Three new ruthenium-sulfur dioxide linkage photoisomeric complexes in the [Ru(NH(3))(4)(SO(2))X]Cl(2)·H(2)O family (X = pyridine (1); 3-chloropyridine (2); 4-chloropyridine (3)) have been developed in order to examine the effects of the trans-ligand on the nature of the photo-induced SO(2) coordination to the ruthenium ion. Solid-state metastable η(1)-O-bound (MS1) and η(2)-side S,O-bound (MS2) photoisomers are crystallographically resolved by probing a light-induced crystal with in situ diffraction. This so-called photocrystallography reveals the highest known photoconversion fraction of 58(3)% (in 1) for any solid-state SO(2) linkage photoisomer. The decay of this MS1 into the MS2 state was modeled via first-order kinetics with a non-zero asymptote. Furthermore, the MS2 decay kinetics of the three compounds were examined according to their systematically varying trans-ligand X; this offers the first experimental evidence that the MS2 state is primarily stabilized by donation from the S-O(bound) electrons into the Ru dσ-orbital rather than π-backbonding as previously envisaged. This has important consequences for the optoelectronic application of these materials since this establishes, for the first time, a design protocol that will enable one to control their photoconversion levels.

Photoconversion Bonding Mechanism in Ruthenium Sulfur Dioxide Linkage Photoisomers Revealed by in Situ Diffraction

One way or another: The N‐bound NO2 group in [Ni(Et4dien)(η2‐O,ON)(η1‐NO2)] (see structure Ni turquoise, N blue, O red) has been shown to undergo reversible conversion into the O‐bound nitrito linkage isomer under both thermal and photoactivation of a single crystal. Et4dien=N,N,N′,N′‐tetraethyldiethylenetriamine.

Metastable linkage isomerism in [Ni(Et4dien)(NO2)2]: a combined thermal and photocrystallographic structural investigation of a nitro/nitrito interconversion.

Dynamic single-crystal diffraction studies using synchrotron radiation

We report a new family of photoactive molecular compounds for which reversible solid state transformations and linkage isomerism have been observed using in situ X-ray diffraction. The interaction of tris(triphenylphosphine)silver(I) with eicosaborate [B20H18]2− afforded a binuclear complex with a bridging boron cluster that underwent a series of isomerization transformations occurring in a single-crystal-to-single-crystal manner without crystal degradation and obeying the criteria for an effective molecular switch.

Reversible single-crystal-to-single-crystal photoisomerization of a silver(I) macropolyhedral borane

With the increase in interest in photocrystallographic experiments, the use of light-emitting diodes (LEDs) provides an alternative, low-budget light source (by comparison to lasers) and allows photocrystallographic experiments to be carried out readily. Here the design of an LED array device suitable for use in single-crystal X-ray diffraction experiments is reported, and the experimental methodology used for determining the structures of metastable species is described.

Photocrystallography – design and methodology for the use of a light‐emitting diode device

4 as problem to be solved. We determined a crystal structure of a complex of ArgRS from Pyrococcus horikoshii, tRNACCU and ATP analog with Rfactor = 0.215 (Rfree = 0.259) at 2.0 Å resolution and could give one solution for this problem using newly obtained structural information about position of ATP. The experimental results show that the ArgRS protein lacking the additional N-terminal domain characteristic for ArgRS possesses sufficient catalytic activity in the aminoacylation reaction for tRNA. Modeling of relative positions of amino acid, Ade76 of tRNA and ATP on ArgRS was made to find the suitable position to tRNA-assisted formation mechanism of Arg-AMP. It was found that formation of hydrogen bond between 2’OH of Ade76 of tRNA and O2 of carboxy group -C-O2H=O1 of arginine can be achieved in one conformation by rotation around C α-C of carboxy group. In ATP-PPi exchange reaction at low pH, reversible conversion between C=O1 and C-O1-Pα is controlled by the formation of this hydrogen bond. On the other hand, at pH8.0, experimental results in the deacylation reaction of Arg-tRNA is also understood by mechanism that NH of guanidium group -NH=C(NH2)2 of Arg-tRNA donates a proton to C=O2 of ester bond of ArgtRNA, resulting in carbonium C-O2H. We discuss in detail these mechanisms.

/pdf/fbpase-allosteric-transition-crystal-structures-of-liver-and-6105nn580f.pdf

FBPase allosteric transition: crystal structures of liver and muscle isoforms from rodents and human

Human liver fructose-1,6-bisphosphatase 1 (fructose 1,6-bisphosphate 1-phosphatase, E.C.3.1.3.11) complexed with the allosteric inhibitor 1-(5-bromo-1,3-thiazol-2-yl)-3-[5-(4-methoxyphenyl)thiophen-2-yl]sulfonylurea and with fructose-2,6-diphosphate

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FBPase allosteric transition: crystal structures of liver and muscle isoforms from rodents and human

Human liver fructose-1,6-bisphosphatase 1 (fructose 1,6-bisphosphate 1-phosphatase, E.C.3.1.3.11) complexed with the allosteric inhibitor 1-(5-bromo-1,3-thiazol-2-yl)-3-[5-(4-methoxyphenyl)thiophen-2-yl]sulfonylurea and with fructose-2,6-diphosphate