PMCCPMCCPMCC

Search tips
Search criteria 

Advanced

 
Logo of actaeInternational Union of Crystallographysearchopen accessarticle submissionjournal home pagethis article
 
Acta Crystallogr Sect E Struct Rep Online. 2009 May 1; 65(Pt 5): m560.
Published online 2009 April 25. doi:  10.1107/S1600536809014366
PMCID: PMC2977606

Bis[4-(dimethyl­amino)pyridinium] tetra­bromidocadmate(II) monohydrate

Abstract

The Cd atom in the hydrated title salt, (C7H11N2)2[CdBr4]·H2O, exists in an approximately tetra­hedral coordination geometry, with Br—Cd—Br angles in the range 105.52 (3)–111.50 (3)°. The cation, anion and water mol­ecule inter­act by O—H(...)Br, N—H(...)Br and N—H(...)O hydrogen bonds, forming a linear chain structure running along the a axis.

Related literature

For other tetra­hedral ammonium tetra­bromidocadmates, see: Altermatt et al. (1979 [triangle]); Battaglia et al. (1991 [triangle]); Casals et al. (1987 [triangle]); Geselle & Fuess (1994 [triangle]); Ishihara et al. (1998 [triangle]); Krishnan et al. (1991 [triangle]); Sato et al. (1986 [triangle]); Waskowska (1994 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-0m560-scheme1.jpg

Experimental

Crystal data

  • (C7H11N2)2[CdBr4]·H2O
  • M r = 696.41
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m560-efi1.jpg
  • a = 7.8918 (2) Å
  • b = 8.1197 (2) Å
  • c = 17.2719 (4) Å
  • α = 95.481 (1)°
  • β = 99.747 (1)°
  • γ = 96.489 (1)°
  • V = 1076.35 (5) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 8.45 mm−1
  • T = 100 K
  • 0.25 × 0.25 × 0.25 mm

Data collection

  • Bruker SMART APEX diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.258, T max = 0.431 (expected range = 0.072–0.121)
  • 6014 measured reflections
  • 3711 independent reflections
  • 3255 reflections with I > 2σ(I)
  • R int = 0.022

Refinement

  • R[F 2 > 2σ(F 2)] = 0.037
  • wR(F 2) = 0.131
  • S = 1.07
  • 3711 reflections
  • 221 parameters
  • H-atom parameters constrained
  • Δρmax = 1.53 e Å−3
  • Δρmin = −1.65 e Å−3

Data collection: APEX2 (Bruker, 2008 [triangle]); cell refinement: APEX2; data reduction: SAINT (Bruker, 2008 [triangle]); 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: pubCIF (Westrip, 2009 [triangle]).

Table 1
Selected bond angles (°)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809014366/sj2619sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809014366/sj2619Isup2.hkl

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

Acknowledgments

The authors thank the University of Malaya (grant No. FS339/2008A) for supporting this study.

supplementary crystallographic information

Experimental

Cadmium chloride (0.5 g, 2 mmol) dissolved in water (10 ml) and 4-dimethylaminopyridine hydrobromide perbromide (0.8 g, 2 mmol) dissolved in ethanol (80 ml) were mixed and the mixture heated for 1 h. Slow evaporation of the filtrate gave colorless crystals.

Refinement

Carbon- and nitrogen-bound H atoms were placed in calculated positions (C—H 0.95 to 0.98 Å, N—H 0.88 Å) and were included in the refinement in the riding model approximation, with U(H) fixed at 1.2–1.5U(C). The water H atoms were placed in chemically sensible positions on the basis of hydrogen-bonding interactions, but were not refined.

The final difference Fourier map had a large peak at 1.3 Å from H5 and a deep hole at 0.7 Å from Br1.

Figures

Fig. 1.
Thermal ellipsoid plot (Barbour, 2001) of (C7H11N2)2(CdBr4).H2O at the 70% probability level. H atoms are drawn as spheres of arbitrary radius.

Crystal data

(C7H11N2)2[CdBr4]·H2OZ = 2
Mr = 696.41F(000) = 664
Triclinic, P1Dx = 2.149 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.8918 (2) ÅCell parameters from 3763 reflections
b = 8.1197 (2) Åθ = 2.4–28.2°
c = 17.2719 (4) ŵ = 8.45 mm1
α = 95.481 (1)°T = 100 K
β = 99.747 (1)°Irregular block, colourless
γ = 96.489 (1)°0.25 × 0.25 × 0.25 mm
V = 1076.35 (5) Å3

Data collection

Bruker SMART APEX diffractometer3711 independent reflections
Radiation source: fine-focus sealed tube3255 reflections with I > 2σ(I)
graphiteRint = 0.022
ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −9→9
Tmin = 0.258, Tmax = 0.431k = −9→9
6014 measured reflectionsl = −20→20

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.131H-atom parameters constrained
S = 1.07w = 1/[σ2(Fo2) + (0.0774P)2 + 6.748P] where P = (Fo2 + 2Fc2)/3
3711 reflections(Δ/σ)max = 0.001
221 parametersΔρmax = 1.53 e Å3
0 restraintsΔρmin = −1.65 e Å3

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

xyzUiso*/Ueq
Cd10.56389 (6)0.31451 (6)0.25658 (3)0.01616 (17)
Br10.43625 (10)0.44170 (10)0.37244 (5)0.0256 (2)
Br20.53082 (10)0.50457 (9)0.14316 (5)0.0237 (2)
Br30.89498 (9)0.31530 (10)0.30001 (4)0.0205 (2)
Br40.41821 (9)0.01732 (9)0.20678 (4)0.0209 (2)
O10.1769 (9)0.6316 (8)0.2453 (4)0.0438 (17)
H110.26660.58540.24310.066*
H120.10050.56270.25750.066*
N10.8619 (9)0.3422 (9)0.0770 (4)0.0280 (16)
H10.79740.38120.10950.034*
N21.1657 (8)0.1572 (8)−0.0724 (4)0.0187 (13)
N30.2927 (8)0.8098 (8)0.4100 (4)0.0233 (14)
H30.30980.72530.37770.028*
N40.1981 (8)1.1958 (7)0.5626 (3)0.0150 (12)
C10.3353 (10)0.8102 (9)0.4877 (5)0.0210 (16)
H1A0.38950.71970.50700.025*
C20.3061 (9)0.9320 (9)0.5412 (5)0.0199 (16)
H20.33520.92460.59630.024*
C30.2300 (9)1.0730 (9)0.5130 (4)0.0143 (14)
C40.1916 (9)1.0680 (9)0.4308 (5)0.0179 (15)
H40.14141.15790.40890.022*
C50.2228 (9)0.9411 (9)0.3813 (4)0.0197 (15)
H50.19550.94380.32580.024*
C60.2363 (11)1.1943 (10)0.6469 (5)0.0258 (18)
H6A0.18011.09010.66080.039*
H6B0.19281.28930.67290.039*
H6C0.36201.20250.66450.039*
C70.1264 (10)1.3411 (9)0.5317 (5)0.0195 (15)
H7A0.20571.39560.50120.029*
H7B0.11221.42030.57590.029*
H7C0.01341.30430.49750.029*
C81.0058 (10)0.2831 (10)0.1052 (5)0.0249 (17)
H81.03810.28450.16080.030*
C91.1099 (10)0.2201 (10)0.0575 (4)0.0199 (15)
H91.21240.17790.08000.024*
C101.0651 (9)0.2175 (8)−0.0254 (4)0.0163 (15)
C110.9084 (10)0.2811 (9)−0.0549 (5)0.0221 (17)
H11A0.87090.2804−0.11020.026*
C120.8130 (10)0.3430 (9)−0.0026 (5)0.0245 (17)
H12A0.71000.3877−0.02200.029*
C131.3311 (10)0.1038 (11)−0.0401 (5)0.0274 (18)
H13A1.39380.18700.00310.041*
H13B1.40060.0925−0.08180.041*
H13C1.3100−0.0040−0.01990.041*
C141.1133 (11)0.1373 (10)−0.1580 (4)0.0242 (17)
H14A1.19680.0788−0.18220.036*
H14B1.11000.2474−0.17660.036*
H14C0.99790.0723−0.17280.036*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Cd10.0151 (3)0.0170 (3)0.0153 (3)0.0015 (2)0.0019 (2)−0.0014 (2)
Br10.0261 (4)0.0246 (4)0.0270 (5)0.0027 (3)0.0108 (3)−0.0031 (3)
Br20.0229 (4)0.0236 (4)0.0244 (4)0.0049 (3)0.0000 (3)0.0067 (3)
Br30.0158 (4)0.0304 (4)0.0148 (4)0.0038 (3)0.0021 (3)0.0002 (3)
Br40.0239 (4)0.0184 (4)0.0187 (4)−0.0008 (3)0.0038 (3)−0.0013 (3)
O10.049 (4)0.037 (4)0.044 (4)0.010 (3)0.004 (3)0.000 (3)
N10.025 (4)0.027 (4)0.034 (4)−0.001 (3)0.019 (3)−0.005 (3)
N20.020 (3)0.026 (3)0.011 (3)0.002 (3)0.004 (2)0.007 (3)
N30.024 (3)0.024 (3)0.023 (4)0.000 (3)0.010 (3)0.000 (3)
N40.019 (3)0.017 (3)0.009 (3)0.003 (2)0.001 (2)0.004 (2)
C10.022 (4)0.016 (4)0.028 (4)0.004 (3)0.007 (3)0.013 (3)
C20.016 (3)0.019 (4)0.024 (4)−0.002 (3)0.003 (3)0.003 (3)
C30.012 (3)0.017 (3)0.013 (4)−0.002 (3)−0.001 (3)0.012 (3)
C40.011 (3)0.020 (4)0.022 (4)−0.001 (3)0.002 (3)0.003 (3)
C50.021 (4)0.023 (4)0.015 (4)0.000 (3)0.007 (3)0.001 (3)
C60.031 (4)0.027 (4)0.017 (4)−0.008 (3)0.010 (3)−0.006 (3)
C70.023 (4)0.013 (3)0.023 (4)0.006 (3)0.003 (3)−0.001 (3)
C80.026 (4)0.026 (4)0.022 (4)−0.002 (3)0.009 (3)−0.007 (3)
C90.022 (4)0.025 (4)0.012 (4)0.000 (3)0.005 (3)−0.001 (3)
C100.019 (4)0.011 (3)0.016 (4)−0.006 (3)−0.004 (3)0.008 (3)
C110.020 (4)0.021 (4)0.020 (4)−0.010 (3)−0.005 (3)0.009 (3)
C120.020 (4)0.015 (4)0.037 (5)0.000 (3)0.003 (3)0.005 (3)
C130.022 (4)0.028 (4)0.031 (5)0.002 (3)0.003 (3)0.001 (4)
C140.031 (4)0.028 (4)0.012 (4)0.001 (3)0.003 (3)0.001 (3)

Geometric parameters (Å, °)

Cd1—Br12.5706 (9)C4—C51.347 (11)
Cd1—Br22.6044 (9)C4—H40.9500
Cd1—Br32.5926 (8)C5—H50.9500
Cd1—Br42.5546 (8)C6—H6A0.9800
O1—H110.8418C6—H6B0.9800
O1—H120.8427C6—H6C0.9800
N1—C81.318 (11)C7—H7A0.9800
N1—C121.364 (11)C7—H7B0.9800
N1—H10.8800C7—H7C0.9800
N2—C101.326 (10)C8—C91.364 (11)
N2—C141.455 (10)C8—H80.9500
N2—C131.460 (10)C9—C101.414 (10)
N3—C11.327 (10)C9—H90.9500
N3—C51.352 (10)C10—C111.427 (11)
N3—H30.8800C11—C121.367 (12)
N4—C31.325 (10)C11—H11A0.9500
N4—C61.438 (10)C12—H12A0.9500
N4—C71.472 (9)C13—H13A0.9800
C1—C21.355 (11)C13—H13B0.9800
C1—H1A0.9500C13—H13C0.9800
C2—C31.439 (10)C14—H14A0.9800
C2—H20.9500C14—H14B0.9800
C3—C41.396 (10)C14—H14C0.9800
Br1—Cd1—Br2109.23 (3)N4—C6—H6C109.5
Br1—Cd1—Br3109.83 (3)H6A—C6—H6C109.5
Br4—Cd1—Br1111.50 (3)H6B—C6—H6C109.5
Br2—Cd1—Br3105.52 (3)N4—C7—H7A109.5
Br2—Cd1—Br4110.72 (3)N4—C7—H7B109.5
Br3—Cd1—Br4109.87 (3)H7A—C7—H7B109.5
H11—O1—H12108.9N4—C7—H7C109.5
C8—N1—C12120.1 (7)H7A—C7—H7C109.5
C8—N1—H1120.0H7B—C7—H7C109.5
C12—N1—H1120.0N1—C8—C9122.4 (8)
C10—N2—C14121.3 (6)N1—C8—H8118.8
C10—N2—C13121.3 (6)C9—C8—H8118.8
C14—N2—C13117.4 (6)C8—C9—C10119.8 (7)
C1—N3—C5119.1 (7)C8—C9—H9120.1
C1—N3—H3120.5C10—C9—H9120.1
C5—N3—H3120.5N2—C10—C9120.4 (7)
C3—N4—C6121.8 (6)N2—C10—C11122.7 (7)
C3—N4—C7120.0 (6)C9—C10—C11116.9 (7)
C6—N4—C7118.2 (6)C12—C11—C10119.1 (7)
N3—C1—C2123.8 (7)C12—C11—H11A120.4
N3—C1—H1A118.1C10—C11—H11A120.4
C2—C1—H1A118.1N1—C12—C11121.6 (7)
C1—C2—C3118.8 (7)N1—C12—H12A119.2
C1—C2—H2120.6C11—C12—H12A119.2
C3—C2—H2120.6N2—C13—H13A109.5
N4—C3—C4123.6 (6)N2—C13—H13B109.5
N4—C3—C2121.4 (6)H13A—C13—H13B109.5
C4—C3—C2114.9 (7)N2—C13—H13C109.5
C5—C4—C3122.9 (7)H13A—C13—H13C109.5
C5—C4—H4118.6H13B—C13—H13C109.5
C3—C4—H4118.6N2—C14—H14A109.5
C4—C5—N3120.5 (7)N2—C14—H14B109.5
C4—C5—H5119.8H14A—C14—H14B109.5
N3—C5—H5119.8N2—C14—H14C109.5
N4—C6—H6A109.5H14A—C14—H14C109.5
N4—C6—H6B109.5H14B—C14—H14C109.5
H6A—C6—H6B109.5
C5—N3—C1—C23.0 (11)C12—N1—C8—C9−0.5 (12)
N3—C1—C2—C3−2.3 (11)N1—C8—C9—C100.4 (12)
C6—N4—C3—C4178.6 (7)C14—N2—C10—C9173.5 (7)
C7—N4—C3—C4−3.1 (10)C13—N2—C10—C9−4.7 (10)
C6—N4—C3—C2−0.5 (10)C14—N2—C10—C11−6.1 (10)
C7—N4—C3—C2177.7 (6)C13—N2—C10—C11175.7 (7)
C1—C2—C3—N4179.9 (7)C8—C9—C10—N2179.7 (7)
C1—C2—C3—C40.6 (10)C8—C9—C10—C11−0.7 (10)
N4—C3—C4—C5−179.1 (7)N2—C10—C11—C12−179.2 (7)
C2—C3—C4—C50.1 (10)C9—C10—C11—C121.2 (10)
C3—C4—C5—N30.6 (11)C8—N1—C12—C111.1 (11)
C1—N3—C5—C4−2.1 (11)C10—C11—C12—N1−1.4 (11)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1—H11···Br10.842.833.351 (7)122
O1—H12···Br3i0.842.673.511 (7)172
N1—H1···Br20.882.563.373 (7)154
N3—H3···O10.882.363.011 (10)131

Symmetry codes: (i) x−1, y, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SJ2619).

References

  • Altermatt, D., Arend, H., Niggli, A. & Petter, W. (1979). Mater. Res. Bull.14, 1391–1396.
  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  • Battaglia, L. P., Corradi, A. M., Bruni, S., Cariati, F. & Koman, M. (1991). Inorg. Chim. Acta, 187, 141–147.
  • Bruker (2008). APEX2 and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Casals, I., González-Duarte, P., Sola, J., Font-Bardía, M., Solans, J. & Solans, X. (1987). J. Chem. Soc. Dalton Trans. pp. 2391–2395.
  • Geselle, M. & Fuess, H. (1994). Acta Cryst. C50, 1582–1585.
  • Ishihara, H., Horiuchi, K., Dou, S.-Q., Gesing, T. M., Buhl, J.-C., Paulus, H. & Fuess, H. (1998). Z. Naturforsch. Teil A, 53, 717–724.
  • Krishnan, V. G., Dou, S.-Q., Paulus, H. & Weiss, A. (1991). Ber. Bunsenges. Phys. Chem.96, 1256–1264.
  • Sato, S., Ikeda, R. & Nakamura, D. (1986). Bull. Chem. Soc. Jpn, 59, 1981–1989.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Waskowska, A. (1994). Z. Kristallogr.209, 752–754.
  • Westrip, S. P. (2009). publCIF In preparation.

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