Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680102092X/ci6081sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680102092X/ci6081Isup2.hkl |
CCDC reference: 180518
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (O-C) = 0.005 Å
- R factor = 0.017
- wR factor = 0.043
- Data-to-parameter ratio = 17.9
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level B:
ABSTM_02 Alert B The ratio of expected to reported Tmax/Tmin(RR) is > 1.50 Tmin and Tmax reported: 0.119 0.180 Tmin and Tmax expected: 0.195 0.491 RR = 1.665 Please check that your absorption correction is appropriate.
Author response: ... The compound contains a heavy osmium atom. The absorption correction used 5 intense reflections in the theta = 4.7 to 21.2 deg. range. The absorption correction is adequate as there are no large peaks in the final difference Fourier. |
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 2.730 Tmax scaled 0.491 Tmin scaled 0.325
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
0 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. |
[Os(C2H6O2PS2)3] | F(000) = 1276 |
Mr = 661.67 | Dx = 2.151 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 14.138 (1) Å | Cell parameters from 25 reflections |
b = 11.228 (4) Å | θ = 11.4–14.2° |
c = 12.970 (1) Å | µ = 7.11 mm−1 |
β = 96.99 (1)° | T = 298 K |
V = 2043.6 (8) Å3 | Plate, violet |
Z = 4 | 0.35 × 0.20 × 0.10 mm |
Nonius MACH-3 four-circle diffractometer | 1691 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.024 |
Graphite monochromator | θmax = 25.0°, θmin = 2.3° |
ω scans | h = −16→10 |
Absorption correction: empirical (using intensity measurements) via ψ scan (North et al., 1968) | k = −13→10 |
Tmin = 0.119, Tmax = 0.180 | l = −15→15 |
3741 measured reflections | 3 standard reflections every 60 min |
1805 independent reflections | intensity decay: none |
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)] = 0.017 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.043 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0282P)2] where P Fo2 + 2Fc2)/3 |
1805 reflections | (Δ/σ)max < 0.001 |
101 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.80 e Å−3 |
[Os(C2H6O2PS2)3] | V = 2043.6 (8) Å3 |
Mr = 661.67 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 14.138 (1) Å | µ = 7.11 mm−1 |
b = 11.228 (4) Å | T = 298 K |
c = 12.970 (1) Å | 0.35 × 0.20 × 0.10 mm |
β = 96.99 (1)° |
Nonius MACH-3 four-circle diffractometer | 1691 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) via ψ scan (North et al., 1968) | Rint = 0.024 |
Tmin = 0.119, Tmax = 0.180 | 3 standard reflections every 60 min |
3741 measured reflections | intensity decay: none |
1805 independent reflections |
R[F2 > 2σ(F2)] = 0.017 | 0 restraints |
wR(F2) = 0.043 | H-atom parameters constrained |
S = 1.09 | Δρmax = 0.34 e Å−3 |
1805 reflections | Δρmin = −0.80 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 | ||
Os1 | 1.0000 | 0.340348 (14) | 0.2500 | 0.03051 (7) | |
S1 | 0.88379 (6) | 0.48689 (8) | 0.29425 (6) | 0.04313 (19) | |
S2 | 0.90608 (6) | 0.35733 (8) | 0.08183 (6) | 0.0421 (2) | |
S3 | 0.90999 (6) | 0.17753 (7) | 0.31041 (7) | 0.04145 (18) | |
P1 | 0.82094 (6) | 0.46934 (8) | 0.14797 (6) | 0.03857 (19) | |
P2 | 1.0000 | 0.06660 (11) | 0.2500 | 0.0392 (3) | |
O1 | 0.71336 (17) | 0.4286 (2) | 0.1381 (2) | 0.0511 (6) | |
O2 | 0.80188 (18) | 0.5910 (2) | 0.08814 (19) | 0.0526 (6) | |
O3 | 0.95068 (18) | −0.0275 (2) | 0.17078 (18) | 0.0528 (6) | |
C1 | 0.6870 (3) | 0.3135 (4) | 0.1744 (4) | 0.0613 (10) | |
H1A | 0.6190 | 0.3045 | 0.1618 | 0.092* | |
H1B | 0.7073 | 0.3070 | 0.2475 | 0.092* | |
H1C | 0.7170 | 0.2524 | 0.1380 | 0.092* | |
C2 | 0.8808 (4) | 0.6652 (4) | 0.0679 (4) | 0.0692 (13) | |
H2A | 0.8571 | 0.7353 | 0.0309 | 0.104* | |
H2B | 0.9212 | 0.6218 | 0.0267 | 0.104* | |
H2C | 0.9168 | 0.6880 | 0.1325 | 0.104* | |
C3 | 0.8866 (3) | 0.0119 (4) | 0.0811 (3) | 0.0668 (11) | |
H3A | 0.8632 | −0.0560 | 0.0409 | 0.100* | |
H3B | 0.9203 | 0.0635 | 0.0391 | 0.100* | |
H3C | 0.8340 | 0.0543 | 0.1041 | 0.100* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Os1 | 0.03257 (11) | 0.02900 (10) | 0.03024 (10) | 0.000 | 0.00492 (6) | 0.000 |
S1 | 0.0479 (5) | 0.0438 (5) | 0.0382 (4) | 0.0089 (4) | 0.0072 (3) | −0.0066 (3) |
S2 | 0.0460 (5) | 0.0464 (5) | 0.0331 (4) | 0.0090 (3) | 0.0019 (3) | −0.0047 (3) |
S3 | 0.0424 (4) | 0.0360 (4) | 0.0474 (4) | −0.0053 (3) | 0.0116 (3) | 0.0020 (3) |
P1 | 0.0374 (4) | 0.0373 (5) | 0.0408 (4) | 0.0060 (3) | 0.0038 (3) | 0.0015 (3) |
P2 | 0.0465 (6) | 0.0292 (6) | 0.0401 (6) | 0.000 | −0.0016 (5) | 0.000 |
O1 | 0.0393 (13) | 0.0486 (14) | 0.0642 (14) | 0.0032 (10) | 0.0012 (11) | 0.0042 (11) |
O2 | 0.0543 (15) | 0.0454 (15) | 0.0587 (14) | 0.0081 (11) | 0.0087 (11) | 0.0108 (11) |
O3 | 0.0665 (16) | 0.0348 (13) | 0.0526 (14) | −0.0008 (11) | −0.0108 (12) | −0.0061 (10) |
C1 | 0.054 (2) | 0.050 (2) | 0.081 (3) | −0.0058 (18) | 0.011 (2) | 0.006 (2) |
C2 | 0.087 (3) | 0.052 (3) | 0.073 (3) | −0.005 (2) | 0.029 (3) | 0.0110 (19) |
C3 | 0.079 (3) | 0.054 (2) | 0.059 (2) | 0.000 (2) | −0.022 (2) | −0.0065 (19) |
Os1—S1 | 2.4424 (10) | P2—S3i | 2.0067 (12) |
Os1—S1i | 2.4424 (10) | O1—C1 | 1.439 (5) |
Os1—S2 | 2.4191 (8) | O2—C2 | 1.443 (5) |
Os1—S2i | 2.4191 (8) | O3—C3 | 1.454 (4) |
Os1—S3 | 2.4120 (10) | C1—H1A | 0.96 |
Os1—S3i | 2.4120 (10) | C1—H1B | 0.96 |
S1—P1 | 2.0044 (12) | C1—H1C | 0.96 |
S2—P1 | 2.0045 (12) | C2—H2A | 0.96 |
S3—P2 | 2.0067 (12) | C2—H2B | 0.96 |
P1—O2 | 1.578 (3) | C2—H2C | 0.96 |
P1—O1 | 1.579 (3) | C3—H3A | 0.96 |
P2—O3 | 1.576 (2) | C3—H3B | 0.96 |
P2—O3i | 1.576 (2) | C3—H3C | 0.96 |
S1—Os1—S1i | 95.30 (5) | O3i—P2—S3i | 114.79 (10) |
S1—Os1—S2 | 81.24 (3) | O3—P2—S3 | 114.79 (10) |
S1—Os1—S2i | 92.64 (3) | O3i—P2—S3 | 114.38 (10) |
S1—Os1—S3 | 92.16 (4) | S3i—P2—S3 | 103.27 (7) |
S1i—Os1—S3 | 169.57 (3) | C1—O1—P1 | 121.3 (2) |
S1i—Os1—S2 | 92.64 (3) | C2—O2—P1 | 120.0 (3) |
S1i—Os1—S2i | 81.24 (3) | C3—O3—P2 | 120.1 (2) |
S1i—Os1—S3 | 169.57 (3) | O1—C1—H1A | 109.5 |
S1i—Os1—S3i | 92.16 (4) | O1—C1—H1B | 109.5 |
S2—Os1—S2i | 170.96 (4) | H1A—C1—H1B | 109.5 |
S2—Os1—S3 | 95.69 (4) | O1—C1—H1C | 109.5 |
S2—Os1—S3i | 91.16 (3) | H1A—C1—H1C | 109.5 |
S2i—Os1—S3 | 91.16 (3) | H1B—C1—H1C | 109.5 |
S2i—Os1—S3i | 95.69 (4) | O2—C2—H2A | 109.5 |
S3—Os1—S3i | 81.43 (5) | O2—C2—H2B | 109.5 |
P1—S1—Os1 | 86.83 (4) | H2A—C2—H2B | 109.5 |
P1—S2—Os1 | 87.47 (4) | O2—C2—H2C | 109.5 |
P2—S3—Os1 | 87.65 (4) | H2A—C2—H2C | 109.5 |
O2—P1—O1 | 96.08 (14) | H2B—C2—H2C | 109.5 |
O2—P1—S1 | 114.19 (11) | O3—C3—H3A | 109.5 |
O1—P1—S1 | 114.64 (10) | O3—C3—H3B | 109.5 |
O2—P1—S2 | 114.09 (10) | H3A—C3—H3B | 109.5 |
O1—P1—S2 | 113.97 (11) | O3—C3—H3C | 109.5 |
S1—P1—S2 | 104.28 (5) | H3A—C3—H3C | 109.5 |
O3—P2—O3i | 95.82 (19) | H3B—C3—H3C | 109.5 |
O3—P2—S3i | 114.38 (10) | ||
S3—Os1—S1—P1 | −92.55 (5) | Os1—S1—P1—S2 | −3.55 (5) |
S3i—Os1—S1—P1 | −40.73 (17) | Os1—S2—P1—O2 | 128.83 (12) |
S2—Os1—S1—P1 | 2.88 (4) | Os1—S2—P1—O1 | −122.15 (11) |
S2i—Os1—S1—P1 | 176.19 (4) | Os1—S2—P1—S1 | 3.58 (5) |
S1i—Os1—S1—P1 | 94.75 (4) | Os1—S3—P2—O3 | −125.17 (11) |
S3—Os1—S2—P1 | 88.44 (5) | Os1—S3—P2—O3i | 125.44 (11) |
S3i—Os1—S2—P1 | 169.94 (4) | O2—P1—O1—C1 | 175.4 (3) |
S1i—Os1—S2—P1 | −97.84 (5) | S1—P1—O1—C1 | −64.5 (3) |
S1—Os1—S2—P1 | −2.88 (4) | S2—P1—O1—C1 | 55.6 (3) |
S2—Os1—S3—P2 | 90.32 (4) | O1—P1—O2—C2 | −176.0 (3) |
S2i—Os1—S3—P2 | −95.58 (4) | S1—P1—O2—C2 | 63.5 (3) |
S1i—Os1—S3—P2 | −52.60 (16) | S2—P1—O2—C2 | −56.4 (3) |
S1—Os1—S3—P2 | 171.72 (3) | O3i—P2—O3—C3 | 175.3 (4) |
Os1—S1—P1—O2 | −128.73 (11) | S3i—P2—O3—C3 | −64.1 (3) |
Os1—S1—P1—O1 | 121.76 (11) | S3—P2—O3—C3 | 55.1 (3) |
Symmetry code: (i) −x+2, y, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Os(C2H6O2PS2)3] |
Mr | 661.67 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 298 |
a, b, c (Å) | 14.138 (1), 11.228 (4), 12.970 (1) |
β (°) | 96.99 (1) |
V (Å3) | 2043.6 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 7.11 |
Crystal size (mm) | 0.35 × 0.20 × 0.10 |
Data collection | |
Diffractometer | Nonius MACH-3 four-circle diffractometer |
Absorption correction | Empirical (using intensity measurements) via ψ scan (North et al., 1968) |
Tmin, Tmax | 0.119, 0.180 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3741, 1805, 1691 |
Rint | 0.024 |
(sin θ/λ)max (Å−1) | 0.594 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.017, 0.043, 1.09 |
No. of reflections | 1805 |
No. of parameters | 101 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.34, −0.80 |
Computer programs: ARGUS-MACH3 (Nonius, 1997), ARGUS-MACH3, XCAD4 (Harms, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.
The crystal structure of tris(dimethyldithiophosphato)osmium(III), (I), was originally described in the Cc space group (Jain et al., 2001). 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 osmium atom and one of P atom, P2, lie on a twofold axis.