metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
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ISSN: 2056-9890
Volume 71| Part 2| February 2015| Pages m19-m20

Crystal structure of di-n-but­yl­bis­­(η5-penta­methyl­cyclo­penta­dien­yl)hafnium(IV)

aLeibniz-Institut für Katalyse e. V. an der Universität Rostock, Albert-Einstein-Str. 29a, 18059 Rostock, Germany, and bA. N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Vavilov St 28, 119991, Moscow, Russian Federation
*Correspondence e-mail: uwe.rosenthal@catalysis.de

Edited by A. V. Yatsenko, Moscow State University, Russia (Received 9 December 2014; accepted 5 January 2015; online 10 January 2015)

The crystal structure of the title compound, [Hf(C10H15)2(C4H9)2], reveals two independent mol­ecules in the asymmetric unit. The diffraction experiment was performed with a racemically twinned crystal showing a 0.529 (5):0.471 (5) component ratio. Each HfIV atom is coordinated by two penta­methyl­cyclo­penta­dienyl and two n-butyl ligands in a distorted tetra­hedral geometry, with the cyclo­penta­dienyl rings inclined to one another by 45.11 (15) and 45.37 (16)°. In contrast to the isostructural di(n-butyl)bis(η5-penta­methyl­cyclo­penta­dien­yl)zirconium(IV) complex with a noticeable difference in the Zr–butyl bonding, the Hf—Cbut­yl bond lengths differ from each other by no more than 0.039 (3) Å.

1. Related literature

For the synthesis of the title compound, see: Schock & Marks (1988[Schock, L. E. & Marks, T. J. (1988). J. Am. Chem. Soc. 110, 7701-7715.]), and for that of the corresponding unsubstituted cyclo­penta­dienyl complex, see: Burlakov et al. (2008[Burlakov, V. V., Bogdanov, V. S., Lyssenko, K. A., Petrovskii, P. V., Beweries, T., Arndt, P., Rosenthal, U. & Shur, V. B. (2008). Russ. Chem. Bull. 57, 1319-1320.]). For the use of these complexes as the starting materials for various reactions, see: Burlakov et al. (2009[Burlakov, V. V., Beweries, T., Bogdanov, V. S., Arndt, P., Baumann, W., Petrovskii, P. V., Spannenberg, A., Lyssenko, K. A., Shur, V. B. & Rosenthal, U. (2009). Organometallics, 28, 2864-2870.]). For the structure of the isostructural zirconocene complex, see: Ernst et al. (2004[Ernst, R. D., Harvey, B. G. & Arif, A. M. (2004). Z. Kristallogr. New Cryst. Struct., 219, 398-400.]), and of an ansa-zirconocene with an additional Zr—N bond, see: Paolucci et al. (1997[Paolucci, G., Pojana, G., Zanon, J., Lucchini, V. & Avtomonov, E. (1997). Organometallics, 16, 5312-5320.]). For [Mo(C5H5)2(C4H9)2], see: Calhorda et al. (1991[Calhorda, M. J., Carrondo, M. A. A. F. de C. T., Dias, A. R., Galvão, A. M., Garcia, M. H., Martins, A. M., Minas da Piedade, M. E., Pinheiro, C. I., Romão, C. C., Simões, J. A. M. & Veiros, L. F. (1991). Organometallics, 10, 483-494.]).

[Scheme 1]

2. Experimental

2.1. Crystal data

  • [Hf(C10H15)2(C4H9)2]

  • Mr = 563.15

  • Orthorhombic, P 21 21 21

  • a = 17.1572 (3) Å

  • b = 17.2320 (3) Å

  • c = 17.2966 (3) Å

  • V = 5113.79 (15) Å3

  • Z = 8

  • Mo Kα radiation

  • μ = 4.09 mm−1

  • T = 170 K

  • 0.39 × 0.27 × 0.17 mm

2.2. Data collection

  • Bruker Kappa APEXII DUO CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.30, Tmax = 0.54

  • 123798 measured reflections

  • 13236 independent reflections

  • 12433 reflections with I > 2σ(I)

  • Rint = 0.037

2.3. Refinement

  • R[F2 > 2σ(F2)] = 0.018

  • wR(F2) = 0.038

  • S = 1.06

  • 13236 reflections

  • 548 parameters

  • H-atom parameters constrained

  • Δρmax = 0.53 e Å−3

  • Δρmin = −0.77 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 999 Friedel pairs

  • Absolute structure parameter: 0.471 (5)

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL2014.

Supporting information


Synthesis and crystallization top

The title compound was synthesized as described by Schock & Marks (1988). To a suspension of Cp*2HfCl2 (1.00 g, 1.94 mmol) in 20 ml of di­ethyl­ether were added 3.0 ml of n-BuLi (1.6 M, 4.8 mmol) in di­ethyl­ether. The solution was stirred for 3 days at RT before the ether was removed in vacuo. The residue was extracted with n-hexane three times, the collected filtrates were reduced in vacuo to 10 ml. At -78°C colorless crystals were formed within two weeks (0,545 g, yield 50%).

1H NMR (300 MHz, C6D6): δ = - 0.14 (t, 4H, α-CH2), 1.05 (t, 6H, CH3), 1.23 (m, 4H, γ-CH2), 1.44 (t, 4H β-CH2), 1.84 (s, 30 H, Me-Cp) ppm., see Schock & Marks (1988).

Refinement top

H atoms were placed in idealized positions with d(C—H) = 0.99 Å (CH2), 0.98 Å (CH3) and refined using a riding model with Uiso(H) fixed at 1.2 Ueq(C) for CH2 and 1.5 Ueq(C) for CH3. The title compound crystallizes as racemic twin (Flack parameter x = 0.471 (5)).

Related literature top

For the synthesis of the title compound, see: Schock & Marks (1988), and for that of the corresponding unsubstituted cyclopentadienyl complex, see: Burlakov et al. (2008). For the use of these complexes as the starting materials for various reactions, see: Burlakov et al. (2009). For the structure of an isostructural zirconocene complex, see: Ernst et al. (2004), and of an ansa-zirconocene with an additional Zr—N bond, see: Paolucci et al. (1997). For [Mo(C5H5)2(C4H9)2], see: Calhorda et al. (1991).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. : Molecular structure of the two molecules of the asymmetric unit with labelling and displacement ellipsoids drawn at 30% probability level. Hydrogen atoms are omitted for clarity.
Di-n-butylbis(η5-pentamethylcyclopentadienyl)hafnium(IV) top
Crystal data top
[Hf(C10H15)2(C4H9)2]Dx = 1.463 Mg m3
Mr = 563.15Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 9300 reflections
a = 17.1572 (3) Åθ = 2.4–28.7°
b = 17.2320 (3) ŵ = 4.09 mm1
c = 17.2966 (3) ÅT = 170 K
V = 5113.79 (15) Å3Prism, colourless
Z = 80.39 × 0.27 × 0.17 mm
F(000) = 2304
Data collection top
Bruker Kappa APEXII DUO CCD
diffractometer
13236 independent reflections
Radiation source: fine-focus sealed tube12433 reflections with I > 2σ(I)
Curved graphite monochromatorRint = 0.037
Detector resolution: 8.3333 pixels mm-1θmax = 28.7°, θmin = 1.7°
ϕ and ω scansh = 1823
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
k = 2323
Tmin = 0.30, Tmax = 0.54l = 2323
123798 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)] = 0.018H-atom parameters constrained
wR(F2) = 0.038 w = 1/[σ2(Fo2) + (0.017P)2 + 1.9262P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.003
13236 reflectionsΔρmax = 0.53 e Å3
548 parametersΔρmin = 0.77 e Å3
0 restraintsAbsolute structure: Flack (1983), 999 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.471 (5)
Crystal data top
[Hf(C10H15)2(C4H9)2]V = 5113.79 (15) Å3
Mr = 563.15Z = 8
Orthorhombic, P212121Mo Kα radiation
a = 17.1572 (3) ŵ = 4.09 mm1
b = 17.2320 (3) ÅT = 170 K
c = 17.2966 (3) Å0.39 × 0.27 × 0.17 mm
Data collection top
Bruker Kappa APEXII DUO CCD
diffractometer
13236 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
12433 reflections with I > 2σ(I)
Tmin = 0.30, Tmax = 0.54Rint = 0.037
123798 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.018H-atom parameters constrained
wR(F2) = 0.038Δρmax = 0.53 e Å3
S = 1.06Δρmin = 0.77 e Å3
13236 reflectionsAbsolute structure: Flack (1983), 999 Friedel pairs
548 parametersAbsolute structure parameter: 0.471 (5)
0 restraints
Special details top

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
C10.10245 (14)1.04413 (14)0.84536 (16)0.0209 (5)
H1A0.07751.02940.79590.025*
H1B0.07111.01920.88650.025*
C20.08748 (16)1.13134 (15)0.85402 (17)0.0234 (6)
H2A0.09621.14630.90860.028*
H2B0.12571.15990.82200.028*
C30.00596 (16)1.15583 (16)0.83060 (19)0.0300 (7)
H3A0.03221.12450.86020.036*
H3B0.00151.14380.77510.036*
C40.0116 (2)1.24120 (17)0.8436 (2)0.0377 (8)
H4A0.02341.27280.81180.057*
H4B0.00391.25400.89830.057*
H4C0.06581.25190.82910.057*
C50.16087 (15)0.86169 (15)0.84278 (16)0.0227 (5)
H5A0.16380.84240.78890.027*
H5B0.19250.82620.87500.027*
C60.07551 (15)0.85520 (15)0.86963 (16)0.0211 (5)
H6A0.06990.88140.92020.025*
H6B0.04160.88250.83210.025*
C70.04807 (17)0.77125 (16)0.87731 (18)0.0260 (6)
H7A0.05950.74350.82850.031*
H7B0.07810.74580.91910.031*
C80.03837 (18)0.76363 (18)0.8950 (2)0.0358 (7)
H8A0.06870.78760.85330.054*
H8B0.05000.78980.94400.054*
H8C0.05210.70860.89910.054*
C90.32937 (14)0.98398 (18)0.74945 (14)0.0213 (5)
C100.29051 (18)1.05690 (15)0.74342 (14)0.0211 (5)
C110.21592 (19)1.04259 (13)0.71054 (13)0.0211 (5)
C120.20807 (17)0.96162 (15)0.69862 (14)0.0227 (5)
C130.27865 (19)0.92560 (15)0.72268 (14)0.0232 (5)
C140.41568 (15)0.9711 (2)0.76112 (17)0.0330 (7)
H14A0.44000.95820.71150.049*
H14B0.42360.92820.79760.049*
H14C0.43941.01840.78190.049*
C150.32455 (19)1.13609 (18)0.75601 (19)0.0328 (7)
H15A0.29751.16160.79900.049*
H15B0.31831.16710.70890.049*
H15C0.38011.13130.76830.049*
C160.16141 (18)1.10256 (19)0.67941 (18)0.0342 (7)
H16A0.16471.10330.62280.051*
H16B0.17581.15360.69980.051*
H16C0.10801.09000.69510.051*
C170.13977 (18)0.9248 (2)0.65925 (18)0.0360 (7)
H17A0.14600.86820.65960.054*
H17B0.13680.94320.60570.054*
H17C0.09180.93870.68670.054*
C180.29965 (19)0.84198 (17)0.71220 (19)0.0365 (8)
H18A0.32520.82270.75910.055*
H18B0.33530.83670.66820.055*
H18C0.25230.81170.70240.055*
C190.32414 (14)1.02052 (19)0.94309 (14)0.0225 (5)
C200.25657 (15)1.06311 (16)0.96461 (15)0.0212 (5)
C210.20008 (14)1.00970 (16)0.99217 (15)0.0220 (6)
C220.23236 (15)0.93384 (15)0.98649 (14)0.0203 (6)
C230.30815 (15)0.94104 (17)0.95437 (16)0.0225 (6)
C240.40301 (17)1.05688 (19)0.93168 (18)0.0334 (7)
H24A0.44021.01710.91480.050*
H24B0.42081.07960.98050.050*
H24C0.39951.09760.89230.050*
C250.25347 (18)1.14995 (16)0.97023 (19)0.0315 (7)
H25A0.20591.16550.99750.047*
H25B0.25341.17240.91820.047*
H25C0.29911.16870.99870.047*
C260.12593 (15)1.02885 (19)1.03341 (15)0.0274 (6)
H26A0.11211.08311.02360.041*
H26B0.13301.02091.08910.041*
H26C0.08410.99501.01460.041*
C270.19842 (17)0.86248 (17)1.02273 (17)0.0300 (7)
H27A0.14680.85241.00060.045*
H27B0.19360.87031.07860.045*
H27C0.23270.81811.01270.045*
C280.36408 (18)0.87419 (18)0.94451 (18)0.0330 (7)
H28A0.41410.89370.92540.049*
H28B0.34250.83700.90730.049*
H28C0.37190.84840.99440.049*
C290.39487 (15)0.54682 (14)0.88712 (16)0.0206 (5)
H29A0.42400.52590.93190.025*
H29B0.42380.52930.84080.025*
C300.40920 (15)0.63443 (15)0.89038 (17)0.0229 (5)
H30A0.37630.66030.85110.028*
H30B0.39340.65410.94180.028*
C310.49422 (17)0.65535 (17)0.8760 (2)0.0368 (8)
H31A0.52680.62780.91450.044*
H31B0.50920.63610.82420.044*
C320.5129 (2)0.74127 (17)0.8802 (2)0.0395 (8)
H32A0.49890.76120.93150.059*
H32B0.48320.76910.84060.059*
H32C0.56880.74910.87140.059*
C330.35133 (16)0.36285 (15)0.88524 (16)0.0230 (5)
H33A0.31970.32400.91340.028*
H33B0.35590.34470.83110.028*
C340.43333 (16)0.36327 (16)0.92074 (17)0.0257 (6)
H34A0.46660.39850.88980.031*
H34B0.42990.38510.97360.031*
C350.47354 (18)0.28392 (17)0.9256 (2)0.0334 (7)
H35A0.52190.28920.95640.040*
H35B0.43880.24720.95300.040*
C360.4937 (2)0.25057 (19)0.8475 (2)0.0411 (8)
H36A0.53130.28460.82150.062*
H36B0.44640.24660.81600.062*
H36C0.51660.19890.85410.062*
C370.2159 (2)0.55026 (15)0.77661 (14)0.0228 (5)
C380.29141 (17)0.53422 (15)0.74613 (13)0.0220 (6)
C390.29843 (15)0.45287 (16)0.73771 (15)0.0227 (6)
C400.22729 (18)0.41820 (16)0.76189 (16)0.0241 (6)
C410.17574 (14)0.47824 (19)0.78436 (14)0.0225 (5)
C420.18260 (18)0.63014 (17)0.78753 (18)0.0305 (7)
H42A0.16600.65090.73740.046*
H42B0.22240.66420.80990.046*
H42C0.13770.62740.82240.046*
C430.34800 (19)0.59149 (19)0.71299 (17)0.0331 (7)
H43A0.34740.58790.65650.050*
H43B0.40050.58000.73210.050*
H43C0.33310.64410.72870.050*
C440.36646 (18)0.4137 (2)0.70034 (19)0.0387 (8)
H44A0.41420.42710.72840.058*
H44B0.37090.43110.64650.058*
H44C0.35890.35740.70160.058*
C450.2069 (2)0.33404 (17)0.75571 (19)0.0361 (7)
H45A0.19690.32090.70150.054*
H45B0.16010.32340.78650.054*
H45C0.25030.30260.77510.054*
C460.08939 (16)0.4674 (2)0.79405 (17)0.0331 (7)
H46A0.07960.42680.83250.050*
H46B0.06640.45210.74450.050*
H46C0.06590.51620.81150.050*
C470.23728 (15)0.55693 (16)1.00118 (15)0.0209 (5)
C480.29283 (17)0.50411 (14)1.03097 (14)0.0218 (6)
C490.26283 (16)0.42810 (16)1.02337 (15)0.0230 (6)
C500.18791 (16)0.43383 (17)0.98829 (16)0.0221 (6)
C510.17114 (15)0.51383 (18)0.97676 (15)0.0222 (5)
C520.23970 (17)0.64415 (16)1.00693 (18)0.0308 (7)
H52A0.28760.66011.03340.046*
H52B0.19440.66251.03630.046*
H52C0.23870.66660.95490.046*
C530.36538 (15)0.52551 (18)1.07501 (16)0.0293 (6)
H53A0.40560.48621.06600.044*
H53B0.35350.52811.13040.044*
H53C0.38430.57621.05730.044*
C540.29470 (18)0.35685 (16)1.06056 (16)0.0299 (6)
H54A0.28090.35661.11550.045*
H54B0.35160.35621.05520.045*
H54C0.27270.31081.03540.045*
C550.13305 (19)0.36651 (18)0.97753 (19)0.0355 (7)
H55A0.08460.38490.95390.053*
H55B0.12150.34311.02790.053*
H55C0.15740.32770.94390.053*
C560.09175 (17)0.54926 (19)0.96328 (18)0.0330 (7)
H56A0.09550.58920.92310.049*
H56B0.07290.57271.01140.049*
H56C0.05530.50880.94660.049*
Hf10.218019 (6)0.981329 (5)0.846352 (5)0.01504 (2)
Hf20.283647 (6)0.477447 (5)0.884701 (5)0.01551 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0178 (12)0.0213 (12)0.0235 (13)0.0033 (9)0.0016 (10)0.0020 (10)
C20.0213 (14)0.0206 (13)0.0282 (15)0.0014 (10)0.0010 (11)0.0015 (11)
C30.0211 (14)0.0229 (14)0.0461 (19)0.0044 (11)0.0013 (13)0.0031 (12)
C40.0388 (19)0.0273 (15)0.047 (2)0.0118 (13)0.0021 (16)0.0025 (14)
C50.0247 (14)0.0205 (12)0.0228 (13)0.0034 (10)0.0026 (11)0.0011 (10)
C60.0182 (13)0.0200 (12)0.0253 (14)0.0014 (10)0.0015 (10)0.0014 (10)
C70.0260 (15)0.0201 (12)0.0320 (15)0.0040 (11)0.0008 (12)0.0015 (12)
C80.0285 (16)0.0370 (16)0.0421 (19)0.0115 (13)0.0016 (13)0.0002 (14)
C90.0154 (12)0.0299 (13)0.0184 (11)0.0004 (12)0.0061 (9)0.0006 (12)
C100.0201 (14)0.0246 (12)0.0187 (12)0.0008 (12)0.0033 (11)0.0057 (10)
C110.0186 (11)0.0284 (13)0.0163 (10)0.0020 (13)0.0021 (11)0.0043 (9)
C120.0212 (14)0.0308 (14)0.0162 (11)0.0028 (11)0.0019 (10)0.0011 (9)
C130.0249 (13)0.0266 (12)0.0182 (11)0.0042 (13)0.0074 (12)0.0006 (9)
C140.0167 (13)0.0515 (19)0.0309 (15)0.0051 (14)0.0056 (11)0.0018 (15)
C150.0354 (17)0.0306 (16)0.0323 (17)0.0080 (13)0.0027 (13)0.0057 (13)
C160.0277 (16)0.0476 (18)0.0272 (16)0.0102 (14)0.0030 (12)0.0139 (14)
C170.0293 (16)0.052 (2)0.0266 (16)0.0082 (14)0.0015 (13)0.0051 (14)
C180.042 (2)0.0298 (15)0.0374 (17)0.0064 (13)0.0169 (14)0.0036 (12)
C190.0205 (12)0.0292 (13)0.0177 (12)0.0007 (12)0.0047 (9)0.0012 (12)
C200.0237 (13)0.0228 (13)0.0172 (12)0.0055 (10)0.0026 (10)0.0014 (11)
C210.0211 (15)0.0256 (13)0.0192 (11)0.0000 (10)0.0003 (9)0.0012 (10)
C220.0223 (16)0.0237 (12)0.0149 (11)0.0030 (10)0.0017 (10)0.0026 (10)
C230.0176 (13)0.0303 (14)0.0196 (13)0.0046 (11)0.0046 (10)0.0034 (11)
C240.0257 (15)0.0470 (17)0.0275 (15)0.0080 (13)0.0011 (12)0.0012 (14)
C250.0351 (16)0.0253 (14)0.0341 (16)0.0023 (12)0.0048 (13)0.0049 (13)
C260.0275 (14)0.0367 (16)0.0180 (12)0.0036 (13)0.0044 (10)0.0022 (12)
C270.0330 (18)0.0307 (14)0.0262 (14)0.0011 (12)0.0005 (12)0.0083 (12)
C280.0283 (16)0.0400 (17)0.0306 (17)0.0106 (13)0.0013 (12)0.0056 (13)
C290.0203 (13)0.0224 (12)0.0190 (12)0.0028 (9)0.0017 (10)0.0002 (10)
C300.0205 (13)0.0228 (13)0.0255 (14)0.0014 (10)0.0029 (11)0.0019 (11)
C310.0221 (15)0.0233 (14)0.065 (2)0.0049 (11)0.0082 (15)0.0028 (14)
C320.0367 (19)0.0283 (16)0.054 (2)0.0094 (14)0.0142 (16)0.0030 (16)
C330.0229 (13)0.0222 (12)0.0237 (13)0.0025 (10)0.0013 (11)0.0024 (11)
C340.0251 (14)0.0254 (13)0.0267 (14)0.0019 (11)0.0019 (11)0.0012 (12)
C350.0308 (16)0.0292 (15)0.0404 (17)0.0067 (12)0.0054 (14)0.0024 (13)
C360.0299 (18)0.0337 (17)0.060 (2)0.0034 (13)0.0035 (17)0.0128 (15)
C370.0228 (13)0.0270 (12)0.0186 (11)0.0028 (13)0.0065 (13)0.0026 (9)
C380.0195 (13)0.0318 (14)0.0147 (10)0.0019 (12)0.0026 (10)0.0036 (10)
C390.0214 (16)0.0298 (14)0.0168 (11)0.0043 (10)0.0029 (10)0.0069 (10)
C400.0204 (15)0.0301 (14)0.0219 (12)0.0012 (12)0.0085 (12)0.0040 (10)
C410.0195 (12)0.0298 (13)0.0182 (12)0.0013 (12)0.0046 (9)0.0013 (12)
C420.0312 (16)0.0313 (16)0.0289 (16)0.0069 (12)0.0045 (13)0.0040 (12)
C430.0319 (16)0.0455 (18)0.0217 (14)0.0090 (14)0.0019 (12)0.0091 (13)
C440.0329 (18)0.058 (2)0.0251 (16)0.0102 (15)0.0009 (13)0.0147 (15)
C450.0346 (19)0.0340 (15)0.0397 (17)0.0056 (14)0.0096 (15)0.0088 (13)
C460.0222 (14)0.051 (2)0.0265 (14)0.0042 (13)0.0032 (11)0.0011 (14)
C470.0236 (15)0.0219 (12)0.0171 (12)0.0018 (10)0.0040 (10)0.0026 (10)
C480.0253 (15)0.0260 (13)0.0142 (10)0.0001 (10)0.0009 (10)0.0033 (9)
C490.0287 (17)0.0255 (13)0.0149 (12)0.0028 (11)0.0011 (10)0.0020 (10)
C500.0233 (14)0.0259 (14)0.0172 (13)0.0041 (11)0.0037 (10)0.0028 (11)
C510.0197 (12)0.0283 (14)0.0187 (12)0.0012 (12)0.0037 (9)0.0017 (12)
C520.0359 (18)0.0273 (14)0.0294 (15)0.0046 (12)0.0036 (12)0.0029 (12)
C530.0293 (14)0.0351 (15)0.0235 (13)0.0000 (13)0.0042 (11)0.0049 (14)
C540.0364 (18)0.0285 (13)0.0249 (14)0.0020 (12)0.0018 (12)0.0061 (11)
C550.0353 (18)0.0373 (17)0.0337 (18)0.0143 (14)0.0021 (14)0.0019 (14)
C560.0235 (15)0.0464 (18)0.0289 (15)0.0084 (13)0.0042 (12)0.0011 (13)
Hf10.01256 (4)0.01658 (4)0.01597 (4)0.00068 (5)0.00096 (4)0.00147 (4)
Hf20.01422 (4)0.01740 (4)0.01492 (4)0.00044 (6)0.00092 (4)0.00109 (4)
Geometric parameters (Å, º) top
C1—C21.532 (3)C29—C301.531 (3)
C1—Hf12.259 (2)C29—Hf22.252 (2)
C1—H1A0.9900C29—H29A0.9900
C1—H1B0.9900C29—H29B0.9900
C2—C31.516 (4)C30—C311.523 (4)
C2—H2A0.9900C30—H30A0.9900
C2—H2B0.9900C30—H30B0.9900
C3—C41.518 (4)C31—C321.517 (4)
C3—H3A0.9900C31—H31A0.9900
C3—H3B0.9900C31—H31B0.9900
C4—H4A0.9800C32—H32A0.9800
C4—H4B0.9800C32—H32B0.9800
C4—H4C0.9800C32—H32C0.9800
C5—C61.540 (4)C33—C341.535 (4)
C5—Hf12.284 (2)C33—Hf22.291 (3)
C5—H5A0.9900C33—H33A0.9900
C5—H5B0.9900C33—H33B0.9900
C6—C71.527 (4)C34—C351.534 (4)
C6—H6A0.9900C34—H34A0.9900
C6—H6B0.9900C34—H34B0.9900
C7—C81.520 (4)C35—C361.509 (5)
C7—H7A0.9900C35—H35A0.9900
C7—H7B0.9900C35—H35B0.9900
C8—H8A0.9800C36—H36A0.9800
C8—H8B0.9800C36—H36B0.9800
C8—H8C0.9800C36—H36C0.9800
C9—C131.408 (4)C37—C381.425 (4)
C9—C101.426 (4)C37—C411.426 (4)
C9—C141.511 (3)C37—C421.502 (4)
C9—Hf12.542 (2)C37—Hf22.534 (3)
C10—C111.422 (4)C38—C391.415 (4)
C10—C151.500 (4)C38—C431.498 (4)
C10—Hf12.532 (3)C38—Hf22.592 (2)
C11—C121.417 (4)C39—C401.422 (4)
C11—C161.494 (4)C39—C441.495 (4)
C11—Hf12.576 (2)C39—Hf22.590 (3)
C12—C131.423 (4)C40—C411.416 (4)
C12—C171.497 (4)C40—C451.496 (4)
C12—Hf12.583 (2)C40—Hf22.547 (3)
C13—C181.496 (4)C41—C461.503 (4)
C13—Hf12.565 (2)C41—Hf22.538 (2)
C14—H14A0.9800C42—H42A0.9800
C14—H14B0.9800C42—H42B0.9800
C14—H14C0.9800C42—H42C0.9800
C15—H15A0.9800C43—H43A0.9800
C15—H15B0.9800C43—H43B0.9800
C15—H15C0.9800C43—H43C0.9800
C16—H16A0.9800C44—H44A0.9800
C16—H16B0.9800C44—H44B0.9800
C16—H16C0.9800C44—H44C0.9800
C17—H17A0.9800C45—H45A0.9800
C17—H17B0.9800C45—H45B0.9800
C17—H17C0.9800C45—H45C0.9800
C18—H18A0.9800C46—H46A0.9800
C18—H18B0.9800C46—H46B0.9800
C18—H18C0.9800C46—H46C0.9800
C19—C231.410 (4)C47—C481.415 (4)
C19—C201.422 (4)C47—C511.421 (4)
C19—C241.504 (4)C47—C521.507 (4)
C19—Hf12.563 (2)C47—Hf22.563 (3)
C20—C211.419 (4)C48—C491.414 (4)
C20—C251.501 (4)C48—C531.505 (4)
C20—Hf12.571 (3)C48—Hf22.576 (2)
C21—C221.423 (4)C49—C501.425 (4)
C21—C261.496 (3)C49—C541.490 (4)
C21—Hf12.587 (3)C49—Hf22.570 (3)
C22—C231.419 (4)C50—C511.422 (4)
C22—C271.498 (4)C50—C551.505 (4)
C22—Hf12.570 (2)C50—Hf22.544 (3)
C23—C281.509 (4)C51—C561.511 (4)
C23—Hf12.523 (3)C51—Hf22.580 (2)
C24—H24A0.9800C52—H52A0.9800
C24—H24B0.9800C52—H52B0.9800
C24—H24C0.9800C52—H52C0.9800
C25—H25A0.9800C53—H53A0.9800
C25—H25B0.9800C53—H53B0.9800
C25—H25C0.9800C53—H53C0.9800
C26—H26A0.9800C54—H54A0.9800
C26—H26B0.9800C54—H54B0.9800
C26—H26C0.9800C54—H54C0.9800
C27—H27A0.9800C55—H55A0.9800
C27—H27B0.9800C55—H55B0.9800
C27—H27C0.9800C55—H55C0.9800
C28—H28A0.9800C56—H56A0.9800
C28—H28B0.9800C56—H56B0.9800
C28—H28C0.9800C56—H56C0.9800
C2—C1—Hf1128.05 (18)C41—C40—C39108.1 (2)
C2—C1—H1A105.3C41—C40—C45125.6 (3)
Hf1—C1—H1A105.3C39—C40—C45126.0 (3)
C2—C1—H1B105.3C41—C40—Hf273.46 (14)
Hf1—C1—H1B105.3C39—C40—Hf275.58 (15)
H1A—C1—H1B106.0C45—C40—Hf2122.48 (19)
C3—C2—C1113.7 (2)C40—C41—C37107.9 (2)
C3—C2—H2A108.8C40—C41—C46123.7 (3)
C1—C2—H2A108.8C37—C41—C46126.6 (3)
C3—C2—H2B108.8C40—C41—Hf274.22 (15)
C1—C2—H2B108.8C37—C41—Hf273.51 (14)
H2A—C2—H2B107.7C46—C41—Hf2129.97 (18)
C2—C3—C4114.4 (3)C37—C42—H42A109.5
C2—C3—H3A108.7C37—C42—H42B109.5
C4—C3—H3A108.7H42A—C42—H42B109.5
C2—C3—H3B108.7C37—C42—H42C109.5
C4—C3—H3B108.7H42A—C42—H42C109.5
H3A—C3—H3B107.6H42B—C42—H42C109.5
C3—C4—H4A109.5C38—C43—H43A109.5
C3—C4—H4B109.5C38—C43—H43B109.5
H4A—C4—H4B109.5H43A—C43—H43B109.5
C3—C4—H4C109.5C38—C43—H43C109.5
H4A—C4—H4C109.5H43A—C43—H43C109.5
H4B—C4—H4C109.5H43B—C43—H43C109.5
C6—C5—Hf1117.75 (17)C39—C44—H44A109.5
C6—C5—H5A107.9C39—C44—H44B109.5
Hf1—C5—H5A107.9H44A—C44—H44B109.5
C6—C5—H5B107.9C39—C44—H44C109.5
Hf1—C5—H5B107.9H44A—C44—H44C109.5
H5A—C5—H5B107.2H44B—C44—H44C109.5
C7—C6—C5112.8 (2)C40—C45—H45A109.5
C7—C6—H6A109.0C40—C45—H45B109.5
C5—C6—H6A109.0H45A—C45—H45B109.5
C7—C6—H6B109.0C40—C45—H45C109.5
C5—C6—H6B109.0H45A—C45—H45C109.5
H6A—C6—H6B107.8H45B—C45—H45C109.5
C8—C7—C6113.6 (2)C41—C46—H46A109.5
C8—C7—H7A108.8C41—C46—H46B109.5
C6—C7—H7A108.8H46A—C46—H46B109.5
C8—C7—H7B108.8C41—C46—H46C109.5
C6—C7—H7B108.8H46A—C46—H46C109.5
H7A—C7—H7B107.7H46B—C46—H46C109.5
C7—C8—H8A109.5C48—C47—C51108.1 (2)
C7—C8—H8B109.5C48—C47—C52126.8 (2)
H8A—C8—H8B109.5C51—C47—C52124.3 (2)
C7—C8—H8C109.5C48—C47—Hf274.54 (14)
H8A—C8—H8C109.5C51—C47—Hf274.62 (14)
H8B—C8—H8C109.5C52—C47—Hf2125.20 (18)
C13—C9—C10108.4 (2)C49—C48—C47108.5 (2)
C13—C9—C14123.0 (3)C49—C48—C53125.1 (2)
C10—C9—C14126.7 (3)C47—C48—C53125.7 (2)
C13—C9—Hf174.90 (15)C49—C48—Hf273.80 (14)
C10—C9—Hf173.30 (14)C47—C48—Hf273.49 (14)
C14—C9—Hf1130.23 (18)C53—C48—Hf2126.25 (18)
C11—C10—C9107.3 (2)C48—C49—C50107.7 (3)
C11—C10—C15124.5 (2)C48—C49—C54126.1 (2)
C9—C10—C15127.5 (3)C50—C49—C54124.9 (3)
C11—C10—Hf175.53 (15)C48—C49—Hf274.31 (14)
C9—C10—Hf174.05 (14)C50—C49—Hf272.84 (14)
C15—C10—Hf1123.85 (18)C54—C49—Hf2128.65 (19)
C12—C11—C10108.3 (2)C51—C50—C49108.0 (2)
C12—C11—C16124.7 (3)C51—C50—C55127.1 (3)
C10—C11—C16126.0 (2)C49—C50—C55124.3 (3)
C12—C11—Hf174.36 (13)C51—C50—Hf275.26 (16)
C10—C11—Hf172.16 (13)C49—C50—Hf274.81 (15)
C16—C11—Hf1128.38 (19)C55—C50—Hf2123.0 (2)
C11—C12—C13107.8 (3)C47—C51—C50107.7 (2)
C11—C12—C17124.0 (3)C47—C51—C56123.7 (3)
C13—C12—C17127.9 (3)C50—C51—C56126.6 (3)
C11—C12—Hf173.76 (13)C47—C51—Hf273.31 (14)
C13—C12—Hf173.26 (14)C50—C51—Hf272.52 (16)
C17—C12—Hf1123.89 (19)C56—C51—Hf2132.66 (18)
C9—C13—C12108.1 (2)C47—C52—H52A109.5
C9—C13—C18125.4 (3)C47—C52—H52B109.5
C12—C13—C18126.1 (3)H52A—C52—H52B109.5
C9—C13—Hf173.09 (14)C47—C52—H52C109.5
C12—C13—Hf174.66 (14)H52A—C52—H52C109.5
C18—C13—Hf1124.00 (18)H52B—C52—H52C109.5
C9—C14—H14A109.5C48—C53—H53A109.5
C9—C14—H14B109.5C48—C53—H53B109.5
H14A—C14—H14B109.5H53A—C53—H53B109.5
C9—C14—H14C109.5C48—C53—H53C109.5
H14A—C14—H14C109.5H53A—C53—H53C109.5
H14B—C14—H14C109.5H53B—C53—H53C109.5
C10—C15—H15A109.5C49—C54—H54A109.5
C10—C15—H15B109.5C49—C54—H54B109.5
H15A—C15—H15B109.5H54A—C54—H54B109.5
C10—C15—H15C109.5C49—C54—H54C109.5
H15A—C15—H15C109.5H54A—C54—H54C109.5
H15B—C15—H15C109.5H54B—C54—H54C109.5
C11—C16—H16A109.5C50—C55—H55A109.5
C11—C16—H16B109.5C50—C55—H55B109.5
H16A—C16—H16B109.5H55A—C55—H55B109.5
C11—C16—H16C109.5C50—C55—H55C109.5
H16A—C16—H16C109.5H55A—C55—H55C109.5
H16B—C16—H16C109.5H55B—C55—H55C109.5
C12—C17—H17A109.5C51—C56—H56A109.5
C12—C17—H17B109.5C51—C56—H56B109.5
H17A—C17—H17B109.5H56A—C56—H56B109.5
C12—C17—H17C109.5C51—C56—H56C109.5
H17A—C17—H17C109.5H56A—C56—H56C109.5
H17B—C17—H17C109.5H56B—C56—H56C109.5
C13—C18—H18A109.5C1—Hf1—C593.18 (10)
C13—C18—H18B109.5C1—Hf1—C23132.49 (10)
H18A—C18—H18B109.5C5—Hf1—C2391.99 (10)
C13—C18—H18C109.5C1—Hf1—C10100.34 (9)
H18A—C18—H18C109.5C5—Hf1—C10131.00 (9)
H18B—C18—H18C109.5C23—Hf1—C10111.17 (9)
C23—C19—C20107.8 (2)C1—Hf1—C9130.25 (9)
C23—C19—C24126.7 (3)C5—Hf1—C9108.73 (10)
C20—C19—C24123.6 (3)C23—Hf1—C991.87 (8)
C23—C19—Hf172.32 (16)C10—Hf1—C932.65 (9)
C20—C19—Hf174.20 (14)C1—Hf1—C19120.14 (10)
C24—C19—Hf1131.54 (18)C5—Hf1—C19124.09 (10)
C21—C20—C19108.1 (2)C23—Hf1—C1932.19 (9)
C21—C20—C25126.9 (3)C10—Hf1—C1988.55 (9)
C19—C20—C25124.1 (2)C9—Hf1—C1983.79 (8)
C21—C20—Hf174.69 (15)C1—Hf1—C13121.94 (10)
C19—C20—Hf173.65 (14)C5—Hf1—C1379.26 (9)
C25—C20—Hf1126.10 (19)C23—Hf1—C13105.43 (9)
C20—C21—C22107.9 (2)C10—Hf1—C1353.63 (8)
C20—C21—C26126.7 (3)C9—Hf1—C1332.01 (9)
C22—C21—C26124.5 (2)C19—Hf1—C13110.79 (9)
C20—C21—Hf173.37 (15)C1—Hf1—C22104.10 (9)
C22—C21—Hf173.31 (14)C5—Hf1—C2277.24 (9)
C26—C21—Hf1127.43 (17)C23—Hf1—C2232.35 (8)
C23—C22—C21107.7 (2)C10—Hf1—C22141.24 (9)
C23—C22—C27126.3 (3)C9—Hf1—C22123.75 (8)
C21—C22—C27125.0 (2)C19—Hf1—C2253.15 (9)
C23—C22—Hf171.99 (14)C13—Hf1—C22128.94 (8)
C21—C22—Hf174.66 (14)C1—Hf1—C2088.24 (9)
C27—C22—Hf1128.22 (19)C5—Hf1—C20128.82 (9)
C19—C23—C22108.5 (2)C23—Hf1—C2053.40 (9)
C19—C23—C28127.0 (3)C10—Hf1—C2098.70 (8)
C22—C23—C28124.1 (3)C9—Hf1—C20108.75 (8)
C19—C23—Hf175.49 (16)C19—Hf1—C2032.15 (8)
C22—C23—Hf175.66 (14)C13—Hf1—C20139.86 (9)
C28—C23—Hf1121.07 (19)C22—Hf1—C2053.09 (9)
C19—C24—H24A109.5C1—Hf1—C1177.56 (10)
C19—C24—H24B109.5C5—Hf1—C11109.83 (9)
H24A—C24—H24B109.5C23—Hf1—C11142.83 (10)
C19—C24—H24C109.5C10—Hf1—C1132.31 (10)
H24A—C24—H24C109.5C9—Hf1—C1153.26 (9)
H24B—C24—H24C109.5C19—Hf1—C11119.82 (9)
C20—C25—H25A109.5C13—Hf1—C1153.02 (8)
C20—C25—H25B109.5C22—Hf1—C11172.75 (9)
H25A—C25—H25B109.5C20—Hf1—C11120.31 (8)
C20—C25—H25C109.5C1—Hf1—C1289.86 (9)
H25A—C25—H25C109.5C5—Hf1—C1279.99 (9)
H25B—C25—H25C109.5C23—Hf1—C12137.47 (9)
C21—C26—H26A109.5C10—Hf1—C1253.46 (9)
C21—C26—H26B109.5C9—Hf1—C1253.12 (8)
H26A—C26—H26B109.5C19—Hf1—C12136.66 (9)
C21—C26—H26C109.5C13—Hf1—C1232.09 (9)
H26A—C26—H26C109.5C22—Hf1—C12153.81 (8)
H26B—C26—H26C109.5C20—Hf1—C12151.19 (8)
C22—C27—H27A109.5C11—Hf1—C1231.88 (8)
C22—C27—H27B109.5C1—Hf1—C2179.19 (9)
H27A—C27—H27B109.5C5—Hf1—C2198.39 (9)
C22—C27—H27C109.5C23—Hf1—C2153.34 (8)
H27A—C27—H27C109.5C10—Hf1—C21130.28 (9)
H27B—C27—H27C109.5C9—Hf1—C21136.78 (8)
C23—C28—H28A109.5C19—Hf1—C2153.02 (8)
C23—C28—H28B109.5C13—Hf1—C21158.72 (9)
H28A—C28—H28B109.5C22—Hf1—C2132.03 (8)
C23—C28—H28C109.5C20—Hf1—C2131.93 (8)
H28A—C28—H28C109.5C11—Hf1—C21144.09 (8)
H28B—C28—H28C109.5C12—Hf1—C21168.85 (8)
C30—C29—Hf2131.33 (18)C29—Hf2—C3391.61 (9)
C30—C29—H29A104.4C29—Hf2—C3798.01 (10)
Hf2—C29—H29A104.4C33—Hf2—C37131.48 (9)
C30—C29—H29B104.4C29—Hf2—C41128.90 (9)
Hf2—C29—H29B104.4C33—Hf2—C41112.16 (10)
H29A—C29—H29B105.6C37—Hf2—C4132.66 (9)
C31—C30—C29112.4 (2)C29—Hf2—C50133.69 (9)
C31—C30—H30A109.1C33—Hf2—C5094.00 (10)
C29—C30—H30A109.1C37—Hf2—C50111.71 (10)
C31—C30—H30B109.1C41—Hf2—C5090.70 (9)
C29—C30—H30B109.1C29—Hf2—C40123.36 (10)
H30A—C30—H30B107.9C33—Hf2—C4081.39 (9)
C32—C31—C30115.2 (3)C37—Hf2—C4053.78 (8)
C32—C31—H31A108.5C41—Hf2—C4032.32 (9)
C30—C31—H31A108.5C50—Hf2—C40102.93 (9)
C32—C31—H31B108.5C29—Hf2—C4787.98 (9)
C30—C31—H31B108.5C33—Hf2—C47127.94 (9)
H31A—C31—H31B107.5C37—Hf2—C4799.97 (9)
C31—C32—H32A109.5C41—Hf2—C47107.96 (9)
C31—C32—H32B109.5C50—Hf2—C4753.41 (9)
H32A—C32—H32B109.5C40—Hf2—C47138.75 (9)
C31—C32—H32C109.5C29—Hf2—C49106.03 (9)
H32A—C32—H32C109.5C33—Hf2—C4977.37 (9)
H32B—C32—H32C109.5C37—Hf2—C49142.08 (10)
C34—C33—Hf2117.53 (17)C41—Hf2—C49122.59 (9)
C34—C33—H33A107.9C50—Hf2—C4932.35 (8)
Hf2—C33—H33A107.9C40—Hf2—C49126.36 (9)
C34—C33—H33B107.9C47—Hf2—C4953.13 (9)
Hf2—C33—H33B107.9C29—Hf2—C4880.52 (9)
H33A—C33—H33B107.2C33—Hf2—C4896.82 (9)
C35—C34—C33115.5 (2)C37—Hf2—C48131.63 (8)
C35—C34—H34A108.4C41—Hf2—C48135.67 (9)
C33—C34—H34A108.4C50—Hf2—C4853.17 (9)
C35—C34—H34B108.4C40—Hf2—C48156.01 (9)
C33—C34—H34B108.4C47—Hf2—C4831.96 (8)
H34A—C34—H34B107.5C49—Hf2—C4831.89 (8)
C36—C35—C34113.2 (3)C29—Hf2—C51119.57 (9)
C36—C35—H35A108.9C33—Hf2—C51125.89 (10)
C34—C35—H35A108.9C37—Hf2—C5189.54 (9)
C36—C35—H35B108.9C41—Hf2—C5182.81 (8)
C34—C35—H35B108.9C50—Hf2—C5132.22 (9)
H35A—C35—H35B107.8C40—Hf2—C51109.15 (9)
C35—C36—H36A109.5C47—Hf2—C5132.07 (8)
C35—C36—H36B109.5C49—Hf2—C5153.15 (9)
H36A—C36—H36B109.5C48—Hf2—C5152.86 (9)
C35—C36—H36C109.5C29—Hf2—C3991.27 (9)
H36A—C36—H36C109.5C33—Hf2—C3979.24 (9)
H36B—C36—H36C109.5C37—Hf2—C3953.24 (9)
C38—C37—C41107.8 (2)C41—Hf2—C3953.20 (8)
C38—C37—C42124.8 (3)C50—Hf2—C39134.93 (9)
C41—C37—C42127.0 (3)C40—Hf2—C3932.12 (9)
C38—C37—Hf276.13 (15)C47—Hf2—C39152.81 (9)
C41—C37—Hf273.82 (14)C49—Hf2—C39151.13 (9)
C42—C37—Hf2122.37 (18)C48—Hf2—C39170.84 (9)
C39—C38—C37107.9 (2)C51—Hf2—C39135.97 (8)
C39—C38—C43123.9 (3)C29—Hf2—C3876.90 (9)
C37—C38—C43127.0 (3)C33—Hf2—C38107.64 (9)
C39—C38—Hf274.07 (15)C37—Hf2—C3832.26 (10)
C37—C38—Hf271.61 (13)C41—Hf2—C3853.35 (9)
C43—C38—Hf2129.46 (18)C50—Hf2—C38142.73 (9)
C38—C39—C40108.2 (2)C40—Hf2—C3853.11 (9)
C38—C39—C44123.9 (3)C47—Hf2—C38122.76 (8)
C40—C39—C44127.4 (3)C49—Hf2—C38174.29 (9)
C38—C39—Hf274.25 (14)C48—Hf2—C38146.89 (8)
C40—C39—Hf272.30 (15)C51—Hf2—C38121.16 (9)
C44—C39—Hf2125.08 (19)C39—Hf2—C3831.68 (9)

Experimental details

Crystal data
Chemical formula[Hf(C10H15)2(C4H9)2]
Mr563.15
Crystal system, space groupOrthorhombic, P212121
Temperature (K)170
a, b, c (Å)17.1572 (3), 17.2320 (3), 17.2966 (3)
V3)5113.79 (15)
Z8
Radiation typeMo Kα
µ (mm1)4.09
Crystal size (mm)0.39 × 0.27 × 0.17
Data collection
DiffractometerBruker Kappa APEXII DUO CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2008)
Tmin, Tmax0.30, 0.54
No. of measured, independent and
observed [I > 2σ(I)] reflections
123798, 13236, 12433
Rint0.037
(sin θ/λ)max1)0.677
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.018, 0.038, 1.06
No. of reflections13236
No. of parameters548
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.53, 0.77
Absolute structureFlack (1983), 999 Friedel pairs
Absolute structure parameter0.471 (5)

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL2014 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

 

Acknowledgements

We would like to thank our technical and analytical staff for assistance. Financial support by Deutsche Forschungsgemeinschaft (RO 1269/9–1) and the Russian Foundation for Basic Research (project code 15–03–03485) is gratefully acknowledged.

References

First citationBruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationBurlakov, V. V., Beweries, T., Bogdanov, V. S., Arndt, P., Baumann, W., Petrovskii, P. V., Spannenberg, A., Lyssenko, K. A., Shur, V. B. & Rosenthal, U. (2009). Organometallics, 28, 2864–2870.  Google Scholar
First citationBurlakov, V. V., Bogdanov, V. S., Lyssenko, K. A., Petrovskii, P. V., Beweries, T., Arndt, P., Rosenthal, U. & Shur, V. B. (2008). Russ. Chem. Bull. 57, 1319–1320.  Google Scholar
First citationCalhorda, M. J., Carrondo, M. A. A. F. de C. T., Dias, A. R., Galvão, A. M., Garcia, M. H., Martins, A. M., Minas da Piedade, M. E., Pinheiro, C. I., Romão, C. C., Simões, J. A. M. & Veiros, L. F. (1991). Organometallics, 10, 483–494.  Google Scholar
First citationErnst, R. D., Harvey, B. G. & Arif, A. M. (2004). Z. Kristallogr. New Cryst. Struct., 219, 398–400.  Google Scholar
First citationFlack, H. D. (1983). Acta Cryst. A39, 876–881.  CrossRef CAS Web of Science IUCr Journals Google Scholar
First citationPaolucci, G., Pojana, G., Zanon, J., Lucchini, V. & Avtomonov, E. (1997). Organometallics, 16, 5312–5320.  Google Scholar
First citationSchock, L. E. & Marks, T. J. (1988). J. Am. Chem. Soc. 110, 7701–7715.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 71| Part 2| February 2015| Pages m19-m20
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