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

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Crystal structure of chlorido­penta­kis(di­methyl sulfoxide-κO)chromium(III) dichloride

aDepartment of Chemistry, Chungnam National University, Daejeon 305-764, Republic of Korea
*Correspondence e-mail: skkang@cnu.ac.kr

Edited by M. Weil, Vienna University of Technology, Austria (Received 6 July 2014; accepted 7 July 2014; online 1 August 2014)

In the complex cation of the title salt, [CrCl(C2H6OS)5]Cl2, the CrIII ion is coordinated by one chloride ligand and five O atoms from dimethyl sulfoxide (DMSO) ligands, leading to a slightly distorted octa­hedral coordination environment [O—Cr—O angles range from 86.69 (16) to 92.87 (16)°]. In the crystal, complex cations are arranged in hexa­gonally packed rows parallel to [010], with the chloride counter-anions situated in between. The inter­actions between cations and anions are mainly ionic in nature.

1. Related literature

For the preparation and structures of DMSO solvates of transition metal cations, see: Abbasi et al. (2007[Abbasi, A., Risberg, E. D., Eriksson, L., Mink, J., Persson, I., Sandström, M., Sidorov, Y. V., Skripkin, M. Y. & Ullström, A.-S. (2007). Inorg. Chem. 46, 7731-7741.]); Al-Najjar et al. (2013[Al-Najjar, N. A., Al-Sudani, A.-R. H., Shanshal, M. A., Mousa, F. H. & Kariuki, B. M. (2013). Acta Cryst. E69, m395-m396.]); Bratsos et al. (2013[Bratsos, I., Calmo, S., Zangrando, E., Balducci, G. & Alessio, E. (2013). Inorg. Chem. 52, 12120-12130.]); Niu et al. (2012[Niu, M., Fan, S. & Liu, G. (2012). Acta Cryst. E68, m67.]); Srivastava et al. (2009[Srivastava, R. S., Fronczek, F. R. & Perkins, R. S. (2009). J. Coord. Chem. 62, 3745-3753.]).

[Scheme 1]

2. Experimental

2.1. Crystal data

  • [CrCl(C2H6OS)5]Cl2

  • Mr = 548.99

  • Triclinic, [P \overline 1]

  • a = 9.5883 (4) Å

  • b = 10.4998 (4) Å

  • c = 13.0088 (5) Å

  • α = 70.633 (4)°

  • β = 83.867 (3)°

  • γ = 89.0009 (18)°

  • V = 1228.26 (9) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 1.23 mm−1

  • T = 296 K

  • 0.10 × 0.06 × 0.05 mm

2.2. Data collection

  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2002[Bruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.905, Tmax = 0.935

  • 19400 measured reflections

  • 4576 independent reflections

  • 2587 reflections with I > 2σ(I)

  • Rint = 0.115

2.3. Refinement

  • R[F2 > 2σ(F2)] = 0.072

  • wR(F2) = 0.138

  • S = 0.98

  • 4576 reflections

  • 227 parameters

  • H-atom parameters constrained

  • Δρmax = 0.59 e Å−3

  • Δρmin = −0.47 e Å−3

Table 1
Selected bond lengths (Å)

Cr1—O3 1.967 (4)
Cr1—O19 1.971 (4)
Cr1—O7 1.975 (4)
Cr1—O11 1.977 (4)
Cr1—O15 1.982 (4)
Cr1—Cl2 2.3096 (18)

Data collection: SMART (Bruker, 2002[Bruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2002[Bruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).

Supporting information


Related literature top

For the preparation and structures of DMSO solvates of transition metal cations, see: Abbasi et al. (2007); Al-Najjar et al. (2013); Bratsos et al. (2013); Niu et al. (2012); Srivastava et al. (2009).

Experimental top

All manipulations were carried out under nitrogen atmosphere using standard Schlenk techniques or in a purified nitrogen-filled drybox, and all solvents were dried and distilled prior to use according to standard methods. The title mononuclear complex was synthesized during an attempt to prepare a chromium(III) complex with 2,6-bis[(5-methyl-4-phenyl-1H-pyrazol-1-yl)methyl]pyridine. To a solution of CrCl3(THF)3 (0.1124 g, 0.3 mmol) in THF (6 ml) was added a solution of the organic ligand (0.126 g, 0.3 mmol) in THF (4 ml) dropwise at 333 K. The solution was stirred vigorously. A green suspension was formed immediately in 5 min, and the mixture was stirred overnight at this temperature. The product was isolated as a green powder by removing the solvent, washed repeatedly with THF followed by diethyl ether, and dried under vacuum. Bright green crystals of the title compound were obtained by slow diffusion of diethyl ether into a concentrated solution of the green solid in DMSO within one to two days.

Refinement top

All H atoms were positioned geometrically and refined using a riding model, with C—H = 0.96 Å, and with Uiso(H) = 1.5Ueq(C).

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound, with the atom-numbering scheme and displacement ellipsoids drawn at the 30% probability level.
[Figure 2] Fig. 2. The crystal structure of the title compound in a perspective view along [100].
Chloridopentakis(dimethyl sulfoxide-κO)chromium(III) dichloride top
Crystal data top
[CrCl(C2H6OS)5]Cl2Z = 2
Mr = 548.99F(000) = 570
Triclinic, P1Dx = 1.484 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.5883 (4) ÅCell parameters from 2991 reflections
b = 10.4998 (4) Åθ = 2.2–28.2°
c = 13.0088 (5) ŵ = 1.23 mm1
α = 70.633 (4)°T = 296 K
β = 83.867 (3)°Block, green
γ = 89.0009 (18)°0.10 × 0.06 × 0.05 mm
V = 1228.26 (9) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
2587 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.115
ϕ and ω scansθmax = 25.5°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1111
Tmin = 0.905, Tmax = 0.935k = 1212
19400 measured reflectionsl = 1515
4576 independent reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.072H-atom parameters constrained
wR(F2) = 0.138 w = 1/[σ2(Fo2) + (0.0582P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max < 0.001
4576 reflectionsΔρmax = 0.59 e Å3
227 parametersΔρmin = 0.47 e Å3
Crystal data top
[CrCl(C2H6OS)5]Cl2γ = 89.0009 (18)°
Mr = 548.99V = 1228.26 (9) Å3
Triclinic, P1Z = 2
a = 9.5883 (4) ÅMo Kα radiation
b = 10.4998 (4) ŵ = 1.23 mm1
c = 13.0088 (5) ÅT = 296 K
α = 70.633 (4)°0.10 × 0.06 × 0.05 mm
β = 83.867 (3)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
4576 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
2587 reflections with I > 2σ(I)
Tmin = 0.905, Tmax = 0.935Rint = 0.115
19400 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0720 restraints
wR(F2) = 0.138H-atom parameters constrained
S = 0.98Δρmax = 0.59 e Å3
4576 reflectionsΔρmin = 0.47 e Å3
227 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cr10.73481 (10)0.87030 (9)0.21633 (7)0.0237 (3)
Cl20.75680 (18)1.04916 (16)0.05360 (12)0.0396 (4)
O30.5471 (4)0.8278 (4)0.1872 (3)0.0355 (11)
S40.49654 (17)0.68654 (16)0.19631 (13)0.0332 (4)
C50.5051 (8)0.6874 (7)0.0590 (5)0.055 (2)
H5A0.46330.7680.01490.082*
H5B0.45540.60980.05710.082*
H5C0.60140.68490.03070.082*
C60.3132 (6)0.6983 (7)0.2227 (5)0.0436 (18)
H6A0.2910.70470.29460.065*
H6B0.2680.61940.21890.065*
H6C0.2810.77710.16910.065*
O70.6490 (4)0.9863 (4)0.2973 (3)0.0296 (10)
S80.53284 (17)1.08678 (15)0.25183 (13)0.0306 (4)
C90.4206 (7)1.0783 (6)0.3701 (5)0.0445 (18)
H9A0.37760.99010.40090.067*
H9B0.34921.14480.35110.067*
H9C0.47371.09560.42280.067*
C100.6119 (7)1.2474 (6)0.2266 (5)0.0452 (19)
H10A0.65711.24670.28920.068*
H10B0.54131.31510.21330.068*
H10C0.68031.26720.16350.068*
O110.9199 (4)0.9089 (4)0.2546 (3)0.0327 (11)
S120.97576 (18)1.05332 (16)0.23286 (13)0.0342 (4)
C131.0000 (8)1.0568 (8)0.3636 (5)0.057 (2)
H13A0.91071.06370.40220.086*
H13B1.05831.13320.35670.086*
H13C1.04440.97530.40340.086*
C141.1538 (7)1.0469 (8)0.1831 (6)0.067 (3)
H14A1.19920.97650.23580.101*
H14B1.19951.13190.17130.101*
H14C1.15931.02860.11520.101*
O150.8145 (4)0.7458 (4)0.1404 (3)0.0339 (11)
S160.93855 (17)0.65183 (16)0.17455 (13)0.0339 (4)
C171.0204 (7)0.6520 (7)0.0464 (5)0.053 (2)
H17A0.95180.63180.00510.079*
H17B1.09170.58490.05750.079*
H17C1.06210.73930.00680.079*
C180.8644 (8)0.4878 (6)0.2216 (6)0.061 (2)
H18A0.81880.4690.29460.091*
H18B0.9370.42350.22190.091*
H18C0.7970.48120.1740.091*
O190.7205 (4)0.7130 (4)0.3520 (3)0.0343 (11)
S200.73602 (17)0.72155 (15)0.46602 (13)0.0306 (4)
C210.6037 (6)0.6113 (6)0.5523 (5)0.0422 (18)
H21A0.51340.64520.53180.063*
H21B0.61030.60510.62690.063*
H21C0.6150.52340.54530.063*
C220.8822 (7)0.6230 (8)0.5089 (6)0.062 (2)
H22A0.8740.53830.49660.092*
H22B0.88640.60680.58560.092*
H22C0.96610.66980.46810.092*
Cl230.25112 (19)0.74394 (19)0.49760 (15)0.0542 (5)
Cl240.2423 (2)0.37459 (18)0.19086 (17)0.0579 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0290 (6)0.0197 (5)0.0227 (5)0.0021 (4)0.0077 (4)0.0062 (4)
Cl20.0555 (12)0.0340 (10)0.0231 (9)0.0017 (8)0.0081 (8)0.0000 (7)
O30.034 (3)0.023 (2)0.053 (3)0.002 (2)0.012 (2)0.014 (2)
S40.0379 (11)0.0255 (9)0.0383 (10)0.0026 (8)0.0171 (8)0.0094 (8)
C50.063 (5)0.066 (5)0.049 (5)0.014 (4)0.016 (4)0.034 (4)
C60.041 (4)0.038 (4)0.051 (5)0.008 (3)0.008 (4)0.013 (4)
O70.039 (3)0.029 (2)0.027 (2)0.013 (2)0.012 (2)0.015 (2)
S80.0377 (10)0.0240 (9)0.0313 (10)0.0053 (8)0.0101 (8)0.0091 (8)
C90.047 (5)0.035 (4)0.044 (4)0.008 (4)0.000 (4)0.005 (3)
C100.056 (5)0.029 (4)0.043 (4)0.002 (4)0.002 (4)0.003 (3)
O110.029 (2)0.026 (2)0.045 (3)0.001 (2)0.018 (2)0.010 (2)
S120.0416 (11)0.0294 (10)0.0357 (10)0.0013 (8)0.0127 (8)0.0137 (8)
C130.067 (5)0.078 (6)0.039 (5)0.003 (4)0.001 (4)0.037 (4)
C140.056 (5)0.081 (6)0.079 (6)0.026 (5)0.026 (5)0.054 (5)
O150.038 (3)0.033 (3)0.039 (3)0.011 (2)0.015 (2)0.021 (2)
S160.0357 (10)0.0292 (10)0.0389 (10)0.0055 (8)0.0094 (8)0.0124 (8)
C170.053 (5)0.043 (5)0.057 (5)0.003 (4)0.011 (4)0.014 (4)
C180.073 (6)0.023 (4)0.064 (5)0.001 (4)0.014 (4)0.009 (4)
O190.050 (3)0.021 (2)0.028 (3)0.002 (2)0.007 (2)0.0026 (19)
S200.0389 (10)0.0239 (9)0.0280 (9)0.0043 (8)0.0089 (8)0.0057 (7)
C210.039 (4)0.044 (4)0.037 (4)0.007 (3)0.002 (3)0.007 (3)
C220.041 (5)0.074 (6)0.067 (6)0.020 (4)0.027 (4)0.014 (5)
Cl230.0512 (12)0.0524 (12)0.0527 (12)0.0007 (10)0.0000 (10)0.0108 (10)
Cl240.0641 (13)0.0360 (11)0.0797 (15)0.0096 (9)0.0272 (11)0.0217 (10)
Geometric parameters (Å, º) top
Cr1—O31.967 (4)S12—C141.768 (7)
Cr1—O191.971 (4)C13—H13A0.96
Cr1—O71.975 (4)C13—H13B0.96
Cr1—O111.977 (4)C13—H13C0.96
Cr1—O151.982 (4)C14—H14A0.96
Cr1—Cl22.3096 (18)C14—H14B0.96
O3—S41.531 (4)C14—H14C0.96
S4—C61.764 (6)O15—S161.539 (4)
S4—C51.777 (6)S16—C181.760 (6)
C5—H5A0.96S16—C171.765 (6)
C5—H5B0.96C17—H17A0.96
C5—H5C0.96C17—H17B0.96
C6—H6A0.96C17—H17C0.96
C6—H6B0.96C18—H18A0.96
C6—H6C0.96C18—H18B0.96
O7—S81.546 (4)C18—H18C0.96
S8—C91.758 (6)O19—S201.538 (4)
S8—C101.775 (6)S20—C221.755 (6)
C9—H9A0.96S20—C211.760 (6)
C9—H9B0.96C21—H21A0.96
C9—H9C0.96C21—H21B0.96
C10—H10A0.96C21—H21C0.96
C10—H10B0.96C22—H22A0.96
C10—H10C0.96C22—H22B0.96
O11—S121.542 (4)C22—H22C0.96
S12—C131.753 (6)
O3—Cr1—O1990.28 (17)O11—S12—C13103.8 (3)
O3—Cr1—O789.61 (16)O11—S12—C14103.4 (3)
O19—Cr1—O790.78 (16)C13—S12—C1498.5 (4)
O3—Cr1—O11176.76 (18)S12—C13—H13A109.5
O19—Cr1—O1186.97 (17)S12—C13—H13B109.5
O7—Cr1—O1188.70 (16)H13A—C13—H13B109.5
O3—Cr1—O1588.69 (16)S12—C13—H13C109.5
O19—Cr1—O1586.69 (16)H13A—C13—H13C109.5
O7—Cr1—O15176.95 (18)H13B—C13—H13C109.5
O11—Cr1—O1592.87 (16)S12—C14—H14A109.5
O3—Cr1—Cl290.00 (13)S12—C14—H14B109.5
O19—Cr1—Cl2177.61 (13)H14A—C14—H14B109.5
O7—Cr1—Cl291.59 (12)S12—C14—H14C109.5
O11—Cr1—Cl292.82 (13)H14A—C14—H14C109.5
O15—Cr1—Cl290.95 (13)H14B—C14—H14C109.5
S4—O3—Cr1124.5 (2)S16—O15—Cr1125.3 (2)
O3—S4—C6101.8 (3)O15—S16—C18104.8 (3)
O3—S4—C5105.0 (3)O15—S16—C17101.7 (3)
C6—S4—C599.0 (3)C18—S16—C1798.8 (3)
S4—C5—H5A109.5S16—C17—H17A109.5
S4—C5—H5B109.5S16—C17—H17B109.5
H5A—C5—H5B109.5H17A—C17—H17B109.5
S4—C5—H5C109.5S16—C17—H17C109.5
H5A—C5—H5C109.5H17A—C17—H17C109.5
H5B—C5—H5C109.5H17B—C17—H17C109.5
S4—C6—H6A109.5S16—C18—H18A109.5
S4—C6—H6B109.5S16—C18—H18B109.5
H6A—C6—H6B109.5H18A—C18—H18B109.5
S4—C6—H6C109.5S16—C18—H18C109.5
H6A—C6—H6C109.5H18A—C18—H18C109.5
H6B—C6—H6C109.5H18B—C18—H18C109.5
S8—O7—Cr1121.5 (2)S20—O19—Cr1123.9 (2)
O7—S8—C9103.2 (3)O19—S20—C22104.6 (3)
O7—S8—C10103.8 (3)O19—S20—C21103.8 (3)
C9—S8—C1098.7 (3)C22—S20—C2198.7 (3)
S8—C9—H9A109.5S20—C21—H21A109.5
S8—C9—H9B109.5S20—C21—H21B109.5
H9A—C9—H9B109.5H21A—C21—H21B109.5
S8—C9—H9C109.5S20—C21—H21C109.5
H9A—C9—H9C109.5H21A—C21—H21C109.5
H9B—C9—H9C109.5H21B—C21—H21C109.5
S8—C10—H10A109.5S20—C22—H22A109.5
S8—C10—H10B109.5S20—C22—H22B109.5
H10A—C10—H10B109.5H22A—C22—H22B109.5
S8—C10—H10C109.5S20—C22—H22C109.5
H10A—C10—H10C109.5H22A—C22—H22C109.5
H10B—C10—H10C109.5H22B—C22—H22C109.5
S12—O11—Cr1123.0 (2)
Selected bond lengths (Å) top
Cr1—O31.967 (4)Cr1—O111.977 (4)
Cr1—O191.971 (4)Cr1—O151.982 (4)
Cr1—O71.975 (4)Cr1—Cl22.3096 (18)
 

Acknowledgements

Financial support from the National Research Foundation of Korea (NRF-2012R1A1A1005839) is gratefully acknowledged.

References

First citationAbbasi, A., Risberg, E. D., Eriksson, L., Mink, J., Persson, I., Sandström, M., Sidorov, Y. V., Skripkin, M. Y. & Ullström, A.-S. (2007). Inorg. Chem. 46, 7731–7741.  Web of Science CSD CrossRef PubMed CAS Google Scholar
First citationAl-Najjar, N. A., Al-Sudani, A.-R. H., Shanshal, M. A., Mousa, F. H. & Kariuki, B. M. (2013). Acta Cryst. E69, m395–m396.  CSD CrossRef CAS IUCr Journals Google Scholar
First citationBratsos, I., Calmo, S., Zangrando, E., Balducci, G. & Alessio, E. (2013). Inorg. Chem. 52, 12120–12130.  Web of Science CSD CrossRef CAS PubMed Google Scholar
First citationBruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationFarrugia, L. J. (2012). J. Appl. Cryst. 45, 849–854.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationNiu, M., Fan, S. & Liu, G. (2012). Acta Cryst. E68, m67.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSrivastava, R. S., Fronczek, F. R. & Perkins, R. S. (2009). J. Coord. Chem. 62, 3745–3753.  Web of Science CSD CrossRef CAS Google Scholar

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