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Volumn 47, Issue 16, 2008, Pages 7080-7082

Synthesis and structure of an aluminum borate chloride consisting of 12-membered borate rings and aluminate clusters

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EID: 50449093593 PISSN: 00201669 EISSN: None Source Type: Journal
DOI: 10.1021/ic8010053 Document Type: Article

Times cited : (49)

References (18)

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- Chemical analysis was done using ICP and XPS. TGA-MS was carried out on a thermal analyzer (NETZSCH STA, 449C) equipped with a quadrupole mass spectrometer (Balzers MID, with a 37-839°C working temperature range and a 10°C/min heating rate, showing stepwise weight loss and evolution of HCl and water molecules. IR: 705, 853, 1018 (BO4, 1183, 1349 (BO 3, 3269 (B-OH, 3490 (μ3-OH) cm-1. 27Al NMR: δ -1.2 (Al(H2O)63+ standard) is typical for the octahedral Al3, 11B NMR shows two resonance signals, a singlet at δ -6.39 (BO4) and a doublet at δ -15.75 and 3.46 (BO3, BF3.Et 2O standard, 1H NMR shows two signals at δ 7.4 and 5.2 TMS standard
- 1H NMR shows two signals at δ 7.4 and 5.2 (TMS standard).

11
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- Crystallographic study. X-ray powder diffraction data were collected on a Bruker D8-Advance diffractometer with a curved germanium primary monochromator (Cu Kα1) in a transmission mode (2θ range, 9-100°, step, 0.0144°, scan speed, 60 s/step, 50 kV, 40 mA) at room temperature. The diffraction pattern can be readily indexed to rhombohedral, a, 15.0613(1) Å and c, 14.0134(2) Å, and the possible space groups R3, R3, R32, R3m, or R3m. The electron diffraction pattern confirms the rhombohedral setting of the structure (see the Supporting Information, The nonlinear optical effect (0.3, KDP as reference) of the powder sample rules out the centrosymmetric space groups. The structure model was initially established in the space group R3m, in which the AlO6 octahedron was used as a rigid fragment in the ab initio structural determination TOPAS 4, Af
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- 3 counts only the framework and the counter chlorine anions. The chemical analyses also indicated the presence of a small amount of Na ions in PKU-8, but the content varies for samples obtained under slightly different reaction conditions. The highest sodium content found in the PKU-8 samples is about Al:Na = 1:0.3.
- 3 counts only the framework and the counter chlorine anions. The chemical analyses also indicated the presence of a small amount of Na ions in PKU-8, but the content varies for samples obtained under slightly different reaction conditions. The highest sodium content found in the PKU-8 samples is about Al:Na = 1:0.3.

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