Zn(asp)
Crystal submitted by: |
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Crystal submitted on: |
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Data collected on: |
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Structure solved by: |
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Table 1 Crystal data and structure refinement for Zn(asp)
Identification code
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Zn(asp)
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Empirical formula
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C12H17N3O13Zn3
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Formula weight
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607.40
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Temperature/K
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100(2)
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Crystal system
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Monoclinic
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Space group
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P21
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a/Å, b/Å, c/Å
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8.484(3), 10.491(3), 10.187(3)
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α/°, β/°, γ/°
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90.00, 93.552(7), 90.00
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Volume/Å3
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905.0(5)
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Z
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2
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ρcalcmg/mm3
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2.247
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m/mm‑1
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4.025
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F(000)
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611
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Crystal size/mm3
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0.20 × 0.10 × 0.10
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Theta range for data collection
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1.94 to 27.46°
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Index ranges
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-10 ≤ h ≤ 2, -12 ≤ k ≤ 13, -12 ≤ l ≤ 11
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Reflections collected
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2561
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Independent reflections
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2432[R(int) = 0.0272]
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Data/restraints/parameters
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2432/170/277
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Goodness-of-fit on F2
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1.063
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Final R indexes [I>2σ (I)]
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R1 = 0.0599, wR2 =
0.1309
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Final R indexes [all data]
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R1 = 0.0799, wR2 = 0.1400
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Largest diff. peak/hole / e Å-3
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1.220/-1.300
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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.
Atom | x | y | z | U(eq) |
Zn1 | 8498.9(17) | 3872(14) | 2717.1(17) | 14.6(5) |
Zn2 | 9632.9(17) | 4619(13) | 8090.1(16) | 15.4(5) |
Zn3 | 5925.8(17) | 1142(14) | 5420.5(18) | 16.1(5) |
O1 | 7051(10) | 5320(9) | 3234(10) | 19(3) |
O2 | 6186(10) | 7049(9) | 4179(10) | 20(3) |
O3 | 10193(10) | 7033(9) | 7623(10) | 19(3) |
O4 | 8617(10) | 5644(8) | 6649(10) | 16(3) |
O5 | 8644(11) | 2948(8) | 8309(10) | 18(3) |
O6 | 7412(10) | 2468(8) | 6394(9) | 14(3) |
O7 | 10550(10) | -41(8) | 10032(10) | 19(3) |
O8 | 9714(10) | -117(8) | 7967(9) | 15(3) |
O9 | 7951(10) | 125(8) | 4285(9) | 14.9(19) |
O10 | 8137(10) | -668(8) | 2256(10) | 18(3) |
O11 | 6721(12) | 2882(9) | 1839(11) | 24(3) |
O12 | 6125(11) | 2444(9) | 3854(11) | 21(3) |
N1 | 10441(12) | 8502(10) | 5504(13) | 18(4) |
N2 | 6453(13) | 229(10) | 7229(12) | 19(4) |
N3 | 4851(12) | -192(11) | 4192(11) | 17(3) |
C1 | 7293(15) | 6370(13) | 3848(15) | 17(3) |
C2 | 8910(15) | 6822(14) | 4171(15) | 20(3) |
C3 | 9151(15) | 7551(12) | 5488(15) | 18(3) |
C4 | 9364(15) | 6700(13) | 6657(15) | 17(3) |
C5 | 7716(14) | 2263(12) | 7561(14) | 13(3) |
C6 | 6912(14) | 1164(13) | 8223(13) | 15(3) |
C7 | 7883(14) | 672(13) | 9442(15) | 14(3) |
C8 | 9510(14) | 136(13) | 9132(15) | 15(3) |
C9 | 7389(14) | -256(13) | 3198(14) | 16(3) |
C10 | 5599(14) | -202(14) | 2959(15) | 21(3) |
C11 | 5169(15) | 1042(14) | 2144(15) | 21(3) |
C12 | 6035(15) | 2184(14) | 2666(16) | 21(3) |
O1WA | 3070(3) | 2230(2) | 9560(2) | 72(7) |
O1WB | 2270(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]
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
Zn1 | 8.6(7) | 12.8(8) | 22.6(10) | 0.3(8) | 1.8(6) | -1.7(7) |
Zn2 | 10.8(7) | 13.7(8) | 21.5(10) | -0.4(8) | 0(7) | -0.8(7) |
Zn3 | 7(7) | 11.7(8) | 29.5(11) | 0.4(8) | -0.5(7) | -0.3(6) |
O1 | 8(4) | 19(4) | 31(6) | -5(4) | -1(4) | 4(4) |
O2 | 16(4) | 18(5) | 27(6) | -2(4) | 10(4) | 0(4) |
O3 | 17(5) | 15(5) | 25(5) | -2(4) | -1(4) | 0(4) |
O4 | 14(4) | 8(4) | 26(5) | -3(4) | -4(4) | 3(3) |
O5 | 17(4) | 13(4) | 24(5) | 10(4) | -1(4) | -6(4) |
O6 | 11(4) | 13(4) | 18(5) | 1(4) | -1(4) | 0(3) |
O7 | 14(4) | 17(5) | 26(5) | -3(4) | -6(4) | 5(4) |
O8 | 9(4) | 16(5) | 19(4) | -4(4) | -1(3) | 3(4) |
O10 | 19(4) | 6(4) | 29(5) | -1(4) | 0(4) | 7(3) |
O11 | 23(5) | 22(5) | 26(5) | 0(4) | 5(4) | -1(4) |
O12 | 20(4) | 14(4) | 28(5) | -1(4) | 5(4) | -6(4) |
N1 | 8(5) | 10(6) | 38(8) | -9(6) | 13(5) | 0(4) |
N2 | 12(5) | 12(6) | 32(8) | -3(6) | -6(5) | -7(5) |
N3 | 10(5) | 19(6) | 20(7) | -1(6) | -6(5) | 5(5) |
C1 | 11(4) | 15(5) | 26(6) | -3(4) | 2(4) | 2(4) |
C2 | 12(5) | 19(5) | 30(6) | 0(5) | -1(5) | 1(4) |
C3 | 11(5) | 12(5) | 31(6) | 0(4) | -1(5) | 2(4) |
C4 | 13(5) | 11(4) | 26(5) | -6(4) | 2(4) | 1(4) |
C5 | 10(4) | 6(4) | 22(5) | 4(4) | 2(4) | 0(4) |
C6 | 15(4) | 6(5) | 24(6) | 5(5) | 9(4) | 1(4) |
C7 | 7(4) | 9(5) | 26(6) | 3(5) | 5(4) | 2(4) |
C8 | 7(4) | 14(5) | 23(5) | -2(5) | 0(4) | 1(4) |
C9 | 13(4) | 8(5) | 29(5) | 2(5) | 8(4) | 4(4) |
C10 | 13(5) | 16(5) | 34(7) | -4(5) | 9(5) | 1(5) |
C11 | 14(5) | 22(5) | 28(6) | -3(5) | 12(5) | 5(4) |
C12 | 15(5) | 20(5) | 29(5) | 0(5) | 9(4) | 0(4) |
Table 4 Bond Lengths for Zn(asp).
Atom | Atom | Length/Å | Atom | Atom | Length/Å |
Zn1 | O1 | 2.043(9) | O5 | C5 | 1.282(16) |
Zn1 | O31 | 2.263(9) | O6 | C5 | 1.220(17) |
Zn1 | O82 | 2.010(9) | O7 | C8 | 1.246(17) |
Zn1 | O11 | 1.997(10) | O8 | C8 | 1.239(18) |
Zn1 | N11 | 2.010(13) | O9 | C9 | 1.244(17) |
Zn2 | O3 | 2.626(10) | O10 | C9 | 1.259(17) |
Zn2 | O4 | 1.974(10) | O11 | C12 | 1.283(18) |
Zn2 | O5 | 1.962(9) | O12 | C12 | 1.24(2) |
Zn2 | O73 | 1.962(10) | N1 | C3 | 1.480(16) |
Zn2 | O102 | 1.969(9) | N2 | C6 | 1.446(18) |
Zn3 | O24 | 2.091(9) | N3 | C10 | 1.442(18) |
Zn3 | O6 | 2.087(9) | C1 | C2 | 1.469(18) |
Zn3 | O9 | 2.382(9) | C2 | C3 | 1.55(2) |
Zn3 | O12 | 2.115(11) | C3 | C4 | 1.49(2) |
Zn3 | N2 | 2.100(12) | C5 | C6 | 1.519(18) |
Zn3 | N3 | 2.053(11) | C6 | C7 | 1.536(19) |
O1 | C1 | 1.277(17) | C7 | C8 | 1.541(17) |
O2 | C1 | 1.242(16) | C9 | C10 | 1.524(17) |
O3 | C4 | 1.225(17) | C10 | C11 | 1.58(2) |
O4 | C4 | 1.276(16) | C11 | C12 | 1.49(2) |
Table 5 Bond Angles for Zn(asp).
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ |
Zn1 | O1 | C1 | 133.4(8) | O4 | C4 | C31 | 118.6(12) |
Zn11 | O3 | Zn2 | 161.1(4) | O5 | Zn2 | O7 | 89.5(4) |
Zn11 | O3 | C4 | 112.5(9) | O5 | Zn2 | O10 | 107.8(4) |
Zn12 | O8 | C8 | 126.8(8) | O5 | C5 | O6 | 124.4(12) |
Zn1 | O11 | C12 | 111.3(10) | O5 | C5 | C66 | 116.0(12) |
Zn11 | N1 | C3 | 115.4(9) | O6 | Zn3 | O91 | 95.5(3) |
Zn2 | O3 | C4 | 76.7(8) | O6 | Zn3 | O12 | 81.6(4) |
Zn2 | O4 | C4 | 105.9(9) | O6 | Zn3 | N26 | 78.3(4) |
Zn2 | O5 | C5 | 133.2(9) | O6 | Zn3 | N31 | 167.6(4) |
Zn2 | O7 | C8 | 130.5(9) | O6 | C5 | C6 | 119.5(11) |
Zn2 | O10 | C9 | 128.3(8) | O7 | Zn2 | O10 | 109.7(4) |
Zn33 | O2 | C1 | 117.6(9) | O7 | C8 | O8 | 122.6(12) |
Zn32 | O6 | C5 | 115.5(8) | O7 | C8 | C7 | 120.4(13) |
Zn34 | O9 | C9 | 109.1(8) | O8 | Zn1 | O11 | 133.2(4) |
Zn3 | O12 | C12 | 126.3(9) | O8 | Zn1 | N1 | 96.3(4) |
Zn3 | N2 | C6 | 109.8(8) | O8 | C8 | C7 | 117.0(12) |
Zn3 | N3 | C10 | 109.5(8) | O96 | Zn3 | O121 | 80.2(3) |
O1 | Zn1 | O3 | 169.0(4) | O9 | Zn3 | N2 | 95.8(4) |
O1 | Zn1 | O8 | 100.1(4) | O9 | Zn3 | N3 | 72.9(4) |
O1 | Zn1 | O11 | 93.0(4) | O91 | C9 | O10 | 127.2(11) |
O1 | Zn1 | N1 | 98.9(4) | O91 | C9 | C102 | 117.0(12) |
O1 | C1 | O2 | 121.8(12) | O10 | C9 | C10 | 115.8(12) |
O1 | C1 | C2 | 120.5(12) | O11 | Zn1 | N1 | 125.9(4) |
O2 | Zn3 | O62 | 96.0(4) | O11 | C12 | O12 | 120.9(13) |
O2 | Zn3 | O91 | 162.0(4) | O11 | C12 | C11 | 117.4(14) |
O2 | Zn3 | O12 | 87.9(4) | O12 | Zn3 | N2 | 159.0(4) |
O2 | Zn3 | N22 | 100.1(4) | O12 | Zn3 | N3 | 91.9(4) |
O2 | Zn3 | N3 | 94.3(4) | O12 | C12 | C11 | 121.8(13) |
O2 | C1 | C2 | 117.7(12) | N1 | C3 | C22 | 113.6(12) |
O35 | Zn1 | O8 | 90.5(3) | N1 | C3 | C4 | 110.0(11) |
O35 | Zn1 | O11 | 81.5(4) | N2 | Zn3 | N3 | 106.6(4) |
O35 | Zn1 | N1 | 77.1(4) | N2 | C6 | C5 | 108.2(11) |
O35 | Zn2 | O4 | 54.2(3) | N2 | C6 | C7 | 116.5(11) |
O35 | Zn2 | O5 | 165.0(3) | N3 | C10 | C9 | 110.4(12) |
O3 | Zn2 | O7 | 91.6(3) | N3 | C10 | C11 | 110.6(11) |
O32 | Zn2 | O101 | 85.9(3) | C1 | C2 | C3 | 115.2(12) |
O32 | C4 | O4 | 120.9(13) | C2 | C3 | C4 | 113.6(11) |
O32 | C4 | C32 | 120.4(12) | C5 | C6 | C7 | 112.4(10) |
O4 | Zn2 | O5 | 113.7(4) | C6 | C7 | C8 | 113.5(12) |
O4 | Zn2 | O7 | 124.7(4) | C9 | C10 | C11 | 108.1(11) |
O4 | Zn2 | O106 | 109.3(4) | C10 | C11 | C12 | 112.7(12) |
Table 6 Hydrogen Bonds for Zn(asp).
D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
N1 | H1A | O91 | 0.9200 | 2.1400 | 2.929(14) | 144.00 |
N1 | H1B | O62 | 0.9200 | 2.0300 | 2.944(15) | 172.00 |
N2 | H2A | O13 | 0.9200 | 2.3700 | 2.983(14) | 124.00 |
N2 | H2B | O8 | 0.9200 | 2.2100 | 2.845(14) | 126.00 |
N3 | H3A | O24 | 0.9200 | 2.3700 | 3.109(15) | 138.00 |
N3 | H3A | O123 | 0.9200 | 2.5000 | 3.317(15) | 148.00 |
N3 | H3B | O43 | 0.9200 | 2.2300 | 3.138(14) | 169.00 |
C2 | H1 | O101 | 0.9900 | 2.5200 | 3.318(17) | 137.00 |
C3 | H3 | O2 | 1.0000 | 2.3800 | 2.823(16) | 106.00 |
C3 | H3 | O91 | 1.0000 | 2.5600 | 3.111(16) | 114.00 |
C7 | H7A | O105 | 0.9900 | 2.6000 | 3.188(18) | 118.00 |
Table 7 Torsion Angles for Zn(asp).
A | B | C | D | Angle/˚ |
Zn1 | O1 | C1 | O2 | -171.8(10) |
Zn1 | O1 | C1 | C2 | 9(2) |
Zn11 | O3 | C4 | O4 | 175.8(9) |
Zn11 | O3 | C4 | C3 | -7.0(15) |
Zn12 | O8 | C8 | O7 | 12.0(18) |
Zn12 | O8 | C8 | C7 | -167.2(8) |
Zn1 | O11 | C12 | O12 | 22.6(16) |
Zn1 | O11 | C12 | C11 | -155.9(9) |
Zn11 | N1 | C3 | C2 | -152.4(9) |
Zn11 | N1 | C3 | C4 | -23.8(13) |
Zn2 | O3 | C4 | O4 | 13.2(11) |
Zn2 | O3 | C4 | C3 | -169.6(13) |
Zn2 | O4 | C4 | O3 | -17.9(15) |
Zn2 | O4 | C4 | C3 | 164.9(10) |
Zn2 | O5 | C5 | O6 | 11(2) |
Zn2 | O5 | C5 | C6 | -166.0(8) |
Zn23 | O7 | C8 | O8 | -152.8(10) |
Zn23 | O7 | C8 | C7 | 26.3(18) |
Zn22 | O10 | C9 | O9 | -21(2) |
Zn22 | O10 | C9 | C10 | 157.9(9) |
Zn34 | O2 | C1 | O1 | 29.7(18) |
Zn34 | O2 | C1 | C2 | -151.1(10) |
Zn3 | O6 | C5 | O5 | 177.7(10) |
Zn3 | O6 | C5 | C6 | -5.0(14) |
Zn3 | O9 | C9 | O10 | 168.9(12) |
Zn3 | O9 | C9 | C10 | -10.0(14) |
Zn3 | O12 | C12 | O11 | -153.9(10) |
Zn3 | O12 | C12 | C11 | 24.6(18) |
Zn3 | N2 | C6 | C5 | -31.2(11) |
Zn3 | N2 | C6 | C7 | -158.9(9) |
Zn3 | N3 | C10 | C9 | 48.2(13) |
Zn3 | N3 | C10 | C11 | -71.4(11) |
O1 | Zn1 | O81 | C81 | -97.6(10) |
O1 | Zn1 | O11 | C12 | -85.8(9) |
O1 | Zn1 | N12 | C32 | -174.4(8) |
O1 | C1 | C2 | C3 | -145.7(13) |
O25 | Zn3 | O6 | C5 | 88.6(9) |
O25 | Zn3 | O12 | C12 | -112.7(11) |
O25 | Zn3 | N2 | C6 | -70.6(8) |
O25 | Zn3 | N3 | C10 | 127.8(9) |
O2 | C1 | C2 | C3 | 35.1(19) |
O32 | Zn1 | O11 | C12 | 84.7(9) |
O3 | Zn2 | O4 | C4 | 8.7(8) |
O3 | Zn2 | O76 | C86 | -78.2(11) |
O3 | Zn2 | O101 | C91 | -47.4(11) |
O4 | Zn2 | O3 | C4 | -9.0(8) |
O4 | Zn2 | O5 | C5 | 18.0(12) |
O4 | Zn2 | O76 | C86 | -124.4(11) |
O4 | Zn2 | O101 | C91 | 2.4(12) |
O5 | Zn2 | O4 | C4 | 178.5(8) |
O5 | Zn2 | O76 | C86 | 116.8(11) |
O5 | Zn2 | O101 | C91 | 126.3(11) |
O5 | C5 | C6 | N2 | -157.5(11) |
O5 | C5 | C6 | C7 | -27.4(16) |
O6 | Zn3 | O25 | C15 | -137.5(10) |
O6 | Zn3 | O9 | C9 | -147.4(9) |
O6 | Zn3 | O12 | C12 | 150.9(11) |
O6 | Zn3 | N2 | C6 | 23.5(8) |
O6 | C5 | C6 | N2 | 25.0(15) |
O6 | C5 | C6 | C7 | 155.1(11) |
O76 | Zn2 | O3 | C4 | -141.9(8) |
O76 | Zn2 | O4 | C4 | 71.5(9) |
O76 | Zn2 | O5 | C5 | 146.1(12) |
O81 | Zn1 | O1 | C1 | -44.8(13) |
O81 | Zn1 | O11 | C12 | 167.3(8) |
O9 | Zn3 | O6 | C5 | -105.3(9) |
O9 | Zn3 | O12 | C12 | 53.8(10) |
O9 | Zn3 | N2 | C6 | 118.0(8) |
O9 | Zn3 | N3 | C10 | -39.3(8) |
O9 | C9 | C10 | N3 | -22.7(17) |
O9 | C9 | C10 | C11 | 98.5(14) |
O101 | Zn2 | O3 | C4 | 108.4(8) |
O101 | Zn2 | O4 | C4 | -61.1(9) |
O101 | Zn2 | O5 | C5 | -103.3(12) |
O10 | C9 | C10 | N3 | 158.3(12) |
O10 | C9 | C10 | C11 | -80.5(15) |
O11 | Zn1 | O1 | C1 | -179.7(13) |
O11 | Zn1 | O32 | C42 | -135.2(9) |
O11 | Zn1 | O81 | C81 | 6.3(12) |
O11 | Zn1 | N12 | C32 | 85.3(9) |
O12 | Zn3 | O25 | C15 | 141.1(11) |
O12 | Zn3 | O6 | C5 | 175.5(9) |
O12 | Zn3 | O9 | C9 | -67.0(9) |
O12 | Zn3 | N2 | C6 | 40.4(16) |
O12 | Zn3 | N3 | C10 | 39.8(9) |
N12 | Zn1 | O1 | C1 | 53.2(13) |
N12 | Zn1 | O11 | C12 | 17.4(11) |
N1 | C3 | C4 | O3 | 19.9(17) |
N1 | C3 | C4 | O4 | -162.8(11) |
N2 | Zn3 | O25 | C15 | -58.4(11) |
N2 | Zn3 | O6 | C5 | -10.5(9) |
N2 | Zn3 | O9 | C9 | 133.8(9) |
N2 | Zn3 | O12 | C12 | 134.2(13) |
N2 | Zn3 | N3 | C10 | -130.3(8) |
N2 | C6 | C7 | C8 | 63.7(14) |
N3 | Zn3 | O25 | C15 | 49.4(11) |
N3 | Zn3 | O9 | C9 | 28.1(9) |
N3 | Zn3 | O12 | C12 | -18.5(11) |
N3 | Zn3 | N2 | C6 | -168.3(8) |
N3 | C10 | C11 | C12 | 75.3(14) |
C1 | C2 | C3 | N1 | -151.5(12) |
C1 | C2 | C3 | C4 | 81.8(15) |
C2 | C3 | C4 | O3 | 148.5(12) |
C2 | C3 | C4 | O4 | -34.2(16) |
C5 | C6 | C7 | C8 | -62.0(15) |
C6 | C7 | C8 | O7 | 164.6(12) |
C6 | C7 | C8 | O8 | -16.2(17) |
C9 | C10 | C11 | C12 | -45.7(16) |
C10 | C11 | C12 | O11 | 131.3(13) |
C10 | C11 | C12 | O12 | -47.2(17) |
Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for Zn(asp).
Atom | x | y | z | U(eq) |
H1 | 9222 | 7387 | 3453 | 24 |
H1A | 10039 | 9252 | 5157 | 21 |
H1B | 11194 | 8218 | 4961 | 21 |
H2 | 9629 | 6078 | 4198 | 24 |
H2A | 5582 | -212 | 7474 | 23 |
H2B | 7262 | -344 | 7146 | 23 |
H3 | 8156 | 8041 | 5595 | 22 |
H3A | 4932 | -985 | 4576 | 20 |
H3B | 3796 | 0 | 4047 | 20 |
H6 | 5910 | 1513 | 8546 | 18 |
H7A | 7276 | -4 | 9863 | 17 |
H7B | 8039 | 1379 | 10081 | 17 |
H10 | 5233 | -965 | 2438 | 25 |
H11A | 5419 | 906 | 1218 | 25 |
H11B | 4019 | 1199 | 2158 | 25 |
[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,
M =607.40,
Monoclinic,
a = 8.484(3) Å, b = 10.491(3) Å, c = 10.187(3) Å, β = 93.552(7)°,
U = 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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