supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers buy article online

ng2360 scheme

Acta Cryst. (2007). E63, m2972    [ doi:10.1107/S1600536807055614 ]

(1,2-Dimethoxyethane-[kappa]O)bis(tri-tert-butoxysilanethiolato-[kappa]2O,S)chromium(II)

A. Ciborska, K. Baranowska and W. Wojnowski

Abstract top

The title compound, [Cr(C4H10O2)(C12H27O3SSi)2], is a molecular chromium(II) thiolate that has the 1,2-dimethoxyethane ligand coordinating through one of its two O atoms. The metal is O,S-chelated by the thiolate anion, and the O atom from the 1,2-dimethoxyethane ligand occupies the apical position of the square-pyramidal coodination geometry. The asymmetric unit contains two molecules. Three C atoms of one tBu group are disordered approximately equally over two positions. One C atom of another tBu group is disordered over two positions, with site occupancies of ca. 0.6 and 0.4.

Comment top

Here we report the structure of the title complex (I), which results from the reaction of CrCl2 with (OtBu)3SiSNa in dimethoxyethane solution. In this complex, tri-tert-butoxysilanethiol serves both as an S-only and as an O,S ligand. The property has also been observed for other silanethiolates, for example (Wojnowski et al., 1985; Becker et al., 1996; Dołęga et al., 2006). Complex (I) is centrosymmetric about the chromium atom (Fig. 1). This coordination geometry is further reflected in the O—Cr—O angles, which are very close to 90°. The Cr—S distances are very similar to average values of ca 2.4 Å observed in the silanethiolates complexes (Ciborska et al., 2007) and thiolate complexes (Okura et al., 1985; Nguyen et al., 2005). The Cr—O(DME) bond length is longer than the Cr—O(THF) distance in Cr(C12H27O3SSi)2(C4H8O). The others important bond lengths and angles are collected in Table 1. Molecules pack in the crystal structure as discrete entities, with no intermolecular contacts (Fig. 2). Compound (I) is a analogue of the recently published THF compound (Ciborska et al., 2007).

Related literature top

For the THF-coordinated analogue, see: Ciborska et al. (2007). For other O,S-chelated chromium compounds, see: Becker et al. (1996); Dołęga et al. (2006); Wojnowski et al. (1985). For synthetic procedures, see: Piękoś & Wojnowski (1962); Wojnowska & Wojnowski (1974). For comparison Cr—S bond lengths, see: Okura et al. (1985); Nguyen et al. (2005); Ciborska et al. (2007).

Experimental top

All manipulations were performer under an atmosphere of nitrogen using standard Schlenk techniques. The (tBuO)3SiSNa was prepared by literature methods (Piękoś & Wojnowski, 1962; Wojnowska &Wojnowski, 1974). A dimethoxyethane solution (15 ml) of CrCl2 (0,196 g, 1,6 mmol) was added to a dimethoxyethane solution (10 ml) of (tBuO)3SiSNa (1 g, 3,3 mmol) at room temperature. The resulting pale green solution was refluxed for 24 h and filtered. Concentration and cooling (−23°C) of this solution gave colourless crystals of (I), suitable for X-ray diffraction analysis.

Refinement top

All H atoms were refined as riding on C atoms with methyl C—H = 0.98 Å, methylene C—H = 0.99 Å and Uiso(H) = 1.2Ueq(C) for CH2 groups and 1.5Ueq(C) for methyl groups. One tert-butyl group in (I) was found disordered in two positions; C10–C12 with probabilities of 0.513 (5) and 0.487 (5), and atom C38 with site occupation factors of 0.42 (5) and 0.58 (5).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduction: CrysAlis RED (Oxford Diffraction, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. A view of the molecule of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms of tert-butyl groups and of 1,2- dimethoxyethan have been omitted.
[Figure 2] Fig. 2. A packing diagram of (I), viewed along the a-axis. Cr atoms are purple, S atoms are yellow, Si atoms are green, O atoms are red, C atoms are white. H atoms of tert-butyl groups and of 1,2- dimethoxyethan have been omitted.
(1,2-Dimethoxyethane-κO)bis(tri-tert-butoxysilanethiolato- κ2O,S)chromium(II) top
Crystal data top
[Cr(C4H10O2)(C12H27O3SSi)2]Z = 4
Mr = 701.09F000 = 1520
Triclinic, P1Dx = 1.164 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 8.6809 (3) ÅCell parameters from 32370 reflections
b = 21.3180 (9) Åθ = 2.1–32.5º
c = 21.7316 (10) ŵ = 0.49 mm−1
α = 87.828 (4)ºT = 150 (2) K
β = 84.745 (4)ºPrism, colourless
γ = 88.372 (3)º0.38 × 0.38 × 0.21 mm
V = 4000.6 (3) Å3
Data collection top
Oxford Diffraction KM4 CCD
diffractometer		12702 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.016
Detector resolution: 8.1883 pixels mm-1θmax = 25.1º
T = 150(2) Kθmin = 2.1º
ω scans, 0.75 deg widthh = −10→10
Absorption correction: nonek = −22→25
27543 measured reflectionsl = −25→25
14104 independent 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)] = 0.035H-atom parameters constrained
wR(F2) = 0.097  w = 1/[σ2(Fo2) + (0.0584P)2 + 1.4202P]
where P = (Fo2 + 2Fc2)/3
S = 1.14(Δ/σ)max = 0.003
14104 reflectionsΔρmax = 0.52 e Å−3
821 parametersΔρmin = −0.42 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Cr(C4H10O2)(C12H27O3SSi)2]γ = 88.372 (3)º
Mr = 701.09V = 4000.6 (3) Å3
Triclinic, P1Z = 4
a = 8.6809 (3) ÅMo Kα
b = 21.3180 (9) ŵ = 0.49 mm−1
c = 21.7316 (10) ÅT = 150 (2) K
α = 87.828 (4)º0.38 × 0.38 × 0.21 mm
β = 84.745 (4)º
Data collection top
Oxford Diffraction KM4 CCD
diffractometer		14104 independent reflections
Absorption correction: none12702 reflections with I > 2σ(I)
27543 measured reflectionsRint = 0.016
Refinement top
R[F2 > 2σ(F2)] = 0.035821 parameters
wR(F2) = 0.097H-atom parameters constrained
S = 1.14Δρmax = 0.52 e Å−3
14104 reflectionsΔρmin = −0.42 e Å−3
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*/UeqOcc. (<1)
C10.70845 (19)0.28522 (10)0.42446 (8)0.0270 (4)
C20.6467 (2)0.35164 (10)0.41363 (9)0.0329 (4)
H2A0.6890.37960.44230.049*
H2B0.53350.35240.42060.049*
H2C0.67760.36580.3710.049*
C30.6515 (2)0.23944 (10)0.38053 (10)0.0320 (4)
H3A0.68960.25150.3380.048*
H3B0.53810.24020.38440.048*
H3C0.690.1970.39070.048*
C40.6634 (2)0.26328 (13)0.49108 (10)0.0433 (6)
H4A0.71270.22220.49910.065*
H4B0.55070.25980.49770.065*
H4C0.69780.29370.51930.065*
C51.0449 (3)0.12730 (9)0.42336 (10)0.0405 (5)
C61.0281 (3)0.14287 (10)0.35535 (10)0.0400 (5)
H6A0.92030.1550.350.06*
H6B1.05780.10590.3310.06*
H6C1.09530.17770.34120.06*
C70.9382 (5)0.07414 (12)0.44652 (16)0.0830 (11)
H7A0.9490.06490.49050.125*
H7B0.96630.03660.42290.125*
H7C0.83080.08680.44110.125*
C81.2114 (4)0.11179 (13)0.43290 (12)0.0617 (8)
H8A1.27430.14860.42130.093*
H8B1.24820.07670.40710.093*
H8C1.22020.10.47650.093*
C91.0542 (2)0.27704 (10)0.57819 (8)0.0295 (4)
C100.9863 (8)0.2200 (3)0.6106 (2)0.070 (2)0.513 (5)
H10A0.8740.22610.61810.105*0.513 (5)
H10B1.03110.21280.65010.105*0.513 (5)
H10C1.00930.18360.58480.105*0.513 (5)
C111.0150 (8)0.3355 (3)0.6132 (2)0.0616 (19)0.513 (5)
H11A1.05850.37190.58940.092*0.513 (5)
H11B1.05840.33190.65330.092*0.513 (5)
H11C0.90230.3410.61970.092*0.513 (5)
C121.2301 (5)0.2685 (3)0.5664 (2)0.0559 (17)0.513 (5)
H12A1.25460.23150.54160.084*0.513 (5)
H12B1.27530.26280.6060.084*0.513 (5)
H12C1.27310.30580.54410.084*0.513 (5)
C10A1.1352 (8)0.2145 (3)0.5844 (2)0.064 (2)0.487 (5)
H10D1.05990.18110.58450.095*0.487 (5)
H10E1.18450.21180.62330.095*0.487 (5)
H10F1.21420.20950.54960.095*0.487 (5)
C11A0.9224 (6)0.2830 (3)0.6298 (2)0.0548 (18)0.487 (5)
H11D0.86610.3230.62430.082*0.487 (5)
H11E0.96550.28150.670.082*0.487 (5)
H11F0.85150.24820.62820.082*0.487 (5)
C12A1.1620 (8)0.3311 (3)0.5788 (3)0.073 (2)0.487 (5)
H12D1.24390.32740.54490.11*0.487 (5)
H12E1.20840.33030.61830.11*0.487 (5)
H12F1.10390.37070.57360.11*0.487 (5)
C131.33304 (18)0.36231 (9)0.24341 (8)0.0213 (4)
C141.4062 (2)0.29707 (9)0.24427 (9)0.0291 (4)
H14A1.36990.27440.28270.044*
H14B1.5190.30010.24180.044*
H14C1.3770.27440.20890.044*
C151.3798 (2)0.40187 (9)0.29508 (8)0.0252 (4)
H15A1.32280.44220.29470.038*
H15B1.49120.40920.28890.038*
H15C1.35560.37970.3350.038*
C161.3752 (2)0.39646 (11)0.18157 (9)0.0333 (5)
H16A1.33810.37290.14830.05*
H16B1.48790.39990.17480.05*
H16C1.32680.43860.18190.05*
C171.0489 (2)0.24676 (8)0.13400 (9)0.0261 (4)
C181.0608 (2)0.20439 (9)0.19140 (10)0.0331 (4)
H18A1.16290.20840.20650.05*
H18B1.04670.16070.18110.05*
H18C0.98040.21680.22360.05*
C191.1709 (3)0.22733 (10)0.08315 (10)0.0392 (5)
H19A1.16780.25690.04760.059*
H19B1.150.1850.07040.059*
H19C1.27340.22750.09860.059*
C200.8874 (3)0.24609 (11)0.11278 (11)0.0417 (5)
H20A0.81280.26250.14520.063*
H20B0.86160.20290.10450.063*
H20C0.88340.27240.0750.063*
C210.9853 (2)0.45813 (8)0.11767 (8)0.0252 (4)
C221.1029 (3)0.44335 (12)0.06350 (10)0.0443 (6)
H22A1.20360.45970.0710.066*
H22B1.06850.4630.02550.066*
H22C1.11230.39780.05920.066*
C230.8264 (3)0.43494 (10)0.10801 (11)0.0413 (5)
H23A0.83320.38980.10070.062*
H23B0.78750.45740.07220.062*
H23C0.75570.44260.14490.062*
C240.9775 (3)0.52780 (9)0.12900 (10)0.0380 (5)
H24A0.90360.5360.16480.057*
H24B0.94370.55070.09240.057*
H24C1.08010.54180.13710.057*
C250.9560 (3)0.48230 (10)0.33693 (11)0.0428 (5)
H25A0.85370.49770.35350.064*
H25B0.95250.47170.29360.064*
H25C1.0320.5150.33970.064*
C261.0141 (2)0.43783 (10)0.43569 (9)0.0342 (4)
H26A0.98610.3990.46020.041*
H26B0.94020.47160.44990.041*
C271.1742 (3)0.45543 (10)0.44773 (9)0.0362 (5)
H27A1.1860.45080.49260.043*
H27B1.25080.42680.42590.043*
C281.3538 (4)0.53529 (15)0.43686 (13)0.0652 (8)
H28A1.36930.52980.48090.098*
H28B1.36830.57940.42370.098*
H28C1.42890.50870.41270.098*
C290.80317 (19)0.06784 (9)0.77367 (10)0.0276 (4)
C300.8774 (2)0.11637 (10)0.72867 (10)0.0333 (4)
H30A0.84530.11020.68730.05*
H30B0.99030.11180.72760.05*
H30C0.84490.15850.74190.05*
C310.8533 (2)0.07277 (10)0.83835 (10)0.0327 (4)
H31A0.82980.11530.85280.049*
H31B0.96480.0640.83770.049*
H31C0.79750.04230.86630.049*
C320.8401 (2)0.00221 (10)0.75049 (13)0.0460 (6)
H32A0.7955−0.02890.78080.069*
H32B0.9526−0.00450.74470.069*
H32C0.7961−0.00220.7110.069*
C330.4360 (2)−0.08711 (8)0.77133 (9)0.0297 (4)
C340.4596 (3)−0.12696 (11)0.82988 (12)0.0496 (6)
H34A0.5705−0.13190.83460.074*
H34B0.4153−0.16830.82670.074*
H34C0.4081−0.10610.86590.074*
C350.5228 (3)−0.11776 (11)0.71600 (12)0.0478 (6)
H35A0.5123−0.09120.67880.072*
H35B0.4797−0.1590.71060.072*
H35C0.6325−0.12290.72290.072*
C360.2675 (3)−0.07706 (12)0.76294 (15)0.0553 (7)
H36A0.2157−0.0570.79930.083*
H36B0.2206−0.11760.75790.083*
H36C0.256−0.050.72610.083*
C370.4894 (3)0.07508 (11)0.62279 (10)0.0473 (6)
C380.631 (3)0.0626 (8)0.5691 (7)0.058 (4)0.42 (5)
H38A0.73050.06870.5860.087*0.42 (5)
H38B0.62080.09210.5340.087*0.42 (5)
H38C0.62750.01950.55520.087*0.42 (5)
C38A0.572 (3)0.0454 (12)0.5682 (5)0.071 (4)0.58 (5)
H38D0.68340.04510.57170.107*0.58 (5)
H38E0.54840.06920.53050.107*0.58 (5)
H38F0.53760.00210.56610.107*0.58 (5)
C390.3213 (4)0.06326 (14)0.61343 (13)0.0683 (9)
H39A0.30780.01820.6090.102*
H39B0.29310.08630.57610.102*
H39C0.25470.07760.64930.102*
C400.5144 (3)0.14403 (11)0.63386 (12)0.0513 (6)
H40A0.44260.15770.66850.077*
H40B0.49540.16930.59660.077*
H40C0.62110.14940.64360.077*
C410.19308 (18)0.24842 (8)0.85513 (8)0.0214 (4)
C420.1260 (2)0.19445 (9)0.89539 (9)0.0252 (4)
H42A0.15260.15480.87520.038*
H42B0.01320.19980.90140.038*
H42C0.16880.19390.93560.038*
C430.1372 (2)0.25078 (9)0.79080 (9)0.0282 (4)
H43A0.17950.28760.76740.042*
H43B0.02390.25370.79410.042*
H43C0.17220.21260.76940.042*
C440.1533 (2)0.31001 (9)0.88668 (10)0.0324 (4)
H44A0.18980.30790.92810.049*
H44B0.04090.31730.89010.049*
H44C0.20350.34450.86220.049*
C450.5522 (2)0.35694 (9)0.95746 (9)0.0280 (4)
C460.5132 (2)0.34058 (11)1.02538 (9)0.0392 (5)
H46A0.40050.34061.03460.059*
H46B0.55730.37171.05030.059*
H46C0.55650.29881.03520.059*
C470.7269 (2)0.35374 (12)0.94174 (10)0.0429 (6)
H47A0.76670.31170.95270.064*
H47B0.77560.3850.96510.064*
H47C0.75070.36250.89730.064*
C480.4835 (3)0.42099 (10)0.94066 (12)0.0496 (6)
H48A0.50340.42950.8960.074*
H48B0.53130.45330.9630.074*
H48C0.37170.42150.95210.074*
C490.5261 (2)0.37284 (9)0.74822 (9)0.0291 (4)
C500.6892 (3)0.39694 (10)0.74655 (10)0.0393 (5)
H50A0.69170.43020.77640.059*
H50B0.72140.41380.70490.059*
H50C0.75990.36240.75730.059*
C510.5195 (3)0.31975 (10)0.70355 (9)0.0373 (5)
H51A0.59430.28640.71340.056*
H51B0.54490.33590.66110.056*
H51C0.41520.30280.70740.056*
C520.4118 (3)0.42558 (11)0.73404 (12)0.0481 (6)
H52A0.30760.40880.73530.072*
H52B0.44090.44410.69280.072*
H52C0.41310.45790.76490.072*
C530.4401 (3)0.04834 (9)0.93200 (10)0.0370 (5)
H53A0.52960.02520.94660.055*
H53B0.41230.03020.89390.055*
H53C0.35240.04550.96370.055*
C540.5027 (2)0.14608 (9)0.97425 (9)0.0298 (4)
H54A0.43590.12841.00970.036*
H54B0.47090.19070.9680.036*
C550.6677 (2)0.14282 (9)0.98987 (9)0.0306 (4)
H55A0.73710.15490.95290.037*
H55B0.68170.17261.02260.037*
C560.8646 (3)0.07441 (11)1.02153 (13)0.0474 (6)
H56A0.92940.0840.98320.071*
H56B0.88640.03121.03580.071*
H56C0.88720.10341.05330.071*
O10.88055 (13)0.28833 (6)0.41183 (5)0.0214 (3)
O20.99325 (16)0.18001 (6)0.46173 (6)0.0299 (3)
O30.98450 (14)0.28511 (6)0.52045 (6)0.0260 (3)
O41.16195 (12)0.35507 (5)0.25458 (5)0.0185 (2)
O51.08382 (14)0.31099 (5)0.14615 (5)0.0215 (3)
O61.03991 (14)0.42900 (6)0.17293 (5)0.0216 (3)
O70.99953 (16)0.42779 (6)0.37185 (6)0.0304 (3)
O81.2029 (2)0.51804 (7)0.42723 (7)0.0471 (4)
O90.63219 (13)0.08135 (5)0.77873 (6)0.0234 (3)
O100.50831 (14)−0.02842 (5)0.78013 (6)0.0230 (3)
O110.53121 (16)0.03569 (6)0.67500 (6)0.0294 (3)
O120.36414 (12)0.23727 (5)0.84763 (5)0.0183 (2)
O130.48026 (13)0.30947 (5)0.92475 (5)0.0213 (3)
O140.47807 (14)0.35165 (6)0.81096 (6)0.0244 (3)
O150.47810 (15)0.11296 (6)0.92004 (6)0.0272 (3)
O160.70647 (16)0.08111 (6)1.01049 (7)0.0341 (3)
Si11.01765 (5)0.25499 (2)0.45317 (2)0.01928 (11)
Si21.03128 (5)0.35793 (2)0.20198 (2)0.01669 (10)
Si30.49386 (5)0.04145 (2)0.74897 (2)0.01813 (10)
Si40.50487 (5)0.28879 (2)0.85326 (2)0.01674 (10)
S11.21321 (5)0.28461 (2)0.40067 (2)0.02403 (10)
S20.83362 (5)0.33759 (2)0.257828 (19)0.02265 (10)
S30.30171 (5)0.09422 (2)0.77934 (2)0.02244 (10)
S40.69667 (5)0.233062 (19)0.82966 (2)0.02145 (10)
Cr11.02010 (3)0.326594 (12)0.334825 (12)0.01619 (7)
Cr20.49821 (3)0.156658 (12)0.818976 (12)0.01619 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0125 (8)0.0450 (11)0.0223 (9)0.0009 (7)0.0012 (7)0.0060 (8)
C20.0218 (9)0.0451 (12)0.0305 (10)0.0097 (8)0.0011 (8)−0.0030 (9)
C30.0188 (9)0.0402 (11)0.0369 (11)−0.0068 (8)−0.0025 (8)0.0043 (9)
C40.0215 (10)0.0783 (17)0.0277 (11)−0.0015 (10)0.0033 (8)0.0155 (11)
C50.0626 (15)0.0214 (10)0.0354 (12)0.0067 (9)0.0042 (10)0.0000 (8)
C60.0509 (13)0.0349 (11)0.0349 (12)0.0085 (10)−0.0058 (10)−0.0119 (9)
C70.140 (3)0.0244 (13)0.078 (2)−0.0131 (16)0.030 (2)−0.0018 (13)
C80.087 (2)0.0579 (16)0.0391 (14)0.0454 (15)−0.0119 (13)−0.0023 (12)
C90.0329 (10)0.0413 (11)0.0146 (9)0.0028 (8)−0.0058 (7)0.0027 (8)
C100.102 (5)0.080 (4)0.030 (3)−0.041 (4)−0.022 (3)0.026 (3)
C110.090 (5)0.068 (4)0.029 (2)0.032 (3)−0.021 (3)−0.019 (2)
C120.038 (3)0.101 (5)0.030 (2)0.011 (3)−0.0137 (19)−0.004 (3)
C10A0.076 (4)0.085 (4)0.030 (3)0.045 (4)−0.024 (3)−0.003 (3)
C11A0.052 (3)0.092 (5)0.017 (2)0.019 (3)0.001 (2)0.002 (2)
C12A0.088 (5)0.096 (5)0.042 (3)−0.038 (4)−0.036 (3)0.004 (3)
C130.0110 (8)0.0328 (10)0.0203 (9)−0.0041 (7)−0.0016 (6)−0.0017 (7)
C140.0159 (8)0.0375 (11)0.0343 (10)0.0020 (7)−0.0011 (7)−0.0101 (8)
C150.0221 (9)0.0309 (10)0.0232 (9)−0.0077 (7)−0.0036 (7)−0.0019 (7)
C160.0210 (9)0.0569 (13)0.0220 (10)−0.0117 (9)−0.0003 (7)0.0033 (9)
C170.0322 (10)0.0198 (9)0.0272 (10)−0.0063 (7)−0.0044 (8)−0.0051 (7)
C180.0373 (11)0.0239 (10)0.0374 (11)−0.0039 (8)0.0003 (9)0.0034 (8)
C190.0539 (13)0.0293 (11)0.0333 (11)−0.0049 (9)0.0073 (10)−0.0116 (9)
C200.0429 (12)0.0384 (12)0.0479 (13)−0.0085 (10)−0.0198 (10)−0.0124 (10)
C210.0294 (9)0.0238 (9)0.0219 (9)0.0032 (7)−0.0045 (7)0.0053 (7)
C220.0558 (14)0.0486 (13)0.0249 (11)0.0208 (11)0.0037 (10)0.0104 (9)
C230.0420 (12)0.0380 (12)0.0467 (13)−0.0044 (9)−0.0235 (10)0.0115 (10)
C240.0496 (13)0.0259 (10)0.0384 (12)0.0018 (9)−0.0068 (10)0.0042 (9)
C250.0599 (15)0.0271 (11)0.0425 (13)0.0091 (10)−0.0138 (11)−0.0014 (9)
C260.0456 (12)0.0309 (10)0.0253 (10)0.0034 (9)0.0026 (9)−0.0088 (8)
C270.0518 (13)0.0317 (11)0.0254 (10)0.0045 (9)−0.0036 (9)−0.0088 (8)
C280.080 (2)0.076 (2)0.0418 (15)−0.0345 (16)−0.0110 (13)−0.0041 (13)
C290.0114 (8)0.0266 (9)0.0457 (12)0.0034 (7)−0.0033 (7)−0.0132 (8)
C300.0174 (9)0.0423 (12)0.0400 (11)0.0005 (8)0.0026 (8)−0.0123 (9)
C310.0201 (9)0.0324 (10)0.0464 (12)0.0046 (8)−0.0099 (8)−0.0016 (9)
C320.0194 (10)0.0354 (12)0.0851 (18)0.0078 (8)−0.0079 (10)−0.0271 (12)
C330.0334 (10)0.0185 (9)0.0368 (11)−0.0073 (7)0.0022 (8)−0.0043 (8)
C340.0620 (16)0.0309 (12)0.0532 (15)−0.0014 (11)0.0054 (12)0.0081 (10)
C350.0631 (16)0.0307 (11)0.0495 (14)−0.0046 (10)0.0020 (12)−0.0135 (10)
C360.0370 (13)0.0374 (13)0.093 (2)−0.0127 (10)−0.0111 (13)−0.0021 (13)
C370.0700 (16)0.0472 (13)0.0224 (10)0.0285 (12)−0.0029 (10)0.0050 (9)
C380.091 (10)0.046 (6)0.028 (4)0.024 (6)0.028 (6)0.005 (4)
C38A0.083 (9)0.094 (8)0.028 (3)0.045 (6)0.015 (4)0.027 (4)
C390.098 (2)0.0595 (17)0.0553 (17)0.0180 (16)−0.0532 (17)−0.0090 (13)
C400.0541 (15)0.0444 (14)0.0511 (15)0.0132 (11)0.0041 (11)0.0219 (11)
C410.0107 (8)0.0222 (9)0.0313 (10)0.0006 (6)0.0003 (7)−0.0044 (7)
C420.0180 (8)0.0286 (9)0.0284 (10)−0.0025 (7)0.0037 (7)−0.0048 (8)
C430.0179 (9)0.0302 (10)0.0367 (11)0.0015 (7)−0.0056 (7)0.0029 (8)
C440.0185 (9)0.0252 (10)0.0528 (13)0.0016 (7)0.0032 (8)−0.0110 (9)
C450.0272 (9)0.0302 (10)0.0275 (10)−0.0094 (8)0.0015 (7)−0.0139 (8)
C460.0341 (11)0.0573 (14)0.0271 (11)−0.0136 (10)0.0022 (8)−0.0164 (10)
C470.0307 (11)0.0610 (15)0.0379 (12)−0.0209 (10)0.0060 (9)−0.0223 (11)
C480.0702 (17)0.0276 (11)0.0519 (15)−0.0037 (11)−0.0034 (12)−0.0173 (10)
C490.0349 (10)0.0264 (10)0.0242 (10)−0.0029 (8)0.0038 (8)0.0072 (8)
C500.0428 (12)0.0351 (11)0.0382 (12)−0.0128 (9)0.0082 (9)0.0014 (9)
C510.0447 (12)0.0409 (12)0.0261 (10)−0.0085 (9)0.0006 (9)−0.0004 (9)
C520.0536 (14)0.0441 (13)0.0429 (13)0.0095 (11)0.0035 (11)0.0192 (10)
C530.0533 (13)0.0257 (10)0.0332 (11)−0.0123 (9)−0.0101 (9)0.0057 (8)
C540.0393 (11)0.0264 (10)0.0238 (10)0.0003 (8)−0.0039 (8)−0.0014 (8)
C550.0409 (11)0.0256 (10)0.0266 (10)−0.0053 (8)−0.0088 (8)−0.0018 (8)
C560.0401 (12)0.0421 (13)0.0629 (16)0.0045 (10)−0.0190 (11)−0.0080 (11)
O10.0136 (6)0.0318 (7)0.0181 (6)0.0003 (5)−0.0008 (4)0.0050 (5)
O20.0395 (8)0.0250 (7)0.0234 (7)0.0021 (6)0.0039 (6)0.0031 (5)
O30.0261 (6)0.0348 (7)0.0171 (6)0.0080 (5)−0.0043 (5)−0.0010 (5)
O40.0129 (5)0.0273 (6)0.0151 (6)−0.0023 (4)−0.0007 (4)0.0008 (5)
O50.0265 (6)0.0201 (6)0.0181 (6)−0.0059 (5)−0.0013 (5)−0.0017 (5)
O60.0243 (6)0.0228 (6)0.0180 (6)−0.0007 (5)−0.0036 (5)0.0011 (5)
O70.0410 (8)0.0251 (7)0.0252 (7)0.0049 (6)−0.0037 (6)−0.0041 (5)
O80.0686 (11)0.0389 (9)0.0363 (9)−0.0143 (8)−0.0139 (8)−0.0025 (7)
O90.0126 (6)0.0205 (6)0.0381 (7)0.0016 (5)−0.0030 (5)−0.0109 (5)
O100.0230 (6)0.0176 (6)0.0290 (7)−0.0011 (5)−0.0046 (5)−0.0023 (5)
O110.0388 (8)0.0280 (7)0.0209 (7)0.0130 (6)−0.0034 (5)−0.0018 (5)
O120.0121 (5)0.0172 (6)0.0256 (6)0.0003 (4)−0.0008 (4)−0.0040 (5)
O130.0213 (6)0.0211 (6)0.0217 (6)−0.0046 (5)0.0003 (5)−0.0057 (5)
O140.0278 (7)0.0197 (6)0.0242 (7)0.0004 (5)0.0041 (5)0.0011 (5)
O150.0363 (7)0.0231 (6)0.0231 (7)−0.0059 (5)−0.0076 (5)0.0021 (5)
O160.0352 (8)0.0284 (7)0.0396 (8)−0.0003 (6)−0.0098 (6)0.0005 (6)
Si10.0178 (2)0.0244 (2)0.0153 (2)0.00282 (18)−0.00170 (17)0.00259 (18)
Si20.0157 (2)0.0206 (2)0.0140 (2)−0.00209 (17)−0.00261 (17)0.00074 (17)
Si30.0157 (2)0.0168 (2)0.0225 (2)0.00117 (17)−0.00403 (17)−0.00487 (18)
Si40.0150 (2)0.0148 (2)0.0202 (2)−0.00163 (16)0.00031 (17)−0.00285 (17)
S10.0148 (2)0.0348 (2)0.0221 (2)0.00182 (17)−0.00275 (16)0.00556 (18)
S20.0143 (2)0.0361 (2)0.0176 (2)−0.00300 (17)−0.00285 (15)0.00343 (17)
S30.0140 (2)0.0221 (2)0.0323 (2)0.00120 (16)−0.00492 (17)−0.01009 (18)
S40.01327 (19)0.0193 (2)0.0319 (2)−0.00123 (15)0.00013 (16)−0.00643 (17)
Cr10.01336 (13)0.02138 (14)0.01365 (14)0.00070 (10)−0.00128 (10)0.00082 (10)
Cr20.01234 (13)0.01478 (13)0.02179 (15)−0.00002 (10)−0.00202 (10)−0.00415 (10)
Geometric parameters (Å, °) top
C1—O11.497 (2)C31—H31C0.98
C1—C31.514 (3)C32—H32A0.98
C1—C21.517 (3)C32—H32B0.98
C1—C41.524 (3)C32—H32C0.98
C2—H2A0.98C33—O101.443 (2)
C2—H2B0.98C33—C361.499 (3)
C2—H2C0.98C33—C351.519 (3)
C3—H3A0.98C33—C341.529 (3)
C3—H3B0.98C34—H34A0.98
C3—H3C0.98C34—H34B0.98
C4—H4A0.98C34—H34C0.98
C4—H4B0.98C35—H35A0.98
C4—H4C0.98C35—H35B0.98
C5—O21.460 (2)C35—H35C0.98
C5—C81.505 (4)C36—H36A0.98
C5—C61.522 (3)C36—H36B0.98
C5—C71.525 (4)C36—H36C0.98
C6—H6A0.98C37—O111.453 (2)
C6—H6B0.98C37—C38A1.482 (12)
C6—H6C0.98C37—C391.521 (4)
C7—H7A0.98C37—C401.523 (4)
C7—H7B0.98C37—C381.64 (2)
C7—H7C0.98C38—H38A0.98
C8—H8A0.98C38—H38B0.98
C8—H8B0.98C38—H38C0.98
C8—H8C0.98C38A—H38D0.98
C9—O31.445 (2)C38A—H38E0.98
C9—C101.490 (5)C38A—H38F0.98
C9—C10A1.497 (6)C39—H39A0.98
C9—C111.500 (5)C39—H39B0.98
C9—C12A1.506 (6)C39—H39C0.98
C9—C121.532 (5)C40—H40A0.98
C9—C11A1.534 (5)C40—H40B0.98
C10—H10A0.98C40—H40C0.98
C10—H10B0.98C41—O121.4923 (19)
C10—H10C0.98C41—C421.515 (3)
C11—H11A0.98C41—C431.520 (3)
C11—H11B0.98C41—C441.521 (2)
C11—H11C0.98C42—H42A0.98
C12—H12A0.98C42—H42B0.98
C12—H12B0.98C42—H42C0.98
C12—H12C0.98C43—H43A0.98
C10A—H10D0.98C43—H43B0.98
C10A—H10E0.98C43—H43C0.98
C10A—H10F0.98C44—H44A0.98
C11A—H11D0.98C44—H44B0.98
C11A—H11E0.98C44—H44C0.98
C11A—H11F0.98C45—O131.446 (2)
C12A—H12D0.98C45—C461.514 (3)
C12A—H12E0.98C45—C481.519 (3)
C12A—H12F0.98C45—C471.524 (3)
C13—O41.4942 (19)C46—H46A0.98
C13—C141.513 (3)C46—H46B0.98
C13—C151.521 (2)C46—H46C0.98
C13—C161.524 (3)C47—H47A0.98
C14—H14A0.98C47—H47B0.98
C14—H14B0.98C47—H47C0.98
C14—H14C0.98C48—H48A0.98
C15—H15A0.98C48—H48B0.98
C15—H15B0.98C48—H48C0.98
C15—H15C0.98C49—O141.448 (2)
C16—H16A0.98C49—C501.517 (3)
C16—H16B0.98C49—C521.520 (3)
C16—H16C0.98C49—C511.524 (3)
C17—O51.450 (2)C50—H50A0.98
C17—C201.517 (3)C50—H50B0.98
C17—C191.519 (3)C50—H50C0.98
C17—C181.522 (3)C51—H51A0.98
C18—H18A0.98C51—H51B0.98
C18—H18B0.98C51—H51C0.98
C18—H18C0.98C52—H52A0.98
C19—H19A0.98C52—H52B0.98
C19—H19B0.98C52—H52C0.98
C19—H19C0.98C53—O151.434 (2)
C20—H20A0.98C53—H53A0.98
C20—H20B0.98C53—H53B0.98
C20—H20C0.98C53—H53C0.98
C21—O61.443 (2)C54—O151.432 (2)
C21—C241.513 (3)C54—C551.501 (3)
C21—C231.514 (3)C54—H54A0.99
C21—C221.522 (3)C54—H54B0.99
C22—H22A0.98C55—O161.415 (2)
C22—H22B0.98C55—H55A0.99
C22—H22C0.98C55—H55B0.99
C23—H23A0.98C56—O161.417 (3)
C23—H23B0.98C56—H56A0.98
C23—H23C0.98C56—H56B0.98
C24—H24A0.98C56—H56C0.98
C24—H24B0.98O1—Si11.6817 (12)
C24—H24C0.98O1—Cr12.1248 (12)
C25—O71.425 (2)O2—Si11.6198 (14)
C25—H25A0.98O3—Si11.6174 (13)
C25—H25B0.98O4—Si21.6809 (11)
C25—H25C0.98O4—Cr12.1201 (11)
C26—O71.429 (2)O5—Si21.6267 (12)
C26—C271.498 (3)O6—Si21.6201 (12)
C26—H26A0.99O7—Cr12.3273 (13)
C26—H26B0.99O9—Si31.6810 (12)
C27—O81.413 (3)O9—Cr22.1234 (12)
C27—H27A0.99O10—Si31.6191 (13)
C27—H27B0.99O11—Si31.6190 (13)
C28—O81.406 (3)O12—Si41.6816 (11)
C28—H28A0.98O12—Cr22.1283 (11)
C28—H28B0.98O13—Si41.6246 (12)
C28—H28C0.98O14—Si41.6195 (13)
C29—O91.4988 (19)O15—Cr22.3463 (13)
C29—C301.513 (3)Si1—S12.0577 (6)
C29—C311.517 (3)Si2—S22.0558 (6)
C29—C321.521 (3)Si3—S32.0570 (6)
C30—H30A0.98Si4—S42.0553 (6)
C30—H30B0.98S1—Cr12.4323 (5)
C30—H30C0.98S2—Cr12.4332 (5)
C31—H31A0.98S3—Cr22.4308 (5)
C31—H31B0.98S4—Cr22.4365 (5)
O1—C1—C3107.83 (14)C35—C33—C34109.37 (19)
O1—C1—C2105.77 (15)C33—C34—H34A109.5
C3—C1—C2112.57 (16)C33—C34—H34B109.5
O1—C1—C4110.98 (14)H34A—C34—H34B109.5
C3—C1—C4109.83 (17)C33—C34—H34C109.5
C2—C1—C4109.79 (17)H34A—C34—H34C109.5
C1—C2—H2A109.5H34B—C34—H34C109.5
C1—C2—H2B109.5C33—C35—H35A109.5
H2A—C2—H2B109.5C33—C35—H35B109.5
C1—C2—H2C109.5H35A—C35—H35B109.5
H2A—C2—H2C109.5C33—C35—H35C109.5
H2B—C2—H2C109.5H35A—C35—H35C109.5
C1—C3—H3A109.5H35B—C35—H35C109.5
C1—C3—H3B109.5C33—C36—H36A109.5
H3A—C3—H3B109.5C33—C36—H36B109.5
C1—C3—H3C109.5H36A—C36—H36B109.5
H3A—C3—H3C109.5C33—C36—H36C109.5
H3B—C3—H3C109.5H36A—C36—H36C109.5
C1—C4—H4A109.5H36B—C36—H36C109.5
C1—C4—H4B109.5O11—C37—C38A104.4 (5)
H4A—C4—H4B109.5O11—C37—C39107.9 (2)
C1—C4—H4C109.5C38A—C37—C39101.7 (12)
H4A—C4—H4C109.5O11—C37—C40110.83 (19)
H4B—C4—H4C109.5C38A—C37—C40119.6 (12)
O2—C5—C8108.47 (19)C39—C37—C40111.5 (2)
O2—C5—C6111.25 (16)O11—C37—C38103.9 (6)
C8—C5—C6110.2 (2)C39—C37—C38122.6 (10)
O2—C5—C7104.55 (19)C40—C37—C3899.7 (9)
C8—C5—C7112.1 (2)C37—C38—H38A109.5
C6—C5—C7110.2 (2)C37—C38—H38B109.5
C5—C6—H6A109.5C37—C38—H38C109.5
C5—C6—H6B109.5C37—C38A—H38D109.5
H6A—C6—H6B109.5C37—C38A—H38E109.5
C5—C6—H6C109.5H38D—C38A—H38E109.5
H6A—C6—H6C109.5C37—C38A—H38F109.5
H6B—C6—H6C109.5H38D—C38A—H38F109.5
C5—C7—H7A109.5H38E—C38A—H38F109.5
C5—C7—H7B109.5C37—C39—H39A109.5
H7A—C7—H7B109.5C37—C39—H39B109.5
C5—C7—H7C109.5H39A—C39—H39B109.5
H7A—C7—H7C109.5C37—C39—H39C109.5
H7B—C7—H7C109.5H39A—C39—H39C109.5
C5—C8—H8A109.5H39B—C39—H39C109.5
C5—C8—H8B109.5C37—C40—H40A109.5
H8A—C8—H8B109.5C37—C40—H40B109.5
C5—C8—H8C109.5H40A—C40—H40B109.5
H8A—C8—H8C109.5C37—C40—H40C109.5
H8B—C8—H8C109.5H40A—C40—H40C109.5
O3—C9—C10106.9 (2)H40B—C40—H40C109.5
O3—C9—C10A112.4 (2)O12—C41—C42106.75 (13)
C10—C9—C10A54.4 (4)O12—C41—C43107.17 (13)
O3—C9—C11106.4 (2)C42—C41—C43112.61 (15)
C10—C9—C11112.5 (4)O12—C41—C44110.51 (13)
C10A—C9—C11141.2 (3)C42—C41—C44109.54 (15)
O3—C9—C12A105.0 (3)C43—C41—C44110.19 (16)
C10—C9—C12A148.1 (3)C41—C42—H42A109.5
C10A—C9—C12A112.8 (4)C41—C42—H42B109.5
C11—C9—C12A56.4 (4)H42A—C42—H42B109.5
O3—C9—C12110.6 (2)C41—C42—H42C109.5
C10—C9—C12110.2 (4)H42A—C42—H42C109.5
C10A—C9—C1257.5 (4)H42B—C42—H42C109.5
C11—C9—C12110.1 (4)C41—C43—H43A109.5
C12A—C9—C1257.8 (4)C41—C43—H43B109.5
O3—C9—C11A106.6 (2)H43A—C43—H43B109.5
C10—C9—C11A59.3 (4)C41—C43—H43C109.5
C10A—C9—C11A109.7 (4)H43A—C43—H43C109.5
C11—C9—C11A55.6 (4)H43B—C43—H43C109.5
C12A—C9—C11A110.3 (4)C41—C44—H44A109.5
C12—C9—C11A142.8 (3)C41—C44—H44B109.5
C9—C10—H10A109.5H44A—C44—H44B109.5
C9—C10—H10B109.5C41—C44—H44C109.5
C9—C10—H10C109.5H44A—C44—H44C109.5
C9—C11—H11A109.5H44B—C44—H44C109.5
C9—C11—H11B109.5O13—C45—C46105.33 (15)
C9—C11—H11C109.5O13—C45—C48109.15 (16)
C9—C12—H12A109.5C46—C45—C48110.58 (18)
C9—C12—H12B109.5O13—C45—C47109.67 (15)
C9—C12—H12C109.5C46—C45—C47110.07 (18)
C9—C10A—H10D109.5C48—C45—C47111.82 (19)
C9—C10A—H10E109.5C45—C46—H46A109.5
H10D—C10A—H10E109.5C45—C46—H46B109.5
C9—C10A—H10F109.5H46A—C46—H46B109.5
H10D—C10A—H10F109.5C45—C46—H46C109.5
H10E—C10A—H10F109.5H46A—C46—H46C109.5
C9—C11A—H11D109.5H46B—C46—H46C109.5
C9—C11A—H11E109.5C45—C47—H47A109.5
H11D—C11A—H11E109.5C45—C47—H47B109.5
C9—C11A—H11F109.5H47A—C47—H47B109.5
H11D—C11A—H11F109.5C45—C47—H47C109.5
H11E—C11A—H11F109.5H47A—C47—H47C109.5
C9—C12A—H12D109.5H47B—C47—H47C109.5
C9—C12A—H12E109.5C45—C48—H48A109.5
H12D—C12A—H12E109.5C45—C48—H48B109.5
C9—C12A—H12F109.5H48A—C48—H48B109.5
H12D—C12A—H12F109.5C45—C48—H48C109.5
H12E—C12A—H12F109.5H48A—C48—H48C109.5
O4—C13—C14107.23 (13)H48B—C48—H48C109.5
O4—C13—C15106.37 (13)O14—C49—C50108.34 (16)
C14—C13—C15112.70 (15)O14—C49—C52104.82 (16)
O4—C13—C16110.83 (13)C50—C49—C52111.11 (18)
C14—C13—C16110.65 (16)O14—C49—C51110.86 (15)
C15—C13—C16108.98 (15)C50—C49—C51110.69 (17)
C13—C14—H14A109.5C52—C49—C51110.85 (19)
C13—C14—H14B109.5C49—C50—H50A109.5
H14A—C14—H14B109.5C49—C50—H50B109.5
C13—C14—H14C109.5H50A—C50—H50B109.5
H14A—C14—H14C109.5C49—C50—H50C109.5
H14B—C14—H14C109.5H50A—C50—H50C109.5
C13—C15—H15A109.5H50B—C50—H50C109.5
C13—C15—H15B109.5C49—C51—H51A109.5
H15A—C15—H15B109.5C49—C51—H51B109.5
C13—C15—H15C109.5H51A—C51—H51B109.5
H15A—C15—H15C109.5C49—C51—H51C109.5
H15B—C15—H15C109.5H51A—C51—H51C109.5
C13—C16—H16A109.5H51B—C51—H51C109.5
C13—C16—H16B109.5C49—C52—H52A109.5
H16A—C16—H16B109.5C49—C52—H52B109.5
C13—C16—H16C109.5H52A—C52—H52B109.5
H16A—C16—H16C109.5C49—C52—H52C109.5
H16B—C16—H16C109.5H52A—C52—H52C109.5
O5—C17—C20108.33 (15)H52B—C52—H52C109.5
O5—C17—C19104.93 (15)O15—C53—H53A109.5
C20—C17—C19111.59 (17)O15—C53—H53B109.5
O5—C17—C18110.92 (14)H53A—C53—H53B109.5
C20—C17—C18110.82 (17)O15—C53—H53C109.5
C19—C17—C18110.11 (17)H53A—C53—H53C109.5
C17—C18—H18A109.5H53B—C53—H53C109.5
C17—C18—H18B109.5O15—C54—C55113.36 (16)
H18A—C18—H18B109.5O15—C54—H54A108.9
C17—C18—H18C109.5C55—C54—H54A108.9
H18A—C18—H18C109.5O15—C54—H54B108.9
H18B—C18—H18C109.5C55—C54—H54B108.9
C17—C19—H19A109.5H54A—C54—H54B107.7
C17—C19—H19B109.5O16—C55—C54109.88 (15)
H19A—C19—H19B109.5O16—C55—H55A109.7
C17—C19—H19C109.5C54—C55—H55A109.7
H19A—C19—H19C109.5O16—C55—H55B109.7
H19B—C19—H19C109.5C54—C55—H55B109.7
C17—C20—H20A109.5H55A—C55—H55B108.2
C17—C20—H20B109.5O16—C56—H56A109.5
H20A—C20—H20B109.5O16—C56—H56B109.5
C17—C20—H20C109.5H56A—C56—H56B109.5
H20A—C20—H20C109.5O16—C56—H56C109.5
H20B—C20—H20C109.5H56A—C56—H56C109.5
O6—C21—C24105.20 (15)H56B—C56—H56C109.5
O6—C21—C23110.35 (15)C1—O1—Si1128.26 (10)
C24—C21—C23110.33 (17)C1—O1—Cr1131.03 (10)
O6—C21—C22108.07 (15)Si1—O1—Cr1100.45 (6)
C24—C21—C22110.91 (18)C5—O2—Si1132.53 (12)
C23—C21—C22111.75 (18)C9—O3—Si1134.27 (12)
C21—C22—H22A109.5C13—O4—Si2127.75 (10)
C21—C22—H22B109.5C13—O4—Cr1131.44 (9)
H22A—C22—H22B109.5Si2—O4—Cr1100.32 (5)
C21—C22—H22C109.5C17—O5—Si2134.02 (11)
H22A—C22—H22C109.5C21—O6—Si2132.50 (11)
H22B—C22—H22C109.5C25—O7—C26114.72 (15)
C21—C23—H23A109.5C25—O7—Cr1124.82 (12)
C21—C23—H23B109.5C26—O7—Cr1120.11 (11)
H23A—C23—H23B109.5C28—O8—C27111.6 (2)
C21—C23—H23C109.5C29—O9—Si3128.18 (10)
H23A—C23—H23C109.5C29—O9—Cr2131.13 (10)
H23B—C23—H23C109.5Si3—O9—Cr2100.59 (5)
C21—C24—H24A109.5C33—O10—Si3133.75 (12)
C21—C24—H24B109.5C37—O11—Si3132.40 (12)
H24A—C24—H24B109.5C41—O12—Si4128.49 (10)
C21—C24—H24C109.5C41—O12—Cr2130.72 (9)
H24A—C24—H24C109.5Si4—O12—Cr2100.56 (5)
H24B—C24—H24C109.5C45—O13—Si4131.78 (11)
O7—C25—H25A109.5C49—O14—Si4135.87 (11)
O7—C25—H25B109.5C54—O15—C53114.05 (14)
H25A—C25—H25B109.5C54—O15—Cr2124.96 (11)
O7—C25—H25C109.5C53—O15—Cr2120.99 (11)
H25A—C25—H25C109.5C55—O16—C56112.09 (16)
H25B—C25—H25C109.5O3—Si1—O2107.82 (7)
O7—C26—C27112.82 (17)O3—Si1—O1104.05 (6)
O7—C26—H26A109O2—Si1—O1110.29 (7)
C27—C26—H26A109O3—Si1—S1116.03 (5)
O7—C26—H26B109O2—Si1—S1117.46 (5)
C27—C26—H26B109O1—Si1—S1100.01 (5)
H26A—C26—H26B107.8O6—Si2—O5107.19 (6)
O8—C27—C26110.52 (18)O6—Si2—O4104.26 (6)
O8—C27—H27A109.5O5—Si2—O4110.56 (6)
C26—C27—H27A109.5O6—Si2—S2115.59 (5)
O8—C27—H27B109.5O5—Si2—S2117.87 (5)
C26—C27—H27B109.5O4—Si2—S2100.31 (4)
H27A—C27—H27B108.1O11—Si3—O10107.53 (7)
O8—C28—H28A109.5O11—Si3—O9110.74 (7)
O8—C28—H28B109.5O10—Si3—O9104.01 (6)
H28A—C28—H28B109.5O11—Si3—S3117.35 (5)
O8—C28—H28C109.5O10—Si3—S3116.14 (5)
H28A—C28—H28C109.5O9—Si3—S399.97 (5)
H28B—C28—H28C109.5O14—Si4—O13106.57 (6)
O9—C29—C30107.24 (15)O14—Si4—O12111.02 (6)
O9—C29—C31106.15 (14)O13—Si4—O12103.98 (6)
C30—C29—C31112.43 (16)O14—Si4—S4117.77 (5)
O9—C29—C32110.89 (14)O13—Si4—S4116.30 (5)
C30—C29—C32110.10 (18)O12—Si4—S4100.19 (4)
C31—C29—C32109.95 (18)Si1—S1—Cr181.32 (2)
C29—C30—H30A109.5Si2—S2—Cr181.086 (19)
C29—C30—H30B109.5Si3—S3—Cr281.412 (19)
H30A—C30—H30B109.5Si4—S4—Cr281.438 (19)
C29—C30—H30C109.5O4—Cr1—O1173.99 (5)
H30A—C30—H30C109.5O4—Cr1—O792.86 (5)
H30B—C30—H30C109.5O1—Cr1—O793.15 (5)
C29—C31—H31A109.5O4—Cr1—S1101.08 (3)
C29—C31—H31B109.5O1—Cr1—S177.90 (3)
H31A—C31—H31B109.5O7—Cr1—S197.94 (4)
C29—C31—H31C109.5O4—Cr1—S278.11 (3)
H31A—C31—H31C109.5O1—Cr1—S2101.12 (3)
H31B—C31—H31C109.5O7—Cr1—S298.87 (4)
C29—C32—H32A109.5S1—Cr1—S2163.19 (2)
C29—C32—H32B109.5O9—Cr2—O12172.66 (5)
H32A—C32—H32B109.5O9—Cr2—O1595.83 (5)
C29—C32—H32C109.5O12—Cr2—O1591.50 (5)
H32A—C32—H32C109.5O9—Cr2—S377.90 (3)
H32B—C32—H32C109.5O12—Cr2—S3100.81 (3)
O10—C33—C36111.03 (16)O15—Cr2—S397.17 (3)
O10—C33—C35108.01 (16)O9—Cr2—S4101.37 (3)
C36—C33—C35111.9 (2)O12—Cr2—S477.80 (3)
O10—C33—C34104.92 (16)O15—Cr2—S498.97 (3)
C36—C33—C34111.35 (19)S3—Cr2—S4163.82 (2)
Table 1
Selected geometric parameters (Å) top
O1—Cr12.1248 (12)O15—Cr22.3463 (13)
O4—Cr12.1201 (11)S1—Cr12.4323 (5)
O7—Cr12.3273 (13)S2—Cr12.4332 (5)
O9—Cr22.1234 (12)S3—Cr22.4308 (5)
O12—Cr22.1283 (11)S4—Cr22.4365 (5)
Acknowledgements top

This work was carried out with financial support from the Polish State Committee (grant No. 3 T09A12028).

references
References top

Becker, B., Radacki, K. & Wojnowski, W. (1996). J. Organomet. Chem. 521, 39–49.

Ciborska, A., Baranowska, K. & Wojnowski, W. (2007). Acta Cryst. E63, m1239–m1241.

Dołęga, A., Chojnacki, J., Konitz, A., Komuda, W. & Wojnowski, W. (2006). Acta Cryst. E62, m636–m639.

Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565–?.

Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.

Nguyen, T., Panda, A., Olmstead, M. M., Richards, A. F., Stender, M., Brynda, M. & Power, P. P. (2005). J. Am. Chem. Soc. 127, 8545–8552.

Okura, I., Kaji, N., Aono, S., Kita, T. & Yamada, A. (1985). Inorg. Chem. 24, 453–454.

Oxford Diffraction (2005). CrysAlis CCD and CrysAlis RED. Versions 1.171. Oxford Diffraction Ltd., Abingdon, Oxfordshire, England.

Piękoś, R. & Wojnowski, W. (1962). Z. Anorg. Allg. Chem. 318, 212–216.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Wojnowska, M. & Wojnowski, W. (1974). Z. Anorg. Allg. Chem. 403, 179–185.

Wojnowski, W., Wojnowska, M. & von Schnering, H. G. (1985). Z. Anorg. Allg. Chem. 531, 153–157.