mer-Tri­chloro­tris­(di­methyl sulfide)­ruthenium(III)

The title compound, mer-[RuCl₃(C₂H₆S)₃], contains discrete mol­ecules with six-coordinate Ru atoms [Ru-Cl 2.3389 (10)-2.3562 (8) Å and Ru-S 2.3801 (8)-2.3879 (10) Å]. The structure is a polymorph of the form previously reported by Jaswal et al. (1990). [Can. J. Chem. 68, 1808-1817].

Key indicators

• Single-crystal X-ray study
• T = 120 K
• Mean [sigma](S-C) = 0.003 Å
• R factor = 0.029
• wR factor = 0.064
• Data-to-parameter ratio = 27.2

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.89

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.49
           From the CIF: _reflns_number_total               3263
           Count of symmetry unique reflns         1772
           Completeness (_total/calc)            184.14%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1491
           Fraction of Friedel pairs measured     0.841
           Are heavy atom types Z>Si present          yes

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   1 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997); cell refinement: COLLECT and DENZO; data reduction: COLLECT and DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976).

mer-trichlorotris(dimethyl sulfide)ruthenium(III)

Crystal data

[RuCl3(C2H6S)3]	F(000) = 788
Mr = 393.80	Dx = 1.783 Mg m^−3
Orthorhombic, Pna21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 5262 reflections
a = 16.391 (2) Å	θ = 2.9–27.5°
b = 8.540 (1) Å	µ = 2.00 mm^−1
c = 10.4825 (10) Å	T = 120 K
V = 1467.3 (3) Å^3	Block, red
Z = 4	0.18 × 0.18 × 0.10 mm

Data collection

Nonius KappaCCD area-detector diffractometer	3263 independent reflections
Radiation source: Nonius rotating anode	2912 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.058
φ and ω scans	θmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.	h = −21→21
Tmin = 0.629, Tmax = 0.818	k = −11→10
11276 measured reflections	l = −12→13

Refinement

Refinement on F^2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.029	w = 1/[σ^2(Fo^2) + (0.0171P)^2 + 0.0078P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.064	(Δ/σ)max = 0.001
S = 1.04	Δρmax = 0.79 e Å^−3
3263 reflections	Δρmin = −0.65 e Å^−3
120 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
1 restraint	Extinction coefficient: 0.0045 (3)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983), 0000 Friedel pairs
Secondary atom site location: difference Fourier map	Absolute structure parameter: −0.04 (3)

Special details

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.

The H atoms are in calculated positions with a common refined isotropic adp.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ru1	0.138500 (16)	0.74481 (2)	0.33416 (3)	0.01249 (9)
Cl1	0.25315 (6)	0.77875 (10)	0.20423 (9)	0.0224 (2)
Cl2	0.02346 (5)	0.74323 (9)	0.46717 (9)	0.0186 (2)
Cl3	0.14814 (5)	0.46959 (8)	0.33899 (11)	0.02330 (19)
S1	0.05396 (6)	0.72744 (10)	0.14917 (10)	0.0198 (2)
S2	0.23383 (6)	0.77039 (11)	0.50511 (10)	0.0205 (2)
S3	0.12723 (4)	1.02262 (8)	0.32995 (11)	0.01613 (17)
C1	−0.0287 (2)	0.5952 (4)	0.1815 (3)	0.0269 (8)
H1A	−0.0648	0.6412	0.2460	0.043 (3)*
H1B	−0.0068	0.4958	0.2133	0.043 (3)*
H1C	−0.0596	0.5765	0.1029	0.043 (3)*
C2	0.1072 (2)	0.6144 (5)	0.0318 (4)	0.0329 (10)
H2A	0.1554	0.6723	0.0029	0.043 (3)*
H2B	0.0711	0.5945	−0.0409	0.043 (3)*
H2C	0.1243	0.5145	0.0693	0.043 (3)*
C3	0.3097 (2)	0.6181 (4)	0.4915 (4)	0.0321 (10)
H3A	0.3400	0.6314	0.4117	0.043 (3)*
H3B	0.2829	0.5156	0.4918	0.043 (3)*
H3C	0.3475	0.6247	0.5638	0.043 (3)*
C4	0.1894 (2)	0.7178 (4)	0.6556 (3)	0.0284 (9)
H4A	0.1460	0.7922	0.6770	0.043 (3)*
H4B	0.2315	0.7205	0.7220	0.043 (3)*
H4C	0.1665	0.6120	0.6500	0.043 (3)*
C5	0.1292 (2)	1.0949 (4)	0.4900 (3)	0.0276 (9)
H5A	0.1824	1.0721	0.5284	0.043 (3)*
H5B	0.0862	1.0438	0.5398	0.043 (3)*
H5C	0.1201	1.2083	0.4894	0.043 (3)*
C6	0.0248 (2)	1.0823 (4)	0.2899 (4)	0.0275 (8)
H6A	0.0125	1.0513	0.2020	0.043 (3)*
H6B	0.0201	1.1962	0.2980	0.043 (3)*
H6C	−0.0139	1.0317	0.3481	0.043 (3)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ru1	0.01246 (14)	0.01152 (15)	0.01350 (14)	−0.00008 (8)	0.00046 (14)	0.00110 (12)
Cl1	0.0191 (5)	0.0259 (5)	0.0222 (5)	0.0018 (4)	0.0088 (4)	0.0028 (5)
Cl2	0.0157 (5)	0.0206 (5)	0.0195 (5)	−0.0018 (3)	0.0050 (4)	0.0028 (3)
Cl3	0.0264 (4)	0.0114 (4)	0.0321 (5)	0.0013 (3)	−0.0004 (5)	0.0020 (5)
S1	0.0233 (5)	0.0179 (4)	0.0181 (4)	−0.0002 (3)	−0.0061 (4)	−0.0028 (4)
S2	0.0180 (5)	0.0218 (5)	0.0216 (5)	−0.0031 (4)	−0.0060 (4)	0.0060 (4)
S3	0.0215 (4)	0.0115 (4)	0.0154 (4)	−0.0005 (3)	0.0022 (5)	0.0013 (5)
C1	0.0217 (18)	0.026 (2)	0.033 (2)	−0.0032 (15)	−0.0036 (17)	−0.0058 (15)
C2	0.036 (2)	0.039 (3)	0.024 (2)	0.0018 (17)	0.0032 (17)	−0.0141 (17)
C3	0.0198 (19)	0.043 (3)	0.033 (2)	0.0051 (17)	−0.0004 (17)	0.0110 (17)
C4	0.028 (2)	0.037 (2)	0.0200 (18)	0.0023 (17)	−0.0049 (17)	0.0044 (17)
C5	0.043 (2)	0.018 (2)	0.022 (2)	−0.0004 (17)	−0.0059 (17)	−0.0062 (14)
C6	0.029 (2)	0.0217 (18)	0.032 (2)	0.0082 (15)	−0.0097 (16)	−0.0001 (15)

Geometric parameters (Å, º)

Ru1—Cl1	2.3389 (10)	C2—H2A	0.9800
Ru1—Cl2	2.3451 (9)	C2—H2B	0.9800
Ru1—Cl3	2.3562 (8)	C2—H2C	0.9800
Ru1—S1	2.3879 (10)	C3—H3A	0.9800
Ru1—S2	2.3876 (11)	C3—H3B	0.9800
Ru1—S3	2.3801 (8)	C3—H3C	0.9800
S1—C1	1.796 (3)	C4—H4A	0.9800
S1—C2	1.791 (4)	C4—H4B	0.9800
S2—C4	1.795 (4)	C4—H4C	0.9800
S2—C3	1.806 (4)	C5—H5A	0.9800
S3—C5	1.787 (4)	C5—H5B	0.9800
S3—C6	1.805 (3)	C5—H5C	0.9800
C1—H1A	0.9800	C6—H6A	0.9800
C1—H1B	0.9800	C6—H6B	0.9800
C1—H1C	0.9800	C6—H6C	0.9800
Cl1—Ru1—Cl2	173.19 (3)	S1—C2—H2A	109.5
Cl1—Ru1—Cl3	94.72 (3)	S1—C2—H2B	109.5
Cl2—Ru1—Cl3	92.03 (3)	H2A—C2—H2B	109.5
Cl1—Ru1—S3	85.87 (3)	S1—C2—H2C	109.5
Cl2—Ru1—S3	87.39 (3)	H2A—C2—H2C	109.5
Cl3—Ru1—S3	179.37 (3)	H2B—C2—H2C	109.5
Cl1—Ru1—S2	84.26 (4)	S2—C3—H3A	109.5
Cl2—Ru1—S2	94.62 (4)	S2—C3—H3B	109.5
Cl3—Ru1—S2	91.79 (3)	H3A—C3—H3B	109.5
S3—Ru1—S2	88.48 (3)	S2—C3—H3C	109.5
Cl1—Ru1—S1	90.06 (4)	H3A—C3—H3C	109.5
Cl2—Ru1—S1	90.91 (4)	H3B—C3—H3C	109.5
Cl3—Ru1—S1	89.68 (3)	S2—C4—H4A	109.5
S3—Ru1—S1	90.10 (3)	S2—C4—H4B	109.5
S2—Ru1—S1	174.22 (4)	H4A—C4—H4B	109.5
C2—S1—C1	99.11 (17)	S2—C4—H4C	109.5
C2—S1—Ru1	107.96 (13)	H4A—C4—H4C	109.5
C1—S1—Ru1	108.87 (12)	H4B—C4—H4C	109.5
C4—S2—C3	99.71 (17)	S3—C5—H5A	109.5
C4—S2—Ru1	111.80 (13)	S3—C5—H5B	109.5
C3—S2—Ru1	109.02 (13)	H5A—C5—H5B	109.5
C5—S3—C6	97.90 (17)	S3—C5—H5C	109.5
C5—S3—Ru1	108.98 (12)	H5A—C5—H5C	109.5
C6—S3—Ru1	110.97 (11)	H5B—C5—H5C	109.5
S1—C1—H1A	109.5	S3—C6—H6A	109.5
S1—C1—H1B	109.5	S3—C6—H6B	109.5
H1A—C1—H1B	109.5	H6A—C6—H6B	109.5
S1—C1—H1C	109.5	S3—C6—H6C	109.5
H1A—C1—H1C	109.5	H6A—C6—H6C	109.5
H1B—C1—H1C	109.5	H6B—C6—H6C	109.5