mo_B0378_0m

Table 1 Crystal data and structure refinement for mo_B0378_0m.
Identification code mo_B0378_0m
Empirical formula C14H31Li2NO3
Formula weight 275.28
Temperature/K 99.99
Crystal system triclinic
Space group P-1
a/Å 9.9122(8)
b/Å 13.2804(10)
c/Å 14.5570(12)
α/° 81.866(3)
β/° 88.357(3)
γ/° 68.748(3)
Volume/Å3 1767.4(2)
Z 4
ρcalcg/cm3 1.035
μ/mm‑1 0.068
F(000) 608.0
Crystal size/mm3 1.32 × 0.96 × 0.27
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.41 to 58
Index ranges -13 ≤ h ≤ 13, -18 ≤ k ≤ 18, -19 ≤ l ≤ 19
Reflections collected 86037
Independent reflections 9360 [Rint = 0.0680, Rsigma = 0.0339]
Data/restraints/parameters 9360/0/455
Goodness-of-fit on F2 1.022
Final R indexes [I>=2σ (I)] R1 = 0.0461, wR2 = 0.1228
Final R indexes [all data] R1 = 0.0538, wR2 = 0.1291
Largest diff. peak/hole / e Å-3 0.50/-0.24

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0378_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O63987.2(7)8065.8(5)6898.2(5)16.55(15)
O36607.1(8)8025.3(6)7767.8(5)17.35(15)
O43846.3(8)5703.4(6)6576.6(5)20.27(16)
O18200.4(8)5746.3(6)9139.5(5)20.33(16)
O51280.1(9)8273.8(7)3157.7(6)30.7(2)
O28986.6(11)7139.8(7)11308.8(6)31.5(2)
N18722.6(10)7718.6(7)9191.0(6)18.55(18)
N21966.6(9)7728.1(7)5687.0(6)16.70(17)
C182755.3(11)8956.5(8)6540.5(7)17.20(19)
C256643.3(12)6643.0(9)5566.9(7)21.2(2)
C78730.9(11)8299.7(9)8240.5(7)20.2(2)
C214617.6(11)7462.2(8)9565.6(7)17.86(19)
C29524.0(12)5831.7(9)8788.5(8)21.6(2)
C87204.6(11)8837.3(8)7787.3(7)18.3(2)
C122358.0(12)6045.4(9)6813.2(8)23.4(2)
C171550.3(11)8530.5(8)6357.3(7)18.5(2)
C111479.9(11)6809.2(9)5993.9(8)22.2(2)
C19874.2(11)6617.5(9)9310.2(7)21.5(2)
C48928.1(12)8361.0(9)9894.5(7)23.3(2)
C141297.1(11)8268.1(9)4767.3(7)22.0(2)
C134743.4(15)4836.2(10)7233.4(9)31.8(3)
C193138.9(13)9557.3(9)5652.4(8)25.1(2)
C243500.9(13)6987.1(10)9325.0(8)27.6(2)
C152077.1(13)7691.2(10)3974.7(7)27.2(2)
C202182.5(13)9760.5(9)7245.7(8)27.4(2)
C233772.6(14)8587.1(10)9837.9(8)27.9(2)
C225412.7(14)6740.0(11)10446.9(8)28.3(2)
C97366.6(13)9362.3(10)6802.4(7)26.0(2)
C58260.2(13)8198.9(9)10823.6(8)26.0(2)
C106224.3(13)9734.1(9)8322.9(8)24.4(2)
C37699.7(13)5084.3(9)8648.2(8)26.9(2)
C286219.8(14)5985.7(12)4930.3(9)32.6(3)
C161890.0(16)7823.6(12)2352.4(9)38.7(3)
C68480.3(19)7031.1(12)12229.6(9)41.6(3)
C278099.5(14)5893.3(14)6009.4(9)41.3(3)
C266915(2)7565.3(13)4935.4(12)51.6(5)
Li16834.9(19)7279.0(15)9045.2(12)20.1(3)
Li24695.0(19)8071.6(15)8084.6(12)19.7(3)
Li35996.7(19)7741.2(15)6641.2(12)20.1(3)
Li44352.2(19)6978.4(14)6087.7(12)19.6(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0378_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
O616.7(3)15.4(3)13.9(3)-2.5(2)-1.7(2)-1.2(3)
O320.7(3)20.8(3)14.0(3)-3.2(3)2.0(3)-11.4(3)
O423.3(4)16.4(3)18.9(3)1.5(3)-1.9(3)-5.9(3)
O120.8(4)20.7(3)21.3(4)-6.0(3)0.1(3)-8.4(3)
O530.1(4)34.5(5)17.8(4)-4.4(3)-6.3(3)0.7(4)
O246.1(5)25.6(4)19.6(4)-5.4(3)3.0(4)-8.5(4)
N121.3(4)20.7(4)14.8(4)-3.7(3)-0.3(3)-8.4(3)
N217.6(4)16.6(4)14.6(4)-1.8(3)-1.3(3)-4.7(3)
C1818.3(4)14.2(4)16.1(4)-1.8(3)-1.9(3)-2.3(4)
C2525.4(5)22.1(5)19.3(5)-9.4(4)6.6(4)-10.4(4)
C721.0(5)25.4(5)17.9(5)-3.0(4)3.1(4)-12.9(4)
C2120.8(5)20.6(4)12.9(4)-2.0(3)1.9(3)-8.6(4)
C219.6(5)23.6(5)21.2(5)-6.9(4)1.4(4)-6.3(4)
C822.2(5)20.5(5)15.1(4)-2.1(3)2.5(4)-11.4(4)
C1228.0(5)22.5(5)21.2(5)-1.6(4)6.5(4)-11.9(4)
C1716.1(4)18.4(4)18.0(4)-4.1(4)1.4(3)-2.3(4)
C1119.7(5)23.4(5)25.8(5)-4.2(4)1.3(4)-10.4(4)
C117.9(5)25.3(5)21.9(5)-5.9(4)-1.3(4)-7.2(4)
C428.6(5)23.6(5)21.2(5)-6.2(4)-2.1(4)-12.3(4)
C1420.4(5)22.1(5)18.5(5)-2.7(4)-4.6(4)-1.6(4)
C1341.8(7)22.3(5)26.8(6)4.3(4)-11.4(5)-8.4(5)
C1928.1(5)20.8(5)24.1(5)5.9(4)-4.0(4)-9.1(4)
C2429.3(6)34.5(6)24.8(5)-2.9(5)2.2(4)-18.8(5)
C1529.2(6)26.7(5)17.4(5)-2.3(4)-3.3(4)-0.1(4)
C2027.6(5)20.4(5)28.1(6)-11.0(4)-4.8(4)1.8(4)
C2336.4(6)25.5(5)20.4(5)-6.4(4)9.8(5)-8.8(5)
C2231.0(6)34.0(6)17.2(5)3.3(4)-0.5(4)-11.0(5)
C931.5(6)31.1(6)18.1(5)2.8(4)1.7(4)-17.0(5)
C532.0(6)24.3(5)20.9(5)-8.4(4)-0.3(4)-7.3(4)
C1028.4(5)20.4(5)24.9(5)-5.3(4)2.6(4)-8.9(4)
C329.6(6)26.0(5)28.4(6)-7.6(4)-5.6(4)-12.2(5)
C2829.6(6)41.3(7)31.3(6)-20.8(5)2.9(5)-12.4(5)
C1644.9(8)45.4(7)19.0(5)-8.6(5)-1.9(5)-6.8(6)
C665.6(10)38.2(7)21.7(6)-6.6(5)9.2(6)-19.4(7)
C2724.6(6)69.2(10)28.8(6)-13.4(6)4.2(5)-13.3(6)
C2687.2(13)36.9(7)41.6(8)-17.5(6)38.7(9)-33.6(8)
Li120.4(8)21.7(8)17.4(8)-1.4(6)0.5(6)-7.3(7)
Li220.7(8)24.3(8)14.1(7)-4.0(6)1.9(6)-7.7(7)
Li322.7(8)22.4(8)15.9(8)-5.6(6)3.4(6)-8.1(7)
Li421.8(8)18.7(8)18.3(8)-4.1(6)1.0(6)-6.9(7)

 

Table 4 Bond Lengths for mo_B0378_0m.
AtomAtomLength/Å AtomAtomLength/Å
O6C181.4059(11) C18C171.5390(14)
O6Li21.8848(19) C18C191.5337(14)
O6Li31.9167(19) C18C201.5341(14)
O6Li41.9201(18) C25C281.5210(15)
O3C81.4096(12) C25C271.5230(18)
O3Li11.9574(19) C25C261.5244(17)
O3Li21.9189(19) C25Li32.2122(19)
O3Li31.8962(19) C25Li42.279(2)
O4C121.4249(13) C7C81.5410(15)
O4C131.4234(13) C21C241.5287(15)
O4Li41.9695(19) C21C231.5270(15)
O1C21.4311(13) C21C221.5325(15)
O1C31.4302(12) C21Li12.243(2)
O1Li11.9819(19) C21Li22.202(2)
O5C151.4097(13) C2C11.5127(14)
O5C161.4116(15) C8C91.5338(14)
O2C51.4176(14) C8C101.5332(14)
O2C61.4243(15) C12C111.5120(15)
N1C71.4873(13) C4C51.5111(16)
N1C11.4836(14) C14C151.5118(15)
N1C41.4844(13) Li1Li22.387(3)
N1Li12.176(2) Li1Li33.536(2)
N2C171.4867(12) Li2Li32.443(2)
N2C111.4771(13) Li2Li43.504(2)
N2C141.4769(13) Li3Li42.416(3)
N2Li42.265(2)    

 

Table 5 Bond Angles for mo_B0378_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C18O6Li2117.70(8) N2C17C18113.04(8)
C18O6Li3130.50(8) N2C11C12112.86(9)
C18O6Li4107.16(8) N1C1C2112.40(8)
Li2O6Li379.97(8) N1C4C5115.52(9)
Li2O6Li4134.16(8) N2C14C15113.43(8)
Li3O6Li478.05(8) O5C15C14106.55(9)
C8O3Li1104.60(8) O2C5C4111.54(9)
C8O3Li2128.77(8) O3Li1O1111.85(9)
C8O3Li3121.82(8) O3Li1N187.83(7)
Li2O3Li176.01(8) O3Li1C21107.58(9)
Li3O3Li1133.14(8) O3Li1Li251.27(6)
Li3O3Li279.62(8) O3Li1Li323.04(5)
C12O4Li4110.15(8) O1Li1N186.74(7)
C13O4C12112.30(9) O1Li1C21114.14(9)
C13O4Li4122.53(9) O1Li1Li2125.75(10)
C2O1Li1104.23(8) O1Li1Li398.70(7)
C3O1C2112.75(8) N1Li1C21145.27(9)
C3O1Li1113.13(8) N1Li1Li2133.22(10)
C15O5C16112.85(9) N1Li1Li3106.32(7)
C5O2C6111.59(10) C21Li1Li256.70(6)
C7N1Li199.46(7) C21Li1Li397.90(7)
C1N1C7110.82(8) Li2Li1Li343.56(6)
C1N1C4109.88(8) O6Li2O399.41(8)
C1N1Li199.90(8) O6Li2C21142.69(10)
C4N1C7110.15(8) O6Li2Li1141.29(10)
C4N1Li1125.69(8) O6Li2Li350.59(6)
C17N2Li496.74(7) O6Li2Li423.14(5)
C11N2C17111.06(8) O3Li2C21110.67(9)
C11N2Li4101.70(7) O3Li2Li152.72(6)
C14N2C17109.63(8) O3Li2Li349.78(6)
C14N2C11108.67(8) O3Li2Li492.03(7)
C14N2Li4128.10(8) C21Li2Li158.36(7)
O6C18C17108.61(8) C21Li2Li3145.78(10)
O6C18C19109.70(8) C21Li2Li4130.87(8)
O6C18C20110.96(8) Li1Li2Li394.12(9)
C19C18C17111.61(8) Li1Li2Li4120.84(8)
C19C18C20108.73(9) Li3Li2Li443.53(6)
C20C18C17107.21(9) O6Li3C25109.47(9)
C28C25C27105.88(10) O6Li3Li190.40(7)
C28C25C26106.15(11) O6Li3Li249.44(6)
C28C25Li3148.16(9) O6Li3Li451.04(6)
C28C25Li483.18(8) O3Li3O699.09(8)
C27C25C26106.81(13) O3Li3C25143.65(10)
C27C25Li396.99(9) O3Li3Li123.83(5)
C27C25Li4130.56(9) O3Li3Li250.60(6)
C26C25Li387.55(9) O3Li3Li4139.90(10)
C26C25Li4117.20(11) C25Li3Li1131.53(8)
Li3C25Li465.06(7) C25Li3Li2144.57(10)
N1C7C8112.53(8) C25Li3Li458.81(7)
C24C21C22105.53(9) Li2Li3Li142.32(6)
C24C21Li1132.96(9) Li4Li3Li1118.75(8)
C24C21Li289.37(8) Li4Li3Li292.32(8)
C23C21C24106.82(9) O6Li4O4115.47(9)
C23C21C22106.66(9) O6Li4N287.24(7)
C23C21Li1113.60(9) O6Li4C25106.69(9)
C23C21Li294.63(8) O6Li4Li222.70(5)
C22C21Li185.29(8) O6Li4Li350.91(6)
C22C21Li2148.68(9) O4Li4N282.85(7)
Li2C21Li164.94(7) O4Li4C25117.07(9)
O1C2C1107.65(8) O4Li4Li2103.55(7)
O3C8C7108.60(8) O4Li4Li3132.48(10)
O3C8C9111.11(8) N2Li4C25144.95(9)
O3C8C10110.11(8) N2Li4Li2105.26(7)
C9C8C7107.45(8) N2Li4Li3131.81(9)
C10C8C7111.18(8) C25Li4Li297.89(7)
C10C8C9108.37(9) C25Li4Li356.13(6)
O4C12C11107.92(8) Li3Li4Li244.14(6)

 

Table 6 Torsion Angles for mo_B0378_0m.
ABCDAngle/˚ ABCDAngle/˚
O6C18C17N2-59.48(10) Li1O3Li3O669.84(13)
O4C12C11N2-54.11(11) Li1O3Li3C25-72.1(2)
O1C2C1N1-59.89(11) Li1O3Li3Li259.45(12)
N1C7C8O3-57.30(10) Li1O3Li3Li432.8(2)
N1C7C8C9-177.58(8) Li1O1C2C152.52(10)
N1C7C8C1064.00(11) Li1N1C7C828.76(10)
N1C4C5O268.85(13) Li1N1C1C231.60(10)
N2C14C15O5177.60(9) Li1N1C4C533.22(14)
C18O6Li2O3-120.24(9) Li2O6C18C17-120.16(9)
C18O6Li2C2195.87(17) Li2O6C18C19117.60(10)
C18O6Li2Li1-159.45(14) Li2O6C18C20-2.56(12)
C18O6Li2Li3-130.69(9) Li2O3C8C7135.15(10)
C18O6Li2Li4167.02(15) Li2O3C8C9-106.87(11)
C7N1C1C2-72.58(11) Li2O3C8C1013.19(13)
C7N1C4C5151.85(9) Li2O3Li3O610.39(8)
C8O3Li3O6-119.07(9) Li2O3Li3C25-131.51(17)
C8O3Li3C2599.02(17) Li2O3Li3Li1-59.45(12)
C8O3Li3Li1171.09(16) Li2O3Li3Li4-26.62(15)
C8O3Li3Li2-129.46(10) Li3O6C18C17138.91(10)
C8O3Li3Li4-156.08(13) Li3O6C18C1916.67(13)
C17N2C11C12-72.68(11) Li3O6C18C20-103.49(11)
C17N2C14C15157.32(9) Li3O6Li2O310.45(8)
C11N2C17C18138.13(9) Li3O6Li2C21-133.43(17)
C11N2C14C15-81.13(11) Li3O6Li2Li1-28.76(16)
C1N1C7C8133.23(9) Li3O6Li2Li4-62.29(12)
C1N1C4C5-85.79(11) Li3O3C8C7-121.76(9)
C4N1C7C8-104.97(10) Li3O3C8C9-3.78(13)
C4N1C1C2165.46(9) Li3O3C8C10116.28(10)
C14N2C17C18-101.77(9) Li4O6C18C1750.13(10)
C14N2C11C12166.65(9) Li4O6C18C19-72.10(10)
C13O4C12C11-169.63(9) Li4O6C18C20167.73(9)
C19C18C17N261.59(11) Li4O6Li2O372.74(13)
C20C18C17N2-179.44(8) Li4O6Li2C21-71.1(2)
C3O1C2C1175.60(8) Li4O6Li2Li133.5(2)
C16O5C15C14179.92(11) Li4O6Li2Li362.29(12)
C6O2C5C4172.58(10) Li4O4C12C1150.04(11)
Li1O3C8C751.53(10) Li4N2C17C1832.80(9)
Li1O3C8C9169.51(9) Li4N2C11C1229.34(10)
Li1O3C8C10-70.42(10) Li4N2C14C1541.34(14)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0378_0m.
AtomxyzU(eq)
H7A93607775784724
H7B91488868827224
H17A13018183695222
H17B6759156611422
H11A15496392547127
H11B4507103616527
H1A100076323997926
H1B107986679908726
H4A85139145963828
H4B99808170999628
H14A12829025467026
H14B2818306476026
H13A46165063785248
H13B57594653706148
H13C44734195724048
H19A38849838579738
H19B227210166539638
H19C35069051519638
H15A30787688394133
H15B21216927406233
H20A19169389781241
H20B132910375698041
H20C293610031739541
H9A79908799644939
H9B78029912683539
H9C64119711649439
H10A528110090800137
H10B667310275835937
H10C60939410895137
H3A74545432800440
H3B68395003894740
H3C84634364865740
H16A13198275180558
H16B18877081239458
H16C28887802230058
H6A744571521220862
H6B863275711256762
H6C901562961254862
H27A79935245636962
H27B84366282642162
H27C88065671552362
H5A7231(17)8310(12)10744(10)30(4)
H12A2058(16)5417(12)6943(10)29(4)
H2A9397(15)6091(11)8137(10)23(3)
H24A2807(18)6981(13)9852(12)40(4)
H22A6161(19)6998(14)10719(12)44(4)
H23A3030(19)8558(14)10348(12)43(4)
H22B4701(18)6747(13)10981(12)38(4)
H24B2830(20)7429(15)8756(13)51(5)
H23B4430(17)8920(13)10077(11)37(4)
H23C3175(18)9124(14)9302(12)39(4)
H28A6990(20)5746(14)4443(13)48(5)
H26A7770(20)7257(17)4518(15)64(6)
H26B5870(30)8020(20)4458(17)85(7)
H2B10325(16)5117(12)8892(10)28(3)
H22C5934(18)5975(14)10349(12)40(4)
H28B5330(20)6465(15)4557(13)48(5)
H24C3964(17)6195(13)9187(11)37(4)
H12B2231(16)6378(12)7408(10)29(4)
H5B8333(17)8766(13)11173(11)37(4)
H26C7240(20)8016(18)5274(15)69(6)
H28C6070(20)5294(17)5291(14)61(6)

Experimental

Single crystals of C14H31Li2NO3 [mo_B0378_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 XT [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. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [mo_B0378_0m]

Crystal Data for C14H31Li2NO3 (=275.28 g/mol): triclinic, space group P-1 (no. 2), a = 9.9122(8) Å, b = 13.2804(10) Å, c = 14.5570(12) Å, α = 81.866(3)°, β = 88.357(3)°, γ = 68.748(3)°, = 1767.4(2) Å3, Z = 4, T = 99.99 K, μ(MoKα) = 0.068 mm-1, Dcalc = 1.035 g/cm3, 86037 reflections measured (4.41° ≤ 2Θ ≤ 58°), 9360 unique (Rint = 0.0680, Rsigma = 0.0339) which were used in all calculations. The final R1 was 0.0461 (I > 2σ(I)) and wR2 was 0.1291 (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), C17(H17A,H17B), C11(H11A,H11B), C1(H1A,H1B), C4(H4A,H4B),
C14(H14A,H14B), C15(H15A,H15B)
2.b Idealised Me refined as rotating group:
C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C9(H9A,H9B,
H9C), C10(H10A,H10B,H10C), C3(H3A,H3B,H3C), C16(H16A,H16B,H16C), C6(H6A,H6B,
H6C), C27(H27A,H27B,H27C)

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