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1.  Synthesis and Structural Characterization of a Metal Cluster and a Coordination Polymer Based on the [Mn6(μ4-O)2]10+ Unit 
A new 1-D coordination polymer {[Mn6O2(O2CMe)10(H2O)4]·2.5H2O}∞ (1·2.5H2O)∞ and the cluster [Mn6O2(O2(O2CPh)10 (py)2(MeCN)(H2O)]·2MeCN (2·2MeCN) are reported. Both compounds were synthesized by room temperature reactions of [Mn3(μ3-O)(O2CR)6(L)2(L′)] (R = Me, L = L′ = py, (1·2.5H2O)∞; R = Ph, L = py, L′ = H2O, 2·2MeCN) in the presence of 3-hydroxymethylpyridine (3hmpH) in acetonitrile. The structures of these complexes are based on hexanuclear mixed-valent manganese carboxylate clusters containing the [Mn4IIMn2III(μ4-O)2]10+ structural core. (1·2.5H2O)∞ consists of zigzag chain polymers constructed from [Mn6O2(O2CMe)10(H2O)4] repeating units linked through acetate ligands, whereas 2·2MeCN comprises a discrete Mn6-benzoate cluster.
PMCID: PMC2902058  PMID: 20634987
2.  Zinc(II) and Nickel(II) Benzoate Complexes from the Use of 1-methyl-4,5-diphenylimidazole 
Two new complexes, [Zn(O2CPh)2(L)2]·2MeOH (1·2MeOH) and [Ni2(O2CPh))4(L)2]·2MeCN (2·2MeCN), have been synthesized and characterized by X-ray analysis in the course of an ongoing investigation of the MII/X−/L [MII = Co, Ni, Cu, Zn; X− = Cl−, Br−, I−, NCS−, NO3−, N3−, PhCO2−; L = 1-methyl-4,5-diphenylimidazole] reaction system, aiming at understanding and assessing the relative strength and the way in which the intermolecular interactions control the supramolecular organization of these compounds. In the mononuclear complex 1·2MeOH, the benzoate ion acts as a monodentate ligand resulting in a distorted tetrahedral N2O2 coordination environment. Complex 2·2MeCN exhibits a dinuclear paddle-wheel structure; each NiII has a square pyramidal NiNO4 chromophore with four benzoate oxygens in the basal plane and the pyridine-type nitrogen atom of one ligand L at the apex. The structure of 1·2MeOH is stabilized by intramolecular π-π interactions between aromatic rings of adjacent 4,5-diphenylimidazole moieties; it is a feature also evidenced in similar compounds of the type [MX2L2].
PMCID: PMC2927736  PMID: 20811497
3.  Tricyclo­[,7]nonane-3,7-diyl bis­(methane­sulfonate) 
The crystal structure of the title compound, C11H18O6S2, was determined to investigate the effect of the eclipsed mesyl groups on the bond length of the vicinal quaternary C atoms. The two quaternary C atoms of the noradamantane skeleton and the two O atoms to which they are connected all located essentially in the same plane [maximum deviation 0.01 Å], resulting in an eclipsing conformation of the C—O bonds. The C—C bond of the quaternary C atoms is 1.597 (3) Å is considerably longer than the other C—C bonds of the mol­ecule.
PMCID: PMC2979816  PMID: 21579828
4.  (2E,4E,6E)-3-Methyl-7-(pyren-1-yl)octa-2,4,6-trienoic acid 
The title compound, C25H20O2, was synthesized by a Wittig reaction between triphen­yl[1-(pyren-1-yl)eth­yl]phospho­nium bromide and ethyl (2E,4E)-3-methyl-6-oxohexa-2,4-dienoate, in the presence of n-butyl lithium, followed by saponification. It was obtained pure in the all-trans configuration following crystallization from ethyl acetate. The asymmetric unit contains two independent mol­ecules (A and B), which are arranged almost parallel to each other within the crystal structure. The triene chain is not coplanar with the pyrene ring system, forming dihedral angles of 52.8 (1) and 42.2 (1)° for mol­ecules A and B, respectively. Inter­molecular hydrogen bonds between the carboxyl groups of the mol­ecules link them into centrosymmetric pairs, AA and BB, each with the R 2 2(8) graph-set motif.
PMCID: PMC2970380  PMID: 21578017

Results 1-4 (4)