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Acta Crystallogr Sect E Struct Rep Online. 2010 March 1; 66(Pt 3): m308.
Published online 2010 February 17. doi:  10.1107/S1600536810005817
PMCID: PMC2983584

catena-Poly[trimethyl­phenyl­ammonium [[bromidocad­mate(II)]-μ-bromido-μ-chlorido]]

Abstract

In the title salt, (C9H14N)[CdBr2Cl], the CdII atom is five-coordinated in a trigonal-bipyramidal coordination environment. All three of the halogen sites show disorder as a result of substitution of Cl for Br or Br for Cl. Two of the three halogen atoms are involved in bridging a pair of CdII atoms, generating a linear polyanionic chain motif.

Related literature

For the crystal structure of bis­[4-(dimethyl­amino)pyridinium]tetra­bromidocadmate monohydrate, see: Lo & Ng (2009 [triangle]).

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Object name is e-66-0m308-scheme1.jpg

Experimental

Crystal data

  • (C9H14N)[CdBr2Cl]
  • M r = 443.88
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m308-efi1.jpg
  • a = 12.9403 (2) Å
  • b = 14.7059 (2) Å
  • c = 7.3866 (1) Å
  • β = 95.1590 (8)°
  • V = 1399.97 (3) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 7.43 mm−1
  • T = 293 K
  • 0.30 × 0.25 × 0.20 mm

Data collection

  • Bruker SMART APEX diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.378, T max = 0.746
  • 6431 measured reflections
  • 3068 independent reflections
  • 2966 reflections with I > 2σ(I)
  • R int = 0.026

Refinement

  • R[F 2 > 2σ(F 2)] = 0.027
  • wR(F 2) = 0.070
  • S = 1.06
  • 3068 reflections
  • 124 parameters
  • 10 restraints
  • H-atom parameters constrained
  • Δρmax = 0.67 e Å−3
  • Δρmin = −0.68 e Å−3
  • Absolute structure: Flack (1983 [triangle]), 1451 Friedel pairs
  • Flack parameter: 0.021 (9)

Data collection: APEX2 (Bruker, 2009 [triangle]); cell refinement: SAINT (Bruker, 2009 [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: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2010 [triangle]).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810005817/ci5034sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810005817/ci5034Isup2.hkl

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

Acknowledgments

The authors thank the University of Malaya (RG020/09AFR) for supporting this study.

supplementary crystallographic information

Experimental

Cadmium chloride hemipentahydrate (0.45 g , 2 mmol) and trimethylphenylammonium tribromide (0.76 g, 2mmol) were heated in ethanol for 1 h. After filtering of the reaction mixture, colourless crystals were obtained upon slow evaporation of the yellow filtrate.

Refinement

The aromatic ring was refined as a rigid hexagon (C—C = 1.39 Å). The N—Cmethyl distances were restrained to 1.50 (1) Å. H atoms were placed at calculated positions (C–H = 0.93–0.96 Å) and were treated as riding on their parent atoms, with U(H) set to 1.2–1.5 times Ueq(C).

Each of the three halogen sites are occupied by Cl or Br atoms. The total site occupancy of the Cl atoms refined to nearly 1 and that of Br atoms to nearly 2. Hence, the total site occupancy was fixed as 1.0 for Cl and 2.0 for Br atoms. The same Uij parameters were used for Br and Cl atoms occupying the same site.

Figures

Fig. 1.
Displacement ellipsoid plot (Barbour, 2001) of a portion of polymeric C9H14N+ [CdBr2Cl]- at the 50% probability level. H are drawn as spheres of arbitrary radius. The disorder in the halogen sites not shown.

Crystal data

(C9H14N)[CdBr2Cl]F(000) = 840
Mr = 443.88Dx = 2.106 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2ycCell parameters from 5267 reflections
a = 12.9403 (2) Åθ = 2.7–28.3°
b = 14.7059 (2) ŵ = 7.43 mm1
c = 7.3866 (1) ÅT = 293 K
β = 95.1590 (8)°Block, colourless
V = 1399.97 (3) Å30.30 × 0.25 × 0.20 mm
Z = 4

Data collection

Bruker SMART APEX diffractometer3068 independent reflections
Radiation source: fine-focus sealed tube2966 reflections with I > 2σ(I)
graphiteRint = 0.026
ω scansθmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −16→16
Tmin = 0.378, Tmax = 0.746k = −19→19
6431 measured reflectionsl = −9→9

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.070w = 1/[σ2(Fo2) + (0.0296P)2 + 0.0436P] where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
3068 reflectionsΔρmax = 0.67 e Å3
124 parametersΔρmin = −0.68 e Å3
10 restraintsAbsolute structure: Flack (1983), 1451 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.021 (9)

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

xyzUiso*/UeqOcc. (<1)
Cd10.50000 (2)0.451513 (19)0.50000 (3)0.04131 (10)
Br10.63269 (6)0.51023 (6)0.29653 (9)0.04153 (19)0.302 (2)
Br20.36460 (4)0.55946 (3)0.61951 (6)0.04104 (14)0.861 (2)
Br30.48809 (5)0.28104 (3)0.54560 (8)0.05001 (16)0.837 (2)
Cl10.63269 (6)0.51023 (6)0.29653 (9)0.04153 (19)0.698 (2)
Cl20.36460 (4)0.55946 (3)0.61951 (6)0.04104 (14)0.139 (2)
Cl30.48809 (5)0.28104 (3)0.54560 (8)0.05001 (16)0.163 (2)
N10.6446 (3)0.8091 (3)0.5732 (4)0.0399 (8)
C10.5525 (2)0.8692 (2)0.5708 (5)0.0405 (9)
C20.4530 (3)0.8337 (2)0.5711 (6)0.0623 (14)
H20.44320.77100.57160.075*
C30.3682 (2)0.8917 (3)0.5705 (8)0.089 (2)
H30.30170.86790.57060.106*
C40.3830 (3)0.9854 (3)0.5696 (8)0.091 (3)
H40.32621.02420.56920.109*
C50.4825 (4)1.02091 (19)0.5694 (7)0.082 (2)
H50.49231.08350.56880.098*
C60.5673 (3)0.9628 (2)0.5700 (6)0.0594 (14)
H60.63390.98660.56980.071*
C70.6156 (6)0.7104 (3)0.5704 (10)0.0697 (16)
H7A0.57140.69750.46200.104*
H7B0.57960.69660.67510.104*
H7C0.67730.67400.57220.104*
C80.7023 (4)0.8299 (5)0.4097 (7)0.0624 (14)
H8A0.65950.81480.30090.094*
H8B0.76500.79460.41530.094*
H8C0.71930.89340.40860.094*
C90.7151 (4)0.8261 (5)0.7446 (7)0.0623 (15)
H9A0.74810.88430.73650.093*
H9B0.76700.77940.75830.093*
H9C0.67490.82550.84760.093*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cd10.04678 (18)0.03161 (15)0.04784 (18)0.00106 (13)0.01690 (13)−0.00100 (13)
Br10.0383 (4)0.0526 (5)0.0341 (3)−0.0033 (3)0.0054 (3)0.0011 (3)
Br20.0381 (3)0.0426 (3)0.0431 (3)0.00585 (18)0.00755 (18)−0.00786 (17)
Br30.0605 (3)0.0296 (2)0.0590 (3)0.0028 (2)0.0003 (2)0.00449 (19)
Cl10.0383 (4)0.0526 (5)0.0341 (3)−0.0033 (3)0.0054 (3)0.0011 (3)
Cl20.0381 (3)0.0426 (3)0.0431 (3)0.00585 (18)0.00755 (18)−0.00786 (17)
Cl30.0605 (3)0.0296 (2)0.0590 (3)0.0028 (2)0.0003 (2)0.00449 (19)
N10.0381 (19)0.042 (2)0.0400 (18)−0.0041 (15)0.0046 (14)0.0012 (14)
C10.040 (2)0.040 (2)0.041 (2)−0.0041 (17)0.0006 (17)−0.0010 (16)
C20.047 (3)0.068 (4)0.072 (4)−0.014 (3)0.005 (2)0.005 (3)
C30.046 (3)0.120 (7)0.098 (5)0.005 (4)0.001 (3)−0.006 (5)
C40.084 (5)0.103 (6)0.082 (5)0.047 (5)−0.013 (4)−0.011 (4)
C50.091 (5)0.064 (4)0.089 (5)0.025 (4)−0.003 (4)−0.008 (4)
C60.065 (4)0.040 (3)0.071 (3)−0.004 (2)−0.004 (3)0.005 (2)
C70.082 (4)0.038 (3)0.090 (5)−0.001 (3)0.007 (3)−0.002 (3)
C80.046 (3)0.093 (5)0.050 (3)0.001 (3)0.017 (2)−0.001 (3)
C90.051 (3)0.085 (4)0.048 (3)0.002 (3)−0.008 (2)0.001 (3)

Geometric parameters (Å, °)

Cd1—Br12.5332 (8)C3—H30.93
Cd1—Br32.5361 (6)C4—C51.39
Cd1—Br22.5782 (5)C4—H40.93
Cd1—Cl1i2.7178 (8)C5—C61.39
Cd1—Br1i2.7178 (8)C5—H50.93
Cd1—Br2ii3.1795 (5)C6—H60.93
Br1—Cd1ii2.7178 (8)C7—H7A0.96
N1—C11.483 (4)C7—H7B0.96
N1—C71.499 (6)C7—H7C0.96
N1—C81.507 (5)C8—H8A0.96
N1—C91.513 (5)C8—H8B0.96
C1—C21.39C8—H8C0.96
C1—C61.39C9—H9A0.96
C2—C31.39C9—H9B0.96
C2—H20.93C9—H9C0.96
C3—C41.39
Br1—Cd1—Br3117.92 (3)C4—C3—H3120.0
Br1—Cd1—Br2120.74 (3)C2—C3—H3120.0
Br3—Cd1—Br2120.79 (2)C3—C4—C5120.0
Br1—Cd1—Cl1i89.70 (2)C3—C4—H4120.0
Br3—Cd1—Cl1i98.00 (2)C5—C4—H4120.0
Br2—Cd1—Cl1i89.78 (2)C6—C5—C4120.0
Br1—Cd1—Br1i89.70 (2)C6—C5—H5120.0
Br3—Cd1—Br1i98.00 (2)C4—C5—H5120.0
Br2—Cd1—Br1i89.78 (2)C5—C6—C1120.0
Cl1i—Cd1—Br1i0.00 (4)C5—C6—H6120.0
Br1—Cd1—Br2ii80.904 (19)C1—C6—H6120.0
Br3—Cd1—Br2ii91.835 (17)N1—C7—H7A109.5
Br2—Cd1—Br2ii89.796 (16)N1—C7—H7B109.5
Cl1i—Cd1—Br2ii168.79 (2)H7A—C7—H7B109.5
Br1i—Cd1—Br2ii168.79 (2)N1—C7—H7C109.5
Cd1—Br1—Cd1ii97.81 (3)H7A—C7—H7C109.5
C1—N1—C7112.1 (4)H7B—C7—H7C109.5
C1—N1—C8109.0 (4)N1—C8—H8A109.5
C7—N1—C8109.1 (5)N1—C8—H8B109.5
C1—N1—C9109.5 (4)H8A—C8—H8B109.5
C7—N1—C9107.6 (4)N1—C8—H8C109.5
C8—N1—C9109.4 (4)H8A—C8—H8C109.5
C2—C1—C6120.0H8B—C8—H8C109.5
C2—C1—N1121.3 (3)N1—C9—H9A109.5
C6—C1—N1118.7 (3)N1—C9—H9B109.5
C3—C2—C1120.0H9A—C9—H9B109.5
C3—C2—H2120.0N1—C9—H9C109.5
C1—C2—H2120.0H9A—C9—H9C109.5
C4—C3—C2120.0H9B—C9—H9C109.5
Br3—Cd1—Br1—Cd1ii103.65 (3)C9—N1—C1—C2−117.8 (4)
Br2—Cd1—Br1—Cd1ii−67.89 (3)C7—N1—C1—C6−179.0 (4)
Cl1i—Cd1—Br1—Cd1ii−157.45 (4)C8—N1—C1—C6−58.1 (4)
Br1i—Cd1—Br1—Cd1ii−157.45 (4)C9—N1—C1—C661.6 (4)
Br2ii—Cd1—Br1—Cd1ii16.407 (19)N1—C1—C2—C3179.4 (4)
C7—N1—C1—C21.6 (5)N1—C1—C6—C5−179.5 (3)
C8—N1—C1—C2122.5 (4)

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CI5034).

References

  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  • Bruker (2009). APEX2 and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Flack, H. D. (1983). Acta Cryst. A39, 876–881.
  • Lo, K. M. & Ng, S. W. (2009). Acta Cryst. E65, m560. [PMC free article] [PubMed]
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Westrip, S. P. (2010). publCIF In preparation.

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