mo_B0483_0m

Table 1 Crystal data and structure refinement for mo_B0483_0m.
Identification code mo_B0483_0m
Empirical formula C26H58Li4N2O6
Formula weight 522.50
Temperature/K 100.0
Crystal system orthorhombic
Space group Pbca
a/Å 16.8564(9)
b/Å 19.0045(15)
c/Å 20.4178(12)
α/° 90
β/° 90
γ/° 90
Volume/Å3 6540.8(7)
Z 8
ρcalcg/cm3 1.061
μ/mm‑1 0.071
F(000) 2304.0
Crystal size/mm3 0.49 × 0.16 × 0.15
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.664 to 54
Index ranges -19 ≤ h ≤ 21, -20 ≤ k ≤ 24, -25 ≤ l ≤ 26
Reflections collected 53100
Independent reflections 7136 [Rint = 0.0439, Rsigma = 0.0273]
Data/restraints/parameters 7136/0/386
Goodness-of-fit on F2 1.026
Final R indexes [I>=2σ (I)] R1 = 0.0390, wR2 = 0.0913
Final R indexes [all data] R1 = 0.0587, wR2 = 0.1020
Largest diff. peak/hole / e Å-3 0.30/-0.19

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0483_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O63454.0(5)6999.5(4)6239.1(4)16.32(19)
O33660.3(5)5703.0(4)7003.6(4)16.47(18)
O15459.5(5)4975.5(5)6983.8(4)22.6(2)
O52665.3(5)7124.6(5)4363.0(4)22.8(2)
O44563.3(5)7077.3(5)4910.3(4)22.4(2)
O24936.7(5)5503.8(5)8695.9(5)27.0(2)
N23380.4(6)8029.4(5)5246.1(5)17.2(2)
N14202.8(7)4583.1(6)7803.6(5)22.1(2)
C83099.5(7)5341.5(7)7385.0(6)17.8(3)
C182956.8(7)7579.6(6)6345.1(6)17.3(3)
C243227.1(7)5645.9(7)5171.1(6)17.8(3)
C173272.0(8)8205.7(7)5942.9(6)19.9(3)
C114151.3(7)8261.8(7)4991.8(6)21.4(3)
C263678.6(8)4955.9(7)5284.3(7)22.4(3)
C215164.8(7)6737.7(7)7484.7(6)19.4(3)
C73404.5(8)4589.9(7)7507.6(6)22.2(3)
C142724.3(8)8274.5(7)4830.6(6)22.5(3)
C252371.0(8)5448.7(7)4993.0(6)22.5(3)
C124795.9(8)7743.7(7)5167.3(7)24.2(3)
C152682.7(8)7855.8(7)4203.2(6)23.9(3)
C25046.1(9)4335.9(7)6847.4(7)25.7(3)
C102956.6(8)5741.7(7)8026.6(6)23.0(3)
C92307.7(8)5278.6(8)7021.0(7)25.1(3)
C192100.3(8)7392.5(8)6161.0(7)25.6(3)
C202971.3(9)7806.3(7)7066.1(6)25.8(3)
C234882.1(8)7204.1(7)8052.1(6)23.2(3)
C14726.8(9)4063.0(7)7487.4(7)29.1(3)
C44175.3(9)4470.8(8)8517.3(6)27.3(3)
C65591.0(8)5822.4(8)9021.4(7)29.7(3)
C225663.4(9)7189.8(8)7020.2(7)28.5(3)
C162672.3(9)6713.9(8)3778.6(6)30.3(3)
C35807.2(9)5260.3(8)6408.0(7)30.1(3)
C54890.8(9)4780.3(8)8851.3(7)29.9(3)
C135170.7(9)6563.4(8)4971.4(9)37.8(4)
Li43453.9(12)6866.6(11)5255.6(10)20.0(4)
Li14677.9(12)5611.5(11)7479.8(11)21.9(5)
Li24050.5(12)6639.0(11)6962.2(10)20.3(4)
Li33275.0(13)6012.5(11)6172.5(10)20.1(4)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0483_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
O621.3(4)11.8(4)15.8(4)-0.3(3)0.5(3)3.4(3)
O319.1(4)14.1(4)16.2(4)3.6(3)0.5(3)-2.9(3)
O124.2(5)22.2(5)21.3(4)-1.3(4)1.0(4)2.8(4)
O533.1(5)18.8(5)16.4(4)2.7(4)-3.8(4)-2.8(4)
O421.4(4)17.0(5)28.6(5)1.2(4)3.8(4)3.1(4)
O224.5(5)27.8(5)28.7(5)8.0(4)-5.7(4)2.0(4)
N220.6(5)14.7(5)16.2(5)2.2(4)-0.5(4)1.8(4)
N130.7(6)17.7(6)17.8(5)4.7(4)2.3(4)4.2(5)
C819.6(6)17.4(6)16.4(6)1.0(5)1.7(5)-3.4(5)
C1821.4(6)14.5(6)16.1(6)-0.3(5)0.0(5)4.5(5)
C2421.8(6)16.0(6)15.6(6)0.0(5)-0.1(5)1.4(5)
C1727.9(7)13.4(6)18.3(6)-2.0(5)-0.2(5)3.3(5)
C1126.4(7)16.0(6)21.9(6)2.5(5)1.7(5)-4.1(5)
C2626.2(7)18.8(7)22.2(6)-0.4(5)0.9(5)3.1(5)
C2119.9(6)18.6(7)19.8(6)2.1(5)-0.6(5)-1.5(5)
C729.8(7)16.6(6)20.3(6)1.9(5)3.0(5)-4.6(5)
C1425.8(7)17.9(7)23.9(6)5.6(5)-2.5(5)5.9(5)
C2523.7(6)22.4(7)21.2(6)1.7(5)-0.3(5)0.2(5)
C1221.4(6)23.6(7)27.6(7)2.9(5)-0.7(5)-4.7(5)
C1529.1(7)22.0(7)20.6(6)7.9(5)-5.3(5)1.0(5)
C232.3(7)18.8(7)25.9(7)-4.2(5)2.8(6)4.7(5)
C1025.4(7)24.1(7)19.7(6)-1.5(5)2.7(5)1.9(5)
C922.0(7)29.7(8)23.7(7)0.7(6)0.6(5)-7.0(6)
C1920.6(6)29.1(8)27.2(7)4.1(6)2.2(5)2.3(5)
C2038.3(8)20.8(7)18.2(6)-1.9(5)2.3(6)7.3(6)
C2321.8(6)24.2(7)23.8(6)0.3(5)-0.2(5)0.3(5)
C140.6(8)15.8(7)31.1(7)3.0(6)4.4(6)8.3(6)
C437.5(8)23.4(7)21.1(6)9.9(5)3.2(6)2.4(6)
C621.9(7)42.7(9)24.5(7)3.4(6)-1.8(6)2.9(6)
C2234.1(8)25.2(8)26.2(7)-1.9(6)5.6(6)-7.1(6)
C1644.5(9)28.4(8)17.9(6)-0.1(6)-7.0(6)-4.8(6)
C327.8(7)34.5(8)28.1(7)1.6(6)6.7(6)-0.3(6)
C539.2(8)28.5(8)21.9(7)9.7(6)-0.6(6)9.2(6)
C1327.0(7)28.5(8)57.7(10)5.8(7)7.7(7)10.1(6)
Li423.8(10)15.8(11)20.5(10)-0.3(8)2.1(8)-0.5(8)
Li121.3(10)18.7(11)25.9(11)-0.3(9)-1.4(9)2.8(9)
Li223.7(10)17.7(11)19.4(10)1.5(8)-2.7(8)-0.7(8)
Li326.0(11)16.9(11)17.5(10)1.3(8)-1.3(8)-0.6(9)

 

Table 4 Bond Lengths for mo_B0483_0m.
AtomAtomLength/Å AtomAtomLength/Å
O6C181.4017(14) N1Li12.213(2)
O6Li42.024(2) C8C71.5385(18)
O6Li21.913(2) C8C101.5337(17)
O6Li31.905(2) C8C91.5324(18)
O3C81.4044(14) C8Li12.717(2)
O3Li11.979(2) C18C171.5403(17)
O3Li21.898(2) C18C191.5337(18)
O3Li31.910(2) C18C201.5340(17)
O1C21.4286(16) C18Li42.736(2)
O1C31.4207(16) C24C261.5336(18)
O1Li12.055(2) C24C251.5345(17)
O5C151.4278(16) C24Li42.358(2)
O5C161.4260(16) C24Li32.162(2)
O5Li42.308(2) C11C121.5094(18)
O4C121.4259(16) C26Li32.790(3)
O4C131.4204(16) C21C231.5344(18)
O4Li42.038(2) C21C221.5310(18)
O2C61.4230(17) C21Li12.292(3)
O2C51.4133(17) C21Li22.168(2)
O2Li12.529(2) C14C151.5095(18)
N2C171.4732(15) C2C11.5053(19)
N2C111.4673(16) C9Li32.758(3)
N2C141.4696(15) C4C51.505(2)
N2Li42.213(2) Li4Li32.496(3)
N1C71.4753(17) Li1Li22.459(3)
N1C11.4744(17) Li2Li32.393(3)
N1C41.4735(16)    

 

Table 5 Bond Angles for mo_B0483_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C18O6Li4104.55(9) N1C1C2111.31(11)
C18O6Li2118.47(9) N1C4C5111.49(11)
C18O6Li3133.71(10) O2C5C4108.80(11)
Li2O6Li4136.14(10) O6Li4O5139.19(11)
Li3O6Li478.83(9) O6Li4O4108.59(10)
Li3O6Li277.63(9) O6Li4N283.35(8)
C8O3Li1105.54(9) O6Li4C1829.73(5)
C8O3Li2135.75(10) O6Li4C24101.27(9)
C8O3Li3114.49(9) O6Li4Li348.47(7)
Li2O3Li178.70(9) O5Li4C18111.12(9)
Li2O3Li377.86(9) O5Li4C2493.31(8)
Li3O3Li1139.31(10) O5Li4Li3131.35(11)
C2O1Li1106.48(10) O4Li4O5102.33(9)
C3O1C2111.35(10) O4Li4N281.50(8)
C3O1Li1116.63(10) O4Li4C18117.71(10)
C15O5Li4112.04(9) O4Li4C24108.46(10)
C16O5C15109.96(10) O4Li4Li3119.87(11)
C16O5Li4122.66(10) N2Li4O575.45(7)
C12O4Li4107.42(9) N2Li4C1859.71(6)
C13O4C12112.35(11) N2Li4C24166.59(11)
C13O4Li4119.73(10) N2Li4Li3130.48(11)
C6O2Li1123.90(9) C24Li4C18119.81(9)
C5O2C6110.58(11) C24Li4Li352.80(7)
C5O2Li1106.84(9) Li3Li4C1871.05(8)
C17N2Li4103.04(9) O3Li1O1111.43(11)
C11N2C17112.52(10) O3Li1O2129.70(10)
C11N2C14111.52(10) O3Li1N184.88(9)
C11N2Li4104.72(9) O3Li1C829.87(5)
C14N2C17113.08(10) O3Li1C21103.32(10)
C14N2Li4111.33(9) O3Li1Li249.19(7)
C7N1Li1101.53(9) O1Li1O2109.00(9)
C1N1C7111.89(11) O1Li1N181.94(9)
C1N1Li1104.14(10) O1Li1C8118.81(10)
C4N1C7112.19(10) O1Li1C21108.77(10)
C4N1C1110.79(10) O1Li1Li2122.07(11)
C4N1Li1115.77(10) O2Li1C8102.92(8)
O3C8C7108.63(10) N1Li1O272.40(7)
O3C8C10109.67(10) N1Li1C860.01(6)
O3C8C9110.82(10) N1Li1C21162.32(12)
O3C8Li144.59(7) N1Li1Li2132.37(11)
C7C8Li180.59(8) C21Li1O290.54(8)
C10C8C7111.95(10) C21Li1C8121.82(9)
C10C8Li189.96(9) C21Li1Li254.16(8)
C9C8C7107.31(11) Li2Li1O2124.07(10)
C9C8C10108.43(11) Li2Li1C872.43(8)
C9C8Li1154.47(10) O6Li2C21143.52(12)
O6C18C17108.61(10) O6Li2Li1147.34(12)
O6C18C19110.03(10) O6Li2Li351.03(7)
O6C18C20111.07(10) O3Li2O6100.82(10)
O6C18Li445.72(6) O3Li2C21111.06(11)
C17C18Li481.00(8) O3Li2Li152.11(8)
C19C18C17111.91(10) O3Li2Li351.28(7)
C19C18C20108.38(11) C21Li2Li158.99(8)
C19C18Li488.52(9) C21Li2Li3147.97(12)
C20C18C17106.81(10) Li3Li2Li197.43(10)
C20C18Li4156.12(10) O6Li3O3100.71(10)
C26C24C25107.08(11) O6Li3C24113.01(11)
C26C24Li4138.57(10) O6Li3C26135.77(10)
C26C24Li396.57(10) O6Li3C9123.15(10)
C25C24Li4114.21(10) O6Li3Li452.70(7)
C25C24Li3109.76(10) O6Li3Li251.34(8)
Li3C24Li466.89(8) O3Li3C24138.93(12)
N2C17C18112.45(10) O3Li3C26105.84(9)
N2C11C12110.92(10) O3Li3C959.14(7)
C24C26Li350.33(7) O3Li3Li4145.65(12)
C23C21Li1115.56(10) O3Li3Li250.86(7)
C23C21Li298.77(10) C24Li3C2633.10(5)
C22C21C23108.30(11) C24Li3C9114.15(10)
C22C21Li1135.87(10) C24Li3Li460.31(8)
C22C21Li2102.67(10) C24Li3Li2144.90(12)
Li2C21Li166.85(8) C9Li3C26100.87(8)
N1C7C8112.31(10) Li4Li3C2687.20(8)
N2C14C15110.96(10) Li4Li3C9150.63(11)
O4C12C11107.11(10) Li2Li3C26131.52(10)
O5C15C14108.67(10) Li2Li3C998.71(9)
O1C2C1107.36(11) Li2Li3Li496.65(10)
C8C9Li375.54(8)     

 

Table 6 Torsion Angles for mo_B0483_0m.
ABCDAngle/˚ ABCDAngle/˚
O6C18C17N253.24(13) Li4O4C12C11-53.82(12)
O3C8C7N154.92(13) Li4N2C17C18-20.59(12)
O3C8C9Li3-0.56(9) Li4N2C11C12-29.74(12)
O1C2C1N157.95(15) Li4N2C14C15-42.02(13)
N2C11C12O457.03(13) Li4C18C17N216.30(10)
N2C14C15O552.43(14) Li4C24C26Li362.18(14)
N1C4C5O256.77(15) Li1O3C8C7-53.99(12)
C8O3Li2O6-99.65(14) Li1O3C8C1068.66(12)
C8O3Li2C2198.40(15) Li1O3C8C9-171.65(11)
C8O3Li2Li1100.74(14) Li1O3Li2O6159.61(11)
C8O3Li2Li3-112.76(14) Li1O3Li2C21-2.34(11)
C17N2C11C1281.45(13) Li1O3Li2Li3146.50(10)
C17N2C14C15-157.46(10) Li1O1C2C1-53.92(13)
C11N2C17C18-132.83(11) Li1O2C5C4-44.64(13)
C11N2C14C1574.54(13) Li1N1C7C8-24.72(12)
C7N1C1C278.79(14) Li1N1C1C2-30.08(14)
C7N1C4C5-154.06(11) Li1N1C4C5-38.17(15)
C7C8C9Li3-119.02(10) Li1C8C7N119.78(10)
C14N2C17C1899.71(12) Li1C8C9Li3-14.2(2)
C14N2C11C12-150.25(11) Li2O6C18C17115.19(11)
C25C24C26Li3-113.04(11) Li2O6C18C19-122.00(11)
C10C8C7N1-66.34(13) Li2O6C18C20-1.99(15)
C10C8C9Li3119.87(10) Li2O6C18Li4171.21(13)
C9C8C7N1174.79(10) Li2O3C8C7-143.64(13)
C19C18C17N2-68.43(13) Li2O3C8C10-20.99(17)
C20C18C17N2173.11(10) Li2O3C8C998.70(15)
C1N1C7C8-135.25(11) Li2O3C8Li1-89.65(14)
C1N1C4C580.09(14) Li3O6C18C17-144.36(12)
C4N1C7C899.50(12) Li3O6C18C19-21.55(17)
C4N1C1C2-155.19(12) Li3O6C18C2098.46(14)
C6O2C5C4177.96(11) Li3O6C18Li4-88.35(14)
C16O5C15C14-176.66(11) Li3O3C8C7118.52(11)
C3O1C2C1177.95(11) Li3O3C8C10-118.83(11)
C13O4C12C11172.48(11) Li3O3C8C90.85(14)
Li4O6C18C17-56.01(12) Li3O3C8Li1172.51(13)
Li4O6C18C1966.80(12) Li3O3Li2O613.11(10)
Li4O6C18C20-173.19(11) Li3O3Li2C21-148.84(12)
Li4O5C15C14-36.62(13) Li3O3Li2Li1-146.50(10)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0483_0m.
AtomxyzU(eq)
H17A28958603598024
H17B37868360612824
H11A42838729517726
H11B41218309451026
H7A30314342780227
H7B34194331708727
H14A28018779472627
H14B22188226507227
H25A23725151460134
H25B20665878490634
H25C21295191535834
H12A53087892497429
H12B48587716564929
H15A21997985395529
H15B31517960392729
H2A54113987664931
H2B46064424653731
H10A34645819824935
H10B26065465831035
H10C27096196793035
H19A20877211571238
H19B17687814619138
H19C18997033646238
H20A27937415734239
H20B26178210712839
H20C35137939718939
H23A53427421826635
H23B45926916837135
H23C45327573788235
H1A44273623740835
H1B51743952778435
H4A41513960860933
H4B36894690869733
H6A55195783949645
H6B56236320889945
H6C60825584889345
H22A53267549681743
H22B58946891667943
H22C60897419726743
H16A22176843350545
H16B26406214389245
H16C31656803353745
H3A61854921622545
H3B60865698651745
H3C53915359608645
H5A48464719933136
H5B53774536870236
H13A56286702470457
H13B49716107482157
H13C53326527543157
H243461(8)5870(7)4763(7)19(3)
H215532(9)6385(8)7682(7)28(4)
H26A3495(9)4707(8)5692(7)27(4)
H26B3604(9)4597(8)4913(8)33(4)
H9A2383(9)5028(8)6603(8)30(4)
H9B1920(10)5014(9)7275(8)40(5)
H9C2093(9)5756(9)6934(7)31(4)
H26C4279(9)5039(8)5329(7)25(4)

Experimental

Single crystals of C26H58Li4N2O6 [mo_B0483_0m] were []. A suitable crystal was selected and [] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 100.0 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 XH [3] refinement package using CGLS 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_B0483_0m]

Crystal Data for C26H58Li4N2O6 (=522.50 g/mol): orthorhombic, space group Pbca (no. 61), a = 16.8564(9) Å, b = 19.0045(15) Å, c = 20.4178(12) Å, = 6540.8(7) Å3, Z = 8, T = 100.0 K, μ(MoKα) = 0.071 mm-1, Dcalc = 1.061 g/cm3, 53100 reflections measured (4.664° ≤ 2Θ ≤ 54°), 7136 unique (Rint = 0.0439, Rsigma = 0.0273) which were used in all calculations. The final R1 was 0.0390 (I > 2σ(I)) and wR2 was 0.1020 (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:
C17(H17A,H17B), C11(H11A,H11B), C7(H7A,H7B), C14(H14A,H14B), C12(H12A,H12B),
C15(H15A,H15B), C2(H2A,H2B), C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B)
2.b Idealised Me refined as rotating group:
C25(H25A,H25B,H25C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,
H20C), C23(H23A,H23B,H23C), C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C16(H16A,
H16B,H16C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C)

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