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The title compound, [Li(C24H20P3)(C4H8O)]n, was obtained by the reaction of bis­(triethyl­phosphane)­platinum(II) chloride with 1,1-di­phenyl-2-(tri­methyl­silyl)-2-li­thia­diphos­phane, (C6H5)2P—P(SiMe3)Li·3C4H8O. The compound is formed in the latter stages of the reaction. It is the first coordination polymer among known triphosphane lithium salts.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805014613/br6191sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805014613/br6191Isup2.hkl
Contains datablock I

CCDC reference: 274334

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.064
  • wR factor = 0.139
  • Data-to-parameter ratio = 24.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT328_ALERT_2_B Check for Possibly Missing H on sp3? Phosphor .. P3
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis RED (Oxford Diffraction, 2003); data reduction: CrysAlis RED; 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: SHELXL97.

catena-Poly[[(tetrahydrofuran-κO)lithium(I)]-µ-1,1,3,3- tetraphenyltriphosphane-κ2P1,P3:κP2] top
Crystal data top
[Li(C24H20P3)(C4H8O)]F(000) = 1008
Mr = 480.35Dx = 1.262 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 11491 reflections
a = 11.332 (5) Åθ = 2–25°
b = 9.519 (5) ŵ = 0.25 mm1
c = 23.514 (8) ÅT = 120 K
β = 94.735 (3)°Plate, orange
V = 2527.8 (19) Å30.31 × 0.27 × 0.10 mm
Z = 4
Data collection top
Kuma KM-4, CCD Camera Sapphire 2, Oxford Diffraction
diffractometer
6563 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.044
Graphite monochromatorθmax = 30.0°, θmin = 2.8°
ω (0.74°, 612 frames) scansh = 1515
22768 measured reflectionsk = 913
7335 independent reflectionsl = 3233
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)] = 0.064Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.139H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0491P)2 + 2.4715P]
where P = (Fo2 + 2Fc2)/3
7335 reflections(Δ/σ)max = 0.001
298 parametersΔρmax = 0.54 e Å3
0 restraintsΔρmin = 0.29 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*/Ueq
Li10.3550 (3)1.1896 (4)0.25179 (16)0.0248 (7)
C10.48652 (17)0.9153 (2)0.14545 (8)0.0199 (4)
C20.5376 (2)1.0175 (3)0.11275 (10)0.0307 (5)
H20.50831.11100.11260.037*
C30.6316 (2)0.9835 (3)0.08017 (11)0.0377 (6)
H30.66451.05360.05750.045*
C40.6766 (2)0.8492 (3)0.08084 (10)0.0358 (6)
H40.74120.82690.05920.043*
C50.6272 (2)0.7471 (3)0.11315 (11)0.0323 (5)
H50.65720.65400.11330.039*
C60.53338 (19)0.7804 (2)0.14556 (9)0.0250 (4)
H60.50100.70960.16810.030*
C70.23450 (17)0.9254 (2)0.13237 (8)0.0189 (4)
C80.24695 (19)0.8798 (2)0.07667 (9)0.0242 (4)
H80.32370.86300.06460.029*
C90.1472 (2)0.8587 (2)0.03865 (10)0.0292 (5)
H90.15670.82710.00100.035*
C100.0345 (2)0.8833 (3)0.05530 (10)0.0322 (5)
H100.03300.86760.02940.039*
C110.0213 (2)0.9312 (3)0.11018 (11)0.0320 (5)
H110.05560.94990.12170.038*
C120.12069 (19)0.9518 (2)0.14849 (9)0.0258 (4)
H120.11080.98420.18600.031*
C130.51649 (17)0.9296 (2)0.36183 (8)0.0201 (4)
C140.5983 (2)0.8340 (3)0.34456 (10)0.0298 (5)
H140.58120.78200.31040.036*
C150.7062 (2)0.8133 (3)0.37716 (12)0.0393 (6)
H150.76160.74720.36490.047*
C160.7325 (2)0.8877 (3)0.42662 (11)0.0376 (6)
H160.80600.87370.44840.045*
C170.6510 (2)0.9836 (3)0.44463 (11)0.0362 (6)
H170.66831.03440.47910.043*
C180.5444 (2)1.0052 (2)0.41235 (10)0.0299 (5)
H180.48971.07210.42460.036*
C190.27435 (17)0.9258 (2)0.37352 (8)0.0183 (4)
C200.19522 (19)1.0267 (2)0.39091 (9)0.0231 (4)
H200.19621.11880.37540.028*
C210.1150 (2)0.9939 (3)0.43076 (9)0.0281 (5)
H210.06101.06320.44180.034*
C220.1136 (2)0.8611 (3)0.45426 (9)0.0281 (5)
H220.05880.83890.48140.034*
C230.1924 (2)0.7604 (2)0.43805 (9)0.0283 (5)
H230.19170.66890.45420.034*
C240.27295 (19)0.7923 (2)0.39812 (9)0.0240 (4)
H240.32720.72280.38760.029*
C250.5175 (2)1.4012 (3)0.21059 (11)0.0331 (5)
H25A0.44751.46380.20880.040*
H25B0.52861.36700.17160.040*
C260.6262 (2)1.4782 (3)0.23503 (14)0.0443 (7)
H26A0.60431.55810.25900.053*
H26B0.67251.51420.20420.053*
C270.6964 (2)1.3694 (3)0.27064 (11)0.0409 (6)
H27A0.77201.34840.25410.049*
H27B0.71401.40320.31020.049*
C280.6184 (2)1.2402 (3)0.26945 (14)0.0448 (7)
H28A0.64821.16760.24410.054*
H28B0.61681.20030.30830.054*
O10.50203 (13)1.28570 (16)0.24824 (7)0.0264 (3)
P10.35909 (4)0.96479 (5)0.18548 (2)0.01665 (11)
P20.37625 (4)0.97047 (5)0.31951 (2)0.01696 (11)
P30.34791 (5)0.81145 (5)0.25340 (2)0.01821 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Li10.0206 (16)0.0259 (18)0.0281 (19)0.0023 (14)0.0032 (14)0.0008 (15)
C10.0190 (9)0.0242 (9)0.0164 (9)0.0046 (7)0.0001 (7)0.0039 (7)
C20.0319 (12)0.0304 (11)0.0304 (11)0.0045 (9)0.0074 (9)0.0039 (9)
C30.0340 (13)0.0528 (16)0.0282 (12)0.0138 (11)0.0125 (10)0.0019 (11)
C40.0226 (11)0.0595 (17)0.0260 (11)0.0083 (10)0.0065 (8)0.0150 (11)
C50.0240 (11)0.0370 (12)0.0362 (13)0.0000 (9)0.0043 (9)0.0141 (10)
C60.0222 (10)0.0260 (10)0.0273 (10)0.0032 (8)0.0053 (8)0.0037 (8)
C70.0213 (9)0.0155 (8)0.0195 (9)0.0021 (7)0.0001 (7)0.0023 (7)
C80.0248 (10)0.0262 (10)0.0214 (10)0.0009 (8)0.0003 (8)0.0001 (8)
C90.0345 (12)0.0312 (11)0.0208 (10)0.0037 (9)0.0050 (8)0.0014 (9)
C100.0282 (11)0.0365 (12)0.0300 (12)0.0081 (9)0.0101 (9)0.0086 (10)
C110.0203 (10)0.0433 (14)0.0320 (12)0.0040 (9)0.0001 (8)0.0061 (10)
C120.0237 (10)0.0315 (11)0.0225 (10)0.0021 (8)0.0030 (8)0.0023 (8)
C130.0186 (9)0.0211 (9)0.0201 (9)0.0031 (7)0.0009 (7)0.0039 (7)
C140.0258 (11)0.0393 (13)0.0241 (10)0.0046 (9)0.0016 (8)0.0005 (9)
C150.0251 (11)0.0541 (16)0.0386 (14)0.0102 (11)0.0013 (10)0.0068 (12)
C160.0240 (11)0.0528 (16)0.0345 (13)0.0045 (10)0.0079 (9)0.0151 (12)
C170.0366 (13)0.0403 (13)0.0293 (12)0.0115 (11)0.0108 (10)0.0019 (10)
C180.0297 (11)0.0292 (11)0.0295 (11)0.0022 (9)0.0060 (9)0.0048 (9)
C190.0205 (9)0.0194 (9)0.0147 (8)0.0006 (7)0.0008 (6)0.0025 (7)
C200.0269 (10)0.0232 (9)0.0189 (9)0.0064 (8)0.0005 (7)0.0016 (8)
C210.0274 (11)0.0370 (12)0.0202 (10)0.0115 (9)0.0039 (8)0.0037 (9)
C220.0262 (10)0.0416 (13)0.0170 (9)0.0012 (9)0.0050 (8)0.0023 (9)
C230.0368 (12)0.0269 (11)0.0220 (10)0.0037 (9)0.0067 (9)0.0000 (8)
C240.0285 (10)0.0210 (9)0.0232 (10)0.0017 (8)0.0072 (8)0.0012 (8)
C250.0303 (12)0.0358 (12)0.0324 (12)0.0040 (10)0.0016 (9)0.0105 (10)
C260.0352 (14)0.0353 (14)0.0612 (18)0.0094 (11)0.0026 (12)0.0043 (13)
C270.0220 (11)0.0674 (19)0.0326 (13)0.0035 (11)0.0023 (9)0.0086 (12)
C280.0286 (13)0.0414 (15)0.0625 (19)0.0076 (11)0.0073 (12)0.0152 (13)
O10.0201 (7)0.0253 (7)0.0333 (8)0.0003 (6)0.0007 (6)0.0047 (6)
P10.0180 (2)0.0166 (2)0.0154 (2)0.00157 (17)0.00164 (16)0.00037 (17)
P20.0184 (2)0.0167 (2)0.0156 (2)0.00007 (17)0.00003 (16)0.00023 (17)
P30.0221 (2)0.0174 (2)0.0151 (2)0.00195 (18)0.00120 (17)0.00009 (18)
Geometric parameters (Å, º) top
Li1—O11.909 (4)C15—H150.9500
Li1—P3i2.569 (4)C16—C171.389 (4)
Li1—P22.623 (4)C16—H160.9500
Li1—P12.650 (4)C17—C181.388 (3)
C1—C61.389 (3)C17—H170.9500
C1—C21.395 (3)C18—H180.9500
C1—P11.849 (2)C19—C241.396 (3)
C2—C31.401 (3)C19—C201.398 (3)
C2—H20.9500C19—P21.835 (2)
C3—C41.376 (4)C20—C211.394 (3)
C3—H30.9500C20—H200.9500
C4—C51.380 (4)C21—C221.380 (3)
C4—H40.9500C21—H210.9500
C5—C61.395 (3)C22—C231.385 (3)
C5—H50.9500C22—H220.9500
C6—H60.9500C23—C241.396 (3)
C7—C121.397 (3)C23—H230.9500
C7—C81.398 (3)C24—H240.9500
C7—P11.845 (2)C25—O11.431 (3)
C8—C91.397 (3)C25—C261.506 (4)
C8—H80.9500C25—H25A0.9900
C9—C101.386 (4)C25—H25B0.9900
C9—H90.9500C26—C271.516 (4)
C10—C111.388 (4)C26—H26A0.9900
C10—H100.9500C26—H26B0.9900
C11—C121.397 (3)C27—C281.514 (4)
C11—H110.9500C27—H27A0.9900
C12—H120.9500C27—H27B0.9900
C13—C141.383 (3)C28—O11.437 (3)
C13—C181.402 (3)C28—H28A0.9900
C13—P21.846 (2)C28—H28B0.9900
C14—C151.403 (3)P1—P32.1751 (10)
C14—H140.9500P2—P32.1745 (10)
C15—C161.373 (4)P3—Li1ii2.569 (4)
O1—Li1—P3i124.24 (18)C24—C19—C20118.31 (19)
O1—Li1—P2111.77 (17)C24—C19—P2121.79 (15)
P3i—Li1—P2115.14 (14)C20—C19—P2119.90 (16)
O1—Li1—P1107.66 (16)C21—C20—C19120.8 (2)
P3i—Li1—P1113.30 (14)C21—C20—H20119.6
P2—Li1—P173.14 (11)C19—C20—H20119.6
C6—C1—C2118.0 (2)C22—C21—C20120.2 (2)
C6—C1—P1123.31 (16)C22—C21—H21119.9
C2—C1—P1118.65 (17)C20—C21—H21119.9
C1—C2—C3120.6 (2)C21—C22—C23119.7 (2)
C1—C2—H2119.7C21—C22—H22120.2
C3—C2—H2119.7C23—C22—H22120.2
C4—C3—C2120.4 (2)C22—C23—C24120.4 (2)
C4—C3—H3119.8C22—C23—H23119.8
C2—C3—H3119.8C24—C23—H23119.8
C3—C4—C5119.6 (2)C23—C24—C19120.5 (2)
C3—C4—H4120.2C23—C24—H24119.8
C5—C4—H4120.2C19—C24—H24119.8
C4—C5—C6120.2 (2)O1—C25—C26106.0 (2)
C4—C5—H5119.9O1—C25—H25A110.5
C6—C5—H5119.9C26—C25—H25A110.5
C1—C6—C5121.1 (2)O1—C25—H25B110.5
C1—C6—H6119.4C26—C25—H25B110.5
C5—C6—H6119.4H25A—C25—H25B108.7
C12—C7—C8118.48 (19)C25—C26—C27104.7 (2)
C12—C7—P1116.88 (16)C25—C26—H26A110.8
C8—C7—P1124.51 (16)C27—C26—H26A110.8
C9—C8—C7120.4 (2)C25—C26—H26B110.8
C9—C8—H8119.8C27—C26—H26B110.8
C7—C8—H8119.8H26A—C26—H26B108.9
C10—C9—C8120.7 (2)C28—C27—C26105.4 (2)
C10—C9—H9119.7C28—C27—H27A110.7
C8—C9—H9119.7C26—C27—H27A110.7
C9—C10—C11119.4 (2)C28—C27—H27B110.7
C9—C10—H10120.3C26—C27—H27B110.7
C11—C10—H10120.3H27A—C27—H27B108.8
C10—C11—C12120.1 (2)O1—C28—C27106.2 (2)
C10—C11—H11119.9O1—C28—H28A110.5
C12—C11—H11119.9C27—C28—H28A110.5
C7—C12—C11120.9 (2)O1—C28—H28B110.5
C7—C12—H12119.6C27—C28—H28B110.5
C11—C12—H12119.6H28A—C28—H28B108.7
C14—C13—C18118.5 (2)C25—O1—C28106.90 (18)
C14—C13—P2123.24 (16)C25—O1—Li1123.15 (18)
C18—C13—P2118.20 (16)C28—O1—Li1128.27 (19)
C13—C14—C15120.5 (2)C7—P1—C1100.95 (9)
C13—C14—H14119.8C7—P1—P3105.84 (7)
C15—C14—H14119.8C1—P1—P3107.34 (7)
C16—C15—C14120.6 (2)C7—P1—Li1120.85 (10)
C16—C15—H15119.7C1—P1—Li1123.90 (10)
C14—C15—H15119.7P3—P1—Li196.02 (9)
C15—C16—C17119.6 (2)C19—P2—C1398.11 (9)
C15—C16—H16120.2C19—P2—P3105.60 (7)
C17—C16—H16120.2C13—P2—P3107.98 (7)
C18—C17—C16120.1 (2)C19—P2—Li1124.94 (10)
C18—C17—H17119.9C13—P2—Li1121.78 (10)
C16—C17—H17119.9P3—P2—Li196.82 (9)
C17—C18—C13120.8 (2)P2—P3—P192.51 (4)
C17—C18—H18119.6P2—P3—Li1ii115.28 (9)
C13—C18—H18119.6P1—P3—Li1ii111.98 (9)
Symmetry codes: (i) x+1/2, y+1/2, z+1/2; (ii) x+1/2, y1/2, z+1/2.
 

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