cu_B0490_0m

Table 1 Crystal data and structure refinement for cu_B0490_0m.
Identification code cu_B0490_0m
Empirical formula C28H64Li5N3O8
Formula weight 605.52
Temperature/K 99.99
Crystal system monoclinic
Space group P21/c
a/Å 18.2841(8)
b/Å 9.1092(4)
c/Å 24.3776(10)
α/° 90
β/° 111.387(2)
γ/° 90
Volume/Å3 3780.6(3)
Z 4
ρcalcg/cm3 1.064
μ/mm‑1 0.586
F(000) 1328.0
Crystal size/mm3 0.35 × 0.2 × 0.19
Radiation CuKα (λ = 1.54178)
2Θ range for data collection/° 5.19 to 135.984
Index ranges -21 ≤ h ≤ 21, -10 ≤ k ≤ 10, -29 ≤ l ≤ 29
Reflections collected 63345
Independent reflections 6869 [Rint = 0.1315, Rsigma = 0.0627]
Data/restraints/parameters 6869/6/431
Goodness-of-fit on F2 1.032
Final R indexes [I>=2σ (I)] R1 = 0.0792, wR2 = 0.2108
Final R indexes [all data] R1 = 0.1013, wR2 = 0.2261
Largest diff. peak/hole / e Å-3 0.74/-0.36

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for cu_B0490_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C1708.4(19)7087(4)2546.3(13)57.9(8)
C2544(2)5842(4)2110.8(14)61.1(8)
C31036(3)4514(5)1489(2)92.2(14)
C42117.4(19)7526(4)2966.7(14)57.0(8)
C52878.0(19)6883(4)3370.2(15)62.3(9)
C63096(3)4759(5)2883(2)89.2(14)
C71366.1(18)7473(3)3615.4(13)47.7(7)
C81164.9(16)6290(3)3989.3(12)44.0(6)
C91199.8(19)7017(3)4561.9(13)53.6(7)
C10340.5(17)5667(4)3669.3(14)54.7(8)
C111548(2)2418(4)3142.7(14)56.0(8)
C122334.7(18)1038(3)4838.0(13)47.5(7)
C131622.2(19)1299(3)4989.8(13)52.3(8)
C14327(2)2255(5)4600(2)79.4(11)
C153236.3(18)2144(3)4459.2(12)46.2(7)
C163972.1(18)1358(3)4851.2(13)49.6(7)
C174927.6(18)1432(3)5822.6(13)52.3(7)
C192917(2)7466(3)6676.0(14)58.4(8)
C202141(2)6922(4)6257.0(15)64.0(9)
C211865(3)4774(5)6720(2)91.0(14)
C224308.4(19)6840(3)7099.5(13)53.6(8)
C234414.8(19)5540(3)7503.6(13)50.0(7)
C243810(2)4219(4)8045.6(15)65.8(9)
C253687(2)7393(3)6039.2(12)48.3(7)
C263857.3(17)6217(3)5650.0(12)41.4(6)
C274669.7(17)5528(3)5955.4(13)49.0(7)
C283837(2)6968(3)5081.6(13)53.2(8)
Li11855(3)4702(6)3377(2)52.4(12)
Li21585(3)3027(5)4029(2)47.5(11)
Li32519(3)4618(5)4792.7(19)41.7(10)
Li43419(3)3039(5)5571.2(19)40.6(10)
Li53093(3)4640(5)6221(2)46.3(11)
N11436.1(14)6881(3)3071.8(10)48.2(6)
N22648.2(14)2417(2)4719.2(9)39.6(5)
N33585.4(14)6768(2)6569.2(10)45.4(6)
O11116.3(15)5797(3)1842.3(10)68.3(7)
O22889.6(14)5326(3)3343.0(11)66.7(6)
O31720.2(11)5156(2)4107.0(8)41.6(4)
O41014.8(13)1921(2)4487.6(9)57.5(6)
O54284.0(11)2143(2)5393.6(8)45.8(5)
O62091.1(14)5355(3)6269.4(11)66.2(6)
O73838.3(13)5565(2)7767.1(9)56.9(6)
O83271.3(10)5139.8(18)5516.0(7)36.8(4)
C183352(2)2335(3)6413.4(14)51.6(7)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for cu_B0490_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
C153.3(19)64(2)52.0(17)11.2(15)14.2(15)0.3(15)
C256(2)69(2)53.7(17)3.5(15)14.1(15)-13.7(16)
C3123(4)81(3)84(3)-23(2)52(3)-35(3)
C462(2)61(2)50.8(16)8.2(14)24.2(15)-14.5(15)
C546.5(18)87(3)56.0(18)13.9(17)21.4(15)-10.8(17)
C696(3)81(3)122(4)34(2)76(3)27(2)
C746.7(17)41.6(15)53.6(16)6.6(12)16.7(14)3.3(12)
C844.3(16)41.8(15)47.7(15)2.5(12)18.7(13)4.9(12)
C960.1(19)50.5(17)56.4(17)3.3(14)28.6(15)7.3(14)
C1040.6(17)61.0(19)63.5(18)9.3(15)20.3(14)1.5(14)
C1154(2)66(2)47.4(16)0.1(15)18.4(15)-5.2(16)
C1263.2(19)31.2(14)50.3(15)-5.8(11)23.4(14)-6.2(13)
C1367(2)43.9(16)51.1(16)0.9(13)27.1(15)-13.3(14)
C1466(2)88(3)100(3)17(2)49(2)-6(2)
C1557.4(18)47.1(16)39.1(13)-4.5(12)23.6(13)1.9(13)
C1662.0(19)40.4(15)53.7(16)-8.7(12)29.9(15)5.1(13)
C1750.2(18)50.9(17)57.1(17)8.4(14)20.9(14)10.6(14)
C1980(2)47.5(18)51.9(17)-11.1(13)29.5(17)12.9(16)
C2064(2)74(2)57.9(18)-8.3(16)27.0(17)22.0(18)
C2176(3)102(3)117(3)-34(3)62(3)-22(2)
C2263(2)48.1(17)50.6(16)-12.3(13)21.4(15)-11.0(14)
C2355.3(18)47.3(17)49.4(16)-5.1(12)21.4(14)-0.9(13)
C2468(2)67(2)65(2)4.8(17)27.4(18)-6.7(18)
C2568(2)29.8(14)50.4(15)-4.0(11)25.3(15)-6.3(13)
C2655.1(17)28.5(13)45.5(14)-2.6(11)24.2(13)-7.5(11)
C2749.7(17)46.3(16)53.7(16)-3.0(13)22.3(14)-8.5(13)
C2876(2)38.8(15)53.2(16)1.9(13)33.9(16)-7.4(14)
Li153(3)58(3)52(3)2(2)26(2)-3(2)
Li249(3)51(3)44(2)-3(2)19(2)-8(2)
Li345(3)35(2)46(2)0.6(18)18(2)3.0(18)
Li449(3)35(2)43(2)-2.5(18)23(2)2.8(19)
Li557(3)40(2)53(3)-5(2)33(2)-1(2)
N145.2(14)54.2(15)44.0(12)5.9(10)14.6(11)-4.4(11)
N250.6(14)30.6(11)42.6(11)-3.5(9)23.1(10)-1.2(9)
N357.0(15)37.1(12)44.8(12)-9(1)21.8(11)-1.4(10)
O182.2(17)69.4(15)59.7(13)-9.4(11)33.5(12)-26.8(13)
O260.1(14)77.6(17)73.2(15)14.7(12)37.4(12)1.3(12)
O342.2(11)40.2(10)44.1(10)3.8(8)17.8(8)2.7(8)
O455.1(13)64.7(14)60.3(12)4.7(10)30.0(11)-10.1(11)
O554.6(12)37.9(10)46.3(10)-0.6(8)20.1(9)10.4(9)
O663.5(15)74.7(16)73.5(15)-11.8(12)40.3(12)2.3(12)
O765.4(14)56.6(13)54.8(12)1.7(10)29.2(11)5.1(10)
O845.3(10)27.5(9)40.7(9)-3.2(7)19.4(8)-1.8(7)
C1862(2)48.2(17)50.5(16)-5.1(13)28.0(16)-4.2(15)

 

Table 4 Bond Lengths for cu_B0490_0m.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.507(5) C24O71.411(4)
C1N11.484(4) C25C261.536(4)
C2O11.422(4) C25N31.484(4)
C3O11.427(5) C26C271.532(4)
C4C51.499(5) C26C281.534(4)
C4N11.481(4) C26O81.401(3)
C5O21.420(4) Li1Li22.383(7)
C6O21.405(5) Li1Li33.215(7)
C7C81.540(4) Li1N12.160(6)
C7N11.479(4) Li1O22.005(6)
C8C91.525(4) Li1O31.929(5)
C8C101.531(4) Li2Li32.483(6)
C8O31.403(3) Li2N22.129(5)
C11Li12.176(6) Li2O31.955(5)
C11Li22.208(6) Li2O42.049(5)
C12C131.497(4) Li3Li42.471(6)
C12N21.453(3) Li3Li53.249(6)
C13O41.436(4) Li3N22.035(5)
C14O41.415(4) Li3O31.840(5)
C15C161.516(4) Li3O81.859(5)
C15N21.455(3) Li4Li52.383(6)
C16O51.426(3) Li4N22.118(5)
C17O51.414(3) Li4O51.963(5)
C19C201.498(5) Li4O81.931(5)
C19N31.483(4) Li4C182.197(5)
C20O61.431(4) Li5N32.176(5)
C21O61.411(5) Li5O61.988(5)
C22C231.507(4) Li5O73.610(5)
C22N31.475(4) Li5O81.916(5)
C23O71.421(4) Li5C182.166(6)

 

Table 5 Bond Angles for cu_B0490_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
N1C1C2113.5(3) O5Li4Li5144.9(3)
O1C2C1110.8(3) O5Li4N288.52(18)
N1C4C5111.7(2) O5Li4C18114.1(2)
O2C5C4112.7(3) O8Li4Li348.08(15)
N1C7C8113.1(2) O8Li4Li551.46(16)
C9C8C7107.4(2) O8Li4N299.8(2)
C9C8C10109.4(2) O8Li4O5120.1(2)
C10C8C7111.2(2) O8Li4C18107.5(2)
O3C8C7109.0(2) C18Li4Li3129.7(2)
O3C8C9110.3(2) C18Li4Li556.27(17)
O3C8C10109.6(2) Li3Li5O7166.36(18)
Li1C11Li265.8(2) Li4Li5Li349.14(16)
N2C12C13110.7(2) Li4Li5O7138.2(2)
O4C13C12108.9(2) N3Li5Li3110.5(2)
N2C15C16115.7(2) N3Li5Li4129.5(2)
O5C16C15108.1(2) N3Li5O755.89(12)
N3C19C20112.0(2) O6Li5Li397.0(2)
O6C20C19111.6(3) O6Li5Li4134.4(3)
N3C22C23113.5(2) O6Li5N386.78(19)
O7C23C22110.1(3) O6Li5O782.31(16)
N3C25C26112.8(2) O6Li5C18116.0(2)
C27C26C25111.4(2) O8Li5Li330.14(13)
C27C26C28108.7(2) O8Li5Li451.99(15)
C28C26C25107.7(2) O8Li5N387.5(2)
O8C26C25108.8(2) O8Li5O6116.0(3)
O8C26C27110.5(2) O8Li5O7139.3(2)
O8C26C28109.7(2) O8Li5C18109.2(2)
C11Li1Li257.74(19) C18Li5Li3100.74(19)
C11Li1Li3102.7(2) C18Li5Li457.52(17)
Li2Li1Li349.99(17) C18Li5N3138.8(3)
N1Li1C11139.7(3) C18Li5O791.72(18)
N1Li1Li2133.2(3) C1N1Li1120.5(2)
N1Li1Li3109.8(2) C4N1C1110.3(2)
O2Li1C11114.7(3) C4N1Li1102.0(2)
O2Li1Li2129.6(3) C7N1C1112.6(2)
O2Li1Li393.4(2) C7N1C4111.3(2)
O2Li1N187.0(2) C7N1Li199.3(2)
O3Li1C11109.8(2) C12N2C15110.3(2)
O3Li1Li252.67(17) C12N2Li294.0(2)
O3Li1Li330.64(13) C12N2Li3140.1(2)
O3Li1N188.4(2) C12N2Li4101.9(2)
O3Li1O2114.7(3) C15N2Li2107.9(2)
C11Li2Li156.44(19) C15N2Li3109.6(2)
C11Li2Li3130.3(3) C15N2Li498.0(2)
Li1Li2Li382.7(2) Li3N2Li273.16(19)
N2Li2C11113.6(2) Li3N2Li472.98(18)
N2Li2Li1110.0(2) Li4N2Li2142.6(2)
N2Li2Li351.67(15) C19N3C25111.2(2)
O3Li2C11107.5(2) C19N3Li5101.5(2)
O3Li2Li151.66(18) C22N3C19111.1(2)
O3Li2Li347.17(15) C22N3C25112.9(2)
O3Li2N297.8(2) C22N3Li5119.5(2)
O3Li2O4120.4(3) C25N3Li599.61(19)
O4Li2C11124.7(3) C2O1C3111.7(3)
O4Li2Li1161.7(3) C5O2Li1104.5(2)
O4Li2Li3103.1(2) C6O2C5114.6(3)
O4Li2N286.6(2) C6O2Li1117.4(3)
Li1Li3Li5176.5(2) C8O3Li1107.2(2)
Li2Li3Li147.31(16) C8O3Li2130.8(2)
Li2Li3Li5132.2(2) C8O3Li3131.1(2)
Li4Li3Li1136.3(2) Li1O3Li275.7(2)
Li4Li3Li2108.6(2) Li3O3Li1117.1(2)
Li4Li3Li546.85(15) Li3O3Li281.6(2)
N2Li3Li186.53(18) C13O4Li2105.7(2)
N2Li3Li255.17(18) C14O4C13112.7(3)
N2Li3Li455.07(16) C14O4Li2131.6(3)
N2Li3Li595.61(18) C16O5Li4109.3(2)
O3Li3Li132.29(14) C17O5C16113.6(2)
O3Li3Li251.19(17) C17O5Li4123.2(2)
O3Li3Li4159.8(3) C20O6Li5105.0(2)
O3Li3Li5144.2(2) C21O6C20115.5(3)
O3Li3N2105.2(2) C21O6Li5117.5(3)
O3Li3O8149.4(3) C23O7Li565.42(16)
O8Li3Li1150.6(2) C24O7C23111.5(2)
O8Li3Li2158.2(3) C24O7Li5103.5(2)
O8Li3Li450.58(15) C26O8Li3129.7(2)
O8Li3Li531.16(13) C26O8Li4127.0(2)
O8Li3N2105.4(2) C26O8Li5108.9(2)
Li5Li4Li384.0(2) Li3O8Li481.3(2)
N2Li4Li351.95(15) Li3O8Li5118.7(2)
N2Li4Li5125.2(2) Li5O8Li476.56(19)
N2Li4C18126.5(2) Li5C18Li466.22(19)
O5Li4Li3115.9(2)     

 

Table 6 Torsion Angles for cu_B0490_0m.
ABCDAngle/˚ ABCDAngle/˚
C1C2O1C3172.0(3) C27C26O8Li4-9.8(3)
C2C1N1C490.2(3) C27C26O8Li577.4(3)
C2C1N1C7-144.9(3) C28C26O8Li3-2.3(4)
C2C1N1Li1-28.2(4) C28C26O8Li4110.1(3)
C4C5O2C684.1(4) C28C26O8Li5-162.8(2)
C4C5O2Li1-45.8(3) Li1Li3O3C8-152.4(4)
C5C4N1C1-158.8(3) Li1Li3O3Li269.1(3)
C5C4N1C775.5(3) Li1Li3O8C2615.0(6)
C5C4N1Li1-29.7(3) Li1Li3O8Li4-116.7(5)
C7C8O3Li1-45.7(3) Li1Li3O8Li5173.9(4)
C7C8O3Li2-131.4(3) Li2Li3O3C8138.5(3)
C7C8O3Li3108.7(3) Li2Li3O3Li1-69.1(3)
C8C7N1C197.8(3) Li2Li3O8C26151.0(6)
C8C7N1C4-137.8(3) Li2Li3O8Li419.3(7)
C8C7N1Li1-30.8(3) Li2Li3O8Li5-50.1(8)
C9C8O3Li1-163.3(2) Li4Li3O3C8139.9(7)
C9C8O3Li2111.0(3) Li4Li3O3Li1-67.7(8)
C9C8O3Li3-8.9(4) Li4Li3O3Li21.5(8)
C10C8O3Li176.1(3) Li4Li3O8C26131.7(3)
C10C8O3Li2-9.5(4) Li4Li3O8Li5-69.4(2)
C10C8O3Li3-129.4(3) Li5Li3O3C827.4(5)
C12C13O4C14-177.8(3) Li5Li3O3Li1179.8(3)
C12C13O4Li2-27.8(3) Li5Li3O3Li2-111.0(4)
C13C12N2C15-168.6(2) Li5Li3O8C26-158.9(4)
C13C12N2Li2-57.8(3) Li5Li3O8Li469.4(2)
C13C12N2Li310.6(4) N1C1C2O1-67.7(3)
C13C12N2Li488.2(3) N1C4C5O254.2(4)
C15C16O5C17173.7(2) N1C7C8C9173.9(2)
C15C16O5Li431.9(3) N1C7C8C10-66.5(3)
C16C15N2C12-64.8(3) N1C7C8O354.5(3)
C16C15N2Li2-166.2(2) N2C12C13O464.0(3)
C16C15N2Li3115.8(3) N2C15C16O5-53.1(3)
C16C15N2Li441.1(3) N2Li3O3C8150.7(2)
C19C20O6C2183.7(4) N2Li3O3Li1-56.9(3)
C19C20O6Li5-47.3(3) N2Li3O3Li212.2(2)
C20C19N3C22-157.7(3) N2Li3O8C26126.2(2)
C20C19N3C2575.6(3) N2Li3O8Li4-5.5(2)
C20C19N3Li5-29.5(3) N2Li3O8Li5-75.0(3)
C22C23O7C24167.3(3) N3C19C20O654.7(4)
C22C23O7Li571.8(2) N3C22C23O7-68.5(3)
C23C22N3C1989.8(3) N3C25C26C27-68.4(3)
C23C22N3C25-144.5(2) N3C25C26C28172.4(3)
C23C22N3Li5-27.9(3) N3C25C26O853.6(3)
C25C26O8Li3115.3(3) O3Li3O8C26-52.5(6)
C25C26O8Li4-132.3(2) O3Li3O8Li4175.8(6)
C25C26O8Li5-45.2(3) O3Li3O8Li5106.4(5)
C26C25N3C19-137.5(3) O8Li3O3C8-30.6(7)
C26C25N3C2296.9(3) O8Li3O3Li1121.8(5)
C26C25N3Li5-31.0(3) O8Li3O3Li2-169.1(6)
C27C26O8Li3-122.1(3)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for cu_B0490_0m.
AtomxyzU(eq)
H1A7538010234669
H1B2587191267769
H2A5504901231573
H2B165969180473
H3A51044911183138
H3B111336391738138
H3C143145301305138
H4A21248601302868
H4B20627346255368
H5A33137281326475
H5B29697187378075
H6A273151342505134
H6B306836852885134
H6C363250642938134
H7A9528236350757
H7B18687947385657
H9A10616298480780
H9B8287838447280
H9C17337382477580
H10A3355092332882
H10B-376476353682
H10C1955035393982
H11A2059(16)2160(40)3075(15)67(10)
H11B1200(20)2470(50)2713(12)103(14)
H11C1450(40)1400(40)3280(30)190(30)
H12A2741530516957
H12B2195397448757
H13A1440360510063
H13B17521978532963
H14A12213584714119
H14B-7026644243119
H14C45129744920119
H15A33923097434055
H15B29911554409755
H16A3844338492559
H16B43631323465859
H17A4771442589379
H17B50931995619079
H17C53651367568279
H19A29458543663470
H19B29587258708570
H20A17147356636377
H20B20697244585377
H21A226050297105136
H21B182237036681136
H21C135651856688136
H22A42977746732064
H22B47676904697664
H23A43674620727760
H23B49465569781460
H24A36943422775699
H24B33984263821399
H24C43184038836199
H25A41258107616558
H25B32037930580458
H27A46734962629873
H27B50676305608473
H27C47894876567973
H28A39406240482380
H28B42407736517880
H28C33187407488180
H18A2890(20)2070(50)6540(17)94(13)
H18B3250(30)1310(40)6240(20)141(19)
H18C3870(20)2140(70)6740(20)160(20)

Experimental

Single crystals of C28H64Li5N3O8 [cu_B0490_0m] were []. A suitable crystal was selected and [] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 99.99 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 ShelXL [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. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [cu_B0490_0m]

Crystal Data for C28H64Li5N3O8 (=605.52 g/mol): monoclinic, space group P21/c (no. 14), a = 18.2841(8) Å, b = 9.1092(4) Å, c = 24.3776(10) Å, β = 111.387(2)°, = 3780.6(3) Å3, Z = 4, T = 99.99 K, μ(CuKα) = 0.586 mm-1, Dcalc = 1.064 g/cm3, 63345 reflections measured (5.19° ≤ 2Θ ≤ 135.984°), 6869 unique (Rint = 0.1315, Rsigma = 0.0627) which were used in all calculations. The final R1 was 0.0792 (I > 2σ(I)) and wR2 was 0.2261 (all data).

Refinement model description

Number of restraints - 6, 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. Restrained distances
C18-H18A ≈ C18-H18B ≈ C18-H18C
with sigma of 0.02
C11-H11A ≈ C11-H11B ≈ C11-H11C
with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C12(H12A,
H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C19(H19A,H19B),
C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B)
3.b Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C24(H24A,H24B,
H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)

This report has been created with Olex2, compiled on 2016.11.07 svn.r3352 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.