Crystal structure of chlorido-penta-kis(dimethyl sulfoxide-κO)chromium(III) dichloride.

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

Related literature

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

Crystal data

[CrCl(C2H6OS)5]Cl2

M = 548.99

Triclinic,

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

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2002 ▶) T min = 0.905, T max = 0.935

19400 measured reflections

4576 independent reflections

2587 reflections with I > 2σ(I)

R int = 0.115

Refinement

R[F 2 > 2σ(F 2)] = 0.072

wR(F 2) = 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

Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); data reduction: SAINT; 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 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536814015852/wm5034sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814015852/wm5034Isup2.hkl

Click here for additional data file.

. DOI: 10.1107/S1600536814015852/wm5034fig1.tif

The asymmetric unit of the title compound, with the atom-numbering scheme and displacement ellipsoids drawn at the 30% probability level.

Click here for additional data file.

. DOI: 10.1107/S1600536814015852/wm5034fig2.tif

The crystal structure of the title compound in a perspective view along [100].

CCDC reference: 1012642

Additional supporting information: crystallographic information; 3D view; checkCIF report

[CrCl(C2H6OS)5]Cl2	Z = 2
Mr = 548.99	F(000) = 570
Triclinic, P1	Dx = 1.484 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.5883 (4) Å	Cell parameters from 2991 reflections
b = 10.4998 (4) Å	θ = 2.2–28.2°
c = 13.0088 (5) Å	µ = 1.23 mm−1
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

Bruker SMART CCD area-detector diffractometer	2587 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.115
φ and ω scans	θmax = 25.5°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −11→11
Tmin = 0.905, Tmax = 0.935	k = −12→12
19400 measured reflections	l = −15→15
4576 independent reflections

Refinement on F2	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.072	H-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 reflections	Δρmax = 0.59 e Å−3
227 parameters	Δρmin = −0.47 e Å−3

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.

	x	y	z	Uiso*/Ueq
Cr1	0.73481 (10)	0.87030 (9)	0.21633 (7)	0.0237 (3)
Cl2	0.75680 (18)	1.04916 (16)	0.05360 (12)	0.0396 (4)
O3	0.5471 (4)	0.8278 (4)	0.1872 (3)	0.0355 (11)
S4	0.49654 (17)	0.68654 (16)	0.19631 (13)	0.0332 (4)
C5	0.5051 (8)	0.6874 (7)	0.0590 (5)	0.055 (2)
H5A	0.4633	0.768	0.0149	0.082*
H5B	0.4554	0.6098	0.0571	0.082*
H5C	0.6014	0.6849	0.0307	0.082*
C6	0.3132 (6)	0.6983 (7)	0.2227 (5)	0.0436 (18)
H6A	0.291	0.7047	0.2946	0.065*
H6B	0.268	0.6194	0.2189	0.065*
H6C	0.281	0.7771	0.1691	0.065*
O7	0.6490 (4)	0.9863 (4)	0.2973 (3)	0.0296 (10)
S8	0.53284 (17)	1.08678 (15)	0.25183 (13)	0.0306 (4)
C9	0.4206 (7)	1.0783 (6)	0.3701 (5)	0.0445 (18)
H9A	0.3776	0.9901	0.4009	0.067*
H9B	0.3492	1.1448	0.3511	0.067*
H9C	0.4737	1.0956	0.4228	0.067*
C10	0.6119 (7)	1.2474 (6)	0.2266 (5)	0.0452 (19)
H10A	0.6571	1.2467	0.2892	0.068*
H10B	0.5413	1.3151	0.2133	0.068*
H10C	0.6803	1.2672	0.1635	0.068*
O11	0.9199 (4)	0.9089 (4)	0.2546 (3)	0.0327 (11)
S12	0.97576 (18)	1.05332 (16)	0.23286 (13)	0.0342 (4)
C13	1.0000 (8)	1.0568 (8)	0.3636 (5)	0.057 (2)
H13A	0.9107	1.0637	0.4022	0.086*
H13B	1.0583	1.1332	0.3567	0.086*
H13C	1.0444	0.9753	0.4034	0.086*
C14	1.1538 (7)	1.0469 (8)	0.1831 (6)	0.067 (3)
H14A	1.1992	0.9765	0.2358	0.101*
H14B	1.1995	1.1319	0.1713	0.101*
H14C	1.1593	1.0286	0.1152	0.101*
O15	0.8145 (4)	0.7458 (4)	0.1404 (3)	0.0339 (11)
S16	0.93855 (17)	0.65183 (16)	0.17455 (13)	0.0339 (4)
C17	1.0204 (7)	0.6520 (7)	0.0464 (5)	0.053 (2)
H17A	0.9518	0.6318	0.0051	0.079*
H17B	1.0917	0.5849	0.0575	0.079*
H17C	1.0621	0.7393	0.0068	0.079*
C18	0.8644 (8)	0.4878 (6)	0.2216 (6)	0.061 (2)
H18A	0.8188	0.469	0.2946	0.091*
H18B	0.937	0.4235	0.2219	0.091*
H18C	0.797	0.4812	0.174	0.091*
O19	0.7205 (4)	0.7130 (4)	0.3520 (3)	0.0343 (11)
S20	0.73602 (17)	0.72155 (15)	0.46602 (13)	0.0306 (4)
C21	0.6037 (6)	0.6113 (6)	0.5523 (5)	0.0422 (18)
H21A	0.5134	0.6452	0.5318	0.063*
H21B	0.6103	0.6051	0.6269	0.063*
H21C	0.615	0.5234	0.5453	0.063*
C22	0.8822 (7)	0.6230 (8)	0.5089 (6)	0.062 (2)
H22A	0.874	0.5383	0.4966	0.092*
H22B	0.8864	0.6068	0.5856	0.092*
H22C	0.9661	0.6698	0.4681	0.092*
Cl23	0.25112 (19)	0.74394 (19)	0.49760 (15)	0.0542 (5)
Cl24	0.2423 (2)	0.37459 (18)	0.19086 (17)	0.0579 (6)

	U11	U22	U33	U12	U13	U23
Cr1	0.0290 (6)	0.0197 (5)	0.0227 (5)	0.0021 (4)	−0.0077 (4)	−0.0062 (4)
Cl2	0.0555 (12)	0.0340 (10)	0.0231 (9)	0.0017 (8)	−0.0081 (8)	0.0000 (7)
O3	0.034 (3)	0.023 (2)	0.053 (3)	0.002 (2)	−0.012 (2)	−0.014 (2)
S4	0.0379 (11)	0.0255 (9)	0.0383 (10)	0.0026 (8)	−0.0171 (8)	−0.0094 (8)
C5	0.063 (5)	0.066 (5)	0.049 (5)	0.014 (4)	−0.016 (4)	−0.034 (4)
C6	0.041 (4)	0.038 (4)	0.051 (5)	−0.008 (3)	−0.008 (4)	−0.013 (4)
O7	0.039 (3)	0.029 (2)	0.027 (2)	0.013 (2)	−0.012 (2)	−0.015 (2)
S8	0.0377 (10)	0.0240 (9)	0.0313 (10)	0.0053 (8)	−0.0101 (8)	−0.0091 (8)
C9	0.047 (5)	0.035 (4)	0.044 (4)	0.008 (4)	0.000 (4)	−0.005 (3)
C10	0.056 (5)	0.029 (4)	0.043 (4)	0.002 (4)	−0.002 (4)	−0.003 (3)
O11	0.029 (2)	0.026 (2)	0.045 (3)	−0.001 (2)	−0.018 (2)	−0.010 (2)
S12	0.0416 (11)	0.0294 (10)	0.0357 (10)	0.0013 (8)	−0.0127 (8)	−0.0137 (8)
C13	0.067 (5)	0.078 (6)	0.039 (5)	−0.003 (4)	−0.001 (4)	−0.037 (4)
C14	0.056 (5)	0.081 (6)	0.079 (6)	−0.026 (5)	0.026 (5)	−0.054 (5)
O15	0.038 (3)	0.033 (3)	0.039 (3)	0.011 (2)	−0.015 (2)	−0.021 (2)
S16	0.0357 (10)	0.0292 (10)	0.0389 (10)	0.0055 (8)	−0.0094 (8)	−0.0124 (8)
C17	0.053 (5)	0.043 (5)	0.057 (5)	0.003 (4)	0.011 (4)	−0.014 (4)
C18	0.073 (6)	0.023 (4)	0.064 (5)	−0.001 (4)	0.014 (4)	0.009 (4)
O19	0.050 (3)	0.021 (2)	0.028 (3)	0.002 (2)	−0.007 (2)	−0.0026 (19)
S20	0.0389 (10)	0.0239 (9)	0.0280 (9)	0.0043 (8)	−0.0089 (8)	−0.0057 (7)
C21	0.039 (4)	0.044 (4)	0.037 (4)	−0.007 (3)	0.002 (3)	−0.007 (3)
C22	0.041 (5)	0.074 (6)	0.067 (6)	0.020 (4)	−0.027 (4)	−0.014 (5)
Cl23	0.0512 (12)	0.0524 (12)	0.0527 (12)	0.0007 (10)	0.0000 (10)	−0.0108 (10)
Cl24	0.0641 (13)	0.0360 (11)	0.0797 (15)	0.0096 (9)	−0.0272 (11)	−0.0217 (10)

Cr1—O3	1.967 (4)	S12—C14	1.768 (7)
Cr1—O19	1.971 (4)	C13—H13A	0.96
Cr1—O7	1.975 (4)	C13—H13B	0.96
Cr1—O11	1.977 (4)	C13—H13C	0.96
Cr1—O15	1.982 (4)	C14—H14A	0.96
Cr1—Cl2	2.3096 (18)	C14—H14B	0.96
O3—S4	1.531 (4)	C14—H14C	0.96
S4—C6	1.764 (6)	O15—S16	1.539 (4)
S4—C5	1.777 (6)	S16—C18	1.760 (6)
C5—H5A	0.96	S16—C17	1.765 (6)
C5—H5B	0.96	C17—H17A	0.96
C5—H5C	0.96	C17—H17B	0.96
C6—H6A	0.96	C17—H17C	0.96
C6—H6B	0.96	C18—H18A	0.96
C6—H6C	0.96	C18—H18B	0.96
O7—S8	1.546 (4)	C18—H18C	0.96
S8—C9	1.758 (6)	O19—S20	1.538 (4)
S8—C10	1.775 (6)	S20—C22	1.755 (6)
C9—H9A	0.96	S20—C21	1.760 (6)
C9—H9B	0.96	C21—H21A	0.96
C9—H9C	0.96	C21—H21B	0.96
C10—H10A	0.96	C21—H21C	0.96
C10—H10B	0.96	C22—H22A	0.96
C10—H10C	0.96	C22—H22B	0.96
O11—S12	1.542 (4)	C22—H22C	0.96
S12—C13	1.753 (6)
O3—Cr1—O19	90.28 (17)	O11—S12—C13	103.8 (3)
O3—Cr1—O7	89.61 (16)	O11—S12—C14	103.4 (3)
O19—Cr1—O7	90.78 (16)	C13—S12—C14	98.5 (4)
O3—Cr1—O11	176.76 (18)	S12—C13—H13A	109.5
O19—Cr1—O11	86.97 (17)	S12—C13—H13B	109.5
O7—Cr1—O11	88.70 (16)	H13A—C13—H13B	109.5
O3—Cr1—O15	88.69 (16)	S12—C13—H13C	109.5
O19—Cr1—O15	86.69 (16)	H13A—C13—H13C	109.5
O7—Cr1—O15	176.95 (18)	H13B—C13—H13C	109.5
O11—Cr1—O15	92.87 (16)	S12—C14—H14A	109.5
O3—Cr1—Cl2	90.00 (13)	S12—C14—H14B	109.5
O19—Cr1—Cl2	177.61 (13)	H14A—C14—H14B	109.5
O7—Cr1—Cl2	91.59 (12)	S12—C14—H14C	109.5
O11—Cr1—Cl2	92.82 (13)	H14A—C14—H14C	109.5
O15—Cr1—Cl2	90.95 (13)	H14B—C14—H14C	109.5
S4—O3—Cr1	124.5 (2)	S16—O15—Cr1	125.3 (2)
O3—S4—C6	101.8 (3)	O15—S16—C18	104.8 (3)
O3—S4—C5	105.0 (3)	O15—S16—C17	101.7 (3)
C6—S4—C5	99.0 (3)	C18—S16—C17	98.8 (3)
S4—C5—H5A	109.5	S16—C17—H17A	109.5
S4—C5—H5B	109.5	S16—C17—H17B	109.5
H5A—C5—H5B	109.5	H17A—C17—H17B	109.5
S4—C5—H5C	109.5	S16—C17—H17C	109.5
H5A—C5—H5C	109.5	H17A—C17—H17C	109.5
H5B—C5—H5C	109.5	H17B—C17—H17C	109.5
S4—C6—H6A	109.5	S16—C18—H18A	109.5
S4—C6—H6B	109.5	S16—C18—H18B	109.5
H6A—C6—H6B	109.5	H18A—C18—H18B	109.5
S4—C6—H6C	109.5	S16—C18—H18C	109.5
H6A—C6—H6C	109.5	H18A—C18—H18C	109.5
H6B—C6—H6C	109.5	H18B—C18—H18C	109.5
S8—O7—Cr1	121.5 (2)	S20—O19—Cr1	123.9 (2)
O7—S8—C9	103.2 (3)	O19—S20—C22	104.6 (3)
O7—S8—C10	103.8 (3)	O19—S20—C21	103.8 (3)
C9—S8—C10	98.7 (3)	C22—S20—C21	98.7 (3)
S8—C9—H9A	109.5	S20—C21—H21A	109.5
S8—C9—H9B	109.5	S20—C21—H21B	109.5
H9A—C9—H9B	109.5	H21A—C21—H21B	109.5
S8—C9—H9C	109.5	S20—C21—H21C	109.5
H9A—C9—H9C	109.5	H21A—C21—H21C	109.5
H9B—C9—H9C	109.5	H21B—C21—H21C	109.5
S8—C10—H10A	109.5	S20—C22—H22A	109.5
S8—C10—H10B	109.5	S20—C22—H22B	109.5
H10A—C10—H10B	109.5	H22A—C22—H22B	109.5
S8—C10—H10C	109.5	S20—C22—H22C	109.5
H10A—C10—H10C	109.5	H22A—C22—H22C	109.5
H10B—C10—H10C	109.5	H22B—C22—H22C	109.5
S12—O11—Cr1	123.0 (2)

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)