mo_B0542_0ma

Table 1 Crystal data and structure refinement for mo_B0542_0ma.
Identification code mo_B0542_0ma
Empirical formula C64H143Li8N8O16
Formula weight 1336.38
Temperature/K 100.02
Crystal system monoclinic
Space group P21/c
a/Å 20.6642(12)
b/Å 19.9484(14)
c/Å 19.8692(11)
α/° 90
β/° 91.024(2)
γ/° 90
Volume/Å3 8189.1(9)
Z 4
ρcalcg/cm3 1.084
μ/mm‑1 0.074
F(000) 2940.0
Crystal size/mm3 0.64 × 0.18 × 0.12
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.518 to 54
Index ranges -25 ≤ h ≤ 26, -22 ≤ k ≤ 25, -25 ≤ l ≤ 24
Reflections collected 77683
Independent reflections 17852 [Rint = 0.0600, Rsigma = 0.0540]
Data/restraints/parameters 17852/0/917
Goodness-of-fit on F2 1.026
Final R indexes [I>=2σ (I)] R1 = 0.0681, wR2 = 0.1608
Final R indexes [all data] R1 = 0.1067, wR2 = 0.1814
Largest diff. peak/hole / e Å-3 0.59/-0.52

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0542_0ma. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C110421.4(11)7968.4(12)8366.1(11)24.6(5)
C210058.7(10)8463.2(11)7885.6(11)19.0(4)
C39583.2(11)8836.8(13)8341.2(12)29.2(5)
C410498.9(12)8995.8(13)7583.0(13)30.0(6)
C511302.0(11)7607.6(13)7648.1(12)27.5(5)
C610956.8(12)6916.8(13)8575.8(12)28.7(5)
C711179.1(12)6246.4(13)8317.7(13)31.7(6)
C812065.1(15)5629.4(15)7928.3(18)49.7(8)
C98906.0(11)8516.1(12)5436.0(12)25.3(5)
C108444.9(10)8145.0(11)5914.5(11)21.2(5)
C118002.4(13)8609.6(14)6305.7(15)40.4(7)
C127996.1(13)7725.5(14)5442.3(14)38.9(7)
C139325.5(13)9436.5(13)6118.1(14)33.9(6)
C149956.5(12)8970.8(13)5232.8(12)29.3(6)
C1510628.3(12)9128.0(14)5528.4(13)30.3(6)
C1611679.1(13)9369.5(17)5211.3(17)47.8(8)
C1710015.7(11)6450.9(12)5389.6(11)24.6(5)
C1810480.1(10)6801.6(12)5901.5(11)21.8(5)
C1910939.0(13)6312.0(14)6268.1(14)37.1(6)
C2010908.3(13)7268.9(14)5479.0(14)36.2(6)
C219626.0(13)5491.6(13)6022.8(14)36.1(6)
C228964.2(13)5977.4(15)5148.7(13)36.0(6)
C238294.8(13)5873.1(15)5430.9(14)38.0(6)
C247232.0(15)5606(2)5109(2)76.8(13)
C258503.2(11)6816.0(13)8303.0(12)28.4(5)
C268860.6(11)6352.8(12)7801.7(12)24.3(5)
C279337.3(13)5938.8(15)8244.5(15)42.3(7)
C288413.1(13)5847.7(13)7438.9(16)40.1(7)
C297606.6(11)7228.2(13)7599.9(12)27.6(5)
C307989.3(11)7859.2(13)8559.9(12)29.0(6)
C317791.0(11)8556.3(14)8334.7(13)31.5(6)
C326922.4(15)9232.9(15)7982.5(18)49.4(8)
Li110023.8(16)7166.8(18)7317.9(17)17.0(7)
Li29708.1(16)8027.2(18)6434.3(17)17.2(7)
Li39219.0(17)6871.5(18)6391.9(18)19.1(7)
Li48897.2(16)7679.3(18)7311.6(18)18.5(7)
N110738.8(8)7390.8(9)8047.2(9)18.3(4)
N29496.9(9)8815.6(9)5751.5(9)19.3(4)
N39439.3(9)6123.8(10)5678.2(9)23.3(4)
N48182.1(8)7413.8(10)8009.8(9)21.2(4)
O19720.9(7)8110.1(7)7387.0(7)15.6(3)
O211847.4(9)6255.7(10)8159.5(11)43.1(5)
O38794.9(6)7725.1(7)6343.1(7)16.1(3)
O411047.0(8)9195.1(11)4991.1(10)44.1(5)
O510125.3(7)7176.8(7)6357.9(7)16.9(3)
O67886.1(10)5670.5(15)4905.0(12)65.4(7)
O79198.5(7)6735.9(7)7341.8(7)16.5(3)
O87116.8(8)8584.6(9)8187.4(10)36.8(4)
C336466.7(11)1781.5(12)5979.3(11)24.2(5)
C346058.7(10)1339.9(11)5478.9(11)18.1(4)
C355571.0(11)972.6(13)5920.5(13)29.1(6)
C366462.3(12)801.9(13)5129.2(14)32.2(6)
C377366.4(11)2138.7(13)5285.9(12)26.2(5)
C387032.9(11)2801.9(13)6233.4(11)27.2(5)
C397280.5(11)3470.7(13)6005.1(12)27.2(5)
C408194.7(13)4082.0(13)5689.6(15)35.0(6)
C416108.0(11)3429.6(12)3060.4(12)26.2(5)
C426549.5(10)3119.9(11)3616.0(11)19.0(4)
C436864.1(14)3642.8(13)4082.3(13)35.6(6)
C447096.0(11)2761.6(12)3245.1(12)26.3(5)
C455610(2)4454.3(15)3461(2)69.3(12)
C464986.0(14)3673(2)2794.9(13)56(1)
C474320.3(19)3871(3)3053.4(17)101(2)
C494853.2(11)1455.4(15)3086.1(12)31.3(6)
C504437.5(10)1785.4(14)3636.3(12)28.2(6)
C513883.7(12)2139(2)3259.8(15)55.2(10)
C524137.4(13)1273.0(15)4117.3(15)43.9(8)
C535353.1(13)433.9(13)3524.6(14)38.2(7)
C545961.2(11)1169.1(13)2820.5(11)24.9(5)
C556619.7(11)999.0(12)3112.4(11)24.3(5)
C567710.3(12)946.3(14)2825.1(15)37.6(6)
C574611.8(10)3137.5(12)5978.1(11)20.7(5)
C584999(1)3569.0(11)5471.4(11)17.6(4)
C595499.9(11)3962.2(12)5900.1(12)25.4(5)
C604578.0(11)4091.4(12)5099.8(12)26.0(5)
C613684.6(10)2770.1(12)5293.9(11)22.8(5)
C624048.2(11)2124.5(12)6254.1(11)24.0(5)
C633810.1(11)1439.1(12)6047.9(12)25.6(5)
C642908.7(13)815.9(13)5668.3(14)34.3(6)
Li56100.4(16)2657.0(18)4972.5(17)16.7(7)
Li65302.0(17)3045.1(19)4071.0(17)18.9(7)
Li75705.3(16)1859.9(18)4070.2(17)16.1(7)
Li84941.9(16)2248.8(18)4975.6(17)17.0(7)
N56803.1(8)2352.4(9)5688.0(9)18.2(4)
N65504.4(10)3745.9(11)3307(1)31.3(5)
N75458.7(8)1140.4(9)3333.1(9)20.2(4)
N84257.6(8)2556.2(9)5693.7(8)16.8(4)
O95734.0(6)1745.6(7)5016.1(7)14.0(3)
O107952.5(8)3440.4(9)5853.7(10)33.2(4)
O116188.7(6)2669.4(7)3994.9(7)13.8(3)
O134817.3(6)2238.2(8)4003.0(7)17.3(3)
O147071.2(7)1065.9(9)2589.7(8)29.5(4)
O155311.3(7)3154.5(7)5019.2(7)15.7(3)
O163141.2(7)1453.9(8)5857.7(9)27.4(4)
C48A3501(3)4611(3)3177(3)24.9(14)
O12A3982.5(19)4074(3)2596(2)38.6(18)
C48B3360(3)4313(4)2826(4)54(2)
O12B4119.9(15)4441.2(17)2921.7(19)23.5(11)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0542_0ma. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
C118.9(11)34.0(14)20.7(11)-1.3(10)0.3(9)-2.4(10)
C213.6(10)20.0(12)23.5(11)-2.2(9)0.8(8)-2.9(8)
C323.6(12)33.9(14)30.1(13)-11.7(11)1.9(10)-3.1(10)
C425.2(12)28.1(14)36.9(14)-0.9(11)1.4(10)-8.7(10)
C515.7(11)39.0(15)27.8(12)5.5(11)4.0(9)-0.8(10)
C624.8(12)37.9(15)23.2(12)8.6(10)-2.6(9)0.5(11)
C729.6(13)31.2(14)34.1(14)10.4(11)-3.9(11)1.6(11)
C840.8(17)38.3(18)70(2)0.2(15)11.6(15)7.8(14)
C926.2(12)24.6(13)24.8(12)7.2(10)-7.2(9)-2.5(10)
C1015.1(10)20.5(12)28.0(12)6.7(9)-2.5(9)1.8(9)
C1127.3(13)32.9(15)61.6(19)13.8(14)15.9(13)9.6(12)
C1231.9(14)38.0(16)46.0(16)13.5(13)-18.1(12)-9.1(12)
C1333.9(14)26.7(14)41.1(15)-4.5(11)-0.4(11)0.0(11)
C1429.1(13)32.7(14)26.3(12)9.2(10)2.5(10)-1.4(11)
C1527.8(13)32.1(14)31.3(13)1.9(11)3.5(10)-1.8(11)
C1622.6(13)58(2)63(2)9.0(16)6.6(13)-3.1(13)
C1728.6(12)24.5(13)21.1(11)-1.3(9)7.8(9)2.2(10)
C1817.8(11)24.0(12)23.7(11)-2.1(9)8.6(9)4.5(9)
C1928.5(13)33.8(15)49.0(16)-5.0(12)-2.7(12)10.5(11)
C2036.4(14)34.9(15)38.2(14)-6.7(12)24.5(12)-4.7(12)
C2140.0(15)22.7(14)45.5(16)6.6(12)-4.2(12)-2.4(11)
C2234.7(14)41.9(16)31.4(14)1.1(12)-4.2(11)3.2(12)
C2334.3(14)36.2(16)43.3(16)6.0(12)-2.4(12)3.7(12)
C2426.6(16)93(3)110(3)22(3)-19.3(19)2.9(18)
C2520.2(11)37.7(15)27.6(12)14.0(11)8.8(10)-0.1(10)
C2617.8(11)21.6(12)33.6(13)13.4(10)7.2(9)-1.4(9)
C2735.6(15)44.6(17)47.1(17)29.0(14)14.6(13)10.0(13)
C2832.0(14)24.0(14)64.6(19)3.9(13)12.2(13)-10.8(11)
C2918.2(11)35.5(14)29.0(12)-2.5(11)3.2(9)0.6(10)
C3020.2(11)42.5(16)24.6(12)-3.6(11)6.0(9)-3(1)
C3121.2(12)39.6(16)33.7(13)-9.3(11)4.1(10)-2.1(11)
C3241.1(17)35.9(17)71(2)-7.6(15)-7.2(15)6.9(13)
Li112.5(16)19.4(19)19.2(17)3.3(14)2.9(13)2.0(14)
Li216.1(17)16.3(18)19.3(17)2.4(14)0.7(14)-1.9(14)
Li319.2(18)17.9(19)20.2(18)1.6(14)1.2(14)-1.2(14)
Li414.3(17)18.0(19)23.3(18)4.7(15)3.4(14)2.7(14)
N111.2(8)26(1)17.7(9)4.4(7)-0.3(7)0.0(7)
N221.9(9)16.9(10)19.2(9)3.8(7)-0.6(7)-4.9(7)
N328.7(10)19.1(10)22.1(10)-0.2(8)1.1(8)-1.7(8)
N411.6(8)31.5(11)20.6(9)3.1(8)3.8(7)1.9(8)
O114.0(7)15.1(8)17.5(7)-0.3(6)-0.9(6)-1.2(6)
O227.6(10)31.3(11)70.3(14)0.3(10)0.6(9)4.0(8)
O310.6(7)19.1(8)18.6(7)4.8(6)-2.4(6)0.4(6)
O423.8(9)64.3(14)44.3(11)17.8(10)5.1(8)-8.2(9)
O513.4(7)20.6(8)16.9(7)-0.7(6)4.1(6)2.5(6)
O631.8(11)106(2)57.8(14)7.4(14)-15.7(10)-5.4(12)
O713.7(7)15.9(8)20.1(7)5.8(6)4.7(6)-0.4(6)
O822.5(9)34.0(11)53.8(12)0.1(9)1.1(8)1.7(8)
C3317.9(11)33.9(14)20.7(11)7.1(10)-0.7(9)3.9(10)
C3413.6(10)18.3(11)22.4(11)7.6(9)2.5(8)2.6(8)
C3521.0(12)31.7(14)34.8(13)19.2(11)2.5(10)-1.1(10)
C3628.5(13)23.7(13)44.6(15)1.0(11)2.5(11)7.5(10)
C3716.6(11)33.8(14)28.3(12)-2.3(10)4.2(9)-0.4(10)
C3819.9(11)43.0(15)18.7(11)-4(1)-2.8(9)-0.7(10)
C3920.0(11)33.7(14)27.7(12)-7(1)-2.7(9)-0.5(10)
C4030.5(14)24.2(14)50.3(16)2.8(12)2.9(12)-2.3(11)
C4128.4(12)26.1(13)24.5(12)9.5(10)11.9(10)5.1(10)
C4217.4(10)18.7(11)21.1(11)2.7(9)7.5(8)-4.0(9)
C4344.4(16)26.5(14)35.9(14)-0.2(11)5.8(12)-18.0(12)
C4419.3(11)27.3(13)32.7(13)6(1)11.2(10)-2.3(10)
C45106(3)23.9(17)79(3)17.4(16)45(2)28.2(18)
C4647.4(18)100(3)20.6(13)26.0(15)9.7(12)41.3(18)
C4771(2)186(5)48(2)72(3)36.7(19)95(3)
C4915.4(11)54.9(17)23.6(12)-17.7(11)-1.5(9)-6.7(11)
C5010.2(10)49.5(16)25.0(12)-14.2(11)0.5(9)-4.4(10)
C5115.4(12)110(3)39.9(16)-28.9(18)-12.2(11)15.3(15)
C5230.5(14)50.4(18)51.6(17)-27.8(14)23.9(13)-22.7(13)
C5340.4(15)27.1(14)47.7(16)-12.9(12)22.0(13)-17.4(12)
C5420.8(11)34.7(14)19.4(11)-4.1(10)7.5(9)-3.5(10)
C5521.0(11)27.9(13)24.3(12)3.4(10)10.1(9)0(1)
C5621.3(12)37.3(16)54.4(17)1.3(13)11.7(12)4.4(11)
C5716.8(10)27.5(13)18(1)-4.3(9)2.2(8)4.5(9)
C5814.3(10)17.6(11)21.1(11)-5.4(9)1.1(8)4.1(8)
C5922.4(11)24.4(13)29.5(12)-9.5(10)0.9(9)3.2(10)
C6021.9(12)21.3(12)34.6(13)-2.3(10)-1.1(10)5.4(9)
C6112(1)32.2(13)24.2(11)6.6(10)0.9(9)4.5(9)
C6220.2(11)33.2(14)18.6(11)5.0(9)3.9(9)2.8(10)
C6319.9(11)28.7(13)28.3(12)8(1)4.5(9)4(1)
C6429.7(13)24.9(14)48.3(16)0.3(12)1.2(12)2.5(11)
Li514.1(16)18.4(19)17.8(17)-0.5(14)1.1(13)0.9(14)
Li616.7(17)22(2)18.5(17)4.1(14)3.0(14)6.0(15)
Li713.0(16)17.3(18)18.0(17)-2.0(14)1.3(13)-1.3(14)
Li811.6(16)21.5(19)17.9(17)-0.7(14)2.4(13)0.6(14)
N511.3(8)26.5(10)16.7(9)-2.5(7)-1.7(7)0.4(7)
N638.3(12)29.9(12)26.2(11)13.2(9)11.5(9)18.6(10)
N715.6(9)23.4(10)22.0(9)-8.1(8)7.7(7)-6.4(7)
N810.0(8)26(1)14.3(8)2.1(7)1.4(7)2.0(7)
O911.1(7)15.2(7)15.6(7)3.3(6)0.6(5)1.4(5)
O1019.0(8)24.1(9)56.5(12)5.0(8)-1.7(8)0.5(7)
O1112.0(7)13.9(7)15.7(7)3.2(6)4.1(5)-1.9(6)
O139.0(7)27.1(9)15.7(7)-1.9(6)-1.0(5)-0.8(6)
O1419.1(8)39.4(11)30.4(9)-0.2(8)12.5(7)0.1(7)
O1515.1(7)15.3(8)16.7(7)-1.7(6)5.4(6)2.4(6)
O1618.7(8)21.9(9)41.8(10)-2.0(7)2.9(7)3.3(7)
C48A8(2)25(3)41(4)1(3)2(2)3(2)
O12A19(2)60(4)37(3)17(3)-5.0(18)7(2)
C48B21(3)70(5)72(5)32(4)1(3)10(3)
O12B21.6(16)16.2(19)33(2)7.3(15)6.9(14)0.0(13)

 

Table 4 Bond Lengths for mo_B0542_0ma.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.556(3) C33N51.459(3)
C1N11.474(3) C34C351.534(3)
C2C31.540(3) C34C361.533(3)
C2C41.529(3) C34O91.389(2)
C2O11.393(2) C37N51.486(3)
C5N11.484(3) C38C391.502(4)
C6C71.507(4) C38N51.478(3)
C6N11.477(3) C39O101.427(3)
C7O21.422(3) C40O101.415(3)
C8O21.408(3) C41C421.548(3)
C9C101.547(3) C41N61.489(3)
C9N21.488(3) C42C431.532(3)
C10C111.525(3) C42C441.536(3)
C10C121.552(3) C42O111.396(2)
C10O31.389(2) C45N61.461(4)
C13N21.483(3) C46C471.529(4)
C14C151.530(3) C46N61.471(4)
C14N21.447(3) C47O12A1.207(5)
C15O41.392(3) C47O12B1.238(5)
C16O41.414(3) C49C501.549(3)
C17C181.552(3) C49N71.476(3)
C17N31.482(3) C50C511.528(4)
C18C191.536(3) C50C521.537(4)
C18C201.544(3) C50O131.394(3)
C18O51.394(2) C53N71.477(3)
C21N31.483(3) C54C551.508(3)
C22C231.516(4) C54N71.469(3)
C22N31.456(3) C55O141.415(3)
C23O61.392(3) C56O141.413(3)
C24O61.424(4) C57C581.557(3)
C25C261.555(3) C57N81.478(3)
C25N41.479(3) C58C591.543(3)
C26C271.548(3) C58C601.538(3)
C26C281.538(4) C58O151.388(2)
C26O71.389(2) C61N81.477(3)
C29N41.476(3) C62C631.507(3)
C30C311.515(4) C62N81.479(3)
C30N41.469(3) C63O161.427(3)
C31O81.420(3) C64O161.409(3)
C32O81.412(3) Li5Li62.535(5)
Li1Li22.532(5) Li5Li72.521(5)
Li1Li32.528(5) Li5Li82.529(5)
Li1Li42.542(5) Li5N52.104(4)
Li1N12.099(4) Li5O91.972(4)
Li1O11.989(4) Li5O111.954(4)
Li1O51.923(4) Li5O151.913(4)
Li1O71.911(4) Li6Li72.507(5)
Li2Li32.518(5) Li6Li82.521(5)
Li2Li42.536(5) Li6N62.111(4)
Li2N22.117(4) Li6O111.988(4)
Li2O11.900(4) Li6O131.899(4)
Li2O31.986(4) Li6O151.896(4)
Li2O51.910(4) Li7Li82.535(5)
Li3Li42.534(5) Li7N72.107(4)
Li3N32.113(4) Li7O91.893(4)
Li3O31.917(4) Li7O111.906(4)
Li3O51.972(4) Li7O131.986(4)
Li3O71.908(4) Li8N82.117(4)
Li4N42.112(4) Li8O91.921(4)
Li4O11.910(4) Li8O131.945(4)
Li4O31.934(4) Li8O151.963(4)
Li4O71.983(4) C48AO12A1.876(9)
C33C341.564(3) C48BO12B1.599(7)

 

Table 5 Bond Angles for mo_B0542_0ma.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
N1C1C2116.43(18) C35C34C33104.93(18)
C3C2C1104.58(18) C36C34C33113.01(18)
C4C2C1113.50(18) C36C34C35107.04(19)
C4C2C3106.57(19) O9C34C33109.96(17)
O1C2C1110.19(18) O9C34C35110.03(17)
O1C2C3110.23(17) O9C34C36111.60(18)
O1C2C4111.46(18) N5C38C39115.10(19)
N1C6C7114.6(2) O10C39C38111.3(2)
O2C7C6111.5(2) N6C41C42114.90(18)
N2C9C10116.31(18) C43C42C41113.4(2)
C9C10C12104.75(19) C43C42C44107.42(19)
C11C10C9113.8(2) C44C42C41105.81(18)
C11C10C12106.2(2) O11C42C41109.13(17)
O3C10C9110.23(17) O11C42C43109.69(18)
O3C10C11111.38(19) O11C42C44111.32(18)
O3C10C12110.15(18) N6C46C47113.0(3)
N2C14C15111.90(19) O12AC47C46110.2(3)
O4C15C14107.3(2) O12BC47C46117.8(4)
N3C17C18115.87(18) N7C49C50115.07(18)
C19C18C17113.2(2) C51C50C49105.7(2)
C19C18C20106.7(2) C51C50C52107.7(2)
C20C18C17105.64(19) C52C50C49113.0(2)
O5C18C17110.00(17) O13C50C49109.27(17)
O5C18C19111.12(19) O13C50C51111.5(2)
O5C18C20110.04(19) O13C50C52109.60(19)
N3C22C23111.6(2) N7C54C55111.64(18)
O6C23C22107.9(2) O14C55C54107.38(18)
N4C25C26116.20(18) N8C57C58116.31(17)
C27C26C25104.9(2) C59C58C57105.76(17)
C28C26C25113.6(2) C60C58C57113.10(17)
C28C26C27106.7(2) C60C58C59106.78(18)
O7C26C25110.16(18) O15C58C57109.84(17)
O7C26C27110.19(18) O15C58C59110.18(17)
O7C26C28110.9(2) O15C58C60111.00(17)
N4C30C31114.3(2) N8C62C63114.96(18)
O8C31C30110.9(2) O16C63C62111.30(19)
Li2Li1Li459.97(13) Li7Li5Li659.45(14)
Li3Li1Li259.69(14) Li7Li5Li860.27(13)
Li3Li1Li459.97(14) Li8Li5Li659.72(14)
N1Li1Li2120.25(18) N5Li5Li6177.0(2)
N1Li1Li3176.4(2) N5Li5Li7120.61(18)
N1Li1Li4123.44(18) N5Li5Li8123.19(18)
O1Li1Li247.86(12) O9Li5Li693.85(16)
O1Li1Li393.84(16) O9Li5Li747.94(12)
O1Li1Li447.97(12) O9Li5Li848.61(12)
O1Li1N188.25(16) O9Li5N587.99(15)
O5Li1Li248.43(12) O11Li5Li650.58(12)
O5Li1Li350.38(12) O11Li5Li748.40(12)
O5Li1Li496.14(16) O11Li5Li896.41(16)
O5Li1N1126.49(18) O11Li5N5126.85(18)
O5Li1O195.66(16) O11Li5O995.63(16)
O7Li1Li295.92(16) O15Li5Li648.01(12)
O7Li1Li348.50(12) O15Li5Li795.53(16)
O7Li1Li450.47(12) O15Li5Li850.13(12)
O7Li1N1134.11(19) O15Li5N5134.10(19)
O7Li1O198.15(16) O15Li5O998.51(16)
O7Li1O598.19(17) O15Li5O1197.85(16)
Li1Li2Li460.21(13) Li7Li6Li560.01(13)
Li3Li2Li160.06(14) Li7Li6Li860.57(14)
Li3Li2Li460.18(14) Li8Li6Li560.03(13)
N2Li2Li1174.4(2) N6Li6Li5125.14(19)
N2Li2Li3125.49(18) N6Li6Li7123.63(18)
N2Li2Li4120.83(18) N6Li6Li8174.14(19)
O1Li2Li150.90(12) O11Li6Li549.41(12)
O1Li2Li396.39(16) O11Li6Li748.51(12)
O1Li2Li448.44(12) O11Li6Li895.79(16)
O1Li2N2124.95(19) O11Li6N690.01(15)
O1Li2O396.52(16) O13Li6Li597.30(17)
O1Li2O599.10(17) O13Li6Li751.36(12)
O3Li2Li195.17(16) O13Li6Li849.81(12)
O3Li2Li348.62(12) O13Li6N6128.4(2)
O3Li2Li448.80(12) O13Li6O1199.24(17)
O3Li2N288.99(15) O15Li6Li548.56(12)
O5Li2Li148.86(12) O15Li6Li796.42(16)
O5Li2Li350.63(12) O15Li6Li850.37(12)
O5Li2Li496.67(16) O15Li6N6129.8(2)
O5Li2N2134.18(19) O15Li6O1197.24(16)
O5Li2O398.78(17) O15Li6O1399.45(17)
Li1Li3Li460.30(14) Li5Li7Li860.01(13)
Li2Li3Li160.25(14) Li6Li7Li560.54(14)
Li2Li3Li460.27(14) Li6Li7Li859.99(14)
N3Li3Li1120.40(18) N7Li7Li5174.43(19)
N3Li3Li2125.27(18) N7Li7Li6124.52(18)
N3Li3Li4174.4(2) N7Li7Li8123.77(17)
O3Li3Li197.13(17) O9Li7Li550.66(12)
O3Li3Li251.04(12) O9Li7Li696.74(16)
O3Li3Li449.15(12) O9Li7Li848.80(12)
O3Li3N3134.18(19) O9Li7N7127.66(19)
O3Li3O599.07(17) O9Li7O1199.95(16)
O5Li3Li148.69(12) O9Li7O1397.18(16)
O5Li3Li248.50(12) O11Li7Li550.06(12)
O5Li3Li495.16(16) O11Li7Li651.37(12)
O5Li3N388.79(16) O11Li7Li897.47(16)
O7Li3Li148.62(12) O11Li7N7130.03(19)
O7Li3Li296.47(17) O11Li7O1399.07(17)
O7Li3Li450.66(12) O13Li7Li595.46(16)
O7Li3N3124.9(2) O13Li7Li648.32(12)
O7Li3O399.08(18) O13Li7Li849.13(11)
O7Li3O596.64(16) O13Li7N790.02(14)
Li2Li4Li159.82(13) Li5Li8Li759.72(13)
Li3Li4Li159.72(14) Li6Li8Li560.26(14)
Li3Li4Li259.56(14) Li6Li8Li759.45(14)
N4Li4Li1123.18(18) N8Li8Li5123.51(18)
N4Li4Li2176.89(19) N8Li8Li6120.47(18)
N4Li4Li3120.65(19) N8Li8Li7176.58(19)
O1Li4Li150.65(12) O9Li8Li550.38(12)
O1Li4Li248.09(12) O9Li8Li695.57(16)
O1Li4Li395.61(16) O9Li8Li747.87(12)
O1Li4N4134.0(2) O9Li8N8134.59(19)
O1Li4O397.94(17) O9Li8O1397.67(16)
O1Li4O798.39(16) O9Li8O1598.56(16)
O3Li4Li196.18(16) O13Li8Li596.29(16)
O3Li4Li250.59(12) O13Li8Li648.25(12)
O3Li4Li348.55(12) O13Li8Li750.56(12)
O3Li4N4126.86(19) O13Li8N8126.48(18)
O3Li4O795.95(17) O13Li8O1595.65(17)
O7Li4Li148.03(12) O15Li8Li548.41(12)
O7Li4Li293.99(16) O15Li8Li648.08(12)
O7Li4Li348.09(12) O15Li8Li793.82(16)
O7Li4N488.00(15) O15Li8N888.14(15)
C1N1C5111.16(18) C33N5C37111.87(18)
C1N1C6109.08(17) C33N5C38109.38(17)
C1N1Li198.63(16) C33N5Li599.52(15)
C5N1Li1104.02(16) C37N5Li5104.91(16)
C6N1C5109.53(17) C38N5C37108.89(17)
C6N1Li1123.81(18) C38N5Li5121.93(17)
C9N2Li297.46(15) C41N6Li697.70(16)
C13N2C9109.94(18) C45N6C41110.9(2)
C13N2Li2110.73(17) C45N6C46110.2(3)
C14N2C9109.26(17) C45N6Li6121.4(2)
C14N2C13109.67(19) C46N6C41109.5(2)
C14N2Li2118.99(17) C46N6Li6106.3(2)
C17N3C21110.42(19) C49N7C53111.3(2)
C17N3Li397.65(16) C49N7Li797.71(16)
C21N3Li3110.36(18) C53N7Li7120.40(18)
C22N3C17110.17(19) C54N7C49111.01(18)
C22N3C21109.2(2) C54N7C53108.98(18)
C22N3Li3118.42(18) C54N7Li7106.88(16)
C25N4Li498.43(16) C57N8C62108.57(16)
C29N4C25111.49(19) C57N8Li898.79(15)
C29N4Li4105.47(16) C61N8C57111.45(18)
C30N4C25108.67(18) C61N8C62109.31(16)
C30N4C29109.61(17) C61N8Li8105.07(15)
C30N4Li4122.63(18) C62N8Li8123.15(17)
C2O1Li1111.92(16) C34O9Li5112.64(15)
C2O1Li2138.63(17) C34O9Li7137.20(16)
C2O1Li4135.87(17) C34O9Li8137.19(16)
Li2O1Li181.24(15) Li7O9Li581.41(15)
Li2O1Li483.47(16) Li7O9Li883.33(15)
Li4O1Li181.37(15) Li8O9Li581.01(15)
C8O2C7112.2(2) C40O10C39111.09(19)
C10O3Li2110.88(16) C42O11Li5127.17(16)
C10O3Li3143.10(17) C42O11Li6107.47(16)
C10O3Li4133.24(17) C42O11Li7150.81(17)
Li3O3Li280.34(16) Li5O11Li680.01(15)
Li3O3Li482.30(16) Li7O11Li581.54(15)
Li4O3Li280.61(15) Li7O11Li680.12(16)
C15O4C16111.7(2) C50O13Li6151.38(18)
C18O5Li1135.04(17) C50O13Li7107.45(16)
C18O5Li2140.51(17) C50O13Li8126.14(18)
C18O5Li3111.55(17) Li6O13Li780.32(15)
Li1O5Li380.93(15) Li6O13Li881.94(16)
Li2O5Li182.70(16) Li8O13Li780.31(15)
Li2O5Li380.87(16) C56O14C55111.45(19)
C23O6C24112.3(3) C58O15Li5138.32(16)
C26O7Li1136.30(17) C58O15Li6135.63(16)
C26O7Li3138.52(18) C58O15Li8113.07(16)
C26O7Li4112.38(16) Li5O15Li881.45(15)
Li1O7Li481.50(15) Li6O15Li583.43(15)
Li3O7Li182.88(16) Li6O15Li881.55(16)
Li3O7Li481.26(16) C64O16C63112.09(18)
C32O8C31111.7(2) C47O12AC48A91.9(5)
N5C33C34116.28(17) C47O12BC48B101.7(4)

 

Table 6 Torsion Angles for mo_B0542_0ma.
ABCDAngle/˚ ABCDAngle/˚
C1C2O1Li1-16.4(2) C41C42O11Li6-36.2(2)
C1C2O1Li2-118.4(2) C41C42O11Li765.0(4)
C1C2O1Li484.2(3) C42C41N6C4590.2(3)
C2C1N1C569.0(2) C42C41N6C46-148.0(2)
C2C1N1C6-170.16(18) C42C41N6Li6-37.6(2)
C2C1N1Li1-39.8(2) C43C42O11Li5-2.0(3)
C3C2O1Li1-131.28(19) C43C42O11Li688.6(2)
C3C2O1Li2126.7(2) C43C42O11Li7-170.2(3)
C3C2O1Li4-30.8(3) C44C42O11Li5116.7(2)
C4C2O1Li1110.6(2) C44C42O11Li6-152.67(18)
C4C2O1Li28.6(3) C44C42O11Li7-51.4(4)
C4C2O1Li4-148.9(2) C46C47O12AC48A-152.7(4)
C6C7O2C8179.0(2) C46C47O12BC48B145.3(5)
C7C6N1C1169.30(19) C47C46N6C41169.8(3)
C7C6N1C5-68.8(3) C47C46N6C45-68.0(4)
C7C6N1Li154.3(3) C47C46N6Li665.2(4)
C9C10O3Li223.0(2) C49C50O13Li666.9(4)
C9C10O3Li3-79.1(3) C49C50O13Li7-35.2(2)
C9C10O3Li4119.8(2) C49C50O13Li8-125.8(2)
C10C9N2C13-75.7(2) C50C49N7C5388.9(3)
C10C9N2C14163.9(2) C50C49N7C54-149.5(2)
C10C9N2Li239.6(2) C50C49N7Li7-38.1(2)
C11C10O3Li2-104.4(2) C51C50O13Li6-49.6(4)
C11C10O3Li3153.5(3) C51C50O13Li7-151.6(2)
C11C10O3Li4-7.6(3) C51C50O13Li8117.7(2)
C12C10O3Li2138.1(2) C52C50O13Li6-168.8(3)
C12C10O3Li336.0(4) C52C50O13Li789.2(2)
C12C10O3Li4-125.1(2) C52C50O13Li8-1.4(3)
C14C15O4C16177.5(2) C54C55O14C56177.2(2)
C15C14N2C9-166.9(2) C55C54N7C49166.8(2)
C15C14N2C1372.5(3) C55C54N7C53-70.2(2)
C15C14N2Li2-56.3(3) C55C54N7Li761.3(2)
C17C18O5Li1119.4(2) C57C58O15Li5-84.4(3)
C17C18O5Li2-81.7(3) C57C58O15Li6121.1(2)
C17C18O5Li320.5(2) C57C58O15Li819.2(2)
C18C17N3C21-74.6(2) C58C57N8C61-72.3(2)
C18C17N3C22164.7(2) C58C57N8C62167.21(17)
C18C17N3Li340.5(2) C58C57N8Li837.7(2)
C19C18O5Li1-6.7(3) C59C58O15Li531.7(3)
C19C18O5Li2152.2(2) C59C58O15Li6-122.8(2)
C19C18O5Li3-105.6(2) C59C58O15Li8135.29(19)
C20C18O5Li1-124.6(2) C60C58O15Li5149.7(2)
C20C18O5Li234.3(3) C60C58O15Li6-4.7(3)
C20C18O5Li3136.5(2) C60C58O15Li8-106.6(2)
C22C23O6C24-175.8(3) C62C63O16C64-179.5(2)
C23C22N3C17-160.2(2) C63C62N8C57-167.22(18)
C23C22N3C2178.3(3) C63C62N8C6171.0(2)
C23C22N3Li3-49.1(3) C63C62N8Li8-52.9(3)
C25C26O7Li184.1(3) Li5Li6O13C50-150.4(3)
C25C26O7Li3-120.0(3) Li5Li6O13Li7-41.61(15)
C25C26O7Li4-17.4(2) Li5Li6O13Li839.86(16)
C26C25N4C2970.6(2) Li5Li6O15C58163.2(3)
C26C25N4C30-168.47(19) Li5Li6O15Li8-82.29(15)
C26C25N4Li4-39.8(2) Li5Li7O9C34-114.2(2)
C27C26O7Li1-31.2(3) Li5Li7O9Li881.87(15)
C27C26O7Li3124.7(3) Li6Li7O9C34-156.7(2)
C27C26O7Li4-132.7(2) Li6Li7O9Li5-42.49(15)
C28C26O7Li1-149.2(2) Li6Li7O9Li839.38(16)
C28C26O7Li36.8(3) Li7Li6O13C50-108.8(4)
C28C26O7Li4109.3(2) Li7Li6O13Li881.47(15)
C30C31O8C32179.4(2) Li7Li6O15C58-157.2(2)
C31C30N4C25167.07(19) Li7Li6O15Li539.62(16)
C31C30N4C29-70.9(2) Li7Li6O15Li8-42.67(16)
C31C30N4Li453.5(3) Li8Li6O13C50169.7(4)
Li1Li2O1C2113.4(3) Li8Li6O13Li7-81.47(15)
Li1Li2O1Li4-82.23(15) Li8Li6O15C58-114.5(2)
Li3Li2O1C2155.8(2) Li8Li6O15Li582.29(15)
Li3Li2O1Li142.42(16) Li8Li7O9C34163.9(3)
Li3Li2O1Li4-39.81(16) Li8Li7O9Li5-81.87(15)
Li4Li2O1C2-164.4(3) N5C33C34C35-158.82(19)
Li4Li2O1Li182.23(15) N5C33C34C3684.9(2)
N1C1C2C3159.55(19) N5C33C34O9-40.5(2)
N1C1C2C4-84.7(2) N5C38C39O10-87.7(2)
N1C1C2O141.1(2) N6C41C42C43-68.4(3)
N1C6C7O287.7(2) N6C41C42C44174.1(2)
N2C9C10C1180.0(3) N6C41C42O1154.2(3)
N2C9C10C12-164.5(2) N6C46C47O12A151.2(5)
N2C9C10O3-46.0(3) N6C46C47O12B97.7(4)
N2C14C15O4173.5(2) N6Li6O13C50-3.1(5)
N2Li2O1C2-61.9(3) N6Li6O13Li7105.7(2)
N2Li2O1Li1-175.3(2) N6Li6O13Li8-172.8(2)
N2Li2O1Li4102.5(2) N6Li6O15C5857.9(4)
N3C17C18C1980.1(2) N6Li6O15Li5-105.3(3)
N3C17C18C20-163.5(2) N6Li6O15Li8172.4(3)
N3C17C18O5-44.8(3) N7C49C50C51174.0(2)
N3C22C23O6-174.1(2) N7C49C50C52-68.4(3)
N4C25C26C27160.4(2) N7C49C50O1353.9(3)
N4C25C26C28-83.3(3) N7C54C55O14-177.73(19)
N4C25C26O741.8(3) N7Li7O9C3459.0(3)
N4C30C31O890.2(2) N7Li7O9Li5173.2(2)
O3Li2O1C2-155.3(2) N7Li7O9Li8-104.9(2)
O3Li2O1Li191.37(16) N8C57C58C59-160.29(17)
O3Li2O1Li49.14(16) N8C57C58C6083.2(2)
O5Li2O1C2104.7(2) N8C57C58O15-41.4(2)
O5Li2O1Li1-8.64(16) N8C62C63O16-85.3(2)
O5Li2O1Li4-90.87(17) O11Li6O13C50-100.5(3)
C33C34O9Li517.8(2) O11Li6O13Li78.32(15)
C33C34O9Li7120.0(2) O11Li6O13Li889.79(16)
C33C34O9Li8-83.8(3) O11Li6O15C58153.96(19)
C34C33N5C37-72.5(2) O11Li6O15Li5-9.25(16)
C34C33N5C38166.73(18) O11Li6O15Li8-91.54(17)
C34C33N5Li537.9(2) O11Li7O9C34-104.8(2)
C35C34O9Li5132.89(19) O11Li7O9Li59.38(16)
C35C34O9Li7-124.9(2) O11Li7O9Li891.25(17)
C35C34O9Li831.3(3) O13Li6O15C58-105.4(2)
C36C34O9Li5-108.4(2) O13Li6O15Li591.43(17)
C36C34O9Li7-6.2(3) O13Li6O15Li89.14(16)
C36C34O9Li8149.9(2) O13Li7O9C34154.61(19)
C38C39O10C40-175.4(2) O13Li7O9Li5-91.19(16)
C39C38N5C33-169.35(19) O13Li7O9Li8-9.32(16)
C39C38N5C3768.1(2) O15Li6O13C50160.5(3)
C39C38N5Li5-54.1(3) O15Li6O13Li7-90.68(17)
C41C42O11Li5-126.8(2) O15Li6O13Li8-9.21(16)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0542_0ma.
AtomxyzU(eq)
H1A107558224862229
H1B101087795869529
H3A93419169807444
H3B98259065870344
H3C92818515853644
H4A107718789724145
H4B107749190793945
H4C102339349737545
H5A111487830723541
H5B115637215753141
H5C115677921791441
H6A105966843888934
H6B113177125883634
H7A111025899866338
H7B109226126791038
H8A118115497752975
H8B120135293828375
H8C125235662781375
H9A90438197508530
H9B86598878520830
H11A76548347650661
H11B78158946600061
H11C82538834666361
H12A82597420517458
H12B77528026514258
H12C76947465571358
H13A90479717583051
H13B97219683623851
H13C90959319652951
H14A97999361497035
H14B99888585492235
H15A106179549579236
H15B107758761582936
H16A119529443482072
H16B118619005548772
H16C116629781548072
H17A98666788505630
H17B102656108514430
H19A112796565650756
H19B111376012594056
H19C106946047659256
H20A106337585522754
H20B111597001516354
H20C112047518577854
H21A99205237573854
H21B92385224610554
H21C98435596645354
H22A90975569490543
H22B89516353482343
H23A83095526578746
H23B81356296563046
H24A695754994717115
H24B708860285309115
H24C720152455442115
H25A81726546853434
H25B88206969865034
H27A95895640795863
H27B90945672856863
H27C96316243848863
H28A81436084710560
H28B81365628776860
H28C86755509721260
H29A77447008718641
H29B73597633748641
H29C73356921785641
H30A83557898888635
H30B76237651879735
H31A79008883869438
H31B80348681792938
H32A71429353756774
H32B70379557833674
H32C64539239790374
H33A61751951633029
H33B67921491620529
H35A52951301614444
H35B5804706626044
H35C5302677563944
H36A6173483489948
H36B6728564546548
H36C67431015480048
H37A76281818554739
H37B76312531517839
H37C72121927486839
H38A73832572648933
H38B66722878654633
H39A70333616560033
H39B72123807636333
H40A79744247528252
H40B86614052561152
H40C81174392606252
H41A63593772281631
H41B59883074273431
H43A65343838437253
H43B70603997381153
H43C72003428436253
H44A73812536357339
H44B73463091299239
H44C69102430293439
H45A594744973811104
H45B520646523621104
H45C574646893054104
H46A49713201264267
H46B50893955240167
H47419138383509121
H47A406935663307121
H49A45881110285338
H49B49631801275038
H51A36182382358283
H51B36171805302283
H51C40622455293483
H52A44781081440966
H52B3929914385566
H52C38151496439566
H53A5229174312457
H53B5007409385557
H53C5753250372257
H54A59731625262530
H54B5852850245430
H55A67311307348729
H55B6623534328729
H56A8006954244556
H56B7732507304556
H56C78361295314956
H57A49172972633025
H57B42963432620225
H59A57923647613038
H59B52754233623438
H59C57514256560838
H60A48564394484539
H60B43324350542839
H60C42773863479039
H61A34082381520034
H61B38242967486934
H61C34413104554834
H62A36982357649529
H62B44162069657529
H63A40661275566531
H63B38751123642731
H64A3149653528051
H64B2448847554851
H64C2967504604551
H48A35145078302437
H48B36864582363437
H48C30514456317837
H48D32674169236381
H48E31244729291881
H48F32233963313981

 

Table 8 Atomic Occupancy for mo_B0542_0ma.
AtomOccupancy AtomOccupancy AtomOccupancy
H470.455(7) H47A0.545(7) C48A0.455(7)
H48A0.455(7) H48B0.455(7) H48C0.455(7)
O12A0.455(7) C48B0.545(7) H48D0.545(7)
H48E0.545(7) H48F0.545(7) O12B0.545(7)

Experimental

Single crystals of C64H143Li8N8O16 [mo_B0542_0ma] were []. A suitable crystal was selected and [] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 100.02 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 [mo_B0542_0ma]

Crystal Data for C64H143Li8N8O16 (=1336.38 g/mol): monoclinic, space group P21/c (no. 14), a = 20.6642(12) Å, b = 19.9484(14) Å, c = 19.8692(11) Å, β = 91.024(2)°, = 8189.1(9) Å3, Z = 4, T = 100.02 K, μ(MoKα) = 0.074 mm-1, Dcalc = 1.084 g/cm3, 77683 reflections measured (4.518° ≤ 2Θ ≤ 54°), 17852 unique (Rint = 0.0600, Rsigma = 0.0540) which were used in all calculations. The final R1 was 0.0681 (I > 2σ(I)) and wR2 was 0.1814 (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. Others
Sof(H47A)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(O12B)=1-FVAR(1)
Sof(H47)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(O12A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C14(H14A,H14B), C15(H15A,
H15B), C17(H17A,H17B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B),
C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C38(H38A,H38B), C39(H39A,H39B),
C41(H41A,H41B), C46(H46A,H46B), C49(H49A,H49B), C54(H54A,H54B), C55(H55A,
H55B), C57(H57A,H57B), C62(H62A,H62B), C63(H63A,H63B)
3.b Aromatic/amide H refined with riding coordinates:
C47(H47), C47(H47A)
3.c Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C11(H11A,
H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C),
C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,
H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,
H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,
H45C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C56(H56A,
H56B,H56C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
C64(H64A,H64B,H64C), C48A(H48A,H48B,H48C), C48B(H48D,H48E,H48F)

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