cis-Dichloridobis(triisopropoxy­phosphine)­platinum(II)

Slawin, A.M.Z.; Waddell, P.G.; Woollins, J.D.

doi:10.1107/S1600536809042226

metal-organic compounds

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Volume 65| Part 11| November 2009| Page m1392

https://doi.org/10.1107/S1600536809042226

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cis-Dichloridobis(triisopropoxyphosphine)platinum(II)

Alexandra M. Z. Slawin,^a Paul G. Waddell ^a and J. Derek Woollins ^a ^*

^aDepartment of Chemistry, University of St Andrews, St Andrews, KY16 9ST, Scotland
^*Correspondence e-mail: jdw3@st-and.ac.uk

(Received 19 August 2009; accepted 14 October 2009; online 17 October 2009)

The title compound, [PtCl₂(C₉H₂₁O₃P)₂], was obtained from a solution of PtCl₂(COD) (COD = 1,5-cyclooctadiene) and triisopropylphosphite in dichloromethane. The complex features a Pt(II) atom coordinated by two Cl and two P atoms, yielding a slightly distorted cis square-planar geometry.

Related literature

For the structure of cis-bis(trimethoxyphosphite)dichloridoplatinum, see: Bao et al. (1987 ), for cis-dichloridobis(dimethoxyphenylphosphino)platinum(II), see: Slawin et al. (2007a ); for dichloridobis(methoxydiphenylphosphino)platinum(II), see: Slawin et al. (2007b ) and for cis-bis(trimethoxyphosphite)dichloridopalladium(II), see Slawin et al. (2009 ).

Experimental

Crystal data

[PtCl₂(C₉H₂₁O₃P)₂]
M_r = 682.47
Monoclinic, P 2₁ /c
a = 10.8962 (4) Å
b = 18.9114 (8) Å
c = 14.2754 (6) Å
β = 104.7461 (10)°
V = 2844.7 (2) Å³
Z = 4
Mo Kα radiation
μ = 5.24 mm⁻¹
T = 125 K
0.22 × 0.22 × 0.13 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.356, T_max = 0.506
24157 measured reflections
4995 independent reflections
4473 reflections with I > 2σ(I)
R_int = 0.040

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.038
S = 1.11
4995 reflections
275 parameters
H-atom parameters constrained
Δρ_max = 0.57 e Å⁻³
Δρ_min = −0.49 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Pt1—Cl1	2.3548 (7)
Pt1—Cl2	2.3547 (9)
Pt1—P1	2.2176 (7)
Pt1—P2	2.2117 (8)

Cl1—Pt1—Cl2	87.18 (2)
Cl1—Pt1—P1	171.35 (2)
Cl1—Pt1—P2	90.80 (2)
Cl2—Pt1—P1	85.34 (2)
Cl2—Pt1—P2	175.09 (3)
P1—Pt1—P2	96.99 (3)

Data collection: SCXmini (Rigaku, 2006 ); cell refinement: PROCESS-AUTO (Rigaku, 1998 ); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalStructure (Rigaku, 2006); software used to prepare material for publication: CrystalStructure.

Supporting information

Crystal structure: contains datablocks General, I. DOI: https://doi.org/10.1107/S1600536809042226/fi2086sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809042226/fi2086Isup2.hkl

checkCIF report

Comment top

The title complex can be compared to similar platinum dichloride complexes containing trimethoxy phosphite; [PtCl₂(P(OMe)₃)₂] (Bao et al., 1987). When compared to the structure of [PtCl₂(P(OMe)Ph₂)₂] and [PtCl₂(P(OMe)₂Ph)₂] (Slawin et al., 2007a, 2007b) we note that the title compound has marginally shorter coordination bond lengths and significantly reduced Cl—Pt—Cl and P—Pt—P angles. Cl(1)—Pt(1)—Cl(2) 87.18?(2) , P(1)—Pt(1)—P(2) 96.99?(3) °

Related literature top

For the structure of cis-bis(trimethoxyphosphite)dichloroplatinum, see: Bao et al. (1987), for cis-dichloridobis(dimethoxyphenylphosphino)platinum(II), see: Slawin et al. (2007a); for dichloridobis(methoxydiphenylphosphino)platinum(II), see: Slawin et al. (2007b) and for cis-bis(trimethoxyphosphite)dichloropalladium(II), see Slawin et al. (2009).. Scheme - P atoms not labelled

Experimental top

0.5 g (1.34 mmol) of PtCl₂(COD) was dissolved in the minimum volume of dichloromethane in a round-bottomed flask. To this 0.52 mL (2.67 mmol) of triisopropylphosphite was added. The solution was stirred for 0.5 h at room temperature. The product was precipitated via slow diffusion of hexane and the product was filtered off and dried under vacuum, [PtCl₂(P(OⁱPr)₃)₂](0.82 mmol,ca 63%). ³¹P-{¹H}NMR: δ 61.7 p.p.m.. J{Pt—P} 5812 Hz.

Structure description top

Computing details top

Data collection: SCXmini (Rigaku, 2006); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalStructure (Rigaku, 2006); software used to prepare material for publication: CrystalStructure (Rigaku, 2006).

Figures top

Fig. 1. The structure of (1) with displacement ellipsoids drawn at the 50% probability level, hydrogen atoms omitted for clarity.

cis-Dichloridobis(triisopropoxyphosphine)platinum(II) top

Crystal data top

[PtCl₂(C₉H₂₁O₃P)₂]	F(000) = 1360.00
M_r = 682.47	D_x = 1.593 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ybc	Cell parameters from 27042 reflections
a = 10.8962 (4) Å	θ = 3.0–27.5°
b = 18.9114 (8) Å	µ = 5.24 mm⁻¹
c = 14.2754 (6) Å	T = 125 K
β = 104.7461 (10)°	Chip, colourless
V = 2844.7 (2) Å³	0.22 × 0.22 × 0.13 mm
Z = 4

Data collection top

Rigaku SCXmini diffractometer	4995 independent reflections
Radiation source: fine-focus sealed tube	4473 reflections with F² > 2σ(F²)
Detector resolution: 6.85 pixels mm^-1	R_int = 0.040
ω scans	θ_max = 25.0°, θ_min = 2.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −12→12
T_min = 0.356, T_max = 0.506	k = −22→22
24157 measured reflections	l = −16→16

Refinement top

Refinement on F²	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.024	w = 1/[σ²(F_o²) + (0.0077P)² + 2.3925P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.038	(Δ/σ)_max = 0.001
S = 1.11	Δρ_max = 0.57 e Å⁻³
4995 reflections	Δρ_min = −0.49 e Å⁻³
275 parameters

Crystal data top

[PtCl₂(C₉H₂₁O₃P)₂]	V = 2844.7 (2) Å³
M_r = 682.47	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 10.8962 (4) Å	µ = 5.24 mm⁻¹
b = 18.9114 (8) Å	T = 125 K
c = 14.2754 (6) Å	0.22 × 0.22 × 0.13 mm
β = 104.7461 (10)°

Data collection top

Rigaku SCXmini diffractometer	4995 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	4473 reflections with F² > 2σ(F²)
T_min = 0.356, T_max = 0.506	R_int = 0.040
24157 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	275 parameters
wR(F²) = 0.038	H-atom parameters constrained
S = 1.11	Δρ_max = 0.57 e Å⁻³
4995 reflections	Δρ_min = −0.49 e Å⁻³

Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 σ(F²) is used only for calculating R-factor (gt).

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

	x	y	z	U_iso*/U_eq
Pt(1)	0.111011 (11)	0.242171 (6)	0.268469 (9)	0.01376 (4)
Cl(1)	0.15473 (8)	0.36409 (4)	0.26788 (6)	0.02227 (18)
Cl(2)	−0.09964 (8)	0.27341 (4)	0.26386 (7)	0.0280 (2)
P(1)	0.04057 (8)	0.13168 (4)	0.25627 (6)	0.01632 (18)
P(2)	0.31368 (8)	0.21699 (4)	0.28526 (6)	0.01501 (17)
O(1)	0.14345 (19)	0.07376 (10)	0.25384 (16)	0.0175 (5)
O(2)	−0.0612 (2)	0.11456 (11)	0.15873 (16)	0.0234 (5)
O(3)	−0.0298 (2)	0.10821 (11)	0.33539 (17)	0.0221 (5)
O(4)	0.4129 (2)	0.27767 (10)	0.32742 (15)	0.0180 (5)
O(5)	0.3566 (2)	0.19463 (12)	0.19174 (17)	0.0256 (5)
O(6)	0.3592 (2)	0.15798 (11)	0.36474 (16)	0.0200 (5)
C(1)	0.1080 (3)	−0.00243 (16)	0.2408 (2)	0.0216 (8)
C(2)	0.1982 (3)	−0.04269 (17)	0.3196 (2)	0.0326 (9)
C(3)	0.1142 (4)	−0.02438 (18)	0.1407 (2)	0.0384 (10)
C(4)	−0.1988 (3)	0.12485 (18)	0.1375 (2)	0.0311 (9)
C(5)	−0.2575 (3)	0.0519 (2)	0.1211 (3)	0.0587 (14)
C(6)	−0.2359 (4)	0.1716 (2)	0.0491 (3)	0.0513 (12)
C(7)	0.0033 (3)	0.13724 (18)	0.4343 (2)	0.0279 (8)
C(8)	0.1093 (3)	0.0943 (2)	0.4968 (2)	0.0382 (10)
C(9)	−0.1176 (3)	0.1367 (2)	0.4670 (3)	0.0449 (11)
C(10)	0.4641 (3)	0.32852 (17)	0.2685 (2)	0.0228 (8)
C(11)	0.5885 (3)	0.29936 (19)	0.2570 (2)	0.0315 (9)
C(12)	0.4805 (3)	0.39815 (17)	0.3221 (2)	0.0321 (9)
C(13)	0.2760 (3)	0.16206 (17)	0.1040 (2)	0.0225 (8)
C(14)	0.3629 (4)	0.1203 (2)	0.0582 (3)	0.0442 (11)
C(15)	0.2054 (4)	0.2179 (2)	0.0382 (2)	0.0534 (12)
C(16)	0.4941 (3)	0.13800 (17)	0.3989 (2)	0.0253 (8)
C(17)	0.5077 (3)	0.0630 (2)	0.3695 (3)	0.0533 (13)
C(18)	0.5323 (3)	0.1501 (2)	0.5057 (2)	0.0466 (11)
H(1)	0.0195	−0.0089	0.2473	0.026*
H(2)	0.2847	−0.0377	0.3120	0.039*
H(3)	0.1744	−0.0928	0.3155	0.039*
H(4)	0.1945	−0.0239	0.3828	0.039*
H(5)	0.0548	0.0043	0.0924	0.046*
H(6)	0.0912	−0.0744	0.1306	0.046*
H(7)	0.2005	−0.0173	0.1338	0.046*
H(8)	−0.2217	0.1481	0.1937	0.037*
H(9)	−0.2317	0.0288	0.0677	0.070*
H(10)	−0.3501	0.0560	0.1049	0.070*
H(11)	−0.2286	0.0237	0.1802	0.070*
H(12)	−0.1912	0.2169	0.0627	0.062*
H(13)	−0.3277	0.1799	0.0326	0.062*
H(14)	−0.2128	0.1484	−0.0054	0.062*
H(15)	0.0324	0.1872	0.4322	0.034*
H(16)	0.0835	0.0446	0.4955	0.046*
H(17)	0.1283	0.1119	0.5636	0.046*
H(18)	0.1850	0.0984	0.4721	0.046*
H(19)	−0.1809	0.1667	0.4239	0.054*
H(20)	−0.1007	0.1547	0.5334	0.054*
H(21)	−0.1500	0.0882	0.4648	0.054*
H(22)	0.4031	0.3342	0.2035	0.027*
H(23)	0.6462	0.2918	0.3210	0.038*
H(24)	0.6265	0.3331	0.2204	0.038*
H(25)	0.5733	0.2543	0.2219	0.038*
H(26)	0.3979	0.4146	0.3288	0.038*
H(27)	0.5160	0.4332	0.2857	0.038*
H(28)	0.5383	0.3918	0.3864	0.038*
H(29)	0.2141	0.1293	0.1225	0.027*
H(30)	0.4276	0.1518	0.0444	0.053*
H(31)	0.3135	0.0991	−0.0023	0.053*
H(32)	0.4041	0.0829	0.1026	0.053*
H(33)	0.1510	0.2441	0.0712	0.064*
H(34)	0.1530	0.1959	−0.0205	0.064*
H(35)	0.2660	0.2505	0.0208	0.064*
H(36)	0.5458	0.1693	0.3674	0.030*
H(37)	0.4570	0.0321	0.4000	0.064*
H(38)	0.5971	0.0490	0.3902	0.064*
H(39)	0.4778	0.0589	0.2989	0.064*
H(40)	0.5205	0.2001	0.5192	0.056*
H(41)	0.6217	0.1373	0.5311	0.056*
H(42)	0.4797	0.1209	0.5367	0.056*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt(1)	0.01280 (7)	0.01280 (7)	0.01598 (7)	0.00090 (6)	0.00422 (5)	0.00039 (6)
Cl(1)	0.0217 (4)	0.0136 (4)	0.0319 (5)	−0.0003 (3)	0.0075 (4)	0.0018 (3)
Cl(2)	0.0155 (4)	0.0193 (4)	0.0505 (6)	0.0030 (3)	0.0111 (4)	−0.0011 (3)
P(1)	0.0143 (4)	0.0152 (4)	0.0197 (5)	−0.0008 (3)	0.0047 (3)	0.0000 (3)
P(2)	0.0131 (4)	0.0171 (4)	0.0152 (4)	0.0002 (3)	0.0043 (3)	−0.0004 (3)
O(1)	0.0145 (12)	0.0139 (11)	0.0237 (13)	−0.0001 (8)	0.0044 (10)	−0.0013 (9)
O(2)	0.0168 (12)	0.0244 (12)	0.0254 (14)	−0.0020 (10)	−0.0012 (11)	−0.0037 (10)
O(3)	0.0226 (13)	0.0195 (12)	0.0279 (14)	−0.0059 (9)	0.0131 (11)	−0.0031 (10)
O(4)	0.0178 (12)	0.0175 (11)	0.0187 (12)	−0.0038 (9)	0.0046 (10)	0.0006 (9)
O(5)	0.0174 (13)	0.0394 (14)	0.0214 (13)	−0.0001 (10)	0.0076 (11)	−0.0091 (10)
O(6)	0.0140 (12)	0.0178 (11)	0.0258 (14)	0.0004 (9)	0.0004 (10)	0.0073 (9)
C(1)	0.0244 (19)	0.0115 (16)	0.030 (2)	−0.0046 (14)	0.0082 (17)	−0.0032 (13)
C(2)	0.046 (2)	0.0159 (18)	0.034 (2)	0.0017 (17)	0.008 (2)	0.0006 (16)
C(3)	0.059 (2)	0.023 (2)	0.031 (2)	−0.0006 (18)	0.008 (2)	−0.0051 (16)
C(4)	0.017 (2)	0.0241 (19)	0.044 (2)	0.0016 (15)	−0.0071 (18)	−0.0037 (17)
C(5)	0.027 (2)	0.035 (2)	0.103 (4)	−0.0081 (19)	−0.005 (2)	−0.005 (2)
C(6)	0.046 (2)	0.041 (2)	0.052 (3)	0.010 (2)	−0.015 (2)	0.002 (2)
C(7)	0.040 (2)	0.0227 (19)	0.026 (2)	−0.0053 (16)	0.0177 (19)	−0.0063 (15)
C(8)	0.053 (2)	0.036 (2)	0.026 (2)	−0.0003 (19)	0.013 (2)	−0.0005 (17)
C(9)	0.057 (3)	0.041 (2)	0.052 (3)	0.007 (2)	0.042 (2)	0.002 (2)
C(10)	0.0162 (19)	0.0271 (19)	0.026 (2)	−0.0051 (14)	0.0073 (16)	0.0091 (15)
C(11)	0.017 (2)	0.041 (2)	0.038 (2)	−0.0048 (16)	0.0108 (18)	0.0048 (18)
C(12)	0.027 (2)	0.024 (2)	0.045 (2)	−0.0072 (16)	0.0079 (19)	0.0070 (17)
C(13)	0.027 (2)	0.0254 (19)	0.0166 (19)	−0.0076 (15)	0.0085 (16)	−0.0053 (14)
C(14)	0.054 (2)	0.047 (2)	0.036 (2)	0.014 (2)	0.019 (2)	−0.011 (2)
C(15)	0.074 (3)	0.065 (3)	0.021 (2)	0.030 (2)	0.012 (2)	0.004 (2)
C(16)	0.0150 (19)	0.0242 (19)	0.034 (2)	0.0035 (14)	0.0006 (17)	0.0058 (15)
C(17)	0.034 (2)	0.039 (2)	0.076 (3)	0.014 (2)	−0.004 (2)	−0.009 (2)
C(18)	0.030 (2)	0.060 (2)	0.041 (2)	0.012 (2)	−0.006 (2)	0.003 (2)

Geometric parameters (Å, º) top

Pt(1)—Cl(1)	2.3548 (7)	C(4)—H(8)	1.000
Pt(1)—Cl(2)	2.3547 (9)	C(5)—H(9)	0.980
Pt(1)—P(1)	2.2176 (7)	C(5)—H(10)	0.980
Pt(1)—P(2)	2.2117 (8)	C(5)—H(11)	0.980
P(1)—O(1)	1.574 (2)	C(6)—H(12)	0.980
P(1)—O(2)	1.577 (2)	C(6)—H(13)	0.980
P(1)—O(3)	1.582 (2)	C(6)—H(14)	0.980
P(2)—O(4)	1.587 (2)	C(7)—H(15)	1.000
P(2)—O(5)	1.580 (2)	C(8)—H(16)	0.980
P(2)—O(6)	1.579 (2)	C(8)—H(17)	0.980
O(1)—C(1)	1.491 (3)	C(8)—H(18)	0.980
O(2)—C(4)	1.466 (4)	C(9)—H(19)	0.980
O(3)—C(7)	1.472 (4)	C(9)—H(20)	0.980
O(4)—C(10)	1.477 (4)	C(9)—H(21)	0.980
O(5)—C(13)	1.470 (3)	C(10)—H(22)	1.000
O(6)—C(16)	1.475 (3)	C(11)—H(23)	0.980
C(1)—C(2)	1.500 (4)	C(11)—H(24)	0.980
C(1)—C(3)	1.506 (5)	C(11)—H(25)	0.980
C(4)—C(5)	1.513 (5)	C(12)—H(26)	0.980
C(4)—C(6)	1.509 (5)	C(12)—H(27)	0.980
C(7)—C(8)	1.505 (4)	C(12)—H(28)	0.980
C(7)—C(9)	1.505 (6)	C(13)—H(29)	1.000
C(10)—C(11)	1.510 (5)	C(14)—H(30)	0.980
C(10)—C(12)	1.510 (4)	C(14)—H(31)	0.980
C(13)—C(14)	1.504 (5)	C(14)—H(32)	0.980
C(13)—C(15)	1.490 (5)	C(15)—H(33)	0.980
C(16)—C(17)	1.497 (5)	C(15)—H(34)	0.980
C(16)—C(18)	1.491 (5)	C(15)—H(35)	0.980
C(1)—H(1)	1.000	C(16)—H(36)	1.000
C(2)—H(2)	0.980	C(17)—H(37)	0.980
C(2)—H(3)	0.980	C(17)—H(38)	0.980
C(2)—H(4)	0.980	C(17)—H(39)	0.980
C(3)—H(5)	0.980	C(18)—H(40)	0.980
C(3)—H(6)	0.980	C(18)—H(41)	0.980
C(3)—H(7)	0.980	C(18)—H(42)	0.980

Cl(2)···C(11)ⁱ	3.410 (3)	H(19)···H(12)ⁱⁱ	2.981
C(7)···C(15)ⁱⁱ	3.591 (5)	H(19)···H(23)ⁱ	3.144
C(11)···Cl(2)ⁱⁱⁱ	3.410 (3)	H(19)···H(36)ⁱ	2.880
C(15)···C(7)^iv	3.591 (5)	H(19)···H(38)ⁱ	3.233
Pt(1)···H(34)ⁱⁱ	3.155	H(19)···H(41)ⁱ	2.992
Pt(1)···H(35)ⁱⁱ	3.571	H(20)···Cl(2)ⁱⁱ	3.557
Cl(1)···H(1)^v	3.035	H(20)···C(2)^vi	3.340
Cl(1)···H(3)^v	3.574	H(20)···H(3)^vi	2.748
Cl(1)···H(6)^v	3.551	H(20)···H(4)^vi	3.036
Cl(1)···H(11)^v	3.162	H(20)···H(12)ⁱⁱ	2.693
Cl(1)···H(17)^iv	2.893	H(20)···H(33)ⁱⁱ	3.275
Cl(1)···H(31)ⁱⁱ	3.369	H(20)···H(41)ⁱ	3.034
Cl(1)···H(34)ⁱⁱ	3.231	H(21)···C(2)^vi	3.364
Cl(2)···H(3)^v	2.807	H(21)···C(8)^vi	3.505
Cl(2)···H(6)^v	3.238	H(21)···H(3)^vi	3.215
Cl(2)···H(20)^iv	3.557	H(21)···H(4)^vi	2.643
Cl(2)···H(23)ⁱ	3.099	H(21)···H(16)^vi	2.635
Cl(2)···H(24)ⁱ	3.101	H(21)···H(36)ⁱ	3.595
Cl(2)···H(25)ⁱ	3.479	H(21)···H(38)ⁱ	2.791
P(2)···H(35)ⁱⁱ	3.584	H(21)···H(41)ⁱ	3.024
O(4)···H(30)ⁱⁱ	3.339	H(22)···C(18)^iv	3.473
O(4)···H(35)ⁱⁱ	3.567	H(22)···H(17)^iv	3.309
O(6)···H(35)ⁱⁱ	3.185	H(22)···H(40)^iv	3.269
C(2)···H(20)^vi	3.340	H(22)···H(42)^iv	2.845
C(2)···H(21)^vi	3.364	H(23)···Cl(2)ⁱⁱⁱ	3.099
C(2)···H(24)^vii	3.170	H(23)···C(6)^xii	3.256
C(2)···H(41)^viii	3.076	H(23)···H(12)^xii	3.457
C(3)···H(5)^ix	3.389	H(23)···H(13)^xii	3.010
C(3)···H(9)^ix	3.526	H(23)···H(14)^xii	2.801
C(3)···H(14)^ix	3.383	H(23)···H(19)ⁱⁱⁱ	3.144
C(5)···H(26)^x	3.186	H(24)···Cl(2)ⁱⁱⁱ	3.101
C(5)···H(31)^ix	3.298	H(24)···C(2)^xiii	3.170
C(6)···H(23)^xi	3.256	H(24)···C(18)^iv	2.992
C(6)···H(28)^xi	3.159	H(24)···H(2)^xiii	2.711
C(6)···H(40)^xi	3.542	H(24)···H(3)^xiii	2.739
C(7)···H(33)ⁱⁱ	3.138	H(24)···H(40)^iv	2.879
C(7)···H(34)ⁱⁱ	3.535	H(24)···H(41)^iv	2.747
C(7)···H(35)ⁱⁱ	3.525	H(24)···H(42)^iv	2.839
C(8)···H(16)^vi	3.382	H(25)···Cl(2)ⁱⁱⁱ	3.479
C(8)···H(21)^vi	3.505	H(25)···C(18)^iv	3.507
C(8)···H(33)ⁱⁱ	3.230	H(25)···H(8)ⁱⁱⁱ	3.106
C(8)···H(35)ⁱⁱ	3.369	H(25)···H(13)ⁱⁱⁱ	3.455
C(9)···H(3)^vi	3.420	H(25)···H(40)^iv	2.933
C(9)···H(4)^vi	3.281	H(25)···H(41)^iv	3.554
C(9)···H(12)ⁱⁱ	3.277	H(25)···H(42)^iv	3.497
C(9)···H(16)^vi	3.475	H(26)···C(5)^v	3.186
C(9)···H(38)ⁱ	3.447	H(26)···C(14)ⁱⁱ	3.456
C(9)···H(41)ⁱ	3.199	H(26)···H(9)^v	3.390
C(10)···H(42)^iv	3.489	H(26)···H(10)^v	2.928
C(11)···H(40)^iv	3.285	H(26)···H(11)^v	2.748
C(11)···H(41)^iv	3.543	H(26)···H(30)ⁱⁱ	3.263
C(11)···H(42)^iv	3.416	H(26)···H(31)ⁱⁱ	2.802
C(12)···H(10)^v	3.574	H(27)···C(17)^xiii	3.273
C(12)···H(13)^xii	3.519	H(27)···H(2)^xiii	2.916
C(12)···H(30)ⁱⁱ	3.497	H(27)···H(7)^xiii	3.151
C(12)···H(31)ⁱⁱ	3.453	H(27)···H(10)^v	3.541
C(12)···H(39)^xiii	3.582	H(27)···H(32)^xiii	3.257
C(14)···H(9)^ix	3.453	H(27)···H(37)^xiii	3.318
C(14)···H(10)ⁱⁱⁱ	3.262	H(27)···H(38)^xiii	3.323
C(14)···H(26)^iv	3.456	H(27)···H(39)^xiii	2.675
C(14)···H(28)^iv	3.479	H(28)···C(6)^xii	3.159
C(15)···H(15)^iv	2.759	H(28)···C(14)ⁱⁱ	3.479
C(15)···H(17)^iv	3.369	H(28)···H(7)^xiii	3.399
C(15)···H(18)^iv	3.591	H(28)···H(9)^xii	3.454
C(16)···H(19)ⁱⁱⁱ	3.510	H(28)···H(10)^xii	3.201
C(17)···H(27)^vii	3.273	H(28)···H(13)^xii	2.603
C(18)···H(2)^viii	3.554	H(28)···H(14)^xii	2.862
C(18)···H(13)^xii	3.538	H(28)···H(30)ⁱⁱ	2.934
C(18)···H(22)ⁱⁱ	3.473	H(28)···H(31)ⁱⁱ	3.245
C(18)···H(24)ⁱⁱ	2.992	H(30)···O(4)^iv	3.339
C(18)···H(25)ⁱⁱ	3.507	H(30)···C(12)^iv	3.497
C(18)···H(35)ⁱⁱ	3.510	H(30)···H(10)ⁱⁱⁱ	2.971
H(1)···Cl(1)^x	3.035	H(30)···H(13)ⁱⁱⁱ	2.766
H(2)···C(18)^viii	3.554	H(30)···H(26)^iv	3.263
H(2)···H(24)^vii	2.711	H(30)···H(28)^iv	2.934
H(2)···H(27)^vii	2.916	H(30)···H(40)^iv	3.031
H(2)···H(41)^viii	2.905	H(31)···Cl(1)^iv	3.369
H(2)···H(42)^viii	3.302	H(31)···C(5)^ix	3.298
H(3)···Cl(1)^x	3.574	H(31)···C(12)^iv	3.453
H(3)···Cl(2)^x	2.807	H(31)···H(9)^ix	2.663
H(3)···C(9)^vi	3.420	H(31)···H(10)^ix	3.348
H(3)···H(20)^vi	2.748	H(31)···H(11)^ix	3.390
H(3)···H(21)^vi	3.215	H(31)···H(26)^iv	2.802
H(3)···H(24)^vii	2.739	H(31)···H(28)^iv	3.245
H(3)···H(41)^viii	2.821	H(32)···H(9)^ix	3.403
H(4)···C(9)^vi	3.281	H(32)···H(10)ⁱⁱⁱ	2.718
H(4)···H(20)^vi	3.036	H(32)···H(27)^vii	3.257
H(4)···H(21)^vi	2.643	H(33)···C(7)^iv	3.138
H(4)···H(38)^viii	3.484	H(33)···C(8)^iv	3.230
H(4)···H(41)^viii	2.978	H(33)···H(15)^iv	2.448
H(5)···C(3)^ix	3.389	H(33)···H(17)^iv	2.734
H(5)···H(5)^ix	2.610	H(33)···H(18)^iv	3.358
H(5)···H(6)^ix	3.442	H(33)···H(20)^iv	3.275
H(5)···H(9)^ix	3.402	H(34)···Pt(1)^iv	3.155
H(6)···Cl(1)^x	3.551	H(34)···Cl(1)^iv	3.231
H(6)···Cl(2)^x	3.238	H(34)···C(7)^iv	3.535
H(6)···H(5)^ix	3.442	H(34)···H(6)^ix	3.563
H(6)···H(14)^ix	2.849	H(34)···H(15)^iv	2.572
H(6)···H(34)^ix	3.563	H(35)···Pt(1)^iv	3.571
H(7)···H(9)^ix	2.989	H(35)···P(2)^iv	3.584
H(7)···H(14)^ix	3.107	H(35)···O(4)^iv	3.567
H(7)···H(27)^vii	3.151	H(35)···O(6)^iv	3.185
H(7)···H(28)^vii	3.399	H(35)···C(7)^iv	3.525
H(8)···H(25)ⁱ	3.106	H(35)···C(8)^iv	3.369
H(9)···C(3)^ix	3.526	H(35)···C(18)^iv	3.510
H(9)···C(14)^ix	3.453	H(35)···H(15)^iv	2.797
H(9)···H(5)^ix	3.402	H(35)···H(17)^iv	3.139
H(9)···H(7)^ix	2.989	H(35)···H(18)^iv	3.018
H(9)···H(26)^x	3.390	H(35)···H(40)^iv	2.932
H(9)···H(28)^xi	3.454	H(35)···H(42)^iv	3.335
H(9)···H(31)^ix	2.663	H(36)···H(19)ⁱⁱⁱ	2.880
H(9)···H(32)^ix	3.403	H(36)···H(21)ⁱⁱⁱ	3.595
H(10)···C(12)^x	3.574	H(37)···H(27)^vii	3.318
H(10)···C(14)ⁱ	3.262	H(37)···H(37)^viii	3.023
H(10)···H(26)^x	2.928	H(37)···H(38)^viii	3.544
H(10)···H(27)^x	3.541	H(37)···H(41)^viii	3.520
H(10)···H(28)^xi	3.201	H(37)···H(42)^viii	3.056
H(10)···H(30)ⁱ	2.971	H(38)···C(9)ⁱⁱⁱ	3.447
H(10)···H(31)^ix	3.348	H(38)···H(4)^viii	3.484
H(10)···H(32)ⁱ	2.718	H(38)···H(19)ⁱⁱⁱ	3.233
H(11)···Cl(1)^x	3.162	H(38)···H(21)ⁱⁱⁱ	2.791
H(11)···H(26)^x	2.748	H(38)···H(27)^vii	3.323
H(11)···H(31)^ix	3.390	H(38)···H(37)^viii	3.544
H(12)···C(9)^iv	3.277	H(38)···H(42)^viii	3.542
H(12)···H(19)^iv	2.981	H(39)···C(12)^vii	3.582
H(12)···H(20)^iv	2.693	H(39)···H(27)^vii	2.675
H(12)···H(23)^xi	3.457	H(40)···C(6)^xii	3.542
H(12)···H(40)^xi	3.425	H(40)···C(11)ⁱⁱ	3.285
H(12)···H(41)^xi	3.390	H(40)···H(12)^xii	3.425
H(13)···C(12)^xi	3.519	H(40)···H(13)^xii	2.787
H(13)···C(18)^xi	3.538	H(40)···H(22)ⁱⁱ	3.269
H(13)···H(23)^xi	3.010	H(40)···H(24)ⁱⁱ	2.879
H(13)···H(25)ⁱ	3.455	H(40)···H(25)ⁱⁱ	2.933
H(13)···H(28)^xi	2.603	H(40)···H(30)ⁱⁱ	3.031
H(13)···H(30)ⁱ	2.766	H(40)···H(35)ⁱⁱ	2.932
H(13)···H(40)^xi	2.787	H(41)···C(2)^viii	3.076
H(13)···H(41)^xi	3.501	H(41)···C(9)ⁱⁱⁱ	3.199
H(14)···C(3)^ix	3.383	H(41)···C(11)ⁱⁱ	3.543
H(14)···H(6)^ix	2.849	H(41)···H(2)^viii	2.905
H(14)···H(7)^ix	3.107	H(41)···H(3)^viii	2.821
H(14)···H(23)^xi	2.801	H(41)···H(4)^viii	2.978
H(14)···H(28)^xi	2.862	H(41)···H(12)^xii	3.390
H(15)···C(15)ⁱⁱ	2.759	H(41)···H(13)^xii	3.501
H(15)···H(33)ⁱⁱ	2.448	H(41)···H(19)ⁱⁱⁱ	2.992
H(15)···H(34)ⁱⁱ	2.572	H(41)···H(20)ⁱⁱⁱ	3.034
H(15)···H(35)ⁱⁱ	2.797	H(41)···H(21)ⁱⁱⁱ	3.024
H(16)···C(8)^vi	3.382	H(41)···H(24)ⁱⁱ	2.747
H(16)···C(9)^vi	3.475	H(41)···H(25)ⁱⁱ	3.554
H(16)···H(16)^vi	2.508	H(41)···H(37)^viii	3.520
H(16)···H(21)^vi	2.635	H(42)···C(10)ⁱⁱ	3.489
H(17)···Cl(1)ⁱⁱ	2.893	H(42)···C(11)ⁱⁱ	3.416
H(17)···C(15)ⁱⁱ	3.369	H(42)···H(2)^viii	3.302
H(17)···H(22)ⁱⁱ	3.309	H(42)···H(22)ⁱⁱ	2.845
H(17)···H(33)ⁱⁱ	2.734	H(42)···H(24)ⁱⁱ	2.839
H(17)···H(35)ⁱⁱ	3.139	H(42)···H(25)ⁱⁱ	3.497
H(18)···C(15)ⁱⁱ	3.591	H(42)···H(35)ⁱⁱ	3.335
H(18)···H(33)ⁱⁱ	3.358	H(42)···H(37)^viii	3.056
H(18)···H(35)ⁱⁱ	3.018	H(42)···H(38)^viii	3.542
H(19)···C(16)ⁱ	3.510

Cl(1)—Pt(1)—Cl(2)	87.18 (2)	C(4)—C(6)—H(12)	109.5
Cl(1)—Pt(1)—P(1)	171.35 (2)	C(4)—C(6)—H(13)	109.5
Cl(1)—Pt(1)—P(2)	90.80 (2)	C(4)—C(6)—H(14)	109.5
Cl(2)—Pt(1)—P(1)	85.34 (2)	H(12)—C(6)—H(13)	109.5
Cl(2)—Pt(1)—P(2)	175.09 (3)	H(12)—C(6)—H(14)	109.5
P(1)—Pt(1)—P(2)	96.99 (3)	H(13)—C(6)—H(14)	109.5
Pt(1)—P(1)—O(1)	115.04 (8)	O(3)—C(7)—H(15)	109.0
Pt(1)—P(1)—O(2)	114.47 (8)	C(8)—C(7)—H(15)	109.0
Pt(1)—P(1)—O(3)	115.43 (8)	C(9)—C(7)—H(15)	109.0
O(1)—P(1)—O(2)	100.50 (11)	C(7)—C(8)—H(16)	109.5
O(1)—P(1)—O(3)	107.34 (12)	C(7)—C(8)—H(17)	109.5
O(2)—P(1)—O(3)	102.31 (12)	C(7)—C(8)—H(18)	109.5
Pt(1)—P(2)—O(4)	116.80 (8)	H(16)—C(8)—H(17)	109.5
Pt(1)—P(2)—O(5)	117.90 (8)	H(16)—C(8)—H(18)	109.5
Pt(1)—P(2)—O(6)	110.65 (9)	H(17)—C(8)—H(18)	109.5
O(4)—P(2)—O(5)	101.20 (12)	C(7)—C(9)—H(19)	109.5
O(4)—P(2)—O(6)	100.33 (10)	C(7)—C(9)—H(20)	109.5
O(5)—P(2)—O(6)	108.15 (12)	C(7)—C(9)—H(21)	109.5
P(1)—O(1)—C(1)	120.80 (19)	H(19)—C(9)—H(20)	109.5
P(1)—O(2)—C(4)	127.4 (2)	H(19)—C(9)—H(21)	109.5
P(1)—O(3)—C(7)	122.4 (2)	H(20)—C(9)—H(21)	109.5
P(2)—O(4)—C(10)	125.05 (18)	O(4)—C(10)—H(22)	109.9
P(2)—O(5)—C(13)	126.2 (2)	C(11)—C(10)—H(22)	109.9
P(2)—O(6)—C(16)	121.6 (2)	C(12)—C(10)—H(22)	109.9
O(1)—C(1)—C(2)	107.3 (2)	C(10)—C(11)—H(23)	109.5
O(1)—C(1)—C(3)	108.2 (2)	C(10)—C(11)—H(24)	109.5
C(2)—C(1)—C(3)	113.1 (3)	C(10)—C(11)—H(25)	109.5
O(2)—C(4)—C(5)	106.3 (2)	H(23)—C(11)—H(24)	109.5
O(2)—C(4)—C(6)	107.0 (3)	H(23)—C(11)—H(25)	109.5
C(5)—C(4)—C(6)	113.1 (3)	H(24)—C(11)—H(25)	109.5
O(3)—C(7)—C(8)	109.3 (2)	C(10)—C(12)—H(26)	109.5
O(3)—C(7)—C(9)	105.9 (2)	C(10)—C(12)—H(27)	109.5
C(8)—C(7)—C(9)	114.4 (3)	C(10)—C(12)—H(28)	109.5
O(4)—C(10)—C(11)	107.7 (2)	H(26)—C(12)—H(27)	109.5
O(4)—C(10)—C(12)	107.0 (2)	H(26)—C(12)—H(28)	109.5
C(11)—C(10)—C(12)	112.3 (2)	H(27)—C(12)—H(28)	109.5
O(5)—C(13)—C(14)	106.6 (2)	O(5)—C(13)—H(29)	109.3
O(5)—C(13)—C(15)	109.9 (2)	C(14)—C(13)—H(29)	109.4
C(14)—C(13)—C(15)	112.3 (3)	C(15)—C(13)—H(29)	109.3
O(6)—C(16)—C(17)	108.1 (2)	C(13)—C(14)—H(30)	109.5
O(6)—C(16)—C(18)	107.1 (3)	C(13)—C(14)—H(31)	109.5
C(17)—C(16)—C(18)	114.2 (3)	C(13)—C(14)—H(32)	109.5
O(1)—C(1)—H(1)	109.4	H(30)—C(14)—H(31)	109.5
C(2)—C(1)—H(1)	109.4	H(30)—C(14)—H(32)	109.5
C(3)—C(1)—H(1)	109.4	H(31)—C(14)—H(32)	109.5
C(1)—C(2)—H(2)	109.5	C(13)—C(15)—H(33)	109.5
C(1)—C(2)—H(3)	109.5	C(13)—C(15)—H(34)	109.5
C(1)—C(2)—H(4)	109.5	C(13)—C(15)—H(35)	109.5
H(2)—C(2)—H(3)	109.5	H(33)—C(15)—H(34)	109.5
H(2)—C(2)—H(4)	109.5	H(33)—C(15)—H(35)	109.5
H(3)—C(2)—H(4)	109.5	H(34)—C(15)—H(35)	109.5
C(1)—C(3)—H(5)	109.5	O(6)—C(16)—H(36)	109.1
C(1)—C(3)—H(6)	109.5	C(17)—C(16)—H(36)	109.1
C(1)—C(3)—H(7)	109.5	C(18)—C(16)—H(36)	109.1
H(5)—C(3)—H(6)	109.5	C(16)—C(17)—H(37)	109.5
H(5)—C(3)—H(7)	109.5	C(16)—C(17)—H(38)	109.5
H(6)—C(3)—H(7)	109.5	C(16)—C(17)—H(39)	109.5
O(2)—C(4)—H(8)	110.1	H(37)—C(17)—H(38)	109.5
C(5)—C(4)—H(8)	110.1	H(37)—C(17)—H(39)	109.5
C(6)—C(4)—H(8)	110.1	H(38)—C(17)—H(39)	109.5
C(4)—C(5)—H(9)	109.5	C(16)—C(18)—H(40)	109.5
C(4)—C(5)—H(10)	109.5	C(16)—C(18)—H(41)	109.5
C(4)—C(5)—H(11)	109.5	C(16)—C(18)—H(42)	109.5
H(9)—C(5)—H(10)	109.5	H(40)—C(18)—H(41)	109.5
H(9)—C(5)—H(11)	109.5	H(40)—C(18)—H(42)	109.5
H(10)—C(5)—H(11)	109.5	H(41)—C(18)—H(42)	109.5

Cl(1)—Pt(1)—P(2)—O(4)	21.21 (10)	Pt(1)—P(2)—O(4)—C(10)	−93.9 (2)
Cl(1)—Pt(1)—P(2)—O(5)	−99.70 (10)	Pt(1)—P(2)—O(5)—C(13)	−25.7 (2)
Cl(1)—Pt(1)—P(2)—O(6)	135.11 (9)	Pt(1)—P(2)—O(6)—C(16)	−172.06 (19)
Cl(2)—Pt(1)—P(1)—O(1)	179.48 (10)	O(4)—P(2)—O(5)—C(13)	−154.4 (2)
Cl(2)—Pt(1)—P(1)—O(2)	63.79 (11)	O(5)—P(2)—O(4)—C(10)	35.4 (2)
Cl(2)—Pt(1)—P(1)—O(3)	−54.62 (9)	O(4)—P(2)—O(6)—C(16)	−48.1 (2)
P(1)—Pt(1)—P(2)—O(4)	−162.57 (9)	O(6)—P(2)—O(4)—C(10)	146.5 (2)
P(1)—Pt(1)—P(2)—O(5)	76.52 (10)	O(5)—P(2)—O(6)—C(16)	57.4 (2)
P(1)—Pt(1)—P(2)—O(6)	−48.67 (9)	O(6)—P(2)—O(5)—C(13)	100.7 (2)
P(2)—Pt(1)—P(1)—O(1)	−4.85 (10)	P(1)—O(1)—C(1)—C(2)	−129.3 (2)
P(2)—Pt(1)—P(1)—O(2)	−120.55 (11)	P(1)—O(1)—C(1)—C(3)	108.3 (2)
P(2)—Pt(1)—P(1)—O(3)	121.04 (9)	P(1)—O(2)—C(4)—C(5)	−115.5 (3)
Pt(1)—P(1)—O(1)—C(1)	−176.87 (19)	P(1)—O(2)—C(4)—C(6)	123.5 (2)
Pt(1)—P(1)—O(2)—C(4)	−86.4 (2)	P(1)—O(3)—C(7)—C(8)	−87.0 (3)
Pt(1)—P(1)—O(3)—C(7)	−31.2 (2)	P(1)—O(3)—C(7)—C(9)	149.3 (2)
O(1)—P(1)—O(2)—C(4)	149.7 (2)	P(2)—O(4)—C(10)—C(11)	−94.7 (2)
O(2)—P(1)—O(1)—C(1)	−53.4 (2)	P(2)—O(4)—C(10)—C(12)	144.3 (2)
O(1)—P(1)—O(3)—C(7)	98.5 (2)	P(2)—O(5)—C(13)—C(14)	−153.8 (2)
O(3)—P(1)—O(1)—C(1)	53.2 (2)	P(2)—O(5)—C(13)—C(15)	84.3 (3)
O(2)—P(1)—O(3)—C(7)	−156.2 (2)	P(2)—O(6)—C(16)—C(17)	−114.9 (3)
O(3)—P(1)—O(2)—C(4)	39.2 (2)	P(2)—O(6)—C(16)—C(18)	121.6 (2)

Symmetry codes: (i) x−1, y, z; (ii) x, −y+1/2, z+1/2; (iii) x+1, y, z; (iv) x, −y+1/2, z−1/2; (v) −x, y+1/2, −z+1/2; (vi) −x, −y, −z+1; (vii) −x+1, y−1/2, −z+1/2; (viii) −x+1, −y, −z+1; (ix) −x, −y, −z; (x) −x, y−1/2, −z+1/2; (xi) x−1, −y+1/2, z−1/2; (xii) x+1, −y+1/2, z+1/2; (xiii) −x+1, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	[PtCl₂(C₉H₂₁O₃P)₂]
M_r	682.47
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	125
a, b, c (Å)	10.8962 (4), 18.9114 (8), 14.2754 (6)
β (°)	104.7461 (10)
V (Å³)	2844.7 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.24
Crystal size (mm)	0.22 × 0.22 × 0.13

Data collection
Diffractometer	Rigaku SCXmini
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.356, 0.506
No. of measured, independent and observed [F² > 2σ(F²)] reflections	24157, 4995, 4473
R_int	0.040
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.038, 1.11
No. of reflections	4995
No. of parameters	275
No. of restraints	?
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.57, −0.49

Computer programs: SCXmini (Rigaku, 2006), PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), CrystalStructure (Rigaku, 2006).

Selected geometric parameters (Å, º) top

Pt(1)—Cl(1)	2.3548 (7)	Pt(1)—P(1)	2.2176 (7)
Pt(1)—Cl(2)	2.3547 (9)	Pt(1)—P(2)	2.2117 (8)

Cl(1)—Pt(1)—Cl(2)	87.18 (2)	Cl(2)—Pt(1)—P(1)	85.34 (2)
Cl(1)—Pt(1)—P(1)	171.35 (2)	Cl(2)—Pt(1)—P(2)	175.09 (3)
Cl(1)—Pt(1)—P(2)	90.80 (2)	P(1)—Pt(1)—P(2)	96.99 (3)

Acknowledgements

We are grateful to the EPSRC for support.

References

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