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

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680102092X/ci6081sup1.cif
Contains datablocks I, gkl007

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680102092X/ci6081Isup2.hkl
Contains datablock I

CCDC reference: 180518

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](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


Amber Alert 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

Comment top

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.

Computing details top

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 top
[Figure 1] Fig. 1. ORTEPII (Johnson, 1976) plot of the title compound with ellipsoids at the 50% probability level.
Tris(dimethyldithiophosphato)osmium(III) top
Crystal data top
[Os(C2H6O2PS2)3]F(000) = 1276
Mr = 661.67Dx = 2.151 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 14.138 (1) ÅCell parameters from 25 reflections
b = 11.228 (4) Åθ = 11.4–14.2°
c = 12.970 (1) ŵ = 7.11 mm1
β = 96.99 (1)°T = 298 K
V = 2043.6 (8) Å3Plate, violet
Z = 40.35 × 0.20 × 0.10 mm
Data collection top
Nonius MACH-3 four-circle
diffractometer
1691 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.024
Graphite monochromatorθmax = 25.0°, θmin = 2.3°
ω scansh = 1610
Absorption correction: empirical (using intensity measurements)
via ψ scan (North et al., 1968)
k = 1310
Tmin = 0.119, Tmax = 0.180l = 1515
3741 measured reflections3 standard reflections every 60 min
1805 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.017Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.043H-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 parametersΔρmax = 0.34 e Å3
0 restraintsΔρmin = 0.80 e Å3
Crystal data top
[Os(C2H6O2PS2)3]V = 2043.6 (8) Å3
Mr = 661.67Z = 4
Monoclinic, C2/cMo Kα radiation
a = 14.138 (1) ŵ = 7.11 mm1
b = 11.228 (4) ÅT = 298 K
c = 12.970 (1) Å0.35 × 0.20 × 0.10 mm
β = 96.99 (1)°
Data collection top
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 = 0.1803 standard reflections every 60 min
3741 measured reflections intensity decay: none
1805 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0170 restraints
wR(F2) = 0.043H-atom parameters constrained
S = 1.09Δρmax = 0.34 e Å3
1805 reflectionsΔρmin = 0.80 e Å3
101 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Os11.00000.340348 (14)0.25000.03051 (7)
S10.88379 (6)0.48689 (8)0.29425 (6)0.04313 (19)
S20.90608 (6)0.35733 (8)0.08183 (6)0.0421 (2)
S30.90999 (6)0.17753 (7)0.31041 (7)0.04145 (18)
P10.82094 (6)0.46934 (8)0.14797 (6)0.03857 (19)
P21.00000.06660 (11)0.25000.0392 (3)
O10.71336 (17)0.4286 (2)0.1381 (2)0.0511 (6)
O20.80188 (18)0.5910 (2)0.08814 (19)0.0526 (6)
O30.95068 (18)0.0275 (2)0.17078 (18)0.0528 (6)
C10.6870 (3)0.3135 (4)0.1744 (4)0.0613 (10)
H1A0.61900.30450.16180.092*
H1B0.70730.30700.24750.092*
H1C0.71700.25240.13800.092*
C20.8808 (4)0.6652 (4)0.0679 (4)0.0692 (13)
H2A0.85710.73530.03090.104*
H2B0.92120.62180.02670.104*
H2C0.91680.68800.13250.104*
C30.8866 (3)0.0119 (4)0.0811 (3)0.0668 (11)
H3A0.86320.05600.04090.100*
H3B0.92030.06350.03910.100*
H3C0.83400.05430.10410.100*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Os10.03257 (11)0.02900 (10)0.03024 (10)0.0000.00492 (6)0.000
S10.0479 (5)0.0438 (5)0.0382 (4)0.0089 (4)0.0072 (3)0.0066 (3)
S20.0460 (5)0.0464 (5)0.0331 (4)0.0090 (3)0.0019 (3)0.0047 (3)
S30.0424 (4)0.0360 (4)0.0474 (4)0.0053 (3)0.0116 (3)0.0020 (3)
P10.0374 (4)0.0373 (5)0.0408 (4)0.0060 (3)0.0038 (3)0.0015 (3)
P20.0465 (6)0.0292 (6)0.0401 (6)0.0000.0016 (5)0.000
O10.0393 (13)0.0486 (14)0.0642 (14)0.0032 (10)0.0012 (11)0.0042 (11)
O20.0543 (15)0.0454 (15)0.0587 (14)0.0081 (11)0.0087 (11)0.0108 (11)
O30.0665 (16)0.0348 (13)0.0526 (14)0.0008 (11)0.0108 (12)0.0061 (10)
C10.054 (2)0.050 (2)0.081 (3)0.0058 (18)0.011 (2)0.006 (2)
C20.087 (3)0.052 (3)0.073 (3)0.005 (2)0.029 (3)0.0110 (19)
C30.079 (3)0.054 (2)0.059 (2)0.000 (2)0.022 (2)0.0065 (19)
Geometric parameters (Å, º) top
Os1—S12.4424 (10)P2—S3i2.0067 (12)
Os1—S1i2.4424 (10)O1—C11.439 (5)
Os1—S22.4191 (8)O2—C21.443 (5)
Os1—S2i2.4191 (8)O3—C31.454 (4)
Os1—S32.4120 (10)C1—H1A0.96
Os1—S3i2.4120 (10)C1—H1B0.96
S1—P12.0044 (12)C1—H1C0.96
S2—P12.0045 (12)C2—H2A0.96
S3—P22.0067 (12)C2—H2B0.96
P1—O21.578 (3)C2—H2C0.96
P1—O11.579 (3)C3—H3A0.96
P2—O31.576 (2)C3—H3B0.96
P2—O3i1.576 (2)C3—H3C0.96
S1—Os1—S1i95.30 (5)O3i—P2—S3i114.79 (10)
S1—Os1—S281.24 (3)O3—P2—S3114.79 (10)
S1—Os1—S2i92.64 (3)O3i—P2—S3114.38 (10)
S1—Os1—S392.16 (4)S3i—P2—S3103.27 (7)
S1i—Os1—S3169.57 (3)C1—O1—P1121.3 (2)
S1i—Os1—S292.64 (3)C2—O2—P1120.0 (3)
S1i—Os1—S2i81.24 (3)C3—O3—P2120.1 (2)
S1i—Os1—S3169.57 (3)O1—C1—H1A109.5
S1i—Os1—S3i92.16 (4)O1—C1—H1B109.5
S2—Os1—S2i170.96 (4)H1A—C1—H1B109.5
S2—Os1—S395.69 (4)O1—C1—H1C109.5
S2—Os1—S3i91.16 (3)H1A—C1—H1C109.5
S2i—Os1—S391.16 (3)H1B—C1—H1C109.5
S2i—Os1—S3i95.69 (4)O2—C2—H2A109.5
S3—Os1—S3i81.43 (5)O2—C2—H2B109.5
P1—S1—Os186.83 (4)H2A—C2—H2B109.5
P1—S2—Os187.47 (4)O2—C2—H2C109.5
P2—S3—Os187.65 (4)H2A—C2—H2C109.5
O2—P1—O196.08 (14)H2B—C2—H2C109.5
O2—P1—S1114.19 (11)O3—C3—H3A109.5
O1—P1—S1114.64 (10)O3—C3—H3B109.5
O2—P1—S2114.09 (10)H3A—C3—H3B109.5
O1—P1—S2113.97 (11)O3—C3—H3C109.5
S1—P1—S2104.28 (5)H3A—C3—H3C109.5
O3—P2—O3i95.82 (19)H3B—C3—H3C109.5
O3—P2—S3i114.38 (10)
S3—Os1—S1—P192.55 (5)Os1—S1—P1—S23.55 (5)
S3i—Os1—S1—P140.73 (17)Os1—S2—P1—O2128.83 (12)
S2—Os1—S1—P12.88 (4)Os1—S2—P1—O1122.15 (11)
S2i—Os1—S1—P1176.19 (4)Os1—S2—P1—S13.58 (5)
S1i—Os1—S1—P194.75 (4)Os1—S3—P2—O3125.17 (11)
S3—Os1—S2—P188.44 (5)Os1—S3—P2—O3i125.44 (11)
S3i—Os1—S2—P1169.94 (4)O2—P1—O1—C1175.4 (3)
S1i—Os1—S2—P197.84 (5)S1—P1—O1—C164.5 (3)
S1—Os1—S2—P12.88 (4)S2—P1—O1—C155.6 (3)
S2—Os1—S3—P290.32 (4)O1—P1—O2—C2176.0 (3)
S2i—Os1—S3—P295.58 (4)S1—P1—O2—C263.5 (3)
S1i—Os1—S3—P252.60 (16)S2—P1—O2—C256.4 (3)
S1—Os1—S3—P2171.72 (3)O3i—P2—O3—C3175.3 (4)
Os1—S1—P1—O2128.73 (11)S3i—P2—O3—C364.1 (3)
Os1—S1—P1—O1121.76 (11)S3—P2—O3—C355.1 (3)
Symmetry code: (i) x+2, y, z+1/2.

Experimental details

Crystal data
Chemical formula[Os(C2H6O2PS2)3]
Mr661.67
Crystal system, space groupMonoclinic, C2/c
Temperature (K)298
a, b, c (Å)14.138 (1), 11.228 (4), 12.970 (1)
β (°) 96.99 (1)
V3)2043.6 (8)
Z4
Radiation typeMo Kα
µ (mm1)7.11
Crystal size (mm)0.35 × 0.20 × 0.10
Data collection
DiffractometerNonius MACH-3 four-circle
diffractometer
Absorption correctionEmpirical (using intensity measurements)
via ψ scan (North et al., 1968)
Tmin, Tmax0.119, 0.180
No. of measured, independent and
observed [I > 2σ(I)] reflections
3741, 1805, 1691
Rint0.024
(sin θ/λ)max1)0.594
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.017, 0.043, 1.09
No. of reflections1805
No. of parameters101
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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.

 

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