catena-Poly­[[(tetra­hydro­furan-κO)­lithium(I)]-μ-1,1,3,3-tetra­phenyl­triphosphane-κ²P¹,P³:κP²]

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.

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

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Computing details

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]

Crystal data

[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) Å^3	0.31 × 0.27 × 0.10 mm
Z = 4

Data collection

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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.064	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.139	H-atom parameters constrained
S = 1.14	w = 1/[σ^2(Fo^2) + (0.0491P)^2 + 2.4715P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Li1—O1	1.909 (4)	C15—H15	0.9500
Li1—P3^i	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—Li1^ii	2.569 (4)
O1—Li1—P3^i	124.24 (18)	C24—C19—C20	118.31 (19)
O1—Li1—P2	111.77 (17)	C24—C19—P2	121.79 (15)
P3^i—Li1—P2	115.14 (14)	C20—C19—P2	119.90 (16)
O1—Li1—P1	107.66 (16)	C21—C20—C19	120.8 (2)
P3^i—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—Li1^ii	115.28 (9)
C13—C18—H18	119.6	P1—P3—Li1^ii	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.