cis-Dichloridobis[tris­(4-chloro­phen­yl)phosphane-κP]platinum(II) acetonitrile monosolvate

Meijboom, R.; Kirsten, L.; Mbhele, T.

doi:10.1107/S1600536812037166

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 9| September 2012| Page m1229

doi:10.1107/S1600536812037166

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cis-Dichloridobis[tris(4-chlorophenyl)phosphane-κP]platinum(II) acetonitrile monosolvate

Reinout Meijboom,^a ^* Leo Kirsten ^a and Thapelo Mbhele ^a

^aResearch Centre for Synthesis and Catalysis, Department of Chemistry, University of Johannesburg, PO Box 524 Auckland Park, Johannesburg, 2006, South Africa
^*Correspondence e-mail: rmeijboom@uj.ac.za

(Received 23 July 2012; accepted 28 August 2012; online 31 August 2012)

The title compound, [PtCl₂(C₁₈H₁₂Cl₃P)₂]·C₂H₃N, packs as monomeric units with a square-planar geometry around the Pt^II atom. The two tris(4-chlorophenyl)phosphane ligands are coordinated in a cis orientation, with P—Pt—P and Cl—Pt—Cl angles of 99.36 (2) and 88.02 (2)°, respectively. In the crystal, C—H⋯N interactions are observed between the phenyl rings and the acetonitrile solvent molecules.

Related literature

For a review on related compounds see: Spessard & Miessler (1996 ). For related structures, see: Davis & Meijboom (2011 ); Ogutu & Meijboom (2011 ).

Experimental

Crystal data

[PtCl₂(C₁₈H₁₂Cl₃P)₂]·C₂H₃N
M_r = 1038.24
Monoclinic, P 2₁ /c
a = 13.3604 (16) Å
b = 14.4950 (16) Å
c = 23.007 (3) Å
β = 120.694 (2)°
V = 3831.3 (8) Å³
Z = 4
Mo Kα radiation
μ = 4.34 mm⁻¹
T = 100 K
0.45 × 0.12 × 0.08 mm

Data collection

Bruker X8 APEXII 4K KappaCCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.563, T_max = 0.746
61516 measured reflections
9570 independent reflections
8248 reflections with I > 2σ(I)
R_int = 0.044

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.052
S = 1.03
9570 reflections
452 parameters
H-atom parameters constrained
Δρ_max = 1.05 e Å⁻³
Δρ_min = −0.82 e Å⁻³

Table 1
Selected bond lengths (Å)

Pt1—P1	2.2502 (7)
Pt1—P2	2.2525 (7)
Pt1—Cl2	2.3342 (7)
Pt1—Cl1	2.3454 (7)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C15—H15⋯N1ⁱ	0.93	2.61	3.437 (6)	148
C22—H22⋯N1	0.93	2.59	3.445 (4)	153
C56—H56⋯N1	0.93	2.68	3.523 (4)	151
Symmetry code: (i) -x+2, -y+2, -z+1.

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus and XPREP (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812037166/zq2178sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812037166/zq2178Isup2.hkl

checkCIF report

Comment top

Transition metal complexes containing phosphane, arsine and stibine ligands are widely being investigated in various fields of organometallic chemistry (Spessard & Miessler, 1996). As part of a systematic investigation involving complexes with the general formula trans/cis-[MX₂(L)₂] (M = Pt, Pd or Rh; X = halogen, Me, Ph; L = Group 15 donor ligand), crystals of the title compound were obtained.

[PtCl₂(L)₂] (L = tertiary phosphane, arsine or stibine) complexes can conveniently be prepared by the substitution of 1,5-cyclooctadiene (COD) from [PtCl₂(COD)]. The title compound, cis-[PtCl₂(C₁₈H₁₂Cl₃P)₂] crystallizes in the monoclinic spacegroup P2₁/c, with the Pt atom on a general position. The cis coordination of the two phosphane ligands results in a distorted square-planar geometry around the Pt atom. This distortion is exemplified by the P1–Pt1–P2 bond angle of 99.36 (2) ° and the Cl1–Pt1–Cl2 bond angle of 88.02 (2) °. The Pt—P bond lengths are 2.2502 (7) and 2.2525 (7) Å, and the Pt—Cl bond lengths are 2.3342 (7) and 2.3454 (7) Å, respectively. The title compound crystallized as a solvated complex with one acetonitrile moiety per molecule.

The title compound compares well with other closely related Pt(II) complexes from the literature containing two chloro and two tertiary phosphane ligands in a cis geometry (Davis & Meijboom, 2011; Ogutu & Meijboom, 2011). The Pt–Cl and Pt–P bond lengths compare well with the typical values for complexes of this kind.

In the crystal structure, intermolecular C—H···N interactions are observed between phenyl rings and the acetonitrile solvent molecules.

Related literature top

For a review on related compounds see: Spessard & Miessler (1996). For related structures, see: Davis & Meijboom (2011); Ogutu & Meijboom (2011).

Experimental top

Tris(4-chlorophenyl)phosphane (0.1235 g, 0.34 mmol) was dissolved in ethanol (25 cm³). Pt(COD)Cl₂ (0.05 g, 0.17 mmol) was added to the solution and the mixture was allowed to reflux for 24 h. The solvent was evaporated and a white solid was obtained. Colourless crystals were obtained by recrystallization from acetonitrile, crystals suitable for a single-crystal X-ray diffraction study.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus and XPREP (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

Fig. 1. Representation of the title compound, showing the numbering scheme and displacement ellipsoids (50% probability). For the carbon rings, the first digit refers to ring number, second digit to atom in the ring. Hydrogen atoms omitted for clarity (except when involved in intermolecular interactions).

cis-Dichloridobis[tris(4-chlorophenyl)phosphane-κP]platinum(II) acetonitrile monosolvate top

Crystal data top

[PtCl₂(C₁₈H₁₂Cl₃P)₂]·C₂H₃N	F(000) = 2024
M_r = 1038.24	D_x = 1.800 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9894 reflections
a = 13.3604 (16) Å	θ = 2.5–28.3°
b = 14.4950 (16) Å	µ = 4.34 mm⁻¹
c = 23.007 (3) Å	T = 100 K
β = 120.694 (2)°	Plate, colourless
V = 3831.3 (8) Å³	0.45 × 0.12 × 0.08 mm
Z = 4

Data collection top

Bruker X8 APEXII 4K KappaCCD diffractometer	9570 independent reflections
Radiation source: fine-focus sealed tube	8248 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.044
ϕ and ω scans	θ_max = 28.4°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −17→17
T_min = 0.563, T_max = 0.746	k = −19→13
61516 measured reflections	l = −30→30

Refinement top

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)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.052	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0147P)² + 7.3P] where P = (F_o² + 2F_c²)/3
9570 reflections	(Δ/σ)_max = 0.003
452 parameters	Δρ_max = 1.05 e Å⁻³
0 restraints	Δρ_min = −0.82 e Å⁻³

Crystal data top

[PtCl₂(C₁₈H₁₂Cl₃P)₂]·C₂H₃N	V = 3831.3 (8) Å³
M_r = 1038.24	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 13.3604 (16) Å	µ = 4.34 mm⁻¹
b = 14.4950 (16) Å	T = 100 K
c = 23.007 (3) Å	0.45 × 0.12 × 0.08 mm
β = 120.694 (2)°

Data collection top

Bruker X8 APEXII 4K KappaCCD diffractometer	9570 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	8248 reflections with I > 2σ(I)
T_min = 0.563, T_max = 0.746	R_int = 0.044
61516 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	0 restraints
wR(F²) = 0.052	H-atom parameters constrained
S = 1.03	Δρ_max = 1.05 e Å⁻³
9570 reflections	Δρ_min = −0.82 e Å⁻³
452 parameters

Special details top

Experimental. The intensity data was collected on a Bruker X8 Apex II 4 K Kappa CCD diffractometer using an exposure time of 20 s/frame. A collection frame width of 0.5 ° covering up to θ = 28.4° resulted in 99% completeness accomplished.

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pt1	0.585232 (9)	0.825075 (7)	0.384838 (5)	0.01073 (3)
P1	0.67506 (6)	0.82097 (5)	0.49834 (3)	0.01152 (12)
P2	0.59721 (6)	0.67465 (5)	0.36454 (3)	0.01171 (12)
Cl1	0.48595 (6)	0.83719 (5)	0.26666 (3)	0.01794 (13)
Cl2	0.55243 (6)	0.98251 (5)	0.38877 (3)	0.01816 (13)
Cl3	0.86117 (7)	1.19197 (5)	0.66505 (4)	0.02474 (15)
Cl4	1.17326 (7)	0.63784 (7)	0.66162 (4)	0.0355 (2)
Cl5	0.32156 (6)	0.68604 (5)	0.58652 (3)	0.02180 (15)
Cl6	0.89015 (7)	0.41498 (6)	0.61659 (4)	0.02883 (17)
Cl7	0.89339 (6)	0.61938 (6)	0.22381 (3)	0.02344 (15)
Cl8	0.12024 (7)	0.45956 (6)	0.24527 (4)	0.02725 (16)
C11	0.7229 (2)	0.93258 (19)	0.54104 (12)	0.0137 (5)
C12	0.6572 (2)	0.97964 (19)	0.56300 (13)	0.0159 (5)
H12	0.5848	0.9568	0.5525	0.019*
C13	0.6988 (3)	1.0603 (2)	0.60045 (13)	0.0179 (6)
H13	0.6558	1.0907	0.6161	0.021*
C14	0.8044 (3)	1.09449 (19)	0.61390 (13)	0.0181 (6)
C15	0.8684 (3)	1.0529 (2)	0.58937 (14)	0.0192 (6)
H15	0.9375	1.0791	0.5968	0.023*
C16	0.8277 (2)	0.9711 (2)	0.55335 (13)	0.0169 (5)
H16	0.8707	0.9417	0.5373	0.020*
C21	0.8113 (2)	0.75688 (19)	0.54211 (13)	0.0138 (5)
C22	0.8897 (2)	0.76648 (19)	0.51909 (13)	0.0164 (5)
H22	0.8670	0.7981	0.4791	0.020*
C23	1.0005 (3)	0.7295 (2)	0.55510 (14)	0.0198 (6)
H23	1.0521	0.7361	0.5396	0.024*
C24	1.0335 (3)	0.6825 (2)	0.61467 (14)	0.0208 (6)
C25	0.9574 (3)	0.6697 (2)	0.63771 (14)	0.0198 (6)
H25	0.9803	0.6367	0.6773	0.024*
C26	0.8463 (2)	0.70648 (19)	0.60112 (13)	0.0160 (5)
H26	0.7943	0.6974	0.6161	0.019*
C31	0.5777 (2)	0.77817 (18)	0.52576 (13)	0.0133 (5)
C32	0.4669 (2)	0.74861 (19)	0.47758 (13)	0.0147 (5)
H32	0.4456	0.7478	0.4323	0.018*
C33	0.3873 (2)	0.72032 (19)	0.49570 (13)	0.0159 (5)
H33	0.3133	0.7006	0.4631	0.019*
C34	0.4203 (2)	0.72202 (19)	0.56347 (13)	0.0152 (5)
C35	0.5291 (3)	0.7526 (2)	0.61265 (13)	0.0171 (6)
H35	0.5494	0.7541	0.6578	0.020*
C36	0.6073 (2)	0.78100 (19)	0.59372 (13)	0.0151 (5)
H36	0.6805	0.8022	0.6264	0.018*
C41	0.6804 (2)	0.59576 (18)	0.43507 (13)	0.0138 (5)
C42	0.6337 (2)	0.56608 (19)	0.47427 (13)	0.0156 (5)
H42	0.5589	0.5841	0.4625	0.019*
C43	0.6973 (3)	0.5104 (2)	0.53008 (14)	0.0186 (6)
H43	0.6665	0.4919	0.5565	0.022*
C44	0.8074 (3)	0.4829 (2)	0.54597 (13)	0.0187 (6)
C45	0.8551 (3)	0.5093 (2)	0.50748 (14)	0.0193 (6)
H45	0.9291	0.4894	0.5188	0.023*
C46	0.7910 (2)	0.5658 (2)	0.45178 (13)	0.0169 (5)
H46	0.8220	0.5837	0.4254	0.020*
C51	0.6685 (2)	0.66152 (18)	0.31555 (12)	0.0134 (5)
C52	0.6501 (3)	0.58608 (19)	0.27372 (13)	0.0167 (5)
H52	0.5916	0.5439	0.2650	0.020*
C53	0.7187 (3)	0.5735 (2)	0.24493 (13)	0.0191 (6)
H53	0.7063	0.5234	0.2168	0.023*
C54	0.8056 (2)	0.6365 (2)	0.25859 (13)	0.0178 (6)
C55	0.8237 (2)	0.7135 (2)	0.29826 (13)	0.0174 (6)
H55	0.8812	0.7561	0.3060	0.021*
C56	0.7539 (3)	0.7259 (2)	0.32641 (13)	0.0173 (6)
H56	0.7643	0.7777	0.3528	0.021*
C61	0.4568 (2)	0.61567 (19)	0.32269 (13)	0.0143 (5)
C62	0.4541 (3)	0.5194 (2)	0.31750 (13)	0.0173 (5)
H62	0.5228	0.4871	0.3314	0.021*
C63	0.3497 (3)	0.4716 (2)	0.29174 (14)	0.0191 (6)
H63	0.3477	0.4078	0.2870	0.023*
C64	0.2487 (2)	0.5204 (2)	0.27325 (14)	0.0185 (6)
C65	0.2489 (3)	0.6155 (2)	0.27701 (14)	0.0198 (6)
H65	0.1799	0.6473	0.2635	0.024*
C66	0.3528 (2)	0.66336 (19)	0.30109 (13)	0.0162 (5)
H66	0.3532	0.7275	0.3028	0.019*
N1	0.8740 (3)	0.9362 (2)	0.40990 (16)	0.0389 (7)
C1	0.8277 (3)	1.0050 (3)	0.39790 (17)	0.0321 (8)
C2	0.7684 (4)	1.0938 (3)	0.3826 (2)	0.0440 (10)
H2A	0.6899	1.0868	0.3457	0.066*
H2B	0.8087	1.1373	0.3703	0.066*
H2C	0.7675	1.1159	0.4217	0.066*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt1	0.01178 (5)	0.01036 (5)	0.00961 (4)	0.00060 (4)	0.00513 (4)	0.00080 (4)
P1	0.0109 (3)	0.0134 (3)	0.0096 (3)	−0.0004 (3)	0.0047 (2)	−0.0002 (2)
P2	0.0129 (3)	0.0107 (3)	0.0107 (3)	0.0003 (3)	0.0054 (3)	0.0004 (2)
Cl1	0.0215 (3)	0.0192 (3)	0.0107 (3)	0.0019 (3)	0.0065 (3)	0.0031 (2)
Cl2	0.0228 (3)	0.0122 (3)	0.0180 (3)	0.0039 (3)	0.0094 (3)	0.0012 (2)
Cl3	0.0278 (4)	0.0162 (4)	0.0257 (3)	−0.0043 (3)	0.0104 (3)	−0.0080 (3)
Cl4	0.0181 (4)	0.0547 (6)	0.0332 (4)	0.0156 (4)	0.0128 (3)	0.0206 (4)
Cl5	0.0199 (3)	0.0288 (4)	0.0209 (3)	−0.0030 (3)	0.0135 (3)	0.0013 (3)
Cl6	0.0252 (4)	0.0309 (4)	0.0222 (3)	0.0049 (3)	0.0062 (3)	0.0138 (3)
Cl7	0.0183 (3)	0.0373 (4)	0.0163 (3)	0.0059 (3)	0.0100 (3)	0.0005 (3)
Cl8	0.0200 (4)	0.0290 (4)	0.0355 (4)	−0.0098 (3)	0.0162 (3)	−0.0115 (3)
C11	0.0142 (13)	0.0126 (13)	0.0113 (11)	−0.0004 (10)	0.0044 (10)	0.0003 (9)
C12	0.0138 (13)	0.0143 (13)	0.0173 (12)	0.0002 (11)	0.0062 (11)	0.0019 (10)
C13	0.0206 (15)	0.0149 (14)	0.0176 (13)	0.0030 (11)	0.0093 (12)	0.0013 (10)
C14	0.0212 (15)	0.0136 (14)	0.0132 (12)	−0.0020 (11)	0.0044 (11)	−0.0013 (10)
C15	0.0173 (14)	0.0198 (15)	0.0195 (13)	−0.0045 (12)	0.0088 (12)	−0.0025 (11)
C16	0.0185 (14)	0.0180 (14)	0.0169 (12)	−0.0017 (12)	0.0109 (11)	−0.0024 (10)
C21	0.0129 (13)	0.0137 (13)	0.0132 (12)	−0.0012 (10)	0.0054 (10)	−0.0018 (10)
C22	0.0191 (14)	0.0164 (14)	0.0142 (12)	0.0004 (11)	0.0088 (11)	0.0002 (10)
C23	0.0165 (14)	0.0244 (16)	0.0199 (13)	0.0004 (12)	0.0104 (12)	0.0014 (11)
C24	0.0143 (14)	0.0225 (16)	0.0203 (13)	0.0025 (12)	0.0049 (11)	0.0029 (12)
C25	0.0196 (14)	0.0219 (15)	0.0154 (12)	0.0029 (12)	0.0071 (11)	0.0039 (11)
C26	0.0163 (14)	0.0167 (13)	0.0149 (12)	−0.0009 (11)	0.0080 (11)	−0.0004 (10)
C31	0.0153 (13)	0.0119 (13)	0.0123 (11)	0.0015 (11)	0.0069 (10)	0.0010 (9)
C32	0.0165 (14)	0.0157 (14)	0.0104 (11)	0.0011 (11)	0.0059 (11)	0.0006 (10)
C33	0.0132 (13)	0.0155 (14)	0.0154 (12)	−0.0003 (11)	0.0047 (11)	0.0016 (10)
C34	0.0174 (14)	0.0113 (13)	0.0201 (13)	−0.0005 (11)	0.0120 (11)	0.0017 (10)
C35	0.0211 (15)	0.0175 (14)	0.0133 (12)	0.0014 (12)	0.0092 (11)	0.0008 (10)
C36	0.0146 (13)	0.0163 (14)	0.0122 (12)	−0.0012 (11)	0.0052 (10)	−0.0014 (10)
C41	0.0169 (14)	0.0100 (12)	0.0139 (12)	−0.0003 (10)	0.0074 (11)	−0.0003 (9)
C42	0.0156 (14)	0.0121 (13)	0.0186 (13)	0.0007 (11)	0.0084 (11)	0.0000 (10)
C43	0.0229 (15)	0.0169 (14)	0.0176 (13)	−0.0033 (12)	0.0115 (12)	0.0011 (11)
C44	0.0196 (14)	0.0150 (14)	0.0154 (12)	0.0020 (12)	0.0045 (11)	0.0054 (10)
C45	0.0147 (14)	0.0195 (15)	0.0196 (13)	0.0023 (12)	0.0056 (11)	0.0041 (11)
C46	0.0166 (14)	0.0170 (14)	0.0165 (12)	−0.0001 (11)	0.0080 (11)	0.0009 (10)
C51	0.0146 (13)	0.0130 (13)	0.0116 (11)	0.0027 (10)	0.0061 (10)	0.0012 (9)
C52	0.0190 (14)	0.0160 (14)	0.0139 (12)	−0.0002 (11)	0.0075 (11)	−0.0008 (10)
C53	0.0238 (15)	0.0180 (14)	0.0132 (12)	0.0026 (12)	0.0078 (12)	−0.0037 (10)
C54	0.0176 (14)	0.0236 (15)	0.0110 (12)	0.0069 (12)	0.0065 (11)	0.0035 (10)
C55	0.0148 (14)	0.0186 (14)	0.0176 (13)	−0.0005 (11)	0.0073 (11)	0.0018 (11)
C56	0.0222 (15)	0.0142 (14)	0.0162 (12)	−0.0013 (12)	0.0104 (12)	−0.0021 (10)
C61	0.0138 (13)	0.0154 (13)	0.0119 (11)	−0.0016 (11)	0.0054 (10)	−0.0019 (10)
C62	0.0175 (14)	0.0158 (14)	0.0179 (12)	0.0012 (11)	0.0086 (11)	−0.0007 (11)
C63	0.0209 (15)	0.0136 (14)	0.0212 (13)	−0.0026 (12)	0.0097 (12)	−0.0031 (11)
C64	0.0170 (14)	0.0222 (15)	0.0178 (13)	−0.0070 (12)	0.0100 (11)	−0.0059 (11)
C65	0.0148 (14)	0.0218 (15)	0.0215 (14)	0.0024 (12)	0.0083 (12)	−0.0038 (11)
C66	0.0160 (13)	0.0146 (14)	0.0159 (12)	0.0016 (11)	0.0065 (11)	−0.0011 (10)
N1	0.048 (2)	0.0372 (19)	0.0442 (18)	−0.0025 (16)	0.0331 (17)	0.0010 (14)
C1	0.043 (2)	0.031 (2)	0.0359 (18)	−0.0123 (17)	0.0299 (17)	−0.0069 (15)
C2	0.060 (3)	0.031 (2)	0.056 (2)	−0.0096 (19)	0.040 (2)	−0.0040 (17)

Geometric parameters (Å, º) top

Pt1—P1	2.2502 (7)	C33—H33	0.9300
Pt1—P2	2.2525 (7)	C34—C35	1.382 (4)
Pt1—Cl2	2.3342 (7)	C35—C36	1.385 (4)
Pt1—Cl1	2.3454 (7)	C35—H35	0.9300
P1—C31	1.820 (3)	C36—H36	0.9300
P1—C21	1.821 (3)	C41—C46	1.393 (4)
P1—C11	1.830 (3)	C41—C42	1.400 (4)
P2—C51	1.820 (3)	C42—C43	1.381 (4)
P2—C41	1.826 (3)	C42—H42	0.9300
P2—C61	1.826 (3)	C43—C44	1.381 (4)
Cl3—C14	1.745 (3)	C43—H43	0.9300
Cl4—C24	1.736 (3)	C44—C45	1.384 (4)
Cl5—C34	1.734 (3)	C45—C46	1.388 (4)
Cl6—C44	1.732 (3)	C45—H45	0.9300
Cl7—C54	1.742 (3)	C46—H46	0.9300
Cl8—C64	1.735 (3)	C51—C52	1.393 (4)
C11—C12	1.394 (4)	C51—C56	1.394 (4)
C11—C16	1.396 (4)	C52—C53	1.390 (4)
C12—C13	1.390 (4)	C52—H52	0.9300
C12—H12	0.9300	C53—C54	1.381 (4)
C13—C14	1.374 (4)	C53—H53	0.9300
C13—H13	0.9300	C54—C55	1.383 (4)
C14—C15	1.381 (4)	C55—C56	1.392 (4)
C15—C16	1.388 (4)	C55—H55	0.9300
C15—H15	0.9300	C56—H56	0.9300
C16—H16	0.9300	C61—C66	1.396 (4)
C21—C26	1.395 (4)	C61—C62	1.400 (4)
C21—C22	1.402 (4)	C62—C63	1.390 (4)
C22—C23	1.383 (4)	C62—H62	0.9300
C22—H22	0.9300	C63—C64	1.384 (4)
C23—C24	1.385 (4)	C63—H63	0.9300
C23—H23	0.9300	C64—C65	1.381 (4)
C24—C25	1.379 (4)	C65—C66	1.390 (4)
C25—C26	1.386 (4)	C65—H65	0.9300
C25—H25	0.9300	C66—H66	0.9300
C26—H26	0.9300	N1—C1	1.130 (5)
C31—C32	1.388 (4)	C1—C2	1.458 (6)
C31—C36	1.404 (3)	C2—H2A	0.9600
C32—C33	1.388 (4)	C2—H2B	0.9600
C32—H32	0.9300	C2—H2C	0.9600
C33—C34	1.387 (4)

P1—Pt1—P2	99.36 (2)	C34—C35—H35	120.5
P1—Pt1—Cl2	88.87 (2)	C36—C35—H35	120.5
P2—Pt1—Cl2	171.49 (2)	C35—C36—C31	120.8 (3)
P1—Pt1—Cl1	176.65 (3)	C35—C36—H36	119.6
P2—Pt1—Cl1	83.69 (2)	C31—C36—H36	119.6
Cl2—Pt1—Cl1	88.02 (2)	C46—C41—C42	119.0 (2)
C31—P1—C21	108.88 (12)	C46—C41—P2	121.3 (2)
C31—P1—C11	103.33 (12)	C42—C41—P2	119.7 (2)
C21—P1—C11	100.23 (12)	C43—C42—C41	120.9 (3)
C31—P1—Pt1	111.04 (9)	C43—C42—H42	119.5
C21—P1—Pt1	116.46 (8)	C41—C42—H42	119.5
C11—P1—Pt1	115.65 (8)	C42—C43—C44	118.7 (3)
C51—P2—C41	102.20 (12)	C42—C43—H43	120.6
C51—P2—C61	110.27 (12)	C44—C43—H43	120.6
C41—P2—C61	99.83 (13)	C43—C44—C45	121.8 (3)
C51—P2—Pt1	110.17 (9)	C43—C44—Cl6	119.8 (2)
C41—P2—Pt1	119.83 (9)	C45—C44—Cl6	118.4 (2)
C61—P2—Pt1	113.57 (9)	C44—C45—C46	119.0 (3)
C12—C11—C16	118.9 (3)	C44—C45—H45	120.5
C12—C11—P1	121.0 (2)	C46—C45—H45	120.5
C16—C11—P1	120.1 (2)	C45—C46—C41	120.5 (3)
C13—C12—C11	120.7 (3)	C45—C46—H46	119.8
C13—C12—H12	119.7	C41—C46—H46	119.8
C11—C12—H12	119.7	C52—C51—C56	119.3 (2)
C14—C13—C12	118.9 (3)	C52—C51—P2	123.1 (2)
C14—C13—H13	120.6	C56—C51—P2	117.26 (19)
C12—C13—H13	120.6	C53—C52—C51	120.3 (3)
C13—C14—C15	122.0 (3)	C53—C52—H52	119.8
C13—C14—Cl3	119.1 (2)	C51—C52—H52	119.8
C15—C14—Cl3	118.9 (2)	C54—C53—C52	119.2 (3)
C14—C15—C16	118.8 (3)	C54—C53—H53	120.4
C14—C15—H15	120.6	C52—C53—H53	120.4
C16—C15—H15	120.6	C53—C54—C55	121.8 (3)
C15—C16—C11	120.6 (3)	C53—C54—Cl7	119.1 (2)
C15—C16—H16	119.7	C55—C54—Cl7	119.1 (2)
C11—C16—H16	119.7	C54—C55—C56	118.6 (3)
C26—C21—C22	118.4 (3)	C54—C55—H55	120.7
C26—C21—P1	123.3 (2)	C56—C55—H55	120.7
C22—C21—P1	118.0 (2)	C55—C56—C51	120.7 (3)
C23—C22—C21	120.9 (2)	C55—C56—H56	119.6
C23—C22—H22	119.6	C51—C56—H56	119.6
C21—C22—H22	119.6	C66—C61—C62	119.1 (3)
C22—C23—C24	119.1 (3)	C66—C61—P2	121.6 (2)
C22—C23—H23	120.4	C62—C61—P2	119.1 (2)
C24—C23—H23	120.4	C63—C62—C61	120.6 (3)
C25—C24—C23	121.5 (3)	C63—C62—H62	119.7
C25—C24—Cl4	118.7 (2)	C61—C62—H62	119.7
C23—C24—Cl4	119.8 (2)	C64—C63—C62	119.0 (3)
C24—C25—C26	119.1 (3)	C64—C63—H63	120.5
C24—C25—H25	120.5	C62—C63—H63	120.5
C26—C25—H25	120.5	C65—C64—C63	121.4 (3)
C25—C26—C21	121.1 (3)	C65—C64—Cl8	120.0 (2)
C25—C26—H26	119.5	C63—C64—Cl8	118.6 (2)
C21—C26—H26	119.5	C64—C65—C66	119.5 (3)
C32—C31—C36	118.5 (2)	C64—C65—H65	120.3
C32—C31—P1	119.19 (19)	C66—C65—H65	120.3
C36—C31—P1	122.1 (2)	C65—C66—C61	120.3 (3)
C33—C32—C31	121.3 (2)	C65—C66—H66	119.8
C33—C32—H32	119.3	C61—C66—H66	119.8
C31—C32—H32	119.3	N1—C1—C2	179.8 (7)
C34—C33—C32	118.7 (3)	C1—C2—H2A	109.5
C34—C33—H33	120.7	C1—C2—H2B	109.5
C32—C33—H33	120.7	H2A—C2—H2B	109.5
C35—C34—C33	121.6 (2)	C1—C2—H2C	109.5
C35—C34—Cl5	119.5 (2)	H2A—C2—H2C	109.5
C33—C34—Cl5	118.9 (2)	H2B—C2—H2C	109.5
C34—C35—C36	119.0 (2)

P2—Pt1—P1—C31	−78.88 (10)	C33—C34—C35—C36	−0.9 (4)
P2—Pt1—P1—C21	46.48 (10)	Cl5—C34—C35—C36	179.9 (2)
Cl2—Pt1—P1—C21	−135.67 (10)	C34—C35—C36—C31	−0.6 (4)
P2—Pt1—P1—C11	163.81 (10)	C32—C31—C36—C35	1.7 (4)
Cl2—Pt1—P1—C11	−18.35 (10)	P1—C31—C36—C35	176.4 (2)
P1—Pt1—P2—C51	−124.32 (9)	C51—P2—C41—C46	19.2 (3)
P1—Pt1—P2—C41	−6.29 (11)	C61—P2—C41—C46	132.6 (2)
Cl1—Pt1—P2—C41	175.10 (11)	Pt1—P2—C41—C46	−102.8 (2)
P1—Pt1—P2—C61	111.42 (9)	C51—P2—C41—C42	−162.1 (2)
Cl1—Pt1—P2—C61	−67.19 (9)	C61—P2—C41—C42	−48.7 (2)
C31—P1—C11—C12	−22.4 (2)	Pt1—P2—C41—C42	75.8 (2)
C21—P1—C11—C12	−134.8 (2)	C46—C41—C42—C43	2.2 (4)
Pt1—P1—C11—C12	99.2 (2)	P2—C41—C42—C43	−176.5 (2)
C31—P1—C11—C16	156.3 (2)	C41—C42—C43—C44	−1.2 (4)
C21—P1—C11—C16	43.9 (2)	C42—C43—C44—C45	−0.2 (4)
Pt1—P1—C11—C16	−82.1 (2)	C42—C43—C44—Cl6	178.8 (2)
C16—C11—C12—C13	−4.3 (4)	C43—C44—C45—C46	0.7 (4)
P1—C11—C12—C13	174.4 (2)	Cl6—C44—C45—C46	−178.3 (2)
C11—C12—C13—C14	1.8 (4)	C44—C45—C46—C41	0.3 (4)
C12—C13—C14—C15	2.3 (4)	C42—C41—C46—C45	−1.7 (4)
C12—C13—C14—Cl3	−176.3 (2)	P2—C41—C46—C45	176.9 (2)
C13—C14—C15—C16	−3.8 (4)	C41—P2—C51—C52	77.3 (2)
Cl3—C14—C15—C16	174.8 (2)	C61—P2—C51—C52	−28.2 (3)
C14—C15—C16—C11	1.2 (4)	Pt1—P2—C51—C52	−154.3 (2)
C12—C11—C16—C15	2.7 (4)	C41—P2—C51—C56	−96.1 (2)
P1—C11—C16—C15	−176.0 (2)	C61—P2—C51—C56	158.5 (2)
C31—P1—C21—C26	−18.6 (3)	Pt1—P2—C51—C56	32.3 (2)
C11—P1—C21—C26	89.4 (2)	C56—C51—C52—C53	2.1 (4)
Pt1—P1—C21—C26	−145.1 (2)	P2—C51—C52—C53	−171.1 (2)
C31—P1—C21—C22	168.0 (2)	C51—C52—C53—C54	0.3 (4)
C11—P1—C21—C22	−84.0 (2)	C52—C53—C54—C55	−2.3 (4)
Pt1—P1—C21—C22	41.6 (2)	C52—C53—C54—Cl7	178.7 (2)
C26—C21—C22—C23	−2.1 (4)	C53—C54—C55—C56	1.7 (4)
P1—C21—C22—C23	171.6 (2)	Cl7—C54—C55—C56	−179.3 (2)
C21—C22—C23—C24	0.0 (4)	C54—C55—C56—C51	0.8 (4)
C22—C23—C24—C25	1.8 (5)	C52—C51—C56—C55	−2.7 (4)
C22—C23—C24—Cl4	−178.6 (2)	P2—C51—C56—C55	170.9 (2)
C23—C24—C25—C26	−1.5 (5)	C51—P2—C61—C66	−119.2 (2)
Cl4—C24—C25—C26	178.9 (2)	C41—P2—C61—C66	133.8 (2)
C24—C25—C26—C21	−0.7 (4)	Pt1—P2—C61—C66	5.0 (2)
C22—C21—C26—C25	2.5 (4)	C51—P2—C61—C62	66.5 (2)
P1—C21—C26—C25	−170.9 (2)	C41—P2—C61—C62	−40.5 (2)
C21—P1—C31—C32	−125.8 (2)	Pt1—P2—C61—C62	−169.33 (18)
C11—P1—C31—C32	128.3 (2)	C66—C61—C62—C63	−0.6 (4)
Pt1—P1—C31—C32	3.7 (2)	P2—C61—C62—C63	173.9 (2)
C21—P1—C31—C36	59.5 (3)	C61—C62—C63—C64	−2.0 (4)
C11—P1—C31—C36	−46.4 (3)	C62—C63—C64—C65	2.9 (4)
Pt1—P1—C31—C36	−171.0 (2)	C62—C63—C64—Cl8	−176.7 (2)
C36—C31—C32—C33	−1.4 (4)	C63—C64—C65—C66	−1.3 (4)
P1—C31—C32—C33	−176.3 (2)	Cl8—C64—C65—C66	178.4 (2)
C31—C32—C33—C34	0.0 (4)	C64—C65—C66—C61	−1.4 (4)
C32—C33—C34—C35	1.2 (4)	C62—C61—C66—C65	2.3 (4)
C32—C33—C34—Cl5	−179.6 (2)	P2—C61—C66—C65	−172.0 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C15—H15···N1ⁱ	0.93	2.61	3.437 (6)	148
C22—H22···N1	0.93	2.59	3.445 (4)	153
C56—H56···N1	0.93	2.68	3.523 (4)	151

Symmetry code: (i) −x+2, −y+2, −z+1.

Experimental details

Crystal data
Chemical formula	[PtCl₂(C₁₈H₁₂Cl₃P)₂]·C₂H₃N
M_r	1038.24
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	100
a, b, c (Å)	13.3604 (16), 14.4950 (16), 23.007 (3)
β (°)	120.694 (2)
V (Å³)	3831.3 (8)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	4.34
Crystal size (mm)	0.45 × 0.12 × 0.08

Data collection
Diffractometer	Bruker X8 APEXII 4K KappaCCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.563, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	61516, 9570, 8248
R_int	0.044
(sin θ/λ)_max (Å⁻¹)	0.669

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.052, 1.03
No. of reflections	9570
No. of parameters	452
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.05, −0.82

Computer programs: APEX2 (Bruker, 2007), SAINT-Plus (Bruker, 2007), SAINT-Plus and XPREP (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2005), WinGX (Farrugia, 1999).

Selected bond lengths (Å) top

Pt1—P1	2.2502 (7)	Pt1—Cl2	2.3342 (7)
Pt1—P2	2.2525 (7)	Pt1—Cl1	2.3454 (7)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C15—H15···N1ⁱ	0.93	2.61	3.437 (6)	148
C22—H22···N1	0.93	2.59	3.445 (4)	153
C56—H56···N1	0.93	2.68	3.523 (4)	151

Symmetry code: (i) −x+2, −y+2, −z+1.

Acknowledgements

Financial assistance from the South African National Research Foundation (SA NRF), the Research Fund of the University of Johannesburg, TESP and SASOL is gratefully acknowledged.

References

Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2007). APEX2, SAINT-Plus, XPREP and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Davis, W. L. & Meijboom, R. (2011). Acta Cryst. E67, m1800. Web of Science CSD CrossRef IUCr Journals Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Ogutu, H. & Meijboom, R. (2011). Acta Cryst. E67, m1662. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spessard, G. O. & Miessler, G. L. (1996). Organometallic Chemistry, pp. 131–135. New Jersey: Prentice Hall. Google Scholar

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Volume 68| Part 9| September 2012| Page m1229

doi:10.1107/S1600536812037166

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

cis-Di­chloridobis[tris­­(4-chloro­phen­yl)phosphane-κP]platinum(II) aceto­nitrile monosolvate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

cis-Dichloridobis[tris(4-chlorophenyl)phosphane-κP]platinum(II) acetonitrile monosolvate