metal-organic compounds
cis-Dichloridobis(triphenylphosphine-κP)platinum(II) chloroform solvate
aSchool of Chemistry and Chemical Engineering, University of Jinan, Jinan 250022, People's Republic of China, and bDepartment of Chemistry, New York University, 100 Washington Square East, New York, NY 10003-6688, USA
*Correspondence e-mail: chm_niey@ujn.edu.cn
In the title compound, [PtCl2(C18H15P)2]·CHCl3, each PtII centre adopts a nearly square-planar coordination geometry formed by two P atoms [Pt—P = 2.2481 (17) and 2.2658 (19) Å] and two Cl anions [Pt—Cl = 2.3244 (19) and 2.3548 (17) Å]. The Cl atoms of the chloroform solvent molecule are disordered over two orientations in a 0.778 (11):0.222 (11) ratio. The crystal packing is stabilized by weak intermolecular C—H⋯Cl hydrogen bonds, exhibiting voids with a volume of 215 Å3.
Related literature
For the preparation of cis-[PtCl2(PPh3)2], see: Bailar & Itatani (1965). For the structure of trans-[PtCl2(PPh3)2], see: Johansson & Otto (2000). For the structures of related cis-complexes, see: Anderson et al. (1982); Al-Fawaz et al. (2004); Fun et al. (2006).
Experimental
Crystal data
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Refinement
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Data collection: SMART (Bruker, 2001); cell SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.
Supporting information
10.1107/S1600536809029961/cv2593sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536809029961/cv2593Isup2.hkl
A mixture of PtCl2(PPh3)2 (314 mg, 0.4 mmol) and (Et4N)2B10H10 (150 mg, 0.4 mmol) in HOCH2CH2OH (38 ml) was heated at 100°C (oil) under N2 atomosphere for 39 h. The resulting mixture was filtered to get a red filtrate, to which ca 400 ml of water was added. The lower layer formed was separated and treated with water. This process was repeated till the lower layer was colourless. The upper water phase combined was extracted with CH2Cl2. The yellow organic layer was dried to result in a reddish solid. Recrystalization in CHCl3/n-hexane(1:4, V: V) afforded a small amount of yellowish crystals of the title compound suitable for X-ray analysis.
All H-atoms were positioned geometrically and refined using a riding model with d(C—H) = 0.93 Å, Uiso=1.2Ueq (C) for aromatic, and d(C—H) = 0.98 Å, Uiso=1.5Ueq (C) for CHCl3. The highest residual peak [1.89 eÅ-3] and deepest hole [-1.27 eÅ-3] are situated 1.05 Å and 0.97 Å, respectively, at atom Pt1.
Data collection: SMART (Bruker, 2001); cell
SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).Fig. 1. View of (I) with atom labels and 25% probability displacement ellipsoids. For the disordered chloroform molecule, only major part is shown for clarity. |
[PtCl2(C18H15P)2]·CHCl3 | F(000) = 1784 |
Mr = 909.90 | Dx = 1.550 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 10.3174 (9) Å | Cell parameters from 8493 reflections |
b = 24.436 (2) Å | θ = 2.2–28.2° |
c = 15.6298 (18) Å | µ = 4.05 mm−1 |
β = 98.199 (1)° | T = 298 K |
V = 3900.3 (7) Å3 | Block, yellowish |
Z = 4 | 0.38 × 0.35 × 0.18 mm |
Bruker SMART CCD area-detector diffractometer | 6877 independent reflections |
Radiation source: fine-focus sealed tube | 4984 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.071 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −12→12 |
Tmin = 0.309, Tmax = 0.530 | k = −29→28 |
18772 measured reflections | l = −14→18 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.119 | H-atom parameters constrained |
S = 0.97 | w = 1/[σ2(Fo2) + (0.0594P)2] where P = (Fo2 + 2Fc2)/3 |
6877 reflections | (Δ/σ)max = 0.001 |
434 parameters | Δρmax = 1.89 e Å−3 |
0 restraints | Δρmin = −1.27 e Å−3 |
[PtCl2(C18H15P)2]·CHCl3 | V = 3900.3 (7) Å3 |
Mr = 909.90 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.3174 (9) Å | µ = 4.05 mm−1 |
b = 24.436 (2) Å | T = 298 K |
c = 15.6298 (18) Å | 0.38 × 0.35 × 0.18 mm |
β = 98.199 (1)° |
Bruker SMART CCD area-detector diffractometer | 6877 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 4984 reflections with I > 2σ(I) |
Tmin = 0.309, Tmax = 0.530 | Rint = 0.071 |
18772 measured reflections |
R[F2 > 2σ(F2)] = 0.048 | 0 restraints |
wR(F2) = 0.119 | H-atom parameters constrained |
S = 0.97 | Δρmax = 1.89 e Å−3 |
6877 reflections | Δρmin = −1.27 e Å−3 |
434 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pt1 | 0.59334 (2) | 0.349888 (10) | 0.548206 (18) | 0.03195 (11) | |
Cl1 | 0.45377 (18) | 0.39079 (8) | 0.43652 (13) | 0.0477 (5) | |
Cl2 | 0.41302 (18) | 0.29552 (8) | 0.57114 (13) | 0.0492 (5) | |
Cl3 | 0.2158 (6) | 0.3208 (3) | 0.2316 (4) | 0.142 (3) | 0.778 (11) |
Cl4 | 0.1897 (12) | 0.3400 (5) | 0.0514 (7) | 0.165 (4) | 0.778 (11) |
Cl5 | 0.4219 (6) | 0.3691 (2) | 0.1644 (6) | 0.141 (3) | 0.778 (11) |
Cl3' | 0.355 (3) | 0.3779 (12) | 0.078 (2) | 0.197 (14) | 0.222 (11) |
Cl4' | 0.348 (3) | 0.3554 (9) | 0.2339 (17) | 0.156 (12) | 0.222 (11) |
Cl5' | 0.147 (4) | 0.3153 (17) | 0.081 (3) | 0.167 (13) | 0.222 (11) |
P1 | 0.75776 (17) | 0.40376 (7) | 0.51837 (12) | 0.0316 (4) | |
P2 | 0.70533 (18) | 0.30561 (7) | 0.66301 (13) | 0.0359 (4) | |
C1 | 0.8924 (7) | 0.3665 (3) | 0.4836 (5) | 0.0416 (18) | |
C2 | 1.0068 (7) | 0.3918 (4) | 0.4670 (6) | 0.054 (2) | |
H2 | 1.0160 | 0.4295 | 0.4733 | 0.065* | |
C3 | 1.1060 (9) | 0.3615 (4) | 0.4413 (7) | 0.072 (3) | |
H3 | 1.1836 | 0.3786 | 0.4326 | 0.086* | |
C4 | 1.0925 (9) | 0.3063 (4) | 0.4282 (6) | 0.068 (3) | |
H4 | 1.1614 | 0.2861 | 0.4120 | 0.081* | |
C5 | 0.9789 (8) | 0.2810 (4) | 0.4387 (6) | 0.061 (2) | |
H5 | 0.9677 | 0.2439 | 0.4264 | 0.074* | |
C6 | 0.8797 (8) | 0.3107 (3) | 0.4677 (5) | 0.048 (2) | |
H6 | 0.8030 | 0.2930 | 0.4767 | 0.058* | |
C7 | 0.7173 (7) | 0.4505 (3) | 0.4270 (5) | 0.0400 (18) | |
C8 | 0.7002 (8) | 0.4296 (3) | 0.3447 (5) | 0.051 (2) | |
H8 | 0.7101 | 0.3922 | 0.3367 | 0.061* | |
C9 | 0.6684 (9) | 0.4631 (4) | 0.2731 (6) | 0.065 (3) | |
H9 | 0.6554 | 0.4486 | 0.2175 | 0.078* | |
C10 | 0.6564 (8) | 0.5200 (4) | 0.2873 (6) | 0.061 (2) | |
H10 | 0.6362 | 0.5433 | 0.2403 | 0.073* | |
C11 | 0.6737 (8) | 0.5407 (4) | 0.3678 (6) | 0.058 (2) | |
H11 | 0.6650 | 0.5782 | 0.3760 | 0.070* | |
C12 | 0.7044 (7) | 0.5067 (3) | 0.4382 (5) | 0.048 (2) | |
H12 | 0.7165 | 0.5214 | 0.4936 | 0.058* | |
C13 | 0.8127 (7) | 0.4487 (3) | 0.6099 (5) | 0.0394 (17) | |
C14 | 0.9418 (8) | 0.4603 (3) | 0.6409 (5) | 0.053 (2) | |
H14 | 1.0093 | 0.4437 | 0.6168 | 0.064* | |
C15 | 0.9694 (10) | 0.4972 (4) | 0.7088 (6) | 0.067 (3) | |
H15 | 1.0560 | 0.5044 | 0.7317 | 0.080* | |
C16 | 0.8705 (10) | 0.5230 (4) | 0.7418 (7) | 0.070 (3) | |
H16 | 0.8902 | 0.5487 | 0.7857 | 0.084* | |
C17 | 0.7427 (10) | 0.5116 (3) | 0.7111 (6) | 0.065 (3) | |
H17 | 0.6756 | 0.5288 | 0.7347 | 0.078* | |
C18 | 0.7138 (8) | 0.4744 (3) | 0.6452 (5) | 0.050 (2) | |
H18 | 0.6268 | 0.4666 | 0.6242 | 0.061* | |
C19 | 0.8622 (7) | 0.3305 (3) | 0.7180 (5) | 0.046 (2) | |
C20 | 0.9782 (8) | 0.3178 (3) | 0.6859 (6) | 0.054 (2) | |
H20 | 0.9755 | 0.2978 | 0.6351 | 0.065* | |
C21 | 1.0977 (9) | 0.3351 (4) | 0.7302 (7) | 0.066 (3) | |
H21 | 1.1753 | 0.3261 | 0.7097 | 0.079* | |
C22 | 1.1006 (10) | 0.3649 (4) | 0.8029 (8) | 0.074 (3) | |
H22 | 1.1808 | 0.3771 | 0.8312 | 0.088* | |
C23 | 0.9906 (10) | 0.3775 (4) | 0.8358 (7) | 0.072 (3) | |
H23 | 0.9962 | 0.3974 | 0.8870 | 0.086* | |
C24 | 0.8702 (9) | 0.3613 (3) | 0.7945 (6) | 0.056 (2) | |
H24 | 0.7945 | 0.3706 | 0.8170 | 0.067* | |
C25 | 0.7459 (7) | 0.2350 (3) | 0.6415 (5) | 0.0449 (19) | |
C26 | 0.6929 (8) | 0.2102 (3) | 0.5647 (6) | 0.053 (2) | |
H26 | 0.6354 | 0.2294 | 0.5242 | 0.063* | |
C27 | 0.7260 (10) | 0.1560 (4) | 0.5481 (7) | 0.072 (3) | |
H27 | 0.6905 | 0.1390 | 0.4969 | 0.086* | |
C28 | 0.8114 (10) | 0.1285 (4) | 0.6082 (8) | 0.075 (3) | |
H28 | 0.8359 | 0.0929 | 0.5965 | 0.090* | |
C29 | 0.8601 (10) | 0.1517 (4) | 0.6835 (8) | 0.073 (3) | |
H29 | 0.9149 | 0.1316 | 0.7243 | 0.088* | |
C30 | 0.8301 (8) | 0.2050 (3) | 0.7013 (6) | 0.057 (2) | |
H30 | 0.8662 | 0.2210 | 0.7533 | 0.069* | |
C31 | 0.6018 (7) | 0.3029 (3) | 0.7490 (5) | 0.0418 (18) | |
C32 | 0.5768 (7) | 0.2541 (3) | 0.7894 (5) | 0.053 (2) | |
H32 | 0.6147 | 0.2217 | 0.7739 | 0.064* | |
C33 | 0.4960 (8) | 0.2537 (4) | 0.8523 (5) | 0.059 (2) | |
H33 | 0.4781 | 0.2208 | 0.8782 | 0.071* | |
C34 | 0.4418 (8) | 0.3009 (4) | 0.8770 (6) | 0.062 (2) | |
H34 | 0.3872 | 0.3006 | 0.9195 | 0.074* | |
C35 | 0.4694 (9) | 0.3492 (4) | 0.8379 (6) | 0.058 (2) | |
H35 | 0.4350 | 0.3819 | 0.8555 | 0.069* | |
C36 | 0.5457 (8) | 0.3501 (3) | 0.7742 (6) | 0.054 (2) | |
H36 | 0.5603 | 0.3830 | 0.7473 | 0.065* | |
C37 | 0.2974 (13) | 0.3240 (6) | 0.1404 (9) | 0.106 (4) | |
H37 | 0.3347 | 0.2879 | 0.1316 | 0.127* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.02648 (17) | 0.03000 (17) | 0.03899 (18) | −0.00180 (11) | 0.00341 (12) | 0.00317 (13) |
Cl1 | 0.0357 (10) | 0.0525 (12) | 0.0525 (12) | 0.0011 (9) | −0.0018 (9) | 0.0159 (10) |
Cl2 | 0.0363 (11) | 0.0537 (12) | 0.0566 (12) | −0.0171 (9) | 0.0036 (9) | 0.0119 (10) |
Cl3 | 0.124 (5) | 0.164 (5) | 0.145 (5) | 0.039 (4) | 0.043 (4) | 0.027 (4) |
Cl4 | 0.175 (10) | 0.188 (10) | 0.120 (6) | 0.021 (7) | −0.017 (6) | −0.015 (6) |
Cl5 | 0.102 (4) | 0.108 (4) | 0.212 (10) | −0.007 (3) | 0.013 (5) | 0.006 (4) |
Cl3' | 0.20 (3) | 0.20 (3) | 0.20 (3) | 0.00 (2) | 0.04 (3) | −0.01 (2) |
Cl4' | 0.17 (3) | 0.149 (19) | 0.15 (2) | 0.022 (17) | 0.006 (18) | −0.001 (15) |
Cl5' | 0.15 (2) | 0.17 (3) | 0.18 (3) | −0.004 (19) | 0.01 (2) | 0.00 (2) |
P1 | 0.0273 (10) | 0.0259 (9) | 0.0416 (11) | −0.0011 (7) | 0.0046 (8) | 0.0021 (8) |
P2 | 0.0331 (11) | 0.0335 (10) | 0.0403 (11) | −0.0019 (8) | 0.0019 (9) | 0.0046 (9) |
C1 | 0.034 (4) | 0.039 (4) | 0.052 (5) | −0.001 (3) | 0.007 (4) | 0.003 (4) |
C2 | 0.041 (5) | 0.059 (5) | 0.065 (6) | −0.003 (4) | 0.015 (4) | 0.000 (5) |
C3 | 0.049 (6) | 0.088 (8) | 0.083 (7) | −0.004 (5) | 0.025 (5) | −0.008 (6) |
C4 | 0.051 (6) | 0.080 (7) | 0.074 (7) | 0.020 (5) | 0.016 (5) | −0.003 (6) |
C5 | 0.058 (6) | 0.057 (6) | 0.069 (6) | 0.019 (5) | 0.011 (5) | −0.006 (5) |
C6 | 0.045 (5) | 0.048 (5) | 0.054 (5) | 0.004 (4) | 0.012 (4) | 0.004 (4) |
C7 | 0.035 (4) | 0.037 (4) | 0.049 (5) | 0.000 (3) | 0.010 (4) | 0.009 (4) |
C8 | 0.055 (5) | 0.047 (5) | 0.052 (5) | 0.002 (4) | 0.014 (4) | 0.009 (4) |
C9 | 0.071 (7) | 0.069 (6) | 0.057 (6) | 0.002 (5) | 0.013 (5) | 0.014 (5) |
C10 | 0.064 (6) | 0.057 (6) | 0.062 (6) | 0.012 (4) | 0.014 (5) | 0.027 (5) |
C11 | 0.062 (6) | 0.047 (5) | 0.067 (6) | 0.008 (4) | 0.013 (5) | 0.013 (5) |
C12 | 0.049 (5) | 0.040 (5) | 0.056 (5) | 0.002 (4) | 0.008 (4) | 0.005 (4) |
C13 | 0.036 (4) | 0.033 (4) | 0.048 (5) | −0.004 (3) | 0.003 (4) | 0.002 (4) |
C14 | 0.046 (5) | 0.052 (5) | 0.061 (5) | −0.006 (4) | 0.005 (4) | −0.001 (5) |
C15 | 0.061 (6) | 0.063 (6) | 0.073 (7) | −0.016 (5) | −0.004 (5) | −0.007 (6) |
C16 | 0.080 (8) | 0.056 (6) | 0.072 (7) | −0.013 (5) | 0.000 (6) | −0.013 (5) |
C17 | 0.067 (7) | 0.056 (6) | 0.072 (6) | 0.002 (5) | 0.008 (5) | −0.014 (5) |
C18 | 0.044 (5) | 0.048 (5) | 0.059 (6) | −0.003 (4) | 0.006 (4) | −0.004 (4) |
C19 | 0.041 (5) | 0.043 (4) | 0.053 (5) | 0.000 (4) | −0.001 (4) | 0.011 (4) |
C20 | 0.049 (6) | 0.054 (5) | 0.058 (6) | 0.000 (4) | 0.001 (4) | 0.007 (5) |
C21 | 0.043 (6) | 0.069 (6) | 0.082 (7) | 0.001 (5) | −0.001 (5) | 0.010 (6) |
C22 | 0.057 (7) | 0.080 (7) | 0.079 (8) | −0.007 (5) | −0.009 (6) | −0.003 (6) |
C23 | 0.067 (7) | 0.072 (7) | 0.070 (7) | −0.010 (5) | −0.008 (6) | −0.007 (6) |
C24 | 0.052 (6) | 0.058 (5) | 0.055 (6) | −0.002 (4) | 0.000 (4) | −0.002 (5) |
C25 | 0.042 (5) | 0.037 (4) | 0.055 (5) | −0.001 (3) | 0.004 (4) | 0.004 (4) |
C26 | 0.052 (5) | 0.043 (5) | 0.064 (6) | −0.001 (4) | 0.009 (4) | 0.004 (5) |
C27 | 0.075 (7) | 0.059 (6) | 0.079 (7) | −0.002 (5) | 0.005 (6) | −0.009 (5) |
C28 | 0.075 (8) | 0.053 (6) | 0.096 (9) | 0.008 (5) | 0.010 (7) | −0.001 (6) |
C29 | 0.070 (7) | 0.059 (6) | 0.087 (8) | 0.010 (5) | 0.003 (6) | 0.012 (6) |
C30 | 0.060 (6) | 0.046 (5) | 0.065 (6) | 0.003 (4) | 0.001 (5) | 0.007 (5) |
C31 | 0.039 (4) | 0.044 (5) | 0.042 (5) | −0.005 (3) | 0.006 (4) | 0.005 (4) |
C32 | 0.057 (6) | 0.049 (5) | 0.054 (5) | −0.001 (4) | 0.008 (4) | 0.011 (4) |
C33 | 0.066 (6) | 0.060 (6) | 0.052 (5) | −0.011 (5) | 0.010 (5) | 0.019 (5) |
C34 | 0.054 (6) | 0.077 (7) | 0.056 (6) | 0.005 (5) | 0.013 (5) | 0.012 (5) |
C35 | 0.052 (6) | 0.064 (6) | 0.058 (6) | 0.012 (4) | 0.010 (5) | 0.004 (5) |
C36 | 0.055 (6) | 0.054 (5) | 0.055 (6) | 0.005 (4) | 0.010 (5) | 0.014 (4) |
C37 | 0.102 (11) | 0.098 (9) | 0.115 (11) | 0.020 (8) | 0.009 (9) | −0.023 (9) |
Pt1—P1 | 2.2481 (17) | C15—C16 | 1.362 (12) |
Pt1—P2 | 2.2658 (19) | C15—H15 | 0.9300 |
Pt1—Cl1 | 2.3244 (19) | C16—C17 | 1.367 (12) |
Pt1—Cl2 | 2.3548 (17) | C16—H16 | 0.9300 |
Cl3—C37 | 1.758 (14) | C17—C18 | 1.373 (11) |
Cl4—C37 | 1.697 (17) | C17—H17 | 0.9300 |
Cl5—C37 | 1.693 (15) | C18—H18 | 0.9300 |
Cl3'—C37 | 1.79 (3) | C19—C20 | 1.397 (11) |
Cl4'—C37 | 1.67 (3) | C19—C24 | 1.404 (11) |
Cl5'—C37 | 1.70 (5) | C20—C21 | 1.390 (12) |
P1—C1 | 1.809 (7) | C20—H20 | 0.9300 |
P1—C13 | 1.828 (8) | C21—C22 | 1.347 (14) |
P1—C7 | 1.829 (7) | C21—H21 | 0.9300 |
P2—C25 | 1.818 (7) | C22—C23 | 1.347 (13) |
P2—C19 | 1.825 (8) | C22—H22 | 0.9300 |
P2—C31 | 1.833 (7) | C23—C24 | 1.375 (12) |
C1—C6 | 1.388 (10) | C23—H23 | 0.9300 |
C1—C2 | 1.389 (10) | C24—H24 | 0.9300 |
C2—C3 | 1.369 (11) | C25—C26 | 1.387 (11) |
C2—H2 | 0.9300 | C25—C30 | 1.390 (11) |
C3—C4 | 1.368 (12) | C26—C27 | 1.399 (11) |
C3—H3 | 0.9300 | C26—H26 | 0.9300 |
C4—C5 | 1.356 (12) | C27—C28 | 1.369 (14) |
C4—H4 | 0.9300 | C27—H27 | 0.9300 |
C5—C6 | 1.383 (10) | C28—C29 | 1.338 (14) |
C5—H5 | 0.9300 | C28—H28 | 0.9300 |
C6—H6 | 0.9300 | C29—C30 | 1.377 (11) |
C7—C8 | 1.372 (10) | C29—H29 | 0.9300 |
C7—C12 | 1.394 (10) | C30—H30 | 0.9300 |
C8—C9 | 1.386 (11) | C31—C36 | 1.374 (10) |
C8—H8 | 0.9300 | C31—C32 | 1.390 (10) |
C9—C10 | 1.415 (12) | C32—C33 | 1.376 (10) |
C9—H9 | 0.9300 | C32—H32 | 0.9300 |
C10—C11 | 1.344 (12) | C33—C34 | 1.362 (11) |
C10—H10 | 0.9300 | C33—H33 | 0.9300 |
C11—C12 | 1.379 (10) | C34—C35 | 1.378 (11) |
C11—H11 | 0.9300 | C34—H34 | 0.9300 |
C12—H12 | 0.9300 | C35—C36 | 1.353 (12) |
C13—C18 | 1.380 (10) | C35—H35 | 0.9300 |
C13—C14 | 1.380 (10) | C36—H36 | 0.9300 |
C14—C15 | 1.391 (11) | C37—H37 | 0.9800 |
C14—H14 | 0.9300 | ||
P1—Pt1—P2 | 97.43 (7) | C24—C19—P2 | 121.3 (6) |
P1—Pt1—Cl1 | 89.85 (7) | C21—C20—C19 | 119.9 (9) |
P2—Pt1—Cl1 | 172.47 (6) | C21—C20—H20 | 120.1 |
P1—Pt1—Cl2 | 176.28 (7) | C19—C20—H20 | 120.1 |
P2—Pt1—Cl2 | 86.26 (7) | C22—C21—C20 | 119.7 (9) |
Cl1—Pt1—Cl2 | 86.48 (7) | C22—C21—H21 | 120.2 |
C1—P1—C13 | 111.8 (3) | C20—C21—H21 | 120.2 |
C1—P1—C7 | 100.3 (3) | C23—C22—C21 | 121.9 (10) |
C13—P1—C7 | 104.3 (3) | C23—C22—H22 | 119.1 |
C1—P1—Pt1 | 113.7 (2) | C21—C22—H22 | 119.1 |
C13—P1—Pt1 | 110.4 (2) | C22—C23—C24 | 120.5 (10) |
C7—P1—Pt1 | 115.6 (2) | C22—C23—H23 | 119.7 |
C25—P2—C19 | 101.0 (4) | C24—C23—H23 | 119.7 |
C25—P2—C31 | 105.9 (3) | C23—C24—C19 | 119.6 (9) |
C19—P2—C31 | 103.7 (4) | C23—C24—H24 | 120.2 |
C25—P2—Pt1 | 114.3 (3) | C19—C24—H24 | 120.2 |
C19—P2—Pt1 | 122.1 (3) | C26—C25—C30 | 118.9 (7) |
C31—P2—Pt1 | 108.3 (3) | C26—C25—P2 | 120.2 (6) |
C6—C1—C2 | 117.7 (7) | C30—C25—P2 | 121.0 (6) |
C6—C1—P1 | 119.4 (5) | C25—C26—C27 | 119.8 (9) |
C2—C1—P1 | 122.8 (6) | C25—C26—H26 | 120.1 |
C3—C2—C1 | 120.3 (8) | C27—C26—H26 | 120.1 |
C3—C2—H2 | 119.9 | C28—C27—C26 | 119.2 (10) |
C1—C2—H2 | 119.9 | C28—C27—H27 | 120.4 |
C4—C3—C2 | 120.8 (9) | C26—C27—H27 | 120.4 |
C4—C3—H3 | 119.6 | C29—C28—C27 | 121.3 (10) |
C2—C3—H3 | 119.6 | C29—C28—H28 | 119.4 |
C5—C4—C3 | 120.2 (8) | C27—C28—H28 | 119.4 |
C5—C4—H4 | 119.9 | C28—C29—C30 | 120.8 (10) |
C3—C4—H4 | 119.9 | C28—C29—H29 | 119.6 |
C4—C5—C6 | 119.5 (9) | C30—C29—H29 | 119.6 |
C4—C5—H5 | 120.2 | C29—C30—C25 | 120.0 (9) |
C6—C5—H5 | 120.2 | C29—C30—H30 | 120.0 |
C5—C6—C1 | 121.2 (8) | C25—C30—H30 | 120.0 |
C5—C6—H6 | 119.4 | C36—C31—C32 | 118.4 (7) |
C1—C6—H6 | 119.4 | C36—C31—P2 | 119.6 (6) |
C8—C7—C12 | 118.8 (7) | C32—C31—P2 | 122.0 (6) |
C8—C7—P1 | 119.0 (6) | C33—C32—C31 | 120.1 (8) |
C12—C7—P1 | 122.2 (6) | C33—C32—H32 | 119.9 |
C7—C8—C9 | 121.4 (8) | C31—C32—H32 | 119.9 |
C7—C8—H8 | 119.3 | C34—C33—C32 | 120.7 (8) |
C9—C8—H8 | 119.3 | C34—C33—H33 | 119.6 |
C8—C9—C10 | 118.0 (9) | C32—C33—H33 | 119.6 |
C8—C9—H9 | 121.0 | C33—C34—C35 | 118.8 (8) |
C10—C9—H9 | 121.0 | C33—C34—H34 | 120.6 |
C11—C10—C9 | 120.9 (8) | C35—C34—H34 | 120.6 |
C11—C10—H10 | 119.5 | C36—C35—C34 | 121.1 (8) |
C9—C10—H10 | 119.5 | C36—C35—H35 | 119.4 |
C10—C11—C12 | 120.2 (8) | C34—C35—H35 | 119.4 |
C10—C11—H11 | 119.9 | C35—C36—C31 | 120.8 (8) |
C12—C11—H11 | 119.9 | C35—C36—H36 | 119.6 |
C11—C12—C7 | 120.6 (8) | C31—C36—H36 | 119.6 |
C11—C12—H12 | 119.7 | Cl4'—C37—Cl5 | 51.1 (10) |
C7—C12—H12 | 119.7 | Cl4'—C37—Cl4 | 134.5 (11) |
C18—C13—C14 | 119.9 (7) | Cl5—C37—Cl4 | 114.9 (10) |
C18—C13—P1 | 114.9 (6) | Cl4'—C37—Cl5' | 133 (2) |
C14—C13—P1 | 125.1 (6) | Cl5—C37—Cl5' | 143.7 (16) |
C13—C14—C15 | 118.9 (8) | Cl4—C37—Cl5' | 31.2 (11) |
C13—C14—H14 | 120.5 | Cl4'—C37—Cl3 | 55.8 (11) |
C15—C14—H14 | 120.5 | Cl5—C37—Cl3 | 106.5 (8) |
C16—C15—C14 | 120.4 (9) | Cl4—C37—Cl3 | 110.0 (9) |
C16—C15—H15 | 119.8 | Cl5'—C37—Cl3 | 86.0 (16) |
C14—C15—H15 | 119.8 | Cl4'—C37—Cl3' | 92.8 (15) |
C15—C16—C17 | 120.7 (9) | Cl5—C37—Cl3' | 48.8 (12) |
C15—C16—H16 | 119.7 | Cl4—C37—Cl3' | 67.4 (13) |
C17—C16—H16 | 119.7 | Cl5'—C37—Cl3' | 98.4 (17) |
C16—C17—C18 | 119.6 (9) | Cl3—C37—Cl3' | 135.1 (12) |
C16—C17—H17 | 120.2 | Cl4'—C37—H37 | 117.1 |
C18—C17—H17 | 120.2 | Cl5—C37—H37 | 108.4 |
C17—C18—C13 | 120.5 (8) | Cl4—C37—H37 | 108.4 |
C17—C18—H18 | 119.8 | Cl5'—C37—H37 | 99.0 |
C13—C18—H18 | 119.8 | Cl3—C37—H37 | 108.4 |
C20—C19—C24 | 118.4 (8) | Cl3'—C37—H37 | 114.8 |
C20—C19—P2 | 120.3 (7) | ||
P2—Pt1—P1—C1 | 65.2 (3) | Pt1—P1—C13—C14 | 137.5 (6) |
Cl1—Pt1—P1—C1 | −116.7 (3) | C18—C13—C14—C15 | 1.2 (12) |
Cl2—Pt1—P1—C1 | −107.5 (11) | P1—C13—C14—C15 | 177.1 (6) |
P2—Pt1—P1—C13 | −61.5 (3) | C13—C14—C15—C16 | −2.4 (13) |
Cl1—Pt1—P1—C13 | 116.6 (3) | C14—C15—C16—C17 | 2.4 (14) |
Cl2—Pt1—P1—C13 | 125.9 (10) | C15—C16—C17—C18 | −1.2 (14) |
P2—Pt1—P1—C7 | −179.5 (3) | C16—C17—C18—C13 | 0.0 (13) |
Cl1—Pt1—P1—C7 | −1.4 (3) | C14—C13—C18—C17 | 0.0 (12) |
Cl2—Pt1—P1—C7 | 7.8 (11) | P1—C13—C18—C17 | −176.4 (6) |
P1—Pt1—P2—C25 | −107.0 (3) | C25—P2—C19—C20 | 44.4 (7) |
Cl1—Pt1—P2—C25 | 87.8 (6) | C31—P2—C19—C20 | 153.9 (6) |
Cl2—Pt1—P2—C25 | 72.6 (3) | Pt1—P2—C19—C20 | −83.8 (7) |
P1—Pt1—P2—C19 | 15.1 (3) | C25—P2—C19—C24 | −133.6 (7) |
Cl1—Pt1—P2—C19 | −150.1 (6) | C31—P2—C19—C24 | −24.0 (7) |
Cl2—Pt1—P2—C19 | −165.4 (3) | Pt1—P2—C19—C24 | 98.3 (7) |
P1—Pt1—P2—C31 | 135.3 (3) | C24—C19—C20—C21 | 0.6 (12) |
Cl1—Pt1—P2—C31 | −30.0 (6) | P2—C19—C20—C21 | −177.4 (6) |
Cl2—Pt1—P2—C31 | −45.2 (3) | C19—C20—C21—C22 | −1.3 (13) |
C13—P1—C1—C6 | 133.7 (6) | C20—C21—C22—C23 | 1.8 (16) |
C7—P1—C1—C6 | −116.3 (7) | C21—C22—C23—C24 | −1.6 (17) |
Pt1—P1—C1—C6 | 7.8 (7) | C22—C23—C24—C19 | 1.0 (14) |
C13—P1—C1—C2 | −50.2 (8) | C20—C19—C24—C23 | −0.5 (12) |
C7—P1—C1—C2 | 59.9 (8) | P2—C19—C24—C23 | 177.5 (7) |
Pt1—P1—C1—C2 | −176.1 (6) | C19—P2—C25—C26 | −142.3 (6) |
C6—C1—C2—C3 | −4.2 (13) | C31—P2—C25—C26 | 109.8 (7) |
P1—C1—C2—C3 | 179.6 (7) | Pt1—P2—C25—C26 | −9.3 (7) |
C1—C2—C3—C4 | 2.6 (15) | C19—P2—C25—C30 | 37.7 (7) |
C2—C3—C4—C5 | 1.5 (16) | C31—P2—C25—C30 | −70.2 (7) |
C3—C4—C5—C6 | −3.8 (15) | Pt1—P2—C25—C30 | 170.7 (6) |
C4—C5—C6—C1 | 2.2 (13) | C30—C25—C26—C27 | −0.8 (12) |
C2—C1—C6—C5 | 1.8 (12) | P2—C25—C26—C27 | 179.1 (6) |
P1—C1—C6—C5 | 178.2 (7) | C25—C26—C27—C28 | −0.4 (14) |
C1—P1—C7—C8 | 49.8 (7) | C26—C27—C28—C29 | 2.3 (16) |
C13—P1—C7—C8 | 165.7 (6) | C27—C28—C29—C30 | −2.8 (17) |
Pt1—P1—C7—C8 | −72.9 (6) | C28—C29—C30—C25 | 1.5 (15) |
C1—P1—C7—C12 | −129.5 (6) | C26—C25—C30—C29 | 0.3 (12) |
C13—P1—C7—C12 | −13.7 (7) | P2—C25—C30—C29 | −179.6 (7) |
Pt1—P1—C7—C12 | 107.8 (6) | C25—P2—C31—C36 | −174.3 (7) |
C12—C7—C8—C9 | −1.1 (12) | C19—P2—C31—C36 | 79.7 (7) |
P1—C7—C8—C9 | 179.5 (6) | Pt1—P2—C31—C36 | −51.3 (7) |
C7—C8—C9—C10 | 1.2 (13) | C25—P2—C31—C32 | 5.0 (8) |
C8—C9—C10—C11 | −0.8 (13) | C19—P2—C31—C32 | −100.9 (7) |
C9—C10—C11—C12 | 0.3 (13) | Pt1—P2—C31—C32 | 128.1 (6) |
C10—C11—C12—C7 | −0.2 (12) | C36—C31—C32—C33 | 0.9 (12) |
C8—C7—C12—C11 | 0.6 (11) | P2—C31—C32—C33 | −178.5 (6) |
P1—C7—C12—C11 | 180.0 (6) | C31—C32—C33—C34 | −1.4 (13) |
C1—P1—C13—C18 | −174.0 (6) | C32—C33—C34—C35 | 0.0 (13) |
C7—P1—C13—C18 | 78.5 (6) | C33—C34—C35—C36 | 1.9 (14) |
Pt1—P1—C13—C18 | −46.3 (6) | C34—C35—C36—C31 | −2.4 (14) |
C1—P1—C13—C14 | 9.9 (8) | C32—C31—C36—C35 | 1.0 (13) |
C7—P1—C13—C14 | −97.7 (7) | P2—C31—C36—C35 | −179.7 (7) |
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3···Cl1i | 0.93 | 2.80 | 3.670 (10) | 157 |
C37—H37···Cl2ii | 0.98 | 2.43 | 3.390 (15) | 165 |
Symmetry codes: (i) x+1, y, z; (ii) x, −y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [PtCl2(C18H15P)2]·CHCl3 |
Mr | 909.90 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 298 |
a, b, c (Å) | 10.3174 (9), 24.436 (2), 15.6298 (18) |
β (°) | 98.199 (1) |
V (Å3) | 3900.3 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 4.05 |
Crystal size (mm) | 0.38 × 0.35 × 0.18 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.309, 0.530 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18772, 6877, 4984 |
Rint | 0.071 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.048, 0.119, 0.97 |
No. of reflections | 6877 |
No. of parameters | 434 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.89, −1.27 |
Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3···Cl1i | 0.930 | 2.80 | 3.670 (10) | 157 |
C37—H37···Cl2ii | 0.980 | 2.43 | 3.390 (15) | 165 |
Symmetry codes: (i) x+1, y, z; (ii) x, −y+1/2, z−1/2. |
Acknowledgements
The authors thank the University of Jinan (grant No. B0605) and the Key Subject Research Foundation of Shandong Province (grant No. XTD 0704) for support of this study.
References
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cis- and trans-Dichloridobis (triphenylphosphine)platinum(II) are useful to prepare other platinum complexes. The structures of the cis-isomer, either in unsolvated form (Fun et al., 2006) or as an acetone (Anderson et al., 1982) or trichoroform solvate (Al-Fawaz et al., 2004) have been reported. During the course of our studies on platinaborane cluster compounds using the cis-isomer as a starting material, we unexpectedly obtained the yellowish crystals of the title compound (I).
As shown in Fig.1, the platinum centre is four-coordinated and adopts a nearly square planar geometry. The Pt—P bond lengths (2.2481 (17) and 2.2658 (19) Å) and Pt—Cl bond lengths (2.3244 (19) and 2.3548 (17) Å), as well as the bond angles around the Pt atom are similar to those in the above-mentioned structures.
Intermolecular C—H···Cl hydrogen bonding is observed between the chloroform and the chloride (Table 1). Moreover, similar C—H···Cl interaction between one of the phenyl groups and the chloride (Table 1) links the molecules into a one-dimensional chain structure.