1,1,3,3,5,5,7,7-Octa­phenyl-2,6-dioxa-4,8-diaza-1,3,5,7-tetra­silacyclo­octa­ne

Zhen Lv; Lina Dai; Xuezhong Zhang; Zhijie Zhang; Zemin Xie

doi:10.1107/S1600536811014851

. 2011 Apr 29;67(Pt 5):o1233. doi: 10.1107/S1600536811014851

1,1,3,3,5,5,7,7-Octaphenyl-2,6-dioxa-4,8-diaza-1,3,5,7-tetrasilacyclooctane

Zhen Lv ^a, Lina Dai ^a, Xuezhong Zhang ^a, Zhijie Zhang ^a,^*, Zemin Xie ^a

PMCID: PMC3089214 PMID: 21754529

Abstract

The title molecule, C₄₈H₄₂N₂O₂Si₄, lies on a twofold rotation axis. The eight-membered ring has a slightly distorted boat conformation.

Related literature

For the hydrolysis of 1,3-bis-(hydroxydiphenylsilanyl)-2,2,4,4-tetraphenylcyclodisilazane, see: Voronkov et al. (1977 ▶).

Experimental

Crystal data

C₄₈H₄₂N₂O₂Si₄
M _r = 791.20
Monoclinic,
a = 12.1188 (18) Å
b = 17.016 (3) Å
c = 20.621 (3) Å
β = 93.216 (3)°
V = 4245.8 (11) Å³
Z = 4
Mo Kα radiation
μ = 0.18 mm⁻¹
T = 173 K
0.35 × 0.35 × 0.05 mm

Data collection

Rigaku MM007-HF CCD (Saturn 724+) diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2007 ▶) T _min = 0.939, T _max = 0.991
14029 measured reflections
4833 independent reflections
4411 reflections with I > 2σ(I)
R _int = 0.039

Refinement

R[F ² > 2σ(F ²)] = 0.052
wR(F ²) = 0.120
S = 1.10
4833 reflections
253 parameters
H-atom parameters constrained
Δρ_max = 0.39 e Å⁻³
Δρ_min = −0.30 e Å⁻³

Data collection: CrystalClear (Rigaku, 2007 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; 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.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811014851/lh5233sup1.cif

e-67-o1233-sup1.cif^{(28.8KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811014851/lh5233Isup2.hkl

e-67-o1233-Isup2.hkl^{(236.8KB, hkl)}

Supplementary material file. DOI: 10.1107/S1600536811014851/lh5233Isup3.cml

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

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

supplementary crystallographic information

Comment

The title compound is one of the hydrolysis products of 1,3-bis-(hydroxydiphenylsilanyl)-2,2,4,4-tetraphenylcyclodisilazane. Voronkov et al. (1977) reported that the hydrolysis of 1,3-bis-(hydroxydiphenylsilanyl)-2,2,4,4-tetraphenylcyclodisilazane in base medium could give 1,1,3,3,5,5,7,7-octaphenyl-2,4-dioxa-6,8,-diaza-1,3,5,7-tetrasilacyclo-octane and we have found that the title compound was also produced. Its crystal structure is presented herein. The molecular structure of the title compound is shown in Fig. 1. The eight-membered ring has a slightly disorted boat conformation.

Experimental

The reaction scheme is shown in Fig. 2. 1 ml aqueous solution of sodium hydroxide (0.1 mol/L) was added to a solution of 1,3-bis-(hydroxydiphenylsilanyl)-2,2,4,4-tetraphenylcyclodisilazane (1 g) in tetrahydrofuran (10 ml). After stirring for 30 min at room temprature, the solvents were removed under reduced pressure. The crude product was recrystallized from n-hexane to give colorless crystals.