C2c

Table 1 Crystal data and structure refinement for C2c.
Identification code C2c
Empirical formula C20H48K2Li2N2O5
Formula weight 488.68
Temperature/K 100.01
Crystal system monoclinic
Space group C2/c
a/Å 23.29(2)
b/Å 13.532(9)
c/Å 21.12(3)
α/° 90
β/° 121.01(3)
γ/° 90
Volume/Å3 5705(10)
Z 8
ρcalcg/cm3 1.138
μ/mm‑1 0.360
F(000) 2128.0
Crystal size/mm3 0.25 × 0.24 × 0.21
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.902 to 53.998
Index ranges ? ≤ h ≤ ?, ? ≤ k ≤ ?, ? ≤ l ≤ ?
Reflections collected 6223
Independent reflections 6223 [Rint = ?, Rsigma = 0.0265]
Data/restraints/parameters 6223/0/377
Goodness-of-fit on F2 1.070
Final R indexes [I>=2σ (I)] R1 = 0.0428, wR2 = 0.0841
Final R indexes [all data] R1 = 0.0622, wR2 = 0.0907
Largest diff. peak/hole / e Å-3 0.26/-0.27

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for C2c. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
K13770.9(2)3803.0(3)7394.3(2)20.12(11)
K24428.3(2)3789.2(3)6125.0(2)19.62(10)
O44317.3(6)2275.7(8)6943.4(6)15.4(3)
O24763.2(6)5327.0(9)8001.6(6)14.8(2)
O13617.8(6)4917.1(9)6301.2(7)18.3(3)
N25143.1(8)661.7(10)6416.0(8)18.5(3)
C74434.6(9)5800.2(13)8309.5(10)17.9(4)
N13870.8(7)6971.2(10)6430.5(8)15.9(3)
O3B2541(4)3582(6)7297(5)25.9(13)
O55454.5(7)2675.1(9)6452.6(7)22.1(3)
C84582.8(11)5347.3(15)9039.2(11)23.9(4)
C24043.2(11)7340.2(15)5897.4(11)27.8(4)
C33185.8(9)6574.1(13)6071.5(10)19.4(4)
C185624.1(11)2085.4(13)6039.2(11)24.6(4)
C13937.4(10)7788.2(13)6915.0(11)23.8(4)
C206320.3(13)2348.5(16)6183.2(15)42.2(6)
C175669.6(11)987.1(13)6276.1(12)22.7(4)
C62426.1(9)5145.3(15)5659.8(13)35.2(5)
C154505.8(11)480.6(17)5736.5(12)36.2(5)
C133718.5(10)1762.1(14)6601.0(12)27.6(4)
C165345.1(11)-251.1(14)6843.4(12)29.6(5)
C195133.4(15)2239.1(16)5209.7(12)43.9(6)
C102651.8(15)5003(2)7992.6(17)45.0(6)
C53066.4(12)5438.4(16)5032.5(11)37.5(5)
C92265.6(11)4079.5(17)7683.8(14)38.3(5)
C43104.6(9)5498.7(13)5781(1)20.7(4)
Li14410.1(14)5622(2)6961.5(15)15.0(6)
Li25146.6(15)1983(2)7006.0(16)17.0(6)
C11B2236(3)2709(3)6966(3)32.1(11)
C12B1579(3)2863(4)6245(3)44.1(13)
C143226.7(14)2160(2)5842.7(17)56.6(9)
C121918(3)2522(4)6137(3)49.5(13)
C111859(4)2874(4)6745(4)43.7(13)
O32356(4)3720(7)7110(5)45(2)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for C2c. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
K124.2(2)13.18(18)30.8(2)1.09(16)19.67(18)0.72(15)
K225.9(2)13.19(18)20.4(2)0.38(15)12.40(17)3.82(15)
O411.1(5)15.9(6)16.4(6)-2.3(5)5.1(5)-0.8(5)
O216.0(6)15.4(6)16.1(6)-0.5(5)10.6(5)-1.0(5)
O112.9(6)12.5(6)19.9(6)1.2(5)1.7(5)2.3(5)
N225.1(8)12.3(7)20.0(8)0.6(6)13.1(7)1.9(6)
C721.3(9)15.8(9)20.5(9)-0.9(7)13.4(8)-0.8(7)
N117.2(7)12.1(7)18.1(8)-1.8(6)8.9(6)-0.1(6)
O3B38(3)15(2)35(4)5(2)26(3)2(2)
O539.0(8)12.3(6)29.5(7)0.7(5)28.0(7)3.9(5)
C833.0(11)22.8(10)24(1)-1.2(8)20.5(10)1.3(8)
C233.5(11)24(1)31.7(11)2.6(8)21(1)0.1(8)
C315.5(8)14.0(8)22.3(10)1.2(7)5.3(8)3.0(7)
C1844.8(12)14.0(9)32.4(11)0.9(8)32.4(10)4.0(8)
C126.6(10)15.5(9)30.2(11)-6.2(8)15.4(9)-0.3(7)
C2064.3(16)23.2(11)74.2(18)-0.5(11)60.7(15)0.9(10)
C1734.6(11)14.8(9)30.3(11)0.1(7)24.9(10)5.3(8)
C614.4(9)22.5(10)50.1(14)-2.6(9)3.4(9)-0.9(8)
C1538.4(12)33.2(12)30.0(12)-6.2(9)12.6(10)-5.8(10)
C1319.1(9)17.6(10)35.0(12)-5.8(8)6.1(9)-1.7(7)
C1641.8(12)18.0(9)38.8(12)8.0(8)27.7(10)4.4(9)
C1988(2)22.9(11)34.5(13)7.2(9)41.5(14)7.2(12)
C1046.0(16)37.2(14)53.5(17)-5.8(12)26.8(14)-5.6(12)
C553.8(14)23.2(11)18.7(10)-3.0(8)6.8(10)0.2(10)
C932.1(12)34.7(12)56.4(15)-0.6(11)28.7(12)0.1(9)
C414.9(8)13.9(9)20.6(10)-0.6(7)0.0(8)1.3(7)
Li113.4(14)14.8(14)15.6(14)0.5(11)6.7(12)0.5(11)
Li220.0(14)14.9(14)18.4(15)1.2(11)11.5(13)2.8(11)
C11B22(2)31(3)45(3)-5(2)19(3)-3(2)
C12B35(3)58(3)33(3)-10(3)13(3)-12(3)
C1433.4(14)25.1(13)55.2(18)-6.8(12)-17.1(13)-2.3(10)
C1236(3)51(3)57(4)4(3)21(3)-3(2)
C1131(3)46(3)54(4)7(3)22(3)-5(3)
O359(5)35(3)43(5)11(3)29(4)18(3)

 

Table 4 Bond Lengths for C2c.
AtomAtomLength/Å AtomAtomLength/Å
K1K213.723(3) N1C31.471(3)
K1K23.709(4) N1C11.459(2)
K1O42.8366(19) N1Li12.172(3)
K1O22.861(2) O3BC91.439(10)
K1O12.623(3) O3BC11B1.370(10)
K1O3B2.781(8) O3BC111.702(11)
K1O512.643(3) O5K112.643(3)
K1Li13.242(3) O5C181.382(2)
K1Li213.277(3) O5Li21.903(3)
K1C11B3.529(6) C8K213.270(3)
K1O33.033(10) C3C41.552(3)
K2K113.723(3) C18C201.530(3)
K2K214.988(7) C18C171.554(3)
K2O42.776(2) C18C191.535(4)
K2O212.775(2) C6C41.541(3)
K2O12.5993(19) C13Li212.778(5)
K2O52.600(2) C13C141.509(4)
K2C813.270(3) C10C91.480(3)
K2Li13.058(3) C5C41.539(4)
K2Li23.005(3) C9O31.418(12)
O4C131.383(2) Li1O211.929(3)
O4Li21.909(3) Li1Li112.507(6)
O4Li211.945(4) Li2K113.277(3)
O2K212.7748(19) Li2O411.945(4)
O2C71.390(2) Li2C1312.778(5)
O2Li111.929(3) Li2Li212.508(6)
O2Li11.949(4) C11BC12B1.518(7)
O1C41.379(2) C11BC121.529(8)
O1Li11.900(3) C11BC110.787(6)
N2C171.469(3) C11BO31.399(12)
N2C151.459(3) C12BC121.036(7)
N2C161.457(2) C12BC110.911(7)
N2Li22.176(3) C12C111.440(8)
C7C81.523(3) C11O31.526(13)
N1C21.464(3)    

11-X,+Y,3/2-Z

 

Table 5 Bond Angles for C2c.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
K2K1K2184.31(10) C16N2C17109.99(15)
O4K1K247.94(4) C16N2C15107.88(17)
O4K1K2176.82(7) C16N2Li2115.91(16)
O4K1O2106.08(7) O2C7C8113.28(16)
O4K1Li196.20(8) C2N1C3112.50(16)
O4K1Li2136.21(8) C2N1Li1111.64(14)
O4K1C11B100.29(10) C3N1Li198.30(13)
O4K1O3122.4(2) C1N1C2107.96(16)
O2K1K2147.67(4) C1N1C3109.48(14)
O2K1K277.79(7) C1N1Li1116.78(15)
O2K1Li136.57(8) C9O3BK1130.6(5)
O2K1Li2194.90(9) C9O3BC1196.9(5)
O2K1C11B153.51(8) C11BO3BK1111.9(5)
O2K1O3131.3(2) C11BO3BC9115.3(6)
O1K1K244.49(6) C11BO3BC1127.0(3)
O1K1K21109.00(7) C11O3BK1132.4(5)
O1K1O490.26(8) K2O5K1190.46(6)
O1K1O272.08(7) C18O5K11129.31(14)
O1K1O3B109.21(14) C18O5K2133.58(13)
O1K1O51149.46(6) C18O5Li2115.11(15)
O1K1Li135.87(6) Li2O5K1190.75(14)
O1K1Li21120.06(7) Li2O5K282.14(11)
O1K1C11B110.79(10) C7C8K2187.55(12)
O1K1O3101.88(16) N1C3C4115.16(14)
O3BK1K21137.20(18) O5C18C20111.02(17)
O3BK1K2137.67(19) O5C18C17110.07(15)
O3BK1O4121.35(19) O5C18C19110.82(19)
O3BK1O2132.4(2) C20C18C17105.60(16)
O3BK1Li1131.76(15) C20C18C19106.58(19)
O3BK1Li21120.40(15) C19C18C17112.58(17)
O3BK1C11B21.1(2) N2C17C18115.19(15)
O3BK1O37.3(3) O4C13Li2140.45(10)
O51K1K2144.30(4) O4C13C14112.7(2)
O51K1K2108.82(9) C14C13Li21150.86(17)
O51K1O471.16(9) O3BC9C10107.3(4)
O51K1O289.59(7) O3C9O3B18.0(4)
O51K1O3B101.21(15) O3C9C10110.0(5)
O51K1Li1120.22(8) O1C4C3109.94(15)
O51K1Li2135.49(6) O1C4C6110.45(17)
O51K1C11B96.58(11) O1C4C5110.81(17)
O51K1O3108.51(16) C6C4C3105.21(15)
Li1K1K251.66(6) C5C4C3112.72(16)
Li1K1K2176.00(8) C5C4C6107.53(17)
Li1K1Li21107.81(9) K2Li1K172.07(9)
Li1K1C11B142.91(10) O2Li1K161.02(9)
Li21K1K275.73(7) O21Li1K1115.18(12)
Li21K1K2150.35(6) O2Li1K2111.19(13)
Li21K1C11B105.06(12) O21Li1K262.92(9)
C11BK1K21140.12(10) O21Li1O294.54(14)
C11BK1K2123.59(10) O21Li1N1119.66(15)
O3K1K21143.7(2) O2Li1N1123.37(15)
O3K1K2131.9(2) O21Li1Li1150.07(13)
O3K1Li1125.61(17) O2Li1Li1149.36(11)
O3K1Li21126.17(18) O1Li1K153.99(10)
O3K1C11B23.1(2) O1Li1K257.73(9)
K1K2K1195.69(10) O1Li1O2114.25(16)
K11K2K2147.73(4) O1Li1O21119.87(17)
K1K2K2147.96(7) O1Li1N187.61(13)
O4K2K149.34(5) O1Li1Li11149.58(10)
O4K2K1184.66(7) N1Li1K1123.79(13)
O4K2K2155.98(6) N1Li1K2124.06(14)
O4K2C81146.94(5) N1Li1Li11122.72(9)
O4K2Li1101.85(10) Li11Li1K1101.09(12)
O4K2Li238.30(7) Li11Li1K2100.90(11)
O21K2K184.69(7) K2Li2K1172.54(9)
O21K2K1149.66(4) O4Li2K11114.87(13)
O21K2K2156.89(4) O41Li2K1159.47(9)
O21K2O4112.86(9) O41Li2K2111.46(13)
O21K2C8146.60(7) O4Li2K264.36(9)
O21K2Li138.23(7) O4Li2O4193.95(14)
O21K2Li2103.17(9) O41Li2N2129.13(16)
O1K2K145.00(4) O4Li2N2115.19(15)
O1K2K11117.65(8) O4Li2C131118.21(16)
O1K2K2179.92(6) O41Li2C13127.47(8)
O1K2O492.10(6) O4Li2Li2150.04(11)
O1K2O2176.05(7) O41Li2Li2148.78(13)
O1K2O5159.77(5) N2Li2K11127.87(13)
O1K2C81103.88(7) N2Li2K2118.50(14)
O1K2Li138.17(6) N2Li2C131103.81(13)
O1K2Li2127.08(8) N2Li2Li21123.63(10)
O5K2K1118.41(6) O5Li2K1153.76(10)
O5K2K1145.23(5) O5Li2K259.01(10)
O5K2K2179.86(4) O5Li2O4122.92(16)
O5K2O476.96(6) O5Li2O41112.11(18)
O5K2O2192.39(7) O5Li2N286.82(14)
O5K2C8178.51(8) O5Li2C131104.42(16)
O5K2Li1126.94(7) O5Li2Li21149.46(11)
O5K2Li238.85(7) C131Li2K1163.16(8)
C81K2K1162.31(7) C131Li2K2131.73(12)
C81K2K1130.46(5) Li21Li2K1199.42(12)
C81K2K2198.08(6) Li21Li2K2102.21(11)
Li1K2K156.27(7) Li21Li2C13168.75(17)
Li1K2K1181.70(7) O3BC11BK147.0(4)
Li1K2K2159.03(7) O3BC11BC12B112.5(5)
Li1K2C8176.02(8) O3BC11BC12123.0(5)
Li2K2K1157.11(7) O3BC11BO318.6(5)
Li2K2K182.08(8) C12BC11BK1124.4(3)
Li2K2K2159.08(7) C12BC11BC1239.7(3)
Li2K2C81113.08(9) C12C11BK1101.2(3)
Li2K2Li1118.11(11) C11C11BK1135.1(6)
K2O4K182.71(7) C11C11BO3B100.6(7)
C13O4K192.04(12) C11C11BC12B28.8(6)
C13O4K2115.95(12) C11C11BC1268.5(7)
C13O4Li2130.10(15) C11C11BO383.6(7)
C13O4Li21112.08(15) O3C11BK158.1(4)
Li2O4K1137.83(10) O3C11BC12B94.0(5)
Li21O4K184.32(12) O3C11BC12109.6(6)
Li21O4K2130.49(11) C12C12BC11B70.7(5)
Li2O4K277.34(10) C11C12BC11B24.6(5)
Li2O4Li2181.17(15) C11C12BC1295.2(7)
K21O2K182.67(7) C12BC12C11B69.5(5)
C7O2K191.68(11) C12BC12C1139.0(4)
C7O2K21112.55(12) C11C12C11B30.5(3)
C7O2Li1114.73(15) C11BC11O3B52.3(6)
C7O2Li11131.67(14) C11BC11C12B126.6(10)
Li1O2K182.41(10) C11BC11C1281.0(7)
Li11O2K1136.61(10) C11BC11O365.6(6)
Li11O2K2178.85(11) C12BC11O3B131.4(7)
Li1O2K21130.58(10) C12BC11C1245.7(5)
Li11O2Li180.57(14) C12BC11O3120.1(7)
K2O1K190.51(7) C12C11O3B108.2(5)
C4O1K1134.25(12) C12C11O3107.6(6)
C4O1K2128.08(13) O3C11O3B14.7(4)
C4O1Li1114.45(14) C9O3K1116.3(5)
Li1O1K190.14(12) C9O3C11106.3(7)
Li1O1K284.10(12) C11BO3K198.8(5)
C17N2Li296.40(13) C11BO3C9114.9(8)
C15N2C17112.62(18) C11BO3C1130.8(3)
C15N2Li2113.76(15) C11O3K1126.3(6)

11-X,+Y,3/2-Z

 

Table 6 Torsion Angles for C2c.
ABCDAngle/˚ ABCDAngle/˚
K1O4C13Li21-84.70(13) C9O3BC11BO374(2)
K1O4C13C1481.0(2) C9O3BC11C11B-135.4(8)
K1O2C7C881.33(16) C9O3BC11C12B115.7(10)
K1O1C4C391.66(18) C9O3BC11C12162.1(5)
K1O1C4C6-24.0(2) C9O3BC11O372(3)
K1O1C4C5-143.06(14) C4O1Li1K1140.15(14)
K1O1Li1K290.50(7) C4O1Li1K2-129.35(15)
K1O1Li1O21100.90(17) C4O1Li1O21-118.95(19)
K1O1Li1O2-10.12(14) C4O1Li1O2130.02(16)
K1O1Li1N1-135.92(9) C4O1Li1N14.22(16)
K1O1Li1Li1139.8(4) C4O1Li1Li11180.0(4)
K1O3BC9C1018.7(5) Li11O2C7C8-96.6(2)
K1O3BC9O3120(3) Li1O2C7C8163.75(15)
K1O3BC11BC12B-116.8(4) Li1O1C4C3-24.9(2)
K1O3BC11BC12-73.1(6) Li1O1C4C6-140.54(17)
K1O3BC11BC11-144.2(7) Li1O1C4C5100.40(18)
K1O3BC11BO3-121(3) Li1N1C3C4-35.94(18)
K1O3BC11C11B47.3(8) Li2O4C13Li2197.2(2)
K1O3BC11C12B-61.6(11) Li2O4C13C14-97.1(3)
K1O3BC11C12-15.2(8) Li21O4C13C14165.7(2)
K1O3BC11O3-105(3) Li2N2C17C18-41.9(2)
K11O5C18C20-15.7(2) Li2O5C18C20-129.40(18)
K11O5C18C17100.89(17) Li2O5C18C17-12.8(2)
K11O5C18C19-133.92(15) Li2O5C18C19112.36(19)
K1C11BC12BC1262.8(5) C11BO3BC9C10-179.3(5)
K1C11BC12BC11-122.5(11) C11BO3BC9O3-78(2)
K1C11BC12C12B-131.6(5) C11BO3BC11C12B-108.9(13)
K1C11BC12C11-134.3(6) C11BO3BC11C12-62.5(7)
K1C11BC11O3B-37.3(7) C11BO3BC11O3-152(3)
K1C11BC11C12B80.6(13) C11BC12BC12C112.2(5)
K1C11BC11C1284.2(8) C11BC12BC11O3B68.9(10)
K1C11BC11O3-29.9(8) C11BC12BC11C12-5.0(12)
K1C11BO3C9-124.5(6) C11BC12BC11O380.6(11)
K1C11BO3C11155.5(7) C11BC12C11O3B45.3(5)
K2O4C13Li21-167.59(16) C11BC12C11C12B176.0(10)
K2O4C13C14-1.9(2) C11BC12C11O360.7(6)
K21O2C7C8-1.43(18) C11BC11O3K130.5(8)
K2O1C4C3-127.16(14) C11BC11O3C9-111.5(7)
K2O1C4C6117.17(16) C12BC11BC12C11-2.7(6)
K2O1C4C5-1.9(2) C12BC11BC11O3B-117.9(10)
K2O1Li1K1-90.50(7) C12BC11BC11C123.6(9)
K2O1Li1O2110.40(15) C12BC11BC11O3-110.5(10)
K2O1Li1O2-100.62(15) C12BC11BO3K1-128.6(4)
K2O1Li1N1133.58(10) C12BC11BO3C9106.9(6)
K2O1Li1Li11-50.7(4) C12BC11BO3C1126.9(6)
K2O5C18C20126.87(17) C12BC12C11O3B-130.7(8)
K2O5C18C17-116.57(17) C12BC12C11C11B-176.0(10)
K2O5C18C198.6(2) C12BC12C11O3-115.2(8)
O2C7C8K211.12(14) C12BC11O3K1-89.1(9)
N1C3C4O144.0(2) C12BC11O3C9128.9(8)
N1C3C4C6162.91(16) C12BC11O3C11B-119.6(11)
N1C3C4C5-80.2(2) C12C11BC12BC11174.8(13)
O3BC9O3K1-42(2) C12C11BC11O3B-121.5(6)
O3BC9O3C11B73(2) C12C11BC11C12B-3.6(9)
O3BC9O3C11104(2) C12C11BC11O3-114.1(6)
O3BC11BC12BC12115.1(7) C12C11BO3K1-91.2(4)
O3BC11BC12BC11-70.1(11) C12C11BO3C9144.3(5)
O3BC11BC12C12B-86.2(7) C12C11BO3C1164.4(7)
O3BC11BC12C11-88.9(8) C12C12BC11O3B73.9(10)
O3BC11BC11C12B117.9(10) C12C12BC11C11B5.0(12)
O3BC11BC11C12121.5(6) C12C12BC11O385.6(9)
O3BC11BC11O37.4(8) C12C11O3K1-40.6(8)
O3BC11BO3K148(2) C12C11O3C9177.4(5)
O3BC11BO3C9-77(2) C12C11O3C11B-71.1(7)
O3BC11BO3C11-157(3) C11O3BC9C10-158.7(3)
O3BC11O3K154(3) C11O3BC9O3-57(2)
O3BC11O3C9-88(3) C11O3BC11BK1144.2(7)
O3BC11O3C11B24(3) C11O3BC11BC12B27.5(6)
O5C18C17N241.2(2) C11O3BC11BC1271.1(7)
C2N1C3C481.69(19) C11O3BC11BO324(3)
C1N1C3C4-158.27(16) C11C11BC12BC12-174.8(13)
C20C18C17N2161.06(17) C11C11BC12C12B2.7(6)
C15N2C17C1877.2(2) C11C11BO3K1-155.5(7)
C16N2C17C18-162.48(17) C11C11BO3C980.0(8)
C19C18C17N2-83.0(2) C11C12BC12C11B-2.2(5)
C10C9O3K142.5(5) O3C11BC12BC12116.3(7)
C10C9O3C11B157.2(5) O3C11BC12BC11-68.9(11)
C10C9O3C11-171.1(4) O3C11BC12C12B-71.7(7)
C9O3BC11BK1-165.3(7) O3C11BC12C11-74.4(7)
C9O3BC11BC12B77.9(7) O3C11BC11O3B-7.4(8)
C9O3BC11BC12121.6(6) O3C11BC11C12B110.5(10)
C9O3BC11BC1150.5(9) O3C11BC11C12114.1(6)

11-X,+Y,3/2-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for C2c.
AtomxyzU(eq)
H2A40556788560442
H2B44847658616242
H2C37067822556942
H3A28887009565123
H3B30326601642923
H1A43988037716836
H1B38307556728236
H1C36288320662136
H20A63203032602963
H20B64371902590163
H20C66502280671263
H6A23374471546253
H6B20705586530953
H6C24405154613253
H15A43241107547654
H15B4190185585754
H15C457628542054
H16A5419-766656744
H16B4992-463693544
H16C5760-138731644
H19A46742136509966
H19B52331766492866
H19C51792914507266
H10A2573(15)5410(20)7562(17)68
H5A35075589510256
H5B27375917468956
H5C29314771483056
H9AA23033655808646
H9AB17874232734046
H9BC24183576807946
H9BD17844208748746
H11A21522323730839
H11B25422319686839
H12A16553279591566
H12B12583188634666
H12C14002222601066
H8A5067(11)5405(16)9406(12)26(5)
H8B4335(11)5698(16)9231(11)28(6)
H7A4569(10)6504(16)8418(11)20(5)
H7B3933(10)5795(14)7964(10)18(5)
H8C4460(11)4628(18)8965(12)35(6)
H13A3754(10)1027(15)6530(11)22(5)
H13B3483(12)1753(18)6915(13)43(7)
H14A2799(16)1780(20)5621(17)72(9)
H14B3145(14)2830(20)5877(15)56(8)
H14C3402(19)2060(30)5510(20)104(15)
H12D18333068579574
H12E15891996587774
H12F23702264632574
H11C19612335710552
H11D13973109656452
H17A5688(11)537(17)5927(12)31(6)
H17B6097(11)913(15)6760(12)24(5)
H10B3114(16)4860(20)8309(16)63(9)
H10C2516(16)5320(30)8316(18)81(10)

 

Table 8 Atomic Occupancy for C2c.
AtomOccupancy AtomOccupancy AtomOccupancy
O3B0.5 H9AA0.5 H9AB0.5
H9BC0.5 H9BD0.5 C11B0.5
H11A0.5 H11B0.5 C12B0.5
H12A0.5 H12B0.5 H12C0.5
C120.5 H12D0.5 H12E0.5
H12F0.5 C110.5 H11C0.5
H11D0.5 O30.5   

Experimental

Single crystals of C20H48K2Li2N2O5 [C2c] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 100.01 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 [C2c]

Crystal Data for C20H48K2Li2N2O5 (=488.68 g/mol): monoclinic, space group C2/c (no. 15), a = 23.29(2) Å, b = 13.532(9) Å, c = 21.12(3) Å, β = 121.01(3)°, = 5705(10) Å3, Z = 8, T = 100.01 K, μ(MoKα) = 0.360 mm-1, Dcalc = 1.138 g/cm3, 6223 reflections measured (4.902° ≤ 2Θ ≤ 53.998°), 6223 unique (Rint = ?, Rsigma = 0.0265) which were used in all calculations. The final R1 was 0.0428 (I > 2σ(I)) and wR2 was 0.0907 (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, All C(H,H,H,H) groups
At 1.5 times of:
All C(H) groups, All C(H,H,H) groups
2. Others
Fixed Sof: O3B(0.5) H9AA(0.5) H9AB(0.5) H9BC(0.5) H9BD(0.5) C11B(0.5)
H11A(0.5) H11B(0.5) C12B(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C12(0.5) H12D(0.5)
H12E(0.5) H12F(0.5) C11(0.5) H11C(0.5) H11D(0.5) O3(0.5)
3.a Secondary CH2 refined with riding coordinates:
C3(H3A,H3B), C9(H9AA,H9AB), C9(H9BC,H9BD), C11B(H11A,H11B), C11(H11C,H11D)
3.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C6(H6A,H6B,H6C),
C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C5(H5A,H5B,H5C),
C12B(H12A,H12B,H12C), C12(H12D,H12E,H12F)

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