metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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catena-Poly[[di­aqua­(4,4′-tri­methyl­ene­di­pyridine-κN)cobalt(II)]-μ-tereph­thalato-κ2O1:O4]

aLiaocheng Vocational and Technical College, LiaoCheng 252000, ShanDong, People's Republic of China
*Correspondence e-mail: q200801@sina.com

(Received 12 December 2008; accepted 22 December 2008; online 8 January 2009)

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[Manna, S. C., Konar, S., Zangrando, E., Okamoto, K., Ribas, J. & Chaudhuri, N. R. (2005). Eur. J. Inorg. Chem. pp. 4646-4654.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(C8H4O4)(C13H14N2)2(H2O)2]

  • Mr = 655.60

  • Monoclinic, P 21 /c

  • 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[Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.]) Tmin = 0.891, Tmax = 0.954

  • 8438 measured reflections

  • 2726 independent reflections

  • 2167 reflections with I > 2σ(I)

  • Rint = 0.068

Refinement
  • R[F2 > 2σ(F2)] = 0.070

  • wR(F2) = 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

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O3—H3A⋯N2i 0.93 1.90 2.820 (5) 171
O3—H3B⋯O2ii 1.03 1.71 2.704 (4) 161
Symmetry codes: (i) [-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) -x, -y, -z.

Data collection: SMART (Bruker, 2001[Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL and local programs.

Supporting information


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 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 top
Bruker SMART 1K CCD area-detector
diffractometer
2726 independent reflections
Radiation source: sealed tube2167 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.068
Detector resolution: 8.192 pixels mm-1θmax = 25.0°, θmin = 1.8°
Thin–slice ω scansh = 1113
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)
k = 811
Tmin = 0.891, Tmax = 0.954l = 1718
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 Å3
0 restraintsΔρmin = 0.62 e Å3
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 mm1
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 reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0700 restraints
wR(F2) = 0.179H-atom parameters constrained
S = 1.13Δρmax = 1.05 e Å3
2726 reflectionsΔρmin = 0.62 e Å3
207 parameters
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)
H10.02630.24930.13590.054*
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)
H40.22630.46040.04050.053*
C50.1259 (4)0.2869 (5)0.0226 (3)0.0449 (12)
H50.14410.24150.07390.054*
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*
H3B0.06790.00890.15450.09 (2)*
H3A0.08370.03070.17530.10 (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)
H170.44360.04820.14840.044*
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, º) 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—C14175 (95)C2—C3—C6—C794.5 (5)
O3i—Co1—O1—C142.6 (4)C4—C3—C6—C784.7 (6)
O3—Co1—O1—C14177.4 (4)C3—C6—C7—C868.8 (6)
N1i—Co1—O1—C1493.7 (4)C6—C7—C8—C9177.5 (4)
N1—Co1—O1—C1486.3 (4)C7—C8—C9—C10118.4 (5)
O1i—Co1—N1—C5130.3 (3)C7—C8—C9—C1262.9 (7)
O1—Co1—N1—C549.7 (3)C12—C9—C10—C110.5 (7)
O3i—Co1—N1—C539.5 (3)C8—C9—C10—C11178.3 (5)
O3—Co1—N1—C5140.5 (3)C13—N2—C11—C101.2 (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—C1121.8 (4)C8—C9—C12—C13178.7 (5)
O3i—Co1—N1—C1149.1 (4)C11—N2—C13—C120.7 (8)
O3—Co1—N1—C130.9 (4)C9—C12—C13—N20.2 (9)
N1i—Co1—N1—C190 (48)Co1—O1—C14—O221.8 (7)
C5—N1—C1—C21.9 (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—C1610.9 (6)
C1—C2—C3—C41.5 (7)O2—C14—C15—C1710.2 (6)
C1—C2—C3—C6177.7 (4)O1—C14—C15—C17171.5 (4)
C2—C3—C4—C52.1 (7)C17—C15—C16—C17ii0.8 (7)
C6—C3—C4—C5177.1 (4)C14—C15—C16—C17ii178.5 (4)
C1—N1—C5—C41.2 (7)C16—C15—C17—C16ii0.8 (7)
Co1—N1—C5—C4170.8 (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, º) 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: (i) x, y, z; (iii) x+1, y1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Co(C8H4O4)(C13H14N2)2(H2O)2]
Mr655.60
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)11.232 (2), 9.3784 (19), 15.182 (3)
β (°) 96.19 (3)
V3)1589.9 (5)
Z2
Radiation typeMo Kα
µ (mm1)0.59
Crystal size (mm)0.20 × 0.14 × 0.08
Data collection
DiffractometerBruker SMART 1K CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2004)
Tmin, Tmax0.891, 0.954
No. of measured, independent and
observed [I > 2σ(I)] reflections
8438, 2726, 2167
Rint0.068
(sin θ/λ)max1)0.594
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.070, 0.179, 1.13
No. of reflections2726
No. of parameters207
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.05, 0.62

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and local programs.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3A···N2i0.931.902.820 (5)171.4
O3—H3B···O2ii1.031.712.704 (4)160.9
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x, y, z.
 

References

First citationBruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationManna, S. C., Konar, S., Zangrando, E., Okamoto, K., Ribas, J. & Chaudhuri, N. R. (2005). Eur. J. Inorg. Chem. pp. 4646–4654.  Web of Science CSD CrossRef Google Scholar
First citationSheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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