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Acta Cryst. (2009). E65, m135    [ doi:10.1107/S1600536808043584 ]

catena-Poly[[diaqua(4,4'-trimethylenedipyridine-[kappa]N)cobalt(II)]-[mu]-terephthalato-[kappa]2O1:O4]

X.-L. Qi

Abstract top

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.

Comment top

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.

Related literature top

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

Experimental top

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 top

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.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and local programs.

Figures top
[Figure 1] 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
[Figure 2] Fig. 2. Partial packing diagram of the title compound.
catena-Poly[[diaqua(4,4'-trimethylenedipyridine-κN)cobalt(II)]- µ-terephthalato-κ2O1:O4] top
Crystal data top
[Co(C8H4O4)(C13H14N2)2(H2O)2]F(000) = 686
Mr = 655.60Dx = 1.369 Mg m−3
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 mm−1
β = 96.19 (3)°T = 293 K
V = 1589.9 (5) Å3Block, purple
Z = 20.20 × 0.14 × 0.08 mm
Data collection top
Bruker SMART 1K CCD area-detector
diffractometer		2726 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 top
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 = 1.13 w = 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 Å−3
0 restraintsΔρmin = −0.62 e Å−3
Crystal data top
[Co(C8H4O4)(C13H14N2)2(H2O)2]V = 1589.9 (5) Å3
Mr = 655.60Z = 2
Monoclinic, P21/cMo Kα radiation
a = 11.232 (2) ŵ = 0.59 mm−1
b = 9.3784 (19) ÅT = 293 K
c = 15.182 (3) Å0.20 × 0.14 × 0.08 mm
β = 96.19 (3)°
Data collection top
Bruker SMART 1K CCD area-detector
diffractometer		2726 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)		2167 reflections with I > 2σ(I)
Tmin = 0.891, Tmax = 0.954Rint = 0.068
8438 measured reflectionsθmax = 25.0°
Refinement top
R[F2 > 2σ(F2)] = 0.070H-atom parameters constrained
wR(F2) = 0.179Δρmax = 1.05 e Å−3
S = 1.13Δρmin = −0.62 e Å−3
2726 reflectionsAbsolute structure: ?
207 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
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) top
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, °) top
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, °) top
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.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O3—H3A···N2i0.931.902.820 (5)171
O3—H3B···O2ii1.031.712.704 (4)161
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x, −y, −z.
references
References top

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.