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Cis/trans isomers of PtX2L2 (X = halogen, L = neutral ligand); the crystal structure of trans-di­chlorobis(di­methyl sulfide)platinum(II) and the pressure dependence of its unit-cell dimensions

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aDepartment of Organic Chemistry, Centre for Chemistry and Chemical Engineering, Lund University, PO Box 124, SE-221 00 Lund, Sweden
*Correspondence e-mail: christian.hansson@inorg.lu.se

(Received 20 October 2005; accepted 7 February 2006)

trans-PtCl2(dms)2 (dms is dimethyl sulfide) crystallizes in the space group P21/n and adopts the molecular point group Ci, which is the most frequently occurring point group for trans-PtX2L2 complexes (78%), as observed in the Cambridge Structural Database (CSD; 2005 release), followed by C1 (16%). Density functional theory calculations show that the observed geometry for trans-PtCl2(dms)2 has slightly higher energy than the most favorable geometry in the point group C2h, but this geometry would require a space group that hampers close packing, thus showing that intermolecular forces determine the point group for the title compound. High-pressure powder diffraction studies of trans-PtCl2(dms)2 show no phase transformation up to 8.0 GPa. The bulk modulus is 8.1 (6) GPa and the pressure derivative 8.1 (4). In the CSD, the number of cis- and trans-PtX2L2 compounds are almost equal, viz. 156 cis and 160 trans compounds, showing no preference for either isomer in the solid state.

1. Introduction

A synthetic procedure resulting in a mixture of cis- and trans-PtCl2(dms)2 was published as early as 1934 (Cox et al., 1934[Cox, E. G., Saenger, H. & Wardlaw, W. (1934). J. Chem. Soc. pp. 182-186.]) and a tentative structure for the trans isomer, based on rotation X-ray photographs, was given. Horn et al. (1990[Horn, G. W., Kumar, R., Maverick, A. W., Fronczek, F. R. & Watkins, S. F. (1990). Acta Cryst. C46, 135-136.]) have determined the structure of the cis isomer but, besides a preliminary report (Johansson, 2001[Johansson, M. (2001). PhD thesis, Lund University, Sweden.]), no detailed structural model for the trans complex has been published previously.

Studies of the effects of high pressure on molecular crystals are at the initial stage but some characteristics have been reported, i.e. conformational changes and compression of weak intermolecular bonds (Boldyreva, 2003[Boldyreva, E. (2003). High-Pressure Induced Structural Changes in Molecular Crystals Preserving the Space Group Symmetry: Anisotropic Distortion/Isosymmetric Polymorphism. INDABA IV `Patterns in Nature', Skukuza, Kruger NP, South Africa.]). As a result one can observe either a structural reconstruction, i.e. a phase transition, or a continuous distortion within the limits of stability of the same phase. No high-pressure investigation on trans-PtCl2(dms)2 has yet been published, and we present here a powder diffraction study up to 8.0 GPa.

Whether the formation of the cis and/or trans isomer of a complex is guided by thermodynamic and/or kinetic effects is an interesting and important question since the cis and trans isomers will have different properties. In many cases it is important to synthesize an isomerically clean product. In, for example, the Heck reaction it is the cis complex that goes into the catalytic cycle (Nilsson, 2005[Nilsson, P. (2005). PhD thesis, Lund University, Sweden.]). Beck et al. (2002[Beck, W., Klapötke, T. M. & Ponikwar, W. (2002). Z. Naturforsch. Teil B, 57, 1120-1124.]) have performed DFT (density functional theory) calculations on the structure and stability of some chelate complexes [X(H3P)Pt(N,O-chelate)], X = Cl or CH3, which exist in either cis or trans form (N donor with respect to the PH3 ligand). They concluded that for X = CH3 the cis isomer has slightly lower total energy than the trans isomer (1 kJ mol−1), while the order is reversed for X = Cl (27 kJ mol−1) in the gas phase and at 0 K. These findings stimulated us to search the Cambridge Structural Database (CSD; 2005 release; Allen, 2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]) for one class of compounds, PtX2L2 (X is one and the same halogen and L is one and the same neutral ligand), to investigate the distribution of the cis and trans isomers. However, one must be cautious when attempting to derive regularities from such data, since they represent the existing set of crystal structures, and any observed trend may change in the future. In order to investigate the relative stabilities of the isomers we have performed DFT calculations in the gas phase optimizing the geometry of those complexes observed as both cis and trans isomers in the solid state in the CSD.

We have applied the question put forward by Brock & Dunitz (1994[Brock, C. P. & Dunitz, J. D. (1994). Chem. Mater. 6, 1118-1127.]) – `Exactly what molecular symmetries are retained in the crystal?' – to trans-PtX2L2, with potential Ci symmetry. Most of these complexes have potential C2h symmetry, but some compounds may also contain stereoisomers not adopting Ci symmetry. We have screened the CSD for the crystal class distribution (Belsky et al., 1995[Belsky, V. K., Zorkaya, O. N. & Zorky, P. M. (1995). Acta Cryst. A51, 473-481.]), which contains information about molecular point-group symmetry.

2. Experimental

2.1. Synthesis

trans-PtCl2(dms)2 was synthesized by the method of Cox et al. (1934[Cox, E. G., Saenger, H. & Wardlaw, W. (1934). J. Chem. Soc. pp. 182-186.]). K2[PtCl4] (1.0005 g, 2.4103 mmol) was dissolved in water (20 ml) in an ice-bath. Dimethyl sulfide (0.40 ml, 5.47 mmol) was added and the reaction mixture was stirred for 16 h. The light-yellow precipitate was filtered off and washed with water (3 × 5 ml). The precipitate was dried and then treated with ice-cold chloroform in order to extract PtCl2(dms)2. The insoluble part of the precipitate {i.e. [Pt(dms)4][PtCl4]} was filtered off and the chloroform was then allowed to evaporate.

The product was recrystallized from acetone. From the mixture of crystals of both cis- and trans-PtCl2(dms)2 a yellow monoclinic plate of trans-PtCl2(dms)2 was selected.

2.2. X-ray measurements and structure determination

Intensity data were collected on a Siemens Bruker SMART CCD diffractometer equipped with a rotating anode (Mo Kα radiation, wavelength 0.71073 Å) at 295 K using exposure times of 20 s per frame. A total of 2300 frames were collected with ω scans and a frame width of 0.2°. The SMART software (Siemens, 1995[Siemens (1995). SMART. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]) was used for the data collection. Completeness of 99.8% was accomplished out to θ = 30.1°. The first 50 frames were recollected at the end of the data collection to check for decay. No decay was observed.

The intensities were merged and integrated with SAINT-Plus (Siemens, 1998[Siemens (1998). SAINT-Plus. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]), and the effects of absorption were corrected using SADABS (Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]). Structure determination was performed with Patterson and difference Fourier methods and refinement by full-matrix least-squares calculations using SHELXL97 (Sheldrick, 1997[Sheldrick, G. M. (1997b). SHELXL97. University of Göttingen, Germany.]b). H-atom positions were calculated as riding on the adjacent C atom (methyl group C—H distance 0.96 Å), while non-H atoms were refined anisotropically. Figures of the complex and its packing arrangement were prepared using DIAMOND (Brandenburg, 2000[Brandenburg, K. (2000). DIAMOND2. Crystal Impact, Bonn, Germany.]).

Experimental details and crystal data are shown in Table 1[link].1

Table 1
Experimental details

Crystal data  
Chemical formula C4H12Cl2PtS2
Mr 390.25
Cell setting, space group Monoclinic, P21/n
Temperature (K) 295 (2)
a, b, c (Å) 8.4637 (13), 6.0176 (10), 10.1812 (16)
α, β, γ (°) 90.00, 105.747 (3), 90.00
V3) 499.08 (14)
Z 2
Dx (Mg m–3) 2.597
Radiation type Mo Kα
No. of reflections for cell parameters 2881
θ range (°) 2.8–31.8
μ (mm–1) 14.94
Specimen form, colour Plate, yellow
Specimen size (mm) 0.28 × 0.12 × 0.06
   
Data collection  
Diffractometer Bruker SMART CCD
Data collection method ω scans
Absorption correction Empirical
Tmin 0.111
Tmax 0.321
No. of measured, independent and observed reflections 5797, 1553, 1018
Criterion for observed reflections I > 2σ(I)
Rint 0.081
θmax (°) 31.8
Range of h, k, l −12 → h → 12
  −8 → k → 8
  −14 → l → 14
   
Refinement  
Refinement on F2
R[F2> 2σ(F2)], wR(F2), S 0.046, 0.109, 0.96
Reflection/profile data 1553
No. of parameters 43
H-atom treatment Constrained to parent site
Weighting scheme w = 1/[σ2(Fo2) + (0.060P)2], where P = (Fo2 + 2Fc2)/3
(Δ/σ)max <0.0001
Δρmax, Δρmin (e Å–3) 1.78, −2.62
Computer programs used: SMART (Bruker, 1995[Siemens (1995). SMART. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]), SAINT-Plus (Bruker, 1998[Siemens (1998). SAINT-Plus. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.]), SHELXS97 (Sheldrick, 1997a[Sheldrick, G. M. (1997a). SHELXS97. University of Göttingen, Germany.]), SHELXL97 (Sheldrick, 1997b[Sheldrick, G. M. (1997b). SHELXL97. University of Göttingen, Germany.]), DIAMOND (Brandenburg, 2000[Brandenburg, K. (2000). DIAMOND2. Crystal Impact, Bonn, Germany.]).

2.3. High-pressure experiments

High-pressure powder diffraction data were collected at Beamline I711, MAX-lab synchrotron source, Lund, Sweden (Cerenius et al., 2000[Cerenius, Y., Ståhl, K., Svensson, A., Ursby, T., Oskarsson, Å., Albersson, J. & Liljas, A. (2000). J. Synchrotron Rad. 7, 203-208.]), using diamond–anvil cell (DAC) techniques [see e.g. Eremets (1996[Eremets, M. (1996). High Pressure Experimental Methods. Oxford University Press.]) for a full review]. The beam was monochromated and focused, and finally the spot size on the sample was reduced by the MAR Desktop slit system to 0.1 × 0.1 mm2. Calibration of the wavelength (λ = 0.9264 Å) and sample–detector distance (d = 120 mm) was performed using powder diffraction data from LaB6 powder in a capillary. The software FIT2D (Hammersley, 1997[Hammersley, A. P. (1997). FIT2D. ESRF Internal Report, ESRF97HA02T: An Introduction and Overview. ESRF, Grenoble, France.]) was used in all data integration and calibration procedures. A Marresearch 165 mm 2000 × 2000 pixels CCD (Marresearch, 2002[Marresearch (2002). Marresearch GmbH, Norderstedt, Germany.]) was used to collect complete powder diffraction rings from samples, contained in a membrane-driven DAC (DXR-6, Diacel Products).

A well grounded powder sample of trans-PtCl2(dms)2 was loaded into the gasket hole (0.15 mm diameter and 0.1 mm deep), together with a small ruby crystal for pressure measurement and the methanol/ethanol (4:1) pressure transmitting medium. Pressure was calibrated by laser-induced fluorescence in the ruby crystal (Piermarini et al., 1975[Piermarini, G. J., Block, S., Barnett, J. D. & Forman, R. A. (1975). J. Appl. Phys. 46, 2774-2780.]). The pressure dependence of the R1 peak shift, calibrated by Mao et al. (1986[Mao, H. K., Xu, J. & Bell, P. M. (1986). J. Geophys. Res. 91, 4673-4676.]), was used to estimate the pressure inside the DAC. The experiments were performed with the DAC mounted on a special stage fitted between the slit system and the CCD of the MAR Desktop. The sample-to-CCD distance was checked by a motorized rotation of the DAC to face a microscope perpendicular to the X-ray beam; this apparatus was used simultaneously for optical inspection and pressure determination by laser-induced ruby fluorescence. Thus, the DAC did not have to be removed from the experimental setup when increasing the pressure, which ensures a good reproducibility in the sample-to-detector distance.

Data were collected at 12 increasing pressures up to 8 GPa and two pressures when decreasing to ambient conditions. No phase transitions were observed, and the unit-cell dimensions appeared to be fully recovered when decreasing from 8 GPa to ambient pressure. Unit-cell dimensions were obtained from the powder diffraction data by using a combination of WinPlotr (Roisnel & Rodriguez-Carvajal, 2001[Roisnel, T. & Rodriguez-Carvajal, J. (2001). Mater. Sci. Forum, 378-381, 118123.]) and TREOR (Werner et al., 1985[Werner, P.-E., Eriksson, L. & Westdahl, M. (1985). J. Appl. Cryst. 18, 367-370.]). Finally, a Le Bail-type peak-fitting procedure (Le Bail et al., 1988[Le Bail, A., Duroy, H. & Fourquet, J. L. (1988). Mater. Res. Bull. 23, 447-452.]) was performed in GSAS (Larson & Von Dreele, 1994[Larson, A. C. & Von Dreele, R. B. (1994). LANSCE MS-H805. Los Alamos National Laboratory, New Mexico, USA.]) before refining the unit-cell dimensions. Powder diffraction data have been deposited in CIF format. Unit-cell parameters are given in Table 2[link] and in Figs. 1[link] and 2[link].

Table 2
Cell parameters of the title compound at different pressures

Pressure (GPa) a (Å) b (Å) c (Å) β (°) Volume (Å3)
0.0001 8.4860 (6) 6.0353 (6) 10.2175 (8) 105.716 (6) 503.73 (5)
0.1370 8.4061 (5) 6.0034 (5) 10.1606 (6) 105.829 (6) 493.31 (4)
0.4110 8.3155 (9) 5.9607 (8) 10.112 (1) 106.02 (1) 481.8 (1)
0.8490 8.1889 (8) 5.9050 (6) 10.010 (1) 106.349 (8) 464.47 (8)
2.2190 7.963 (1) 5.7915 (8) 9.820 (1) 106.93 (1) 433.3 (1)
3.0410 7.867 (1) 5.7418 (7) 9.735 (1) 107.300 (9) 419.83 (9)
3.5890 7.8065 (7) 5.7061 (4) 9.6871 (7) 107.409 (6) 411.74 (6)
4.2740 7.7447 (7) 5.6735 (5) 9.6219 (7) 107.559 (7) 403.08 (6)
5.3980 7.6626 (7) 5.6223 (4) 9.5448 (7) 107.815 (7) 391.48 (6)
5.8090 7.6343 (8) 5.6073 (4) 9.5122 (7) 107.911 (7) 387.46 (6)
6.3020 7.5999 (7) 5.5911 (4) 9.4814 (7) 107.995 (7) 383.18 (5)
7.1790 7.5511 (7) 5.5626 (4) 9.4311 (7) 108.221 (8) 376.28 (6)
7.4800 7.5316 (7) 5.5530 (4) 9.4148 (8) 108.253 (8) 373.94 (6)
8.0010 7.5335 (8) 5.5545 (4) 9.4126 (9) 108.256 (9) 374.04 (6)
[Figure 1]
Figure 1
The relative change in unit-cell parameters versus pressure. Open squares, circles and triangles represent the a, b and c axes, respectively. Filled circles represent the β angle. The parameters at ambient pressure which were used for the normalization were a0 = 8.4860 (7), b0 = 6.0353 (6), c0 = 10.2175 (1) Å and β0 = 105.716 (6)°.
[Figure 2]
Figure 2
The pressure dependence of the unit-cell volume. The solid line represents a fit of the Vinet equation-of-state. The refined parameters V0, K0 and [K'_0] are 503 (2) Å3, 8.1 (6) GPa and 8.1 (4), respectively.

2.4. DFT calculations

Quantum chemical geometry optimizations were performed with the density functional method at the s-VWN level, as implemented in the Turbomole5.5 software (Alrichs et al., 1989[Alrichs, R., Bär, M., Häser, M., Horn, H. & Kölmel, C. (1989). Chem. Phys. Lett. 162, 165-169.]). Two models were used: one with a combination of larger basis sets (6-31g* for the lighter atoms hydrogen, carbon, nitrogen and oxygen, def-TZVPP for platinum, and TZVPP for all other atoms) and another with a combination of smaller basis sets [default in Turbomole 5.5; SV(P) for all atoms but hydrogen and ECP for platinum].

Results are given in Tables 3[link] and 4[link].

Table 3
Calculated energy differences for compounds existing as both cis and trans isomers found in the CSD

The first column is based on the larger basis set combination and the second on the smaller basis set combination (see §2[link]).

Compound EtransEcis (kJ mol−1) EtransEcis (kJ mol−1)
PtCl2(dms)2 −18.1 −19.7
PtCl2(py)2 −41.9 −41.9
PtCl2(MeCN)2 −19.5 −13.2
PtCl2(EtCN)2 −18.0 −10.3
PtCl2(PhCN)2 −16.2 2.4
PtCl2(NH2-cBu)2 −47.3 −46.3
PtCl2(tx)2 −17.2 −11.9
PtCl2(Ph2S)2 −1.3 13.5
PtCl2[S=C(OEt)(NMe2)]2 1.0 3.0
PtCl2(Pr2SO)2 15.8 15.8
PtCl2(PPh3)2 16.5 15.8
PtCl2(AsPh3)2 11.1 11.8

Table 4
Selected bond distances (Å), angles (°) and torsion angles (°) for trans-PtCl2(dms)2

`Crystal' is the observed geometry in the solid state, C2h is the structure optimized by DFT calculations with the larger basis set combination (see §2[link]) using the crystal data as starting parameters and Ci is similar to C2h but the torsion angles were fixed to those observed in the solid state. No symmetry constraints were used in the calculations.

  Crystal C2h Ci
Pt1—Cl1 2.289 (2) 2.300 2.300
Pt1—S1 2.3024 (19) 2.288 2.286
S1—C1 1.799 (10) 1.794 1.792
S1—C2 1.778 (9) 1.794 1.793
       
Cl1—Pt1—S1 87.54 (8) 88.7 88.2
C2—S1—C1 98.8 (5) 98.7 100.3
C2—S1—Pt1 108.6 (3) 104.3 106.7
C1—S1—Pt1 105.2 (4) 104.8 103.2
       
Cl1—Pt1—S1—C1 −59.3 (5) −51.7 −59.3
Cl1—Pt1—S1—C2 45.7 (4) 51.5 45.7

3. Results and discussion

The CSD was searched using the ConQuest software (Bruno et al., 2002[Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M., Macrae, C. F., McCabe, P., Pearson, J. & Taylor, R. (2002). Acta Cryst. B58, 389-397.]) for compounds belonging to the class of mononuclear complexes PtX2L2, where X is a halogen and L is a ligand with a donor atom belonging to groups 14, 15 or 16. Simple solvates are included but no chelates are included, and eight structures with no coordinates, obscure connectivity or disorder have been excluded. There are 156 cis complexes and 160 trans complexes (deposited material), which may be regarded as a fairly large data set, indicating that there is no preference for either of the two isomers in the solid state.

The next step in the analysis was to choose compounds in the CSD that are reported as both cis and trans isomers, optimize the geometries with DFT calculations, using the crystallographically observed geometry as the starting geometry, and compare the total energy of the optimized structures in the gas phase. We have found 12 compounds reported as both cis and trans complexes, and their energy differences are given in Table 3[link]. There is no clear-cut cis/trans division; of the 12 complexes the larger basis set combination has eight trans complexes as the favoured complex in the gas phase at 0 K, while the smaller basis set combination favours six trans complexes. The densities for trans- and cis-PtCl2(MeCN)2 are equal, while for all the others the trans compound has a larger density, which may indicate that the crystallization process may favour the trans compounds.

The title complex has a pseudo-square-planar geometry, SP-4–1 (Fig. 3[link]), with PtII on an inversion centre, thus conforming to the molecular point group Ci, which is the highest allowed for the complex in the space group observed (P21/n). Other possible point groups, C2h, C2v, C2 and Cs, do not conform to this space group. Relevant geometrical parameters from the crystal structure determination as well as two geometries in the gas phase optimized by DFT calculations are given in Table 4[link]. There is a very good agreement between observed and calculated (in the gas phase) bond distances and angles (maybe with the exception of the C—S—Pt angles). The Cl—Pt—S—C angles show the largest discrepancies, which is not surprising since packing effects should have a large influence on these angles. The calculated geometry is not only close to Ci but also very close to the highest symmetry possible for the complex, C2h. There are many energy minima in the conformational space, with energies fairly close to the minimum for the C2h conformation shown in Table 4[link]. A systematic study of the conformational space with starting parameters obeying Ci was performed changing the Cl—Pt—S—C torsion angles by 10° between each subsequent calculation. One minimum, with Cl—Pt—S—C angles of 10 and 115° for one-half of the molecule, is observed with an energy of only 2.3 kJ  mol−1 above the lowest C2h minimum. All calculations converged to either the lowest C2h or to this minimum. In conclusion the observed conformation in the solid state is not at either the anticipated global (C2h) or the local minimum, but slightly (5–7° for relevant torsion angles) off the global minimum. The energy difference between the lowest C2h minimum and the observed geometry in the solid state is probably very small; a DFT optimization calculation starting from the crystal structure parameters and keeping the Cl—Pt—S—C torsion angles fixed at the observed value resulted in an energy only 1.7 kJ mol−1 larger than the lowest C2h minimum (the larger basis set combination was used). It is evidently more advantageous to crystallize in P21/n, which allows close packing (Kitaigorodsky, 1973[Kitaigorodsky, A. I. (1973). Molecular Crystals and Molecules, ch. 1. New York/London: Academic Press.]), than in P2/m, which is required for the C2h point group.

[Figure 3]
Figure 3
The atomic numbering scheme for trans-PtCl2(dms)2. Displacement ellipsoids are shown at the 30% probability level.

A comparison of the Pt—Cl and Pt—S distances in the two isomers as observed in the crystal structures shows that the Pt—Cl distances are 0.028 (3) Å longer and the Pt—S distances are 0.031 (3) Å shorter in the cis complex (Horn et al., 1990[Horn, G. W., Kumar, R., Maverick, A. W., Fronczek, F. R. & Watkins, S. F. (1990). Acta Cryst. C46, 135-136.]). The differences are probably significant even when taking packing effects into account and show that sulfur has a larger trans influence than chlorine, which has been shown previously by Lövqvist (1996[Lövqvist, K. (1996). PhD thesis, Lund University, Sweden.]).

The packing of trans-PtCl2(dms)2 is shown in Fig. 4[link]. The PtII centre forms an I-centred monoclinic unit cell, but the other atoms break the I-centring, thus giving a primitive unit cell. The complexes are stacked along the b axis, with agostic interactions Pt⋯H of 3.08 and 3.31 Å. These rows may be regarded as forming layers in the bc plane, which feature a ring of six methyl groups with soft H⋯H interactions of 2.68 and 2.97 Å. The Pt—Cl bond in the two adjacent layers points slightly off the inversion centre of the ring, with a Cl⋯Cl distance of 4.037 (3) Å. The five close Cl⋯H interactions on each side of a layer are in the range 2.96–3.28 Å. Mulliken analysis of the crystallographically observed geometry and the larger basis set combination resulted in Pt = −0.6, S = 0.4, Cl = −0.2 and CH3 = 0.04 (the smaller basis-set combination gives Pt = −0.3, S = 0.2, Cl = −0.2 and CH3 = 0.12). It is thus reasonable to assume that electrostatic interactions contribute to stabilizing the packing arrangement as manifested in the synthon –Cl⋯(CH3)n⋯Cl–. Most PtII–Cl complexes in the CSD have Cl⋯Cl distances in the interval 3.8–3.9 Å (deposited material), and it is assumed that there are no Cl⋯Cl contacts at ambient pressure.

[Figure 4]
Figure 4
A stereoview of the packing arrangement of trans-PtCl2(dms)2.

The result of the high-pressure experiments is shown in Table 2[link] and in Figs. 1[link] and 2[link]. There is a decrease of cell volume by 26% with no phase transformation when the compound is exposed to pressures of up to 8.0 GPa. One way of describing the compression of a material is to estimate its bulk modulus by fitting an equation-of-state (EOS) to the unit-cell volume data. After first testing the Murnaghan (1937[Murnaghan, F. D. (1937). Am. J. Math. 49, 235-260.]) and Birch–Murnaghan (Birch, 1947[Birch, F. (1947). Phys. Rev. 71, 809-824.]) EOS, we found that the EOS of Vinet et al. (1986[Vinet, P., Ferrante, J., Smith, J. R. & Rose, J. H. (1986). J. Phys. C, 19, L467-L473.]), derived from cohesive energies in condensed systems, best describes the pV data. It can be expressed as

[p = 3K_0y^{-2/3}(1-y^{-1/3})\exp[3(K'_0-1)(1-y^{1/3})/2],]

where y = V/V0, and K0, [K'_0] and V0 are the bulk modulus, its pressure derivative and the unit-cell volume at ambient pressure, respectively. The parameters K0, [K'_0] and V0 were fitted to the unit-cell volume data using the software EOSFIT5.2 (Angel, 2001[Angel, R. J. (2001). High-Pressure, High-Temperature Crystal Chemistry, edited by R. M. Hazen & R. T. Downs, p. 35. Reviews in Mineralogy and Geochemistry, Vol. 41. Washington, DC: Mineralogical Society of America.]). The fitted bulk modulus, K0 = 8.1 (6) GPa, is consistent with highly compressible materials such as mol­ecular crystals. Comparable values are found for other mol­ecular crystalline materials, e.g. lithium- and potassium­cyclo­pentadienide (Dinnebier et al., 2005[Dinnebier, R. E., van Smaalen, S., Olbrich, F. & Carlson, S. (2005). Inorg. Chem. 44, 964-968.]), for which K0 was fitted to 8 and 5 GPa, respectively ([K'_0] = 7 and 11, respectively). The fitted pressure derivative for trans-PtCl2(dms)2 is [K'_0] = 8.1 (4) and describes a large curvature in the pV data. For minerals a [K'_0] value of around 4 is frequently found, but for `softer' materials, such as the cyclopentadienides mentioned above, higher values are common. Other examples are 4-(5-methyl-1,3,4-oxadiazole-2-yl)-N,N′-dimethylphenyl­amine (6.3 GPa and 6.8 for the bulk modulus and its pressure dependence, respectively) and 2,5-diphenyl-1,3,4-oxadiazole (7.3 GPa and 6.8; Franco et al., 2002[Franco, O., Reck, G., Orgzall, I. & Schulz, B. (2002). J. Phys. Chem. Solids, 63, 1805-1813.]). The volume decrease in the title compound shows the largest effect on the a axis, i.e. perpendicular to the layers, and about the same for the b and c parameters, i.e. within the layers. This result would be explained if the Cl atoms move towards the ring formed by the methyl groups, thus successively filling the void in the ring. Now the Cl atoms must slide beside each other resulting in the β angle increasing with pressure, which is also observed (Table 2[link]).

trans-PtCl2(dms)2 retains the molecular point group Ci rather than the other possibilities, C1, Cs, C2, C2v and C2h, in the solid state. In order to investigate if the retention of Ci in the solid state is a general feature for trans-PtX2L2 complexes, we have investigated the 160 compounds found in the CSD. The structural class (Belsky et al., 1995[Belsky, V. K., Zorkaya, O. N. & Zorky, P. M. (1995). Acta Cryst. A51, 473-481.]; Belsky & Zorkii, 1977[Belsky, V. K. & Zorkii, P. M. (1977). Acta Cryst. A33, 1004-1006.]) distribution for these compounds (deposited material) shows that the molecular symmetry Ci is retained in 78% of the structures (compared with 99% for structures in general in the CSD; Pidcock et al., 2003[Pidcock, E., Motherwell, W. D. S. & Cole, J. C. (2003). Acta Cryst. B59, 634-640.]), followed by C1 (16%), C2 (4%) and C2h (2%). More than 60% of the complexes have potential C2h molecular symmetry, but this symmetry is retained in only 2% of cases. Molecular symmetry C2h requires platinum in crystallographic point symmetry 2/m, which is found in space groups that hamper close packing (Kitaigorodsky, 1973[Kitaigorodsky, A. I. (1973). Molecular Crystals and Molecules, ch. 1. New York/London: Academic Press.]). Inversion centres thus seem to be especially favourable for crystal packing, as is also proposed by Brock & Dunitz (1994[Brock, C. P. & Dunitz, J. D. (1994). Chem. Mater. 6, 1118-1127.]).

In conclusion, there is no preference in frequency of either cis or trans isomers of PtX2L2 compounds in the CSD (2005 release). The molecular point group Ci is retained in the crystal for 78% of reported trans-PtX2L2 complexes, followed by C1 with 16%. The high-pressure investigation shows that the unit-cell volume is decreased by 26% up to 8.0 GPa without any phase transition.

Supporting information


Computing details top

Data collection: SMART (Bruker, 1995) for trans-PtCl2dms2; MAR CCD for tptcl2dms2_0.000GPa_publ, tptcl2dms2_0.137GPa_publ, tptcl2dms2_0.411GPa_publ, tptcl2dms2_0.849GPa_publ, tptcl2dms2_2.219GPa_publ, tptcl2dms2_3.041GPa_publ, tptcl2dms2_3.589GPa_publ, tptcl2dms2_4.274GPa_publ, tptcl2dms2_5.398GPa_publ, tptcl2dms2_5.809GPa_publ, tptcl2dms2_6.302GPa_publ, tptcl2dms2_7.179GPa_publ, tptcl2dms2_7.480GPa_publ, tptcl2dms2_8.001GPa_publ. Cell refinement: SAINT-Plus (Bruker, 1998) for trans-PtCl2dms2. Data reduction: SAINT-Plus (Bruker, 1998) for trans-PtCl2dms2; Fit2D for tptcl2dms2_0.000GPa_publ, tptcl2dms2_0.137GPa_publ, tptcl2dms2_0.411GPa_publ, tptcl2dms2_0.849GPa_publ, tptcl2dms2_2.219GPa_publ, tptcl2dms2_3.041GPa_publ, tptcl2dms2_3.589GPa_publ, tptcl2dms2_4.274GPa_publ, tptcl2dms2_5.398GPa_publ, tptcl2dms2_5.809GPa_publ, tptcl2dms2_6.302GPa_publ, tptcl2dms2_7.179GPa_publ, tptcl2dms2_7.480GPa_publ, tptcl2dms2_8.001GPa_publ. Program(s) used to solve structure: SHELXS ver 5.10 (Sheldrick, 1997) for trans-PtCl2dms2. Program(s) used to refine structure: SHELXL ver 5.10 (Sheldrick, 1997) for trans-PtCl2dms2; GSAS for tptcl2dms2_0.000GPa_publ, tptcl2dms2_0.137GPa_publ, tptcl2dms2_0.411GPa_publ, tptcl2dms2_0.849GPa_publ, tptcl2dms2_2.219GPa_publ, tptcl2dms2_3.041GPa_publ, tptcl2dms2_3.589GPa_publ, tptcl2dms2_4.274GPa_publ, tptcl2dms2_5.398GPa_publ, tptcl2dms2_5.809GPa_publ, tptcl2dms2_6.302GPa_publ, tptcl2dms2_7.179GPa_publ, tptcl2dms2_7.480GPa_publ, tptcl2dms2_8.001GPa_publ. Molecular graphics: DIAMOND (Brandenburg, 2000) for trans-PtCl2dms2.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
(trans-PtCl2dms2) trans-dichlorodi(dimethylsulfide)platinum(II) top
Crystal data top
C4H12Cl2PtS2F(000) = 360
Mr = 390.25Dx = 2.597 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.4637 (13) ÅCell parameters from 2881 reflections
b = 6.0176 (10) Åθ = 2.8–31.8°
c = 10.1812 (16) ŵ = 14.94 mm1
β = 105.747 (3)°T = 295 K
V = 499.08 (14) Å3Plate, yellow
Z = 20.28 × 0.12 × 0.06 mm
Data collection top
Bruker SMART CCD
diffractometer
1553 independent reflections
Radiation source: Rotating anode1018 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.081
ω–scansθmax = 31.8°, θmin = 2.8°
Absorption correction: empirical
SADABS (Sheldrick, 1996)
h = 1212
Tmin = 0.111, Tmax = 0.321k = 88
5797 measured reflectionsl = 1414
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)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.109H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2) + (0.060P)2]
where P = (Fo2 + 2Fc2)/3
1553 reflections(Δ/σ)max < 0.001
43 parametersΔρmax = 1.78 e Å3
0 restraintsΔρmin = 2.62 e Å3
Crystal data top
C4H12Cl2PtS2V = 499.08 (14) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nMo Kα radiation
a = 8.4637 (13) ŵ = 14.94 mm1
b = 6.0176 (10) ÅT = 295 K
c = 10.1812 (16) Å0.28 × 0.12 × 0.06 mm
β = 105.747 (3)°
Data collection top
Bruker SMART CCD
diffractometer
1553 independent reflections
Absorption correction: empirical
SADABS (Sheldrick, 1996)
1018 reflections with I > 2σ(I)
Tmin = 0.111, Tmax = 0.321Rint = 0.081
5797 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0460 restraints
wR(F2) = 0.109H-atom parameters constrained
S = 0.96Δρmax = 1.78 e Å3
1553 reflectionsΔρmin = 2.62 e Å3
43 parameters
Special details top

Experimental. DFT calculations were performed using the SVWN method and the basis sets def-TZVPP; ecp: def-ecp for platinum atoms, TZVPP for chlorine-, phosphorus- and sulfur atoms, and 6–31g* for carbon-, hydrogen- and nitrogen atoms.

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
xyzUiso*/Ueq
Pt10.00000.00000.00000.03065 (15)
S10.0931 (3)0.1946 (3)0.20090 (19)0.0383 (4)
Cl10.2561 (3)0.0429 (4)0.0311 (3)0.0474 (5)
C20.0294 (15)0.0530 (14)0.3311 (10)0.049 (2)
H2A0.09160.08150.35470.074*
H2B0.08520.01760.29880.074*
H2C0.04740.14650.41020.074*
C10.0389 (17)0.4335 (16)0.1828 (10)0.062 (3)
H1A0.01920.53020.11390.093*
H1B0.01640.51150.26810.093*
H1C0.15140.38620.15670.093*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.0341 (2)0.0336 (2)0.0264 (2)0.00096 (18)0.01192 (15)0.00056 (17)
S10.0429 (11)0.0435 (10)0.0303 (9)0.0012 (9)0.0132 (7)0.0040 (8)
Cl10.0384 (11)0.0656 (14)0.0431 (12)0.0050 (9)0.0196 (9)0.0057 (9)
C20.075 (7)0.046 (5)0.030 (4)0.004 (4)0.021 (4)0.009 (3)
C10.099 (10)0.044 (4)0.043 (6)0.023 (6)0.020 (6)0.003 (4)
Geometric parameters (Å, º) top
Pt1—Cl12.289 (2)C2—H2A0.9600
Pt1—Cl1i2.289 (2)C2—H2B0.9600
Pt1—S12.3024 (19)C2—H2C0.9600
Pt1—S1i2.3024 (19)C1—H1A0.9600
S1—C21.778 (9)C1—H1B0.9600
S1—C11.799 (10)C1—H1C0.9600
Cl1—Pt1—Cl1i180.00 (11)H2A—C2—H2B109.5
Cl1—Pt1—S187.54 (8)S1—C2—H2C109.5
Cl1i—Pt1—S192.46 (8)H2A—C2—H2C109.5
Cl1—Pt1—S1i92.46 (8)H2B—C2—H2C109.5
Cl1i—Pt1—S1i87.54 (8)S1—C1—H1A109.5
S1—Pt1—S1i180.0S1—C1—H1B109.5
C2—S1—C198.8 (5)H1A—C1—H1B109.5
C2—S1—Pt1108.6 (3)S1—C1—H1C109.5
C1—S1—Pt1105.2 (4)H1A—C1—H1C109.5
S1—C2—H2A109.5H1B—C1—H1C109.5
S1—C2—H2B109.5
Symmetry code: (i) x, y, z.
(tptcl2dms2_0.000GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 503.73 (5) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 10.2175 (8) ÅT = 295 K
b = 6.0353 (6) ÅYellow
c = 8.4860 (7) Åcylinder, 0.3 × 0.3 mm
β = 105.716 (6)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 24.053 #4(LX) = 0.487 #5(LY) = 56.657 #6(trns) = 0.000 #7(asym) = -0.0241 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0155 parameters
Rwp = 0.0250 restraints
Rexp = 0.008(Δ/σ)max = 0.04
χ2 = 10.433Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 14914.7 2: -4489.36 3: 1998.02 4: -1301.99 5: -184.871 6: 391.248 7: -476.595 8: 134.606 9: 101.756 10: -103.360 11: 243.570 12: -11.4511
1453 data points
Crystal data top
C4H12Cl2PtS2β = 105.716 (6)°
Mr = 390.25V = 503.73 (5) Å3
Monoclinic, P21/nZ = 2
a = 10.2175 (8) ÅSynchrotron radiation, λ = 0.9249 Å
b = 6.0353 (6) ÅT = 295 K
c = 8.4860 (7) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0151453 data points
Rwp = 0.0255 parameters
Rexp = 0.0080 restraints
χ2 = 10.433
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_0.137GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 493.40 (7) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 8.4070 (6) ÅT = 295 K
b = 6.0038 (5) ÅYellow
c = 10.1607 (9) Åcylinder, 0.3 × 0.3 mm
β = 105.829 (7)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 23.330 #4(LX) = 4.199 #5(LY) = 17.907 #6(trns) = 0.000 #7(asym) = 0.0558 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0149 parameters
Rwp = 0.0230 restraints
Rexp = 0.007(Δ/σ)max = 0.12
χ2 = 9.986Background function: GSAS Background function number 1 with 14 terms. Shifted Chebyshev function of 1st kind 1: 17544.3 2: -1723.37 3: 3594.87 4: -1070.73 5: -882.421 6: 72.8259 7: -815.020 8: 417.042 9: 266.055 10: -207.867 11: 290.725 12: -123.815 13: 146.183 14: 0.923252
1453 data points
Crystal data top
C4H12Cl2PtS2β = 105.829 (7)°
Mr = 390.25V = 493.40 (7) Å3
Monoclinic, P21/nZ = 2
a = 8.4070 (6) ÅSynchrotron radiation, λ = 0.9249 Å
b = 6.0038 (5) ÅT = 295 K
c = 10.1607 (9) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0141453 data points
Rwp = 0.0239 parameters
Rexp = 0.0070 restraints
χ2 = 9.986(Δ/σ)max = 0.12
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_0.411GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 481.76 (10) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 8.3155 (9) ÅT = 295 K
b = 5.9607 (8) ÅYellow
c = 10.1123 (13) Åcylinder, 0.3 × 0.3 mm
β = 106.021 (11)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 15.399 #4(LX) = 7.895 #5(LY) = 10.692 #6(trns) = 0.000 #7(asym) = 0.0880 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0199 parameters
Rwp = 0.0330 restraints
Rexp = 0.007(Δ/σ)max = 0.07
χ2 = 21.437Background function: GSAS Background function number 1 with 14 terms. Shifted Chebyshev function of 1st kind 1: 17544.3 2: -1723.37 3: 3594.87 4: -1070.73 5: -882.421 6: 72.8259 7: -815.020 8: 417.042 9: 266.055 10: -207.867 11: 290.725 12: -123.815 13: 146.183 14: 0.923252
1453 data points
Crystal data top
C4H12Cl2PtS2β = 106.021 (11)°
Mr = 390.25V = 481.76 (10) Å3
Monoclinic, P21/nZ = 2
a = 8.3155 (9) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.9607 (8) ÅT = 295 K
c = 10.1123 (13) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0191453 data points
Rwp = 0.0339 parameters
Rexp = 0.0070 restraints
χ2 = 21.437
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_0.849GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 464.47 (9) Å3
Mr = 390.25Z = 2
Monoclinic, P21/n? radiation, λ = 0.9249 Å
a = 8.1889 (8) ÅT = 295 K
b = 5.9050 (6) ÅYellow
c = 10.0100 (11) Åcylinder, 0.3 × 0.3 mm
β = 106.349 (8)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 14.252 #4(LX) = 3.577 #5(LY) = 42.720 #6(trns) = 0.000 #7(asym) = -0.2305 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0209 parameters
Rwp = 0.0290 restraints
Rexp = 0.008(Δ/σ)max = 0.24
χ2 = 14.213Background function: GSAS Background function number 1 with 12 terms. Shifted Chebyshev function of 1st kind 1: 14702.2 2: -801.697 3: 3033.11 4: -769.432 5: -814.527 6: 65.9191 7: -760.341 8: 398.713 9: 232.968 10: -208.985 11: 365.053 12: -108.993
1453 data points
Crystal data top
C4H12Cl2PtS2β = 106.349 (8)°
Mr = 390.25V = 464.47 (9) Å3
Monoclinic, P21/nZ = 2
a = 8.1889 (8) Å? radiation, λ = 0.9249 Å
b = 5.9050 (6) ÅT = 295 K
c = 10.0100 (11) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0201453 data points
Rwp = 0.0299 parameters
Rexp = 0.0080 restraints
χ2 = 14.213(Δ/σ)max = 0.24
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_2.219GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 433.28 (10) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.9633 (13) ÅT = 295 K
b = 5.7915 (8) ÅYellow
c = 9.8203 (12) Åcylinder, 0.3 × 0.3 mm
β = 106.933 (10)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 22.272 #4(LX) = 1.268 #5(LY) = 54.449 #6(trns) = 0.000 #7(asym) = -0.0107 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0239 parameters
Rwp = 0.0350 restraints
Rexp = 0.008(Δ/σ)max = 0.07
χ2 = 22.468Background function: GSAS Background function number 1 with 14 terms. Shifted Chebyshev function of 1st kind 1: 16323.8 2: -1179.26 3: 3230.77 4: -835.427 5: -520.062 6: -239.890 7: -684.504 8: 433.192 9: 239.561 10: -183.214 11: 133.121 12: -298.543 13: 184.337 14: 74.8771
1453 data points
Crystal data top
C4H12Cl2PtS2β = 106.933 (10)°
Mr = 390.25V = 433.28 (10) Å3
Monoclinic, P21/nZ = 2
a = 7.9633 (13) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.7915 (8) ÅT = 295 K
c = 9.8203 (12) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0231453 data points
Rwp = 0.0359 parameters
Rexp = 0.0080 restraints
χ2 = 22.468
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_3.041GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 419.83 (9) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.8667 (12) ÅT = 295 K
b = 5.7418 (7) ÅYellow
c = 9.7349 (11) Åcylinder, 0.3 × 0.3 mm
β = 107.299 (9)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 21.987 #4(LX) = 2.301 #5(LY) = 49.132 #6(trns) = 0.000 #7(asym) = -0.1328 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0219 parameters
Rwp = 0.0340 restraints
Rexp = 0.008(Δ/σ)max = 0.06
χ2 = 19.981Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 15919.1 2: -813.040 3: 3165.85 4: -910.777 5: -552.463 6: -27.2954 7: -689.474 8: 166.274 9: 237.419 10: -160.846
1453 data points
Crystal data top
C4H12Cl2PtS2β = 107.299 (9)°
Mr = 390.25V = 419.83 (9) Å3
Monoclinic, P21/nZ = 2
a = 7.8667 (12) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.7418 (7) ÅT = 295 K
c = 9.7349 (11) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0211453 data points
Rwp = 0.0349 parameters
Rexp = 0.0080 restraints
χ2 = 19.981
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_3.589GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 411.74 (5) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.8065 (7) ÅT = 295 K
b = 5.7061 (4) ÅYellow
c = 9.6871 (7) Åcylinder, 0.3 × 0.3 mm
β = 107.409 (6)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 25.814 #4(LX) = 4.707 #5(LY) = 21.572 #6(trns) = 0.000 #7(asym) = 0.0246 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0139 parameters
Rwp = 0.0210 restraints
Rexp = 0.007(Δ/σ)max = 0.06
χ2 = 9.610Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 19104.8 2: -1183.62 3: 3807.35 4: -1198.99 5: -644.656 6: 35.5141 7: -756.546 8: 393.985 9: 348.089 10: -264.405
1453 data points
Crystal data top
C4H12Cl2PtS2β = 107.409 (6)°
Mr = 390.25V = 411.74 (5) Å3
Monoclinic, P21/nZ = 2
a = 7.8065 (7) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.7061 (4) ÅT = 295 K
c = 9.6871 (7) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0131453 data points
Rwp = 0.0219 parameters
Rexp = 0.0070 restraints
χ2 = 9.610
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_4.274GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 403.08 (6) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.7447 (7) ÅT = 295 K
b = 5.6735 (5) ÅYellow
c = 9.6219 (7) Åcylinder, 0.3 × 0.3 mm
β = 107.559 (7)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 25.503 #4(LX) = 5.080 #5(LY) = 20.012 #6(trns) = 0.000 #7(asym) = 0.0382 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0149 parameters
Rwp = 0.0220 restraints
Rexp = 0.007(Δ/σ)max = 0.06
χ2 = 10.176Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 18695.6 2: -936.709 3: 3634.68 4: -1186.61 5: -530.824 6: -2.11428 7: -737.818 8: 354.038 9: 317.528 10: -249.133
1453 data points
Crystal data top
C4H12Cl2PtS2β = 107.559 (7)°
Mr = 390.25V = 403.08 (6) Å3
Monoclinic, P21/nZ = 2
a = 7.7447 (7) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.6735 (5) ÅT = 295 K
c = 9.6219 (7) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0141453 data points
Rwp = 0.0229 parameters
Rexp = 0.0070 restraints
χ2 = 10.176
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_5.398GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 391.48 (5) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.6626 (7) ÅT = 295 K
b = 5.6223 (4) ÅYellow
c = 9.5448 (7) Åcylinder, 0.3 × 0.3 mm
β = 107.815 (7)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 24.891 #4(LX) = 4.098 #5(LY) = 34.644 #6(trns) = 0.000 #7(asym) = 0.0595 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0139 parameters
Rwp = 0.0200 restraints
Rexp = 0.007(Δ/σ)max = 0.05
χ2 = 9.486Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 21383.8 2: -846.217 3: 3860.94 4: -1378.03 5: -455.919 6: 175.649 7: -722.233 8: 591.181 9: 466.361 10: -394.047
1453 data points
Crystal data top
C4H12Cl2PtS2β = 107.815 (7)°
Mr = 390.25V = 391.48 (5) Å3
Monoclinic, P21/nZ = 2
a = 7.6626 (7) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.6223 (4) ÅT = 295 K
c = 9.5448 (7) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0131453 data points
Rwp = 0.0209 parameters
Rexp = 0.0070 restraints
χ2 = 9.486
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_5.809GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 387.46 (6) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.6343 (8) ÅT = 295 K
b = 5.6073 (4) ÅYellow
c = 9.5122 (7) Åcylinder, 0.3 × 0.3 mm
β = 107.911 (7)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 29.610 #4(LX) = 3.214 #5(LY) = 43.460 #6(trns) = 0.000 #7(asym) = -0.0803 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0129 parameters
Rwp = 0.0190 restraints
Rexp = 0.006(Δ/σ)max = 0.08
χ2 = 9.120Background function: GSAS Background function number 1 with 14 terms. Shifted Chebyshev function of 1st kind 1: 22761.4 2: -777.612 3: 4108.43 4: -1587.94 5: -695.207 6: 75.6433 7: -824.620 8: 536.946 9: 487.648 10: -266.760 11: 327.023 12: 39.5019 13: 374.400 14: 222.108
1453 data points
Crystal data top
C4H12Cl2PtS2β = 107.911 (7)°
Mr = 390.25V = 387.46 (6) Å3
Monoclinic, P21/nZ = 2
a = 7.6343 (8) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.6073 (4) ÅT = 295 K
c = 9.5122 (7) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0121453 data points
Rwp = 0.0199 parameters
Rexp = 0.0060 restraints
χ2 = 9.120
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_6.302GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 383.18 (5) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.5999 (7) ÅT = 295 K
b = 5.5911 (4) ÅYellow
c = 9.4814 (7) Åcylinder, 0.3 × 0.3 mm
β = 107.995 (7)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 26.913 #4(LX) = 3.275 #5(LY) = 52.810 #6(trns) = 0.000 #7(asym) = -0.2437 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0119 parameters
Rwp = 0.0170 restraints
Rexp = 0.006(Δ/σ)max = 0.06
χ2 = 7.236Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 23304.8 2: -907.157 3: 4089.03 4: -1772.91 5: -594.810 6: -22.0385 7: -882.801 8: 285.606 9: 403.010 10: -356.673
1453 data points
Crystal data top
C4H12Cl2PtS2β = 107.995 (7)°
Mr = 390.25V = 383.18 (5) Å3
Monoclinic, P21/nZ = 2
a = 7.5999 (7) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.5911 (4) ÅT = 295 K
c = 9.4814 (7) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0111453 data points
Rwp = 0.0179 parameters
Rexp = 0.0060 restraints
χ2 = 7.236
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_7.179GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 376.28 (5) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.5511 (7) ÅT = 295 K
b = 5.5626 (4) ÅYellow
c = 9.4311 (7) Åcylinder, 0.3 × 0.3 mm
β = 108.221 (8)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 33.250 #4(LX) = 4.192 #5(LY) = 59.953 #6(trns) = 0.000 #7(asym) = 0.1116 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0099 parameters
Rwp = 0.0140 restraints
Rexp = 0.006(Δ/σ)max = 0.08
χ2 = 4.973Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 22977.7 2: -820.928 3: 3784.06 4: -1768.46 5: -549.023 6: 7.12432 7: -703.674 8: 431.695 9: 479.986 10: -322.118
1453 data points
Crystal data top
C4H12Cl2PtS2β = 108.221 (8)°
Mr = 390.25V = 376.28 (5) Å3
Monoclinic, P21/nZ = 2
a = 7.5511 (7) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.5626 (4) ÅT = 295 K
c = 9.4311 (7) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0091453 data points
Rwp = 0.0149 parameters
Rexp = 0.0060 restraints
χ2 = 4.973
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_7.480GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 373.94 (6) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.5316 (7) ÅT = 295 K
b = 5.5530 (4) ÅYellow
c = 9.4148 (8) Åcylinder, 0.3 × 0.3 mm
β = 108.253 (8)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 39.954 #4(LX) = 1.913 #5(LY) = 80.740 #6(trns) = 0.000 #7(asym) = 0.2152 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0099 parameters
Rwp = 0.0130 restraints
Rexp = 0.006(Δ/σ)max = 0.08
χ2 = 4.162Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 22401.3 2: -720.024 3: 3582.51 4: -1760.75 5: -700.758 6: 102.978 7: -902.042 8: 299.650 9: 317.562 10: -317.216
1453 data points
Crystal data top
C4H12Cl2PtS2β = 108.253 (8)°
Mr = 390.25V = 373.94 (6) Å3
Monoclinic, P21/nZ = 2
a = 7.5316 (7) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.5530 (4) ÅT = 295 K
c = 9.4148 (8) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0091453 data points
Rwp = 0.0139 parameters
Rexp = 0.0060 restraints
χ2 = 4.162
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*
(tptcl2dms2_8.001GPa_publ) trans-bis(dimethyl sulfide)platinum dichloride. top
Crystal data top
C4H12Cl2PtS2V = 374.05 (6) Å3
Mr = 390.25Z = 2
Monoclinic, P21/nSynchrotron radiation, λ = 0.9249 Å
a = 7.5335 (8) ÅT = 295 K
b = 5.5545 (4) ÅYellow
c = 9.4126 (9) Åcylinder, 0.3 × 0.3 mm
β = 108.256 (9)°Specimen preparation: Prepared at 295 K
Data collection top
MAR Desktop Beamline
diffractometer
Specimen mounting: diamond-anvil cell
Radiation source: Synchrotron, MAX-lab bemline I711Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 32.510 #4(LX) = 4.215 #5(LY) = 74.050 #6(trns) = 0.000 #7(asym) = 0.1757 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0040 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.0119 parameters
Rwp = 0.0150 restraints
Rexp = 0.006(Δ/σ)max = 0.08
χ2 = 5.712Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 22926.2 2: -573.762 3: 3936.17 4: -1756.64 5: -589.832 6: 17.5958 7: -634.628 8: 250.588 9: 507.526 10: -322.147
1453 data points
Crystal data top
C4H12Cl2PtS2β = 108.256 (9)°
Mr = 390.25V = 374.05 (6) Å3
Monoclinic, P21/nZ = 2
a = 7.5335 (8) ÅSynchrotron radiation, λ = 0.9249 Å
b = 5.5545 (4) ÅT = 295 K
c = 9.4126 (9) Åcylinder, 0.3 × 0.3 mm
Data collection top
MAR Desktop Beamline
diffractometer
Data collection mode: transmission
Specimen mounting: diamond-anvil cellScan method: Stationary detector
Refinement top
Rp = 0.0111453 data points
Rwp = 0.0159 parameters
Rexp = 0.0060 restraints
χ2 = 5.712
Special details top

Experimental. High-pressure measurement at ambient pressure in diamond-anvil cell

Refinement. Profile refinement, Lebail type, was performed to obtain unit-cell dimensions.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
PT10.10.20.30.025*

Experimental details

(trans-PtCl2dms2)(tptcl2dms2_0.000GPa_publ)(tptcl2dms2_0.137GPa_publ)(tptcl2dms2_0.411GPa_publ)
Crystal data
Chemical formulaC4H12Cl2PtS2C4H12Cl2PtS2C4H12Cl2PtS2C4H12Cl2PtS2
Mr390.25390.25390.25390.25
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)295295295295
a, b, c (Å)8.4637 (13), 6.0176 (10), 10.1812 (16)10.2175 (8), 6.0353 (6), 8.4860 (7)8.4070 (6), 6.0038 (5), 10.1607 (9)8.3155 (9), 5.9607 (8), 10.1123 (13)
α, β, γ (°)90, 105.747 (3), 9090, 105.716 (6), 9090, 105.829 (7), 9090, 106.021 (11), 90
V3)499.08 (14)503.73 (5)493.40 (7)481.76 (10)
Z2222
Radiation typeMo KαSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 Å
µ (mm1)14.94???
Specimen shape, size (mm)0.28 × 0.12 × 0.06Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3
Data collection
DiffractometerBruker SMART CCD
diffractometer
MAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
Specimen mountingDiamond-anvil cellDiamond-anvil cellDiamond-anvil cell
Data collection modeTransmissionTransmissionTransmission
Data collection methodω–scansStationary detectorStationary detectorStationary detector
Absorption correctionEmpirical
SADABS (Sheldrick, 1996)
Tmin, Tmax0.111, 0.321
No. of measured, independent and
observed [I > 2σ(I)] reflections
5797, 1553, 1018
Rint0.081
θ values (°)θmax = 31.8, θmin = 2.82θfixed = ?2θfixed = ?2θfixed = ?
(sin θ/λ)max1)0.740
Refinement
R factors and goodness of fitR[F2 > 2σ(F2)] = 0.046, wR(F2) = 0.109, S = 0.96Rp = 0.015, Rwp = 0.025, Rexp = 0.008, χ2 = 10.433Rp = 0.014, Rwp = 0.023, Rexp = 0.007, χ2 = 9.986Rp = 0.019, Rwp = 0.033, Rexp = 0.007, χ2 = 21.437
No. of reflections/data points1553145314531453
No. of parameters43599
H-atom treatmentH-atom parameters constrained???
(Δ/σ)max< 0.0010.040.120.07
Δρmax, Δρmin (e Å3)1.78, 2.62


(tptcl2dms2_0.849GPa_publ)(tptcl2dms2_2.219GPa_publ)(tptcl2dms2_3.041GPa_publ)(tptcl2dms2_3.589GPa_publ)
Crystal data
Chemical formulaC4H12Cl2PtS2C4H12Cl2PtS2C4H12Cl2PtS2C4H12Cl2PtS2
Mr390.25390.25390.25390.25
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)295295295295
a, b, c (Å)8.1889 (8), 5.9050 (6), 10.0100 (11)7.9633 (13), 5.7915 (8), 9.8203 (12)7.8667 (12), 5.7418 (7), 9.7349 (11)7.8065 (7), 5.7061 (4), 9.6871 (7)
α, β, γ (°)90, 106.349 (8), 9090, 106.933 (10), 9090, 107.299 (9), 9090, 107.409 (6), 90
V3)464.47 (9)433.28 (10)419.83 (9)411.74 (5)
Z2222
Radiation type?, λ = 0.9249 ÅSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 Å
µ (mm1)????
Specimen shape, size (mm)Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3
Data collection
DiffractometerMAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
Specimen mountingDiamond-anvil cellDiamond-anvil cellDiamond-anvil cellDiamond-anvil cell
Data collection modeTransmissionTransmissionTransmissionTransmission
Data collection methodStationary detectorStationary detectorStationary detectorStationary detector
Absorption correction
Tmin, Tmax
No. of measured, independent and
observed [I > 2σ(I)] reflections
Rint
θ values (°)2θfixed = ?2θfixed = ?2θfixed = ?2θfixed = ?
(sin θ/λ)max1)
Refinement
R factors and goodness of fitRp = 0.020, Rwp = 0.029, Rexp = 0.008, χ2 = 14.213Rp = 0.023, Rwp = 0.035, Rexp = 0.008, χ2 = 22.468Rp = 0.021, Rwp = 0.034, Rexp = 0.008, χ2 = 19.981Rp = 0.013, Rwp = 0.021, Rexp = 0.007, χ2 = 9.610
No. of reflections/data points1453145314531453
No. of parameters9999
H-atom treatment????
(Δ/σ)max0.240.070.060.06
Δρmax, Δρmin (e Å3)


(tptcl2dms2_4.274GPa_publ)(tptcl2dms2_5.398GPa_publ)(tptcl2dms2_5.809GPa_publ)(tptcl2dms2_6.302GPa_publ)
Crystal data
Chemical formulaC4H12Cl2PtS2C4H12Cl2PtS2C4H12Cl2PtS2C4H12Cl2PtS2
Mr390.25390.25390.25390.25
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)295295295295
a, b, c (Å)7.7447 (7), 5.6735 (5), 9.6219 (7)7.6626 (7), 5.6223 (4), 9.5448 (7)7.6343 (8), 5.6073 (4), 9.5122 (7)7.5999 (7), 5.5911 (4), 9.4814 (7)
α, β, γ (°)90, 107.559 (7), 9090, 107.815 (7), 9090, 107.911 (7), 9090, 107.995 (7), 90
V3)403.08 (6)391.48 (5)387.46 (6)383.18 (5)
Z2222
Radiation typeSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 Å
µ (mm1)????
Specimen shape, size (mm)Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3
Data collection
DiffractometerMAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
Specimen mountingDiamond-anvil cellDiamond-anvil cellDiamond-anvil cellDiamond-anvil cell
Data collection modeTransmissionTransmissionTransmissionTransmission
Data collection methodStationary detectorStationary detectorStationary detectorStationary detector
Absorption correction
Tmin, Tmax
No. of measured, independent and
observed [I > 2σ(I)] reflections
Rint
θ values (°)2θfixed = ?2θfixed = ?2θfixed = ?2θfixed = ?
(sin θ/λ)max1)
Refinement
R factors and goodness of fitRp = 0.014, Rwp = 0.022, Rexp = 0.007, χ2 = 10.176Rp = 0.013, Rwp = 0.020, Rexp = 0.007, χ2 = 9.486Rp = 0.012, Rwp = 0.019, Rexp = 0.006, χ2 = 9.120Rp = 0.011, Rwp = 0.017, Rexp = 0.006, χ2 = 7.236
No. of reflections/data points1453145314531453
No. of parameters9999
H-atom treatment????
(Δ/σ)max0.060.050.080.06
Δρmax, Δρmin (e Å3)


(tptcl2dms2_7.179GPa_publ)(tptcl2dms2_7.480GPa_publ)(tptcl2dms2_8.001GPa_publ)
Crystal data
Chemical formulaC4H12Cl2PtS2C4H12Cl2PtS2C4H12Cl2PtS2
Mr390.25390.25390.25
Crystal system, space groupMonoclinic, P21/nMonoclinic, P21/nMonoclinic, P21/n
Temperature (K)295295295
a, b, c (Å)7.5511 (7), 5.5626 (4), 9.4311 (7)7.5316 (7), 5.5530 (4), 9.4148 (8)7.5335 (8), 5.5545 (4), 9.4126 (9)
α, β, γ (°)90, 108.221 (8), 9090, 108.253 (8), 9090, 108.256 (9), 90
V3)376.28 (5)373.94 (6)374.05 (6)
Z222
Radiation typeSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 ÅSynchrotron, λ = 0.9249 Å
µ (mm1)???
Specimen shape, size (mm)Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3Cylinder, 0.3 × 0.3
Data collection
DiffractometerMAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
MAR Desktop Beamline
diffractometer
Specimen mountingDiamond-anvil cellDiamond-anvil cellDiamond-anvil cell
Data collection modeTransmissionTransmissionTransmission
Data collection methodStationary detectorStationary detectorStationary detector
Absorption correction
Tmin, Tmax
No. of measured, independent and
observed [I > 2σ(I)] reflections
Rint
θ values (°)2θfixed = ?2θfixed = ?2θfixed = ?
(sin θ/λ)max1)
Refinement
R factors and goodness of fitRp = 0.009, Rwp = 0.014, Rexp = 0.006, χ2 = 4.973Rp = 0.009, Rwp = 0.013, Rexp = 0.006, χ2 = 4.162Rp = 0.011, Rwp = 0.015, Rexp = 0.006, χ2 = 5.712
No. of reflections/data points145314531453
No. of parameters999
H-atom treatment???
(Δ/σ)max0.080.080.08
Δρmax, Δρmin (e Å3)

Computer programs: SMART (Bruker, 1995), MAR CCD, SAINT-Plus (Bruker, 1998), Fit2D, SHELXS ver 5.10 (Sheldrick, 1997), SHELXL ver 5.10 (Sheldrick, 1997), GSAS, DIAMOND (Brandenburg, 2000).

 

Footnotes

Current address: MAX-laboratory, Box 118, SE-221 00 Lund, Sweden.

§Current address: Solid State Analysis, AstraZeneca R&D Mölndal, SE-431 83 Mölndal, Sweden.

On leave from Zhongshan University, Guangzhou, People's Republic of China.

1Supplementary data for this paper are available from the IUCr electronic archives (Reference: RY5001 ). Services for accessing these data are described at the back of the journal.

Acknowledgements

Financial assistance from the Crafoord Foundation, the Swedish Research Council and Lund University for a scholarship to SY is gratefully acknowledged. MAX-laboratory and Yngve Cerenius are acknowledged for the allocated beam time and technical support.

References

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