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Inorganic Chemistry Communications (v.11, #1)

Editorial Board (pp. ifc).
Contents List (pp. iii-xi).
Editorial Board (pp. ifc).
Contents List (pp. iii-xi).

The design and synthesis of pyrazine amide ligands suitable for the “tiles” approach to molecular weaving with octahedral metal ions by David L. Cockriel; James M. McClain; Kaushal C. Patel; Robert Ullom; Travis R. Hasley; Stephen J. Archibald; Timothy J. Hubin (pp. 1-4).
A mixed oxidation state Co3+–Co2+–Co3+ complex, [Co(1)2Co(H2O)2Cl2Co(1)2]Cl2, demonstrating the potential for molecular weaving has been obtained and characterized by X-ray crystal structure determination.The pyrazine-containing ligands1 (pyrazine-2-carboxylic acid (pyridine-2-ylmethyl)-amide) and2 (pyrazine-2,5-dicarboxylic acid bis-[(pyridine-2-ylmethyl)-amide]) have been synthesized and characterized in order to probe their ability to form polynuclear transition metal complexes. A mixed oxidation state Co3+–Co2+–Co3+ complex with deprotonated ligand1, [Co(1)2Co(H2O)2Cl2Co(1)2]Cl2, has been obtained and characterized by X-ray crystal structure determination. The central octahedral cobalt(II) ion in the complex is coordinated by one pyrazine nitrogen from each of the surrounding octahedral cobalt(III), ions which are meridianally coordinated by two of the ligands1. Key aspects of both ligands are their rigid meridianal coordination, coupled with the pyrazine core, which demands coordination of metal ions on opposite sides of the ligand strand.

Keywords: Cobalt; Molecular weaving; Amide; Pyrazine


The design and synthesis of pyrazine amide ligands suitable for the “tiles” approach to molecular weaving with octahedral metal ions by David L. Cockriel; James M. McClain; Kaushal C. Patel; Robert Ullom; Travis R. Hasley; Stephen J. Archibald; Timothy J. Hubin (pp. 1-4).
A mixed oxidation state Co3+–Co2+–Co3+ complex, [Co(1)2Co(H2O)2Cl2Co(1)2]Cl2, demonstrating the potential for molecular weaving has been obtained and characterized by X-ray crystal structure determination.The pyrazine-containing ligands1 (pyrazine-2-carboxylic acid (pyridine-2-ylmethyl)-amide) and2 (pyrazine-2,5-dicarboxylic acid bis-[(pyridine-2-ylmethyl)-amide]) have been synthesized and characterized in order to probe their ability to form polynuclear transition metal complexes. A mixed oxidation state Co3+–Co2+–Co3+ complex with deprotonated ligand1, [Co(1)2Co(H2O)2Cl2Co(1)2]Cl2, has been obtained and characterized by X-ray crystal structure determination. The central octahedral cobalt(II) ion in the complex is coordinated by one pyrazine nitrogen from each of the surrounding octahedral cobalt(III), ions which are meridianally coordinated by two of the ligands1. Key aspects of both ligands are their rigid meridianal coordination, coupled with the pyrazine core, which demands coordination of metal ions on opposite sides of the ligand strand.

Keywords: Cobalt; Molecular weaving; Amide; Pyrazine


Synthesis, spectroscopic and X-ray characterization of new molecular organotitanium(IV) phosphonate by Andrej Pevec; Alojz Demšar; Jiri Pinkas; Marek Necas (pp. 5-7).
A dinuclear cage cluster has been synthesized in which two titanium atoms are bridged by two bidentate monoanionic and by two bidentate dianionic phosphonate groups. The OH group of the monoanionic phosphonate and oxygen atom of the dianionic phosphonate are connected by strong intramolecular hydrogen bond. The NMR spectroscopy reveals the fast proton migration within the hydrogen bond.Dititanate [{Ti(C5Me4Et)(μ-O2P(OH)Me)(μ-O2P(O)Me)}2] (1) was prepared from (C5Me4Et)TiF3 and MeP(O)(OSiMe3)2. The molecular structure of compound1 has been determined by single-crystal X-ray diffraction analysis. In the cage cluster, two titanium atoms are bridged by two bidentate monoanionic and by two bidentate dianionic phosphonate groups. The OH group of the monoanionic phosphonate and oxygen atom of the dianionic phosphonate are connected by strong intramolecular hydrogen bond. The NMR spectroscopy reveals the fast proton migration within the hydrogen bond.

Keywords: Titanium; Phosphonate; Crystal structure; Hydrogen bond


Synthesis, spectroscopic and X-ray characterization of new molecular organotitanium(IV) phosphonate by Andrej Pevec; Alojz Demšar; Jiri Pinkas; Marek Necas (pp. 5-7).
A dinuclear cage cluster has been synthesized in which two titanium atoms are bridged by two bidentate monoanionic and by two bidentate dianionic phosphonate groups. The OH group of the monoanionic phosphonate and oxygen atom of the dianionic phosphonate are connected by strong intramolecular hydrogen bond. The NMR spectroscopy reveals the fast proton migration within the hydrogen bond.Dititanate [{Ti(C5Me4Et)(μ-O2P(OH)Me)(μ-O2P(O)Me)}2] (1) was prepared from (C5Me4Et)TiF3 and MeP(O)(OSiMe3)2. The molecular structure of compound1 has been determined by single-crystal X-ray diffraction analysis. In the cage cluster, two titanium atoms are bridged by two bidentate monoanionic and by two bidentate dianionic phosphonate groups. The OH group of the monoanionic phosphonate and oxygen atom of the dianionic phosphonate are connected by strong intramolecular hydrogen bond. The NMR spectroscopy reveals the fast proton migration within the hydrogen bond.

Keywords: Titanium; Phosphonate; Crystal structure; Hydrogen bond


CS2 elimination and C–S bond cleavage in [Zn(dmpzdtc)2] – Leading to formation of a cyclic octanuclear complex [Zn4(μ-dmpz)5(μ-OH)(μ3-S)(py)]2·py(dmpzdtc=3,5-dimethylpyrazole-1-dithiocarboxylate, dmpz=3,5-dimethylpyrazolate) by Hua-Zhou Wu; Hong-Xi Li; Mei-Ling Cheng; Wen-Hua Zhang; Yong Zhang; Jian-Ping Lang (pp. 8-10).
One cyclic octanuclear Zn(II) sulfide complex, [Zn4(μ-dmpz)5(μ-OH)(μ3-S)(py)]2·py was isolated from CS2 elimination and C–S bond cleavage reactions of [Zn(dmpzdtc)2] in MeCN and pyridine. This complex was structurally characterized by elemental analysis, IR, and X-ray crystallography and their luminescent properties were studied.Complex [Zn(dmpzdtc)2] (1) (dmpzdtc=3,5-dimethylpyrazole-1-dithiocarboxylate) in MeCN and pyridine underwent unique CS2 elimination and C–S bond cleavage reactions to afford a novel cyclic octanuclear zinc sulfide complex [Zn4(μ-dmpz)5(μ-OH) (μ3-S)(py)]2·py (2·py) dmpz=3,5-dimethylpyrazolate). Single-crystal X-ray diffraction revealed that2 consists of two [Zn4(μ-dmpz)3(μ-OH)(μ3-S)(py)] fragments linked by two pairs of μ-dmpz ligands, forming an unique metallocyclic structure. The luminescent property of this complex in solid state was also investigated.

Keywords: Zinc; 3,5-Dimethylpyrazolate; 3,5-Dimethylpyrazole-1-dithiocarboxylate; CS; 2; elimination; C–S bond cleavage


CS2 elimination and C–S bond cleavage in [Zn(dmpzdtc)2] – Leading to formation of a cyclic octanuclear complex [Zn4(μ-dmpz)5(μ-OH)(μ3-S)(py)]2·py(dmpzdtc=3,5-dimethylpyrazole-1-dithiocarboxylate, dmpz=3,5-dimethylpyrazolate) by Hua-Zhou Wu; Hong-Xi Li; Mei-Ling Cheng; Wen-Hua Zhang; Yong Zhang; Jian-Ping Lang (pp. 8-10).
One cyclic octanuclear Zn(II) sulfide complex, [Zn4(μ-dmpz)5(μ-OH)(μ3-S)(py)]2·py was isolated from CS2 elimination and C–S bond cleavage reactions of [Zn(dmpzdtc)2] in MeCN and pyridine. This complex was structurally characterized by elemental analysis, IR, and X-ray crystallography and their luminescent properties were studied.Complex [Zn(dmpzdtc)2] (1) (dmpzdtc=3,5-dimethylpyrazole-1-dithiocarboxylate) in MeCN and pyridine underwent unique CS2 elimination and C–S bond cleavage reactions to afford a novel cyclic octanuclear zinc sulfide complex [Zn4(μ-dmpz)5(μ-OH) (μ3-S)(py)]2·py (2·py) dmpz=3,5-dimethylpyrazolate). Single-crystal X-ray diffraction revealed that2 consists of two [Zn4(μ-dmpz)3(μ-OH)(μ3-S)(py)] fragments linked by two pairs of μ-dmpz ligands, forming an unique metallocyclic structure. The luminescent property of this complex in solid state was also investigated.

Keywords: Zinc; 3,5-Dimethylpyrazolate; 3,5-Dimethylpyrazole-1-dithiocarboxylate; CS; 2; elimination; C–S bond cleavage


Cyclopentanone thiosemicarbazone (Hcptsc) induces a new bonding pattern in (Ph3P)Cu(μ-Br)(μ3-S,N–Hcptsc)CuBr(PPh3) dimer by Tarlok S. Lobana; Poonam Kumari; Ray J. Butcher (pp. 11-14).
Cyclopentanone thiosemicarbazone (Hcptsc) with copper(I) bromide has formed an asymmetric dimer (Ph3P)Cu(μ-Br) (μ3-S,N–Hcptsc)CuBr(PPh3) (1) with a new {Cu(μ-Br)(μ3-S,N)Cu} bonding core.Reaction of cyclopentanone thiosemicarbazone (Hcptsc) with copper(I) bromide and Ph3P in 1:1:1 molar ratio in acetonitrile has formed an asymmetric dimer, [(Ph3P)Cu(μ-Br)(μ3-S,N–Hcptsc)CuBr(PPh3)] (1), with a new {Cu(μ-Br)(μ3-S,N)Cu} bonding core in metal-thiosemicarbazone chemistry.

Keywords: Cyclopentanone thiosemicarbazone; Copper; Triphenyl phosphine; Asymmetric dimer; Bridging mode


Cyclopentanone thiosemicarbazone (Hcptsc) induces a new bonding pattern in (Ph3P)Cu(μ-Br)(μ3-S,N–Hcptsc)CuBr(PPh3) dimer by Tarlok S. Lobana; Poonam Kumari; Ray J. Butcher (pp. 11-14).
Cyclopentanone thiosemicarbazone (Hcptsc) with copper(I) bromide has formed an asymmetric dimer (Ph3P)Cu(μ-Br) (μ3-S,N–Hcptsc)CuBr(PPh3) (1) with a new {Cu(μ-Br)(μ3-S,N)Cu} bonding core.Reaction of cyclopentanone thiosemicarbazone (Hcptsc) with copper(I) bromide and Ph3P in 1:1:1 molar ratio in acetonitrile has formed an asymmetric dimer, [(Ph3P)Cu(μ-Br)(μ3-S,N–Hcptsc)CuBr(PPh3)] (1), with a new {Cu(μ-Br)(μ3-S,N)Cu} bonding core in metal-thiosemicarbazone chemistry.

Keywords: Cyclopentanone thiosemicarbazone; Copper; Triphenyl phosphine; Asymmetric dimer; Bridging mode


The conversion of 1,1′-dibromoferrocene to 1,2-dibromoferrocene: The ferrocene-chemist’s dream reaction by Ian R. Butler (pp. 15-19).
The conversion of 1,1′-dibromoferrocene to a range of 2-substituted bromoferrocenes is described. The products are useful in the preparation of a wide number of 1,2-disubstituted ferrocenes.The conversion of 1,1′-dibromoferrocene to a range of 2-substituted bromoferrocenes is described. The products are useful in the preparation of a wide number of 1,2-disubstituted ferrocenes. This includes the preparation of 1,2-dibromoferrocene and 2-(diisopropylphosphino)bromoferrocene in what is a clean and simple synthesis. The synthesis may be carried out on a large scale and for the first time produces multigram quantities of these important precursor compounds. In addition the synthetic procedure may be modified to produce a new family of ferrocene-based tris-phosphine ligands such as bis(2-diphenylphosphinoferrocenyl)phenylphosphine.

Keywords: Ferrocene; Lithiation; Bromoferrocene; Phosphine cycopentadienyl; Iron


The conversion of 1,1′-dibromoferrocene to 1,2-dibromoferrocene: The ferrocene-chemist’s dream reaction by Ian R. Butler (pp. 15-19).
The conversion of 1,1′-dibromoferrocene to a range of 2-substituted bromoferrocenes is described. The products are useful in the preparation of a wide number of 1,2-disubstituted ferrocenes.The conversion of 1,1′-dibromoferrocene to a range of 2-substituted bromoferrocenes is described. The products are useful in the preparation of a wide number of 1,2-disubstituted ferrocenes. This includes the preparation of 1,2-dibromoferrocene and 2-(diisopropylphosphino)bromoferrocene in what is a clean and simple synthesis. The synthesis may be carried out on a large scale and for the first time produces multigram quantities of these important precursor compounds. In addition the synthetic procedure may be modified to produce a new family of ferrocene-based tris-phosphine ligands such as bis(2-diphenylphosphinoferrocenyl)phenylphosphine.

Keywords: Ferrocene; Lithiation; Bromoferrocene; Phosphine cycopentadienyl; Iron


Performance of modified montmorillonite clay in mercury adsorption process and thermodynamic studies by Denis L. Guerra; Claudio Airoldi; Rúbia Ribeiro Viana (pp. 20-23).
The present investigation is to study the performance of montmorillonite, obtained from amazon region, in form natural and modified. The chemical modification process was developed with intercalation of pyridine (P) and (APS) 3-aminopropyltriethoxysilane. After intercalation process, the resulting and original material were used for mercury cation adsorption from aqueous solution. The mercury adsorption process were investigated at pH 6.0 and temperature at 298±1K.The montmorillonite clay sample from amazon region, Pará State, Brazil, was used for intercalation process with pyridine (P) and organofunctionalization with 3-aminopropyltriethoxysilane (APS). The montmorillonite-P/APS shows variation of d001 values, by changing d001 from 1.15 to 2.10nm. The original and modified samples were used for mercury cation adsorption from aqueous solution at room temperature and pH 6.0. The energetic effect caused by mercury cation adsorption was determined though calorimetric titration at the solid–liquid interface and gave a net thermal effect that enabled the calculation of the exothermic values and the equilibrium constant.

Keywords: Montmorillonite; Adsorption isotherms; Mercury; Calorimetry


RETRACTED: Performance of modified montmorillonite clay in mercury adsorption process and thermodynamic studies by Denis L. Guerra; Claudio Airoldi; R bia Ribeiro Viana (pp. 20-23).
This article has been retracted: please see Elsevier Policy on Article Withdrawal (http://www.elsevier.com/locate/withdrawalpolicy).This article has been retracted at the request of the Editors because of concerns about the validity of results reported in this article and other publications in Elsevier journals by the same authors, namely: J. Colloid Interface Sci., 337 (2009) 122130, doi:10.1016/j.jcis.2009.05.013. Inorg. Chem. Commun., 12 (2009) 11451149, doi:10.1016/j.inoche.2009.08.029. J. Environ. Radioact., 101 (2010) 122133, doi:10.1016/j.jenvrad.2009.09.005. Process Safety Environ. Prot., 88 (2010) 5361, doi:10.1016/j.psep.2009.10.002. J. Phys. Chem. Solids, 70 (2009) 14131421, doi:10.1016/j.jpcs.2009.08.012. Appl. Surf. Sci., 256 (2009) 702709, doi:10.1016/j.apsusc.2009.08.045. Inorg. Chem. Commun., 11 (2008) 2023, doi:10.1016/j.inoche.2007.09.029. Inorg. Chem. Commun., 12 (2009) 11071111, doi:10.1016/j.inoche.2009.08.033. J. Hazard. Mat., 172 (2009) 507514, doi:10.1016/j.jhazmat.2009.07.016. J. Hazard. Mat., 171 (2009) 514523, doi:10.1016/j.jhazmat.2009.06.032. J. Colloid Interface Sci., 338 (2009) 3039, doi:10.1016/j.jcis.2009.06.004.Publication of an article in a peer-reviewed journal is an important building-block in the development of science. Elsevier has defined policies and ethical guidelines and takes its duties of guardianship over the scholarly record extremely seriously.The Editors of the Elsevier journals involved found that the allegations of fraud are conclusive and they have decided that these papers should be retracted from the journals.

A novel sandwich polyoxotungstogermanate: Synthesis, crystal structure and magnetic property of [Pr(GeW11O39)2]13− by Ning Jiang; Lin Xu; Fengyan Li; Guanggang Gao; Lihua Fan (pp. 24-27).
A new sandwich-type lanthanide polyoxometalate K11.5H1.5[Pr(GeW11O39)2]·29H2O (1), which is assembled by the lancunary Keggin-type polyanion [GeW11O39]8− and trivalent lanthanide cation, and PrIII cation sandwiched between two [GeW11O39]8− anions is of eight coordination and occupies square anti-prismatic geometry.A novel sandwich-type polyoxometalate built on the lancunary Keggin-type polyanion [GeW11O39]8− and trivalent rare earth ion, K11.5H1.5[Pr(GeW11O39)2]·29H2O (1) has been synthesized and characterized by IR spectroscopy, UV electronic spectroscopy, luminescence spectroscopy, cyclic voltammetry and single crystal X-ray diffraction. This is the first report of crystal structure for the sandwich Keggin-type polyoxotungstogermanate containing lanthanide. In compound1, PrIII cation sandwiched between two [GeW11O39]8− anions is of eight coordination and occupies square anti-prismatic geometry. The magnetic investigation of compound1 demonstrate the presence of an antiferromagnetic interaction in1.

Keywords: Polyoxometalate; Lanthanide; Sandwich-type; Magnetic property


A novel sandwich polyoxotungstogermanate: Synthesis, crystal structure and magnetic property of [Pr(GeW11O39)2]13− by Ning Jiang; Lin Xu; Fengyan Li; Guanggang Gao; Lihua Fan (pp. 24-27).
A new sandwich-type lanthanide polyoxometalate K11.5H1.5[Pr(GeW11O39)2]·29H2O (1), which is assembled by the lancunary Keggin-type polyanion [GeW11O39]8− and trivalent lanthanide cation, and PrIII cation sandwiched between two [GeW11O39]8− anions is of eight coordination and occupies square anti-prismatic geometry.A novel sandwich-type polyoxometalate built on the lancunary Keggin-type polyanion [GeW11O39]8− and trivalent rare earth ion, K11.5H1.5[Pr(GeW11O39)2]·29H2O (1) has been synthesized and characterized by IR spectroscopy, UV electronic spectroscopy, luminescence spectroscopy, cyclic voltammetry and single crystal X-ray diffraction. This is the first report of crystal structure for the sandwich Keggin-type polyoxotungstogermanate containing lanthanide. In compound1, PrIII cation sandwiched between two [GeW11O39]8− anions is of eight coordination and occupies square anti-prismatic geometry. The magnetic investigation of compound1 demonstrate the presence of an antiferromagnetic interaction in1.

Keywords: Polyoxometalate; Lanthanide; Sandwich-type; Magnetic property


Assembly of a novel Ag(I) supramolecular architecture constructed from flexible ligand containing asymmetrical tricarboxylate by Qing-Ran Wu; Xiao-Li Chen; Huai-Ming Hu; Ting Qin; Feng Fu; Bo Zhang; Xing-Long Wu; Meng-Lin Yang; Gang-Lin Xue; Li-Feng Xu (pp. 28-32).
[Ag(H2cpop)(bpy)] n (1) was hydrothermal synthesized and characterized. H3cpop comes from the in situ decarboxylation of H4odp in the hydrothermal reactions. Compound1 shows 1D chain bearing hooks with carboxyl groups. The two chains are recognized each other to form zipper structure by hydrogen bonding interaction between the bearing carboxyl groups. The double chain structure is further interconnected by supramolecular interactions resulted a 3D supramolecular architecture.A novel Ag(I) compound [Ag(H2cpop)(bpy)] n (1) (H3cpop=4-(4-carboxyphenoxy) phthalic acid, bpy=4,4′-bipyridine), has been hydrothermally synthesized and structurally characterized. H3cpop came from the in situ decarboxylation of H4odp (H4odp=4,4′-oxydiphthalic acid) in the hydrothermal reactions. Compound1 was obtained from the self-assembly of Ag(I) salt with bpy and H4odp ligands to form a 1D chain bearing hooks with carboxyl groups. The two chains are recognized each other to generate molecular zipper structure by hydrogen bonding interaction between the bearing carboxyl groups. Compound1 is stable in air, and show intense photoluminescence at room temperature.

Keywords: Supramolecular architecture; Crystal structure; Luminescence


Assembly of a novel Ag(I) supramolecular architecture constructed from flexible ligand containing asymmetrical tricarboxylate by Qing-Ran Wu; Xiao-Li Chen; Huai-Ming Hu; Ting Qin; Feng Fu; Bo Zhang; Xing-Long Wu; Meng-Lin Yang; Gang-Lin Xue; Li-Feng Xu (pp. 28-32).
[Ag(H2cpop)(bpy)] n (1) was hydrothermal synthesized and characterized. H3cpop comes from the in situ decarboxylation of H4odp in the hydrothermal reactions. Compound1 shows 1D chain bearing hooks with carboxyl groups. The two chains are recognized each other to form zipper structure by hydrogen bonding interaction between the bearing carboxyl groups. The double chain structure is further interconnected by supramolecular interactions resulted a 3D supramolecular architecture.A novel Ag(I) compound [Ag(H2cpop)(bpy)] n (1) (H3cpop=4-(4-carboxyphenoxy) phthalic acid, bpy=4,4′-bipyridine), has been hydrothermally synthesized and structurally characterized. H3cpop came from the in situ decarboxylation of H4odp (H4odp=4,4′-oxydiphthalic acid) in the hydrothermal reactions. Compound1 was obtained from the self-assembly of Ag(I) salt with bpy and H4odp ligands to form a 1D chain bearing hooks with carboxyl groups. The two chains are recognized each other to generate molecular zipper structure by hydrogen bonding interaction between the bearing carboxyl groups. Compound1 is stable in air, and show intense photoluminescence at room temperature.

Keywords: Supramolecular architecture; Crystal structure; Luminescence


Synthesis and crystal structure of the first oxofree ‘3+3’ rhenium(V) complex by Irvin Booysen; Thomas I.A. Gerber; Eric Hosten; Peter Mayer (pp. 33-35).
A novel oxofree ‘3+3’ rhenium(V) complex salt, [Re(L3)2](ReO4) (1) (H2L3= N-(2-aminobenzylidene)benzene-1,2-diamine), was prepared from trans-{ReO2(py)4]Cl and H2L3 in acetonitrile. The molecular structure of1 was assigned by elemental analysis, IR,1H NMR and X-ray crystallography. Its synthesis is the first example of the substitution of two oxo groups from a rhenium(V) center to yield an oxofree rhenium(V) complex.A new oxofree rhenium(V) complex salt, [Re(L3)2](ReO4)(H2L3= N-(2-aminobenzylidene)benzene-1,2-diamine), has been synthesized and characterized by single crystal X-ray structure determination, IR and NMR spectroscopy. The chelates L3 are coordinated as dianionic tridentate N, N, N-donor diamidoimines. The rhenium(V) ion is centered in a distorted trigonal prism.

Keywords: Rhenium(V); Oxofree; X-ray crystallography; IR; NMR


Synthesis and crystal structure of the first oxofree ‘3+3’ rhenium(V) complex by Irvin Booysen; Thomas I.A. Gerber; Eric Hosten; Peter Mayer (pp. 33-35).
A novel oxofree ‘3+3’ rhenium(V) complex salt, [Re(L3)2](ReO4) (1) (H2L3= N-(2-aminobenzylidene)benzene-1,2-diamine), was prepared from trans-{ReO2(py)4]Cl and H2L3 in acetonitrile. The molecular structure of1 was assigned by elemental analysis, IR,1H NMR and X-ray crystallography. Its synthesis is the first example of the substitution of two oxo groups from a rhenium(V) center to yield an oxofree rhenium(V) complex.A new oxofree rhenium(V) complex salt, [Re(L3)2](ReO4)(H2L3= N-(2-aminobenzylidene)benzene-1,2-diamine), has been synthesized and characterized by single crystal X-ray structure determination, IR and NMR spectroscopy. The chelates L3 are coordinated as dianionic tridentate N, N, N-donor diamidoimines. The rhenium(V) ion is centered in a distorted trigonal prism.

Keywords: Rhenium(V); Oxofree; X-ray crystallography; IR; NMR


Telluroxanthone: A new type of triplet emitter by Horst Kunkely; Arnd Vogler (pp. 36-38).
Telluroxanthone shows a r.t. phosphorescence at λmax=510nm. The emitting state is of the CT type involving Te as donor and the carbonyl substituent as acceptor. An analogy between the emitting CT triplet of telluroxanthone and emitting MLCT triplets of transition metals complexes is emphasized.Telluroxanthone shows a r.t. phosphorescence at λmax=510nm. The emitting state is of the CT type involving Te as donor and the carbonyl substituent as acceptor. An analogy between the emitting CT triplet of telluroxanthone and emitting MLCT triplets of transition metals complexes is emphasized.

Keywords: Electronic spectra; Phosphorescence; Tellurium


Telluroxanthone: A new type of triplet emitter by Horst Kunkely; Arnd Vogler (pp. 36-38).
Telluroxanthone shows a r.t. phosphorescence at λmax=510nm. The emitting state is of the CT type involving Te as donor and the carbonyl substituent as acceptor. An analogy between the emitting CT triplet of telluroxanthone and emitting MLCT triplets of transition metals complexes is emphasized.Telluroxanthone shows a r.t. phosphorescence at λmax=510nm. The emitting state is of the CT type involving Te as donor and the carbonyl substituent as acceptor. An analogy between the emitting CT triplet of telluroxanthone and emitting MLCT triplets of transition metals complexes is emphasized.

Keywords: Electronic spectra; Phosphorescence; Tellurium


Synthesis and crystal structures of manganese(II) complexes with the ligands from in situ oxidation of 2-mercaptonanicotinic acid by Hong-Ping Xiao; Bao-Lin Liu; Xiao-Qiang Liang; Jing-Lin Zuo; Xiao-Zeng You (pp. 39-43).
The reactions of manganese(II) chloride tetrahydrate with 2-mercaptonanicotinic acid in the presence of nitrogen donor ligands are described in . By in situ oxidation of 2-mercaptonanicotinic acid (L1) with the existence of different co-ligands, the unexpected oxidative formation of the disulfide bond and S–O bond are observed. Three manganese(II) coordination polymers have been prepared and structurally characterized.Three manganese(II) complexes, [Mn(L2)(phen)(H2O)] n· nH2O (1), [Mn(L2)(2,2′-bipy)(H2O)] n·2 nH2O (2) and [Mn(4,4′-bipy)2(H2O)2] n·2 nL3 (3) (phen=1,10-phenanthroline, 2,2′-bipy=2,2′-bipyridine, 4,4′-bipy=4,4′-bipyridine, L2=2-sulfonato-nicotinate and L3=2-(3-carboxy-pyridine-2-yl disulfanyl)-nicotinic acid anion), have been prepared from in situ metal/ligand solution reactions. By in situ oxidation of 2-mercaptonanicotinic acid (L1) with the existence of different co-ligands, the unexpected oxidative formation of the disulfide bond and S–O bond are observed.

Keywords: Crystal structures; Manganese(II) complexes; 2-Mercaptonanicotinic acid; 2-Sulfonato-nicotinate; In situ metal/ligand reaction


Synthesis and crystal structures of manganese(II) complexes with the ligands from in situ oxidation of 2-mercaptonanicotinic acid by Hong-Ping Xiao; Bao-Lin Liu; Xiao-Qiang Liang; Jing-Lin Zuo; Xiao-Zeng You (pp. 39-43).
The reactions of manganese(II) chloride tetrahydrate with 2-mercaptonanicotinic acid in the presence of nitrogen donor ligands are described in . By in situ oxidation of 2-mercaptonanicotinic acid (L1) with the existence of different co-ligands, the unexpected oxidative formation of the disulfide bond and S–O bond are observed. Three manganese(II) coordination polymers have been prepared and structurally characterized.Three manganese(II) complexes, [Mn(L2)(phen)(H2O)] n· nH2O (1), [Mn(L2)(2,2′-bipy)(H2O)] n·2 nH2O (2) and [Mn(4,4′-bipy)2(H2O)2] n·2 nL3 (3) (phen=1,10-phenanthroline, 2,2′-bipy=2,2′-bipyridine, 4,4′-bipy=4,4′-bipyridine, L2=2-sulfonato-nicotinate and L3=2-(3-carboxy-pyridine-2-yl disulfanyl)-nicotinic acid anion), have been prepared from in situ metal/ligand solution reactions. By in situ oxidation of 2-mercaptonanicotinic acid (L1) with the existence of different co-ligands, the unexpected oxidative formation of the disulfide bond and S–O bond are observed.

Keywords: Crystal structures; Manganese(II) complexes; 2-Mercaptonanicotinic acid; 2-Sulfonato-nicotinate; In situ metal/ligand reaction


Microwave-assisted synthesis of [Os2Cl3(PEt2Ph)6]Cl, featuring the first reported X-ray crystal structure by Bennett J. Tardiff; Andreas Decken; G. Sean McGrady (pp. 44-46).
The complex [Os2Cl3(PEt2Ph)6]Cl has been synthesized in a facile manner using a microwave reactor; its single crystal X-ray structure and a full characterization by NMR spectroscopy are reported for the first time.The microwave-assisted synthesis of [Os2Cl3(PEt2Ph)6]Cl, a useful intermediate in osmium chemistry, was performed in a minimum amount of time under aerobic conditions, and the product readily crystallized from the reaction solution. Its single crystal X-ray structure and a full characterization by NMR spectroscopy are reported for the first time.

Keywords: Osmium; Phosphine; Microwave synthesis; X-ray structure


Microwave-assisted synthesis of [Os2Cl3(PEt2Ph)6]Cl, featuring the first reported X-ray crystal structure by Bennett J. Tardiff; Andreas Decken; G. Sean McGrady (pp. 44-46).
The complex [Os2Cl3(PEt2Ph)6]Cl has been synthesized in a facile manner using a microwave reactor; its single crystal X-ray structure and a full characterization by NMR spectroscopy are reported for the first time.The microwave-assisted synthesis of [Os2Cl3(PEt2Ph)6]Cl, a useful intermediate in osmium chemistry, was performed in a minimum amount of time under aerobic conditions, and the product readily crystallized from the reaction solution. Its single crystal X-ray structure and a full characterization by NMR spectroscopy are reported for the first time.

Keywords: Osmium; Phosphine; Microwave synthesis; X-ray structure


Synthesis, structure and cytotoxic activity evaluation of a dinuclear complex of Cd(II) with N′, N2-bis[(1 E)-1-(2-pyridyl)ethylidene]propanedihydrazide by Nenad R. Filipović; Alessia Bacchi; Milan Lazić; Giancarlo Pelizzi; Siniša Radulović; Dušan M. Sladić; Tamara R. Todorović; Katarina K. Anđelković (pp. 47-50).
A new dinuclear complex of Cd(II) with N′, N2-bis[(1 E)-1-(2-pyridyl)ethylidene]propanedihydrazide (H2L) was synthesized and its crystal structure determined. In the complex dinuclear cation [Cd2(H2O)2(H2L)2]4+, each cadmium atom is heptacoordinated by two tridentate H2L ligands and one water molecule. The complex showed a pronounced cytotoxic activity to murine melanoma B16 cells and human cervical cancer HeLa cells.A new dinuclear complex of Cd(II) with N,N2-bis[(1 E) -1-(2-pyridyl)ethylidene]propanedihydrazide (H2L) was synthesized and its crystal structure determined. The basic structural unit of the complex is the binuclear [Cd2(H2O)2(H2L)2]4+ cation, where each cadmium atom is heptacoordinated by two tridentate H2L ligands, by means of the NNO chelating system, and one water molecule. A 12-membered macrocycle is defined at the core of the binuclear cation. The complex showed a pronounced cytotoxic activity to murine melanoma B16 cells and human cervical cancer HeLa cells.

Keywords: Cd(II) complex; Hydrazone ligand; X-ray analysis; Cytotoxic activity


Synthesis, structure and cytotoxic activity evaluation of a dinuclear complex of Cd(II) with N′, N2-bis[(1 E)-1-(2-pyridyl)ethylidene]propanedihydrazide by Nenad R. Filipović; Alessia Bacchi; Milan Lazić; Giancarlo Pelizzi; Siniša Radulović; Dušan M. Sladić; Tamara R. Todorović; Katarina K. Anđelković (pp. 47-50).
A new dinuclear complex of Cd(II) with N′, N2-bis[(1 E)-1-(2-pyridyl)ethylidene]propanedihydrazide (H2L) was synthesized and its crystal structure determined. In the complex dinuclear cation [Cd2(H2O)2(H2L)2]4+, each cadmium atom is heptacoordinated by two tridentate H2L ligands and one water molecule. The complex showed a pronounced cytotoxic activity to murine melanoma B16 cells and human cervical cancer HeLa cells.A new dinuclear complex of Cd(II) with N,N2-bis[(1 E) -1-(2-pyridyl)ethylidene]propanedihydrazide (H2L) was synthesized and its crystal structure determined. The basic structural unit of the complex is the binuclear [Cd2(H2O)2(H2L)2]4+ cation, where each cadmium atom is heptacoordinated by two tridentate H2L ligands, by means of the NNO chelating system, and one water molecule. A 12-membered macrocycle is defined at the core of the binuclear cation. The complex showed a pronounced cytotoxic activity to murine melanoma B16 cells and human cervical cancer HeLa cells.

Keywords: Cd(II) complex; Hydrazone ligand; X-ray analysis; Cytotoxic activity


Ruthenium and rhodium complexes anchored to europium oxide nanoparticles by Joan Marie D. Zapiter; Brian M. Tissue; Karen J. Brewer (pp. 51-56).
Modification of Eu2O3 nanoparticles with [Ru(deeb)2Cl2] and [Rh(deeb)2Cl2]PF6 leads to a new class of materials of interest in studying energy transfer between nanoparticles and surface-attached complexes.We report the synthesis of ruthenium and rhodium polypyridyl complexes with ester substituents and the attachment of these complexes onto europium oxide nanoparticles through the surface-anchoring deeb ligand (deeb=diethyl-2,2′-bipyridine-4,4′-dicarboxylate). Characterization by1H NMR, electronic absorption and IR spectroscopies, and mass spectrometry showed structural and photochemical properties consistent with deeb complexes. Solid luminescence spectra of Eu2O3 nanoparticles modified with [Rh(deeb)2Cl2](PF6) at 77K show the characteristic emission of Eu2O3 which will be used in the future to study interfacial energy dynamics.

Keywords: Lanthanide oxides; Deeb ligand; Transition metal complexes; Eu; 3+; luminescence; Energy transfer; Inert-gas condensation


Ruthenium and rhodium complexes anchored to europium oxide nanoparticles by Joan Marie D. Zapiter; Brian M. Tissue; Karen J. Brewer (pp. 51-56).
Modification of Eu2O3 nanoparticles with [Ru(deeb)2Cl2] and [Rh(deeb)2Cl2]PF6 leads to a new class of materials of interest in studying energy transfer between nanoparticles and surface-attached complexes.We report the synthesis of ruthenium and rhodium polypyridyl complexes with ester substituents and the attachment of these complexes onto europium oxide nanoparticles through the surface-anchoring deeb ligand (deeb=diethyl-2,2′-bipyridine-4,4′-dicarboxylate). Characterization by1H NMR, electronic absorption and IR spectroscopies, and mass spectrometry showed structural and photochemical properties consistent with deeb complexes. Solid luminescence spectra of Eu2O3 nanoparticles modified with [Rh(deeb)2Cl2](PF6) at 77K show the characteristic emission of Eu2O3 which will be used in the future to study interfacial energy dynamics.

Keywords: Lanthanide oxides; Deeb ligand; Transition metal complexes; Eu; 3+; luminescence; Energy transfer; Inert-gas condensation


Polynuclear paddle-wheel copper(II) propionate with di-2-pyridylamine or 1,10-phenanthroline: Preparation, characterization and X-ray structure by Sujittra Youngme; Achareeya Cheansirisomboon; Chanaiporn Danvirutai; Chaveng Pakawatchai; Narongsak Chaichit (pp. 57-62).
The synthesis, spectroscopic, magnetic and structural characterization of two new polynuclear copper(II) propionate are described. Both compounds exhibit the typical paddle-wheel type structure. The complex [Cu4(dpyam)2(OCOC2H5)2(μ-O2CC2H5)6(H2O)2][Cu2(μ-O2CC2H5)4(H2O)2]·(DMF)21, where dpyam=di-2-pyridylamine, the “outer” Cu ions, with a CuN2O2O′ chromophore, have an intermediate five-coordinate geometry. The “inner” Cu ions, with a CuO4O′ chromophore, have a square pyramidal geometry. The two Cu(II) ions in the inner unit are bridged by four syn, syn-η11:μ propionates, showing the paddle-wheel cage type. The “outer” and “inner” linked by propionate bridges show syn, anti11:μ coordination mode. The 1D structure of complex [Cu6(phen)2(H2O)2(μ-O2CC2H5)12] n[Cu2(μ-O2CC2H5)4(H2O)2]2 n·(H2O)0.5 n2; where phen=1,10-phenanthroline, consists of zig-zag chains of mononuclear Cu(μ-O2CC2H5)2(H2O)(phen) repeating units running along the b-axis, which are connected along the unit cell diagonal via Cu2(μ-O2CC2H5)4 paddle-wheel dinuclear units. Within mononuclear and dinuclear units, the Cu(II) ions have a square pyramidal geometry. However, the outer sphere of both compounds consists of the Cu2(μ-O2CC2H5)4(H2O)2 paddle-wheel molecule in which Cu(II) ions involve a square pyramidal geometry.The synthesis, spectroscopic, magnetic and structural characterization of two new polynuclear copper(II) propionate are described. Both compounds exhibit the typical paddle-wheel type structure. The complex [Cu4(dpyam)2(OCOC2H5)2(μ-O2CC2H5)6(H2O)2][Cu2(μ- O2CC2H5)4(H2O)2]·(DMF)21; where dpyam=di-2-pyridylamine, the “outer” Cu ions, with a CuN2O2O′ chromophore, have an intermediate five-coordinate geometry. The “inner” Cu ions, with a CuO4O′ chromophore, have a square pyramidal geometry. The two Cu(II) ions in the inner unit are bridged by four syn, syn-η11:μ propionates, showing the paddle-wheel cage type. The “outer” and “inner” linked by propionate bridges showing syn, anti11:μ coordination mode. The 1D structure of complex [Cu6(phen)2(H2O)2(μ-O2CC2H5)12] n[Cu2(μ-O2CC2H5)4(H2O)2]2 n·(H2O)0.5 n2; where phen=1,10-phenanthroline, consists of zig-zag chains of mononuclear Cu(μ-O2CC2H5)2(H2O)(phen) repeating units running along the b-axis, which are connected along the unit cell diagonal via Cu2(μ-O2CC2H5)4 paddle-wheel dinuclear units. Within mononuclear and dinuclear units, the Cu(II) ions have a square pyramidal geometry. However, the outer sphere of both compounds consists of the Cu2(μ-O2CC2H5)4(H2O)2 paddle-wheel molecule in which Cu(II) ions involve a square pyramidal geometry.

Keywords: Copper(II); Di-2-pyridylamine; 1,10-Phenanthroline; Crystal structures; μ-Propionato bridges; EPR


Polynuclear paddle-wheel copper(II) propionate with di-2-pyridylamine or 1,10-phenanthroline: Preparation, characterization and X-ray structure by Sujittra Youngme; Achareeya Cheansirisomboon; Chanaiporn Danvirutai; Chaveng Pakawatchai; Narongsak Chaichit (pp. 57-62).
The synthesis, spectroscopic, magnetic and structural characterization of two new polynuclear copper(II) propionate are described. Both compounds exhibit the typical paddle-wheel type structure. The complex [Cu4(dpyam)2(OCOC2H5)2(μ-O2CC2H5)6(H2O)2][Cu2(μ-O2CC2H5)4(H2O)2]·(DMF)21, where dpyam=di-2-pyridylamine, the “outer” Cu ions, with a CuN2O2O′ chromophore, have an intermediate five-coordinate geometry. The “inner” Cu ions, with a CuO4O′ chromophore, have a square pyramidal geometry. The two Cu(II) ions in the inner unit are bridged by four syn, syn-η11:μ propionates, showing the paddle-wheel cage type. The “outer” and “inner” linked by propionate bridges show syn, anti11:μ coordination mode. The 1D structure of complex [Cu6(phen)2(H2O)2(μ-O2CC2H5)12] n[Cu2(μ-O2CC2H5)4(H2O)2]2 n·(H2O)0.5 n2; where phen=1,10-phenanthroline, consists of zig-zag chains of mononuclear Cu(μ-O2CC2H5)2(H2O)(phen) repeating units running along the b-axis, which are connected along the unit cell diagonal via Cu2(μ-O2CC2H5)4 paddle-wheel dinuclear units. Within mononuclear and dinuclear units, the Cu(II) ions have a square pyramidal geometry. However, the outer sphere of both compounds consists of the Cu2(μ-O2CC2H5)4(H2O)2 paddle-wheel molecule in which Cu(II) ions involve a square pyramidal geometry.The synthesis, spectroscopic, magnetic and structural characterization of two new polynuclear copper(II) propionate are described. Both compounds exhibit the typical paddle-wheel type structure. The complex [Cu4(dpyam)2(OCOC2H5)2(μ-O2CC2H5)6(H2O)2][Cu2(μ- O2CC2H5)4(H2O)2]·(DMF)21; where dpyam=di-2-pyridylamine, the “outer” Cu ions, with a CuN2O2O′ chromophore, have an intermediate five-coordinate geometry. The “inner” Cu ions, with a CuO4O′ chromophore, have a square pyramidal geometry. The two Cu(II) ions in the inner unit are bridged by four syn, syn-η11:μ propionates, showing the paddle-wheel cage type. The “outer” and “inner” linked by propionate bridges showing syn, anti11:μ coordination mode. The 1D structure of complex [Cu6(phen)2(H2O)2(μ-O2CC2H5)12] n[Cu2(μ-O2CC2H5)4(H2O)2]2 n·(H2O)0.5 n2; where phen=1,10-phenanthroline, consists of zig-zag chains of mononuclear Cu(μ-O2CC2H5)2(H2O)(phen) repeating units running along the b-axis, which are connected along the unit cell diagonal via Cu2(μ-O2CC2H5)4 paddle-wheel dinuclear units. Within mononuclear and dinuclear units, the Cu(II) ions have a square pyramidal geometry. However, the outer sphere of both compounds consists of the Cu2(μ-O2CC2H5)4(H2O)2 paddle-wheel molecule in which Cu(II) ions involve a square pyramidal geometry.

Keywords: Copper(II); Di-2-pyridylamine; 1,10-Phenanthroline; Crystal structures; μ-Propionato bridges; EPR


A novel Lindqvist type polyoxoniobate coordinated to four copper complex moieties: {Nb6O19[Cu(2,2′-bipy)]2[Cu(2,2′-bipy)2]2}·19H2O by Jing-Ping Wang; Hong-Yu Niu; Jing-Yang Niu (pp. 63-65).
A novel polyoxoniobate derivative Nb6O19[Cu(2,2′-bipy)]2[Cu(2,2′-bipy)2]2·19H2O1 has been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction method and IR spectroscopy. The structure analysis indicates that the Lindquist polyoxoniobate [Nb6O19]8− is capped by two divalent Cu atoms through three bridging oxygen atoms on two opposite {Nb3O3} group and supports two [Cu(2,2′-bipy)2] fragments via the terminal oxygen atoms which are also located in opposite orientations.A novel polyoxoniobate derivative {Nb6O19[Cu(2,2′-bipy)]2[Cu(2,2′-bipy)2]2}·19H2O1 has been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction method, IR spectroscopy. The structure analysis indicates that the Lindqvist polyoxoniobate [Nb6O19]8− is capped by two divalent Cu atoms through three bridging oxygen atoms on two opposite {Nb3O3} groups and supports two [Cu(2,2′-bipy)2] fragments via the terminal oxygen atoms which are also located in opposite orientations.

Keywords: Polyoxometalates; Lindqvist type; Polyoxoniobate; Crystal structure


A novel Lindqvist type polyoxoniobate coordinated to four copper complex moieties: {Nb6O19[Cu(2,2′-bipy)]2[Cu(2,2′-bipy)2]2}·19H2O by Jing-Ping Wang; Hong-Yu Niu; Jing-Yang Niu (pp. 63-65).
A novel polyoxoniobate derivative Nb6O19[Cu(2,2′-bipy)]2[Cu(2,2′-bipy)2]2·19H2O1 has been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction method and IR spectroscopy. The structure analysis indicates that the Lindquist polyoxoniobate [Nb6O19]8− is capped by two divalent Cu atoms through three bridging oxygen atoms on two opposite {Nb3O3} group and supports two [Cu(2,2′-bipy)2] fragments via the terminal oxygen atoms which are also located in opposite orientations.A novel polyoxoniobate derivative {Nb6O19[Cu(2,2′-bipy)]2[Cu(2,2′-bipy)2]2}·19H2O1 has been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction method, IR spectroscopy. The structure analysis indicates that the Lindqvist polyoxoniobate [Nb6O19]8− is capped by two divalent Cu atoms through three bridging oxygen atoms on two opposite {Nb3O3} groups and supports two [Cu(2,2′-bipy)2] fragments via the terminal oxygen atoms which are also located in opposite orientations.

Keywords: Polyoxometalates; Lindqvist type; Polyoxoniobate; Crystal structure


Crystal structure, TGA and magnetic properties of a novel 2D coordination polymer [Mn2(btr)(μ-ox)2(H2O)2]·2H2O by Yong-Quan Huang; Peng Cheng (pp. 66-68).
The self-assembly of Mn(II) ions, oxalate anions and 4,4′-bis-1,2,4-triazole gave a novel 2D coordination polymer, which is characterized via X-ray single-crystal diffraction, TGA and varied temperature magnetic susceptibility.The self-assembly of Mn(II) ions, oxalate anions and 4,4′-bis-1,2,4-triazole (btr) gave a novel 2D coordination polymer, which are characterized via X-ray single-crystal diffraction, TGA and varied temperature magnetic susceptibility. The crystal structure reveal that Mn(II) centers are linked via bis(bidentate) oxalate anion to form 1D zigzag chains, furthermore btr link these 1D chains into 2D coordination layers. Strong antiferromagnetic interactions between Mn(II) ions are found with J=−2.06cm−1.

Keywords: Crystal structures; Coordination polymers; TGA; Magnetic properties


Crystal structure, TGA and magnetic properties of a novel 2D coordination polymer [Mn2(btr)(μ-ox)2(H2O)2]·2H2O by Yong-Quan Huang; Peng Cheng (pp. 66-68).
The self-assembly of Mn(II) ions, oxalate anions and 4,4′-bis-1,2,4-triazole gave a novel 2D coordination polymer, which is characterized via X-ray single-crystal diffraction, TGA and varied temperature magnetic susceptibility.The self-assembly of Mn(II) ions, oxalate anions and 4,4′-bis-1,2,4-triazole (btr) gave a novel 2D coordination polymer, which are characterized via X-ray single-crystal diffraction, TGA and varied temperature magnetic susceptibility. The crystal structure reveal that Mn(II) centers are linked via bis(bidentate) oxalate anion to form 1D zigzag chains, furthermore btr link these 1D chains into 2D coordination layers. Strong antiferromagnetic interactions between Mn(II) ions are found with J=−2.06cm−1.

Keywords: Crystal structures; Coordination polymers; TGA; Magnetic properties


Tetranuclear pyrophosphate-bridged Cu(II) complex with 2,2′-dipyridylamine: Crystal structure, spectroscopy and magnetism by Jing-Yuan Xu; Jin-Lei Tian; Qing-Wei Zhang; Jing Zhao; Shi-Ping Yan; Dai-Zheng Liao (pp. 69-72).
Use of pyrophosphate, 2,2′-dipyridylamine with Cu(NO3)2·3H2O has enabled the synthesis of two copper(II) complexes, tetranuclear [Cu4(hdpa)4(μ-P2O7)2]·11H2O with extensive π–π stackings and H-bonding water clusters and polymer single-helical structure [Cu(hdpa)(HPO4)] n, under different reaction conditions; magnetic studies reveal that the tetranuclear one has dominant antiferromagnetic behavior.Use of pyrophosphate, 2,2′-dipyridylamine (hdpa) with Cu(NO3)2·3H2O has enabled to synthesize a novel tetranuclear copper(II) complex, [Cu4(hdpa)4(μ-P2O7)2]·11H2O1, which was characterized by single crystal X-ray diffraction, IR, ESR spectrum, and variable-temperature magnetic susceptibilities (4.2–300K). Extensive π–π stackings and H-bonding water clusters resulting from 11 free water molecules join Cu4 units to make a 3D network. According to the molecular structure, the experimental data were fitted to the expressions derived from the HamiltonianH=-2J12S^1S^2-2J13(S^1S^3+S^2S^4)-2J14(S^1S^4+S^2S^4) showing dominant antiferromagnetic behaviors.

Keywords: Crystal structure; Tetranuclear Cu(II) complex; Pyrophosphate-bridge; Magnetism; H-bonding water clusters


Tetranuclear pyrophosphate-bridged Cu(II) complex with 2,2′-dipyridylamine: Crystal structure, spectroscopy and magnetism by Jing-Yuan Xu; Jin-Lei Tian; Qing-Wei Zhang; Jing Zhao; Shi-Ping Yan; Dai-Zheng Liao (pp. 69-72).
Use of pyrophosphate, 2,2′-dipyridylamine with Cu(NO3)2·3H2O has enabled the synthesis of two copper(II) complexes, tetranuclear [Cu4(hdpa)4(μ-P2O7)2]·11H2O with extensive π–π stackings and H-bonding water clusters and polymer single-helical structure [Cu(hdpa)(HPO4)] n, under different reaction conditions; magnetic studies reveal that the tetranuclear one has dominant antiferromagnetic behavior.Use of pyrophosphate, 2,2′-dipyridylamine (hdpa) with Cu(NO3)2·3H2O has enabled to synthesize a novel tetranuclear copper(II) complex, [Cu4(hdpa)4(μ-P2O7)2]·11H2O1, which was characterized by single crystal X-ray diffraction, IR, ESR spectrum, and variable-temperature magnetic susceptibilities (4.2–300K). Extensive π–π stackings and H-bonding water clusters resulting from 11 free water molecules join Cu4 units to make a 3D network. According to the molecular structure, the experimental data were fitted to the expressions derived from the HamiltonianH=-2J12S^1S^2-2J13(S^1S^3+S^2S^4)-2J14(S^1S^4+S^2S^4) showing dominant antiferromagnetic behaviors.

Keywords: Crystal structure; Tetranuclear Cu(II) complex; Pyrophosphate-bridge; Magnetism; H-bonding water clusters


Tetranuclear nickel(II) complex with tripodal hydroxyl ligand functionalized by additional salicylaldehyde donor pendant: Synthesis, crystal structure and magnetic property by Jing-Wen Ran; Su-Yun Zhang; Bin Xu; Yuanzhi Xia; Dong Guo; Jing-Yan Zhang; Yahong Li (pp. 73-76).
The tetranuclear cubane-like [Ni4(H3hbhpd)4]·4H2O complex has been prepared and structurally characterized. Magnetic studies indicate ferromagnetic behavior for the complex. The magnetic data were fitted based on the H=−2 J1( S1 S2+ S3 S4)−2 J2( S1 S3+ S1 S4+ S2 S3+ S2 S4) and the parameters are given as g=2.21, J1=0.32, J2=8.27, D=−0.05cm−1.The tetranuclear cubane-like [Ni4(H3hbhpd)4]·4H2O complex has been prepared by the reaction of nickel(II) acetate with H5hbhpd, where H5hbhpd is 2(2-hydroxy-benzylamino)-2-hydroxymethyl-propane-1,3-diol. The X-ray diffraction analysis of the complex showed a Ni4O4 cubane arrangement of four nickel atoms. Magnetic studies indicate ferromagnetic behavior for the complex. The magnetic data were fitted and the parameters are given as g=2.21, J1=0.32, J2=8.27, D=−0.05cm−1.

Keywords: Tetranuclear; Cubane-like; Nickel complex; Magnetic properties


Tetranuclear nickel(II) complex with tripodal hydroxyl ligand functionalized by additional salicylaldehyde donor pendant: Synthesis, crystal structure and magnetic property by Jing-Wen Ran; Su-Yun Zhang; Bin Xu; Yuanzhi Xia; Dong Guo; Jing-Yan Zhang; Yahong Li (pp. 73-76).
The tetranuclear cubane-like [Ni4(H3hbhpd)4]·4H2O complex has been prepared and structurally characterized. Magnetic studies indicate ferromagnetic behavior for the complex. The magnetic data were fitted based on the H=−2 J1( S1 S2+ S3 S4)−2 J2( S1 S3+ S1 S4+ S2 S3+ S2 S4) and the parameters are given as g=2.21, J1=0.32, J2=8.27, D=−0.05cm−1.The tetranuclear cubane-like [Ni4(H3hbhpd)4]·4H2O complex has been prepared by the reaction of nickel(II) acetate with H5hbhpd, where H5hbhpd is 2(2-hydroxy-benzylamino)-2-hydroxymethyl-propane-1,3-diol. The X-ray diffraction analysis of the complex showed a Ni4O4 cubane arrangement of four nickel atoms. Magnetic studies indicate ferromagnetic behavior for the complex. The magnetic data were fitted and the parameters are given as g=2.21, J1=0.32, J2=8.27, D=−0.05cm−1.

Keywords: Tetranuclear; Cubane-like; Nickel complex; Magnetic properties


New bis(pyranodithiolene) tungsten(IV) and (VI) complexes as chemical analogues of the active sites of tungsten enzymes by Hideki Sugimoto; Kunihisa Sugimoto (pp. 77-80).
A first example of tungsten complexes, (Et4N)2[WO(L0)2]((Et4N)2[1a]) and (Et4N)2[WO2(L0)2]((Et4N)2[1b]), containing pyranodithiolene were synthesized as new models of reaction center of tungsten enzymes. The pyrane ring affected the WO bond stretchings in1a and1b, the redox potential of1a, and LMCT bands of1b.First examples of tungsten complexes, (Et4N)2[WO(L0)2]((Et4N)2 [1a]) and (Et4N)2[WO2(L0)2]((Et4N)2 [1b]), containing pyranodithiolene were synthesized as new models of reaction center of tungsten enzymes. The complexes were characterized by IR, UV–Vis, Raman spectroscopies, and cyclic voltammogram (CV). The crystal structures were determined by X-ray crystallography. The pyrane ring affected the WO bond stretchings in1a and1b, the redox potential of1a, and LMCT bands of1b.

Keywords: Crystal structure; Enzyme model; Pyranodithiolene; Synthesis; Tungsten


New bis(pyranodithiolene) tungsten(IV) and (VI) complexes as chemical analogues of the active sites of tungsten enzymes by Hideki Sugimoto; Kunihisa Sugimoto (pp. 77-80).
A first example of tungsten complexes, (Et4N)2[WO(L0)2]((Et4N)2[1a]) and (Et4N)2[WO2(L0)2]((Et4N)2[1b]), containing pyranodithiolene were synthesized as new models of reaction center of tungsten enzymes. The pyrane ring affected the WO bond stretchings in1a and1b, the redox potential of1a, and LMCT bands of1b.First examples of tungsten complexes, (Et4N)2[WO(L0)2]((Et4N)2 [1a]) and (Et4N)2[WO2(L0)2]((Et4N)2 [1b]), containing pyranodithiolene were synthesized as new models of reaction center of tungsten enzymes. The complexes were characterized by IR, UV–Vis, Raman spectroscopies, and cyclic voltammogram (CV). The crystal structures were determined by X-ray crystallography. The pyrane ring affected the WO bond stretchings in1a and1b, the redox potential of1a, and LMCT bands of1b.

Keywords: Crystal structure; Enzyme model; Pyranodithiolene; Synthesis; Tungsten


Unprecedented sodium–oxygen clusters in the solid-state structure of trisodium hydrogentetravalproate monohydrate: A model for the physiological activity of the anticonvulsant drug Epilim® by Gjorgi Petruševski; Panče Naumov; Gligor Jovanovski; Seik Weng Ng (pp. 81-84).
The first structure determination of one form of sodium valproate, which is the basis of the anticonvulsant drug Epilim® for treatment of epilepsy and bipolar disorders, revealed that the compound is, in fact, a 3:1 co-crystal of sodium valproate and valproic acid. The anion symmetry-directed formation of stable sodium–oxygen clusters protected by a lipophilic alkyl layer may be the key for the strong physiological activity of this important compound.The first crystal structure determination of one of the solid forms of sodium valproate revealed that the crystal is a 3:1 solvate of sodium valproate and valproic acid. The anion symmetry-directed formation of stable sodium–oxygen clusters protected by alkyl layer which can act as lipophilic micelles may be important for understanding the strong anticonvulsant activity of the valproate ion.

Keywords: Anticonvulsants; Bilayers; Clusters; Epilim; Hygroscopicity; Hydrates


Unprecedented sodium–oxygen clusters in the solid-state structure of trisodium hydrogentetravalproate monohydrate: A model for the physiological activity of the anticonvulsant drug Epilim® by Gjorgi Petruševski; Panče Naumov; Gligor Jovanovski; Seik Weng Ng (pp. 81-84).
The first structure determination of one form of sodium valproate, which is the basis of the anticonvulsant drug Epilim® for treatment of epilepsy and bipolar disorders, revealed that the compound is, in fact, a 3:1 co-crystal of sodium valproate and valproic acid. The anion symmetry-directed formation of stable sodium–oxygen clusters protected by a lipophilic alkyl layer may be the key for the strong physiological activity of this important compound.The first crystal structure determination of one of the solid forms of sodium valproate revealed that the crystal is a 3:1 solvate of sodium valproate and valproic acid. The anion symmetry-directed formation of stable sodium–oxygen clusters protected by alkyl layer which can act as lipophilic micelles may be important for understanding the strong anticonvulsant activity of the valproate ion.

Keywords: Anticonvulsants; Bilayers; Clusters; Epilim; Hygroscopicity; Hydrates


A three-dimensional supramolecular complex [Cs(DB24C8)][CuBr2] based on C–H⋯π and Cs⋯Br weak interactions by Mancheng Hu; Xiuhang Wang; Yucheng Jiang; Shu’ni Li (pp. 85-88).
This is a novel 0D supramolecular complex whose dimensionality is increased to 3D by C–H⋯π and Cs⋯Br weak interactions. In the pictogram, the ligands were omitted for clarity and the cesium cations were linked by dashed lines according to the connectivity defined by C–H⋯π bonds.A new supramolecular complex [Cs(DB24C8)][CuBr2] (1) (DB24C8=Dibenzo-24-Crown-8) has been prepared, characterized and structurally investigated. The structure of complex1 features a two-dimensional (2D) (4,4) network in the ac plane based on C–H⋯π interactions and the dimensionality is further increased to 3D by Cs⋯Br weak interactions.

Keywords: DB24C8 complex; C–H⋯π interaction; Cs⋯Br interaction; (4,4) Network; Supramolecular structure


A three-dimensional supramolecular complex [Cs(DB24C8)][CuBr2] based on C–H⋯π and Cs⋯Br weak interactions by Mancheng Hu; Xiuhang Wang; Yucheng Jiang; Shu’ni Li (pp. 85-88).
This is a novel 0D supramolecular complex whose dimensionality is increased to 3D by C–H⋯π and Cs⋯Br weak interactions. In the pictogram, the ligands were omitted for clarity and the cesium cations were linked by dashed lines according to the connectivity defined by C–H⋯π bonds.A new supramolecular complex [Cs(DB24C8)][CuBr2] (1) (DB24C8=Dibenzo-24-Crown-8) has been prepared, characterized and structurally investigated. The structure of complex1 features a two-dimensional (2D) (4,4) network in the ac plane based on C–H⋯π interactions and the dimensionality is further increased to 3D by Cs⋯Br weak interactions.

Keywords: DB24C8 complex; C–H⋯π interaction; Cs⋯Br interaction; (4,4) Network; Supramolecular structure


Identification of ONO⋯ONO interactions among inorganic coordination complex molecules in the crystal lattice of a chiral Mn(IV) compound by Chullikkattil P. Pradeep; Panthapally S. Zacharias; Samar K. Das (pp. 89-93).
The chiral Schiff base ligand H2L on reaction with Mn(CH3COO)2·4H2O affords a chiral Mn(IV) compound [MnL2]·DMF (1). Crystal structure analysis of compound1 revealed an interesting O⋯O non-covalent, non-hydrogen bonded interaction between –NO2 groups present on adjacent [MnIVL2] complex units which leads to the formation of chainlike arrangement in the crystal lattice of the relevant complex. This is the first report of ONO⋯ONO non-covalent interactions in an inorganic complex.The chiral Schiff base ligand H2L on reaction with Mn(CH3COO)2·4H2O in methanol gave a yellow precipitate, which on recrystallization from dimethylformamide (DMF) solvent solvent gave dark-brown needle shaped crystals of a chiral Mn(IV) compound [MnL2]·DMF (1). Crystal structure analysis of compound1 revealed an interesting O⋯O non-covalent interaction between –NO2 groups present on adjacent [MnIVL2] complex units which leads to the formation of chainlike arrangement in the crystal lattice of the relevant complex.

Keywords: Chiral Mn(IV) complex; Crystal structure; Nitro–nitro interaction; Supramolecular chemistry


Identification of ONO⋯ONO interactions among inorganic coordination complex molecules in the crystal lattice of a chiral Mn(IV) compound by Chullikkattil P. Pradeep; Panthapally S. Zacharias; Samar K. Das (pp. 89-93).
The chiral Schiff base ligand H2L on reaction with Mn(CH3COO)2·4H2O affords a chiral Mn(IV) compound [MnL2]·DMF (1). Crystal structure analysis of compound1 revealed an interesting O⋯O non-covalent, non-hydrogen bonded interaction between –NO2 groups present on adjacent [MnIVL2] complex units which leads to the formation of chainlike arrangement in the crystal lattice of the relevant complex. This is the first report of ONO⋯ONO non-covalent interactions in an inorganic complex.The chiral Schiff base ligand H2L on reaction with Mn(CH3COO)2·4H2O in methanol gave a yellow precipitate, which on recrystallization from dimethylformamide (DMF) solvent solvent gave dark-brown needle shaped crystals of a chiral Mn(IV) compound [MnL2]·DMF (1). Crystal structure analysis of compound1 revealed an interesting O⋯O non-covalent interaction between –NO2 groups present on adjacent [MnIVL2] complex units which leads to the formation of chainlike arrangement in the crystal lattice of the relevant complex.

Keywords: Chiral Mn(IV) complex; Crystal structure; Nitro–nitro interaction; Supramolecular chemistry


Synthesis, crystal structure and magnetic properties of a cyanide-bridged heterobimetallic trinuclearCr2IIIMnII complex based on K[Cr(salen)(CN)2] building block by Zhong-Hai Ni; Li-Fang Zhang; Chun-Hua Ge; Ai-Li Cui; Hui-Zhong Kou; Jianzhuang Jiang (pp. 94-96).
The cyanide-containing building block K[Cr(salen)(CN)2] (H2salen= N, N′-bis(salicyl)ethylenediamine) featuring two trans cyanide groups has been successfully exploited to assembly cyanide-bridged low-dimensional complexes. A new cyanide-bridged heterobimetallic trinuclearCr2IIIMnII complex [Cr(salen)(CN)2]2[Mn(phen)2]·2H2O has been investigated structurally and magnetically.A new cyanide-containing building block K[Cr(salen)(CN)2] (H2salen= N, N′-bis(salicyl)ethylenediamine) with two trans cyanide groups has been exploited to assembly cyanide-bridged low-dimensional complexes. A cyanide-bridged heterobimetallic centrosymmetric trinuclear CrIII–MnII–CrIII complex [Cr(salen)(CN)2]2[Mn(phen)2]·2H2O (1) has been synthesized and its structure has been characterized by X-ray diffraction analysis. The magnetic coupling between Mn(II) and Cr(III) ions in the title complex was found to be antiferromagnetic with JMnCr=−2.02(2)cm−1 on the basis of the HamiltonianH^=-2JS^MnS^Cr(1)+S^MnS^Cr(2).

Keywords: Crystal structure; Magnetic properties; Cyanide-bridged; Chromium; Manganese


Synthesis, crystal structure and magnetic properties of a cyanide-bridged heterobimetallic trinuclearCr2IIIMnII complex based on K[Cr(salen)(CN)2] building block by Zhong-Hai Ni; Li-Fang Zhang; Chun-Hua Ge; Ai-Li Cui; Hui-Zhong Kou; Jianzhuang Jiang (pp. 94-96).
The cyanide-containing building block K[Cr(salen)(CN)2] (H2salen= N, N′-bis(salicyl)ethylenediamine) featuring two trans cyanide groups has been successfully exploited to assembly cyanide-bridged low-dimensional complexes. A new cyanide-bridged heterobimetallic trinuclearCr2IIIMnII complex [Cr(salen)(CN)2]2[Mn(phen)2]·2H2O has been investigated structurally and magnetically.A new cyanide-containing building block K[Cr(salen)(CN)2] (H2salen= N, N′-bis(salicyl)ethylenediamine) with two trans cyanide groups has been exploited to assembly cyanide-bridged low-dimensional complexes. A cyanide-bridged heterobimetallic centrosymmetric trinuclear CrIII–MnII–CrIII complex [Cr(salen)(CN)2]2[Mn(phen)2]·2H2O (1) has been synthesized and its structure has been characterized by X-ray diffraction analysis. The magnetic coupling between Mn(II) and Cr(III) ions in the title complex was found to be antiferromagnetic with JMnCr=−2.02(2)cm−1 on the basis of the HamiltonianH^=-2JS^MnS^Cr(1)+S^MnS^Cr(2).

Keywords: Crystal structure; Magnetic properties; Cyanide-bridged; Chromium; Manganese


Synthesis of phenanthroline derivatives by Sonogashira reaction and the use of their ruthenium complexes as optical sensors by Miso Jeong; Hyungoog Nam; Ok-Jae Sohn; Jong Il Rhee; Hyung Jin Kim; Chang-Woo Cho; Sunwoo Lee (pp. 97-100).
The phenanthroline derivatives, which have alkynyl groups, were synthesized by palladium-catalyzed, Sonogashira cross-coupling reaction. Their ruthenium complex7a and7b were synthesized under mild conditions. The former showed relative fluorescence intensity changes between fully oxygenated and fully deoxygenated atmospheres, while the latter showed a linear fluorescence intensity response between pH 6 and 13.The phenanthroline derivatives, which have alkynyl groups, were synthesized by palladium-catalyzed, Sonogashira cross-coupling reaction to provide the following coupled products: 4,7-bis(4-phenylethynyl-phenyl)-[1,10]phenanthroline (6a) and 4,7-bis{4-(4-hydroxy-buty-1-ynyl)-phenyl)-[1,10]phenanthroline (6b) at 87 and 89% yield, respectively. Their ruthenium complexes, tris{4,7-bis(4-phenylethynyl-phenyl)-[1,10]phenanthroline} ruthenium(II) bis(hexafluorophosphate) (7a) and tris[4,7-bis{4-(4-hydroxy-buty-1-ynyl)-phenyl)-[1, 10]phenanthroline}ruthenium(II)bis(hexafluoro-phosphate) (7b), were synthesized under mild conditions. The former showed relative fluorescence intensity changes between fully oxygenated and fully deoxygenated atmospheres, while the latter showed a linear fluorescence intensity response between pH 6 and 13.

Keywords: Ruthenium; Palladium; Sonogashira; Phenanthroline; pH Sensor; pO; 2; Sensor; Fluorescence


Synthesis of phenanthroline derivatives by Sonogashira reaction and the use of their ruthenium complexes as optical sensors by Miso Jeong; Hyungoog Nam; Ok-Jae Sohn; Jong Il Rhee; Hyung Jin Kim; Chang-Woo Cho; Sunwoo Lee (pp. 97-100).
The phenanthroline derivatives, which have alkynyl groups, were synthesized by palladium-catalyzed, Sonogashira cross-coupling reaction. Their ruthenium complex7a and7b were synthesized under mild conditions. The former showed relative fluorescence intensity changes between fully oxygenated and fully deoxygenated atmospheres, while the latter showed a linear fluorescence intensity response between pH 6 and 13.The phenanthroline derivatives, which have alkynyl groups, were synthesized by palladium-catalyzed, Sonogashira cross-coupling reaction to provide the following coupled products: 4,7-bis(4-phenylethynyl-phenyl)-[1,10]phenanthroline (6a) and 4,7-bis{4-(4-hydroxy-buty-1-ynyl)-phenyl)-[1,10]phenanthroline (6b) at 87 and 89% yield, respectively. Their ruthenium complexes, tris{4,7-bis(4-phenylethynyl-phenyl)-[1,10]phenanthroline} ruthenium(II) bis(hexafluorophosphate) (7a) and tris[4,7-bis{4-(4-hydroxy-buty-1-ynyl)-phenyl)-[1, 10]phenanthroline}ruthenium(II)bis(hexafluoro-phosphate) (7b), were synthesized under mild conditions. The former showed relative fluorescence intensity changes between fully oxygenated and fully deoxygenated atmospheres, while the latter showed a linear fluorescence intensity response between pH 6 and 13.

Keywords: Ruthenium; Palladium; Sonogashira; Phenanthroline; pH Sensor; pO; 2; Sensor; Fluorescence


Host–guest encapsulation of organosulphonate ligands into a host framework assembled from Keggin polyoxometalate anions and in situ generated organonitrogen cations by Jian Lü; Fu-Xian Xiao; Tao-Hai Li; Rong Cao (pp. 101-104).
A three-dimensional supramolecular framework constructed by [SiMo12O40]4− Keggin anions and in situ generated mix H2pip2+ and H2pesp ligands is reported, within which the [SiMo12O40]4− Keggin anions and in situ generated H2pip cations self-assemble into a hybrid porous host via intensive fourfold hydrogen bonds and the H2pesp precursor ligands trap in the void of host framework as guests.The synthesis and crystal structure of a novel supramolecular compound, formulated as (H2pesp)(H2pip)2[SiMo12O40]·4H2O1 (pesp2−=piperazine-1,4-bis(2-ethanesulfonic acid) anion, pip=piperazine), is described. Compound1 is characterized by elemental analyses, infrared spectrum, thermogravimetric analysis, and single-crystal X-ray analysis. X-ray crystallography reveals that1 displays a three-dimensional supramolecular framework constructed by [SiMo12O40]4− Keggin anions and in situ generated mix H2pip2+ and H2pesp ligands. In the structure of1, [SiMo12O40]4− Keggin anions and in situ generated H2pip cations self-assemble into a hybrid porous host via intensive fourfold hydrogen bonds, within which the H2pesp precursor ligands are trapped as guests.

Keywords: Polyoxometalate; Organosulphonate; Host–guest; Supramolecular; In situ


Host–guest encapsulation of organosulphonate ligands into a host framework assembled from Keggin polyoxometalate anions and in situ generated organonitrogen cations by Jian Lü; Fu-Xian Xiao; Tao-Hai Li; Rong Cao (pp. 101-104).
A three-dimensional supramolecular framework constructed by [SiMo12O40]4− Keggin anions and in situ generated mix H2pip2+ and H2pesp ligands is reported, within which the [SiMo12O40]4− Keggin anions and in situ generated H2pip cations self-assemble into a hybrid porous host via intensive fourfold hydrogen bonds and the H2pesp precursor ligands trap in the void of host framework as guests.The synthesis and crystal structure of a novel supramolecular compound, formulated as (H2pesp)(H2pip)2[SiMo12O40]·4H2O1 (pesp2−=piperazine-1,4-bis(2-ethanesulfonic acid) anion, pip=piperazine), is described. Compound1 is characterized by elemental analyses, infrared spectrum, thermogravimetric analysis, and single-crystal X-ray analysis. X-ray crystallography reveals that1 displays a three-dimensional supramolecular framework constructed by [SiMo12O40]4− Keggin anions and in situ generated mix H2pip2+ and H2pesp ligands. In the structure of1, [SiMo12O40]4− Keggin anions and in situ generated H2pip cations self-assemble into a hybrid porous host via intensive fourfold hydrogen bonds, within which the H2pesp precursor ligands are trapped as guests.

Keywords: Polyoxometalate; Organosulphonate; Host–guest; Supramolecular; In situ


A new water layer trapped in a ladder-like coordination polymer by FuXian Xiao; Jian Lü; Zhenggang Guo; Taohai Li; Yafeng Li; Rong Cao (pp. 105-109).
A novel two-dimensional water layer which is trapped in a one-dimensional neodymium-organic arrays, [Nd2(BC)2(OX)(H2O)6] n·10 nH2O (BC2−=1,3-benzenedicarboxylate anion andOX2-=C2O42-), is reported. Interestingly, there is puckered 16-membered rings existing in the water layer.A novel two-dimensional water layer which is trapped in a one-dimensional neodymium-organic arrays, [Nd2(BC)2(OX)(H2O)6] n·10 nH2O (BC2−=1,3-benzenedicarboxylate anion andOX2-=C2O42-), is reported. There are puckered 6-, 12- and 16-membered rings existing in the water layer. The cyclic 6- and 12-membered rings in turn fuse together to generate the water tape, namely T6(3)12(3)6(2). The water layer is formed via the assembly of the T6(3)12(3)6(2) water tapes.

Keywords: Neodymium; Water layer; 16-membered ring; Trapped


A new water layer trapped in a ladder-like coordination polymer by FuXian Xiao; Jian Lü; Zhenggang Guo; Taohai Li; Yafeng Li; Rong Cao (pp. 105-109).
A novel two-dimensional water layer which is trapped in a one-dimensional neodymium-organic arrays, [Nd2(BC)2(OX)(H2O)6] n·10 nH2O (BC2−=1,3-benzenedicarboxylate anion andOX2-=C2O42-), is reported. Interestingly, there is puckered 16-membered rings existing in the water layer.A novel two-dimensional water layer which is trapped in a one-dimensional neodymium-organic arrays, [Nd2(BC)2(OX)(H2O)6] n·10 nH2O (BC2−=1,3-benzenedicarboxylate anion andOX2-=C2O42-), is reported. There are puckered 6-, 12- and 16-membered rings existing in the water layer. The cyclic 6- and 12-membered rings in turn fuse together to generate the water tape, namely T6(3)12(3)6(2). The water layer is formed via the assembly of the T6(3)12(3)6(2) water tapes.

Keywords: Neodymium; Water layer; 16-membered ring; Trapped


The behaviour ofNH4+ in a water nanodrop encapsulated within a highly charged porous metal–oxide nanocontainer: A thermoanalytical study by Adam Bielański; Andrzej Małecki; Anna Lubańska; Ekkehard Diemann; Hartmut Bögge; Achim Müller (pp. 110-113).
The properties and especially the thermal stability ofNH4+ in a nanodrop of water encapsulated into a structurally well defined porous molybdenum-oxide based nanocontainer has been studied with thermoanalytical methods (TG/MS, DTA, DTG); this gives new insights into the behaviour of electrolytes under confined conditions.The properties and especially the thermal stability ofNH4+ in a nanodrop of water encapsulated into a structurally well defined porous molybdenum-oxide based nanocontainer has been studied with thermoanalytical methods (TG/MS, DTA, DTG); this gives new insights into the behaviour of electrolytes under confined conditions.

Keywords: Electrolytes; Porous nanocontainers; Polyoxomolybdates; Confined conditions; Thermogravimetry/mass spectrometry


The behaviour ofNH4+ in a water nanodrop encapsulated within a highly charged porous metal–oxide nanocontainer: A thermoanalytical study by Adam Bielański; Andrzej Małecki; Anna Lubańska; Ekkehard Diemann; Hartmut Bögge; Achim Müller (pp. 110-113).
The properties and especially the thermal stability ofNH4+ in a nanodrop of water encapsulated into a structurally well defined porous molybdenum-oxide based nanocontainer has been studied with thermoanalytical methods (TG/MS, DTA, DTG); this gives new insights into the behaviour of electrolytes under confined conditions.The properties and especially the thermal stability ofNH4+ in a nanodrop of water encapsulated into a structurally well defined porous molybdenum-oxide based nanocontainer has been studied with thermoanalytical methods (TG/MS, DTA, DTG); this gives new insights into the behaviour of electrolytes under confined conditions.

Keywords: Electrolytes; Porous nanocontainers; Polyoxomolybdates; Confined conditions; Thermogravimetry/mass spectrometry


Solvent induced oxidative addition and phenyl migration in trans-[RhCl(CO)(SbPh3)3]: Crystal structure of trans- mer-[Rh(Cl)2(Ph)(SbPh3)3] by Stefanus Otto; Andreas Roodt (pp. 114-116).
Phenyl migration and oxidative addition was observed in nitromethane containing solutions of trans-[RhCl(CO)(SbPh3) n] ( n=2 or 3) and free SbPh3. A Rh(III) product resulting from phenyl migration and oxidative addition to Rh(I), [Rh(Cl)2(Ph)(SbPh3)3], was characterised by X-ray crystallography.Phenyl migration and oxidative addition were observed in nitromethane containing solutions of trans-[RhCl(CO)(SbPh3) n] ( n=2 or 3) and free SbPh3. A Rh(III) product resulting from phenyl migration and oxidative addition to Rh(I), trans- mer-[Rh(Cl)2(Ph)(SbPh3)3], was characterised by X-ray crystallography.

Keywords: Rhodium; Phenyl migration; Oxidative addition; Triphenyl antimony; Crystal structure


Solvent induced oxidative addition and phenyl migration in trans-[RhCl(CO)(SbPh3)3]: Crystal structure of trans- mer-[Rh(Cl)2(Ph)(SbPh3)3] by Stefanus Otto; Andreas Roodt (pp. 114-116).
Phenyl migration and oxidative addition was observed in nitromethane containing solutions of trans-[RhCl(CO)(SbPh3) n] ( n=2 or 3) and free SbPh3. A Rh(III) product resulting from phenyl migration and oxidative addition to Rh(I), [Rh(Cl)2(Ph)(SbPh3)3], was characterised by X-ray crystallography.Phenyl migration and oxidative addition were observed in nitromethane containing solutions of trans-[RhCl(CO)(SbPh3) n] ( n=2 or 3) and free SbPh3. A Rh(III) product resulting from phenyl migration and oxidative addition to Rh(I), trans- mer-[Rh(Cl)2(Ph)(SbPh3)3], was characterised by X-ray crystallography.

Keywords: Rhodium; Phenyl migration; Oxidative addition; Triphenyl antimony; Crystal structure


Novel nickel(II) complex bearing phthalimido ligands derived from oxime-mediated transformation of phthalonitrile by Maximilian N. Kopylovich; Matti Haukka; Alexander M. Kirillov; Vadim Yu. Kukushkin; Armando J.L. Pombeiro (pp. 117-120).
The oxime-mediated transformation of phthalonitrile to phthalimido species, in the presence of nickel(II) nitrate and ethylenediamine, resulted in a rare inorganic phthalimido-ethylenediamine nickel(II) coordination compound, which was fully characterized and whose molecular structure was established by single crystal X-ray diffraction analysis.The new heteroligand phthalimido-ethylenediamine nickel(II) complex [Ni{ trans-(pti)2}(en)2] (2) has been prepared via the oxime-mediated transformation of phthalonitrile to the phthalimido (or phthalimidato) (pti) moiety in the presence of Ni(NO3)2·6H2O, 2-propanone oxime and ethylenediamine (en). Compound2 has been characterized by IR, FAB+-MS and1H NMR spectroscopy, elemental and single crystal X-ray diffraction analyses, showing a slightly distorted octahedral geometry around the centrosymmetric Ni centre with trans phthalimido ligands and ethylenediamine moieties in the equatorial sites.

Keywords: Nickel; Phthalonitrile; Oxime-mediated transformation; Phthalimide; Crystal structure


Novel nickel(II) complex bearing phthalimido ligands derived from oxime-mediated transformation of phthalonitrile by Maximilian N. Kopylovich; Matti Haukka; Alexander M. Kirillov; Vadim Yu. Kukushkin; Armando J.L. Pombeiro (pp. 117-120).
The oxime-mediated transformation of phthalonitrile to phthalimido species, in the presence of nickel(II) nitrate and ethylenediamine, resulted in a rare inorganic phthalimido-ethylenediamine nickel(II) coordination compound, which was fully characterized and whose molecular structure was established by single crystal X-ray diffraction analysis.The new heteroligand phthalimido-ethylenediamine nickel(II) complex [Ni{ trans-(pti)2}(en)2] (2) has been prepared via the oxime-mediated transformation of phthalonitrile to the phthalimido (or phthalimidato) (pti) moiety in the presence of Ni(NO3)2·6H2O, 2-propanone oxime and ethylenediamine (en). Compound2 has been characterized by IR, FAB+-MS and1H NMR spectroscopy, elemental and single crystal X-ray diffraction analyses, showing a slightly distorted octahedral geometry around the centrosymmetric Ni centre with trans phthalimido ligands and ethylenediamine moieties in the equatorial sites.

Keywords: Nickel; Phthalonitrile; Oxime-mediated transformation; Phthalimide; Crystal structure


A penta-coordinated bis-(8-aminoquinoline) monobenzoato zinc(II) benzoate complex favored by self-assembly formation by Abhilasha M. Baruah; Rupam Sarma; Jubaraj B. Baruah (pp. 121-124).
The structure of bis-(8-aminoquinoline) monobenzoato zinc(II) benzoate is determined and its synthetic method and solution chemistry is discussed.A simple method to synthesize a penta-coordinated bis-(8-aminoquinoline) monobenzoato zinc(II) benzoate complex and its reason for formation is explained.

Keywords: Self-assembly; Penta-coordinated zinc complex; 8-Aminoquinoline; Crystal structure


A penta-coordinated bis-(8-aminoquinoline) monobenzoato zinc(II) benzoate complex favored by self-assembly formation by Abhilasha M. Baruah; Rupam Sarma; Jubaraj B. Baruah (pp. 121-124).
The structure of bis-(8-aminoquinoline) monobenzoato zinc(II) benzoate is determined and its synthetic method and solution chemistry is discussed.A simple method to synthesize a penta-coordinated bis-(8-aminoquinoline) monobenzoato zinc(II) benzoate complex and its reason for formation is explained.

Keywords: Self-assembly; Penta-coordinated zinc complex; 8-Aminoquinoline; Crystal structure


Unprecedented 7-connected 36·413·62 structural topology: Praseodymium-based coordination polymers built from mixed carboxylate ligands by Peng Ren; Wei Shi; Peng Cheng (pp. 125-128).
A novel coordination polymer [Pr(dpdc)(nta)] n has been successfully synthesized through hydrothermal route. The particular interest is that it not only contains two different carboxylate bridging ligands, but also represents an unprecedented 7-connected 36·413·62 topology.A new lanthanide coordination polymer [Pr(dpdc)(nta)] n (1) (H2dpdc=2,2′-diphenyldicarboxylate acid, Hnta=nicotinic acid) has been prepared and characterized by IR, element analysis, TGA, and single-crystal X-ray diffraction.1 is built up from two different carboxylate ligands and shows an unusual two-dimensional (2D) 7-connected 36·413·62 topological network. The zero-field splitting parameter was obtained by varied magnetic susceptibilities measurement (2–300K).

Keywords: Praseodymium; N,; O ligand; 7-Connected topology; Magnetic properties; Hydrothermal synthesis


Unprecedented 7-connected 36·413·62 structural topology: Praseodymium-based coordination polymers built from mixed carboxylate ligands by Peng Ren; Wei Shi; Peng Cheng (pp. 125-128).
A novel coordination polymer [Pr(dpdc)(nta)] n has been successfully synthesized through hydrothermal route. The particular interest is that it not only contains two different carboxylate bridging ligands, but also represents an unprecedented 7-connected 36·413·62 topology.A new lanthanide coordination polymer [Pr(dpdc)(nta)] n (1) (H2dpdc=2,2′-diphenyldicarboxylate acid, Hnta=nicotinic acid) has been prepared and characterized by IR, element analysis, TGA, and single-crystal X-ray diffraction.1 is built up from two different carboxylate ligands and shows an unusual two-dimensional (2D) 7-connected 36·413·62 topological network. The zero-field splitting parameter was obtained by varied magnetic susceptibilities measurement (2–300K).

Keywords: Praseodymium; N,; O ligand; 7-Connected topology; Magnetic properties; Hydrothermal synthesis

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