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The title compound, [PtCl2(C8H19P)(C18H15P)]·0.5C4H8O, was obtained in the reaction of bis­(triphenyl­phosphine)­platinum(II) chloride with 1,1,3,3-tetra-tert-butyl-2-trimethyl­silyltriphosphine. The 31P{1H} NMR spectrum of the reaction mixture shows the formation of the title compound together with a significant amount of triphenyl­phosphine and 1,1,3,3-tetra-tert-butyl­triphosphine.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807005259/bt2255sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807005259/bt2255Isup2.hkl
Contains datablock I

CCDC reference: 236970

Key indicators

  • Single-crystal X-ray study
  • T = 180 K
  • Mean [sigma](C-C) = 0.005 Å
  • Disorder in main residue
  • R factor = 0.019
  • wR factor = 0.047
  • Data-to-parameter ratio = 15.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.26 Ratio PLAT412_ALERT_2_B Short Intra XH3 .. XHn H26A .. H21E .. 1.73 Ang.
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.40 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C23 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C28 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C27 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C29 PLAT301_ALERT_3_C Main Residue Disorder ......................... 9.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc.
Alert level G ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.278 0.479 Tmin and Tmax expected: 0.223 0.458 RR = 1.189 Please check that your absorption correction is appropriate.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: X-AREA (Stoe & Cie, 1997); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

cis-Dichloro(di-tert-butylphosphine-κP)(triphenylphosphine- κP)platinum(II) tetrahydrofuran hemisolvate top
Crystal data top
[PtCl2(C8H19P)(C18H15P)]·0.5C4H8OF(000) = 1408
Mr = 1421.03Dx = 1.644 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 8000 reflections
a = 16.3384 (14) Åθ = 1.5–25°
b = 11.9630 (8) ŵ = 5.20 mm1
c = 16.5346 (14) ÅT = 180 K
β = 117.346 (9)°Parallelepiped, pale yellow
V = 2870.6 (5) Å30.33 × 0.25 × 0.15 mm
Z = 2
Data collection top
Stoe IPDS
diffractometer
4328 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
area–detector scansθmax = 25.1°, θmin = 2.2°
Absorption correction: numerical
(Six faces defined; X-RED; Stoe & Cie, 1997)
h = 1917
Tmin = 0.278, Tmax = 0.480k = 014
11449 measured reflectionsl = 019
4926 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.047H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.032P)2]
where P = (Fo2 + 2Fc2)/3
4926 reflections(Δ/σ)max = 0.001
326 parametersΔρmax = 0.77 e Å3
9 restraintsΔρmin = 0.95 e Å3
Special details top

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
xyzUiso*/UeqOcc. (<1)
Pt10.816183 (7)0.473615 (9)0.039440 (7)0.01584 (5)
Cl10.92824 (5)0.50826 (7)0.19056 (5)0.02612 (17)
Cl20.89698 (6)0.30851 (8)0.04433 (6)0.0396 (2)
P10.75050 (5)0.63678 (6)0.04673 (5)0.01472 (15)
P20.71798 (5)0.43698 (7)0.10731 (5)0.01967 (16)
H10.654 (2)0.513 (3)0.146 (2)0.025 (9)*
C10.81973 (18)0.7580 (3)0.04729 (18)0.0177 (6)
C20.90766 (19)0.7443 (3)0.0562 (2)0.0225 (7)
H20.93260.67130.0620.027*
C30.9598 (2)0.8368 (3)0.0566 (2)0.0316 (8)
H31.01970.82610.06190.038*
C40.9252 (2)0.9439 (3)0.0495 (2)0.0305 (8)
H40.96191.00670.05210.037*
C50.8366 (2)0.9589 (3)0.0386 (2)0.0265 (7)
H50.8121.03220.03240.032*
C60.7834 (2)0.8669 (3)0.0367 (2)0.0224 (7)
H60.72240.87770.02830.027*
C70.72801 (18)0.6466 (3)0.14498 (19)0.0181 (6)
C80.7025 (2)0.7479 (3)0.1693 (2)0.0303 (8)
H80.70180.81430.13750.036*
C90.6783 (2)0.7523 (3)0.2394 (3)0.0349 (8)
H90.66220.82180.2560.042*
C100.6777 (2)0.6556 (3)0.2854 (2)0.0370 (9)
H100.66180.65850.3340.044*
C110.7004 (3)0.5547 (3)0.2597 (3)0.0402 (9)
H110.69860.48790.28990.048*
C120.7256 (2)0.5502 (3)0.1909 (2)0.0287 (7)
H120.74140.48030.17450.034*
C130.63647 (18)0.6690 (2)0.04664 (19)0.0166 (6)
C140.5580 (2)0.6328 (3)0.0417 (2)0.0271 (7)
H140.56330.59660.01160.032*
C150.4714 (2)0.6500 (4)0.1156 (3)0.0400 (10)
H150.41750.62610.11230.048*
C160.4636 (2)0.7015 (3)0.1930 (2)0.0390 (9)
H160.40450.71220.24330.047*
C170.5413 (2)0.7379 (3)0.1982 (2)0.0303 (8)
H170.53570.77380.25180.036*
C180.62786 (19)0.7217 (3)0.1247 (2)0.0214 (7)
H180.68130.74690.1280.026*
C190.6404 (2)0.3125 (3)0.1299 (3)0.0317 (8)
C200.5861 (5)0.3351 (5)0.0764 (5)0.0522 (19)0.852 (13)
H20A0.54360.2730.08560.063*0.852 (13)
H20B0.5510.40460.09820.063*0.852 (13)
H20C0.6290.34210.01150.063*0.852 (13)
C210.6910 (4)0.2013 (4)0.0981 (6)0.058 (2)0.852 (13)
H21A0.72880.20270.03180.07*0.852 (13)
H21B0.73070.18940.12730.07*0.852 (13)
H21C0.64610.14040.11480.07*0.852 (13)
C220.5703 (4)0.3039 (6)0.2307 (4)0.0452 (15)0.852 (13)
H22A0.60210.28230.26620.054*0.852 (13)
H22B0.54020.37650.2520.054*0.852 (13)
H22C0.52390.24750.23830.054*0.852 (13)
C20A0.6325 (19)0.295 (2)0.0405 (19)0.029 (7)*0.148 (13)
H20D0.59390.22990.04690.035*0.148 (13)
H20E0.60460.36170.02860.035*0.148 (13)
H20F0.6940.28350.01030.035*0.148 (13)
C21A0.6852 (19)0.204 (2)0.153 (2)0.037 (7)*0.148 (13)
H21D0.74870.19430.10570.044*0.148 (13)
H21E0.6850.21540.21210.044*0.148 (13)
H21F0.6490.13770.15630.044*0.148 (13)
C22A0.550 (2)0.344 (3)0.221 (2)0.033 (8)*0.148 (13)
H22D0.56740.37630.26490.039*0.148 (13)
H22E0.51360.39860.20640.039*0.148 (13)
H22F0.5130.27650.24630.039*0.148 (13)
C230.7717 (2)0.4534 (3)0.1851 (2)0.0310 (8)
C240.6994 (3)0.4913 (4)0.2792 (3)0.0590 (13)
H24A0.72930.50730.31750.071*
H24B0.66890.55910.27320.071*
H24C0.65350.4320.30730.071*
C250.8436 (3)0.5461 (4)0.1456 (3)0.0559 (13)
H25A0.89380.52140.08750.067*
H25B0.81490.61320.13580.067*
H25C0.86820.56320.18820.067*
C260.8163 (4)0.3463 (4)0.1957 (4)0.0707 (15)
H26A0.76870.28940.22580.085*
H26B0.86090.31920.13550.085*
H26C0.84790.36140.23250.085*
O10.6019 (4)0.9992 (6)0.0225 (5)0.0670 (18)*0.5
C270.5263 (6)0.9822 (10)0.0632 (6)0.058 (3)*0.5
H27A0.52830.90520.08420.07*0.5
H27B0.52981.0350.10760.07*0.5
C280.4400 (6)0.9990 (15)0.0591 (8)0.125 (6)*0.5
H28A0.40770.9270.06560.15*0.5
H28B0.3991.05020.10810.15*0.5
C290.4672 (5)1.0495 (10)0.0329 (7)0.065 (3)*0.5
H29A0.44161.12570.02730.078*0.5
H29B0.44581.00270.06880.078*0.5
C300.5670 (5)1.0521 (9)0.0745 (6)0.059 (3)*0.5
H30A0.58781.13090.0840.071*0.5
H30B0.59221.01570.13490.071*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pt10.01787 (7)0.01566 (7)0.01269 (7)0.00382 (4)0.00591 (5)0.00152 (4)
Cl10.0239 (3)0.0299 (4)0.0161 (4)0.0020 (3)0.0019 (3)0.0010 (3)
Cl20.0428 (5)0.0342 (5)0.0324 (5)0.0231 (4)0.0093 (4)0.0014 (4)
P10.0161 (3)0.0149 (4)0.0120 (3)0.0011 (3)0.0054 (3)0.0002 (3)
P20.0229 (4)0.0191 (4)0.0143 (4)0.0035 (3)0.0062 (3)0.0020 (3)
C10.0196 (14)0.0188 (15)0.0141 (14)0.0008 (11)0.0072 (11)0.0004 (11)
C20.0217 (14)0.0237 (16)0.0215 (15)0.0021 (12)0.0094 (12)0.0031 (13)
C30.0233 (15)0.039 (2)0.0349 (19)0.0022 (14)0.0151 (14)0.0052 (16)
C40.0386 (18)0.0247 (17)0.0288 (18)0.0106 (14)0.0159 (15)0.0026 (14)
C50.0405 (17)0.0158 (16)0.0271 (18)0.0014 (12)0.0188 (15)0.0016 (13)
C60.0256 (15)0.0215 (16)0.0220 (16)0.0010 (13)0.0125 (12)0.0004 (13)
C70.0169 (13)0.0255 (16)0.0115 (13)0.0020 (11)0.0061 (11)0.0024 (12)
C80.0457 (19)0.0227 (17)0.0316 (18)0.0060 (14)0.0257 (16)0.0045 (15)
C90.0458 (19)0.033 (2)0.038 (2)0.0078 (15)0.0291 (16)0.0141 (16)
C100.0364 (18)0.059 (3)0.0201 (17)0.0030 (17)0.0169 (15)0.0006 (17)
C110.045 (2)0.045 (2)0.035 (2)0.0118 (17)0.0221 (17)0.0199 (17)
C120.0351 (17)0.0269 (17)0.0272 (17)0.0081 (13)0.0170 (14)0.0094 (14)
C130.0190 (13)0.0134 (14)0.0161 (14)0.0019 (11)0.0069 (11)0.0024 (11)
C140.0232 (15)0.0370 (19)0.0177 (15)0.0034 (13)0.0065 (13)0.0015 (14)
C150.0177 (15)0.063 (3)0.034 (2)0.0072 (16)0.0068 (14)0.0046 (19)
C160.0211 (16)0.060 (3)0.0226 (18)0.0035 (15)0.0017 (13)0.0060 (17)
C170.0280 (16)0.036 (2)0.0195 (16)0.0051 (14)0.0047 (13)0.0059 (15)
C180.0212 (14)0.0210 (16)0.0192 (15)0.0066 (12)0.0070 (12)0.0025 (12)
C190.0317 (17)0.0261 (18)0.0357 (19)0.0034 (13)0.0142 (15)0.0074 (15)
C200.061 (4)0.050 (3)0.059 (4)0.029 (3)0.039 (3)0.020 (3)
C210.057 (3)0.022 (2)0.075 (5)0.006 (2)0.013 (3)0.001 (3)
C220.029 (2)0.044 (3)0.048 (3)0.007 (2)0.006 (2)0.011 (3)
C230.0411 (18)0.036 (2)0.0211 (17)0.0036 (14)0.0190 (15)0.0009 (14)
C240.068 (3)0.080 (3)0.021 (2)0.012 (2)0.014 (2)0.011 (2)
C250.062 (3)0.081 (4)0.042 (2)0.029 (2)0.039 (2)0.015 (2)
C260.109 (4)0.070 (3)0.072 (3)0.034 (3)0.075 (3)0.010 (3)
Geometric parameters (Å, º) top
Pt1—P22.2533 (8)C19—C22A1.59 (3)
Pt1—P12.2572 (7)C19—C21A1.62 (3)
Pt1—Cl22.3564 (8)C20—H20A0.98
Pt1—Cl12.3589 (8)C20—H20B0.98
P1—C71.827 (3)C20—H20C0.98
P1—C131.833 (3)C21—H21A0.98
P1—C11.836 (3)C21—H21B0.98
P2—C231.871 (4)C21—H21C0.98
P2—C191.878 (3)C22—H22A0.98
P2—H11.30 (3)C22—H22B0.98
C1—C21.385 (4)C22—H22C0.98
C1—C61.409 (4)C20A—H20D0.98
C2—C31.394 (5)C20A—H20E0.98
C2—H20.95C20A—H20F0.98
C3—C41.384 (5)C21A—H21D0.98
C3—H30.95C21A—H21E0.98
C4—C51.387 (5)C21A—H21F0.98
C4—H40.95C22A—H22D0.98
C5—C61.393 (5)C22A—H22E0.98
C5—H50.95C22A—H22F0.98
C6—H60.95C23—C261.523 (6)
C7—C121.392 (5)C23—C251.527 (5)
C7—C81.399 (5)C23—C241.527 (5)
C8—C91.387 (5)C24—H24A0.98
C8—H80.95C24—H24B0.98
C9—C101.387 (6)C24—H24C0.98
C9—H90.95C25—H25A0.98
C10—C111.386 (6)C25—H25B0.98
C10—H100.95C25—H25C0.98
C11—C121.377 (5)C26—H26A0.98
C11—H110.95C26—H26B0.98
C12—H120.95C26—H26C0.98
C13—C181.384 (4)O1—C28i1.104 (14)
C13—C141.390 (4)O1—C29i1.227 (11)
C14—C151.397 (4)O1—C301.384 (8)
C14—H140.95O1—C271.403 (8)
C15—C161.373 (6)C27—C281.456 (8)
C15—H150.95C27—H27A0.99
C16—C171.382 (5)C27—H27B0.99
C16—H160.95C28—C291.502 (9)
C17—C181.391 (4)C28—H28A0.99
C17—H170.95C28—H28B0.99
C18—H180.95C29—C301.449 (7)
C19—C211.527 (6)C29—H29A0.99
C19—C221.532 (6)C29—H29B0.99
C19—C201.536 (7)C30—H30A0.99
C19—C20A1.55 (3)C30—H30B0.99
P2—Pt1—P196.02 (3)C21—C19—P2114.4 (3)
P2—Pt1—Cl289.11 (3)C22—C19—P2111.6 (3)
P1—Pt1—Cl2174.64 (3)C20—C19—P2105.2 (3)
P2—Pt1—Cl1175.64 (3)C20A—C19—P2105.0 (9)
P1—Pt1—Cl187.03 (3)C22A—C19—P2104.4 (11)
Cl2—Pt1—Cl187.76 (3)C21A—C19—P2110.1 (10)
C7—P1—C13101.17 (13)C19—C20—H20A109.5
C7—P1—C1108.64 (13)C19—C20—H20B109.5
C13—P1—C1102.93 (13)C19—C20—H20C109.5
C7—P1—Pt1113.46 (10)C19—C21—H21A109.5
C13—P1—Pt1117.44 (9)C19—C21—H21B109.5
C1—P1—Pt1112.10 (10)C19—C21—H21C109.5
C23—P2—C19115.70 (16)C19—C22—H22A109.5
C23—P2—Pt1113.15 (11)C19—C22—H22B109.5
C19—P2—Pt1116.72 (12)C19—C22—H22C109.5
C23—P2—H196.4 (17)C19—C20A—H20D109.5
C19—P2—H198.1 (15)C19—C20A—H20E109.5
Pt1—P2—H1113.8 (16)H20D—C20A—H20E109.5
C2—C1—C6118.7 (3)C19—C20A—H20F109.5
C2—C1—P1120.9 (2)H20D—C20A—H20F109.5
C6—C1—P1120.4 (2)H20E—C20A—H20F109.5
C1—C2—C3120.6 (3)C19—C21A—H21D109.5
C1—C2—H2119.7C19—C21A—H21E109.5
C3—C2—H2119.7H21D—C21A—H21E109.5
C4—C3—C2120.6 (3)C19—C21A—H21F109.5
C4—C3—H3119.7H21D—C21A—H21F109.5
C2—C3—H3119.7H21E—C21A—H21F109.5
C3—C4—C5119.5 (3)C19—C22A—H22D109.5
C3—C4—H4120.3C19—C22A—H22E109.5
C5—C4—H4120.3H22D—C22A—H22E109.5
C4—C5—C6120.3 (3)C19—C22A—H22F109.5
C4—C5—H5119.9H22D—C22A—H22F109.5
C6—C5—H5119.9H22E—C22A—H22F109.5
C5—C6—C1120.3 (3)C26—C23—C25110.2 (4)
C5—C6—H6119.9C26—C23—C24108.7 (4)
C1—C6—H6119.9C25—C23—C24107.7 (3)
C12—C7—C8118.3 (3)C26—C23—P2113.0 (3)
C12—C7—P1120.0 (2)C25—C23—P2107.1 (2)
C8—C7—P1121.3 (2)C24—C23—P2110.1 (3)
C9—C8—C7120.7 (3)C23—C24—H24A109.5
C9—C8—H8119.7C23—C24—H24B109.5
C7—C8—H8119.7H24A—C24—H24B109.5
C8—C9—C10120.2 (3)C23—C24—H24C109.5
C8—C9—H9119.9H24A—C24—H24C109.5
C10—C9—H9119.9H24B—C24—H24C109.5
C11—C10—C9119.1 (4)C23—C25—H25A109.5
C11—C10—H10120.4C23—C25—H25B109.5
C9—C10—H10120.4H25A—C25—H25B109.5
C12—C11—C10120.8 (4)C23—C25—H25C109.5
C12—C11—H11119.6H25A—C25—H25C109.5
C10—C11—H11119.6H25B—C25—H25C109.5
C11—C12—C7120.8 (3)C23—C26—H26A109.5
C11—C12—H12119.6C23—C26—H26B109.5
C7—C12—H12119.6H26A—C26—H26B109.5
C18—C13—C14119.7 (3)C23—C26—H26C109.5
C18—C13—P1120.6 (2)H26A—C26—H26C109.5
C14—C13—P1119.5 (2)H26B—C26—H26C109.5
C13—C14—C15119.6 (3)C30—O1—C27105.7 (5)
C13—C14—H14120.2O1—C27—C28110.8 (6)
C15—C14—H14120.2O1—C27—H27A109.5
C16—C15—C14120.2 (3)C28—C27—H27A109.5
C16—C15—H15119.9O1—C27—H27B109.5
C14—C15—H15119.9C28—C27—H27B109.5
C15—C16—C17120.4 (3)H27A—C27—H27B108.1
C15—C16—H16119.8C27—C28—C29105.1 (5)
C17—C16—H16119.8C27—C28—H28A110.7
C16—C17—C18119.7 (3)C29—C28—H28A110.7
C16—C17—H17120.2C27—C28—H28B110.7
C18—C17—H17120.2C29—C28—H28B110.7
C13—C18—C17120.4 (3)H28A—C28—H28B108.8
C13—C18—H18119.8C30—C29—C28103.6 (5)
C17—C18—H18119.8C30—C29—H29A111
C21—C19—C22109.4 (4)C28—C29—H29A111
C21—C19—C20108.7 (4)C30—C29—H29B111
C22—C19—C20107.3 (4)C28—C29—H29B111
C22—C19—C20A132.7 (10)H29A—C29—H29B109
C21—C19—C22A130.6 (12)O1—C30—C29113.0 (6)
C20—C19—C22A88.2 (13)O1—C30—H30A109
C20A—C19—C22A118.6 (15)C29—C30—H30A109
C22—C19—C21A83.1 (12)O1—C30—H30B109
C20—C19—C21A136.2 (12)C29—C30—H30B109
C20A—C19—C21A111.4 (15)H30A—C30—H30B107.8
C22A—C19—C21A106.8 (15)
Symmetry code: (i) x+1, y+2, z.
 

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