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Acta Crystallogr Sect E Struct Rep Online. 2009 August 1; 65(Pt 8): m859.
Published online 2009 July 1. doi:  10.1107/S1600536809024398
PMCID: PMC2977134

Bis[4-(dimethyl­amino)pyridinium] tetra­bromidocobaltate(II)

Abstract

The metal atom in the title salt, (C7H11N2)2[CoBr4], shows a slightly distorted tetra­hedral coordination. The cation forms an N—H(...)Br hydrogen bond to one of the two Br atoms. The CoII atom lies on a special position of 2 site symmetry.

Related literature

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

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Object name is e-65-0m859-scheme1.jpg

Experimental

Crystal data

  • (C7H11N2)2[CoBr4]
  • M r = 624.93
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m859-efi1.jpg
  • a = 10.4020 (2) Å
  • b = 12.1601 (2) Å
  • c = 16.9167 (2) Å
  • β = 104.270 (1)°
  • V = 2073.76 (6) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 8.54 mm−1
  • T = 140 K
  • 0.40 × 0.35 × 0.30 mm

Data collection

  • Bruker SMART APEX diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.131, T max = 0.184 (expected range = 0.055–0.077)
  • 8405 measured reflections
  • 2386 independent reflections
  • 2228 reflections with I > 2σ(I)
  • R int = 0.024

Refinement

  • R[F 2 > 2σ(F 2)] = 0.021
  • wR(F 2) = 0.054
  • S = 1.06
  • 2386 reflections
  • 111 parameters
  • 1 restraint
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.49 e Å−3
  • Δρmin = −0.75 e Å−3

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

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809024398/bt2980sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809024398/bt2980Isup2.hkl

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

Acknowledgments

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

supplementary crystallographic information

Experimental

Cobalt nitrate hexahydrate (0.89 g, 3 mmol) dissolved in a minimum volume of water was mixed with 4-dimethylaminopyridinium hydrobromide perbromide (1.1 g, 3 mmol) dissolved in 50 ml ethanol. The mixture was heated for 1 hour. The red solution slowly turned to blue solution. This was set aside for the growth of crystals.

Refinement

Hydrogen atoms were placed at calculated positions (C–H 0.95–0.98 Å) and were treated as riding on their parent atoms, with U(H) set to 1.2U~eq~(C). The amino H-atom was refined with a distance restraint of 0.84±0.01 Å.

Figures

Fig. 1.
Anisotropic displacement ellipsoid plot (Barbour, 2001) of the title compound at the 70% probability level. H atoms are drawn as spheres of arbitrary radius.

Crystal data

(C7H11N2)2[CoBr4]F(000) = 1204
Mr = 624.93Dx = 2.002 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 6526 reflections
a = 10.4020 (2) Åθ = 2.5–28.4°
b = 12.1601 (2) ŵ = 8.54 mm1
c = 16.9167 (2) ÅT = 140 K
β = 104.270 (1)°Block, blue
V = 2073.76 (6) Å30.40 × 0.35 × 0.30 mm
Z = 4

Data collection

Bruker SMART APEX diffractometer2386 independent reflections
Radiation source: fine-focus sealed tube2228 reflections with I > 2σ(I)
graphiteRint = 0.024
ω scansθmax = 27.5°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −11→13
Tmin = 0.131, Tmax = 0.184k = −15→15
8405 measured reflectionsl = −21→21

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)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.054H atoms treated by a mixture of independent and constrained refinement
S = 1.06w = 1/[σ2(Fo2) + (0.0282P)2 + 3.2278P] where P = (Fo2 + 2Fc2)/3
2386 reflections(Δ/σ)max = 0.001
111 parametersΔρmax = 0.49 e Å3
1 restraintΔρmin = −0.75 e Å3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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

xyzUiso*/Ueq
Br10.66045 (2)0.777934 (17)0.345907 (13)0.02380 (7)
Br20.36829 (2)0.555780 (17)0.314578 (12)0.02431 (7)
Co10.50000.67093 (3)0.25000.01636 (9)
N10.7776 (2)0.51482 (16)0.39578 (13)0.0268 (4)
H10.746 (3)0.5670 (19)0.3610 (16)0.044 (9)*
N20.94584 (19)0.27718 (16)0.56095 (11)0.0238 (4)
C10.8017 (2)0.53686 (18)0.47578 (15)0.0267 (5)
H1A0.78090.60760.49290.032*
C20.8555 (2)0.46012 (18)0.53283 (14)0.0235 (4)
H20.87090.47700.58920.028*
C30.88849 (19)0.35447 (17)0.50763 (12)0.0183 (4)
C40.8593 (2)0.33468 (17)0.42225 (12)0.0194 (4)
H40.87820.26500.40240.023*
C50.8047 (2)0.41504 (19)0.36914 (13)0.0243 (4)
H50.78510.40090.31220.029*
C60.9690 (3)0.2937 (3)0.64888 (14)0.0364 (6)
H6A0.88710.31940.66160.055*
H6B1.03900.34880.66680.055*
H6C0.99660.22410.67720.055*
C70.9865 (2)0.17184 (19)0.53287 (15)0.0289 (5)
H7A1.03640.18500.49160.043*
H7B0.90760.12770.50900.043*
H7C1.04260.13230.57920.043*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Br10.01960 (12)0.02113 (11)0.02904 (12)−0.00386 (8)0.00292 (9)−0.00728 (8)
Br20.03047 (13)0.02293 (12)0.02059 (11)−0.00884 (8)0.00829 (9)0.00109 (7)
Co10.01504 (19)0.01626 (17)0.01751 (18)0.0000.00345 (14)0.000
N10.0223 (10)0.0229 (9)0.0346 (10)0.0040 (7)0.0060 (8)0.0059 (8)
N20.0206 (9)0.0335 (10)0.0166 (8)0.0013 (7)0.0029 (7)0.0029 (7)
C10.0198 (11)0.0233 (10)0.0391 (13)−0.0010 (8)0.0110 (9)−0.0074 (9)
C20.0178 (10)0.0300 (11)0.0245 (10)−0.0046 (8)0.0085 (8)−0.0094 (8)
C30.0112 (9)0.0249 (10)0.0190 (9)−0.0028 (7)0.0042 (7)−0.0007 (8)
C40.0170 (10)0.0218 (9)0.0191 (9)0.0013 (8)0.0040 (7)−0.0012 (7)
C50.0214 (10)0.0290 (11)0.0212 (10)0.0004 (9)0.0030 (8)0.0005 (8)
C60.0301 (13)0.0608 (17)0.0166 (10)−0.0005 (12)0.0027 (9)0.0048 (10)
C70.0251 (12)0.0268 (11)0.0320 (12)0.0034 (9)0.0019 (9)0.0071 (9)

Geometric parameters (Å, °)

Br1—Co12.4033 (3)C2—C31.422 (3)
Br2—Co12.4019 (3)C2—H20.9500
Co1—Br2i2.4019 (3)C3—C41.421 (3)
Co1—Br1i2.4033 (3)C4—C51.354 (3)
N1—C11.341 (3)C4—H40.9500
N1—C51.348 (3)C5—H50.9500
N1—H10.872 (10)C6—H6A0.9800
N2—C31.337 (3)C6—H6B0.9800
N2—C61.461 (3)C6—H6C0.9800
N2—C71.464 (3)C7—H7A0.9800
C1—C21.360 (3)C7—H7B0.9800
C1—H1A0.9500C7—H7C0.9800
Br2—Co1—Br2i108.678 (18)C4—C3—C2116.79 (19)
Br2—Co1—Br1112.808 (7)C5—C4—C3120.1 (2)
Br2i—Co1—Br1104.098 (8)C5—C4—H4119.9
Br2—Co1—Br1i104.099 (8)C3—C4—H4119.9
Br2i—Co1—Br1i112.808 (7)N1—C5—C4121.0 (2)
Br1—Co1—Br1i114.444 (18)N1—C5—H5119.5
C1—N1—C5121.0 (2)C4—C5—H5119.5
C1—N1—H1119 (2)N2—C6—H6A109.5
C5—N1—H1120 (2)N2—C6—H6B109.5
C3—N2—C6121.6 (2)H6A—C6—H6B109.5
C3—N2—C7120.84 (18)N2—C6—H6C109.5
C6—N2—C7117.52 (19)H6A—C6—H6C109.5
N1—C1—C2121.4 (2)H6B—C6—H6C109.5
N1—C1—H1A119.3N2—C7—H7A109.5
C2—C1—H1A119.3N2—C7—H7B109.5
C1—C2—C3119.6 (2)H7A—C7—H7B109.5
C1—C2—H2120.2N2—C7—H7C109.5
C3—C2—H2120.2H7A—C7—H7C109.5
N2—C3—C4120.97 (19)H7B—C7—H7C109.5
N2—C3—C2122.24 (19)
C5—N1—C1—C20.7 (3)C1—C2—C3—N2177.6 (2)
N1—C1—C2—C30.7 (3)C1—C2—C3—C4−1.6 (3)
C6—N2—C3—C4−176.2 (2)N2—C3—C4—C5−178.1 (2)
C7—N2—C3—C43.1 (3)C2—C3—C4—C51.0 (3)
C6—N2—C3—C24.7 (3)C1—N1—C5—C4−1.2 (3)
C7—N2—C3—C2−176.0 (2)C3—C4—C5—N10.3 (3)

Symmetry codes: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
N1—H1···Br10.87 (1)2.71 (2)3.454 (2)144 (3)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT2980).

References

  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  • Bruker (2008). APEX2 and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • 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. (2009). publCIF In preparation.

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