Identification code | JG208_auto |
Empirical formula | C12H6Li4O4 |
Formula weight | 241.93 |
Temperature/K | 102(3) |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 9.7425(5) |
b/Å | 5.9515(3) |
c/Å | 8.3569(6) |
α/° | 90 |
β/° | 105.758(7) |
γ/° | 90 |
Volume/Å3 | 466.34(5) |
Z | 2 |
ρcalcg/cm3 | 1.723 |
μ/mm‑1 | 0.996 |
F(000) | 244.0 |
Crystal size/mm3 | 0.11 × 0.07 × 0.03 |
Radiation | Cu Kα (λ = 1.54184) |
2Θ range for data collection/° | 9.432 to 147.194 |
Index ranges | -12 ≤ h ≤ 12, -7 ≤ k ≤ 7, -8 ≤ l ≤ 10 |
Reflections collected | 5116 |
Independent reflections | 931 [Rint = 0.0402, Rsigma = 0.0200] |
Data/restraints/parameters | 931/0/103 |
Goodness-of-fit on F2 | 1.079 |
Final R indexes [I>=2σ (I)] | R1 = 0.0490, wR2 = 0.1403 |
Final R indexes [all data] | R1 = 0.0552, wR2 = 0.1481 |
Largest diff. peak/hole / e Å-3 | 0.37/-0.25 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
O1 | 4134.6(13) | 5129(3) | 2685.4(17) | 22.8(4) |
O2 | 4185.7(14) | 8105(2) | 4352.9(17) | 22.8(4) |
C1 | 3569.1(19) | 6174(4) | 3754(2) | 21.2(5) |
C2 | 2382.7(19) | 5349(3) | 4204(2) | 21.5(5) |
C3 | 1602(2) | 6724(3) | 5093(2) | 21.7(5) |
C4 | 308.5(19) | 6077(3) | 5302(2) | 20.8(5) |
C5 | 1764(2) | 3180(4) | 3637(2) | 22.2(5) |
C6 | 513(2) | 2482(3) | 3895(2) | 21.7(5) |
Li1 | 3845(4) | 4114(7) | 422(4) | 27.8(8) |
Li2 | 5691(4) | 3169(6) | 3316(4) | 26.4(8) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
O1 | 18.3(7) | 32.4(8) | 22.1(8) | -1.6(6) | 13.1(5) | 0.9(5) |
O2 | 17.3(7) | 29.9(8) | 25.4(8) | -1.7(6) | 12.9(6) | -1.8(5) |
C1 | 16.6(9) | 30.2(10) | 19.4(10) | 0.7(8) | 9.6(7) | 2.1(7) |
C2 | 16.6(9) | 30.1(10) | 20.9(10) | 0.9(8) | 10.5(7) | 0.6(7) |
C3 | 18.6(9) | 29.2(10) | 20.3(10) | -0.1(7) | 10.3(7) | -0.2(7) |
C4 | 18.1(9) | 28.1(10) | 18.9(10) | 1.3(8) | 9.8(7) | 0.8(8) |
C5 | 18.5(9) | 30.0(11) | 21.4(10) | 0.3(8) | 10.7(7) | 2.2(7) |
C6 | 19.0(9) | 28.7(10) | 19.7(10) | 0.5(8) | 9.3(7) | 0.0(7) |
Li1 | 23.0(15) | 36.6(19) | 28.5(18) | -0.4(15) | 15.2(13) | 0.9(14) |
Li2 | 25.8(17) | 33.2(18) | 23.9(17) | 1.7(14) | 13.3(13) | 2.7(14) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O1 | C1 | 1.325(2) | C5 | Li15 | 2.561(4) | |
O1 | Li1 | 1.932(4) | C6 | C44 | 1.455(3) | |
O1 | Li21 | 2.020(4) | Li1 | O26 | 1.952(4) | |
O1 | Li2 | 1.872(4) | Li1 | O27 | 1.970(4) | |
O2 | C1 | 1.330(3) | Li1 | C58 | 2.561(4) | |
O2 | Li12 | 1.952(4) | Li1 | Li19 | 2.745(7) | |
O2 | Li11 | 1.970(4) | Li1 | Li28 | 3.146(5) | |
O2 | Li23 | 2.064(4) | Li1 | Li2 | 2.653(5) | |
O2 | Li21 | 2.266(4) | Li1 | Li21 | 2.624(5) | |
C1 | C2 | 1.398(3) | Li2 | O17 | 2.020(4) | |
C1 | Li21 | 2.366(4) | Li2 | O23 | 2.064(4) | |
C1 | Li23 | 2.390(4) | Li2 | O27 | 2.266(4) | |
C2 | C3 | 1.451(3) | Li2 | C17 | 2.366(4) | |
C2 | C5 | 1.449(3) | Li2 | C13 | 2.390(4) | |
C2 | Li23 | 2.546(4) | Li2 | C23 | 2.546(4) | |
C3 | C4 | 1.374(3) | Li2 | C33 | 2.612(4) | |
C3 | Li23 | 2.612(4) | Li2 | Li17 | 2.624(5) | |
C4 | C44 | 1.447(4) | Li2 | Li15 | 3.146(5) | |
C4 | C64 | 1.455(3) | Li2 | Li27 | 3.396(4) | |
C5 | C6 | 1.359(3) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C1 | O1 | Li1 | 146.08(16) | Li21 | Li1 | Li28 | 124.06(14) | |
C1 | O1 | Li21 | 87.45(15) | Li2 | Li1 | Li28 | 93.98(13) | |
C1 | O1 | Li2 | 123.81(16) | O1 | Li2 | O17 | 126.5(2) | |
Li1 | O1 | Li21 | 83.16(16) | O1 | Li2 | O27 | 89.37(15) | |
Li2 | O1 | Li1 | 88.43(17) | O17 | Li2 | O27 | 62.89(11) | |
Li2 | O1 | Li21 | 121.46(9) | O17 | Li2 | O23 | 94.13(16) | |
C1 | O2 | Li12 | 142.15(15) | O1 | Li2 | O23 | 109.24(17) | |
C1 | O2 | Li11 | 128.90(16) | O1 | Li2 | C17 | 119.43(18) | |
C1 | O2 | Li21 | 77.49(14) | O17 | Li2 | C17 | 34.01(8) | |
C1 | O2 | Li23 | 86.70(15) | O17 | Li2 | C13 | 122.35(18) | |
Li12 | O2 | Li11 | 88.85(15) | O1 | Li2 | C13 | 100.50(16) | |
Li12 | O2 | Li21 | 119.81(16) | O17 | Li2 | C23 | 121.42(17) | |
Li11 | O2 | Li23 | 102.50(16) | O1 | Li2 | C23 | 112.02(18) | |
Li12 | O2 | Li23 | 81.55(16) | O1 | Li2 | C33 | 139.2(2) | |
Li11 | O2 | Li21 | 77.19(15) | O17 | Li2 | C33 | 92.64(14) | |
Li23 | O2 | Li21 | 158.50(10) | O17 | Li2 | Li17 | 46.98(12) | |
O1 | C1 | O2 | 115.56(15) | O1 | Li2 | Li1 | 46.72(12) | |
O1 | C1 | C2 | 122.82(19) | O1 | Li2 | Li17 | 136.40(19) | |
O1 | C1 | Li21 | 58.54(13) | O17 | Li2 | Li1 | 85.68(16) | |
O1 | C1 | Li23 | 134.64(16) | O17 | Li2 | Li15 | 88.27(14) | |
O2 | C1 | C2 | 121.60(17) | O1 | Li2 | Li15 | 83.34(14) | |
O2 | C1 | Li21 | 69.23(13) | O17 | Li2 | Li27 | 28.05(5) | |
O2 | C1 | Li23 | 59.55(13) | O1 | Li2 | Li27 | 103.3(2) | |
C2 | C1 | Li23 | 79.80(14) | O23 | Li2 | O27 | 156.63(19) | |
C2 | C1 | Li21 | 144.22(17) | O23 | Li2 | C17 | 123.68(18) | |
Li21 | C1 | Li23 | 126.87(13) | O23 | Li2 | C13 | 33.75(8) | |
C1 | C2 | C3 | 121.72(19) | O27 | Li2 | C13 | 158.36(18) | |
C1 | C2 | C5 | 121.71(18) | O27 | Li2 | C17 | 33.28(8) | |
C1 | C2 | Li23 | 67.48(13) | O27 | Li2 | C23 | 125.64(16) | |
C3 | C2 | Li23 | 76.16(14) | O23 | Li2 | C23 | 61.17(11) | |
C5 | C2 | C3 | 116.16(16) | O27 | Li2 | C33 | 100.70(13) | |
C5 | C2 | Li23 | 136.41(16) | O23 | Li2 | C33 | 74.71(13) | |
C2 | C3 | Li23 | 71.19(13) | O23 | Li2 | Li1 | 142.17(17) | |
C4 | C3 | C2 | 122.23(19) | O23 | Li2 | Li17 | 47.38(11) | |
C4 | C3 | Li23 | 140.92(17) | O27 | Li2 | Li1 | 46.40(10) | |
C3 | C4 | C44 | 120.8(2) | O27 | Li2 | Li17 | 109.32(17) | |
C3 | C4 | C64 | 122.13(19) | O27 | Li2 | Li15 | 137.25(17) | |
C44 | C4 | C64 | 117.0(2) | O23 | Li2 | Li15 | 37.68(10) | |
C2 | C5 | Li15 | 95.23(14) | O27 | Li2 | Li27 | 73.22(15) | |
C6 | C5 | C2 | 122.09(18) | O23 | Li2 | Li27 | 88.40(13) | |
C6 | C5 | Li15 | 110.30(16) | C17 | Li2 | C13 | 139.84(17) | |
C5 | C6 | C44 | 121.50(19) | C17 | Li2 | C23 | 117.74(15) | |
O1 | Li1 | O26 | 100.68(19) | C13 | Li2 | C23 | 32.72(8) | |
O1 | Li1 | O27 | 97.03(17) | C13 | Li2 | C33 | 59.49(10) | |
O1 | Li1 | C58 | 128.25(16) | C17 | Li2 | C33 | 85.34(12) | |
O1 | Li1 | Li19 | 102.7(2) | C13 | Li2 | Li15 | 63.67(11) | |
O1 | Li1 | Li2 | 44.85(12) | C17 | Li2 | Li17 | 77.22(14) | |
O1 | Li1 | Li28 | 136.81(18) | C13 | Li2 | Li1 | 147.21(18) | |
O1 | Li1 | Li21 | 49.86(12) | C17 | Li2 | Li15 | 121.74(16) | |
O26 | Li1 | O27 | 91.15(15) | C13 | Li2 | Li17 | 76.55(14) | |
O27 | Li1 | C58 | 119.31(18) | C17 | Li2 | Li1 | 72.89(13) | |
O26 | Li1 | C58 | 113.05(17) | C13 | Li2 | Li27 | 122.08(16) | |
O26 | Li1 | Li19 | 45.85(12) | C17 | Li2 | Li27 | 55.46(11) | |
O27 | Li1 | Li19 | 45.30(11) | C23 | Li2 | C33 | 32.65(8) | |
O26 | Li1 | Li28 | 85.19(13) | C23 | Li2 | Li1 | 146.72(19) | |
O26 | Li1 | Li21 | 51.08(13) | C23 | Li2 | Li15 | 95.81(13) | |
O26 | Li1 | Li2 | 116.08(18) | C23 | Li2 | Li17 | 89.03(14) | |
O27 | Li1 | Li2 | 56.41(12) | C23 | Li2 | Li27 | 139.00(16) | |
O27 | Li1 | Li21 | 100.67(18) | C33 | Li2 | Li15 | 112.15(15) | |
O27 | Li1 | Li28 | 39.82(10) | C33 | Li2 | Li1 | 143.12(16) | |
C58 | Li1 | Li19 | 129.0(2) | C33 | Li2 | Li17 | 77.16(13) | |
C58 | Li1 | Li28 | 85.77(13) | C33 | Li2 | Li27 | 117.47(14) | |
C58 | Li1 | Li21 | 138.36(17) | Li1 | Li2 | Li15 | 104.62(16) | |
C58 | Li1 | Li2 | 130.67(18) | Li17 | Li2 | Li15 | 55.94(14) | |
Li19 | Li1 | Li28 | 52.35(13) | Li17 | Li2 | Li1 | 124.17(19) | |
Li21 | Li1 | Li19 | 71.71(18) | Li17 | Li2 | Li27 | 50.32(10) | |
Li2 | Li1 | Li19 | 85.15(18) | Li15 | Li2 | Li27 | 67.76(12) | |
Li21 | Li1 | Li2 | 80.12(13) | Li1 | Li2 | Li27 | 73.91(17) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H3 | 1960(30) | 8270(40) | 5480(30) | 19(6) |
H5 | 2240(30) | 2150(40) | 2990(30) | 28(6) |
H6 | 130(20) | 1000(40) | 3480(30) | 20(5) |
Experimental
Single crystals of C12H6Li4O4 [JG208_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 102(3) 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.
Crystal structure determination of [JG208_auto]
Crystal Data for C12H6Li4O4 (M =241.93 g/mol): monoclinic, space group P21/c (no. 14), a = 9.7425(5) Å, b = 5.9515(3) Å, c = 8.3569(6) Å, β = 105.758(7)°, V = 466.34(5) Å3, Z = 2, T = 102(3) K, μ(Cu Kα) = 0.996 mm-1, Dcalc = 1.723 g/cm3, 5116 reflections measured (9.432° ≤ 2Θ ≤ 147.194°), 931 unique (Rint = 0.0402, Rsigma = 0.0200) which were used in all calculations. The final R1 was 0.0490 (I > 2σ(I)) and wR2 was 0.1481 (all data).
Refinement model description
Number of restraints - 0, number of constraints - unknown.
Details:
N/A
This report has been created with Olex2, compiled on 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction. Please let us know if there are any errors or if you would like to have additional features.