l l ] Crystal data for [1-2H][CoCI4] O.SC,H,CH,: crystal size: O.lOx0.20 x 0.20 mm, monoclinic, space group C2/c. a =19.478(7), b =11.245(1), c = 26.43(1)A, !3=10424(2). V = 5611(3)A3, p,,,,,=1.48gcm-3, 20,,, =46": JL = 0.52 mm-1, M~, , rad,at,on ( ; , = 0,71069 A) for z = 8, intensity datawere collected using the w-28 scan mode on an Enraf Nonius CAD-4 diffractometer and were corrected for Lorentz, polarization, and absorption effects, but not for extinction. The structure was solved with direct methods. Least-squares refinement based on 1301 reflections with l,,e,>2.0u(IJ (out of 4043 unique reflections), and 298 parameters on convergence gave final values of R = 0.081 and R, = 0.065. Methylene and aromatic hydrogen atoms were placed in calculated positions (d(C,H) =1.08 and 1.00 A, respectively) with their positional and thermal parameters fixed, temperature factors being based upon the carbon atoms to which they are bonded. Quaternary ammonium hydrogen atoms were located by inspection of a al and thermal were fixed, temperature factors being based upon the atoms to which they are bonded. The toluene molecule was observed to lie on a crystallographic twofold axis and exhibit threefold disorder with the carbon atoms of the methyl group displaying site occupancies of0.4 (CS5) and 0.3 (CS5B).

A series of alpha-substituted beta-alanine (beta) linked polyamides (DbaPyPyPy-beta*-PyPyPy) were prepared and examined. This resulted in the observation that while most substituents disrupt DNA binding, (R)-alpha-methoxy-beta-alanine (beta((R)-OMe)) maintains strong binding affinity and preferentially adopts a hairpin versus extended binding mode, providing an alternative hairpin linker to gamma-aminobutyric acid (gamma). A generalized variant of a fluorescent intercalator displacement assay conducted on a series of hairpin deoxyoligonucleotides containing a systematically varied A/T-rich binding site size was developed to distinguish between the extended binding of the parent beta-alanine 1 (DbaPyPyPy-beta-PyPyPy) and the hairpin binding of 3 (DbaPyPyPy-beta((R)-OMe)-PyPyPy).

An unprecedented addition pattern for the novel hexakis‐cyclopropanated C60 (±)‐1 was prepared by a sequence of tether‐directed regioselective remote functionalizations. The X‐ray crystal structure revealed the positioning of the six addends in a distinct helical array along an equatorial belt.

The construction of molecules such as knots and links can be facilitated by using metal–ligand coordination complexes as template structures; however, the control of the stereochemistry by cooperative steric interactions among metal–ligand sites remains a challenge. A simple, but general, cantilever control mechanism is demonstrated here through the stereoselective synthesis of a trinuclear copper(I)‐bipyridine triskelion (see picture).