cu_B0133_0m

Table 1 Crystal data and structure refinement for cu_B0133_0m.
Identification code cu_B0133_0m
Empirical formula C40H104Li16N8O11
Formula weight 984.35
Temperature/K 99.99
Crystal system monoclinic
Space group P21/n
a/Å 12.1310(3)
b/Å 15.2270(4)
c/Å 16.3851(4)
α/° 90
β/° 92.206(2)
γ/° 90
Volume/Å3 3024.39(13)
Z 2
ρcalcg/cm3 1.081
μ/mm‑1 0.561
F(000) 1072.0
Crystal size/mm3 0.312 × 0.159 × 0.134
Radiation CuKα (λ = 1.54178)
2Θ range for data collection/° 7.928 to 139.972
Index ranges -14 ≤ h ≤ 12, -18 ≤ k ≤ 18, -19 ≤ l ≤ 19
Reflections collected 17423
Independent reflections 5646 [Rint = 0.0334, Rsigma = 0.0374]
Data/restraints/parameters 5646/73/494
Goodness-of-fit on F2 1.319
Final R indexes [I>=2σ (I)] R1 = 0.0962, wR2 = 0.2786
Final R indexes [all data] R1 = 0.1148, wR2 = 0.3136
Largest diff. peak/hole / e Å-3 0.97/-0.84

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for cu_B0133_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O550005000500025.1(5)
O27200.2(13)3769.6(11)5138.8(10)34.9(5)
O34333.0(13)3703.4(11)6484.9(10)35.4(5)
O45038.6(13)2869.9(10)4972.1(10)34.9(5)
O16499.3(14)4602.6(11)6656(1)36.9(5)
N46501(2)1491.1(14)4639.4(15)50.3(6)
N33666(2)1908.8(16)6700.4(16)52.8(7)
C187547(2)6138.8(18)5287(2)46.0(7)
N16123(2)4038.2(19)8275.6(14)57.6(7)
C134701(2)2248.2(18)4376.2(18)46.4(7)
C194080(3)5978.0(19)6806.9(17)46.1(7)
N29108(2)3559.9(19)6211(2)64.9(8)
C16888(3)5144(2)7310.1(17)52.7(8)
C58235(2)3818(2)4789(2)51.8(8)
C93348(2)3536(2)6879.7(19)50.6(7)
C122700(4)1720(4)6155(3)57.1(12)
C113958(4)1098(2)7154(3)52.9(11)
C103378(3)2608(2)7273(2)50.2(11)
Li26620(3)4949(3)5501(3)36.9(9)
C26223(4)4998(3)8073(3)53.8(13)
C156053(6)758(3)5123(4)65.0(16)
Li76535(4)2659(3)5313(3)41.2(10)
Li54118(3)3880(3)5263(3)35.7(9)
Li84862(4)2606(3)6100(3)40.6(9)
Li14931(3)4890(3)6260(2)35.2(9)
C145709(4)1793(3)4021(3)52.2(13)
Li65782(3)3941(3)4511(2)35.4(9)
Li37409(3)3666(3)6293(3)41(1)
C37209(5)3721(4)8559(4)67.0(17)
C167540(5)1201(4)4300(4)62.9(16)
Li45712(4)3629(3)7087(3)42.8(10)
C45346(6)3926(6)8933(3)83(2)
C89708(5)2864(5)6720(5)60(2)
C79654(6)4392(6)6347(6)62(2)
C69110(5)3305(5)5355(4)57(2)
C8A9488(6)2667(6)5991(5)80(2)
C7A9846(7)3966(10)6781(7)110(4)
C6A9120(5)4091(5)5390(4)61.7(19)
C15A6970(12)695(6)4942(7)76(4)
C16A6920(9)1662(7)3796(6)68(3)
C14A5263(8)1390(5)4535(6)56(2)
C4A5303(11)4563(10)8591(7)80(4)
C3A6432(14)3287(11)8876(7)102(5)
C2A7131(9)4476(9)8064(6)72(3)
C10A2819(19)2771(15)6691(15)85(6)
C11A4110(20)1882(17)7625(14)99(8)
C12A3080(30)1280(20)6380(20)124(13)
O6B6445(2)2636(2)6541.5(18)77.4(8)
C17B6891(9)1943(6)6982(7)120(3)
CNT161303140619850
C17A6634(17)2168(10)6688(13)324(10)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for cu_B0133_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
O519.4(10)28.3(11)27.4(10)1.0(8)-0.1(8)1.4(7)
O223.6(9)41.0(9)40.5(9)4.7(7)5.5(6)6.9(6)
O329.0(9)40.2(9)37.4(9)3.9(7)6.1(7)2.0(6)
O432.7(9)32.0(9)40.0(9)-3.3(6)-0.3(7)-0.3(6)
O134.2(9)41.4(10)34.5(8)-0.8(7)-5.8(7)-1.1(7)
N463.2(16)36.2(12)52.1(13)0.4(10)11.1(11)12.7(10)
N352.8(15)47.8(13)58.1(14)12.6(11)6.9(11)-8.7(11)
C1832.1(14)44.4(15)61.0(17)8.0(12)-6.5(12)-5.8(10)
N162.9(17)74.9(18)34.4(12)9.9(11)-5.7(11)3.2(13)
C1348.9(15)40.5(13)49.6(14)-9.8(12)-1.1(12)-2.2(11)
C1954.8(17)45.8(15)38.2(13)-2.3(11)7.4(12)12.3(13)
N230.0(13)68.4(17)95(2)12.9(15)-12.2(13)9.8(11)
C154.2(17)62.8(18)40.2(14)-7.2(13)-9.7(12)-5.6(13)
C529.9(14)56.7(16)70.1(19)10.2(14)19.5(13)8.7(11)
C937.4(15)63.0(18)52.3(15)10.3(13)15.1(12)0.5(12)
C1249(2)51(3)72(3)7(2)5.2(19)-8.3(19)
C1162(2)35.1(18)62(2)15.0(16)12.9(18)-1.2(15)
C1051(2)50(2)50(2)5.7(16)16.0(17)-3.7(16)
Li230(2)38(2)43(2)4.5(16)-1.7(16)1.0(15)
C261(3)61(3)39(2)-5.2(18)-9.2(19)5(2)
C1587(4)41(2)69(3)7(2)24(3)5(3)
Li738(2)36(2)50(2)4.8(18)5.6(18)6.2(17)
Li528(2)35(2)43(2)2.4(16)0.6(16)3.0(15)
Li839(2)42(2)41(2)6.3(18)6.6(17)0.3(17)
Li133(2)38(2)33.7(19)1.6(16)0.5(15)3.7(16)
C1464(3)45(2)47(2)-7(2)2(2)5(2)
Li632(2)38(2)37(2)1.1(16)3.5(16)6.3(15)
Li328(2)43(2)51(2)9.2(19)-5.4(17)3.1(16)
C377(4)60(3)62(3)12(2)-28(3)-1(3)
C1668(4)56(3)66(3)-2(2)21(3)23(2)
Li438(2)54(3)37(2)7.1(19)-0.1(17)5.3(19)
C4102(5)107(5)41(3)0(3)13(3)-18(4)
C834(3)76(5)70(5)21(4)-3(3)22(3)
C737(4)78(5)71(5)16(4)-6(3)-13(3)
C644(4)63(5)64(4)3(3)4(3)6(3)
C8A50(4)102(6)88(5)35(4)5(3)23(4)
C7A38(4)185(12)105(7)-31(8)-30(5)5(5)
C6A30(3)70(4)86(4)13(3)6(3)2(2)
C15A119(10)41(4)70(6)-7(4)1(6)31(5)
C16A88(7)59(5)58(5)-5(4)18(5)23(5)
C14A78(6)31(4)59(5)-8(3)0(4)-2(3)
C4A79(8)106(10)56(6)-19(7)13(5)-11(7)
C3A119(11)147(12)40(5)44(7)-11(6)9(9)
C2A62(6)103(9)48(5)2(5)-16(4)-2(6)
C10A84(13)88(13)84(13)-11(10)10(10)-13(10)
C11A111(17)102(16)89(14)-5(12)60(13)19(13)
C12A150(30)100(20)130(30)-37(19)50(20)-50(20)
O6B60.8(16)102(2)70.4(16)-16.6(15)10.3(13)-7.5(15)
C17B120(6)115(8)126(6)30(5)9(5)12(5)
C17A440(20)112(8)430(30)63(12)98(19)102(9)

 

Table 4 Bond Lengths for cu_B0133_0m.
AtomAtomLength/Å AtomAtomLength/Å
O5Li22.101(4) C19Li612.176(5)
O5Li212.101(4) N2Li32.076(5)
O5Li512.068(4) N2C81.517(6)
O5Li52.068(4) N2C71.443(8)
O5Li112.077(4) N2C61.454(8)
O5Li12.077(4) N2C8A1.484(9)
O5Li62.049(4) N2C7A1.412(9)
O5Li612.049(4) N2C6A1.570(8)
O2C51.402(3) C1C21.530(6)
O2Li22.026(4) C1C2A1.618(11)
O2Li71.900(5) C5C61.588(7)
O2Li61.987(4) C5C6A1.487(7)
O2Li31.904(5) C9C101.553(5)
O3C91.404(3) C9C10A1.36(2)
O3Li52.027(4) Li2Li53.453(5)
O3Li81.907(5) Li2Li512.337(6)
O3Li11.986(4) Li2Li12.439(6)
O3Li41.912(5) Li2Li113.392(5)
O4C131.410(3) Li2Li62.427(6)
O4Li71.906(5) Li2Li613.368(5)
O4Li51.969(4) Li2Li32.514(6)
O4Li81.912(5) Li2Li43.497(6)
O4Li62.024(4) Li7Li53.470(6)
O1C11.418(3) Li7Li82.447(6)
O1Li21.976(5) Li7Li62.506(5)
O1Li12.034(4) Li7Li32.434(6)
O1Li31.912(5) Li7Li43.442(6)
O1Li41.914(5) Li7O6B2.020(5)
N4C151.484(6) Li5C1812.180(5)
N4Li72.093(5) Li5Li212.337(6)
N4C141.443(5) Li5Li82.523(6)
N4C161.465(6) Li5Li113.361(6)
N4C15A1.420(9) Li5Li12.426(6)
N4C16A1.514(10) Li5Li62.406(6)
N4C14A1.512(10) Li5Li613.341(6)
N3C121.475(5) Li8Li13.489(6)
N3C111.477(4) Li8Li63.519(6)
N3C101.470(5) Li8Li33.490(6)
N3Li82.076(5) Li8Li42.444(6)
N3C10A1.67(2) Li8O6B2.026(5)
N3C11A1.59(3) Li1Li213.392(5)
N3C12A1.29(3) Li1Li513.361(6)
C18Li22.168(5) Li1Li63.405(6)
C18Li512.180(5) Li1Li612.331(6)
N1C21.505(6) Li1Li42.514(6)
N1C31.462(6) Li6C1912.176(5)
N1Li42.087(5) Li6Li213.368(5)
N1C41.468(7) Li6Li513.341(6)
N1C4A1.391(13) Li6Li112.331(6)
N1C3A1.546(12) Li6Li33.485(6)
N1C2A1.447(12) Li3Li42.479(6)
C13C141.540(6) Li3O6B2.008(5)
C13C14A1.493(8) Li4O6B1.984(6)
C19Li12.165(5) O6BC17B1.377(5)

11-X,1-Y,1-Z

 

Table 5 Bond Angles for cu_B0133_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Li21O5Li2180.0 Li1Li5Li1190.26(16)
Li5O5Li2168.18(15) Li1Li5Li6144.24(13)
Li5O5Li2111.82(15) Li61Li5Li259.41(11)
Li51O5Li268.18(15) Li6Li5Li244.64(14)
Li51O5Li21111.82(15) Li61Li5Li7120.16(15)
Li5O5Li51180.0 Li6Li5Li746.24(13)
Li5O5Li11108.35(16) Li6Li5Li891.06(19)
Li51O5Li1108.35(16) Li61Li5Li1161.07(12)
Li5O5Li171.65(16) Li6Li5Li1143.91(13)
Li51O5Li1171.65(16) Li6Li5Li189.59(19)
Li1O5Li271.43(16) Li6Li5Li6189.45(16)
Li11O5Li2108.57(16) O3Li8O4100.8(2)
Li11O5Li2171.43(16) O3Li8N392.3(2)
Li1O5Li21108.57(16) O3Li8Li7116.2(2)
Li11O5Li1180.0 O3Li8Li552.24(15)
Li6O5Li271.55(16) O3Li8Li126.93(11)
Li61O5Li2108.45(16) O3Li8Li681.86(15)
Li6O5Li21108.45(16) O3Li8Li382.68(17)
Li61O5Li2171.55(16) O3Li8Li450.31(15)
Li61O5Li5171.53(16) O3Li8O6B100.9(2)
Li6O5Li571.53(16) O4Li8N3132.2(2)
Li61O5Li5108.47(16) O4Li8Li750.04(15)
Li6O5Li51108.47(16) O4Li8Li550.46(14)
Li6O5Li1168.79(16) O4Li8Li181.93(15)
Li6O5Li1111.21(16) O4Li8Li627.45(11)
Li61O5Li11111.21(16) O4Li8Li381.87(16)
Li61O5Li168.79(16) O4Li8Li4116.5(2)
Li61O5Li6180.0(2) O4Li8O6B101.6(2)
C5O2Li2113.6(2) N3Li8Li7151.1(2)
C5O2Li7120.0(2) N3Li8Li5114.1(2)
C5O2Li6123.5(2) N3Li8Li1119.3(2)
C5O2Li3108.9(2) N3Li8Li6153.3(2)
Li7O2Li2126.19(19) N3Li8Li3145.7(2)
Li7O2Li680.24(18) N3Li8Li4107.3(2)
Li7O2Li379.5(2) Li7Li8Li588.55(19)
Li6O2Li274.41(17) Li7Li8Li189.35(17)
Li3O2Li279.46(18) Li7Li8Li645.41(13)
Li3O2Li6127.16(19) Li7Li8Li344.20(15)
C9O3Li5113.6(2) Li5Li8Li144.06(13)
C9O3Li8107.3(2) Li5Li8Li643.14(13)
C9O3Li1125.0(2) Li5Li8Li389.45(16)
C9O3Li4119.6(2) Li1Li8Li658.14(11)
Li8O3Li579.73(18) Li1Li8Li360.88(12)
Li8O3Li1127.30(19) Li3Li8Li659.64(12)
Li8O3Li479.6(2) Li4Li8Li789.5(2)
Li1O3Li574.38(16) Li4Li8Li590.16(19)
Li4O3Li5126.46(19) Li4Li8Li146.11(14)
Li4O3Li180.29(18) Li4Li8Li689.06(17)
C13O4Li7109.8(2) Li4Li8Li345.26(15)
C13O4Li5122.63(19) O6BLi8N3120.8(2)
C13O4Li8119.2(2) O6BLi8Li752.68(16)
C13O4Li6113.88(19) O6BLi8Li5119.4(2)
Li7O4Li5127.09(19) O6BLi8Li186.03(18)
Li7O4Li879.7(2) O6BLi8Li685.86(17)
Li7O4Li679.17(18) O6BLi8Li329.95(14)
Li5O4Li674.10(17) O6BLi8Li451.66(17)
Li8O4Li581.08(19) O5Li1C19112.80(19)
Li8O4Li6126.75(19) O5Li1Li254.75(13)
C1O1Li2122.3(2) O5Li1Li2135.96(10)
C1O1Li1113.3(2) O5Li1Li554.00(14)
C1O1Li3119.3(2) O5Li1Li5135.74(10)
C1O1Li4109.1(2) O5Li1Li890.43(14)
Li2O1Li174.93(17) O5Li1Li6155.04(14)
Li3O1Li280.56(19) O5Li1Li634.13(9)
Li3O1Li1127.24(19) O5Li1Li4124.7(2)
Li3O1Li480.8(2) O3Li1O5106.66(19)
Li4O1Li2128.1(2) O3Li1O195.13(17)
Li4O1Li179.05(18) O3Li1C19115.9(2)
C15N4Li7111.0(3) O3Li1Li2116.6(2)
C14N4C15111.5(4) O3Li1Li2191.65(16)
C14N4Li795.7(2) O3Li1Li553.58(14)
C14N4C16112.9(3) O3Li1Li51141.53(19)
C16N4C15108.3(4) O3Li1Li825.77(11)
C16N4Li7117.2(3) O3Li1Li61131.7(2)
C15AN4Li7122.7(5) O3Li1Li683.96(15)
C15AN4C16A108.7(6) O3Li1Li448.57(14)
C15AN4C14A109.6(7) O1Li1O5105.15(18)
C16AN4Li7109.6(4) O1Li1C19119.2(2)
C16AN4C14A106.3(6) O1Li1Li21140.18(18)
C14AN4Li798.4(3) O1Li1Li251.46(14)
C12N3Li8111.5(3) O1Li1Li5190.74(16)
C11N3C12108.2(3) O1Li1Li5115.4(2)
C11N3Li8120.5(3) O1Li1Li880.16(14)
C10N3C12109.0(3) O1Li1Li61131.3(2)
C10N3C11110.0(3) O1Li1Li682.35(15)
C10N3Li896.9(2) O1Li1Li448.37(14)
C10AN3Li892.0(8) C19Li1Li2127.3(2)
C11AN3Li8104.2(9) C19Li1Li2192.21(16)
C11AN3C10A102.5(12) C19Li1Li5193.63(16)
C12AN3Li8124.6(15) C19Li1Li5125.2(2)
C12AN3C10A104(2) C19Li1Li8141.6(2)
C12AN3C11A122(2) C19Li1Li6157.77(16)
Li2C18Li5165.03(16) C19Li1Li6146.92(18)
C2N1Li495.9(2) C19Li1Li4122.5(2)
C3N1C2108.2(3) Li2Li1Li2190.71(16)
C3N1Li4112.2(3) Li2Li1Li5144.06(13)
C3N1C4108.9(4) Li21Li1Li889.85(13)
C4N1C2109.6(4) Li2Li1Li890.95(16)
C4N1Li4120.9(3) Li2Li1Li645.45(14)
C4AN1Li4111.7(5) Li21Li1Li659.40(11)
C4AN1C3A110.4(9) Li2Li1Li489.82(19)
C4AN1C2A116.6(8) Li51Li1Li2161.50(12)
C3AN1Li4114.6(6) Li5Li1Li2143.54(13)
C2AN1Li495.0(4) Li5Li1Li290.42(19)
C2AN1C3A107.9(8) Li5Li1Li5189.74(16)
O4C13C14110.5(3) Li51Li1Li8120.52(15)
O4C13C14A110.4(4) Li5Li1Li846.32(13)
Li1C19Li6164.94(16) Li51Li1Li659.17(12)
C8N2Li3118.4(3) Li5Li1Li644.97(14)
C7N2Li3111.8(4) Li5Li1Li490.78(19)
C7N2C8108.6(5) Li61Li1Li2145.66(14)
C7N2C6111.5(5) Li61Li1Li289.79(19)
C6N2Li397.0(3) Li61Li1Li5145.73(14)
C6N2C8109.0(5) Li61Li1Li589.20(19)
C8AN2Li3113.9(4) Li6Li1Li861.37(12)
C8AN2C6A104.5(5) Li61Li1Li8135.51(19)
C7AN2Li3121.9(5) Li61Li1Li689.17(16)
C7AN2C8A111.5(6) Li61Li1Li4179.6(3)
C7AN2C6A108.4(7) Li4Li1Li21134.32(19)
C6AN2Li393.3(3) Li4Li1Li51133.88(19)
O1C1C2111.3(3) Li4Li1Li844.48(14)
O1C1C2A104.9(5) Li4Li1Li690.54(16)
O2C5C6108.9(3) N4C14C13113.3(3)
O2C5C6A112.2(3) O5Li6C191113.44(19)
O3C9C10110.5(2) O5Li6Li255.23(13)
C10AC9O3117.0(10) O5Li6Li2136.29(10)
N3C10C9113.3(3) O5Li6Li7125.0(2)
O5Li2C18112.90(18) O5Li6Li5135.96(10)
O5Li2Li5155.23(14) O5Li6Li554.60(13)
O5Li2Li533.78(9) O5Li6Li1156.17(14)
O5Li2Li1135.48(10) O5Li6Li134.66(10)
O5Li2Li153.82(13) O5Li6Li391.32(15)
O5Li2Li6135.25(10) O2Li6O5107.81(19)
O5Li2Li653.23(13) O2Li6O495.19(17)
O5Li2Li3124.2(2) O2Li6C191115.0(2)
O5Li2Li489.71(15) O2Li6Li253.53(14)
O2Li2O5104.41(18) O2Li6Li21143.19(19)
O2Li2C18120.3(2) O2Li6Li748.35(14)
O2Li2Li582.12(14) O2Li6Li5117.2(2)
O2Li2Li51130.5(2) O2Li6Li5192.65(16)
O2Li2Li1115.1(2) O2Li6Li11132.6(2)
O2Li2Li1190.16(16) O2Li6Li184.54(15)
O2Li2Li652.07(14) O2Li6Li325.82(11)
O2Li2Li61138.90(18) O4Li6O5105.59(19)
O2Li2Li348.14(14) O4Li6C191117.9(2)
O2Li2Li480.27(15) O4Li6Li2190.51(16)
O1Li2O5106.35(19) O4Li6Li2116.2(2)
O1Li2O294.78(18) O4Li6Li748.34(14)
O1Li2C18115.8(2) O4Li6Li51140.72(19)
O1Li2Li51132.5(2) O4Li6Li551.92(14)
O1Li2Li583.41(15) O4Li6Li182.77(15)
O1Li2Li153.62(14) O4Li6Li11131.0(2)
O1Li2Li11140.83(19) O4Li6Li380.62(15)
O1Li2Li6115.3(2) C191Li6Li2193.76(16)
O1Li2Li6192.51(16) C191Li6Li2125.5(2)
O1Li2Li348.61(15) C191Li6Li7121.6(2)
O1Li2Li425.52(11) C191Li6Li5127.5(2)
C18Li2Li5146.62(18) C191Li6Li5192.85(16)
C18Li2Li5157.73(15) C191Li6Li1157.29(15)
C18Li2Li1194.38(16) C191Li6Li1148.08(18)
C18Li2Li1124.4(2) C191Li6Li3140.81(19)
C18Li2Li6191.93(16) Li2Li6Li2191.52(16)
C18Li2Li6128.8(2) Li2Li6Li790.43(19)
C18Li2Li3122.9(2) Li2Li6Li5144.39(13)
C18Li2Li4141.3(2) Li21Li6Li160.12(12)
Li51Li2Li589.01(17) Li2Li6Li145.75(14)
Li51Li2Li1145.65(14) Li2Li6Li346.16(14)
Li51Li2Li189.41(19) Li21Li6Li3121.81(16)
Li51Li2Li689.0(2) Li7Li6Li21133.78(19)
Li51Li2Li6145.61(14) Li7Li6Li51134.82(19)
Li51Li2Li3178.7(3) Li7Li6Li190.31(16)
Li51Li2Li4135.4(2) Li7Li6Li344.28(14)
Li5Li2Li460.81(12) Li5Li6Li2143.95(13)
Li1Li2Li544.64(13) Li51Li6Li2161.96(11)
Li11Li2Li558.80(11) Li5Li6Li291.2(2)
Li1Li2Li1189.29(16) Li5Li6Li789.85(19)
Li1Li2Li6143.80(13) Li5Li6Li5190.55(16)
Li1Li2Li391.07(19) Li5Li6Li145.44(14)
Li1Li2Li445.96(13) Li51Li6Li159.76(12)
Li11Li2Li4119.58(15) Li51Li6Li390.54(14)
Li6Li2Li544.17(14) Li5Li6Li391.49(17)
Li61Li2Li558.64(11) Li11Li6Li290.95(19)
Li6Li2Li188.81(19) Li11Li6Li2146.41(14)
Li6Li2Li1143.39(13) Li11Li6Li7178.6(2)
Li61Li2Li1160.48(11) Li11Li6Li5146.56(14)
Li6Li2Li6188.48(16) Li11Li6Li590.36(19)
Li6Li2Li389.71(19) Li11Li6Li190.83(16)
Li6Li2Li489.84(17) Li11Li6Li3137.1(2)
Li61Li2Li489.76(14) Li1Li6Li361.73(12)
Li3Li2Li590.44(16) O2Li3O1101.02(19)
Li3Li2Li11133.09(19) O2Li3N292.1(2)
Li3Li2Li61134.9(2) O2Li3Li252.40(14)
Li3Li2Li445.12(14) O2Li3Li750.16(16)
N1C2C1111.7(3) O2Li3Li882.23(16)
O2Li7O4102.2(2) O2Li3Li182.01(14)
O2Li7N4132.6(3) O2Li3Li627.03(11)
O2Li7Li227.84(11) O2Li3Li4116.2(2)
O2Li7Li583.28(15) O2Li3O6B102.1(2)
O2Li7Li8118.3(2) O1Li3N2131.7(3)
O2Li7Li651.40(14) O1Li3Li250.83(15)
O2Li7Li350.31(15) O1Li3Li7115.7(2)
O2Li7Li483.34(17) O1Li3Li881.58(16)
O2Li7O6B101.8(2) O1Li3Li127.26(11)
O4Li7N489.4(2) O1Li3Li681.72(15)
O4Li7Li283.24(15) O1Li3Li449.66(16)
O4Li7Li526.92(11) O1Li3O6B99.9(2)
O4Li7Li850.24(15) N2Li3Li2112.7(2)
O4Li7Li652.49(15) N2Li3Li7108.4(2)
O4Li7Li3118.2(2) N2Li3Li8146.6(2)
O4Li7Li482.61(16) N2Li3Li1152.3(2)
O4Li7O6B102.0(2) N2Li3Li6119.1(2)
N4Li7Li2153.2(2) N2Li3Li4151.5(3)
N4Li7Li5116.29(19) Li2Li3Li889.68(16)
N4Li7Li8104.5(2) Li2Li3Li143.62(13)
N4Li7Li6112.7(2) Li2Li3Li644.13(13)
N4Li7Li3152.0(2) Li7Li3Li290.09(19)
N4Li7Li4144.0(2) Li7Li3Li844.51(15)
Li5Li7Li259.37(11) Li7Li3Li188.48(16)
Li8Li7Li290.51(17) Li7Li3Li645.97(14)
Li8Li7Li546.63(14) Li7Li3Li489.0(2)
Li8Li7Li690.53(19) Li8Li3Li159.55(12)
Li8Li7Li445.24(15) Li6Li3Li860.59(12)
Li6Li7Li243.87(13) Li6Li3Li158.02(11)
Li6Li7Li543.91(13) Li4Li3Li288.93(19)
Li6Li7Li489.82(16) Li4Li3Li844.46(15)
Li3Li7Li245.89(13) Li4Li3Li145.33(13)
Li3Li7Li591.40(17) Li4Li3Li689.27(16)
Li3Li7Li891.3(2) O6BLi3N2122.6(2)
Li3Li7Li689.75(19) O6BLi3Li2119.9(2)
Li3Li7Li446.06(15) O6BLi3Li753.06(17)
Li4Li7Li260.48(12) O6BLi3Li830.25(13)
Li4Li7Li561.18(12) O6BLi3Li185.01(17)
O6BLi7N4120.7(2) O6BLi3Li687.03(17)
O6BLi7Li286.12(18) O6BLi3Li451.18(17)
O6BLi7Li587.42(18) O3Li4O1101.7(2)
O6BLi7Li852.90(17) O3Li4N1129.5(2)
O6BLi7Li6120.2(2) O3Li4Li282.90(16)
O6BLi7Li352.60(18) O3Li4Li782.32(17)
O6BLi7Li430.41(14) O3Li4Li527.61(11)
O5Li5C181113.77(19) O3Li4Li850.10(15)
O5Li5Li2156.59(14) O3Li4Li151.14(14)
O5Li5Li234.40(9) O3Li4Li3117.1(2)
O5Li5Li790.19(15) O3Li4O6B102.2(2)
O5Li5Li8124.8(2) O1Li4N190.5(2)
O5Li5Li154.35(13) O1Li4Li226.41(11)
O5Li5Li1135.91(10) O1Li4Li781.69(16)
O5Li5Li653.87(13) O1Li4Li582.42(16)
O5Li5Li6135.58(10) O1Li4Li8117.0(2)
O3Li5O5105.49(19) O1Li4Li152.58(15)
O3Li5C181119.3(2) O1Li4Li349.58(15)
O3Li5Li21131.4(2) O1Li4O6B100.7(2)
O3Li5Li282.63(15) N1Li4Li2116.8(2)
O3Li5Li780.16(14) N1Li4Li7148.2(2)
O3Li5Li848.04(14) N1Li4Li5149.8(2)
O3Li5Li11140.59(19) N1Li4Li8152.5(3)
O3Li5Li152.04(14) N1Li4Li1110.2(2)
O3Li5Li6115.6(2) N1Li4Li3108.0(2)
O3Li5Li6191.11(16) Li2Li4Li558.97(11)
O4Li5O5106.91(19) Li7Li4Li260.60(12)
O4Li5O394.76(18) Li7Li4Li559.80(12)
O4Li5C181114.5(2) Li8Li4Li290.65(17)
O4Li5Li283.76(15) Li8Li4Li745.30(15)
O4Li5Li21132.5(2) Li8Li4Li545.83(14)
O4Li5Li725.99(11) Li8Li4Li189.42(19)
O4Li5Li848.46(14) Li8Li4Li390.3(2)
O4Li5Li1116.0(2) Li1Li4Li244.22(13)
O4Li5Li1192.38(17) Li1Li4Li789.32(16)
O4Li5Li653.98(15) Li1Li4Li543.60(13)
O4Li5Li61141.6(2) Li3Li4Li245.94(13)
C181Li5Li2148.11(19) Li3Li4Li744.98(15)
C181Li5Li2157.24(15) Li3Li4Li589.53(17)
C181Li5Li7140.49(19) Li3Li4Li190.15(19)
C181Li5Li8121.4(2) O6BLi4N1123.6(2)
C181Li5Li1192.24(16) O6BLi4Li286.76(18)
C181Li5Li1129.3(2) O6BLi4Li731.02(13)
C181Li5Li6124.8(2) O6BLi4Li586.63(18)
C181Li5Li6195.03(16) O6BLi4Li853.23(17)
Li21Li5Li290.99(17) O6BLi4Li1120.3(2)
Li21Li5Li7136.7(2) O6BLi4Li352.05(17)
Li2Li5Li760.77(12) N2C6C5113.9(5)
Li21Li5Li8178.4(2) C5C6AN2113.2(4)
Li21Li5Li190.81(19) C13C14AN4112.1(5)
Li21Li5Li1146.53(15) N1C2AC1110.0(6)
Li21Li5Li690.4(2) C9C10AN3112.8(15)
Li21Li5Li6146.58(14) Li7O6BLi874.4(2)
Li8Li5Li290.37(16) Li3O6BLi774.3(2)
Li8Li5Li744.83(14) Li3O6BLi8119.8(2)
Li8Li5Li11134.97(19) Li4O6BLi7118.6(2)
Li8Li5Li61133.85(19) Li4O6BLi875.1(2)
Li1Li5Li244.95(14) Li4O6BLi376.8(2)
Li11Li5Li259.70(12) C17BO6BLi7120.0(6)
Li1Li5Li790.13(16) C17BO6BLi8121.1(6)
Li11Li5Li790.14(14) C17BO6BLi3119.0(6)
Li1Li5Li889.62(19) C17BO6BLi4121.4(6)

11-X,1-Y,1-Z

 

Table 6 Torsion Angles for cu_B0133_0m.
ABCDAngle/˚ ABCDAngle/˚
O2C5C6N2-50.8(6) Li1O3C9C10A152.8(12)
O2C5C6AN248.5(5) Li1O1C1C264.5(3)
O3C9C10N3-52.1(4) Li1O1C1C2A118.0(5)
O3C9C10AN346.7(18) Li6O2C5C6-158.5(3)
O4C13C14N447.8(4) Li6O2C5C6A152.6(3)
O4C13C14AN4-51.7(7) Li6O4C13C1470.1(3)
O1C1C2N149.7(4) Li6O4C13C14A119.5(5)
O1C1C2AN1-61.5(8) Li3O2C5C628.6(4)
C12N3C10C9-76.1(4) Li3O2C5C6A-20.3(4)
C11N3C10C9165.5(3) Li3O1C1C2-111.5(3)
Li2O2C5C6115.0(4) Li3O1C1C2A-57.9(5)
Li2O2C5C6A66.2(4) Li3N2C6C540.2(5)
Li2O1C1C2150.9(3) Li3N2C6AC5-44.9(5)
Li2O1C1C2A-155.5(5) C3N1C2C169.8(4)
C15N4C14C1368.0(4) C16N4C14C13-169.9(4)
Li7O2C5C6-60.0(4) Li4O3C9C10-56.7(3)
Li7O2C5C6A-108.9(4) Li4O3C9C10A-107.9(13)
Li7O4C13C14-16.5(3) Li4O1C1C2-21.5(3)
Li7O4C13C14A32.9(5) Li4O1C1C2A32.0(5)
Li7N4C14C13-47.2(4) Li4N1C2C1-45.9(3)
Li7N4C14AC1339.5(6) Li4N1C2AC151.4(7)
Li5O3C9C10117.1(3) C4N1C2C1-171.7(4)
Li5O3C9C10A65.9(13) C8N2C6C5163.5(5)
Li5O4C13C14156.0(3) C7N2C6C5-76.6(6)
Li5O4C13C14A-154.6(5) C8AN2C6AC570.8(5)
Li8O3C9C1031.0(3) C7AN2C6AC5-170.2(6)
Li8O3C9C10A-20.2(13) C15AN4C14AC13168.8(6)
Li8O4C13C14-105.6(3) C16AN4C14AC13-73.8(7)
Li8O4C13C14A-56.2(5) C4AN1C2AC1-66.0(10)
Li8N3C10C939.5(3) C3AN1C2AC1169.2(8)
Li8N3C10AC9-42.8(15) C11AN3C10AC962.2(18)
Li1O3C9C10-156.0(2) C12AN3C10AC9-169(2)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for cu_B0133_0m.
AtomxyzU(eq)
H13A42682545393256
H13B42211803462456
H13C48822466382856
H13D38912167438656
H1AA68325767714363
H1AB76745011743863
H1BC63235582745063
H1BD75695455716663
H5AA84614440473662
H5AB81973552423762
H5BC81984244433262
H5BD84223236456262
H9AA27173575648061
H9AB32443984730861
H9BC35133544747661
H9BD28334026675561
H12A28661222580186
H12B25262237581886
H12C20661575648386
H11A3309880742879
H11B45481226756379
H11C4212652677379
H10A39232608773960
H10B26462478749160
H2A65875309854165
H2B54765252798365
H15A6630536550497
H15B5806285475497
H15C5429969543097
H14A54541285368863
H14B60782209365663
H3A772737778118100
H3B715431038720100
H3C747240709030100
H16A8040994474394
H16B78811693401894
H16C7393721391294
H4A562442389422124
H4B527233009058124
H4C462541648758124
H8A96503003730190
H8B104872852658390
H8C93742289660690
H7A91704869615193
H7B103414404605293
H7C98224469693393
H6A89572668531369
H6B98563408515069
H8AA1010427145624120
H8AB888023465717120
H8AC973023526488120
H7AA955745426931165
H7AB1056640386538165
H7AC992835987271165
H6AA90334723551174
H6AB98454011514374
H15D67986245518115
H15E77737134892115
H15F66652004626115
H16D772617063827102
H16E660622123582102
H16F669911773431102
H14C5091986407468
H14D49751124503568
H4AA557548269106121
H4AB465142048689121
H4AC510750308200121
H3AA673935359387153
H3AB698229058633153
H3AC577229438987153
H2AA76844034790986
H2AB74354806854286
H10C245528246142102
H10D223726707088102
H11D348919017987149
H11E459323907735149
H11F453213407723149
H12D34977346400185
H12E288514285805185
H12F239912146678185
H19A4620(30)6410(30)7070(30)72(11)
H18A7990(50)5980(40)4570(40)128(19)
H18B7510(40)6810(30)5210(30)90(13)
H19B3280(40)6340(30)6790(30)105(16)
H18C7960(30)6060(30)5880(30)76(12)
H17A639614366932180
H17B698421117558180
H17C761017906770180
H19C3750(30)5490(30)7260(30)81(11)
H17D660716806297487
H17E617520287149487
H17F739822616886487

 

Table 8 Atomic Occupancy for cu_B0133_0m.
AtomOccupancy AtomOccupancy AtomOccupancy
H13A0.628(6) H13B0.628(6) H13C0.372(6)
H13D0.372(6) H1AA0.656(7) H1AB0.656(7)
H1BC0.344(7) H1BD0.344(7) H5AA0.466(7)
H5AB0.466(7) H5BC0.534(7) H5BD0.534(7)
H9AA0.789(7) H9AB0.789(7) H9BC0.211(7)
H9BD0.211(7) C120.789(7) H12A0.789(7)
H12B0.789(7) H12C0.789(7) C110.789(7)
H11A0.789(7) H11B0.789(7) H11C0.789(7)
C100.789(7) H10A0.789(7) H10B0.789(7)
C20.656(7) H2A0.656(7) H2B0.656(7)
C150.628(6) H15A0.628(6) H15B0.628(6)
H15C0.628(6) C140.628(6) H14A0.628(6)
H14B0.628(6) C30.656(7) H3A0.656(7)
H3B0.656(7) H3C0.656(7) C160.628(6)
H16A0.628(6) H16B0.628(6) H16C0.628(6)
C40.656(7) H4A0.656(7) H4B0.656(7)
H4C0.656(7) C80.466(7) H8A0.466(7)
H8B0.466(7) H8C0.466(7) C70.466(7)
H7A0.466(7) H7B0.466(7) H7C0.466(7)
C60.466(7) H6A0.466(7) H6B0.466(7)
C8A0.534(7) H8AA0.534(7) H8AB0.534(7)
H8AC0.534(7) C7A0.534(7) H7AA0.534(7)
H7AB0.534(7) H7AC0.534(7) C6A0.534(7)
H6AA0.534(7) H6AB0.534(7) C15A0.372(6)
H15D0.372(6) H15E0.372(6) H15F0.372(6)
C16A0.372(6) H16D0.372(6) H16E0.372(6)
H16F0.372(6) C14A0.372(6) H14C0.372(6)
H14D0.372(6) C4A0.344(7) H4AA0.344(7)
H4AB0.344(7) H4AC0.344(7) C3A0.344(7)
H3AA0.344(7) H3AB0.344(7) H3AC0.344(7)
C2A0.344(7) H2AA0.344(7) H2AB0.344(7)
C10A0.211(7) H10C0.211(7) H10D0.211(7)
C11A0.211(7) H11D0.211(7) H11E0.211(7)
H11F0.211(7) C12A0.211(7) H12D0.211(7)
H12E0.211(7) H12F0.211(7) CNT10

Experimental

Single crystals of C40H104Li16N8O11 [cu_B0133_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 ShelXT [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 [cu_B0133_0m]

Crystal Data for C40H104Li16N8O11 (=984.35 g/mol): monoclinic, space group P21/n (no. 14), a = 12.1310(3) Å, b = 15.2270(4) Å, c = 16.3851(4) Å, β = 92.206(2)°, = 3024.39(13) Å3, Z = 2, T = 99.99 K, μ(CuKα) = 0.561 mm-1, Dcalc = 1.081 g/cm3, 17423 reflections measured (7.928° ≤ 2Θ ≤ 139.972°), 5646 unique (Rint = 0.0334, Rsigma = 0.0374) which were used in all calculations. The final R1 was 0.0962 (I > 2σ(I)) and wR2 was 0.3136 (all data).

Refinement model description

Number of restraints - 73, 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,H,H) groups
2. Restrained distances
O6B-C17B
1.4 with sigma of 0.005
3. Rigid bond restraints
H19C, H19B, H19A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C10 ≈ C10A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C12 ≈ C12A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C11 ≈ C11A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C2 ≈ C2A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3 ≈ C3A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C4 ≈ C4A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C6 ≈ C6A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C8 ≈ C8A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C7 ≈ C7A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C14 ≈ C14A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C15 ≈ C15A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C16 ≈ C16A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
Sof(H5BC)=Sof(H5BD)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C7A)=Sof(H7AA)=
Sof(H7AB)=Sof(H7AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
Sof(H5AA)=Sof(H5AB)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C7)=Sof(H7A)=
Sof(H7B)=Sof(H7C)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
Sof(H13C)=Sof(H13D)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=
Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(2)
Sof(H13A)=Sof(H13B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C14)=Sof(H14A)=
Sof(H14B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(2)
Sof(H1BC)=Sof(H1BD)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C3A)=Sof(H3AA)=
Sof(H3AB)=Sof(H3AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(3)
Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=
Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(3)
Sof(H9BC)=Sof(H9BD)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11D)=
Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(4)
Sof(H9AA)=Sof(H9AB)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11)=Sof(H11A)=
Sof(H11B)=Sof(H11C)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(4)
Fixed Sof: CNT1(0)
Fixed Uiso: CNT1(0.05)
Fixed X: CNT1(0.61303)
Fixed Y: CNT1(0.313981)
Fixed Z: CNT1(0.61979)
6.a Secondary CH2 refined with riding coordinates:
C13(H13A,H13B), C13(H13C,H13D), C1(H1AA,H1AB), C1(H1BC,H1BD), C5(H5AA,H5AB),
C5(H5BC,H5BD), C9(H9AA,H9AB), C9(H9BC,H9BD), C10(H10A,H10B), C2(H2A,H2B),
C14(H14A,H14B), C6(H6A,H6B), C6A(H6AA,H6AB), C14A(H14C,H14D), C2A(H2AA,H2AB),
C10A(H10C,H10D)
6.b Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C3(H3A,H3B,
H3C), C16(H16A,H16B,H16C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C),
C8A(H8AA,H8AB,H8AC), C7A(H7AA,H7AB,H7AC), C15A(H15D,H15E,H15F), C16A(H16D,H16E,
H16F), C4A(H4AA,H4AB,H4AC), C3A(H3AA,H3AB,H3AC), C11A(H11D,H11E,H11F),
C12A(H12D,H12E,H12F), C17B(H17A,H17B,H17C), C17A(H17D,H17E,H17F)

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