trans-Dichloridobis[tris­(4-meth­oxy­lphen­yl)phosphane-κP]platinum(II) acetone disolvate

Muller, A.

doi:10.1107/S1600536812045643

metal-organic compounds

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Volume 68| Part 12| December 2012| Page m1475

doi:10.1107/S1600536812045643

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trans-Dichloridobis[tris(4-methoxylphenyl)phosphane-κP]platinum(II) acetone disolvate

Alfred Muller ^a ^*

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

(Received 24 October 2012; accepted 5 November 2012; online 14 November 2012)

In the title compound, [PtCl₂(C₂₁H₂₁O₃P)₂]·2C₃H₆O, the asymmetric unit contains a Pt^II ion situated on an inversion center, one chloride anion, one tris(4-methoxylphenyl)phosphane (L) ligand and one acetone solvent molecule. The Pt^II ion is coordinated by two P atoms [Pt—P = 2.3196 (5) Å] from two L ligands and two chloride anions [Pt—Cl = 2.3075 (5) Å] in a distorted square-planar geometry with P—Pt—Cl angles of 88.016 (16) and 91.984 (16)°. The effective cone angle of the phosphane ligand was calculated to be 156°. Weak C—H⋯O and C—H⋯Cl hydrogen bonds hold molecules together.

Related literature

For related compounds, see: Spessard & Miessler (1996 ); van Blerk & Holzapfel (2009 ); Muller & Meijboom (2010 ). For background to cone angles, see: Tolman (1977 ); Otto (2001 ).

Experimental

Crystal data

[PtCl₂(C₂₁H₂₁O₃P)₂]·2C₃H₆O
M_r = 1086.84
Triclinic, $[P \overline 1]$
a = 10.486 (1) Å
b = 11.0360 (11) Å
c = 11.3630 (11) Å
α = 85.787 (2)°
β = 63.924 (2)°
γ = 78.370 (2)°
V = 1156.70 (19) Å³
Z = 1
Mo Kα radiation
μ = 3.27 mm⁻¹
T = 100 K
0.19 × 0.13 × 0.11 mm

Data collection

Bruker APEX DUO 4K CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008 ) T_min = 0.679, T_max = 0.746
31470 measured reflections
5799 independent reflections
5763 reflections with I > 2σ(I)
R_int = 0.042

Refinement

R[F² > 2σ(F²)] = 0.019
wR(F²) = 0.040
S = 1.04
5799 reflections
282 parameters
H-atom parameters constrained
Δρ_max = 0.68 e Å⁻³
Δρ_min = −0.51 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C6—H6⋯Cl1	0.95	2.7	3.493 (2)	142
C10—H10⋯O1Sⁱ	0.95	2.57	3.235 (3)	127
C12—H12⋯O2ⁱⁱ	0.95	2.53	3.357 (2)	146
Symmetry codes: (i) -x, -y+1, -z+1; (ii) -x+1, -y+2, -z.

Data collection: APEX2 (Bruker, 2011 ); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT and XPREP (Bruker, 2008); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 ); software used to prepare material for publication: publCIF (Westrip, 2010 ) and WinGX (Farrugia, 2012 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536812045643/cv5352sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812045643/cv5352Isup2.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 (Muller & Meijboom, 2010; van Blerk & Holzapfel, 2009) involving complexes with the general formula trans/cis-[MX₂(L)₂] (M = Pt or Pd; X = halogen, Me, Ph; L = Group 15 donor ligand), crystals of the title compound were obtained by the substitution of 1,5-cyclooctadiene (COD) with the tris(4-methoxyphenyl)phosphane from cis-[PtCl₂(COD)].

Molecules of the title compound (Fig. 1) crystallizes in the P1 (Z = 1) space group with the Pt atom on an inversion center and two acetone solvate molecules accompanying it. Each pair of equivalent ligands is in a trans orientation with only slight distortion observed in the P—Pt—Cl angles from the ideal square-planar geometry. The orientation of the phosphanes is such that there is one 4-methoxyphenyl substituent close to the coordination plane, i.e. Cl1—Pt1—P1—C8 = -14.92 (7)°. The steric demand of phosphane ligand can be described by using an adaptation of the Tolman cone angle model (Tolman, 1977). By adjusting the Pt—P bond distance to 2.28 Å, and using the geometry from the title compound, an effective cone angle value (Otto, 2001) of 156° was obtained. The packing of the title compound shows weak C—H···Cl/O interactions (Table 1).

Related literature top

For related compounds, see: Spessard & Miessler (1996); van Blerk & Holzapfel (2009); Muller & Meijboom (2010). For background to cone angles, see: Tolman (1977); Otto (2001).

Experimental top

trans-Dichloridobis[tris(4-methoxylphenyl)phosphane]platinum(II) was prepared from reaction of cis-[PtCl₂(1,5-cyclooctadiene)] (10.8 mg, 0.0289 mmol) and tris(4-methoxyphenyl)phosphane (10 mg, 0.0259 mmol) in acetone. The mixture was refluxed for 4hrs, then filtered and crystals suitable for a single-crystal X-ray diffraction study was obtained by recrystallization from acetone. Analytical data: ³¹P {H} NMR (CDCl₃, 161.99 MHz): δ = 16.4 (t, ¹J(³¹P-¹⁹⁵Pt) = 2586 Hz).

Computing details top

Data collection: APEX2 (Bruker, 2011); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT and XPREP (Bruker, 2008); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: publCIF (Westrip, 2010) and WinGX (Farrugia, 2012).

Figures top

Fig. 1. A view of the title complex, showing the atom-numbering scheme and 50% probability displacement ellipsoids [symmetry code: (') 1 - x, 1 - y, 1 - z]. Hydrogen atoms and solvent molecules were omitted for clarity.

trans-Dichloridobis[tris(4-methoxylphenyl)phosphane- κP]platinum(II) acetone disolvate top

Crystal data top

[PtCl₂(C₂₁H₂₁O₃P)₂]·2C₃H₆O	Z = 1
M_r = 1086.84	F(000) = 548
Triclinic, P1	D_x = 1.56 Mg m⁻³
a = 10.486 (1) Å	Mo Kα radiation, λ = 0.71069 Å
b = 11.0360 (11) Å	Cell parameters from 9903 reflections
c = 11.3630 (11) Å	θ = 2.2–32.7°
α = 85.787 (2)°	µ = 3.27 mm⁻¹
β = 63.924 (2)°	T = 100 K
γ = 78.370 (2)°	Rectangle, colourless
V = 1156.70 (19) Å³	0.19 × 0.13 × 0.11 mm

Data collection top

Bruker APEX DUO 4K CCD diffractometer	5799 independent reflections
Graphite monochromator	5763 reflections with I > 2σ(I)
Detector resolution: 8.4 pixels mm^-1	R_int = 0.042
ϕ and ω scans	θ_max = 28.4°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −13→14
T_min = 0.679, T_max = 0.746	k = −14→14
31470 measured reflections	l = −15→15

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)] = 0.019	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.040	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.016P)² + 0.4415P] where P = (F_o² + 2F_c²)/3
5799 reflections	(Δ/σ)_max = 0.001
282 parameters	Δρ_max = 0.68 e Å⁻³
0 restraints	Δρ_min = −0.51 e Å⁻³

Crystal data top

[PtCl₂(C₂₁H₂₁O₃P)₂]·2C₃H₆O	γ = 78.370 (2)°
M_r = 1086.84	V = 1156.70 (19) Å³
Triclinic, P1	Z = 1
a = 10.486 (1) Å	Mo Kα radiation
b = 11.0360 (11) Å	µ = 3.27 mm⁻¹
c = 11.3630 (11) Å	T = 100 K
α = 85.787 (2)°	0.19 × 0.13 × 0.11 mm
β = 63.924 (2)°

Data collection top

Bruker APEX DUO 4K CCD diffractometer	5799 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2008)	5763 reflections with I > 2σ(I)
T_min = 0.679, T_max = 0.746	R_int = 0.042
31470 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.019	0 restraints
wR(F²) = 0.040	H-atom parameters constrained
S = 1.04	Δρ_max = 0.68 e Å⁻³
5799 reflections	Δρ_min = −0.51 e Å⁻³
282 parameters

Special details top

Experimental. The intensity data was collected on a Bruker Apex DUO 4 K CCD diffractometer using an exposure time of 20 s/frame. A total of 2352 frames were collected with a frame width of 0.5° covering up to θ = 28.66° with 99.3% completeness accomplished.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq
Pt1	0.5	0.5	0.5	0.00927 (3)
Cl1	0.52266 (5)	0.28766 (4)	0.49934 (4)	0.01424 (9)
P1	0.49557 (5)	0.49994 (4)	0.29769 (5)	0.01069 (9)
O2	0.31108 (15)	0.97824 (13)	0.08244 (15)	0.0210 (3)
O3	0.06877 (15)	0.21272 (14)	0.30254 (14)	0.0212 (3)
O1	1.08770 (15)	0.32059 (15)	−0.12406 (14)	0.0225 (3)
O1S	0.08106 (17)	0.10043 (16)	0.63614 (17)	0.0353 (4)
C20	0.4006 (2)	0.32915 (18)	0.19434 (19)	0.0146 (4)
H20	0.4908	0.3216	0.1189	0.017*
C6	0.7760 (2)	0.35873 (19)	0.1910 (2)	0.0190 (4)
H6	0.7519	0.3277	0.2769	0.023*
C19	0.2972 (2)	0.26563 (18)	0.1987 (2)	0.0174 (4)
H19	0.3177	0.2136	0.1272	0.021*
C18	0.1634 (2)	0.27795 (18)	0.3078 (2)	0.0153 (4)
C5	0.9129 (2)	0.3196 (2)	0.0926 (2)	0.0220 (5)
H5	0.9821	0.2622	0.1112	0.026*
C17	0.1346 (2)	0.35162 (18)	0.4140 (2)	0.0160 (4)
H17	0.0441	0.3598	0.4891	0.019*
C1	0.67224 (19)	0.44348 (17)	0.16598 (18)	0.0128 (4)
C8	0.43388 (19)	0.64708 (17)	0.23846 (18)	0.0123 (4)
C3	0.8488 (2)	0.44858 (19)	−0.06024 (19)	0.0165 (4)
H3	0.8737	0.4804	−0.1459	0.02*
C15	0.37324 (19)	0.40419 (17)	0.29972 (18)	0.0124 (4)
C12	0.4759 (2)	0.84717 (19)	0.14382 (19)	0.0171 (4)
H12	0.5356	0.9077	0.1135	0.02*
C11	0.3432 (2)	0.86913 (18)	0.13752 (19)	0.0149 (4)
C16	0.2402 (2)	0.41291 (18)	0.40867 (19)	0.0141 (4)
H16	0.221	0.4624	0.4817	0.017*
C10	0.2547 (2)	0.78264 (19)	0.1844 (2)	0.0183 (4)
H10	0.1631	0.7982	0.1827	0.022*
C7	1.1264 (2)	0.3620 (2)	−0.2550 (2)	0.0215 (4)
H7A	1.0643	0.3361	−0.2886	0.032*
H7B	1.2276	0.326	−0.3104	0.032*
H7C	1.1137	0.4525	−0.2561	0.032*
C4	0.9497 (2)	0.36409 (18)	−0.03364 (19)	0.0158 (4)
C1S	0.2096 (2)	0.0584 (2)	0.5897 (2)	0.0253 (5)
C9	0.3009 (2)	0.67246 (18)	0.2342 (2)	0.0164 (4)
H9	0.2397	0.613	0.2661	0.02*
C14	0.1812 (2)	0.9985 (2)	0.0649 (2)	0.0245 (5)
H14A	0.1845	0.9306	0.0121	0.037*
H14B	0.1726	1.0769	0.0201	0.037*
H14C	0.0975	1.002	0.1507	0.037*
C2	0.7115 (2)	0.48623 (19)	0.03891 (19)	0.0165 (4)
H2	0.6423	0.5428	0.0196	0.02*
C13	0.5205 (2)	0.73802 (18)	0.19384 (19)	0.0151 (4)
H13	0.6107	0.7241	0.1982	0.018*
C21	−0.0678 (2)	0.2190 (2)	0.4155 (2)	0.0253 (5)
H21A	−0.0516	0.1871	0.4915	0.038*
H21B	−0.126	0.169	0.3992	0.038*
H21C	−0.119	0.3052	0.4327	0.038*
C2S	0.2949 (3)	0.0285 (2)	0.4466 (2)	0.0388 (7)
H2S1	0.2289	0.0343	0.4057	0.058*
H2S2	0.3517	−0.0557	0.4346	0.058*
H2S3	0.3602	0.0873	0.4056	0.058*
C3S	0.2896 (3)	0.0339 (2)	0.6725 (3)	0.0385 (6)
H3S1	0.2234	0.0597	0.7632	0.058*
H3S2	0.3685	0.0805	0.6393	0.058*
H3S3	0.3295	−0.0548	0.6693	0.058*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt1	0.00961 (5)	0.00951 (5)	0.00805 (5)	−0.00186 (3)	−0.00334 (4)	0.00087 (4)
Cl1	0.0185 (2)	0.0105 (2)	0.0130 (2)	−0.00282 (17)	−0.00628 (18)	0.00104 (17)
P1	0.0110 (2)	0.0113 (2)	0.0095 (2)	−0.00231 (18)	−0.00417 (18)	0.00079 (18)
O2	0.0229 (7)	0.0151 (7)	0.0244 (8)	−0.0027 (6)	−0.0113 (6)	0.0078 (6)
O3	0.0204 (7)	0.0245 (8)	0.0227 (8)	−0.0114 (6)	−0.0098 (6)	−0.0001 (6)
O1	0.0129 (7)	0.0352 (9)	0.0120 (7)	0.0017 (6)	−0.0010 (6)	−0.0017 (6)
O1S	0.0215 (8)	0.0367 (10)	0.0382 (10)	−0.0019 (7)	−0.0049 (8)	−0.0059 (8)
C20	0.0154 (9)	0.0151 (10)	0.0121 (9)	−0.0033 (7)	−0.0050 (8)	0.0009 (7)
C6	0.0204 (10)	0.0200 (11)	0.0131 (10)	0.0004 (8)	−0.0062 (8)	0.0029 (8)
C19	0.0227 (10)	0.0158 (10)	0.0157 (10)	−0.0039 (8)	−0.0097 (8)	−0.0013 (8)
C18	0.0174 (9)	0.0133 (9)	0.0196 (10)	−0.0060 (7)	−0.0113 (8)	0.0048 (8)
C5	0.0180 (10)	0.0261 (12)	0.0160 (10)	0.0057 (8)	−0.0062 (8)	0.0004 (9)
C17	0.0145 (9)	0.0168 (10)	0.0165 (10)	−0.0039 (7)	−0.0065 (8)	0.0018 (8)
C1	0.0114 (8)	0.0132 (9)	0.0135 (9)	−0.0038 (7)	−0.0043 (7)	−0.0004 (7)
C8	0.0136 (9)	0.0129 (9)	0.0097 (9)	−0.0014 (7)	−0.0048 (7)	0.0007 (7)
C3	0.0174 (9)	0.0199 (10)	0.0092 (9)	−0.0028 (8)	−0.0034 (8)	0.0004 (8)
C15	0.0131 (8)	0.0116 (9)	0.0133 (9)	−0.0029 (7)	−0.0066 (7)	0.0024 (7)
C12	0.0192 (10)	0.0166 (10)	0.0160 (10)	−0.0074 (8)	−0.0070 (8)	0.0026 (8)
C11	0.0179 (9)	0.0131 (9)	0.0112 (9)	−0.0006 (7)	−0.0050 (8)	0.0004 (7)
C16	0.0160 (9)	0.0140 (9)	0.0125 (9)	−0.0027 (7)	−0.0062 (8)	−0.0002 (7)
C10	0.0152 (9)	0.0177 (10)	0.0228 (11)	−0.0028 (8)	−0.0098 (8)	0.0040 (8)
C7	0.0166 (10)	0.0268 (12)	0.0142 (10)	−0.0046 (8)	0.0001 (8)	−0.0028 (9)
C4	0.0121 (9)	0.0187 (10)	0.0141 (10)	−0.0024 (7)	−0.0030 (8)	−0.0037 (8)
C1S	0.0250 (11)	0.0141 (10)	0.0307 (13)	−0.0049 (9)	−0.0064 (10)	0.0028 (9)
C9	0.0158 (9)	0.0147 (10)	0.0182 (10)	−0.0055 (8)	−0.0065 (8)	0.0043 (8)
C14	0.0261 (11)	0.0195 (11)	0.0297 (12)	0.0009 (9)	−0.0167 (10)	0.0052 (9)
C2	0.0147 (9)	0.0192 (10)	0.0144 (10)	−0.0003 (8)	−0.0064 (8)	0.0008 (8)
C13	0.0156 (9)	0.0166 (10)	0.0133 (9)	−0.0043 (8)	−0.0060 (8)	0.0003 (8)
C21	0.0204 (10)	0.0275 (12)	0.0306 (13)	−0.0112 (9)	−0.0108 (10)	0.0027 (10)
C2S	0.0381 (14)	0.0278 (14)	0.0300 (14)	0.0102 (11)	−0.0042 (11)	0.0084 (11)
C3S	0.0387 (14)	0.0326 (14)	0.0456 (16)	−0.0033 (11)	−0.0208 (13)	−0.0010 (12)

Geometric parameters (Å, º) top

Pt1—Cl1ⁱ	2.3075 (5)	C3—C4	1.386 (3)
Pt1—Cl1	2.3075 (5)	C3—H3	0.95
Pt1—P1	2.3196 (5)	C15—C16	1.390 (3)
Pt1—P1ⁱ	2.3197 (5)	C12—C13	1.378 (3)
P1—C15	1.8110 (19)	C12—C11	1.396 (3)
P1—C1	1.8151 (19)	C12—H12	0.95
P1—C8	1.8185 (19)	C11—C10	1.380 (3)
O2—C11	1.366 (2)	C16—H16	0.95
O2—C14	1.433 (2)	C10—C9	1.391 (3)
O3—C18	1.361 (2)	C10—H10	0.95
O3—C21	1.435 (3)	C7—H7A	0.98
O1—C4	1.366 (2)	C7—H7B	0.98
O1—C7	1.426 (2)	C7—H7C	0.98
O1S—C1S	1.212 (3)	C1S—C3S	1.492 (3)
C20—C19	1.386 (3)	C1S—C2S	1.495 (3)
C20—C15	1.397 (3)	C9—H9	0.95
C20—H20	0.95	C14—H14A	0.98
C6—C5	1.381 (3)	C14—H14B	0.98
C6—C1	1.401 (3)	C14—H14C	0.98
C6—H6	0.95	C2—H2	0.95
C19—C18	1.394 (3)	C13—H13	0.95
C19—H19	0.95	C21—H21A	0.98
C18—C17	1.391 (3)	C21—H21B	0.98
C5—C4	1.390 (3)	C21—H21C	0.98
C5—H5	0.95	C2S—H2S1	0.98
C17—C16	1.387 (3)	C2S—H2S2	0.98
C17—H17	0.95	C2S—H2S3	0.98
C1—C2	1.390 (3)	C3S—H3S1	0.98
C8—C9	1.388 (3)	C3S—H3S2	0.98
C8—C13	1.406 (3)	C3S—H3S3	0.98
C3—C2	1.384 (3)

Cl1ⁱ—Pt1—Cl1	180.0000 (10)	C17—C16—C15	122.03 (18)
Cl1ⁱ—Pt1—P1	91.984 (16)	C17—C16—H16	119
Cl1—Pt1—P1	88.016 (16)	C15—C16—H16	119
Cl1ⁱ—Pt1—P1ⁱ	88.016 (16)	C11—C10—C9	119.42 (18)
Cl1—Pt1—P1ⁱ	91.984 (16)	C11—C10—H10	120.3
P1—Pt1—P1ⁱ	180	C9—C10—H10	120.3
C15—P1—C1	107.86 (9)	O1—C7—H7A	109.5
C15—P1—C8	103.27 (8)	O1—C7—H7B	109.5
C1—P1—C8	103.77 (9)	H7A—C7—H7B	109.5
C15—P1—Pt1	110.80 (6)	O1—C7—H7C	109.5
C1—P1—Pt1	112.70 (6)	H7A—C7—H7C	109.5
C8—P1—Pt1	117.60 (6)	H7B—C7—H7C	109.5
C11—O2—C14	116.83 (16)	O1—C4—C3	124.33 (18)
C18—O3—C21	117.38 (16)	O1—C4—C5	115.86 (17)
C4—O1—C7	116.81 (15)	C3—C4—C5	119.80 (18)
C19—C20—C15	120.62 (18)	O1S—C1S—C3S	121.7 (2)
C19—C20—H20	119.7	O1S—C1S—C2S	121.3 (2)
C15—C20—H20	119.7	C3S—C1S—C2S	117.0 (2)
C5—C6—C1	120.95 (18)	C8—C9—C10	121.71 (18)
C5—C6—H6	119.5	C8—C9—H9	119.1
C1—C6—H6	119.5	C10—C9—H9	119.1
C20—C19—C18	120.17 (18)	O2—C14—H14A	109.5
C20—C19—H19	119.9	O2—C14—H14B	109.5
C18—C19—H19	119.9	H14A—C14—H14B	109.5
O3—C18—C17	124.15 (18)	O2—C14—H14C	109.5
O3—C18—C19	115.85 (18)	H14A—C14—H14C	109.5
C17—C18—C19	119.99 (18)	H14B—C14—H14C	109.5
C6—C5—C4	120.14 (18)	C3—C2—C1	121.79 (17)
C6—C5—H5	119.9	C3—C2—H2	119.1
C4—C5—H5	119.9	C1—C2—H2	119.1
C16—C17—C18	118.99 (18)	C12—C13—C8	120.71 (17)
C16—C17—H17	120.5	C12—C13—H13	119.6
C18—C17—H17	120.5	C8—C13—H13	119.6
C2—C1—C6	117.78 (17)	O3—C21—H21A	109.5
C2—C1—P1	121.60 (14)	O3—C21—H21B	109.5
C6—C1—P1	120.56 (15)	H21A—C21—H21B	109.5
C9—C8—C13	117.93 (17)	O3—C21—H21C	109.5
C9—C8—P1	121.10 (14)	H21A—C21—H21C	109.5
C13—C8—P1	120.97 (14)	H21B—C21—H21C	109.5
C2—C3—C4	119.52 (18)	C1S—C2S—H2S1	109.5
C2—C3—H3	120.2	C1S—C2S—H2S2	109.5
C4—C3—H3	120.2	H2S1—C2S—H2S2	109.5
C16—C15—C20	118.19 (17)	C1S—C2S—H2S3	109.5
C16—C15—P1	117.96 (14)	H2S1—C2S—H2S3	109.5
C20—C15—P1	123.68 (15)	H2S2—C2S—H2S3	109.5
C13—C12—C11	120.23 (18)	C1S—C3S—H3S1	109.5
C13—C12—H12	119.9	C1S—C3S—H3S2	109.5
C11—C12—H12	119.9	H3S1—C3S—H3S2	109.5
O2—C11—C10	124.34 (17)	C1S—C3S—H3S3	109.5
O2—C11—C12	115.70 (17)	H3S1—C3S—H3S3	109.5
C10—C11—C12	119.96 (18)	H3S2—C3S—H3S3	109.5

Cl1ⁱ—Pt1—P1—C15	−133.32 (7)	C1—P1—C15—C16	166.68 (14)
Cl1—Pt1—P1—C15	46.68 (7)	C8—P1—C15—C16	−83.88 (16)
Cl1ⁱ—Pt1—P1—C1	105.72 (7)	Pt1—P1—C15—C16	42.91 (16)
Cl1—Pt1—P1—C1	−74.28 (7)	C1—P1—C15—C20	−18.18 (18)
Cl1ⁱ—Pt1—P1—C8	−14.92 (7)	C8—P1—C15—C20	91.26 (17)
Cl1—Pt1—P1—C8	165.08 (7)	Pt1—P1—C15—C20	−141.95 (14)
C15—C20—C19—C18	1.2 (3)	C14—O2—C11—C10	−4.5 (3)
C21—O3—C18—C17	−1.4 (3)	C14—O2—C11—C12	175.03 (18)
C21—O3—C18—C19	177.40 (17)	C13—C12—C11—O2	−177.95 (18)
C20—C19—C18—O3	179.52 (17)	C13—C12—C11—C10	1.6 (3)
C20—C19—C18—C17	−1.6 (3)	C18—C17—C16—C15	0.8 (3)
C1—C6—C5—C4	−0.1 (3)	C20—C15—C16—C17	−1.2 (3)
O3—C18—C17—C16	179.38 (17)	P1—C15—C16—C17	174.19 (15)
C19—C18—C17—C16	0.6 (3)	O2—C11—C10—C9	177.62 (19)
C5—C6—C1—C2	0.3 (3)	C12—C11—C10—C9	−1.8 (3)
C5—C6—C1—P1	−176.99 (17)	C7—O1—C4—C3	−2.8 (3)
C15—P1—C1—C2	88.16 (17)	C7—O1—C4—C5	178.13 (18)
C8—P1—C1—C2	−20.94 (18)	C2—C3—C4—O1	179.84 (19)
Pt1—P1—C1—C2	−149.22 (14)	C2—C3—C4—C5	−1.1 (3)
C15—P1—C1—C6	−94.64 (17)	C6—C5—C4—O1	179.66 (19)
C8—P1—C1—C6	156.27 (16)	C6—C5—C4—C3	0.5 (3)
Pt1—P1—C1—C6	27.99 (18)	C13—C8—C9—C10	1.7 (3)
C15—P1—C8—C9	14.06 (18)	P1—C8—C9—C10	−177.47 (16)
C1—P1—C8—C9	126.52 (16)	C11—C10—C9—C8	0.2 (3)
Pt1—P1—C8—C9	−108.28 (16)	C4—C3—C2—C1	1.3 (3)
C15—P1—C8—C13	−165.06 (16)	C6—C1—C2—C3	−0.9 (3)
C1—P1—C8—C13	−52.59 (17)	P1—C1—C2—C3	176.36 (16)
Pt1—P1—C8—C13	72.60 (17)	C11—C12—C13—C8	0.4 (3)
C19—C20—C15—C16	0.2 (3)	C9—C8—C13—C12	−2.0 (3)
C19—C20—C15—P1	−174.93 (15)	P1—C8—C13—C12	177.19 (15)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C6—H6···Cl1	0.95	2.7	3.493 (2)	142
C10—H10···O1Sⁱⁱ	0.95	2.57	3.235 (3)	127
C12—H12···O2ⁱⁱⁱ	0.95	2.53	3.357 (2)	146

Symmetry codes: (ii) −x, −y+1, −z+1; (iii) −x+1, −y+2, −z.

Experimental details

Crystal data
Chemical formula	[PtCl₂(C₂₁H₂₁O₃P)₂]·2C₃H₆O
M_r	1086.84
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	10.486 (1), 11.0360 (11), 11.3630 (11)
α, β, γ (°)	85.787 (2), 63.924 (2), 78.370 (2)
V (Å³)	1156.70 (19)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	3.27
Crystal size (mm)	0.19 × 0.13 × 0.11

Data collection
Diffractometer	Bruker APEX DUO 4K CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2008)
T_min, T_max	0.679, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	31470, 5799, 5763
R_int	0.042
(sin θ/λ)_max (Å⁻¹)	0.669

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.019, 0.040, 1.04
No. of reflections	5799
No. of parameters	282
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.68, −0.51

Computer programs: APEX2 (Bruker, 2011), SAINT (Bruker, 2008), SAINT and XPREP (Bruker, 2008), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2005), publCIF (Westrip, 2010) and WinGX (Farrugia, 2012).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C6—H6···Cl1	0.95	2.7	3.493 (2)	141.5
C10—H10···O1Sⁱ	0.95	2.57	3.235 (3)	127.4
C12—H12···O2ⁱⁱ	0.95	2.53	3.357 (2)	146.1

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+2, −z.

Acknowledgements

Research Fund of the University of Johannesburg is gratefully acknowledged.

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115–119. Web of Science CrossRef CAS IUCr Journals Google Scholar
Blerk, C. van & Holzapfel, C. W. (2009). Acta Cryst. E65, m1536. Web of Science CSD CrossRef IUCr Journals Google Scholar
Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2008). SADABS, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849–854. Web of Science CrossRef CAS IUCr Journals Google Scholar
Muller, A. & Meijboom, R. (2010). Acta Cryst. E66, m1420. Web of Science CSD CrossRef IUCr Journals Google Scholar
Otto, S. (2001). Acta Cryst. C57, 793–795. Web of Science CSD CrossRef CAS 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. Upper Saddle River, New Jersey, USA: Prentice Hall. Google Scholar
Tolman, C. A. (1977). Chem. Rev. 77, 313–348. CrossRef CAS Web of Science Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 68| Part 12| December 2012| Page m1475

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

trans-Di­chloridobis[tris­­(4-meth­­oxy­lphen­yl)phosphane-κP]platinum(II) acetone disolvate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

trans-Dichloridobis[tris(4-methoxylphenyl)phosphane-κP]platinum(II) acetone disolvate