Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801020931/ci6082sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801020931/ci6082Isup2.hkl |
CCDC reference: 180517
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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.
Fig. 1. ORTEPII (Johnson, 1976) plot of the title compound with ellipsoids at the 50% probability level. |
[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) Å3 | Red, block |
Z = 4 | 0.30 × 0.25 × 0.20 mm |
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 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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.17 | w = 1/[σ2(Fo2) + (0.0356P)2 + 2.6319P] where P = (Fo2 + 2Fc2)/3 |
1796 reflections | (Δ/σ)max < 0.001 |
101 parameters | Δρmax = 0.31 e Å−3 |
0 restraints | Δρmin = −0.72 e Å−3 |
[Ru(C2H6O2PS2)3] | V = 2035.4 (2) Å3 |
Mr = 572.54 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 14.1212 (6) Å | µ = 1.64 mm−1 |
b = 11.1919 (8) Å | T = 298 K |
c = 12.9788 (7) Å | 0.30 × 0.25 × 0.20 mm |
β = 97.121 (4)° |
Nonius MACH3 four-circle diffractometer | 1700 reflections with I > 2σ(I) |
Absorption correction: empirical via ψ scan (North et al., 1968) | Rint = 0.001 |
Tmin = 0.474, Tmax = 0.554 | 3 standard reflections every 60 min |
3583 measured reflections | intensity decay: 1% |
1796 independent reflections |
R[F2 > 2σ(F2)] = 0.023 | 0 restraints |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.17 | Δρmax = 0.31 e Å−3 |
1796 reflections | Δρmin = −0.72 e Å−3 |
101 parameters |
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 | ||
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* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
Ru1—S1 | 2.4442 (7) | P2—S3i | 2.0004 (9) |
Ru1—S1i | 2.4442 (7) | O1—C1 | 1.447 (4) |
Ru1—S2 | 2.4123 (7) | O2—C2 | 1.437 (4) |
Ru1—S2i | 2.4123 (7) | O3—C3 | 1.450 (4) |
Ru1—S3 | 2.4012 (7) | C1—H1A | 0.96 |
Ru1—S3i | 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—O3i | 1.5777 (19) | C3—H3C | 0.96 |
S1—Ru1—S1i | 96.92 (4) | O3i—P2—S3i | 114.77 (8) |
S1—Ru1—S2 | 81.37 (2) | O3—P2—S3 | 114.77 (8) |
S1—Ru1—S2i | 91.57 (2) | O3i—P2—S3 | 114.25 (8) |
S1—Ru1—S3 | 91.27 (3) | S3i—P2—S3 | 103.68 (6) |
S1—Ru1—S3i | 168.50 (3) | C1—O1—P1 | 121.14 (19) |
S1i—Ru1—S2 | 91.57 (2) | C2—O2—P1 | 120.0 (2) |
S1i—Ru1—S2i | 81.37 (2) | C3—O3—P2 | 119.62 (19) |
S1i—Ru1—S3 | 168.50 (3) | O1—C1—H1A | 109.5 |
S1i—Ru1—S3i | 91.27 (3) | O1—C1—H1B | 109.5 |
S2—Ru1—S2i | 169.38 (4) | H1A—C1—H1B | 109.5 |
S2—Ru1—S3 | 97.65 (3) | O1—C1—H1C | 109.5 |
S2—Ru1—S3i | 90.38 (2) | H1A—C1—H1C | 109.5 |
S2i—Ru1—S3 | 90.38 (2) | H1B—C1—H1C | 109.5 |
S2i—Ru1—S3i | 97.65 (3) | O2—C2—H2A | 109.5 |
S3i—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—O3i | 95.66 (15) | H3B—C3—H3C | 109.5 |
O3—P2—S3i | 114.25 (8) | ||
S3i—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) |
S2i—Ru1—S1—P1 | 174.81 (3) | Ru1—S2—P1—S1 | 3.47 (4) |
S1i—Ru1—S1—P1 | 93.31 (3) | Ru1—S3—P2—O3 | −125.29 (9) |
S3i—Ru1—S2—P1 | 169.19 (3) | Ru1—S3—P2—O3i | 125.63 (9) |
S3—Ru1—S2—P1 | 87.37 (3) | O2—P1—O1—C1 | 175.9 (2) |
S1i—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) |
S2i—Ru1—S3—P2 | −97.68 (3) | S1—P1—O2—C2 | 64.1 (3) |
S1i—Ru1—S3—P2 | −53.73 (13) | S2—P1—O2—C2 | −56.4 (3) |
S1—Ru1—S3—P2 | 170.74 (3) | O3i—P2—O3—C3 | 176.6 (3) |
Ru1—S1—P1—O1 | 122.12 (9) | S3i—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. |
Experimental details
Crystal data | |
Chemical formula | [Ru(C2H6O2PS2)3] |
Mr | 572.54 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 298 |
a, b, c (Å) | 14.1212 (6), 11.1919 (8), 12.9788 (7) |
β (°) | 97.121 (4) |
V (Å3) | 2035.4 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.64 |
Crystal size (mm) | 0.30 × 0.25 × 0.20 |
Data collection | |
Diffractometer | Nonius MACH3 four-circle diffractometer |
Absorption correction | Empirical via ψ scan (North et al., 1968) |
Tmin, Tmax | 0.474, 0.554 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3583, 1796, 1700 |
Rint | 0.001 |
(sin θ/λ)max (Å−1) | 0.594 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.023, 0.065, 1.17 |
No. of reflections | 1796 |
No. of parameters | 101 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.31, −0.72 |
Computer programs: ARGUS-MACH3 (Nonius, 1997), ARGUS-MACH3, XCAD4 (Harms, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.
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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.