ (I)] R1 = 0.0629, wR2 = 0.1743
Final R indexes [all data] R1 = 0.0801, wR2 = 0.1871
Largest diff. peak/hole / e Å-3 0.37/-0.33

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for JG_209_auto. Ueq is defined as 1/3 of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O15163(3)6493(4)5824.7(12)24.4(5)
O26266(3)2556(4)6069.8(12)23.8(5)
O33664(3)1843(4)9907.4(12)21.3(5)
O42506(3)5834(4)9683.8(12)22.2(5)
C15555(4)4581(6)6363.0(17)21.0(6)
C25205(3)4612(6)7150.1(16)20.6(6)
C35755(4)2611(5)7737.7(17)20.7(6)
C45269(4)2462(6)8476.7(17)21.2(6)
C54122(4)4286(5)8731.8(17)20.2(6)
C63694(4)6440(6)8160.1(17)20.3(6)
C74206(4)6589(5)7432.0(18)21.2(6)
C83436(3)3978(5)9423.9(16)19.1(6)
Li14601(7)9975(11)5945(3)30.9(12)
Li23480(7)5327(12)4933(3)32.2(12)
Li37918(8)514(13)5837(4)39.0(14)
Li44138(7)-1576(10)9528(3)27.2(11)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for JG_209_auto. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
O136.9(13)18.5(11)19.3(10)2.7(8)9.2(9)4.0(9)
O232.8(12)19.0(11)22.1(10)-2.2(8)11.5(9)3.3(9)
O329.4(11)13.4(10)22.6(10)2.4(8)9.0(8)-0.9(8)
O428.6(11)17.9(11)22.3(10)-0.2(8)10.7(8)1.1(8)
C126.3(15)14.4(14)23.1(13)0.1(11)6.7(11)1.7(11)
C225.5(15)17.0(15)20.6(13)-1.1(11)7.4(11)0.6(11)
C327.4(15)12.5(14)23.2(14)-0.4(11)7.1(11)0.5(11)
C429.1(16)13.0(14)22.2(14)1.4(11)6.2(11)0.1(12)
C526.2(15)13.1(14)22.9(13)-0.5(11)8.6(11)-2.1(11)
C626.2(15)14.1(14)21.5(13)-0.3(10)6.7(11)0.5(11)
C728.6(16)13.7(14)22.5(13)0.2(11)7.6(12)-0.3(11)
C827.6(15)10.0(14)20.6(13)1.2(10)6.3(11)-0.8(10)
Li136(3)22(3)34(3)0(2)5(2)0(2)
Li232(3)35(3)32(3)1(2)11(2)3(2)
Li345(4)43(4)30(3)-3(3)10(3)12(3)
Li438(3)16(2)29(3)-1(2)10(2)-3(2)

 

Table 4 Bond Lengths for JG_209_auto.
AtomAtomLength/Å AtomAtomLength/Å
O1C11.332(3) Li1C172.560(6)
O1Li11.871(6) Li1C862.593(7)
O1Li21.970(6) Li1Li193.312(11)
O1Li212.060(6) Li1Li22.983(8)
O2C11.333(3) Li1Li273.280(8)
O2Li121.921(6) Li1Li293.371(8)
O2Li212.029(6) Li1Li313.358(8)
O2Li31.839(6) Li1Li372.855(9)
O3C81.354(3) Li2O112.060(6)
O3Li232.031(6) Li2O212.029(6)
O3Li342.223(7) Li2O362.031(6)
O3Li41.931(6) Li2O432.570(6)
O3Li451.944(6) Li2C112.422(6)
O4C81.352(3) Li2Li123.280(8)
O4Li131.962(6) Li2Li212.567(12)
O4Li262.570(6) Li2Li312.666(9)
O4Li342.011(6) Li2Li462.704(8)
O4Li471.966(6) Li3O3102.223(7)
C1C21.385(4) Li3O4102.011(6)
C1Li122.560(6) Li3C4112.353(7)
C1Li212.422(6) Li3C5112.567(7)
C1Li22.736(7) Li3C8102.468(6)
C2C31.441(4) Li3Li113.358(8)
C2C71.447(4) Li3Li122.855(9)
C3C41.358(4) Li3Li212.666(9)
C4C51.461(4) Li3Li2123.399(9)
C4Li382.353(7) Li3Li483.050(9)
C5C61.464(4) Li3Li4133.258(8)
C5C81.378(4) Li4O351.944(6)
C5Li382.568(7) Li4O421.966(6)
C5Li472.503(6) Li4C522.503(6)
C6C71.350(4) Li4C622.460(6)
C6Li472.460(6) Li4C822.361(6)
C8Li132.593(7) Li4C852.754(6)
C8Li342.468(6) Li4Li232.704(8)
C8Li472.361(6) Li4Li3113.050(9)
C8Li452.754(6) Li4Li3143.258(8)
Li1O271.921(6) Li4Li452.540(11)
Li1O461.962(6)    

11-X,1-Y,1-Z; 2+X,-1+Y,+Z; 31/2-X,-1/2+Y,3/2-Z; 4-1/2+X,1/2-Y,1/2+Z; 51-X,-Y,2-Z; 61/2-X,1/2+Y,3/2-Z; 7+X,1+Y,+Z; 83/2-X,1/2+Y,3/2-Z; 91-X,2-Y,1-Z; 101/2+X,1/2-Y,-1/2+Z; 113/2-X,-1/2+Y,3/2-Z; 121-X,-Y,1-Z; 131/2+X,-1/2-Y,-1/2+Z; 14-1/2+X,-1/2-Y,1/2+Z

 

Table 5 Bond Angles for JG_209_auto.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1O1Li1132.4(2) O21Li2C1133.40(12)
C1O1Li2188.4(2) O21Li2C1130.3(3)
C1O1Li2110.4(3) O21Li2Li12144.0(3)
Li1O1Li21132.5(3) O21Li2Li188.0(2)
Li1O1Li2101.9(3) O21Li2Li2184.4(3)
Li2O1Li2179.1(3) O21Li2Li3143.54(18)
C1O2Li12102.2(2) O21Li2Li46131.9(3)
C1O2Li2189.7(2) O36Li2O11148.5(3)
C1O2Li3157.8(3) O36Li2O4388.8(2)
Li12O2Li21117.2(3) O36Li2C1113.6(2)
Li3O2Li1298.8(3) O36Li2C11123.1(3)
Li3O2Li2187.0(3) O36Li2Li12116.4(3)
C8O3Li23110.2(3) O36Li2Li180.1(2)
C8O3Li3483.5(2) O36Li2Li21160.5(4)
C8O3Li45112.0(2) O36Li2Li3154.5(2)
C8O3Li4124.2(2) O36Li2Li4645.42(17)
Li23O3Li3477.5(2) O43Li2C181.26(18)
Li45O3Li23135.6(3) O43Li2Li1236.72(14)
Li4O3Li2386.0(3) O43Li2Li1131.8(2)
Li4O3Li34151.6(2) O43Li2Li31134.6(3)
Li45O3Li3493.8(2) O43Li2Li4643.67(15)
Li4O3Li4581.9(3) C11Li2O43114.0(2)
C8O4Li13101.4(2) C11Li2C1120.7(2)
C8O4Li26160.5(2) C11Li2Li1111.2(2)
C8O4Li3492.3(3) C1Li2Li161.65(17)
C8O4Li4788.7(2) C1Li2Li1249.36(15)
Li13O4Li2691.7(2) C11Li2Li12111.1(2)
Li13O4Li34115.4(3) C11Li2Li2166.5(2)
Li13O4Li47132.8(3) C11Li2Li3175.3(2)
Li34O4Li2695.0(2) C11Li2Li46135.6(3)
Li47O4Li2671.8(2) Li1Li2Li12110.2(2)
Li47O4Li34110.0(3) Li21Li2O43102.8(3)
O1C1O2114.1(2) Li21Li2C154.2(2)
O1C1C2123.7(3) Li21Li2Li1269.2(3)
O1C1Li12117.9(2) Li21Li2Li180.5(3)
O1C1Li2158.25(19) Li21Li2Li31120.4(4)
O1C1Li242.46(19) Li21Li2Li46142.0(4)
O2C1C2122.1(3) Li31Li2C1134.3(3)
O2C1Li1247.17(19) Li31Li2Li172.7(2)
O2C1Li293.3(2) Li31Li2Li12170.4(3)
O2C1Li2156.9(2) Li31Li2Li4697.2(3)
C2C1Li1299.2(2) Li46Li2C196.1(2)
C2C1Li2127.5(2) Li46Li2Li1273.2(2)
C2C1Li21172.5(3) Li46Li2Li1107.8(2)
Li12C1Li276.5(2) O2Li3O31096.3(3)
Li21C1Li1285.1(2) O2Li3O410112.1(3)
Li21C1Li259.3(2) O2Li3C411137.5(3)
C1C2C3122.3(3) O2Li3C511145.3(3)
C1C2C7122.6(3) O2Li3C810113.5(3)
C3C2C7115.1(2) O2Li3Li1241.69(19)
C4C3C2122.6(3) O2Li3Li1180.4(2)
C3C4C5122.6(3) O2Li3Li2149.5(2)
C3C4Li3897.4(2) O2Li3Li212110.7(3)
C5C4Li3881.0(2) O2Li3Li413146.0(3)
C4C5C6113.8(2) O2Li3Li48115.8(3)
C4C5Li3864.8(2) O310Li3C411120.4(3)
C4C5Li47138.8(2) O310Li3C51188.2(2)
C6C5Li3896.9(2) O310Li3C81033.02(12)
C6C5Li4771.2(2) O310Li3Li1169.29(18)
C8C5C4123.9(3) O310Li3Li12119.8(3)
C8C5C6122.2(3) O310Li3Li2148.06(18)
C8C5Li38108.7(2) O310Li3Li212113.6(2)
C8C5Li4767.9(2) O310Li3Li4839.51(16)
Li47C5Li3873.9(2) O310Li3Li41376.13(19)
C5C6Li4774.5(2) O410Li3O31064.86(19)
C7C6C5122.7(3) O410Li3C411103.2(3)
C7C6Li47141.1(3) O410Li3C511100.9(3)
C6C7C2122.6(3) O410Li3C81033.18(13)
O3C8C5123.2(3) O410Li3Li1290.4(3)
O3C8Li13109.8(2) O410Li3Li1131.86(16)
O3C8Li3463.5(2) O410Li3Li2180.0(2)
O3C8Li4540.89(17) O410Li3Li21248.88(19)
O3C8Li47137.0(2) O410Li3Li4890.0(3)
O4C8O3114.6(2) O410Li3Li41334.54(16)
O4C8C5122.1(2) C411Li3C51134.19(13)
O4C8Li1347.88(18) C411Li3C810109.1(3)
O4C8Li3454.5(2) C411Li3Li12118.3(3)
O4C8Li4756.35(19) C411Li3Li11130.2(3)
O4C8Li45121.9(2) C411Li3Li21165.8(4)
C5C8Li13108.5(2) C411Li3Li21275.6(2)
C5C8Li34160.7(3) C411Li3Li41369.84(19)
C5C8Li45101.9(2) C411Li3Li4886.2(2)
C5C8Li4779.3(2) C511Li3Li11132.5(2)
Li13C8Li45147.6(2) C511Li3Li12152.0(3)
Li34C8Li1383.1(2) C511Li3Li21131.8(3)
Li34C8Li4571.2(2) C511Li3Li21298.7(2)
Li47C8Li1393.1(2) C511Li3Li41368.38(18)
Li47C8Li3484.8(2) C511Li3Li4852.06(17)
Li47C8Li45103.61(18) C810Li3C51188.5(2)
O1Li1O27118.5(3) C810Li3Li1150.05(16)
O1Li1O46112.5(3) C810Li3Li12113.5(3)
O1Li1C17147.1(3) C810Li3Li2166.0(2)
O1Li1C8692.6(2) C810Li3Li21280.9(2)
O1Li1Li1979.2(2) C810Li3Li41346.19(15)
O1Li1Li240.26(18) C810Li3Li4858.76(19)
O1Li1Li27143.6(3) Li12Li3Li1163.8(2)
O1Li1Li29119.4(3) Li12Li3Li21269.7(2)
O1Li1Li3188.3(2) Li11Li3Li21258.09(17)
O1Li1Li3779.4(2) Li12Li3Li413113.8(3)
O27Li1O46119.2(3) Li12Li3Li48154.6(3)
O27Li1C1730.59(12) Li21Li3Li1275.2(2)
O27Li1C86147.4(3) Li21Li3Li1158.0(2)
O27Li1Li1980.6(3) Li21Li3Li212115.4(3)
O27Li1Li2140.7(3) Li21Li3Li4879.9(2)
O27Li1Li2767.8(2) Li21Li3Li413110.1(2)
O27Li1Li2932.38(15) Li413Li3Li1165.90(18)
O27Li1Li3739.54(19) Li48Li3Li11106.4(2)
O27Li1Li31119.7(3) Li48Li3Li212127.1(2)
O46Li1C1798.9(2) Li413Li3Li21247.88(16)
O46Li1C8630.73(12) Li48Li3Li41379.3(2)
O46Li1Li1978.7(2) O3Li4O3598.1(3)
O46Li1Li2994.0(2) O35Li4O42121.7(3)
O46Li1Li2751.55(17) O3Li4O42112.7(3)
O46Li1Li272.8(2) O35Li4C5296.7(2)
O46Li1Li37139.6(3) O3Li4C52164.2(3)
O46Li1Li3132.75(15) O3Li4C62132.0(3)
C17Li1C86120.2(2) O35Li4C62113.8(3)
C17Li1Li1998.3(3) O35Li4C8527.11(11)
C17Li1Li2945.71(15) O3Li4C82147.3(3)
C17Li1Li2754.19(16) O35Li4C82100.1(2)
C17Li1Li2161.8(3) O3Li4C85112.1(2)
C17Li1Li3770.0(2) O35Li4Li23129.6(3)
C17Li1Li31115.7(2) O3Li4Li2348.54(19)
C86Li1Li1997.3(3) O3Li4Li314104.1(2)
C86Li1Li259.86(17) O35Li4Li31491.0(2)
C86Li1Li29124.6(2) O3Li4Li311137.0(3)
C86Li1Li2781.55(19) O35Li4Li31146.65(17)
C86Li1Li3146.86(16) O3Li4Li4549.29(19)
C86Li1Li37162.0(3) O35Li4Li4548.8(2)
Li19Li1Li2953.01(19) O42Li4C5263.29(17)
Li19Li1Li3150.67(19) O42Li4C6280.6(2)
Li27Li1Li1966.2(2) O42Li4C8594.6(2)
Li2Li1Li1964.5(2) O42Li4C8234.92(12)
Li27Li1Li2945.4(2) O42Li4Li2364.5(2)
Li2Li1Li27110.2(2) O42Li4Li311107.9(2)
Li2Li1Li29117.5(2) O42Li4Li31435.44(16)
Li27Li1Li3161.58(18) O42Li4Li45134.1(4)
Li2Li1Li3149.29(18) C52Li4C8583.75(18)
Li37Li1Li1965.5(2) C52Li4Li23123.2(3)
Li37Li1Li2105.5(2) C52Li4Li31481.29(19)
Li31Li1Li2987.4(2) C52Li4Li31154.00(17)
Li37Li1Li2949.86(19) C52Li4Li45145.1(4)
Li37Li1Li2795.2(2) C62Li4C5234.30(12)
Li37Li1Li31116.2(2) C62Li4C85112.4(2)
O1Li2O11100.9(3) C62Li4Li23116.4(3)
O1Li2O21106.9(3) C62Li4Li31167.63(18)
O1Li2O36109.7(3) C62Li4Li314109.9(2)
O11Li2O4388.8(2) C62Li4Li45144.9(4)
O1Li2O43108.2(3) C82Li4C5232.74(11)
O1Li2C11110.7(3) C82Li4C6262.12(16)
O1Li2C127.16(12) C82Li4C8576.39(18)
O11Li2C1133.36(12) C82Li4Li2399.5(2)
O11Li2C197.1(2) C82Li4Li31448.99(16)
O11Li2Li1277.8(2) C82Li4Li31173.40(19)
O1Li2Li137.86(17) C85Li4Li31150.02(16)
O11Li2Li1123.3(3) C85Li4Li31465.51(17)
O1Li2Li1276.0(2) C82Li4Li45140.8(4)
O11Li2Li2148.9(2) Li23Li4C85121.3(2)
O1Li2Li2152.0(2) Li23Li4Li311169.4(3)
O11Li2Li31108.6(3) Li23Li4Li31468.8(2)
O1Li2Li31109.0(3) Li311Li4Li314100.7(2)
O11Li2Li46127.3(3) Li45Li4C8566.7(2)
O1Li2Li46113.1(3) Li45Li4Li2389.1(3)
O21Li2O1166.33(19) Li45Li4Li314101.4(3)
O21Li2O3696.8(3) Li45Li4Li31191.7(3)
O21Li2O43140.1(3)     

11-X,1-Y,1-Z; 2+X,-1+Y,+Z; 31/2-X,-1/2+Y,3/2-Z; 4-1/2+X,1/2-Y,1/2+Z; 51-X,-Y,2-Z; 61/2-X,1/2+Y,3/2-Z; 7+X,1+Y,+Z; 83/2-X,1/2+Y,3/2-Z; 91-X,2-Y,1-Z; 101/2+X,1/2-Y,-1/2+Z; 113/2-X,-1/2+Y,3/2-Z; 121-X,-Y,1-Z; 131/2+X,-1/2-Y,-1/2+Z; 14-1/2+X,-1/2-Y,1/2+Z

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for JG_209_auto.
AtomxyzU(eq)
H36590(40)1330(70)7620(20)27(9)
H45640(40)970(70)8830(20)25(9)
H62880(50)7820(70)8240(20)33(10)
H73810(40)8040(60)7041(19)13(7)

Experimental

Single crystals of C8H4Li4O4 [JG_209_auto] were []. A suitable crystal was selected and [mounted on a Mitegen loop using Paratone-N oil] on a SuperNova, Dual, Cu at home/near, AtlasS2 diffractometer. The crystal was kept at 100.01(10) K during data collection. Using Olex2 [1], the structure was solved with the SHELXT [2] structure solution program using Intrinsic Phasing and refined with the SHELXL [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. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [JG_209_auto]

Crystal Data for C8H4Li4O4 (=191.87 g/mol): monoclinic, space group P21/n (no. 14), a = 8.4602(5) Å, b = 5.1400(2) Å, c = 16.5862(9) Å, β = 99.445(6)°, = 711.48(6) Å3, Z = 4, T = 100.01(10) K, μ(Cu Kα) = 1.102 mm-1, Dcalc = 1.791 g/cm3, 8592 reflections measured (10.814° ≤ 2Θ ≤ 153.122°), 1491 unique (Rint = 0.0949, Rsigma = 0.0602) which were used in all calculations. The final R1 was 0.0629 (I > 2σ(I)) and wR2 was 0.1871 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

N/A

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