mo_B0517_0m

Table 1 Crystal data and structure refinement for mo_B0517_0m.
Identification code mo_B0517_0m
Empirical formula C22H50Li4N2O6
Formula weight 466.40
Temperature/K 100.01
Crystal system monoclinic
Space group P21/c
a/Å 15.696(3)
b/Å 9.3886(17)
c/Å 19.721(4)
α/° 90
β/° 92.353(7)
γ/° 90
Volume/Å3 2903.8(10)
Z 4
ρcalcg/cm3 1.067
μ/mm‑1 0.073
F(000) 1024.0
Crystal size/mm3 0.35 × 0.23 × 0.14
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.056 to 52
Index ranges -19 ≤ h ≤ 19, -11 ≤ k ≤ 11, -24 ≤ l ≤ 24
Reflections collected 76371
Independent reflections 5705 [Rint = 0.0453, Rsigma = 0.0203]
Data/restraints/parameters 5705/0/340
Goodness-of-fit on F2 1.058
Final R indexes [I>=2σ (I)] R1 = 0.0358, wR2 = 0.0855
Final R indexes [all data] R1 = 0.0457, wR2 = 0.0915
Largest diff. peak/hole / e Å-3 0.28/-0.19

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0517_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C12563.8(8)352.0(14)4781.9(7)26.2(3)
C23253.2(8)1131.3(15)5188.7(6)28.9(3)
C33975.1(9)3335.5(19)5262.0(8)40.8(4)
C41195.1(8)807.5(13)4202.6(6)19.5(3)
C51426.8(8)1749.6(13)3614.5(6)20.7(3)
C61436.2(9)4179.0(14)3315.4(6)27.2(3)
C71324.8(8)912.6(12)5449.2(6)19.2(3)
C81019.8(7)2330.5(12)5752.2(5)16.8(2)
C9774.1(8)2015.0(14)6483.6(6)24.6(3)
C10238.8(8)2925.6(14)5357.4(6)22.9(3)
C113798.9(7)8432.0(13)6864.1(6)18.7(2)
C123958.9(8)7511.4(13)6250.1(6)19.8(3)
C135027.9(8)5866.4(15)6634.8(7)30.0(3)
C143159.1(8)8243.3(13)7964.1(6)19.3(3)
C153820.2(8)7350.9(13)8345.5(6)21.0(3)
C164247.0(8)5006.0(15)8556.2(7)28.3(3)
C172258.8(7)8182.1(12)6917.5(6)17.1(2)
C181670.4(7)6872.4(12)6862.4(6)16.1(2)
C191353.6(8)6430.0(14)7557.9(6)22.8(3)
C20900.9(8)7285.6(14)6400.6(7)24.7(3)
C212414.6(11)5816.6(16)4724.3(6)31.1(3)
C223297.1(9)3031.2(14)7183.1(6)22.3(3)
Li12113.8(13)3415(2)4819.4(10)21.9(4)
Li21863.8(14)5276(2)5657.6(10)23.7(4)
Li32200.3(13)3759(2)6604.2(10)21.7(4)
Li43200.7(13)5482(2)7107.4(10)20.6(4)
N11748.8(6)1111.6(11)4802.8(5)17.9(2)
N23095.0(6)7845(1)7242.9(5)15.8(2)
O13348.9(6)2503.1(11)4893.9(4)28.3(2)
O21414.1(6)3179.4(9)3856.3(4)21.6(2)
O31690.1(5)3305.8(8)5748.3(4)17.42(18)
O44153.6(5)6083.7(9)6453.4(4)20.46(19)
O53638.4(5)5891.2(9)8211.5(4)21.8(2)
O62121.2(5)5752.6(8)6578.6(4)16.50(18)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0517_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
C128.9(7)24.4(7)25.3(6)-3.9(5)0.9(5)7.5(5)
C225.2(7)37.9(8)23.6(6)-3.1(6)-1.0(5)9.1(6)
C326.7(7)60.9(11)34.7(8)-10.3(7)-1.8(6)-13.9(7)
C424.1(6)18.1(6)16.3(5)-3.4(5)0.9(5)-5.1(5)
C525.3(6)21.6(6)15.2(5)-4.2(5)0.8(5)-4.7(5)
C637.3(7)26.8(7)17.3(6)6.4(5)-0.9(5)-7.5(6)
C725.4(6)15.7(6)16.3(5)2.8(4)1.0(5)-3.6(5)
C819.7(6)17.4(6)13.4(5)0.6(4)1.4(4)-4.4(5)
C929.6(7)27.3(7)17.1(6)1.3(5)5.0(5)-6.5(5)
C1021.3(6)25.5(6)21.7(6)-0.8(5)0.1(5)-0.6(5)
C1118.2(6)16.8(6)21.0(6)-0.6(5)0.0(5)-2.3(5)
C1219.7(6)20.9(6)18.9(6)1.2(5)1.4(4)-1.2(5)
C1319.3(6)31.6(7)39.1(7)0.0(6)0.4(5)3.6(6)
C1420.6(6)19.3(6)17.9(6)-5.5(5)-0.9(4)2.0(5)
C1520.4(6)24.3(6)17.8(6)-4.8(5)-2.2(5)0.8(5)
C1626.8(7)31.5(7)26.2(6)5.3(6)-2.4(5)10.2(6)
C1718.5(6)14.7(6)17.8(5)0.2(4)-0.8(4)3.3(5)
C1815.6(5)15.7(6)16.8(5)0.2(4)-0.3(4)2.3(4)
C1922.2(6)24.8(6)21.9(6)1.1(5)6.1(5)-1.2(5)
C2019.6(6)23.5(6)30.3(7)1.5(5)-6.5(5)1.4(5)
C2151.7(9)26.2(7)15.4(6)-0.3(5)2.0(6)-15.8(7)
C2226.6(7)19.6(6)20.4(6)0.3(5)-3.8(5)3.0(5)
Li127.1(11)22.7(10)16.1(9)0.0(8)3.1(8)-6.4(9)
Li234.1(12)19.4(10)17.3(9)0.3(8)-0.7(8)-3.8(9)
Li328.1(11)19(1)17.8(9)-0.2(8)-2.5(8)-1.4(8)
Li419.4(10)20(1)22.1(10)-1.1(8)-1.6(8)0.3(8)
N121.0(5)18.1(5)14.5(5)-1.7(4)1.3(4)-0.4(4)
N215.4(5)17.2(5)14.9(5)-1.7(4)-0.3(4)0.2(4)
O122.1(5)39.5(6)23.2(4)-5.4(4)-0.3(4)-5.6(4)
O232.8(5)18.7(4)13.3(4)1.3(3)0.2(3)-6.6(4)
O321.6(4)16.8(4)13.9(4)-0.6(3)0.3(3)-5.9(3)
O417.8(4)19.7(4)23.9(4)-2.8(3)1.0(3)1.5(3)
O523.2(4)20.7(4)21.2(4)0.5(3)-3.6(3)4.7(4)
O618.6(4)15.1(4)15.7(4)-2.8(3)-1.2(3)1.4(3)

 

Table 4 Bond Lengths for mo_B0517_0m.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.5095(18) C18C191.5354(16)
C1N11.4667(16) C18C201.5324(16)
C2O11.4235(17) C18Li42.759(2)
C3O11.4302(16) C18O61.3970(14)
C4C51.5146(16) C21Li12.313(3)
C4N11.4675(14) C21Li22.127(2)
C5O21.4250(15) C22Li32.139(2)
C6O21.4223(14) C22Li42.311(2)
C7C81.5433(16) Li1Li22.448(3)
C7N11.4740(14) Li1Li33.532(3)
C8C91.5371(16) Li1N12.237(2)
C8C101.5306(16) Li1O12.119(2)
C8Li12.762(2) Li1O22.166(2)
C8O31.3951(14) Li1O31.977(2)
C9Li32.776(2) Li2Li32.390(3)
C11C121.5169(16) Li2Li43.482(3)
C11N21.4664(15) Li2O31.879(2)
C12O41.4286(15) Li2O61.898(2)
C13O41.4186(15) Li3Li42.437(3)
C14C151.5101(16) Li3O31.887(2)
C14N21.4701(14) Li3O61.876(2)
C15O51.4224(15) Li4N22.241(2)
C16O51.4185(14) Li4O42.092(2)
C17C181.5390(16) Li4O52.289(2)
C17N21.4715(15) Li4O61.969(2)

 

Table 5 Bond Angles for mo_B0517_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
N1C1C2110.89(10) Li2Li3C997.64(9)
O1C2C1107.87(10) Li2Li3Li143.76(7)
N1C4C5110.55(9) Li2Li3Li492.33(10)
O2C5C4106.67(9) Li4Li3C9158.48(10)
N1C7C8112.57(9) Li4Li3Li1117.67(9)
C7C8Li181.31(8) O3Li3C958.61(6)
C9C8C7106.91(9) O3Li3C22135.09(12)
C9C8Li1151.98(9) O3Li3Li124.54(5)
C10C8C7111.88(9) O3Li3Li250.48(7)
C10C8C9108.73(10) O3Li3Li4139.18(12)
C10C8Li191.92(8) O6Li3C9122.27(10)
O3C8C7108.54(9) O6Li3C22112.59(11)
O3C8C9110.48(9) O6Li3Li193.71(8)
O3C8C10110.25(9) O6Li3Li251.12(7)
O3C8Li142.67(6) O6Li3Li452.38(7)
C8C9Li374.59(8) O6Li3O3100.13(10)
N2C11C12110.21(9) C18Li4Li252.52(5)
O4C12C11110.55(9) C22Li4C18122.46(9)
N2C14C15111.05(9) C22Li4Li291.91(8)
O5C15C14108.27(9) C22Li4Li353.46(7)
N2C17C18112.39(9) Li3Li4C1872.60(8)
C17C18Li481.36(8) Li3Li4Li243.29(7)
C19C18C17111.62(9) N2Li4C1858.97(6)
C19C18Li491.56(8) N2Li4C22169.41(11)
C20C18C17107.21(9) N2Li4Li296.20(8)
C20C18C19108.85(10) N2Li4Li3130.99(10)
C20C18Li4152.02(9) N2Li4O575.01(7)
O6C18C17108.49(9) O4Li4C18113.81(9)
O6C18C19110.01(9) O4Li4C22105.19(9)
O6C18C20110.62(9) O4Li4Li286.04(8)
O6C18Li442.48(6) O4Li4Li3113.14(10)
Li2C21Li166.77(8) O4Li4N282.23(8)
Li3C22Li466.29(8) O4Li4O5110.30(9)
C8Li1Li350.91(5) O5Li4C18108.21(8)
C21Li1C8123.23(9) O5Li4C2295.12(8)
C21Li1Li252.98(7) O5Li4Li2159.69(9)
C21Li1Li389.54(7) O5Li4Li3131.45(10)
Li2Li1C872.07(7) O6Li4C1828.63(4)
Li2Li1Li342.47(7) O6Li4C22102.42(9)
N1Li1C859.17(6) O6Li4Li225.29(5)
N1Li1C21173.84(11) O6Li4Li348.99(7)
N1Li1Li2130.68(10) O6Li4N282.49(8)
N1Li1Li395.88(7) O6Li4O4105.08(10)
O1Li1C8113.39(9) O6Li4O5134.46(10)
O1Li1C21102.14(10) C1N1C4111.78(9)
O1Li1Li2114.41(10) C1N1C7112.82(9)
O1Li1Li388.30(7) C1N1Li1104.32(9)
O1Li1N180.99(8) C4N1C7113.55(9)
O1Li1O2116.68(10) C4N1Li1110.05(9)
O2Li1C8103.86(8) C7N1Li1103.55(8)
O2Li1C2197.25(9) C11N2C14111.97(9)
O2Li1Li2125.13(11) C11N2C17111.98(9)
O2Li1Li3151.72(9) C11N2Li4104.49(8)
O2Li1N176.59(7) C14N2C17113.05(9)
O3Li1C828.57(4) C14N2Li4111.39(9)
O3Li1C21101.73(9) C17N2Li4103.30(8)
O3Li1Li248.85(7) C2O1C3111.64(11)
O3Li1Li323.35(5) C2O1Li1106.40(9)
O3Li1N182.40(8) C3O1Li1114.97(11)
O3Li1O1104.86(10) C5O2Li1112.09(9)
O3Li1O2129.01(11) C6O2C5111.69(9)
C21Li2Li160.25(8) C6O2Li1124.27(9)
C21Li2Li3137.18(13) C8O3Li1108.76(9)
C21Li2Li4116.40(10) C8O3Li2139.37(10)
Li1Li2Li4119.10(10) C8O3Li3115.83(9)
Li3Li2Li193.77(10) Li2O3Li178.76(9)
Li3Li2Li444.38(7) Li2O3Li378.76(9)
O3Li2C21112.52(11) Li3O3Li1132.11(10)
O3Li2Li152.39(7) C12O4Li4106.03(9)
O3Li2Li350.76(7) C13O4C12113.53(9)
O3Li2Li493.53(8) C13O4Li4120.96(9)
O3Li2O699.62(10) C15O5Li4112.86(8)
O6Li2C21133.93(12) C16O5C15110.45(9)
O6Li2Li1141.33(12) C16O5Li4121.85(9)
O6Li2Li350.31(7) C18O6Li2117.99(9)
O6Li2Li426.31(6) C18O6Li3140.71(10)
C9Li3Li182.11(6) C18O6Li4108.89(9)
C22Li3C9119.07(10) Li2O6Li4128.40(10)
C22Li3Li1120.00(9) Li3O6Li278.56(9)
C22Li3Li2139.01(12) Li3O6Li478.62(9)
C22Li3Li460.25(8)     

 

Table 6 Torsion Angles for mo_B0517_0m.
ABCDAngle/˚ ABCDAngle/˚
C1C2O1C3178.22(11) C22Li3O6C18-103.78(15)
C1C2O1Li152.05(12) C22Li3O6Li2135.62(12)
C2C1N1C4153.82(10) C22Li3O6Li42.22(11)
C2C1N1C7-76.76(13) Li1C8C9Li39.2(2)
C2C1N1Li134.94(12) Li1C8O3Li294.58(15)
C4C5O2C6-167.07(10) Li1C8O3Li3-162.03(13)
C4C5O2Li148.29(12) Li1Li2O3C8-105.78(14)
C5C4N1C1-83.07(12) Li1Li2O3Li3137.43(10)
C5C4N1C7147.89(10) Li1Li2O6C18-167.70(16)
C5C4N1Li132.36(12) Li1Li2O6Li3-25.81(19)
C7C8C9Li3112.80(9) Li1Li2O6Li439.5(2)
C7C8O3Li153.20(11) Li1Li3O3C8156.81(17)
C7C8O3Li2147.78(13) Li1Li3O3Li2-63.42(13)
C7C8O3Li3-108.83(11) Li1Li3O6C18131.49(13)
C8C7N1C1131.70(10) Li1Li3O6Li210.89(8)
C8C7N1C4-99.79(11) Li1Li3O6Li4-122.51(8)
C8C7N1Li119.53(12) Li2Li3O3C8-139.77(11)
C9C8O3Li1170.12(10) Li2Li3O3Li163.42(13)
C9C8O3Li2-95.30(15) Li2Li3O6C18120.60(15)
C9C8O3Li38.09(14) Li2Li3O6Li4-133.40(10)
C9Li3O3C8-4.91(8) Li3Li2O3C8116.79(14)
C9Li3O3Li1-161.72(12) Li3Li2O3Li1-137.43(10)
C9Li3O3Li2134.86(9) Li3Li2O6C18-141.89(11)
C9Li3O6C1848.48(19) Li3Li2O6Li465.34(12)
C9Li3O6Li2-72.12(11) Li4C18O6Li2-157.73(13)
C9Li3O6Li4154.48(12) Li4C18O6Li395.10(16)
C10C8C9Li3-126.25(10) Li4Li2O3C8129.64(12)
C10C8O3Li1-69.66(12) Li4Li2O3Li1-124.58(9)
C10C8O3Li224.91(17) Li4Li2O3Li312.85(8)
C10C8O3Li3128.31(11) Li4Li2O6C18152.77(15)
C11C12O4C13-85.37(12) Li4Li2O6Li3-65.34(12)
C11C12O4Li449.77(11) Li4Li3O3C8-168.79(15)
C12C11N2C14153.81(9) Li4Li3O3Li134.4(2)
C12C11N2C17-78.01(12) Li4Li3O3Li2-29.03(18)
C12C11N2Li433.12(11) Li4Li3O6C18-105.99(15)
C14C15O5C16179.63(9) Li4Li3O6Li2133.40(10)
C14C15O5Li439.42(12) N1C1C2O1-61.00(13)
C15C14N2C11-77.40(12) N1C4C5O2-53.15(12)
C15C14N2C17154.99(10) N1C7C8C9-167.93(9)
C15C14N2Li439.20(12) N1C7C8C1073.13(12)
C17C18O6Li2-104.57(11) N1C7C8Li1-15.44(9)
C17C18O6Li3148.26(13) N1C7C8O3-48.74(12)
C17C18O6Li453.15(11) N2C11C12O4-58.44(12)
C18C17N2C11132.96(10) N2C14C15O5-52.24(13)
C18C17N2C14-99.44(11) N2C17C18C1971.53(12)
C18C17N2Li421.08(11) N2C17C18C20-169.35(9)
C19C18O6Li2133.06(11) N2C17C18Li4-16.72(9)
C19C18O6Li325.89(18) N2C17C18O6-49.85(12)
C19C18O6Li4-69.21(11) O3C8C9Li3-5.13(9)
C20C18O6Li212.76(14) O3Li2O6C18-128.87(10)
C20C18O6Li3-94.41(16) O3Li2O6Li313.01(10)
C20C18O6Li4170.49(10) O3Li2O6Li478.36(14)
C21Li2O3C8-109.85(15) O3Li3O6C18107.62(14)
C21Li2O3Li1-4.07(11) O3Li3O6Li2-12.98(10)
C21Li2O3Li3133.37(13) O3Li3O6Li4-146.39(11)
C21Li2O6C1896.50(18) O6Li2O3C8103.86(14)
C21Li2O6Li3-121.61(18) O6Li2O3Li1-150.36(11)
C21Li2O6Li4-56.3(2) O6Li2O3Li3-12.93(10)
C22Li3O3C896.28(17) O6Li3O3C8-126.66(10)
C22Li3O3Li1-60.5(2) O6Li3O3Li176.53(15)
C22Li3O3Li2-123.96(17) O6Li3O3Li213.10(10)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0517_0m.
AtomxyzU(eq)
H1A2731263430531
H1B2498-619496831
H2A30931225566735
H2B3797598517935
H3A38233406573861
H3B39974291506461
H3C45342879523761
H4A593974431123
H4B1256-205407323
H5A20011503346125
H5B10091627322925
H6A19494019305841
H6B14475148350141
H6C9294059301541
H7A1727445577923
H7B829273537423
H9A12731653674437
H9B3201299647937
H9C5732892669437
H10A393785558434
H10B-2162209534134
H10C3933164489434
H11A43228473716222
H11B36579413671522
H12A34467514594024
H12B44407910600224
H13A53736075624445
H13B51174874677445
H13C51976500701145
H14A25988110816723
H14B33159262800623
H15A43977591819525
H15B38037541883925
H16A48175219839842
H16B41094005846342
H16C42355182904642
H17A23438565645720
H17B19808931718420
H19A9485642750034
H19B10727241776734
H19C18396124785134
H20A10957547595137
H20B6078098659837
H20C5086476635737
H21A2880(12)6400(20)4949(9)58(5)
H21B2710(11)5319(19)4350(9)48(5)
H21C2016(13)6480(20)4492(10)66(6)
H22A3228(11)2750(19)7662(10)51(5)
H22B3217(13)2140(20)6928(10)65(6)
H22C3922(11)3225(18)7153(8)45(5)

Experimental

Single crystals of C22H50Li4N2O6 [mo_B0517_0m] 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 ShelXT [2] structure solution program using Intrinsic Phasing 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_B0517_0m]

Crystal Data for C22H50Li4N2O6 (=466.40 g/mol): monoclinic, space group P21/c (no. 14), a = 15.696(3) Å, b = 9.3886(17) Å, c = 19.721(4) Å, β = 92.353(7)°, = 2903.8(10) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 0.073 mm-1, Dcalc = 1.067 g/cm3, 76371 reflections measured (5.056° ≤ 2Θ ≤ 52°), 5705 unique (Rint = 0.0453, Rsigma = 0.0203) which were used in all calculations. The final R1 was 0.0358 (I > 2σ(I)) and wR2 was 0.0915 (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:
C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C11(H11A,
H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B)
2.b Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C20(H20A,H20B,
H20C)

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