In the structure of mer,cis-[RhCl3(C2H6OS)3], the RhIII ion is coordinated by one O and two S atoms, the latter in a cis position, from three dimethyl sulfoxide molecules and three chloride ions in a mer configuration in a distorted octahedral coordination.
Supporting information
CCDC reference: 624504
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (S-C) = 0.005 Å
- R factor = 0.034
- wR factor = 0.086
- Data-to-parameter ratio = 26.7
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for S3
Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for S2 - O2 .. 5.13 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Rh1 - O3 .. 7.36 su
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Rh1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S2
PLAT431_ALERT_2_C Short Inter HL..A Contact Cl3 .. S3 .. 3.40 Ang.
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
7 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: PLATON (Spek,2003).
mer,
cis-trichlorotris(dimethyl sulfoxide)rhodium(III)
top
Crystal data top
[RhCl3(C2H6OS)3] | F(000) = 1776 |
Mr = 443.64 | Dx = 1.821 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 23874 reflections |
a = 10.0230 (4) Å | θ = 3.9–32.2° |
b = 11.2803 (5) Å | µ = 1.93 mm−1 |
c = 28.6327 (14) Å | T = 293 K |
V = 3237.3 (2) Å3 | Block, yellow |
Z = 8 | 0.5 × 0.4 × 0.2 mm |
Data collection top
Bruker X-calibur-3 CCD detector diffractometer | 3896 independent reflections |
Radiation source: fine-focus sealed tube | 2918 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
Detector resolution: 12 pixels mm-1 | θmax = 28.0°, θmin = 3.9° |
ω scans | h = −13→10 |
Absorption correction: numerical (X-RED; Stoe & Cie, 1997) | k = −14→14 |
Tmin = 0.382, Tmax = 0.680 | l = −37→36 |
23874 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
wR(F2) = 0.086 | w = 1/[σ2(Fo2) + (0.0384P)2 + 3.6685P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
3896 reflections | Δρmax = 0.58 e Å−3 |
146 parameters | Δρmin = −0.87 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00141 (14) |
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. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.00896 (2) | 0.65005 (2) | 0.122589 (8) | 0.03562 (10) | |
Cl1 | 0.05012 (11) | 0.85120 (8) | 0.10843 (4) | 0.0599 (3) | |
Cl2 | −0.04489 (10) | 0.44986 (8) | 0.13166 (4) | 0.0601 (3) | |
Cl3 | 0.14941 (11) | 0.60054 (11) | 0.05962 (4) | 0.0684 (3) | |
S1 | 0.18215 (9) | 0.65261 (8) | 0.17210 (3) | 0.0419 (2) | |
O1 | 0.1673 (3) | 0.7372 (2) | 0.21049 (9) | 0.0601 (7) | |
C11 | 0.3361 (4) | 0.6830 (4) | 0.14432 (18) | 0.0705 (12) | |
H11A | 0.3325 | 0.7600 | 0.1301 | 0.106* | |
H11B | 0.3528 | 0.6242 | 0.1208 | 0.106* | |
H11C | 0.4066 | 0.6814 | 0.1670 | 0.106* | |
C12 | 0.2139 (4) | 0.5109 (4) | 0.19515 (15) | 0.0636 (11) | |
H12A | 0.1364 | 0.4833 | 0.2116 | 0.095* | |
H12B | 0.2882 | 0.5149 | 0.2162 | 0.095* | |
H12C | 0.2342 | 0.4571 | 0.1702 | 0.095* | |
S2 | −0.12839 (10) | 0.68289 (8) | 0.18485 (3) | 0.0480 (2) | |
O2 | −0.0960 (3) | 0.6083 (3) | 0.22510 (11) | 0.0852 (10) | |
C21 | −0.2965 (4) | 0.6599 (4) | 0.16877 (18) | 0.0716 (13) | |
H21A | −0.3077 | 0.5798 | 0.1581 | 0.107* | |
H21B | −0.3202 | 0.7138 | 0.1442 | 0.107* | |
H21C | −0.3530 | 0.6734 | 0.1953 | 0.107* | |
C22 | −0.1362 (5) | 0.8327 (4) | 0.20234 (17) | 0.0730 (13) | |
H22A | −0.0494 | 0.8584 | 0.2123 | 0.109* | |
H22B | −0.1981 | 0.8406 | 0.2277 | 0.109* | |
H22C | −0.1653 | 0.8805 | 0.1766 | 0.109* | |
S3 | −0.15890 (11) | 0.58509 (10) | 0.03404 (4) | 0.0588 (3) | |
O3 | −0.1563 (3) | 0.6630 (2) | 0.07747 (10) | 0.0589 (7) | |
C31 | −0.1258 (7) | 0.6858 (5) | −0.01104 (19) | 0.1022 (19) | |
H31A | −0.0322 | 0.7041 | −0.0114 | 0.153* | |
H31B | −0.1760 | 0.7572 | −0.0060 | 0.153* | |
H31C | −0.1510 | 0.6514 | −0.0404 | 0.153* | |
C32 | −0.3360 (5) | 0.5662 (6) | 0.0268 (2) | 0.113 (2) | |
H32A | −0.3687 | 0.5121 | 0.0500 | 0.169* | |
H32B | −0.3540 | 0.5352 | −0.0037 | 0.169* | |
H32C | −0.3796 | 0.6414 | 0.0304 | 0.169* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.03959 (15) | 0.03351 (14) | 0.03376 (14) | 0.00049 (11) | −0.00004 (11) | 0.00109 (10) |
Cl1 | 0.0772 (7) | 0.0418 (5) | 0.0608 (6) | −0.0085 (5) | −0.0049 (5) | 0.0170 (4) |
Cl2 | 0.0551 (5) | 0.0347 (4) | 0.0905 (8) | −0.0038 (4) | −0.0049 (5) | 0.0015 (5) |
Cl3 | 0.0630 (6) | 0.0922 (8) | 0.0499 (6) | −0.0043 (6) | 0.0131 (5) | −0.0192 (6) |
S1 | 0.0442 (5) | 0.0385 (4) | 0.0430 (5) | 0.0031 (4) | −0.0073 (4) | −0.0014 (4) |
O1 | 0.0704 (18) | 0.0589 (16) | 0.0509 (15) | 0.0149 (14) | −0.0202 (13) | −0.0169 (13) |
C11 | 0.043 (2) | 0.075 (3) | 0.094 (3) | −0.011 (2) | −0.005 (2) | −0.003 (3) |
C12 | 0.076 (3) | 0.049 (2) | 0.065 (3) | 0.010 (2) | −0.025 (2) | 0.011 (2) |
S2 | 0.0497 (5) | 0.0461 (5) | 0.0481 (5) | 0.0099 (4) | 0.0110 (4) | 0.0080 (4) |
O2 | 0.092 (2) | 0.096 (2) | 0.067 (2) | 0.032 (2) | 0.0311 (18) | 0.0311 (18) |
C21 | 0.048 (2) | 0.068 (3) | 0.099 (4) | 0.008 (2) | 0.013 (2) | 0.004 (3) |
C22 | 0.088 (3) | 0.057 (3) | 0.074 (3) | 0.015 (2) | 0.020 (3) | −0.017 (2) |
S3 | 0.0642 (6) | 0.0589 (6) | 0.0533 (6) | −0.0019 (5) | −0.0186 (5) | −0.0018 (5) |
O3 | 0.0605 (16) | 0.0557 (16) | 0.0606 (17) | 0.0095 (13) | −0.0120 (14) | −0.0125 (13) |
C31 | 0.153 (6) | 0.078 (3) | 0.076 (4) | −0.015 (4) | −0.028 (4) | 0.021 (3) |
C32 | 0.071 (3) | 0.143 (6) | 0.125 (5) | 0.000 (4) | −0.037 (3) | −0.053 (4) |
Geometric parameters (Å, º) top
Rh1—O3 | 2.106 (3) | S2—C21 | 1.766 (4) |
Rh1—S1 | 2.2414 (9) | C21—H21A | 0.9600 |
Rh1—S2 | 2.2826 (9) | C21—H21B | 0.9600 |
Rh1—Cl2 | 2.3363 (9) | C21—H21C | 0.9600 |
Rh1—Cl1 | 2.3416 (9) | C22—H22A | 0.9600 |
Rh1—Cl3 | 2.3545 (10) | C22—H22B | 0.9600 |
S1—O1 | 1.463 (3) | C22—H22C | 0.9600 |
S1—C12 | 1.759 (4) | S3—O3 | 1.523 (3) |
S1—C11 | 1.770 (4) | S3—C31 | 1.752 (5) |
C11—H11A | 0.9600 | S3—C32 | 1.799 (5) |
C11—H11B | 0.9600 | C31—H31A | 0.9600 |
C11—H11C | 0.9600 | C31—H31B | 0.9600 |
C12—H12A | 0.9600 | C31—H31C | 0.9600 |
C12—H12B | 0.9600 | C32—H32A | 0.9600 |
C12—H12C | 0.9600 | C32—H32B | 0.9600 |
S2—O2 | 1.463 (3) | C32—H32C | 0.9600 |
S2—C22 | 1.764 (4) | | |
| | | |
O3—Rh1—S1 | 175.12 (7) | O2—S2—C21 | 109.4 (2) |
O3—Rh1—S2 | 89.63 (8) | C22—S2—C21 | 99.9 (2) |
S1—Rh1—S2 | 88.34 (4) | O2—S2—Rh1 | 112.84 (13) |
O3—Rh1—Cl2 | 87.33 (8) | C22—S2—Rh1 | 113.83 (16) |
S1—Rh1—Cl2 | 96.95 (4) | C21—S2—Rh1 | 110.37 (17) |
S2—Rh1—Cl2 | 86.03 (4) | S2—C21—H21A | 109.5 |
O3—Rh1—Cl1 | 88.01 (8) | S2—C21—H21B | 109.5 |
S1—Rh1—Cl1 | 87.74 (4) | H21A—C21—H21B | 109.5 |
S2—Rh1—Cl1 | 94.83 (4) | S2—C21—H21C | 109.5 |
Cl2—Rh1—Cl1 | 175.26 (4) | H21A—C21—H21C | 109.5 |
O3—Rh1—Cl3 | 90.97 (8) | H21B—C21—H21C | 109.5 |
S1—Rh1—Cl3 | 91.40 (4) | S2—C22—H22A | 109.5 |
S2—Rh1—Cl3 | 175.61 (4) | S2—C22—H22B | 109.5 |
Cl2—Rh1—Cl3 | 89.65 (4) | H22A—C22—H22B | 109.5 |
Cl1—Rh1—Cl3 | 89.54 (4) | S2—C22—H22C | 109.5 |
O1—S1—C12 | 109.23 (19) | H22A—C22—H22C | 109.5 |
O1—S1—C11 | 107.5 (2) | H22B—C22—H22C | 109.5 |
C12—S1—C11 | 100.8 (2) | O3—S3—C31 | 103.0 (2) |
O1—S1—Rh1 | 113.88 (11) | O3—S3—C32 | 100.3 (2) |
C12—S1—Rh1 | 111.45 (14) | C31—S3—C32 | 100.3 (3) |
C11—S1—Rh1 | 113.17 (16) | S3—O3—Rh1 | 118.33 (15) |
S1—C11—H11A | 109.5 | S3—C31—H31A | 109.5 |
S1—C11—H11B | 109.5 | S3—C31—H31B | 109.5 |
H11A—C11—H11B | 109.5 | H31A—C31—H31B | 109.5 |
S1—C11—H11C | 109.5 | S3—C31—H31C | 109.5 |
H11A—C11—H11C | 109.5 | H31A—C31—H31C | 109.5 |
H11B—C11—H11C | 109.5 | H31B—C31—H31C | 109.5 |
S1—C12—H12A | 109.5 | S3—C32—H32A | 109.5 |
S1—C12—H12B | 109.5 | S3—C32—H32B | 109.5 |
H12A—C12—H12B | 109.5 | H32A—C32—H32B | 109.5 |
S1—C12—H12C | 109.5 | S3—C32—H32C | 109.5 |
H12A—C12—H12C | 109.5 | H32A—C32—H32C | 109.5 |
H12B—C12—H12C | 109.5 | H32B—C32—H32C | 109.5 |
O2—S2—C22 | 109.7 (2) | | |
| | | |
S2—Rh1—S1—O1 | −35.72 (14) | Cl1—Rh1—S2—O2 | −132.59 (18) |
Cl2—Rh1—S1—O1 | −121.52 (14) | O3—Rh1—S2—C22 | −94.7 (2) |
Cl1—Rh1—S1—O1 | 59.18 (14) | S1—Rh1—S2—C22 | 80.8 (2) |
Cl3—Rh1—S1—O1 | 148.66 (14) | Cl2—Rh1—S2—C22 | 177.9 (2) |
S2—Rh1—S1—C12 | 88.40 (17) | Cl1—Rh1—S2—C22 | −6.8 (2) |
Cl2—Rh1—S1—C12 | 2.61 (17) | O3—Rh1—S2—C21 | 16.67 (18) |
Cl1—Rh1—S1—C12 | −176.70 (17) | S1—Rh1—S2—C21 | −167.77 (16) |
Cl3—Rh1—S1—C12 | −87.22 (17) | Cl2—Rh1—S2—C21 | −70.68 (17) |
S2—Rh1—S1—C11 | −158.83 (17) | Cl1—Rh1—S2—C21 | 104.64 (17) |
Cl2—Rh1—S1—C11 | 115.37 (18) | C31—S3—O3—Rh1 | −106.4 (3) |
Cl1—Rh1—S1—C11 | −63.93 (18) | C32—S3—O3—Rh1 | 150.4 (3) |
Cl3—Rh1—S1—C11 | 25.55 (18) | S2—Rh1—O3—S3 | −145.35 (18) |
O3—Rh1—S2—O2 | 139.4 (2) | Cl2—Rh1—O3—S3 | −59.31 (17) |
S1—Rh1—S2—O2 | −45.00 (18) | Cl1—Rh1—O3—S3 | 119.81 (18) |
Cl2—Rh1—S2—O2 | 52.09 (18) | Cl3—Rh1—O3—S3 | 30.30 (18) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C12—H12B···O2i | 0.96 | 2.30 | 3.171 (5) | 151 |
C22—H22B···O1ii | 0.96 | 2.51 | 3.357 (5) | 147 |
C31—H31B···Cl3iii | 0.96 | 2.83 | 3.580 (6) | 136 |
Symmetry codes: (i) x+1/2, y, −z+1/2; (ii) x−1/2, y, −z+1/2; (iii) x−1/2, −y+3/2, −z. |