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Acta Crystallogr Sect E Struct Rep Online. 2010 July 1; 66(Pt 7): m829.
Published online 2010 June 23. doi:  10.1107/S1600536810022385
PMCID: PMC3007002

catena-Poly[[bis­(pyridine-κN)zinc(II)]-μ-benzene-1,4-dicarboxyl­ato-κ2 O 1:O 4]

Abstract

In the title coordination polymer, [Zn(C8H4O4)(C5H5N)2]n, the ZnII atom, located on a twofold rotation axis, is tetra­coordinated by two monodentate O atoms from two different carboxyl­ate groups and two pyridyl N atoms, forming a distorted tetra­hedral geometry. The ZnII atoms are bridged by terephthalate ligands, generating an infinite zigzag chain along [101].

Related literature

For related structures, see: Li et al. (2007 [triangle]); Mori et al. (2004 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m829-scheme1.jpg

Experimental

Crystal data

  • [Zn(C8H4O4)(C5H5N)2]
  • M r = 387.68
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m829-efi1.jpg
  • a = 20.054 (8) Å
  • b = 6.299 (2) Å
  • c = 14.761 (6) Å
  • β = 111.500 (6)°
  • V = 1734.9 (11) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.44 mm−1
  • T = 173 K
  • 0.24 × 0.20 × 0.15 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: numerical (SADABS; Bruker, 1998 [triangle]) T min = 0.724, T max = 0.813
  • 7306 measured reflections
  • 1975 independent reflections
  • 1915 reflections with I > 2σ(I)
  • R int = 0.039

Refinement

  • R[F 2 > 2σ(F 2)] = 0.036
  • wR(F 2) = 0.082
  • S = 1.03
  • 1975 reflections
  • 114 parameters
  • H-atom parameters constrained
  • Δρmax = 0.35 e Å−3
  • Δρmin = −0.22 e Å−3

Data collection: SMART (Bruker, 1998 [triangle]); cell refinement: SAINT (Bruker, 1998 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 [triangle]).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810022385/is2548sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810022385/is2548Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the National High Technology Research and Development Program ("863" Program) of China (No. 2009AA063201).

supplementary crystallographic information

Comment

A great number of the crystal structures of one-dimensional chain complexes have been extensively investigated (Li et al. 2007; Mori et al. 2004), in most of which interchain hydrogen bonds or π–π interactions connect the chains to produce two-dimensional or three-dimensional structures. Here, we report the synthesis and crystal structure of a new one-dimensional zigzag coordination polymer.

In the title coordination polymer, each Zn(II) atom is four-coordinated. The coordination environment around the Zn(II) ions represents a slightly distorted tetrahedral geometry with two pyridyl N and two monodentate O atoms from two different carboxylates. The Zn centers are interconnected by terephthalate ligands to form an infinite zigzag chain. The Zn—O bond distance between Zn(II) and carboxylate O atom is 1.9622 (18) Å, and the Zn—N bond distance between Zn(II) and the N atom of the pyridine is 2.038 (2) Å.

Experimental

A solution containing a 2:1 molar ratio of 1,4-benzenedicarboxylic acid (0.022 g) and zinc nitrate hexahydrate (0.041 g) in a mixture of pyridine (2 ml) and N,N-dimethylformamide (2 ml) was sealed in a 5 ml transparent vitreous reactor and kept at 343 K for 5 days, and then cooled to room temperature. The mixture was filtered and colorless crystals suitable for the X-ray investigation were collected.

Refinement

All H atoms were positioned geometrically (C—H = 0.95 Å) and treated as riding, with Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
A view of the molecular structure of the title compound, with displacement ellipsoids drawn at the 30% probability level. Hydrogen atoms have been omitted for clarity.
Fig. 2.
An illustration of the zigzag chain formed by bridging terephthalate ligands. H atoms have been omitted.

Crystal data

[Zn(C8H4O4)(C5H5N)2]F(000) = 792
Mr = 387.68Dx = 1.484 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 968 reflections
a = 20.054 (8) Åθ = 2.2–27.5°
b = 6.299 (2) ŵ = 1.44 mm1
c = 14.761 (6) ÅT = 173 K
β = 111.500 (6)°Block, colorless
V = 1734.9 (11) Å30.24 × 0.20 × 0.15 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer1975 independent reflections
Radiation source: sealed tube1915 reflections with I > 2σ(I)
graphiteRint = 0.039
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: numerical (SADABS; Bruker, 1998)h = −26→19
Tmin = 0.724, Tmax = 0.813k = −8→8
7306 measured reflectionsl = −19→19

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.082H-atom parameters constrained
S = 1.03w = 1/[σ2(Fo2) + (0.030P)2 + 3.5P] where P = (Fo2 + 2Fc2)/3
1975 reflections(Δ/σ)max < 0.001
114 parametersΔρmax = 0.35 e Å3
0 restraintsΔρmin = −0.22 e Å3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2 σ (F2) is used only for calculating R-factors (gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

xyzUiso*/Ueq
Zn10.00000.39350 (5)0.25000.02669 (12)
O10.07418 (8)0.5959 (2)0.32459 (12)0.0340 (4)
O20.12091 (8)0.3122 (3)0.41504 (13)0.0409 (4)
N10.04941 (9)0.1981 (3)0.18419 (13)0.0300 (4)
C10.18900 (10)0.6311 (3)0.44879 (15)0.0245 (4)
C20.24474 (11)0.5421 (3)0.52709 (15)0.0271 (4)
H20.24100.39960.54570.032*
C30.19468 (11)0.8406 (3)0.42210 (15)0.0265 (4)
H30.15700.90280.36910.032*
C40.12371 (11)0.5003 (3)0.39400 (15)0.0271 (4)
C50.02091 (13)0.0111 (4)0.14623 (17)0.0343 (5)
H5−0.0249−0.02580.14650.041*
C60.05508 (15)−0.1297 (4)0.10692 (19)0.0456 (6)
H60.0332−0.26120.08090.055*
C70.12141 (17)−0.0777 (5)0.1057 (2)0.0539 (8)
H70.1460−0.17200.07840.065*
C80.15136 (16)0.1135 (5)0.1447 (2)0.0543 (8)
H80.19710.15320.14470.065*
C90.11451 (13)0.2473 (4)0.18390 (19)0.0411 (6)
H90.13590.37830.21150.049*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Zn10.01866 (18)0.02270 (19)0.0321 (2)0.0000.00149 (14)0.000
O10.0219 (7)0.0257 (8)0.0404 (9)−0.0005 (6)−0.0049 (6)0.0005 (7)
O20.0300 (8)0.0289 (9)0.0483 (10)−0.0076 (7)−0.0041 (7)0.0063 (7)
N10.0251 (9)0.0318 (10)0.0317 (10)0.0023 (7)0.0087 (7)0.0032 (8)
C10.0182 (9)0.0249 (10)0.0265 (10)−0.0011 (7)0.0036 (8)−0.0023 (8)
C20.0231 (10)0.0205 (9)0.0318 (11)0.0005 (8)0.0033 (8)0.0014 (8)
C30.0190 (9)0.0270 (10)0.0274 (10)0.0024 (8)0.0011 (8)0.0021 (8)
C40.0200 (10)0.0258 (11)0.0299 (11)−0.0003 (8)0.0025 (8)−0.0010 (9)
C50.0328 (12)0.0342 (12)0.0334 (12)0.0020 (9)0.0090 (10)−0.0010 (10)
C60.0526 (16)0.0428 (15)0.0383 (13)0.0090 (12)0.0131 (12)−0.0037 (11)
C70.0598 (19)0.063 (2)0.0457 (16)0.0222 (15)0.0280 (14)0.0043 (14)
C80.0421 (15)0.075 (2)0.0576 (18)0.0072 (14)0.0328 (14)0.0088 (16)
C90.0349 (13)0.0465 (15)0.0450 (14)−0.0031 (11)0.0185 (11)0.0069 (12)

Geometric parameters (Å, °)

Zn1—O11.9621 (15)C3—C2i1.384 (3)
Zn1—N12.0363 (19)C3—H30.9500
O1—C41.286 (2)C5—C61.372 (3)
O2—C41.231 (3)C5—H50.9500
N1—C51.339 (3)C6—C71.377 (4)
N1—C91.343 (3)C6—H60.9500
C1—C31.394 (3)C7—C81.374 (4)
C1—C21.397 (3)C7—H70.9500
C1—C41.507 (3)C8—C91.380 (4)
C2—C3i1.384 (3)C8—H80.9500
C2—H20.9500C9—H90.9500
O1—Zn1—O1ii98.96 (9)O2—C4—O1123.93 (19)
O1—Zn1—N1ii121.77 (8)O2—C4—C1120.10 (18)
O1—Zn1—N1105.02 (8)O1—C4—C1115.94 (18)
O1ii—Zn1—N1121.77 (8)N1—C5—C6122.9 (2)
N1ii—Zn1—N1105.60 (11)N1—C5—H5118.6
C4—O1—Zn1110.39 (13)C6—C5—H5118.6
C5—N1—C9117.9 (2)C5—C6—C7119.1 (3)
C5—N1—Zn1121.59 (15)C5—C6—H6120.4
C9—N1—Zn1120.36 (17)C7—C6—H6120.4
C3—C1—C2119.33 (19)C8—C7—C6118.6 (3)
C3—C1—C4120.72 (18)C8—C7—H7120.7
C2—C1—C4119.95 (19)C6—C7—H7120.7
C3i—C2—C1120.8 (2)C7—C8—C9119.5 (3)
C3i—C2—H2119.6C7—C8—H8120.3
C1—C2—H2119.6C9—C8—H8120.3
C2i—C3—C1119.91 (19)N1—C9—C8122.1 (3)
C2i—C3—H3120.0N1—C9—H9119.0
C1—C3—H3120.0C8—C9—H9119.0

Symmetry codes: (i) −x+1/2, −y+3/2, −z+1; (ii) −x, y, −z+1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS2548).

References

  • Bruker (1998). SMART, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Li, J. K., Ma, C. L., He, G. F. & Qiu, L. L. (2007). J. Coord. Chem.61, 251–261.
  • Mori, W., Takamizawa, S., Kato, C. N., Ohmura, T. & Sato, T. (2004). Micropor. Mesopor. Mater.73, 31–46.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography