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The crystal structure of 5-O-tert-butyldimethylsilyl-3,4-O-carbonyl-1,2-O-cyclohexylidene-2-oxo-3-oxa-4-bornanylcarbonyl-D-myo-inositol has been studied by single-crystal X-ray diffraction at both room temperature and 173 K. At room temperature, the tert-butyldimethylsilyl group exhibits dynamical disorder. A molecular dynamics simulation was used to model the disorder and this indicates that the group librates between two stable conformations in the crystal. Approximate relative energies of the different forms and energy barriers for the transition were obtained by empirical force field methods. Calculations of the thermal motion of the atoms are in good qualitative, but fair to poor quantitative agreement with the X-­ray data.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100005309/ns0003sup1.cif
Contains datablocks global, 173K, 298K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100005309/ns0003173Ksup2.hkl
Contains datablock mp068low

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768100005309/ns0003298Ksup3.hkl
Contains datablock mp068high

CCDC references: 148927; 148928

Computing details top

For both compounds, data collection: "Collect" data collection software, Nonius B.V., 1998.; data reduction: DENZO-SMN (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

(173K) top
Crystal data top
C29H44O10SiF(000) = 624
Mr = 580.73Dx = 1.210 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71070 Å
Hall symbol: P 2y1Cell parameters from 6915 reflections
a = 7.537 (1) Åθ = 2.2–27.5°
b = 10.183 (1) ŵ = 0.13 mm1
c = 20.843 (1) ÅT = 173 K
β = 94.93 (1)°Block, colourless
V = 1593.8 (3) Å30.20 × 0.15 × 0.13 mm
Z = 2
Data collection top
Enraf Nonius Kappa CCD
diffractometer
3310 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.029
Graphite monochromatorθmax = 27.5°, θmin = 2.2°
a 175° ψ–scan and 2 ωh = 89
6915 measured reflectionsk = 711
4237 independent reflectionsl = 2323
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)] = 0.051H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.128 w = 1/[σ2(Fo2) + (0.0643P)2 + 0.7367P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.011
4237 reflectionsΔρmax = 0.33 e Å3
433 parametersΔρmin = 0.30 e Å3
1 restraintAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.0 (2)
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
C10.5376 (6)0.8283 (4)0.2125 (2)0.0412 (11)
O20.3726 (3)0.8806 (3)0.21383 (13)0.0388 (7)
C30.2486 (5)0.7721 (4)0.21512 (19)0.0346 (9)
H30.21040.74370.17010.104 (3)*
C40.0877 (5)0.7939 (4)0.25159 (19)0.0387 (10)
H40.00260.85740.22900.104 (3)*
O50.1396 (4)0.8342 (3)0.31560 (14)0.0478 (8)
C60.0466 (6)0.7549 (5)0.3584 (2)0.0501 (12)
C70.1324 (7)0.8161 (6)0.3694 (3)0.0702 (16)
H7A0.20620.82280.32790.104 (3)*
H7B0.11380.90580.38700.104 (3)*
C80.2297 (9)0.7332 (7)0.4164 (4)0.099 (2)
H8A0.34030.77890.42610.104 (3)*
H8B0.26370.64800.39600.104 (3)*
C90.1145 (13)0.7085 (8)0.4789 (3)0.122 (3)
H9A0.09330.79260.50220.104 (3)*
H9B0.17820.64910.50670.104 (3)*
C100.0632 (10)0.6475 (7)0.4660 (3)0.100 (2)
H10A0.13730.63650.50720.104 (3)*
H10B0.04250.55950.44660.104 (3)*
C110.1609 (8)0.7323 (6)0.4212 (2)0.0740 (17)
H11A0.27350.68880.41210.104 (3)*
H11B0.19060.81770.44200.104 (3)*
O120.0253 (4)0.6324 (3)0.32671 (13)0.0437 (7)
C130.0001 (5)0.6551 (4)0.2593 (2)0.0379 (10)
H130.13000.65920.24520.104 (3)*
C140.0851 (5)0.5387 (4)0.22745 (18)0.0361 (10)
H140.03640.45580.24470.104 (3)*
C150.2936 (5)0.5305 (4)0.23423 (19)0.0349 (10)
H150.33760.49670.19340.104 (3)*
C160.3646 (5)0.6677 (4)0.2483 (2)0.0329 (9)
H160.37280.68320.29590.104 (3)*
O170.5365 (3)0.6971 (3)0.22414 (14)0.0417 (7)
O180.6659 (4)0.8887 (3)0.20132 (16)0.0573 (9)
O190.3526 (3)0.4494 (3)0.28583 (12)0.0403 (7)
Si200.39989 (18)0.29041 (13)0.28804 (6)0.0517 (4)
C210.4731 (13)0.2360 (6)0.2125 (3)0.132 (4)
H21A0.38430.26050.17740.104 (3)*
H21B0.48760.14040.21330.104 (3)*
H21C0.58730.27760.20570.104 (3)*
C220.1941 (9)0.1977 (7)0.3020 (5)0.136 (3)
H22A0.15860.21810.34510.104 (3)*
H22B0.21700.10330.29880.104 (3)*
H22C0.09840.22300.26960.104 (3)*
C230.5590 (9)0.2701 (6)0.3575 (3)0.096 (2)
C240.5895 (14)0.1220 (8)0.3710 (4)0.188 (6)
H24A0.68460.08970.34590.104 (3)*
H24B0.47950.07350.35880.104 (3)*
H24C0.62400.10880.41700.104 (3)*
C250.4983 (13)0.3345 (9)0.4172 (3)0.134 (3)
H25A0.37650.30650.42330.104 (3)*
H25B0.50140.43010.41230.104 (3)*
H25C0.57780.30850.45480.104 (3)*
C260.7331 (9)0.3442 (10)0.3408 (6)0.228 (7)
H26A0.75060.33120.29520.104 (3)*
H26B0.83590.30920.36740.104 (3)*
H26C0.72090.43820.34950.104 (3)*
O270.0223 (3)0.5502 (3)0.15949 (13)0.0379 (7)
C280.0098 (5)0.4380 (5)0.1265 (2)0.0433 (11)
O290.0191 (6)0.3328 (4)0.14909 (18)0.0965 (16)
C300.0844 (5)0.4660 (4)0.05944 (19)0.0313 (9)
O310.1429 (3)0.3402 (2)0.03029 (12)0.0345 (7)
C320.2592 (5)0.3710 (4)0.02114 (18)0.0320 (9)
C330.2752 (5)0.5170 (4)0.02418 (19)0.0359 (10)
C340.0892 (6)0.5582 (5)0.0459 (2)0.0533 (12)
H34A0.06060.50790.08430.104 (3)*
H34B0.08630.65320.05580.104 (3)*
C350.0419 (5)0.5248 (4)0.0126 (2)0.0459 (12)
H35A0.10260.60440.03070.104 (3)*
H35B0.13210.46010.00130.104 (3)*
C360.2534 (4)0.5524 (4)0.04849 (18)0.0304 (9)
C370.4073 (5)0.5001 (4)0.0850 (2)0.0457 (12)
H37A0.37670.50910.13140.104 (3)*
H37B0.42790.40730.07430.104 (3)*
H37C0.51550.55050.07250.104 (3)*
C380.2265 (6)0.6970 (4)0.0627 (2)0.0413 (11)
H38A0.12490.72940.04100.104 (3)*
H38B0.20340.70980.10930.104 (3)*
H38C0.33390.74560.04710.104 (3)*
O390.3239 (3)0.2874 (3)0.05710 (13)0.0412 (7)
C400.4383 (7)0.5672 (5)0.0645 (2)0.0604 (14)
H40A0.54590.53980.04490.104 (3)*
H40B0.44010.53090.10810.104 (3)*
H40C0.43410.66330.06660.104 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.035 (2)0.036 (3)0.051 (3)0.004 (2)0.006 (2)0.005 (2)
O20.0368 (15)0.0263 (16)0.0519 (18)0.0034 (12)0.0041 (12)0.0016 (13)
C30.035 (2)0.026 (2)0.043 (2)0.0012 (18)0.0014 (17)0.001 (2)
C40.036 (2)0.036 (2)0.043 (3)0.003 (2)0.0011 (18)0.004 (2)
O50.0480 (16)0.048 (2)0.0482 (19)0.0041 (14)0.0054 (14)0.0150 (15)
C60.056 (3)0.055 (3)0.039 (3)0.001 (2)0.002 (2)0.015 (2)
C70.062 (3)0.071 (4)0.080 (4)0.002 (3)0.025 (3)0.021 (3)
C80.096 (5)0.109 (6)0.098 (6)0.009 (4)0.049 (4)0.029 (4)
C90.188 (8)0.118 (6)0.067 (5)0.046 (6)0.060 (5)0.029 (4)
C100.151 (6)0.112 (6)0.034 (3)0.011 (5)0.002 (4)0.002 (4)
C110.094 (4)0.084 (5)0.041 (3)0.008 (3)0.013 (3)0.012 (3)
O120.0531 (17)0.0392 (18)0.0383 (19)0.0015 (14)0.0005 (13)0.0028 (14)
C130.033 (2)0.038 (3)0.041 (3)0.0005 (19)0.0035 (18)0.003 (2)
C140.040 (2)0.036 (3)0.030 (2)0.0008 (19)0.0093 (17)0.004 (2)
C150.037 (2)0.029 (2)0.038 (2)0.0064 (18)0.0063 (18)0.002 (2)
C160.031 (2)0.022 (2)0.044 (3)0.0028 (17)0.0043 (18)0.0016 (18)
O170.0321 (15)0.0300 (18)0.062 (2)0.0051 (12)0.0018 (13)0.0054 (15)
O180.0379 (17)0.049 (2)0.084 (2)0.0075 (16)0.0026 (16)0.0013 (18)
O190.0515 (16)0.0308 (16)0.0362 (17)0.0096 (13)0.0104 (13)0.0015 (14)
Si200.0705 (8)0.0325 (7)0.0497 (8)0.0120 (6)0.0089 (6)0.0034 (6)
C210.274 (11)0.050 (4)0.073 (5)0.059 (5)0.030 (5)0.002 (3)
C220.083 (5)0.054 (4)0.265 (11)0.015 (3)0.013 (6)0.018 (6)
C230.135 (6)0.063 (4)0.082 (5)0.046 (4)0.040 (4)0.002 (4)
C240.281 (12)0.091 (6)0.163 (9)0.078 (7)0.148 (9)0.002 (6)
C250.221 (9)0.115 (7)0.056 (4)0.001 (6)0.044 (5)0.016 (5)
C260.048 (4)0.175 (10)0.45 (2)0.000 (5)0.030 (7)0.150 (12)
O270.0449 (15)0.0276 (17)0.0384 (17)0.0034 (12)0.0117 (12)0.0056 (14)
C280.046 (2)0.022 (3)0.059 (3)0.0086 (19)0.009 (2)0.006 (3)
O290.177 (4)0.030 (2)0.070 (3)0.016 (2)0.067 (3)0.0081 (18)
C300.033 (2)0.022 (2)0.038 (2)0.0054 (17)0.0044 (18)0.0077 (19)
O310.0355 (14)0.0262 (16)0.0397 (16)0.0003 (11)0.0095 (12)0.0064 (13)
C320.031 (2)0.033 (3)0.031 (2)0.0032 (18)0.0029 (18)0.002 (2)
C330.049 (2)0.025 (3)0.032 (2)0.0026 (19)0.0034 (18)0.0027 (19)
C340.070 (3)0.051 (3)0.040 (3)0.020 (2)0.013 (2)0.005 (2)
C350.036 (2)0.042 (3)0.061 (3)0.010 (2)0.011 (2)0.014 (2)
C360.031 (2)0.022 (2)0.037 (2)0.0009 (17)0.0050 (17)0.0024 (18)
C370.039 (2)0.044 (3)0.055 (3)0.0031 (19)0.007 (2)0.006 (2)
C380.049 (2)0.024 (2)0.049 (3)0.0049 (18)0.004 (2)0.003 (2)
O390.0443 (15)0.0370 (17)0.0404 (16)0.0086 (14)0.0075 (12)0.0076 (15)
C400.087 (3)0.039 (3)0.049 (3)0.008 (3)0.027 (3)0.002 (2)
Geometric parameters (Å, º) top
C1—O181.186 (5)O19—Si201.658 (3)
C1—O21.356 (5)Si20—C211.799 (7)
C1—O171.358 (5)Si20—C231.811 (6)
O2—C31.449 (5)Si20—C221.860 (7)
C3—C41.502 (5)C23—C251.511 (10)
C3—C161.506 (5)C23—C241.548 (9)
C4—O51.418 (5)C23—C261.579 (11)
C4—C131.574 (6)O27—C281.345 (5)
O5—C61.430 (5)C28—O291.184 (5)
C6—O121.414 (5)C28—C301.488 (6)
C6—C71.521 (7)C30—O311.469 (4)
C6—C111.521 (7)C30—C351.542 (6)
C7—C81.526 (8)C30—C361.548 (5)
C8—C91.524 (10)O31—C321.362 (4)
C9—C101.521 (10)C32—O391.209 (5)
C10—C111.509 (9)C32—C331.493 (5)
O12—C131.420 (5)C33—C401.517 (6)
C13—C141.526 (5)C33—C361.552 (5)
C14—O271.459 (4)C33—C341.566 (6)
C14—C151.568 (5)C34—C351.538 (6)
C15—O191.398 (5)C36—C381.513 (5)
C15—C161.516 (5)C36—C371.536 (5)
C16—O171.461 (5)
O18—C1—O2124.4 (4)C21—Si20—C23115.6 (4)
O18—C1—O17124.3 (4)O19—Si20—C22108.6 (3)
O2—C1—O17111.3 (4)C21—Si20—C22107.7 (4)
C1—O2—C3107.1 (3)C23—Si20—C22108.7 (4)
O2—C3—C4116.5 (3)C25—C23—C24108.9 (6)
O2—C3—C16101.4 (3)C25—C23—C26106.9 (7)
C4—C3—C16109.5 (3)C24—C23—C26113.1 (7)
O5—C4—C3110.5 (3)C25—C23—Si20112.5 (5)
O5—C4—C13104.3 (3)C24—C23—Si20109.5 (5)
C3—C4—C13106.4 (3)C26—C23—Si20105.9 (6)
C4—O5—C6108.2 (3)C28—O27—C14117.2 (3)
O12—C6—O5104.5 (3)O29—C28—O27123.1 (4)
O12—C6—C7111.4 (4)O29—C28—C30126.1 (4)
O5—C6—C7110.6 (4)O27—C28—C30110.8 (4)
O12—C6—C11107.5 (4)O31—C30—C28107.3 (3)
O5—C6—C11110.5 (4)O31—C30—C35104.8 (3)
C7—C6—C11112.1 (4)C28—C30—C35117.7 (3)
C6—C7—C8110.6 (5)O31—C30—C36102.7 (3)
C9—C8—C7111.7 (6)C28—C30—C36119.1 (3)
C10—C9—C8111.1 (5)C35—C30—C36103.3 (3)
C11—C10—C9111.1 (6)C32—O31—C30105.9 (3)
C10—C11—C6110.4 (5)O39—C32—O31121.6 (4)
C6—O12—C13108.5 (3)O39—C32—C33130.4 (4)
O12—C13—C14106.1 (3)O31—C32—C33107.9 (3)
O12—C13—C4103.1 (3)C32—C33—C40114.7 (3)
C14—C13—C4117.2 (3)C32—C33—C36100.8 (3)
O27—C14—C13104.3 (3)C40—C33—C36118.4 (4)
O27—C14—C15109.3 (3)C32—C33—C34102.0 (3)
C13—C14—C15117.2 (3)C40—C33—C34116.9 (4)
O19—C15—C16108.2 (3)C36—C33—C34101.4 (3)
O19—C15—C14110.5 (3)C35—C34—C33104.0 (3)
C16—C15—C14107.6 (3)C34—C35—C30101.4 (3)
O17—C16—C3101.2 (3)C38—C36—C37109.5 (3)
O17—C16—C15115.5 (3)C38—C36—C30115.4 (3)
C3—C16—C15112.4 (3)C37—C36—C30112.1 (3)
C1—O17—C16106.4 (3)C38—C36—C33114.7 (3)
C15—O19—Si20130.7 (2)C37—C36—C33112.5 (3)
O19—Si20—C21111.0 (2)C30—C36—C3391.7 (3)
O19—Si20—C23105.0 (2)
(298K) top
Crystal data top
C29H44O10SiF(000) = 624
Mr = 580.73Dx = 1.184 Mg m3
Monoclinic, P21Mo Kα radiation, λ = 0.71070 Å
Hall symbol: P 2y1Cell parameters from 6199 reflections
a = 7.5722 (4) Åθ = 3.4–26.4°
b = 10.2402 (5) ŵ = 0.12 mm1
c = 21.1352 (9) ÅT = 298 K
β = 96.188 (2)°Block, colourless
V = 1629.29 (14) Å30.5 × 0.4 × 0.3 mm
Z = 2
Data collection top
Enraf Nonius Kappa CCD
diffractometer
5230 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.019
Graphite monochromatorθmax = 26.4°, θmin = 3.4°
a 175° ψ–scan and 2 ωh = 09
6439 measured reflectionsk = 1212
6199 independent reflectionsl = 2626
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)] = 0.073H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.198 w = 1/[σ2(Fo2) + (0.0996P)2 + 0.6765P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.049
6199 reflectionsΔρmax = 0.55 e Å3
435 parametersΔρmin = 0.80 e Å3
7 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.4 (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*/Ueq
C10.5463 (5)0.8249 (4)0.2097 (2)0.0655 (10)
O20.3830 (3)0.8758 (2)0.21123 (13)0.0590 (6)
C30.2591 (4)0.7685 (3)0.21270 (18)0.0515 (7)
H30.21960.74060.16910.127 (3)*
C40.1003 (5)0.7903 (4)0.24825 (18)0.0590 (9)
H40.01650.85190.22570.127 (3)*
O50.1551 (4)0.8332 (3)0.31087 (15)0.0748 (8)
C60.0617 (6)0.7564 (5)0.3535 (2)0.0792 (13)
C70.1121 (8)0.8171 (7)0.3641 (3)0.106 (2)
H7A0.18650.82320.32390.127 (3)*
H7B0.09200.90490.38060.127 (3)*
C80.2074 (13)0.7366 (11)0.4110 (5)0.156 (4)
H8A0.31290.78280.42090.127 (3)*
H8B0.24430.65370.39170.127 (3)*
C90.0855 (17)0.7121 (13)0.4725 (4)0.193 (5)
H9A0.14540.65530.50010.127 (3)*
H9B0.06150.79440.49450.127 (3)*
C100.0842 (13)0.6516 (12)0.4599 (3)0.157 (4)
H10A0.06100.56570.44160.127 (3)*
H10B0.15900.64080.49980.127 (3)*
C110.1822 (10)0.7338 (9)0.4148 (3)0.120 (2)
H11A0.21610.81690.43450.127 (3)*
H11B0.28940.68900.40550.127 (3)*
O120.0401 (4)0.6329 (3)0.32271 (14)0.0718 (7)
C130.0128 (5)0.6547 (4)0.25581 (17)0.0569 (8)
H130.11450.65880.24150.127 (3)*
C140.0976 (4)0.5375 (4)0.22527 (16)0.0534 (8)
H140.05000.45710.24200.127 (3)*
C150.3034 (4)0.5284 (3)0.23272 (16)0.0506 (7)
H150.34440.49410.19360.127 (3)*
C160.3755 (4)0.6648 (3)0.24568 (17)0.0512 (8)
H160.38590.68080.29160.127 (3)*
O170.5461 (3)0.6937 (3)0.22228 (14)0.0648 (7)
O180.6728 (4)0.8837 (3)0.19854 (19)0.0860 (10)
O190.3622 (4)0.4481 (3)0.28416 (12)0.0633 (7)
Si200.4279 (3)0.29636 (16)0.28631 (7)0.1166 (7)
C210.4766 (19)0.2334 (8)0.2127 (3)0.205 (7)
H21A0.42020.28630.17890.127 (3)*
H21B0.43330.14540.20800.127 (3)*
H21C0.60280.23410.21110.127 (3)*
C220.2297 (13)0.2017 (11)0.2936 (12)0.43 (2)
H22A0.23020.17170.33660.127 (3)*
H22B0.22680.12790.26540.127 (3)*
H22C0.12680.25510.28250.127 (3)*
C230.5605 (16)0.2660 (8)0.3581 (3)0.252 (9)
C240.5776 (19)0.1140 (9)0.3705 (5)0.203 (6)
H24A0.67670.08050.35080.127 (3)*
H24B0.47070.07130.35280.127 (3)*
H24C0.59580.09790.41550.127 (3)*
C250.4790 (19)0.3250 (12)0.4167 (3)0.205 (6)
H25A0.35220.31590.41070.127 (3)*
H25B0.50950.41590.42070.127 (3)*
H25C0.52540.27960.45460.127 (3)*
C260.7268 (15)0.3513 (17)0.3384 (13)0.57 (3)
H26A0.72360.35340.29290.127 (3)*
H26B0.83600.31220.35640.127 (3)*
H26C0.71890.43870.35430.127 (3)*
O270.0327 (3)0.5484 (3)0.15776 (12)0.0594 (6)
C280.0094 (5)0.4382 (4)0.12628 (19)0.0616 (9)
O290.0141 (8)0.3343 (4)0.1486 (2)0.138 (2)
C300.0833 (4)0.4665 (3)0.05901 (16)0.0479 (7)
O310.1426 (3)0.3419 (2)0.03012 (11)0.0512 (5)
C320.2589 (4)0.3723 (3)0.02149 (16)0.0494 (7)
C330.2732 (5)0.5188 (4)0.02458 (17)0.0563 (8)
C340.0874 (7)0.5569 (5)0.0450 (2)0.0768 (12)
H34A0.06070.50660.08170.127 (3)*
H34B0.08280.64920.05510.127 (3)*
C350.0430 (5)0.5236 (5)0.0141 (2)0.0696 (11)
H35A0.10290.60100.03200.127 (3)*
H35B0.13080.46000.00410.127 (3)*
C360.2515 (4)0.5522 (3)0.04784 (15)0.0468 (7)
C370.4049 (5)0.5008 (5)0.0824 (2)0.0680 (10)
H37A0.37680.51190.12740.127 (3)*
H37B0.42300.40970.07290.127 (3)*
H37C0.51120.54840.06840.127 (3)*
C380.2234 (6)0.6969 (4)0.0617 (2)0.0640 (10)
H38A0.12620.72820.04020.127 (3)*
H38B0.19690.70960.10670.127 (3)*
H38C0.32930.74410.04680.127 (3)*
O390.3236 (4)0.2899 (3)0.05682 (13)0.0653 (7)
C400.4371 (8)0.5681 (5)0.0654 (2)0.0889 (15)
H40A0.54130.52940.05110.127 (3)*
H40B0.42970.54470.10900.127 (3)*
H40C0.44390.66140.06180.127 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.055 (2)0.058 (2)0.082 (3)0.0043 (18)0.0011 (17)0.0049 (19)
O20.0576 (14)0.0415 (13)0.0765 (16)0.0050 (11)0.0015 (11)0.0020 (12)
C30.0504 (16)0.0408 (17)0.0618 (19)0.0058 (14)0.0014 (14)0.0012 (14)
C40.0545 (18)0.054 (2)0.068 (2)0.0166 (16)0.0015 (15)0.0047 (17)
O50.0763 (17)0.072 (2)0.0763 (18)0.0024 (14)0.0113 (14)0.0264 (15)
C60.079 (3)0.094 (4)0.065 (2)0.009 (2)0.009 (2)0.027 (2)
C70.095 (3)0.117 (5)0.109 (4)0.007 (3)0.030 (3)0.039 (4)
C80.154 (7)0.182 (9)0.147 (8)0.008 (6)0.084 (6)0.042 (7)
C90.282 (14)0.208 (11)0.107 (6)0.015 (10)0.100 (8)0.033 (7)
C100.181 (8)0.226 (11)0.062 (4)0.014 (8)0.010 (4)0.000 (5)
C110.130 (5)0.156 (7)0.070 (3)0.004 (5)0.012 (3)0.025 (4)
O120.0848 (18)0.0720 (18)0.0592 (16)0.0020 (15)0.0102 (13)0.0072 (13)
C130.0518 (18)0.062 (2)0.0552 (19)0.0056 (16)0.0018 (14)0.0079 (16)
C140.0545 (17)0.0495 (19)0.0541 (18)0.0026 (15)0.0032 (14)0.0032 (15)
C150.0574 (18)0.0410 (17)0.0520 (17)0.0068 (14)0.0003 (13)0.0007 (14)
C160.0469 (16)0.0478 (19)0.0577 (19)0.0084 (14)0.0002 (13)0.0018 (15)
O170.0505 (13)0.0555 (15)0.0879 (19)0.0127 (11)0.0056 (12)0.0007 (14)
O180.0597 (16)0.072 (2)0.126 (3)0.0104 (15)0.0083 (17)0.003 (2)
O190.0769 (16)0.0505 (14)0.0596 (14)0.0139 (13)0.0056 (11)0.0032 (12)
Si200.207 (2)0.0690 (9)0.0717 (8)0.0648 (11)0.0035 (10)0.0114 (7)
C210.413 (19)0.101 (6)0.099 (5)0.126 (9)0.019 (7)0.006 (4)
C220.180 (12)0.078 (6)0.99 (7)0.023 (7)0.09 (2)0.042 (18)
C230.50 (2)0.145 (9)0.089 (5)0.180 (13)0.054 (8)0.003 (5)
C240.309 (15)0.127 (7)0.151 (8)0.092 (9)0.071 (9)0.027 (6)
C250.357 (17)0.167 (10)0.082 (5)0.074 (11)0.017 (7)0.016 (5)
C260.111 (8)0.176 (16)1.39 (10)0.014 (9)0.09 (2)0.12 (3)
O270.0717 (15)0.0479 (14)0.0550 (13)0.0048 (12)0.0101 (11)0.0070 (11)
C280.070 (2)0.0390 (18)0.071 (2)0.0088 (16)0.0144 (17)0.0085 (17)
O290.246 (6)0.0476 (19)0.098 (3)0.013 (3)0.080 (3)0.0079 (18)
C300.0511 (17)0.0351 (16)0.0555 (17)0.0002 (13)0.0026 (13)0.0118 (13)
O310.0534 (12)0.0342 (11)0.0631 (13)0.0001 (9)0.0068 (10)0.0091 (10)
C320.0492 (16)0.0455 (18)0.0528 (17)0.0048 (14)0.0018 (13)0.0054 (15)
C330.073 (2)0.0417 (18)0.0509 (18)0.0055 (16)0.0065 (15)0.0022 (14)
C340.106 (3)0.064 (3)0.063 (2)0.031 (2)0.021 (2)0.005 (2)
C350.056 (2)0.068 (3)0.087 (3)0.0138 (19)0.0187 (18)0.024 (2)
C360.0497 (16)0.0370 (16)0.0523 (16)0.0026 (13)0.0003 (13)0.0004 (13)
C370.057 (2)0.072 (3)0.075 (2)0.0098 (19)0.0081 (17)0.005 (2)
C380.083 (3)0.0363 (17)0.070 (2)0.0073 (17)0.0046 (19)0.0087 (16)
O390.0745 (16)0.0501 (14)0.0680 (15)0.0100 (13)0.0084 (12)0.0106 (13)
C400.119 (4)0.065 (3)0.074 (3)0.012 (3)0.033 (3)0.000 (2)
Geometric parameters (Å, º) top
C1—O181.177 (5)O19—Si201.630 (3)
C1—O21.346 (5)Si20—C231.755 (6)
C1—O171.370 (5)Si20—C211.760 (6)
O2—C31.448 (4)Si20—C221.807 (7)
C3—C161.503 (5)C23—C251.563 (10)
C3—C41.502 (5)C23—C261.622 (11)
C4—O51.414 (5)C23—C241.582 (9)
C4—C131.554 (6)O27—C281.331 (4)
O5—C61.437 (6)C28—O291.171 (6)
C6—O121.423 (6)C28—C301.499 (5)
C6—C111.520 (7)C30—O311.464 (4)
C6—C71.494 (7)C30—C361.544 (4)
C7—C81.530 (11)C30—C351.534 (5)
C8—C91.531 (15)O31—C321.362 (4)
C9—C101.476 (13)C32—O391.196 (4)
C10—C111.525 (13)C32—C331.505 (5)
O12—C131.424 (5)C33—C401.520 (6)
C13—C141.536 (5)C33—C361.560 (5)
C14—O271.463 (4)C33—C341.565 (6)
C14—C151.552 (5)C34—C351.544 (7)
C15—O191.398 (4)C36—C381.520 (5)
C15—C161.513 (5)C36—C371.530 (5)
C16—O171.463 (4)
O18—C1—O2125.2 (4)C23—Si20—C21123.0 (5)
O18—C1—O17124.0 (4)O19—Si20—C22105.1 (5)
O2—C1—O17110.8 (3)C23—Si20—C22103.6 (8)
C1—O2—C3107.8 (3)C21—Si20—C2297.7 (8)
O2—C3—C16101.4 (3)C25—C23—C26112.2 (12)
O2—C3—C4117.0 (3)C25—C23—C24106.4 (9)
C16—C3—C4109.5 (3)C26—C23—C24121.4 (12)
O5—C4—C3110.1 (3)C25—C23—Si20112.2 (6)
O5—C4—C13105.5 (3)C26—C23—Si2094.0 (8)
C3—C4—C13107.0 (3)C24—C23—Si20110.3 (6)
C4—O5—C6107.5 (3)C28—O27—C14117.4 (3)
O12—C6—O5103.9 (3)O29—C28—O27123.4 (4)
O12—C6—C11106.4 (5)O29—C28—C30125.7 (4)
O5—C6—C11109.1 (5)O27—C28—C30110.8 (3)
O12—C6—C7112.2 (4)O31—C30—C28107.1 (3)
O5—C6—C7111.5 (5)O31—C30—C36102.7 (2)
C11—C6—C7113.1 (5)C28—C30—C36118.2 (3)
C6—C7—C8111.0 (6)O31—C30—C35104.9 (3)
C9—C8—C7110.8 (8)C28—C30—C35117.9 (3)
C8—C9—C10111.9 (6)C36—C30—C35104.3 (3)
C9—C10—C11111.9 (9)C32—O31—C30106.1 (2)
C6—C11—C10109.3 (6)O39—C32—O31121.6 (3)
C6—O12—C13108.1 (3)O39—C32—C33130.8 (3)
O12—C13—C14105.8 (3)O31—C32—C33107.4 (3)
O12—C13—C4103.0 (3)C40—C33—C32114.0 (3)
C14—C13—C4116.9 (3)C40—C33—C36118.5 (4)
O27—C14—C13103.8 (3)C32—C33—C36100.2 (3)
O27—C14—C15109.4 (3)C40—C33—C34117.7 (4)
C13—C14—C15117.7 (3)C32—C33—C34101.4 (3)
O19—C15—C16108.9 (3)C36—C33—C34102.3 (3)
O19—C15—C14110.3 (3)C35—C34—C33103.7 (3)
C16—C15—C14107.6 (3)C34—C35—C30101.4 (3)
O17—C16—C3101.3 (3)C38—C36—C37110.0 (3)
O17—C16—C15116.1 (3)C38—C36—C30115.4 (3)
C3—C16—C15112.7 (3)C37—C36—C30112.8 (3)
C1—O17—C16106.5 (3)C38—C36—C33113.6 (3)
C15—O19—Si20130.8 (2)C37—C36—C33112.8 (3)
O19—Si20—C23109.7 (3)C30—C36—C3391.3 (3)
O19—Si20—C21114.6 (3)
 

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