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Acta Crystallogr Sect E Struct Rep Online. 2008 October 1; 64(Pt 10): m1254.
Published online 2008 September 6. doi:  10.1107/S1600536808027980
PMCID: PMC2959288

catena-Poly[cadmium(II)-μ-benzene-1,2-diamine-κ2 N:N′-di-μ-chlorido]

Abstract

The title compound, [CdCl2(C6H8N2)]n, is a coordination polymer prepared by the hydro­thermal reaction of cadmium chloride and o-diamino­benzene. The cadmium cation, located on an inversion center, is octa­hedrally coordinated by four Cl atoms at equatorial sites and two N atoms from two ligands at the axial sites. Cd atoms are bridged by Cl atoms, forming extended chains parallel to [010]. Neighboring chains are connected by N—H(...)Cl hydrogen bonds.

Related literature

For related literature, see: Choi et al. (1999 [triangle]); Spingler et al. (2001 [triangle]); Fu & Zhao (2007 [triangle]).

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Object name is e-64-m1254-scheme1.jpg

Experimental

Crystal data

  • [CdCl2(C6H8N2)]
  • M r = 291.44
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1254-efi1.jpg
  • a = 6.1235 (6) Å
  • b = 7.5473 (5) Å
  • c = 10.1081 (6) Å
  • β = 105.23 (10)°
  • V = 450.75 (6) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 2.95 mm−1
  • T = 293 (2) K
  • 0.18 × 0.15 × 0.14 mm

Data collection

  • Rigaku SCXmini diffractometer
  • Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 [triangle]) T min = 0.595, T max = 0.660
  • 4700 measured reflections
  • 1109 independent reflections
  • 1020 reflections with I > 2σ(I)
  • R int = 0.029

Refinement

  • R[F 2 > 2σ(F 2)] = 0.018
  • wR(F 2) = 0.040
  • S = 1.22
  • 1109 reflections
  • 56 parameters
  • H-atom parameters constrained
  • Δρmax = 0.25 e Å−3
  • Δρmin = −0.35 e Å−3

Data collection: CrystalClear (Rigaku, 2005 [triangle]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL/PC (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97 and PRPKAPPA (Ferguson, 1999 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808027980/bx2174sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808027980/bx2174Isup2.hkl

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

Acknowledgments

This work was supported by a Start-up Grant from Southeast University to ZRQ.

supplementary crystallographic information

Comment

Coordination frameworks have received much attention over the past decade due to their potential applications. Scientists have dedicated much attention to coordination compounds which constructed by ligands with diamino coordination sites (Choi et al., 1999; Fu et al., 2007), since cis-diamminedichloroplatium(II) received Food and Drug Administration's approval in 1979 for use as an anticancer drug (Spingler et al., 2001). The title compound, [CdCl2(C6H8N2)]n, is a coordination polymer prepared by the hydrothermal reaction of cadmium chloride and o-diaminobenzene.The Cd cation is located on the inversion center and octahedrally coordinated by four Cl atoms at equatorial sites and two N atoms from two ligands at the axial sites. Cd cations are bridged by Cl atoms to form a one-dimensional extended chain. The neighboring chains are binded by N—H···Cl hydrogen bonds.(Table 1) to form a two-dimensional network (Fig. 2).

Experimental

A mixture of CdCl2 (0.0366 g, 0.2 mmol) and benzene-1,2-diamine (0.0216 g, 0.2 mmol) in H2O (4 ml) was heated in Pyrex tube at 100°C for two days. After slowly cooling down to room temperature over a period of 10 h, colorless crystals of the title compound suitable for diffraction were isolated.

Refinement

Positional parameters of all the H atoms were calculated geometrically and were allowed to ride on the C, N atoms to which they are bonded, with C—H = 0.93 Å, N—H = 0.90 Å and with Uiso(H) = 1.2 Ueq(C).

Figures

Fig. 1.
A partial packing diagram of the title compound, with the displacement ellipsoids were drawn at the 30% probability level. [Symmetry codes: (A) 1-x, -y, 1-z; (B) 1-x, -12+y, 1-z; (C) +x, 1/2-y, +z.]
Fig. 2.
Part of the structure of (I), showing two-dimensional extended polymeric network. Dotted lines show intermolecular hydrogen bonding.

Crystal data

[CdCl2(C6H8N2)]F(000) = 280
Mr = 291.44Dx = 2.147 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 4460 reflections
a = 6.1235 (6) Åθ = 3.1–27.5°
b = 7.5473 (5) ŵ = 2.95 mm1
c = 10.1081 (6) ÅT = 293 K
β = 105.230 (1)°Prism, colourless
V = 450.75 (6) Å30.18 × 0.15 × 0.14 mm
Z = 2

Data collection

Rigaku SCXmini diffractometer1109 independent reflections
Radiation source: fine-focus sealed tube1020 reflections with I > 2σ(I)
graphiteRint = 0.029
Detector resolution: 13.6612 pixels mm-1θmax = 27.5°, θmin = 3.4°
CCD profile fitting scansh = −7→7
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005)k = −9→9
Tmin = 0.595, Tmax = 0.660l = −13→13
4700 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.018H-atom parameters constrained
wR(F2) = 0.040w = 1/[σ2(Fo2) + (0.0114P)2 + 0.0467P] where P = (Fo2 + 2Fc2)/3
S = 1.22(Δ/σ)max < 0.001
1109 reflectionsΔρmax = 0.25 e Å3
56 parametersΔρmin = −0.35 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.115 (2)

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
Cd10.50000.00000.50000.02699 (11)
Cl10.26524 (11)0.25000.58281 (8)0.03186 (18)
Cl20.62145 (13)0.25000.35295 (7)0.03336 (19)
N10.8292 (3)0.0596 (2)0.67983 (17)0.0290 (4)
H1A0.8687−0.05460.70420.043*
H1B0.93410.10800.64390.043*
C20.7996 (3)0.1574 (2)0.79569 (18)0.0249 (4)
C30.7561 (3)0.0677 (3)0.9058 (2)0.0348 (5)
H30.7530−0.05550.90560.042*
C40.7174 (3)0.1588 (3)1.0153 (2)0.0411 (5)
H40.69130.09711.08930.049*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cd10.03100 (15)0.02342 (14)0.02722 (15)−0.00010 (7)0.00882 (10)−0.00260 (7)
Cl10.0293 (4)0.0263 (4)0.0466 (4)0.0000.0218 (3)0.000
Cl20.0499 (4)0.0270 (4)0.0289 (4)0.0000.0205 (3)0.000
N10.0290 (9)0.0270 (8)0.0324 (9)−0.0003 (7)0.0108 (8)−0.0011 (7)
C20.0180 (8)0.0319 (10)0.0234 (9)−0.0015 (7)0.0031 (7)−0.0008 (8)
C30.0284 (10)0.0391 (12)0.0348 (11)−0.0017 (9)0.0045 (9)0.0089 (10)
C40.0308 (11)0.0662 (15)0.0271 (10)−0.0034 (10)0.0093 (9)0.0071 (10)

Geometric parameters (Å, °)

Cd1—N1i2.3758 (17)N1—H1A0.9113
Cd1—N12.3758 (17)N1—H1B0.8946
Cd1—Cl22.6274 (5)C2—C31.387 (3)
Cd1—Cl2i2.6274 (5)C2—C2iii1.398 (4)
Cd1—Cl1i2.6381 (5)C3—C41.375 (3)
Cd1—Cl12.6381 (5)C3—H30.9300
Cl1—Cd1ii2.6381 (5)C4—C4iii1.377 (5)
Cl2—Cd1ii2.6274 (5)C4—H40.9300
N1—C21.436 (2)
N1i—Cd1—N1180.00 (7)Cd1—Cl2—Cd1ii91.80 (2)
N1i—Cd1—Cl290.71 (4)C2—N1—Cd1117.26 (11)
N1—Cd1—Cl289.29 (4)C2—N1—H1A110.3
N1i—Cd1—Cl2i89.29 (4)Cd1—N1—H1A98.0
N1—Cd1—Cl2i90.71 (4)C2—N1—H1B112.2
Cl2—Cd1—Cl2i180.0Cd1—N1—H1B108.8
N1i—Cd1—Cl1i92.61 (4)H1A—N1—H1B109.2
N1—Cd1—Cl1i87.39 (4)C3—C2—C2iii119.20 (13)
Cl2—Cd1—Cl1i94.319 (17)C3—C2—N1119.72 (18)
Cl2i—Cd1—Cl1i85.682 (17)C2iii—C2—N1120.96 (10)
N1i—Cd1—Cl187.39 (4)C4—C3—C2120.8 (2)
N1—Cd1—Cl192.61 (4)C4—C3—H3119.6
Cl2—Cd1—Cl185.682 (17)C2—C3—H3119.6
Cl2i—Cd1—Cl194.318 (17)C3—C4—C4iii119.98 (13)
Cl1i—Cd1—Cl1180.00 (3)C3—C4—H4120.0
Cd1ii—Cl1—Cd191.32 (2)C4iii—C4—H4120.0

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

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N1—H1B···Cl1iv0.892.513.3960 (18)171.

Symmetry codes: (iv) x+1, y, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BX2174).

References

  • Choi, K. Y., Kim, Y. J., Ryu, H. & Suh, I. H. (1999). Inorg. Chem. Commun.2, 176–180.
  • Ferguson, G. (1999). PRPKAPPA University of Guelph, Canada.
  • Fu, D.-W. & Zhao, H. (2007). Acta Cryst. E63, m1630.
  • Rigaku (2005). CrystalClear Rigaku Corporation, Tokyo, Japan.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Spingler, B., Whittington, D. A. & Lippard, S. J. (2001). Inorg. Chem.40, 5596–5602. [PubMed]

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