Co(p-Glu)(bipy)
| 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 Co(p-Glu)(bipy)
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Identification code
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Co(p-Glu)(bipy)
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Empirical formula
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C20H28CoN4O10
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Formula weight
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543.39
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Temperature/K
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150.0
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Crystal system
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Monoclinic
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Space group
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P21/n
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a/Å, b/Å, c/Å
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7.5041(8), 11.4525(12), 14.0448(15)
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α/°, β/°, γ/°
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90.00, 98.9770(10), 90.00
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Volume/Å3
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1192.2(2)
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Z
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2
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ρcalcmg/mm3
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1.514
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m/mm‑1
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0.719
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F(000)
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566
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Crystal size/mm3
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0.1 × 0.1 × 0.1
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Theta range for data collection
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3.31 to 27.39°
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Index ranges
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-6 ≤ h ≤ 9, -15 ≤ k ≤ 15, -18 ≤ l ≤ 15
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Reflections collected
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6644
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Independent reflections
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2871[R(int) = 0.0552]
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Data/restraints/parameters
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2871/7/172
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Goodness-of-fit on F2
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1.013
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Final R indexes [I>2σ (I)]
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R1 = 0.0764, wR2 =
0.2166
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Final R indexes [all data]
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R1 = 0.0817, wR2 = 0.2263
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Largest diff. peak/hole / e Å-3
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3.098/-0.873
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Table 2 Atomic Coordinates (Å×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for Co(p-Glu)(bipy). Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
| Atom | x | y | z | U(eq) |
| Co1 | 0 | 5000 | 5000 | 5.5(2) |
| O1W | 2521(3) | 5163.6(17) | 5849.5(17) | 11.9(5) |
| O2 | 1202(3) | 5143(16) | 3741.9(16) | 11.6(5) |
| C4 | 51(3) | 645(3) | 4990(13) | 8.3(6) |
| N5 | 214(3) | 3111(2) | 4964.3(14) | 10.2(5) |
| C6 | 1004(4) | 1281(2) | 5759(2) | 15.7(6) |
| C7 | -776(4) | 1291(2) | 4201(2) | 14.6(6) |
| C10 | 1026(4) | 2491(2) | 5717(2) | 16.1(6) |
| C8 | 480(4) | 5262(3) | 2865(2) | 13.4(5) |
| C16 | -646(4) | 2498(2) | 4216(2) | 14.1(6) |
| O3 | -1147(3) | 5097.3(17) | 2535.4(18) | 18.6(6) |
| C5 | 1758(4) | 5701(2) | 2187(19) | 17.9(6) |
| N3 | 1030(3) | 5565(2) | 1171.9(16) | 19.3(5) |
| C1 | 2047(4) | 7047(3) | 2283(2) | 22.7(6) |
| O4 | -259(3) | 6607(2) | -146.7(16) | 21.1(5) |
| C3 | 877(4) | 7567(2) | 1387(2) | 22.7(6) |
| C9 | 470(4) | 6545(2) | 705(2) | 17.9(6) |
| O5W | 5351(3) | 3832.6(17) | 5862.4(16) | 23(5) |
Table 3 Anisotropic Displacement Parameters (Å2×103) for Co(p-Glu)(bipy). The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
| Co1 | 6.8(4) | 3.3(4) | 6.1(4) | 0.53(12) | -0.1(2) | -0.45(12) |
| O1W | 9.3(10) | 11.5(8) | 14.2(10) | 0(7) | -0.5(8) | -0.2(7) |
| O2 | 10.5(10) | 14.7(9) | 9.6(10) | 1.1(6) | 1.3(8) | -1.3(6) |
| C4 | 7.3(13) | 5.7(14) | 11.8(14) | -1.1(7) | 1.2(11) | 0.9(7) |
| N5 | 16.3(11) | 3.5(11) | 10.3(12) | 0.9(6) | 0.7(9) | -0.3(7) |
| C6 | 23.7(14) | 7.5(13) | 13(13) | 0.9(10) | -6.5(11) | 0.6(11) |
| C7 | 22.8(14) | 7.5(13) | 10.8(12) | -2(10) | -5.7(11) | 1.5(10) |
| C10 | 24.9(15) | 7.2(12) | 13.6(13) | 1(10) | -4.8(11) | -1.9(11) |
| C8 | 16.5(13) | 13.1(10) | 10.4(12) | 0.2(11) | 1.6(10) | 2.5(11) |
| C16 | 21.5(14) | 6.5(12) | 12.4(12) | 0.1(10) | -3.3(10) | 0.5(10) |
| O3 | 14.4(12) | 31.9(13) | 8.7(11) | -0.5(7) | -0.6(9) | -3.8(7) |
| C5 | 21.1(13) | 19.9(13) | 13.9(12) | 1.1(10) | 6.2(10) | -0.2(11) |
| N3 | 28.9(13) | 16.3(12) | 13(11) | 1.2(9) | 4(9) | -1.1(10) |
| C1 | 28.4(16) | 21(14) | 18.8(14) | 0.1(11) | 4.2(12) | -6.8(12) |
| O4 | 28.8(11) | 15.1(11) | 19.9(10) | 4(8) | 5.1(9) | 0.7(8) |
| C3 | 27.7(15) | 16.9(13) | 22.9(14) | -1.9(11) | 2.1(12) | -0.1(12) |
| C9 | 19.2(13) | 17.5(13) | 18.4(13) | 1.3(10) | 7.8(11) | -1.7(10) |
| O5W | 17.9(10) | 16.8(10) | 34.2(12) | -4.4(9) | 3.5(9) | 0.1(8) |
Table 4 Bond Lengths for Co(p-Glu)(bipy).
| Atom | Atom | Length/Å | Atom | Atom | Length/Å |
| Co1 | O1W | 2.082(2) | N5 | C16 | 1.343(3) |
| Co1 | O1W1 | 2.082(2) | C6 | C10 | 1.387(4) |
| Co1 | O2 | 2.112(2) | C7 | C16 | 1.386(4) |
| Co1 | O21 | 2.112(2) | C8 | O3 | 1.251(4) |
| Co1 | N51 | 2.170(3) | C8 | C5 | 1.538(4) |
| Co1 | N5 | 2.170(3) | C5 | N3 | 1.453(3) |
| O2 | C8 | 1.273(4) | C5 | C1 | 1.559(4) |
| C4 | C4 | 1.479(7) | N3 | C9 | 1.333(4) |
| C4 | C6 | 1.402(4) | C1 | C3 | 1.538(4) |
| C4 | C72 | 1.396(3) | O4 | C9 | 1.237(3) |
| N5 | C10 | 1.339(3) | C3 | C9 | 1.513(4) |
Table 5 Bond Angles for Co(p-Glu)(bipy).
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ |
| O1W | Co1 | O1W | 180.0 | C7 | C4 | C4 | 121.8(2) |
| O1W | Co1 | O2 | 90.23(9) | C7 | C4 | C6 | 116.5(3) |
| O1W | Co1 | O21 | 90.23(9) | C10 | N5 | Co1 | 122.48(18) |
| O1W | Co1 | O2 | 89.77(9) | C10 | N5 | C162 | 116.4(3) |
| O1W1 | Co1 | O21 | 89.77(9) | C10 | C6 | C4 | 119.6(3) |
| O1W | Co1 | N51 | 87.76(8) | C8 | O2 | Co12 | 130.2(2) |
| O1W1 | Co1 | N5 | 92.24(8) | C8 | C5 | C1 | 111.2(2) |
| O1W | Co1 | N51 | 92.23(8) | C16 | N5 | Co1 | 120.74(18) |
| O1W | Co1 | N5 | 87.77(8) | C16 | C7 | C4 | 119.7(3) |
| O21 | Co1 | O21 | 180.00(5) | O3 | C8 | O2 | 125.8(3) |
| O21 | Co1 | N5 | 90.86(7) | O3 | C8 | C5 | 119.1(3) |
| O2 | Co1 | N51 | 89.14(7) | N3 | C5 | C8 | 113.4(2) |
| O2 | Co1 | N5 | 89.14(7) | N3 | C5 | C1 | 102.5(2) |
| O21 | Co1 | N5 | 90.86(7) | N3 | C9 | C3 | 108.8(3) |
| O2 | C8 | C51 | 115.0(3) | O4 | C9 | N3 | 125.6(3) |
| N5 | Co1 | N5 | 179.999(1) | O4 | C9 | C3 | 125.6(3) |
| N5 | C10 | C6 | 123.8(3) | C3 | C1 | C5 | 104.9(2) |
| N5 | C16 | C7 | 123.9(3) | C9 | N3 | C5 | 115.7(2) |
| C6 | C4 | C4 | 121.7(2) | C9 | C3 | C1 | 104.6(2) |
Table 6 Hydrogen Bonds for Co(p-Glu)(bipy).
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
| O1W | H1WA | O5W | 0.841(18) | 1.83(2) | 2.612(3) | 153(3) |
| N3 | H3 | O41 | 0.88 | 2.02 | 2.888(3) | 168.1 |
| O5W | H5WB | O22 | 0.854(18) | 1.970(19) | 2.816(3) | 170(3) |
| O5W | H5WA | O43 | 0.872(18) | 1.866(19) | 2.737(3) | 176(3) |
Table 7 Torsion Angles for Co(p-Glu)(bipy).
| A | B | C | D | Angle/˚ |
| Co1 | O2 | C8 | O3 | -14.7(4) |
| Co1 | O2 | C8 | C5 | 162.41(17) |
| Co1 | N5 | C10 | C6 | 172.2(2) |
| Co1 | N5 | C16 | C7 | -170.8(2) |
| O1W1 | Co1 | O2 | C8 | 9.5(2) |
| O1W | Co1 | O2 | C8 | -170.5(2) |
| O1W1 | Co1 | N5 | C10 | -144.5(2) |
| O1W | Co1 | N5 | C10 | 35.5(2) |
| O1W | Co1 | N5 | C16 | -152.0(2) |
| O1W1 | Co1 | N5 | C16 | 28.0(2) |
| O21 | Co1 | O2 | C8 | -61(7) |
| O2 | Co1 | N5 | C10 | 125.7(2) |
| O21 | Co1 | N5 | C10 | -54.3(2) |
| O21 | Co1 | N5 | C16 | 118.2(2) |
| O2 | Co1 | N5 | C16 | -61.8(2) |
| O2 | C8 | C5 | N3 | 166.2(2) |
| O2 | C8 | C5 | C1 | -78.9(3) |
| C42 | C4 | C6 | C10 | -178.5(3) |
| C42 | C4 | C7 | C16 | 179.9(3) |
| C4 | C6 | C10 | N5 | -1.6(5) |
| C4 | C7 | C16 | N5 | -1.4(5) |
| N51 | Co1 | O2 | C8 | -82.7(2) |
| N5 | Co1 | O2 | C8 | 97.3(2) |
| N51 | Co1 | N5 | C10 | -67(3) |
| N51 | Co1 | N5 | C16 | 106(3) |
| C6 | C4 | C7 | C16 | -0.9(3) |
| C7 | C4 | C6 | C10 | 2.3(3) |
| C10 | N5 | C16 | C7 | 2.1(4) |
| C8 | C5 | N3 | C9 | 106.1(3) |
| C8 | C5 | C1 | C3 | -103.4(3) |
| C16 | N5 | C10 | C6 | -0.6(4) |
| O3 | C8 | C5 | N3 | -16.4(4) |
| O3 | C8 | C5 | C1 | 98.5(3) |
| C5 | N3 | C9 | O4 | -176.7(3) |
| C5 | N3 | C9 | C3 | 3.4(3) |
| C5 | C1 | C3 | C9 | -16.6(3) |
| N3 | C5 | C1 | C3 | 18.1(3) |
| C1 | C5 | N3 | C9 | -13.9(3) |
| C1 | C3 | C9 | N3 | 8.9(3) |
| C1 | C3 | C9 | O4 | -171.0(3) |
Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for Co(p-Glu)(bipy).
| Atom | x | y | z | U(eq) |
| H6 | 1631 | 885 | 6305 | 19 |
| H7 | -1426 | 905 | 3655 | 18 |
| H10 | 1654 | 2903 | 6254 | 19 |
| H16 | -1198 | 2917 | 3664 | 17 |
| H5 | 2945 | 5291 | 2334 | 22 |
| H3 | 962 | 4881 | 884 | 23 |
| H1B | 1656 | 7341 | 2880 | 27 |
| H1A | 3333 | 7249 | 2296 | 27 |
| H3A | -249 | 7903 | 1554 | 27 |
| H3B | 1541 | 8185 | 1095 | 27 |
| H1WA | 3180(4) | 4590(2) | 5780(3) | 34 |
| H1WB | 2970(4) | 5809(19) | 5770(3) | 34 |
| H5WB | 6440(3) | 4080(3) | 5940(3) | 34 |
| H5WA | 5280(5) | 3119(19) | 5640(3) | 34 |
[RSC Journal Format]
Experimental
Single crystals of C20H28CoN4O10
[Co(p-Glu)(bipy)]
were recrystallised from
[solvents]
mounted in inert oil and transferred to the cold gas stream of the diffractometer.
Crystal structure determination of
[Co(p-Glu)(bipy)]
Crystal Data.
C20H28CoN4O10,
M =543.39,
Monoclinic,
a = 7.5041(8) Å, b = 11.4525(12) Å, c = 14.0448(15) Å, β = 98.9770(10)°,
U = 1192.2(2) Å3,
T = 150.0,
space group P21/n (no. 14),
Z = 2,
μ(Mo-Kα) = 0.719,
6644 reflections measured,
2871 unique (Rint = 0.0552) which were used in all calculations.
The final wR(F2) was 0.2263 (all data).
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