Published by De Gruyter

Volume 73 Issue 3-4

Issue of Zeitschrift für Naturforschung B

Contents
Journal Overview

Publicly Available April 2, 2018

Frontmatter

Page range: i-iv

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Publicly Available April 2, 2018

In this Issue

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February 22, 2018

Does Lewis basicity correlate with catalytic performance in zerovalent group 8 complexes?

Holger Braunschweig, Carina Brunecker, Rian D. Dewhurst, Christoph Schneider

Page range: 149-153

Abstract

A set of 18 zerovalent group 8 metal complexes of the form [ML n (CO) 5− n ] (M=Fe, Ru, Os; L=neutral donor; n =0–2) were screened for their catalytic performance in aldehyde hydrosilylation and olefin hydroboration reactions. Although none of the untested catalysts were found to perform better than the previously-published complex [Fe(CO) 4 (IMes)] (IMes=1,3-Dimesityliidazol-2-ylidene), the results suggest that the Lewis basicity of the metal complex does not play a critical role in the catalysis of these two reactions.

March 15, 2018

Crystal structure and luminescence properties of a new dinuclear bismuth(III) coordination polymer containing three types of ligands

Yu-Quan Feng, Zhi-Guo Zhong, Hong-Wei Wang, Zheng-Zheng Xing, Lu Wang

Page range: 155-160

Abstract

A new dinuclear bismuth(III) coordination polymer {[Bi(H 2 O)] 2 (C 7 H 3 NO 4 ) 2 (C 12 H 8 N 2 ) 2 (N 3 ) 2 ·2H 2 O} n ( 1 ) containing three types of ligands has been synthesized using a solvothermal method and characterized by infrared (IR) spectroscopy, energy-dispersive X-ray spectroscopy, and X-ray single-crystal structural analysis. The compound can be viewed as a three-dimensional supramolecular network that is constructed by Bi 3+ cations, N 3 − anions, pyridine-2,5-dicarboxylate (2,5-pdc 2− ), and 1,10-phenanthroline (phen) ligands. Moreover, the luminescence properties, quantum yield, luminescence decay, and thermal stabilities of 1 were also investigated.

March 24, 2018

Syntheses, structures, and catalytic properties of two arene-ruthenium(II) complexes bearing N-(2-pyridinyl)aminodiphenylphosphine sulfide ligands

Fule Wu, Jiling Gu, Xin Chen, Ai-Quan Jia, Qian-Feng Zhang

Page range: 161-166

Abstract

Treatment of [(arene)Ru( μ -Cl)Cl] 2 with Ph 2 P(S)NH(2-py) in the presence or absence of base gave two arene-ruthenium(II) complexes [( η 6 - p -cymene)Ru{ κ 2 - N , N -Ph 2 P(S)N(2-py)}Cl] ( 1 ) and [( η 6 -benzene)Ru{ κ 1 - N -Ph 2 P(S)NH(2-py)}Cl 2 ] ( 2 ), which have been characterized by infrared, nuclear magnetic resonance spectroscopies, and mass spectrometry along with microanalyses. Crystal structures of Ph 2 P(S)NH(2-py) · ¼C 6 H 14 , 1 and 2 · ½CH 2 Cl 2 were determined by single-crystal X-ray diffraction. Two arene-ruthenium(II) complexes were tested as precatalysts for the transfer hydrogenation of acetophenone to give 1-phenyl ethanol.

March 20, 2018

Synthesis, characterization, anticancer and antimicrobial study of arene ruthenium(II) complexes with 1,2,4-triazole ligands containing an α-diimine moiety

Joel M. Gichumbi, Holger B. Friedrich, Bernard Omondi, Geraldine G. Lazarus, Moganavelli Singh, Hafizah Y. Chenia

Page range: 167-178

Abstract

The reaction of the ruthenium arene dimers [( η 6 -arene)Ru( μ -Cl)Cl] 2 (where arene=benzene or p -cymene) with the ligands 4-benzylidene-3,5-di(2′-pyridyl)-4-amino-1,2,4-triazole ( L 1 ), 2-methoxybenzylidene-3,5-di(2′-pyridyl)-4-amino-1,2,4-triazole ( L 2 ), 4-methylbenzylidene-3,5-di(2′-pyridyl)-4-amino-1,2,4-triazole ( L 3 ) and indole-3-carbaldehyde-3,5-di(2′-pyridyl)-4-amino-1,2,4-triazole ( L 4 ) in a 1:2 ratio gives the new complexes [( η 6 -arene)RuCl(L)] + [arene=C 6 H 6 (with L=L 1 ( 1 ), L 2 ( 3 ), L 4 ( 7 ), with PF 6 − as a counter ion, and L 4 ( 6 ), with Cl − as a counter ion) or p -cymene with L=L 1 ( 2 ), L 2 ( 4 ), L 3 ( 5 ), L 4 ( 8 ) with PF 6 − as a counter ion]. All complexes were fully characterized using 1 H and 13 C NMR, elemental analyses, UV/Vis and IR spectroscopy. The single crystal X-ray structures of ligand L 2 and complex 1 have been determined. The structure of 1 has the Ru atom coordinated with the arene group and to the N , N ′-bidentate ligand and to the Cl atom. The arene group occupies the apex, while the ligand and the Cl atom are at the base of a pseudo-octahedral three-legged piano stool. The cytotoxicity of these mononuclear complexes was established in the human epithelial colorectal adenocarcinoma cell line (Caco-2) and for selectivity in the non-cancerous human embryonic kidney cell line (HEK293), using 5-fluorouracil (5-FU) as the reference anticancer drug. Compounds 1 and 7 were relatively inactive toward the Caco-2 tumor cells (IC 50 >200), while complexes 2–5 showed moderate anti-proliferative properties (IC 50 >100–200). Compound 6 , however, displayed better anti-proliferative properties with an IC 50 value lower than that of the reference drug, 5-FU, and was therefore further investigated for its antimicrobial activity against six Gram-positive and four Gram-negative bacteria.

March 19, 2018

Green synthesis of α-aminophosphonates using ZnO nanoparticles as an efficient catalyst

Elham Ezzatzadeh

Page range: 179-184

Abstract

Synthesis of α -aminophosphonate derivatives via the Kabachnik–Fields reaction is described using 1-(6-hydroxy-2-isopropenyl-1-benzofuran-yl)-1-ethanone, extracted from rhizomes of Petasites hybridus , primary amines and trialkyl phosphites in the presence of ZnO nanoparticles in water at room temperature. This procedure has advantages such as using natural products as precursors, employing water as a green solvent, good yields and easy separation of products.

March 14, 2018

Nano-NiZr₄(PO₄)₆ as a superior catalyst for the synthesis of propargylamines under ultrasound irradiation

Hossein Shahbazi-Alavi, Seyed Hadi Nazemzadeh, Abolfazl Ziarati, Javad Safaei-Ghomi

Page range: 185-189

Abstract

An easy and rapid method for the synthesis of propargylamines has been achieved through a three-component reaction of phenylacetylene, aromatic aldehydes, and morpholine or piperidine using nano-NiZr 4 (PO 4 ) 6 under ultrasound irradiation. Atom economy, a wide range of products, excellent yields in short times, reusability of the catalyst, and low catalyst loading are some of the important features of this protocol.

March 14, 2018

Efficient pseudo five-component synthesis of 4,4′-(arylmethylene)-bis(3-methyl-1-phenyl-1H-pyrazol-5-ol) derivatives promoted by a novel ionic liquid catalyst

Zahra Abshirini, Abdolkarim Zare

Page range: 191-195

Abstract

In this research, initial production and characterization of a novel Brønsted-acidic ionic liquid, namely, N , N , N ′, N ′-tetramethylethylenediaminium- N , N ′-disulfonic acid hydrogen sulfate ([TMEDSA][HSO 4 ] 2 ), has been described (characterization was achieved using Fourier-transform infrared spectroscopy, 1 H nuclear magnetic resonance (NMR), 13 C NMR, and mass and thermal gravimetric spectra). Thereafter, utilization of [TMEDSA][HSO 4 ] 2 as a highly effectual catalyst for the synthesis of 4,4′-(arylmethylene)-bis(3-methyl-1-phenyl-1 H -pyrazol-5-ol) derivatives through the one-pot pseudo five-component reaction of phenylhydrazine (2 eq.) with ethyl acetoacetate (2 eq.) and arylaldehydes (1 eq.) in relatively mild conditions, has been reported.

March 15, 2018

Hydrothermal synthesis and crystal structure of a bisupporting Keggin-polyoxometalate hybrid compound decorated with a copper(II) complex unit

Shu Kui Shi, Zhan Guo, Rui Feng, Lin Yu Jin, Yan Bai, Dong Bin Dang

Page range: 197-202

Abstract

A bisupporting Keggin-type polyoxometalate compound, {[Cu II (phen) 2 ] 2 [(HBW 12 O 40 )]}[Cu II Cl 2 (phen)] 2 · 2H 2 O (phen=1,10-phenathroline) ( 1 ), has been synthesized through the hydrothermal method and characterized by IR spectroscopy, elemental analysis, UV/Vis/NIR spectroscopy, and powder and single crystal X-ray diffraction. The bisupporting Keggin-polyoxometalate consists of one Keggin-type [HBW 12 O 40 ] 4− core and two covalently linked copper(II) complex fragments [Cu(phen) 2 ] 2+ . In the crystal structure π···π interactions, C–H···Cl, O–H···Cl, O–H···O and C–H···O hydrogen bonds lead to a three-dimensional supramolecular structure.

March 12, 2018

Synthesis, crystal structure, luminescence and electrochemical properties of a Salamo-type trinuclear cobalt(II) complex

Zong-Li Ren, Jing Hao, Ping Hao, Xiu-Yan Dong, Yang Bai, Wen-Kui Dong

Page range: 203-210

Abstract

A trinuclear Co(II) complex, [{CoL(C 4 H 9 OH)} 2 -(OAc) 2 Co]·C 3 H 7 NO, was synthesized by the reaction of a Salamo-type chelating ligand (H 2 L=4,42′-dinitro-2,2′-[1,2-ethylenedioxybis(nitrilomethylidyne)]diphenol) with cobalt(II) acetate tetrahydrate in n -butanol, and characterized by elemental analyses, X-ray crystallography, FT-IR and UV/Vis spectra. In the Co(II) complex, there are two ligand L 2− units, two μ 2 -acetate ions, two coordinated n -butanol molecules and one non-coordinated N , N -dimethylformamide molecule. The Co(II) atoms in the structure of the Co(II) complex adopt slightly distorted octahedra geometries. Furthermore, through intermolecular C–H···O, O–H···O and C–H···π interactions, infinite layer-like, plane-like and 3D supramolecular structures are constructed. The fluorescence and electrochemical properties of the Co(II) complex have also been investigated.

March 9, 2018

New cholic acid analogs: synthesis and 17β-hydroxydehydrogenase (17β-HSD) inhibition activity

Najim A. Al-Masoudi, Abbas Sami, Nabeel A. Abdul-Rida, Martin Fortscher

Page range: 211-223

Abstract

The 17 β -hydroxysteroid dehydrogenase (17 β -HSD) enzyme family is involved in the biosynthesis of active steroids and its inhibition constitutes an interesting approach for treating estrogen-, androgen-dependent cancers and osteoporosis. In this study, a new series of cholic acid analogs was designed with the goal of improving the biological activity as 17 β -HSD1 and 17 β -HSD2 inhibitors. To this end, 23-cholyl amides 4–7 , 3- O - p -toluenesulfonyl-23-cholyl amides 10–12 , 23-cholyl-carbohydrazide 14 , carbothioamide analog 15 , and 23-cholyl-acylhydrazone derivatives 18–22 were synthesized from cholic acid ( 3 ) via coupling, sulfonation and substitution reactions. Basic treatment of keto group of 5 with p -bromoaniline afforded 8 , meanwhile acidic treatment of 3 with thiosemicarbazide furnished the 23-cholyl-thiadiazole derivative 16 . The synthesized compounds were evaluated for their inhibition activity against 17 β -HSD1 and 17 β -HSD2, and were found inactive at 1.0 μ m concentration (inhibition <10%). However, the steroids 12 , 21 and 22 showed inhibition of 21.1, 23.9 and 21.3%, respectively, against 17 β -HSD2 at the same concentration. Therefore, these steroidal analogs can be further structurally modified to optimize their inhibition activity against 17 β -HSD2 for the development of potential therapeutics.

February 27, 2018

Synthesis, vibrational spectra and single-crystal structure determination of lithium tricyanomethanide Li[C(CN)₃]

Olaf Reckeweg, Maurice Conrad, Armin Schulz, Francis J. DiSalvo, Thomas Schleid

Page range: 225-229

Abstract

The long-elusive structure of lithium tricyanomethanide Li[C(CN) 3 ] has been determined on the basis of material synthesized via a metathesis reaction of Ag[C(CN) 3 ] with LiCl in water driven by AgCl precipitation and subsequently recrystallization from methanol. Li[C(CN) 3 ] crystallizes in the non-centrosymmetric orthorhombic space group Ima 2 with the unit-cell parameters a =751.06(4), b =1059.75(6) and c =563.27(3) pm adopting a unique structure with planar [C(CN) 3 ] − anions exhibiting nearly ideal trigonal planar D 3 h symmetry. The Li + cations are coordinated by five independent tricyanomethanide anions forming a distorted square pyramid with Li–N distances between 202 and 249 pm. The vibrational frequencies were also determined and along with other properties of Li[C(CN) 3 ] compared with those of related compounds.

February 26, 2018

Silber(I)-cyanid-Komplexe mit Aminen und Azaaromaten

Mark Strey, Cindy Döring

Page range: 231-241

Abstract

Silver cyanide can be treated with liquid amines or azaaromatics L to give crystalline complexes of various compositions, among them complexes of the simple type cyanido(amine)silver(I): L =isobutylamine and 4-picoline. Other AgCN: L ratios obtained were: 1:2 (benzylamine and 4-benzylpiperidine), 2:1 (2,4-lutidine), 2:3 (morpholine and 3,4-lutidine) and 3:4 (3,5-lutidine). The packing diagrams were analyzed in terms of Ag–Ag and Ag–CN contacts and N–H ··· N hydrogen bonds. The contacts often give rise to chains, which are sometimes linked to layers by hydrogen bonds.

February 24, 2018

The alkaline earth-palladium-germanides Sr₃Pd₄Ge₄ and BaPdGe

Sebastian Stein, Samir F. Matar, Kai Heinz Schmolke, Jutta Kösters, Rainer Pöttgen

Page range: 243-250

Abstract

The germanides Sr 3 Pd 4 Ge 4 and BaPdGe were obtained from high-temperature reactions in sealed niobium ampoules and their structures have been determined from single-crystal X-ray diffraction data: a =444.2(1), b =438.1(1), c =2472.2(7) pm, space group Immm , U 3 Ni 4 Si 4 type, wR 2=0.0471, 576 unique reflections, 25 parameters for Sr 3 Pd 4 Ge 4 and a =677.09(8), space group P 2 1 3, LaIrSi type, wR 2=0.0322, 409 unique reflections, nine parameters for BaPdGe. Both germanides have pronounced three-dimensional [Pd 4 Ge 4 ] δ − and [PdGe] δ − polyanionic networks with Pd–Ge bonding interactions. This is confirmed by the density functional theory (DFT)-based electronic structure investigations, the trends of charge transfer and crystal orbital overlap population (COOP) analyses.

February 19, 2018

Equiatomic rare earth rhodium plumbides RERhPb (RE=Y, La–Nd, Sm, Gd–Lu) with ZrNiAl-type structure

Lukas Heletta, Rainer Pöttgen

Page range: 251-258

Abstract

The equiatomic plumbides RE RhPb ( RE =Y, La–Nd, Sm, Gd–Lu) were synthesized by induction melting of the elements in sealed niobium ampoules. The samples were characterized by X-ray powder diffraction, confirming their ZrNiAl-type structure, space group P 6̅2 m . Four structures were refined from single-crystal X-ray diffractometer data: a =769.42(5), c =415.60(3) pm, wR =0.0415, 343 F 2 values, 15 variables for LaRhPb, a =767.91(6), c =369.37(4) pm, wR =0.0798, 284 F 2 values, 15 variables for ErRhPb, a =767.01(8), c =366.21(4) pm, wR =0.0380, 341 F 2 values, 15 variables for YbRhPb and a =766.9(1), c =363.42(6) pm, wR =0.0699, 290 F 2 values, 15 variables for LuRhPb. The RE RhPb plumbides contain two crystallographically independent rhodium atoms, both in tricapped trigonal prismatic coordination: Rh1@Pb 3 RE 6 and Rh2@ RE 6 Pb 3 . Short Rh–Pb distances (277 and 284 pm in ErRhPb) are indicative of covalent Rh–Pb bonding. The crystal chemical details of the RE RhPb series are compared with the silver plumbides RE AgPb which show different transition metal-lead coloring. Temperature dependent magnetic susceptibility data show Pauli paramagnetism for YRhPb, LaRhPb and LuRhPb. An antiferromagnetic ground state below the Néel temperatures of 13.5, 21.0 and 6.9 K was found for PrRhPb, TbRhPb and DyRhPb, respectively. HoRhPb exhibits Curie-Weiss behavior in the observed temperature range.

Notes

March 12, 2018

Synthesis and crystal structure of [azido-bis(cis-1,2-diaminocyclohexane)copper(II)] chloride trihydrate

Sidra Nawaz, Muhammad Monim-ul-Mehboob, Muhammad Nawaz Tahir, Irshad Hussain, Habib-ur-Rehman, Syed Zajif Hussain, Saeed Ahmad

Page range: 259-263

Abstract

A new copper(II) complex containing cis -1,2-diaminocyclohexane (Dach) and azide as ligands, [Cu(Dach) 2 (N 3 )]Cl · 3H 2 O ( 1 ), was prepared and characterized by IR spectroscopy, thermal analysis and X-ray crystallography. The structure of 1 consists of a complex cation, [Cu(Dach) 2 (N 3 )] + , a chloride counter-ion and three water molecules. The coordination environment of the copper(II) atom in 1 is distorted square pyramidal attained by four nitrogen atoms of cis -1,2-diaminocyclohexane molecules and an azide ion. Thermogravimetric and differential scanning calorimetric analyses validated the molecular formula of complex 1 .

March 10, 2018

A Co(II) complex from a pyridylamide ligand: synthesis and structural characterization

Xiao-Hong Zhu, Ding-Yun Jiang, Tao Hu, Deng-Hao Li

Page range: 265-268

Abstract

The hydrothermal reaction of N 3 ,N 5 -di(pyridin-4-yl)pyridine-3,5-dicarboxamide (L) with Co(NO 3 ) 2 ·6H 2 O and ErCl 3 ·6H 2 O yields a new complex, {[Co(L) 2 (NO 3 ) 1.15 (Cl) 0.85 ]·4DMF} n ( 1 ). Complex 1 has been characterized by single-crystal and powder X-ray diffraction, IR, and elemental and thermogravimetric analysis. It crystallizes in the orthorhombic space group Fddd and shows a chain structure.

About this journal

Objective
Zeitschrift fuer Naturforschung B (ZNB) publishes novel research in all areas of inorganic chemistry, organic chemistry, and analytical chemistry. In particular, the journal focuses on solid state chemistry, coordination chemistry, main group element chemistry, synthetic organic chemistry, natural product chemistry and, to a lesser extent, on analytical chemistry. For more than 65 years Zeitschrift fuer Naturforschung B has been open to contributions from all fields of experimental and theoretical chemistry. Zeitschrift fuer Naturforschung B publishes 12 issues per volume/year. Sometimes double issues occur.

Topics

Solid state chemistry
Coordination chemistry
Main group element chemistry
Organic chemistry
Natural product chemistry

Article formats
Original (full) papers, research notes and preliminary communications, reports on specific research topics of current interest (reviews)

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Volume 73 Issue 3-4

Issue of Zeitschrift für Naturforschung B

Frontmatter

In this Issue

Does Lewis basicity correlate with catalytic performance in zerovalent group 8 complexes?

Abstract

Crystal structure and luminescence properties of a new dinuclear bismuth(III) coordination polymer containing three types of ligands

Abstract

Syntheses, structures, and catalytic properties of two arene-ruthenium(II) complexes bearing N-(2-pyridinyl)aminodiphenylphosphine sulfide ligands

Abstract

Synthesis, characterization, anticancer and antimicrobial study of arene ruthenium(II) complexes with 1,2,4-triazole ligands containing an α-diimine moiety

Abstract

Green synthesis of α-aminophosphonates using ZnO nanoparticles as an efficient catalyst

Abstract

Nano-NiZr4(PO4)6 as a superior catalyst for the synthesis of propargylamines under ultrasound irradiation

Abstract

Efficient pseudo five-component synthesis of 4,4′-(arylmethylene)-bis(3-methyl-1-phenyl-1H-pyrazol-5-ol) derivatives promoted by a novel ionic liquid catalyst

Abstract

Hydrothermal synthesis and crystal structure of a bisupporting Keggin-polyoxometalate hybrid compound decorated with a copper(II) complex unit

Abstract

Synthesis, crystal structure, luminescence and electrochemical properties of a Salamo-type trinuclear cobalt(II) complex

Abstract

New cholic acid analogs: synthesis and 17β-hydroxydehydrogenase (17β-HSD) inhibition activity

Abstract

Synthesis, vibrational spectra and single-crystal structure determination of lithium tricyanomethanide Li[C(CN)3]

Abstract

Silber(I)-cyanid-Komplexe mit Aminen und Azaaromaten

Abstract

The alkaline earth-palladium-germanides Sr3Pd4Ge4 and BaPdGe

Abstract

Equiatomic rare earth rhodium plumbides RERhPb (RE=Y, La–Nd, Sm, Gd–Lu) with ZrNiAl-type structure

Abstract

Synthesis and crystal structure of [azido-bis(cis-1,2-diaminocyclohexane)copper(II)] chloride trihydrate

Abstract

A Co(II) complex from a pyridylamide ligand: synthesis and structural characterization

Abstract

Nano-NiZr₄(PO₄)₆ as a superior catalyst for the synthesis of propargylamines under ultrasound irradiation

Synthesis, vibrational spectra and single-crystal structure determination of lithium tricyanomethanide Li[C(CN)₃]

The alkaline earth-palladium-germanides Sr₃Pd₄Ge₄ and BaPdGe