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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoIUCrDATA
ISSN: 2414-3146
Volume 1| Part 5| May 2016| x160696
doi:10.1107/S2414314616006969

Bis­(penta­fluoro­benzene­thiol­ato-κS){(penta­fluoro­phen­yl)phenyl­[3,4,5,6-tetra­fluoro-2-(penta­fluoro­phenyl­sulfanyl)phen­yl]phosphane-κ2P,S}platinum(II) di­chloro­methane hemisolvate

Sylvain Bernèsa* and Hugo Torrensb

aInstituto de Física, Universidad Autónoma de Puebla, Av. San Claudio y 18 Sur, 72570 Puebla, Pue., Mexico, and bFacultad de Química, Universidad Nacional Autónoma de México, Ciudad Universitaria, 04510 México D.F., Mexico
*Correspondence e-mail: sylvain_bernes@hotmail.com

Edited by K. Fejfarova, Institute of Biotechnology CAS, Czech Republic (Received 12 April 2016; accepted 25 April 2016; online 4 May 2016)

In the title compound, [Pt(C6F5S)2(C24H5F14PS)]·0.5CH2Cl2, the complex features a square-planar PtII atom coordinated by two thiol­ate ligands and one chelating bidentate P/S ligand, forming a five-membered metallacycle. The monodentate SC6F5 ligands give a weak parallel displaced π–π inter­action. In the chelating ligand, the geometry for both S and P donor atoms is consistent with sp3 hybridization. The complex conformation is identical to that previously described for the compound bearing 2,3,5,6-tetra­fluoro­phenyl­thiol­ate in place of penta­fluoro­phenyl­thiol­ate groups. The lattice solvent, CH2Cl2, is disordered over inversion centers in P-1, affording a hemisolvate.

CCDC reference: 1476213

3D view (loading...)
[Scheme 3D1]
Chemical scheme
[Scheme 1]

Structure description

The title complex, [Pt(SC6F5)2(1,2-C6F4(SC6F5)(PPh(C6F5)))] (Fig. 1[link]), is a product resulting from the C—F bond activation of [Pt2(μ-SC6F5)2(SC6F5)2(PPh(C6F5)2)2]. The chemistry has been described for this compound and for other related compounds with different fluorinated thiol­ate groups and phosphanes (Villanueva et al., 2004[Villanueva, L., Arroyo, M., Bernès, S. & Torrens, H. (2004). Chem. Commun. pp. 1942-1943.]; Bernès et al., 2016[Bernès, S., Meléndez, F. J. & Torrens, H. (2016). Acta Cryst. C72, 268-273.]).

[Figure 1]
Figure 1
The structure of the title compound, with displacement ellipsoids for non-H atoms at the 20% probability level. Labels for F atoms (green ellipsoids) are identical to those of the C atom to which they are bonded.

The PtII center is coordinated by two cis thiol­ates and one chelating bidentate ligand, giving a square-planar coordination geometry. The thiol­ates have their C6F5 rings almost parallel, giving a parallel displaced π–π inter­action; the angle between rings is 4.8 (4)°, and the distance between ring centroids is 4.322 (6) Å. One C6F5 ring is affected by libration, clearly visible on C3—F3, C4—F4 and C5—F5 groups (see Fig. 1[link]). The chelate ring coordinates via P and S donors, at normal distances [Pt1—P1 = 2.2315 (11) Å; Pt1—S3 = 2.2757 (12) Å, shorter than Pt—Sthiol­ate bond lengths]. Both S and P atoms are tetra­hedrally hybridized, assuming that one lone pair is present on S3. Angles around P1 are in the range 104.1 (2)–116.75 (15)°, while bond angles around S3 are in the range 102.4 (2)–109.13 (17)°. The complex conformation is identical to that previously described for the compound bearing 2,3,5,6-tetra­fluoro­phenyl­thiol­ate in place of penta­fluoro­phenyl­thiol­ate groups (Villanueva et al., 2004[Villanueva, L., Arroyo, M., Bernès, S. & Torrens, H. (2004). Chem. Commun. pp. 1942-1943.]).

The complex crystallized with di­chloro­methane as a lattice solvent. The mol­ecule is located close to the inversion centers of the triclinic cell, and its occupancy was then fixed to 1/2. As the main complex is in a general position, the chemical composition thus corresponds to a hemisolvate.

Synthesis and crystallization

The synthesis and crystallization of this complex is similar to that described for [Pt(SC6F4H)2(1,2-C6F4(SC6F4H)(PPh(C6F5)))] in: Villanueva et al. (2004[Villanueva, L., Arroyo, M., Bernès, S. & Torrens, H. (2004). Chem. Commun. pp. 1942-1943.]).

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1[link]. A free refinement of the occupancy for di­chloro­methane C37/Cl1/Cl2 converged to 0.47. In the final cycles, this parameter was fixed to 1/2.

Table 1
Experimental details

Crystal data
Chemical formula [Pt(C6F5S)2(C24H5F14PS)]·0.5CH2Cl2
Mr 1258.10
Crystal system, space group Triclinic, P[\overline{1}]
Temperature (K) 296
a, b, c (Å) 11.2908 (10), 13.8516 (14), 14.6956 (17)
α, β, γ (°) 104.477 (8), 96.359 (8), 111.675 (7)
V (Å3) 2014.6 (4)
Z 2
Radiation type Mo Kα
μ (mm−1) 3.89
Crystal size (mm) 0.65 × 0.40 × 0.24
 
Data collection
Diffractometer Bruker P4
Absorption correction ψ scan (XSCANS; Bruker, 1997[Bruker (1997). XSCANS. Bruker AXS Inc., Madison, Wisconsin, USA.])
Tmin, Tmax 0.521, 0.897
No. of measured, independent and observed [I > 2σ(I)] reflections 15487, 9078, 7392
Rint 0.036
(sin θ/λ)max (Å−1) 0.650
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.089, 1.02
No. of reflections 9078
No. of parameters 614
H-atom treatment H-atom parameters constrained
Δρmax, Δρmin (e Å−3) 0.99, −0.74
Computer programs: XSCANS (Bruker, 1997[Bruker (1997). XSCANS. Bruker AXS Inc., Madison, Wisconsin, USA.]), SHELXS2013 and SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and SHELXL2014 (Sheldrick, 2015[Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.]).

Structural data

CCDC reference: 1476213

Crystal structure: contains datablock I. DOI: 10.1107/S2414314616006969/ff4006sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S2414314616006969/ff4006Isup2.hkl

checkCIF report


Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Experimental top

The synthesis and crystallization of this complex is similar to that described for [Pt(SC6F4H)2(1,2-C6F4(SC6F4H)(PPh(C6F5)))] in: Villanueva et al. (2004).

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. A free refinement of the occupancy for dichloromethane C37/Cl1/Cl2 converged to 0.47. In the final cycles, this parameter was fixed to 1/2.

Structure description top

The title complex, [Pt(SC6F5)2(1,2-C6F4(SC6F5)(PPh(C6F5)))] (Fig. 1), is a product resulting from the C—F bond activation of [Pt2(µ-SC6F5)2(SC6F5)2(PPh(C6F5)2)2]. The chemistry has been described for this compound and for other related compounds with different fluorinated thiolate groups and phosphanes (Villanueva et al., 2004; Bernès et al., 2016).

The PtII center is coordinated by two cis thiolates and one chelating bidentate ligand, giving a square-planar coordination geometry. The thiolates have their C6F5 rings almost parallel, giving a parallel displaced π–π interaction; the angle between rings is 4.8 (4)°, and the distance between ring centroids is 4.322 (6) Å. One C6F5 ring is affected by libration, clearly visible on C3—F3, C4—F4 and C5—F5 groups (see Fig. 1). The chelate ring coordinates via P and S donors, at normal distances [Pt1—P1 = 2.2315 (11) Å; Pt1—S3 = 2.2757 (12) Å, shorter than Pt—Sthiolate bond lengths]. Both S and P atoms are tetrahedrally hybridized, assuming that one lone pair is present on S3. Angles around P1 are in the range 104.1 (2)–116.75 (15)°, while bond angles around S3 are in the range 102.4 (2)–109.13 (17)°. The complex conformation is identical to that previously described for the compound bearing 2,3,5,6-tetrafluorophenylthiolate in place of pentafluorophenylthiolate groups (Villanueva et al., 2004).

The complex was crystallized with dichloromethane as lattice solvent. This molecule is placed close to the inversion centers of the triclinic cell, and its occupancy was then fixed to 1/2. As the main complex is in a general position, the chemical composition thus corresponds to an hemisolvate.

Computing details top

Data collection: XSCANS (Bruker, 1997); cell refinement: XSCANS (Bruker, 1997); data reduction: XSCANS (Bruker, 1997); program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).

Figures top
[Figure 1] Fig. 1. The structure of the title compound, with displacement ellipsoids for non-H atoms at the 20% probability level. Labels for F atoms (green ellipsoids) are identical to those of the C atom to which they are bonded.
Bis(pentafluorobenzenethiolato-κS){(pentafluorophenyl)phenyl[3,4,5,6-tetrafluoro-2-(pentafluorophenylsulfanyl)phenyl]phosphane-κ2P,S}platinum(II) dichloromethane hemisolvate top
Crystal data top
[Pt(C6F5S)2(C24H5F14PS)]·0.5CH2Cl2Z = 2
Mr = 1258.10F(000) = 1198
Triclinic, P1Dx = 2.074 Mg m−3
a = 11.2908 (10) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.8516 (14) ÅCell parameters from 75 reflections
c = 14.6956 (17) Åθ = 3.6–12.5°
α = 104.477 (8)°µ = 3.89 mm−1
β = 96.359 (8)°T = 296 K
γ = 111.675 (7)°Plate, yellow
V = 2014.6 (4) Å30.65 × 0.40 × 0.24 mm
Data collection top
Bruker P4
diffractometer		7392 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube, FN4Rint = 0.036
Graphite monochromatorθmax = 27.5°, θmin = 1.8°
2θ/ω scansh = −14→8
Absorption correction: ψ scan
(XSCANS; Bruker, 1997)		k = −16→16
Tmin = 0.521, Tmax = 0.897l = −19→19
15487 measured reflections3 standard reflections every 97 reflections
9078 independent reflections intensity decay: 1.5%
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.089H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0456P)2 + 0.2045P]
where P = (Fo2 + 2Fc2)/3
9078 reflections(Δ/σ)max = 0.002
614 parametersΔρmax = 0.99 e Å−3
0 restraintsΔρmin = −0.74 e Å−3
0 constraints
Crystal data top
[Pt(C6F5S)2(C24H5F14PS)]·0.5CH2Cl2γ = 111.675 (7)°
Mr = 1258.10V = 2014.6 (4) Å3
Triclinic, P1Z = 2
a = 11.2908 (10) ÅMo Kα radiation
b = 13.8516 (14) ŵ = 3.89 mm−1
c = 14.6956 (17) ÅT = 296 K
α = 104.477 (8)°0.65 × 0.40 × 0.24 mm
β = 96.359 (8)°
Data collection top
Bruker P4
diffractometer		7392 reflections with I > 2σ(I)
Absorption correction: ψ scan
(XSCANS; Bruker, 1997)		Rint = 0.036
Tmin = 0.521, Tmax = 0.8973 standard reflections every 97 reflections
15487 measured reflections intensity decay: 1.5%
9078 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0370 restraints
wR(F2) = 0.089H-atom parameters constrained
S = 1.02Δρmax = 0.99 e Å−3
9078 reflectionsΔρmin = −0.74 e Å−3
614 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pt10.65934 (2)0.65231 (2)0.20934 (2)0.04309 (7)
P10.66292 (11)0.81991 (9)0.24844 (8)0.0446 (2)
S10.67412 (16)0.65984 (11)0.36926 (9)0.0672 (4)
S20.64217 (13)0.47144 (9)0.15065 (9)0.0547 (3)
S30.64754 (11)0.64869 (9)0.05284 (8)0.0475 (2)
C10.5663 (6)0.5315 (4)0.3703 (3)0.0612 (13)
C20.6101 (8)0.4739 (5)0.4213 (4)0.0757 (17)
F20.7365 (5)0.5210 (4)0.4704 (3)0.1082 (13)
C30.5288 (14)0.3739 (7)0.4240 (7)0.127 (4)
F30.5813 (10)0.3252 (5)0.4758 (6)0.210 (4)
C40.4052 (16)0.3291 (8)0.3786 (9)0.157 (7)
F40.3278 (10)0.2290 (5)0.3779 (6)0.282 (6)
C50.3544 (11)0.3813 (12)0.3270 (7)0.165 (7)
F50.2305 (6)0.3384 (8)0.2828 (4)0.268 (6)
C60.4387 (8)0.4863 (7)0.3266 (5)0.101 (2)
F60.3857 (4)0.5362 (7)0.2785 (4)0.164 (3)
C70.7545 (4)0.4551 (4)0.2305 (3)0.0497 (10)
C80.8822 (5)0.5310 (4)0.2722 (4)0.0620 (13)
F80.9267 (3)0.6259 (3)0.2523 (3)0.0864 (10)
C90.9678 (6)0.5139 (5)0.3327 (5)0.0808 (17)
F91.0905 (4)0.5897 (4)0.3704 (4)0.1235 (16)
C100.9278 (6)0.4175 (5)0.3555 (5)0.0793 (17)
F101.0090 (5)0.3995 (4)0.4144 (4)0.1265 (17)
C110.8028 (6)0.3391 (4)0.3152 (5)0.0739 (15)
F110.7620 (4)0.2454 (3)0.3374 (3)0.1091 (13)
C120.7197 (5)0.3587 (4)0.2537 (4)0.0582 (12)
F120.5975 (3)0.2795 (2)0.2166 (3)0.0790 (9)
C130.7970 (5)0.6531 (4)0.0211 (3)0.0537 (11)
C140.7924 (6)0.5610 (5)−0.0456 (4)0.0671 (14)
F140.6794 (4)0.4732 (3)−0.0847 (3)0.0896 (11)
C150.9053 (8)0.5589 (6)−0.0719 (5)0.092 (2)
F150.8988 (6)0.4678 (4)−0.1353 (4)0.142 (2)
C161.0213 (8)0.6482 (7)−0.0332 (6)0.096 (2)
F161.1287 (5)0.6446 (5)−0.0603 (4)0.153 (2)
C171.0287 (6)0.7398 (6)0.0309 (5)0.0805 (17)
F171.1407 (4)0.8280 (4)0.0671 (4)0.1148 (14)
C180.9160 (5)0.7421 (4)0.0597 (4)0.0607 (12)
F180.9254 (3)0.8324 (3)0.1254 (2)0.0766 (9)
C190.6525 (4)0.7785 (4)0.0507 (3)0.0508 (11)
C200.6550 (5)0.8036 (4)−0.0341 (4)0.0579 (12)
F200.6669 (3)0.7372 (3)−0.1115 (2)0.0757 (9)
C210.6500 (5)0.8998 (5)−0.0397 (4)0.0694 (15)
F210.6537 (4)0.9256 (3)−0.1213 (3)0.0968 (12)
C220.6388 (5)0.9701 (4)0.0404 (5)0.0675 (15)
F220.6332 (4)1.0638 (3)0.0362 (3)0.0926 (11)
C230.6337 (5)0.9442 (4)0.1259 (4)0.0591 (12)
F230.6178 (3)1.0127 (3)0.1998 (3)0.0800 (9)
C240.6438 (4)0.8506 (4)0.1336 (4)0.0515 (11)
C250.5295 (4)0.8324 (3)0.3027 (4)0.0511 (11)
C260.4054 (5)0.7983 (4)0.2474 (4)0.0616 (13)
F260.3832 (3)0.7639 (3)0.1508 (3)0.0839 (10)
C270.3012 (5)0.7975 (5)0.2881 (5)0.0782 (17)
F270.1825 (3)0.7649 (4)0.2310 (4)0.1137 (15)
C280.3180 (6)0.8296 (5)0.3867 (5)0.0766 (18)
F280.2158 (4)0.8293 (3)0.4255 (4)0.1141 (15)
C290.4365 (6)0.8610 (4)0.4428 (5)0.0700 (16)
F290.4538 (4)0.8940 (3)0.5394 (3)0.0961 (12)
C300.5405 (5)0.8624 (4)0.4017 (4)0.0580 (12)
F300.6563 (3)0.8964 (3)0.4627 (2)0.0738 (8)
C310.8149 (4)0.9318 (4)0.3230 (3)0.0478 (10)
C320.8251 (5)1.0370 (4)0.3632 (4)0.0572 (12)
H32A0.75141.05210.35670.069*
C330.9454 (5)1.1192 (4)0.4130 (4)0.0663 (14)
H33A0.95291.19000.44030.080*
C341.0556 (5)1.0972 (5)0.4227 (4)0.0708 (15)
H34A1.13701.15330.45510.085*
C351.0437 (5)0.9921 (5)0.3841 (4)0.0688 (14)
H35A1.11690.97660.39200.083*
C360.9245 (4)0.9097 (4)0.3341 (3)0.0545 (11)
H36A0.91740.83880.30770.065*
C371.0152 (16)1.0944 (13)0.1602 (11)0.102 (5)0.5
H37A0.97691.03700.18840.123*0.5
H37B1.10641.13560.19370.123*0.5
Cl10.9371 (4)1.1786 (4)0.1773 (3)0.1127 (13)0.5
Cl21.0064 (5)1.0342 (4)0.0376 (3)0.1166 (14)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.04474 (10)0.03828 (10)0.04831 (10)0.01929 (7)0.01035 (7)0.01377 (7)
P10.0437 (6)0.0404 (6)0.0534 (6)0.0214 (5)0.0117 (5)0.0142 (5)
S10.0982 (10)0.0519 (7)0.0473 (6)0.0300 (7)0.0092 (7)0.0137 (5)
S20.0682 (7)0.0411 (6)0.0552 (7)0.0264 (6)0.0074 (6)0.0123 (5)
S30.0457 (6)0.0452 (6)0.0483 (6)0.0172 (5)0.0088 (5)0.0123 (5)
C10.073 (3)0.064 (3)0.045 (3)0.027 (3)0.021 (3)0.014 (2)
C20.115 (5)0.061 (3)0.066 (3)0.042 (4)0.048 (4)0.026 (3)
F20.131 (4)0.145 (4)0.097 (3)0.089 (3)0.035 (3)0.065 (3)
C30.227 (12)0.080 (5)0.113 (7)0.071 (7)0.114 (8)0.053 (5)
F30.390 (12)0.148 (5)0.229 (7)0.166 (7)0.191 (8)0.150 (6)
C40.176 (13)0.090 (7)0.116 (9)−0.032 (7)0.101 (10)−0.010 (6)
F40.396 (12)0.098 (4)0.229 (8)−0.045 (6)0.218 (9)0.011 (4)
C50.107 (8)0.191 (13)0.078 (6)−0.037 (8)0.049 (6)−0.017 (6)
F50.109 (4)0.344 (11)0.123 (4)−0.084 (6)0.048 (4)−0.043 (6)
C60.089 (5)0.132 (7)0.058 (4)0.023 (5)0.027 (4)0.020 (4)
F60.079 (3)0.319 (9)0.094 (3)0.076 (4)0.015 (2)0.076 (5)
C70.052 (3)0.044 (2)0.059 (3)0.027 (2)0.016 (2)0.015 (2)
C80.054 (3)0.049 (3)0.089 (4)0.024 (2)0.023 (3)0.023 (3)
F80.0592 (18)0.0622 (19)0.140 (3)0.0174 (15)0.026 (2)0.045 (2)
C90.052 (3)0.068 (4)0.110 (5)0.021 (3)−0.001 (3)0.020 (3)
F90.061 (2)0.094 (3)0.184 (5)0.018 (2)−0.019 (3)0.032 (3)
C100.072 (4)0.071 (4)0.100 (5)0.043 (3)−0.006 (3)0.025 (3)
F100.119 (3)0.110 (3)0.143 (4)0.059 (3)−0.033 (3)0.038 (3)
C110.090 (4)0.053 (3)0.088 (4)0.040 (3)0.008 (3)0.025 (3)
F110.124 (3)0.073 (2)0.140 (4)0.046 (2)0.003 (3)0.054 (2)
C120.062 (3)0.044 (3)0.067 (3)0.026 (2)0.012 (2)0.012 (2)
F120.0678 (19)0.0492 (16)0.106 (3)0.0121 (15)0.0022 (18)0.0277 (17)
C130.057 (3)0.062 (3)0.053 (3)0.030 (2)0.021 (2)0.025 (2)
C140.086 (4)0.064 (3)0.059 (3)0.039 (3)0.023 (3)0.016 (3)
F140.106 (3)0.067 (2)0.077 (2)0.033 (2)0.018 (2)−0.0010 (17)
C150.120 (6)0.099 (5)0.092 (5)0.073 (5)0.054 (5)0.029 (4)
F150.181 (5)0.128 (4)0.147 (4)0.100 (4)0.085 (4)0.017 (3)
C160.092 (5)0.132 (7)0.107 (5)0.076 (5)0.058 (5)0.049 (5)
F160.121 (4)0.205 (6)0.184 (5)0.106 (4)0.095 (4)0.060 (4)
C170.056 (3)0.101 (5)0.092 (4)0.033 (3)0.031 (3)0.038 (4)
F170.059 (2)0.143 (4)0.140 (4)0.031 (2)0.040 (2)0.052 (3)
C180.060 (3)0.066 (3)0.060 (3)0.030 (3)0.020 (2)0.017 (3)
F180.0597 (18)0.071 (2)0.077 (2)0.0132 (15)0.0176 (16)0.0061 (17)
C190.042 (2)0.055 (3)0.059 (3)0.020 (2)0.009 (2)0.026 (2)
C200.051 (3)0.064 (3)0.059 (3)0.017 (2)0.010 (2)0.029 (2)
F200.087 (2)0.086 (2)0.0540 (17)0.0305 (18)0.0163 (16)0.0286 (16)
C210.057 (3)0.077 (4)0.076 (4)0.017 (3)0.004 (3)0.049 (3)
F210.099 (3)0.102 (3)0.092 (2)0.026 (2)0.011 (2)0.065 (2)
C220.051 (3)0.058 (3)0.100 (4)0.021 (2)0.001 (3)0.043 (3)
F220.087 (2)0.068 (2)0.134 (3)0.0332 (18)0.006 (2)0.058 (2)
C230.051 (3)0.052 (3)0.078 (3)0.026 (2)0.008 (2)0.024 (3)
F230.089 (2)0.0583 (18)0.105 (3)0.0456 (17)0.015 (2)0.0261 (18)
C240.043 (2)0.049 (2)0.067 (3)0.021 (2)0.011 (2)0.023 (2)
C250.048 (2)0.037 (2)0.065 (3)0.0167 (19)0.013 (2)0.011 (2)
C260.056 (3)0.054 (3)0.073 (3)0.024 (2)0.017 (3)0.016 (3)
F260.0481 (17)0.100 (3)0.089 (2)0.0215 (17)0.0051 (16)0.024 (2)
C270.049 (3)0.071 (4)0.121 (6)0.026 (3)0.026 (3)0.037 (4)
F270.051 (2)0.137 (4)0.156 (4)0.039 (2)0.022 (2)0.050 (3)
C280.071 (4)0.058 (3)0.118 (5)0.035 (3)0.051 (4)0.031 (3)
F280.089 (3)0.104 (3)0.178 (4)0.052 (2)0.086 (3)0.047 (3)
C290.084 (4)0.049 (3)0.087 (4)0.031 (3)0.045 (3)0.021 (3)
F290.126 (3)0.068 (2)0.099 (3)0.039 (2)0.066 (2)0.0197 (19)
C300.057 (3)0.042 (2)0.074 (3)0.019 (2)0.024 (3)0.015 (2)
F300.074 (2)0.076 (2)0.0663 (18)0.0274 (17)0.0228 (17)0.0169 (16)
C310.047 (2)0.046 (2)0.049 (2)0.019 (2)0.012 (2)0.0139 (19)
C320.054 (3)0.047 (3)0.068 (3)0.022 (2)0.011 (2)0.014 (2)
C330.070 (3)0.043 (3)0.073 (3)0.012 (2)0.014 (3)0.015 (2)
C340.048 (3)0.069 (4)0.074 (4)0.005 (3)0.002 (3)0.021 (3)
C350.052 (3)0.078 (4)0.072 (3)0.028 (3)0.009 (3)0.016 (3)
C360.047 (2)0.057 (3)0.058 (3)0.023 (2)0.009 (2)0.013 (2)
C370.099 (10)0.095 (10)0.093 (10)0.021 (8)0.002 (8)0.035 (8)
Cl10.103 (3)0.120 (3)0.107 (3)0.035 (2)0.025 (2)0.039 (2)
Cl20.107 (3)0.123 (4)0.132 (4)0.043 (3)0.047 (3)0.060 (3)
Geometric parameters (Å, º) top
Pt1—P12.2315 (11)C17—F171.327 (8)
Pt1—S32.2757 (12)C17—C181.392 (7)
Pt1—S12.3107 (13)C18—F181.336 (6)
Pt1—S22.3627 (12)C19—C201.375 (7)
P1—C311.821 (5)C19—C241.407 (7)
P1—C251.823 (5)C20—F201.327 (6)
P1—C241.851 (5)C20—C211.376 (8)
S1—C11.750 (6)C21—F211.335 (6)
S2—C71.747 (5)C21—C221.379 (8)
S3—C131.784 (5)C22—F221.339 (6)
S3—C191.787 (5)C22—C231.391 (8)
C1—C61.344 (9)C23—F231.330 (6)
C1—C21.396 (8)C23—C241.373 (7)
C2—F21.353 (8)C25—C261.384 (7)
C2—C31.364 (10)C25—C301.387 (7)
C3—C41.314 (18)C26—F261.341 (6)
C3—F31.356 (13)C26—C271.376 (7)
C4—F41.335 (11)C27—F271.348 (7)
C4—C51.38 (2)C27—C281.374 (10)
C5—F51.313 (13)C28—F281.341 (6)
C5—C61.416 (15)C28—C291.343 (9)
C6—F61.338 (11)C29—F291.345 (7)
C7—C121.387 (7)C29—C301.376 (7)
C7—C81.386 (7)C30—F301.344 (6)
C8—F81.343 (6)C31—C361.383 (6)
C8—C91.366 (8)C31—C321.385 (6)
C9—F91.339 (7)C32—C331.377 (7)
C9—C101.383 (9)C32—H32A0.9300
C10—F101.324 (7)C33—C341.386 (8)
C10—C111.372 (8)C33—H33A0.9300
C11—F111.344 (6)C34—C351.374 (8)
C11—C121.377 (8)C34—H34A0.9300
C12—F121.349 (6)C35—C361.371 (7)
C13—C181.380 (7)C35—H35A0.9300
C13—C141.380 (7)C36—H36A0.9300
C14—F141.334 (7)C37—Cl11.692 (17)
C14—C151.381 (9)C37—Cl21.760 (15)
C15—F151.339 (8)C37—H37A0.9700
C15—C161.362 (11)C37—H37B0.9700
C16—F161.332 (7)Cl2—Cl2i1.217 (9)
C16—C171.346 (10)
P1—Pt1—S389.63 (4)F17—C17—C18119.3 (6)
P1—Pt1—S189.40 (5)C16—C17—C18119.2 (6)
S3—Pt1—S1178.81 (4)F18—C18—C13120.6 (4)
P1—Pt1—S2173.59 (4)F18—C18—C17118.6 (5)
S3—Pt1—S284.72 (4)C13—C18—C17120.8 (5)
S1—Pt1—S296.28 (5)C20—C19—C24120.5 (5)
C31—P1—C25107.8 (2)C20—C19—S3119.5 (4)
C31—P1—C24104.1 (2)C24—C19—S3119.8 (4)
C25—P1—C24106.7 (2)F20—C20—C19120.6 (5)
C31—P1—Pt1116.75 (15)F20—C20—C21118.5 (5)
C25—P1—Pt1114.57 (15)C19—C20—C21120.9 (5)
C24—P1—Pt1105.86 (15)F21—C21—C20121.5 (6)
C1—S1—Pt1106.76 (17)F21—C21—C22119.4 (5)
C7—S2—Pt1108.35 (15)C20—C21—C22119.1 (5)
C13—S3—C19102.4 (2)F22—C22—C21120.0 (5)
C13—S3—Pt1109.13 (17)F22—C22—C23119.8 (6)
C19—S3—Pt1105.85 (16)C21—C22—C23120.2 (5)
C6—C1—C2117.3 (7)F23—C23—C24121.0 (5)
C6—C1—S1122.4 (6)F23—C23—C22117.8 (5)
C2—C1—S1120.2 (5)C24—C23—C22121.2 (5)
F2—C2—C3120.0 (8)C23—C24—C19117.9 (5)
F2—C2—C1118.2 (5)C23—C24—P1124.1 (4)
C3—C2—C1121.8 (9)C19—C24—P1117.7 (3)
C4—C3—F3122.7 (11)C26—C25—C30115.4 (4)
C4—C3—C2120.3 (11)C26—C25—P1121.6 (4)
F3—C3—C2117.0 (12)C30—C25—P1122.4 (4)
C3—C4—F4119.8 (17)F26—C26—C27117.7 (5)
C3—C4—C5121.3 (10)F26—C26—C25120.2 (4)
F4—C4—C5118.8 (16)C27—C26—C25122.1 (5)
F5—C5—C4121.9 (14)F27—C27—C26119.8 (6)
F5—C5—C6120.0 (16)F27—C27—C28120.1 (5)
C4—C5—C6118.1 (11)C26—C27—C28120.1 (6)
F6—C6—C1122.2 (8)F28—C28—C29121.0 (7)
F6—C6—C5116.7 (10)F28—C28—C27119.5 (6)
C1—C6—C5121.1 (10)C29—C28—C27119.5 (5)
C12—C7—C8114.9 (5)C28—C29—F29119.7 (5)
C12—C7—S2120.0 (4)C28—C29—C30120.1 (6)
C8—C7—S2125.0 (4)F29—C29—C30120.1 (6)
F8—C8—C9117.2 (5)F30—C30—C29116.6 (5)
F8—C8—C7119.6 (5)F30—C30—C25120.7 (4)
C9—C8—C7123.2 (5)C29—C30—C25122.7 (5)
F9—C9—C8120.7 (6)C36—C31—C32120.0 (4)
F9—C9—C10119.4 (6)C36—C31—P1117.3 (3)
C8—C9—C10119.9 (5)C32—C31—P1122.6 (4)
F10—C10—C11119.8 (6)C33—C32—C31119.3 (5)
F10—C10—C9120.9 (6)C33—C32—H32A120.3
C11—C10—C9119.3 (5)C31—C32—H32A120.3
F11—C11—C10120.0 (5)C32—C33—C34120.6 (5)
F11—C11—C12120.7 (6)C32—C33—H33A119.7
C10—C11—C12119.2 (5)C34—C33—H33A119.7
F12—C12—C11117.0 (5)C35—C34—C33119.5 (5)
F12—C12—C7119.5 (5)C35—C34—H34A120.2
C11—C12—C7123.5 (5)C33—C34—H34A120.2
C18—C13—C14118.5 (5)C36—C35—C34120.4 (5)
C18—C13—S3124.0 (4)C36—C35—H35A119.8
C14—C13—S3117.4 (4)C34—C35—H35A119.8
F14—C14—C13120.5 (5)C35—C36—C31120.1 (5)
F14—C14—C15119.4 (5)C35—C36—H36A119.9
C13—C14—C15120.1 (6)C31—C36—H36A119.9
F15—C15—C16120.9 (6)Cl1—C37—Cl2112.9 (9)
F15—C15—C14119.0 (7)Cl1—C37—H37A109.0
C16—C15—C14120.1 (6)Cl2—C37—H37A109.0
F16—C16—C17119.7 (8)Cl1—C37—H37B109.0
F16—C16—C15119.1 (7)Cl2—C37—H37B109.0
C17—C16—C15121.2 (6)H37A—C37—H37B107.8
F17—C17—C16121.5 (6)Cl2i—Cl2—C37160.4 (8)
Pt1—S1—C1—C6−55.3 (5)C13—S3—C19—C2061.7 (4)
Pt1—S1—C1—C2127.6 (4)Pt1—S3—C19—C20176.0 (4)
C6—C1—C2—F2−176.2 (5)C13—S3—C19—C24−123.0 (4)
S1—C1—C2—F21.1 (7)Pt1—S3—C19—C24−8.7 (4)
C6—C1—C2—C32.5 (8)C24—C19—C20—F20178.1 (4)
S1—C1—C2—C3179.8 (5)S3—C19—C20—F20−6.7 (7)
F2—C2—C3—C4178.2 (7)C24—C19—C20—C210.4 (8)
C1—C2—C3—C4−0.5 (11)S3—C19—C20—C21175.6 (4)
F2—C2—C3—F3−1.2 (9)F20—C20—C21—F211.6 (8)
C1—C2—C3—F3−179.9 (5)C19—C20—C21—F21179.4 (5)
F3—C3—C4—F4−3.8 (14)F20—C20—C21—C22−179.5 (5)
C2—C3—C4—F4176.9 (7)C19—C20—C21—C22−1.8 (8)
F3—C3—C4—C5179.5 (8)F21—C21—C22—F22−0.8 (8)
C2—C3—C4—C50.1 (15)C20—C21—C22—F22−179.7 (5)
C3—C4—C5—F5−178.6 (8)F21—C21—C22—C23179.5 (5)
F4—C4—C5—F54.6 (16)C20—C21—C22—C230.6 (8)
C3—C4—C5—C6−1.8 (16)F22—C22—C23—F232.8 (7)
F4—C4—C5—C6−178.5 (7)C21—C22—C23—F23−177.5 (5)
C2—C1—C6—F6177.9 (6)F22—C22—C23—C24−177.7 (4)
S1—C1—C6—F60.6 (9)C21—C22—C23—C242.0 (8)
C2—C1—C6—C5−4.1 (9)F23—C23—C24—C19176.2 (4)
S1—C1—C6—C5178.6 (6)C22—C23—C24—C19−3.3 (7)
F5—C5—C6—F6−1.1 (12)F23—C23—C24—P1−10.0 (7)
C4—C5—C6—F6−178.0 (8)C22—C23—C24—P1170.5 (4)
F5—C5—C6—C1−179.2 (7)C20—C19—C24—C232.1 (7)
C4—C5—C6—C13.9 (13)S3—C19—C24—C23−173.1 (4)
Pt1—S2—C7—C12139.5 (4)C20—C19—C24—P1−172.1 (4)
Pt1—S2—C7—C8−42.9 (4)S3—C19—C24—P112.7 (5)
C12—C7—C8—F8178.2 (4)C31—P1—C24—C23−60.2 (4)
S2—C7—C8—F80.5 (7)C25—P1—C24—C2353.7 (5)
C12—C7—C8—C9−0.8 (8)Pt1—P1—C24—C23176.2 (4)
S2—C7—C8—C9−178.5 (5)C31—P1—C24—C19113.6 (4)
F8—C8—C9—F90.4 (9)C25—P1—C24—C19−132.5 (4)
C7—C8—C9—F9179.4 (6)Pt1—P1—C24—C19−10.0 (4)
F8—C8—C9—C10−179.7 (6)C31—P1—C25—C26149.1 (4)
C7—C8—C9—C10−0.7 (10)C24—P1—C25—C2637.7 (5)
F9—C9—C10—F100.3 (11)Pt1—P1—C25—C26−79.1 (4)
C8—C9—C10—F10−179.6 (6)C31—P1—C25—C30−39.8 (5)
F9—C9—C10—C11−178.7 (6)C24—P1—C25—C30−151.1 (4)
C8—C9—C10—C111.4 (10)Pt1—P1—C25—C3092.0 (4)
F10—C10—C11—F111.7 (10)C30—C25—C26—F26−177.6 (5)
C9—C10—C11—F11−179.4 (6)P1—C25—C26—F26−6.0 (7)
F10—C10—C11—C12−179.6 (6)C30—C25—C26—C271.9 (8)
C9—C10—C11—C12−0.7 (10)P1—C25—C26—C27173.6 (4)
F11—C11—C12—F12−0.7 (8)F26—C26—C27—F27−1.3 (8)
C10—C11—C12—F12−179.4 (5)C25—C26—C27—F27179.1 (5)
F11—C11—C12—C7177.8 (5)F26—C26—C27—C28178.5 (5)
C10—C11—C12—C7−0.9 (9)C25—C26—C27—C28−1.0 (9)
C8—C7—C12—F12−179.9 (4)F27—C27—C28—F28−0.7 (9)
S2—C7—C12—F12−2.1 (6)C26—C27—C28—F28179.4 (5)
C8—C7—C12—C111.5 (8)F27—C27—C28—C29179.4 (6)
S2—C7—C12—C11179.4 (4)C26—C27—C28—C29−0.4 (9)
C19—S3—C13—C1845.1 (5)F28—C28—C29—F29−0.8 (8)
Pt1—S3—C13—C18−66.8 (5)C27—C28—C29—F29179.0 (5)
C19—S3—C13—C14−135.4 (4)F28—C28—C29—C30−179.0 (5)
Pt1—S3—C13—C14112.7 (4)C27—C28—C29—C300.8 (9)
C18—C13—C14—F14180.0 (5)C28—C29—C30—F30179.0 (5)
S3—C13—C14—F140.5 (7)F29—C29—C30—F300.8 (7)
C18—C13—C14—C150.6 (8)C28—C29—C30—C250.2 (8)
S3—C13—C14—C15−178.9 (5)F29—C29—C30—C25−178.1 (4)
F14—C14—C15—F15−0.8 (10)C26—C25—C30—F30179.7 (4)
C13—C14—C15—F15178.6 (6)P1—C25—C30—F308.1 (7)
F14—C14—C15—C16179.5 (6)C26—C25—C30—C29−1.5 (7)
C13—C14—C15—C16−1.1 (11)P1—C25—C30—C29−173.1 (4)
F15—C15—C16—F160.9 (12)C25—P1—C31—C36143.3 (4)
C14—C15—C16—F16−179.4 (7)C24—P1—C31—C36−103.6 (4)
F15—C15—C16—C17−179.7 (7)Pt1—P1—C31—C3612.6 (4)
C14—C15—C16—C170.0 (12)C25—P1—C31—C32−40.3 (5)
F16—C16—C17—F171.1 (12)C24—P1—C31—C3272.8 (4)
C15—C16—C17—F17−178.3 (7)Pt1—P1—C31—C32−171.0 (3)
F16—C16—C17—C18−179.1 (6)C36—C31—C32—C331.0 (7)
C15—C16—C17—C181.5 (12)P1—C31—C32—C33−175.3 (4)
C14—C13—C18—F18−179.2 (5)C31—C32—C33—C340.1 (8)
S3—C13—C18—F180.3 (8)C32—C33—C34—C35−1.4 (9)
C14—C13—C18—C171.0 (8)C33—C34—C35—C361.7 (9)
S3—C13—C18—C17−179.5 (5)C34—C35—C36—C31−0.6 (8)
F17—C17—C18—F18−2.0 (9)C32—C31—C36—C35−0.7 (7)
C16—C17—C18—F18178.1 (6)P1—C31—C36—C35175.8 (4)
F17—C17—C18—C13177.8 (5)Cl1—C37—Cl2—Cl2i−137 (2)
C16—C17—C18—C13−2.0 (10)
Symmetry code: (i) −x+2, −y+2, −z.

Experimental details

Crystal data
Chemical formula[Pt(C6F5S)2(C24H5F14PS)]·0.5CH2Cl2
Mr1258.10
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)11.2908 (10), 13.8516 (14), 14.6956 (17)
α, β, γ (°)104.477 (8), 96.359 (8), 111.675 (7)
V (Å3)2014.6 (4)
Z2
Radiation typeMo Kα
µ (mm−1)3.89
Crystal size (mm)0.65 × 0.40 × 0.24
Data collection
DiffractometerBruker P4
Absorption correctionψ scan
(XSCANS; Bruker, 1997)
Tmin, Tmax0.521, 0.897
No. of measured, independent and
observed [I > 2σ(I)] reflections		15487, 9078, 7392
Rint0.036
(sin θ/λ)max (Å−1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.089, 1.02
No. of reflections9078
No. of parameters614
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.99, −0.74

Computer programs: XSCANS (Bruker, 1997), SHELXS2013 (Sheldrick, 2008), SHELXL2014 (Sheldrick, 2015), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

SB acknowledges support by the Instituto de Física Luis Rivera Terrazas (Puebla, Mexico).

References

First citationBernès, S., Meléndez, F. J. & Torrens, H. (2016). Acta Cryst. C72, 268–273.  Google Scholar
 First citationBruker (1997). XSCANS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationSheldrick, G. M. (2015). Acta Cryst. C71, 3–8.  Web of Science CrossRef IUCr Journals Google Scholar
 First citationVillanueva, L., Arroyo, M., Bernès, S. & Torrens, H. (2004). Chem. Commun. pp. 1942–1943.  Web of Science CSD CrossRef Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoIUCrDATA
ISSN: 2414-3146
Volume 1| Part 5| May 2016| x160696
doi:10.1107/S2414314616006969
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