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Acta Crystallogr Sect E Struct Rep Online. 2008 April 1; 64(Pt 4): m544.
Published online 2008 March 14. doi:  10.1107/S1600536808006685
PMCID: PMC2960972

catena-Poly[[dichloridocobalt(II)]-μ-1,2-di-4-pyridylethane-κ2 N:N′]

Abstract

In the title compound, [CoCl2(C12H12N2)], the CoII atom is coordinated in a tetra­hedral geometry by the N atoms of two different 1,3-di-4-pyridylpropane ligands. The compound adopts a linear chain structure.

Related literature

For related literature, see: Carlucci et al. (2003 [triangle]); Fujita et al. (1998 [triangle]).

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Object name is e-64-0m544-scheme1.jpg

Experimental

Crystal data

  • [CoCl2(C12H12N2)]
  • M r = 314.07
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m544-efi1.jpg
  • a = 5.3979 (17) Å
  • b = 8.806 (3) Å
  • c = 14.018 (4) Å
  • α = 87.988 (5)°
  • β = 84.165 (5)°
  • γ = 84.475 (5)°
  • V = 659.6 (4) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.68 mm−1
  • T = 298 (2) K
  • 0.27 × 0.21 × 0.18 mm

Data collection

  • Bruker APEXII area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.659, T max = 0.751
  • 3306 measured reflections
  • 2297 independent reflections
  • 1942 reflections with I > 2σ(I)
  • R int = 0.022

Refinement

  • R[F 2 > 2σ(F 2)] = 0.047
  • wR(F 2) = 0.134
  • S = 1.02
  • 2297 reflections
  • 154 parameters
  • H-atom parameters constrained
  • Δρmax = 0.98 e Å−3
  • Δρmin = −1.01 e Å−3

Data collection: APEX2 (Bruker, 2004 [triangle]); cell refinement: SAINT (Bruker, 2004 [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.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808006685/ng2432sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808006685/ng2432Isup2.hkl

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

Acknowledgments

The author is grateful to Shuren University for financial support.

supplementary crystallographic information

Comment

In recent years, a wide range of 1-D infinite frameworks have been generated by using simple linear bifunctional ligands (Fujita et al., 1998), such as 4,4'-bipyridine (bpy). 1,3-bis(4-pyridyl)propane (bpp) ligand is typical building element for the assembly of infinite architectures. A double-helical chain was synthesized based on transition metal salts and bpp ligand (Carlucci et al., 2003). In this paper, we report the synthesis and crystal structure of the title complex,(I).

As shown in Fig. 1, the complex I is connected to two bpp ligands. The CoII atom in compound I is tetrahedrally coordinatted by two N atoms of two different pyridyl groups and two chloride anions. This coordination mode of cobalt atom is very rare so far. The CoII ions are linked by bpp liagnds and form a zigzag chain. The Co—N bond lengths range from 2.036 (3) to 2.038 (3)Å (Table1). While the Co—Cl bond lengths range from 2.2399 (10) to 2.2484 (11) Å.

Experimental

CoCl2(0.023 g, 0.012 mmol), bpp(0.021 g, 0.013 mmol) were added in a mixed solvent of methanol and benzene, the mixture was heated for ten hours under reflux. During the process stirring and influx were required. The resultant was then filtered to give a pure solution which was infiltrated by diethyl ether freely in a closed vessel, Six weeks later some single crystals was obtained.

Refinement

The H atoms (pyridine ring) were placed in calculated positions [Csp2—H = 0.93 Å] and refined using a riding model, with Uiso(H) = 1.2Ueq(C). The maximum peak hole is located on the Co1 with 1.01 Å.

Figures

Fig. 1.
The asymmetric unit of (I), showing 30% probability displacement ellipsoids. (symmetrical code: (i) 1 - x, -y, 1 - z).

Crystal data

[CoCl2(C12H12N2)]Z = 2
Mr = 314.07F000 = 318
Triclinic, P1Dx = 1.581 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 5.3979 (17) ÅCell parameters from 2297 reflections
b = 8.806 (3) Åθ = 1.5–25.1º
c = 14.018 (4) ŵ = 1.68 mm1
α = 87.988 (5)ºT = 298 (2) K
β = 84.165 (5)ºBlock, pink
γ = 84.475 (5)º0.27 × 0.21 × 0.18 mm
V = 659.6 (4) Å3

Data collection

Bruker APEXII area-detector diffractometer2297 independent reflections
Radiation source: fine-focus sealed tube1942 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.022
T = 298(2) Kθmax = 25.1º
[var phi] and ω scansθmin = 1.5º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −4→6
Tmin = 0.659, Tmax = 0.752k = −9→10
3306 measured reflectionsl = −16→16

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.047H-atom parameters constrained
wR(F2) = 0.134  w = 1/[σ2(Fo2) + (0.1008P)2] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
2297 reflectionsΔρmax = 0.98 e Å3
154 parametersΔρmin = −1.01 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none

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 > 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
Co10.88487 (8)0.54658 (4)0.74750 (3)0.0386 (2)
Cl11.00798 (18)0.70640 (10)0.62711 (6)0.0535 (3)
Cl21.14897 (18)0.42183 (11)0.84306 (6)0.0533 (3)
N10.7275 (5)0.3806 (3)0.68363 (19)0.0403 (6)
N20.6308 (5)0.6763 (3)0.8353 (2)0.0421 (7)
C10.5435 (7)0.4131 (4)0.6281 (3)0.0456 (8)
H10.48510.51510.62000.055*
C20.4336 (7)0.3066 (4)0.5819 (3)0.0489 (9)
H20.30530.33620.54380.059*
C30.5184 (7)0.1528 (4)0.5933 (2)0.0466 (8)
C40.7079 (8)0.1187 (4)0.6500 (3)0.0564 (10)
H40.77110.01760.65850.068*
C50.8076 (7)0.2329 (4)0.6950 (3)0.0518 (9)
H50.93430.20620.73440.062*
C60.4098 (7)0.0307 (4)0.5416 (3)0.0536 (9)
H6A0.25470.07300.51760.064*
H6B0.3720−0.05230.58640.064*
C70.4596 (8)0.7756 (4)0.7979 (3)0.0561 (10)
H70.46110.78580.73160.067*
C80.2815 (8)0.8629 (5)0.8552 (3)0.0628 (11)
H80.16520.93040.82700.075*
C90.2745 (7)0.8507 (4)0.9545 (3)0.0508 (9)
C100.4501 (8)0.7480 (5)0.9904 (3)0.0582 (10)
H100.45270.73541.05650.070*
C110.6216 (7)0.6636 (4)0.9308 (3)0.0532 (9)
H110.73720.59420.95780.064*
C120.0852 (8)0.9406 (4)1.0232 (3)0.0610 (11)
H12A−0.01640.86971.05980.073*
H12B0.17460.99031.06800.073*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.0492 (3)0.0344 (3)0.0329 (3)−0.0032 (2)−0.0083 (2)−0.00010 (19)
Cl10.0644 (6)0.0466 (5)0.0484 (5)−0.0056 (4)−0.0054 (4)0.0137 (4)
Cl20.0599 (6)0.0565 (6)0.0444 (5)−0.0006 (4)−0.0178 (4)0.0065 (4)
N10.0491 (16)0.0361 (15)0.0366 (15)−0.0040 (12)−0.0079 (12)−0.0013 (11)
N20.0495 (16)0.0389 (15)0.0389 (15)−0.0014 (12)−0.0116 (12)−0.0018 (12)
C10.055 (2)0.0361 (18)0.046 (2)−0.0001 (15)−0.0103 (16)−0.0003 (15)
C20.055 (2)0.049 (2)0.045 (2)−0.0050 (16)−0.0140 (16)−0.0012 (16)
C30.057 (2)0.044 (2)0.0397 (19)−0.0111 (16)−0.0043 (16)−0.0026 (15)
C40.076 (3)0.0332 (19)0.063 (3)−0.0038 (17)−0.020 (2)−0.0002 (17)
C50.064 (2)0.039 (2)0.055 (2)−0.0021 (16)−0.0222 (18)−0.0003 (16)
C60.066 (2)0.049 (2)0.049 (2)−0.0170 (18)−0.0087 (18)−0.0057 (17)
C70.070 (2)0.060 (2)0.0354 (19)0.0119 (19)−0.0096 (17)0.0024 (17)
C80.068 (3)0.065 (3)0.050 (2)0.023 (2)−0.0088 (19)0.0051 (19)
C90.060 (2)0.047 (2)0.043 (2)0.0028 (17)−0.0025 (16)−0.0014 (16)
C100.070 (3)0.065 (3)0.0367 (19)0.012 (2)−0.0080 (17)−0.0022 (17)
C110.061 (2)0.053 (2)0.045 (2)0.0080 (17)−0.0085 (17)−0.0017 (17)
C120.070 (3)0.061 (3)0.047 (2)0.012 (2)−0.0005 (19)0.0018 (18)

Geometric parameters (Å, °)

Co1—N12.036 (3)C5—H50.9300
Co1—N22.038 (3)C6—C6i1.521 (7)
Co1—Cl22.2399 (10)C6—H6A0.9700
Co1—Cl12.2484 (11)C6—H6B0.9700
N1—C11.327 (4)C7—C81.379 (5)
N1—C51.340 (4)C7—H70.9300
N2—C111.335 (5)C8—C91.390 (5)
N2—C71.343 (5)C8—H80.9300
C1—C21.370 (5)C9—C101.368 (5)
C1—H10.9300C9—C121.514 (5)
C2—C31.397 (5)C10—C111.364 (5)
C2—H20.9300C10—H100.9300
C3—C41.362 (5)C11—H110.9300
C3—C61.512 (5)C12—C12ii1.500 (8)
C4—C51.385 (5)C12—H12A0.9700
C4—H40.9300C12—H12B0.9700
N1—Co1—N2112.50 (11)C3—C6—C6i111.5 (4)
N1—Co1—Cl2105.20 (8)C3—C6—H6A109.3
N2—Co1—Cl2106.04 (8)C6i—C6—H6A109.3
N1—Co1—Cl1105.09 (9)C3—C6—H6B109.3
N2—Co1—Cl1104.94 (9)C6i—C6—H6B109.3
Cl2—Co1—Cl1123.22 (4)H6A—C6—H6B108.0
C1—N1—C5116.8 (3)N2—C7—C8121.8 (3)
C1—N1—Co1121.9 (2)N2—C7—H7119.1
C5—N1—Co1121.3 (2)C8—C7—H7119.1
C11—N2—C7117.5 (3)C7—C8—C9120.5 (4)
C11—N2—Co1122.3 (2)C7—C8—H8119.7
C7—N2—Co1120.2 (2)C9—C8—H8119.7
N1—C1—C2124.5 (3)C10—C9—C8116.2 (3)
N1—C1—H1117.8C10—C9—C12119.4 (3)
C2—C1—H1117.8C8—C9—C12124.4 (4)
C1—C2—C3118.7 (3)C11—C10—C9121.0 (4)
C1—C2—H2120.7C11—C10—H10119.5
C3—C2—H2120.7C9—C10—H10119.5
C4—C3—C2117.2 (3)N2—C11—C10122.9 (3)
C4—C3—C6121.9 (3)N2—C11—H11118.5
C2—C3—C6120.9 (3)C10—C11—H11118.5
C3—C4—C5120.7 (3)C12ii—C12—C9115.1 (4)
C3—C4—H4119.6C12ii—C12—H12A108.5
C5—C4—H4119.6C9—C12—H12A108.5
N1—C5—C4122.1 (3)C12ii—C12—H12B108.5
N1—C5—H5118.9C9—C12—H12B108.5
C4—C5—H5118.9H12A—C12—H12B107.5
N2—Co1—N1—C158.9 (3)C6—C3—C4—C5178.7 (4)
Cl2—Co1—N1—C1173.9 (3)C1—N1—C5—C41.1 (6)
Cl1—Co1—N1—C1−54.7 (3)Co1—N1—C5—C4−178.1 (3)
N2—Co1—N1—C5−121.9 (3)C3—C4—C5—N1−1.4 (7)
Cl2—Co1—N1—C5−6.9 (3)C4—C3—C6—C6i−72.0 (6)
Cl1—Co1—N1—C5124.5 (3)C2—C3—C6—C6i105.6 (5)
N1—Co1—N2—C11106.3 (3)C11—N2—C7—C80.6 (6)
Cl2—Co1—N2—C11−8.2 (3)Co1—N2—C7—C8178.6 (3)
Cl1—Co1—N2—C11−140.0 (3)N2—C7—C8—C90.2 (7)
N1—Co1—N2—C7−71.5 (3)C7—C8—C9—C10−0.6 (7)
Cl2—Co1—N2—C7174.0 (3)C7—C8—C9—C12−179.5 (4)
Cl1—Co1—N2—C742.2 (3)C8—C9—C10—C110.3 (6)
C5—N1—C1—C2−0.5 (6)C12—C9—C10—C11179.2 (4)
Co1—N1—C1—C2178.8 (3)C7—N2—C11—C10−1.0 (6)
N1—C1—C2—C30.1 (6)Co1—N2—C11—C10−178.9 (3)
C1—C2—C3—C4−0.3 (6)C9—C10—C11—N20.6 (7)
C1—C2—C3—C6−178.0 (3)C10—C9—C12—C12ii175.1 (5)
C2—C3—C4—C51.0 (6)C8—C9—C12—C12ii−6.1 (8)

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG2432).

References

  • Bruker (2004). APEX2 and SAINT Bruker AXS Inc, Madison, Wisconsin, USA.
  • Carlucci, L., Ciani, G., Proserpio, D. M. & Rizzato, S. (2003). CrystEngComm, 5, 190–199.
  • Fujita, M., Sasaki, O., Watanabe, K., Ogura, K. & Yamaguchi, K. (1998). New J. Chem. pp. 189–191.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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