Startseite Naturwissenschaften Crystal structure of hexakis(4-(dimethylamino)pyridin-1-ium) decavanadate-water (1:16), C42H98N12O44V10
Artikel Open Access

Crystal structure of hexakis(4-(dimethylamino)pyridin-1-ium) decavanadate-water (1:16), C42H98N12O44V10

  • , , , EMAIL logo und EMAIL logo
Veröffentlicht/Copyright: 15. Oktober 2015

Abstract

C42H98N12O44V10, triclinic, P1̅ (no. 2), a = 11.202(2) Å, b = 11.616(2) Å, c = 14.927(3) Å, α = 92.72(3)°, β = 102.58(3)°, γ = 100.25(3)°, V = 1858.0 Å3, Z = 1, Rgt(F) = 0.0385, wRref(F2) = 0.1116, T = 103 K.

CCDC no.:: 1267/4143

Table 1

Data collection and handling.

Crystal:Orange blocks,
size 0.20×0.23×0.30 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:13.03 cm−1
Diffractometer, scan mode:multiwire proportional, φ and ω
2θmax:54.98°
N(hkl)measured, N(hkl)unique:18122, 8329
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 6429
N(param)refined:487
Programs:SHELX [7]
Table 2

Atomic coordinates and displacement parameters (in Å2).

AtomSitexyzUiso
H(11A)2i1.20700.73730.47510.015
H(21A)2i0.96150.12670.68160.018
H(31A)2i1.2276−0.02970.16590.021
H(14A)2i1.05200.79740.52400.016
H(13A)2i1.18350.57150.38580.016
H(24A)2i0.98250.28510.77740.018
H(34A)2i1.07450.06000.18730.020
H(17A)2i0.70360.59540.44460.025
H(17B)2i0.64030.46260.43740.025
H(17C)2i0.61410.53550.35200.025
H(15A)2i0.85590.68540.48360.014
H(26A)2i1.47430.25860.74360.032
H(26B)2i1.55580.30740.84190.032
H(26C)2i1.53960.39130.76270.032
H(12A)2i0.99060.45380.33950.015
H(32A)2i1.0045−0.2633−0.02070.017
H(25A)2i1.17700.39270.84210.017
H(23A)2i1.12030.06420.64100.019
H(27A)2i1.33600.46700.89650.045
H(27B)2i1.45170.52370.85970.045
H(27C)2i1.46790.44020.93920.045
H(22A)2i1.31920.16550.69990.018
H(35A)2i0.8762−0.01040.10630.017
H(36A)2i0.8505−0.3131−0.09070.033
H(36B)2i0.7333−0.2694−0.14540.033
H(36C)2i0.7198−0.3559−0.06910.033
H(37A)2i0.7210−0.07860.04640.031
H(37B)2i0.6361−0.20370.02060.031
H(37C)2i0.6487−0.1174−0.05590.031
H(33A)2i1.1989−0.18820.06760.022
H(16A)2i0.83430.37110.29800.027
H(16B)2i0.69850.38960.25730.027
H(16C)2i0.72540.31730.34300.027
H(28A)2i1.23840.51660.22690.022
H(28B)2i1.21310.62160.21540.022
H(27D)2i1.36050.47430.36140.033
H(27E)2i1.30520.34320.32240.033
H(26D)2i0.3230−0.1142−0.23040.035
H(26E)2i0.2183−0.1290−0.20690.035
H(25D)2i0.83940.42280.03130.038
H(25C)2i0.77030.4233−0.05680.038
H(24B)2i0.92300.42720.18500.040
H(24C)2i1.02870.46600.15240.040
H(23B)2i0.3052−0.2655−0.03070.048
H(23C)2i0.4046−0.16380.00230.048
H(22B)2i0.4641−0.04930.16100.042
H(22C)2i0.5565−0.01280.12900.042
H(21C)2i0.0509−0.2790−0.24970.044
H(21B)2i−0.0094−0.2056−0.28660.044
Table 3

Atomic coordinates and displacement parameters (in Å2).

AtomSitexyzU11U22U33U12U13U23
V(1)2i1.61077(4)0.02353(4)0.44295(3)0.0055(2)0.0077(2)0.0072(2)0.0004(2)0.0019(2)−0.0006(2)
V(2)2i1.44181(4)0.14902(4)0.30707(3)0.0093(2)0.0100(2)0.0090(2)0.0017(2)0.0023(2)0.0014(2)
V(3)2i1.50669(4)−0.23303(4)0.48580(3)0.0077(2)0.0070(2)0.0093(2)0.0011(2)0.0006(2)−0.0009(2)
V(4)2i1.34178(4)−0.10954(4)0.34518(3)0.0066(2)0.0078(2)0.0076(2)0.0006(2)0.0008(2)−0.0011(2)
V(5)2i1.76819(4)−0.10001(4)0.59014(3)0.0062(2)0.0097(2)0.0111(2)0.0020(2)0.0015(2)0.0002(2)
O(6)2i1.6057(2)0.0941(2)0.3450(1)0.0069(9)0.0116(9)0.0102(9)0.0003(7)0.0023(7)−0.0010(7)
O(8)2i1.4637(2)0.2091(2)0.2162(1)0.013(1)0.017(1)0.011(1)0.0025(8)0.0018(8)0.0022(8)
O(7)2i1.5071(2)0.2679(2)0.3978(1)0.0089(9)0.0096(9)0.011(1)0.0000(7)0.0020(8)0.0014(7)
O(4)2i1.2801(2)0.1618(2)0.3110(1)0.0093(9)0.0107(9)0.0098(9)0.0008(7)0.0005(7)0.0005(7)
O(3)2i1.3807(2)−0.0129(2)0.2593(1)0.0090(9)0.0111(9)0.0079(9)0.0016(7)0.0016(7)−0.0008(7)
O(2)2i1.7519(2)−0.0122(2)0.4711(1)0.0069(9)0.0097(9)0.0107(9)0.0009(7)0.0021(7)−0.0015(7)
O(1)2i1.4480(2)−0.3575(2)0.4259(1)0.013(1)0.0083(9)0.015(1)0.0009(8)0.0026(8)0.0002(8)
O(14)2i1.7982(2)0.0548(2)0.6461(1)0.0067(9)0.0096(9)0.0094(9)0.0011(7)0.0007(7)−0.0010(7)
O(13)2i1.6733(2)−0.2264(2)0.5103(1)0.0092(9)0.0095(9)0.0109(9)0.0018(7)0.0007(7)−0.0010(7)
O(12)2i1.9091(2)−0.1212(2)0.6027(1)0.0087(9)0.016(1)0.014(1)0.0034(8)0.0019(8)−0.0004(8)
O(11)2i1.6473(2)0.1642(2)0.5270(1)0.0062(9)0.0073(9)0.0093(9)0.0007(7)0.0023(7)−0.0001(7)
O(10)2i1.4269(2)0.0517(2)0.4379(1)0.0072(9)0.0073(9)0.0089(9)0.0012(7)0.0012(7)−0.0005(7)
O(9)2i1.5174(2)−0.1264(2)0.3865(1)0.0065(9)0.0072(9)0.0091(9)0.0009(7)0.0016(7)−0.0014(7)
O(5)2i1.2808(2)−0.2336(2)0.2844(1)0.0098(9)0.0114(9)0.011(1)0.0011(8)0.0014(8)−0.0014(8)
N(11)2i1.1338(2)0.6941(2)0.4585(2)0.008(1)0.012(1)0.015(1)−0.0023(9)0.0015(9)0.0018(9)
N(21)2i1.0355(2)0.1660(2)0.7046(2)0.008(1)0.019(1)0.015(1)−0.004(1)−0.0005(9)0.006(1)
N(12)2i0.7819(2)0.4909(2)0.3744(2)0.009(1)0.010(1)0.018(1)−0.0005(9)0.004(1)−0.0030(9)
N(32)2i0.7976(2)−0.1907(2)−0.0173(2)0.012(1)0.015(1)0.012(1)0.003(1)−0.0015(9)−0.0005(9)
N(22)2i1.3893(2)0.3539(2)0.8153(2)0.010(1)0.019(1)0.014(1)−0.002(1)0.003(1)−0.006(1)
N(31)2i1.1533(2)−0.0576(2)0.1343(2)0.011(1)0.022(1)0.014(1)−0.002(1)−0.003(1)0.004(1)
C(14)2i1.0378(3)0.7276(2)0.4867(2)0.015(1)0.011(1)0.012(1)0.001(1)0.003(1)−0.000(1)
C(13)2i1.1161(3)0.5935(2)0.4043(2)0.012(1)0.018(1)0.012(1)0.005(1)0.004(1)0.004(1)
C(24)2i1.0518(3)0.2619(2)0.7629(2)0.012(1)0.021(2)0.016(1)0.003(1)0.007(1)0.008(1)
C(34)2i1.0584(3)−0.0059(3)0.1454(2)0.023(2)0.015(1)0.011(1)−0.001(1)0.003(1)0.003(1)
C(17)2i0.6759(3)0.5239(2)0.4047(2)0.011(1)0.014(1)0.026(2)−0.000(1)0.009(1)−0.001(1)
C(15)2i0.9204(3)0.6616(2)0.4620(2)0.011(1)0.011(1)0.014(1)0.002(1)0.005(1)0.002(1)
C(26)2i1.4991(3)0.3254(3)0.7886(2)0.009(1)0.030(2)0.022(2)0.000(1)0.003(1)−0.003(1)
C(12)2i1.0008(3)0.5233(2)0.3763(2)0.014(1)0.014(1)0.011(1)0.004(1)0.004(1)0.001(1)
C(32)2i1.0164(3)−0.1985(2)0.0216(2)0.013(1)0.015(1)0.015(1)0.003(1)0.002(1)0.001(1)
C(25)2i1.1679(3)0.3267(2)0.8016(2)0.013(1)0.016(1)0.015(1)0.003(1)0.004(1)0.000(1)
C(23)2i1.1336(3)0.1309(2)0.6817(2)0.016(2)0.015(1)0.016(2)−0.002(1)0.002(1)−0.000(1)
C(27)2i1.4133(3)0.4549(3)0.8835(2)0.023(2)0.034(2)0.027(2)−0.002(2)0.003(1)−0.017(2)
C(22)2i1.2525(3)0.1910(2)0.7170(2)0.010(1)0.017(1)0.017(2)0.003(1)0.004(1)0.001(1)
C(35)2i0.9402(3)−0.0473(2)0.0970(2)0.015(1)0.016(1)0.011(1)0.004(1)0.001(1)0.002(1)
C(31)2i0.9136(3)−0.1474(2)0.0316(2)0.014(1)0.013(1)0.009(1)0.002(1)0.004(1)0.005(1)
C(36)2i0.7732(3)−0.2909(3)−0.0866(2)0.021(2)0.017(2)0.022(2)0.002(1)−0.003(1)−0.003(1)
C(37)2i0.6918(3)−0.1436(3)−0.0001(2)0.012(1)0.032(2)0.016(2)0.005(1)0.001(1)0.002(1)
C(33)2i1.1325(3)−0.1529(3)0.0738(2)0.015(2)0.022(2)0.019(2)0.006(1)0.005(1)0.006(1)
C(21)2i1.2743(3)0.2925(2)0.7796(2)0.012(1)0.014(1)0.012(1)0.001(1)0.004(1)0.003(1)
C(11)2i0.8967(3)0.5558(2)0.4029(2)0.011(1)0.010(1)0.009(1)0.001(1)0.003(1)0.006(1)
C(16)2i0.7580(3)0.3829(2)0.3128(2)0.014(2)0.017(2)0.021(2)−0.001(1)0.004(1)−0.005(1)
O(28)2i1.1972(2)0.5513(2)0.1844(1)0.021(1)0.014(1)0.017(1)0.0014(9)0.0019(9)−0.0028(8)
O(27)2i1.3017(2)0.4243(2)0.3210(2)0.033(1)0.019(1)0.027(1)0.011(1)−0.005(1)−0.003(1)
O(26)2i0.2879(2)−0.1126(2)−0.1853(2)0.028(1)0.035(1)0.025(1)−0.002(1)0.016(1)−0.003(1)
O(25)2i0.7688(2)0.4266(2)−0.0026(2)0.039(2)0.036(1)0.025(1)0.015(1)0.011(1)0.009(1)
O(24)2i0.9607(2)0.4143(2)0.1430(2)0.024(1)0.033(1)0.039(2)−0.007(1)0.012(1)−0.009(1)
O(23)2i0.3763(2)−0.2279(2)−0.0340(2)0.026(1)0.049(2)0.034(2)−0.011(1)0.004(1)−0.008(1)
O(22)2i0.4880(2)−0.0658(2)0.1145(2)0.034(2)0.035(1)0.034(2)−0.010(1)0.023(1)−0.018(1)
O(21)2i0.0389(2)−0.2121(2)−0.2325(2)0.029(1)0.057(2)0.028(1)0.021(1)0.005(1)0.016(1)

Source of material

The title compound is prepared by adding N,N-dimethyl-4-aminopyridine into the acidified solution of sodium metavanadate and the mixture was heated at 80 °C for 24h. After heating, the product was deposited from the solution on slow evaporation as block-shaped yellow crystals.

Experimental details

The hydrogen atoms were generated geometrically and refined isotropically using the riding model, except for six hydrogen atoms of water molecules (H21C, H23B, H23C, H24B, H24C and H25D), which were found directly and refined as riding with d(O–H) = 0.85 Å.

Discussion

The chemistry of decavanadate have attracted wide attention not only because it is a typical example for the studying of the bidirectional hydrogen bonding [1, 2], but also it has various biological effects [3–5]. Herein, we report a new decavanadate salt which coniains an polyoxoanion of [V10O28]6−, six protonated N,N-dimethyl-4-aminopyridine cations and water molecules. The crystal structure is shown in Figure 1. The polyoxoanion [V10O28]6− exhibits a well-known cage structure which consists of six fused VO6 octahedra with D2h symmetry [6]. The bond lengths of the terminal V–O bonds are 1.6–1.7 Å while the bond lengths of the bridging V–O bonds are 1.8–2.0 Å. The protonated N,N-dimethyl-4-amino pyridines are the only kind of cations in the crystal structure. Two cations interact with the anion cluster through the N–H⋯O hydrogen bond with the disiance 2.7 Å (N31⋯O3) and the angle 160.7° (N31–H31A⋯O3). Sixteen water molecules were found in the unit cell. There are O–H⋯O hydrogen bonds between the water molecule and the polyoxoanion with a distance of 3.01 Å (O27⋯O4) and O–H⋯O hydrogen bonds between the water molecules (O⋯O: 2.745(4) and 2.750(3) Å).


Corresponding author: Zicheng Xiao and Pingfan Wu, School of Chemistry and Chemical Engineering, Faculty of Light Industry, Hubei University of Technology, Wuhan 430068, Hubei Province, P. R. China, e-mail: (Z. Xiao), (P. Wu)

Acknowledgments:

This work was supported by NFSC (grant No. 21271068) and the National Natural Science Foundation of Hubei Province (grant No. 211CDB082).

References

1. Day, V. W.; Klemperer, W. G.; Maltbie, D. J.: Where Are the Protons in H3V10O283−? J. Am. Chem. Soc. 109 (1987) 2991–3002.10.1021/ja00244a022Suche in Google Scholar

2. Kojima, T; Antonio, M. R.; Ozeki, T.: Solvent-Driven Association and Dissociation of the Hydrogen-Bonded Protonated Decavanadates. J. Am. Chem. Soc. 133 (2011) 7248–7251.Suche in Google Scholar

3. Rhule, J. T.; Hill, C. L.; Judd, D. A.: Polyoxometalates in Medicine. Chem. Rev. 98 (1998) 327–358.Suche in Google Scholar

4. Aureliano, M.; Crans, D. C.: Decavanadate (V10O286−) and oxovanadates: Oxometalates with many biological activities. J. Inorg. Biochem. 103 (2009) 536–546.Suche in Google Scholar

5. Aureliano, M; Gandara R. M. C.: Decavanadate effects in biological systems. J. Inorg. Biochem. 99 (2005) 979–985.10.1016/j.jinorgbio.2005.02.024Suche in Google Scholar PubMed

6. Evans, H. T., Jr.: The Molecular Structure of the Isopoly Complex Ion, Decavanadate (V10O286−). Inorg. Chem. 5 (1966) 967–977.Suche in Google Scholar

7. Sheldrick, G. M.: A short history of SHELX. Acta Crytallogr. A64 (2008) 112–122.Suche in Google Scholar

Received: 2014-4-21
Accepted: 2014-8-22
Published Online: 2015-10-15
Published in Print: 2015-12-1

©2015 Baolin Wu et al., published by De Gruyter.

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Artikel in diesem Heft

  1. Frontmatter
  2. Crystal structure of bis(ethyltriphenylphos-phonium) tetrabromidozincate(II), C40H40Br4P2Zn
  3. Crystal structure of chlorido-(2-ethoxy-6-(((quinolin-8-yl)methyl)-phenolato-κ3N,N′,O)-copper(II), C18H15ClCuN2O2
  4. Crystal structure of bis(ethyltriphenylphos-phonium) tetrabromidocobaltate(II), C40H40Br4CoP2
  5. Crystal structure of di(pyrrolidin-1-yl)methane-thione, C9H16N2S
  6. Crystal structure of ammonium phenylglyoxylate, C8H9NO3
  7. Crystal structure of 2-hydroxy-2-methyl-2-phenyl acetic acid hemihydrate, C9H11O3.50
  8. Crystal structure of 2-((E)-2-(1H-benzo[d]imidazol-2-yl)vinyl)-1H-benzo[d]imidazolium dichloride dihydrate, C16H18Cl2N4O2
  9. Crystal structure of 1,2-dimethylimidazolium iodide, C5H9IN2
  10. Crystal structure of catena-poly[(μ2-4,4′-bipyridine-κ2N:N′)-tetraqua-cobalt(II)] – (3-(carboxylatomethyl)benzoic acid) – water (1/2/2), C28H34CoN2O14
  11. Crystal structure of bis(2,2′-bipyridine-κ2N,N′)-bis(thiophene-3,4-dicarboxylato-κ2O,O′)-cadmium(II), C32H22CdN4O8S2
  12. Crystal structure of tetraaqua-(4,4′-diamino-1,1′-biphenyl-2,2′-disulfonato-κN)(4,4′-bipyridyl-κN)zinc(II) trihydrate, C22H32N4O13S2Zn
  13. Crystal structure of poly[[[(1,3-dimethyl-2-imidazolidinone-κ1O11) zinc(II)]-μ-1,4-benzenedi-carboxylato-κ4O1,O2:O3,O4]—1,3-dimethyl-2-imidazolidinone (1:1)], [Zn(C5H10N2O)(C8H4O4)]· C5H10N2O, C18H24N4O6Zn
  14. Crystal structure of poly[[(1,3-dimethyl-2-imidazolidinone-κ1O) zinc(II)]-μ-furan-2,5-dicarboxylato-κ4O,O′:O′′,O′′′], [Zn(C5H10N2O)(C6H2O5)], C22H24N4O12Zn2
  15. Crystal structure of catena-poly[(μ2-4,4′-bipyridine-κ2N:N′)-tetraquamanganese(II)] – (3-(carboxylatomethyl)benzoic acid) – water (1/2/2), C28H34MnN2O14
  16. Crystal structure of chlorido-tricarbonyl-bis(2-pyridylmethanone-N,N′)-rhenium(I), C14H8ClN2O4Re
  17. Crystal structure of (2-(benzoyl)phenolato-κ2O,O′)-trans-dichlorido -cis- bis(methoxido) niobium(V), C15H15Cl2NbO4
  18. Crystal structure of potassium diaqua dihydroxy(methylenediphosphonato-κ2-O,O′)cobaltate(III), CH10CoKO10P2
  19. Crystal structure of hexakis(4-(dimethylamino)pyridin-1-ium) decavanadate-water (1:16), C42H98N12O44V10
  20. Crystal structure of 4-diethylaminobenzaldehyde isonicotinoylhydrazone monohydrate, C17H20N4O·H2O, C17H22N4O2
  21. Crystal structure of bis[μ-1-[(2-ethyl-1H-imidazol-1-yl)methyl]-1H-benzotriazole-κ2N:N′]bis[dibromido]dimercury(II), C24H26Br4Hg2N10
  22. Crystal structure of poly{bis-[(4,4′-biphenyl-dicarboxylate-κ2O:O′)-μ-1,1′-oxy-bis-(ethane-2,1-diyl)-bis-(1H-imidazole)-κ2N:N′] zinc(II)}dihydrate, C48H48N8O12Zn2
  23. Crystal structure of sodium poly[(μ4-2,2′,2′′-nitrilotriacetato-κ4O,O′,O′′,N)magnesium(II)] monohydrate
  24. The crystal structure of 1-(2-(2-chloroethoxy)phenyl)ethanone
  25. The crystal structure of tris(μ2-1,3-bis(4,4,4-Trifluoro-3-oxido-1-(oxo)but-2-en-1-yl)phenyl-/κ4O,O′:O′′,O′′′)-bis(1,2-dimethoxyethane-O,O′)-diterbium(III)
  26. Crystal structure of (S)-2-(2,2′-diethoxy-[1,1′-binaphthalen]-6-yl)-4,4,5,5-tetra-methyl-2-imidazoline-1-oxyle, C31H33N2O3
  27. Crystal structure of cis-tetrachloridobis-(pyridine-κN)platinum(IV), C10H10Cl4N2Pt
  28. Crystal structure of catena-poly[aqua-(μ2-5-norbornene-2,3-dicarboxylato-κ3O,O′:O′′)-(1,10-phenanthroline-κ2N,N′)zinc(II)], [Zn(C9H8O4)(C12H8N2)(H2O)]n
Heruntergeladen am 27.3.2026 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2014-0150/html
Button zum nach oben scrollen