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ISSN: 2056-9890

cis-Di­chloridobis(triisoprop­oxy­phosphine)­platinum(II)

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[Bao, Q.-B., Geib, S. J., Rheingold, A. L. & Brill, T. B. (1987). Inorg. Chem. 26, 3453-3458.]), for cis-dichlorido­bis(di­meth­oxy­phenyl­phosphino)platinum(II), see: Slawin et al. (2007a[Slawin, A. M. Z., Waddell, P. G. & Woollins, J. D. (2007a). Acta Cryst. E63, m2017.]); for dichloridobis(methoxy­diphenyl­phosphino)platinum(II), see: Slawin et al. (2007b[Slawin, A. M. Z., Waddell, P. G. & Woollins, J. D. (2007b). Acta Cryst. E63, m2018.]) and for cis-bis­(trimethoxy­phos­phite)dichlorido­palladium(II), see Slawin et al. (2009[Slawin, A. M. Z., Waddell, P. G. & Woollins, J. D. (2009). Acta Cryst. E65, m1391.]).

[Scheme 1]

Experimental

Crystal data
  • [PtCl2(C9H21O3P)2]

  • Mr = 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[Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.356, Tmax = 0.506

  • 24157 measured reflections

  • 4995 independent reflections

  • 4473 reflections with I > 2σ(I)

  • Rint = 0.040

Refinement
  • R[F2 > 2σ(F2)] = 0.024

  • wR(F2) = 0.038

  • S = 1.11

  • 4995 reflections

  • 275 parameters

  • H-atom parameters constrained

  • Δρmax = 0.57 e Å−3

  • Δρmin = −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[Rigaku (2006). SCXmini Benchtop Crystallography System Software and CrystalStructure. Rigaku Americas Corporation, The Woodlands, Texas, USA.]); cell refinement: PROCESS-AUTO (Rigaku, 1998[Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.]); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: CrystalStructure (Rigaku, 2006[Rigaku (2006). SCXmini Benchtop Crystallography System Software and CrystalStructure. Rigaku Americas Corporation, The Woodlands, Texas, USA.]); software used to prepare material for publication: CrystalStructure.

Supporting information


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.

Refinement top

All H atoms were included in calculated positions (C—H distances are 0.98 Å for methyl H atoms, 1.00 Å for methylene H atoms) and were refined as riding atoms with Uiso(H) = 1.2 Ueq(parent atom, methylene H atoms) or Uiso(H) = 1.5 Ueq(parent atom, methyl H atoms). The highest peak in the difference map is 1.23 Å from atom Pt1.

Structure description 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) °

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

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
[Figure 1] 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
Mr = 682.47Dx = 1.593 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ybcCell parameters from 27042 reflections
a = 10.8962 (4) Åθ = 3.0–27.5°
b = 18.9114 (8) ŵ = 5.24 mm1
c = 14.2754 (6) ÅT = 125 K
β = 104.7461 (10)°Chip, colourless
V = 2844.7 (2) Å30.22 × 0.22 × 0.13 mm
Z = 4
Data collection top
Rigaku SCXmini
diffractometer
4995 independent reflections
Radiation source: fine-focus sealed tube4473 reflections with F2 > 2σ(F2)
Detector resolution: 6.85 pixels mm-1Rint = 0.040
ω scansθmax = 25.0°, θmin = 2.1°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1212
Tmin = 0.356, Tmax = 0.506k = 2222
24157 measured reflectionsl = 1616
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.024 w = 1/[σ2(Fo2) + (0.0077P)2 + 2.3925P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.038(Δ/σ)max = 0.001
S = 1.11Δρmax = 0.57 e Å3
4995 reflectionsΔρmin = 0.49 e Å3
275 parameters
Crystal data top
[PtCl2(C9H21O3P)2]V = 2844.7 (2) Å3
Mr = 682.47Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.8962 (4) ŵ = 5.24 mm1
b = 18.9114 (8) ÅT = 125 K
c = 14.2754 (6) Å0.22 × 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)
Tmin = 0.356, Tmax = 0.506Rint = 0.040
24157 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.024275 parameters
wR(F2) = 0.038H-atom parameters constrained
S = 1.11Δρmax = 0.57 e Å3
4995 reflectionsΔρmin = 0.49 e Å3
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
xyzUiso*/Ueq
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)0.01950.00890.24730.026*
H(2)0.28470.03770.31200.039*
H(3)0.17440.09280.31550.039*
H(4)0.19450.02390.38280.039*
H(5)0.05480.00430.09240.046*
H(6)0.09120.07440.13060.046*
H(7)0.20050.01730.13380.046*
H(8)0.22170.14810.19370.037*
H(9)0.23170.02880.06770.070*
H(10)0.35010.05600.10490.070*
H(11)0.22860.02370.18020.070*
H(12)0.19120.21690.06270.062*
H(13)0.32770.17990.03260.062*
H(14)0.21280.14840.00540.062*
H(15)0.03240.18720.43220.034*
H(16)0.08350.04460.49550.046*
H(17)0.12830.11190.56360.046*
H(18)0.18500.09840.47210.046*
H(19)0.18090.16670.42390.054*
H(20)0.10070.15470.53340.054*
H(21)0.15000.08820.46480.054*
H(22)0.40310.33420.20350.027*
H(23)0.64620.29180.32100.038*
H(24)0.62650.33310.22040.038*
H(25)0.57330.25430.22190.038*
H(26)0.39790.41460.32880.038*
H(27)0.51600.43320.28570.038*
H(28)0.53830.39180.38640.038*
H(29)0.21410.12930.12250.027*
H(30)0.42760.15180.04440.053*
H(31)0.31350.09910.00230.053*
H(32)0.40410.08290.10260.053*
H(33)0.15100.24410.07120.064*
H(34)0.15300.19590.02050.064*
H(35)0.26600.25050.02080.064*
H(36)0.54580.16930.36740.030*
H(37)0.45700.03210.40000.064*
H(38)0.59710.04900.39020.064*
H(39)0.47780.05890.29890.064*
H(40)0.52050.20010.51920.056*
H(41)0.62170.13730.53110.056*
H(42)0.47970.12090.53670.056*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
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)1.000C(16)—H(36)1.000
C(2)—H(2)0.980C(17)—H(37)0.980
C(2)—H(3)0.980C(17)—H(38)0.980
C(2)—H(4)0.980C(17)—H(39)0.980
C(3)—H(5)0.980C(18)—H(40)0.980
C(3)—H(6)0.980C(18)—H(41)0.980
C(3)—H(7)0.980C(18)—H(42)0.980
Cl(2)···C(11)i3.410 (3)H(19)···H(12)ii2.981
C(7)···C(15)ii3.591 (5)H(19)···H(23)i3.144
C(11)···Cl(2)iii3.410 (3)H(19)···H(36)i2.880
C(15)···C(7)iv3.591 (5)H(19)···H(38)i3.233
Pt(1)···H(34)ii3.155H(19)···H(41)i2.992
Pt(1)···H(35)ii3.571H(20)···Cl(2)ii3.557
Cl(1)···H(1)v3.035H(20)···C(2)vi3.340
Cl(1)···H(3)v3.574H(20)···H(3)vi2.748
Cl(1)···H(6)v3.551H(20)···H(4)vi3.036
Cl(1)···H(11)v3.162H(20)···H(12)ii2.693
Cl(1)···H(17)iv2.893H(20)···H(33)ii3.275
Cl(1)···H(31)ii3.369H(20)···H(41)i3.034
Cl(1)···H(34)ii3.231H(21)···C(2)vi3.364
Cl(2)···H(3)v2.807H(21)···C(8)vi3.505
Cl(2)···H(6)v3.238H(21)···H(3)vi3.215
Cl(2)···H(20)iv3.557H(21)···H(4)vi2.643
Cl(2)···H(23)i3.099H(21)···H(16)vi2.635
Cl(2)···H(24)i3.101H(21)···H(36)i3.595
Cl(2)···H(25)i3.479H(21)···H(38)i2.791
P(2)···H(35)ii3.584H(21)···H(41)i3.024
O(4)···H(30)ii3.339H(22)···C(18)iv3.473
O(4)···H(35)ii3.567H(22)···H(17)iv3.309
O(6)···H(35)ii3.185H(22)···H(40)iv3.269
C(2)···H(20)vi3.340H(22)···H(42)iv2.845
C(2)···H(21)vi3.364H(23)···Cl(2)iii3.099
C(2)···H(24)vii3.170H(23)···C(6)xii3.256
C(2)···H(41)viii3.076H(23)···H(12)xii3.457
C(3)···H(5)ix3.389H(23)···H(13)xii3.010
C(3)···H(9)ix3.526H(23)···H(14)xii2.801
C(3)···H(14)ix3.383H(23)···H(19)iii3.144
C(5)···H(26)x3.186H(24)···Cl(2)iii3.101
C(5)···H(31)ix3.298H(24)···C(2)xiii3.170
C(6)···H(23)xi3.256H(24)···C(18)iv2.992
C(6)···H(28)xi3.159H(24)···H(2)xiii2.711
C(6)···H(40)xi3.542H(24)···H(3)xiii2.739
C(7)···H(33)ii3.138H(24)···H(40)iv2.879
C(7)···H(34)ii3.535H(24)···H(41)iv2.747
C(7)···H(35)ii3.525H(24)···H(42)iv2.839
C(8)···H(16)vi3.382H(25)···Cl(2)iii3.479
C(8)···H(21)vi3.505H(25)···C(18)iv3.507
C(8)···H(33)ii3.230H(25)···H(8)iii3.106
C(8)···H(35)ii3.369H(25)···H(13)iii3.455
C(9)···H(3)vi3.420H(25)···H(40)iv2.933
C(9)···H(4)vi3.281H(25)···H(41)iv3.554
C(9)···H(12)ii3.277H(25)···H(42)iv3.497
C(9)···H(16)vi3.475H(26)···C(5)v3.186
C(9)···H(38)i3.447H(26)···C(14)ii3.456
C(9)···H(41)i3.199H(26)···H(9)v3.390
C(10)···H(42)iv3.489H(26)···H(10)v2.928
C(11)···H(40)iv3.285H(26)···H(11)v2.748
C(11)···H(41)iv3.543H(26)···H(30)ii3.263
C(11)···H(42)iv3.416H(26)···H(31)ii2.802
C(12)···H(10)v3.574H(27)···C(17)xiii3.273
C(12)···H(13)xii3.519H(27)···H(2)xiii2.916
C(12)···H(30)ii3.497H(27)···H(7)xiii3.151
C(12)···H(31)ii3.453H(27)···H(10)v3.541
C(12)···H(39)xiii3.582H(27)···H(32)xiii3.257
C(14)···H(9)ix3.453H(27)···H(37)xiii3.318
C(14)···H(10)iii3.262H(27)···H(38)xiii3.323
C(14)···H(26)iv3.456H(27)···H(39)xiii2.675
C(14)···H(28)iv3.479H(28)···C(6)xii3.159
C(15)···H(15)iv2.759H(28)···C(14)ii3.479
C(15)···H(17)iv3.369H(28)···H(7)xiii3.399
C(15)···H(18)iv3.591H(28)···H(9)xii3.454
C(16)···H(19)iii3.510H(28)···H(10)xii3.201
C(17)···H(27)vii3.273H(28)···H(13)xii2.603
C(18)···H(2)viii3.554H(28)···H(14)xii2.862
C(18)···H(13)xii3.538H(28)···H(30)ii2.934
C(18)···H(22)ii3.473H(28)···H(31)ii3.245
C(18)···H(24)ii2.992H(30)···O(4)iv3.339
C(18)···H(25)ii3.507H(30)···C(12)iv3.497
C(18)···H(35)ii3.510H(30)···H(10)iii2.971
H(1)···Cl(1)x3.035H(30)···H(13)iii2.766
H(2)···C(18)viii3.554H(30)···H(26)iv3.263
H(2)···H(24)vii2.711H(30)···H(28)iv2.934
H(2)···H(27)vii2.916H(30)···H(40)iv3.031
H(2)···H(41)viii2.905H(31)···Cl(1)iv3.369
H(2)···H(42)viii3.302H(31)···C(5)ix3.298
H(3)···Cl(1)x3.574H(31)···C(12)iv3.453
H(3)···Cl(2)x2.807H(31)···H(9)ix2.663
H(3)···C(9)vi3.420H(31)···H(10)ix3.348
H(3)···H(20)vi2.748H(31)···H(11)ix3.390
H(3)···H(21)vi3.215H(31)···H(26)iv2.802
H(3)···H(24)vii2.739H(31)···H(28)iv3.245
H(3)···H(41)viii2.821H(32)···H(9)ix3.403
H(4)···C(9)vi3.281H(32)···H(10)iii2.718
H(4)···H(20)vi3.036H(32)···H(27)vii3.257
H(4)···H(21)vi2.643H(33)···C(7)iv3.138
H(4)···H(38)viii3.484H(33)···C(8)iv3.230
H(4)···H(41)viii2.978H(33)···H(15)iv2.448
H(5)···C(3)ix3.389H(33)···H(17)iv2.734
H(5)···H(5)ix2.610H(33)···H(18)iv3.358
H(5)···H(6)ix3.442H(33)···H(20)iv3.275
H(5)···H(9)ix3.402H(34)···Pt(1)iv3.155
H(6)···Cl(1)x3.551H(34)···Cl(1)iv3.231
H(6)···Cl(2)x3.238H(34)···C(7)iv3.535
H(6)···H(5)ix3.442H(34)···H(6)ix3.563
H(6)···H(14)ix2.849H(34)···H(15)iv2.572
H(6)···H(34)ix3.563H(35)···Pt(1)iv3.571
H(7)···H(9)ix2.989H(35)···P(2)iv3.584
H(7)···H(14)ix3.107H(35)···O(4)iv3.567
H(7)···H(27)vii3.151H(35)···O(6)iv3.185
H(7)···H(28)vii3.399H(35)···C(7)iv3.525
H(8)···H(25)i3.106H(35)···C(8)iv3.369
H(9)···C(3)ix3.526H(35)···C(18)iv3.510
H(9)···C(14)ix3.453H(35)···H(15)iv2.797
H(9)···H(5)ix3.402H(35)···H(17)iv3.139
H(9)···H(7)ix2.989H(35)···H(18)iv3.018
H(9)···H(26)x3.390H(35)···H(40)iv2.932
H(9)···H(28)xi3.454H(35)···H(42)iv3.335
H(9)···H(31)ix2.663H(36)···H(19)iii2.880
H(9)···H(32)ix3.403H(36)···H(21)iii3.595
H(10)···C(12)x3.574H(37)···H(27)vii3.318
H(10)···C(14)i3.262H(37)···H(37)viii3.023
H(10)···H(26)x2.928H(37)···H(38)viii3.544
H(10)···H(27)x3.541H(37)···H(41)viii3.520
H(10)···H(28)xi3.201H(37)···H(42)viii3.056
H(10)···H(30)i2.971H(38)···C(9)iii3.447
H(10)···H(31)ix3.348H(38)···H(4)viii3.484
H(10)···H(32)i2.718H(38)···H(19)iii3.233
H(11)···Cl(1)x3.162H(38)···H(21)iii2.791
H(11)···H(26)x2.748H(38)···H(27)vii3.323
H(11)···H(31)ix3.390H(38)···H(37)viii3.544
H(12)···C(9)iv3.277H(38)···H(42)viii3.542
H(12)···H(19)iv2.981H(39)···C(12)vii3.582
H(12)···H(20)iv2.693H(39)···H(27)vii2.675
H(12)···H(23)xi3.457H(40)···C(6)xii3.542
H(12)···H(40)xi3.425H(40)···C(11)ii3.285
H(12)···H(41)xi3.390H(40)···H(12)xii3.425
H(13)···C(12)xi3.519H(40)···H(13)xii2.787
H(13)···C(18)xi3.538H(40)···H(22)ii3.269
H(13)···H(23)xi3.010H(40)···H(24)ii2.879
H(13)···H(25)i3.455H(40)···H(25)ii2.933
H(13)···H(28)xi2.603H(40)···H(30)ii3.031
H(13)···H(30)i2.766H(40)···H(35)ii2.932
H(13)···H(40)xi2.787H(41)···C(2)viii3.076
H(13)···H(41)xi3.501H(41)···C(9)iii3.199
H(14)···C(3)ix3.383H(41)···C(11)ii3.543
H(14)···H(6)ix2.849H(41)···H(2)viii2.905
H(14)···H(7)ix3.107H(41)···H(3)viii2.821
H(14)···H(23)xi2.801H(41)···H(4)viii2.978
H(14)···H(28)xi2.862H(41)···H(12)xii3.390
H(15)···C(15)ii2.759H(41)···H(13)xii3.501
H(15)···H(33)ii2.448H(41)···H(19)iii2.992
H(15)···H(34)ii2.572H(41)···H(20)iii3.034
H(15)···H(35)ii2.797H(41)···H(21)iii3.024
H(16)···C(8)vi3.382H(41)···H(24)ii2.747
H(16)···C(9)vi3.475H(41)···H(25)ii3.554
H(16)···H(16)vi2.508H(41)···H(37)viii3.520
H(16)···H(21)vi2.635H(42)···C(10)ii3.489
H(17)···Cl(1)ii2.893H(42)···C(11)ii3.416
H(17)···C(15)ii3.369H(42)···H(2)viii3.302
H(17)···H(22)ii3.309H(42)···H(22)ii2.845
H(17)···H(33)ii2.734H(42)···H(24)ii2.839
H(17)···H(35)ii3.139H(42)···H(25)ii3.497
H(18)···C(15)ii3.591H(42)···H(35)ii3.335
H(18)···H(33)ii3.358H(42)···H(37)viii3.056
H(18)···H(35)ii3.018H(42)···H(38)viii3.542
H(19)···C(16)i3.510
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)109.4H(30)—C(14)—H(31)109.5
C(2)—C(1)—H(1)109.4H(30)—C(14)—H(32)109.5
C(3)—C(1)—H(1)109.4H(31)—C(14)—H(32)109.5
C(1)—C(2)—H(2)109.5C(13)—C(15)—H(33)109.5
C(1)—C(2)—H(3)109.5C(13)—C(15)—H(34)109.5
C(1)—C(2)—H(4)109.5C(13)—C(15)—H(35)109.5
H(2)—C(2)—H(3)109.5H(33)—C(15)—H(34)109.5
H(2)—C(2)—H(4)109.5H(33)—C(15)—H(35)109.5
H(3)—C(2)—H(4)109.5H(34)—C(15)—H(35)109.5
C(1)—C(3)—H(5)109.5O(6)—C(16)—H(36)109.1
C(1)—C(3)—H(6)109.5C(17)—C(16)—H(36)109.1
C(1)—C(3)—H(7)109.5C(18)—C(16)—H(36)109.1
H(5)—C(3)—H(6)109.5C(16)—C(17)—H(37)109.5
H(5)—C(3)—H(7)109.5C(16)—C(17)—H(38)109.5
H(6)—C(3)—H(7)109.5C(16)—C(17)—H(39)109.5
O(2)—C(4)—H(8)110.1H(37)—C(17)—H(38)109.5
C(5)—C(4)—H(8)110.1H(37)—C(17)—H(39)109.5
C(6)—C(4)—H(8)110.1H(38)—C(17)—H(39)109.5
C(4)—C(5)—H(9)109.5C(16)—C(18)—H(40)109.5
C(4)—C(5)—H(10)109.5C(16)—C(18)—H(41)109.5
C(4)—C(5)—H(11)109.5C(16)—C(18)—H(42)109.5
H(9)—C(5)—H(10)109.5H(40)—C(18)—H(41)109.5
H(9)—C(5)—H(11)109.5H(40)—C(18)—H(42)109.5
H(10)—C(5)—H(11)109.5H(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) x1, y, z; (ii) x, y+1/2, z+1/2; (iii) x+1, y, z; (iv) x, y+1/2, z1/2; (v) x, y+1/2, z+1/2; (vi) x, y, z+1; (vii) x+1, y1/2, z+1/2; (viii) x+1, y, z+1; (ix) x, y, z; (x) x, y1/2, z+1/2; (xi) x1, y+1/2, z1/2; (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]
Mr682.47
Crystal system, space groupMonoclinic, P21/c
Temperature (K)125
a, b, c (Å)10.8962 (4), 18.9114 (8), 14.2754 (6)
β (°) 104.7461 (10)
V3)2844.7 (2)
Z4
Radiation typeMo Kα
µ (mm1)5.24
Crystal size (mm)0.22 × 0.22 × 0.13
Data collection
DiffractometerRigaku SCXmini
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.356, 0.506
No. of measured, independent and
observed [F2 > 2σ(F2)] reflections
24157, 4995, 4473
Rint0.040
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.038, 1.11
No. of reflections4995
No. of parameters275
No. of restraints?
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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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First citationHigashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationRigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationRigaku (2006). SCXmini Benchtop Crystallography System Software and CrystalStructure. Rigaku Americas Corporation, The Woodlands, Texas, USA.  Google Scholar
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First citationSlawin, A. M. Z., Waddell, P. G. & Woollins, J. D. (2007b). Acta Cryst. E63, m2018.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationSlawin, A. M. Z., Waddell, P. G. & Woollins, J. D. (2009). Acta Cryst. E65, m1391.  Web of Science CrossRef IUCr Journals Google Scholar

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