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

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ISSN: 2056-9890
Volume 67| Part 5| May 2011| Page o1234

2,2,4,4-Tetra­phenyl-1,3-bis­­(3,3,5,5-tetra­methyl-1,1-di­phenyl-5-vinyl­tris­ilox­an-1-yl)­cyclo­disilazane

aInstitute of Chemistry, Chinese Academy of Sciences, Beijing 100190, People's Republic of China
*Correspondence e-mail: zhangzj@iccas.ac.cn

(Received 12 April 2011; accepted 20 April 2011; online 29 April 2011)

The title mol­ecule, C60H70N2O4Si8, lies on an inversion center. In the asymmetric unit, one of the phenyl rings is disordered over two sets of sites with refined occupancies 0.58 (2) and 0.42 (2). In addition, in two substitution sites of the terminal dimeth­yl(vin­yl)silyl unit, a methyl group and the vinyl group are disordered over the same site with refined occupancies 0.523 (13) and 0.477 (13).

Related literature

For similar cyclo­disilaza­nes to the title compound and their synthesis, see: Zhu et al. (2007[Zhu, Y. P., Guo, L., Zhang, Z. J., Xie, Z. M. & Xu, C. H. (2007). J. Appl. Polym. Sci. 105, 749-756.]).

[Scheme 1]

Experimental

Crystal data
  • C60H70N2O4Si8

  • Mr = 1107.90

  • Triclinic, [P \overline 1]

  • a = 10.731 (2) Å

  • b = 11.021 (2) Å

  • c = 13.859 (3) Å

  • α = 88.320 (9)°

  • β = 76.120 (6)°

  • γ = 78.860 (8)°

  • V = 1561.0 (6) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 0.22 mm−1

  • T = 173 K

  • 0.41 × 0.28 × 0.22 mm

Data collection
  • Rigaku Saturn724+ CCD diffractometer

  • Absorption correction: multi-scan (CrystalClear; Rigaku, 2007[Rigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.916, Tmax = 0.954

  • 12950 measured reflections

  • 6338 independent reflections

  • 5389 reflections with I > 2σ(I)

  • Rint = 0.040

Refinement
  • R[F2 > 2σ(F2)] = 0.072

  • wR(F2) = 0.169

  • S = 1.11

  • 6338 reflections

  • 390 parameters

  • 74 restraints

  • H-atom parameters constrained

  • Δρmax = 0.55 e Å−3

  • Δρmin = −0.32 e Å−3

Data collection: CrystalClear (Rigaku, 2007[Rigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

Organocyclodisilazanes exhibit high thermal stability, and have been used to enhance the thermal properties of silicone rubbers (Zhu et al., 2007). Different functional groups can be introduced to cyclodisilazanes to improve their reactivity.

The molecular structure of the title compound is shown in Fig. 1. The molecule lies on an inversion center. In the asymmetric unit, one of the phenyl rings is disordered over two sets of sites with refined occupancies 0.58 (2) and 0.42 (2). In addition, in the the terminal dimethyl(vinyl)silyl group one of the methyl groups and the vinyl group are disordered over their respective sites with refined occupancies 0.523 (13) and 0.477 (13).

Related literature top

For similar cyclodisilazanes to the title compound and their synthesis, see: Zhu et al. (2007).

Experimental top

The reaction scheme is shown in Fig. 2. 2 g 1,3-bis-(hydroxydiphenylsilanyl)-2,2,4,4-tetraphenylcyclodisilazane was dissolved in 20 ml tetrahydrofuran and added dropwisely to 2 ml n-butyllithum (2.5 mol/L solution in n-hexane) at 263K, then warmed to room temperature. An excessive amount of 1-vinyl-3-chloro-1,1,3,3-tetramethyldisiloxane was added to the mixture. After stirring for 30 min, solvents and unreacted disiloxane were removed under reduced pressure. The crude product was recrystallized from n-hexane to give colorless crystal.

Refinement top

All H atoms were located in difference maps but were constrained in a riding-model approximation with Uiso(H) = 1.2Ueq(Caryl) or Uiso(H) = 1.5Ueq(Cmethyl). C—H distances were constrained to 0.95 and 0.98 Å for aryl and methyl H atoms respectively.

Computing details top

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalClear (Rigaku, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound shown with 30% ellipsoids. H atoms are not shown (symmetry code: (A) -x+1, -y+1, -z+1). The disorder is not shown.
[Figure 2] Fig. 2. The synthesis of the title compound.
2,2,4,4-Tetraphenyl-1,3-bis(3,3,5,5-tetramethyl-1,1-diphenyl-5- vinyltrisiloxan-1-yl)cyclodisilazane top
Crystal data top
C60H70N2O4Si8Z = 1
Mr = 1107.90F(000) = 588
Triclinic, P1Dx = 1.179 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.731 (2) ÅCell parameters from 4640 reflections
b = 11.021 (2) Åθ = 1.5–26.4°
c = 13.859 (3) ŵ = 0.22 mm1
α = 88.320 (9)°T = 173 K
β = 76.120 (6)°Block, colorless
γ = 78.860 (8)°0.41 × 0.28 × 0.22 mm
V = 1561.0 (6) Å3
Data collection top
Rigaku Saturn724+ CCD
diffractometer
6338 independent reflections
Radiation source: sealed tube5389 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ω scans at fixed χ = 45°θmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2007)
h = 1313
Tmin = 0.916, Tmax = 0.954k = 1313
12950 measured reflectionsl = 1717
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.072Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.169H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.0572P)2 + 1.4799P]
where P = (Fo2 + 2Fc2)/3
6338 reflections(Δ/σ)max = 0.001
390 parametersΔρmax = 0.55 e Å3
74 restraintsΔρmin = 0.32 e Å3
Crystal data top
C60H70N2O4Si8γ = 78.860 (8)°
Mr = 1107.90V = 1561.0 (6) Å3
Triclinic, P1Z = 1
a = 10.731 (2) ÅMo Kα radiation
b = 11.021 (2) ŵ = 0.22 mm1
c = 13.859 (3) ÅT = 173 K
α = 88.320 (9)°0.41 × 0.28 × 0.22 mm
β = 76.120 (6)°
Data collection top
Rigaku Saturn724+ CCD
diffractometer
6338 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2007)
5389 reflections with I > 2σ(I)
Tmin = 0.916, Tmax = 0.954Rint = 0.040
12950 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.07274 restraints
wR(F2) = 0.169H-atom parameters constrained
S = 1.11Δρmax = 0.55 e Å3
6338 reflectionsΔρmin = 0.32 e Å3
390 parameters
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)
Si10.25363 (13)0.87059 (11)0.07043 (8)0.0648 (3)
Si20.35367 (9)0.85862 (8)0.26534 (7)0.0431 (2)
Si30.44457 (8)0.58120 (7)0.30819 (6)0.0318 (2)
Si40.49207 (8)0.61058 (7)0.52203 (6)0.0325 (2)
O10.3102 (4)0.8299 (3)0.1668 (2)0.0902 (11)
O20.3845 (2)0.72946 (19)0.32207 (15)0.0411 (5)
N10.4736 (2)0.5313 (2)0.42053 (17)0.0314 (5)
C40.3722 (5)0.7923 (5)0.0386 (3)0.0848 (15)
H4A0.38300.70250.03030.127*
H4B0.45650.81740.04510.127*
H4C0.34020.81510.09840.127*
C50.2206 (6)0.9597 (5)0.3495 (4)0.111 (2)
H5A0.14350.92090.36580.167*
H5B0.19951.03890.31750.167*
H5C0.24710.97370.41050.167*
C60.5004 (6)0.9265 (6)0.2308 (5)0.125 (3)
H6A0.56950.87030.18480.187*
H6B0.53000.94000.29060.187*
H6C0.48031.00580.19850.187*
C70.3206 (3)0.5015 (3)0.2770 (2)0.0361 (6)
C80.3566 (3)0.3802 (3)0.2406 (2)0.0452 (8)
H8A0.44610.34090.22660.054*
C90.2644 (4)0.3153 (4)0.2242 (3)0.0568 (9)
H9A0.29100.23220.20020.068*
C100.1356 (4)0.3712 (4)0.2427 (3)0.0636 (11)
H10A0.07270.32660.23150.076*
C110.0964 (4)0.4913 (4)0.2774 (3)0.0625 (11)
H11A0.00680.53010.28950.075*
C120.1883 (3)0.5556 (4)0.2945 (3)0.0500 (8)
H12A0.16040.63860.31880.060*
C130.5940 (3)0.5541 (3)0.2047 (2)0.0390 (7)
C140.7229 (9)0.5085 (12)0.2155 (7)0.046 (2)0.58 (2)
H140.73640.49150.28020.055*0.58 (2)
C150.8279 (8)0.4885 (15)0.1357 (6)0.060 (3)0.58 (2)
H150.91330.46310.14620.072*0.58 (2)
C160.8121 (10)0.5046 (13)0.0405 (8)0.054 (2)0.58 (2)
H160.88510.48520.01470.064*0.58 (2)
C14'0.7159 (15)0.5652 (18)0.2198 (11)0.056 (4)0.42 (2)
H14'0.72470.57530.28560.067*0.42 (2)
C15'0.8242 (12)0.562 (2)0.1404 (9)0.065 (4)0.42 (2)
H15'0.90820.56070.15200.078*0.42 (2)
C16'0.8082 (16)0.5605 (18)0.0437 (12)0.061 (4)0.42 (2)
H16'0.87960.56710.01070.073*0.42 (2)
C170.6879 (4)0.5495 (4)0.0261 (3)0.0604 (10)
H17A0.67630.57140.03840.072*
C180.5815 (3)0.5621 (3)0.1065 (2)0.0489 (8)
H18A0.49630.57690.09470.059*
C190.3401 (3)0.7168 (3)0.5883 (2)0.0379 (7)
C200.2205 (3)0.7236 (3)0.5635 (2)0.0455 (8)
H20A0.21640.67580.50880.055*
C210.1073 (4)0.7988 (3)0.6170 (3)0.0542 (9)
H21A0.02690.80160.59880.065*
C220.1108 (4)0.8692 (3)0.6962 (3)0.0571 (10)
H22A0.03310.92020.73280.069*
C230.2274 (4)0.8653 (3)0.7220 (3)0.0596 (10)
H23A0.23010.91370.77680.072*
C240.3415 (4)0.7910 (3)0.6683 (3)0.0488 (8)
H24A0.42180.79060.68610.059*
C250.6302 (3)0.6964 (3)0.4937 (2)0.0396 (7)
C260.6095 (4)0.8199 (4)0.4685 (3)0.0632 (11)
H26A0.52330.86260.46950.076*
C270.7126 (5)0.8820 (4)0.4419 (4)0.0888 (16)
H27A0.69650.96660.42440.107*
C280.8367 (5)0.8235 (5)0.4405 (4)0.0767 (13)
H28A0.90690.86700.42160.092*
C290.8607 (4)0.7013 (4)0.4664 (3)0.0577 (10)
H29A0.94700.66030.46670.069*
C300.7575 (3)0.6387 (3)0.4920 (2)0.0475 (8)
H30A0.77450.55390.50880.057*
C10.0010 (15)0.8122 (14)0.1453 (11)0.143 (6)0.523 (13)
H1A0.01720.79540.20920.172*0.523 (13)
H1B0.08050.80420.13310.172*0.523 (13)
C20.0907 (15)0.8463 (12)0.0740 (10)0.088 (4)0.523 (13)
H20.06580.86100.01270.105*0.523 (13)
C30.2438 (10)1.0414 (7)0.0555 (6)0.047 (2)0.523 (13)
H3A0.18111.08510.11300.071*0.523 (13)
H3B0.21511.06720.00530.071*0.523 (13)
H3C0.33021.06130.05090.071*0.523 (13)
C1'0.269 (2)1.105 (2)0.0102 (17)0.202 (11)0.477 (13)
H1'10.35551.06570.02060.242*0.477 (13)
H1'20.24151.19160.00290.242*0.477 (13)
C2'0.187 (2)1.041 (2)0.0620 (16)0.147 (9)0.477 (13)
H2'0.09981.07780.09370.177*0.477 (13)
C3'0.1027 (19)0.797 (2)0.0976 (15)0.122 (7)0.477 (13)
H3'10.03880.83820.15580.183*0.477 (13)
H3'20.12760.70900.11110.183*0.477 (13)
H3'30.06380.80600.04000.183*0.477 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.0854 (9)0.0687 (7)0.0447 (6)0.0075 (6)0.0297 (6)0.0025 (5)
Si20.0505 (5)0.0395 (5)0.0392 (5)0.0033 (4)0.0152 (4)0.0057 (4)
Si30.0321 (4)0.0377 (4)0.0253 (4)0.0043 (3)0.0083 (3)0.0021 (3)
Si40.0369 (4)0.0349 (4)0.0267 (4)0.0082 (3)0.0087 (3)0.0027 (3)
O10.164 (3)0.0658 (19)0.0599 (19)0.024 (2)0.064 (2)0.0151 (15)
O20.0486 (13)0.0378 (12)0.0338 (11)0.0020 (9)0.0093 (9)0.0046 (9)
N10.0355 (13)0.0341 (13)0.0264 (12)0.0079 (10)0.0098 (10)0.0009 (9)
C40.109 (4)0.082 (3)0.053 (3)0.007 (3)0.022 (3)0.007 (2)
C50.144 (5)0.077 (3)0.071 (3)0.053 (3)0.005 (3)0.006 (3)
C60.106 (4)0.127 (5)0.170 (6)0.065 (4)0.064 (4)0.101 (5)
C70.0369 (16)0.0471 (18)0.0243 (14)0.0078 (13)0.0077 (12)0.0034 (12)
C80.051 (2)0.052 (2)0.0345 (16)0.0103 (15)0.0155 (14)0.0023 (14)
C90.076 (3)0.053 (2)0.049 (2)0.0226 (19)0.0210 (19)0.0023 (16)
C100.068 (3)0.089 (3)0.050 (2)0.045 (2)0.0208 (19)0.007 (2)
C110.039 (2)0.094 (3)0.058 (2)0.018 (2)0.0143 (17)0.003 (2)
C120.0349 (17)0.062 (2)0.053 (2)0.0062 (15)0.0121 (15)0.0067 (16)
C130.0381 (17)0.0496 (18)0.0278 (15)0.0054 (14)0.0076 (12)0.0044 (13)
C140.032 (3)0.067 (6)0.037 (4)0.010 (4)0.009 (3)0.011 (4)
C150.034 (3)0.095 (7)0.048 (4)0.011 (4)0.007 (3)0.009 (4)
C160.040 (4)0.071 (6)0.042 (4)0.012 (4)0.005 (3)0.006 (5)
C14'0.049 (5)0.076 (8)0.035 (5)0.003 (6)0.010 (4)0.003 (6)
C15'0.045 (5)0.098 (9)0.053 (5)0.019 (6)0.012 (4)0.007 (6)
C16'0.058 (6)0.072 (8)0.044 (5)0.008 (6)0.002 (4)0.010 (6)
C170.050 (2)0.101 (3)0.0295 (17)0.017 (2)0.0073 (15)0.0096 (18)
C180.0416 (18)0.072 (2)0.0311 (16)0.0078 (16)0.0085 (14)0.0045 (15)
C190.0443 (17)0.0364 (16)0.0327 (15)0.0079 (13)0.0086 (13)0.0032 (12)
C200.0467 (19)0.0465 (19)0.0401 (18)0.0099 (15)0.0024 (14)0.0070 (14)
C210.0421 (19)0.060 (2)0.055 (2)0.0064 (16)0.0035 (16)0.0028 (17)
C220.057 (2)0.047 (2)0.051 (2)0.0069 (17)0.0053 (17)0.0043 (16)
C230.078 (3)0.047 (2)0.045 (2)0.0090 (18)0.0144 (19)0.0126 (16)
C240.060 (2)0.0404 (18)0.0448 (19)0.0044 (15)0.0214 (16)0.0045 (14)
C250.0485 (18)0.0440 (18)0.0308 (15)0.0164 (14)0.0124 (13)0.0038 (12)
C260.066 (3)0.057 (2)0.077 (3)0.0246 (19)0.029 (2)0.024 (2)
C270.087 (4)0.066 (3)0.130 (5)0.043 (3)0.041 (3)0.046 (3)
C280.073 (3)0.082 (3)0.089 (3)0.052 (3)0.019 (2)0.017 (3)
C290.046 (2)0.076 (3)0.053 (2)0.0228 (18)0.0060 (16)0.0019 (19)
C300.0470 (19)0.054 (2)0.0413 (18)0.0131 (15)0.0065 (15)0.0004 (15)
C10.144 (10)0.154 (10)0.133 (9)0.024 (8)0.039 (8)0.000 (7)
C20.099 (7)0.080 (7)0.089 (7)0.026 (6)0.026 (6)0.003 (6)
C30.063 (5)0.039 (4)0.042 (4)0.001 (3)0.025 (3)0.009 (3)
C1'0.222 (14)0.194 (13)0.196 (14)0.045 (9)0.055 (9)0.013 (9)
C2'0.146 (12)0.171 (12)0.129 (11)0.044 (9)0.027 (8)0.016 (8)
C3'0.118 (10)0.127 (11)0.119 (10)0.028 (8)0.025 (8)0.018 (8)
Geometric parameters (Å, º) top
Si1—O11.613 (3)C16—C171.389 (12)
Si1—C21.808 (15)C16—H160.9500
Si1—C41.837 (5)C14'—C15'1.392 (19)
Si1—C31.874 (8)C14'—H14'0.9500
Si1—C2'1.89 (2)C15'—C16'1.39 (2)
Si1—C3'1.90 (2)C15'—H15'0.9500
Si2—O11.603 (3)C16'—C171.398 (18)
Si2—O21.622 (2)C16'—H16'0.9500
Si2—C51.817 (5)C17—C181.379 (5)
Si2—C61.828 (5)C17—H17A0.9500
Si3—O21.635 (2)C18—H18A0.9500
Si3—N11.715 (2)C19—C201.394 (5)
Si3—C131.859 (3)C19—C241.402 (4)
Si3—C71.865 (3)C20—C211.388 (5)
Si4—N11.748 (2)C20—H20A0.9500
Si4—N1i1.749 (2)C21—C221.374 (5)
Si4—C191.865 (3)C21—H21A0.9500
Si4—C251.867 (3)C22—C231.374 (6)
Si4—Si4i2.4940 (17)C22—H22A0.9500
N1—Si4i1.749 (2)C23—C241.391 (5)
C4—H4A0.9800C23—H23A0.9500
C4—H4B0.9800C24—H24A0.9500
C4—H4C0.9800C25—C261.385 (5)
C5—H5A0.9800C25—C301.386 (5)
C5—H5B0.9800C26—C271.382 (6)
C5—H5C0.9800C26—H26A0.9500
C6—H6A0.9800C27—C281.360 (6)
C6—H6B0.9800C27—H27A0.9500
C6—H6C0.9800C28—C291.375 (6)
C7—C81.393 (4)C28—H28A0.9500
C7—C121.395 (4)C29—C301.386 (5)
C8—C91.390 (5)C29—H29A0.9500
C8—H8A0.9500C30—H30A0.9500
C9—C101.367 (6)C1—C21.306 (9)
C9—H9A0.9500C1—H1A0.9500
C10—C111.373 (6)C1—H1B0.9500
C10—H10A0.9500C2—H20.9500
C11—C121.388 (5)C3—H3A0.9800
C11—H11A0.9500C3—H3B0.9800
C12—H12A0.9500C3—H3C0.9800
C13—C181.397 (4)C1'—C2'1.298 (10)
C13—C14'1.402 (17)C1'—H1'10.9500
C13—C141.419 (11)C1'—H1'20.9500
C14—C151.365 (12)C2'—H2'0.9500
C14—H140.9500C3'—H3'10.9800
C15—C161.372 (14)C3'—H3'20.9800
C15—H150.9500C3'—H3'30.9800
O1—Si1—C2116.9 (5)C13—C14—H14119.1
O1—Si1—C4107.6 (2)C14—C15—C16121.1 (8)
C2—Si1—C4110.8 (5)C14—C15—H15119.5
O1—Si1—C3108.2 (3)C16—C15—H15119.5
C2—Si1—C3104.9 (5)C15—C16—C17119.0 (8)
C4—Si1—C3108.1 (3)C15—C16—H16120.5
O1—Si1—C2'115.7 (7)C17—C16—H16120.5
C2—Si1—C2'86.9 (8)C15'—C14'—C13121.2 (12)
C4—Si1—C2'118.0 (7)C15'—C14'—H14'119.4
C3—Si1—C2'18.1 (7)C13—C14'—H14'119.4
O1—Si1—C3'100.8 (6)C14'—C15'—C16'119.3 (13)
C2—Si1—C3'19.4 (7)C14'—C15'—H15'120.4
C4—Si1—C3'108.9 (7)C16'—C15'—H15'120.4
C3—Si1—C3'122.4 (7)C15'—C16'—C17120.5 (12)
C2'—Si1—C3'104.3 (8)C15'—C16'—H16'119.7
O1—Si2—O2108.31 (14)C17—C16'—H16'119.7
O1—Si2—C5110.3 (2)C18—C17—C16119.3 (5)
O2—Si2—C5107.30 (19)C18—C17—C16'117.6 (7)
O1—Si2—C6109.3 (3)C16—C17—C16'25.4 (6)
O2—Si2—C6109.92 (19)C18—C17—H17A120.4
C5—Si2—C6111.7 (3)C16—C17—H17A120.4
O2—Si3—N1106.34 (11)C16'—C17—H17A115.8
O2—Si3—C13109.79 (13)C17—C18—C13122.6 (3)
N1—Si3—C13113.21 (13)C17—C18—H18A118.7
O2—Si3—C7108.97 (13)C13—C18—H18A118.7
N1—Si3—C7109.71 (12)C20—C19—C24117.1 (3)
C13—Si3—C7108.74 (14)C20—C19—Si4122.4 (2)
N1—Si4—N1i89.00 (11)C24—C19—Si4120.5 (2)
N1—Si4—C19114.02 (13)C21—C20—C19121.4 (3)
N1i—Si4—C19114.79 (12)C21—C20—H20A119.3
N1—Si4—C25114.72 (13)C19—C20—H20A119.3
N1i—Si4—C25114.17 (13)C22—C21—C20120.4 (4)
C19—Si4—C25109.14 (14)C22—C21—H21A119.8
N1—Si4—Si4i44.52 (8)C20—C21—H21A119.8
N1i—Si4—Si4i44.48 (8)C23—C22—C21119.6 (3)
C19—Si4—Si4i125.40 (11)C23—C22—H22A120.2
C25—Si4—Si4i125.46 (11)C21—C22—H22A120.2
Si2—O1—Si1153.0 (2)C22—C23—C24120.4 (3)
Si2—O2—Si3145.38 (14)C22—C23—H23A119.8
Si3—N1—Si4131.82 (15)C24—C23—H23A119.8
Si3—N1—Si4i137.03 (14)C23—C24—C19121.1 (3)
Si4—N1—Si4i91.00 (11)C23—C24—H24A119.5
Si1—C4—H4A109.5C19—C24—H24A119.5
Si1—C4—H4B109.5C26—C25—C30117.3 (3)
H4A—C4—H4B109.5C26—C25—Si4120.6 (3)
Si1—C4—H4C109.5C30—C25—Si4122.0 (2)
H4A—C4—H4C109.5C27—C26—C25120.9 (4)
H4B—C4—H4C109.5C27—C26—H26A119.6
Si2—C5—H5A109.5C25—C26—H26A119.6
Si2—C5—H5B109.5C28—C27—C26120.8 (4)
H5A—C5—H5B109.5C28—C27—H27A119.6
Si2—C5—H5C109.5C26—C27—H27A119.6
H5A—C5—H5C109.5C27—C28—C29120.0 (4)
H5B—C5—H5C109.5C27—C28—H28A120.0
Si2—C6—H6A109.5C29—C28—H28A120.0
Si2—C6—H6B109.5C28—C29—C30119.2 (4)
H6A—C6—H6B109.5C28—C29—H29A120.4
Si2—C6—H6C109.5C30—C29—H29A120.4
H6A—C6—H6C109.5C29—C30—C25121.8 (3)
H6B—C6—H6C109.5C29—C30—H30A119.1
C8—C7—C12117.0 (3)C25—C30—H30A119.1
C8—C7—Si3120.2 (2)C2—C1—H1A120.0
C12—C7—Si3122.7 (2)C2—C1—H1B120.0
C9—C8—C7121.4 (3)H1A—C1—H1B120.0
C9—C8—H8A119.3C1—C2—Si1131.9 (13)
C7—C8—H8A119.3C1—C2—H2114.1
C10—C9—C8119.9 (4)Si1—C2—H2114.1
C10—C9—H9A120.0Si1—C3—H3A109.5
C8—C9—H9A120.0Si1—C3—H3B109.5
C9—C10—C11120.4 (3)H3A—C3—H3B109.5
C9—C10—H10A119.8Si1—C3—H3C109.5
C11—C10—H10A119.8H3A—C3—H3C109.5
C10—C11—C12119.6 (4)H3B—C3—H3C109.5
C10—C11—H11A120.2C2'—C1'—H1'1120.0
C12—C11—H11A120.2C2'—C1'—H1'2120.0
C11—C12—C7121.6 (4)H1'1—C1'—H1'2120.0
C11—C12—H12A119.2C1'—C2'—Si1116 (2)
C7—C12—H12A119.2C1'—C2'—H2'122.1
C18—C13—C14'116.4 (7)Si1—C2'—H2'122.1
C18—C13—C14114.9 (5)Si1—C3'—H3'1109.5
C14'—C13—C1425.3 (6)Si1—C3'—H3'2109.5
C18—C13—Si3119.4 (2)H3'1—C3'—H3'2109.5
C14'—C13—Si3121.1 (6)Si1—C3'—H3'3109.5
C14—C13—Si3125.1 (4)H3'1—C3'—H3'3109.5
C15—C14—C13121.9 (8)H3'2—C3'—H3'3109.5
C15—C14—H14119.1
O2—Si2—O1—Si1171.8 (6)C14—C13—C14'—C15'82 (2)
C5—Si2—O1—Si154.7 (7)Si3—C13—C14'—C15'171.0 (9)
C6—Si2—O1—Si168.4 (7)C13—C14'—C15'—C16'6.8 (19)
C2—Si1—O1—Si2108.4 (8)C14'—C15'—C16'—C177 (2)
C4—Si1—O1—Si2126.1 (6)C15—C16—C17—C188.1 (12)
C3—Si1—O1—Si29.6 (8)C15—C16—C17—C16'85 (2)
C2'—Si1—O1—Si28.2 (10)C15'—C16'—C17—C1811.2 (15)
C3'—Si1—O1—Si2119.9 (9)C15'—C16'—C17—C1689 (2)
O1—Si2—O2—Si336.2 (3)C16—C17—C18—C1312.4 (9)
C5—Si2—O2—Si3155.2 (3)C16'—C17—C18—C1316.5 (11)
C6—Si2—O2—Si383.2 (4)C14'—C13—C18—C1716.4 (10)
N1—Si3—O2—Si2163.1 (2)C14—C13—C18—C1711.7 (8)
C13—Si3—O2—Si240.3 (3)Si3—C13—C18—C17176.5 (3)
C7—Si3—O2—Si278.7 (3)N1—Si4—C19—C205.1 (3)
O2—Si3—N1—Si419.6 (2)N1i—Si4—C19—C2095.6 (3)
C13—Si3—N1—Si4101.0 (2)C25—Si4—C19—C20134.8 (3)
C7—Si3—N1—Si4137.33 (19)Si4i—Si4—C19—C2045.1 (3)
O2—Si3—N1—Si4i166.09 (19)N1—Si4—C19—C24176.9 (2)
C13—Si3—N1—Si4i73.3 (2)N1i—Si4—C19—C2482.4 (3)
C7—Si3—N1—Si4i48.4 (2)C25—Si4—C19—C2447.2 (3)
N1i—Si4—N1—Si3176.1 (3)Si4i—Si4—C19—C24132.9 (2)
C19—Si4—N1—Si367.1 (2)C24—C19—C20—C211.3 (5)
C25—Si4—N1—Si359.8 (2)Si4—C19—C20—C21176.8 (3)
Si4i—Si4—N1—Si3176.1 (3)C19—C20—C21—C220.3 (6)
N1i—Si4—N1—Si4i0.0C20—C21—C22—C230.3 (6)
C19—Si4—N1—Si4i116.82 (13)C21—C22—C23—C240.2 (6)
C25—Si4—N1—Si4i116.28 (14)C22—C23—C24—C191.3 (6)
O2—Si3—C7—C8166.1 (2)C20—C19—C24—C231.8 (5)
N1—Si3—C7—C877.9 (3)Si4—C19—C24—C23176.3 (3)
C13—Si3—C7—C846.4 (3)N1—Si4—C25—C2693.3 (3)
O2—Si3—C7—C1218.2 (3)N1i—Si4—C25—C26166.0 (3)
N1—Si3—C7—C1297.9 (3)C19—Si4—C25—C2636.0 (3)
C13—Si3—C7—C12137.8 (3)Si4i—Si4—C25—C26143.9 (3)
C12—C7—C8—C91.2 (5)N1—Si4—C25—C3083.4 (3)
Si3—C7—C8—C9174.8 (3)N1i—Si4—C25—C3017.3 (3)
C7—C8—C9—C100.9 (5)C19—Si4—C25—C30147.3 (3)
C8—C9—C10—C110.0 (6)Si4i—Si4—C25—C3032.9 (3)
C9—C10—C11—C120.6 (6)C30—C25—C26—C270.6 (6)
C10—C11—C12—C70.3 (6)Si4—C25—C26—C27176.3 (4)
C8—C7—C12—C110.6 (5)C25—C26—C27—C280.5 (8)
Si3—C7—C12—C11175.3 (3)C26—C27—C28—C290.4 (8)
O2—Si3—C13—C1876.5 (3)C27—C28—C29—C301.1 (7)
N1—Si3—C13—C18164.8 (3)C28—C29—C30—C251.0 (6)
C7—Si3—C13—C1842.6 (3)C26—C25—C30—C290.1 (5)
O2—Si3—C13—C14'82.7 (10)Si4—C25—C30—C29176.9 (3)
N1—Si3—C13—C14'36.0 (10)O1—Si1—C2—C18.0 (18)
C7—Si3—C13—C14'158.2 (10)C4—Si1—C2—C1131.8 (15)
O2—Si3—C13—C14112.6 (7)C3—Si1—C2—C1111.8 (16)
N1—Si3—C13—C146.0 (7)C2'—Si1—C2—C1109.3 (17)
C7—Si3—C13—C14128.3 (7)C3'—Si1—C2—C144 (3)
C18—C13—C14—C157.4 (10)O1—Si1—C2'—C1'94.4 (19)
C14'—C13—C14—C1592 (2)C2—Si1—C2'—C1'147 (2)
Si3—C13—C14—C15178.7 (7)C4—Si1—C2'—C1'35 (2)
C13—C14—C15—C164.1 (14)C3—Si1—C2'—C1'25.3 (18)
C14—C15—C16—C174.2 (14)C3'—Si1—C2'—C1'155.9 (19)
C18—C13—C14'—C15'11.2 (15)
Symmetry code: (i) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formulaC60H70N2O4Si8
Mr1107.90
Crystal system, space groupTriclinic, P1
Temperature (K)173
a, b, c (Å)10.731 (2), 11.021 (2), 13.859 (3)
α, β, γ (°)88.320 (9), 76.120 (6), 78.860 (8)
V3)1561.0 (6)
Z1
Radiation typeMo Kα
µ (mm1)0.22
Crystal size (mm)0.41 × 0.28 × 0.22
Data collection
DiffractometerRigaku Saturn724+ CCD
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku, 2007)
Tmin, Tmax0.916, 0.954
No. of measured, independent and
observed [I > 2σ(I)] reflections
12950, 6338, 5389
Rint0.040
(sin θ/λ)max1)0.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.072, 0.169, 1.11
No. of reflections6338
No. of parameters390
No. of restraints74
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.55, 0.32

Computer programs: CrystalClear (Rigaku, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

The authors would like to thank the National Natural Science Foundation of China (grant No. 50803070) for financial support.

References

First citationRigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationZhu, Y. P., Guo, L., Zhang, Z. J., Xie, Z. M. & Xu, C. H. (2007). J. Appl. Polym. Sci. 105, 749–756.  CrossRef CAS Google Scholar

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Volume 67| Part 5| May 2011| Page o1234
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