The space group of tris­(di­methyl­di­thio­phosphato)­ruthenium(III)

The space group of tris­(di­methyl­di­thio­phosphato)­ruth­en­ium(III), [Ru(C₂H6O₂PS₂)₃], originally reported as Cc, is revised to C2/c.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](O-C) = 0.004 Å
• R factor = 0.023
• wR factor = 0.065
• Data-to-parameter ratio = 17.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



CRYSC_01  Alert C The word below has not been recognised as a standard
          identifier.
          Block

CRYSC_01  Alert C No recognised colour has been given for crystal colour.

General Notes



ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      1.301
          Tmax scaled      0.721 Tmin scaled      0.617


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

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S1. Comment

The crystal structure of tris(dimethyldithiophosphato)ruthenium(III), (I), was originally described in the Cc space group (Jain et al., 2000). A check for additional symmetry by using the program PLATON (Spek, 1990) indicated that the correct space group for this structure is C2/c. When the structure is refined in C2/c, the ruthenium atom and one of the P atom, P2, lie on a twofold axis.

Computing details

Data collection: ARGUS-MACH3 (Nonius, 1997); cell refinement: ARGUS-MACH3; data reduction: XCAD4 (Harms, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures

Fig. 1. ORTEPII (Johnson, 1976) plot of the title compound with ellipsoids at the 50% probability level.

Tris(dimethyldithiophosphato)ruthenium(III)

Crystal data

[Ru(C2H6O2PS2)3]	F(000) = 1148
Mr = 572.54	Dx = 1.868 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 14.1212 (6) Å	Cell parameters from 25 reflections
b = 11.1919 (8) Å	θ = 10.3–17.1°
c = 12.9788 (7) Å	µ = 1.64 mm^−1
β = 97.121 (4)°	T = 298 K
V = 2035.4 (2) Å^3	Red, block
Z = 4	0.30 × 0.25 × 0.20 mm

Data collection

Nonius MACH3 four-circle diffractometer	1700 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.001
Graphite monochromator	θmax = 25.0°, θmin = 2.3°
ω scans	h = −16→5
Absorption correction: empirical via ψ scan (North et al., 1968)	k = −13→1
Tmin = 0.474, Tmax = 0.554	l = −15→15
3583 measured reflections	3 standard reflections every 60 min
1796 independent reflections	intensity decay: 1%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.065	H-atom parameters constrained
S = 1.17	w = 1/[σ^2(Fo^2) + (0.0356P)^2 + 2.6319P] where P = (Fo^2 + 2Fc^2)/3
1796 reflections	(Δ/σ)max < 0.001
101 parameters	Δρmax = 0.31 e Å^−3
0 restraints	Δρmin = −0.72 e Å^−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.

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

	x	y	z	Uiso*/Ueq
Ru1	1.0000	0.33918 (2)	0.2500	0.02875 (11)
S1	0.88251 (5)	0.48400 (6)	0.29564 (5)	0.04069 (18)
S2	0.90740 (5)	0.35912 (6)	0.08177 (5)	0.03952 (18)
S3	0.91187 (5)	0.17707 (6)	0.31317 (6)	0.03933 (17)
P1	0.82184 (5)	0.46879 (6)	0.14903 (5)	0.03589 (17)
P2	1.0000	0.06662 (8)	0.2500	0.0371 (2)
O1	0.71434 (13)	0.42760 (19)	0.13718 (16)	0.0480 (5)
O2	0.80274 (15)	0.59144 (18)	0.09043 (16)	0.0500 (5)
O3	0.94879 (15)	−0.02801 (17)	0.17196 (15)	0.0501 (5)
C1	0.6878 (2)	0.3112 (3)	0.1728 (3)	0.0594 (8)
H1A	0.6197	0.3022	0.1601	0.089*
H1B	0.7082	0.3039	0.2458	0.089*
H1C	0.7177	0.2502	0.1360	0.089*
C2	0.8815 (3)	0.6663 (3)	0.0716 (3)	0.0642 (10)
H2A	0.8577	0.7366	0.0346	0.096*
H2B	0.9226	0.6233	0.0311	0.096*
H2C	0.9167	0.6891	0.1367	0.096*
C3	0.8843 (3)	0.0123 (3)	0.0831 (3)	0.0639 (9)
H3A	0.8606	−0.0554	0.0424	0.096*
H3B	0.9178	0.0645	0.0414	0.096*
H3C	0.8319	0.0546	0.1066	0.096*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ru1	0.03156 (17)	0.02694 (17)	0.02841 (17)	0.000	0.00629 (11)	0.000
S1	0.0448 (4)	0.0417 (4)	0.0361 (3)	0.0089 (3)	0.0072 (3)	−0.0068 (3)
S2	0.0440 (4)	0.0433 (4)	0.0306 (3)	0.0094 (3)	0.0021 (3)	−0.0046 (3)
S3	0.0409 (4)	0.0336 (3)	0.0451 (4)	−0.0052 (3)	0.0122 (3)	0.0024 (3)
P1	0.0356 (4)	0.0333 (4)	0.0388 (4)	0.0056 (3)	0.0047 (3)	0.0019 (3)
P2	0.0446 (5)	0.0266 (5)	0.0385 (5)	0.000	−0.0012 (4)	0.000
O1	0.0355 (10)	0.0462 (11)	0.0614 (13)	0.0017 (9)	0.0017 (9)	0.0045 (10)
O2	0.0525 (12)	0.0405 (11)	0.0573 (12)	0.0099 (9)	0.0083 (10)	0.0122 (9)
O3	0.0640 (13)	0.0313 (10)	0.0501 (12)	−0.0023 (9)	−0.0131 (10)	−0.0050 (8)
C1	0.0497 (19)	0.0527 (19)	0.076 (2)	−0.0072 (15)	0.0080 (17)	0.0035 (17)
C2	0.080 (3)	0.0450 (19)	0.071 (2)	−0.0013 (16)	0.026 (2)	0.0125 (16)
C3	0.077 (2)	0.0508 (19)	0.0560 (19)	−0.0002 (17)	−0.0232 (17)	−0.0071 (16)

Geometric parameters (Å, º)

Ru1—S1	2.4442 (7)	P2—S3^i	2.0004 (9)
Ru1—S1^i	2.4442 (7)	O1—C1	1.447 (4)
Ru1—S2	2.4123 (7)	O2—C2	1.437 (4)
Ru1—S2^i	2.4123 (7)	O3—C3	1.450 (4)
Ru1—S3	2.4012 (7)	C1—H1A	0.96
Ru1—S3^i	2.4012 (7)	C1—H1B	0.96
S1—P1	1.9948 (10)	C1—H1C	0.96
S2—P1	1.9974 (9)	C2—H2A	0.96
S3—P2	2.0004 (9)	C2—H2B	0.96
P1—O1	1.576 (2)	C2—H2C	0.96
P1—O2	1.576 (2)	C3—H3A	0.96
P2—O3	1.5777 (19)	C3—H3B	0.96
P2—O3^i	1.5777 (19)	C3—H3C	0.96
S1—Ru1—S1^i	96.92 (4)	O3^i—P2—S3^i	114.77 (8)
S1—Ru1—S2	81.37 (2)	O3—P2—S3	114.77 (8)
S1—Ru1—S2^i	91.57 (2)	O3^i—P2—S3	114.25 (8)
S1—Ru1—S3	91.27 (3)	S3^i—P2—S3	103.68 (6)
S1—Ru1—S3^i	168.50 (3)	C1—O1—P1	121.14 (19)
S1^i—Ru1—S2	91.57 (2)	C2—O2—P1	120.0 (2)
S1^i—Ru1—S2^i	81.37 (2)	C3—O3—P2	119.62 (19)
S1^i—Ru1—S3	168.50 (3)	O1—C1—H1A	109.5
S1^i—Ru1—S3^i	91.27 (3)	O1—C1—H1B	109.5
S2—Ru1—S2^i	169.38 (4)	H1A—C1—H1B	109.5
S2—Ru1—S3	97.65 (3)	O1—C1—H1C	109.5
S2—Ru1—S3^i	90.38 (2)	H1A—C1—H1C	109.5
S2^i—Ru1—S3	90.38 (2)	H1B—C1—H1C	109.5
S2^i—Ru1—S3^i	97.65 (3)	O2—C2—H2A	109.5
S3^i—Ru1—S3	81.84 (3)	O2—C2—H2B	109.5
P1—S1—Ru1	86.35 (3)	H2A—C2—H2B	109.5
P1—S2—Ru1	87.17 (3)	O2—C2—H2C	109.5
P2—S3—Ru1	87.24 (3)	H2A—C2—H2C	109.5
O1—P1—O2	95.88 (11)	H2B—C2—H2C	109.5
O1—P1—S1	114.38 (9)	O3—C3—H3A	109.5
O2—P1—S1	114.43 (9)	O3—C3—H3B	109.5
O1—P1—S2	113.90 (9)	H3A—C3—H3B	109.5
O2—P1—S2	113.63 (9)	O3—C3—H3C	109.5
S1—P1—S2	104.94 (4)	H3A—C3—H3C	109.5
O3—P2—O3^i	95.66 (15)	H3B—C3—H3C	109.5
O3—P2—S3^i	114.25 (8)
S3^i—Ru1—S1—P1	−41.82 (13)	Ru1—S1—P1—S2	−3.42 (4)
S3—Ru1—S1—P1	−94.78 (3)	Ru1—S2—P1—O1	−122.37 (9)
S2—Ru1—S1—P1	2.77 (3)	Ru1—S2—P1—O2	129.19 (9)
S2^i—Ru1—S1—P1	174.81 (3)	Ru1—S2—P1—S1	3.47 (4)
S1^i—Ru1—S1—P1	93.31 (3)	Ru1—S3—P2—O3	−125.29 (9)
S3^i—Ru1—S2—P1	169.19 (3)	Ru1—S3—P2—O3^i	125.63 (9)
S3—Ru1—S2—P1	87.37 (3)	O2—P1—O1—C1	175.9 (2)
S1^i—Ru1—S2—P1	−99.53 (3)	S1—P1—O1—C1	−63.9 (2)
S1—Ru1—S2—P1	−2.76 (3)	S2—P1—O1—C1	56.8 (3)
S2—Ru1—S3—P2	89.28 (3)	O1—P1—O2—C2	−175.7 (2)
S2^i—Ru1—S3—P2	−97.68 (3)	S1—P1—O2—C2	64.1 (3)
S1^i—Ru1—S3—P2	−53.73 (13)	S2—P1—O2—C2	−56.4 (3)
S1—Ru1—S3—P2	170.74 (3)	O3^i—P2—O3—C3	176.6 (3)
Ru1—S1—P1—O1	122.12 (9)	S3^i—P2—O3—C3	−63.0 (3)
Ru1—S1—P1—O2	−128.65 (9)	S3—P2—O3—C3	56.6 (3)

Symmetry code: (i) −x+2, y, −z+1/2.