4,4′,4′′-(Methanetriyl)triphenyl tris(2,2,5,5-tetramethyl-1-oxyl-3-pyrroline-3-carboxylate) benzene trisolvate

Abstract

Key indicators: single-crystal X-ray study; T = 164 K; mean (C-C) = 0.005 Å; some non-H atoms missing; disorder in main residue; R factor = 0.072; wR factor = 0.194; data-to-parameter ratio = 19.3.In the asymmetric unit of the title compound, C 46 H 52 N 3 O 9 Á-3C 6 H 6 , two of the benzene solvent molecules are located in general positions and two are disposed about inversion centers. One of the benzene molecules on an inversion center was grossly disordered and was excluded using the SQUEEZE subroutine in PLATON [Spek (2009). Acta Cryst. D65, 148-155]. In addition, one of the 2,2,5,5-tetramethyl-1-oxyl-3-pyrrolin-3-ylcarbonyl groups is disordered over two orientations with refined occupancies of 0.506 (2) and 0.494 (2). The 1-oxyl-3-pyrroline-3-carboxylate groups are essentially planar, with mean deviations from the planes of 0.026 (2), 0.012 (2), 0.034 (4) and 0.011 (4) Å . In the crystal structure, molecules are connected by five weak intermolecular C-HÁ Á ÁO and four weak intermolecular C-HÁ Á Á (benzene) interactions. Related literature ExperimentalCrystal data

Crystal structure of 4′-{[4-(2,2′:6′,2′′-terpyridyl-4′-yl)phenyl]ethynyl}biphenyl-4-yl (2,2,5,5-tetramethyl-1-oxyl-3-pyrrolin-3-yl)formate benzene 2.5-solvate

“…It is essentially planar with the two outer rings B (N3/C35-C39) and C (N4/ C40-C44) being inclined to the central pyridine ring A (N2/ C30-C34) by 8.70 (15) and 14.55 (14) , respectively. The conformation of the nitroxyl group in (1) is similar to that found in (3), with a planar pyrroline (N1/C1-C4) ring assuming an angle of 72.61 (15) to the central pyridine ring A [see also Margraf et al (2009) and Schuetz et al (2010)]. In (3) this dihedral angle is 88.44 (7) , while in (2) the same dihedral angle is 21.6 (2) .…”

The crystal structure of 4′-{4-[(2,2,5,5-tetramethyl-N-oxyl-3-pyrrolin-3-yl)ethynyl]phenyl}-2,2′:6′,2′′-terpyridine

“…deviation from the mean plane = 0.003 Å ) and 1.98 (5) (N2, C6-C10, r.m.s deviation from the mean plane = 0.006 Å ), respectively. The pyrroline-N-oxyl unit commonly found for such nitroxyls is seen in the structure and its mean plane (N3, C19-C22, r.m.s deviation from the mean plane = 0.006 Å ) subtends a dihedral angle of 88.44 (7) to the mean plane of the central pyridine ring (for similar structural motifs, see Margraf et al, 2009 andSchuetz et al, 2010). The subunits are linked by a 4-ethinylenephenylene group.…”