fac-Aqua-dichloridotris(tetra-methyl-ene sulfoxide-κS)ruthenium(II).

The title mol-ecule, [RuCl(2)(C(4)H(8)OS)(3)(H(2)O)], is the isomer with the two chloride ligands cis and the three S-coordinated tetra-methyl-ene sulfoxide ligands facial relative to the Ru(II) center. The Ru-Cl distances are 2.4161 (7) and 2.4317 (7) Å, the Ru-O distance is 2.1540 (19) Å, and the Ru-S distances are in the range 2.2254 (8)-2.2657 (7) Å, with the shortest being that trans to the aqua ligand. The coordinated water mol-ecule forms inter-molecular hydrogen bonds with Cl and sulfoxide O atoms.

Related literature

For background literature, see: Aldinucci et al. (2007 ▶). For related structures, see: Srivastava & Fronczek (2003 ▶); Srivastava et al. (2004 ▶); Allen (2002 ▶). For hydrogen-bonding patterns, see: Etter (1990 ▶).

Experimental

Crystal data

[RuCl2(C4H8OS)3(H2O)]

M = 502.48

Monoclinic,

a = 14.302 (3) Å

b = 7.7877 (15) Å

c = 17.248 (3) Å

β = 109.917 (9)°

V = 1806.2 (6) Å3

Z = 4

Mo Kα radiation

μ = 1.52 mm−1

T = 90.0 (5) K

0.22 × 0.10 × 0.05 mm

Data collection

Nonius KappaCCD diffractometer (with an Oxford Cryosystems Cryostream cooler)

Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997 ▶) T min = 0.731, T max = 0.928

25916 measured reflections

5982 independent reflections

4610 reflections with I > 2σ(I)

R int = 0.045

Refinement

R[F 2 > 2σ(F 2)] = 0.037

wR(F 2) = 0.076

S = 1.02

5982 reflections

199 parameters

H-atom parameters constrained

Δρmax = 0.87 e Å−3

Δρmin = −1.12 e Å−3

Data collection: COLLECT (Nonius, 2000 ▶); cell refinement: SCALEPACK (Otwinowski & Minor, 1997 ▶); data reduction: DENZO (Otwinowski & Minor, 1997 ▶) and SCALEPACK; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809000439/pv2128sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809000439/pv2128Isup2.hkl

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

[RuCl2(C4H8OS)3(H2O)]	F(000) = 1024
Mr = 502.48	Dx = 1.848 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 6027 reflections
a = 14.302 (3) Å	θ = 2.5–31.5°
b = 7.7877 (15) Å	µ = 1.52 mm−1
c = 17.248 (3) Å	T = 90 K
β = 109.917 (9)°	Needle, colorless
V = 1806.2 (6) Å3	0.22 × 0.10 × 0.05 mm
Z = 4

Nonius KappaCCD diffractometer (with an Oxford Cryosystems Cryostream cooler)	5982 independent reflections
Radiation source: fine-focus sealed tube	4610 reflections with I > 2σ(I)
graphite	Rint = 0.045
ω and φ scans	θmax = 31.5°, θmin = 2.9°
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997)	h = −20→21
Tmin = 0.731, Tmax = 0.928	k = −11→11
25916 measured reflections	l = −25→25

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076	H-atom parameters constrained
S = 1.02	w = 1/[σ2(Fo2) + (0.0256P)2 + 2.7566P] where P = (Fo2 + 2Fc2)/3
5982 reflections	(Δ/σ)max = 0.002
199 parameters	Δρmax = 0.87 e Å−3
0 restraints	Δρmin = −1.12 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.

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.

	x	y	z	Uiso*/Ueq
Ru1	0.589322 (15)	0.17421 (3)	0.298795 (12)	0.00590 (5)
Cl1	0.63294 (5)	−0.00620 (8)	0.41988 (4)	0.01063 (12)
Cl2	0.59746 (5)	−0.07251 (8)	0.21491 (4)	0.00956 (12)
S1	0.55748 (5)	0.33080 (8)	0.18270 (4)	0.00718 (12)
S2	0.59211 (5)	0.41572 (8)	0.37280 (4)	0.00785 (12)
S3	0.42982 (5)	0.11754 (8)	0.27675 (4)	0.00811 (12)
O1	0.64973 (14)	0.3915 (2)	0.16851 (11)	0.0112 (4)
O2	0.49707 (14)	0.5110 (2)	0.35546 (12)	0.0125 (4)
O3	0.35604 (14)	0.1775 (3)	0.19762 (12)	0.0133 (4)
O4	0.74739 (13)	0.1973 (2)	0.32611 (11)	0.0094 (4)
H41	0.7697	0.1034	0.3254	0.014*
H42	0.7735	0.2581	0.3021	0.014*
C1	0.4799 (2)	0.2324 (3)	0.08568 (16)	0.0117 (5)
H1A	0.5196	0.2111	0.0495	0.014*
H1B	0.4527	0.1216	0.0965	0.014*
C2	0.3955 (2)	0.3583 (4)	0.04466 (17)	0.0142 (6)
H2A	0.3353	0.3260	0.0573	0.017*
H2B	0.3790	0.3561	−0.0159	0.017*
C3	0.4301 (2)	0.5380 (4)	0.07805 (16)	0.0129 (5)
H3A	0.4794	0.5831	0.0545	0.016*
H3B	0.3731	0.6183	0.0645	0.016*
C4	0.4770 (2)	0.5151 (3)	0.17114 (16)	0.0109 (5)
H4A	0.4256	0.4934	0.1964	0.013*
H4B	0.5157	0.6181	0.1970	0.013*
C5	0.6859 (2)	0.5663 (3)	0.36345 (16)	0.0108 (5)
H5A	0.7141	0.5249	0.3218	0.013*
H5B	0.6559	0.6808	0.3463	0.013*
C6	0.7667 (2)	0.5771 (4)	0.44766 (17)	0.0152 (6)
H6A	0.8007	0.6897	0.4548	0.018*
H6B	0.8167	0.4854	0.4538	0.018*
C7	0.7149 (2)	0.5548 (4)	0.51139 (17)	0.0145 (6)
H7A	0.7644	0.5366	0.5671	0.017*
H7B	0.6748	0.6576	0.5128	0.017*
C8	0.6484 (2)	0.3978 (3)	0.48391 (16)	0.0110 (5)
H8A	0.5967	0.3964	0.5101	0.013*
H8B	0.6881	0.2911	0.4990	0.013*
C9	0.3821 (2)	0.1780 (4)	0.35774 (17)	0.0132 (5)
H9A	0.4359	0.1791	0.4121	0.016*
H9B	0.3507	0.2928	0.3471	0.016*
C10	0.3059 (2)	0.0401 (4)	0.35450 (18)	0.0148 (6)
H10A	0.2462	0.0530	0.3046	0.018*
H10B	0.2856	0.0455	0.4039	0.018*
C11	0.3595 (2)	−0.1292 (4)	0.35214 (18)	0.0149 (6)
H11A	0.4113	−0.1516	0.4063	0.018*
H11B	0.3117	−0.2258	0.3390	0.018*
C12	0.4068 (2)	−0.1113 (3)	0.28551 (18)	0.0119 (5)
H12A	0.3614	−0.1562	0.2323	0.014*
H12B	0.4699	−0.1764	0.3010	0.014*

	U11	U22	U33	U12	U13	U23
Ru1	0.00693 (9)	0.00402 (9)	0.00659 (9)	0.00017 (7)	0.00210 (7)	0.00032 (7)
Cl1	0.0146 (3)	0.0069 (3)	0.0095 (3)	0.0008 (2)	0.0030 (2)	0.0025 (2)
Cl2	0.0109 (3)	0.0061 (3)	0.0119 (3)	0.0004 (2)	0.0042 (2)	−0.0016 (2)
S1	0.0081 (3)	0.0058 (3)	0.0071 (3)	−0.0008 (2)	0.0020 (2)	0.0000 (2)
S2	0.0099 (3)	0.0056 (3)	0.0077 (3)	0.0003 (2)	0.0026 (2)	0.0005 (2)
S3	0.0086 (3)	0.0069 (3)	0.0087 (3)	0.0000 (2)	0.0028 (2)	0.0008 (2)
O1	0.0116 (9)	0.0101 (9)	0.0133 (9)	−0.0033 (7)	0.0060 (8)	0.0002 (7)
O2	0.0117 (9)	0.0097 (9)	0.0171 (10)	0.0036 (7)	0.0060 (8)	0.0003 (8)
O3	0.0093 (9)	0.0158 (9)	0.0127 (9)	−0.0009 (8)	0.0009 (7)	0.0055 (8)
O4	0.0108 (9)	0.0049 (8)	0.0132 (9)	−0.0012 (7)	0.0049 (7)	−0.0001 (7)
C1	0.0127 (13)	0.0110 (12)	0.0102 (12)	−0.0029 (10)	0.0024 (10)	−0.0015 (10)
C2	0.0131 (13)	0.0156 (14)	0.0110 (13)	−0.0005 (10)	0.0005 (10)	0.0025 (10)
C3	0.0146 (13)	0.0125 (12)	0.0113 (13)	0.0028 (11)	0.0038 (10)	0.0071 (10)
C4	0.0115 (12)	0.0086 (12)	0.0121 (13)	0.0040 (10)	0.0034 (10)	0.0024 (10)
C5	0.0143 (13)	0.0061 (11)	0.0123 (12)	−0.0014 (10)	0.0052 (10)	0.0009 (10)
C6	0.0160 (14)	0.0133 (13)	0.0135 (13)	−0.0039 (11)	0.0014 (11)	−0.0030 (11)
C7	0.0197 (15)	0.0130 (13)	0.0083 (12)	−0.0027 (11)	0.0014 (11)	−0.0033 (10)
C8	0.0161 (13)	0.0092 (12)	0.0080 (12)	0.0007 (10)	0.0044 (10)	0.0006 (10)
C9	0.0135 (13)	0.0131 (12)	0.0159 (13)	−0.0003 (11)	0.0086 (11)	−0.0031 (11)
C10	0.0138 (13)	0.0178 (14)	0.0156 (14)	−0.0047 (11)	0.0087 (11)	0.0012 (11)
C11	0.0180 (14)	0.0121 (12)	0.0156 (14)	−0.0055 (11)	0.0068 (11)	0.0024 (11)
C12	0.0107 (12)	0.0063 (11)	0.0199 (14)	−0.0030 (10)	0.0067 (11)	0.0009 (10)

Ru1—O4	2.1540 (19)	C3—H3B	0.9900
Ru1—S3	2.2254 (8)	C4—H4A	0.9900
Ru1—S1	2.2546 (7)	C4—H4B	0.9900
Ru1—S2	2.2657 (7)	C5—C6	1.519 (4)
Ru1—Cl1	2.4161 (7)	C5—H5A	0.9900
Ru1—Cl2	2.4317 (7)	C5—H5B	0.9900
S1—O1	1.498 (2)	C6—C7	1.531 (4)
S1—C4	1.807 (3)	C6—H6A	0.9900
S1—C1	1.831 (3)	C6—H6B	0.9900
S2—O2	1.487 (2)	C7—C8	1.521 (4)
S2—C8	1.814 (3)	C7—H7A	0.9900
S2—C5	1.830 (3)	C7—H7B	0.9900
S3—O3	1.487 (2)	C8—H8A	0.9900
S3—C9	1.813 (3)	C8—H8B	0.9900
S3—C12	1.828 (3)	C9—C10	1.517 (4)
O4—H41	0.8000	C9—H9A	0.9900
O4—H42	0.8000	C9—H9B	0.9900
C1—C2	1.529 (4)	C10—C11	1.532 (4)
C1—H1A	0.9900	C10—H10A	0.9900
C1—H1B	0.9900	C10—H10B	0.9900
C2—C3	1.530 (4)	C11—C12	1.525 (4)
C2—H2A	0.9900	C11—H11A	0.9900
C2—H2B	0.9900	C11—H11B	0.9900
C3—C4	1.525 (4)	C12—H12A	0.9900
C3—H3A	0.9900	C12—H12B	0.9900
O4—Ru1—S3	172.92 (5)	C3—C4—S1	104.15 (18)
O4—Ru1—S1	91.63 (5)	C3—C4—H4A	110.9
S3—Ru1—S1	94.04 (3)	S1—C4—H4A	110.9
O4—Ru1—S2	89.52 (5)	C3—C4—H4B	110.9
S3—Ru1—S2	94.66 (3)	S1—C4—H4B	110.9
S1—Ru1—S2	90.62 (3)	H4A—C4—H4B	108.9
O4—Ru1—Cl1	85.23 (5)	C6—C5—S2	107.04 (18)
S3—Ru1—Cl1	88.86 (3)	C6—C5—H5A	110.3
S1—Ru1—Cl1	175.45 (2)	S2—C5—H5A	110.3
S2—Ru1—Cl1	92.63 (3)	C6—C5—H5B	110.3
O4—Ru1—Cl2	86.37 (5)	S2—C5—H5B	110.3
S3—Ru1—Cl2	89.75 (2)	H5A—C5—H5B	108.6
S1—Ru1—Cl2	86.28 (3)	C5—C6—C7	106.5 (2)
S2—Ru1—Cl2	174.78 (2)	C5—C6—H6A	110.4
Cl1—Ru1—Cl2	90.24 (3)	C7—C6—H6A	110.4
O1—S1—C4	107.13 (12)	C5—C6—H6B	110.4
O1—S1—C1	106.01 (12)	C7—C6—H6B	110.4
C4—S1—C1	93.82 (12)	H6A—C6—H6B	108.6
O1—S1—Ru1	113.14 (8)	C8—C7—C6	105.8 (2)
C4—S1—Ru1	117.12 (9)	C8—C7—H7A	110.6
C1—S1—Ru1	117.49 (9)	C6—C7—H7A	110.6
O2—S2—C8	107.31 (12)	C8—C7—H7B	110.6
O2—S2—C5	108.06 (12)	C6—C7—H7B	110.6
C8—S2—C5	93.85 (12)	H7A—C7—H7B	108.7
O2—S2—Ru1	117.48 (8)	C7—C8—S2	105.84 (18)
C8—S2—Ru1	116.59 (9)	C7—C8—H8A	110.6
C5—S2—Ru1	110.80 (9)	S2—C8—H8A	110.6
O3—S3—C9	106.85 (13)	C7—C8—H8B	110.6
O3—S3—C12	106.88 (12)	S2—C8—H8B	110.6
C9—S3—C12	93.64 (13)	H8A—C8—H8B	108.7
O3—S3—Ru1	117.39 (8)	C10—C9—S3	104.01 (19)
C9—S3—Ru1	116.73 (10)	C10—C9—H9A	111.0
C12—S3—Ru1	112.49 (9)	S3—C9—H9A	111.0
Ru1—O4—H41	108.3	C10—C9—H9B	111.0
Ru1—O4—H42	125.1	S3—C9—H9B	111.0
H41—O4—H42	105.9	H9A—C9—H9B	109.0
C2—C1—S1	106.96 (18)	C9—C10—C11	104.5 (2)
C2—C1—H1A	110.3	C9—C10—H10A	110.9
S1—C1—H1A	110.3	C11—C10—H10A	110.9
C2—C1—H1B	110.3	C9—C10—H10B	110.9
S1—C1—H1B	110.3	C11—C10—H10B	110.9
H1A—C1—H1B	108.6	H10A—C10—H10B	108.9
C1—C2—C3	108.0 (2)	C12—C11—C10	107.2 (2)
C1—C2—H2A	110.1	C12—C11—H11A	110.3
C3—C2—H2A	110.1	C10—C11—H11A	110.3
C1—C2—H2B	110.1	C12—C11—H11B	110.3
C3—C2—H2B	110.1	C10—C11—H11B	110.3
H2A—C2—H2B	108.4	H11A—C11—H11B	108.5
C4—C3—C2	105.0 (2)	C11—C12—S3	106.86 (19)
C4—C3—H3A	110.7	C11—C12—H12A	110.4
C2—C3—H3A	110.7	S3—C12—H12A	110.4
C4—C3—H3B	110.7	C11—C12—H12B	110.4
C2—C3—H3B	110.7	S3—C12—H12B	110.4
H3A—C3—H3B	108.8	H12A—C12—H12B	108.6
O4—Ru1—S1—O1	−0.88 (10)	S1—Ru1—S3—C12	129.51 (10)
S3—Ru1—S1—O1	−176.63 (9)	S2—Ru1—S3—C12	−139.54 (10)
S2—Ru1—S1—O1	88.66 (9)	Cl1—Ru1—S3—C12	−46.99 (10)
Cl2—Ru1—S1—O1	−87.14 (9)	Cl2—Ru1—S3—C12	43.26 (10)
O4—Ru1—S1—C4	−126.24 (11)	O1—S1—C1—C2	−105.28 (19)
S3—Ru1—S1—C4	58.01 (11)	C4—S1—C1—C2	3.8 (2)
S2—Ru1—S1—C4	−36.70 (11)	Ru1—S1—C1—C2	127.11 (16)
Cl2—Ru1—S1—C4	147.50 (11)	S1—C1—C2—C3	23.5 (3)
O4—Ru1—S1—C1	123.22 (11)	C1—C2—C3—C4	−46.0 (3)
S3—Ru1—S1—C1	−52.53 (11)	C2—C3—C4—S1	47.2 (2)
S2—Ru1—S1—C1	−147.24 (10)	O1—S1—C4—C3	78.5 (2)
Cl2—Ru1—S1—C1	36.96 (10)	C1—S1—C4—C3	−29.5 (2)
O4—Ru1—S2—O2	158.55 (10)	Ru1—S1—C4—C3	−153.17 (15)
S3—Ru1—S2—O2	−27.18 (9)	O2—S2—C5—C6	117.47 (19)
S1—Ru1—S2—O2	66.92 (9)	C8—S2—C5—C6	7.9 (2)
Cl1—Ru1—S2—O2	−116.25 (9)	Ru1—S2—C5—C6	−112.51 (17)
O4—Ru1—S2—C8	−72.00 (12)	S2—C5—C6—C7	−33.1 (3)
S3—Ru1—S2—C8	102.28 (11)	C5—C6—C7—C8	48.6 (3)
S1—Ru1—S2—C8	−163.62 (11)	C6—C7—C8—S2	−41.6 (3)
Cl1—Ru1—S2—C8	13.20 (11)	O2—S2—C8—C7	−90.7 (2)
O4—Ru1—S2—C5	33.70 (11)	C5—S2—C8—C7	19.5 (2)
S3—Ru1—S2—C5	−152.03 (9)	Ru1—S2—C8—C7	135.11 (16)
S1—Ru1—S2—C5	−57.93 (10)	O3—S3—C9—C10	80.2 (2)
Cl1—Ru1—S2—C5	118.90 (10)	C12—S3—C9—C10	−28.6 (2)
S1—Ru1—S3—O3	4.88 (10)	Ru1—S3—C9—C10	−146.10 (16)
S2—Ru1—S3—O3	95.83 (10)	S3—C9—C10—C11	48.1 (2)
Cl1—Ru1—S3—O3	−171.62 (10)	C9—C10—C11—C12	−48.9 (3)
Cl2—Ru1—S3—O3	−81.37 (10)	C10—C11—C12—S3	26.8 (3)
S1—Ru1—S3—C9	−123.92 (11)	O3—S3—C12—C11	−107.7 (2)
S2—Ru1—S3—C9	−32.96 (11)	C9—S3—C12—C11	1.2 (2)
Cl1—Ru1—S3—C9	59.59 (11)	Ru1—S3—C12—C11	122.10 (17)
Cl2—Ru1—S3—C9	149.83 (11)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H41···O1i	0.80	1.99	2.785 (3)	169
O4—H42···Cl2ii	0.80	2.37	3.116 (2)	156

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H41⋯O1i	0.80	1.99	2.785 (3)	169
O4—H42⋯Cl2ii	0.80	2.37	3.116 (2)	156

Symmetry codes: (i) ; (ii) .