metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890
Volume 66| Part 7| July 2010| Pages m765-m766

{Ba[Au(SCN)2]2}n: a three-dimensional net comprised of monomeric and trimeric gold(I) units

aDepartment of Physical Sciences, Morehead State University, Morehead, KY 40351, USA, and bDepartment of Chemistry, University of Cincinnati, Cincinnati, OH 45221-0172, USA
*Correspondence e-mail: jeanette.krause@uc.edu

(Received 26 March 2010; accepted 3 June 2010; online 9 June 2010)

The noteworthy structural feature of the title complex, poly[acetonitrile­tetra-μ2-thio­cyanato-barium(II)digold(I)], {[Au2Ba(SCN)4(CH3CN)]}n, is that the bis­(thio­cyanato)­aurate(I) anion adopts both monomeric and trimeric motifs. The trimer unit has an Au⋯Au distance of 3.1687 (3) Å. In both the monomeric and trimeric units, the AuI atoms are also bonded to two S atoms. Within the trimeric unit, the AuI atoms exist in differing environments; one Au atom has a T-shaped three-coordinate geometry while the other has a square-planar four-coordinate geometry. The AuI atom of the monomer adopts a linear two-coordinate geometry. The extended structure can be described as a three-dimensional coordination polymer consisting of chains of Ba atoms bridged by thio­cyanate N atoms. These chains are cross-linked via the gold monomeric and trimeric units.

Related literature

For further information on gold chemistry, see: Anderson et al. (2007[Anderson, K. M., Goeta, A. E. & Steed, J. W. (2007). Inorg. Chem. 46, 6444-5451.]); Bondi (1964[Bondi, A. (1964). J. Phys. Chem. 68, 441-451.]); Pathaneni & Desiraju (1993[Pathaneni, S. S. & Desiraju, G. R. (1993). J. Chem. Soc. Dalton Trans. pp. 319-322.]); Arvapally et al. (2007[Arvapally, R. K., Sinha, P., Hettiarachchi, S. R., Coker, N. L., Bedel, C. E., Patterson, H. H., Elder, R. C., Wilson, A. K. & Omary, M. A. (2007). J. Phys. Chem. 111, 10689-10699.]); Beavers et al. (2009[Beavers, C. M., Paw, U. L. & Olmstead, M. M. (2009). Acta Cryst. E65, m300-m301.]); Coker (2003[Coker, N. L. (2003). PhD dissertation, University of Cincinnati, USA.]); Coker et al. (2004[Coker, N. L., Krause-Bauer, J. A. & Elder, R. C. (2004). J. Am. Chem. Soc. 126, 12-13.], 2006[Coker, N. L., Bedel, C. E., Krause, J. A. & Elder, R. C. (2006). Acta Cryst. E62, m319-m321.]); Katz et al. (2008[Katz, M. J., Sakai, K. & Leznoff, D. B. (2008). Chem. Soc. Rev. 37, 1884-1895.]); Puddephatt (2008[Puddephatt, R. J. (2008). Chem. Soc. Rev. 37, 2012-2027.]); Schmidbaur & Schier (2008[Schmidbaur, H. & Schier, A. (2008). Chem. Soc. Rev. 37, 1931-1951.]); Schwerdtferger et al. (1990[Schwerdtferger, P., Boyd, P., Burrell, A., Robinson, W. & Taylor, M. (1990). Inorg. Chem. 29, 3593-3607.]); Stroud et al. (2009[Stroud, T. L., Coker, N. L. & Krause, J. A. (2009). Acta Cryst. E65, m1509-m1510.]). For a description of the Cambridge Structural Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.])

[Scheme 1]

Experimental

Crystal data
  • [Au2Ba(NCS)4(C2H3N)]

  • Mr = 804.65

  • Monoclinic, P 21 /n

  • a = 11.5586 (3) Å

  • b = 7.4859 (2) Å

  • c = 18.5798 (4) Å

  • β = 106.450 (1)°

  • V = 1541.84 (7) Å3

  • Z = 4

  • Cu Kα radiation

  • μ = 59.69 mm−1

  • T = 150 K

  • 0.15 × 0.05 × 0.02 mm

Data collection
  • Bruker SMART6000 CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2003[Sheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.]) Tmin = 0.060, Tmax = 0.302

  • 12455 measured reflections

  • 2743 independent reflections

  • 2559 reflections with I > 2σ(I)

  • Rint = 0.053

Refinement
  • R[F2 > 2σ(F2)] = 0.031

  • wR(F2) = 0.079

  • S = 1.04

  • 2743 reflections

  • 167 parameters

  • H-atom parameters constrained

  • Δρmax = 2.17 e Å−3

  • Δρmin = −1.27 e Å−3

Data collection: SMART (Bruker, 2003[Bruker (2003). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2003[Bruker (2003). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and DIAMOND (Brandenburg, 2009[Brandenburg, K. (2009). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The propensity for gold complexes to adopt fascinating structures, high stability and unexpected stoichiometries arising from various gold-gold interactions, termed aurophilicty or more generally metallophilicity, ultimately result in intriguing physical properties (Schmidbaur & Schier, 2008; Katz et al., 2008; Puddephatt, 2008).

Over the course of our research on gold(I)-thiocyanate complexes we have observed a variety of interesting bonding motifs and luminescent properties (Coker et al., 2004; Arvapally et al., 2007) attributed to the [Au(SCN)2]- anion. The [Au(SCN)2]- anion has been observed as a monomer as well as adopting polymeric geometries. For example, in the tetraphenyl arsonium (Schwerdtferger et al., 1990) and phosphonium (Coker, 2003) salts, the [Au(SCN)2]- exists as a monomer. However, we have observed (Coker et al., 2004) that the alkali (K+, Rb+ and Cs+) salts of this anion preferentially adopt a linear one-dimensional polymeric chain motif with Au—Au distances in the 3.0065 (5)-3.2654 (2) Å range. Ammonium or tetramethylammonium salts of bis(thiocyanato)aurate(I) exhibit a slight variation on this one-dimensional bonding theme; tending toward linear or nearly linear motifs with alternating sets of gold-gold distances; NH4+ with distances of 3.1794 (2) and 3.2654 (2) Å (Coker et al., 2006) and Me4N+ with shorter distances of 3.1409 (3), 3.1723 (3) Å (Coker et al., 2004). Alternatively, the [Au(SCN)2]- anion crystallizes as a dimer unit with a gold-gold bond distance of 3.0700 (8) Å in the tetrabutylammonium salt complex (Coker et al., 2004).

More recently our investigations have turned to the alkaline earth salts of gold(I)-thiocyanate. Our motivation is to further explore the influence of the cation on the highly structurally-versatile behavior of the [Au(SCN)2]- anion. In the present work, the structure of the barium salt, (I), is presented.

The geometry of the anion in (I) (Fig. 1) is such that both monomeric and trimeric gold units are present with Au—Au and Au—S bond distances of 3.1687 (3) Å and 2.294 (2)-2.314 (2) Å, respectively. Within the trimer unit of (I), the gold atoms exist in differing environments; Au1 has a T-shaped three-coordinate geometry while Au2 has a square planar four-coordinate geometry. The monomeric gold, Au3, adopts a linear two-coordinate geometry. The S—Au1—Au2—S torsion angles, are intermediate between staggered and eclipsed (Table 1) geometries. As commented on by Pathaneni & Desiraju (1993) and further expanded by Anderson et al. (2007), complexes with larger Au—Au distances more frequently adopt an eclipsed conformation (L—Au—Au—L torsions ~ 0 or ±180°) presumably to lessen steric hindrance while the staggered conformation (L—Au—Au—L torsions \sim ±90°) is observed for smaller Au—Au distances. However it should be noted that there is a large spread of intermediates transitioning from eclipsed to staggered conformations with torsion angles in the ±50 to ±140° range.

The Au—Au bond distance observed in (I) is less than the sum of the van der Waals radii of 3.32 Å for a gold-gold interaction (Bondi, 1964). Furthermore, the recent literature (Schmidbaur & Schier, 2008; Katz et al., 2008; Puddephatt, 2008; Anderson et al., 2007) categorizes gold-gold distances in the range 2.5-3.5 Å as having significant Au—Au bonding character. In the structure presented here, the Au—Au distance is comparable to those cited for the large variety of gold complexes discussed in the literature (see, for instance, the varied works in Chem. Soc. Rev. (2008), 37, 1745–2140, a dedicated issue summarizing gold chemistry). The distance also agrees well with our work on the metallocrown complexes (dbz-18-crown-6-Ba)[bis(thiocyanato)aurate(I)] (Au—Au = 3.1109 (10) Å, Au—S = 2.288 (4)-2.305 (4) Å) (Stroud et al., 2009) and [CH3CN-(dbz-18-crown-6-Na)]2[Au(SCN)2]2.dbz-18-crown-6.CH3CN (Au—Au = 3.0661 (4) Å, Au—S = 2.291 (2)-2.303 (2) Å) (Coker, 2003) where dbz-18-crown-6 = (6,7,9,10,17,18,20,21-octahydro- 5,8,11,16,19,22-hexaoxa-dibenzo[a,j]cyclooctadecene. The Au—S bond distances for (I) are consistent with other metal-thiocyanate complexes (average M—S distance of 2.39 Å where M = Pt, Pd, Ag or Au) reported in the literature (Cambridge Structural Database, Allen, 2002).

The extended structure of (I) (Fig. 2) can be described as a three-dimensional coordination polymer generated by Ba···N intermolecular interactions. As is common, a high coordination number about the barium atom in (I) is achieved. The nine-coordinate Ba atom is bound to the nitrogen atoms of the thiocyanate groups, a coordinated acetonitrile molecule (N7) and a long contact with a thiocyanate sulfur (S4) of the monomeric gold unit (Ba—N distances range: 2.777 (6)-3.0444 (7) Å; Ba···S4 = 3.422 (2) Å). The core barium bridged unit consists of a barium-barium pair (Ba···Ba = 4.4341 (5) Å) bridged by three µ-N(thiocyanate) groups arising from N2 and N3 of the trimer and N4 of the monomer gold units. Furthermore, these barium chains are propogated through the lattice parallel to the b-axis. The gold trimer units crosslink neighboring barium chains in a diagonal fashion along the [1 0 1] direction. The monomeric gold units crosslink the barium chains in a diagonal fashion along the [-2 0 2] direction completing the three-dimensional net.

A similar situation where a gold-cyanato anion, [Au(CN)2]-, adopts multiple gold bonding motifs is observed for [poly[triaquatetra-µ-cyanido-tetracyanidobis(1,4,10,13-tetraoxa- 7,16-diazacyclo-octadecane) dibarium(II)tetragold(I) (Beavers et al., 2009). In that case, the coordination polymer consists of the [Au(CN)2]- anion in monomer, dimer and trimer environments (Au—Au = 3.2670 (2)-3.5655 (2) Å) while the barium atoms are bound to the diaza-18-crown-6 and solvent water molecules (Ba···N,O distances span the range 2.761 (2)-2.959 (3) Å).

To echo Katz et al. (2008) and Puddephatt (2008), taking advantage of AuI aurophilic or other transition metal metallophilic interactions leads to a very useful design strategy to increase structural dimensionality of metal complexes. These complexes are highly prized due to their tunable physical properties, e.g. magnetic, vapochromic and optical properties.

Related literature top

For further information on gold chemistry, see: Anderson et al. (2007); Bondi (1964); Pathaneni & Desiraju (1993); Arvapally et al. (2007); Beavers et al. (2009); Coker (2003); Coker et al. (2004, 2006); Katz et al. (2008); Puddephatt et al. (2008); Schmidbaur & Schier (2008); Schwerdtferger et al. (1990); Stroud et al. (2009). For a description of the Cambridge Structural Database, see: Allen (2002)

Experimental top

Reaction of barium hydroxide (1 equiv) with ammonium thiocyanate (2 equiv) in water results in the formation of barium thiocyanate with the release of ammonia gas. (I) was prepared following the method described by Coker et al. (2004). Crystals were obtained from slow diffusion of acetonitrile-diethyl ether solution at -4 °C.

Refinement top

The H-atoms were placed in calculated positions (C—H = 0.98 Å) and treated with a riding model. The isotropic displacement parameters were defined as 1.5Ueq of the adjacent atom. The largest residual electron-density peaks are located near the gold trimer unit (approx. 1.6 Å from S2 and S3).

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2009); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. : (a) Asymmetric unit of (I). (b) Partially extended structure of (I) showing the gold monomer (Au3, drawn in green) and trimer (Au1 and Au2, drawn in orange) units and the coordination about the barium atoms. Atomic labelling scheme and 50% probability ellipsoids are shown. [Symmetry codes: (i) x-3/2, y-1/2, -z+1/2; (ii) x, y-1, z; (iii) -x+2, -y+2, -z+1; (iv) -x+1, -y+1, -z+1].
[Figure 2] Fig. 2. : The three-dimensional polymeric network of (I) in the ac plane (Au atoms of the monomer and trimer units drawn in green and orange, respectively.)
poly[acetonitriletetra-µ2-thiocyanato-barium(II)digold(I)] top
Crystal data top
[Au2Ba(NCS)4(C2H3N)]F(000) = 1408
Mr = 804.65Dx = 3.466 Mg m3
Monoclinic, P21/nCu Kα radiation, λ = 1.54178 Å
Hall symbol: -P 2ynCell parameters from 7754 reflections
a = 11.5586 (3) Åθ = 4.1–67.6°
b = 7.4859 (2) ŵ = 59.69 mm1
c = 18.5798 (4) ÅT = 150 K
β = 106.450 (1)°Blade, colourless
V = 1541.84 (7) Å30.15 × 0.05 × 0.02 mm
Z = 4
Data collection top
Bruker SMART6000 CCD
diffractometer
2743 independent reflections
Radiation source: fine-focus sealed tube2559 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.053
Detector resolution: 0.8 pixels mm-1θmax = 67.6°, θmin = 5.0°
ω scansh = 1313
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
k = 88
Tmin = 0.060, Tmax = 0.302l = 2122
12455 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0458P)2 + 5.0574P]
where P = (Fo2 + 2Fc2)/3
2743 reflections(Δ/σ)max = 0.001
167 parametersΔρmax = 2.17 e Å3
0 restraintsΔρmin = 1.27 e Å3
Crystal data top
[Au2Ba(NCS)4(C2H3N)]V = 1541.84 (7) Å3
Mr = 804.65Z = 4
Monoclinic, P21/nCu Kα radiation
a = 11.5586 (3) ŵ = 59.69 mm1
b = 7.4859 (2) ÅT = 150 K
c = 18.5798 (4) Å0.15 × 0.05 × 0.02 mm
β = 106.450 (1)°
Data collection top
Bruker SMART6000 CCD
diffractometer
2743 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
2559 reflections with I > 2σ(I)
Tmin = 0.060, Tmax = 0.302Rint = 0.053
12455 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0310 restraints
wR(F2) = 0.079H-atom parameters constrained
S = 1.04Δρmax = 2.17 e Å3
2743 reflectionsΔρmin = 1.27 e Å3
167 parameters
Special details top

Experimental. A suitable crystal was mounted in a loop with paratone-N and immediately transferred to the goniostat bathed in a cold stream.

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.

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) top
xyzUiso*/Ueq
Au10.72117 (3)0.76278 (4)0.517412 (17)0.02210 (12)
Au20.50000.50000.50000.02498 (14)
Au31.00001.00000.50000.02274 (14)
Ba10.84629 (4)0.32246 (6)0.29512 (2)0.01596 (13)
S10.84496 (18)0.5362 (3)0.57927 (10)0.0253 (4)
N10.8661 (6)0.3726 (9)0.4462 (4)0.0262 (14)
C10.8583 (7)0.4404 (11)0.4997 (4)0.0245 (17)
S20.60587 (19)0.9988 (3)0.45766 (12)0.0306 (5)
N20.7123 (6)1.0410 (9)0.3392 (3)0.0215 (13)
C20.6706 (7)1.0228 (10)0.3884 (4)0.0218 (16)
S30.44661 (19)0.4332 (3)0.37321 (11)0.0342 (5)
N30.6338 (6)0.5268 (9)0.3097 (3)0.0210 (14)
C30.5617 (7)0.4914 (10)0.3398 (4)0.0193 (16)
S41.03510 (17)0.9889 (2)0.38459 (11)0.0226 (4)
N40.8861 (6)0.6993 (9)0.3176 (4)0.0246 (14)
C40.9461 (7)0.8143 (10)0.3464 (4)0.0213 (16)
N71.0607 (6)0.3524 (10)0.2496 (4)0.0303 (16)
C71.1298 (8)0.3672 (13)0.2172 (4)0.0303 (19)
C81.2207 (9)0.3905 (18)0.1769 (5)0.053 (3)
H11.30140.37710.21200.079*
H21.21280.50990.15440.079*
H31.20890.30010.13730.079*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Au10.02219 (19)0.0297 (2)0.01858 (19)0.00115 (12)0.01254 (14)0.00146 (11)
Au20.0244 (3)0.0357 (3)0.0208 (3)0.00001 (18)0.0161 (2)0.00502 (17)
Au30.0219 (2)0.0266 (3)0.0183 (3)0.00347 (17)0.00345 (18)0.00422 (16)
Ba10.0183 (2)0.0182 (2)0.0161 (2)0.00030 (16)0.01252 (17)0.00024 (15)
S10.0277 (10)0.0341 (11)0.0173 (9)0.0060 (8)0.0114 (8)0.0013 (8)
N10.034 (4)0.030 (4)0.016 (3)0.008 (3)0.010 (3)0.002 (3)
C10.024 (4)0.030 (4)0.022 (4)0.007 (3)0.009 (3)0.009 (3)
S20.0326 (11)0.0418 (12)0.0264 (11)0.0127 (9)0.0229 (9)0.0109 (8)
N20.026 (3)0.023 (3)0.018 (3)0.003 (3)0.010 (3)0.001 (2)
C20.018 (4)0.027 (4)0.023 (4)0.003 (3)0.008 (3)0.002 (3)
S30.0276 (10)0.0560 (14)0.0246 (10)0.0114 (10)0.0165 (9)0.0004 (9)
N30.023 (3)0.029 (4)0.015 (3)0.006 (3)0.011 (3)0.002 (2)
C30.021 (4)0.021 (4)0.015 (4)0.004 (3)0.005 (3)0.001 (3)
S40.0199 (9)0.0266 (10)0.0226 (10)0.0036 (7)0.0083 (7)0.0036 (7)
N40.024 (3)0.024 (4)0.028 (4)0.002 (3)0.012 (3)0.000 (3)
C40.027 (4)0.023 (4)0.019 (4)0.002 (3)0.015 (3)0.000 (3)
N70.025 (3)0.045 (4)0.024 (4)0.007 (3)0.012 (3)0.006 (3)
C70.029 (4)0.047 (5)0.015 (4)0.011 (4)0.006 (3)0.000 (3)
C80.034 (5)0.103 (9)0.027 (5)0.014 (6)0.019 (4)0.002 (5)
Geometric parameters (Å, º) top
Au1—S22.301 (2)Ba1—S4ii3.422 (2)
Au1—S12.305 (2)S1—C11.689 (8)
Au1—Au23.1687 (3)N1—C11.142 (10)
Au2—S32.314 (2)S2—C21.671 (8)
Au2—S3i2.315 (2)N2—C21.156 (10)
Au3—S42.2940 (19)S3—C31.677 (8)
Ba1—N12.777 (6)N3—C31.158 (10)
Ba1—N72.845 (7)S4—C41.690 (8)
Ba1—N2ii2.868 (6)N4—C41.140 (10)
Ba1—N42.869 (7)N7—C71.134 (11)
Ba1—N2iii2.899 (6)C7—C81.463 (12)
Ba1—N32.971 (6)C8—H10.9800
Ba1—N3iii3.000 (6)C8—H20.9800
Ba1—N4iii3.044 (7)C8—H30.9800
S2—Au1—S1177.06 (8)N1—Ba1—S4ii75.45 (14)
S2—Au1—Au295.00 (6)N7—Ba1—S4ii73.29 (16)
S1—Au1—Au287.88 (5)N2ii—Ba1—S4ii69.32 (14)
S3—Au2—S3i180.000 (1)N4—Ba1—S4ii126.36 (14)
S3—Au2—Au1i77.71 (5)N2iii—Ba1—S4ii142.31 (13)
S3—Au2—Au1102.29 (5)N3—Ba1—S4ii139.60 (12)
Au1i—Au2—Au1180.000 (11)N3iii—Ba1—S4ii67.75 (13)
S4—Au3—S4iv180.00 (9)N4iii—Ba1—S4ii115.49 (13)
N1—Ba1—N7117.4 (2)C1—S1—Au194.2 (3)
N1—Ba1—N2ii72.97 (19)C1—N1—Ba1159.3 (6)
N7—Ba1—N2ii136.8 (2)N1—C1—S1178.5 (8)
N1—Ba1—N475.90 (19)C2—S2—Au197.4 (3)
N7—Ba1—N481.3 (2)C2—N2—Ba1v133.8 (6)
N2ii—Ba1—N4139.29 (18)C2—N2—Ba1vi124.5 (6)
N1—Ba1—N2iii136.58 (19)Ba1v—N2—Ba1vi100.50 (19)
N7—Ba1—N2iii73.17 (19)N2—C2—S2178.0 (7)
N2ii—Ba1—N2iii130.30 (9)C3—S3—Au2108.0 (3)
N4—Ba1—N2iii63.85 (19)C3—N3—Ba1130.8 (5)
N1—Ba1—N370.83 (18)C3—N3—Ba1vi132.9 (5)
N7—Ba1—N3143.0 (2)Ba1—N3—Ba1vi95.91 (17)
N2ii—Ba1—N379.92 (18)N3—C3—S3173.1 (7)
N4—Ba1—N365.37 (18)C4—S4—Au399.9 (2)
N2iii—Ba1—N377.90 (17)C4—S4—Ba1v97.6 (3)
N1—Ba1—N3iii139.16 (18)Au3—S4—Ba1v99.81 (6)
N7—Ba1—N3iii68.39 (19)C4—N4—Ba1149.5 (6)
N2ii—Ba1—N3iii77.89 (17)C4—N4—Ba1vi113.3 (6)
N4—Ba1—N3iii141.35 (18)Ba1—N4—Ba1vi97.1 (2)
N2iii—Ba1—N3iii84.24 (18)N4—C4—S4176.9 (7)
N3—Ba1—N3iii131.05 (9)C7—N7—Ba1165.8 (7)
N1—Ba1—N4iii122.71 (19)N7—C7—C8178.3 (10)
N7—Ba1—N4iii119.52 (18)C7—C8—H1109.5
N2ii—Ba1—N4iii62.04 (18)C7—C8—H2109.5
N4—Ba1—N4iii118.15 (17)H1—C8—H2109.5
N2iii—Ba1—N4iii68.49 (18)C7—C8—H3109.5
N3—Ba1—N4iii68.12 (18)H1—C8—H3109.5
N3iii—Ba1—N4iii62.93 (18)H2—C8—H3109.5
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y1, z; (iii) x+3/2, y1/2, z+1/2; (iv) x+2, y+2, z+1; (v) x, y+1, z; (vi) x+3/2, y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Au2Ba(NCS)4(C2H3N)]
Mr804.65
Crystal system, space groupMonoclinic, P21/n
Temperature (K)150
a, b, c (Å)11.5586 (3), 7.4859 (2), 18.5798 (4)
β (°) 106.450 (1)
V3)1541.84 (7)
Z4
Radiation typeCu Kα
µ (mm1)59.69
Crystal size (mm)0.15 × 0.05 × 0.02
Data collection
DiffractometerBruker SMART6000 CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2003)
Tmin, Tmax0.060, 0.302
No. of measured, independent and
observed [I > 2σ(I)] reflections
12455, 2743, 2559
Rint0.053
(sin θ/λ)max1)0.600
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.079, 1.04
No. of reflections2743
No. of parameters167
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)2.17, 1.27

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2009).

 

Acknowledgements

Funding for the diffractometer through NSF–MRI grant CHE-0215950 is gratefully acknowledged. The authors thank Dr Allen G. Oliver (University of Notre Dame) for insightful discussion.

References

First citationAllen, F. H. (2002). Acta Cryst. B58, 380–388.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationAnderson, K. M., Goeta, A. E. & Steed, J. W. (2007). Inorg. Chem. 46, 6444–5451.  Web of Science CrossRef PubMed CAS Google Scholar
First citationArvapally, R. K., Sinha, P., Hettiarachchi, S. R., Coker, N. L., Bedel, C. E., Patterson, H. H., Elder, R. C., Wilson, A. K. & Omary, M. A. (2007). J. Phys. Chem. 111, 10689–10699.  CAS Google Scholar
First citationBeavers, C. M., Paw, U. L. & Olmstead, M. M. (2009). Acta Cryst. E65, m300–m301.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationBondi, A. (1964). J. Phys. Chem. 68, 441–451.  CrossRef CAS Web of Science Google Scholar
First citationBrandenburg, K. (2009). DIAMOND. Crystal Impact GbR, Bonn, Germany.  Google Scholar
First citationBruker (2003). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationCoker, N. L. (2003). PhD dissertation, University of Cincinnati, USA.  Google Scholar
First citationCoker, N. L., Bedel, C. E., Krause, J. A. & Elder, R. C. (2006). Acta Cryst. E62, m319–m321.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationCoker, N. L., Krause-Bauer, J. A. & Elder, R. C. (2004). J. Am. Chem. Soc. 126, 12–13.  Web of Science CrossRef PubMed CAS Google Scholar
First citationKatz, M. J., Sakai, K. & Leznoff, D. B. (2008). Chem. Soc. Rev. 37, 1884–1895.  Web of Science CrossRef PubMed CAS Google Scholar
First citationPathaneni, S. S. & Desiraju, G. R. (1993). J. Chem. Soc. Dalton Trans. pp. 319–322.  CrossRef Web of Science Google Scholar
First citationPuddephatt, R. J. (2008). Chem. Soc. Rev. 37, 2012–2027.  Web of Science CrossRef PubMed CAS Google Scholar
First citationSchmidbaur, H. & Schier, A. (2008). Chem. Soc. Rev. 37, 1931–1951.  Web of Science CrossRef PubMed CAS Google Scholar
First citationSchwerdtferger, P., Boyd, P., Burrell, A., Robinson, W. & Taylor, M. (1990). Inorg. Chem. 29, 3593–3607.  Google Scholar
First citationSheldrick, G. M. (2003). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationStroud, T. L., Coker, N. L. & Krause, J. A. (2009). Acta Cryst. E65, m1509–m1510.  Web of Science CSD CrossRef IUCr Journals Google Scholar

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Volume 66| Part 7| July 2010| Pages m765-m766
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