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
CCDC reference: 274334
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (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
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 = 480.35 | Dx = 1.262 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 11491 reflections |
a = 11.332 (5) Å | θ = 2–25° |
b = 9.519 (5) Å | µ = 0.25 mm−1 |
c = 23.514 (8) Å | T = 120 K |
β = 94.735 (3)° | Plate, orange |
V = 2527.8 (19) Å3 | 0.31 × 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 tube | Rint = 0.044 |
Graphite monochromator | θmax = 30.0°, θmin = 2.8° |
ω (0.74°, 612 frames) scans | h = −15→15 |
22768 measured reflections | k = −9→13 |
7335 independent reflections | l = −32→33 |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.139 | H-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 parameters | Δρmax = 0.54 e Å−3 |
0 restraints | Δρmin = −0.29 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Li1 | 0.3550 (3) | 1.1896 (4) | 0.25179 (16) | 0.0248 (7) | |
C1 | 0.48652 (17) | 0.9153 (2) | 0.14545 (8) | 0.0199 (4) | |
C2 | 0.5376 (2) | 1.0175 (3) | 0.11275 (10) | 0.0307 (5) | |
H2 | 0.5083 | 1.1110 | 0.1126 | 0.037* | |
C3 | 0.6316 (2) | 0.9835 (3) | 0.08017 (11) | 0.0377 (6) | |
H3 | 0.6645 | 1.0536 | 0.0575 | 0.045* | |
C4 | 0.6766 (2) | 0.8492 (3) | 0.08084 (10) | 0.0358 (6) | |
H4 | 0.7412 | 0.8269 | 0.0592 | 0.043* | |
C5 | 0.6272 (2) | 0.7471 (3) | 0.11315 (11) | 0.0323 (5) | |
H5 | 0.6572 | 0.6540 | 0.1133 | 0.039* | |
C6 | 0.53338 (19) | 0.7804 (2) | 0.14556 (9) | 0.0250 (4) | |
H6 | 0.5010 | 0.7096 | 0.1681 | 0.030* | |
C7 | 0.23450 (17) | 0.9254 (2) | 0.13237 (8) | 0.0189 (4) | |
C8 | 0.24695 (19) | 0.8798 (2) | 0.07667 (9) | 0.0242 (4) | |
H8 | 0.3237 | 0.8630 | 0.0646 | 0.029* | |
C9 | 0.1472 (2) | 0.8587 (2) | 0.03865 (10) | 0.0292 (5) | |
H9 | 0.1567 | 0.8271 | 0.0010 | 0.035* | |
C10 | 0.0345 (2) | 0.8833 (3) | 0.05530 (10) | 0.0322 (5) | |
H10 | −0.0330 | 0.8676 | 0.0294 | 0.039* | |
C11 | 0.0213 (2) | 0.9312 (3) | 0.11018 (11) | 0.0320 (5) | |
H11 | −0.0556 | 0.9499 | 0.1217 | 0.038* | |
C12 | 0.12069 (19) | 0.9518 (2) | 0.14849 (9) | 0.0258 (4) | |
H12 | 0.1108 | 0.9842 | 0.1860 | 0.031* | |
C13 | 0.51649 (17) | 0.9296 (2) | 0.36183 (8) | 0.0201 (4) | |
C14 | 0.5983 (2) | 0.8340 (3) | 0.34456 (10) | 0.0298 (5) | |
H14 | 0.5812 | 0.7820 | 0.3104 | 0.036* | |
C15 | 0.7062 (2) | 0.8133 (3) | 0.37716 (12) | 0.0393 (6) | |
H15 | 0.7616 | 0.7472 | 0.3649 | 0.047* | |
C16 | 0.7325 (2) | 0.8877 (3) | 0.42662 (11) | 0.0376 (6) | |
H16 | 0.8060 | 0.8737 | 0.4484 | 0.045* | |
C17 | 0.6510 (2) | 0.9836 (3) | 0.44463 (11) | 0.0362 (6) | |
H17 | 0.6683 | 1.0344 | 0.4791 | 0.043* | |
C18 | 0.5444 (2) | 1.0052 (2) | 0.41235 (10) | 0.0299 (5) | |
H18 | 0.4897 | 1.0721 | 0.4246 | 0.036* | |
C19 | 0.27435 (17) | 0.9258 (2) | 0.37352 (8) | 0.0183 (4) | |
C20 | 0.19522 (19) | 1.0267 (2) | 0.39091 (9) | 0.0231 (4) | |
H20 | 0.1962 | 1.1188 | 0.3754 | 0.028* | |
C21 | 0.1150 (2) | 0.9939 (3) | 0.43076 (9) | 0.0281 (5) | |
H21 | 0.0610 | 1.0632 | 0.4418 | 0.034* | |
C22 | 0.1136 (2) | 0.8611 (3) | 0.45426 (9) | 0.0281 (5) | |
H22 | 0.0588 | 0.8389 | 0.4814 | 0.034* | |
C23 | 0.1924 (2) | 0.7604 (2) | 0.43805 (9) | 0.0283 (5) | |
H23 | 0.1917 | 0.6689 | 0.4542 | 0.034* | |
C24 | 0.27295 (19) | 0.7923 (2) | 0.39812 (9) | 0.0240 (4) | |
H24 | 0.3272 | 0.7228 | 0.3876 | 0.029* | |
C25 | 0.5175 (2) | 1.4012 (3) | 0.21059 (11) | 0.0331 (5) | |
H25A | 0.4475 | 1.4638 | 0.2088 | 0.040* | |
H25B | 0.5286 | 1.3670 | 0.1716 | 0.040* | |
C26 | 0.6262 (2) | 1.4782 (3) | 0.23503 (14) | 0.0443 (7) | |
H26A | 0.6043 | 1.5581 | 0.2590 | 0.053* | |
H26B | 0.6725 | 1.5142 | 0.2042 | 0.053* | |
C27 | 0.6964 (2) | 1.3694 (3) | 0.27064 (11) | 0.0409 (6) | |
H27A | 0.7720 | 1.3484 | 0.2541 | 0.049* | |
H27B | 0.7140 | 1.4032 | 0.3102 | 0.049* | |
C28 | 0.6184 (2) | 1.2402 (3) | 0.26945 (14) | 0.0448 (7) | |
H28A | 0.6482 | 1.1676 | 0.2441 | 0.054* | |
H28B | 0.6168 | 1.2003 | 0.3083 | 0.054* | |
O1 | 0.50203 (13) | 1.28570 (16) | 0.24824 (7) | 0.0264 (3) | |
P1 | 0.35909 (4) | 0.96479 (5) | 0.18548 (2) | 0.01665 (11) | |
P2 | 0.37625 (4) | 0.97047 (5) | 0.31951 (2) | 0.01696 (11) | |
P3 | 0.34791 (5) | 0.81145 (5) | 0.25340 (2) | 0.01821 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Li1 | 0.0206 (16) | 0.0259 (18) | 0.0281 (19) | 0.0023 (14) | 0.0032 (14) | −0.0008 (15) |
C1 | 0.0190 (9) | 0.0242 (9) | 0.0164 (9) | −0.0046 (7) | 0.0001 (7) | −0.0039 (7) |
C2 | 0.0319 (12) | 0.0304 (11) | 0.0304 (11) | −0.0045 (9) | 0.0074 (9) | 0.0039 (9) |
C3 | 0.0340 (13) | 0.0528 (16) | 0.0282 (12) | −0.0138 (11) | 0.0125 (10) | 0.0019 (11) |
C4 | 0.0226 (11) | 0.0595 (17) | 0.0260 (11) | −0.0083 (10) | 0.0065 (8) | −0.0150 (11) |
C5 | 0.0240 (11) | 0.0370 (12) | 0.0362 (13) | 0.0000 (9) | 0.0043 (9) | −0.0141 (10) |
C6 | 0.0222 (10) | 0.0260 (10) | 0.0273 (10) | −0.0032 (8) | 0.0053 (8) | −0.0037 (8) |
C7 | 0.0213 (9) | 0.0155 (8) | 0.0195 (9) | −0.0021 (7) | −0.0001 (7) | 0.0023 (7) |
C8 | 0.0248 (10) | 0.0262 (10) | 0.0214 (10) | 0.0009 (8) | 0.0003 (8) | 0.0001 (8) |
C9 | 0.0345 (12) | 0.0312 (11) | 0.0208 (10) | −0.0037 (9) | −0.0050 (8) | −0.0014 (9) |
C10 | 0.0282 (11) | 0.0365 (12) | 0.0300 (12) | −0.0081 (9) | −0.0101 (9) | 0.0086 (10) |
C11 | 0.0203 (10) | 0.0433 (14) | 0.0320 (12) | −0.0040 (9) | 0.0001 (8) | 0.0061 (10) |
C12 | 0.0237 (10) | 0.0315 (11) | 0.0225 (10) | −0.0021 (8) | 0.0030 (8) | 0.0023 (8) |
C13 | 0.0186 (9) | 0.0211 (9) | 0.0201 (9) | −0.0031 (7) | −0.0009 (7) | 0.0039 (7) |
C14 | 0.0258 (11) | 0.0393 (13) | 0.0241 (10) | 0.0046 (9) | 0.0016 (8) | −0.0005 (9) |
C15 | 0.0251 (11) | 0.0541 (16) | 0.0386 (14) | 0.0102 (11) | 0.0013 (10) | 0.0068 (12) |
C16 | 0.0240 (11) | 0.0528 (16) | 0.0345 (13) | −0.0045 (10) | −0.0079 (9) | 0.0151 (12) |
C17 | 0.0366 (13) | 0.0403 (13) | 0.0293 (12) | −0.0115 (11) | −0.0108 (10) | 0.0019 (10) |
C18 | 0.0297 (11) | 0.0292 (11) | 0.0295 (11) | −0.0022 (9) | −0.0060 (9) | −0.0048 (9) |
C19 | 0.0205 (9) | 0.0194 (9) | 0.0147 (8) | 0.0006 (7) | −0.0008 (6) | −0.0025 (7) |
C20 | 0.0269 (10) | 0.0232 (9) | 0.0189 (9) | 0.0064 (8) | 0.0005 (7) | −0.0016 (8) |
C21 | 0.0274 (11) | 0.0370 (12) | 0.0202 (10) | 0.0115 (9) | 0.0039 (8) | −0.0037 (9) |
C22 | 0.0262 (10) | 0.0416 (13) | 0.0170 (9) | −0.0012 (9) | 0.0050 (8) | −0.0023 (9) |
C23 | 0.0368 (12) | 0.0269 (11) | 0.0220 (10) | −0.0037 (9) | 0.0067 (9) | 0.0000 (8) |
C24 | 0.0285 (10) | 0.0210 (9) | 0.0232 (10) | 0.0017 (8) | 0.0072 (8) | −0.0012 (8) |
C25 | 0.0303 (12) | 0.0358 (12) | 0.0324 (12) | −0.0040 (10) | −0.0016 (9) | 0.0105 (10) |
C26 | 0.0352 (14) | 0.0353 (14) | 0.0612 (18) | −0.0094 (11) | −0.0026 (12) | 0.0043 (13) |
C27 | 0.0220 (11) | 0.0674 (19) | 0.0326 (13) | −0.0035 (11) | −0.0023 (9) | 0.0086 (12) |
C28 | 0.0286 (13) | 0.0414 (15) | 0.0625 (19) | 0.0076 (11) | −0.0073 (12) | 0.0152 (13) |
O1 | 0.0201 (7) | 0.0253 (7) | 0.0333 (8) | 0.0003 (6) | −0.0007 (6) | 0.0047 (6) |
P1 | 0.0180 (2) | 0.0166 (2) | 0.0154 (2) | −0.00157 (17) | 0.00164 (16) | −0.00037 (17) |
P2 | 0.0184 (2) | 0.0167 (2) | 0.0156 (2) | 0.00007 (17) | −0.00003 (16) | 0.00023 (17) |
P3 | 0.0221 (2) | 0.0174 (2) | 0.0151 (2) | −0.00195 (18) | 0.00120 (17) | 0.00009 (18) |
Geometric parameters (Å, º) top
Li1—O1 | 1.909 (4) | C15—H15 | 0.9500 |
Li1—P3i | 2.569 (4) | C16—C17 | 1.389 (4) |
Li1—P2 | 2.623 (4) | C16—H16 | 0.9500 |
Li1—P1 | 2.650 (4) | C17—C18 | 1.388 (3) |
C1—C6 | 1.389 (3) | C17—H17 | 0.9500 |
C1—C2 | 1.395 (3) | C18—H18 | 0.9500 |
C1—P1 | 1.849 (2) | C19—C24 | 1.396 (3) |
C2—C3 | 1.401 (3) | C19—C20 | 1.398 (3) |
C2—H2 | 0.9500 | C19—P2 | 1.835 (2) |
C3—C4 | 1.376 (4) | C20—C21 | 1.394 (3) |
C3—H3 | 0.9500 | C20—H20 | 0.9500 |
C4—C5 | 1.380 (4) | C21—C22 | 1.380 (3) |
C4—H4 | 0.9500 | C21—H21 | 0.9500 |
C5—C6 | 1.395 (3) | C22—C23 | 1.385 (3) |
C5—H5 | 0.9500 | C22—H22 | 0.9500 |
C6—H6 | 0.9500 | C23—C24 | 1.396 (3) |
C7—C12 | 1.397 (3) | C23—H23 | 0.9500 |
C7—C8 | 1.398 (3) | C24—H24 | 0.9500 |
C7—P1 | 1.845 (2) | C25—O1 | 1.431 (3) |
C8—C9 | 1.397 (3) | C25—C26 | 1.506 (4) |
C8—H8 | 0.9500 | C25—H25A | 0.9900 |
C9—C10 | 1.386 (4) | C25—H25B | 0.9900 |
C9—H9 | 0.9500 | C26—C27 | 1.516 (4) |
C10—C11 | 1.388 (4) | C26—H26A | 0.9900 |
C10—H10 | 0.9500 | C26—H26B | 0.9900 |
C11—C12 | 1.397 (3) | C27—C28 | 1.514 (4) |
C11—H11 | 0.9500 | C27—H27A | 0.9900 |
C12—H12 | 0.9500 | C27—H27B | 0.9900 |
C13—C14 | 1.383 (3) | C28—O1 | 1.437 (3) |
C13—C18 | 1.402 (3) | C28—H28A | 0.9900 |
C13—P2 | 1.846 (2) | C28—H28B | 0.9900 |
C14—C15 | 1.403 (3) | P1—P3 | 2.1751 (10) |
C14—H14 | 0.9500 | P2—P3 | 2.1745 (10) |
C15—C16 | 1.373 (4) | P3—Li1ii | 2.569 (4) |
| | | |
O1—Li1—P3i | 124.24 (18) | C24—C19—C20 | 118.31 (19) |
O1—Li1—P2 | 111.77 (17) | C24—C19—P2 | 121.79 (15) |
P3i—Li1—P2 | 115.14 (14) | C20—C19—P2 | 119.90 (16) |
O1—Li1—P1 | 107.66 (16) | C21—C20—C19 | 120.8 (2) |
P3i—Li1—P1 | 113.30 (14) | C21—C20—H20 | 119.6 |
P2—Li1—P1 | 73.14 (11) | C19—C20—H20 | 119.6 |
C6—C1—C2 | 118.0 (2) | C22—C21—C20 | 120.2 (2) |
C6—C1—P1 | 123.31 (16) | C22—C21—H21 | 119.9 |
C2—C1—P1 | 118.65 (17) | C20—C21—H21 | 119.9 |
C1—C2—C3 | 120.6 (2) | C21—C22—C23 | 119.7 (2) |
C1—C2—H2 | 119.7 | C21—C22—H22 | 120.2 |
C3—C2—H2 | 119.7 | C23—C22—H22 | 120.2 |
C4—C3—C2 | 120.4 (2) | C22—C23—C24 | 120.4 (2) |
C4—C3—H3 | 119.8 | C22—C23—H23 | 119.8 |
C2—C3—H3 | 119.8 | C24—C23—H23 | 119.8 |
C3—C4—C5 | 119.6 (2) | C23—C24—C19 | 120.5 (2) |
C3—C4—H4 | 120.2 | C23—C24—H24 | 119.8 |
C5—C4—H4 | 120.2 | C19—C24—H24 | 119.8 |
C4—C5—C6 | 120.2 (2) | O1—C25—C26 | 106.0 (2) |
C4—C5—H5 | 119.9 | O1—C25—H25A | 110.5 |
C6—C5—H5 | 119.9 | C26—C25—H25A | 110.5 |
C1—C6—C5 | 121.1 (2) | O1—C25—H25B | 110.5 |
C1—C6—H6 | 119.4 | C26—C25—H25B | 110.5 |
C5—C6—H6 | 119.4 | H25A—C25—H25B | 108.7 |
C12—C7—C8 | 118.48 (19) | C25—C26—C27 | 104.7 (2) |
C12—C7—P1 | 116.88 (16) | C25—C26—H26A | 110.8 |
C8—C7—P1 | 124.51 (16) | C27—C26—H26A | 110.8 |
C9—C8—C7 | 120.4 (2) | C25—C26—H26B | 110.8 |
C9—C8—H8 | 119.8 | C27—C26—H26B | 110.8 |
C7—C8—H8 | 119.8 | H26A—C26—H26B | 108.9 |
C10—C9—C8 | 120.7 (2) | C28—C27—C26 | 105.4 (2) |
C10—C9—H9 | 119.7 | C28—C27—H27A | 110.7 |
C8—C9—H9 | 119.7 | C26—C27—H27A | 110.7 |
C9—C10—C11 | 119.4 (2) | C28—C27—H27B | 110.7 |
C9—C10—H10 | 120.3 | C26—C27—H27B | 110.7 |
C11—C10—H10 | 120.3 | H27A—C27—H27B | 108.8 |
C10—C11—C12 | 120.1 (2) | O1—C28—C27 | 106.2 (2) |
C10—C11—H11 | 119.9 | O1—C28—H28A | 110.5 |
C12—C11—H11 | 119.9 | C27—C28—H28A | 110.5 |
C7—C12—C11 | 120.9 (2) | O1—C28—H28B | 110.5 |
C7—C12—H12 | 119.6 | C27—C28—H28B | 110.5 |
C11—C12—H12 | 119.6 | H28A—C28—H28B | 108.7 |
C14—C13—C18 | 118.5 (2) | C25—O1—C28 | 106.90 (18) |
C14—C13—P2 | 123.24 (16) | C25—O1—Li1 | 123.15 (18) |
C18—C13—P2 | 118.20 (16) | C28—O1—Li1 | 128.27 (19) |
C13—C14—C15 | 120.5 (2) | C7—P1—C1 | 100.95 (9) |
C13—C14—H14 | 119.8 | C7—P1—P3 | 105.84 (7) |
C15—C14—H14 | 119.8 | C1—P1—P3 | 107.34 (7) |
C16—C15—C14 | 120.6 (2) | C7—P1—Li1 | 120.85 (10) |
C16—C15—H15 | 119.7 | C1—P1—Li1 | 123.90 (10) |
C14—C15—H15 | 119.7 | P3—P1—Li1 | 96.02 (9) |
C15—C16—C17 | 119.6 (2) | C19—P2—C13 | 98.11 (9) |
C15—C16—H16 | 120.2 | C19—P2—P3 | 105.60 (7) |
C17—C16—H16 | 120.2 | C13—P2—P3 | 107.98 (7) |
C18—C17—C16 | 120.1 (2) | C19—P2—Li1 | 124.94 (10) |
C18—C17—H17 | 119.9 | C13—P2—Li1 | 121.78 (10) |
C16—C17—H17 | 119.9 | P3—P2—Li1 | 96.82 (9) |
C17—C18—C13 | 120.8 (2) | P2—P3—P1 | 92.51 (4) |
C17—C18—H18 | 119.6 | P2—P3—Li1ii | 115.28 (9) |
C13—C18—H18 | 119.6 | P1—P3—Li1ii | 111.98 (9) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+1/2, y−1/2, −z+1/2. |