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The title compound, cis-[W(CO)2(dppe)2] [dppe is 1,2-ethane­diyl­bis­(di­phenyl­phosphine), C26H24P2], was obtained as a by-product during the preparation of the di­nitro­gen complex trans-[W(CO)(N2)(dppe)2]. The crystal structure of the benzene sesquisolvate, i.e. cis-[W(C26H24P2)2(CO)2]·1.5C6H6, has been determined.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801010893/bt6052sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801010893/bt6052Isup2.hkl
Contains datablock I

CCDC reference: 170863

Key indicators

  • Single-crystal X-ray study
  • T = 180 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.022
  • wR factor = 0.053
  • Data-to-parameter ratio = 14.3

checkCIF results

No syntax errors found

Structure: phili

ADDSYM reports no extra symmetry
Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.50 From the CIF: _reflns_number_total 18050 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 19213 Completeness (_total/calc) 93.95% Alert C: < 95% complete PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 271 O2 -C6 -W1 -C5 51.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 272 O2 -C6 -W1 -P4 -43.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 273 O2 -C6 -W1 -P1 137.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 274 O2 -C6 -W1 -P2 -43.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 275 O2 -C6 -W1 -P3 -143.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 276 O1 -C5 -W1 -C6 52.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 277 O1 -C5 -W1 -P4 139.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 278 O1 -C5 -W1 -P1 -42.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 279 O1 -C5 -W1 -P2 -142.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 280 O1 -C5 -W1 -P3 -34.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 287 C49 -P4 -W1 -P1 -107.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 288 C43 -P4 -W1 -P1 132.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 289 C4 -P4 -W1 -P1 10.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 302 C7 -P1 -W1 -P4 13.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 303 C1 -P1 -W1 -P4 -107.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 304 C13 -P1 -W1 -P4 137.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 341 O4 -C69 -W2 -C68 -57.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 342 O4 -C69 -W2 -P7 38.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 343 O4 -C69 -W2 -P8 -144.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 344 O4 -C69 -W2 -P5 138.00 2.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 345 O4 -C69 -W2 -P6 24.00 3.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 346 O3 -C68 -W2 -C69 -52.00 4.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 347 O3 -C68 -W2 -P7 -136.00 4.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 348 O3 -C68 -W2 -P8 40.00 4.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 349 O3 -C68 -W2 -P5 46.00 4.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 350 O3 -C68 -W2 -P6 145.00 4.00 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 357 C100-P7 -W2 -P8 49.10 0.30 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 358 C66 -P7 -W2 -P8 169.50 0.30 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 359 C94 -P7 -W2 -P8 -74.80 0.30 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 372 C112-P8 -W2 -P7 168.20 0.30 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 373 C106-P8 -W2 -P7 46.50 0.30 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 374 C65 -P8 -W2 -P7 -70.00 0.30 1.555 1.555 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
33 Alert Level C = Please check

Comment top

Reaction of the germylenes Cp*GeX (Cp* = C5Me5; X = Cl, Br, I) with the bis-dinitrogen complex trans-[W(dppe)2(N2)2] has been recently shown to provide a convenient route to the complexes trans-[X(dppe)2WGe(η1-Cp*)] (X = Cl, Br, I) bearing a transition metal–germanium triple bond (Filippou et al., 2000). In order to test the influence of a carbonyl ligand on the course of this reaction, the dinitrogen complex trans-[W(CO)(N2)(dppe)2], (2), was prepared from trans-[W(CO)(DMF)(dppe)2] (DMF is N,N'-dimethylformamide), (1) (Ishida et al., 1991). Yellow single crystals of the title compound, (3), as benzene sesquisolvate (1.5C6H6), (3a), were obtained from the washing solution after the isolation of complex (2).

Complex (3) was first prepared by Chatt & Watson (1961), however, its molecular structure in the solid state was unknown to this day. Two distorted octahedral molecules with marginally different bonding parameters and three molecules of benzene are present in the asymmetric unit of the cell. The W—P bonds trans to the carbonyl ligands have an average value of 2.5490 (9) Å, which is considerably larger than that of the W—P bonds cis to the carbonyl ligands [2.4525 (9) Å] indicating the strong trans influence of the CO groups.

Experimental top

Complex (1) (220 mg, 0.203 mmol) was suspended in benzene (20 ml) and the suspension stirred under an atmosphere of dry nitrogen. IR monitoring of the reaction revealed a gradual increase in intensity of the ν(NN) and ν(CO) absorption of the product (2) at 2071 and 1801 cm-1, respectively, and of the ν(CO) absorption of uncoordinated DMF at 1684 cm-1. After approximately 10 h, all starting material had dissolved and the colour of the solution had changed from red to orange. Pentane (25 ml) was then added to the solution to precipitate complex (2) as an orange solid, which was washed with pentane (2 x 5 ml) and dried in vacuo at 253 K. The supernatant solution was combined with the pentane washings and allowed to stand for one day at ambient temperature to afford yellow crystals of (3a). IR of the crystals (KBr, cm-1): 1852 (versus), 1778 (versus) [ν(CO)]; (THF, cm-1): 1857 (versus), 1795 (s) [ν(CO]; (C6H6, cm-1): 1857(versus), 1795 (s) [ν(CO)]. During data collection the crystal was in cold N2 gas of the Cryostream cooler (Oxford Cryosystems, 1992) mounted on a φ-axis diffractometer supplied with an area detector.

Structure description top

Reaction of the germylenes Cp*GeX (Cp* = C5Me5; X = Cl, Br, I) with the bis-dinitrogen complex trans-[W(dppe)2(N2)2] has been recently shown to provide a convenient route to the complexes trans-[X(dppe)2WGe(η1-Cp*)] (X = Cl, Br, I) bearing a transition metal–germanium triple bond (Filippou et al., 2000). In order to test the influence of a carbonyl ligand on the course of this reaction, the dinitrogen complex trans-[W(CO)(N2)(dppe)2], (2), was prepared from trans-[W(CO)(DMF)(dppe)2] (DMF is N,N'-dimethylformamide), (1) (Ishida et al., 1991). Yellow single crystals of the title compound, (3), as benzene sesquisolvate (1.5C6H6), (3a), were obtained from the washing solution after the isolation of complex (2).

Complex (3) was first prepared by Chatt & Watson (1961), however, its molecular structure in the solid state was unknown to this day. Two distorted octahedral molecules with marginally different bonding parameters and three molecules of benzene are present in the asymmetric unit of the cell. The W—P bonds trans to the carbonyl ligands have an average value of 2.5490 (9) Å, which is considerably larger than that of the W—P bonds cis to the carbonyl ligands [2.4525 (9) Å] indicating the strong trans influence of the CO groups.

Computing details top

Data collection: IPDS2.87 (Stoe & Cie, 1997); cell refinement: IPDS2.87; data reduction: IPDS2.87; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. DIAMOND plot (Brandenburg, 1996) of one molecule (3a) and one solvate molecule showing 50% probability displacement ellipsoids. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. DIAMOND plot (Brandenburg, 1996) of one solvate molecule. H atoms have been omitted for clarity.
[Figure 3] Fig. 3. DIAMOND plot (Brandenburg, 1996) of the second molecule of (3a) and one solvate molecule showing 50% probability displacement ellipsoids. H atoms have been omitted for clarity.
cis-Dicarbonylbis[1,2-ethanediylbis(diphenylphosphine)-P,P']tungsten(0) benzene sesquisolvate top
Crystal data top
[W(CO)2(C26H24P2)2]·1.5C6H6Z = 4
Mr = 1153.82F(000) = 2340
Triclinic, P1Dx = 1.486 Mg m3
a = 12.675 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 18.259 (3) ÅCell parameters from 5000 reflections
c = 22.864 (4) Åθ = 2.5–25.0°
α = 89.15 (2)°µ = 2.41 mm1
β = 87.73 (2)°T = 180 K
γ = 77.31 (2)°Block, yellow
V = 5158.1 (16) Å30.40 × 0.24 × 0.12 mm
Data collection top
Stoe IPDS
diffractometer
18050 independent reflections
Radiation source: fine-focus sealed X-ray tube15173 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
Detector resolution: 6.667 pixels mm-1θmax = 25.5°, θmin = 2.2°
φ–oscillat., φ–incr. = 1.1°, 218 exposures scansh = 1515
Absorption correction: numerical
(NUMABS32 in X-RED1.08; Stoe & Cie, 1997)
k = 2222
Tmin = 0.446, Tmax = 0.761l = 2727
47419 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.022H-atom parameters not refined
wR(F2) = 0.053 w = 1/[σ2(Fo2) + (0.0344P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.94(Δ/σ)max = 0.020
18050 reflectionsΔρmax = 0.70 e Å3
1262 parametersΔρmin = 1.27 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00038 (5)
Crystal data top
[W(CO)2(C26H24P2)2]·1.5C6H6γ = 77.31 (2)°
Mr = 1153.82V = 5158.1 (16) Å3
Triclinic, P1Z = 4
a = 12.675 (2) ÅMo Kα radiation
b = 18.259 (3) ŵ = 2.41 mm1
c = 22.864 (4) ÅT = 180 K
α = 89.15 (2)°0.40 × 0.24 × 0.12 mm
β = 87.73 (2)°
Data collection top
Stoe IPDS
diffractometer
18050 independent reflections
Absorption correction: numerical
(NUMABS32 in X-RED1.08; Stoe & Cie, 1997)
15173 reflections with I > 2σ(I)
Tmin = 0.446, Tmax = 0.761Rint = 0.034
47419 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0220 restraints
wR(F2) = 0.053H-atom parameters not refined
S = 0.94Δρmax = 0.70 e Å3
18050 reflectionsΔρmin = 1.27 e Å3
1262 parameters
Special details top

Experimental. Crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on Gaussian integration was applied. NUMABS32 is implemented in X-RED1.08 (Stoe, 1997).

Recrystallized from benzene/pentane.

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
xyzUiso*/Ueq
C10.0567 (2)0.08281 (14)0.00638 (13)0.0207 (6)
H1A0.09120.04210.02080.025*
H1B0.00540.06350.03300.025*
C20.0045 (2)0.15016 (15)0.02841 (13)0.0218 (6)
H2A0.06440.13600.04880.026*
H2B0.04510.16580.05820.026*
C30.0797 (2)0.41255 (14)0.01953 (12)0.0178 (6)
H3A0.11270.44810.00410.021*
H3B0.00730.41330.00440.021*
C40.0687 (2)0.43615 (13)0.08380 (12)0.0177 (6)
H4A0.01520.48440.08800.021*
H4B0.13910.44360.09680.021*
C50.2212 (2)0.21815 (14)0.13778 (12)0.0204 (6)
C60.0211 (2)0.20042 (14)0.15866 (13)0.0184 (6)
C70.2809 (2)0.09249 (14)0.00053 (12)0.0193 (6)
C80.3761 (2)0.10931 (16)0.01877 (13)0.0260 (7)
H80.37710.12980.05670.031*
C90.4693 (3)0.09624 (19)0.01714 (16)0.0354 (8)
H90.53360.10750.00330.042*
C100.4699 (3)0.06689 (17)0.07299 (15)0.0332 (7)
H100.53360.05900.09750.040*
C110.3770 (3)0.04948 (16)0.09217 (14)0.0294 (7)
H110.37660.02870.13000.035*
C120.2837 (2)0.06221 (15)0.05641 (13)0.0257 (7)
H120.22010.05000.07030.031*
C130.1974 (2)0.02836 (14)0.09817 (13)0.0220 (6)
C140.2278 (2)0.04351 (15)0.07374 (15)0.0295 (7)
H140.23270.04930.03240.035*
C150.2510 (3)0.10671 (17)0.11016 (18)0.0381 (9)
H150.27160.15530.09340.046*
C160.2441 (3)0.09905 (18)0.17042 (18)0.0405 (9)
H160.25910.14230.19490.049*
C170.2154 (3)0.02848 (18)0.19474 (16)0.0358 (8)
H170.21160.02300.23610.043*
C180.1919 (2)0.03520 (16)0.15853 (14)0.0281 (7)
H180.17200.08360.17560.034*
C190.2981 (2)0.34186 (14)0.02100 (13)0.0206 (6)
C200.3365 (2)0.34696 (15)0.07702 (14)0.0249 (6)
H200.29950.33090.11010.030*
C210.4286 (2)0.37544 (17)0.08486 (16)0.0322 (8)
H210.45340.37930.12310.039*
C220.4836 (3)0.39792 (17)0.03703 (17)0.0362 (8)
H220.54610.41750.04230.043*
C230.4478 (3)0.39197 (19)0.01862 (17)0.0396 (8)
H230.48640.40660.05170.048*
C240.3548 (3)0.36448 (18)0.02630 (15)0.0323 (7)
H240.33000.36130.06470.039*
C250.1674 (2)0.30082 (14)0.06597 (13)0.0209 (6)
C260.2468 (3)0.24288 (16)0.09088 (14)0.0293 (7)
H260.29940.21310.06680.035*
C270.2493 (3)0.22869 (18)0.15056 (15)0.0408 (9)
H270.30310.18880.16680.049*
C280.1745 (3)0.27201 (18)0.18664 (14)0.0414 (9)
H280.17740.26230.22740.050*
C290.0963 (3)0.32897 (18)0.16305 (14)0.0351 (8)
H290.04490.35900.18760.042*
C300.0918 (3)0.34320 (15)0.10273 (13)0.0249 (6)
H300.03640.38230.08670.030*
C310.1257 (2)0.30292 (15)0.02895 (13)0.0218 (6)
C320.1301 (3)0.29034 (18)0.08864 (14)0.0313 (7)
H320.09640.24270.10440.038*
C330.1837 (3)0.34719 (19)0.12579 (15)0.0393 (9)
H330.18530.33820.16650.047*
C340.2343 (3)0.41665 (18)0.10284 (16)0.0390 (9)
H340.27070.45530.12790.047*
C350.2316 (3)0.42948 (16)0.04326 (16)0.0323 (8)
H350.26720.47670.02750.039*
C360.1769 (2)0.37336 (15)0.00637 (14)0.0249 (7)
H360.17430.38290.03420.030*
C370.1807 (2)0.19977 (14)0.05331 (13)0.0197 (6)
C380.2846 (2)0.22993 (15)0.03403 (14)0.0261 (7)
H380.29440.26730.00420.031*
C390.3734 (2)0.20602 (17)0.05780 (16)0.0336 (8)
H390.44370.22770.04470.040*
C400.3604 (3)0.15053 (18)0.10079 (16)0.0362 (8)
H400.42140.13390.11680.043*
C410.2578 (3)0.11967 (18)0.12008 (15)0.0333 (7)
H410.24820.08130.14910.040*
C420.1693 (2)0.14455 (15)0.09729 (13)0.0244 (6)
H420.09960.12390.11160.029*
C430.1228 (2)0.40100 (15)0.14248 (12)0.0196 (6)
C440.1702 (2)0.47767 (15)0.14474 (13)0.0248 (6)
H440.12580.51320.13960.030*
C450.2808 (3)0.50274 (18)0.15430 (15)0.0350 (8)
H450.31160.55510.15550.042*
C460.3460 (3)0.45221 (19)0.16202 (15)0.0365 (8)
H460.42190.46950.16820.044*
C470.3005 (3)0.37595 (19)0.16080 (15)0.0341 (8)
H470.34540.34090.16670.041*
C480.1898 (2)0.35059 (16)0.15104 (14)0.0265 (7)
H480.15940.29820.15020.032*
C490.0672 (2)0.38774 (14)0.20284 (12)0.0182 (6)
C500.0819 (2)0.33411 (15)0.24794 (12)0.0228 (6)
H500.07640.28420.24000.027*
C510.1045 (3)0.35286 (16)0.30442 (13)0.0287 (7)
H510.11440.31580.33450.034*
C520.1126 (3)0.42533 (16)0.31644 (14)0.0300 (7)
H520.12630.43840.35500.036*
C530.1009 (3)0.47881 (16)0.27235 (14)0.0312 (8)
H530.10810.52830.28040.037*
C540.0785 (2)0.45995 (15)0.21605 (13)0.0263 (7)
H540.07080.49700.18600.032*
C550.3289 (3)0.0429 (2)0.25960 (15)0.0408 (9)
H550.25810.06810.26970.049*
C560.3534 (3)0.0336 (2)0.25133 (17)0.0478 (10)
H560.29960.06170.25650.057*
C570.4564 (4)0.0699 (2)0.23546 (18)0.0527 (11)
H570.47310.12270.22960.063*
C580.5336 (3)0.0297 (2)0.22824 (17)0.0473 (10)
H580.60400.05440.21700.057*
C590.5094 (3)0.0471 (2)0.23737 (15)0.0374 (8)
H590.56320.07520.23270.045*
C600.4077 (3)0.08256 (19)0.25310 (15)0.0352 (8)
H600.39150.13530.25960.042*
C640.0622 (2)0.06863 (13)0.51810 (12)0.0174 (6)
H64A0.00790.09150.50080.021*
H64B0.09630.02320.49540.021*
C650.0443 (2)0.04766 (14)0.58212 (12)0.0178 (6)
H65A0.11370.02060.59810.021*
H65B0.00720.01400.58490.021*
C660.0627 (2)0.40574 (14)0.50395 (13)0.0196 (6)
H66A0.01120.44320.52790.024*
H66B0.10740.43290.47900.024*
C670.0002 (2)0.36402 (15)0.46533 (13)0.0221 (6)
H67A0.05060.33430.43590.026*
H67B0.05460.40080.44420.026*
C680.0245 (2)0.30023 (14)0.64989 (13)0.0217 (6)
C690.1780 (2)0.22006 (13)0.64331 (12)0.0186 (6)
C700.2775 (2)0.06683 (14)0.53169 (12)0.0176 (6)
C710.3289 (2)0.06565 (16)0.58430 (14)0.0273 (7)
H710.30580.10560.61130.033*
C720.4146 (3)0.00592 (19)0.59785 (14)0.0350 (8)
H720.44990.00580.63370.042*
C730.4480 (2)0.05278 (17)0.55915 (15)0.0324 (8)
H730.50490.09390.56890.039*
C740.3982 (2)0.05153 (16)0.50626 (15)0.0301 (7)
H740.42180.09150.47940.036*
C750.3144 (2)0.00773 (15)0.49241 (14)0.0246 (6)
H750.28140.00840.45580.029*
C760.1744 (2)0.14707 (13)0.43603 (12)0.0173 (6)
C770.1037 (2)0.13361 (14)0.39429 (13)0.0215 (6)
H770.03730.12110.40660.026*
C780.1294 (3)0.13829 (15)0.33421 (13)0.0277 (7)
H780.08040.12910.30630.033*
C790.2251 (3)0.15604 (16)0.31569 (13)0.0301 (7)
H790.24300.15820.27510.036*
C800.2957 (3)0.17075 (16)0.35656 (14)0.0288 (7)
H800.36150.18370.34380.035*
C810.2705 (2)0.16667 (15)0.41636 (13)0.0231 (6)
H810.31910.17730.44400.028*
C820.1197 (2)0.25116 (14)0.45073 (13)0.0210 (6)
C830.1128 (2)0.26995 (16)0.39135 (13)0.0278 (7)
H830.08140.31080.37980.033*
C840.1514 (3)0.22957 (18)0.34889 (15)0.0369 (8)
H840.14540.24280.30880.044*
C850.1981 (3)0.17070 (19)0.36474 (16)0.0399 (9)
H850.22290.14250.33570.048*
C860.2089 (2)0.15275 (17)0.42388 (16)0.0328 (8)
H860.24330.11320.43520.039*
C870.1695 (2)0.19239 (15)0.46638 (14)0.0260 (7)
H870.17660.17930.50650.031*
C880.1951 (2)0.36705 (14)0.53337 (13)0.0202 (6)
C890.2944 (2)0.36600 (16)0.51039 (14)0.0273 (7)
H890.29890.32960.48180.033*
C900.3881 (3)0.41777 (17)0.52870 (16)0.0348 (8)
H900.45560.41610.51270.042*
C910.3828 (3)0.47109 (17)0.56977 (15)0.0347 (8)
H910.44620.50670.58180.042*
C920.2840 (3)0.47250 (16)0.59344 (15)0.0293 (7)
H920.27990.50930.62170.035*
C930.1915 (2)0.42066 (15)0.57620 (13)0.0238 (6)
H930.12480.42130.59350.029*
C940.1848 (2)0.40720 (14)0.60417 (13)0.0199 (6)
C950.1554 (2)0.40619 (16)0.66344 (14)0.0279 (7)
H950.12170.36780.67840.034*
C960.1749 (3)0.46077 (18)0.70117 (15)0.0346 (8)
H960.15440.45930.74150.042*
C970.2235 (3)0.51665 (17)0.68011 (16)0.0346 (8)
H970.23600.55410.70570.042*
C980.2543 (3)0.51797 (17)0.62115 (16)0.0360 (8)
H980.28810.55640.60650.043*
C990.2359 (3)0.46323 (15)0.58350 (14)0.0291 (7)
H990.25840.46410.54340.035*
C1000.2806 (2)0.31550 (13)0.51004 (13)0.0189 (6)
C1010.3709 (2)0.27392 (15)0.53816 (14)0.0251 (7)
H1010.36420.25850.57770.030*
C1020.4702 (2)0.25534 (16)0.50807 (15)0.0305 (7)
H1020.53150.22790.52750.037*
C1030.4814 (3)0.27612 (17)0.45033 (15)0.0324 (7)
H1030.54970.26250.43000.039*
C1040.3921 (2)0.31720 (16)0.42196 (14)0.0287 (7)
H1040.39910.33200.38220.034*
C1050.2926 (2)0.33646 (15)0.45204 (13)0.0242 (6)
H1050.23180.36450.43250.029*
C1060.0211 (2)0.09898 (14)0.70056 (12)0.0185 (6)
C1070.0392 (2)0.02238 (15)0.71493 (13)0.0233 (6)
H1070.03950.01320.68500.028*
C1080.0567 (2)0.00221 (16)0.77250 (14)0.0291 (7)
H1080.06870.05430.78150.035*
C1090.0565 (3)0.04919 (17)0.81662 (14)0.0297 (7)
H1090.06730.03260.85590.036*
C1100.0406 (3)0.12476 (17)0.80302 (14)0.0312 (7)
H1100.04230.16000.83290.037*
C1110.0221 (2)0.14937 (15)0.74560 (13)0.0251 (7)
H1110.00990.20160.73700.030*
C1120.1572 (2)0.13844 (15)0.62982 (12)0.0185 (6)
C1130.2295 (2)0.20760 (17)0.62562 (14)0.0286 (7)
H1130.20280.25180.61870.034*
C1140.3401 (3)0.21248 (19)0.63138 (16)0.0385 (8)
H1140.38860.26000.62820.046*
C1150.3799 (3)0.1493 (2)0.64160 (16)0.0379 (8)
H1150.45580.15300.64550.046*
C1160.3092 (2)0.07998 (18)0.64617 (14)0.0308 (7)
H1160.33650.03610.65360.037*
C1170.1991 (2)0.07481 (16)0.63996 (13)0.0249 (6)
H1170.15110.02710.64260.030*
C1180.3829 (3)0.3607 (2)0.24672 (16)0.0421 (9)
H1180.31540.36730.22850.050*
C1190.4170 (3)0.4222 (2)0.26757 (17)0.0425 (9)
H1190.37280.47110.26380.051*
C1200.5155 (3)0.4120 (2)0.29381 (17)0.0420 (9)
H1200.53940.45420.30770.050*
C1210.5789 (3)0.3412 (2)0.29997 (17)0.0428 (9)
H1210.64630.33430.31840.051*
C1220.5445 (3)0.2800 (2)0.27924 (19)0.0483 (10)
H1220.58830.23090.28350.058*
C1230.4472 (3)0.2900 (2)0.25258 (18)0.0466 (9)
H1230.42420.24780.23810.056*
C1240.4182 (6)0.3112 (3)0.1971 (3)0.103 (2)
H1240.37520.29600.16410.124*
C1250.3828 (6)0.3547 (4)0.2418 (3)0.118 (3)
H1250.31450.36770.24000.141*
C1260.4465 (5)0.3778 (3)0.2874 (3)0.0836 (17)
H1260.42320.40880.31670.100*
C1270.5429 (4)0.3582 (3)0.2927 (2)0.0693 (14)
H1270.58620.37390.32550.083*
C1280.5753 (4)0.3155 (3)0.2497 (3)0.0844 (17)
H1280.64260.30110.25230.101*
C1290.5119 (5)0.2919 (3)0.2014 (3)0.0929 (19)
H1290.53630.26200.17170.111*
O10.29683 (17)0.20155 (12)0.16661 (10)0.0333 (5)
O20.01867 (18)0.18177 (11)0.20206 (9)0.0274 (5)
O30.07439 (19)0.33201 (11)0.68894 (10)0.0328 (5)
O40.24602 (18)0.21534 (11)0.67749 (9)0.0330 (5)
P10.16134 (5)0.11139 (3)0.04946 (3)0.01610 (14)
P20.16596 (5)0.31656 (3)0.01343 (3)0.01513 (14)
P30.05951 (5)0.22916 (4)0.02246 (3)0.01666 (15)
P40.02454 (5)0.36378 (3)0.13046 (3)0.01466 (14)
P50.15145 (5)0.13630 (3)0.51568 (3)0.01438 (14)
P60.06789 (5)0.30062 (4)0.50950 (3)0.01712 (15)
P70.15107 (5)0.33925 (3)0.55260 (3)0.01510 (14)
P80.01016 (5)0.13389 (3)0.62530 (3)0.01491 (14)
W10.092175 (8)0.237475 (5)0.090426 (4)0.01303 (4)
W20.063529 (8)0.239684 (5)0.587227 (4)0.01369 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0218 (14)0.0192 (13)0.0226 (16)0.0069 (10)0.0026 (13)0.0053 (11)
C20.0208 (14)0.0253 (14)0.0207 (15)0.0072 (11)0.0040 (12)0.0019 (11)
C30.0197 (13)0.0169 (12)0.0177 (15)0.0062 (10)0.0007 (12)0.0019 (10)
C40.0195 (13)0.0144 (12)0.0196 (15)0.0049 (10)0.0010 (12)0.0022 (10)
C50.0294 (15)0.0146 (12)0.0181 (15)0.0074 (10)0.0021 (13)0.0017 (10)
C60.0232 (14)0.0139 (12)0.0193 (16)0.0055 (10)0.0043 (13)0.0030 (11)
C70.0231 (14)0.0154 (12)0.0199 (15)0.0049 (10)0.0018 (12)0.0018 (11)
C80.0247 (15)0.0325 (15)0.0220 (16)0.0078 (12)0.0041 (13)0.0053 (12)
C90.0226 (16)0.0487 (19)0.036 (2)0.0107 (14)0.0030 (15)0.0049 (15)
C100.0285 (17)0.0375 (17)0.0324 (19)0.0059 (13)0.0084 (15)0.0030 (14)
C110.0342 (17)0.0303 (15)0.0231 (17)0.0061 (13)0.0027 (14)0.0054 (13)
C120.0289 (16)0.0267 (14)0.0234 (16)0.0096 (12)0.0010 (14)0.0057 (12)
C130.0183 (14)0.0199 (13)0.0288 (17)0.0062 (10)0.0030 (13)0.0052 (11)
C140.0335 (17)0.0203 (14)0.0356 (19)0.0069 (12)0.0071 (15)0.0013 (12)
C150.0358 (18)0.0200 (15)0.060 (3)0.0083 (12)0.0117 (18)0.0071 (15)
C160.0330 (18)0.0320 (17)0.057 (3)0.0088 (13)0.0124 (18)0.0254 (16)
C170.0326 (18)0.0431 (19)0.0295 (19)0.0043 (14)0.0025 (16)0.0157 (15)
C180.0252 (15)0.0265 (15)0.0302 (18)0.0008 (12)0.0039 (14)0.0070 (13)
C190.0207 (14)0.0188 (13)0.0222 (16)0.0042 (10)0.0009 (13)0.0002 (11)
C200.0218 (15)0.0273 (14)0.0272 (17)0.0090 (11)0.0014 (13)0.0033 (12)
C210.0223 (15)0.0399 (17)0.038 (2)0.0123 (13)0.0078 (15)0.0021 (14)
C220.0234 (16)0.0355 (17)0.054 (2)0.0155 (13)0.0048 (17)0.0040 (16)
C230.0335 (18)0.049 (2)0.042 (2)0.0225 (15)0.0093 (17)0.0088 (16)
C240.0322 (17)0.0410 (18)0.0270 (18)0.0160 (14)0.0018 (15)0.0069 (14)
C250.0317 (16)0.0162 (12)0.0168 (15)0.0102 (11)0.0021 (13)0.0007 (11)
C260.0411 (18)0.0255 (15)0.0205 (16)0.0067 (13)0.0062 (15)0.0022 (12)
C270.066 (2)0.0320 (17)0.0220 (18)0.0074 (16)0.0117 (17)0.0074 (14)
C280.076 (3)0.0399 (19)0.0130 (16)0.0236 (17)0.0001 (18)0.0038 (13)
C290.052 (2)0.0356 (17)0.0213 (17)0.0173 (15)0.0071 (16)0.0046 (13)
C300.0353 (17)0.0232 (14)0.0178 (15)0.0099 (12)0.0026 (14)0.0005 (11)
C310.0189 (14)0.0263 (14)0.0231 (16)0.0104 (11)0.0080 (13)0.0060 (12)
C320.0340 (17)0.0376 (17)0.0232 (17)0.0090 (13)0.0073 (15)0.0024 (13)
C330.045 (2)0.051 (2)0.0238 (18)0.0133 (16)0.0157 (17)0.0115 (15)
C340.0396 (19)0.0384 (18)0.042 (2)0.0129 (14)0.0210 (18)0.0223 (15)
C350.0291 (16)0.0254 (15)0.045 (2)0.0098 (12)0.0121 (16)0.0103 (14)
C360.0265 (15)0.0257 (14)0.0256 (17)0.0115 (11)0.0068 (14)0.0029 (12)
C370.0197 (14)0.0193 (13)0.0219 (15)0.0073 (10)0.0015 (12)0.0043 (11)
C380.0232 (15)0.0232 (14)0.0330 (18)0.0069 (11)0.0058 (14)0.0024 (12)
C390.0212 (15)0.0329 (16)0.048 (2)0.0093 (12)0.0043 (15)0.0025 (15)
C400.0285 (17)0.0412 (18)0.044 (2)0.0196 (14)0.0055 (16)0.0016 (15)
C410.0360 (18)0.0374 (17)0.0307 (19)0.0168 (14)0.0036 (16)0.0070 (14)
C420.0217 (14)0.0280 (14)0.0258 (17)0.0099 (11)0.0057 (13)0.0029 (12)
C430.0198 (14)0.0273 (14)0.0114 (14)0.0043 (11)0.0009 (12)0.0019 (11)
C440.0243 (15)0.0243 (14)0.0244 (16)0.0032 (11)0.0027 (13)0.0026 (12)
C450.0307 (17)0.0369 (17)0.0319 (19)0.0037 (14)0.0023 (15)0.0026 (14)
C460.0213 (16)0.054 (2)0.0308 (19)0.0011 (14)0.0033 (15)0.0004 (16)
C470.0244 (16)0.0479 (19)0.033 (2)0.0152 (14)0.0017 (15)0.0007 (15)
C480.0236 (15)0.0292 (15)0.0276 (17)0.0080 (12)0.0026 (14)0.0020 (12)
C490.0158 (13)0.0210 (13)0.0172 (14)0.0020 (10)0.0013 (12)0.0045 (11)
C500.0316 (16)0.0225 (14)0.0155 (15)0.0080 (11)0.0021 (13)0.0033 (11)
C510.0408 (18)0.0299 (15)0.0160 (16)0.0083 (13)0.0051 (14)0.0011 (12)
C520.0352 (17)0.0323 (16)0.0208 (16)0.0016 (13)0.0088 (14)0.0102 (13)
C530.0394 (18)0.0220 (14)0.0314 (18)0.0025 (12)0.0114 (15)0.0085 (13)
C540.0340 (17)0.0184 (13)0.0251 (17)0.0017 (11)0.0074 (14)0.0012 (12)
C550.0304 (18)0.064 (2)0.0246 (19)0.0026 (16)0.0005 (16)0.0027 (16)
C560.052 (2)0.068 (3)0.031 (2)0.031 (2)0.0083 (19)0.0064 (18)
C570.073 (3)0.0353 (19)0.045 (2)0.0029 (18)0.015 (2)0.0018 (17)
C580.0314 (19)0.058 (2)0.042 (2)0.0119 (17)0.0049 (18)0.0015 (18)
C590.0306 (17)0.054 (2)0.0283 (19)0.0117 (15)0.0050 (16)0.0002 (16)
C600.0406 (19)0.0377 (17)0.0240 (18)0.0021 (14)0.0037 (16)0.0002 (14)
C640.0196 (13)0.0153 (12)0.0176 (14)0.0040 (10)0.0021 (12)0.0021 (10)
C650.0211 (14)0.0163 (12)0.0170 (14)0.0071 (10)0.0021 (12)0.0004 (10)
C660.0195 (14)0.0145 (12)0.0239 (16)0.0020 (10)0.0010 (12)0.0030 (11)
C670.0217 (14)0.0227 (13)0.0206 (15)0.0020 (11)0.0030 (13)0.0049 (11)
C680.0283 (15)0.0190 (13)0.0189 (15)0.0082 (11)0.0008 (13)0.0068 (11)
C690.0258 (15)0.0140 (12)0.0154 (14)0.0034 (10)0.0029 (12)0.0028 (10)
C700.0160 (13)0.0191 (13)0.0168 (14)0.0028 (10)0.0035 (12)0.0020 (11)
C710.0214 (15)0.0328 (15)0.0238 (17)0.0030 (12)0.0006 (13)0.0041 (13)
C720.0258 (16)0.0489 (19)0.0239 (17)0.0061 (14)0.0044 (14)0.0035 (14)
C730.0215 (15)0.0303 (16)0.038 (2)0.0093 (12)0.0035 (15)0.0074 (14)
C740.0283 (16)0.0224 (14)0.0351 (19)0.0028 (12)0.0067 (15)0.0015 (13)
C750.0251 (15)0.0213 (13)0.0259 (17)0.0019 (11)0.0015 (13)0.0010 (12)
C760.0228 (14)0.0108 (11)0.0160 (14)0.0011 (10)0.0011 (12)0.0007 (10)
C770.0223 (14)0.0204 (13)0.0207 (15)0.0024 (10)0.0016 (13)0.0024 (11)
C780.0361 (18)0.0257 (14)0.0199 (16)0.0031 (12)0.0060 (14)0.0019 (12)
C790.0430 (19)0.0312 (16)0.0132 (15)0.0029 (13)0.0035 (14)0.0022 (12)
C800.0295 (16)0.0302 (15)0.0253 (17)0.0053 (12)0.0070 (14)0.0025 (13)
C810.0249 (15)0.0229 (14)0.0211 (16)0.0044 (11)0.0012 (13)0.0004 (11)
C820.0181 (13)0.0198 (13)0.0229 (16)0.0015 (10)0.0058 (12)0.0040 (11)
C830.0300 (16)0.0292 (15)0.0229 (17)0.0034 (12)0.0035 (14)0.0006 (12)
C840.0386 (19)0.0427 (19)0.0253 (18)0.0019 (15)0.0106 (16)0.0066 (14)
C850.0344 (18)0.0402 (18)0.043 (2)0.0008 (14)0.0193 (17)0.0162 (16)
C860.0262 (16)0.0283 (15)0.045 (2)0.0052 (12)0.0087 (15)0.0077 (14)
C870.0224 (15)0.0247 (14)0.0289 (17)0.0008 (11)0.0038 (14)0.0013 (12)
C880.0215 (14)0.0174 (13)0.0207 (15)0.0029 (10)0.0006 (12)0.0050 (11)
C890.0257 (15)0.0238 (14)0.0310 (18)0.0018 (11)0.0043 (14)0.0021 (12)
C900.0235 (16)0.0356 (17)0.042 (2)0.0007 (13)0.0042 (15)0.0008 (15)
C910.0283 (17)0.0301 (16)0.040 (2)0.0052 (13)0.0042 (15)0.0007 (14)
C920.0323 (17)0.0216 (14)0.0320 (18)0.0027 (12)0.0037 (15)0.0037 (12)
C930.0235 (15)0.0217 (14)0.0257 (17)0.0039 (11)0.0010 (13)0.0008 (12)
C940.0223 (14)0.0164 (12)0.0212 (15)0.0044 (10)0.0030 (12)0.0025 (11)
C950.0301 (16)0.0295 (15)0.0269 (18)0.0129 (12)0.0028 (14)0.0060 (13)
C960.0389 (18)0.0427 (18)0.0253 (18)0.0156 (14)0.0052 (16)0.0153 (14)
C970.0383 (18)0.0281 (16)0.040 (2)0.0098 (13)0.0069 (16)0.0133 (14)
C980.047 (2)0.0267 (16)0.040 (2)0.0196 (14)0.0122 (17)0.0040 (14)
C990.0434 (19)0.0240 (14)0.0233 (17)0.0138 (13)0.0054 (15)0.0022 (12)
C1000.0208 (14)0.0142 (12)0.0221 (15)0.0045 (10)0.0009 (12)0.0023 (10)
C1010.0279 (16)0.0233 (14)0.0227 (16)0.0016 (11)0.0055 (13)0.0013 (12)
C1020.0220 (15)0.0295 (15)0.038 (2)0.0007 (12)0.0041 (15)0.0015 (14)
C1030.0237 (16)0.0319 (16)0.041 (2)0.0066 (12)0.0068 (15)0.0082 (14)
C1040.0310 (16)0.0303 (15)0.0244 (17)0.0074 (12)0.0058 (14)0.0003 (13)
C1050.0226 (15)0.0251 (14)0.0236 (16)0.0031 (11)0.0002 (13)0.0044 (12)
C1060.0181 (13)0.0222 (13)0.0161 (14)0.0064 (10)0.0007 (12)0.0018 (11)
C1070.0268 (15)0.0216 (13)0.0241 (16)0.0105 (11)0.0045 (13)0.0032 (11)
C1080.0314 (17)0.0268 (15)0.0314 (18)0.0110 (12)0.0084 (15)0.0119 (13)
C1090.0334 (17)0.0404 (17)0.0176 (16)0.0130 (13)0.0054 (14)0.0105 (13)
C1100.0434 (19)0.0325 (16)0.0190 (16)0.0109 (14)0.0004 (15)0.0021 (13)
C1110.0363 (17)0.0215 (14)0.0177 (15)0.0073 (12)0.0001 (14)0.0028 (11)
C1120.0185 (13)0.0267 (14)0.0105 (14)0.0053 (11)0.0012 (11)0.0004 (11)
C1130.0263 (16)0.0297 (15)0.0288 (18)0.0042 (12)0.0009 (14)0.0033 (13)
C1140.0239 (16)0.0437 (19)0.042 (2)0.0049 (14)0.0024 (16)0.0016 (16)
C1150.0193 (16)0.060 (2)0.034 (2)0.0090 (15)0.0035 (15)0.0013 (17)
C1160.0290 (17)0.0443 (18)0.0238 (17)0.0190 (14)0.0023 (14)0.0016 (14)
C1170.0268 (15)0.0286 (15)0.0204 (16)0.0088 (12)0.0009 (13)0.0028 (12)
C1180.0359 (19)0.060 (2)0.030 (2)0.0098 (16)0.0018 (17)0.0007 (17)
C1190.043 (2)0.0421 (19)0.040 (2)0.0055 (15)0.0084 (18)0.0002 (16)
C1200.042 (2)0.050 (2)0.038 (2)0.0206 (16)0.0073 (18)0.0062 (17)
C1210.0305 (18)0.060 (2)0.039 (2)0.0124 (16)0.0009 (17)0.0013 (18)
C1220.043 (2)0.044 (2)0.055 (3)0.0024 (16)0.002 (2)0.0023 (18)
C1230.052 (2)0.049 (2)0.043 (2)0.0176 (17)0.0019 (19)0.0112 (17)
C1240.120 (5)0.096 (4)0.115 (5)0.061 (4)0.063 (5)0.043 (4)
C1250.124 (5)0.121 (5)0.138 (6)0.084 (4)0.078 (5)0.053 (5)
C1260.117 (5)0.056 (3)0.086 (4)0.034 (3)0.032 (4)0.015 (3)
C1270.059 (3)0.062 (3)0.077 (4)0.011 (2)0.013 (3)0.011 (3)
C1280.054 (3)0.104 (4)0.094 (5)0.016 (3)0.005 (3)0.003 (4)
C1290.082 (4)0.108 (5)0.096 (5)0.039 (3)0.008 (4)0.028 (4)
O10.0321 (12)0.0384 (12)0.0308 (13)0.0085 (9)0.0188 (11)0.0073 (10)
O20.0380 (12)0.0298 (11)0.0173 (12)0.0155 (9)0.0055 (10)0.0034 (9)
O30.0442 (13)0.0253 (11)0.0265 (12)0.0047 (9)0.0135 (11)0.0078 (9)
O40.0388 (13)0.0332 (11)0.0254 (12)0.0016 (9)0.0150 (11)0.0031 (9)
P10.0188 (3)0.0137 (3)0.0166 (4)0.0049 (2)0.0021 (3)0.0009 (3)
P20.0192 (3)0.0145 (3)0.0125 (3)0.0056 (2)0.0001 (3)0.0008 (2)
P30.0184 (3)0.0173 (3)0.0154 (4)0.0057 (2)0.0049 (3)0.0003 (3)
P40.0178 (3)0.0138 (3)0.0127 (3)0.0041 (2)0.0007 (3)0.0009 (2)
P50.0161 (3)0.0131 (3)0.0135 (3)0.0021 (2)0.0009 (3)0.0006 (2)
P60.0180 (3)0.0162 (3)0.0166 (4)0.0023 (2)0.0013 (3)0.0001 (3)
P70.0192 (3)0.0117 (3)0.0143 (4)0.0034 (2)0.0006 (3)0.0014 (2)
P80.0186 (3)0.0133 (3)0.0133 (3)0.0044 (2)0.0006 (3)0.0001 (2)
W10.01676 (6)0.01236 (5)0.01092 (6)0.00498 (4)0.00204 (4)0.00010 (4)
W20.01794 (6)0.01075 (5)0.01221 (6)0.00287 (4)0.00012 (4)0.00031 (4)
Geometric parameters (Å, º) top
C1—C21.532 (4)C68—W21.974 (3)
C1—P11.850 (3)C69—O41.175 (3)
C2—P31.861 (3)C69—W21.945 (3)
C3—C41.530 (4)C70—C711.388 (4)
C3—P21.855 (3)C70—C751.401 (4)
C4—P41.853 (3)C70—P51.854 (3)
C5—O11.167 (3)C71—C721.401 (4)
C5—W11.961 (3)C72—C731.382 (5)
C6—O21.175 (4)C73—C741.383 (5)
C6—W11.956 (3)C74—C751.382 (4)
C7—C121.396 (4)C76—C771.395 (4)
C7—C81.398 (4)C76—C811.400 (4)
C7—P11.835 (3)C76—P51.847 (3)
C8—C91.390 (5)C77—C781.405 (4)
C9—C101.391 (5)C78—C791.372 (5)
C10—C111.375 (4)C79—C801.387 (4)
C11—C121.389 (4)C80—C811.396 (4)
C13—C181.385 (4)C82—C871.396 (4)
C13—C141.402 (4)C82—C831.399 (4)
C13—P11.853 (3)C82—P61.849 (3)
C14—C151.398 (4)C83—C841.394 (4)
C15—C161.385 (5)C84—C851.374 (5)
C16—C171.379 (5)C85—C861.395 (5)
C17—C181.402 (4)C86—C871.391 (4)
C19—C241.382 (5)C88—C891.388 (4)
C19—C201.399 (4)C88—C931.404 (4)
C19—P21.848 (3)C88—P61.860 (3)
C20—C211.398 (4)C89—C901.399 (4)
C21—C221.379 (5)C90—C911.377 (5)
C22—C231.382 (5)C91—C921.390 (4)
C23—C241.397 (5)C92—C931.383 (4)
C25—C301.394 (4)C94—C951.392 (4)
C25—C261.401 (4)C94—C991.394 (4)
C25—P21.841 (3)C94—P71.851 (3)
C26—C271.390 (4)C95—C961.396 (4)
C27—C281.385 (5)C96—C971.375 (5)
C28—C291.370 (5)C97—C981.390 (5)
C29—C301.404 (4)C98—C991.392 (4)
C31—C321.393 (4)C100—C1051.387 (4)
C31—C361.403 (4)C100—C1011.401 (4)
C31—P31.853 (3)C100—P71.845 (3)
C32—C331.404 (4)C101—C1021.387 (4)
C33—C341.390 (5)C102—C1031.379 (5)
C34—C351.389 (5)C103—C1041.391 (4)
C35—C361.397 (4)C104—C1051.389 (4)
C37—C381.398 (4)C106—C1111.393 (4)
C37—C421.402 (4)C106—C1071.403 (4)
C37—P31.846 (3)C106—P81.853 (3)
C38—C391.384 (5)C107—C1081.395 (4)
C39—C401.389 (5)C108—C1091.388 (4)
C40—C411.386 (5)C109—C1101.383 (4)
C41—C421.380 (5)C110—C1111.393 (4)
C43—C481.390 (4)C112—C1171.392 (4)
C43—C441.398 (4)C112—C1131.392 (4)
C43—P41.852 (3)C112—P81.846 (3)
C44—C451.386 (4)C113—C1141.385 (5)
C45—C461.372 (5)C114—C1151.371 (5)
C46—C471.385 (5)C115—C1161.386 (4)
C47—C481.388 (4)C116—C1171.380 (4)
C49—C541.396 (4)C118—C1231.374 (5)
C49—C501.401 (4)C118—C1191.386 (5)
C49—P41.849 (3)C119—C1201.380 (5)
C50—C511.397 (4)C120—C1211.373 (5)
C51—C521.382 (4)C121—C1221.382 (5)
C52—C531.382 (5)C122—C1231.372 (5)
C53—C541.393 (4)C124—C1291.318 (8)
C55—C601.369 (5)C124—C1251.404 (9)
C55—C561.376 (5)C125—C1261.349 (7)
C56—C571.388 (6)C126—C1271.357 (7)
C57—C581.362 (6)C127—C1281.353 (8)
C58—C591.382 (5)C128—C1291.397 (8)
C59—C601.369 (5)P1—W12.4613 (9)
C64—C651.528 (4)P2—W12.5391 (9)
C64—P51.848 (3)P3—W12.5508 (8)
C65—P81.856 (3)P4—W12.4542 (8)
C66—C671.526 (4)P5—W22.5502 (9)
C66—P71.851 (3)P6—W22.5560 (9)
C67—P61.855 (3)P7—W22.4367 (9)
C68—O31.159 (4)P8—W22.4577 (9)
C2—C1—P1109.81 (18)C97—C96—C95120.2 (3)
C1—C2—P3109.37 (19)C96—C97—C98119.6 (3)
C4—C3—P2109.13 (17)C97—C98—C99120.3 (3)
C3—C4—P4110.74 (17)C98—C99—C94120.5 (3)
O1—C5—W1175.2 (2)C105—C100—C101118.8 (3)
O2—C6—W1175.1 (2)C105—C100—P7123.4 (2)
C12—C7—C8117.6 (3)C101—C100—P7117.8 (2)
C12—C7—P1124.6 (2)C102—C101—C100119.8 (3)
C8—C7—P1117.7 (2)C103—C102—C101121.0 (3)
C9—C8—C7120.4 (3)C102—C103—C104119.6 (3)
C8—C9—C10121.0 (3)C105—C104—C103119.6 (3)
C11—C10—C9119.1 (3)C100—C105—C104121.2 (3)
C10—C11—C12120.2 (3)C111—C106—C107117.8 (3)
C11—C12—C7121.7 (3)C111—C106—P8120.2 (2)
C18—C13—C14118.8 (3)C107—C106—P8121.9 (2)
C18—C13—P1121.6 (2)C108—C107—C106120.9 (3)
C14—C13—P1119.6 (2)C109—C108—C107120.1 (3)
C15—C14—C13120.0 (3)C110—C109—C108119.6 (3)
C16—C15—C14120.5 (3)C109—C110—C111120.2 (3)
C17—C16—C15119.8 (3)C106—C111—C110121.3 (3)
C16—C17—C18120.1 (3)C117—C112—C113118.2 (3)
C13—C18—C17120.8 (3)C117—C112—P8122.0 (2)
C24—C19—C20118.3 (3)C113—C112—P8119.7 (2)
C24—C19—P2122.1 (2)C114—C113—C112120.5 (3)
C20—C19—P2119.1 (2)C115—C114—C113120.5 (3)
C21—C20—C19120.7 (3)C114—C115—C116119.8 (3)
C22—C21—C20120.0 (3)C117—C116—C115119.9 (3)
C21—C22—C23119.9 (3)C116—C117—C112121.1 (3)
C22—C23—C24120.0 (4)C123—C118—C119119.7 (3)
C19—C24—C23121.1 (3)C120—C119—C118119.8 (3)
C30—C25—C26118.0 (3)C121—C120—C119120.3 (3)
C30—C25—P2123.1 (2)C120—C121—C122119.8 (3)
C26—C25—P2118.9 (2)C123—C122—C121120.1 (3)
C27—C26—C25120.4 (3)C122—C123—C118120.4 (3)
C28—C27—C26120.8 (3)C129—C124—C125119.1 (6)
C29—C28—C27119.5 (3)C126—C125—C124119.6 (6)
C28—C29—C30120.3 (3)C125—C126—C127122.0 (6)
C25—C30—C29120.9 (3)C128—C127—C126117.7 (5)
C32—C31—C36118.8 (3)C127—C128—C129121.4 (5)
C32—C31—P3122.6 (2)C124—C129—C128120.1 (6)
C36—C31—P3118.5 (2)C7—P1—C1102.98 (13)
C31—C32—C33120.8 (3)C7—P1—C1398.97 (13)
C34—C33—C32119.8 (3)C1—P1—C1399.83 (13)
C35—C34—C33119.8 (3)C7—P1—W1120.74 (9)
C34—C35—C36120.4 (3)C1—P1—W1110.39 (9)
C35—C36—C31120.3 (3)C13—P1—W1120.71 (10)
C38—C37—C42118.0 (3)C25—P2—C19101.09 (14)
C38—C37—P3122.5 (2)C25—P2—C3101.31 (12)
C42—C37—P3119.5 (2)C19—P2—C397.66 (12)
C39—C38—C37120.9 (3)C25—P2—W1124.46 (9)
C38—C39—C40120.3 (3)C19—P2—W1121.28 (9)
C41—C40—C39119.5 (3)C3—P2—W1106.21 (10)
C42—C41—C40120.3 (3)C37—P3—C3199.22 (13)
C41—C42—C37121.0 (3)C37—P3—C2100.54 (13)
C48—C43—C44118.0 (3)C31—P3—C2101.38 (13)
C48—C43—P4118.8 (2)C37—P3—W1118.78 (9)
C44—C43—P4123.2 (2)C31—P3—W1126.42 (9)
C45—C44—C43121.1 (3)C2—P3—W1106.55 (9)
C46—C45—C44120.2 (3)C49—P4—C4397.63 (12)
C45—C46—C47119.7 (3)C49—P4—C4100.68 (12)
C46—C47—C48120.3 (3)C43—P4—C4103.80 (12)
C47—C48—C43120.8 (3)C49—P4—W1120.12 (8)
C54—C49—C50117.6 (2)C43—P4—W1120.20 (9)
C54—C49—P4122.2 (2)C4—P4—W1111.47 (9)
C50—C49—P4120.1 (2)C76—P5—C64101.57 (12)
C51—C50—C49121.1 (3)C76—P5—C7099.06 (12)
C52—C51—C50119.9 (3)C64—P5—C7096.01 (12)
C51—C52—C53120.1 (3)C76—P5—W2126.55 (8)
C52—C53—C54119.9 (3)C64—P5—W2105.40 (9)
C53—C54—C49121.4 (3)C70—P5—W2122.44 (9)
C60—C55—C56119.4 (3)C82—P6—C67100.46 (14)
C55—C56—C57120.1 (4)C82—P6—C8899.81 (12)
C58—C57—C56120.0 (4)C67—P6—C88100.76 (12)
C57—C58—C59119.8 (3)C82—P6—W2126.08 (8)
C60—C59—C58119.9 (3)C67—P6—W2107.07 (9)
C55—C60—C59120.8 (3)C88—P6—W2118.68 (9)
C65—C64—P5108.02 (17)C100—P7—C66103.15 (13)
C64—C65—P8109.74 (17)C100—P7—C9499.15 (13)
C67—C66—P7110.55 (17)C66—P7—C9499.15 (12)
C66—C67—P6111.2 (2)C100—P7—W2119.86 (8)
O3—C68—W2175.8 (2)C66—P7—W2111.28 (9)
O4—C69—W2173.7 (2)C94—P7—W2121.02 (10)
C71—C70—C75118.5 (2)C112—P8—C10697.90 (13)
C71—C70—P5122.5 (2)C112—P8—C65103.34 (12)
C75—C70—P5118.5 (2)C106—P8—C65100.96 (12)
C70—C71—C72120.4 (3)C112—P8—W2121.56 (9)
C73—C72—C71120.2 (3)C106—P8—W2119.08 (9)
C72—C73—C74119.8 (3)C65—P8—W2111.01 (9)
C75—C74—C73120.2 (3)C6—W1—C585.14 (12)
C74—C75—C70120.9 (3)C6—W1—P486.79 (7)
C77—C76—C81118.1 (3)C5—W1—P493.28 (8)
C77—C76—P5123.8 (2)C6—W1—P193.86 (7)
C81—C76—P5118.0 (2)C5—W1—P186.65 (8)
C76—C77—C78120.8 (3)P4—W1—P1179.34 (3)
C79—C78—C77120.3 (3)C6—W1—P2165.95 (7)
C78—C79—C80119.7 (3)C5—W1—P295.55 (9)
C79—C80—C81120.4 (3)P4—W1—P279.16 (3)
C80—C81—C76120.6 (3)P1—W1—P2100.19 (3)
C87—C82—C83118.0 (3)C6—W1—P393.74 (8)
C87—C82—P6118.3 (2)C5—W1—P3166.09 (7)
C83—C82—P6123.6 (2)P4—W1—P3100.51 (3)
C84—C83—C82121.0 (3)P1—W1—P379.58 (3)
C85—C84—C83120.4 (3)P2—W1—P388.89 (3)
C84—C85—C86119.4 (3)C69—W2—C6885.48 (11)
C87—C86—C85120.4 (3)C69—W2—P784.13 (9)
C86—C87—C82120.7 (3)C68—W2—P794.94 (8)
C89—C88—C93118.1 (3)C69—W2—P891.53 (9)
C89—C88—P6122.5 (2)C68—W2—P886.68 (8)
C93—C88—P6119.3 (2)P7—W2—P8175.23 (2)
C88—C89—C90120.9 (3)C69—W2—P596.46 (8)
C91—C90—C89120.2 (3)C68—W2—P5165.38 (8)
C90—C91—C92119.5 (3)P7—W2—P599.68 (3)
C93—C92—C91120.5 (3)P8—W2—P578.80 (3)
C92—C93—C88120.7 (3)C69—W2—P6163.43 (8)
C95—C94—C99118.5 (3)C68—W2—P691.79 (8)
C95—C94—P7121.4 (2)P7—W2—P679.82 (3)
C99—C94—P7120.1 (2)P8—W2—P6104.65 (3)
C94—C95—C96120.9 (3)P5—W2—P690.30 (3)
P1—C1—C2—P354.7 (2)C48—C43—P4—W125.0 (3)
P2—C3—C4—P451.8 (2)C44—C43—P4—W1156.5 (2)
C12—C7—C8—C90.3 (4)C3—C4—P4—C49159.78 (18)
P1—C7—C8—C9180.0 (2)C3—C4—P4—C4399.54 (19)
C7—C8—C9—C100.5 (5)C3—C4—P4—W131.24 (19)
C8—C9—C10—C111.2 (5)C77—C76—P5—C6424.3 (2)
C9—C10—C11—C120.9 (5)C81—C76—P5—C64152.83 (19)
C10—C11—C12—C70.1 (5)C77—C76—P5—C70122.4 (2)
C8—C7—C12—C110.5 (4)C81—C76—P5—C7054.7 (2)
P1—C7—C12—C11179.8 (2)C77—C76—P5—W295.0 (2)
C18—C13—C14—C150.6 (4)C81—C76—P5—W287.9 (2)
P1—C13—C14—C15177.4 (2)C65—C64—P5—C76174.53 (16)
C13—C14—C15—C160.0 (5)C65—C64—P5—C7073.97 (18)
C14—C15—C16—C170.8 (5)C65—C64—P5—W252.08 (17)
C15—C16—C17—C180.8 (5)C71—C70—P5—C76147.0 (3)
C14—C13—C18—C170.5 (5)C75—C70—P5—C7641.3 (3)
P1—C13—C18—C17177.5 (2)C71—C70—P5—C64110.3 (3)
C16—C17—C18—C130.2 (5)C75—C70—P5—C6461.5 (3)
C24—C19—C20—C211.1 (4)C71—C70—P5—W22.3 (3)
P2—C19—C20—C21171.5 (2)C75—C70—P5—W2174.0 (2)
C19—C20—C21—C220.9 (4)C87—C82—P6—C67174.6 (2)
C20—C21—C22—C230.3 (5)C83—C82—P6—C676.2 (3)
C21—C22—C23—C241.2 (5)C87—C82—P6—C8882.5 (2)
C20—C19—C24—C230.2 (4)C83—C82—P6—C8896.7 (2)
P2—C19—C24—C23172.2 (2)C87—C82—P6—W254.3 (2)
C22—C23—C24—C191.0 (5)C83—C82—P6—W2126.5 (2)
C30—C25—C26—C270.0 (5)C66—C67—P6—C82173.17 (18)
P2—C25—C26—C27179.0 (3)C66—C67—P6—C8884.6 (2)
C25—C26—C27—C280.9 (6)C66—C67—P6—W240.08 (19)
C26—C27—C28—C290.8 (6)C89—C88—P6—C824.2 (3)
C27—C28—C29—C300.2 (6)C93—C88—P6—C82175.7 (2)
C26—C25—C30—C291.0 (4)C89—C88—P6—C67106.9 (3)
P2—C25—C30—C29180.0 (2)C93—C88—P6—C6773.0 (2)
C28—C29—C30—C251.1 (5)C89—C88—P6—W2136.7 (2)
C36—C31—C32—C330.7 (5)C93—C88—P6—W243.4 (3)
P3—C31—C32—C33178.2 (3)C105—C100—P7—C669.2 (3)
C31—C32—C33—C340.8 (5)C101—C100—P7—C66171.0 (2)
C32—C33—C34—C350.0 (5)C105—C100—P7—C94110.9 (2)
C33—C34—C35—C361.0 (5)C101—C100—P7—C9469.3 (2)
C34—C35—C36—C311.2 (5)C105—C100—P7—W2115.1 (2)
C32—C31—C36—C350.3 (4)C101—C100—P7—W264.7 (2)
P3—C31—C36—C35177.3 (2)C67—C66—P7—C10092.2 (2)
C42—C37—C38—C390.1 (4)C67—C66—P7—C94166.1 (2)
P3—C37—C38—C39179.4 (2)C67—C66—P7—W237.6 (2)
C37—C38—C39—C401.0 (5)C95—C94—P7—C100137.1 (2)
C38—C39—C40—C410.5 (5)C99—C94—P7—C10046.0 (2)
C39—C40—C41—C420.8 (5)C95—C94—P7—C66117.8 (2)
C40—C41—C42—C371.7 (5)C99—C94—P7—C6659.0 (2)
C38—C37—C42—C411.2 (4)C95—C94—P7—W23.9 (3)
P3—C37—C42—C41178.1 (2)C99—C94—P7—W2179.30 (19)
C48—C43—C44—C451.0 (4)C117—C112—P8—C10661.8 (3)
P4—C43—C44—C45179.5 (2)C113—C112—P8—C106115.4 (2)
C43—C44—C45—C460.3 (5)C117—C112—P8—C6541.5 (3)
C44—C45—C46—C470.6 (5)C113—C112—P8—C65141.3 (2)
C45—C46—C47—C480.9 (5)C117—C112—P8—W2166.9 (2)
C46—C47—C48—C430.1 (5)C113—C112—P8—W216.0 (3)
C44—C43—C48—C470.8 (4)C111—C106—P8—C11292.9 (3)
P4—C43—C48—C47179.3 (2)C107—C106—P8—C11283.9 (3)
C54—C49—C50—C511.5 (4)C111—C106—P8—C65161.8 (2)
P4—C49—C50—C51174.2 (2)C107—C106—P8—C6521.4 (3)
C49—C50—C51—C520.0 (5)C111—C106—P8—W240.1 (3)
C50—C51—C52—C531.5 (5)C107—C106—P8—W2143.1 (2)
C51—C52—C53—C541.4 (5)C64—C65—P8—C11298.2 (2)
C52—C53—C54—C490.2 (5)C64—C65—P8—C106160.90 (18)
C50—C49—C54—C531.6 (4)C64—C65—P8—W233.7 (2)
P4—C49—C54—C53174.0 (2)O2—C6—W1—C551 (3)
C60—C55—C56—C571.2 (6)O2—C6—W1—P443 (3)
C55—C56—C57—C580.2 (6)O2—C6—W1—P1137 (3)
C56—C57—C58—C590.7 (6)O2—C6—W1—P243 (3)
C57—C58—C59—C600.6 (6)O2—C6—W1—P3143 (3)
C56—C55—C60—C591.3 (5)O1—C5—W1—C652 (3)
C58—C59—C60—C550.4 (5)O1—C5—W1—P4139 (3)
P5—C64—C65—P855.6 (2)O1—C5—W1—P142 (3)
P7—C66—C67—P650.3 (2)O1—C5—W1—P2142 (3)
C75—C70—C71—C721.0 (5)O1—C5—W1—P334 (3)
P5—C70—C71—C72170.8 (3)C49—P4—W1—C661.34 (13)
C70—C71—C72—C730.7 (5)C43—P4—W1—C659.68 (13)
C71—C72—C73—C741.6 (5)C4—P4—W1—C6178.63 (12)
C72—C73—C74—C750.9 (5)C49—P4—W1—C523.60 (14)
C73—C74—C75—C700.8 (5)C43—P4—W1—C5144.62 (14)
C71—C70—C75—C741.7 (5)C4—P4—W1—C593.69 (13)
P5—C70—C75—C74170.3 (2)C49—P4—W1—P1107 (2)
C81—C76—C77—C781.2 (4)C43—P4—W1—P1132 (2)
P5—C76—C77—C78175.93 (19)C4—P4—W1—P110 (2)
C76—C77—C78—C790.2 (4)C49—P4—W1—P2118.62 (11)
C77—C78—C79—C801.2 (4)C43—P4—W1—P2120.36 (11)
C78—C79—C80—C810.8 (4)C4—P4—W1—P21.33 (9)
C79—C80—C81—C760.6 (4)C49—P4—W1—P3154.56 (11)
C77—C76—C81—C801.5 (4)C43—P4—W1—P333.54 (11)
P5—C76—C81—C80175.7 (2)C4—P4—W1—P388.15 (9)
C87—C82—C83—C842.1 (4)C7—P1—W1—C6155.89 (12)
P6—C82—C83—C84178.7 (2)C1—P1—W1—C684.11 (13)
C82—C83—C84—C850.7 (5)C13—P1—W1—C631.53 (13)
C83—C84—C85—C861.5 (5)C7—P1—W1—C570.99 (13)
C84—C85—C86—C872.1 (5)C1—P1—W1—C5169.01 (14)
C85—C86—C87—C820.6 (4)C13—P1—W1—C553.37 (14)
C83—C82—C87—C861.4 (4)C7—P1—W1—P413 (2)
P6—C82—C87—C86179.3 (2)C1—P1—W1—P4107 (2)
C93—C88—C89—C901.1 (5)C13—P1—W1—P4137 (2)
P6—C88—C89—C90178.8 (3)C7—P1—W1—P224.05 (10)
C88—C89—C90—C910.4 (5)C1—P1—W1—P295.95 (11)
C89—C90—C91—C920.8 (5)C13—P1—W1—P2148.40 (11)
C90—C91—C92—C930.3 (5)C7—P1—W1—P3111.01 (10)
C91—C92—C93—C881.8 (5)C1—P1—W1—P38.99 (11)
C89—C88—C93—C922.1 (4)C13—P1—W1—P3124.64 (11)
P6—C88—C93—C92177.8 (2)C25—P2—W1—C6139.1 (3)
C99—C94—C95—C961.2 (4)C19—P2—W1—C687.2 (3)
P7—C94—C95—C96175.7 (2)C3—P2—W1—C622.6 (3)
C94—C95—C96—C970.1 (5)C25—P2—W1—C5128.72 (13)
C95—C96—C97—C980.7 (5)C19—P2—W1—C54.90 (12)
C96—C97—C98—C990.2 (5)C3—P2—W1—C5114.72 (12)
C97—C98—C99—C941.1 (5)C25—P2—W1—P4138.99 (11)
C95—C94—C99—C981.7 (4)C19—P2—W1—P487.39 (10)
P7—C94—C99—C98175.2 (2)C3—P2—W1—P422.43 (9)
C105—C100—C101—C1020.8 (4)C25—P2—W1—P141.14 (11)
P7—C100—C101—C102179.4 (2)C19—P2—W1—P192.48 (10)
C100—C101—C102—C1031.1 (4)C3—P2—W1—P1157.70 (9)
C101—C102—C103—C1040.9 (5)C25—P2—W1—P338.07 (11)
C102—C103—C104—C1050.3 (4)C19—P2—W1—P3171.69 (10)
C101—C100—C105—C1040.3 (4)C3—P2—W1—P378.49 (9)
P7—C100—C105—C104179.9 (2)C37—P3—W1—C63.04 (12)
C103—C104—C105—C1000.1 (4)C31—P3—W1—C6132.28 (15)
C111—C106—C107—C1080.5 (4)C2—P3—W1—C6109.35 (13)
P8—C106—C107—C108176.4 (2)C37—P3—W1—C588.0 (4)
C106—C107—C108—C1090.1 (5)C31—P3—W1—C5142.8 (4)
C107—C108—C109—C1101.0 (5)C2—P3—W1—C524.4 (4)
C108—C109—C110—C1111.6 (5)C37—P3—W1—P484.38 (10)
C107—C106—C111—C1100.2 (5)C31—P3—W1—P444.85 (13)
P8—C106—C111—C110177.1 (3)C2—P3—W1—P4163.22 (10)
C109—C110—C111—C1061.2 (5)C37—P3—W1—P196.28 (10)
C117—C112—C113—C1140.0 (4)C31—P3—W1—P1134.48 (13)
P8—C112—C113—C114177.3 (3)C2—P3—W1—P116.11 (10)
C112—C113—C114—C1150.3 (5)C37—P3—W1—P2163.14 (9)
C113—C114—C115—C1160.0 (5)C31—P3—W1—P233.91 (13)
C114—C115—C116—C1170.5 (5)C2—P3—W1—P284.46 (11)
C115—C116—C117—C1120.8 (5)O4—C69—W2—C6857 (2)
C113—C112—C117—C1160.5 (4)O4—C69—W2—P738 (2)
P8—C112—C117—C116176.6 (2)O4—C69—W2—P8144 (2)
C123—C118—C119—C1200.3 (6)O4—C69—W2—P5138 (2)
C118—C119—C120—C1210.8 (6)O4—C69—W2—P624 (3)
C119—C120—C121—C1220.7 (6)O3—C68—W2—C6952 (4)
C120—C121—C122—C1230.0 (6)O3—C68—W2—P7136 (4)
C121—C122—C123—C1180.6 (6)O3—C68—W2—P840 (4)
C119—C118—C123—C1220.4 (6)O3—C68—W2—P546 (4)
C129—C124—C125—C1262.1 (12)O3—C68—W2—P6145 (4)
C124—C125—C126—C1272.4 (11)C100—P7—W2—C6973.81 (13)
C125—C126—C127—C1281.5 (9)C66—P7—W2—C69165.86 (12)
C126—C127—C128—C1290.2 (8)C94—P7—W2—C6950.19 (12)
C125—C124—C129—C1280.9 (11)C100—P7—W2—C68158.74 (13)
C127—C128—C129—C1240.1 (10)C66—P7—W2—C6880.93 (13)
C12—C7—P1—C11.1 (3)C94—P7—W2—C6834.75 (12)
C8—C7—P1—C1179.1 (2)C100—P7—W2—P849.1 (3)
C12—C7—P1—C13101.2 (2)C66—P7—W2—P8169.5 (3)
C8—C7—P1—C1378.5 (2)C94—P7—W2—P874.8 (3)
C12—C7—P1—W1124.7 (2)C100—P7—W2—P521.77 (10)
C8—C7—P1—W155.5 (2)C66—P7—W2—P598.56 (10)
C2—C1—P1—C790.8 (2)C94—P7—W2—P5145.77 (10)
C2—C1—P1—C13167.5 (2)C100—P7—W2—P6110.33 (10)
C2—C1—P1—W139.4 (2)C66—P7—W2—P610.00 (10)
C18—C13—P1—C7130.7 (3)C94—P7—W2—P6125.68 (10)
C14—C13—P1—C751.3 (3)C112—P8—W2—C69143.71 (13)
C18—C13—P1—C1124.3 (3)C106—P8—W2—C6921.97 (13)
C14—C13—P1—C153.6 (3)C65—P8—W2—C6994.56 (12)
C18—C13—P1—W13.4 (3)C112—P8—W2—C6858.32 (13)
C14—C13—P1—W1174.59 (19)C106—P8—W2—C6863.42 (13)
C30—C25—P2—C19118.2 (3)C65—P8—W2—C68179.94 (12)
C26—C25—P2—C1962.8 (3)C112—P8—W2—P7168.2 (3)
C30—C25—P2—C318.0 (3)C106—P8—W2—P746.5 (3)
C26—C25—P2—C3163.1 (2)C65—P8—W2—P770.0 (3)
C30—C25—P2—W1100.9 (2)C112—P8—W2—P5120.00 (11)
C26—C25—P2—W178.1 (3)C106—P8—W2—P5118.26 (10)
C24—C19—P2—C2517.7 (3)C65—P8—W2—P51.73 (9)
C20—C19—P2—C25170.0 (2)C112—P8—W2—P632.65 (11)
C24—C19—P2—C385.5 (2)C106—P8—W2—P6154.39 (10)
C20—C19—P2—C386.8 (2)C65—P8—W2—P689.08 (9)
C24—C19—P2—W1160.3 (2)C76—P5—W2—C69128.37 (14)
C20—C19—P2—W127.5 (2)C64—P5—W2—C69114.04 (12)
C4—C3—P2—C25179.99 (19)C70—P5—W2—C696.35 (14)
C4—C3—P2—C1977.0 (2)C76—P5—W2—C68134.7 (3)
C4—C3—P2—W148.78 (19)C64—P5—W2—C6817.1 (3)
C38—C37—P3—C313.0 (3)C70—P5—W2—C6890.6 (3)
C42—C37—P3—C31177.8 (2)C76—P5—W2—P743.25 (11)
C38—C37—P3—C2100.6 (2)C64—P5—W2—P7160.84 (8)
C42—C37—P3—C278.7 (2)C70—P5—W2—P791.47 (11)
C38—C37—P3—W1143.8 (2)C76—P5—W2—P8141.35 (11)
C42—C37—P3—W137.0 (2)C64—P5—W2—P823.75 (8)
C32—C31—P3—C3799.6 (3)C70—P5—W2—P883.94 (11)
C36—C31—P3—C3777.9 (2)C76—P5—W2—P636.47 (11)
C32—C31—P3—C23.2 (3)C64—P5—W2—P681.12 (9)
C36—C31—P3—C2179.3 (2)C70—P5—W2—P6171.19 (11)
C32—C31—P3—W1123.8 (2)C82—P6—W2—C69145.0 (3)
C36—C31—P3—W158.7 (3)C67—P6—W2—C6927.6 (3)
C1—C2—P3—C3779.5 (2)C88—P6—W2—C6985.3 (3)
C1—C2—P3—C31178.8 (2)C82—P6—W2—C68134.92 (15)
C1—C2—P3—W145.0 (2)C67—P6—W2—C68107.77 (13)
C54—C49—P4—C4380.4 (3)C88—P6—W2—C685.21 (13)
C50—C49—P4—C4395.1 (2)C82—P6—W2—P7130.38 (13)
C54—C49—P4—C425.3 (3)C67—P6—W2—P713.08 (10)
C50—C49—P4—C4159.3 (2)C88—P6—W2—P799.91 (11)
C54—C49—P4—W1148.0 (2)C82—P6—W2—P847.89 (13)
C50—C49—P4—W136.6 (3)C67—P6—W2—P8165.19 (10)
C48—C43—P4—C49106.6 (2)C88—P6—W2—P881.82 (11)
C44—C43—P4—C4971.9 (3)C82—P6—W2—P530.60 (13)
C48—C43—P4—C4150.4 (2)C67—P6—W2—P586.70 (10)
C44—C43—P4—C431.1 (3)C88—P6—W2—P5160.31 (10)

Experimental details

Crystal data
Chemical formula[W(CO)2(C26H24P2)2]·1.5C6H6
Mr1153.82
Crystal system, space groupTriclinic, P1
Temperature (K)180
a, b, c (Å)12.675 (2), 18.259 (3), 22.864 (4)
α, β, γ (°)89.15 (2), 87.73 (2), 77.31 (2)
V3)5158.1 (16)
Z4
Radiation typeMo Kα
µ (mm1)2.41
Crystal size (mm)0.40 × 0.24 × 0.12
Data collection
DiffractometerStoe IPDS
Absorption correctionNumerical
(NUMABS32 in X-RED1.08; Stoe & Cie, 1997)
Tmin, Tmax0.446, 0.761
No. of measured, independent and
observed [I > 2σ(I)] reflections
47419, 18050, 15173
Rint0.034
(sin θ/λ)max1)0.606
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.022, 0.053, 0.94
No. of reflections18050
No. of parameters1262
H-atom treatmentH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.70, 1.27

Computer programs: IPDS2.87 (Stoe & Cie, 1997), IPDS2.87, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 1996), SHELXL97.

 

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