fac-Aqua­dichloridotris(tetra­methyl­ene sulfoxide-κS)ruthenium(II)

Srivastava, R.S.; Gonzales, C.F.; Fronczek, F.R.

doi:10.1107/S1600536809000439

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 2| February 2009| Page m170

doi:10.1107/S1600536809000439

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fac-Aquadichloridotris(tetramethylene sulfoxide-κS)ruthenium(II)

Radhey S. Srivastava,^a Carlos F. Gonzales ^a and Frank R. Fronczek ^b ^*

^aDepartment of Chemistry, University of Louisiana at Lafayette, Lafayette, LA 70504, USA, and ^bDepartment of Chemistry, Louisiana State University, Baton Rouge, LA 70803-1804, USA
^*Correspondence e-mail: ffroncz@lsu.edu

(Received 5 December 2008; accepted 6 January 2009; online 10 January 2009)

The title molecule, [RuCl₂(C₄H₈OS)₃(H₂O)], is the isomer with the two chloride ligands cis and the three S-coordinated tetramethylene 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 molecule forms intermolecular 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_r = 502.48
Monoclinic, P 2₁ /n
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[F² > 2σ(F²)] = 0.037
wR(F²) = 0.076
S = 1.02
5982 reflections
199 parameters
H-atom parameters constrained
Δρ_max = 0.87 e Å⁻³
Δρ_min = −1.12 e Å⁻³

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) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

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.

Supporting information

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

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

checkCIF report

Comment top

During the course of our studies on ruthenium-DMSO/TMSO complexes, mer-RuCl₃(TMSO)₃ was refluxed with methyl-p-tolylsulfide in absolute ethanol for 1 h. In view of anticancer properties of Ru-DMSO/TMSO complexes, we envision to interact mer-RuCl₃(TMSO)₃, (1) with sulfur donor ligands, because sulfur-containing ligands are able to bind the metal center strongly and prevent interactions with sulfur-containing enzymes (Aldinucci et al., 2007). In fact, these reactions are believed to be responsible for the nephrotoxicity induced by the platinum (II)-based drugs. However, the compound (2) was hydrolyzed on long standing in solution, and finally the title compound, fac-[RuCl₂(TMSO)₃(H₂O)] (3) was isolated. A plausible mechanism of the formation of (3) is shown in scheme 2.

There are three geometrical isomers of the title compound: trans,mer; cis,mer; and fac. The reported structure is found to be the latter, with chloro groups cis and TMSO groups facial, as shown in Fig. 1. More isomers are possible, considering that the TMSO ligands may be coordinated to Ru through either S or O in the same complex, (Srivastava & Fronczek, 2003; Srivastava et al., 2004); however, all are S-coordinated here. Relevant bond distances are given in the supplementary Tables. Most noteworthy is that the Ru—S3 distance, trans to water, is 0.03–0.04 Å shorter than the two Ru—S distances trans to Cl. While a search of the Cambridge Structural Database (version 5.29, Jan. 2008; Allen, 2002) for Ru complexes with S-bonded TMSO trans to water produced no hits, eleven examples of such DMSO complexes were found, refcodes AQAXIZ, AQAXOF, AQAXUL, BINBAC, CECSUZ, QUDRUC, TEXMOZ, TEXNEQ, TEXNIU, WOHNEM, AND WOHNIQ. Those have mean Ru—O distance 2.142 Å and mean Ru—S distance 2.256 Å. Our Ru—O distance, 2.1540 (19) Å, is near the high end of that sample, and our Ru—S distance, Ru1 S3 2.2254 (8) Å, is shorter than any in that sample.

The coordinated water molecule donates an intermolecular hydrogen bond to sulfoxide O and another to Cl, on two different molecules related by unit translation in the b direction. Thus, rings of graph set (Etter, 1990) symbol R²₂(9) form chains along [010], propagated by the 2₁ axis, as shown in Fig. 2.

Related literature top

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 top

mer-RuCl₃(TMSO)₃ (0.166 g, 0.233 mmol) was refluxed with methyl-p-tolylsulfide (73 µl, 0.533 mmol) in absolute ethanol (15 ml) for 2 h, followed by cooling to room temperature. Upon standing for eight months, colorless needles of the title compound formed.

Computing details top

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor 1997); 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 (Sheldrick, 2008).

Figures top

	Fig. 1. A plot of the title compound with displacement ellipsoids drawn at the 50% level and H atoms having arbitrary radius.
	Fig. 2. A portion of a hydrogen-bonded chain in the [010] direction.
	Fig. 3. The formation of the title compound.

fac-Aquadichloridotris(tetramethylene sulfoxide-κS)ruthenium(II) top

Crystal data top

[RuCl₂(C₄H₈OS)₃(H₂O)]	F(000) = 1024
M_r = 502.48	D_x = 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

Data collection top

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 monochromator	R_int = 0.045
ω and ϕ scans	θ_max = 31.5°, θ_min = 2.9°
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997)	h = −20→21
T_min = 0.731, T_max = 0.928	k = −11→11
25916 measured reflections	l = −25→25

Refinement top

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(F_o²) + (0.0256P)² + 2.7566P] where P = (F_o² + 2F_c²)/3
5982 reflections	(Δ/σ)_max = 0.002
199 parameters	Δρ_max = 0.87 e Å⁻³
0 restraints	Δρ_min = −1.12 e Å⁻³

Crystal data top

[RuCl₂(C₄H₈OS)₃(H₂O)]	V = 1806.2 (6) Å³
M_r = 502.48	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 14.302 (3) Å	µ = 1.52 mm⁻¹
b = 7.7877 (15) Å	T = 90 K
c = 17.248 (3) Å	0.22 × 0.10 × 0.05 mm
β = 109.917 (9)°

Data collection top

Nonius KappaCCD diffractometer (with an Oxford Cryosystems Cryostream cooler)	5982 independent reflections
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997)	4610 reflections with I > 2σ(I)
T_min = 0.731, T_max = 0.928	R_int = 0.045
25916 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.076	H-atom parameters constrained
S = 1.02	Δρ_max = 0.87 e Å⁻³
5982 reflections	Δρ_min = −1.12 e Å⁻³
199 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.

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

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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)

Hydrogen-bond geometry (Å, º) top

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) −x+3/2, y−1/2, −z+1/2; (ii) −x+3/2, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	[RuCl₂(C₄H₈OS)₃(H₂O)]
M_r	502.48
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	90
a, b, c (Å)	14.302 (3), 7.7877 (15), 17.248 (3)
β (°)	109.917 (9)
V (Å³)	1806.2 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.52
Crystal size (mm)	0.22 × 0.10 × 0.05

Data collection
Diffractometer	Nonius KappaCCD diffractometer (with an Oxford Cryosystems Cryostream cooler)
Absorption correction	Multi-scan (SCALEPACK; Otwinowski & Minor, 1997)
T_min, T_max	0.731, 0.928
No. of measured, independent and observed [I > 2σ(I)] reflections	25916, 5982, 4610
R_int	0.045
(sin θ/λ)_max (Å⁻¹)	0.735

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.076, 1.02
No. of reflections	5982
No. of parameters	199
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.87, −1.12

Computer programs: COLLECT (Nonius, 2000), SCALEPACK (Otwinowski & Minor, 1997), DENZO and SCALEPACK (Otwinowski & Minor 1997), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O4—H41···O1ⁱ	0.80	1.99	2.785 (3)	169.1
O4—H42···Cl2ⁱⁱ	0.80	2.37	3.116 (2)	156.1

Symmetry codes: (i) −x+3/2, y−1/2, −z+1/2; (ii) −x+3/2, y+1/2, −z+1/2.

Acknowledgements

Financial support provided by the Research Corporation (Cottrell College Science Award, #CC 6234 to RSS) and the BoR, Louisiana, is greatly appreciated. The purchase of the diffractometer was made possible by grant No. LEQSF (1999–2000)-ENH-TR-13, administered by the Louisiana Board of Regents.

References

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