research communications\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 73| Part 12| December 2017| Pages 1823-1826
https://doi.org/10.1107/S2056989017015560

Crystal structure of the formal 20 electron zirconocene penta­fulvene complex Cp2Zr(η5,η1-adamantyl­­idene­penta­fulvene):toluene:n-hexane = 1:0.125:0.125

CROSSMARK_Color_square_no_text.svg
Malte Fischer,a Marc Schmidtmanna and Rüdiger Beckhausa*

aInstitut für Chemie, Fakultät für Mathematik und Naturwissenschaften, Carl von Ossietzky Universität Oldenburg, 26129 Oldenburg, Germany
*Correspondence e-mail: ruediger.beckhaus@uni-oldenburg.de

Edited by M. Weil, Vienna University of Technology, Austria (Received 12 September 2017; accepted 25 October 2017; online 3 November 2017)

The crystal structure of a solvated zirconocene penta­fulvene complex with a bulky adamantyl­idene substitution pattern, namely (η5,η1-adamantyl­idene­penta­fulvene)bis­(η5-cyclo­penta­dien­yl)zirconium(IV)–toluene–n-hexane (8/1/1), [Zr(C15H18)(C5H5)2]·0.125C7H8·0.125C6H14, is reported. Reducing zirconocene dichloride with magnesium results in the formation of a low-valent zirconocene reagent that reacts readily with adamantyl­idene­penta­fulvene to give the aforementioned complex. Single crystal X-ray diffraction proves the dianion-like η5:η1 binding mode of the fulvene ligand to the central ZrIV atom. The asymmetric unit contains four independent mol­ecules of [η5:η1-adamantyl­idene­penta­fulvene]bis­[(η5)-cyclo­penta­dien­yl]zirconium(IV), together with half a mol­ecule of toluene disordered with half a mol­ecule of n-hexane (the solvent mol­ecules have no direct influence on the complex). In each of the four complex mol­ecules, the central ZrIV atom has a distorted tetra­hedral coordination environment. The measured crystal consisted of two domains with a refined ratio of 0.77:0.23.

CCDC reference: 1582067

Similar articles

1. Chemical context

Over the last few decades, penta­fulvenes have found plenty of applications in organometallic chemistry (Preethalayam et al., 2017[Preethalayam, P., Krishnan, K. S., Thulasi, S., Chand, S. S., Joseph, J., Nair, V., Jaroschik, F. & Radhakrishnan, K. V. (2017). Chem. Rev. 117, 3930-3989.]; Neuenschwander, 1989[Neuenschwander, M. (1989). Fulvenes, vol. 2, ch. 16, pp. 1131-1268, New York: John Wiley & Sons.]), one of which is their use as versatile ligands for a variety of early and late transition metals featuring a multitude of coordination modes and reactivity patterns (Preethalayam et al., 2017[Preethalayam, P., Krishnan, K. S., Thulasi, S., Chand, S. S., Joseph, J., Nair, V., Jaroschik, F. & Radhakrishnan, K. V. (2017). Chem. Rev. 117, 3930-3989.]; Kreindlin & Rybinskaya, 2004[Kreindlin, A. Z. & Rybinskaya, M. A. (2004). Russ. Chem. Rev. 73, 417-432.]). Whereas for late transition metals η2- and η4-bindng modes are known (Kim et al., 2000[Kim, H. J., Choi, N.-S. & Lee, S. W. J. (2000). J. Organomet. Chem. 616, 67-73.]; Rais & Bergman, 2004[Rais, D. & Bergman, R. G. (2004). Chem. Eur. J. 10, 3970-3978.]), most metals are bound in an η6-manner, either in a neutral olefinic η2:η2:η2 (Konietzny et al., 2010[Konietzny, S., Finze, M. & Reiss, G. J. (2010). J. Organomet. Chem. 695, 2089-2092.]) or in a dianionic η5:η1 fashion (Ebert et al., 2014[Ebert, H., Timmermann, V., Oswald, T., Saak, W., Schmidtmann, M., Friedemann, M., Haase, D. & Beckhaus, R. (2014). Organometallics, 33, 1440-1452.]). The change of polarity at the exocyclic carbon atom of the penta­fulvene ligand, resulting from its bonding to the central metal atom, enables a multitude of insertion reactions and C—H-activation reactions that are of great inter­est to our research group (Ebert et al., 2014[Ebert, H., Timmermann, V., Oswald, T., Saak, W., Schmidtmann, M., Friedemann, M., Haase, D. & Beckhaus, R. (2014). Organometallics, 33, 1440-1452.]; Manssen et al., 2015[Manssen, M., Lauterbach, N., Dörfler, J., Schmidtmann, M., Saak, W., Doye, S. & Beckhaus, R. (2015). Angew. Chem. Int. Ed. 54, 4383-4387.], 2017[Manssen, M., Lauterbach, N., Woriescheck, T., Schmidtmann, M. & Beckhaus, R. (2017). Organometallics, 36, 867-876.]; Oswald et al., 2016[Oswald, T., Beermann, T., Saak, W. & Beckhaus, R. (2016). Z. Kristallogr. New Cryst. Struct. 232, 143-145.]) . In this context we have recently reported the syntheses of the first zirconocene-based penta­fulvene complexes and their reactivities (Jaroschik et al., 2017[Jaroschik, F., Penkhues, M., Bahlmann, B., Nicolas, E., Fischer, M., Massicot, F., Martinez, A., Harakat, D., Schmidtmann, M., Kokkuvayil Vasu, R., Vasse, J.-V. & Beckhaus, R. (2017). Organometallics, 36, 2004-2013.]). Here we report the synthesis and crystal structure of the solvated title compound, (η5,η1-adamantyl­idene­penta­fulvene)bis­(η5-cyclo­penta­dien­yl)zirconium(IV), 1.

[Scheme 1]

2. Structural commentary

Compound 1 crystallizes in the triclinic space group P[\overline{1}] with four formula units per asymmetric unit together with one disordered solvent mol­ecule (ratio toluene:n-hexane = 1:1). Fig. 1[link] shows one of the complex mol­ecules present in the crystal of 1. As a result of the high similarities with respect to structural parameters (bond lengths and angles) of the four complexes in the asymmetric unit, only this complex (Zr1) is discussed in detail. The mol­ecular structure shows the zirconium(IV) atom to be in a distorted tetra­hedral coordination environment. The zirconium atom lies 0.21 Å above the plane defined by the three centroids of the penta­fulvene and cyclo­penta­dienyl ligands, which is in good agreement with related complexes, e.g. 0.20 Å for the analogous complex with a 6,6′-di-para-tolyl­fulvene substitution pattern (Jaroschik et al., 2017[Jaroschik, F., Penkhues, M., Bahlmann, B., Nicolas, E., Fischer, M., Massicot, F., Martinez, A., Harakat, D., Schmidtmann, M., Kokkuvayil Vasu, R., Vasse, J.-V. & Beckhaus, R. (2017). Organometallics, 36, 2004-2013.]) and 0.20 Å for Cp3ZrH (Edelbach et al., 1999[Edelbach, E. L., Rahman, A. K. F., Lachicotte, R. J. & Jones, W. D. (1999). Organometallics, 18, 3170-3177.]). The mol­ecular structure of 1 in the solid state clearly confirms the π–η5:σ–η1 binding mode of the fulvene moiety to the central metal atom. Characteristic parameters for this coordination mode are the deviation (bend angle θ) of the Cexo—Cipso bond toward the central zirconium(IV) atom (29.4°) as well as the ring slippage (Δ) toward the Cipso atom of the five-membered ring of the penta­fulvene ligand (0.318 Å). The bond between the zirconium(IV) atom and the exocyclic carbon atom [Zr1—C16 = 2.605 (3) Å] is considerably longer than those of other zirconium complexes [Kraft et al., 2002[Kraft, B. M., Lachicotte, R. J. & Jones, W. D. (2002). Organometallics, 21, 727-731.] (2.37 Å); Novarino et al., 2011[Novarino, E., Guerrero Rios, I., van der Veer, S., Meetsma, A., Hessen, B. & Bouwkamp, M. W. (2011). Organometallics, 30, 92-99.] (2.37 Å)], indicating a weak Zr—Cexo contact, but in good agreement with [π–η5:σ–η1-C5H4=C(para-tol­yl)2]Zr(THF) (2.70 and 2.71 Å) reported previously by our group (Ebert et al., 2014[Ebert, H., Timmermann, V., Oswald, T., Saak, W., Schmidtmann, M., Friedemann, M., Haase, D. & Beckhaus, R. (2014). Organometallics, 33, 1440-1452.]). Regarding the fulvene moiety, the coordination to the zirconocene fragment leads to the loss of the alternating single- and double-bond pattern of free penta­fulvene. This is indicated by the narrow range of the C—C bond lengths within the five-membered ring of the fulvene ligand [1.406 (4) to 1.437 (4) Å] in comparison with free fulvene [1.327 (3) to 1.459 (2) Å] (Garcia et al., 1989[Garcia, J. G., McLaughlin, M. L. & Fronczek, F. R. (1989). Acta Cryst. C45, 1099-1100.]). Hence, the hybridization of the exocyclic carbon atom lies between sp2 and sp3, which is further confirmed by the sum of angles around the C16 carbon atom [C11—C16—C17 = 116.9 (2)°, C17—C16—C21 = 109.4 (2)°, C11—C16—C21 = 118.7 (3)° = 345°].

[Figure 1]
Figure 1
One of the four independent complex mol­ecules in the crystal structure of 1. Displacement ellipsoids are drawn at the 50% probability level. H atoms and solvent mol­ecules have been omitted for clarity.

3. Supra­molecular features

No significant supra­molecular features between the complex mol­ecules or between the complex mol­ecules and the solvent mol­ecules are observed. Hence the inter­molecular forces appear to be dominated by van der Waals inter­actions only. In the crystal structure of 1, the solvent mol­ecules are located in the voids resulting from the packing arrangements of the complex mol­ecules. Fig. 2[link] shows the packing without solvent mol­ecules and Fig. 3[link] the packing with the contribution of the solvents.

[Figure 2]
Figure 2
A view along the a axis showing the packing of mol­ecules in the crystal structure of compound 1. Solvent mol­ecules have been omitted for clarity. No significant supra­molecular features can be observed. Color code: C grey, H white, Zr plum spheres.
[Figure 3]
Figure 3
A view along the a axis showing the packing of mol­ecules in the asymmetric unit. Color code: C grey, H white, Zr plum spheres. Solvent mol­ecules are highlighted in black.

4. Synthesis and crystallization

All reactions were carried out under a dry nitro­gen atmos­phere using Schlenk techniques or in a glove box. Zirconocene dichloride was purchased from Strem Chemicals and used as received. Adamantyl­idene­penta­fulvene was prepared according to a published procedure (Miller & Bercaw, 2006[Miller, S. A. & Bercaw, J. E. (2006). Organometallics, 25, 3576-3592.]). Solvents were dried according to standard procedures over Na/K alloy with benzo­phenone as indicator and distilled under a nitro­gen atmosphere.

Zirconocene dichloride (1.000 g, 3.421 mmol), magnesium (0.083 g, 3.421 mmol) and adamantylidenefulvene (0.884 g, 3.421 mmol) were added to a Schlenk tube under argon. THF (40 ml) was added, and the reaction was stirred for 16 h at room temperature. THF was evaporated under vacuum and 40 ml of toluene were added to the crude product. After filtration, toluene was evaporated under vacuum to give 1 as a yellow solid in 81% yield.

Crystals suitable for single crystal X-ray diffraction were obtained from a saturated solution of 1 in toluene, layered with n-hexane at room temperature.

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1[link].

Table 1
Experimental details

Crystal data
Chemical formula [Zr(C15H18)(C5H5)2]·0.125C7H8·0.125C6H14
Mr 441.98
Crystal system, space group Triclinic, P[\overline{1}]
Temperature (K) 105
a, b, c (Å) 13.6751 (6), 16.0733 (7), 19.5889 (9)
α, β, γ (°) 98.6919 (18), 109.4236 (16), 90.5484 (16)
V (Å3) 4005.8 (3)
Z 8
Radiation type Mo Kα
μ (mm−1) 0.56
Crystal size (mm) 0.28 × 0.24 × 0.04
 
Data collection
Diffractometer Bruker APEXII CCD
Absorption correction Multi-scan (TWINABS; Bruker, 2013[Bruker (2013). APEX2, SAINT and TWINABS. Bruker AXS Inc., Madison, Wisconsin, USA.])
Tmin, Tmax 0.900, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections 67120, 67120, 48102
(sin θ/λ)max (Å−1) 0.746
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.110, 1.01
No. of reflections 67120
No. of parameters 1058
No. of restraints 72
H-atom treatment H-atom parameters constrained
Δρmax, Δρmin (e Å−3) 1.04, −0.91
Computer programs: APEX2 and SAINT (Bruker, 2013[Bruker (2013). APEX2, SAINT and TWINABS. Bruker AXS Inc., Madison, Wisconsin, USA.]), SHELXS2013 (Sheldrick, 2015a[Sheldrick, G. M. (2015a). Acta Cryst. A71, 3-8.]), SHELXL2014 (Sheldrick, 2015b[Sheldrick, G. M. (2015b). Acta Cryst. C71, 3-8.]), DIAMOND (Brandenburg & Putz, 2006[Brandenburg, K. & Putz, H. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) and publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

The measured crystal consisted of two domains. TWINABS was therefore used to model the absorption correction and to generate a reflection file in the HKLF5 format. The refined ratio of the two domains was 0.77:0.23. Hydrogen atoms bonded to the carbon atoms were located from difference-Fourier maps but were subsequently fixed to idealized positions using appropriate riding models with Uiso(H) = 1.2Ueq(C). Reflections (001) and (00[\overline{1}]) were obstructed from the primary beam stop and consequently omitted from the refinement. The solvent mol­ecules toluene and n-hexane were located from difference maps and refined with RIGU commands, with site occupancies fixed to 0.50 each.

Supporting information

CCDC reference: 1582067

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2056989017015560/wm5418sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989017015560/wm5418Isup2.hkl

Supporting information file. DOI: https://doi.org/10.1107/S2056989017015560/wm5418Isup3.cdx

checkCIF report


Computing details top

Data collection: APEX2 (Bruker, 2013); cell refinement: SAINT (Bruker, 2013); data reduction: SAINT (Bruker, 2013); program(s) used to solve structure: SHELXS2013 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg & Putz, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

(η5,η1-Adamantylidenepentafulvene)bis(η5-cyclopentadienyl)zirconium(IV)–toluene–n-hexane (8/1/1) top
Crystal data top
[Zr(C15H18)(C5H5)2]·0.125C7H8·0.125C6H14Z = 8
Mr = 441.98F(000) = 1844
Triclinic, P1Dx = 1.466 Mg m−3
a = 13.6751 (6) ÅMo Kα radiation, λ = 0.71073 Å
b = 16.0733 (7) ÅCell parameters from 6013 reflections
c = 19.5889 (9) Åθ = 2.2–31.9°
α = 98.6919 (18)°µ = 0.56 mm−1
β = 109.4236 (16)°T = 105 K
γ = 90.5484 (16)°Plate, yellow
V = 4005.8 (3) Å30.28 × 0.24 × 0.04 mm
Data collection top
Bruker APEXII CCD
diffractometer		67120 independent reflections
Radiation source: sealed tube48102 reflections with I > 2σ(I)
φ and ω scansθmax = 32.0°, θmin = 1.3°
Absorption correction: multi-scan
(TWINABS; Bruker, 2013)		h = −20→20
Tmin = 0.900, Tmax = 1.000k = −23→23
67120 measured reflectionsl = −29→29
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: difference Fourier map
wR(F2) = 0.110H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.040P)2 + 4.P]
where P = (Fo2 + 2Fc2)/3
67120 reflections(Δ/σ)max = 0.002
1058 parametersΔρmax = 1.04 e Å−3
72 restraintsΔρmin = −0.91 e Å−3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 2-component twin

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr10.34828 (2)0.23916 (2)0.66261 (2)0.01264 (6)
C10.4036 (2)0.11710 (19)0.7380 (2)0.0277 (7)
H10.45760.13130.78400.033*
C20.4159 (2)0.08779 (19)0.6707 (2)0.0295 (8)
H20.47990.07570.66340.035*
C30.3174 (2)0.07918 (17)0.61545 (19)0.0239 (6)
H30.30340.06450.56410.029*
C40.2435 (2)0.09648 (18)0.65087 (19)0.0236 (6)
H40.17020.09160.62760.028*
C50.2957 (2)0.12171 (19)0.72507 (19)0.0260 (7)
H50.26450.13910.76120.031*
C60.2160 (2)0.33703 (19)0.69904 (18)0.0222 (6)
H60.23470.35910.74980.027*
C70.15621 (19)0.26119 (18)0.66255 (18)0.0211 (6)
H70.12480.22440.68410.025*
C80.1513 (2)0.24974 (19)0.58924 (18)0.0232 (6)
H80.11780.20290.55270.028*
C90.2046 (2)0.3198 (2)0.57885 (19)0.0258 (6)
H90.21310.32860.53420.031*
C100.2429 (2)0.37398 (18)0.6462 (2)0.0251 (7)
H100.28050.42670.65500.030*
C110.50795 (18)0.31699 (16)0.70541 (16)0.0149 (5)
C120.45190 (19)0.35608 (17)0.64371 (16)0.0162 (5)
H120.42860.41160.64640.019*
C130.43710 (19)0.29892 (18)0.57876 (16)0.0175 (5)
H130.39930.30810.53050.021*
C140.48798 (19)0.22570 (18)0.59757 (16)0.0175 (5)
H140.49040.17690.56420.021*
C150.53463 (18)0.23734 (17)0.67431 (16)0.0158 (5)
H150.57700.19870.70130.019*
C160.48953 (19)0.32835 (18)0.77477 (16)0.0175 (5)
C170.5652 (2)0.29025 (19)0.83666 (16)0.0202 (6)
H170.58050.23260.81710.024*
C180.5207 (2)0.2850 (2)0.89840 (18)0.0282 (7)
H18A0.45530.24880.87900.034*
H18B0.57070.25950.93770.034*
C190.4996 (2)0.3735 (2)0.92980 (19)0.0327 (8)
H190.47030.36980.96980.039*
C200.4203 (2)0.4103 (2)0.86754 (18)0.0304 (7)
H20A0.35500.37400.84820.036*
H20B0.40440.46720.88680.036*
C210.4643 (2)0.41597 (19)0.80549 (17)0.0225 (6)
H210.41280.44050.76540.027*
C220.6668 (2)0.3476 (2)0.86836 (18)0.0243 (6)
H22A0.71780.32330.90800.029*
H22B0.69710.35100.82940.029*
C230.5999 (3)0.4300 (2)0.96032 (19)0.0333 (8)
H23A0.65120.40621.00030.040*
H23B0.58570.48690.98080.040*
C240.5656 (2)0.4735 (2)0.83771 (19)0.0281 (7)
H24A0.59490.47900.79860.034*
H24B0.55040.53050.85740.034*
C250.6443 (2)0.4363 (2)0.89874 (19)0.0286 (7)
H250.71010.47310.91870.034*
Zr20.33274 (2)0.74120 (2)0.66375 (2)0.01197 (5)
C260.4932 (2)0.8472 (3)0.6977 (2)0.0361 (9)
H260.50290.88910.73950.043*
C270.4365 (2)0.8540 (2)0.6258 (2)0.0276 (7)
H270.40310.90240.60940.033*
C280.4371 (2)0.7770 (2)0.58141 (18)0.0273 (7)
H280.40100.76250.53020.033*
C290.5009 (3)0.7261 (2)0.6268 (2)0.0380 (10)
H290.51880.67130.61110.046*
C300.5334 (2)0.7678 (3)0.6977 (2)0.0423 (10)
H300.57600.74640.73960.051*
C310.3605 (3)0.6196 (2)0.7418 (2)0.0377 (8)
H310.38380.63720.79340.045*
C320.4224 (3)0.6016 (2)0.6991 (3)0.0407 (10)
H320.49610.60200.71670.049*
C330.3600 (4)0.5831 (2)0.6271 (3)0.0476 (12)
H330.38280.56970.58610.057*
C340.2572 (3)0.5873 (2)0.6246 (3)0.0499 (12)
H340.19730.57800.58170.060*
C350.2586 (3)0.6076 (2)0.6958 (3)0.0417 (11)
H350.19920.61240.71060.050*
C360.22181 (19)0.83159 (16)0.70249 (15)0.0148 (5)
C370.15190 (18)0.75914 (17)0.66475 (16)0.0166 (5)
H370.12180.72260.68720.020*
C380.13525 (19)0.75110 (19)0.58924 (16)0.0194 (6)
H380.09460.70700.55240.023*
C390.1891 (2)0.81971 (18)0.57744 (16)0.0195 (5)
H390.19150.82960.53140.023*
C400.2386 (2)0.87093 (17)0.64555 (15)0.0162 (5)
H400.27700.92300.65290.019*
C410.30012 (19)0.83558 (17)0.77373 (16)0.0165 (5)
C420.3601 (2)0.92080 (19)0.80907 (17)0.0222 (6)
H420.37950.94640.77150.027*
C430.4583 (2)0.9108 (2)0.87292 (18)0.0302 (7)
H43A0.49590.96650.89500.036*
H43B0.50480.87370.85470.036*
C440.4288 (2)0.8724 (2)0.93092 (18)0.0316 (7)
H440.49320.86550.97230.038*
C450.3719 (2)0.7856 (2)0.89559 (18)0.0280 (7)
H45A0.41820.74820.87750.034*
H45B0.35320.75960.93260.034*
C460.2733 (2)0.79519 (19)0.83160 (16)0.0195 (6)
H460.23610.73870.80900.023*
C470.2898 (2)0.97955 (19)0.83913 (18)0.0265 (7)
H47A0.32711.03540.86150.032*
H47B0.22630.98770.79850.032*
C480.3582 (3)0.9296 (2)0.96019 (19)0.0323 (8)
H48A0.33930.90440.99760.039*
H48B0.39510.98530.98370.039*
C490.2023 (2)0.85360 (19)0.86180 (17)0.0226 (6)
H49A0.13770.86020.82140.027*
H49B0.18310.82810.89890.027*
C500.2600 (2)0.9406 (2)0.89689 (18)0.0266 (7)
H500.21390.97840.91590.032*
Zr30.17259 (2)0.02164 (2)0.35641 (2)0.01183 (5)
C510.2177 (3)0.15654 (19)0.3091 (2)0.0295 (7)
H510.24070.14750.26800.035*
C520.2799 (2)0.16506 (18)0.3813 (2)0.0263 (7)
H520.35350.16500.39870.032*
C530.2165 (2)0.17380 (18)0.42502 (18)0.0233 (6)
H530.23900.17690.47680.028*
C540.1140 (2)0.17722 (18)0.3784 (2)0.0243 (7)
H540.05520.18710.39340.029*
C550.1135 (2)0.16350 (19)0.3063 (2)0.0286 (7)
H550.05410.15960.26320.034*
C56−0.0062 (2)−0.0617 (2)0.3120 (2)0.0342 (9)
H56−0.0303−0.08680.26170.041*
C57−0.0243 (2)0.02045 (19)0.34153 (19)0.0242 (7)
H57−0.06460.06020.31480.029*
C580.0274 (2)0.0321 (2)0.41629 (19)0.0266 (7)
H580.02810.08160.44980.032*
C590.0777 (3)−0.0391 (2)0.4347 (2)0.0337 (8)
H590.1209−0.04620.48250.040*
C600.0545 (2)−0.09897 (19)0.3716 (2)0.0370 (10)
H600.0758−0.15510.36910.044*
C610.2692 (2)−0.06680 (17)0.30162 (17)0.0183 (6)
C620.2524 (2)−0.11713 (18)0.35200 (17)0.0202 (6)
H620.2097−0.16800.33850.024*
C630.3090 (2)−0.0795 (2)0.42394 (19)0.0248 (6)
H630.3086−0.09890.46730.030*
C640.3669 (2)−0.0073 (2)0.42099 (19)0.0249 (6)
H640.41160.03030.46190.030*
C650.3463 (2)−0.00141 (19)0.34688 (18)0.0224 (6)
H650.37830.03940.32920.027*
C660.1889 (2)−0.05370 (18)0.23524 (17)0.0196 (6)
C670.2210 (3)−0.0062 (2)0.18306 (19)0.0269 (7)
H670.26930.04350.21200.032*
C680.1258 (3)0.0237 (2)0.1271 (2)0.0364 (8)
H68A0.08980.06350.15300.044*
H68B0.14820.05380.09380.044*
C690.0517 (3)−0.0514 (3)0.0829 (2)0.0415 (9)
H69−0.0107−0.03140.04700.050*
C700.0179 (3)−0.0972 (2)0.1348 (2)0.0365 (8)
H70A−0.0307−0.14600.10630.044*
H70B−0.0188−0.05870.16100.044*
C710.1129 (2)−0.1280 (2)0.19077 (18)0.0257 (6)
H710.0901−0.15830.22440.031*
C720.2770 (3)−0.0669 (2)0.1411 (2)0.0370 (9)
H72A0.3000−0.03700.10790.044*
H72B0.3391−0.08660.17640.044*
C730.1075 (4)−0.1122 (3)0.0413 (2)0.0483 (11)
H73A0.0593−0.16100.01190.058*
H73B0.1296−0.08280.00740.058*
C740.1684 (3)−0.1886 (2)0.1486 (2)0.0331 (8)
H74A0.2301−0.20880.18380.040*
H74B0.1208−0.23810.12050.040*
C750.2020 (3)−0.1429 (2)0.0962 (2)0.0401 (9)
H750.2381−0.18230.06940.048*
Zr40.16561 (2)0.52009 (2)0.35633 (2)0.01146 (5)
C760.2956 (2)0.41870 (19)0.3221 (2)0.0279 (7)
H760.27490.39250.27220.034*
C770.2735 (2)0.38672 (19)0.3785 (2)0.0290 (7)
H770.23810.33400.37390.035*
C780.3130 (2)0.4463 (2)0.44286 (19)0.0263 (7)
H780.30610.44240.48900.032*
C790.3649 (2)0.51291 (19)0.42664 (18)0.0223 (6)
H790.40110.56100.46060.027*
C800.3538 (2)0.49636 (19)0.35210 (19)0.0241 (6)
H800.38070.53110.32650.029*
C810.2010 (3)0.65239 (19)0.30234 (18)0.0259 (7)
H810.21820.64150.25880.031*
C820.2712 (2)0.66405 (17)0.37391 (18)0.0216 (6)
H820.34470.66550.38770.026*
C830.2138 (2)0.67337 (17)0.42211 (17)0.0201 (6)
H830.24150.67820.47400.024*
C840.1083 (2)0.67435 (18)0.37968 (19)0.0237 (6)
H840.05250.68340.39810.028*
C850.0999 (2)0.65966 (19)0.30595 (19)0.0267 (7)
H850.03730.65530.26530.032*
C860.00649 (18)0.44439 (17)0.29543 (16)0.0164 (5)
C87−0.02264 (19)0.51655 (18)0.33577 (16)0.0178 (5)
H87−0.06150.56070.31500.021*
C880.0155 (2)0.5111 (2)0.41062 (17)0.0226 (6)
H880.01030.55230.44930.027*
C890.0627 (2)0.4343 (2)0.41867 (17)0.0223 (6)
H890.09450.41440.46370.027*
C900.0549 (2)0.39190 (17)0.34873 (17)0.0195 (6)
H900.07790.33730.33840.023*
C910.0358 (2)0.44995 (18)0.23175 (16)0.0194 (6)
C920.0661 (2)0.36983 (19)0.19246 (18)0.0241 (6)
H920.11390.33870.22920.029*
C930.1192 (3)0.3925 (2)0.1394 (2)0.0361 (9)
H93A0.18370.42820.16720.043*
H93B0.13830.34040.11420.043*
C940.0470 (3)0.4397 (3)0.0825 (2)0.0421 (10)
H940.08280.45440.04850.051*
C950.0195 (3)0.5201 (2)0.12220 (19)0.0365 (8)
H95A−0.02720.55150.08590.044*
H95B0.08340.55650.14990.044*
C96−0.0342 (2)0.4987 (2)0.17498 (18)0.0259 (6)
H96−0.05250.55180.20050.031*
C97−0.0340 (2)0.3136 (2)0.1473 (2)0.0322 (8)
H97A−0.01570.26110.12200.039*
H97B−0.06950.29790.18060.039*
C98−0.0529 (3)0.3835 (3)0.0383 (2)0.0464 (10)
H98A−0.10020.41380.00140.056*
H98B−0.03520.33130.01220.056*
C99−0.1345 (3)0.4425 (2)0.1305 (2)0.0351 (8)
H99A−0.17060.42850.16380.042*
H99B−0.18190.47350.09410.042*
C100−0.1066 (3)0.3612 (2)0.0908 (2)0.0380 (9)
H100−0.17140.32500.06240.046*
C1010.2208 (8)0.2642 (6)−0.0633 (9)0.050 (2)0.5
C1020.2427 (5)0.1823 (5)−0.0513 (6)0.0411 (18)0.5
H1020.22440.1372−0.09150.049*0.5
C1030.2883 (7)0.1677 (6)0.0150 (6)0.057 (2)0.5
H1030.29620.11090.02290.068*0.5
C1040.3251 (10)0.2308 (9)0.0735 (9)0.077 (4)0.5
H1040.36080.22030.12180.092*0.5
C1050.3052 (7)0.3174 (6)0.0563 (7)0.062 (3)0.5
H1050.33170.36380.09500.074*0.5
C1060.2523 (10)0.3332 (6)−0.0101 (9)0.058 (3)0.5
H1060.23760.3887−0.01980.070*0.5
C1070.1697 (15)0.2892 (17)−0.1291 (12)0.126 (7)0.5
H10F0.16290.3503−0.12130.189*0.5
H10G0.10050.2600−0.15060.189*0.5
H10H0.20920.2754−0.16240.189*0.5
C1080.2677 (9)0.2072 (9)0.1250 (9)0.107 (5)0.5
H10A0.23110.23680.15590.160*0.5
H10B0.31060.16560.15090.160*0.5
H10C0.21690.17840.07900.160*0.5
C1090.3356 (8)0.2694 (8)0.1086 (7)0.065 (3)0.5
H10D0.31550.32730.12080.078*0.5
H10E0.40890.26560.13900.078*0.5
C1100.3242 (14)0.2513 (13)0.0296 (10)0.115 (6)0.5
H11A0.38940.27040.02340.138*0.5
H11B0.31320.18960.01260.138*0.5
C1110.2397 (13)0.2919 (13)−0.0149 (9)0.092 (5)0.5
H11C0.25720.3530−0.00950.111*0.5
H11D0.17630.2840−0.00220.111*0.5
C1120.2243 (10)0.2438 (11)−0.0980 (8)0.083 (4)0.5
H11E0.28810.2525−0.11000.100*0.5
H11F0.20980.1825−0.10190.100*0.5
C1130.1355 (10)0.2802 (9)−0.1492 (6)0.046 (2)0.5
H11G0.07810.2844−0.12970.069*0.5
H11H0.11270.2437−0.19720.069*0.5
H11I0.15720.3365−0.15440.069*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.01101 (10)0.00916 (11)0.01929 (14)0.00180 (8)0.00651 (10)0.00375 (10)
C10.0270 (14)0.0175 (15)0.037 (2)0.0013 (11)0.0042 (13)0.0142 (14)
C20.0225 (13)0.0138 (14)0.061 (2)0.0082 (10)0.0222 (15)0.0144 (15)
C30.0317 (15)0.0100 (12)0.0349 (18)0.0012 (10)0.0178 (13)0.0030 (11)
C40.0185 (12)0.0142 (13)0.043 (2)−0.0006 (10)0.0150 (13)0.0071 (13)
C50.0326 (15)0.0188 (15)0.0362 (19)0.0034 (11)0.0209 (14)0.0128 (13)
C60.0154 (11)0.0207 (14)0.0286 (17)0.0068 (10)0.0069 (11)−0.0012 (12)
C70.0126 (11)0.0178 (14)0.0348 (18)0.0027 (9)0.0092 (11)0.0077 (12)
C80.0135 (11)0.0214 (15)0.0298 (17)0.0037 (10)0.0021 (11)0.0016 (13)
C90.0187 (12)0.0278 (16)0.0337 (18)0.0105 (11)0.0080 (12)0.0145 (14)
C100.0153 (11)0.0129 (13)0.048 (2)0.0046 (9)0.0106 (13)0.0084 (13)
C110.0108 (10)0.0124 (12)0.0214 (14)0.0000 (8)0.0056 (10)0.0024 (10)
C120.0142 (11)0.0112 (12)0.0247 (15)−0.0008 (8)0.0082 (10)0.0039 (10)
C130.0156 (11)0.0185 (13)0.0178 (14)−0.0023 (9)0.0046 (10)0.0033 (11)
C140.0150 (11)0.0169 (13)0.0223 (15)−0.0014 (9)0.0097 (10)0.0010 (11)
C150.0107 (10)0.0146 (12)0.0239 (15)0.0010 (8)0.0081 (10)0.0036 (11)
C160.0154 (11)0.0191 (13)0.0181 (14)0.0041 (9)0.0063 (10)0.0016 (11)
C170.0198 (12)0.0227 (15)0.0173 (14)0.0052 (10)0.0050 (11)0.0032 (11)
C180.0286 (15)0.0373 (19)0.0205 (16)0.0072 (13)0.0085 (13)0.0095 (14)
C190.0316 (16)0.048 (2)0.0198 (17)0.0105 (15)0.0118 (13)0.0015 (15)
C200.0266 (15)0.0396 (19)0.0239 (17)0.0113 (13)0.0100 (13)−0.0023 (14)
C210.0227 (13)0.0214 (15)0.0216 (16)0.0072 (11)0.0064 (11)0.0001 (12)
C220.0192 (12)0.0288 (17)0.0217 (16)0.0049 (11)0.0045 (11)−0.0005 (13)
C230.0331 (16)0.039 (2)0.0194 (17)0.0084 (14)0.0029 (13)−0.0061 (15)
C240.0315 (15)0.0203 (15)0.0277 (18)0.0040 (12)0.0071 (13)−0.0034 (13)
C250.0254 (14)0.0284 (18)0.0258 (18)0.0015 (12)0.0045 (13)−0.0049 (14)
Zr20.01016 (10)0.00995 (11)0.01683 (13)0.00053 (8)0.00541 (9)0.00342 (10)
C260.0283 (15)0.051 (2)0.0274 (19)−0.0275 (15)0.0169 (14)−0.0126 (16)
C270.0225 (13)0.0207 (15)0.048 (2)0.0009 (11)0.0193 (14)0.0150 (14)
C280.0214 (13)0.0385 (19)0.0226 (16)−0.0117 (12)0.0111 (12)−0.0015 (14)
C290.0312 (16)0.0276 (17)0.075 (3)0.0058 (13)0.040 (2)0.0155 (18)
C300.0115 (12)0.073 (3)0.050 (2)−0.0005 (15)0.0089 (14)0.038 (2)
C310.069 (3)0.0175 (15)0.033 (2)0.0068 (15)0.0220 (19)0.0119 (14)
C320.0271 (16)0.0268 (18)0.079 (3)0.0139 (13)0.0219 (19)0.029 (2)
C330.101 (4)0.0120 (15)0.056 (3)0.0115 (18)0.059 (3)0.0083 (16)
C340.054 (2)0.0108 (16)0.061 (3)−0.0111 (15)−0.013 (2)0.0071 (17)
C350.0412 (19)0.0165 (15)0.091 (4)0.0084 (13)0.048 (2)0.0222 (19)
C360.0141 (10)0.0109 (12)0.0195 (14)0.0013 (8)0.0066 (10)0.0006 (10)
C370.0109 (10)0.0165 (13)0.0222 (15)0.0016 (9)0.0062 (10)0.0014 (11)
C380.0138 (11)0.0226 (14)0.0176 (14)0.0033 (10)0.0019 (10)−0.0017 (11)
C390.0204 (12)0.0201 (14)0.0186 (14)0.0098 (10)0.0060 (11)0.0051 (11)
C400.0190 (11)0.0128 (12)0.0183 (14)0.0054 (9)0.0075 (10)0.0043 (10)
C410.0157 (11)0.0155 (13)0.0179 (14)−0.0033 (9)0.0060 (10)0.0012 (10)
C420.0256 (13)0.0209 (14)0.0188 (15)−0.0105 (11)0.0085 (11)−0.0022 (12)
C430.0242 (14)0.042 (2)0.0197 (16)−0.0152 (13)0.0050 (12)−0.0020 (14)
C440.0265 (15)0.045 (2)0.0178 (16)−0.0069 (14)0.0018 (12)0.0026 (15)
C450.0320 (15)0.0330 (18)0.0203 (16)0.0007 (13)0.0084 (13)0.0097 (14)
C460.0220 (12)0.0194 (14)0.0178 (14)−0.0039 (10)0.0078 (11)0.0025 (11)
C470.0362 (16)0.0173 (14)0.0244 (17)−0.0071 (12)0.0110 (13)−0.0031 (12)
C480.0362 (17)0.039 (2)0.0190 (17)−0.0152 (14)0.0099 (14)−0.0044 (15)
C490.0242 (13)0.0226 (15)0.0220 (16)−0.0065 (11)0.0120 (12)−0.0029 (12)
C500.0316 (15)0.0217 (16)0.0257 (17)−0.0086 (12)0.0141 (13)−0.0077 (13)
Zr30.01074 (10)0.00897 (11)0.01757 (13)0.00172 (8)0.00685 (9)0.00275 (9)
C510.0496 (19)0.0124 (14)0.036 (2)−0.0010 (12)0.0284 (17)0.0020 (13)
C520.0173 (12)0.0122 (13)0.050 (2)−0.0018 (10)0.0132 (13)0.0039 (14)
C530.0305 (14)0.0122 (13)0.0247 (17)−0.0042 (11)0.0081 (13)−0.0013 (12)
C540.0213 (13)0.0104 (13)0.047 (2)0.0022 (10)0.0197 (14)0.0032 (13)
C550.0314 (15)0.0122 (14)0.0326 (19)−0.0019 (11)−0.0032 (13)0.0073 (13)
C560.0212 (14)0.042 (2)0.039 (2)−0.0178 (13)0.0184 (14)−0.0141 (16)
C570.0123 (11)0.0239 (15)0.042 (2)0.0035 (10)0.0122 (12)0.0133 (14)
C580.0259 (14)0.0272 (16)0.0342 (19)−0.0019 (12)0.0219 (14)0.0007 (14)
C590.0302 (16)0.044 (2)0.040 (2)0.0052 (14)0.0217 (15)0.0230 (17)
C600.0292 (15)0.0121 (14)0.085 (3)0.0031 (11)0.0368 (19)0.0135 (17)
C610.0165 (11)0.0135 (12)0.0295 (16)0.0053 (9)0.0148 (11)0.0010 (11)
C620.0189 (12)0.0144 (13)0.0314 (17)0.0070 (10)0.0122 (12)0.0072 (12)
C630.0219 (13)0.0240 (15)0.0307 (18)0.0106 (11)0.0085 (12)0.0112 (13)
C640.0150 (12)0.0263 (16)0.0308 (18)0.0064 (10)0.0038 (12)0.0058 (13)
C650.0132 (11)0.0202 (14)0.0377 (19)0.0033 (10)0.0133 (12)0.0058 (13)
C660.0243 (13)0.0161 (13)0.0221 (15)0.0063 (10)0.0135 (12)0.0014 (11)
C670.0404 (17)0.0208 (15)0.0267 (17)0.0073 (12)0.0206 (14)0.0041 (13)
C680.057 (2)0.035 (2)0.0243 (18)0.0160 (16)0.0213 (17)0.0064 (15)
C690.056 (2)0.045 (2)0.0195 (18)0.0146 (18)0.0081 (17)0.0051 (16)
C700.0372 (18)0.040 (2)0.0255 (19)0.0024 (15)0.0056 (15)−0.0041 (16)
C710.0312 (15)0.0217 (15)0.0236 (16)−0.0004 (12)0.0111 (13)−0.0027 (12)
C720.057 (2)0.0297 (19)0.040 (2)0.0103 (16)0.0371 (19)0.0060 (16)
C730.080 (3)0.041 (2)0.028 (2)0.008 (2)0.026 (2)−0.0011 (18)
C740.048 (2)0.0225 (17)0.0300 (19)0.0049 (14)0.0192 (16)−0.0050 (14)
C750.065 (2)0.032 (2)0.032 (2)0.0141 (17)0.0308 (19)−0.0003 (16)
Zr40.01103 (10)0.00883 (11)0.01512 (13)0.00078 (8)0.00556 (9)0.00119 (9)
C760.0174 (12)0.0202 (15)0.042 (2)0.0051 (10)0.0097 (13)−0.0080 (14)
C770.0152 (12)0.0145 (14)0.056 (2)0.0041 (10)0.0095 (14)0.0077 (14)
C780.0182 (12)0.0272 (16)0.0357 (19)0.0060 (11)0.0073 (12)0.0160 (14)
C790.0137 (11)0.0221 (15)0.0281 (17)0.0006 (10)0.0032 (11)0.0033 (12)
C800.0142 (11)0.0229 (15)0.0384 (19)0.0026 (10)0.0136 (12)0.0037 (13)
C810.0452 (18)0.0130 (14)0.0231 (16)−0.0045 (12)0.0168 (14)0.0020 (12)
C820.0210 (12)0.0116 (13)0.0348 (18)−0.0014 (10)0.0135 (12)0.0022 (12)
C830.0232 (13)0.0134 (13)0.0212 (15)−0.0016 (10)0.0068 (11)−0.0026 (11)
C840.0202 (12)0.0118 (13)0.0387 (19)0.0015 (10)0.0114 (13)−0.0003 (12)
C850.0286 (14)0.0130 (14)0.0289 (18)−0.0022 (11)−0.0039 (13)0.0067 (13)
C860.0102 (10)0.0137 (12)0.0246 (15)−0.0031 (8)0.0051 (10)0.0029 (11)
C870.0123 (10)0.0184 (13)0.0260 (16)0.0025 (9)0.0090 (10)0.0072 (11)
C880.0195 (12)0.0271 (16)0.0270 (16)0.0031 (11)0.0149 (12)0.0054 (13)
C890.0195 (12)0.0282 (16)0.0251 (16)0.0027 (11)0.0106 (11)0.0146 (13)
C900.0167 (11)0.0134 (12)0.0319 (17)0.0002 (9)0.0108 (11)0.0080 (11)
C910.0189 (12)0.0178 (14)0.0201 (15)−0.0058 (10)0.0066 (11)−0.0009 (11)
C920.0249 (14)0.0213 (15)0.0239 (16)−0.0087 (11)0.0102 (12)−0.0069 (12)
C930.0405 (18)0.040 (2)0.0284 (19)−0.0181 (15)0.0214 (16)−0.0151 (16)
C940.059 (2)0.046 (2)0.0190 (18)−0.0270 (18)0.0164 (17)−0.0082 (16)
C950.047 (2)0.037 (2)0.0199 (17)−0.0193 (16)0.0041 (15)0.0050 (15)
C960.0285 (14)0.0235 (16)0.0192 (16)−0.0075 (12)−0.0004 (12)0.0035 (12)
C970.0335 (16)0.0238 (17)0.033 (2)−0.0135 (13)0.0094 (15)−0.0082 (15)
C980.060 (2)0.047 (2)0.0222 (19)−0.0241 (19)0.0063 (18)−0.0071 (17)
C990.0296 (16)0.036 (2)0.0288 (19)−0.0106 (14)−0.0046 (14)0.0076 (15)
C1000.0388 (18)0.036 (2)0.0271 (19)−0.0216 (15)0.0002 (15)−0.0054 (16)
C1010.041 (4)0.032 (4)0.093 (7)0.004 (3)0.044 (5)0.013 (5)
C1020.028 (3)0.020 (3)0.074 (5)0.006 (2)0.019 (3)0.000 (3)
C1030.050 (5)0.036 (5)0.071 (6)0.004 (4)0.010 (4)−0.008 (4)
C1040.066 (7)0.067 (7)0.067 (7)0.026 (5)−0.006 (6)−0.015 (5)
C1050.048 (5)0.040 (5)0.095 (7)−0.002 (4)0.034 (5)−0.017 (5)
C1060.055 (5)0.020 (4)0.107 (8)−0.008 (4)0.042 (5)0.001 (4)
C1070.090 (13)0.167 (17)0.145 (12)−0.007 (11)0.045 (9)0.083 (11)
C1080.072 (8)0.101 (11)0.146 (13)−0.006 (7)0.015 (8)0.067 (10)
C1090.038 (5)0.063 (7)0.088 (8)−0.005 (5)0.009 (5)0.023 (6)
C1100.114 (11)0.130 (15)0.104 (9)0.010 (9)0.028 (8)0.049 (9)
C1110.079 (9)0.152 (16)0.058 (7)0.031 (10)0.035 (6)0.025 (9)
C1120.052 (6)0.133 (13)0.083 (8)0.016 (7)0.045 (6)0.021 (8)
C1130.057 (6)0.048 (5)0.034 (5)−0.009 (4)0.019 (4)0.003 (4)
Geometric parameters (Å, º) top
Zr1—C112.334 (2)C51—C551.413 (4)
Zr1—C152.482 (2)C51—H510.9500
Zr1—C122.487 (2)C52—C531.401 (4)
Zr1—C32.578 (3)C52—H520.9500
Zr1—C12.601 (3)C53—C541.403 (4)
Zr1—C92.604 (3)C53—H530.9500
Zr1—C162.605 (3)C54—C551.395 (5)
Zr1—C62.613 (3)C54—H540.9500
Zr1—C52.614 (3)C55—H550.9500
Zr1—C102.615 (3)C56—C601.410 (6)
Zr1—C82.619 (3)C56—C571.418 (5)
Zr1—C22.620 (3)C56—H560.9500
Zr1—C142.620 (2)C57—C581.380 (5)
Zr1—C132.623 (3)C57—H570.9500
Zr1—C42.631 (3)C58—C591.373 (5)
Zr1—C72.653 (2)C58—H580.9500
C1—C21.397 (5)C59—C601.389 (5)
C1—C51.415 (4)C59—H590.9500
C1—H10.9500C60—H600.9500
C2—C31.409 (5)C61—C621.439 (4)
C2—H20.9500C61—C651.441 (4)
C3—C41.412 (4)C61—C661.442 (4)
C3—H30.9500C62—C631.400 (5)
C4—C51.383 (5)C62—H620.9500
C4—H40.9500C63—C641.417 (4)
C5—H50.9500C63—H630.9500
C6—C101.411 (4)C64—C651.402 (5)
C6—C71.412 (4)C64—H640.9500
C6—H60.9500C65—H650.9500
C7—C81.399 (4)C66—C711.524 (4)
C7—H70.9500C66—C671.532 (4)
C8—C91.412 (4)C67—C681.533 (5)
C8—H80.9500C67—C721.551 (4)
C9—C101.400 (5)C67—H671.0000
C9—H90.9500C68—C691.520 (5)
C10—H100.9500C68—H68A0.9900
C11—C151.437 (4)C68—H68B0.9900
C11—C121.437 (4)C69—C701.524 (5)
C11—C161.448 (4)C69—C731.546 (5)
C12—C131.406 (4)C69—H691.0000
C12—H120.9500C70—C711.537 (5)
C13—C141.408 (4)C70—H70A0.9900
C13—H130.9500C70—H70B0.9900
C14—C151.406 (4)C71—C741.547 (4)
C14—H140.9500C71—H711.0000
C15—H150.9500C72—C751.538 (5)
C16—C171.523 (4)C72—H72A0.9900
C16—C211.535 (4)C72—H72B0.9900
C17—C181.536 (4)C73—C751.522 (6)
C17—C221.547 (4)C73—H73A0.9900
C17—H171.0000C73—H73B0.9900
C18—C191.531 (5)C74—C751.528 (5)
C18—H18A0.9900C74—H74A0.9900
C18—H18B0.9900C74—H74B0.9900
C19—C231.527 (5)C75—H751.0000
C19—C201.538 (5)Zr4—C862.329 (2)
C19—H191.0000Zr4—C872.468 (2)
C20—C211.538 (4)Zr4—C902.502 (3)
C20—H20A0.9900Zr4—C832.571 (3)
C20—H20B0.9900Zr4—C912.574 (3)
C21—C241.547 (4)Zr4—C782.594 (3)
C21—H211.0000Zr4—C762.605 (3)
C22—C251.534 (4)Zr4—C882.619 (2)
C22—H22A0.9900Zr4—C812.622 (3)
C22—H22B0.9900Zr4—C772.623 (3)
C23—C251.534 (5)Zr4—C792.625 (3)
C23—H23A0.9900Zr4—C842.628 (3)
C23—H23B0.9900Zr4—C822.631 (3)
C24—C251.523 (5)Zr4—C802.632 (2)
C24—H24A0.9900Zr4—C852.633 (3)
C24—H24B0.9900Zr4—C892.643 (3)
C25—H251.0000C76—C771.402 (5)
Zr2—C362.337 (2)C76—C801.409 (4)
Zr2—C402.470 (3)C76—H760.9500
Zr2—C372.499 (2)C77—C781.404 (5)
Zr2—C342.573 (3)C77—H770.9500
Zr2—C332.600 (3)C78—C791.410 (4)
Zr2—C282.602 (3)C78—H780.9500
Zr2—C262.603 (3)C79—C801.400 (4)
Zr2—C392.606 (3)C79—H790.9500
Zr2—C412.609 (3)C80—H800.9500
Zr2—C352.612 (3)C81—C821.394 (5)
Zr2—C312.613 (3)C81—C851.413 (4)
Zr2—C302.614 (3)C81—H810.9500
Zr2—C382.628 (3)C82—C831.407 (4)
Zr2—C272.630 (3)C82—H820.9500
Zr2—C292.633 (3)C83—C841.408 (4)
Zr2—C322.641 (3)C83—H830.9500
C26—C271.385 (5)C84—C851.393 (5)
C26—C301.394 (6)C84—H840.9500
C26—H260.9500C85—H850.9500
C27—C281.402 (5)C86—C901.434 (4)
C27—H270.9500C86—C871.439 (4)
C28—C291.392 (5)C86—C911.446 (4)
C28—H280.9500C87—C881.400 (4)
C29—C301.371 (6)C87—H870.9500
C29—H290.9500C88—C891.405 (4)
C30—H300.9500C88—H880.9500
C31—C351.377 (6)C89—C901.404 (4)
C31—C321.379 (5)C89—H890.9500
C31—H310.9500C90—H900.9500
C32—C331.369 (6)C91—C961.529 (4)
C32—H320.9500C91—C921.531 (4)
C33—C341.393 (6)C92—C931.534 (4)
C33—H330.9500C92—C971.549 (4)
C34—C351.376 (6)C92—H921.0000
C34—H340.9500C93—C941.526 (6)
C35—H350.9500C93—H93A0.9900
C36—C371.437 (4)C93—H93B0.9900
C36—C411.441 (4)C94—C951.521 (5)
C36—C401.442 (4)C94—C981.545 (5)
C37—C381.405 (4)C94—H941.0000
C37—H370.9500C95—C961.527 (4)
C38—C391.410 (4)C95—H95A0.9900
C38—H380.9500C95—H95B0.9900
C39—C401.405 (4)C96—C991.548 (4)
C39—H390.9500C96—H961.0000
C40—H400.9500C97—C1001.529 (5)
C41—C461.528 (4)C97—H97A0.9900
C41—C421.531 (4)C97—H97B0.9900
C42—C431.530 (5)C98—C1001.527 (5)
C42—C471.546 (4)C98—H98A0.9900
C42—H421.0000C98—H98B0.9900
C43—C441.532 (5)C99—C1001.535 (5)
C43—H43A0.9900C99—H99A0.9900
C43—H43B0.9900C99—H99B0.9900
C44—C481.528 (5)C100—H1001.0000
C44—C451.535 (5)C101—C1061.357 (18)
C44—H441.0000C101—C1071.37 (2)
C45—C461.533 (4)C101—C1021.390 (12)
C45—H45A0.9900C102—C1031.298 (14)
C45—H45B0.9900C102—H1020.9500
C46—C491.551 (4)C103—C1041.360 (15)
C46—H461.0000C103—H1030.9500
C47—C501.535 (4)C104—C1051.488 (19)
C47—H47A0.9900C104—H1040.9500
C47—H47B0.9900C105—C1061.33 (2)
C48—C501.528 (5)C105—H1050.9500
C48—H48A0.9900C106—H1060.9500
C48—H48B0.9900C107—H10F0.9800
C49—C501.541 (4)C107—H10G0.9800
C49—H49A0.9900C107—H10H0.9800
C49—H49B0.9900C108—C1091.498 (15)
C50—H501.0000C108—H10A0.9800
Zr3—C612.332 (2)C108—H10B0.9800
Zr3—C652.471 (2)C108—H10C0.9800
Zr3—C622.495 (3)C109—C1101.49 (2)
Zr3—C532.567 (3)C109—H10D0.9900
Zr3—C662.577 (3)C109—H10E0.9900
Zr3—C562.588 (3)C110—C1111.43 (2)
Zr3—C592.597 (3)C110—H11A0.9900
Zr3—C572.610 (2)C110—H11B0.9900
Zr3—C522.612 (3)C111—C1121.64 (2)
Zr3—C582.616 (3)C111—H11C0.9900
Zr3—C642.616 (3)C111—H11D0.9900
Zr3—C602.625 (3)C112—C1131.48 (2)
Zr3—C512.627 (3)C112—H11E0.9900
Zr3—C632.634 (3)C112—H11F0.9900
Zr3—C552.646 (3)C113—H11G0.9800
Zr3—C542.650 (3)C113—H11H0.9800
C51—C521.371 (5)C113—H11I0.9800
C11—Zr1—C1534.54 (9)C62—Zr3—C52122.63 (9)
C11—Zr1—C1234.50 (9)C53—Zr3—C5231.38 (9)
C15—Zr1—C1254.73 (9)C66—Zr3—C52103.48 (10)
C11—Zr1—C3126.33 (9)C56—Zr3—C52149.13 (11)
C15—Zr1—C392.23 (9)C59—Zr3—C52130.06 (12)
C12—Zr1—C3135.13 (9)C57—Zr3—C52119.87 (9)
C11—Zr1—C198.03 (10)C61—Zr3—C58146.65 (10)
C15—Zr1—C179.87 (9)C65—Zr3—C58157.88 (11)
C12—Zr1—C1131.46 (9)C62—Zr3—C58115.14 (10)
C3—Zr1—C152.17 (11)C53—Zr3—C5881.23 (10)
C11—Zr1—C9110.83 (10)C66—Zr3—C58135.81 (10)
C15—Zr1—C9127.83 (9)C56—Zr3—C5851.37 (10)
C12—Zr1—C977.99 (9)C59—Zr3—C5830.55 (10)
C3—Zr1—C9110.24 (11)C57—Zr3—C5830.64 (10)
C1—Zr1—C9150.55 (10)C52—Zr3—C58112.24 (10)
C11—Zr1—C1633.52 (9)C61—Zr3—C6455.60 (10)
C15—Zr1—C1659.31 (8)C65—Zr3—C6431.85 (10)
C12—Zr1—C1660.17 (9)C62—Zr3—C6452.98 (10)
C3—Zr1—C16132.33 (10)C53—Zr3—C6487.56 (10)
C1—Zr1—C1683.66 (10)C66—Zr3—C6487.85 (10)
C9—Zr1—C16117.42 (10)C56—Zr3—C64137.06 (12)
C11—Zr1—C6106.60 (9)C59—Zr3—C64103.17 (11)
C15—Zr1—C6141.11 (9)C57—Zr3—C64154.31 (10)
C12—Zr1—C694.71 (9)C52—Zr3—C6473.56 (10)
C3—Zr1—C6125.77 (9)C58—Zr3—C64126.11 (11)
C1—Zr1—C6115.03 (10)C61—Zr3—C6096.13 (10)
C9—Zr1—C651.85 (10)C65—Zr3—C60122.75 (10)
C16—Zr1—C685.69 (9)C62—Zr3—C6068.12 (9)
C11—Zr1—C5125.43 (10)C53—Zr3—C60129.84 (10)
C15—Zr1—C5111.34 (9)C66—Zr3—C6095.70 (11)
C12—Zr1—C5159.73 (10)C56—Zr3—C6031.37 (12)
C3—Zr1—C551.83 (10)C59—Zr3—C6030.85 (12)
C1—Zr1—C531.50 (9)C57—Zr3—C6051.40 (10)
C9—Zr1—C5119.68 (10)C52—Zr3—C60160.80 (12)
C16—Zr1—C5100.67 (10)C58—Zr3—C6050.58 (10)
C6—Zr1—C589.99 (10)C64—Zr3—C60108.34 (11)
C11—Zr1—C1092.94 (9)C61—Zr3—C5194.79 (10)
C15—Zr1—C10123.24 (9)C65—Zr3—C5176.03 (10)
C12—Zr1—C1069.00 (8)C62—Zr3—C51127.84 (9)
C3—Zr1—C10137.93 (10)C53—Zr3—C5151.35 (10)
C1—Zr1—C10146.14 (10)C66—Zr3—C5182.54 (10)
C9—Zr1—C1031.11 (10)C56—Zr3—C51126.29 (13)
C16—Zr1—C1088.26 (9)C59—Zr3—C51146.06 (11)
C6—Zr1—C1031.31 (10)C57—Zr3—C51107.42 (10)
C5—Zr1—C10120.21 (9)C52—Zr3—C5130.34 (11)
C11—Zr1—C8141.75 (10)C58—Zr3—C51117.02 (10)
C15—Zr1—C8153.01 (10)C64—Zr3—C5194.32 (11)
C12—Zr1—C8109.33 (9)C60—Zr3—C51157.22 (12)
C3—Zr1—C886.62 (10)C61—Zr3—C6355.18 (10)
C1—Zr1—C8119.21 (10)C65—Zr3—C6352.87 (10)
C9—Zr1—C831.38 (9)C62—Zr3—C6331.52 (10)
C16—Zr1—C8136.36 (9)C53—Zr3—C63110.49 (10)
C6—Zr1—C851.55 (10)C66—Zr3—C6387.45 (10)
C5—Zr1—C888.99 (10)C56—Zr3—C63105.99 (12)
C10—Zr1—C851.39 (9)C59—Zr3—C6378.33 (10)
C11—Zr1—C298.90 (9)C57—Zr3—C63126.84 (10)
C15—Zr1—C268.29 (9)C52—Zr3—C63104.08 (10)
C12—Zr1—C2121.92 (9)C58—Zr3—C63107.37 (10)
C3—Zr1—C231.45 (10)C64—Zr3—C6331.31 (9)
C1—Zr1—C231.05 (11)C60—Zr3—C6377.23 (10)
C9—Zr1—C2141.18 (11)C51—Zr3—C63125.18 (10)
C16—Zr1—C2101.20 (10)C61—Zr3—C55119.01 (11)
C6—Zr1—C2141.32 (10)C65—Zr3—C55106.90 (10)
C5—Zr1—C251.35 (9)C62—Zr3—C55153.18 (10)
C10—Zr1—C2168.14 (9)C53—Zr3—C5551.44 (11)
C8—Zr1—C2117.29 (10)C66—Zr3—C5594.64 (10)
C11—Zr1—C1455.37 (9)C56—Zr3—C5599.36 (12)
C15—Zr1—C1431.84 (9)C59—Zr3—C55119.17 (11)
C12—Zr1—C1452.94 (9)C57—Zr3—C5576.46 (10)
C3—Zr1—C1482.72 (9)C52—Zr3—C5550.86 (10)
C1—Zr1—C1497.79 (10)C58—Zr3—C5588.63 (11)
C9—Zr1—C14103.26 (9)C64—Zr3—C55123.40 (10)
C16—Zr1—C1487.24 (8)C60—Zr3—C55127.48 (10)
C6—Zr1—C14145.34 (9)C51—Zr3—C5531.09 (10)
C5—Zr1—C14124.67 (9)C63—Zr3—C55154.65 (10)
C10—Zr1—C14114.65 (9)C61—Zr3—C54145.55 (9)
C8—Zr1—C14121.68 (10)C65—Zr3—C54119.91 (9)
C2—Zr1—C1473.34 (9)C62—Zr3—C54171.19 (10)
C11—Zr1—C1355.30 (9)C53—Zr3—C5431.14 (10)
C15—Zr1—C1352.91 (9)C66—Zr3—C54125.18 (10)
C12—Zr1—C1331.79 (9)C56—Zr3—C5499.94 (10)
C3—Zr1—C13105.38 (9)C59—Zr3—C5495.31 (10)
C1—Zr1—C13128.67 (9)C57—Zr3—C5469.09 (9)
C9—Zr1—C1375.52 (9)C52—Zr3—C5450.89 (8)
C16—Zr1—C1387.61 (9)C58—Zr3—C5467.01 (9)
C6—Zr1—C13114.57 (9)C64—Zr3—C54118.49 (10)
C5—Zr1—C13154.74 (9)C60—Zr3—C54116.25 (9)
C10—Zr1—C1383.54 (9)C51—Zr3—C5450.77 (9)
C8—Zr1—C13101.47 (9)C63—Zr3—C54140.09 (11)
C2—Zr1—C13103.79 (9)C55—Zr3—C5430.54 (11)
C14—Zr1—C1331.15 (9)C52—C51—C55108.4 (3)
C11—Zr1—C4148.27 (10)C52—C51—Zr374.22 (18)
C15—Zr1—C4119.31 (9)C55—C51—Zr375.18 (18)
C12—Zr1—C4165.27 (10)C52—C51—H51125.8
C3—Zr1—C431.43 (9)C55—C51—H51125.8
C1—Zr1—C451.37 (10)Zr3—C51—H51116.8
C9—Zr1—C4100.62 (10)C51—C52—C53108.6 (3)
C16—Zr1—C4130.95 (10)C51—C52—Zr375.44 (17)
C6—Zr1—C495.81 (9)C53—C52—Zr372.53 (16)
C5—Zr1—C430.58 (10)C51—C52—H52125.7
C10—Zr1—C4117.07 (9)C53—C52—H52125.7
C8—Zr1—C469.97 (10)Zr3—C52—H52118.2
C2—Zr1—C451.17 (9)C52—C53—C54107.5 (3)
C14—Zr1—C4114.13 (9)C52—C53—Zr376.09 (17)
C13—Zr1—C4133.51 (9)C54—C53—Zr377.70 (17)
C11—Zr1—C7137.70 (9)C52—C53—H53126.3
C15—Zr1—C7172.12 (9)C54—C53—H53126.3
C12—Zr1—C7120.17 (9)Zr3—C53—H53112.5
C3—Zr1—C795.22 (9)C55—C54—C53108.0 (3)
C1—Zr1—C7102.75 (9)C55—C54—Zr374.56 (17)
C9—Zr1—C751.36 (9)C53—C54—Zr371.16 (16)
C16—Zr1—C7113.32 (9)C55—C54—H54126.0
C6—Zr1—C731.10 (9)C53—C54—H54126.0
C5—Zr1—C771.72 (9)Zr3—C54—H54120.1
C10—Zr1—C751.17 (9)C54—C55—C51107.3 (3)
C8—Zr1—C730.76 (10)C54—C55—Zr374.90 (18)
C2—Zr1—C7117.66 (9)C51—C55—Zr373.74 (19)
C14—Zr1—C7152.20 (10)C54—C55—H55126.3
C13—Zr1—C7126.86 (9)C51—C55—H55126.3
C4—Zr1—C767.17 (9)Zr3—C55—H55117.1
C2—C1—C5107.4 (3)C60—C56—C57106.8 (3)
C2—C1—Zr175.22 (18)C60—C56—Zr375.73 (17)
C5—C1—Zr174.78 (18)C57—C56—Zr375.00 (16)
C2—C1—H1126.3C60—C56—H56126.6
C5—C1—H1126.3C57—C56—H56126.6
Zr1—C1—H1115.9Zr3—C56—H56115.1
C1—C2—C3108.5 (3)C58—C57—C56107.4 (3)
C1—C2—Zr173.73 (17)C58—C57—Zr374.91 (15)
C3—C2—Zr172.64 (16)C56—C57—Zr373.34 (15)
C1—C2—H2125.8C58—C57—H57126.3
C3—C2—H2125.8C56—C57—H57126.3
Zr1—C2—H2119.7Zr3—C57—H57117.5
C2—C3—C4107.0 (3)C59—C58—C57109.5 (3)
C2—C3—Zr175.91 (17)C59—C58—Zr373.97 (16)
C4—C3—Zr176.36 (16)C57—C58—Zr374.45 (15)
C2—C3—H3126.5C59—C58—H58125.3
C4—C3—H3126.5C57—C58—H58125.3
Zr1—C3—H3113.8Zr3—C58—H58118.1
C5—C4—C3108.6 (3)C58—C59—C60108.3 (3)
C5—C4—Zr174.04 (17)C58—C59—Zr375.48 (17)
C3—C4—Zr172.21 (15)C60—C59—Zr375.68 (18)
C5—C4—H4125.7C58—C59—H59125.9
C3—C4—H4125.7C60—C59—H59125.9
Zr1—C4—H4119.8Zr3—C59—H59115.2
C4—C5—C1108.3 (3)C59—C60—C56107.9 (3)
C4—C5—Zr175.38 (17)C59—C60—Zr373.47 (17)
C1—C5—Zr173.72 (17)C56—C60—Zr372.90 (17)
C4—C5—H5125.9C59—C60—H60126.0
C1—C5—H5125.9C56—C60—H60126.0
Zr1—C5—H5117.0Zr3—C60—H60119.5
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C11—C12—H12125.5C68—C67—H67109.6
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C11—C15—H15125.5C71—C70—H70B109.6
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C18—C17—H17109.6C67—C72—H72B109.8
C22—C17—H17109.6H72A—C72—H72B108.3
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C17—C18—H18A109.7C69—C73—H73A109.8
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C20—C19—H19109.6H74A—C74—H74B108.2
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C21—C20—H20B109.6C73—C75—H75109.5
C19—C20—H20B109.6C74—C75—H75109.5
H20A—C20—H20B108.2C72—C75—H75109.5
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C17—C22—H22B109.7C86—Zr4—C78118.07 (10)
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C25—C23—H23A109.8C91—Zr4—C78125.61 (10)
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C21—C24—H24A109.7C78—Zr4—C7651.81 (11)
C25—C24—H24B109.7C86—Zr4—C8855.31 (10)
C21—C24—H24B109.7C87—Zr4—C8831.78 (9)
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C30—C26—H26126.1C85—C81—H81126.0
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C26—C27—H27125.9C81—C82—H82126.0
C28—C27—H27125.9C83—C82—H82126.0
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C29—C28—C27106.9 (3)C82—C83—C84107.8 (3)
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C27—C28—H28126.6C84—C83—H83126.1
Zr2—C28—H28114.5Zr4—C83—H83113.2
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C30—C29—H29125.6C85—C84—H84126.0
C28—C29—H29125.6C83—C84—H84126.0
Zr2—C29—H29118.9Zr4—C84—H84119.0
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C29—C30—H30125.9C84—C85—H85126.0
C26—C30—H30125.9C81—C85—H85126.0
Zr2—C30—H30116.5Zr4—C85—H85117.6
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C35—C31—Zr274.7 (2)C90—C86—C91123.6 (2)
C32—C31—Zr275.9 (2)C87—C86—C91122.2 (3)
C35—C31—H31126.3C90—C86—Zr479.46 (15)
C32—C31—H31126.3C87—C86—Zr477.95 (15)
Zr2—C31—H31115.4C91—C86—Zr482.42 (15)
C33—C32—C31108.7 (3)C88—C87—C86109.0 (3)
C33—C32—Zr273.2 (2)C88—C87—Zr480.04 (15)
C31—C32—Zr273.68 (19)C86—C87—Zr467.31 (13)
C33—C32—H32125.7C88—C87—H87125.5
C31—C32—H32125.7C86—C87—H87125.5
Zr2—C32—H32119.2Zr4—C87—H87118.7
C32—C33—C34107.8 (3)C87—C88—C89108.2 (3)
C32—C33—Zr276.5 (2)C87—C88—Zr468.18 (14)
C34—C33—Zr273.3 (2)C89—C88—Zr475.48 (15)
C32—C33—H33126.1C87—C88—H88125.9
C34—C33—H33126.1C89—C88—H88125.9
Zr2—C33—H33116.2Zr4—C88—H88122.1
C35—C34—C33107.4 (4)C90—C89—C88108.3 (3)
C35—C34—Zr276.2 (2)C90—C89—Zr468.67 (15)
C33—C34—Zr275.4 (2)C88—C89—Zr473.56 (15)
C35—C34—H34126.3C90—C89—H89125.8
C33—C34—H34126.3C88—C89—H89125.8
Zr2—C34—H34114.5Zr4—C89—H89123.5
C34—C35—C31108.6 (3)C89—C90—C86108.9 (2)
C34—C35—Zr273.1 (2)C89—C90—Zr479.80 (16)
C31—C35—Zr274.76 (19)C86—C90—Zr466.23 (14)
C34—C35—H35125.7C89—C90—H90125.6
C31—C35—H35125.7C86—C90—H90125.6
Zr2—C35—H35118.3Zr4—C90—H90119.9
C37—C36—C41124.0 (3)C86—C91—C96116.4 (2)
C37—C36—C40105.3 (2)C86—C91—C92118.5 (3)
C41—C36—C40122.2 (2)C96—C91—C92109.5 (3)
C37—C36—Zr278.98 (14)C86—C91—Zr463.74 (15)
C41—C36—Zr283.75 (15)C96—C91—Zr4123.97 (19)
C40—C36—Zr277.67 (14)C92—C91—Zr4118.07 (19)
C38—C37—C36109.0 (2)C91—C92—C93110.1 (3)
C38—C37—Zr279.23 (14)C91—C92—C97108.7 (2)
C36—C37—Zr266.65 (13)C93—C92—C97108.3 (3)
C38—C37—H37125.5C91—C92—H92109.9
C36—C37—H37125.5C93—C92—H92109.9
Zr2—C37—H37120.1C97—C92—H92109.9
C37—C38—C39108.3 (3)C94—C93—C92110.6 (3)
C37—C38—Zr269.08 (14)C94—C93—H93A109.5
C39—C38—Zr273.52 (15)C92—C93—H93A109.5
C37—C38—H38125.9C94—C93—H93B109.5
C39—C38—H38125.9C92—C93—H93B109.5
Zr2—C38—H38123.2H93A—C93—H93B108.1
C40—C39—C38108.2 (3)C95—C94—C93108.7 (3)
C40—C39—Zr268.67 (15)C95—C94—C98109.7 (3)
C38—C39—Zr275.23 (16)C93—C94—C98109.4 (3)
C40—C39—H39125.9C95—C94—H94109.6
C38—C39—H39125.9C93—C94—H94109.6
Zr2—C39—H39121.8C98—C94—H94109.6
C39—C40—C36108.9 (2)C94—C95—C96110.2 (3)
C39—C40—Zr279.35 (16)C94—C95—H95A109.6
C36—C40—Zr267.57 (14)C96—C95—H95A109.6
C39—C40—H40125.5C94—C95—H95B109.6
C36—C40—H40125.5C96—C95—H95B109.6
Zr2—C40—H40119.2H95A—C95—H95B108.1
C36—C41—C46118.4 (2)C95—C96—C91111.0 (3)
C36—C41—C42116.8 (2)C95—C96—C99108.7 (3)
C46—C41—C42109.7 (2)C91—C96—C99108.3 (3)
C36—C41—Zr262.95 (14)C95—C96—H96109.6
C46—C41—Zr2120.21 (18)C91—C96—H96109.6
C42—C41—Zr2121.86 (16)C99—C96—H96109.6
C43—C42—C41111.0 (3)C100—C97—C92109.8 (3)
C43—C42—C47108.4 (3)C100—C97—H97A109.7
C41—C42—C47108.7 (2)C92—C97—H97A109.7
C43—C42—H42109.6C100—C97—H97B109.7
C41—C42—H42109.6C92—C97—H97B109.7
C47—C42—H42109.6H97A—C97—H97B108.2
C42—C43—C44109.7 (2)C100—C98—C94109.2 (3)
C42—C43—H43A109.7C100—C98—H98A109.8
C44—C43—H43A109.7C94—C98—H98A109.8
C42—C43—H43B109.7C100—C98—H98B109.8
C44—C43—H43B109.7C94—C98—H98B109.8
H43A—C43—H43B108.2H98A—C98—H98B108.3
C48—C44—C43110.2 (3)C100—C99—C96109.6 (3)
C48—C44—C45109.7 (3)C100—C99—H99A109.7
C43—C44—C45108.7 (3)C96—C99—H99A109.7
C48—C44—H44109.4C100—C99—H99B109.7
C43—C44—H44109.4C96—C99—H99B109.7
C45—C44—H44109.4H99A—C99—H99B108.2
C46—C45—C44109.9 (3)C98—C100—C97109.8 (3)
C46—C45—H45A109.7C98—C100—C99109.4 (3)
C44—C45—H45A109.7C97—C100—C99109.4 (3)
C46—C45—H45B109.7C98—C100—H100109.4
C44—C45—H45B109.7C97—C100—H100109.4
H45A—C45—H45B108.2C99—C100—H100109.4
C41—C46—C45110.7 (2)C106—C101—C107109.2 (14)
C41—C46—C49108.4 (2)C106—C101—C102123.9 (14)
C45—C46—C49108.4 (3)C107—C101—C102126.8 (17)
C41—C46—H46109.8C103—C102—C101119.8 (10)
C45—C46—H46109.8C103—C102—H102120.1
C49—C46—H46109.8C101—C102—H102120.1
C50—C47—C42109.7 (3)C102—C103—C104122.4 (11)
C50—C47—H47A109.7C102—C103—H103118.8
C42—C47—H47A109.7C104—C103—H103118.8
C50—C47—H47B109.7C103—C104—C105115.0 (14)
C42—C47—H47B109.7C103—C104—H104122.5
H47A—C47—H47B108.2C105—C104—H104122.5
C50—C48—C44109.4 (3)C106—C105—C104123.4 (11)
C50—C48—H48A109.8C106—C105—H105118.3
C44—C48—H48A109.8C104—C105—H105118.3
C50—C48—H48B109.8C105—C106—C101115.1 (11)
C44—C48—H48B109.8C105—C106—H106122.4
H48A—C48—H48B108.2C101—C106—H106122.4
C50—C49—C46109.6 (2)C101—C107—H10F109.5
C50—C49—H49A109.7C101—C107—H10G109.5
C46—C49—H49A109.7H10F—C107—H10G109.5
C50—C49—H49B109.7C101—C107—H10H109.5
C46—C49—H49B109.7H10F—C107—H10H109.5
H49A—C49—H49B108.2H10G—C107—H10H109.5
C48—C50—C47109.5 (3)C109—C108—H10A109.5
C48—C50—C49109.2 (3)C109—C108—H10B109.5
C47—C50—C49109.4 (3)H10A—C108—H10B109.5
C48—C50—H50109.6C109—C108—H10C109.5
C47—C50—H50109.6H10A—C108—H10C109.5
C49—C50—H50109.6H10B—C108—H10C109.5
C61—Zr3—C6534.77 (10)C110—C109—C108109.6 (13)
C61—Zr3—C6234.46 (10)C110—C109—H10D109.7
C65—Zr3—C6254.74 (9)C108—C109—H10D109.7
C61—Zr3—C53129.88 (9)C110—C109—H10E109.7
C65—Zr3—C5396.00 (9)C108—C109—H10E109.7
C62—Zr3—C53140.09 (10)H10D—C109—H10E108.2
C61—Zr3—C6633.70 (10)C111—C110—C109112.4 (15)
C65—Zr3—C6660.12 (10)C111—C110—H11A109.1
C62—Zr3—C6659.95 (10)C109—C110—H11A109.1
C53—Zr3—C66133.08 (9)C111—C110—H11B109.1
C61—Zr3—C56102.48 (10)C109—C110—H11B109.1
C65—Zr3—C56137.01 (10)H11A—C110—H11B107.9
C62—Zr3—C5687.42 (11)C110—C111—C112102.9 (14)
C53—Zr3—C56126.91 (10)C110—C111—H11C111.2
C66—Zr3—C5684.74 (10)C112—C111—H11C111.2
C61—Zr3—C59119.11 (11)C110—C111—H11D111.2
C65—Zr3—C59131.17 (11)C112—C111—H11D111.2
C62—Zr3—C5985.40 (10)H11C—C111—H11D109.1
C53—Zr3—C59100.06 (11)C113—C112—C111107.4 (11)
C66—Zr3—C59126.39 (11)C113—C112—H11E110.2
C56—Zr3—C5951.76 (12)C111—C112—H11E110.2
C61—Zr3—C57133.05 (10)C113—C112—H11F110.2
C65—Zr3—C57167.57 (10)C111—C112—H11F110.2
C62—Zr3—C57117.43 (9)H11E—C112—H11F108.5
C53—Zr3—C5795.31 (10)C112—C113—H11G109.5
C66—Zr3—C57108.03 (10)C112—C113—H11H109.5
C56—Zr3—C5731.66 (10)H11G—C113—H11H109.5
C59—Zr3—C5751.17 (11)C112—C113—H11I109.5
C61—Zr3—C52100.23 (9)H11G—C113—H11I109.5
C65—Zr3—C5269.21 (9)H11H—C113—H11I109.5
C5—C1—C2—C33.6 (3)C52—C53—C54—C554.9 (3)
Zr1—C1—C2—C3−64.8 (2)Zr3—C53—C54—C55−66.0 (2)
C5—C1—C2—Zr168.4 (2)C52—C53—C54—Zr370.9 (2)
C1—C2—C3—C4−5.1 (3)C53—C54—C55—C51−3.4 (3)
Zr1—C2—C3—C4−70.7 (2)Zr3—C54—C55—C51−67.2 (2)
C1—C2—C3—Zr165.6 (2)C53—C54—C55—Zr363.8 (2)
C2—C3—C4—C54.7 (3)C52—C51—C55—C540.5 (4)
Zr1—C3—C4—C5−65.6 (2)Zr3—C51—C55—C5467.9 (2)
C2—C3—C4—Zr170.4 (2)C52—C51—C55—Zr3−67.4 (2)
C3—C4—C5—C1−2.5 (3)C60—C56—C57—C581.9 (3)
Zr1—C4—C5—C1−67.0 (2)Zr3—C56—C57—C58−67.75 (19)
C3—C4—C5—Zr164.4 (2)C60—C56—C57—Zr369.68 (19)
C2—C1—C5—C4−0.7 (3)C56—C57—C58—C590.4 (3)
Zr1—C1—C5—C468.1 (2)Zr3—C57—C58—C59−66.3 (2)
C2—C1—C5—Zr1−68.7 (2)C56—C57—C58—Zr366.69 (18)
C10—C6—C7—C83.0 (3)C57—C58—C59—C60−2.6 (3)
Zr1—C6—C7—C8−65.35 (19)Zr3—C58—C59—C60−69.2 (2)
C10—C6—C7—Zr168.39 (18)C57—C58—C59—Zr366.6 (2)
C6—C7—C8—C9−2.1 (3)C58—C59—C60—C563.8 (3)
Zr1—C7—C8—C9−67.22 (19)Zr3—C59—C60—C56−65.3 (2)
C6—C7—C8—Zr165.09 (19)C58—C59—C60—Zr369.1 (2)
C7—C8—C9—C100.4 (3)C57—C56—C60—C59−3.5 (3)
Zr1—C8—C9—C10−68.36 (19)Zr3—C56—C60—C5965.6 (2)
C7—C8—C9—Zr168.7 (2)C57—C56—C60—Zr3−69.17 (18)
C8—C9—C10—C61.5 (3)C65—C61—C62—C635.2 (3)
Zr1—C9—C10—C6−66.8 (2)C66—C61—C62—C63−142.3 (3)
C8—C9—C10—Zr168.37 (19)Zr3—C61—C62—C63−68.98 (19)
C7—C6—C10—C9−2.8 (3)C65—C61—C62—Zr374.18 (16)
Zr1—C6—C10—C966.66 (19)C66—C61—C62—Zr3−73.3 (2)
C7—C6—C10—Zr1−69.49 (19)C61—C62—C63—C64−3.0 (3)
C15—C11—C12—C135.4 (3)Zr3—C62—C63—C64−63.5 (2)
C16—C11—C12—C13−142.9 (3)C61—C62—C63—Zr360.50 (17)
Zr1—C11—C12—C13−69.05 (17)C62—C63—C64—C65−0.6 (3)
C15—C11—C12—Zr174.44 (16)Zr3—C63—C64—C65−60.95 (19)
C16—C11—C12—Zr1−73.8 (2)C62—C63—C64—Zr360.38 (19)
C11—C12—C13—C14−3.4 (3)C63—C64—C65—C613.9 (3)
Zr1—C12—C13—C14−64.32 (18)Zr3—C64—C65—C61−61.37 (17)
C11—C12—C13—Zr160.92 (16)C63—C64—C65—Zr365.3 (2)
C12—C13—C14—C15−0.1 (3)C62—C61—C65—C64−5.6 (3)
Zr1—C13—C14—C15−60.85 (17)C66—C61—C65—C64142.2 (3)
C12—C13—C14—Zr160.76 (17)Zr3—C61—C65—C6469.4 (2)
C13—C14—C15—C113.5 (3)C62—C61—C65—Zr3−74.98 (16)
Zr1—C14—C15—C11−61.09 (16)C66—C61—C65—Zr372.8 (2)
C13—C14—C15—Zr164.62 (17)C62—C61—C66—C71−39.4 (4)
C12—C11—C15—C14−5.5 (3)C65—C61—C66—C71178.7 (2)
C16—C11—C15—C14144.0 (2)Zr3—C61—C66—C71−110.9 (2)
Zr1—C11—C15—C1469.13 (18)C62—C61—C66—C67−173.9 (2)
C12—C11—C15—Zr1−74.59 (16)C65—C61—C66—C6744.2 (4)
C16—C11—C15—Zr174.8 (2)Zr3—C61—C66—C67114.6 (2)
C15—C11—C16—C1743.8 (4)C62—C61—C66—Zr371.5 (2)
C12—C11—C16—C17−172.9 (2)C65—C61—C66—Zr3−70.4 (2)
Zr1—C11—C16—C17115.8 (2)C61—C66—C67—C68−164.5 (3)
C15—C11—C16—C21178.4 (2)C71—C66—C67—C6857.4 (3)
C12—C11—C16—C21−38.3 (4)Zr3—C66—C67—C68−89.6 (3)
Zr1—C11—C16—C21−109.6 (2)C61—C66—C67—C7276.2 (3)
C15—C11—C16—Zr1−72.1 (2)C71—C66—C67—C72−62.0 (3)
C12—C11—C16—Zr171.3 (2)Zr3—C66—C67—C72151.0 (2)
C11—C16—C17—C18−164.1 (3)C66—C67—C68—C69−58.8 (3)
C21—C16—C17—C1857.3 (3)C72—C67—C68—C6960.4 (4)
Zr1—C16—C17—C18−90.2 (3)C67—C68—C69—C7059.2 (4)
C11—C16—C17—C2276.6 (3)C67—C68—C69—C73−60.5 (4)
C21—C16—C17—C22−61.9 (3)C68—C69—C70—C71−59.6 (4)
Zr1—C16—C17—C22150.59 (18)C73—C69—C70—C7160.1 (4)
C16—C17—C18—C19−60.0 (3)C61—C66—C71—C70165.1 (2)
C22—C17—C18—C1959.0 (3)C67—C66—C71—C70−57.2 (3)
C17—C18—C19—C23−59.6 (4)Zr3—C66—C71—C7090.9 (3)
C17—C18—C19—C2060.3 (3)C61—C66—C71—C74−76.0 (3)
C23—C19—C20—C2159.9 (3)C67—C66—C71—C7461.7 (3)
C18—C19—C20—C21−60.4 (4)Zr3—C66—C71—C74−150.2 (2)
C11—C16—C21—C20165.5 (2)C69—C70—C71—C6659.2 (3)
C17—C16—C21—C20−56.9 (3)C69—C70—C71—C74−59.7 (4)
Zr1—C16—C21—C2092.4 (3)C66—C67—C72—C7560.9 (4)
C11—C16—C21—C24−76.0 (3)C68—C67—C72—C75−59.9 (4)
C17—C16—C21—C2461.7 (3)C68—C69—C73—C7560.1 (4)
Zr1—C16—C21—C24−149.0 (2)C70—C69—C73—C75−59.5 (4)
C19—C20—C21—C1659.3 (3)C66—C71—C74—C75−60.9 (4)
C19—C20—C21—C24−59.7 (3)C70—C71—C74—C7559.1 (4)
C16—C17—C22—C2560.6 (3)C69—C73—C75—C7459.6 (4)
C18—C17—C22—C25−60.2 (3)C69—C73—C75—C72−60.1 (4)
C18—C19—C23—C2559.9 (4)C71—C74—C75—C73−59.9 (4)
C20—C19—C23—C25−59.1 (3)C71—C74—C75—C7260.1 (4)
C16—C21—C24—C25−59.8 (3)C67—C72—C75—C7360.3 (4)
C20—C21—C24—C2560.3 (3)C67—C72—C75—C74−60.1 (4)
C21—C24—C25—C23−60.8 (3)C80—C76—C77—C783.1 (3)
C21—C24—C25—C2258.6 (3)Zr4—C76—C77—C78−65.7 (2)
C19—C23—C25—C2459.9 (4)C80—C76—C77—Zr468.8 (2)
C19—C23—C25—C22−60.0 (4)C76—C77—C78—C79−3.3 (3)
C17—C22—C25—C24−59.2 (3)Zr4—C77—C78—C79−69.4 (2)
C17—C22—C25—C2360.7 (3)C76—C77—C78—Zr466.1 (2)
C30—C26—C27—C283.0 (3)C77—C78—C79—C802.4 (3)
Zr2—C26—C27—C28−65.75 (19)Zr4—C78—C79—C80−67.0 (2)
C30—C26—C27—Zr268.7 (2)C77—C78—C79—Zr469.4 (2)
C26—C27—C28—C29−4.1 (3)C78—C79—C80—C76−0.5 (3)
Zr2—C27—C28—C29−70.00 (19)Zr4—C79—C80—C76−66.35 (19)
C26—C27—C28—Zr265.91 (19)C78—C79—C80—Zr465.88 (19)
C27—C28—C29—C303.7 (3)C77—C76—C80—C79−1.6 (3)
Zr2—C28—C29—C30−66.1 (2)Zr4—C76—C80—C7967.0 (2)
C27—C28—C29—Zr269.80 (19)C77—C76—C80—Zr4−68.6 (2)
C28—C29—C30—C26−1.9 (3)C85—C81—C82—C833.6 (3)
Zr2—C29—C30—C26−67.5 (2)Zr4—C81—C82—C83−64.6 (2)
C28—C29—C30—Zr265.6 (2)C85—C81—C82—Zr468.1 (2)
C27—C26—C30—C29−0.7 (3)C81—C82—C83—C84−4.8 (3)
Zr2—C26—C30—C2968.6 (2)Zr4—C82—C83—C84−70.89 (19)
C27—C26—C30—Zr2−69.24 (19)C81—C82—C83—Zr466.1 (2)
C35—C31—C32—C333.2 (4)C82—C83—C84—C854.2 (3)
Zr2—C31—C32—C33−65.4 (3)Zr4—C83—C84—C85−66.8 (2)
C35—C31—C32—Zr268.6 (2)C82—C83—C84—Zr470.98 (19)
C31—C32—C33—C34−1.6 (4)C83—C84—C85—C81−2.0 (3)
Zr2—C32—C33—C34−67.2 (3)Zr4—C84—C85—C81−67.0 (2)
C31—C32—C33—Zr265.7 (2)C83—C84—C85—Zr464.9 (2)
C32—C33—C34—C35−0.7 (4)C82—C81—C85—C84−1.0 (4)
Zr2—C33—C34—C35−70.1 (2)Zr4—C81—C85—C8467.3 (2)
C32—C33—C34—Zr269.4 (3)C82—C81—C85—Zr4−68.2 (2)
C33—C34—C35—C312.7 (4)C90—C86—C87—C885.4 (3)
Zr2—C34—C35—C31−66.9 (2)C91—C86—C87—C88−142.9 (3)
C33—C34—C35—Zr269.6 (3)Zr4—C86—C87—C88−70.01 (19)
C32—C31—C35—C34−3.7 (4)C90—C86—C87—Zr475.38 (16)
Zr2—C31—C35—C3465.8 (2)C91—C86—C87—Zr4−72.9 (2)
C32—C31—C35—Zr2−69.4 (2)C86—C87—C88—C89−3.7 (3)
C41—C36—C37—C38−143.3 (2)Zr4—C87—C88—C89−65.40 (19)
C40—C36—C37—C385.1 (3)C86—C87—C88—Zr461.68 (16)
Zr2—C36—C37—C38−68.67 (19)C87—C88—C89—C900.5 (3)
C41—C36—C37—Zr2−74.6 (2)Zr4—C88—C89—C90−60.19 (18)
C40—C36—C37—Zr273.81 (16)C87—C88—C89—Zr460.69 (18)
C36—C37—C38—C39−3.0 (3)C88—C89—C90—C862.9 (3)
Zr2—C37—C38—C39−63.50 (19)Zr4—C89—C90—C86−60.38 (16)
C36—C37—C38—Zr260.52 (17)C88—C89—C90—Zr463.30 (19)
C37—C38—C39—C40−0.5 (3)C87—C86—C90—C89−5.0 (3)
Zr2—C38—C39—C40−61.15 (18)C91—C86—C90—C89142.7 (3)
C37—C38—C39—Zr260.66 (18)Zr4—C86—C90—C8969.21 (19)
C38—C39—C40—C363.8 (3)C87—C86—C90—Zr4−74.26 (16)
Zr2—C39—C40—C36−61.64 (17)C91—C86—C90—Zr473.5 (2)
C38—C39—C40—Zr265.41 (19)C90—C86—C91—C96171.3 (2)
C37—C36—C40—C39−5.4 (3)C87—C86—C91—C96−46.2 (4)
C41—C36—C40—C39143.7 (2)Zr4—C86—C91—C96−116.8 (2)
Zr2—C36—C40—C3969.33 (18)C90—C86—C91—C9237.3 (4)
C37—C36—C40—Zr2−74.77 (17)C87—C86—C91—C92179.8 (2)
C41—C36—C40—Zr274.4 (2)Zr4—C86—C91—C92109.2 (2)
C37—C36—C41—C46−39.3 (4)C90—C86—C91—Zr4−71.9 (2)
C40—C36—C41—C46177.4 (2)C87—C86—C91—Zr470.6 (2)
Zr2—C36—C41—C46−111.5 (2)C86—C91—C92—C93−166.3 (3)
C37—C36—C41—C42−173.9 (2)C96—C91—C92—C9356.8 (3)
C40—C36—C41—C4242.8 (3)Zr4—C91—C92—C93−92.6 (3)
Zr2—C36—C41—C42113.9 (2)C86—C91—C92—C9775.3 (3)
C37—C36—C41—Zr272.2 (2)C96—C91—C92—C97−61.6 (3)
C40—C36—C41—Zr2−71.2 (2)Zr4—C91—C92—C97149.0 (2)
C36—C41—C42—C43−164.6 (2)C91—C92—C93—C94−59.1 (3)
C46—C41—C42—C4357.1 (3)C97—C92—C93—C9459.6 (4)
Zr2—C41—C42—C43−91.2 (3)C92—C93—C94—C9559.8 (3)
C36—C41—C42—C4776.3 (3)C92—C93—C94—C98−60.0 (4)
C46—C41—C42—C47−62.0 (3)C93—C94—C95—C96−59.5 (4)
Zr2—C41—C42—C47149.7 (2)C98—C94—C95—C9660.2 (4)
C41—C42—C43—C44−59.4 (3)C94—C95—C96—C9159.2 (4)
C47—C42—C43—C4459.9 (3)C94—C95—C96—C99−59.8 (4)
C42—C43—C44—C48−60.1 (3)C86—C91—C96—C95164.8 (3)
C42—C43—C44—C4560.1 (4)C92—C91—C96—C95−57.3 (3)
C48—C44—C45—C4660.4 (3)Zr4—C91—C96—C9589.9 (3)
C43—C44—C45—C46−60.2 (3)C86—C91—C96—C99−75.9 (3)
C36—C41—C46—C45165.6 (2)C92—C91—C96—C9962.0 (3)
C42—C41—C46—C45−56.9 (3)Zr4—C91—C96—C99−150.8 (2)
Zr2—C41—C46—C4592.1 (3)C91—C92—C97—C10060.0 (4)
C36—C41—C46—C49−75.6 (3)C93—C92—C97—C100−59.6 (4)
C42—C41—C46—C4961.9 (3)C95—C94—C98—C100−59.8 (5)
Zr2—C41—C46—C49−149.14 (18)C93—C94—C98—C10059.4 (4)
C44—C45—C46—C4159.1 (3)C95—C96—C99—C10059.9 (4)
C44—C45—C46—C49−59.7 (3)C91—C96—C99—C100−60.8 (4)
C43—C42—C47—C50−60.4 (3)C94—C98—C100—C97−60.1 (4)
C41—C42—C47—C5060.3 (3)C94—C98—C100—C9960.0 (4)
C43—C44—C48—C5059.3 (3)C92—C97—C100—C9860.8 (4)
C45—C44—C48—C50−60.3 (4)C92—C97—C100—C99−59.3 (3)
C41—C46—C49—C50−60.3 (3)C96—C99—C100—C98−60.5 (4)
C45—C46—C49—C5059.9 (3)C96—C99—C100—C9759.8 (4)
C44—C48—C50—C47−59.3 (3)C106—C101—C102—C1036.1 (14)
C44—C48—C50—C4960.5 (3)C107—C101—C102—C103−177.2 (13)
C42—C47—C50—C4860.4 (3)C101—C102—C103—C104−6.5 (15)
C42—C47—C50—C49−59.2 (3)C102—C103—C104—C1052.5 (17)
C46—C49—C50—C48−60.6 (3)C103—C104—C105—C1062.4 (18)
C46—C49—C50—C4759.2 (4)C104—C105—C106—C101−2.8 (17)
C55—C51—C52—C532.5 (4)C107—C101—C106—C105−178.5 (13)
Zr3—C51—C52—C53−65.5 (2)C102—C101—C106—C105−1.4 (16)
C55—C51—C52—Zr368.0 (2)C108—C109—C110—C11186.9 (18)
C51—C52—C53—C54−4.6 (3)C109—C110—C111—C112−165.7 (13)
Zr3—C52—C53—C54−72.0 (2)C110—C111—C112—C113178.6 (14)
C51—C52—C53—Zr367.4 (2)
 

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ISSN: 2056-9890
Volume 73| Part 12| December 2017| Pages 1823-1826
https://doi.org/10.1107/S2056989017015560
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