trans-Di­chloro­bis­[ethane-1,2-diyl­bis­(di­phenyl­phophine)-κ²P,P′]­tungsten(II) pentane hemisolvate

trans-[WCl₂(dppe)₂] [dppe is ethane-1,2-diyl­bis­(di­phenyl­phosphine), C₂₆H₂₄P₂] was formed as by-product in the reaction of trans-[W(dppe)₂(N₂)₂] with the m-ter­phenyl­tin(II) chloride, [Sn(Cl)(C₆H₃-2,6-Mes₂)]₂ (Mes is 2,4,6-tri­methyl­phenyl), which yields mainly the stannyl­idyne complex trans-[Cl(dppe)₂W[triple bond]Sn—C₆H₃-2,6-Mes₂]. The crystal structure of the ­pentane hemisolvate, trans-[WCl₂(dppe)₂]·0.5C₅H₁₂, has been determined. The geometric parameters of the title compound are compared with those of trans-[MoCl₂(dppe)₂]·0.5C₅H₁₂.

Key indicators

• Single-crystal X-ray study
• T = 180 K
• Mean [sigma](C-C) = 0.008 Å
• Disorder in solvent or counterion
• R factor = 0.036
• wR factor = 0.084
• Data-to-parameter ratio = 15.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_302  Alert C Anion/Solvent Disorder .........................      50.00 Perc.


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 1 Alert Level C = Please check

---

Computing details

Data collection: IPDS2.87 (Stoe & Cie, 1997); cell refinement: IPDS2.87; data reduction: IPDS2.87; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND2.1c (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.

trans-Dichlorobis[ethane-1,2-diylbis(diphenylphophine)-κ2P,P']tungsten(II) hemipentane solvate

Crystal data

[WCl2(C26H24P2)2]·0.5C5H12	F(000) = 4392
Mr = 1087.61	Dx = 1.514 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1723 reflections
a = 49.230 (13) Å	θ = 3.0–25.0°
b = 10.955 (2) Å	µ = 2.70 mm^−1
c = 17.937 (4) Å	T = 180 K
β = 99.49 (3)°	Plate, yellow
V = 9542 (4) Å^3	0.24 × 0.20 × 0.08 mm
Z = 8

Data collection

Stoe IPDS diffractometer	8465 independent reflections
Radiation source: fine-focus sealed X-ray tube	6743 reflections with I > 2σ(I)
Planar graphite monochromator	Rint = 0.056
Detector resolution: 6.667 pixels mm^-1	θmax = 25.5°, θmin = 2.2°
φ–oscill., φ–incr. = 1.3°, 185 exposures scans	h = −59→59
Absorption correction: part of the refinement model (ΔF) (Walker & Stuart, 1983)	k = −13→13
Tmin = 0.563, Tmax = 0.813	l = −21→21
32126 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.036	H-atom parameters constrained
wR(F^2) = 0.084	w = 1/[σ^2(Fo^2) + (0.0538P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.95	(Δ/σ)max = 0.029
8465 reflections	Δρmax = 1.39 e Å^−3
553 parameters	Δρmin = −2.54 e Å^−3
11 restraints	Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00009 (2)

Special details

Experimental. During data collection the crystal was in cold N₂ gas of a cryostream cooler (Oxford Cryosystems).

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. It is remarkable that the pentane solvent molecule of (4α) could not be localized in the difference map until the absorption correction was carried out. The calculation was carried out with ABSCORE (Stoe & Cie, 1997), a modification of DIFABS (Walker & Stuart, 1983). In contrast to DIFABS, ABSCORE loads and provides F² instead of F values. For a better convergence in the following least-squares cycles, geometrical restraints had to be applied to the disordered solvent, which could only be refined isotropicaly.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.38687 (10)	0.5703 (4)	1.1446 (3)	0.0232 (10)
H1A	0.3820	0.5716	1.1960	0.028*
H1B	0.3967	0.4928	1.1387	0.028*
C2	0.40592 (9)	0.6776 (4)	1.1360 (3)	0.0225 (10)
H2A	0.4237	0.6677	1.1705	0.027*
H2B	0.3974	0.7551	1.1486	0.027*
C3	0.35449 (9)	0.7141 (4)	0.7625 (3)	0.0195 (10)
H3A	0.3581	0.7518	0.7149	0.023*
H3B	0.3563	0.6246	0.7579	0.023*
C4	0.32507 (9)	0.7453 (4)	0.7743 (3)	0.0207 (10)
H4A	0.3118	0.6974	0.7383	0.025*
H4B	0.3215	0.8329	0.7634	0.025*
C5	0.32991 (9)	0.6493 (4)	1.1263 (3)	0.0185 (10)
C6	0.31244 (9)	0.7420 (4)	1.0924 (3)	0.0217 (10)
H6	0.3125	0.7636	1.0411	0.026*
C7	0.29512 (10)	0.8020 (4)	1.1338 (3)	0.0266 (11)
H7	0.2835	0.8656	1.1111	0.032*
C8	0.29471 (10)	0.7698 (4)	1.2079 (3)	0.0289 (12)
H8	0.2829	0.8116	1.2361	0.035*
C9	0.31155 (10)	0.6762 (4)	1.2413 (3)	0.0260 (11)
H9	0.3111	0.6533	1.2921	0.031*
C10	0.32903 (10)	0.6166 (4)	1.2003 (3)	0.0226 (10)
H10	0.3405	0.5527	1.2232	0.027*
C11	0.34450 (10)	0.4135 (4)	1.0710 (3)	0.0209 (10)
C12	0.31864 (10)	0.3756 (4)	1.0833 (3)	0.0231 (10)
H12	0.3057	0.4342	1.0946	0.028*
C13	0.31167 (11)	0.2520 (4)	1.0793 (3)	0.0301 (12)
H13	0.2939	0.2270	1.0874	0.036*
C14	0.33057 (13)	0.1650 (4)	1.0635 (3)	0.0341 (13)
H14	0.3259	0.0808	1.0610	0.041*
C15	0.35614 (14)	0.2033 (4)	1.0518 (3)	0.0356 (13)
H15	0.3692	0.1443	1.0416	0.043*
C16	0.36331 (11)	0.3256 (4)	1.0544 (3)	0.0261 (11)
H16	0.3810	0.3499	1.0449	0.031*
C17	0.43762 (9)	0.5592 (4)	1.0387 (3)	0.0233 (10)
C18	0.43203 (11)	0.4544 (5)	0.9945 (3)	0.0324 (12)
H18	0.4146	0.4450	0.9632	0.039*
C19	0.45199 (12)	0.3633 (5)	0.9959 (4)	0.0458 (16)
H19	0.4481	0.2926	0.9654	0.055*
C20	0.47720 (12)	0.3756 (6)	1.0413 (4)	0.0498 (18)
H20	0.4906	0.3131	1.0424	0.060*
C21	0.48299 (11)	0.4781 (5)	1.0852 (4)	0.0409 (15)
H21	0.5005	0.4867	1.1161	0.049*
C22	0.46336 (10)	0.5694 (5)	1.0846 (4)	0.0346 (13)
H22	0.4675	0.6394	1.1157	0.042*
C23	0.43309 (9)	0.8166 (4)	1.0323 (3)	0.0265 (11)
C24	0.45031 (10)	0.8185 (5)	0.9777 (4)	0.0333 (13)
H24	0.4520	0.7476	0.9483	0.040*
C25	0.46502 (11)	0.9238 (5)	0.9660 (4)	0.0470 (17)
H25	0.4765	0.9251	0.9284	0.056*
C26	0.46275 (12)	1.0265 (5)	1.0097 (5)	0.0515 (19)
H26	0.4729	1.0979	1.0023	0.062*
C27	0.44586 (13)	1.0260 (5)	1.0638 (4)	0.0505 (18)
H27	0.4444	1.0970	1.0933	0.061*
C28	0.43089 (11)	0.9208 (4)	1.0753 (4)	0.0349 (13)
H28	0.4192	0.9206	1.1125	0.042*
C29	0.41222 (10)	0.7247 (4)	0.8089 (3)	0.0252 (11)
C30	0.41998 (11)	0.6019 (5)	0.8131 (3)	0.0318 (12)
H30	0.4093	0.5446	0.8354	0.038*
C31	0.44294 (11)	0.5629 (6)	0.7853 (4)	0.0443 (15)
H31	0.4476	0.4787	0.7868	0.053*
C32	0.45922 (12)	0.6462 (7)	0.7553 (4)	0.0526 (18)
H32	0.4751	0.6191	0.7363	0.063*
C33	0.45252 (14)	0.7687 (8)	0.7527 (5)	0.063 (2)
H33	0.4639	0.8259	0.7328	0.076*
C34	0.42901 (12)	0.8083 (6)	0.7794 (4)	0.0463 (16)
H34	0.4244	0.8926	0.7775	0.056*
C35	0.37959 (9)	0.9362 (4)	0.8282 (3)	0.0196 (10)
C36	0.39137 (10)	1.0112 (4)	0.8885 (3)	0.0258 (11)
H36	0.3994	0.9758	0.9354	0.031*
C37	0.39130 (11)	1.1381 (4)	0.8794 (3)	0.0313 (12)
H37	0.3994	1.1890	0.9199	0.038*
C38	0.37941 (12)	1.1895 (4)	0.8110 (4)	0.0362 (13)
H38	0.3792	1.2757	0.8052	0.043*
C39	0.36794 (11)	1.1164 (4)	0.7513 (3)	0.0323 (12)
H39	0.3600	1.1522	0.7045	0.039*
C40	0.36805 (10)	0.9897 (4)	0.7599 (3)	0.0264 (11)
H40	0.3602	0.9395	0.7187	0.032*
C41	0.29821 (9)	0.8438 (4)	0.8909 (3)	0.0179 (9)
C42	0.30870 (10)	0.9624 (4)	0.8843 (3)	0.0216 (10)
H42	0.3261	0.9736	0.8692	0.026*
C43	0.29329 (11)	1.0632 (4)	0.9001 (3)	0.0276 (11)
H43	0.3002	1.1432	0.8945	0.033*
C44	0.26828 (11)	1.0483 (4)	0.9236 (3)	0.0327 (12)
H44	0.2581	1.1179	0.9346	0.039*
C45	0.25778 (11)	0.9315 (4)	0.9315 (3)	0.0321 (12)
H45	0.2405	0.9212	0.9479	0.038*
C46	0.27282 (10)	0.8301 (4)	0.9151 (3)	0.0246 (10)
H46	0.2657	0.7506	0.9203	0.030*
C47	0.29343 (9)	0.5885 (4)	0.8573 (3)	0.0165 (9)
C48	0.27319 (9)	0.5806 (4)	0.7934 (3)	0.0240 (11)
H48	0.2724	0.6406	0.7549	0.029*
C49	0.25388 (10)	0.4853 (4)	0.7850 (3)	0.0258 (11)
H49	0.2404	0.4804	0.7406	0.031*
C50	0.25449 (10)	0.3986 (4)	0.8411 (3)	0.0269 (11)
H50	0.2413	0.3344	0.8358	0.032*
C51	0.27443 (11)	0.4058 (4)	0.9053 (3)	0.0288 (12)
H51	0.2748	0.3467	0.9442	0.035*
C52	0.29397 (10)	0.4998 (4)	0.9130 (3)	0.0229 (10)
H52	0.3078	0.5030	0.9567	0.028*
Cl1	0.36390 (2)	0.48302 (9)	0.89323 (7)	0.0224 (2)
Cl2	0.36182 (2)	0.87317 (9)	1.01853 (7)	0.0223 (2)
P1	0.35457 (2)	0.57693 (9)	1.07266 (7)	0.0161 (2)
P2	0.41167 (2)	0.68045 (10)	1.03708 (7)	0.0184 (2)
P3	0.38003 (2)	0.76985 (10)	0.84188 (7)	0.0172 (2)
P4	0.31954 (2)	0.71174 (9)	0.87264 (7)	0.0150 (2)
W	0.365565 (3)	0.680222 (13)	0.956128 (10)	0.01356 (7)
C53	0.5374 (4)	0.821 (2)	1.1865 (18)	0.131 (10)*	0.50
H53A	0.5479	0.8859	1.1668	0.197*	0.50
H53B	0.5306	0.7633	1.1458	0.197*	0.50
H53C	0.5494	0.7775	1.2272	0.197*	0.50
C54	0.5128 (4)	0.8766 (15)	1.2177 (13)	0.104 (7)*	0.50
H54A	0.5198	0.9347	1.2587	0.124*	0.50
H54B	0.5013	0.9233	1.1770	0.124*	0.50
C55	0.4947 (6)	0.7809 (17)	1.249 (2)	0.132 (9)*	0.50
H55A	0.4782	0.7659	1.2098	0.159*	0.50
H55B	0.5051	0.7034	1.2561	0.159*	0.50
C56	0.4849 (6)	0.814 (3)	1.3231 (17)	0.178 (13)*	0.50
H56A	0.4968	0.8803	1.3479	0.213*	0.50
H56B	0.4875	0.7422	1.3569	0.213*	0.50
C57	0.4547 (10)	0.856 (10)	1.315 (3)	0.55 (6)*	0.50
H57A	0.4500	0.8731	1.3646	0.827*	0.50
H57B	0.4426	0.7907	1.2903	0.827*	0.50
H57C	0.4521	0.9295	1.2834	0.827*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.025 (2)	0.025 (2)	0.019 (3)	0.0023 (19)	0.001 (2)	0.0039 (18)
C2	0.020 (2)	0.028 (2)	0.017 (3)	−0.0005 (19)	−0.0064 (19)	0.0001 (19)
C3	0.027 (2)	0.016 (2)	0.015 (3)	−0.0024 (17)	0.002 (2)	−0.0014 (17)
C4	0.021 (2)	0.026 (2)	0.015 (3)	−0.0023 (18)	0.002 (2)	0.0033 (18)
C5	0.023 (2)	0.014 (2)	0.019 (3)	−0.0019 (16)	0.005 (2)	−0.0057 (17)
C6	0.021 (2)	0.023 (2)	0.021 (3)	0.0004 (18)	0.003 (2)	0.0000 (18)
C7	0.023 (2)	0.023 (2)	0.033 (3)	0.0062 (19)	0.002 (2)	0.003 (2)
C8	0.027 (3)	0.027 (2)	0.035 (3)	0.007 (2)	0.012 (2)	−0.002 (2)
C9	0.033 (3)	0.027 (2)	0.020 (3)	−0.001 (2)	0.009 (2)	0.001 (2)
C10	0.030 (3)	0.012 (2)	0.027 (3)	0.0021 (18)	0.006 (2)	0.0031 (18)
C11	0.036 (3)	0.0112 (19)	0.016 (3)	−0.0007 (18)	0.007 (2)	0.0018 (17)
C12	0.036 (3)	0.016 (2)	0.017 (3)	−0.0009 (19)	0.002 (2)	0.0030 (18)
C13	0.041 (3)	0.024 (3)	0.024 (3)	−0.013 (2)	0.003 (2)	0.003 (2)
C14	0.062 (4)	0.016 (2)	0.022 (3)	−0.005 (2)	0.001 (3)	0.0009 (19)
C15	0.062 (4)	0.020 (3)	0.026 (3)	0.007 (2)	0.012 (3)	−0.002 (2)
C16	0.041 (3)	0.017 (2)	0.023 (3)	0.003 (2)	0.013 (2)	0.0001 (19)
C17	0.021 (2)	0.022 (2)	0.026 (3)	0.0056 (18)	0.004 (2)	0.0087 (19)
C18	0.026 (3)	0.027 (3)	0.042 (4)	0.005 (2)	0.003 (2)	0.002 (2)
C19	0.035 (3)	0.031 (3)	0.072 (5)	0.012 (2)	0.010 (3)	−0.002 (3)
C20	0.034 (3)	0.041 (3)	0.075 (5)	0.021 (3)	0.012 (3)	0.016 (3)
C21	0.019 (2)	0.045 (3)	0.056 (5)	0.006 (2)	−0.003 (3)	0.016 (3)
C22	0.024 (3)	0.031 (3)	0.046 (4)	0.001 (2)	0.000 (3)	0.009 (2)
C23	0.017 (2)	0.019 (2)	0.040 (4)	−0.0007 (18)	−0.007 (2)	0.008 (2)
C24	0.022 (2)	0.030 (3)	0.048 (4)	−0.003 (2)	0.004 (2)	0.012 (2)
C25	0.026 (3)	0.038 (3)	0.076 (5)	−0.009 (2)	0.003 (3)	0.026 (3)
C26	0.033 (3)	0.032 (3)	0.083 (6)	−0.015 (3)	−0.009 (3)	0.021 (3)
C27	0.045 (4)	0.020 (3)	0.076 (6)	−0.009 (2)	−0.018 (4)	0.001 (3)
C28	0.035 (3)	0.025 (3)	0.040 (4)	−0.007 (2)	−0.010 (3)	0.000 (2)
C29	0.021 (2)	0.030 (2)	0.025 (3)	0.0008 (19)	0.006 (2)	0.001 (2)
C30	0.030 (3)	0.029 (3)	0.036 (4)	0.003 (2)	0.006 (2)	−0.005 (2)
C31	0.028 (3)	0.053 (4)	0.051 (4)	0.012 (3)	0.002 (3)	−0.018 (3)
C32	0.027 (3)	0.092 (5)	0.041 (4)	0.017 (3)	0.012 (3)	−0.005 (3)
C33	0.040 (4)	0.084 (5)	0.073 (6)	0.007 (4)	0.030 (4)	0.025 (4)
C34	0.037 (3)	0.047 (3)	0.060 (5)	0.006 (3)	0.022 (3)	0.019 (3)
C35	0.022 (2)	0.018 (2)	0.019 (3)	−0.0038 (17)	0.003 (2)	0.0028 (17)
C36	0.031 (3)	0.017 (2)	0.028 (3)	−0.0034 (18)	0.001 (2)	0.0047 (19)
C37	0.041 (3)	0.018 (2)	0.034 (4)	−0.007 (2)	0.004 (3)	−0.005 (2)
C38	0.053 (3)	0.014 (2)	0.042 (4)	0.001 (2)	0.009 (3)	0.006 (2)
C39	0.041 (3)	0.022 (2)	0.032 (3)	0.002 (2)	0.002 (3)	0.011 (2)
C40	0.035 (3)	0.020 (2)	0.023 (3)	−0.0041 (19)	0.002 (2)	0.0053 (19)
C41	0.020 (2)	0.016 (2)	0.015 (3)	−0.0004 (16)	−0.0045 (19)	−0.0003 (16)
C42	0.025 (2)	0.017 (2)	0.021 (3)	−0.0009 (18)	−0.001 (2)	0.0018 (18)
C43	0.038 (3)	0.015 (2)	0.026 (3)	−0.0002 (19)	−0.005 (2)	−0.0040 (18)
C44	0.041 (3)	0.020 (2)	0.035 (4)	0.009 (2)	0.002 (3)	−0.009 (2)
C45	0.032 (3)	0.028 (3)	0.038 (4)	0.006 (2)	0.009 (3)	−0.005 (2)
C46	0.027 (2)	0.018 (2)	0.028 (3)	0.0002 (19)	0.005 (2)	0.0000 (19)
C47	0.015 (2)	0.0140 (19)	0.020 (3)	0.0007 (16)	0.0043 (19)	−0.0022 (17)
C48	0.025 (2)	0.017 (2)	0.028 (3)	0.0003 (18)	−0.001 (2)	0.0032 (19)
C49	0.020 (2)	0.025 (2)	0.028 (3)	−0.0027 (19)	−0.006 (2)	−0.004 (2)
C50	0.024 (2)	0.022 (2)	0.034 (3)	−0.0083 (19)	0.004 (2)	−0.008 (2)
C51	0.033 (3)	0.020 (2)	0.034 (3)	−0.008 (2)	0.008 (2)	0.003 (2)
C52	0.024 (2)	0.026 (2)	0.017 (3)	−0.0044 (18)	−0.001 (2)	0.0010 (18)
Cl1	0.0301 (6)	0.0130 (5)	0.0243 (7)	0.0009 (4)	0.0051 (5)	−0.0034 (4)
Cl2	0.0264 (6)	0.0128 (5)	0.0268 (7)	0.0006 (4)	0.0019 (5)	−0.0029 (4)
P1	0.0195 (5)	0.0114 (5)	0.0173 (7)	0.0008 (4)	0.0024 (5)	0.0001 (4)
P2	0.0169 (5)	0.0147 (5)	0.0227 (7)	0.0005 (4)	0.0002 (5)	0.0027 (5)
P3	0.0197 (6)	0.0119 (5)	0.0203 (7)	−0.0004 (4)	0.0036 (5)	0.0010 (4)
P4	0.0180 (5)	0.0105 (5)	0.0160 (7)	0.0003 (4)	0.0016 (5)	0.0000 (4)
W	0.01620 (10)	0.00847 (9)	0.01562 (12)	0.00015 (7)	0.00152 (7)	0.00036 (7)

Geometric parameters (Å, º)

C1—C2	1.528 (6)	C30—H30	0.9500
C1—P1	1.877 (5)	C31—C32	1.381 (9)
C1—H1A	0.9900	C31—H31	0.9500
C1—H1B	0.9900	C32—C33	1.381 (10)
C2—P2	1.842 (5)	C32—H32	0.9500
C2—H2A	0.9900	C33—C34	1.393 (9)
C2—H2B	0.9900	C33—H33	0.9500
C3—C4	1.536 (6)	C34—H34	0.9500
C3—P3	1.841 (5)	C35—C40	1.393 (7)
C3—H3A	0.9900	C35—C36	1.405 (7)
C3—H3B	0.9900	C35—P3	1.838 (4)
C4—P4	1.865 (5)	C36—C37	1.400 (7)
C4—H4A	0.9900	C36—H36	0.9500
C4—H4B	0.9900	C37—C38	1.388 (8)
C5—C10	1.383 (7)	C37—H37	0.9500
C5—C6	1.403 (7)	C38—C39	1.381 (8)
C5—P1	1.848 (4)	C38—H38	0.9500
C6—C7	1.386 (7)	C39—C40	1.397 (6)
C6—H6	0.9500	C39—H39	0.9500
C7—C8	1.377 (8)	C40—H40	0.9500
C7—H7	0.9500	C41—C46	1.396 (7)
C8—C9	1.390 (7)	C41—C42	1.411 (6)
C8—H8	0.9500	C41—P4	1.848 (4)
C9—C10	1.385 (7)	C42—C43	1.395 (6)
C9—H9	0.9500	C42—H42	0.9500
C10—H10	0.9500	C43—C44	1.376 (8)
C11—C12	1.391 (7)	C43—H43	0.9500
C11—C16	1.402 (6)	C44—C45	1.396 (7)
C11—P1	1.857 (4)	C44—H44	0.9500
C12—C13	1.396 (6)	C45—C46	1.393 (7)
C12—H12	0.9500	C45—H45	0.9500
C13—C14	1.394 (8)	C46—H46	0.9500
C13—H13	0.9500	C47—C52	1.390 (6)
C14—C15	1.376 (8)	C47—C48	1.393 (7)
C14—H14	0.9500	C47—P4	1.854 (4)
C15—C16	1.385 (7)	C48—C49	1.403 (6)
C15—H15	0.9500	C48—H48	0.9500
C16—H16	0.9500	C49—C50	1.382 (7)
C17—C22	1.397 (7)	C49—H49	0.9500
C17—C18	1.397 (7)	C50—C51	1.386 (8)
C17—P2	1.840 (4)	C50—H50	0.9500
C18—C19	1.398 (7)	C51—C52	1.400 (6)
C18—H18	0.9500	C51—H51	0.9500
C19—C20	1.374 (9)	C52—H52	0.9500
C19—H19	0.9500	Cl1—W	2.4324 (11)
C20—C21	1.374 (10)	Cl2—W	2.4131 (11)
C20—H20	0.9500	P1—W	2.5130 (13)
C21—C22	1.389 (7)	P2—W	2.4847 (14)
C21—H21	0.9500	P3—W	2.4803 (13)
C22—H22	0.9500	P4—W	2.5251 (15)
C23—C28	1.391 (8)	C53—C54	1.543 (5)
C23—C24	1.397 (8)	C53—H53A	0.9800
C23—P2	1.837 (5)	C53—H53B	0.9800
C24—C25	1.396 (7)	C53—H53C	0.9800
C24—H24	0.9500	C54—C55	1.538 (5)
C25—C26	1.386 (10)	C54—H54A	0.9900
C25—H25	0.9500	C54—H54B	0.9900
C26—C27	1.378 (10)	C55—C56	1.536 (5)
C26—H26	0.9500	C55—H55A	0.9900
C27—C28	1.402 (7)	C55—H55B	0.9900
C27—H27	0.9500	C56—C57	1.541 (5)
C28—H28	0.9500	C56—H56A	0.9900
C29—C34	1.395 (7)	C56—H56B	0.9900
C29—C30	1.397 (7)	C57—H57A	0.9800
C29—P3	1.848 (5)	C57—H57B	0.9800
C30—C31	1.376 (7)	C57—H57C	0.9800
C2—C1—P1	111.4 (3)	C35—C36—H36	120.1
C2—C1—H1A	109.4	C38—C37—C36	119.9 (5)
P1—C1—H1A	109.4	C38—C37—H37	120.1
C2—C1—H1B	109.4	C36—C37—H37	120.1
P1—C1—H1B	109.4	C39—C38—C37	120.6 (4)
H1A—C1—H1B	108.0	C39—C38—H38	119.7
C1—C2—P2	107.8 (3)	C37—C38—H38	119.7
C1—C2—H2A	110.1	C38—C39—C40	119.8 (5)
P2—C2—H2A	110.1	C38—C39—H39	120.1
C1—C2—H2B	110.1	C40—C39—H39	120.1
P2—C2—H2B	110.1	C35—C40—C39	120.6 (5)
H2A—C2—H2B	108.5	C35—C40—H40	119.7
C4—C3—P3	111.0 (3)	C39—C40—H40	119.7
C4—C3—H3A	109.4	C46—C41—C42	118.9 (4)
P3—C3—H3A	109.4	C46—C41—P4	122.4 (3)
C4—C3—H3B	109.4	C42—C41—P4	118.6 (3)
P3—C3—H3B	109.4	C43—C42—C41	119.5 (4)
H3A—C3—H3B	108.0	C43—C42—H42	120.2
C3—C4—P4	112.0 (3)	C41—C42—H42	120.2
C3—C4—H4A	109.2	C44—C43—C42	120.9 (4)
P4—C4—H4A	109.2	C44—C43—H43	119.6
C3—C4—H4B	109.2	C42—C43—H43	119.6
P4—C4—H4B	109.2	C43—C44—C45	120.3 (4)
H4A—C4—H4B	107.9	C43—C44—H44	119.8
C10—C5—C6	119.3 (4)	C45—C44—H44	119.8
C10—C5—P1	121.1 (3)	C46—C45—C44	119.4 (5)
C6—C5—P1	119.6 (4)	C46—C45—H45	120.3
C7—C6—C5	119.9 (5)	C44—C45—H45	120.3
C7—C6—H6	120.0	C45—C46—C41	121.0 (4)
C5—C6—H6	120.0	C45—C46—H46	119.5
C8—C7—C6	120.2 (4)	C41—C46—H46	119.5
C8—C7—H7	119.9	C52—C47—C48	118.3 (4)
C6—C7—H7	119.9	C52—C47—P4	118.2 (4)
C7—C8—C9	120.2 (4)	C48—C47—P4	123.5 (3)
C7—C8—H8	119.9	C47—C48—C49	121.0 (4)
C9—C8—H8	119.9	C47—C48—H48	119.5
C10—C9—C8	119.8 (5)	C49—C48—H48	119.5
C10—C9—H9	120.1	C50—C49—C48	120.0 (5)
C8—C9—H9	120.1	C50—C49—H49	120.0
C5—C10—C9	120.5 (4)	C48—C49—H49	120.0
C5—C10—H10	119.7	C49—C50—C51	119.6 (4)
C9—C10—H10	119.7	C49—C50—H50	120.2
C12—C11—C16	118.9 (4)	C51—C50—H50	120.2
C12—C11—P1	122.3 (3)	C50—C51—C52	120.3 (5)
C16—C11—P1	118.8 (4)	C50—C51—H51	119.9
C11—C12—C13	120.3 (5)	C52—C51—H51	119.9
C11—C12—H12	119.8	C47—C52—C51	120.8 (5)
C13—C12—H12	119.8	C47—C52—H52	119.6
C14—C13—C12	120.5 (5)	C51—C52—H52	119.6
C14—C13—H13	119.8	C5—P1—C11	103.0 (2)
C12—C13—H13	119.8	C5—P1—C1	102.3 (2)
C15—C14—C13	118.8 (4)	C11—P1—C1	99.6 (2)
C15—C14—H14	120.6	C5—P1—W	119.33 (15)
C13—C14—H14	120.6	C11—P1—W	120.95 (15)
C14—C15—C16	121.6 (5)	C1—P1—W	108.39 (15)
C14—C15—H15	119.2	C23—P2—C17	100.6 (2)
C16—C15—H15	119.2	C23—P2—C2	103.9 (2)
C15—C16—C11	119.9 (5)	C17—P2—C2	100.9 (2)
C15—C16—H16	120.0	C23—P2—W	116.71 (16)
C11—C16—H16	120.0	C17—P2—W	125.01 (17)
C22—C17—C18	118.4 (4)	C2—P2—W	106.98 (15)
C22—C17—P2	120.8 (4)	C35—P3—C3	103.5 (2)
C18—C17—P2	120.9 (4)	C35—P3—C29	102.4 (2)
C19—C18—C17	120.3 (5)	C3—P3—C29	100.1 (2)
C19—C18—H18	119.9	C35—P3—W	120.25 (15)
C17—C18—H18	119.9	C3—P3—W	104.79 (15)
C20—C19—C18	120.3 (6)	C29—P3—W	122.46 (17)
C20—C19—H19	119.8	C41—P4—C47	101.30 (19)
C18—C19—H19	119.8	C41—P4—C4	100.9 (2)
C19—C20—C21	120.1 (5)	C47—P4—C4	102.1 (2)
C19—C20—H20	120.0	C41—P4—W	118.83 (15)
C21—C20—H20	120.0	C47—P4—W	121.39 (15)
C20—C21—C22	120.4 (5)	C4—P4—W	109.34 (15)
C20—C21—H21	119.8	Cl2—W—Cl1	173.65 (4)
C22—C21—H21	119.8	Cl2—W—P3	95.21 (4)
C21—C22—C17	120.6 (5)	Cl1—W—P3	87.74 (4)
C21—C22—H22	119.7	Cl2—W—P2	81.97 (4)
C17—C22—H22	119.7	Cl1—W—P2	103.27 (4)
C28—C23—C24	119.2 (5)	P3—W—P2	97.09 (5)
C28—C23—P2	122.8 (4)	Cl2—W—P1	88.01 (4)
C24—C23—P2	117.7 (4)	Cl1—W—P1	89.45 (4)
C25—C24—C23	120.5 (6)	P3—W—P1	174.87 (4)
C25—C24—H24	119.8	P2—W—P1	79.37 (4)
C23—C24—H24	119.8	Cl2—W—P4	91.47 (4)
C26—C25—C24	119.6 (6)	Cl1—W—P4	83.58 (4)
C26—C25—H25	120.2	P3—W—P4	78.91 (4)
C24—C25—H25	120.2	P2—W—P4	172.02 (4)
C27—C26—C25	120.6 (5)	P1—W—P4	105.05 (4)
C27—C26—H26	119.7	C54—C53—H53A	109.5
C25—C26—H26	119.7	C54—C53—H53B	109.5
C26—C27—C28	120.0 (6)	H53A—C53—H53B	109.5
C26—C27—H27	120.0	C54—C53—H53C	109.5
C28—C27—H27	120.0	H53A—C53—H53C	109.5
C23—C28—C27	120.1 (6)	H53B—C53—H53C	109.5
C23—C28—H28	119.9	C55—C54—C53	113.4 (8)
C27—C28—H28	119.9	C55—C54—H54A	108.9
C34—C29—C30	118.6 (5)	C53—C54—H54A	108.9
C34—C29—P3	122.6 (4)	C55—C54—H54B	108.9
C30—C29—P3	118.8 (4)	C53—C54—H54B	108.9
C31—C30—C29	120.9 (5)	H54A—C54—H54B	107.7
C31—C30—H30	119.6	C56—C55—C54	115.8 (8)
C29—C30—H30	119.6	C56—C55—H55A	108.4
C30—C31—C32	120.0 (6)	C54—C55—H55A	108.4
C30—C31—H31	120.0	C56—C55—H55B	108.3
C32—C31—H31	120.0	C54—C55—H55B	108.3
C31—C32—C33	120.3 (5)	H55A—C55—H55B	107.4
C31—C32—H32	119.9	C55—C56—C57	114.8 (8)
C33—C32—H32	119.9	C55—C56—H56A	108.6
C32—C33—C34	119.9 (6)	C57—C56—H56A	108.6
C32—C33—H33	120.0	C55—C56—H56B	108.6
C34—C33—H33	120.0	C57—C56—H56B	108.5
C33—C34—C29	120.2 (6)	H56A—C56—H56B	107.5
C33—C34—H34	119.9	C56—C57—H57A	109.5
C29—C34—H34	119.9	C56—C57—H57B	109.6
C40—C35—C36	119.2 (4)	H57A—C57—H57B	109.5
C40—C35—P3	121.9 (4)	C56—C57—H57C	109.4
C36—C35—P3	118.9 (4)	H57A—C57—H57C	109.5
C37—C36—C35	119.9 (5)	H57B—C57—H57C	109.5
C37—C36—H36	120.1
P1—C1—C2—P2	−53.5 (4)	C18—C17—P2—C23	−136.0 (4)
P3—C3—C4—P4	−44.9 (4)	C22—C17—P2—C2	−62.1 (4)
C10—C5—C6—C7	1.8 (7)	C18—C17—P2—C2	117.5 (4)
P1—C5—C6—C7	−175.9 (4)	C22—C17—P2—W	178.0 (3)
C5—C6—C7—C8	−0.9 (7)	C18—C17—P2—W	−2.4 (5)
C6—C7—C8—C9	−0.4 (8)	C1—C2—P2—C23	177.1 (3)
C7—C8—C9—C10	0.9 (8)	C1—C2—P2—C17	−79.0 (3)
C6—C5—C10—C9	−1.3 (7)	C1—C2—P2—W	53.1 (3)
P1—C5—C10—C9	176.3 (4)	C40—C35—P3—C3	−16.3 (4)
C8—C9—C10—C5	0.0 (7)	C36—C35—P3—C3	164.1 (4)
C16—C11—C12—C13	0.1 (7)	C40—C35—P3—C29	87.5 (4)
P1—C11—C12—C13	178.1 (4)	C36—C35—P3—C29	−92.1 (4)
C11—C12—C13—C14	0.5 (8)	C40—C35—P3—W	−132.6 (4)
C12—C13—C14—C15	−0.2 (8)	C36—C35—P3—W	47.7 (4)
C13—C14—C15—C16	−0.8 (9)	C4—C3—P3—C35	−72.3 (3)
C14—C15—C16—C11	1.4 (9)	C4—C3—P3—C29	−177.8 (3)
C12—C11—C16—C15	−1.1 (8)	C4—C3—P3—W	54.6 (3)
P1—C11—C16—C15	−179.1 (4)	C34—C29—P3—C35	−2.4 (6)
C22—C17—C18—C19	−0.7 (8)	C30—C29—P3—C35	178.1 (4)
P2—C17—C18—C19	179.7 (5)	C34—C29—P3—C3	104.1 (5)
C17—C18—C19—C20	0.5 (9)	C30—C29—P3—C3	−75.5 (5)
C18—C19—C20—C21	−0.5 (10)	C34—C29—P3—W	−141.0 (5)
C19—C20—C21—C22	0.7 (10)	C30—C29—P3—W	39.4 (5)
C20—C21—C22—C17	−0.9 (9)	C46—C41—P4—C47	21.4 (5)
C18—C17—C22—C21	0.9 (8)	C42—C41—P4—C47	−162.2 (4)
P2—C17—C22—C21	−179.5 (4)	C46—C41—P4—C4	126.2 (4)
C28—C23—C24—C25	−0.4 (8)	C42—C41—P4—C4	−57.4 (4)
P2—C23—C24—C25	173.6 (4)	C46—C41—P4—W	−114.3 (4)
C23—C24—C25—C26	0.9 (9)	C42—C41—P4—W	62.1 (4)
C24—C25—C26—C27	−0.8 (9)	C52—C47—P4—C41	−108.3 (4)
C25—C26—C27—C28	0.3 (10)	C48—C47—P4—C41	71.2 (4)
C24—C23—C28—C27	−0.1 (8)	C52—C47—P4—C4	147.8 (4)
P2—C23—C28—C27	−173.7 (4)	C48—C47—P4—C4	−32.7 (4)
C26—C27—C28—C23	0.1 (9)	C52—C47—P4—W	26.0 (4)
C34—C29—C30—C31	−3.2 (9)	C48—C47—P4—W	−154.5 (3)
P3—C29—C30—C31	176.3 (5)	C3—C4—P4—C41	140.6 (3)
C29—C30—C31—C32	2.4 (9)	C3—C4—P4—C47	−115.2 (3)
C30—C31—C32—C33	−0.2 (10)	C3—C4—P4—W	14.6 (3)
C31—C32—C33—C34	−1.0 (12)	C35—P3—W—Cl2	−7.75 (18)
C32—C33—C34—C29	0.1 (12)	C3—P3—W—Cl2	−123.49 (15)
C30—C29—C34—C33	2.0 (10)	C29—P3—W—Cl2	123.9 (2)
P3—C29—C34—C33	−177.6 (6)	C35—P3—W—Cl1	166.61 (18)
C40—C35—C36—C37	0.3 (7)	C3—P3—W—Cl1	50.88 (15)
P3—C35—C36—C37	179.9 (4)	C29—P3—W—Cl1	−61.7 (2)
C35—C36—C37—C38	0.5 (8)	C35—P3—W—P2	−90.29 (18)
C36—C37—C38—C39	−0.9 (8)	C3—P3—W—P2	153.98 (15)
C37—C38—C39—C40	0.6 (8)	C29—P3—W—P2	41.4 (2)
C36—C35—C40—C39	−0.5 (7)	C35—P3—W—P4	82.72 (18)
P3—C35—C40—C39	179.8 (4)	C3—P3—W—P4	−33.01 (15)
C38—C39—C40—C35	0.1 (8)	C29—P3—W—P4	−145.6 (2)
C46—C41—C42—C43	−1.5 (7)	C23—P2—W—Cl2	−52.5 (2)
P4—C41—C42—C43	−178.1 (4)	C17—P2—W—Cl2	−179.69 (19)
C41—C42—C43—C44	1.4 (8)	C2—P2—W—Cl2	63.21 (16)
C42—C43—C44—C45	−0.5 (8)	C23—P2—W—Cl1	131.1 (2)
C43—C44—C45—C46	−0.2 (8)	C17—P2—W—Cl1	3.94 (19)
C44—C45—C46—C41	0.1 (8)	C2—P2—W—Cl1	−113.16 (16)
C42—C41—C46—C45	0.8 (8)	C23—P2—W—P3	41.8 (2)
P4—C41—C46—C45	177.2 (4)	C17—P2—W—P3	−85.40 (19)
C52—C47—C48—C49	−0.3 (7)	C2—P2—W—P3	157.50 (16)
P4—C47—C48—C49	−179.8 (4)	C23—P2—W—P1	−142.0 (2)
C47—C48—C49—C50	1.0 (7)	C17—P2—W—P1	90.84 (19)
C48—C49—C50—C51	−0.6 (7)	C2—P2—W—P1	−26.26 (16)
C49—C50—C51—C52	−0.4 (8)	C5—P1—W—Cl2	35.71 (17)
C48—C47—C52—C51	−0.8 (7)	C11—P1—W—Cl2	165.40 (19)
P4—C47—C52—C51	178.7 (4)	C1—P1—W—Cl2	−80.70 (16)
C50—C51—C52—C47	1.2 (7)	C5—P1—W—Cl1	−138.47 (17)
C10—C5—P1—C11	61.3 (4)	C11—P1—W—Cl1	−8.78 (19)
C6—C5—P1—C11	−121.0 (4)	C1—P1—W—Cl1	105.12 (16)
C10—C5—P1—C1	−41.8 (4)	C5—P1—W—P2	117.92 (17)
C6—C5—P1—C1	135.9 (4)	C11—P1—W—P2	−112.39 (19)
C10—C5—P1—W	−161.4 (3)	C1—P1—W—P2	1.51 (16)
C6—C5—P1—W	16.3 (4)	C5—P1—W—P4	−55.27 (17)
C12—C11—P1—C5	20.3 (5)	C11—P1—W—P4	74.42 (19)
C16—C11—P1—C5	−161.8 (4)	C1—P1—W—P4	−171.68 (16)
C12—C11—P1—C1	125.4 (4)	C41—P4—W—Cl2	−6.97 (17)
C16—C11—P1—C1	−56.6 (4)	C47—P4—W—Cl2	−133.68 (17)
C12—C11—P1—W	−116.2 (4)	C4—P4—W—Cl2	108.03 (16)
C16—C11—P1—W	61.8 (4)	C41—P4—W—Cl1	169.06 (17)
C2—C1—P1—C5	−97.1 (4)	C47—P4—W—Cl1	42.35 (17)
C2—C1—P1—C11	157.2 (3)	C4—P4—W—Cl1	−75.94 (16)
C2—C1—P1—W	29.9 (4)	C41—P4—W—P3	−101.99 (17)
C28—C23—P2—C17	−136.6 (4)	C47—P4—W—P3	131.30 (17)
C24—C23—P2—C17	49.6 (5)	C4—P4—W—P3	13.01 (16)
C28—C23—P2—C2	−32.5 (5)	C41—P4—W—P1	81.36 (17)
C24—C23—P2—C2	153.8 (4)	C47—P4—W—P1	−45.35 (17)
C28—C23—P2—W	85.0 (5)	C4—P4—W—P1	−163.64 (16)
C24—C23—P2—W	−88.8 (4)	C53—C54—C55—C56	138 (3)
C22—C17—P2—C23	44.4 (5)	C54—C55—C56—C57	103 (5)