Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807055614/ng2360sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807055614/ng2360Isup2.hkl |
CCDC reference: 672631
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.
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).
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).
[Cr(C4H10O2)(C12H27O3SSi)2] | Z = 4 |
Mr = 701.09 | F(000) = 1520 |
Triclinic, P1 | Dx = 1.164 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.6809 (3) Å | Cell parameters from 32370 reflections |
b = 21.3180 (9) Å | θ = 2.1–32.5° |
c = 21.7316 (10) Å | µ = 0.49 mm−1 |
α = 87.828 (4)° | T = 150 K |
β = 84.745 (4)° | Prism, colourless |
γ = 88.372 (3)° | 0.38 × 0.38 × 0.21 mm |
V = 4000.6 (3) Å3 |
Oxford Diffraction KM4 CCD diffractometer | 12702 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
Detector resolution: 8.1883 pixels mm-1 | θmax = 25.1°, θmin = 2.1° |
ω scans, 0.75 deg width | h = −10→10 |
27543 measured reflections | k = −22→25 |
14104 independent reflections | l = −25→25 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0584P)2 + 1.4202P] where P = (Fo2 + 2Fc2)/3 |
14104 reflections | (Δ/σ)max = 0.003 |
821 parameters | Δρmax = 0.52 e Å−3 |
0 restraints | Δρmin = −0.42 e Å−3 |
[Cr(C4H10O2)(C12H27O3SSi)2] | γ = 88.372 (3)° |
Mr = 701.09 | V = 4000.6 (3) Å3 |
Triclinic, P1 | Z = 4 |
a = 8.6809 (3) Å | Mo Kα radiation |
b = 21.3180 (9) Å | µ = 0.49 mm−1 |
c = 21.7316 (10) Å | T = 150 K |
α = 87.828 (4)° | 0.38 × 0.38 × 0.21 mm |
β = 84.745 (4)° |
Oxford Diffraction KM4 CCD diffractometer | 12702 reflections with I > 2σ(I) |
27543 measured reflections | Rint = 0.016 |
14104 independent reflections |
R[F2 > 2σ(F2)] = 0.035 | 0 restraints |
wR(F2) = 0.097 | H-atom parameters constrained |
S = 1.14 | Δρmax = 0.52 e Å−3 |
14104 reflections | Δρmin = −0.42 e Å−3 |
821 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.70845 (19) | 0.28522 (10) | 0.42446 (8) | 0.0270 (4) | |
C2 | 0.6467 (2) | 0.35164 (10) | 0.41363 (9) | 0.0329 (4) | |
H2A | 0.689 | 0.3796 | 0.4423 | 0.049* | |
H2B | 0.5335 | 0.3524 | 0.4206 | 0.049* | |
H2C | 0.6776 | 0.3658 | 0.371 | 0.049* | |
C3 | 0.6515 (2) | 0.23944 (10) | 0.38053 (10) | 0.0320 (4) | |
H3A | 0.6896 | 0.2515 | 0.338 | 0.048* | |
H3B | 0.5381 | 0.2402 | 0.3844 | 0.048* | |
H3C | 0.69 | 0.197 | 0.3907 | 0.048* | |
C4 | 0.6634 (2) | 0.26328 (13) | 0.49108 (10) | 0.0433 (6) | |
H4A | 0.7127 | 0.2222 | 0.4991 | 0.065* | |
H4B | 0.5507 | 0.2598 | 0.4977 | 0.065* | |
H4C | 0.6978 | 0.2937 | 0.5193 | 0.065* | |
C5 | 1.0449 (3) | 0.12730 (9) | 0.42336 (10) | 0.0405 (5) | |
C6 | 1.0281 (3) | 0.14287 (10) | 0.35535 (10) | 0.0400 (5) | |
H6A | 0.9203 | 0.155 | 0.35 | 0.06* | |
H6B | 1.0578 | 0.1059 | 0.331 | 0.06* | |
H6C | 1.0953 | 0.1777 | 0.3412 | 0.06* | |
C7 | 0.9382 (5) | 0.07414 (12) | 0.44652 (16) | 0.0830 (11) | |
H7A | 0.949 | 0.0649 | 0.4905 | 0.125* | |
H7B | 0.9663 | 0.0366 | 0.4229 | 0.125* | |
H7C | 0.8308 | 0.0868 | 0.4411 | 0.125* | |
C8 | 1.2114 (4) | 0.11179 (13) | 0.43290 (12) | 0.0617 (8) | |
H8A | 1.2743 | 0.1486 | 0.4213 | 0.093* | |
H8B | 1.2482 | 0.0767 | 0.4071 | 0.093* | |
H8C | 1.2202 | 0.1 | 0.4765 | 0.093* | |
C9 | 1.0542 (2) | 0.27704 (10) | 0.57819 (8) | 0.0295 (4) | |
C10 | 0.9863 (8) | 0.2200 (3) | 0.6106 (2) | 0.070 (2) | 0.513 (5) |
H10A | 0.874 | 0.2261 | 0.6181 | 0.105* | 0.513 (5) |
H10B | 1.0311 | 0.2128 | 0.6501 | 0.105* | 0.513 (5) |
H10C | 1.0093 | 0.1836 | 0.5848 | 0.105* | 0.513 (5) |
C11 | 1.0150 (8) | 0.3355 (3) | 0.6132 (2) | 0.0616 (19) | 0.513 (5) |
H11A | 1.0585 | 0.3719 | 0.5894 | 0.092* | 0.513 (5) |
H11B | 1.0584 | 0.3319 | 0.6533 | 0.092* | 0.513 (5) |
H11C | 0.9023 | 0.341 | 0.6197 | 0.092* | 0.513 (5) |
C12 | 1.2301 (5) | 0.2685 (3) | 0.5664 (2) | 0.0559 (17) | 0.513 (5) |
H12A | 1.2546 | 0.2315 | 0.5416 | 0.084* | 0.513 (5) |
H12B | 1.2753 | 0.2628 | 0.606 | 0.084* | 0.513 (5) |
H12C | 1.2731 | 0.3058 | 0.5441 | 0.084* | 0.513 (5) |
C10A | 1.1352 (8) | 0.2145 (3) | 0.5844 (2) | 0.064 (2) | 0.487 (5) |
H10D | 1.0599 | 0.1811 | 0.5845 | 0.095* | 0.487 (5) |
H10E | 1.1845 | 0.2118 | 0.6233 | 0.095* | 0.487 (5) |
H10F | 1.2142 | 0.2095 | 0.5496 | 0.095* | 0.487 (5) |
C11A | 0.9224 (6) | 0.2830 (3) | 0.6298 (2) | 0.0548 (18) | 0.487 (5) |
H11D | 0.8661 | 0.323 | 0.6243 | 0.082* | 0.487 (5) |
H11E | 0.9655 | 0.2815 | 0.67 | 0.082* | 0.487 (5) |
H11F | 0.8515 | 0.2482 | 0.6282 | 0.082* | 0.487 (5) |
C12A | 1.1620 (8) | 0.3311 (3) | 0.5788 (3) | 0.073 (2) | 0.487 (5) |
H12D | 1.2439 | 0.3274 | 0.5449 | 0.11* | 0.487 (5) |
H12E | 1.2084 | 0.3303 | 0.6183 | 0.11* | 0.487 (5) |
H12F | 1.1039 | 0.3707 | 0.5736 | 0.11* | 0.487 (5) |
C13 | 1.33304 (18) | 0.36231 (9) | 0.24341 (8) | 0.0213 (4) | |
C14 | 1.4062 (2) | 0.29707 (9) | 0.24427 (9) | 0.0291 (4) | |
H14A | 1.3699 | 0.2744 | 0.2827 | 0.044* | |
H14B | 1.519 | 0.3001 | 0.2418 | 0.044* | |
H14C | 1.377 | 0.2744 | 0.2089 | 0.044* | |
C15 | 1.3798 (2) | 0.40187 (9) | 0.29508 (8) | 0.0252 (4) | |
H15A | 1.3228 | 0.4422 | 0.2947 | 0.038* | |
H15B | 1.4912 | 0.4092 | 0.2889 | 0.038* | |
H15C | 1.3556 | 0.3797 | 0.335 | 0.038* | |
C16 | 1.3752 (2) | 0.39646 (11) | 0.18157 (9) | 0.0333 (5) | |
H16A | 1.3381 | 0.3729 | 0.1483 | 0.05* | |
H16B | 1.4879 | 0.3999 | 0.1748 | 0.05* | |
H16C | 1.3268 | 0.4386 | 0.1819 | 0.05* | |
C17 | 1.0489 (2) | 0.24676 (8) | 0.13400 (9) | 0.0261 (4) | |
C18 | 1.0608 (2) | 0.20439 (9) | 0.19140 (10) | 0.0331 (4) | |
H18A | 1.1629 | 0.2084 | 0.2065 | 0.05* | |
H18B | 1.0467 | 0.1607 | 0.1811 | 0.05* | |
H18C | 0.9804 | 0.2168 | 0.2236 | 0.05* | |
C19 | 1.1709 (3) | 0.22733 (10) | 0.08315 (10) | 0.0392 (5) | |
H19A | 1.1678 | 0.2569 | 0.0476 | 0.059* | |
H19B | 1.15 | 0.185 | 0.0704 | 0.059* | |
H19C | 1.2734 | 0.2275 | 0.0986 | 0.059* | |
C20 | 0.8874 (3) | 0.24609 (11) | 0.11278 (11) | 0.0417 (5) | |
H20A | 0.8128 | 0.2625 | 0.1452 | 0.063* | |
H20B | 0.8616 | 0.2029 | 0.1045 | 0.063* | |
H20C | 0.8834 | 0.2724 | 0.075 | 0.063* | |
C21 | 0.9853 (2) | 0.45813 (8) | 0.11767 (8) | 0.0252 (4) | |
C22 | 1.1029 (3) | 0.44335 (12) | 0.06350 (10) | 0.0443 (6) | |
H22A | 1.2036 | 0.4597 | 0.071 | 0.066* | |
H22B | 1.0685 | 0.463 | 0.0255 | 0.066* | |
H22C | 1.1123 | 0.3978 | 0.0592 | 0.066* | |
C23 | 0.8264 (3) | 0.43494 (10) | 0.10801 (11) | 0.0413 (5) | |
H23A | 0.8332 | 0.3898 | 0.1007 | 0.062* | |
H23B | 0.7875 | 0.4574 | 0.0722 | 0.062* | |
H23C | 0.7557 | 0.4426 | 0.1449 | 0.062* | |
C24 | 0.9775 (3) | 0.52780 (9) | 0.12900 (10) | 0.0380 (5) | |
H24A | 0.9036 | 0.536 | 0.1648 | 0.057* | |
H24B | 0.9437 | 0.5507 | 0.0924 | 0.057* | |
H24C | 1.0801 | 0.5418 | 0.1371 | 0.057* | |
C25 | 0.9560 (3) | 0.48230 (10) | 0.33693 (11) | 0.0428 (5) | |
H25A | 0.8537 | 0.4977 | 0.3535 | 0.064* | |
H25B | 0.9525 | 0.4717 | 0.2936 | 0.064* | |
H25C | 1.032 | 0.515 | 0.3397 | 0.064* | |
C26 | 1.0141 (2) | 0.43783 (10) | 0.43569 (9) | 0.0342 (4) | |
H26A | 0.9861 | 0.399 | 0.4602 | 0.041* | |
H26B | 0.9402 | 0.4716 | 0.4499 | 0.041* | |
C27 | 1.1742 (3) | 0.45543 (10) | 0.44773 (9) | 0.0362 (5) | |
H27A | 1.186 | 0.4508 | 0.4926 | 0.043* | |
H27B | 1.2508 | 0.4268 | 0.4259 | 0.043* | |
C28 | 1.3538 (4) | 0.53529 (15) | 0.43686 (13) | 0.0652 (8) | |
H28A | 1.3693 | 0.5298 | 0.4809 | 0.098* | |
H28B | 1.3683 | 0.5794 | 0.4237 | 0.098* | |
H28C | 1.4289 | 0.5087 | 0.4127 | 0.098* | |
C29 | 0.80317 (19) | 0.06784 (9) | 0.77367 (10) | 0.0276 (4) | |
C30 | 0.8774 (2) | 0.11637 (10) | 0.72867 (10) | 0.0333 (4) | |
H30A | 0.8453 | 0.1102 | 0.6873 | 0.05* | |
H30B | 0.9903 | 0.1118 | 0.7276 | 0.05* | |
H30C | 0.8449 | 0.1585 | 0.7419 | 0.05* | |
C31 | 0.8533 (2) | 0.07277 (10) | 0.83835 (10) | 0.0327 (4) | |
H31A | 0.8298 | 0.1153 | 0.8528 | 0.049* | |
H31B | 0.9648 | 0.064 | 0.8377 | 0.049* | |
H31C | 0.7975 | 0.0423 | 0.8663 | 0.049* | |
C32 | 0.8401 (2) | 0.00221 (10) | 0.75049 (13) | 0.0460 (6) | |
H32A | 0.7955 | −0.0289 | 0.7808 | 0.069* | |
H32B | 0.9526 | −0.0045 | 0.7447 | 0.069* | |
H32C | 0.7961 | −0.0022 | 0.711 | 0.069* | |
C33 | 0.4360 (2) | −0.08711 (8) | 0.77133 (9) | 0.0297 (4) | |
C34 | 0.4596 (3) | −0.12696 (11) | 0.82988 (12) | 0.0496 (6) | |
H34A | 0.5705 | −0.1319 | 0.8346 | 0.074* | |
H34B | 0.4153 | −0.1683 | 0.8267 | 0.074* | |
H34C | 0.4081 | −0.1061 | 0.8659 | 0.074* | |
C35 | 0.5228 (3) | −0.11776 (11) | 0.71600 (12) | 0.0478 (6) | |
H35A | 0.5123 | −0.0912 | 0.6788 | 0.072* | |
H35B | 0.4797 | −0.159 | 0.7106 | 0.072* | |
H35C | 0.6325 | −0.1229 | 0.7229 | 0.072* | |
C36 | 0.2675 (3) | −0.07706 (12) | 0.76294 (15) | 0.0553 (7) | |
H36A | 0.2157 | −0.057 | 0.7993 | 0.083* | |
H36B | 0.2206 | −0.1176 | 0.7579 | 0.083* | |
H36C | 0.256 | −0.05 | 0.7261 | 0.083* | |
C37 | 0.4894 (3) | 0.07508 (11) | 0.62279 (10) | 0.0473 (6) | |
C38 | 0.631 (3) | 0.0626 (8) | 0.5691 (7) | 0.058 (4) | 0.42 (5) |
H38A | 0.7305 | 0.0687 | 0.586 | 0.087* | 0.42 (5) |
H38B | 0.6208 | 0.0921 | 0.534 | 0.087* | 0.42 (5) |
H38C | 0.6275 | 0.0195 | 0.5552 | 0.087* | 0.42 (5) |
C38A | 0.572 (3) | 0.0454 (12) | 0.5682 (5) | 0.071 (4) | 0.58 (5) |
H38D | 0.6834 | 0.0451 | 0.5717 | 0.107* | 0.58 (5) |
H38E | 0.5484 | 0.0692 | 0.5305 | 0.107* | 0.58 (5) |
H38F | 0.5376 | 0.0021 | 0.5661 | 0.107* | 0.58 (5) |
C39 | 0.3213 (4) | 0.06326 (14) | 0.61343 (13) | 0.0683 (9) | |
H39A | 0.3078 | 0.0182 | 0.609 | 0.102* | |
H39B | 0.2931 | 0.0863 | 0.5761 | 0.102* | |
H39C | 0.2547 | 0.0776 | 0.6493 | 0.102* | |
C40 | 0.5144 (3) | 0.14403 (11) | 0.63386 (12) | 0.0513 (6) | |
H40A | 0.4426 | 0.1577 | 0.6685 | 0.077* | |
H40B | 0.4954 | 0.1693 | 0.5966 | 0.077* | |
H40C | 0.6211 | 0.1494 | 0.6436 | 0.077* | |
C41 | 0.19308 (18) | 0.24842 (8) | 0.85513 (8) | 0.0214 (4) | |
C42 | 0.1260 (2) | 0.19445 (9) | 0.89539 (9) | 0.0252 (4) | |
H42A | 0.1526 | 0.1548 | 0.8752 | 0.038* | |
H42B | 0.0132 | 0.1998 | 0.9014 | 0.038* | |
H42C | 0.1688 | 0.1939 | 0.9356 | 0.038* | |
C43 | 0.1372 (2) | 0.25078 (9) | 0.79080 (9) | 0.0282 (4) | |
H43A | 0.1795 | 0.2876 | 0.7674 | 0.042* | |
H43B | 0.0239 | 0.2537 | 0.7941 | 0.042* | |
H43C | 0.1722 | 0.2126 | 0.7694 | 0.042* | |
C44 | 0.1533 (2) | 0.31001 (9) | 0.88668 (10) | 0.0324 (4) | |
H44A | 0.1898 | 0.3079 | 0.9281 | 0.049* | |
H44B | 0.0409 | 0.3173 | 0.8901 | 0.049* | |
H44C | 0.2035 | 0.3445 | 0.8622 | 0.049* | |
C45 | 0.5522 (2) | 0.35694 (9) | 0.95746 (9) | 0.0280 (4) | |
C46 | 0.5132 (2) | 0.34058 (11) | 1.02538 (9) | 0.0392 (5) | |
H46A | 0.4005 | 0.3406 | 1.0346 | 0.059* | |
H46B | 0.5573 | 0.3717 | 1.0503 | 0.059* | |
H46C | 0.5565 | 0.2988 | 1.0352 | 0.059* | |
C47 | 0.7269 (2) | 0.35374 (12) | 0.94174 (10) | 0.0429 (6) | |
H47A | 0.7667 | 0.3117 | 0.9527 | 0.064* | |
H47B | 0.7756 | 0.385 | 0.9651 | 0.064* | |
H47C | 0.7507 | 0.3625 | 0.8973 | 0.064* | |
C48 | 0.4835 (3) | 0.42099 (10) | 0.94066 (12) | 0.0496 (6) | |
H48A | 0.5034 | 0.4295 | 0.896 | 0.074* | |
H48B | 0.5313 | 0.4533 | 0.963 | 0.074* | |
H48C | 0.3717 | 0.4215 | 0.9521 | 0.074* | |
C49 | 0.5261 (2) | 0.37284 (9) | 0.74822 (9) | 0.0291 (4) | |
C50 | 0.6892 (3) | 0.39694 (10) | 0.74655 (10) | 0.0393 (5) | |
H50A | 0.6917 | 0.4302 | 0.7764 | 0.059* | |
H50B | 0.7214 | 0.4138 | 0.7049 | 0.059* | |
H50C | 0.7599 | 0.3624 | 0.7573 | 0.059* | |
C51 | 0.5195 (3) | 0.31975 (10) | 0.70355 (9) | 0.0373 (5) | |
H51A | 0.5943 | 0.2864 | 0.7134 | 0.056* | |
H51B | 0.5449 | 0.3359 | 0.6611 | 0.056* | |
H51C | 0.4152 | 0.3028 | 0.7074 | 0.056* | |
C52 | 0.4118 (3) | 0.42558 (11) | 0.73404 (12) | 0.0481 (6) | |
H52A | 0.3076 | 0.4088 | 0.7353 | 0.072* | |
H52B | 0.4409 | 0.4441 | 0.6928 | 0.072* | |
H52C | 0.4131 | 0.4579 | 0.7649 | 0.072* | |
C53 | 0.4401 (3) | 0.04834 (9) | 0.93200 (10) | 0.0370 (5) | |
H53A | 0.5296 | 0.0252 | 0.9466 | 0.055* | |
H53B | 0.4123 | 0.0302 | 0.8939 | 0.055* | |
H53C | 0.3524 | 0.0455 | 0.9637 | 0.055* | |
C54 | 0.5027 (2) | 0.14608 (9) | 0.97425 (9) | 0.0298 (4) | |
H54A | 0.4359 | 0.1284 | 1.0097 | 0.036* | |
H54B | 0.4709 | 0.1907 | 0.968 | 0.036* | |
C55 | 0.6677 (2) | 0.14282 (9) | 0.98987 (9) | 0.0306 (4) | |
H55A | 0.7371 | 0.1549 | 0.9529 | 0.037* | |
H55B | 0.6817 | 0.1726 | 1.0226 | 0.037* | |
C56 | 0.8646 (3) | 0.07441 (11) | 1.02153 (13) | 0.0474 (6) | |
H56A | 0.9294 | 0.084 | 0.9832 | 0.071* | |
H56B | 0.8864 | 0.0312 | 1.0358 | 0.071* | |
H56C | 0.8872 | 0.1034 | 1.0533 | 0.071* | |
O1 | 0.88055 (13) | 0.28833 (6) | 0.41183 (5) | 0.0214 (3) | |
O2 | 0.99325 (16) | 0.18001 (6) | 0.46173 (6) | 0.0299 (3) | |
O3 | 0.98450 (14) | 0.28511 (6) | 0.52045 (6) | 0.0260 (3) | |
O4 | 1.16195 (12) | 0.35507 (5) | 0.25458 (5) | 0.0185 (2) | |
O5 | 1.08382 (14) | 0.31099 (5) | 0.14615 (5) | 0.0215 (3) | |
O6 | 1.03991 (14) | 0.42900 (6) | 0.17293 (5) | 0.0216 (3) | |
O7 | 0.99953 (16) | 0.42779 (6) | 0.37185 (6) | 0.0304 (3) | |
O8 | 1.2029 (2) | 0.51804 (7) | 0.42723 (7) | 0.0471 (4) | |
O9 | 0.63219 (13) | 0.08135 (5) | 0.77873 (6) | 0.0234 (3) | |
O10 | 0.50831 (14) | −0.02842 (5) | 0.78013 (6) | 0.0230 (3) | |
O11 | 0.53121 (16) | 0.03569 (6) | 0.67500 (6) | 0.0294 (3) | |
O12 | 0.36414 (12) | 0.23727 (5) | 0.84763 (5) | 0.0183 (2) | |
O13 | 0.48026 (13) | 0.30947 (5) | 0.92475 (5) | 0.0213 (3) | |
O14 | 0.47807 (14) | 0.35165 (6) | 0.81096 (6) | 0.0244 (3) | |
O15 | 0.47810 (15) | 0.11296 (6) | 0.92004 (6) | 0.0272 (3) | |
O16 | 0.70647 (16) | 0.08111 (6) | 1.01049 (7) | 0.0341 (3) | |
Si1 | 1.01765 (5) | 0.25499 (2) | 0.45317 (2) | 0.01928 (11) | |
Si2 | 1.03128 (5) | 0.35793 (2) | 0.20198 (2) | 0.01669 (10) | |
Si3 | 0.49386 (5) | 0.04145 (2) | 0.74897 (2) | 0.01813 (10) | |
Si4 | 0.50487 (5) | 0.28879 (2) | 0.85326 (2) | 0.01674 (10) | |
S1 | 1.21321 (5) | 0.28461 (2) | 0.40067 (2) | 0.02403 (10) | |
S2 | 0.83362 (5) | 0.33759 (2) | 0.257828 (19) | 0.02265 (10) | |
S3 | 0.30171 (5) | 0.09422 (2) | 0.77934 (2) | 0.02244 (10) | |
S4 | 0.69667 (5) | 0.233062 (19) | 0.82966 (2) | 0.02145 (10) | |
Cr1 | 1.02010 (3) | 0.326594 (12) | 0.334825 (12) | 0.01619 (7) | |
Cr2 | 0.49821 (3) | 0.156658 (12) | 0.818976 (12) | 0.01619 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0125 (8) | 0.0450 (11) | 0.0223 (9) | 0.0009 (7) | 0.0012 (7) | 0.0060 (8) |
C2 | 0.0218 (9) | 0.0451 (12) | 0.0305 (10) | 0.0097 (8) | 0.0011 (8) | −0.0030 (9) |
C3 | 0.0188 (9) | 0.0402 (11) | 0.0369 (11) | −0.0068 (8) | −0.0025 (8) | 0.0043 (9) |
C4 | 0.0215 (10) | 0.0783 (17) | 0.0277 (11) | −0.0015 (10) | 0.0033 (8) | 0.0155 (11) |
C5 | 0.0626 (15) | 0.0214 (10) | 0.0354 (12) | 0.0067 (9) | 0.0042 (10) | 0.0000 (8) |
C6 | 0.0509 (13) | 0.0349 (11) | 0.0349 (12) | 0.0085 (10) | −0.0058 (10) | −0.0119 (9) |
C7 | 0.140 (3) | 0.0244 (13) | 0.078 (2) | −0.0131 (16) | 0.030 (2) | −0.0018 (13) |
C8 | 0.087 (2) | 0.0579 (16) | 0.0391 (14) | 0.0454 (15) | −0.0119 (13) | −0.0023 (12) |
C9 | 0.0329 (10) | 0.0413 (11) | 0.0146 (9) | 0.0028 (8) | −0.0058 (7) | 0.0027 (8) |
C10 | 0.102 (5) | 0.080 (4) | 0.030 (3) | −0.041 (4) | −0.022 (3) | 0.026 (3) |
C11 | 0.090 (5) | 0.068 (4) | 0.029 (2) | 0.032 (3) | −0.021 (3) | −0.019 (2) |
C12 | 0.038 (3) | 0.101 (5) | 0.030 (2) | 0.011 (3) | −0.0137 (19) | −0.004 (3) |
C10A | 0.076 (4) | 0.085 (4) | 0.030 (3) | 0.045 (4) | −0.024 (3) | −0.003 (3) |
C11A | 0.052 (3) | 0.092 (5) | 0.017 (2) | 0.019 (3) | 0.001 (2) | 0.002 (2) |
C12A | 0.088 (5) | 0.096 (5) | 0.042 (3) | −0.038 (4) | −0.036 (3) | 0.004 (3) |
C13 | 0.0110 (8) | 0.0328 (10) | 0.0203 (9) | −0.0041 (7) | −0.0016 (6) | −0.0017 (7) |
C14 | 0.0159 (8) | 0.0375 (11) | 0.0343 (10) | 0.0020 (7) | −0.0011 (7) | −0.0101 (8) |
C15 | 0.0221 (9) | 0.0309 (10) | 0.0232 (9) | −0.0077 (7) | −0.0036 (7) | −0.0019 (7) |
C16 | 0.0210 (9) | 0.0569 (13) | 0.0220 (10) | −0.0117 (9) | −0.0003 (7) | 0.0033 (9) |
C17 | 0.0322 (10) | 0.0198 (9) | 0.0272 (10) | −0.0063 (7) | −0.0044 (8) | −0.0051 (7) |
C18 | 0.0373 (11) | 0.0239 (10) | 0.0374 (11) | −0.0039 (8) | 0.0003 (9) | 0.0034 (8) |
C19 | 0.0539 (13) | 0.0293 (11) | 0.0333 (11) | −0.0049 (9) | 0.0073 (10) | −0.0116 (9) |
C20 | 0.0429 (12) | 0.0384 (12) | 0.0479 (13) | −0.0085 (10) | −0.0198 (10) | −0.0124 (10) |
C21 | 0.0294 (9) | 0.0238 (9) | 0.0219 (9) | 0.0032 (7) | −0.0045 (7) | 0.0053 (7) |
C22 | 0.0558 (14) | 0.0486 (13) | 0.0249 (11) | 0.0208 (11) | 0.0037 (10) | 0.0104 (9) |
C23 | 0.0420 (12) | 0.0380 (12) | 0.0467 (13) | −0.0044 (9) | −0.0235 (10) | 0.0115 (10) |
C24 | 0.0496 (13) | 0.0259 (10) | 0.0384 (12) | 0.0018 (9) | −0.0068 (10) | 0.0042 (9) |
C25 | 0.0599 (15) | 0.0271 (11) | 0.0425 (13) | 0.0091 (10) | −0.0138 (11) | −0.0014 (9) |
C26 | 0.0456 (12) | 0.0309 (10) | 0.0253 (10) | 0.0034 (9) | 0.0026 (9) | −0.0088 (8) |
C27 | 0.0518 (13) | 0.0317 (11) | 0.0254 (10) | 0.0045 (9) | −0.0036 (9) | −0.0088 (8) |
C28 | 0.080 (2) | 0.076 (2) | 0.0418 (15) | −0.0345 (16) | −0.0110 (13) | −0.0041 (13) |
C29 | 0.0114 (8) | 0.0266 (9) | 0.0457 (12) | 0.0034 (7) | −0.0033 (7) | −0.0132 (8) |
C30 | 0.0174 (9) | 0.0423 (12) | 0.0400 (11) | 0.0005 (8) | 0.0026 (8) | −0.0123 (9) |
C31 | 0.0201 (9) | 0.0324 (10) | 0.0464 (12) | 0.0046 (8) | −0.0099 (8) | −0.0016 (9) |
C32 | 0.0194 (10) | 0.0354 (12) | 0.0851 (18) | 0.0078 (8) | −0.0079 (10) | −0.0271 (12) |
C33 | 0.0334 (10) | 0.0185 (9) | 0.0368 (11) | −0.0073 (7) | 0.0022 (8) | −0.0043 (8) |
C34 | 0.0620 (16) | 0.0309 (12) | 0.0532 (15) | −0.0014 (11) | 0.0054 (12) | 0.0081 (10) |
C35 | 0.0631 (16) | 0.0307 (11) | 0.0495 (14) | −0.0046 (10) | 0.0020 (12) | −0.0135 (10) |
C36 | 0.0370 (13) | 0.0374 (13) | 0.093 (2) | −0.0127 (10) | −0.0111 (13) | −0.0021 (13) |
C37 | 0.0700 (16) | 0.0472 (13) | 0.0224 (10) | 0.0285 (12) | −0.0029 (10) | 0.0050 (9) |
C38 | 0.091 (10) | 0.046 (6) | 0.028 (4) | 0.024 (6) | 0.028 (6) | 0.005 (4) |
C38A | 0.083 (9) | 0.094 (8) | 0.028 (3) | 0.045 (6) | 0.015 (4) | 0.027 (4) |
C39 | 0.098 (2) | 0.0595 (17) | 0.0553 (17) | 0.0180 (16) | −0.0532 (17) | −0.0090 (13) |
C40 | 0.0541 (15) | 0.0444 (14) | 0.0511 (15) | 0.0132 (11) | 0.0041 (11) | 0.0219 (11) |
C41 | 0.0107 (8) | 0.0222 (9) | 0.0313 (10) | 0.0006 (6) | 0.0003 (7) | −0.0044 (7) |
C42 | 0.0180 (8) | 0.0286 (9) | 0.0284 (10) | −0.0025 (7) | 0.0037 (7) | −0.0048 (8) |
C43 | 0.0179 (9) | 0.0302 (10) | 0.0367 (11) | 0.0015 (7) | −0.0056 (7) | 0.0029 (8) |
C44 | 0.0185 (9) | 0.0252 (10) | 0.0528 (13) | 0.0016 (7) | 0.0032 (8) | −0.0110 (9) |
C45 | 0.0272 (9) | 0.0302 (10) | 0.0275 (10) | −0.0094 (8) | 0.0015 (7) | −0.0139 (8) |
C46 | 0.0341 (11) | 0.0573 (14) | 0.0271 (11) | −0.0136 (10) | 0.0022 (8) | −0.0164 (10) |
C47 | 0.0307 (11) | 0.0610 (15) | 0.0379 (12) | −0.0209 (10) | 0.0060 (9) | −0.0223 (11) |
C48 | 0.0702 (17) | 0.0276 (11) | 0.0519 (15) | −0.0037 (11) | −0.0034 (12) | −0.0173 (10) |
C49 | 0.0349 (10) | 0.0264 (10) | 0.0242 (10) | −0.0029 (8) | 0.0038 (8) | 0.0072 (8) |
C50 | 0.0428 (12) | 0.0351 (11) | 0.0382 (12) | −0.0128 (9) | 0.0082 (9) | 0.0014 (9) |
C51 | 0.0447 (12) | 0.0409 (12) | 0.0261 (10) | −0.0085 (9) | 0.0006 (9) | −0.0004 (9) |
C52 | 0.0536 (14) | 0.0441 (13) | 0.0429 (13) | 0.0095 (11) | 0.0035 (11) | 0.0192 (10) |
C53 | 0.0533 (13) | 0.0257 (10) | 0.0332 (11) | −0.0123 (9) | −0.0101 (9) | 0.0057 (8) |
C54 | 0.0393 (11) | 0.0264 (10) | 0.0238 (10) | 0.0003 (8) | −0.0039 (8) | −0.0014 (8) |
C55 | 0.0409 (11) | 0.0256 (10) | 0.0266 (10) | −0.0053 (8) | −0.0088 (8) | −0.0018 (8) |
C56 | 0.0401 (12) | 0.0421 (13) | 0.0629 (16) | 0.0045 (10) | −0.0190 (11) | −0.0080 (11) |
O1 | 0.0136 (6) | 0.0318 (7) | 0.0181 (6) | 0.0003 (5) | −0.0008 (4) | 0.0050 (5) |
O2 | 0.0395 (8) | 0.0250 (7) | 0.0234 (7) | 0.0021 (6) | 0.0039 (6) | 0.0031 (5) |
O3 | 0.0261 (6) | 0.0348 (7) | 0.0171 (6) | 0.0080 (5) | −0.0043 (5) | −0.0010 (5) |
O4 | 0.0129 (5) | 0.0273 (6) | 0.0151 (6) | −0.0023 (4) | −0.0007 (4) | 0.0008 (5) |
O5 | 0.0265 (6) | 0.0201 (6) | 0.0181 (6) | −0.0059 (5) | −0.0013 (5) | −0.0017 (5) |
O6 | 0.0243 (6) | 0.0228 (6) | 0.0180 (6) | −0.0007 (5) | −0.0036 (5) | 0.0011 (5) |
O7 | 0.0410 (8) | 0.0251 (7) | 0.0252 (7) | 0.0049 (6) | −0.0037 (6) | −0.0041 (5) |
O8 | 0.0686 (11) | 0.0389 (9) | 0.0363 (9) | −0.0143 (8) | −0.0139 (8) | −0.0025 (7) |
O9 | 0.0126 (6) | 0.0205 (6) | 0.0381 (7) | 0.0016 (5) | −0.0030 (5) | −0.0109 (5) |
O10 | 0.0230 (6) | 0.0176 (6) | 0.0290 (7) | −0.0011 (5) | −0.0046 (5) | −0.0023 (5) |
O11 | 0.0388 (8) | 0.0280 (7) | 0.0209 (7) | 0.0130 (6) | −0.0034 (5) | −0.0018 (5) |
O12 | 0.0121 (5) | 0.0172 (6) | 0.0256 (6) | 0.0003 (4) | −0.0008 (4) | −0.0040 (5) |
O13 | 0.0213 (6) | 0.0211 (6) | 0.0217 (6) | −0.0046 (5) | 0.0003 (5) | −0.0057 (5) |
O14 | 0.0278 (7) | 0.0197 (6) | 0.0242 (7) | 0.0004 (5) | 0.0041 (5) | 0.0011 (5) |
O15 | 0.0363 (7) | 0.0231 (6) | 0.0231 (7) | −0.0059 (5) | −0.0076 (5) | 0.0021 (5) |
O16 | 0.0352 (8) | 0.0284 (7) | 0.0396 (8) | −0.0003 (6) | −0.0098 (6) | 0.0005 (6) |
Si1 | 0.0178 (2) | 0.0244 (2) | 0.0153 (2) | 0.00282 (18) | −0.00170 (17) | 0.00259 (18) |
Si2 | 0.0157 (2) | 0.0206 (2) | 0.0140 (2) | −0.00209 (17) | −0.00261 (17) | 0.00074 (17) |
Si3 | 0.0157 (2) | 0.0168 (2) | 0.0225 (2) | 0.00117 (17) | −0.00403 (17) | −0.00487 (18) |
Si4 | 0.0150 (2) | 0.0148 (2) | 0.0202 (2) | −0.00163 (16) | 0.00031 (17) | −0.00285 (17) |
S1 | 0.0148 (2) | 0.0348 (2) | 0.0221 (2) | 0.00182 (17) | −0.00275 (16) | 0.00556 (18) |
S2 | 0.0143 (2) | 0.0361 (2) | 0.0176 (2) | −0.00300 (17) | −0.00285 (15) | 0.00343 (17) |
S3 | 0.0140 (2) | 0.0221 (2) | 0.0323 (2) | 0.00120 (16) | −0.00492 (17) | −0.01009 (18) |
S4 | 0.01327 (19) | 0.0193 (2) | 0.0319 (2) | −0.00123 (15) | 0.00013 (16) | −0.00643 (17) |
Cr1 | 0.01336 (13) | 0.02138 (14) | 0.01365 (14) | 0.00070 (10) | −0.00128 (10) | 0.00082 (10) |
Cr2 | 0.01234 (13) | 0.01478 (13) | 0.02179 (15) | −0.00002 (10) | −0.00202 (10) | −0.00415 (10) |
C1—O1 | 1.497 (2) | C31—H31C | 0.98 |
C1—C3 | 1.514 (3) | C32—H32A | 0.98 |
C1—C2 | 1.517 (3) | C32—H32B | 0.98 |
C1—C4 | 1.524 (3) | C32—H32C | 0.98 |
C2—H2A | 0.98 | C33—O10 | 1.443 (2) |
C2—H2B | 0.98 | C33—C36 | 1.499 (3) |
C2—H2C | 0.98 | C33—C35 | 1.519 (3) |
C3—H3A | 0.98 | C33—C34 | 1.529 (3) |
C3—H3B | 0.98 | C34—H34A | 0.98 |
C3—H3C | 0.98 | C34—H34B | 0.98 |
C4—H4A | 0.98 | C34—H34C | 0.98 |
C4—H4B | 0.98 | C35—H35A | 0.98 |
C4—H4C | 0.98 | C35—H35B | 0.98 |
C5—O2 | 1.460 (2) | C35—H35C | 0.98 |
C5—C8 | 1.505 (4) | C36—H36A | 0.98 |
C5—C6 | 1.522 (3) | C36—H36B | 0.98 |
C5—C7 | 1.525 (4) | C36—H36C | 0.98 |
C6—H6A | 0.98 | C37—O11 | 1.453 (2) |
C6—H6B | 0.98 | C37—C38A | 1.482 (12) |
C6—H6C | 0.98 | C37—C39 | 1.521 (4) |
C7—H7A | 0.98 | C37—C40 | 1.523 (4) |
C7—H7B | 0.98 | C37—C38 | 1.64 (2) |
C7—H7C | 0.98 | C38—H38A | 0.98 |
C8—H8A | 0.98 | C38—H38B | 0.98 |
C8—H8B | 0.98 | C38—H38C | 0.98 |
C8—H8C | 0.98 | C38A—H38D | 0.98 |
C9—O3 | 1.445 (2) | C38A—H38E | 0.98 |
C9—C10 | 1.490 (5) | C38A—H38F | 0.98 |
C9—C10A | 1.497 (6) | C39—H39A | 0.98 |
C9—C11 | 1.500 (5) | C39—H39B | 0.98 |
C9—C12A | 1.506 (6) | C39—H39C | 0.98 |
C9—C12 | 1.532 (5) | C40—H40A | 0.98 |
C9—C11A | 1.534 (5) | C40—H40B | 0.98 |
C10—H10A | 0.98 | C40—H40C | 0.98 |
C10—H10B | 0.98 | C41—O12 | 1.4923 (19) |
C10—H10C | 0.98 | C41—C42 | 1.515 (3) |
C11—H11A | 0.98 | C41—C43 | 1.520 (3) |
C11—H11B | 0.98 | C41—C44 | 1.521 (2) |
C11—H11C | 0.98 | C42—H42A | 0.98 |
C12—H12A | 0.98 | C42—H42B | 0.98 |
C12—H12B | 0.98 | C42—H42C | 0.98 |
C12—H12C | 0.98 | C43—H43A | 0.98 |
C10A—H10D | 0.98 | C43—H43B | 0.98 |
C10A—H10E | 0.98 | C43—H43C | 0.98 |
C10A—H10F | 0.98 | C44—H44A | 0.98 |
C11A—H11D | 0.98 | C44—H44B | 0.98 |
C11A—H11E | 0.98 | C44—H44C | 0.98 |
C11A—H11F | 0.98 | C45—O13 | 1.446 (2) |
C12A—H12D | 0.98 | C45—C46 | 1.514 (3) |
C12A—H12E | 0.98 | C45—C48 | 1.519 (3) |
C12A—H12F | 0.98 | C45—C47 | 1.524 (3) |
C13—O4 | 1.4942 (19) | C46—H46A | 0.98 |
C13—C14 | 1.513 (3) | C46—H46B | 0.98 |
C13—C15 | 1.521 (2) | C46—H46C | 0.98 |
C13—C16 | 1.524 (3) | C47—H47A | 0.98 |
C14—H14A | 0.98 | C47—H47B | 0.98 |
C14—H14B | 0.98 | C47—H47C | 0.98 |
C14—H14C | 0.98 | C48—H48A | 0.98 |
C15—H15A | 0.98 | C48—H48B | 0.98 |
C15—H15B | 0.98 | C48—H48C | 0.98 |
C15—H15C | 0.98 | C49—O14 | 1.448 (2) |
C16—H16A | 0.98 | C49—C50 | 1.517 (3) |
C16—H16B | 0.98 | C49—C52 | 1.520 (3) |
C16—H16C | 0.98 | C49—C51 | 1.524 (3) |
C17—O5 | 1.450 (2) | C50—H50A | 0.98 |
C17—C20 | 1.517 (3) | C50—H50B | 0.98 |
C17—C19 | 1.519 (3) | C50—H50C | 0.98 |
C17—C18 | 1.522 (3) | C51—H51A | 0.98 |
C18—H18A | 0.98 | C51—H51B | 0.98 |
C18—H18B | 0.98 | C51—H51C | 0.98 |
C18—H18C | 0.98 | C52—H52A | 0.98 |
C19—H19A | 0.98 | C52—H52B | 0.98 |
C19—H19B | 0.98 | C52—H52C | 0.98 |
C19—H19C | 0.98 | C53—O15 | 1.434 (2) |
C20—H20A | 0.98 | C53—H53A | 0.98 |
C20—H20B | 0.98 | C53—H53B | 0.98 |
C20—H20C | 0.98 | C53—H53C | 0.98 |
C21—O6 | 1.443 (2) | C54—O15 | 1.432 (2) |
C21—C24 | 1.513 (3) | C54—C55 | 1.501 (3) |
C21—C23 | 1.514 (3) | C54—H54A | 0.99 |
C21—C22 | 1.522 (3) | C54—H54B | 0.99 |
C22—H22A | 0.98 | C55—O16 | 1.415 (2) |
C22—H22B | 0.98 | C55—H55A | 0.99 |
C22—H22C | 0.98 | C55—H55B | 0.99 |
C23—H23A | 0.98 | C56—O16 | 1.417 (3) |
C23—H23B | 0.98 | C56—H56A | 0.98 |
C23—H23C | 0.98 | C56—H56B | 0.98 |
C24—H24A | 0.98 | C56—H56C | 0.98 |
C24—H24B | 0.98 | O1—Si1 | 1.6817 (12) |
C24—H24C | 0.98 | O1—Cr1 | 2.1248 (12) |
C25—O7 | 1.425 (2) | O2—Si1 | 1.6198 (14) |
C25—H25A | 0.98 | O3—Si1 | 1.6174 (13) |
C25—H25B | 0.98 | O4—Si2 | 1.6809 (11) |
C25—H25C | 0.98 | O4—Cr1 | 2.1201 (11) |
C26—O7 | 1.429 (2) | O5—Si2 | 1.6267 (12) |
C26—C27 | 1.498 (3) | O6—Si2 | 1.6201 (12) |
C26—H26A | 0.99 | O7—Cr1 | 2.3273 (13) |
C26—H26B | 0.99 | O9—Si3 | 1.6810 (12) |
C27—O8 | 1.413 (3) | O9—Cr2 | 2.1234 (12) |
C27—H27A | 0.99 | O10—Si3 | 1.6191 (13) |
C27—H27B | 0.99 | O11—Si3 | 1.6190 (13) |
C28—O8 | 1.406 (3) | O12—Si4 | 1.6816 (11) |
C28—H28A | 0.98 | O12—Cr2 | 2.1283 (11) |
C28—H28B | 0.98 | O13—Si4 | 1.6246 (12) |
C28—H28C | 0.98 | O14—Si4 | 1.6195 (13) |
C29—O9 | 1.4988 (19) | O15—Cr2 | 2.3463 (13) |
C29—C30 | 1.513 (3) | Si1—S1 | 2.0577 (6) |
C29—C31 | 1.517 (3) | Si2—S2 | 2.0558 (6) |
C29—C32 | 1.521 (3) | Si3—S3 | 2.0570 (6) |
C30—H30A | 0.98 | Si4—S4 | 2.0553 (6) |
C30—H30B | 0.98 | S1—Cr1 | 2.4323 (5) |
C30—H30C | 0.98 | S2—Cr1 | 2.4332 (5) |
C31—H31A | 0.98 | S3—Cr2 | 2.4308 (5) |
C31—H31B | 0.98 | S4—Cr2 | 2.4365 (5) |
O1—C1—C3 | 107.83 (14) | C35—C33—C34 | 109.37 (19) |
O1—C1—C2 | 105.77 (15) | C33—C34—H34A | 109.5 |
C3—C1—C2 | 112.57 (16) | C33—C34—H34B | 109.5 |
O1—C1—C4 | 110.98 (14) | H34A—C34—H34B | 109.5 |
C3—C1—C4 | 109.83 (17) | C33—C34—H34C | 109.5 |
C2—C1—C4 | 109.79 (17) | H34A—C34—H34C | 109.5 |
C1—C2—H2A | 109.5 | H34B—C34—H34C | 109.5 |
C1—C2—H2B | 109.5 | C33—C35—H35A | 109.5 |
H2A—C2—H2B | 109.5 | C33—C35—H35B | 109.5 |
C1—C2—H2C | 109.5 | H35A—C35—H35B | 109.5 |
H2A—C2—H2C | 109.5 | C33—C35—H35C | 109.5 |
H2B—C2—H2C | 109.5 | H35A—C35—H35C | 109.5 |
C1—C3—H3A | 109.5 | H35B—C35—H35C | 109.5 |
C1—C3—H3B | 109.5 | C33—C36—H36A | 109.5 |
H3A—C3—H3B | 109.5 | C33—C36—H36B | 109.5 |
C1—C3—H3C | 109.5 | H36A—C36—H36B | 109.5 |
H3A—C3—H3C | 109.5 | C33—C36—H36C | 109.5 |
H3B—C3—H3C | 109.5 | H36A—C36—H36C | 109.5 |
C1—C4—H4A | 109.5 | H36B—C36—H36C | 109.5 |
C1—C4—H4B | 109.5 | O11—C37—C38A | 104.4 (5) |
H4A—C4—H4B | 109.5 | O11—C37—C39 | 107.9 (2) |
C1—C4—H4C | 109.5 | C38A—C37—C39 | 101.7 (12) |
H4A—C4—H4C | 109.5 | O11—C37—C40 | 110.83 (19) |
H4B—C4—H4C | 109.5 | C38A—C37—C40 | 119.6 (12) |
O2—C5—C8 | 108.47 (19) | C39—C37—C40 | 111.5 (2) |
O2—C5—C6 | 111.25 (16) | O11—C37—C38 | 103.9 (6) |
C8—C5—C6 | 110.2 (2) | C39—C37—C38 | 122.6 (10) |
O2—C5—C7 | 104.55 (19) | C40—C37—C38 | 99.7 (9) |
C8—C5—C7 | 112.1 (2) | C37—C38—H38A | 109.5 |
C6—C5—C7 | 110.2 (2) | C37—C38—H38B | 109.5 |
C5—C6—H6A | 109.5 | C37—C38—H38C | 109.5 |
C5—C6—H6B | 109.5 | C37—C38A—H38D | 109.5 |
H6A—C6—H6B | 109.5 | C37—C38A—H38E | 109.5 |
C5—C6—H6C | 109.5 | H38D—C38A—H38E | 109.5 |
H6A—C6—H6C | 109.5 | C37—C38A—H38F | 109.5 |
H6B—C6—H6C | 109.5 | H38D—C38A—H38F | 109.5 |
C5—C7—H7A | 109.5 | H38E—C38A—H38F | 109.5 |
C5—C7—H7B | 109.5 | C37—C39—H39A | 109.5 |
H7A—C7—H7B | 109.5 | C37—C39—H39B | 109.5 |
C5—C7—H7C | 109.5 | H39A—C39—H39B | 109.5 |
H7A—C7—H7C | 109.5 | C37—C39—H39C | 109.5 |
H7B—C7—H7C | 109.5 | H39A—C39—H39C | 109.5 |
C5—C8—H8A | 109.5 | H39B—C39—H39C | 109.5 |
C5—C8—H8B | 109.5 | C37—C40—H40A | 109.5 |
H8A—C8—H8B | 109.5 | C37—C40—H40B | 109.5 |
C5—C8—H8C | 109.5 | H40A—C40—H40B | 109.5 |
H8A—C8—H8C | 109.5 | C37—C40—H40C | 109.5 |
H8B—C8—H8C | 109.5 | H40A—C40—H40C | 109.5 |
O3—C9—C10 | 106.9 (2) | H40B—C40—H40C | 109.5 |
O3—C9—C10A | 112.4 (2) | O12—C41—C42 | 106.75 (13) |
C10—C9—C10A | 54.4 (4) | O12—C41—C43 | 107.17 (13) |
O3—C9—C11 | 106.4 (2) | C42—C41—C43 | 112.61 (15) |
C10—C9—C11 | 112.5 (4) | O12—C41—C44 | 110.51 (13) |
C10A—C9—C11 | 141.2 (3) | C42—C41—C44 | 109.54 (15) |
O3—C9—C12A | 105.0 (3) | C43—C41—C44 | 110.19 (16) |
C10—C9—C12A | 148.1 (3) | C41—C42—H42A | 109.5 |
C10A—C9—C12A | 112.8 (4) | C41—C42—H42B | 109.5 |
C11—C9—C12A | 56.4 (4) | H42A—C42—H42B | 109.5 |
O3—C9—C12 | 110.6 (2) | C41—C42—H42C | 109.5 |
C10—C9—C12 | 110.2 (4) | H42A—C42—H42C | 109.5 |
C10A—C9—C12 | 57.5 (4) | H42B—C42—H42C | 109.5 |
C11—C9—C12 | 110.1 (4) | C41—C43—H43A | 109.5 |
C12A—C9—C12 | 57.8 (4) | C41—C43—H43B | 109.5 |
O3—C9—C11A | 106.6 (2) | H43A—C43—H43B | 109.5 |
C10—C9—C11A | 59.3 (4) | C41—C43—H43C | 109.5 |
C10A—C9—C11A | 109.7 (4) | H43A—C43—H43C | 109.5 |
C11—C9—C11A | 55.6 (4) | H43B—C43—H43C | 109.5 |
C12A—C9—C11A | 110.3 (4) | C41—C44—H44A | 109.5 |
C12—C9—C11A | 142.8 (3) | C41—C44—H44B | 109.5 |
C9—C10—H10A | 109.5 | H44A—C44—H44B | 109.5 |
C9—C10—H10B | 109.5 | C41—C44—H44C | 109.5 |
C9—C10—H10C | 109.5 | H44A—C44—H44C | 109.5 |
C9—C11—H11A | 109.5 | H44B—C44—H44C | 109.5 |
C9—C11—H11B | 109.5 | O13—C45—C46 | 105.33 (15) |
C9—C11—H11C | 109.5 | O13—C45—C48 | 109.15 (16) |
C9—C12—H12A | 109.5 | C46—C45—C48 | 110.58 (18) |
C9—C12—H12B | 109.5 | O13—C45—C47 | 109.67 (15) |
C9—C12—H12C | 109.5 | C46—C45—C47 | 110.07 (18) |
C9—C10A—H10D | 109.5 | C48—C45—C47 | 111.82 (19) |
C9—C10A—H10E | 109.5 | C45—C46—H46A | 109.5 |
H10D—C10A—H10E | 109.5 | C45—C46—H46B | 109.5 |
C9—C10A—H10F | 109.5 | H46A—C46—H46B | 109.5 |
H10D—C10A—H10F | 109.5 | C45—C46—H46C | 109.5 |
H10E—C10A—H10F | 109.5 | H46A—C46—H46C | 109.5 |
C9—C11A—H11D | 109.5 | H46B—C46—H46C | 109.5 |
C9—C11A—H11E | 109.5 | C45—C47—H47A | 109.5 |
H11D—C11A—H11E | 109.5 | C45—C47—H47B | 109.5 |
C9—C11A—H11F | 109.5 | H47A—C47—H47B | 109.5 |
H11D—C11A—H11F | 109.5 | C45—C47—H47C | 109.5 |
H11E—C11A—H11F | 109.5 | H47A—C47—H47C | 109.5 |
C9—C12A—H12D | 109.5 | H47B—C47—H47C | 109.5 |
C9—C12A—H12E | 109.5 | C45—C48—H48A | 109.5 |
H12D—C12A—H12E | 109.5 | C45—C48—H48B | 109.5 |
C9—C12A—H12F | 109.5 | H48A—C48—H48B | 109.5 |
H12D—C12A—H12F | 109.5 | C45—C48—H48C | 109.5 |
H12E—C12A—H12F | 109.5 | H48A—C48—H48C | 109.5 |
O4—C13—C14 | 107.23 (13) | H48B—C48—H48C | 109.5 |
O4—C13—C15 | 106.37 (13) | O14—C49—C50 | 108.34 (16) |
C14—C13—C15 | 112.70 (15) | O14—C49—C52 | 104.82 (16) |
O4—C13—C16 | 110.83 (13) | C50—C49—C52 | 111.11 (18) |
C14—C13—C16 | 110.65 (16) | O14—C49—C51 | 110.86 (15) |
C15—C13—C16 | 108.98 (15) | C50—C49—C51 | 110.69 (17) |
C13—C14—H14A | 109.5 | C52—C49—C51 | 110.85 (19) |
C13—C14—H14B | 109.5 | C49—C50—H50A | 109.5 |
H14A—C14—H14B | 109.5 | C49—C50—H50B | 109.5 |
C13—C14—H14C | 109.5 | H50A—C50—H50B | 109.5 |
H14A—C14—H14C | 109.5 | C49—C50—H50C | 109.5 |
H14B—C14—H14C | 109.5 | H50A—C50—H50C | 109.5 |
C13—C15—H15A | 109.5 | H50B—C50—H50C | 109.5 |
C13—C15—H15B | 109.5 | C49—C51—H51A | 109.5 |
H15A—C15—H15B | 109.5 | C49—C51—H51B | 109.5 |
C13—C15—H15C | 109.5 | H51A—C51—H51B | 109.5 |
H15A—C15—H15C | 109.5 | C49—C51—H51C | 109.5 |
H15B—C15—H15C | 109.5 | H51A—C51—H51C | 109.5 |
C13—C16—H16A | 109.5 | H51B—C51—H51C | 109.5 |
C13—C16—H16B | 109.5 | C49—C52—H52A | 109.5 |
H16A—C16—H16B | 109.5 | C49—C52—H52B | 109.5 |
C13—C16—H16C | 109.5 | H52A—C52—H52B | 109.5 |
H16A—C16—H16C | 109.5 | C49—C52—H52C | 109.5 |
H16B—C16—H16C | 109.5 | H52A—C52—H52C | 109.5 |
O5—C17—C20 | 108.33 (15) | H52B—C52—H52C | 109.5 |
O5—C17—C19 | 104.93 (15) | O15—C53—H53A | 109.5 |
C20—C17—C19 | 111.59 (17) | O15—C53—H53B | 109.5 |
O5—C17—C18 | 110.92 (14) | H53A—C53—H53B | 109.5 |
C20—C17—C18 | 110.82 (17) | O15—C53—H53C | 109.5 |
C19—C17—C18 | 110.11 (17) | H53A—C53—H53C | 109.5 |
C17—C18—H18A | 109.5 | H53B—C53—H53C | 109.5 |
C17—C18—H18B | 109.5 | O15—C54—C55 | 113.36 (16) |
H18A—C18—H18B | 109.5 | O15—C54—H54A | 108.9 |
C17—C18—H18C | 109.5 | C55—C54—H54A | 108.9 |
H18A—C18—H18C | 109.5 | O15—C54—H54B | 108.9 |
H18B—C18—H18C | 109.5 | C55—C54—H54B | 108.9 |
C17—C19—H19A | 109.5 | H54A—C54—H54B | 107.7 |
C17—C19—H19B | 109.5 | O16—C55—C54 | 109.88 (15) |
H19A—C19—H19B | 109.5 | O16—C55—H55A | 109.7 |
C17—C19—H19C | 109.5 | C54—C55—H55A | 109.7 |
H19A—C19—H19C | 109.5 | O16—C55—H55B | 109.7 |
H19B—C19—H19C | 109.5 | C54—C55—H55B | 109.7 |
C17—C20—H20A | 109.5 | H55A—C55—H55B | 108.2 |
C17—C20—H20B | 109.5 | O16—C56—H56A | 109.5 |
H20A—C20—H20B | 109.5 | O16—C56—H56B | 109.5 |
C17—C20—H20C | 109.5 | H56A—C56—H56B | 109.5 |
H20A—C20—H20C | 109.5 | O16—C56—H56C | 109.5 |
H20B—C20—H20C | 109.5 | H56A—C56—H56C | 109.5 |
O6—C21—C24 | 105.20 (15) | H56B—C56—H56C | 109.5 |
O6—C21—C23 | 110.35 (15) | C1—O1—Si1 | 128.26 (10) |
C24—C21—C23 | 110.33 (17) | C1—O1—Cr1 | 131.03 (10) |
O6—C21—C22 | 108.07 (15) | Si1—O1—Cr1 | 100.45 (6) |
C24—C21—C22 | 110.91 (18) | C5—O2—Si1 | 132.53 (12) |
C23—C21—C22 | 111.75 (18) | C9—O3—Si1 | 134.27 (12) |
C21—C22—H22A | 109.5 | C13—O4—Si2 | 127.75 (10) |
C21—C22—H22B | 109.5 | C13—O4—Cr1 | 131.44 (9) |
H22A—C22—H22B | 109.5 | Si2—O4—Cr1 | 100.32 (5) |
C21—C22—H22C | 109.5 | C17—O5—Si2 | 134.02 (11) |
H22A—C22—H22C | 109.5 | C21—O6—Si2 | 132.50 (11) |
H22B—C22—H22C | 109.5 | C25—O7—C26 | 114.72 (15) |
C21—C23—H23A | 109.5 | C25—O7—Cr1 | 124.82 (12) |
C21—C23—H23B | 109.5 | C26—O7—Cr1 | 120.11 (11) |
H23A—C23—H23B | 109.5 | C28—O8—C27 | 111.6 (2) |
C21—C23—H23C | 109.5 | C29—O9—Si3 | 128.18 (10) |
H23A—C23—H23C | 109.5 | C29—O9—Cr2 | 131.13 (10) |
H23B—C23—H23C | 109.5 | Si3—O9—Cr2 | 100.59 (5) |
C21—C24—H24A | 109.5 | C33—O10—Si3 | 133.75 (12) |
C21—C24—H24B | 109.5 | C37—O11—Si3 | 132.40 (12) |
H24A—C24—H24B | 109.5 | C41—O12—Si4 | 128.49 (10) |
C21—C24—H24C | 109.5 | C41—O12—Cr2 | 130.72 (9) |
H24A—C24—H24C | 109.5 | Si4—O12—Cr2 | 100.56 (5) |
H24B—C24—H24C | 109.5 | C45—O13—Si4 | 131.78 (11) |
O7—C25—H25A | 109.5 | C49—O14—Si4 | 135.87 (11) |
O7—C25—H25B | 109.5 | C54—O15—C53 | 114.05 (14) |
H25A—C25—H25B | 109.5 | C54—O15—Cr2 | 124.96 (11) |
O7—C25—H25C | 109.5 | C53—O15—Cr2 | 120.99 (11) |
H25A—C25—H25C | 109.5 | C55—O16—C56 | 112.09 (16) |
H25B—C25—H25C | 109.5 | O3—Si1—O2 | 107.82 (7) |
O7—C26—C27 | 112.82 (17) | O3—Si1—O1 | 104.05 (6) |
O7—C26—H26A | 109 | O2—Si1—O1 | 110.29 (7) |
C27—C26—H26A | 109 | O3—Si1—S1 | 116.03 (5) |
O7—C26—H26B | 109 | O2—Si1—S1 | 117.46 (5) |
C27—C26—H26B | 109 | O1—Si1—S1 | 100.01 (5) |
H26A—C26—H26B | 107.8 | O6—Si2—O5 | 107.19 (6) |
O8—C27—C26 | 110.52 (18) | O6—Si2—O4 | 104.26 (6) |
O8—C27—H27A | 109.5 | O5—Si2—O4 | 110.56 (6) |
C26—C27—H27A | 109.5 | O6—Si2—S2 | 115.59 (5) |
O8—C27—H27B | 109.5 | O5—Si2—S2 | 117.87 (5) |
C26—C27—H27B | 109.5 | O4—Si2—S2 | 100.31 (4) |
H27A—C27—H27B | 108.1 | O11—Si3—O10 | 107.53 (7) |
O8—C28—H28A | 109.5 | O11—Si3—O9 | 110.74 (7) |
O8—C28—H28B | 109.5 | O10—Si3—O9 | 104.01 (6) |
H28A—C28—H28B | 109.5 | O11—Si3—S3 | 117.35 (5) |
O8—C28—H28C | 109.5 | O10—Si3—S3 | 116.14 (5) |
H28A—C28—H28C | 109.5 | O9—Si3—S3 | 99.97 (5) |
H28B—C28—H28C | 109.5 | O14—Si4—O13 | 106.57 (6) |
O9—C29—C30 | 107.24 (15) | O14—Si4—O12 | 111.02 (6) |
O9—C29—C31 | 106.15 (14) | O13—Si4—O12 | 103.98 (6) |
C30—C29—C31 | 112.43 (16) | O14—Si4—S4 | 117.77 (5) |
O9—C29—C32 | 110.89 (14) | O13—Si4—S4 | 116.30 (5) |
C30—C29—C32 | 110.10 (18) | O12—Si4—S4 | 100.19 (4) |
C31—C29—C32 | 109.95 (18) | Si1—S1—Cr1 | 81.32 (2) |
C29—C30—H30A | 109.5 | Si2—S2—Cr1 | 81.086 (19) |
C29—C30—H30B | 109.5 | Si3—S3—Cr2 | 81.412 (19) |
H30A—C30—H30B | 109.5 | Si4—S4—Cr2 | 81.438 (19) |
C29—C30—H30C | 109.5 | O4—Cr1—O1 | 173.99 (5) |
H30A—C30—H30C | 109.5 | O4—Cr1—O7 | 92.86 (5) |
H30B—C30—H30C | 109.5 | O1—Cr1—O7 | 93.15 (5) |
C29—C31—H31A | 109.5 | O4—Cr1—S1 | 101.08 (3) |
C29—C31—H31B | 109.5 | O1—Cr1—S1 | 77.90 (3) |
H31A—C31—H31B | 109.5 | O7—Cr1—S1 | 97.94 (4) |
C29—C31—H31C | 109.5 | O4—Cr1—S2 | 78.11 (3) |
H31A—C31—H31C | 109.5 | O1—Cr1—S2 | 101.12 (3) |
H31B—C31—H31C | 109.5 | O7—Cr1—S2 | 98.87 (4) |
C29—C32—H32A | 109.5 | S1—Cr1—S2 | 163.19 (2) |
C29—C32—H32B | 109.5 | O9—Cr2—O12 | 172.66 (5) |
H32A—C32—H32B | 109.5 | O9—Cr2—O15 | 95.83 (5) |
C29—C32—H32C | 109.5 | O12—Cr2—O15 | 91.50 (5) |
H32A—C32—H32C | 109.5 | O9—Cr2—S3 | 77.90 (3) |
H32B—C32—H32C | 109.5 | O12—Cr2—S3 | 100.81 (3) |
O10—C33—C36 | 111.03 (16) | O15—Cr2—S3 | 97.17 (3) |
O10—C33—C35 | 108.01 (16) | O9—Cr2—S4 | 101.37 (3) |
C36—C33—C35 | 111.9 (2) | O12—Cr2—S4 | 77.80 (3) |
O10—C33—C34 | 104.92 (16) | O15—Cr2—S4 | 98.97 (3) |
C36—C33—C34 | 111.35 (19) | S3—Cr2—S4 | 163.82 (2) |
Experimental details
Crystal data | |
Chemical formula | [Cr(C4H10O2)(C12H27O3SSi)2] |
Mr | 701.09 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 150 |
a, b, c (Å) | 8.6809 (3), 21.3180 (9), 21.7316 (10) |
α, β, γ (°) | 87.828 (4), 84.745 (4), 88.372 (3) |
V (Å3) | 4000.6 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.49 |
Crystal size (mm) | 0.38 × 0.38 × 0.21 |
Data collection | |
Diffractometer | Oxford Diffraction KM4 CCD diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 27543, 14104, 12702 |
Rint | 0.016 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.097, 1.14 |
No. of reflections | 14104 |
No. of parameters | 821 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.52, −0.42 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2005), CrysAlis RED (Oxford Diffraction, 2005), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
O1—Cr1 | 2.1248 (12) | O15—Cr2 | 2.3463 (13) |
O4—Cr1 | 2.1201 (11) | S1—Cr1 | 2.4323 (5) |
O7—Cr1 | 2.3273 (13) | S2—Cr1 | 2.4332 (5) |
O9—Cr2 | 2.1234 (12) | S3—Cr2 | 2.4308 (5) |
O12—Cr2 | 2.1283 (11) | S4—Cr2 | 2.4365 (5) |
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).