Lithium tetra­kis(diphenyl­phosphino)borate diethyl ether solvate

Dornhaus, F.; Bolte, M.

doi:10.1107/S1600536806051130

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Lithium tetrakis(diphenylphosphino)borate diethyl ether solvate

F. Dornhaus and M. Bolte

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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051130/hb2216sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051130/hb2216Isup2.hkl Contains datablock I

CCDC reference: 633860

checkCIF report

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.003 Å
R factor = 0.038
wR factor = 0.097
Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT220_ALERT_2_A Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       5.14 Ratio

Author Response: C2 belongs to a diethyl ether molecule which might be slightly disordered. However, a model without disorder was chosen for refinement, since it gave a better result.


Alert level B
PLAT222_ALERT_3_B Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       4.16 Ratio
PLAT241_ALERT_2_B Check High      Ueq as Compared to Neighbors for         C2

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         O1

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.66
           From the CIF: _reflns_number_total               8770
           Count of symmetry unique reflns         5463
           Completeness (_total/calc)            160.53%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      3307
           Fraction of Friedel pairs measured     0.605
           Are heavy atom types Z>Si present        yes

   1 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   2 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
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

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: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.

Lithium tetrakis(diphenylphosphino)borate diethyl ether solvate top

Crystal data top

Li⁺·C₄₈H₄₀BP₄⁻·C₄H₁₀O	F(000) = 876
M_r = 832.55	D_x = 1.233 Mg m⁻³
Monoclinic, P2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2yb	Cell parameters from 22354 reflections
a = 11.7386 (7) Å	θ = 3.1–27.3°
b = 13.2135 (11) Å	µ = 0.21 mm⁻¹
c = 14.4602 (9) Å	T = 173 K
β = 91.216 (5)°	Block, yellow
V = 2242.4 (3) Å³	0.50 × 0.49 × 0.47 mm
Z = 2

Data collection top

Stoe IPDS-II two-circle diffractometer	8770 independent reflections
Radiation source: fine-focus sealed tube	8251 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.038
ω scans	θ_max = 27.7°, θ_min = 3.1°
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995)	h = −14→15
T_min = 0.904, T_max = 0.909	k = −17→15
16919 measured reflections	l = −18→18

Refinement top

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.038	w = 1/[σ²(F_o²) + (0.0682P)² + 0.0442P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.097	(Δ/σ)_max = 0.001
S = 1.05	Δρ_max = 0.28 e Å⁻³
8770 reflections	Δρ_min = −0.23 e Å⁻³
533 parameters	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
1 restraint	Extinction coefficient: 0.0061 (12)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983), 3383 Friedel pairs
Secondary atom site location: difference Fourier map	Absolute structure parameter: −0.04 (5)

Special details top

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 BF₃^.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) top

	x	y	z	U_iso*/U_eq
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)
H33	0.7637	0.7473	0.9964	0.044*
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)
H75	0.7497	0.3201	0.3755	0.046*
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) top

	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)
C24	0.0310 (12)	0.0322 (12)	0.0275 (10)	−0.0080 (10)	0.0040 (8)	−0.0015 (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)
C4	0.084 (3)	0.086 (3)	0.076 (2)	−0.031 (3)	0.008 (2)	0.012 (2)

Geometric parameters (Å, º) top

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—C35	1.388 (4)	C1—C2	1.451 (6)
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
C14—C13—H13	119.6	C72—C71—C76	118.78 (19)
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
C36—C35—H35	120.1	H1A—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)
P2—B1—P4—C71	166.29 (9)	C76—C71—C72—C73	1.4 (3)
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)
C34—C35—C36—C31	0.4 (4)	C31—C32—Li1—P4	24.76 (19)
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)
P3—C51—C56—C55	178.1 (2)

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