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Acta Crystallogr Sect E Struct Rep Online. 2009 February 1; 65(Pt 2): m135.
Published online 2009 January 8. doi:  10.1107/S1600536808043584
PMCID: PMC2968293

catena-Poly[[diaqua­(4,4′-trimethyl­ene­dipyridine-κN)cobalt(II)]-μ-tereph­thalato-κ2 O 1:O 4]

Abstract

The title compound, [Co(C8H4O4)(C13H14N2)2(H2O)2]n, was obtained by the reaction of CoCl2, 4,4′-trimethyl­enedipyridine and terephthalic acid in a 1:1:1 ratio. The octa­hedrally coordinated cobalt ions are bridged by 4,4′-trimethyl­enedipyridine ligands, generating a chain. These chains are further linked by O—H(...)O and O—H(...)N hydrogen bonds, giving a three-dimensional network.

Related literature

For a related structure, see Manna et al. (2005 [triangle]).

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Object name is e-65-0m135-scheme1.jpg

Experimental

Crystal data

  • [Co(C8H4O4)(C13H14N2)2(H2O)2]
  • M r = 655.60
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m135-efi1.jpg
  • a = 11.232 (2) Å
  • b = 9.3784 (19) Å
  • c = 15.182 (3) Å
  • β = 96.19 (3)°
  • V = 1589.9 (5) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 0.59 mm−1
  • T = 293 (2) K
  • 0.20 × 0.14 × 0.08 mm

Data collection

  • Bruker SMART 1K CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 2004 [triangle]) T min = 0.891, T max = 0.954
  • 8438 measured reflections
  • 2726 independent reflections
  • 2167 reflections with I > 2σ(I)
  • R int = 0.068

Refinement

  • R[F 2 > 2σ(F 2)] = 0.070
  • wR(F 2) = 0.179
  • S = 1.13
  • 2726 reflections
  • 207 parameters
  • H-atom parameters constrained
  • Δρmax = 1.05 e Å−3
  • Δρmin = −0.62 e Å−3

Data collection: SMART (Bruker, 2001 [triangle]); cell refinement: SAINT (Bruker, 2001 [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 and local programs.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808043584/bt2833sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808043584/bt2833Isup2.hkl

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

supplementary crystallographic information

Comment

Co is six-coordinated by two terephthalate O atoms, two N atoms of 4,4'-trimethylenedipyridines and two water molecules in a distorted octahedral fashion. The Co—O and Co—N bond lengthes are in the normal range. The 4,4'-trimethylenedipyridine and terephthalate ligands adopt bidentate coordinated modes. As shown in Fig. 2, a chain structure is formed. These chains are further linked by O—H···O and O—H···N hydrogen bonds to generate a three-dimensional network.

Experimental

CoCl2(1.0 mmol), terephthalic acid (1 mmol), and 4,4'-trimethylenedipyridine (1 mmol) were dissolved in water (10 ml). The solution was heated in a 25 ml Teflon lined reaction vessel at 433 K for ca 3 days and then cooled to room temperature. Purple crystals were obtained in a yield of 65%.

Refinement

All non-water H atoms were positioned geometrically and refined by using a riding model with C—H = 0.93–0.96 Å and with Uiso(H) = 1.2 times Ueq(C), the water H atoms are firstly found, then refined freely.

Figures

Fig. 1.
An ORTEP view of the Co centre and its surrounding ligands with 50% displacement ellipsoids for non-H atoms. Symmetry code: (A) -x,-y,-z
Fig. 2.
Partial packing diagram of the title compound.

Crystal data

[Co(C8H4O4)(C13H14N2)2(H2O)2]F(000) = 686
Mr = 655.60Dx = 1.369 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 11.232 (2) ÅCell parameters from 3657 reflections
b = 9.3784 (19) Åθ = 1.4–27.9°
c = 15.182 (3) ŵ = 0.59 mm1
β = 96.19 (3)°T = 293 K
V = 1589.9 (5) Å3Block, purple
Z = 20.20 × 0.14 × 0.08 mm

Data collection

Bruker SMART 1K CCD area-detector diffractometer2726 independent reflections
Radiation source: sealed tube2167 reflections with I > 2σ(I)
graphiteRint = 0.068
Detector resolution: 8.192 pixels mm-1θmax = 25.0°, θmin = 1.8°
Thin–slice ω scansh = −11→13
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)k = −8→11
Tmin = 0.891, Tmax = 0.954l = −17→18
8438 measured reflections

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)] = 0.070Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.179H-atom parameters constrained
S = 1.13w = 1/[σ2(Fo2) + (0.0794P)2 + 1.059P] where P = (Fo2 + 2Fc2)/3
2726 reflections(Δ/σ)max < 0.001
207 parametersΔρmax = 1.05 e Å3
0 restraintsΔρmin = −0.62 e Å3

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

xyzUiso*/Ueq
Co10.00000.00000.00000.0323 (3)
O10.1776 (3)−0.0428 (3)−0.0026 (2)0.0398 (8)
O20.2160 (3)−0.0377 (4)−0.1445 (2)0.0560 (10)
O30.0130 (3)−0.0481 (3)0.1394 (2)0.0409 (8)
N10.0522 (3)0.2209 (4)0.0279 (2)0.0369 (9)
N20.7841 (4)0.5278 (5)0.2442 (3)0.0562 (12)
C10.0265 (4)0.2912 (5)0.1005 (3)0.0451 (11)
H1−0.02630.24930.13590.054*
C20.0747 (4)0.4234 (5)0.1253 (3)0.0479 (12)
H20.05440.46740.17650.057*
C30.1530 (4)0.4901 (5)0.0739 (3)0.0378 (10)
C40.1764 (4)0.4190 (5)−0.0026 (3)0.0443 (11)
H40.22630.4604−0.04050.053*
C50.1259 (4)0.2869 (5)−0.0226 (3)0.0449 (12)
H50.14410.2415−0.07390.054*
C60.2111 (4)0.6317 (5)0.1003 (4)0.0541 (14)
H6A0.16000.68370.13670.065*
H6B0.21830.68770.04740.065*
C70.3359 (4)0.6137 (5)0.1519 (4)0.0544 (14)
H7A0.36180.70560.17640.065*
H7B0.32900.54960.20130.065*
C80.4310 (5)0.5574 (6)0.0989 (4)0.0612 (15)
H8A0.43610.61910.04820.073*
H8B0.40730.46340.07670.073*
C90.5539 (4)0.5470 (5)0.1508 (3)0.0436 (11)
C100.6121 (4)0.4186 (5)0.1644 (4)0.0516 (13)
H100.57550.33470.14290.062*
H3B−0.0679−0.00890.15450.09 (2)*
H3A0.0837−0.03070.17530.10 (2)*
C110.7261 (4)0.4149 (6)0.2103 (4)0.0553 (14)
H110.76390.32680.21760.066*
C120.6140 (5)0.6664 (6)0.1852 (4)0.0579 (14)
H120.57870.75590.17800.070*
C130.7273 (5)0.6521 (6)0.2307 (4)0.0602 (15)
H130.76600.73410.25310.072*
C140.2472 (4)−0.0357 (4)−0.0632 (3)0.0364 (10)
C150.3786 (3)−0.0193 (4)−0.0300 (3)0.0314 (9)
C160.4142 (4)0.0107 (4)0.0580 (3)0.0365 (10)
H160.35660.01880.09740.044*
C170.4659 (4)−0.0292 (4)−0.0888 (3)0.0366 (10)
H170.4436−0.0482−0.14840.044*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.0153 (5)0.0487 (5)0.0327 (5)−0.0044 (3)0.0010 (3)0.0013 (3)
O10.0221 (16)0.0495 (18)0.048 (2)−0.0006 (12)0.0036 (14)0.0055 (13)
O20.0219 (18)0.099 (3)0.046 (2)−0.0012 (16)0.0005 (15)−0.0105 (18)
O30.0268 (17)0.0538 (19)0.041 (2)−0.0043 (13)−0.0021 (14)0.0020 (14)
N10.028 (2)0.041 (2)0.042 (2)−0.0028 (15)0.0054 (16)−0.0006 (16)
N20.033 (2)0.089 (4)0.046 (3)0.002 (2)−0.0009 (19)0.011 (2)
C10.035 (3)0.054 (3)0.047 (3)−0.003 (2)0.009 (2)−0.001 (2)
C20.041 (3)0.058 (3)0.044 (3)0.004 (2)0.000 (2)−0.009 (2)
C30.024 (2)0.043 (2)0.044 (3)0.0035 (18)−0.0083 (18)−0.001 (2)
C40.036 (3)0.048 (3)0.049 (3)−0.011 (2)0.003 (2)0.003 (2)
C50.038 (3)0.049 (3)0.049 (3)−0.009 (2)0.008 (2)0.000 (2)
C60.034 (3)0.048 (3)0.077 (4)0.000 (2)−0.009 (2)−0.011 (2)
C70.037 (3)0.056 (3)0.068 (4)0.001 (2)−0.006 (2)−0.019 (3)
C80.039 (3)0.078 (4)0.062 (4)0.001 (3)−0.012 (3)−0.014 (3)
C90.032 (3)0.053 (3)0.045 (3)0.003 (2)−0.002 (2)−0.002 (2)
C100.044 (3)0.049 (3)0.062 (4)−0.006 (2)0.006 (2)0.007 (2)
C110.041 (3)0.064 (4)0.062 (4)0.012 (3)0.009 (3)0.022 (3)
C120.046 (3)0.054 (3)0.071 (4)0.004 (2)−0.009 (3)−0.005 (3)
C130.045 (3)0.069 (4)0.064 (4)−0.016 (3)−0.008 (3)−0.006 (3)
C140.020 (2)0.043 (3)0.046 (3)−0.0023 (17)0.0015 (19)0.0016 (19)
C150.018 (2)0.037 (2)0.039 (3)0.0000 (16)0.0010 (17)−0.0018 (17)
C160.018 (2)0.054 (3)0.039 (3)−0.0029 (18)0.0095 (18)−0.0022 (19)
C170.023 (2)0.046 (3)0.040 (3)−0.0013 (17)0.0032 (18)−0.0042 (18)

Geometric parameters (Å, °)

Co1—O1i2.039 (3)C6—H6A0.9700
Co1—O12.039 (3)C6—H6B0.9700
Co1—O3i2.154 (3)C7—C81.500 (7)
Co1—O32.154 (3)C7—H7A0.9700
Co1—N1i2.183 (3)C7—H7B0.9700
Co1—N12.183 (3)C8—C91.517 (7)
O1—C141.271 (5)C8—H8A0.9700
O2—C141.247 (6)C8—H8B0.9700
O3—H3B1.0283C9—C101.375 (7)
O3—H3A0.9271C9—C121.381 (7)
N1—C51.339 (5)C10—C111.390 (7)
N1—C11.342 (6)C10—H100.9300
N2—C111.318 (7)C11—H110.9300
N2—C131.334 (7)C12—C131.388 (7)
C1—C21.389 (7)C12—H120.9300
C1—H10.9300C13—H130.9300
C2—C31.386 (7)C14—C151.515 (6)
C2—H20.9300C15—C161.381 (6)
C3—C41.388 (6)C15—C171.398 (6)
C3—C61.515 (6)C16—C17ii1.389 (6)
C4—C51.383 (6)C16—H160.9300
C4—H40.9300C17—C16ii1.389 (6)
C5—H50.9300C17—H170.9300
C6—C71.540 (7)
O1i—Co1—O1180.00 (16)C7—C6—H6B109.1
O1i—Co1—O3i90.88 (12)H6A—C6—H6B107.9
O1—Co1—O3i89.12 (12)C8—C7—C6115.3 (5)
O1i—Co1—O389.12 (12)C8—C7—H7A108.5
O1—Co1—O390.88 (12)C6—C7—H7A108.5
O3i—Co1—O3180.00 (16)C8—C7—H7B108.5
O1i—Co1—N1i86.99 (12)C6—C7—H7B108.5
O1—Co1—N1i93.01 (12)H7A—C7—H7B107.5
O3i—Co1—N1i91.14 (12)C7—C8—C9113.9 (4)
O3—Co1—N1i88.86 (12)C7—C8—H8A108.8
O1i—Co1—N193.01 (12)C9—C8—H8A108.8
O1—Co1—N186.99 (12)C7—C8—H8B108.8
O3i—Co1—N188.86 (12)C9—C8—H8B108.8
O3—Co1—N191.14 (12)H8A—C8—H8B107.7
N1i—Co1—N1180.0 (2)C10—C9—C12116.7 (5)
C14—O1—Co1133.1 (3)C10—C9—C8121.7 (4)
Co1—O3—H3B100.2C12—C9—C8121.6 (4)
Co1—O3—H3A120.2C9—C10—C11119.6 (5)
H3B—O3—H3A121.8C9—C10—H10120.2
C5—N1—C1116.4 (4)C11—C10—H10120.2
C5—N1—Co1119.8 (3)N2—C11—C10124.4 (5)
C1—N1—Co1123.3 (3)N2—C11—H11117.8
C11—N2—C13115.7 (4)C10—C11—H11117.8
N1—C1—C2123.3 (4)C9—C12—C13119.6 (5)
N1—C1—H1118.4C9—C12—H12120.2
C2—C1—H1118.4C13—C12—H12120.2
C3—C2—C1120.2 (4)N2—C13—C12124.0 (5)
C3—C2—H2119.9N2—C13—H13118.0
C1—C2—H2119.9C12—C13—H13118.0
C2—C3—C4116.3 (4)O2—C14—O1125.9 (4)
C2—C3—C6121.9 (4)O2—C14—C15119.4 (4)
C4—C3—C6121.8 (4)O1—C14—C15114.7 (4)
C5—C4—C3120.2 (4)C16—C15—C17118.8 (4)
C5—C4—H4119.9C16—C15—C14120.8 (4)
C3—C4—H4119.9C17—C15—C14120.4 (4)
N1—C5—C4123.5 (4)C15—C16—C17ii121.3 (4)
N1—C5—H5118.2C15—C16—H16119.3
C4—C5—H5118.2C17ii—C16—H16119.3
C3—C6—C7112.4 (4)C16ii—C17—C15119.9 (4)
C3—C6—H6A109.1C16ii—C17—H17120.1
C7—C6—H6A109.1C15—C17—H17120.1
C3—C6—H6B109.1
O1i—Co1—O1—C14−175 (95)C2—C3—C6—C794.5 (5)
O3i—Co1—O1—C142.6 (4)C4—C3—C6—C7−84.7 (6)
O3—Co1—O1—C14−177.4 (4)C3—C6—C7—C868.8 (6)
N1i—Co1—O1—C1493.7 (4)C6—C7—C8—C9177.5 (4)
N1—Co1—O1—C14−86.3 (4)C7—C8—C9—C10118.4 (5)
O1i—Co1—N1—C5−130.3 (3)C7—C8—C9—C12−62.9 (7)
O1—Co1—N1—C549.7 (3)C12—C9—C10—C11−0.5 (7)
O3i—Co1—N1—C5−39.5 (3)C8—C9—C10—C11178.3 (5)
O3—Co1—N1—C5140.5 (3)C13—N2—C11—C10−1.2 (8)
N1i—Co1—N1—C582 (48)C9—C10—C11—N21.1 (8)
O1i—Co1—N1—C158.2 (4)C10—C9—C12—C130.0 (8)
O1—Co1—N1—C1−121.8 (4)C8—C9—C12—C13−178.7 (5)
O3i—Co1—N1—C1149.1 (4)C11—N2—C13—C120.7 (8)
O3—Co1—N1—C1−30.9 (4)C9—C12—C13—N2−0.2 (9)
N1i—Co1—N1—C1−90 (48)Co1—O1—C14—O2−21.8 (7)
C5—N1—C1—C2−1.9 (7)Co1—O1—C14—C15156.4 (3)
Co1—N1—C1—C2169.9 (3)O2—C14—C15—C16167.4 (4)
N1—C1—C2—C30.5 (7)O1—C14—C15—C16−10.9 (6)
C1—C2—C3—C41.5 (7)O2—C14—C15—C17−10.2 (6)
C1—C2—C3—C6−177.7 (4)O1—C14—C15—C17171.5 (4)
C2—C3—C4—C5−2.1 (7)C17—C15—C16—C17ii−0.8 (7)
C6—C3—C4—C5177.1 (4)C14—C15—C16—C17ii−178.5 (4)
C1—N1—C5—C41.2 (7)C16—C15—C17—C16ii0.8 (7)
Co1—N1—C5—C4−170.8 (4)C14—C15—C17—C16ii178.5 (4)
C3—C4—C5—N10.8 (7)

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

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O3—H3A···N2iii0.931.902.820 (5)171
O3—H3B···O2i1.031.712.704 (4)161

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT2833).

References

  • Bruker (2001). SMART and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Manna, S. C., Konar, S., Zangrando, E., Okamoto, K., Ribas, J. & Chaudhuri, N. R. (2005). Eur. J. Inorg. Chem. pp. 4646–4654.
  • Sheldrick, G. M. (2004). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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