Bis(μ-diisopropyl­phosphanido-κ2P:P)bis­[hydrido(triisopropyl­phosphane-κP)platinum(II)]

Arnold, N.; Braunschweig, H.; Damme, A.

doi:10.1107/S1600536812022829

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 6| June 2012| Page m808

doi:10.1107/S1600536812022829

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Bis(μ-diisopropylphosphanido-κ²P:P)bis[hydrido(triisopropylphosphane-κP)platinum(II)]

Nicole Arnold,^a Holger Braunschweig ^a ^* and Alexander Damme ^a

^aInstitut für Anorganische Chemie, Universität Würzburg, Am Hubland, D-97074 Würzburg, Germany
^*Correspondence e-mail: h.braunschweig@mail.uni-wuerzburg.de

(Received 11 April 2012; accepted 18 May 2012; online 26 May 2012)

In the centrosymmetric molecular structure of the title compound [Pt₂(C₆H₁₄P)₂H₂(C₉H₂₁P)₂], each Pt^II atom is bound on one side to a phosphane ligand (PiPr₃) and a hydrido ligand. On the other side, it is bound to two phosphanide ligands (μ-PiPr₂), which engage a bridging position between the two Pt^II atoms, forming a distorted square-planar structure motif. The Pt⋯Pt distance is 3.6755 (2) Å. A comparable molecular structure was observed for bis(μ-di-tert-butylphosphanido)bis[hydrido(triethylphosphane)platinum(II)] [Itazaki et al. (2004 ). Organometallics, 23, 1610–1621].

Related literature

For the syntheses of similar phosphido-bridged complexes of platinum(II) with phosphine ligands, see: Itazaki et al. (2004) or with other ligands such as carbonyl, see: Albinati et al. (2008 ). For Pt—H bond lengths in related structures, see: Chiang et al. (1984 ); Knobler et al. (1983 ).

Experimental

Crystal data

[Pt₂(C₆H₁₄P)₂H₂(C₉H₂₁P)₂]
M_r = 946.94
Monoclinic, P 2₁ /n
a = 8.8301 (3) Å
b = 14.8153 (5) Å
c = 14.1688 (5) Å
β = 90.097 (2)°
V = 1853.57 (11) Å³
Z = 2
Mo Kα radiation
μ = 7.73 mm⁻¹
T = 100 K
0.53 × 0.13 × 0.11 mm

Data collection

Bruker X8 APEXII diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008 ) T_min = 0.360, T_max = 0.745
38282 measured reflections
3943 independent reflections
3478 reflections with I > 2σ(I)
R_int = 0.051

Refinement

R[F² > 2σ(F²)] = 0.018
wR(F²) = 0.038
S = 1.03
3943 reflections
177 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.72 e Å⁻³
Δρ_min = −0.66 e Å⁻³

Data collection: APEX2 (Bruker, 2010 ); cell refinement: SAINT-Plus (Bruker, 2010); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812022829/hp2036sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812022829/hp2036Isup2.hkl

checkCIF report

Comment top

Bis[µ-di(isopropyl)phosphino]-di(hydrido)-bis[tri(isopropyl)phosphine]-di(platinum), bridged by the µ-PiPr₂ ligands, displays a slightly distorted square-planar geometry. The two platinum centers show a Pt(1)–Pt(1ⁱ) distance of 3.6755 (2) Å. The Pt–Pt distance is comparable to that in bis[µ-di(tert-butyl)phosphino]-di(hydrido)-bis[tri(ethyl)phosphine]-di(platinum) [Pt₂H₂(µ-P^tBu₂)₂(PEt₃)₂] (3.646 Å).

The bond angles P(13)–Pt(1)–P(13ⁱ) [77.47 (3)°] and Pt(1)–P(13)–Pt(1ⁱ) [102.53 (3)°] are slightly out of range of the structural parameters of the complexes without Pt–Pt bonding from Itazaki et al. (2004) [P–Pt–P 74.6–77.2° and Pt–P–Pt 102.8–105.4°]. This could be due to the less sterical hindrance of the iso-propyl groups by contrast with the tert-butyl groups in the reference substance [Pt₂H₂(µ-P^tBu₂)₂(PEt₃)₂].

Chiang et al. (1984) reported the bond length of a terminal Pt–H bond determined by neutron diffraction method. They found for the Pt–H bond on a five coordinate platinum centre a bond length of 1.610 (2) Å in the compound [Pt₂H₃(Ph₂PCH₂CH₂PPh₂)₂]⁺[BPh₄]^-. In the title compound [Pt₂H₂(µ-PiPr₂)₂(PiPr₃)₂] [1.57 (3) Å] the bonding disctance of Pt–H is 2.5% shorter than in the neutron experiment of Chiang et al., due to the smaller coordination number of four in the former species.

The group of Knobler et al. (1983) also determined the Pt–H bond length by X-Ray diffraction in [Pt₂H₃(Ph₂PCH₂CH₂PPh₂)₂]⁺[BPh₄]^- to be 1.527 Å, however without further refinement.

The bonding dictances Pt–P in trans-position to the hydrido ligand are with 2.3773 (7) Å longer than the bonding distances in trans-position to the phosphine ligand 2.3343 (7) Å.

Related literature top

For the syntheses of similar phosphido-bridged complexes of platinum(II) with phosphine ligands, see: Itazaki et al. (2004) or with other ligands such as carbonyl, see: Albinati et al. (2008). For Pt—H bond lengths in related structures, see: Chiang et al. (1984); Knobler et al. (1983).

Experimental top

Bis(tri-iso-propylphosphine)platinum (50.0 mg, 0.09 mmol) dissolved in 1 ml benzene was added to a solution of dichloro(2,3,5,6-tetramethylphenyl)borane (29.5 mg, 0.09 mmol) in 1 ml benzene. The solvent was removed under reduced pressure and the obtained dark brown residue was disolved in hexanes. The title compound was obtained as a off-white solid. Colourless crystals suitable for X-ray analysis were grown from a hexanes solution at 238 K.

Computing details top

Data collection: APEX2 (Bruker, 2010); cell refinement: SAINT-Plus (Bruker, 2010); data reduction: SAINT-Plus (Bruker, 2010); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. The molecular structure of the title compound showing the atom numbering scheme and displacement ellipsoides for the non-H atoms at the 50% probability level. Hydrogen atoms are omitted for clarity.

Bis(µ-diisopropylphosphanido- κ²P:P)bis[hydrido(triisopropylphosphane- κP)platinum(II)] top

Crystal data top

[Pt₂(C₆H₁₄P)₂H₂(C₉H₂₁P)₂]	F(000) = 936
M_r = 946.94	D_x = 1.697 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 8162 reflections
a = 8.8301 (3) Å	θ = 2.7–26.7°
b = 14.8153 (5) Å	µ = 7.73 mm⁻¹
c = 14.1688 (5) Å	T = 100 K
β = 90.097 (2)°	Needle, colourless
V = 1853.57 (11) Å³	0.53 × 0.13 × 0.11 mm
Z = 2

Data collection top

Bruker X8 APEXII diffractometer	3943 independent reflections
Radiation source: rotating anode	3478 reflections with I > 2σ(I)
Multi-layer mirror monochromator	R_int = 0.051
Detector resolution: 8.333 pixels mm^-1	θ_max = 26.8°, θ_min = 2.0°
ϕ and ω scans	h = −11→11
Absorption correction: multi-scan (SADABS; Bruker, 2008)	k = −18→18
T_min = 0.360, T_max = 0.745	l = −17→17
38282 measured reflections

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)] = 0.018	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.038	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ²(F_o²) + (0.0141P)² + 0.9947P] where P = (F_o² + 2F_c²)/3
3943 reflections	(Δ/σ)_max = 0.009
177 parameters	Δρ_max = 0.72 e Å⁻³
0 restraints	Δρ_min = −0.66 e Å⁻³

Crystal data top

[Pt₂(C₆H₁₄P)₂H₂(C₉H₂₁P)₂]	V = 1853.57 (11) Å³
M_r = 946.94	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 8.8301 (3) Å	µ = 7.73 mm⁻¹
b = 14.8153 (5) Å	T = 100 K
c = 14.1688 (5) Å	0.53 × 0.13 × 0.11 mm
β = 90.097 (2)°

Data collection top

Bruker X8 APEXII diffractometer	3943 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2008)	3478 reflections with I > 2σ(I)
T_min = 0.360, T_max = 0.745	R_int = 0.051
38282 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.018	0 restraints
wR(F²) = 0.038	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	Δρ_max = 0.72 e Å⁻³
3943 reflections	Δρ_min = −0.66 e Å⁻³
177 parameters

Special details top

Experimental. The crystal was immersed in a film of perfluoropolyether oil, mounted on a polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold nitrogen (Oxford Cryostream 700).

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	0.068246 (11)	1.032840 (7)	0.882448 (6)	0.00916 (4)
P3	0.15611 (8)	0.99092 (5)	0.73662 (5)	0.01104 (15)
C4	0.0188 (3)	1.01911 (19)	0.64139 (19)	0.0155 (6)
H4	0.0570	0.9925	0.5811	0.019*
C5	−0.1344 (3)	0.9764 (2)	0.6632 (2)	0.0230 (7)
H5A	−0.1717	0.9993	0.7238	0.034*
H5B	−0.1233	0.9107	0.6667	0.034*
H5C	−0.2067	0.9918	0.6132	0.034*
C6	0.0005 (3)	1.1205 (2)	0.6271 (2)	0.0218 (7)
H6A	−0.0818	1.1318	0.5822	0.033*
H6B	0.0951	1.1457	0.6023	0.033*
H6C	−0.0234	1.1491	0.6876	0.033*
C7	0.3257 (3)	1.05748 (19)	0.70284 (18)	0.0141 (6)
H7	0.2888	1.1209	0.6953	0.017*
C8	0.3981 (3)	1.0330 (2)	0.60752 (19)	0.0195 (7)
H8A	0.4768	1.0773	0.5921	0.029*
H8B	0.3202	1.0334	0.5581	0.029*
H8C	0.4434	0.9727	0.6116	0.029*
C9	0.4449 (3)	1.0616 (2)	0.7817 (2)	0.0199 (7)
H9A	0.4974	1.0034	0.7859	0.030*
H9B	0.3951	1.0747	0.8419	0.030*
H9C	0.5184	1.1093	0.7675	0.030*
C10	0.1983 (3)	0.86919 (18)	0.71777 (19)	0.0156 (6)
H10	0.1209	0.8361	0.7558	0.019*
C11	0.3510 (3)	0.8423 (2)	0.7605 (2)	0.0212 (7)
H11A	0.3587	0.7763	0.7627	0.032*
H11B	0.3591	0.8667	0.8246	0.032*
H11C	0.4331	0.8666	0.7215	0.032*
C12	0.1825 (4)	0.8318 (2)	0.6177 (2)	0.0235 (7)
H12A	0.2552	0.8620	0.5761	0.035*
H12B	0.0794	0.8427	0.5946	0.035*
H12C	0.2028	0.7668	0.6181	0.035*
P13	0.00800 (7)	0.90365 (5)	0.97455 (5)	0.01004 (14)
C14	−0.1496 (3)	0.82851 (18)	0.93640 (18)	0.0141 (6)
H14	−0.1686	0.7858	0.9897	0.017*
C15	−0.2950 (3)	0.8827 (2)	0.9230 (2)	0.0220 (7)
H15A	−0.2809	0.9267	0.8721	0.033*
H15B	−0.3194	0.9145	0.9817	0.033*
H15C	−0.3782	0.8418	0.9066	0.033*
C16	−0.1193 (3)	0.7706 (2)	0.8494 (2)	0.0197 (7)
H16A	−0.2015	0.7268	0.8415	0.030*
H16B	−0.0231	0.7385	0.8573	0.030*
H16C	−0.1139	0.8094	0.7934	0.030*
C17	0.1654 (3)	0.82156 (18)	0.99243 (18)	0.0129 (6)
H17	0.1924	0.7960	0.9293	0.015*
C18	0.1266 (3)	0.7430 (2)	1.0573 (2)	0.0222 (7)
H18A	0.2147	0.7032	1.0633	0.033*
H18B	0.0414	0.7090	1.0307	0.033*
H18C	0.0987	0.7662	1.1197	0.033*
C19	0.3042 (3)	0.8713 (2)	1.0303 (2)	0.0216 (7)
H19A	0.2810	0.8971	1.0923	0.032*
H19B	0.3318	0.9199	0.9866	0.032*
H19C	0.3890	0.8290	1.0362	0.032*
H2	0.099 (3)	1.131 (2)	0.845 (2)	0.040 (9)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt1	0.01140 (6)	0.00952 (6)	0.00656 (6)	0.00047 (4)	0.00126 (4)	−0.00011 (4)
P3	0.0133 (4)	0.0122 (4)	0.0076 (3)	0.0013 (3)	0.0004 (3)	−0.0003 (3)
C4	0.0205 (16)	0.0180 (16)	0.0081 (13)	0.0010 (12)	−0.0003 (11)	−0.0021 (11)
C5	0.0195 (17)	0.0312 (19)	0.0182 (15)	−0.0033 (14)	−0.0068 (13)	−0.0003 (13)
C6	0.0242 (17)	0.0225 (18)	0.0187 (15)	0.0058 (14)	−0.0075 (12)	0.0020 (13)
C7	0.0161 (15)	0.0142 (15)	0.0118 (14)	−0.0016 (12)	0.0010 (11)	0.0002 (11)
C8	0.0206 (16)	0.0240 (18)	0.0140 (15)	−0.0027 (13)	0.0056 (12)	0.0024 (12)
C9	0.0155 (16)	0.0264 (17)	0.0179 (15)	−0.0036 (13)	−0.0011 (12)	0.0028 (13)
C10	0.0203 (16)	0.0105 (14)	0.0160 (14)	0.0000 (12)	0.0059 (12)	−0.0014 (12)
C11	0.0253 (17)	0.0175 (17)	0.0208 (16)	0.0049 (13)	0.0050 (13)	0.0028 (13)
C12	0.0338 (19)	0.0163 (16)	0.0204 (16)	0.0022 (14)	0.0037 (13)	−0.0076 (13)
P13	0.0118 (4)	0.0099 (3)	0.0085 (3)	0.0007 (3)	0.0010 (3)	−0.0005 (3)
C14	0.0178 (15)	0.0125 (15)	0.0121 (14)	−0.0047 (12)	0.0017 (11)	−0.0003 (11)
C15	0.0154 (16)	0.0255 (18)	0.0250 (16)	−0.0012 (13)	−0.0018 (12)	−0.0051 (14)
C16	0.0186 (16)	0.0195 (17)	0.0209 (15)	−0.0076 (13)	0.0024 (12)	−0.0062 (13)
C17	0.0150 (15)	0.0111 (15)	0.0125 (13)	0.0039 (11)	0.0023 (11)	−0.0006 (11)
C18	0.0283 (18)	0.0182 (17)	0.0201 (16)	0.0104 (14)	0.0030 (13)	0.0050 (13)
C19	0.0155 (16)	0.0229 (17)	0.0265 (17)	0.0036 (13)	−0.0028 (12)	−0.0021 (14)

Geometric parameters (Å, º) top

Pt1—P3	2.2940 (7)	C11—H11A	0.9800
Pt1—P13ⁱ	2.3343 (7)	C11—H11B	0.9800
Pt1—P13	2.3773 (7)	C11—H11C	0.9800
Pt1—H2	1.57 (3)	C12—H12A	0.9800
P3—C7	1.857 (3)	C12—H12B	0.9800
P3—C4	1.860 (3)	C12—H12C	0.9800
P3—C10	1.861 (3)	P13—C14	1.862 (3)
C4—C6	1.524 (4)	P13—C17	1.864 (3)
C4—C5	1.526 (4)	P13—Pt1ⁱ	2.3343 (7)
C4—H4	1.0000	C14—C16	1.526 (4)
C5—H5A	0.9800	C14—C15	1.526 (4)
C5—H5B	0.9800	C14—H14	1.0000
C5—H5C	0.9800	C15—H15A	0.9800
C6—H6A	0.9800	C15—H15B	0.9800
C6—H6B	0.9800	C15—H15C	0.9800
C6—H6C	0.9800	C16—H16A	0.9800
C7—C9	1.534 (4)	C16—H16B	0.9800
C7—C8	1.538 (4)	C16—H16C	0.9800
C7—H7	1.0000	C17—C18	1.523 (4)
C8—H8A	0.9800	C17—C19	1.527 (4)
C8—H8B	0.9800	C17—H17	1.0000
C8—H8C	0.9800	C18—H18A	0.9800
C9—H9A	0.9800	C18—H18B	0.9800
C9—H9B	0.9800	C18—H18C	0.9800
C9—H9C	0.9800	C19—H19A	0.9800
C10—C12	1.529 (4)	C19—H19B	0.9800
C10—C11	1.530 (4)	C19—H19C	0.9800
C10—H10	1.0000

P3—Pt1—P13ⁱ	171.67 (3)	C10—C11—H11A	109.5
P3—Pt1—P13	110.66 (2)	C10—C11—H11B	109.5
P13ⁱ—Pt1—P13	77.47 (3)	H11A—C11—H11B	109.5
P3—Pt1—H2	83.5 (12)	C10—C11—H11C	109.5
P13ⁱ—Pt1—H2	88.4 (12)	H11A—C11—H11C	109.5
P13—Pt1—H2	165.8 (12)	H11B—C11—H11C	109.5
C7—P3—C4	102.65 (13)	C10—C12—H12A	109.5
C7—P3—C10	108.41 (13)	C10—C12—H12B	109.5
C4—P3—C10	104.12 (13)	H12A—C12—H12B	109.5
C7—P3—Pt1	111.26 (9)	C10—C12—H12C	109.5
C4—P3—Pt1	111.81 (9)	H12A—C12—H12C	109.5
C10—P3—Pt1	117.37 (9)	H12B—C12—H12C	109.5
C6—C4—C5	110.0 (2)	C14—P13—C17	101.90 (12)
C6—C4—P3	112.7 (2)	C14—P13—Pt1ⁱ	106.05 (9)
C5—C4—P3	109.69 (19)	C17—P13—Pt1ⁱ	111.17 (9)
C6—C4—H4	108.1	C14—P13—Pt1	119.34 (9)
C5—C4—H4	108.1	C17—P13—Pt1	115.63 (9)
P3—C4—H4	108.1	Pt1ⁱ—P13—Pt1	102.53 (3)
C4—C5—H5A	109.5	C16—C14—C15	110.1 (2)
C4—C5—H5B	109.5	C16—C14—P13	116.01 (19)
H5A—C5—H5B	109.5	C15—C14—P13	110.48 (19)
C4—C5—H5C	109.5	C16—C14—H14	106.6
H5A—C5—H5C	109.5	C15—C14—H14	106.6
H5B—C5—H5C	109.5	P13—C14—H14	106.6
C4—C6—H6A	109.5	C14—C15—H15A	109.5
C4—C6—H6B	109.5	C14—C15—H15B	109.5
H6A—C6—H6B	109.5	H15A—C15—H15B	109.5
C4—C6—H6C	109.5	C14—C15—H15C	109.5
H6A—C6—H6C	109.5	H15A—C15—H15C	109.5
H6B—C6—H6C	109.5	H15B—C15—H15C	109.5
C9—C7—C8	111.3 (2)	C14—C16—H16A	109.5
C9—C7—P3	112.72 (19)	C14—C16—H16B	109.5
C8—C7—P3	115.95 (19)	H16A—C16—H16B	109.5
C9—C7—H7	105.3	C14—C16—H16C	109.5
C8—C7—H7	105.3	H16A—C16—H16C	109.5
P3—C7—H7	105.3	H16B—C16—H16C	109.5
C7—C8—H8A	109.5	C18—C17—C19	109.8 (2)
C7—C8—H8B	109.5	C18—C17—P13	114.37 (19)
H8A—C8—H8B	109.5	C19—C17—P13	109.31 (19)
C7—C8—H8C	109.5	C18—C17—H17	107.7
H8A—C8—H8C	109.5	C19—C17—H17	107.7
H8B—C8—H8C	109.5	P13—C17—H17	107.7
C7—C9—H9A	109.5	C17—C18—H18A	109.5
C7—C9—H9B	109.5	C17—C18—H18B	109.5
H9A—C9—H9B	109.5	H18A—C18—H18B	109.5
C7—C9—H9C	109.5	C17—C18—H18C	109.5
H9A—C9—H9C	109.5	H18A—C18—H18C	109.5
H9B—C9—H9C	109.5	H18B—C18—H18C	109.5
C12—C10—C11	110.6 (2)	C17—C19—H19A	109.5
C12—C10—P3	117.8 (2)	C17—C19—H19B	109.5
C11—C10—P3	111.9 (2)	H19A—C19—H19B	109.5
C12—C10—H10	105.1	C17—C19—H19C	109.5
C11—C10—H10	105.1	H19A—C19—H19C	109.5
P3—C10—H10	105.1	H19B—C19—H19C	109.5

P13ⁱ—Pt1—P3—C7	31.4 (2)	C7—P3—C10—C11	48.1 (2)
P13—Pt1—P3—C7	−135.55 (10)	C4—P3—C10—C11	156.87 (19)
P13ⁱ—Pt1—P3—C4	−82.7 (2)	Pt1—P3—C10—C11	−79.0 (2)
P13—Pt1—P3—C4	110.32 (10)	P3—Pt1—P13—C14	−65.19 (10)
P13ⁱ—Pt1—P3—C10	157.11 (18)	P13ⁱ—Pt1—P13—C14	116.73 (10)
P13—Pt1—P3—C10	−9.88 (11)	P3—Pt1—P13—C17	56.96 (10)
C7—P3—C4—C6	−51.8 (2)	P13ⁱ—Pt1—P13—C17	−121.13 (10)
C10—P3—C4—C6	−164.7 (2)	P3—Pt1—P13—Pt1ⁱ	178.09 (2)
Pt1—P3—C4—C6	67.6 (2)	P13ⁱ—Pt1—P13—Pt1ⁱ	0.0
C7—P3—C4—C5	−174.7 (2)	C17—P13—C14—C16	−57.0 (2)
C10—P3—C4—C5	72.3 (2)	Pt1ⁱ—P13—C14—C16	−173.41 (19)
Pt1—P3—C4—C5	−55.3 (2)	Pt1—P13—C14—C16	71.7 (2)
C4—P3—C7—C9	167.9 (2)	C17—P13—C14—C15	176.81 (19)
C10—P3—C7—C9	−82.4 (2)	Pt1ⁱ—P13—C14—C15	60.41 (19)
Pt1—P3—C7—C9	48.1 (2)	Pt1—P13—C14—C15	−54.5 (2)
C4—P3—C7—C8	−62.2 (2)	C14—P13—C17—C18	−53.1 (2)
C10—P3—C7—C8	47.5 (2)	Pt1ⁱ—P13—C17—C18	59.6 (2)
Pt1—P3—C7—C8	178.02 (18)	Pt1—P13—C17—C18	175.91 (17)
C7—P3—C10—C12	−81.7 (2)	C14—P13—C17—C19	−176.60 (19)
C4—P3—C10—C12	27.1 (3)	Pt1ⁱ—P13—C17—C19	−63.98 (19)
Pt1—P3—C10—C12	151.27 (19)	Pt1—P13—C17—C19	52.4 (2)

Symmetry code: (i) −x, −y+2, −z+2.

Experimental details

Crystal data
Chemical formula	[Pt₂(C₆H₁₄P)₂H₂(C₉H₂₁P)₂]
M_r	946.94
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	100
a, b, c (Å)	8.8301 (3), 14.8153 (5), 14.1688 (5)
β (°)	90.097 (2)
V (Å³)	1853.57 (11)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	7.73
Crystal size (mm)	0.53 × 0.13 × 0.11

Data collection
Diffractometer	Bruker X8 APEXII diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2008)
T_min, T_max	0.360, 0.745
No. of measured, independent and observed [I > 2σ(I)] reflections	38282, 3943, 3478
R_int	0.051

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.018, 0.038, 1.03
No. of reflections	3943
No. of parameters	177
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.72, −0.66

Computer programs: APEX2 (Bruker, 2010), SAINT-Plus (Bruker, 2010), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

Acknowledgements

Financial support by the DFG is gratefully acknowledged.

References

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