Startseite Crystal structure of catena-poly[(μ2-butane-1,4-diyl-bis(pyridine-3-carboxylato-κN))silver(I)] tetrafluoroborate, C16H16AgN2O4BF4
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Crystal structure of catena-poly[(μ2-butane-1,4-diyl-bis(pyridine-3-carboxylato-κN))silver(I)] tetrafluoroborate, C16H16AgN2O4BF4

  • Iván Brito EMAIL logo , Alejandro Cárdenas , Michael Bolte , Jaime Llanos und Fernando Cataldo
Veröffentlicht/Copyright: 20. Januar 2017

Abstract

C16H16AgN2O4BF4, monoclinic, C2/c (no. 15), a = 17.416(2) Å, b = 13.1378(14) Å, c = 7.8246(10) Å, β = 96.566(10)°, V = 1778.6(4) Å3, Z = 4, Rgt(F) = 0.025, wRref(F2) = 0.065, T = 173(2) K.

CCDC no.:: 1526217

A part of the title crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Colourless block
Size:0.33 × 0.29 × 0.27 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:12.0 cm−1
Diffractometer, scan mode:Bruker IPDS II, ω-scans
2θmax, completeness:51.2°, >98%
N(hkl)measured, N(hkl)unique, Rint:6065, 1665, 0.040
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1628
N(param)refined:138
Programs:SHELX [4], Stoe X-AREA [5], PLATON [6], Absorption correction [7]
Table 2

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
B10.50000.1947(4)0.25000.0355(9)
F10.49888(13)0.1296(2)0.3902(3)0.0736(7)
F20.43400(13)0.2507(2)0.2252(3)0.0808(7)
Ag10.00000.41148(2)0.25000.03182(14)
O10.24415(10)0.39577(13)0.7796(2)0.0287(4)
O20.35544(10)0.38911(17)0.6619(2)0.0383(5)
C10.27884(13)0.38919(17)0.6561(3)0.0228(4)
C20.39934(15)0.3959(2)0.8319(3)0.0387(6)
H2Aa0.40340.32830.88800.046*
H2Ba0.37420.44370.90610.046*
H2Ca0.37590.35160.91420.046*
H2Da0.39930.46680.87470.046*
C3a0.4811(3)0.4359(4)0.7999(6)0.0320(11)
H3Aa0.47620.50360.74420.038*
H3Ba0.51400.44310.91110.038*
C3′a0.4817(3)0.3616(5)0.8148(6)0.0302(10)
H3′1a0.51200.35920.92980.036*
H3′2a0.48110.29250.76430.036*
C110.24134(13)0.38121(17)0.4755(3)0.0215(4)
C120.16232(13)0.39673(17)0.4456(3)0.0236(4)
H120.13450.41010.54070.028*
N130.12357(12)0.39359(15)0.2868(3)0.0265(4)
C140.16398(15)0.37346(19)0.1540(3)0.0296(5)
H140.13740.37190.04100.036*
C150.24237(15)0.35503(19)0.1754(3)0.0296(5)
H150.26880.33980.07880.036*
C160.28246(13)0.35883(17)0.3387(3)0.0244(4)
H160.33650.34650.35630.029*

aOccupancy: 0.50.

Source of material

A solution of AgBF4 (19.46 mg, 0.1 mmol) in water was slowly added to a solution of the ligand, butane-1,4-diyl bis(pyridine-3-carboxylate) (L) (30.03 mg, 0.1 mmol) in THF (4 ml). Colourless crystals suitable for X-ray were obtained after a few days (85%).

Experimental details

All H atoms were located in the difference Fourier map, but refined with fixed individual displacement parameters, using a riding mode with C—H distances of 0.95 Å (for aromatic rings), 0.99 Å (for CH2), with Uiso(H) values of 1.2Ueq(C) (for CH in aromatic and CH2).

Discussion

The design of polymeric organic-inorganic materials with novel topologies and structural motifs is of current interest in the field of coordination chemistry [1] . This paper forms part of our continuing study of the synthesis, structural characterization and physical properties of coordination polymers [2].

In the title compound the molecule lies on a twofold rotation axis which passes through the mid point of the C3—C3′ bond, giving one half molecule per asymmetric unit. The Ag atom exists in a linear AgN2 coordination geometry; it lies on an two-fold axis. The bond distances and angles Ag—N and N—Ag⋯NA(A = −x, y, 1/2 − z) are 2.151(2) Å and 167.46(11)° respectively (cf. the figure). The ligand has a gauche conformation and links two Ag atoms using its two pyridinyl groups. In the structure of {[Ag(L)]}n linear one-dimensional chains are formed. Weak interactions are observed between F and Ag atoms. The most obvious difference between the ligand of the title compound and the uncoordinated ligand [3] is the angle between the planes of pyridine rings (24.73(11)° and 44.71(19)°) respectively, which is a consequence of the flexible organic components of the title compound. The C3 atom and H-atoms related to C2 atoms are disordered (site-occupancy factor of 0.5). The BF4 anion lies on an two-fold axis.

Acknowledgements

IB thanks to Fondequip (EQM13–0021).

References

1 Blake, A. J.; Champness, N. R.; Chung, S. S.; Li, W. S.; Schröder, M.: In situ ligand synthesis and construction of an unprecedented three-dimensional array with silver(I): a new approach to inorganic crystal engineering. Chem. Commun. (1997) 1675–1676.10.1039/a702972aSuche in Google Scholar

2 Vallejos, J.; Brito, I.; Cárdenas, A.; Bolte, M.; Conejeros, S.; Alemany, P.; Llanos, J.: Self-Assembly of discrete metallocycles versus coordination polymers based on Cu(I) and Ag(I) ions and flexible ligands: structural diversification and luminescent properties. Polymers 8 (2016) 2–16.10.3390/polym8020046Suche in Google Scholar PubMed PubMed Central

3 Brito, I.; Vallejos, J.; López-Rodríguez, M.; Cárdenas, A.: Ethane-1,2-diylbis(pyridine-3-carboxylate). Acta Crystallogr. E66 (2010) o114.10.1107/S1600536809052106Suche in Google Scholar PubMed PubMed Central

4 Sheldrick, G. M.: A short history of SHELX. Acta Crystallogr. A64 (2008) 112–122.10.1107/S0108767307043930Suche in Google Scholar PubMed

5 Stoe & Cie. X-AREA. Stoe & Cie, Darmstadt, Germany, 2001.Suche in Google Scholar

6 Spek, A. L.: Structure validation in chemical crystallography. Acta Crystallogr. D65 (2009) 148–155.10.1107/S090744490804362XSuche in Google Scholar PubMed PubMed Central

7 Blessing, R. H.: An empirical correction for absorption anisotropy. Acta Crystallogr. A51 (1995) 33–38.10.1107/S0108767394005726Suche in Google Scholar PubMed

Received: 2016-7-19
Accepted: 2017-1-9
Published Online: 2017-1-20
Published in Print: 2017-3-1

©2017 Iván Brito 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. Cover and Frontmatter
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  4. Crystal structure of 1,1′-(3,4-diphenylthieno[2,3-b]thiophene-2,5-diyl)bis[1-phenyl-methanone], C32H20O2S2
  5. Crystal structure of 4a-hydroxy-9-(3,5-dibromo-phenyl)-3,4,4a,5,6,7,9,9a-octahydro-2H-xanthene-1,8-dione, C19H18Br2O4
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  7. Crystal structure of pyridinium bis(naphthalane-2,3-diolato-κ2O,O′)borate monohydrate, C25H20BNO5
  8. Crystal structure of 1,1′-((1E,1′E)-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(azanylylidene))bis(methanylylidene))bis(naphthalen-2-olato)nickel(II), C72H52N4O8Ni2
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  11. Crystal structure of poly-[(μ6-benzene-1,2,4,5-tetracarboxylato)-(μ2-1,2-bis(imidazol-1-ylmethyl)benzene)dicobalt(II)], Co2C24H16N4O8
  12. Crystal structure of catena-(bis(μ2-1, 2-bis(imidazole-1-ylmethyl)benzene-κN:N′)-dichlororido-nickel(II)), C28H28Cl2N8Ni
  13. Crystal structure of (Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-hydroxy-3-(4-methoxyphenyl)prop-2-en-1-one, C15H16N2O3
  14. Crystal structure of (Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-hydroxy-3-phenylprop-2-en-1-one, C14H14N2O2
  15. Crystal structure of (E)-2-(4-hydroxy-3-methoxybenzylidene)-6-methoxy-3,4-dihydronaphthalen-1(2H)-one, C19H18O4
  16. Crystal structure of (Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-(4-ethoxyphenyl)-3-hydroxyprop-2-en-1-one, C16H18N2O3
  17. Crystal structure of (Z)-1-(1,5-dimethyl-1H-pyrazol-3-yl)-3-hydroxy-3-(p-toly)prop-2-en-1-one, C15H16N2O2
  18. Crystal structure of 1-acetyl-3-(3-chlorophenyl)-5-(4-isopropylphenyl)-4,5-dihydro-(1H)-pyrazole, C20H21ClN2O
  19. The crystal structure of 1-methyl-2,4-dinitro-5-iodoimidazole, C4H3IN4O4
  20. The crystal structure of 4-chloro-3,5-dinitroaniline, C6H4ClN3O4
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  23. Crystal structure of catena-poly[diaqua-bis(μ2-ethane-1,2-diyl-bis(pyridine-3-carboxylate-κ2N:N′))copper(II)] dinitrate, C28H28CuN6O16
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  25. The twinned crystal structure of (4SR)-7-benzyl-2,4,8,8-tetramethyl-7,8-dihydroimidazo[5,1-c][1,2,4]triazine-3,6(2H,4H)-dione, C16H20N4O2
  26. Crystal structure of (Z)-3-hydroxy-3-(4-methoxyphenyl)-1-(pyridin-2-yl)prop-2-en-1-one, C15H13NO3
  27. Crystal structure of 2-amino-4-(2,3-dichlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H12Cl2N2O2
  28. Crystal structure of catena-poly[(μ2-butane-1,4-diyl-bis(pyridine-3-carboxylato-κN))silver(I)] tetrafluoroborate, C16H16AgN2O4BF4
  29. Crystal structure of poly[diaqua-(1,10-phenanthroline-κ2N,N′)-(μ2-2,5-dihydroxytere-phthalato)-bis(μ4-2,5-dihydroxyterephthalato)dicerium(III)], C24H16CeN2O10
  30. Crystal structure of 5,7,4′-trihydroxy-3,8,3′-trymethoxyflavone, C18H16O8
  31. Crystal structure of N-(3,4-dichlorobenzylidene)-4-methylaniline, C14H11Cl2N
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  33. Crystal structure of 2-amino-4-(3-fluorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carbonitrile, C16H13FN2O2
  34. Crystal structure of 1,1,(3,4-dihydroxythieno[2,3-b] thiophene-2,5-diyl)bis(2-bromoethanone), C10H6Br2O4S2
  35. The crystal structure of N,N′-(4,4′-oxydibenzyl)-bisisonicotinamide 3.5 hydrate, C24H24N4O6
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  51. Crystal structure of 4,10,16,22-tetrahydroxy-6,12,18,24-tetramethoxy-2,8,14,20-tetraethylphenylresorcin[4]arene – ethyl acetate (1/1), C68H72O10
  52. Crystal structure of chlorido-(N-(2,5-dichlorophenyl)-1-(pyridin-2-yl)methanimine-κ2N,N′)(η6-1-isopropyl-4-methyl benzene) ruthenium (II) tetrafluoroborate, C22H22Cl3N2BF4Ru
  53. Crystal structure of 3-(5-methyl-1-p-tolyl-1H-1,2,3-triazol-4-yl)-1-phenyl-1H-pyrazole-4-carbaldehyde, a rare Z′ = 3 structure, C20H17N5O
  54. Crystal structure of 5-(5-(4-chlorophenyl)-1-phenyl-1H-pyrazol-3-yl)-N-phenyl-1,3,4-thiadiazol-2-amine, C23H16ClN5S
  55. Crystal structure of 7-hydroxy-3-(4-hydroxyphenyl)-4H-1-benzopyran-4-one-N,N-dimethylformamide (1/1), C18H17NO5
  56. Crystal structure of halogen-bonded 2-chloro-1,10-phenanthroline—1,4-diiodotetrafluorobenzene (2/1), C30H14Cl2F4I2N4
  57. Crystal structure of 1-(4,4-dimethyl-2,6-dithioxo-1,3,5-triazinan-1-yl)-3-(diethylaminocarbonyl)thiourea, C11H20N6OS3
  58. Crystal structure of methyl 1-(4-fluorobenzyl)-3-phenyl-1H-pyrazole-5-carboxylate, C18H15FN2O2
  59. Crystal structure of 1,1-dimethyl-3-(4-methylphenyl)urea, C10H14N2O
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