Acta Crystallographica Section E Structure Reports
Online
ISSN 1600-5368
Lithium tetrakis(diphenylphosphino)borate
diethyl ether solvate
Franz Dornhaus and Michael Bolte*
Institut fu¨r Anorganische Chemie, J. W. Goethe-Universita¨t Frankfurt, Max-von-Laue-Strasse 7, 60438 Frankfurt/Main, Germany
Correspondence e-mail: [email protected]
Key indicators
Single-crystal X-ray study
T= 173 K
Mean(C–C) = 0.003 A˚
Rfactor = 0.038
wRfactor = 0.097
Data-to-parameter ratio = 16.5
For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.
Received 21 November 2006 Accepted 27 November 2006 In the title compound, Li+C48H40BP4 C4H10O, the Li
+
cation is coordinated by two P atoms, two aromatic C atoms and the ether O atom.
Comment
In contrast to the well established tetraalkyl- and tetraaryl-borates, there are only two examples of tetraphosphinoborate anions, namely the parent compound B(PH2)4 (Baudler &
Block, 1988, 1989) and the ethyl derivative B(PEt2)4 (Fritz &
Pfannerer, 1970; Fritz & Sattler, 1975). To our knowledge, none of them has been structurally characterized. We report here the synthesis and structure of the title compound, (I) (Fig. 1), which is a lithium salt and diethylether solvate of the phenyl derivative, B(PPh2)4 . The compound is stable at room
temperature but the solution decomposes immediately upon contact with stainless steel canulas or catalytic amounts of zirconium oxide with formation of a colourless precipitate. The decomposition products were not identified.
The bond lengths and angles in (I) can be regarded as normal (Cambridge Structural Database; Version 5.27, November 2005 updated August 2006; Mogul Version 1.1; Allen, 2002). Compound (I) contains tetrakis(diphenyl-phosphino)borate anions, Li cations and diethyl ether solvent molecules. The Li cation is coordinated by two P atoms, two aromatic C atoms and the ether O atom (Table 1). The B—P distances of the Li-coordinating P atoms are longer than the other two B—P distances.
Experimental
Reactions and manipulations were carried out under an atmosphere of dry nitrogen using standard Schlenk techniques. Solvents were freshly distilled under argon from sodium/benzophenone (diethyl ether, C6D6) or sodium–lead alloy (pentane) prior to use. A solution
pitate was filtered off. All volatiles were removed from the pale-yellow filtratein vacuo. The yellow residue was washed with pentane (25 ml) and redissolved in a minimum amount of diethyl ether. X-ray quality crystals of (I) separated upon cooling to 278 K. Yield 176 mg (38%).
Crystal data
Li+C48H40BP4 C4H10O Mr= 832.55
Monoclinic,P21 a= 11.7386 (7) A˚ b= 13.2135 (11) A˚ c= 14.4602 (9) A˚ = 91.216 (5)
V= 2242.4 (3) A˚3
Z= 2
Dx= 1.233 Mg m 3 MoKradiation = 0.21 mm 1 T= 173 (2) K Block, yellow 0.500.490.47 mm
Data collection
Stoe IPDS-II two-circle diffractometer !scans
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995)
Tmin= 0.904,Tmax= 0.909
16919 measured reflections 8770 independent reflections 8251 reflections withI> 2(I) Rint= 0.038
max= 27.7
Refinement
Refinement onF2 R[F2> 2(F2)] = 0.038 wR(F2) = 0.097 S= 1.05 8770 reflections 533 parameters
H-atom parameters constrained w= 1/[2(F
o2) + (0.0682P)2
+ 0.0442P]
whereP= (Fo2+ 2Fc2)/3
(/)max= 0.001 max= 0.28 e A˚ 3 min= 0.23 e A˚ 3
Extinction correction:SHELXL97 Extinction coefficient: 0.0061 (12) Absolute structure: Flack (1983),
3383 Friedel pairs Flack parameter: 0.04 (5)
Table 1
Selected bond lengths (A˚ ).
B1—P2 2.013 (2)
B1—P1 2.015 (2)
B1—P3 2.032 (2)
B1—P4 2.053 (2)
Li1—P3 2.599 (5)
Li1—P4 2.532 (4)
Li1—C31 2.543 (5)
Li1—C32 2.560 (5)
Li1—O1 1.881 (5)
The H atoms were positioned geometrically (C—H = 0.95–0.99 A˚ ) and refined as riding withUiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C).
Data collection: X-AREA (Stoe & Cie, 2001); cell refinement:
X-AREA; data reduction: X-AREA; program(s) used to solve structure:SHELXS97(Sheldrick, 1997); program(s) used to refine structure:SHELXL97(Sheldrick, 1997); molecular graphics:XPin
SHELXTL-Plus(Sheldrick, 1991); software used to prepare material for publication:SHELXL97.
References
Allen, F. H. (2002).Acta Cryst.B58, 380–388.
Baudler, M. & Block, C. (1988).Z. Anorg. Allg. Chem.567, 7–12. Baudler, M. & Block, C. (1989).Z. Anorg. Allg. Chem.569, 7–15. Blessing, R. H. (1995).Acta Cryst.A51, 33–38.
Flack, H. D. (1983).Acta Cryst.A39, 876–881.
Fritz, G. & Pfannerer, F. (1970).Z. Anorg. Allg. Chem.373, 30–35. Fritz, G. & Sattler, E. (1975).Z. Anorg. Allg. Chem.413, 193–228.
Sheldrick, G. M. (1991).SHELXTL-Plus. Release 4.1. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Go¨ttingen, Germany.
Spek, A. L. (2003).J. Appl. Cryst.36, 7–13.
[image:2.610.313.564.72.274.2]Stoe & Cie (2001).X-AREA. Stoe & Cie, Darmstadt, Germany.
Figure 1
supporting information
Acta Cryst. (2007). E63, m39–m40 [https://doi.org/10.1107/S1600536806051130]
Lithium tetrakis(diphenylphosphino)borate diethyl ether solvate
Franz Dornhaus and Michael Bolte
Lithium tetrakis(diphenylphosphino)borate diethyl ether solvate
Crystal data
Li+·C
48H40BP4−·C4H10O
Mr = 832.55 Monoclinic, P21
Hall symbol: P 2yb
a = 11.7386 (7) Å
b = 13.2135 (11) Å
c = 14.4602 (9) Å
β = 91.216 (5)°
V = 2242.4 (3) Å3
Z = 2
F(000) = 876
Dx = 1.233 Mg m−3
Mo Kα radiation, λ = 0.71073 Å Cell parameters from 22354 reflections
θ = 3.1–27.3°
µ = 0.21 mm−1
T = 173 K Block, yellow
0.50 × 0.49 × 0.47 mm
Data collection
Stoe IPDS-II two-circle diffractometer
Radiation source: fine-focus sealed tube Graphite monochromator
ω scans
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
Tmin = 0.904, Tmax = 0.909
16919 measured reflections 8770 independent reflections 8251 reflections with I > 2σ(I)
Rint = 0.038
θmax = 27.7°, θmin = 3.1°
h = −14→15
k = −17→15
l = −18→18
Refinement
Refinement on F2
Least-squares matrix: full
R[F2 > 2σ(F2)] = 0.038
wR(F2) = 0.097
S = 1.05 8770 reflections 533 parameters 1 restraint
Primary atom site location: structure-invariant direct methods
Secondary atom site location: difference Fourier map
Hydrogen site location: inferred from neighbouring sites
H-atom parameters constrained
w = 1/[σ2(F
o2) + (0.0682P)2 + 0.0442P]
where P = (Fo2 + 2Fc2)/3
(Δ/σ)max = 0.001
Δρmax = 0.28 e Å−3
Δρmin = −0.23 e Å−3
Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Extinction coefficient: 0.0061 (12)
Absolute structure: Flack (1983), 3383 Friedel pairs
Special details
Experimental. The NMR spectra were recorded on a Bruker AV 400 spectrometer. NMR measurement was performed in undeuterated diethyl ether solution. Approximately 0.1 ml of C6D6 was added to the sample to provide a lock signal. The 11B NMR spectrum was referenced against external BF
3.OEt2. Abbreviations: qi = quintet. 11B{1H} NMR (Et2O, 128.38
MHz): δ = -13.3 (qi, 1J
PB = 22.5 Hz) p.p.m..
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)
x y z Uiso*/Ueq
B1 0.71798 (18) 0.40289 (17) 0.75468 (13) 0.0180 (4)
P1 0.67919 (5) 0.26593 (4) 0.70151 (3) 0.01957 (11)
P2 0.81746 (4) 0.40271 (4) 0.86984 (3) 0.02002 (11)
P3 0.59887 (5) 0.51452 (4) 0.75322 (3) 0.02022 (11)
P4 0.82487 (5) 0.48489 (4) 0.67279 (3) 0.02072 (11)
C11 0.79815 (19) 0.17820 (15) 0.72808 (14) 0.0227 (4)
C12 0.8405 (2) 0.15454 (17) 0.81677 (14) 0.0282 (5)
H12 0.8019 0.1787 0.8695 0.034*
C13 0.9382 (2) 0.09619 (19) 0.82852 (17) 0.0371 (5)
H13 0.9657 0.0809 0.8892 0.045*
C14 0.9961 (2) 0.0599 (2) 0.7524 (2) 0.0399 (6)
H14 1.0641 0.0218 0.7611 0.048*
C15 0.9545 (2) 0.07954 (18) 0.66447 (18) 0.0349 (5)
H15 0.9928 0.0538 0.6123 0.042*
C16 0.8557 (2) 0.13733 (17) 0.65232 (15) 0.0278 (4)
H16 0.8268 0.1494 0.5915 0.033*
C21 0.55944 (19) 0.20858 (15) 0.76311 (13) 0.0208 (4)
C22 0.45621 (19) 0.26258 (18) 0.76551 (13) 0.0255 (4)
H22 0.4522 0.3282 0.7389 0.031*
C23 0.3598 (2) 0.22203 (19) 0.80602 (15) 0.0300 (5)
H23 0.2924 0.2615 0.8096 0.036*
C24 0.3617 (2) 0.12410 (18) 0.84130 (15) 0.0302 (5)
H24 0.2957 0.0958 0.8681 0.036*
C25 0.4617 (2) 0.06859 (18) 0.83665 (15) 0.0317 (5)
H25 0.4636 0.0012 0.8594 0.038*
C26 0.5596 (2) 0.11023 (17) 0.79905 (15) 0.0275 (4)
H26 0.6275 0.0712 0.7978 0.033*
C31 0.85221 (18) 0.53581 (16) 0.90069 (13) 0.0227 (4)
C32 0.7774 (2) 0.60524 (17) 0.94080 (14) 0.0273 (4)
H32 0.6999 0.5870 0.9487 0.033*
C33 0.8154 (3) 0.70120 (19) 0.96934 (16) 0.0370 (6)
C34 0.9282 (3) 0.7290 (2) 0.95826 (18) 0.0441 (7)
H34 0.9541 0.7935 0.9787 0.053*
C35 1.0031 (2) 0.6622 (2) 0.91719 (18) 0.0412 (6)
H35 1.0801 0.6814 0.9082 0.049*
C36 0.9650 (2) 0.5667 (2) 0.88919 (16) 0.0320 (5)
H36 1.0171 0.5215 0.8615 0.038*
C41 0.74612 (19) 0.36203 (15) 0.97580 (13) 0.0223 (4)
C42 0.6545 (2) 0.29499 (18) 0.97678 (15) 0.0328 (5)
H42 0.6172 0.2771 0.9202 0.039*
C43 0.6166 (3) 0.2535 (2) 1.06010 (17) 0.0414 (6)
H43 0.5541 0.2078 1.0595 0.050*
C44 0.6701 (3) 0.27912 (19) 1.14292 (15) 0.0398 (6)
H44 0.6448 0.2509 1.1993 0.048*
C45 0.7604 (2) 0.3459 (2) 1.14311 (14) 0.0345 (5)
H45 0.7965 0.3643 1.2001 0.041*
C46 0.7993 (2) 0.38676 (17) 1.06081 (13) 0.0271 (4)
H46 0.8623 0.4318 1.0622 0.033*
C51 0.47021 (18) 0.49705 (16) 0.82368 (13) 0.0238 (4)
C52 0.3609 (2) 0.50769 (19) 0.78484 (15) 0.0301 (5)
H52 0.3526 0.5216 0.7206 0.036*
C53 0.2638 (2) 0.4984 (2) 0.83790 (17) 0.0374 (6)
H53 0.1905 0.5060 0.8096 0.045*
C54 0.2734 (2) 0.4783 (2) 0.93123 (17) 0.0401 (6)
H54 0.2073 0.4712 0.9675 0.048*
C55 0.3803 (2) 0.4686 (2) 0.97106 (16) 0.0389 (6)
H55 0.3875 0.4549 1.0354 0.047*
C56 0.4787 (2) 0.4785 (2) 0.91863 (15) 0.0318 (5)
H56 0.5517 0.4726 0.9479 0.038*
C61 0.53104 (18) 0.52610 (17) 0.63757 (13) 0.0240 (4)
C62 0.4934 (2) 0.62226 (19) 0.60950 (16) 0.0336 (5)
H62 0.5053 0.6783 0.6498 0.040*
C63 0.4393 (2) 0.6377 (2) 0.52449 (18) 0.0393 (6)
H63 0.4141 0.7034 0.5070 0.047*
C64 0.4223 (2) 0.5564 (2) 0.46525 (16) 0.0371 (6)
H64 0.3858 0.5664 0.4067 0.045*
C65 0.4583 (2) 0.4607 (2) 0.49133 (15) 0.0320 (5)
H65 0.4467 0.4052 0.4504 0.038*
C66 0.51149 (19) 0.44515 (18) 0.57698 (14) 0.0261 (4)
H66 0.5348 0.3789 0.5945 0.031*
C71 0.78031 (18) 0.47701 (17) 0.55017 (13) 0.0234 (4)
C72 0.7439 (2) 0.56466 (19) 0.50429 (15) 0.0289 (5)
H72 0.7427 0.6273 0.5364 0.035*
C73 0.7092 (2) 0.5606 (2) 0.41138 (16) 0.0377 (6)
H73 0.6843 0.6204 0.3807 0.045*
C74 0.7108 (2) 0.4707 (2) 0.36440 (15) 0.0416 (6)
H74 0.6863 0.4684 0.3014 0.050*
C75 0.7483 (2) 0.3823 (2) 0.40842 (15) 0.0383 (6)
C76 0.7837 (2) 0.38614 (18) 0.50083 (14) 0.0289 (5)
H76 0.8104 0.3264 0.5307 0.035*
C81 0.97120 (19) 0.43626 (18) 0.66047 (13) 0.0251 (4)
C82 1.0130 (2) 0.34390 (18) 0.69276 (15) 0.0290 (5)
H82 0.9667 0.3018 0.7296 0.035*
C83 1.1233 (2) 0.3131 (2) 0.67090 (18) 0.0375 (5)
H83 1.1502 0.2490 0.6917 0.045*
C84 1.1935 (2) 0.3739 (2) 0.61991 (19) 0.0433 (7)
H84 1.2679 0.3518 0.6052 0.052*
C85 1.1547 (2) 0.4677 (3) 0.59023 (19) 0.0465 (7)
H85 1.2033 0.5108 0.5563 0.056*
C86 1.0450 (2) 0.4989 (2) 0.60991 (16) 0.0374 (6)
H86 1.0191 0.5632 0.5891 0.045*
Li1 0.7702 (4) 0.6387 (3) 0.7664 (3) 0.0349 (9)
C1 0.6386 (4) 0.8379 (3) 0.7698 (3) 0.0702 (11)
H1A 0.5966 0.9017 0.7749 0.105*
H1B 0.6426 0.8047 0.8304 0.105*
H1C 0.5993 0.7935 0.7252 0.105*
C2 0.7531 (4) 0.8584 (3) 0.7388 (5) 0.107 (2)
H2A 0.7488 0.8938 0.6785 0.129*
H2B 0.7924 0.9035 0.7838 0.129*
O1 0.81664 (18) 0.76846 (15) 0.72935 (14) 0.0453 (4)
C3 0.9336 (3) 0.7801 (3) 0.6986 (2) 0.0594 (8)
H3A 0.9698 0.8376 0.7318 0.071*
H3B 0.9774 0.7182 0.7141 0.071*
C4 0.9376 (4) 0.7981 (4) 0.5995 (3) 0.0820 (13)
H4A 1.0171 0.8052 0.5812 0.123*
H4B 0.8959 0.8603 0.5842 0.123*
H4C 0.9026 0.7409 0.5664 0.123*
Atomic displacement parameters (Å2)
U11 U22 U33 U12 U13 U23
B1 0.0182 (10) 0.0175 (9) 0.0185 (8) −0.0003 (9) 0.0011 (7) −0.0001 (7)
P1 0.0224 (3) 0.0169 (2) 0.0194 (2) −0.0001 (2) −0.00025 (17) −0.00132 (17)
P2 0.0221 (3) 0.0203 (2) 0.0176 (2) 0.0008 (2) 0.00002 (17) −0.00128 (17)
P3 0.0201 (3) 0.0181 (2) 0.0224 (2) 0.00179 (19) 0.00086 (17) −0.00032 (17)
P4 0.0214 (3) 0.0206 (2) 0.0203 (2) −0.0008 (2) 0.00266 (17) 0.00129 (17)
C11 0.0238 (11) 0.0164 (9) 0.0278 (9) −0.0009 (8) 0.0006 (8) −0.0021 (7)
C12 0.0357 (13) 0.0211 (10) 0.0278 (10) 0.0018 (9) −0.0029 (8) −0.0031 (8)
C13 0.0405 (15) 0.0291 (12) 0.0412 (12) 0.0075 (11) −0.0119 (10) 0.0002 (9)
C14 0.0289 (13) 0.0274 (12) 0.0633 (16) 0.0069 (10) −0.0038 (11) −0.0035 (11)
C15 0.0325 (13) 0.0277 (12) 0.0447 (13) 0.0025 (10) 0.0081 (10) −0.0074 (9)
C16 0.0280 (12) 0.0244 (10) 0.0309 (10) 0.0002 (9) 0.0024 (8) −0.0042 (8)
C21 0.0257 (11) 0.0190 (9) 0.0176 (8) −0.0014 (8) −0.0034 (7) −0.0035 (6)
C22 0.0260 (11) 0.0213 (9) 0.0290 (9) −0.0014 (9) −0.0012 (7) 0.0000 (8)
C23 0.0268 (12) 0.0305 (11) 0.0326 (11) −0.0008 (9) 0.0009 (8) −0.0037 (8)
C25 0.0382 (14) 0.0252 (11) 0.0317 (11) −0.0038 (10) 0.0008 (9) 0.0051 (8)
C26 0.0298 (12) 0.0206 (10) 0.0322 (10) 0.0002 (9) 0.0001 (8) 0.0015 (8)
C31 0.0248 (11) 0.0242 (10) 0.0190 (8) −0.0010 (8) 0.0006 (7) −0.0007 (7)
C32 0.0294 (12) 0.0250 (10) 0.0278 (10) −0.0026 (9) 0.0051 (8) −0.0028 (8)
C33 0.0504 (16) 0.0271 (12) 0.0338 (12) −0.0049 (11) 0.0078 (10) −0.0069 (9)
C34 0.0598 (19) 0.0322 (13) 0.0404 (13) −0.0191 (13) 0.0011 (12) −0.0045 (10)
C35 0.0356 (14) 0.0427 (15) 0.0455 (13) −0.0194 (12) 0.0026 (10) −0.0023 (11)
C36 0.0242 (12) 0.0376 (13) 0.0341 (11) −0.0065 (10) −0.0004 (8) −0.0016 (9)
C41 0.0295 (11) 0.0181 (9) 0.0193 (8) 0.0038 (8) 0.0021 (7) −0.0004 (7)
C42 0.0440 (14) 0.0306 (12) 0.0239 (10) −0.0101 (10) 0.0024 (9) −0.0046 (8)
C43 0.0597 (18) 0.0293 (13) 0.0358 (12) −0.0134 (12) 0.0129 (11) −0.0006 (9)
C44 0.0632 (18) 0.0309 (13) 0.0259 (10) 0.0045 (12) 0.0142 (10) 0.0060 (9)
C45 0.0484 (15) 0.0355 (13) 0.0195 (9) 0.0089 (11) 0.0004 (9) −0.0005 (8)
C46 0.0327 (12) 0.0272 (11) 0.0214 (9) 0.0049 (9) −0.0020 (7) −0.0011 (7)
C51 0.0239 (11) 0.0215 (10) 0.0261 (9) 0.0012 (8) 0.0022 (7) −0.0040 (7)
C52 0.0242 (11) 0.0374 (13) 0.0287 (10) 0.0063 (10) 0.0014 (8) 0.0001 (9)
C53 0.0220 (12) 0.0501 (16) 0.0402 (12) 0.0067 (11) 0.0040 (9) −0.0030 (11)
C54 0.0308 (14) 0.0525 (15) 0.0375 (12) −0.0035 (12) 0.0132 (10) −0.0033 (11)
C55 0.0352 (14) 0.0541 (16) 0.0275 (11) −0.0068 (12) 0.0051 (9) 0.0007 (10)
C56 0.0274 (12) 0.0395 (13) 0.0285 (10) −0.0032 (10) 0.0000 (8) 0.0018 (9)
C61 0.0206 (10) 0.0286 (11) 0.0230 (9) 0.0030 (8) 0.0020 (7) 0.0054 (7)
C62 0.0373 (14) 0.0295 (12) 0.0340 (11) 0.0086 (10) 0.0001 (9) 0.0065 (9)
C63 0.0368 (15) 0.0400 (14) 0.0411 (12) 0.0116 (11) 0.0020 (10) 0.0171 (10)
C64 0.0290 (13) 0.0549 (16) 0.0274 (10) 0.0070 (11) −0.0006 (8) 0.0138 (10)
C65 0.0289 (12) 0.0432 (14) 0.0237 (10) 0.0026 (10) −0.0010 (8) 0.0020 (8)
C66 0.0255 (12) 0.0285 (11) 0.0243 (9) 0.0020 (9) 0.0010 (8) 0.0041 (8)
C71 0.0203 (10) 0.0301 (11) 0.0199 (8) 0.0005 (8) 0.0035 (7) 0.0051 (7)
C72 0.0264 (12) 0.0317 (11) 0.0287 (10) 0.0000 (9) 0.0039 (8) 0.0094 (8)
C73 0.0331 (13) 0.0521 (15) 0.0280 (11) 0.0065 (12) 0.0023 (9) 0.0179 (10)
C74 0.0397 (15) 0.0652 (18) 0.0198 (10) 0.0122 (13) 0.0008 (9) 0.0062 (10)
C75 0.0397 (14) 0.0513 (16) 0.0239 (10) 0.0059 (12) 0.0038 (9) −0.0058 (9)
C76 0.0316 (12) 0.0330 (12) 0.0223 (9) 0.0071 (10) 0.0037 (8) 0.0009 (8)
C81 0.0200 (11) 0.0339 (11) 0.0214 (9) −0.0029 (9) 0.0002 (7) 0.0002 (8)
C82 0.0220 (11) 0.0305 (12) 0.0346 (10) −0.0045 (9) 0.0006 (8) −0.0027 (8)
C83 0.0256 (13) 0.0365 (13) 0.0504 (14) 0.0022 (10) −0.0009 (10) −0.0051 (11)
C84 0.0196 (12) 0.065 (2) 0.0454 (13) 0.0048 (12) 0.0032 (9) −0.0070 (12)
C85 0.0257 (13) 0.071 (2) 0.0429 (13) −0.0060 (13) 0.0082 (10) 0.0136 (13)
C86 0.0260 (12) 0.0468 (15) 0.0395 (11) −0.0048 (11) 0.0033 (9) 0.0119 (10)
Li1 0.044 (3) 0.0260 (19) 0.0351 (19) −0.0035 (18) 0.0035 (16) 0.0006 (15)
C1 0.066 (3) 0.0347 (16) 0.110 (3) 0.0058 (16) 0.008 (2) −0.0179 (17)
C2 0.076 (3) 0.0269 (17) 0.219 (6) 0.0063 (19) 0.027 (4) 0.020 (3)
O1 0.0521 (12) 0.0258 (8) 0.0583 (11) −0.0060 (9) 0.0055 (9) 0.0027 (8)
C3 0.053 (2) 0.053 (2) 0.072 (2) −0.0173 (16) 0.0005 (15) 0.0069 (15)
Geometric parameters (Å, º)
B1—P2 2.013 (2) C46—H46 0.9500
B1—P1 2.015 (2) C51—C56 1.396 (3)
B1—P3 2.032 (2) C51—C52 1.397 (3)
B1—P4 2.053 (2) C52—C53 1.393 (3)
Li1—P3 2.599 (5) C52—H52 0.9500
Li1—P4 2.532 (4) C53—C54 1.378 (4)
Li1—C31 2.543 (5) C53—H53 0.9500
Li1—C32 2.560 (5) C54—C55 1.376 (4)
Li1—O1 1.881 (5) C54—H54 0.9500
P1—C21 1.843 (2) C55—C56 1.402 (3)
P1—C11 1.849 (2) C55—H55 0.9500
P2—C41 1.842 (2) C56—H56 0.9500
P2—C31 1.858 (2) C61—C66 1.399 (3)
P3—C61 1.843 (2) C61—C62 1.402 (3)
P3—C51 1.854 (2) C62—C63 1.387 (3)
P4—C71 1.841 (2) C62—H62 0.9500
P4—C81 1.846 (2) C63—C64 1.386 (4)
C11—C12 1.401 (3) C63—H63 0.9500
C11—C16 1.407 (3) C64—C65 1.383 (4)
C12—C13 1.390 (3) C64—H64 0.9500
C12—H12 0.9500 C65—C66 1.390 (3)
C13—C14 1.391 (4) C65—H65 0.9500
C13—H13 0.9500 C66—H66 0.9500
C14—C15 1.378 (4) C71—C72 1.397 (3)
C14—H14 0.9500 C71—C76 1.398 (3)
C15—C16 1.396 (3) C72—C73 1.397 (3)
C15—H15 0.9500 C72—H72 0.9500
C16—H16 0.9500 C73—C74 1.369 (4)
C21—C26 1.400 (3) C73—H73 0.9500
C21—C22 1.407 (3) C74—C75 1.397 (4)
C22—C23 1.393 (3) C74—H74 0.9500
C22—H22 0.9500 C75—C76 1.392 (3)
C23—C24 1.391 (3) C75—H75 0.9500
C23—H23 0.9500 C76—H76 0.9500
C24—C25 1.388 (4) C81—C82 1.392 (3)
C24—H24 0.9500 C81—C86 1.413 (3)
C25—C26 1.394 (3) C82—C83 1.400 (3)
C25—H25 0.9500 C82—H82 0.9500
C26—H26 0.9500 C83—C84 1.376 (4)
C31—C36 1.398 (3) C83—H83 0.9500
C31—C32 1.404 (3) C84—C85 1.386 (5)
C32—C33 1.403 (3) C84—H84 0.9500
C32—H32 0.9500 C85—C86 1.387 (4)
C33—C34 1.386 (4) C85—H85 0.9500
C33—H33 0.9500 C86—H86 0.9500
C34—H34 0.9500 C1—H1A 0.9800
C35—C36 1.395 (4) C1—H1B 0.9800
C35—H35 0.9500 C1—H1C 0.9800
C36—H36 0.9500 C2—O1 1.411 (5)
C41—C42 1.393 (3) C2—H2A 0.9900
C41—C46 1.405 (3) C2—H2B 0.9900
C42—C43 1.405 (3) O1—C3 1.460 (4)
C42—H42 0.9500 C3—C4 1.453 (5)
C43—C44 1.382 (4) C3—H3A 0.9900
C43—H43 0.9500 C3—H3B 0.9900
C44—C45 1.380 (4) C4—H4A 0.9800
C44—H44 0.9500 C4—H4B 0.9800
C45—C46 1.392 (3) C4—H4C 0.9800
C45—H45 0.9500
P2—B1—P1 115.91 (11) C53—C52—H52 119.2
P2—B1—P3 113.35 (10) C51—C52—H52 119.2
P1—B1—P3 119.88 (11) C54—C53—C52 120.4 (2)
P2—B1—P4 97.29 (9) C54—C53—H53 119.8
P1—B1—P4 112.95 (9) C52—C53—H53 119.8
P3—B1—P4 92.27 (9) C55—C54—C53 118.9 (2)
C21—P1—C11 102.84 (9) C55—C54—H54 120.6
C21—P1—B1 110.69 (8) C53—C54—H54 120.6
C11—P1—B1 108.68 (9) C54—C55—C56 121.3 (2)
C41—P2—C31 100.25 (9) C54—C55—H55 119.3
C41—P2—B1 114.98 (10) C56—C55—H55 119.3
C31—P2—B1 108.55 (9) C51—C56—C55 120.4 (2)
C61—P3—C51 99.65 (9) C51—C56—H56 119.8
C61—P3—B1 110.71 (9) C55—C56—H56 119.8
C51—P3—B1 118.17 (9) C66—C61—C62 117.7 (2)
C61—P3—Li1 109.43 (12) C66—C61—P3 124.53 (17)
C51—P3—Li1 132.56 (11) C62—C61—P3 117.72 (18)
B1—P3—Li1 85.78 (12) C63—C62—C61 121.7 (2)
C71—P4—C81 97.66 (9) C63—C62—H62 119.2
C71—P4—B1 111.17 (9) C61—C62—H62 119.2
C81—P4—B1 116.96 (10) C64—C63—C62 119.4 (2)
C71—P4—Li1 119.35 (12) C64—C63—H63 120.3
C81—P4—Li1 125.31 (13) C62—C63—H63 120.3
B1—P4—Li1 87.14 (11) C65—C64—C63 120.0 (2)
C12—C11—C16 117.4 (2) C65—C64—H64 120.0
C12—C11—P1 125.58 (16) C63—C64—H64 120.0
C16—C11—P1 116.87 (16) C64—C65—C66 120.5 (2)
C13—C12—C11 120.8 (2) C64—C65—H65 119.8
C13—C12—H12 119.6 C66—C65—H65 119.8
C11—C12—H12 119.6 C65—C66—C61 120.6 (2)
C12—C13—C14 120.7 (2) C65—C66—H66 119.7
C12—C13—H13 119.6 C61—C66—H66 119.7
C15—C14—C13 119.7 (2) C72—C71—P4 119.23 (17)
C15—C14—H14 120.1 C76—C71—P4 121.98 (16)
C13—C14—H14 120.1 C73—C72—C71 120.3 (2)
C14—C15—C16 119.8 (2) C73—C72—H72 119.8
C14—C15—H15 120.1 C71—C72—H72 119.8
C16—C15—H15 120.1 C74—C73—C72 120.3 (2)
C15—C16—C11 121.6 (2) C74—C73—H73 119.9
C15—C16—H16 119.2 C72—C73—H73 119.9
C11—C16—H16 119.2 C73—C74—C75 120.5 (2)
C26—C21—C22 117.1 (2) C73—C74—H74 119.8
C26—C21—P1 124.50 (17) C75—C74—H74 119.8
C22—C21—P1 118.00 (16) C76—C75—C74 119.5 (2)
C23—C22—C21 121.5 (2) C76—C75—H75 120.3
C23—C22—H22 119.2 C74—C75—H75 120.3
C21—C22—H22 119.2 C75—C76—C71 120.7 (2)
C24—C23—C22 120.4 (2) C75—C76—H76 119.7
C24—C23—H23 119.8 C71—C76—H76 119.7
C22—C23—H23 119.8 C82—C81—C86 118.1 (2)
C25—C24—C23 118.7 (2) C82—C81—P4 126.51 (17)
C25—C24—H24 120.6 C86—C81—P4 115.34 (18)
C23—C24—H24 120.6 C81—C82—C83 120.0 (2)
C24—C25—C26 121.0 (2) C81—C82—H82 120.0
C24—C25—H25 119.5 C83—C82—H82 120.0
C26—C25—H25 119.5 C84—C83—C82 121.2 (3)
C25—C26—C21 121.1 (2) C84—C83—H83 119.4
C25—C26—H26 119.4 C82—C83—H83 119.4
C21—C26—H26 119.4 C83—C84—C85 119.5 (2)
C36—C31—C32 117.4 (2) C83—C84—H84 120.3
C36—C31—P2 116.85 (17) C85—C84—H84 120.3
C32—C31—P2 125.57 (17) C84—C85—C86 120.1 (3)
C36—C31—Li1 95.57 (17) C84—C85—H85 119.9
C32—C31—Li1 74.70 (15) C86—C85—H85 119.9
P2—C31—Li1 104.18 (13) C85—C86—C81 121.0 (3)
C33—C32—C31 120.9 (2) C85—C86—H86 119.5
C33—C32—Li1 97.90 (18) C81—C86—H86 119.5
C31—C32—Li1 73.37 (15) O1—Li1—P4 120.1 (2)
C33—C32—H32 119.5 O1—Li1—C31 126.7 (2)
C31—C32—H32 119.5 P4—Li1—C31 83.28 (14)
Li1—C32—H32 98.7 O1—Li1—C32 115.7 (2)
C34—C33—C32 120.3 (2) P4—Li1—C32 112.62 (17)
C34—C33—H33 119.9 C31—Li1—C32 31.94 (9)
C32—C33—H33 119.9 O1—Li1—P3 141.6 (2)
C33—C34—C35 119.8 (2) P4—Li1—P3 70.05 (11)
C33—C34—H34 120.1 C31—Li1—P3 89.91 (14)
C35—C34—H34 120.1 C32—Li1—P3 88.43 (14)
C34—C35—C36 119.8 (2) C2—C1—H1A 109.5
C34—C35—H35 120.1 C2—C1—H1B 109.5
C35—C36—C31 121.9 (2) C2—C1—H1C 109.5
C35—C36—H36 119.1 H1A—C1—H1C 109.5
C31—C36—H36 119.1 H1B—C1—H1C 109.5
C42—C41—C46 117.86 (19) O1—C2—C1 111.6 (3)
C42—C41—P2 123.96 (15) O1—C2—H2A 109.3
C46—C41—P2 117.30 (17) C1—C2—H2A 109.3
C41—C42—C43 121.0 (2) O1—C2—H2B 109.3
C41—C42—H42 119.5 C1—C2—H2B 109.3
C43—C42—H42 119.5 H2A—C2—H2B 108.0
C44—C43—C42 120.1 (3) C2—O1—C3 116.3 (3)
C44—C43—H43 120.0 C2—O1—Li1 125.7 (3)
C42—C43—H43 120.0 C3—O1—Li1 117.6 (2)
C45—C44—C43 119.5 (2) C4—C3—O1 111.6 (3)
C45—C44—H44 120.2 C4—C3—H3A 109.3
C43—C44—H44 120.2 O1—C3—H3A 109.3
C44—C45—C46 120.8 (2) C4—C3—H3B 109.3
C44—C45—H45 119.6 O1—C3—H3B 109.3
C46—C45—H45 119.6 H3A—C3—H3B 108.0
C45—C46—C41 120.7 (2) C3—C4—H4A 109.5
C45—C46—H46 119.7 C3—C4—H4B 109.5
C41—C46—H46 119.7 H4A—C4—H4B 109.5
C56—C51—C52 117.33 (19) C3—C4—H4C 109.5
C56—C51—P3 121.34 (17) H4A—C4—H4C 109.5
C52—C51—P3 121.23 (15) H4B—C4—H4C 109.5
C53—C52—C51 121.7 (2)
P2—B1—P1—C21 81.82 (13) C54—C55—C56—C51 −1.0 (4)
P3—B1—P1—C21 −60.11 (13) C51—P3—C61—C66 −92.07 (19)
P4—B1—P1—C21 −167.15 (10) B1—P3—C61—C66 33.1 (2)
P2—B1—P1—C11 −30.41 (13) Li1—P3—C61—C66 126.0 (2)
P3—B1—P1—C11 −172.35 (10) C51—P3—C61—C62 85.98 (19)
P4—B1—P1—C11 80.62 (12) B1—P3—C61—C62 −148.84 (17)
P1—B1—P2—C41 −73.44 (13) Li1—P3—C61—C62 −56.0 (2)
P3—B1—P2—C41 70.95 (13) C66—C61—C62—C63 −0.4 (3)
P4—B1—P2—C41 166.61 (8) P3—C61—C62—C63 −178.6 (2)
P1—B1—P2—C31 175.25 (10) C61—C62—C63—C64 −0.4 (4)
P3—B1—P2—C31 −40.37 (13) C62—C63—C64—C65 0.5 (4)
P4—B1—P2—C31 55.30 (11) C63—C64—C65—C66 0.2 (4)
P2—B1—P3—C61 168.68 (10) C64—C65—C66—C61 −1.0 (4)
P1—B1—P3—C61 −48.48 (13) C62—C61—C66—C65 1.1 (3)
P4—B1—P3—C61 69.74 (11) P3—C61—C66—C65 179.17 (17)
P2—B1—P3—C51 −77.38 (13) C81—P4—C71—C72 −121.65 (18)
P1—B1—P3—C51 65.46 (13) B1—P4—C71—C72 115.49 (18)
P4—B1—P3—C51 −176.32 (8) Li1—P4—C71—C72 16.5 (2)
P2—B1—P3—Li1 59.49 (13) C81—P4—C71—C76 57.2 (2)
P1—B1—P3—Li1 −157.67 (13) B1—P4—C71—C76 −65.7 (2)
P4—B1—P3—Li1 −39.45 (11) Li1—P4—C71—C76 −164.66 (19)
P1—B1—P4—C71 44.11 (14) P4—C71—C72—C73 −179.73 (18)
P3—B1—P4—C71 −79.82 (10) C71—C72—C73—C74 −0.1 (4)
P2—B1—P4—C81 55.36 (12) C72—C73—C74—C75 −0.7 (4)
P1—B1—P4—C81 −66.82 (13) C73—C74—C75—C76 0.3 (4)
P3—B1—P4—C81 169.24 (8) C74—C75—C76—C71 1.0 (4)
P2—B1—P4—Li1 −73.25 (13) C72—C71—C76—C75 −1.8 (3)
P1—B1—P4—Li1 164.57 (14) P4—C71—C76—C75 179.33 (18)
P3—B1—P4—Li1 40.64 (12) C71—P4—C81—C82 −111.0 (2)
C21—P1—C11—C12 −59.3 (2) B1—P4—C81—C82 7.5 (2)
B1—P1—C11—C12 58.0 (2) Li1—P4—C81—C82 114.5 (2)
C21—P1—C11—C16 125.26 (17) C71—P4—C81—C86 66.46 (19)
B1—P1—C11—C16 −117.38 (17) B1—P4—C81—C86 −175.03 (16)
C16—C11—C12—C13 2.5 (3) Li1—P4—C81—C86 −68.1 (2)
P1—C11—C12—C13 −172.91 (19) C86—C81—C82—C83 −3.2 (3)
C11—C12—C13—C14 0.0 (4) P4—C81—C82—C83 174.15 (18)
C12—C13—C14—C15 −1.9 (4) C81—C82—C83—C84 1.9 (4)
C13—C14—C15—C16 1.3 (4) C82—C83—C84—C85 0.5 (4)
C14—C15—C16—C11 1.2 (4) C83—C84—C85—C86 −1.6 (4)
C12—C11—C16—C15 −3.1 (3) C84—C85—C86—C81 0.2 (4)
P1—C11—C16—C15 172.71 (18) C82—C81—C86—C85 2.2 (4)
C11—P1—C21—C26 −13.89 (19) P4—C81—C86—C85 −175.5 (2)
B1—P1—C21—C26 −129.82 (17) C71—P4—Li1—O1 −58.9 (3)
C11—P1—C21—C22 173.49 (15) C81—P4—Li1—O1 67.0 (3)
B1—P1—C21—C22 57.56 (17) B1—P4—Li1—O1 −171.6 (3)
C26—C21—C22—C23 3.1 (3) C71—P4—Li1—C31 172.33 (10)
P1—C21—C22—C23 176.28 (16) C81—P4—Li1—C31 −61.82 (16)
C21—C22—C23—C24 −3.3 (3) B1—P4—Li1—C31 59.58 (12)
C22—C23—C24—C25 1.0 (3) C71—P4—Li1—C32 159.44 (14)
C23—C24—C25—C26 1.2 (3) C81—P4—Li1—C32 −74.7 (2)
C24—C25—C26—C21 −1.3 (3) B1—P4—Li1—C32 46.69 (18)
C22—C21—C26—C25 −0.8 (3) C71—P4—Li1—P3 79.98 (12)
P1—C21—C26—C25 −173.53 (17) C81—P4—Li1—P3 −154.17 (9)
C41—P2—C31—C36 128.96 (17) B1—P4—Li1—P3 −32.78 (9)
B1—P2—C31—C36 −110.15 (17) C36—C31—Li1—O1 −36.8 (3)
C41—P2—C31—C32 −46.01 (19) C32—C31—Li1—O1 80.1 (3)
B1—P2—C31—C32 74.88 (19) P2—C31—Li1—O1 −156.3 (2)
C41—P2—C31—Li1 −127.15 (14) C36—C31—Li1—P4 85.99 (16)
B1—P2—C31—Li1 −6.26 (15) C32—C31—Li1—P4 −157.09 (17)
C36—C31—C32—C33 −1.0 (3) P2—C31—Li1—P4 −33.53 (14)
P2—C31—C32—C33 173.98 (17) C36—C31—Li1—C32 −116.9 (2)
Li1—C31—C32—C33 −89.3 (2) P2—C31—Li1—C32 123.56 (17)
C36—C31—C32—Li1 88.4 (2) C36—C31—Li1—P3 155.91 (16)
P2—C31—C32—Li1 −96.69 (18) C32—C31—Li1—P3 −87.17 (16)
C31—C32—C33—C34 0.0 (4) P2—C31—Li1—P3 36.39 (14)
Li1—C32—C33—C34 −75.3 (3) C33—C32—Li1—O1 1.3 (3)
C32—C33—C34—C35 1.2 (4) C31—C32—Li1—O1 −118.7 (3)
C33—C34—C35—C36 −1.4 (4) C33—C32—Li1—P4 144.7 (2)
C32—C31—C36—C35 0.8 (3) C33—C32—Li1—C31 120.0 (2)
P2—C31—C36—C35 −174.62 (19) C33—C32—Li1—P3 −147.66 (18)
Li1—C31—C36—C35 76.4 (3) C31—C32—Li1—P3 92.35 (15)
C31—P2—C41—C42 144.6 (2) C61—P3—Li1—O1 36.3 (4)
B1—P2—C41—C42 28.5 (2) C51—P3—Li1—O1 −88.1 (3)
C31—P2—C41—C46 −46.40 (18) B1—P3—Li1—O1 146.8 (3)
B1—P2—C41—C46 −162.56 (16) C61—P3—Li1—P4 −77.28 (11)
C46—C41—C42—C43 0.0 (4) C51—P3—Li1—P4 158.30 (10)
P2—C41—C42—C43 168.9 (2) B1—P3—Li1—P4 33.21 (8)
C41—C42—C43—C44 0.1 (4) C61—P3—Li1—C31 −160.16 (11)
C42—C43—C44—C45 0.3 (4) C51—P3—Li1—C31 75.42 (18)
C43—C44—C45—C46 −0.9 (4) B1—P3—Li1—C31 −49.67 (11)
C44—C45—C46—C41 1.0 (4) C61—P3—Li1—C32 167.93 (11)
C42—C41—C46—C45 −0.6 (3) C51—P3—Li1—C32 43.5 (2)
P2—C41—C46—C45 −170.22 (18) B1—P3—Li1—C32 −81.58 (12)
C61—P3—C51—C56 176.16 (19) C1—C2—O1—C3 −179.8 (4)
B1—P3—C51—C56 56.3 (2) C1—C2—O1—Li1 −7.7 (7)
Li1—P3—C51—C56 −55.9 (3) P4—Li1—O1—C2 145.0 (4)
C61—P3—C51—C52 −7.6 (2) C31—Li1—O1—C2 −109.8 (5)
B1—P3—C51—C52 −127.45 (19) C32—Li1—O1—C2 −74.4 (5)
Li1—P3—C51—C52 120.3 (2) P3—Li1—O1—C2 49.5 (5)
C56—C51—C52—C53 −1.2 (4) P4—Li1—O1—C3 −43.0 (3)
P3—C51—C52—C53 −177.6 (2) C31—Li1—O1—C3 62.3 (3)
C51—C52—C53—C54 0.0 (4) C32—Li1—O1—C3 97.6 (3)
C52—C53—C54—C55 0.7 (4) P3—Li1—O1—C3 −138.5 (3)
C53—C54—C55—C56 −0.2 (5) C2—O1—C3—C4 −77.8 (5)
C52—C51—C56—C55 1.7 (4) Li1—O1—C3—C4 109.4 (4)
