Abstract
Single-crystal diffraction data of dodecasil 1H (D1H), a clathrasil (SiO2) with 1-aminoadamantane and NH3 as guest molecules, were collected from a small crystal (V = 2.5 × 105 lxm 3) with synchrotron radiation (SR) (A =0.78914~) at the five-circle diffractometer of HASYLAB (DESY, Hamburg, Germany). The space group is P6/mmm with a = 13.826 (3), c = 11.186 (3) A,, V = 1852 (1) A 3, the content of the unit cell is 34SiOdCIoHIsNHz)5NH3, F(000) = 1154, Dx = 2.043 g cm- 3, Mr = 2278.4 g mol- 1. The structure refinement is based on 784 unique reflections (R = 2.62%, wR = 1.76%). The results are compared with studies using a conventional X-ray source. All O-atom sites were found to be split (average O---O distance 0.5 A) indicating a disorder of the SiO2 host framework. The mean Si--O distance, Si--O---Si angle and Ueq (oxygen) from anisotropic refinement without splitting were 1.568 A, 170.7 °, 0.065 A 2, respectively, changed to 1.596 (11) A, 155 (3) °, 0.038 (6) A 2. Simulations based on distance least-squares calculations qualitatively match the results of the refinement. Additional data collected on a conventional diffractometer with monochromatized Mo Ka radiation revealed only limited evidence for split O-atom positions. Anisotropic refinement of non-split O atoms with data collected at 155 K [a = 13.748 (3), c = 11.128 (3) A] with Mo Ka radiation gave only a minor decrease of the large O-atom r.m.s, amplitudes perpendicular to
Published Version
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