DESIGNATION OF ABSOLUTE CONFIGURATION OF MULTIHETEREOCYCLIC 9,13-DICHLORO-22,22-DIPYRROLIDINE-1-YL1H,2H,13H,19H-9,13-(EPIAZENOPHOSPHAZENO)-9λ5,11λ5,13λ5-[1,3,5,2,4] BENZOXADIAZADİPHOSPHONINO[4',5':2,3][1,3,2]DIAZAPHOSPHOLO[2,1-D] [1,3,5,2,4]BENZOXADIAZADIPHOSPHONINE BY X-RAY CRYSTALLOGRAPHIC DATA

Year 2019, Volume: 61 Issue: 1, 15 - 30, 31.12.2019

Gamze Elmas , Aytuğ Okumuş , Satiye Sevim İsaoğlu Tuncer Hökelek , Zeynel Kılıç

Abstract

The title compound, 9,13-dichloro-22,22-dipyrrolidine-1-yl-1H,2H,13H,19H-9,13-(epiazenophosphazeno)-9λ5,11λ5,13λ5-1,3,5,2,4]benzoxadiazadiphosphonino [4',5':2,3][1,3,2]diazaphospholo[2,1-d][1,3,5,2,4]benzoxadiazadiphosphonine;
2(C24H32Cl2N8O2P4). 0.5 C6H12, a cyclotetraphosphazene derivative, has a geminaldipyrrolidino-2-trans-6-dichloro-ansa-spiro-ansa (gem-dipyrrolidino-2-trans-6-dichloroasa) structure in which the tricyclic parts are consisted of three eight-membered rings,
containing a tetrameric N4P4 and two ansa rings. However, all these rings are not planar. The asymmetric unit contains two crystallographically independent molecules and one half of the cyclohexane solvent molecule. In both molecules, it is expected that two P (P1 and P3/P1′ and P3′) atoms are stereogenic centres. Both gem-dipyrrolidino-2-trans-6-dichloro-asa molecules have trans structures according to the Cl atoms, and they are in the racemic forms. Besides, it is found that the absolute configurations of P1, P3 and P1′, P3′ phosphorus centers are RR and SS, respectively. The title compound has P-1 space group, a Sohncke chiral space
group, with the cell parameters of a = 9.6682(2), b = 13.8587(3), c = 24.0250(4) Å, � =105.249(2)°, � = 96.298(3)° and � = 98.367(3)°.

Keywords

Cyclotetraphosphazene, ansa-spiro-ansa-Structure, Pyrrolidine, X-ray crystallography

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