Inorganic Chemistry Communications (v.9, #4)

Contents List (iii-ix).

An original Sm(III)–orotic acid complex with an unprecedented coordination mode μ42 κO,O′:η2 κO′,N:η1κ″:η1κO‴ for HL2− in the novel bi-layered structure has been synthesized, which exhibits an antiferromagnetic-like interaction and luminescent property.The first structurally characterized orotato samarium(III) complex, [Sm2(HL)2(ox)(H2O)2] n  · 2.5nH2O (1), with a novel bi-layered structure has been synthesized and structurally characterized by X-ray crystallography, in which orotic acid ligands exhibit two coordination modes of μ32κO,O′:η2κO′,N:η1κ″ and μ42κO,O′:η2κO′,N:η1κ″:η1κO‴ for HL2− with the latter being novel coordination mode. The temperature dependence of the magnetic susceptibilities of the title complex reveals that the title complex follow the Curie–Wiess paramagnetic behavior down to 5 K. The title complex exhibits strong luminescent emissions based on the f–f transitions of Sm(III) ion and 4G5/2 lifetime.
Keywords: Crystal structure; Luminescence; Magnetism; Samarium(III) orotate(-2) complex;

A novel 2D framework containing nanometer channel by significant hydrogen bonds and π–π interactions by Hong-Ping Zhou; Yong-Min Zhu; Chun-Mei Cui; Peng Wang; Hong-Wu Li; Jie-Ying Wu; Yi Xie; Min-Hua Jiang; Xu-Tang Tao; Yu-Peng Tian (351-354).
2D structure of 1 is formed by intermolecular hydrogen bond O-H⋯O and π–π interactions. The solid state fluorescent property was investigated at room temperature.A novel 2D framework containing nanometer channel, Cd(HA)2(H2O)2 (1) (H2A: 9-ethylcarbazole-3,6-dicarboxylic acid) has been prepared by hydrothermal synthesis. Single crystal X-ray analysis has revealed that the 2D framework of the title compound is formed by significant hydrogen bonds and π–π interactions. The solid state fluorescent property was investigated at room temperature.
Keywords: Hydrothermal synthesis; Crystal structure; Hydrogen bonds;

Novel gold(I) complexes, [Au(R,S-Hpyrrld)(PPh3)] · CHCl3 1 (H2pyrrld = 2-pyrrolidone-5-carboxylic acid) and [Au(R,S-othf)(PPh3)] 2 (Hothf = 5-oxo-2-tetrahydrofurancarboxylic acid), were prepared, structurally characterized, and their antimicrobial activities were tested.Novel gold(I) complexes with hard (O donor) and soft (P donor) Lewis bases, [Au(R,S-Hpyrrld)(PPh3)] · CHCl3 1 (H2pyrrld = 2-pyrrolidone-5-carboxylic acid) and [Au(R,S-othf)(PPh3)] 2 (Hothf = 5-oxo-2-tetrahydrofurancarboxylic acid), were prepared by the AgCl elimination reaction in CHCl3 between [AuCl(PPh3)] and the Ag–O bonding precursors such as [Ag2(R-Hpyrrld)(S-Hpyrrld)] and [Ag2(R-othf)(S-othf)]. Molecular structure of 1 was determined as a discrete monomer of the 2-coordinate AuOP core. In the preparation of 1 and 2, the use of the Ag–O bonding precursors is crucial. Both complexes 1 and 2 showed selective antimicrobial activities against Gram-positive bacteria and yeasts.
Keywords: Gold(I) complexes; Triphenylphosphine; 2-Pyrrolidone-5-carboxylic acid; 5-Oxo-2-tetrahydrofurancarboxylic acid; X-ray crystal structure; Antimicrobial activities;

Borane adducts of the water soluble phosphine PTA (PTA = 1,3,5-triaza-7-phosphaadamantane) by Sandra Bolaño; Alberto Albinati; Jorge Bravo; Luca Gonsalvi; Maurizio Peruzzini (360-363).
Boronation of the water soluble phosphine PTA in dry THF affords the N-boronated adduct N-B-PTABH3, which represents the first N-coordinated adduct of this popular water soluble phosphine (N-B-PTABH3  = 1-boranyl-1,3,5-triaza-7-phosphaadamantane). In situ 31P NMR spectroscopy suggests the occurrence of a stepwise boronation, resulting in the addition of as many as four equivalents of BH3 to PTA to give the polyboranyl species N x , P y -B-PTA(BH3)(x+y) (x  = 1–3, y  = 0, 1). Hydrolysis of the monoboranyl adduct occurs slowly in the presence of water yielding back PTA and boric acid; H3BO3.Boronation of the water soluble phosphine PTA (PTA = l,3,5-triaza-7-phosphaadamantane) in dry THF easily affords the N-boronated adduct N-B-PTABH3 which represents the first N-coordinated adduct of this popular water soluble phosphine (N-B-PTABH3  = 1-boranyl-1,3,5-triaza-7-phosphaadamantane). In situ 31P NMR spectroscopy suggests the occurrence of a stepwise boronation resulting in the addition of as many as four equivalents of BH3 to PTA to give the polyboranyl species N x , P y -B-PTA(BH3)(x+y) (x  = 1–3, y  = 0, 1). Hydrolysis of the monoboranyl adduct occurs slowly in the presence of water yielding back PTA and boric acid, H3BO3.
Keywords: Water soluble phosphines; Borane; Amino-borane; Phosphino-borane NMR spectroscopy;

A 3-D framework {[Cu5(BTB)4(4,4′-bipy)2(H2O)6][Cu(4,4′-bipy) (H2O)4]} n  · 8nH2O is obtained from the diffusion method. By BTB3−linking the 1-D chains, a 2-D layer [Cu2(BTB)2]2− based on [Cu2(COO)4] SBUs has been generated. The adjacent layers are further linked through [Cu(4,4′-bipy)2] linker to produce the 3-D framework containing the guest water molecules and 1-D chains [Cu(4,4′-bipy)(H2O)4] n .A 3-D novel coordination polymer {[Cu5(BTB)4(4,4′-bipy)2(H2O)6][Cu(4,4′-bipy)(H2O)4]} n  · 8nH2O (H3BTB = 1,2,3-benzene-tricarboxylic acid), containing 1-D chains [Cu(4,4′-bipy)(H2O)4] n , is obtained from the diffusion method. A negative 2-D layered structure [Cu2(BTB)2]2− along the bc-plane based on tetranuclear paddle-wheel clusters has been generated from 1-D chains along the b  −  c vector linked by BTB3−. A 3-D metal–organic framework is further constructed from the negative 2-D layer [Cu2(BTB)2]2− and long linker [Cu(4,4′-bipy)2]2+. The compound produces blue fluorescence with emission at 417 nm possibly assigned to LMCT.
Keywords: Copper(II); 1,2,3-Benzenetricarboxylic acid; Diffusion; Structure; Fluorescence;

Preparation and X-ray structure of a (catecholato)copper(II) complex with a Schönberg adduct by Beáta Tapodi; Gábor Speier; Michel Giorgi; Marius Réglier; Takuzo Funabiki; László Korecz; Antal Rockenbauer (367-370).
The reaction of metallic copper, triphenylphosphine and 1,2-naphthoquinone leads to the copper(II) catecholate complex bis(4-triphenylphosphoniono)(naphthalene-1,2-dioxolato)copper(II), the first example of a metal complex ligated by a Schönberg adduct.The reaction of metallic copper, triphenylphosphine and 1,2-naphthoquinone leads to the copper(II) catecholate complex bis(4-triphenylphosphoniono)(naphthalene-1,2-dioxolato)copper(II), the first molecular structure of a Schönberg adduct coordinated to a metal ion.
Keywords: Copper; Catecholate; Schönberg adduct;

A novel chiral framework constructed through three-fold interpenetration of (4,4) nets of Ni(II)–muconate–4,4′-bipyridine by Baiquan Chen; Feilong Jiang; Lei Han; Benlai Wu; Daqiang Yuan; Mingyan Wu; Maochun Hong (371-374).
A novel three-fold interpenetrated structure in chiral space group, P3121, has been synthesized by hydrothermal method. Crystal structural analysis reveals that both trans,trans-muconic acid and 4,4′-bipyridine act as linear bridges between square-planar nodes Ni(II), with a chiral configuration of 4,4′-bipyridine.The assembly of Ni(II) ions with linear spacers trans,trans-muconic acid (H2L) and 4,4′-bipyridine (4,4′-bpy) has afforded a compound, [Ni(L)(4,4′-bpy)(H2O)2] n (1). Single crystal X-ray diffraction analysis reveals that both 4,4′-bpy and deprotonated H2L act as linear bridges to bind square-planar Ni(II) nodes. Achiral ligands 4,4′-bpy induced in a chiral configuration link metal nodes into chiral chains, which are further bound into homochiral sheets by rigid L. Finally, a novel 3D chiral framework forms through three-fold slantwise interpenetration of those chiral (4, 4) nets. The magnetic studies in the range 2–300 K show that magnetic behavior of 1 possesses a large zero-field splitting of Ni(II) ions and an anti-ferromagnetic interaction between metal centers.
Keywords: Interpenetration framework; Magnetism; Muconate; Chirality;

A new nickelacyclic compound (η5-cyclopentadienyl)(η5-(1-(η5-cyclopentadienyl))-2-phenyl-3-ethyl-1-nickelaindenyl)nickel was synthesised in the reaction of (E)-1-lithio-1-phenyl-2-(2′-lithiophenyl)ethane with nickelocene. The compound was characterised by high resolution mass spectrometry, magnetic moment determination and X-ray single crystal analysis. It crystallises from hexane/THF mixture in the monoclinic crystal system and the P21/n space group.A new nickelacyclic compound (η5-cyclopentadienyl)(η5-(1-(η5-cyclopentadienyl))-2-phenyl-3-ethyl-1-nickelaindenyl)nickel was synthesised in the reaction of (E)-1-lithio-1-phenyl-2-(2′-lithiophenyl)ethane with nickelocene. The compound was characterised by high resolution mass spectrometry, magnetic moment determination and X-ray single crystal analysis. It crystallises from hexane/THF mixture in the monoclinic crystal system and the P21/n space group.
Keywords: Nickel; Alkali metals; Clusters; Cyclopentadienyl; Metallacyclic compounds;

The first Ln3+–iminodiacetate coordination polymer Ce2(IDA)2(C2O4)(phen)2 (phen = 1,10-phenanthroline) has the 2D-layered structure consisting of the fused 12- and 16-membered rings. The layers are further interacted with each other to form 3D framework through hydrogen bonds and π–π interactions.The first Ln3+–iminodiacetate coordination polymer Ce2(IDA)2(C2O4)(phen)2 (phen = 1,10-phenanthroline) has the 2D-layered structure consisting of the fused 12- and 16-membered rings. The layers are further interacted with each other to form 3D framework through hydrogen bonds and π–π interactions.
Keywords: Cerium; Iminodiacetate; Oxalate; Coordination polymer; Crystal structure;

First two manganese(II) trialkoxysilanethiolates have been prepared and characterized. Both contain solvent as coligand. In [Mn{SSi(OBu t )3}2(NCMe)], manganese is five-coordinate – silanethiolate ligand interacts with a metal simultaneously through sulfur and oxygen atoms and thus exhibits chelating character. Octahedral, methanol ligated complex (see figure) may serve as an example of a structure “reinforced” by a set of intramolecular and interligand O–HO hydrogen bonds.First manganese(II) trialkoxysilanethiolates have been prepared using tri-tert-butoxysilanethiol as the ligand source and their structure determined by X-ray diffraction. Acetonitrile or methanol used as reaction solvents was found to enter Mn coordination sphere. Obtained heteroleptic silanethiolate complexes represent two distinct structural types. Either O,S-chelation by tri-tert-butoxysilanethiolate ligand and simultaneous electronic assistance provided by acetonitrile in [Mn{SSi(OBu t )3}2(MeCN)] or formation of four intramolecular, interligand O–H ⋯ O hydrogen bonds in the case of [Mn{SSi(OBu t )3}2(MeOH)4] serve to stabilize the complexes.
Keywords: Manganese complexes; Silanethiolates; Crystal structure; Hydrogen bonds;

The reactions of oxidative coupling of dimethylacetylene dicarboxylate (DMA) with palladium(0) olefin complexes hearing a pyridylthioether as ancillary ligand give rise to the corresponding palladacylopentadienyl complexes as the main product and in some cases to the highly symmetric hexamethyl mellitate molecule, especially when a low alkyne (DMA)/complex ratio is employed. A palusible mechanism based on several pieces of experimental evidence is proposed, and the most effective complexes promoting the hexamethyl mellitate synthesis were identified.The reactions of oxidative coupling of dimethylacetylene dicarboxylate (DMA) with palladium (0) olefin complexes bearing a pyridylthioether as ancillary ligand give rise to the corresponding palladacyclopentadienyl complexes as the main product and in some cases to the highly symmetric hexamethyl mellitate molecule, especially when a low alkyne(DMA)/complex ratio is employed. A plausible mechanism based on several pieces of experimental evidence is proposed, and the most effective complexes promoting the hexamethyl mellitate synthesis were identified.
Keywords: Hexamethyl mellitate; Oxidative coupling; Pd(0) and Pd(II) pyridylthioether complexes; Activated alkynes;

Reaction of metallic samarium firstly with 2 equivalents of azobenzene in THF with the aid of catalytic amount of iodine and then with 1 equivalent of sodium cyclopentadienide successively afforded the title complex. It was found that two-electron reduction and hydride-addition of azobenzene cooperated in the reaction. The hydride-addition reaction happened in the absence of any hydride-reagents.Reaction of metallic samarium firstly with 2 equivalents of azobenzene in THF with the aid of catalytic amount of iodine and then with 1 equivalent of sodium cyclopentadienide successively afforded the title complex [(THF)3Na(μ-η55-C5H5)(η2-PhNHNPh)Sm]2(μ-η23-N2Ph2)2 (1). It was found that two-electron reduction and hydride-addition of azobenzene cooperated in the reaction. The hydride-addition reaction happened in the absence of any hydride-reagents. It is the first ate samarium–azobenzene complex and also the first samarium complex containing two different kinds of reduced azobenzene species.
Keywords: Metallic samarium; Azobenzene; Reduction; Crystal structure;

4,4′-Di(p-methylphenyl)-2,2′-bipyridine was conveniently synthesized from 2-bromopyridine through halogen-dance reaction and successive coupling-reactions. Its corresponding ruthenium complex was used as a good sensitizer for dye-sensitized nanocrystalline TiO2 solar cells with an overall photo-to-electric conversion efficiency of 5.5% (AM1.5, 75 mW cm−2).4,4′-Di(p-methylphenyl)-2,2′-bipyridine was conveniently synthesized from 2-bromopyridine through halogen-dance reaction, selective Kharash coupling and homo coupling of 2-bromopyridine derivative. Its corresponding ruthenium complex: cis-N,N-4,4′-di(p-methylphenyl)-2,2′-bipyridine-N,N-4,4′-dicarboxy-2,2′-bipyrine-N,N-dithiocyanato ruthenium(II) (dye-1) was also obtained and characterized by element analysis, MALDI-TOF MS and H NMR spectra. Compared with cis-N,N-2,2′-bipyridine-N,N-4,4′-dicarboxy-2,2′-bipyridine-N,N-dithiocyanato ruthenium(II), dye-1 displayed red-shifted MLCT absorptions and enhanced molar extinction coefficients for its rigid π-conjugation. As a result, dye-1 sensitized nanocrystalline TiO2 electrode gave higher short circuit photocurrent density of 12.6 mA cm−2 and overall photo-to-electric conversion efficiency of 5.5% (AM1.5, 75 mW cm−2).
Keywords: Ruthenium complex; π-Conjugated polypyridine; Solar cell; Sensitizer;

The structure of the complex is quite unusual. It consists of one-dimensional [(UO2)33-OH)32-OH) (C7H4O4N)2] ribbons along the b-axis. These ribbons are linked to form a two-dimensional layer structure by the potassium ion that serves to bridge between the two adjacent ribbons. p-Nitrobenzoic acids make the layers a three-dimensional architecture.A novel 3D uranyl complex is reported as synthesized via hydrothermal treatment of uranium oxynitrate and p-nitrobenzoic acid. The structure of the complex is quite unusual. It consists of one-dimensional [(UO2)33-OH)32-OH) (C7H4O4N)2] ribbons along the b-axis. These ribbons are linked to form a two-dimensional layer structure by the potassium ion that serves to bridge between the two adjacent ribbons. p-Nitrobenzoic acids make the layers a three-dimensional architecture. The complex is studied by DSC-TGA in order to get more information about its thermal stability.
Keywords: Simulation; Uranyl complex; Hydrothermal synthesis; Coordination polymer;

This hybrid anion is formed by the replacement of one terminal oxo group of hexamolybdate with the strong electron-donating group, p-N,N-dimethyl-phenylimido.A new monofunctionized arylimido derivative of hexamolybdate, (Bu4N)2[Mo6O18NC6H4N(CH3)2p], is synthesized by α-octamolybdate and hydrochloride salt of N,N-dimethyl-1,4-dianiline with DCC as a dehydrating agent. The derivative’s crystal data has been obtained and the IR, UV–Vis, 1H NMR spectra and cyclic voltammetry properties have also been studied.
Keywords: Polyoxometalates; Organoimido derivatives; DCC; C–H⋯O hydrogen bond; Crystal data;

Three dimensional host cage with diameter of cavity up to 1.4 nm is architected fully by chiral octahedras M(ox)3(M = Mo/Na); the guest molecule Mo(phen)3 with diameter close to 1 nm occupy the cavities with hydrogen bond interactions; the supra-molecule shows chirality in both molecule and supra-molecule levels.The structural characterization of three dimensions complex 1 {[Mo(phen)3][MoNa(ox)3]} n (phen=1,10-phenanthroline, ox = oxalate) assembled in mixed-solvo-thermal reaction condition shows that there exists nanocages, with diameter up to1.4 nm size, occupied by guest molecules Mo(phen)3 with diameter close to 1 nm, and that the complex 1 exhibits chirality in both molecule and supramolecule levels, and respond to EPR signal as well.
Keywords: Nanoporous; Cage structure; Host–guest structure; Oxalate ligand;

The reaction between [{(η5-C5Me5)RhCl(μ-Cl)}2] and (C6F5)2PCH2P(C6F5)2 in refluxing benzene yields the singly linked complex [{(η5,κP-C5Me4CH2C6F4-2-P(C6F5)CH2P(C6F5)2)}RhCl2], in which only one of the phosphorus atoms is coordinated to the rhodium.The reaction between [{(η5-C5Me5)RhCl(μ-Cl)}2] and (C6F5)2PCH2P(C6F5)2 in refluxing benzene yields the singly linked complex [{(η5,κP-C5Me 4CH2C6F4-2-P(C6F5)CH2P(C6F5)2)}RhCl2] in which only one phosphorus atom is coordinated to the rhodium.
Keywords: Cyclopentadienyl ligands; Fluorinated ligands; Phosphine ligands; C–C coupling;

Synthesis and structures of novel diastereomeric cyclopalladated ferrocenylimines derived from chiral β-amino alcohols by Ling-Zhi Du; Jun-Fang Gong; Chen Xu; Yu Zhu; Yang-Jie Wu; Mao-Ping Song (410-414).
Two pairs of novel diastereomeric cyclopalladated ferrocenylimines (S p,  S C)-3 and (R p,  S C)-4 with both planar and central chirality have been synthesized starting from inexpensive and readily available chiral β-amino alcohols. The two pairs of diastereomers were characterized by elemental analysis, IR, 1H NMR and specific rotations. Furthermore, the structures and absolute configurations of complexes (S p,  S C)-3a and (R p,  S C)-4b have been determined by single-crystal X-ray diffraction.Two pairs of novel diastereomeric cyclopalladated ferrocenylimines (S p,  S C)-3 and (R p,  S C)-4 with both planar and central chirality have been synthesized starting from inexpensive and readily available chiral β-amino alcohols. The two pairs of diastereomers were characterized by elemental analysis, IR, 1H NMR and specific rotations. Furthermore, the structures and absolute configurations of complexes (S p,  S C)-3a and (R p,  S C)-4b have been determined by single-crystal X-ray diffraction.
Keywords: Ferrocenylimines; Chiral amino alcohols; Planar chiral palladacycles; Crystal structures; Synthesis;

Structure characterization of a novel 3-D cadmium-halo coordination polymer linked by piperazine bridge by Jie-Hui Yu; Jing Lu; Xiao Zhang; Ling Ye; Qin Hou; Ji-Qing Xu (415-417).
A novel 3-D cadmium-halo coordination polymer [CdBr2(piperazine)] (1) with porous structures is constructed through a linkage of 1-D [CdBr2] chains by piperazine bridges.A simple hydrothermal reaction of 3CdSO4  · 8H2O, KBr and piperazine gives a three-dimensional (3-D) cadmium-halo coordination polymer [CdBr2(piperazine)] (1) with porous structures in the different directions, constructed through a linkage of 1-D [CdBr2] chains by piperazine bridges.
Keywords: Cadmium halide; Piperazine; Crystal structure; Fluorescence;

A first-row transition metal assisted modification of the Michaelis–Arbuzov rearrangement has been discovered that allows the reaction to take place under ambient conditions using a mild phosphine nucleophile and has been used as a novel method for the construction of a new P–C bond.A first-row transition metal assisted modification of the Michaelis–Arbuzov rearrangement has been discovered that allows the reaction to take place under ambient conditions using a mild phosphine nucleophile. This reaction has been used as a novel synthetic strategy for the assembly of P–C bonds in typically difficult to construct 3-methylpyridyl substituted phosphine and phosphonium ligands. Metal complexes of these ligands were characterized crystallographically. One of the products also contains the previously unknown pyridylFeCl 3 - species.
Keywords: X-ray diffraction; N,P ligands; Ligand design; Nucleophilic substitution;

Olefin polymerization behavior of the cyclopentadienyl cobalt complexes bearing pendant sulfur or oxygen ligands by Xiu-Feng Hou; Yin-Qiang Cheng; Peng-Cheng Zhang; Guo-Xin Jin (423-425).
Three cobalt complexes with sulfur or oxygen functionalized cyclopentadienyl ligands [η5-C5H4(CH2)2SCH2CH3]CoI2 (1), [η5-C5H4(CH2)2OCH3]Co(L)I2 (L = Py(3), PPh3(4)) have been synthesized and characterized. Complexes 1, 3 and 4 can be used as a catalyst for ethylene polymerization in the presence of MAO as co-catalyst and exhibited high activities.Four half-sandwich cobalt complexes bearing pendant sulfur or oxygen ligands have been reported and tested as catalysts for olefin polymerization in the presence of MAO. The molecular structure of complexes 1 has been determined by X-ray crystallographic analysis. Complexes 1 and 2 exhibited high activities of up to 106  g PE mol−1Co h−1 with moderate molecular weight (M w  ≈ 104  g mol−1) of polyethylene in the ethylene polymerization.
Keywords: Cobalt; Functional cyclopentadienyl group; Ethylene polymerization; Molecular structure;

Convenient syntheses of uranyl(VI) cis-dihalide complexes as anhydrous starting materials by Paul B. Duval; Shanmugaperumal Kannan; Charles L. Barnes (426-428).
The targeted syntheses of uranyl(VI) complexes UO2X2L (X = Cl, Br) possessing halide ligands exclusively at cis equatorial coordination sites are reported, supported by a neutral tridentate ligand (L), N,N,N′,N′-tetraalkylpyridine-2,6-dicarboxamide (1). A monomeric pentagonal bipyramidal geometry is observed in the solid state for the isostructural chloride (2a) and bromide (3a) derivatives as determined by X-ray crystallography.The targeted syntheses of uranyl(VI) complexes UO2X2L (X = Cl, Br) possessing halide ligands exclusively at cis equatorial coordination sites are reported, supported by a neutral tridentate ligand (L), N,N,N′,N′-tetraalkylpyridine-2,6-dicarboxamide (1). A monomeric pentagonal bipyramidal geometry is observed in the solid state for the isostructural chloride (2a) and bromide (3a) derivatives as determined by X-ray crystallography.
Keywords: Uranium; Uranyl complexes;

Lanthanide(III) nitrato complexes with the Schiff base ligand bis(pyridin-2-ylmethylene)-cyclohexane-1,2-diamine have been synthesized and characterized with X-ray crystallography. Lighter lanthanides form H-bonded dimers and heavier lanthanides form monomers.The novel lanthanide(III) complexes [Ln(NO3)3(MeOH)L] (Ln = La 1, Pr 2), and [Ln(NO3)3L] · MeOH (Ln = Sm 3, Gd 4) where L =  N,N′-bis(pyridin-2-ylmethylene)cyclohexane-1,2-diamine, have been obtained by direct reaction of the Schiff base ligand and the corresponding hydrated lanthanide(III) nitrates in methanol. All complexes were characterized spectroscopically and thermogravimetrically. Complexes 2 and 3 were also characterized with crystallographic studies. In the molecular structure of 2, Pr(III) is surrounded by all four nitrogen atoms of the Schiff base and seven oxygen atoms belonging to three bidentate chelating nitrato ligands and a coordinated methanol molecule, while in 3, Sm(III) is surrounded by all four nitrogen atoms of the Schiff base and six oxygen atoms belonging to three bidentate chelating nitrato ligands.
Keywords: Crystal structure; Lanthanide complexes; Schiff bases; Tetradentate ligands;

Preparation and structural characterisation of bis(4′-(3-pyridyl)-2,2′:6′,2″-terpyridine)ruthenium(II) hexafluorophosphate by Edwin C. Constable; Catherine E. Housecroft; Markus Neuburger; Silvia Schaffner; Frank Schaper (433-436).
The preparation of a 2,2′:6′,2″-terpyridine ligand with pendant 3-pyridyl groups is reported together with the synthesis and structural characterisation of a ruthenium(II) complex; the vectorial arrangement of the pyridyl substituent lone pairs in the complex make this a potentially useful metallotecton for metallosupramolecular chemistry.A convenient synthesis of the ligand 4′-(3-pyridyl)-2,2′:6′,2″-terpyridine (2) is presented and the preparation, spectroscopic and structural characterisation of the metallotecton [Ru(2)2]2+ are reported.
Keywords: Ruthenium(II); X-ray; 2,2′:6′,2″-Terpyridine; Synthesis;