Zn(asp)

Crystal submitted by:
Crystal submitted on:
Data collected on:
Structure solved by:
Table 1 Crystal data and structure refinement for Zn(asp)
Identification code Zn(asp)
Empirical formula C12H17N3O13Zn3
Formula weight 607.40
Temperature/K 100(2)
Crystal system Monoclinic
Space group P21
a/Å, b/Å, c/Å 8.484(3), 10.491(3), 10.187(3)
α/°, β/°, γ/° 90.00, 93.552(7), 90.00
Volume/Å3 905.0(5)
Z 2
ρcalcmg/mm3 2.247
m/mm‑1 4.025
F(000) 611
Crystal size/mm3 0.20 × 0.10 × 0.10
Theta range for data collection 1.94 to 27.46°
Index ranges -10 ≤ h ≤ 2, -12 ≤ k ≤ 13, -12 ≤ l ≤ 11
Reflections collected 2561
Independent reflections 2432[R(int) = 0.0272]
Data/restraints/parameters 2432/170/277
Goodness-of-fit on F2 1.063
Final R indexes [I>2σ (I)] R1 = 0.0599, wR2 = 0.1309
Final R indexes [all data] R1 = 0.0799, wR2 = 0.1400
Largest diff. peak/hole / e Å-3 1.220/-1.300

Table 2 Atomic Coordinates (Å×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for Zn(asp). Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn18498.9(17)3872(14)2717.1(17)14.6(5)
Zn29632.9(17)4619(13)8090.1(16)15.4(5)
Zn35925.8(17)1142(14)5420.5(18)16.1(5)
O17051(10)5320(9)3234(10)19(3)
O26186(10)7049(9)4179(10)20(3)
O310193(10)7033(9)7623(10)19(3)
O48617(10)5644(8)6649(10)16(3)
O58644(11)2948(8)8309(10)18(3)
O67412(10)2468(8)6394(9)14(3)
O710550(10)-41(8)10032(10)19(3)
O89714(10)-117(8)7967(9)15(3)
O97951(10)125(8)4285(9)14.9(19)
O108137(10)-668(8)2256(10)18(3)
O116721(12)2882(9)1839(11)24(3)
O126125(11)2444(9)3854(11)21(3)
N110441(12)8502(10)5504(13)18(4)
N26453(13)229(10)7229(12)19(4)
N34851(12)-192(11)4192(11)17(3)
C17293(15)6370(13)3848(15)17(3)
C28910(15)6822(14)4171(15)20(3)
C39151(15)7551(12)5488(15)18(3)
C49364(15)6700(13)6657(15)17(3)
C57716(14)2263(12)7561(14)13(3)
C66912(14)1164(13)8223(13)15(3)
C77883(14)672(13)9442(15)14(3)
C89510(14)136(13)9132(15)15(3)
C97389(14)-256(13)3198(14)16(3)
C105599(14)-202(14)2959(15)21(3)
C115169(15)1042(14)2144(15)21(3)
C126035(15)2184(14)2666(16)21(3)
O1WA3070(3)2230(2)9560(2)72(7)
O1WB2270(9)2480(7)10240(8)74(10)
Table 3 Anisotropic Displacement Parameters (Å2×103) for Zn(asp). The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
Zn18.6(7)12.8(8)22.6(10)0.3(8)1.8(6)-1.7(7)
Zn210.8(7)13.7(8)21.5(10)-0.4(8)0(7)-0.8(7)
Zn37(7)11.7(8)29.5(11)0.4(8)-0.5(7)-0.3(6)
O18(4)19(4)31(6)-5(4)-1(4)4(4)
O216(4)18(5)27(6)-2(4)10(4)0(4)
O317(5)15(5)25(5)-2(4)-1(4)0(4)
O414(4)8(4)26(5)-3(4)-4(4)3(3)
O517(4)13(4)24(5)10(4)-1(4)-6(4)
O611(4)13(4)18(5)1(4)-1(4)0(3)
O714(4)17(5)26(5)-3(4)-6(4)5(4)
O89(4)16(5)19(4)-4(4)-1(3)3(4)
O1019(4)6(4)29(5)-1(4)0(4)7(3)
O1123(5)22(5)26(5)0(4)5(4)-1(4)
O1220(4)14(4)28(5)-1(4)5(4)-6(4)
N18(5)10(6)38(8)-9(6)13(5)0(4)
N212(5)12(6)32(8)-3(6)-6(5)-7(5)
N310(5)19(6)20(7)-1(6)-6(5)5(5)
C111(4)15(5)26(6)-3(4)2(4)2(4)
C212(5)19(5)30(6)0(5)-1(5)1(4)
C311(5)12(5)31(6)0(4)-1(5)2(4)
C413(5)11(4)26(5)-6(4)2(4)1(4)
C510(4)6(4)22(5)4(4)2(4)0(4)
C615(4)6(5)24(6)5(5)9(4)1(4)
C77(4)9(5)26(6)3(5)5(4)2(4)
C87(4)14(5)23(5)-2(5)0(4)1(4)
C913(4)8(5)29(5)2(5)8(4)4(4)
C1013(5)16(5)34(7)-4(5)9(5)1(5)
C1114(5)22(5)28(6)-3(5)12(5)5(4)
C1215(5)20(5)29(5)0(5)9(4)0(4)
Table 4 Bond Lengths for Zn(asp).
AtomAtomLength/ÅAtomAtomLength/Å
Zn1O12.043(9)O5C51.282(16)
Zn1O312.263(9)O6C51.220(17)
Zn1O822.010(9)O7C81.246(17)
Zn1O111.997(10)O8C81.239(18)
Zn1N112.010(13)O9C91.244(17)
Zn2O32.626(10)O10C91.259(17)
Zn2O41.974(10)O11C121.283(18)
Zn2O51.962(9)O12C121.24(2)
Zn2O731.962(10)N1C31.480(16)
Zn2O1021.969(9)N2C61.446(18)
Zn3O242.091(9)N3C101.442(18)
Zn3O62.087(9)C1C21.469(18)
Zn3O92.382(9)C2C31.55(2)
Zn3O122.115(11)C3C41.49(2)
Zn3N22.100(12)C5C61.519(18)
Zn3N32.053(11)C6C71.536(19)
O1C11.277(17)C7C81.541(17)
O2C11.242(16)C9C101.524(17)
O3C41.225(17)C10C111.58(2)
O4C41.276(16)C11C121.49(2)

12-X,-1/2+Y,1-Z; 22-X,1/2+Y,1-Z; 32-X,1/2+Y,2-Z; 41-X,-1/2+Y,1-Z

Table 5 Bond Angles for Zn(asp).
AtomAtomAtomAngle/˚AtomAtomAtomAngle/˚
Zn1O1C1133.4(8)O4C4C31118.6(12)
Zn11O3Zn2161.1(4)O5Zn2O789.5(4)
Zn11O3C4112.5(9)O5Zn2O10107.8(4)
Zn12O8C8126.8(8)O5C5O6124.4(12)
Zn1O11C12111.3(10)O5C5C66116.0(12)
Zn11N1C3115.4(9)O6Zn3O9195.5(3)
Zn2O3C476.7(8)O6Zn3O1281.6(4)
Zn2O4C4105.9(9)O6Zn3N2678.3(4)
Zn2O5C5133.2(9)O6Zn3N31167.6(4)
Zn2O7C8130.5(9)O6C5C6119.5(11)
Zn2O10C9128.3(8)O7Zn2O10109.7(4)
Zn33O2C1117.6(9)O7C8O8122.6(12)
Zn32O6C5115.5(8)O7C8C7120.4(13)
Zn34O9C9109.1(8)O8Zn1O11133.2(4)
Zn3O12C12126.3(9)O8Zn1N196.3(4)
Zn3N2C6109.8(8)O8C8C7117.0(12)
Zn3N3C10109.5(8)O96Zn3O12180.2(3)
O1Zn1O3169.0(4)O9Zn3N295.8(4)
O1Zn1O8100.1(4)O9Zn3N372.9(4)
O1Zn1O1193.0(4)O91C9O10127.2(11)
O1Zn1N198.9(4)O91C9C102117.0(12)
O1C1O2121.8(12)O10C9C10115.8(12)
O1C1C2120.5(12)O11Zn1N1125.9(4)
O2Zn3O6296.0(4)O11C12O12120.9(13)
O2Zn3O91162.0(4)O11C12C11117.4(14)
O2Zn3O1287.9(4)O12Zn3N2159.0(4)
O2Zn3N22100.1(4)O12Zn3N391.9(4)
O2Zn3N394.3(4)O12C12C11121.8(13)
O2C1C2117.7(12)N1C3C22113.6(12)
O35Zn1O890.5(3)N1C3C4110.0(11)
O35Zn1O1181.5(4)N2Zn3N3106.6(4)
O35Zn1N177.1(4)N2C6C5108.2(11)
O35Zn2O454.2(3)N2C6C7116.5(11)
O35Zn2O5165.0(3)N3C10C9110.4(12)
O3Zn2O791.6(3)N3C10C11110.6(11)
O32Zn2O10185.9(3)C1C2C3115.2(12)
O32C4O4120.9(13)C2C3C4113.6(11)
O32C4C32120.4(12)C5C6C7112.4(10)
O4Zn2O5113.7(4)C6C7C8113.5(12)
O4Zn2O7124.7(4)C9C10C11108.1(11)
O4Zn2O106109.3(4)C10C11C12112.7(12)

12-X,1/2+Y,1-Z; 22-X,-1/2+Y,1-Z; 32-X,-1/2+Y,2-Z; 41-X,1/2+Y,1-Z; 51-X,-1/2+Y,1-Z; 62-X,1/2+Y,2-Z

Table 6 Hydrogen Bonds for Zn(asp).
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1AO910.92002.14002.929(14)144.00
N1H1BO620.92002.03002.944(15)172.00
N2H2AO130.92002.37002.983(14)124.00
N2H2BO80.92002.21002.845(14)126.00
N3H3AO240.92002.37003.109(15)138.00
N3H3AO1230.92002.50003.317(15)148.00
N3H3BO430.92002.23003.138(14)169.00
C2H1O1010.99002.52003.318(17)137.00
C3H3O21.00002.38002.823(16)106.00
C3H3O911.00002.56003.111(16)114.00
C7H7AO1050.99002.60003.188(18)118.00

1+X,1+Y,+Z; 22-X,1/2+Y,1-Z; 31-X,-1/2+Y,1-Z; 4+X,-1+Y,+Z; 5+X,+Y,1+Z

Table 7 Torsion Angles for Zn(asp).
ABCDAngle/˚
Zn1O1C1O2-171.8(10)
Zn1O1C1C29(2)
Zn11O3C4O4175.8(9)
Zn11O3C4C3-7.0(15)
Zn12O8C8O712.0(18)
Zn12O8C8C7-167.2(8)
Zn1O11C12O1222.6(16)
Zn1O11C12C11-155.9(9)
Zn11N1C3C2-152.4(9)
Zn11N1C3C4-23.8(13)
Zn2O3C4O413.2(11)
Zn2O3C4C3-169.6(13)
Zn2O4C4O3-17.9(15)
Zn2O4C4C3164.9(10)
Zn2O5C5O611(2)
Zn2O5C5C6-166.0(8)
Zn23O7C8O8-152.8(10)
Zn23O7C8C726.3(18)
Zn22O10C9O9-21(2)
Zn22O10C9C10157.9(9)
Zn34O2C1O129.7(18)
Zn34O2C1C2-151.1(10)
Zn3O6C5O5177.7(10)
Zn3O6C5C6-5.0(14)
Zn3O9C9O10168.9(12)
Zn3O9C9C10-10.0(14)
Zn3O12C12O11-153.9(10)
Zn3O12C12C1124.6(18)
Zn3N2C6C5-31.2(11)
Zn3N2C6C7-158.9(9)
Zn3N3C10C948.2(13)
Zn3N3C10C11-71.4(11)
O1Zn1O81C81-97.6(10)
O1Zn1O11C12-85.8(9)
O1Zn1N12C32-174.4(8)
O1C1C2C3-145.7(13)
O25Zn3O6C588.6(9)
O25Zn3O12C12-112.7(11)
O25Zn3N2C6-70.6(8)
O25Zn3N3C10127.8(9)
O2C1C2C335.1(19)
O32Zn1O11C1284.7(9)
O3Zn2O4C48.7(8)
O3Zn2O76C86-78.2(11)
O3Zn2O101C91-47.4(11)
O4Zn2O3C4-9.0(8)
O4Zn2O5C518.0(12)
O4Zn2O76C86-124.4(11)
O4Zn2O101C912.4(12)
O5Zn2O4C4178.5(8)
O5Zn2O76C86116.8(11)
O5Zn2O101C91126.3(11)
O5C5C6N2-157.5(11)
O5C5C6C7-27.4(16)
O6Zn3O25C15-137.5(10)
O6Zn3O9C9-147.4(9)
O6Zn3O12C12150.9(11)
O6Zn3N2C623.5(8)
O6C5C6N225.0(15)
O6C5C6C7155.1(11)
O76Zn2O3C4-141.9(8)
O76Zn2O4C471.5(9)
O76Zn2O5C5146.1(12)
O81Zn1O1C1-44.8(13)
O81Zn1O11C12167.3(8)
O9Zn3O6C5-105.3(9)
O9Zn3O12C1253.8(10)
O9Zn3N2C6118.0(8)
O9Zn3N3C10-39.3(8)
O9C9C10N3-22.7(17)
O9C9C10C1198.5(14)
O101Zn2O3C4108.4(8)
O101Zn2O4C4-61.1(9)
O101Zn2O5C5-103.3(12)
O10C9C10N3158.3(12)
O10C9C10C11-80.5(15)
O11Zn1O1C1-179.7(13)
O11Zn1O32C42-135.2(9)
O11Zn1O81C816.3(12)
O11Zn1N12C3285.3(9)
O12Zn3O25C15141.1(11)
O12Zn3O6C5175.5(9)
O12Zn3O9C9-67.0(9)
O12Zn3N2C640.4(16)
O12Zn3N3C1039.8(9)
N12Zn1O1C153.2(13)
N12Zn1O11C1217.4(11)
N1C3C4O319.9(17)
N1C3C4O4-162.8(11)
N2Zn3O25C15-58.4(11)
N2Zn3O6C5-10.5(9)
N2Zn3O9C9133.8(9)
N2Zn3O12C12134.2(13)
N2Zn3N3C10-130.3(8)
N2C6C7C863.7(14)
N3Zn3O25C1549.4(11)
N3Zn3O9C928.1(9)
N3Zn3O12C12-18.5(11)
N3Zn3N2C6-168.3(8)
N3C10C11C1275.3(14)
C1C2C3N1-151.5(12)
C1C2C3C481.8(15)
C2C3C4O3148.5(12)
C2C3C4O4-34.2(16)
C5C6C7C8-62.0(15)
C6C7C8O7164.6(12)
C6C7C8O8-16.2(17)
C9C10C11C12-45.7(16)
C10C11C12O11131.3(13)
C10C11C12O12-47.2(17)

12-X,1/2+Y,1-Z; 22-X,-1/2+Y,1-Z; 32-X,-1/2+Y,2-Z; 41-X,1/2+Y,1-Z; 51-X,-1/2+Y,1-Z; 62-X,1/2+Y,2-Z

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for Zn(asp).
AtomxyzU(eq)
H192227387345324
H1A100399252515721
H1B111948218496121
H296296078419824
H2A5582-212747423
H2B7262-344714623
H381568041559522
H3A4932-985457620
H3B37960404720
H659101513854618
H7A7276-4986317
H7B803913791008117
H105233-965243825
H11A5419906121825
H11B40191199215825

[RSC Journal Format]

Experimental

Single crystals of C12H17N3O13Zn3 [Zn(asp)] were recrystallised from [solvents] mounted in inert oil and transferred to the cold gas stream of the diffractometer.

Crystal structure determination of [Zn(asp)]

Crystal Data. C12H17N3O13Zn3, =607.40, Monoclinic, a = 8.484(3) Å, b = 10.491(3) Å, c = 10.187(3) Å, β = 93.552(7)°, = 905.0(5) Å3, T = 100(2), space group P21 (no. 4), Z = 2, μ(Mo-Kα) = 4.025, 2561 reflections measured, 2432 unique (Rint = 0.0272) which were used in all calculations. The final wR(F2) was 0.1400 (all data).

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