bluuebunny/crossref_metadata_2025 huggingface dataset:
Secondary Bonding Interactionsi in Some Di- and Trihaloanilinium Halides
Authors: López-Duplá Esperanza , Jones Peter G. , Vancea Fabiola
Published: August 2018

Six solvent-free structures of di- and trihaloanilinium halides are presented. All involve clearly defined hydrophilic regions built up from classical hydrogen bonding systems. The 2,4-dibromo-, 2,6- dichloro-, 2,4,6-trichloro- and 2,4,6-tribromoanilinium derivatives form ribbon structures involving annelated R2
4 (8) rings with NH2 donors (two hydrogens from the positively charged NH3 groups) and halide acceptors. The 2,5-dibromo- and 2,4,5-trichloro derivatives form layers with two types of ring, R2
4 (8) and R4
8 (16). All structures also involve other secondary interactions (C-H. . . X hydrogen bonds and/or X. . . X contacts, X = halogen), some of which link the ribbons or layers into a second or third dimension. The shortest X. . . X contacts generally involve the anions. In the 2,4-dibromo, 2,4,6-trichloro and tribromo derivatives, somewhat more extensive halogen aggregates (triangles, angled X3 or X4 chains) are formed between neutral halogens. In two appendices, the packing patterns of (I) the disordered structure 3,4,5-trichloroanilinium chloride and (II) the known structures of unsubstituted anilinium halides are briefly presented.
Simple Synthesis, Characterization and Structure of Diorganotin(IV) Complexes Containing the N-(2-Salicylidene)-N'-benzoylhydrazone Ligand
Authors: Dey Dilip Kumar , Samanta Brajagopal , Lycka Antonin , Dahlenburg Lutz
Published: August 2018

Two diorganotin(IV) complexes of general formula R2Sn[2-OC6H4CH=NDN=C(O)Ph] (R = Ph, 1; R = Me, 2) have been synthesized from the corresponding diorganotin(IV) dichloride and the Schiff base derived from salicylaldehyde and benzoyl hydrazide. The two compounds have been characterized by elemental analysis, IR and NMR (1H, 13C, 15N, 119Sn) spectra, and their structures have been confirmed by single crystal X-ray structure analysis. Crystals of complex 1 re triclinic, space group P1̄ , a = 11.1631(5), b = 13.462(2), c = 16.511(1) Å , α = 106.193(9), β = 106.379(8), γ = 94.932(8)°, Z = 4, R1 = 0.0461, wR2 = 0.0939 for 13194 unique reflections. Crystals of 2 are monoclinic, space group P21, a = 10.2073(5), b = 14.645(2), c = 10.411(3) Å, β = 92.572(9)°, Z = 4, R1 = 0.0395, wR2 = 0.0835 for 5050 unique reflections. The central tin atom of either complex adopts a distorted trigonal bipyramidal coordination with two ligand oxygen atoms in axial positions, the nitrogen atom of the ligand and two organic groups on tin occupying equatorial sites. The δ(119Sn) values for the complexes 1 and 2 are -329.2 and -150.3, respectively, thus indicating penta-coordinated tin centres.
Organoaluminium and -Gallium Compounds with O-Oximato Substituents
Authors: Mitzel Norbert W. , Lustig Christian , Woski Markus
Published: August 2018

The organoaluminium and -gallium acetonoximates (tBu2MON=CMe2)2 (M = Al, Ga) have been prepared by the reaction of acetoneoxime with tri-tert-butylaluminium and -gallium. The compounds (Me2MON=CMe2)2 (M = Al, Ga), described previously, were synthesized for comparison. All compounds have been characterised by NMR spectroscopy (1H, 13C, 27Al), by mass spectrometry and elemental analyses. The crystal structures of the four compounds have been determined, and it was shown that all form dimers with six-membered M2O2N2 rings by aggregation through the imino N atoms. The compounds (Me2MON= CMe2)2 adopt boat conformations, whereas the compounds (tBu2MON=CMe2)2 prefer chair conformations. Large differences in the M-O-N angles have been found between the methyl and the tert-butyl analogues.
Cu(II) Ion-Selective Electrodes Based on Cu(II) Complex with Cyclized Salophen
Authors: Al-Saraj Manal R. , Saadeh Salman M. , Abdel-Latif Monzir S.
Published: August 2018

Several versions of Cu(II) ion selective electrodes (ISE), based on cyclized N,N'-bis(salicylidene)-o-phenylenediamine (salophen) complexes with Cu(II), were fabricated for determination of Cu(II) in aqueous solutions. The response of the ISE was optimized by variation of membrane composition and evaluation of various experimental conditions. Near Nernstian slopes (~ 28-32 mV/decade) were obtained for some preparations. The linear range of the ISE ranged from 5 × 10-5 to 1 × 10-2
M Cu(II). Coated-wire and coated disc ISE resulted practically in a similar response as screen printed electrodes (SPE). The potentiometric selectivity coefficients (Kij) for all electrodes were determined for Na+, NH4
+, Ca2+, Mg2+, Ni2+, Pb2+, Zn2+, Cd2+, Co2+, Fe3+, Hg2+, CO3
2-, H2PO4
-, HPO4
2-, SO4
2-, CH3COO-, Br-, I-, NO3
-, and SCN-. The selectivity coefficients were in the range from 10-2 to 10-3 for all ions tested except Hg2+, I-, and to less extent Fe3+. Fabricated ISE using the Cu(II)-salophen complex are reliable and stable.
Zu den pseudobinären Zustandssystemen Bi2Ch3-BiX3 und den ternären Phasen auf diesen Schnitten (Ch = S, Se, Te; X = Cl, Br, I), I: Bismutsulfidhalogenide/The Pseudobinary Systems Bi2Ch3-BiX3 and the Ternary Phases on their Boundary Lines (Ch = S, Se, Te; X = Cl, Br, I), I: Bismuth Sulfide Halides
Authors: Oppermann Heinrich , Petasch Uwe
Published: August 2018

The phase diagrams of the systems Bi2S3-BiX3 were constructed from results of DTA and total pressure measurements and x-ray analysis. The phases: BiSCl, Bi4S5Cl2 and Bi19S27Cl3 for X = Cl; BiSBr and Bi19S27Br3 for X = Br; BiSI and Bi19S27I3 for X = I exist on the boundary lines. The enthalpies of formation and standard entropies of the phases follow from the coexistence decomposition pressure functions. The data are:

ΔH°B(BiSClf,298) =−49,6 ± 1,6 kcal/mol S°(BiSClf,298) = 30,3 ± 2,5 cal/K·mol

ΔH°B(Bi4S5Cl2,f,298) =−144,4 ± 3 kcal/mol S°(Bi4S5Cl2,f,298) = 114,0 ± 4,6 cal/K·mol

ΔH°B(Bi19S27Cl3,f,298) = −520 ± 10 kcal/mol S°(Bi19S27Cl3,f,298) = 490 ± 10 cal/K·mol

ΔH°B(BiSBrf,298) = −40,2 ± 1,4 kcal/mol S°(BiSBrf,298) = 32,0 ± 3 cal/K·mol

ΔH°B(Bi19S27Br3,f,298) = −493,6 ± 6,7 kcal/mol S°(Bi19S27Br3,f,298) = 499,8 ± 17 cal/K·mol

ΔH°B(BiSIf,298) =−27,8 ± 1,4 kcal/mol S°(BiSIf,298) = 36,1 ± 2,5 cal/K·mol

ΔH°B(Bi19S27I3,f,298) =−464,4 ± 15 kcal/mol S°(Bi19S27I3,f,298) = 502,7 ± 15 cal/K·mol
Ligand Properties of Tri(2-thienyl)- and Tri(2-furyl)phosphine and -arsine (2-C4H3E)3P/As (E = O, S) in Gold(I) Complexes
Authors: Monkowius Uwe , Nogai Stefan , Schmidbaur Hubert
Published: August 2018

Tri(2-thienyl)- and tri(2-furyl)phosphine and -arsine (L) have been introduced as ligands to gold(I) chloride and acetate (AuX). Structural studies have shown that in the 1:1 complexes of the type L-Au-X the gold atoms are bound exclusively to the phosphorus/arsenic centers without any intraor intermolecular approach of the donor atoms of the three heterocycles towards the metal atoms. Intermolecular aurophilic bonding is found in the crystals of the [tri(thienyl)phosphine]gold acetate complex, but is absent in crystals of the chloride complexes. The phosphines L have been quaternized with methyl iodide and the resulting phosphonium salts [LMe]I structurally characterized to provide reference data as to the preferred configurational and conformational motifs. The mass spectra of the gold complexes indicate a high stability of the dinuclear cationic species [(LAu)2X]+ with X = Cl, OAc for all ligands L.
Regioselective Glycosylation of Glucosamine and Galactosamine Derivates Using O-Pivaloyl Galactosyl Donors
Authors: Oßwald Mathia , Lang Uwe , Friedrich-Bochnitschek Siglinde , Pfrengle Waldemar , Kunz Horst
Published: August 2018

Penta-O-pivaloyl-galactopyranose and tetra-O-pivaloyl-galactopyranosyl bromide after electrophilic activation reacted with 6-O-protected 2-azido-galactosides to give the precursor structures of the Thomsen-Friedenreich antigen disaccharide with high regioselectivity, but low yield.With 4,6-Obenzylidene protected 2-azidogalactosides and 2-O-pivaloyl phenylthio galactosides, T-antigen disaccharides of this type were obtained in good yields. Glycosylation reactions of 4,6-O-benzylidene protected glucosamine derivatives with O-pivaloyl protected galactosyl bromide efficiently gave lactolactosamine disaccharides. Even a thioglycoside was efficiently galactosylated by this method resulting in the formation of a disaccharide thioglycoside useful itself as a potential glycosyl donor.
Guest-Host Systems of 1,3,5-Tristyrylbenzenes
Authors: Meier Herbert , Karpouk Elena , Lehmann Matthias , Schollmeyer Dieter , Enkelmann Volker
Published: August 2018

(E,E,E)-1,3,5-Tris(3,4,5-trimethoxystyryl)benzene (1a) forms monoclinic crystals of the space group P21/c. Incorporation of three transoid diacetyl guest molecules between the three arms leads to triclinic crystals of the space group P1. The styryl groups, originally present in a nonsymmetrical conformation, are simultaneously transformed to a C3 arrangement. (E,E,E)-1,3,5-Tris- (3,4,5-tripropoxystyryl)benzene (1b) forms monoclinic crystals of the space group P21/c. The C3 arrangement of the styryl groups is present in the first, the unsymmetrical arrangement in the second modification. Incorporation of two acetone guests in the largest and the middle-sized angle space between the styryl arms in the unsymmetrical arrangement, leads to monoclinic crystals of the space group P21/n. The third (smallest) angle space is filled with a propoxy chain of the neighboring molecule. The pure host crystals show significant deviations from planarity which are strongly reduced by the incorporation of the guest molecules.
Synthesis of Some New Chiral Tricyclic and Macrocyclic Pyridine Derivatives as Antimicrobial Agents
Authors: Amr Abd El-Galil E. , Mohamed Ashraf M. , Ibrahim Alhussein A.
Published: August 2018

A series of chiral macrocyclic pyridines has been prepared starting from N2,N2-(pyridine- 2,6-dicarbonyl)diamino acid hydrazides (2a-c) and N,N-bis-(1-carboxy-2-substituted)-2,6- diaminocarbonyl)pyridines (3a,b). The coupling of (2a-c) with 2,6-pyridine dicarbonyldichloride (4) gave the compounds (5a-c). Compounds 2a-c were coupled with 2,6-diacetylpyridine (6) to yield compounds (7a-c) and with heterocyclic aldehydes (8) or (10) to give the compounds (9a-c) or (11a-c). In addition, the hydrazides (2a-c) were reacted with diformylcalix[4]arene 12 to afford the macrocyclic calix[4]arene hydrazone derivatives (13a-c) in reasonable yields. Finally, reaction of diaminocalix-[4]arene derivatives (14a,b) with hydrazides 2a,b or acids (3a,b), using azide or mixed anhydride methods afforded macrocyclic calix[4]arene derivatives 15a,b and 16a,b, respectively. The structure assignments of the new compounds are based on chemical and spectroscopic evidence. The biological activity screening tests showed that many of the obtained compounds exhibit high antimicrobial activity comparable to ampicillin and chloramphenicol which are used as reference compounds.
Neue Strukturverfeinerung und Eigenschaften von Cr3C2/Structure Refinement and Properties of Cr3C2
Authors: Glaser Jochen , Schmitt Ruth , Meyer H.-Jürgen
Published: August 2018

Cr3C2 was obtained from arc-melting of pellets made of carbon and chromium. The structure of Cr3C2 was determined by single crystal X-ray diffraction (Pnma, Z = 4, a = 553.99(6), b = 283.27(4), c = 1149.4(1) pm, R1 = 0.019 and wR2 = 0.037 for all collected reflections). The crystal structure contains isolated carbon atoms which reside inside of trigonal prismatic voids of metal atoms. The compound exhibits temperature independent paramagnetism. The electronic structure of Cr3C2 has been investigated using extended Hückel calculations.
Crystal Structure of Eu2PdSi3
Authors: Rodewald U. Ch. , Hoffmann R.-D. , Pöttgen R. , Sampathkumaran E.V.
Published: August 2018

Single crystals of Eu2PdSi3 were obtained from an arc-melted sample that was further annealed at 1020 K for seven days in a silica tube. The structure of Eu2PdSi3 was refined from single crystal X-ray diffractometer data: P6/mmm, a = 831.88(12), c = 435.88(9) pm, wR2 = 0.1175, 265 F2 values, and 13 variable parameters. It crystallizes with the U2RuSi3 structure, a superstructure of the AlB2 type. The palladium and silicon atoms form a planar two-dimensional [PdSi3] network. The two crystallographically different europium atoms have hexagonal prismatic coordinations Eu1Si12 and Eu2Pd4Si8. The Pd-Si and Si-Si distances within the [PdSi3] network are 244 and 236 pm, respectively.
Reduktion von Isochinolin und Indol mit Cäsium in flüssigem Ammoniak / Reduction of Isoquinoline and Indole with Cesium in Liquid Ammonia
Authors: Suchentrunk Christof , Korber Nikolaus
Published: August 2018

Isoquinoline and indole were reduced with solutions of cesium in liquid ammonia and the resulting crystalline compounds isolated as ammonia-rich solvate crystals. The reduction of isoquinoline yields the anion bisisoquinoline-2,2’-diide in the compound Cs2C18H14N2 · (7/2) NH3 as the result of a coupling reaction. Indole is reduced to the 5,8-dihydroindolide anion in the ammoniate CsC8H8N · 3NH3. Both anions display interactions between their aromatic π-systems and the cesium cations.
Synthesis and Liquid Crystalline Properties of Novel Imides and Thioimides with Chiral Aliphatic Tails
Authors: Orzeszko Andrzej , Melon-Ksyta Dorota , Kowalczyk Ewa , Czupryński Krzysztof
Published: August 2018

Three chiral compounds (R)-octan-2-ol, (S)-citronellol and (S)-citronellyl bromide were used for the synthesis of novel ester imides with biphenyl moieties as mesogenic units. Observations by means of polarising microscopy as well as DSC measurements revealed the presence of SmC* and/or SmA phases for all the compounds examined. It was found that the biphenyl units with long chiral alkoxy substituents induce smectic C phases.
Transfer of the Fluorous Biphasic Concept to the Palladium-Catalyzed Addition Polymerization of Norbornene
Authors: Lassahn Paul-Gerhard , Tzschucke Christoph , Bannwarth Willi , Janiaka Christoph
Published: August 2018

Two perfluorinated palladium(II) pre-catalysts of the type (ArF
3P)2PdCl2 (ArF = m-C8F17-C2H4- C6H4 - and p-C7F15-CH2-O-C6H4-) could be highly activated with the co-catalyst B(C6F5)3/AlEt3 or methylalumoxane (MAO) for the vinyl/addition polymerization of norbornene. Their recycling was studied by using the FBS concept (Fluorous Biphasic System).
Zur Kenntnis rhomboedrischer Perowskite (La,Sr)(Mn,Fe)O3/Contributions to the Chemistry of Rhombohedral Perovskites (La,Sr)(Mn,Fe)O3
Authors: Börger Alexander , Langbein Hubert
Published: August 2018

Perovskites La1−xSrxMn1−xFexO3+δ (x = 0.1 - 0.5) were prepared by a freeze-drying method and for comparison by conventional solid state reaction. Freeze-dried precursors are more reactive, forming the final perovskites at lower temperatures and within shorter reaction times. Under the reaction conditions employed (air atmosphere, 800 - 1350 °C), the perovskite La0.9Sr0.1Mn0.9Fe0.1O3 was obtained in an orthorhombic modification. By annealing under oxygen at 800 °C, however, a rhombohedral modification La0.9Sr0.1Mn0.9Fe0.1O3.1 with an excess oxygen content can be prepared. The structures of the other perovskites of the series (x = 0.2 - 0.5) were refiṉed on the assumption of a rhombohedral distortion of the ideal perovskite structure (space group R3c). There are characteristic correlations between composition of samples, volume and distortion of the AO12- and BO6-polyhedra in the ABO3 structure.
Amine and Imine Nitrogen Atoms of a New Schiff Base Type Ligand Simultaneously Coordinated to a Dinuclear Mn2O2 Core
Authors: Seoka Won K. , Karaghiosoff Konstantin , Klapötkeb Thomas M. , Mayer Peter
Published: August 2018

The dinuclear Mn(IV) complex [Mn(C-X-salpn)(μ-O)]2·Me2CO (H2salpn=N,N’-bis(salicylidene)- 1,3-diaminopropane and X = CH2C(=O)CH3) crystallizes in the monoclinic space group C2/c with a = 27.388(6), b = 10.388(2), c = 19.797(4) Å , β = 133.11(3)°, V = 4111(1) Å3 and Z = 4. It contains a new Schiff base type ligand, which is related to salpn by the addition of acetone to one of the two C=N moieties. Main feature of the centrosymmetric structure is a planar Mn2O2 four-membered ring. The coordination environment of the manganese atoms is roughly octahedral comprising two phenolic oxygen atoms as well as two amine and two imine nitrogen atoms of the ligand. The Mn···Mn distance is 2.740(8) Å and the Mn-O-Mn bridging angle amounts to 97.2(1)°.
A New Tetranortriterpenoid from Dysoxylum lenticellatum
Authors: Qi Shu-Hua , Wub Da-Gang , Zhang Si , Luo Xiao-Dong
Published: August 2018

A new tetranortriterpenoid, named lenticellatumin (1), three known terpenoids, dysoxylumin C (2), eichlerianic acid (3) and dysoxylumin F (4), together with three ceramides, 1-O-β -D-glucopyranosyl-( 2S,3S,4R,8Z)-2-N-(2’-hydroxytetracosanoyl) octadecasphinga-8-ene (5), (2S,3S,4R,8E)-2- N-(2’-hydroxytetracosanoyl) octadecasphinga-8-ene (6), (2S,3R,4E)-2-N-(2’-hydroxytetracosanoyl) octadecasphinga-4-ene (7), were isolated from the twig of Dysoxylum lenticellatum. Their structures were determined from spectroscopic analysis. Activity screening showed that compound 5 exhibited strong antifeedant activity against pieris brassicae L., while 6, 7 displayed weak activities.
Synthesis and Spectroscopy of LiClO4 Complexes of (–)-Sparteine, 2-Methyl- and 2-Oxosparteine, and 2-Cyano-2-methylsparteine
Authors: Jasiewicz Beata , Rafałowicz Tomasz , Sikorska Ewa , Khmelinskii Igor , Koput Jacek , Sikorski Marek , Boczoń Władysław
Published: August 2018

Complexes formed between (-)-sparteine, 2-methyl- and 2-oxosparteine and 2-cyano-2- methylsparteine with lithium perchlorate (LiClO4) were obtained in the solid state. The complexes, C15H26N2LiClO4, C16H28N2LiClO4, C15H24N2OLiClO4, and C17H27N3Li2Cl2O8 have been isolated and characterised by UV/vis, NMR, and IR, spectroscopy and by their mass spectra. Three of the four complexes present the 1:1 stoichiometry, while the 2-cyano-2-methylsparteine complex has the 1:2 stoichiometry.
Synthesis and Characterization of N-Methyl-Substituted Germocanes. Crystal Structure of MeN(CH2CH2O)2GeBr2
Authors: Karlov Sergey S. , Yakubova Elmira Kh. , Gauchenova Ekaterina V. , Selina Anastasia A. , Churakov Andrei V. , Howard Judith A. K. , Tyurin Daniil A. , Lorberth Jörg , Zaitseva Galina S.
Published: August 2018

The reaction of GeHal4 with MeN(CH2CH2OSiMe3)2 affords dihalogermocanes MeN(CH2 CH2O)2GeHal2 (1, Hal = Br; 2, Hal = Cl). Treatment of Me2Ge(NMe2)2 with MeN(CH2CH2OH)2 leads to dimethylgermocane MeN(CH2CH2O)2GeMe2 (3). The composition and structure of 1-3 were established by elemental analyses, 1H, 13C NMR spectroscopy, and mass spectrometry. The crystal structure of 1 is reported; structural data obtained from geometry DFT optimization on 1 are in good agreement with experimental results. Values of the electron density in the N→Ge bond critical point and the Laplacian of charge density for 1-3 indicate a closed-shell interaction between the Ge and N atoms.
Molecular Structure and Thermal Analysis of Potassium Hydrogenphthalate Monohydrate
Authors: Li Yu-Feng , Zhang Tong-Lai , Zhang Jian-Guo , Yu Kai-Bei
Published: August 2018

Single crystals of potassium hydrogenphthalate monohydrate, KHPhth(H2O), were grown from aqueous solution using a slow cooling method and the structure was determined by X-ray diffraction analysis. The crystals belong to the monoclinic space group P21/c. Its unit cell parameters are as follows: a = 1.1235(1), b = 0.6689(1), c = 1.1998(2) nm, β = 98.85°, V = 0.8909(1) nm3, Dc = 1.657 g/cm3, Z = 4, F(000) = 456. The thermal decomposition of the complex was studied using differential scanning calorimetry (DSC), thermogravimetry-derivative thermogravimetry (TGGTG) and FT-IR techniques. With a linear heat rate, the diagrams show three endothermic processes. RCOOK and K2CO3 are produced at 330 and 467°C, respectively, according to FT-IR analysis.
Kinetics of Oxidation of Benzaldehydes by Quinolinium Dichromate
Authors: Medien Hesham A. A.
Published: August 2018

Quinolinium dichromate (QDC) in sulfuric acid oxidizes benzaldehydes to the corresponding acids in a 50% (v/v) acetic acid-water medium. The reaction is first order each in [QDC], [substrate] and [H+]. The reaction rates have been determined at different temperatures and the activation parameters calculated. The rate decreases with an increase in the water content of the medium. The effects of substituents have been studied. A suitable mechanism is proposed.
Synthesis and Enzymatic Evaluation of Nucleosides Derived from 5-Iodo-2’-Halo-2’-Deoxyuridines
Authors: Kniess Torsten , Grote Michaela , Noll Bernhard , Johannsen Bernd
Published: August 2018

The synthesis of new nucleosides by alkenylation of 5-iodo-2’-halo-2’-deoxyuridines with E-(1-tributylstannyl)-propene-1-ol via STILLE-coupling is described. The new compounds are characterized by 1H NMR and elemental analysis. All nucleosides are evaluated by an enzymatic assay to be substrates of herpes simplex virus type 1 thymidine kinase (HSV-1 TK) and compared with uridine, thymidine and (E)-5-(2-iodovinyl)-2’-fluoro-2’-deoxyuridine (IVFRU).
Polysulfonylamine, CLXVII [1]. Wasserstoffbrücken in kristallinen Onium-dimesylamiden: Ein robustes Dreipunktmuster als Bestandteil eines 2D-, eines zweifach verwobenen 2D- und eines 3D-Wasserstoffbrücken-Netzwerks / Polysulfonylamines, CLXVII [1]. Hydrogen Bonding in Crystalline Onium Dimesylamides: A Robust Three-Point Pattern Integrated into a 2D, a Twofold Interwoven 2D, or a 3D Hydrogen-Bond Network
Authors: Wijaya Karna , Moers Oliver , Blaschette Armand , Jones Peter G.
Published: August 2018

As an exercise in crystal engineering, preparations and low-temperature X-ray structures are reported for three ionic solids of general formula BH+(MeSO2)2N−, where BH+ is 2,4,6- triaminopyrimidinium (compound 1, triclinic, space group P1, Z = 2), 2,6-diaminopyridinium (2, monoclinic, C2/c, Z = 8), or 2,4-diaminopyrimidin-6(1H)-on-3-ium (3, monoclinic, P21/c, Z = 4). As a common feature, the onium cations in question exhibit a trifunctional hydrogen-bond donor sequence H-N-C-N(H)-C-N-H that is complementary to a W-shaped O-S-N-S-O fragment of the anion. Consequently, each structure displays a [DDD:AAA] three-point hydrogen-bond pattern formed by two lateral N-H···O bonds and a central N-H···N interaction. This grouping is integrated as a robust supramolecular synthon into two-dimensional (1, 2) or three-dimensional (3) hydrogen-bond networks, in which all good donors and all good acceptors are involved (excepting one S=O group in 2). In structure 1, the approximately planar cation-anion layers are perfect mosaics composed of 6-membered pyrimidine heterocycles and seven crystallographically independent types of 8-, 10-, 12- or 24-membered rings based upon hydrogen bonding. In contrast, the corresponding layers in structure 2 are marred by large 40-membered voids; in order to achieve dense packing, the imperfect layers adopt a strongly corrugated shape and interpenetrate to form twofold interwoven and nearly planar double-layers. Each structure features close C-H···O contacts consistent with weak hydrogen bonding; in the layer structures 1 and 2, some of these interactions serve as links between adjacent or interwoven layers.
Molecular Structure and Reactivity of Tri(1-cyclohepta-2,4,6-trienyl)amine, N(C7H7)3
Authors: Herberhold Max , Liu Jinnan , Milius Wolfgang
Published: August 2018

Compared with the tertiary phosphane P(C7H7)3 (1), the amine N(C7H7)3 (2) possesses the structure of a flattened trigonal pyramid with a sum of CNC angles of 350.0° (cf. 300.2° (av.) in 1). The heteroatom (with the lone pair) is situated 27.0 pm above the C3 basal plane in 2, but 86.4 pm in 1. The amines N(C7H7)3 (2), NH(C7H7)2 (2a) and N(Ph)(C7H7)2 (2b) react with tropylium tetrafluoroborate, [C7H7]BF4, to give N-tropylidene-(1-cyclohepta-2,4,6-trienyl)-immonium tetrafluoroborates, [(C7H6)N(R)(C7H7)]BF4 3 (R = H, from 2 and 2a), 4 (R = Ph, from 2b), which have been characterized by their IR and NMR (1H, 13C) spectra.
Synthese und Kristallstrukturanalyse eines 2,4-Diaryl-2,3-dihydro-1H-1,5-benzodiazepins / Synthesis and Crystal Structure Analysis of a 2,4-Diaryl-2,3-dihydro-1H-1,5-benzodiazepine
Authors: Hormaza Angelina , Schollmeyer Dieter , Meier Herbert
Published: August 2018

The enone unit of chalcones is a synthetically valuable substructure for the formation of heterocycles. Whereas propoxy groups as solubilizing side chains on the phenyl groups do not much affect the generation of pyrazole and pyridine rings, they reduce significantly the yield of the diazepine ring system 4. We attribute this effect to the large twist angles between the ring planes, which are demonstrated by a crystal structure analysis.
Synthesis of Highly Flexible Difluorinated Cyclopropanoid Nucleoside Analogues
Authors: Csuk René , Eversmann Leo
Published: August 2018

A novel class of (difluorocyclopropyl)propyl nucleoside analogues containing a propyl spacer between the cyclopropane moiety and the heterocycle has been prepared in an easy sequence.
Structure of trans-Isoshinanolone in the Crystal and in Solution
Authors: Bringmann Gerhard , Pfeifer Robert-Michael , Breuning Matthias , Reichert Matthias , Messer Kim , Schraut Michaela , Tóth Gabor
Published: August 2018

The first X-ray structure analysis of authentic, not derivatized (racemic) trans-isoshinanolone, a wide-spread acetogenic tetralone, is described. In the crystal, two slightly different conformers are found, along with the corresponding enantiomers. The ‘homomeric’ conformers differ by their H-bonding interactions with the respective neighboring molecules. Rows of a single enantiomeric species, but with the two conformers linked ‘head-to-head’, ‘tail-to-tail’, are surrounded by four analogous rows of the corresponding enantiomers. Apparently the interactions between these heterochiral rows are the reason for the enhanced crystallization tendency of the racemate as compared to that of enantiomerically pure isoshinanolone. The structures in the crystal are compared with those calculated (gas phase) and with the structure in solution.
Fascicularones C and D, Tricyclo[5.4.0.02.5]undecane Sesquiterpenoids from the Liquid Culture of Naematoloma fasciculare
Authors: Shiono Yoshihito , Wakamatsu Hiroko , Murayama Tetsuya , Ikeda Michimasa
Published: August 2018

Two novel sesquiterpenoids of tricyclo[5.4.0.02.5]undecane skeleton, fascicularones C (5) and D (6) have been isolated from liquid culture of a poisonous mushroom, Naematoloma fasciculare. Their structures were elucidated on the basis of spectroscopic methods. Compounds 5 and 6 promoted radicle elongation of lettuce seedling.
Carbamoyl and Thiocarbamoyl Derivatives of 3-Aminopropyl-dimethyl-phosphine Oxide
Authors: Lachkova Victoria , Keck Helmut , Scopelliti Rosario , Kläui Wolfgang , Varbanov Sabi , Hägele Gerhard
Published: August 2018

A series of fourteen new 3-[N-substituted carbamoyl (or thiocarbamoyl)]-aminopropyl-dimethyl-phosphine oxides have been synthesized and characterized. The compounds were prepared via reaction of the 3-aminopropyl-dimethyl-phosphine oxide with the corresponding isocyanates or isothiocyanates. The composition of the compounds was proved by elemental analysis and the structures were confirmed by IR, 1H, 31P, 31P{1H} NMR spectroscopy and by mass spectrometry. The structures of 3[(N-phenyl-thiocarbamoyl)amino]propyl-dimethyl-phosphine oxide (5), 3[(N-4- chlorophenyl-thiocarbamoyl)amino]propyl-dimethyl-phosphine oxide (6), and 3[(N-benzyl-thiocarbamoyl) amino]propyl-dimethyl-phosphine oxide (9) have been confirmed by X-ray diffraction.
A Conformational Analysis of the Spirocyclic Quaternary Ammonium Cation [(CH2)4N(CH2)4]+ in its Bromide and Picrate Salts
Authors: Monkowius Uwe , Nogai Stefan , Schmidbaur Hubert
Published: August 2018

High-yield syntheses of the bromide (1a) and picrate salts (1b) of the 5-azonia-spiro[4]nonane cation [(CH2)4N(CH2)4]+ are reported. In the single crystal X-ray diffraction analyses of the two salts the spirocyclic quaternary ammonium cations have their five-membered rings in envelop and twist conformations modified by packing forces. The conformation found experimentally for 1a has C2-symmetry as predicted for the gas phase by quantum-chemical calculations (RI-DFT, RI-MP2), but the five-membered rings are intermediate between the expected envelop and the twist form. For 1b, both of the two independent cations can be described as a combination of rings in an envelop and a twist conformation. According to the NMR spectra, in solution the cations are highly flexible and pseudosymmetrical (point group D2d)
A Speculative Discussion of the Structural Details of 1-Bromo-2-iodo-benzenes
Authors: Schmidbaur Hubert , Minge Oliver , Nogai Stefan
Published: August 2018

The crystal and molecular structures of 2,4-dibromo-1-iodo-benzene (1) and 1,3-dibromo-2-iodobenzene (2) have been determined by single crystal X-ray diffraction. The proximity of two or three large halogen substituents (Br/I) induces only minor distortions of the C-C-Br/I angles (ca. 2°) and the halogen atoms remain in the plane of the molecules. These undistorted structures lead to short intramolecular, sub-van-der-Waals Br-I contacts [in the range 3.465(4) to 3.530(4) Å ]. The results suggest that the peripheral Br-I interactions have an attractive component which alleviates the repulsion out of steric crowding. The influence is associated with an absorption in the visible region and is possibly responsible for the enhanced reactivity of the 1,2-dihalobenzene molecules
Die Reaktion von Phenylpentazol mit n-Butyllithium. Synthese von 1,1-Di-n-butyl-2-phenylhydrazin / The Reaction of Phenylpentazole with n-Butyl Lithium. Synthesis of 1,1-Di-n-butyl-2-phenylhydrazine
Authors: Biesemeier Frank , Müller Ulrich
Published: August 2018

The reaction of phenylpentazole, C6H5-cyclo-N5, with n-butyl lithium in tetrahydrofuran or in diethylether does not yield a lithium pentazolide such as Li(THF)4
+N5−. Instead, a mixture of several primary products is obtained, which probably include lithium 1-n-butyl-5-phenyl-pentaazadienide, Li+[n-C4H9− N=N−N−N=N−C6H5]− and di-n-butyl-phenylhydrazide, Li+[(n-C4H9)2N−N−C6H5]−. After hydrolysis 1,1-di-n- butyl-2-phenylhydrazine, (n- C4H9)2N−NH−C6H5, is ob- tained with good yield. This compound is an oil that was characterized by NMR, mass and IR spectroscopy
Synthesis of the Four Diastereoisomers of the N-Terminal Amino Acids of Nikkomycins via Aminoalkylation with Preformed Ternary Iminium Salts
Authors: Delbos-Krampe Jeanne , Risch Nikolaus , Flörke Ulrich
Published: August 2018

An efficient and convenient two step synthesis of each of the four possible diastereoisomers of the N-terminal amino acid component of nikkomycins is described. We first synthesized α-amino-β-oxo acids by aminoalkylation of ketones with iminium salts. The second step using Pearlman’s catalyst gave directly nonnatural and natural precursors 13 - 16 of nikkomycins 1 which were easily separated by chromatography on silica gel.
A New Efficient Synthesis of Substituted Luminols Using Multicomponent Reactions
Authors: Neumann Helfried , Klaus Stefan , Klawonn Markus , Strübing Dirk , Hübner Sandra , Gördes Dirk , Wangelin Axel Jacobi von , Lalk Michael , Beller Matthias
Published: August 2018

A new general synthesis of substituted luminols (5-amino-2,3-dihydrophthalazine-1,4-diones) is presented. Diversely substituted luminol derivatives can be synthesized in three steps. The products are of interest as new materials, which exhibit chemiluminescence.
Eine neue Modifikation von Lanthanmonogermanid – lT-LaGe /A New Modification of Lanthanummonogermanide – lT-LaGe
Authors: Mattausch Hansjürgen , Simon Arndt
Published: August 2018

Single crystals of the low temperature modification of LaGe are obtained as a byproduct in the reaction of La metal, LaBr3 and Ge powder at 1000 °C as silver colored, moisture sensitive needles. lT-LaGe crystallizes in space group Cmcm with a = 4.5590(10), b = 13.766(2), c = 6.745(2)Å . The Ge atoms form cis-trans-cis-trans-chains with dGe−Ge = 2.621(1) and 2.799(1) Å in contrast to Ge zigzag chains found in the high temperature modification of LaGe crystallizing in the FeB structure type. In both structures the Ge atoms are surrounded by trigonal prisms of lanthanum atoms with CN = 6+1 but different connection of the prisms.
Reaction of N1,N2-Diarylamidines with 2,3-Diphenylcyclopropenone
Authors: Gomaa Mohsen Abdel-Motaal
Published: August 2018

Reaction of N1,N2-diarylacetamidines 1a - c with 2,3-diphenylcyclopropenone 2 led to formation of addition products 2-methyl-1-aryl-2-arylamino-4,5-diphenyl-1,2-dihydro-3H-pyrrol-3-ones 3a - c. While N1,N2-diarylformamidines 1d - f reacted with 2,3-diphenylcyclopropenone 2 to afford 3-aryl-(N-4-arylformamidoyl)amino-2,3-diphenyl propionic acids 7a - c.
Solvent-Free Synthesis of 2,4,6-Triaryl Pyridines
Authors: Kidwai Mazaahir , Rastogi Shweta , Thakur Ruby , Saxena Shilpi
Published: August 2018

A modified method to prepare 1,3,5-triarylpyridines by a [3+2+1] ring annulation reaction is described. Three-component condensation of neat reactants when subjected to microwaves afforded the required product in shorter reaction time with higher yield in comparison to conventional methodologies. The microwave accelerated reaction technique without external solvent renders the whole synthesis into a truly ecofriendly protocol.
Some Novel Amino Acid-Schiff Bases and their Complexes Synthesis, Characterization, Solid State Conductivity Behaviors and Potentiometric Studies
Authors: Sarı Nurşen , Gürkan Perihan
Published: August 2018

Three new Schiff bases derived from the condensation reaction of thiophene-2-carbaldehyde and DL-alanine, DL-valine and DL-phenylalanine have been synthesized and their Co(II), Ni(II) and Cu(II) complexes have been prepared. The Schiff bases and the complexes have been characterized by their analytical and spectral data. The protonation constants of the Schiff bases and stability constants of the complexes have been determined potentiometrically in aqueous medium at 25 °C and 0.1 M KCl ionic strength. Solid state conductivities of the synthesized substances were using the four-probe technique on a compressed pellet at room temperature.
Ultrasound-Promoted Reduction of Conjugated Enones, α-Diketones and Acyloins with NaBH4 under Aprotic Condition
Authors: Zeynizadeh Behzad , Yahyaei Saiedeh
Published: August 2018

A variety of conjugated enones are reduced regioselectively to their corresponding allylic alcohols with NaBH4 under ultrasound irradiation. Reduction reactions were performed in THF at room temperature and the product alcohols were obtained in high to excellent yields. This system is also efficient for the reduction of α-diketones and acyloins to vicinal diols.
1,4-Bis(p-pentazolylphenyl)butan, 1-p-Azidophenyl-4-p-pentazolylphenyl- butan und 1,4-Bis(p-azidophenyl)butan / 1,4-Bis(p-pentazolylphenyl)butane, 1-p-Azidophenyl-4-p-pentazolylphenyl-butane and 1,4-Bis(p-azidophenyl)butane
Authors: Biesemeier Frank , Harms Klaus , Müller Ulrich
Published: August 2018

1,4-Bis(p-pentazolylphenyl)butane (1), 1-p-azidophenyl-4-p-pentazolylphenyl-butane (2) and 1,4-bis(p-azidophenyl)butane (3) were obtained by the reaction of 1,4-diphenylbutane-4’,4”- bis(diazonium) ions with sodium azide in methanol at −50 °C. In the 1H and 13C NMR spectra the three compounds can be distinguished unequivocally. At −50 °C a mixture with a composition 1:2:3 of 10:30:60 was obtained. By recrystallization first from dichloromethane/methanol and then from dichloromethane/petroleum ether the pentazole components were enriched to a composition ratio of 21:62:17. The rate constants of the decompositions 1→2 and 2→3 at 0 °C were determined from the variation of the 1H NMR intensities. At room temperature all of the material is converted to 3. 3 crystallizes in two monoclinic modifications. At −70 °C a modification 3-LT having space group P21/c (a = 950.8, b = 1192.6, c = 701.3 pm, β = 92.55°, Z = 2; R = 0.075) was obtained. The modification crystallizing at room temperature (3-HT) has space group I2/a (a = 1514.5, b = 498.1, c = 2027.9 pm, β = 92.73°, Z = 4; R = 0.040). Whereas both modifications consist of nearly identical molecules, their packings are quite different. When the low temperature modification is warmed to room temperature, its crystals jump like flees and are disrupted to a fine powder.
Pyridopyridazines, Benzimidazolopyrimidines Triazolopyrimidines, 9-Oxo-2,3,6,7-tetraazabicyclo[3.3.1]nona-3,7-diene and Aroylcinnolines from 2-Arylhydrazono-3-oxopropanals
Authors: Al-Zaydi Khadijah M. , Elnagdi Mohamed H.
Published: August 2018

The reaction of the 2-arylhydrazonopropanal 3a with 2-amino1,1,3-tricyanopropene 4 afforded the pyridopyridazines 6. On the other hand, reaction of 3b with 4 afforded 7. Compounds 3a,b also condensed with 2-aminobenzimidazole and 3(5)-amino-1,2,4-triazole to yield azolopyrimidines 10 and 13. Refluxing compounds 3a,b in acetic acid in the presence of ammonium acetate afforded 2,3,6,7-tetraaza-bicyclo[3.3.1]nona-3,7-diene 14 and aroylcinnoline 15 respectively.
The Synthesis, Crystal Structure and Spectroscopic Properties of a Dinuclear μ–Pyrazolato–N,N’–Bridged Dinickel(II) Complex of 1,3–Bis(salicylideneamino)propan–2–ol
Authors: Zeyrek C. T. , Elmali A. , Elerman Y.
Published: August 2018

The title compound [Ni2(L)(3,5 prz)], prz = pyrazolate with the formally pentadentate ligand L = 1,3-bis(salicylideneamino)propan-2-olate, was synthesized and identified using elemental analysis and IR spectroscopy. It crystallizes in the monoclinic space group P21/c with cell parameters a = 29.873(4), b = 11.131(2), c = 13.166(3) Å , β = 107.770(10)°, V = 4169.0(13) Å3, Z = 4, Dcal = 1.618 Mg/m3. The nickel ions are bridged by the alkoxo group of the ligand and the N atoms of the μ-pyrazolate group. Each nickel(II) ion is coordinated by two N atoms and two O atoms, forming a square with trans-N2O2 geometry. The Ni···Ni distance and the Ni−O−Ni angle are 3.371(1) Å and 126.4(1)°, respectively.
Ring Size Influence on the Cyclocondensation Mode of GABA – Nitrile Imine Adducts
Authors: Thaher Bassam A. Abu , Zahra Jalal A. , El-Abadelah Mustafa M. , Voelter W.
Published: August 2018

γ -Aminobutyric acid (GABA) adds onto nitrile imine 1,3-dipolar species (generated in situ from their N-arylhydrazonoyl chloride precursors 1a-c ) to deliver the corresponding acyclic amidrazone adducts 10a-c. In the presence of 1,1’-carbonyldiimidazole, the latter adducts undergo cyclocondensation involving the activated carboxyl and the amidrazone-CH2NH groups to afford the respective N-[1-(arylhydrazono)-2-oxopropan-1-yl] pyrrolidin-2-ones (11a-c). The constitution of 10 and 11 is evidenced from analytical and spectral (IR , MS and NMR) data.
A Second Modification of Mercury(I) Orthoarsenate(V): Preparation and Crystal Structure of β-(Hg2)3(AsO4)2
Authors: Weil Matthias
Published: August 2018

Light-yellow crystals of a second modification of mercury(I) orthoarsenate(V), β-(Hg2)3(AsO4)2, were obtained during a diffusion-controlled precipitation reaction starting from diluted solutions of Hg2(NO3)2, Hg(NO3)2, and H3AsO4. The crystal structure was determined from a single crystal X-ray diffraction data set. The previously reported crystal structure of synthetic chursinite, α-(Hg2)3(AsO4)2, has also been re-investigated and refined with better accuracy and precision. Both phases crystallize in space group type P21/c (no. 14) [α- (β -): Z = 2 (4), a = 8.7915(6) (10.2034(18)), b = 5.0699(4) (8.5875(14)), c = 15.6839(10) (13.5172(19)) Å , β = 128.761(1) (101.016(3))°, 1661 (3528) structure factors, 74 (146) parameters, RF2 > 2σ (F2)] = 0.0195 (0.0492)] and are made up from Hg2
2+ dumbbells and AsO4
3− tetrahedra as the main building units, but the topologies of the structures are quite different.
Quaternäre Strontium-Kupfer(I)-Lanthanoid(III)-Selenide mit Cer und Praseodym: SrCuCeSe3 und SrCuPrSe3, ein ungleiches Geschwisterpaar / Quaternary Strontium Copper(I) Lanthanoid(III) Selenides with Cerium and Praseodymium: SrCuCeSe3 and SrCuPrSe3, Unequal Brother and Sister
Authors: Strobel Sabine , Schleid Thomas
Published: August 2018

Quaternary strontium copper(I) lanthanoid(III) selenides are formed by the oxidation of elemental strontium, copper and the corresponding lanthanoid with selenium. Orange to red needle-shaped single crystals of SrCuPrSe3 and SrCuCeSe3 have been synthesized by heating mixtures of Sr, Cu, Pr / Ce and Se with CsI as a flux in evacuated silica tubes to 800°C for 7 d. Both compounds crystallize orthorhombically in space group Pnma with four formula units per unit cell, but with unlike lattice constants (a = 1097.32(6), b = 416.51(2), c = 1349.64(8) pm for SrCuPrSe3 and a = 846.13(5), b = 421.69(2), c = 1663.42(9) pm for SrCuCeSe3) and therefore different structure types. The Pr3+ cations in SrCuPrSe3 are surrounded octahedrally by six Se2− anions forming chains of edge-sharing [PrSe6]9− octahedra that are joined by common vertices. Together with [CuSe4]7− tetrahedra they form [CuPrSe3]2− layers piled up parallel (001). Between those layers the Sr2+ cations are coordinated by seven Se2− anions in the shape of capped trigonal prisms linking the structure in the third dimension. On the other hand in SrCuCeSe3 the Ce3+ cations as well as the Sr2+ cations adopt a coordination number of seven. Since the bonding distances between cerium and selenium match with those of strontium and selenium the two crystallographically independent sites of these cations are occupied statistically by Ce3+ and Sr2+ with equal ratios. Nevertheless, there is a close structural relationship between SrCuPrSe3 and SrCuCeSe3. Similar to SrCuPrSe3 where Cu+ and Pr3+ cations together with Se2− anions form [CuPrSe3]2− layers parallel (001), the Cu+ cations and [(Ce1/Sr1)Se7]11.5− polyhedra in SrCuCeSe3 build strongly puckered layers which are connected by (Ce2)3+/(Sr2)2+ cations. The copper selenium part in both compounds correlates as well, with [CuSe4]
7− tetrahedra linked by common vertices to form [CuSe3]5− chains running along [010].
“Weak” OH···πHydrogen Bonds in the Structures of Two Phenols
Authors: Kuś Piotr , Jones Peter G.
Published: August 2018

Crystallographic studies of α, α’-di(4-hydroxyphenyl)-1,4-diisopropylbenzene (1) and α, α’-di- (3,5-dimethyl-4-hydroxyphenyl)-1,4-diisopropylbenzene (2) were performed. Both compounds display the anti conformation. Compound 1 crystallizes as the 1:1 hydrate; the packing involves three classical hydrogen bonds and one non-classical OH···π bond. Both OH groups of 2 form non-classical OH···π hydrogen bonds to aromatic rings.
Enamines in Heterocyclic Synthesis: A Route to 4-Substituted Pyrazoles and Condensed Pyrazoles
Authors: Hassaneen Huwaida M. E. , Hassaneen Hamdi M. , Elnagdi Mohamed H.
Published: August 2018

The reaction of nitrile imines, generated in situ, from hydrazonoyl halides 3a - e with enamines 2a - c affords pyrazoles 8a - g. These pyrazoles have been used to prepare condensed pyrazoles.
Experimental Gas Phase 1H NMR Spectra and Basis Set Dependence of ab initio GIAOMO Calculations of 1H and 13C NMR Absolute Shieldings and Chemical Shifts of Small Hydrocarbons
Authors: Zuschneid Thomas , Fischer Holger , Handel Thomas , Albert Klaus , Häfelinger Günter
Published: August 2018

High-resolution gas phase measurements of 1H NMR spectra at 400 MHz and atmospheric pressure of seven small hydrocarbons are presented. The developed new method and the experimental set-up are described. Ab initio GIAO MO calculations of 1H and 13C NMR absolute shieldings on the HF, MP2 and B3LYP levels using 25 standard gaussian basis sets are reported for these hydrocarbons, based on experimental re distances. The measured gas phase 1H chemical shifts have been converted to an absolute σ0 shielding scale by use of the literature shielding of methane. These and gas phase 13C literature values have been transferred with literature ZPV data to estimated σe
exp shieldings which are used to evaluate the basis set dependence of the calculated σe shieldings utilizing linear least squares regressions. Exponential extrapolations of Dunning basis set calculations allow the determination of basis set limits for 1H and 13C shieldings.

1H and 13C chemical shifts have been derived from the HF calculated shieldings with shieldings of TMS which has been geometry optimized and GIAO calculated in each basis. Standard deviations (esd) as low as 0.09 ppm for 1H and 0.76 ppm for 13C calculations have been obtained.

The statistically best basis set for simultaneous calculation of 1H and 13C absolute shieldings or relative shifts is 6-311G* within the HF and B3LYP methods. Aiming for highest accuracy and precision, 1H and 13C have to be treated separately. In this case, best results are obtained using MP2/6-311G** or higher for 1H shieldings and MP2/cc-pVTZ for 13C shieldings.
The Modulated Structure of SrAuSn2
Authors: Esmailzadeh Saeid , Hoffmann Rolf-Dieter , Pöttgen Rainer
Published: August 2018

The ternary stannide SrAuSn2 was synthesized by induction melting of the elements under an argon atmosphere in a sealed niobium ampoule in a water-cooled sample chamber of a high-frequency furnace. The structure of SrAuSn2 was investigated by X-ray powder and single crystal diffraction. It was found to be favourable to describe as a commensurately modulated structure. The 3+1 dimensional superspace group symmetry P : Cmcm(α, 0, 0) : 0s0 with the unit cell dimensions a = 460.20(14), b = 2038.8(8), c = 460.34(19) pm and the modulation wave vector q =¼ [100]*. The Sn1 atoms were those with the strongest modulation while the rest of the atoms showed rather small deviations from the average structure. The SrAuSn2 structure is closely related to the CeNiSi2 type. Geometrically these structures are built up from distorted ThCr2Si2 and AlB2 slabs. The gold atoms are located in the ThCr2Si2 slab. They have a distorted square pyramidal tin coordination at Au-Sn distances ranging from 266 to 294 pm. These pyramids are condensed via common edges forming two-dimensional layers. The latter are condensed via the Sn1 atoms within the AlB2 slabs that form one-dimensional zigzag chains with Sn1-Sn1 distances ranging from 282 to 288 pm. These chains show the strong modulations. Together, the gold and tin atoms build up a three-dimensional [AuSn2] network, in which the strontium atoms fill distorted hexagonal channels.
Synthesis and Crystal Structure Analysis of C60 Fulleride Dianions in Solvates of [A([2.2.2]crypt)]2[C60] (A = K, Rb, Cs)
Authors: Hoffmann Stephan D. , Fässler Thomas F.
Published: August 2018

Reduction of C60 with the alkali metals A = K, Rb and Cs in tetrahydrofuran as a solvent and addition of [2.2.2]crypt [1], dimethylformamide and cyclohexane lead to the formation of crystalline samples of [A([2.2.2]crypt)]2[C60](C6H12)2(C3H7NO)2(C4H8O)2 (A = K, Rb, Cs) 1a, 1b and 1c as major fractions. As a by-product of compound 1a, a second minor fraction containing [K([2.2.2]crypt)]2[C60](C3H7NO)4 2 was obtained. The structures of the four compounds have been determined by single-crystal X-ray analyses. The [C60]2− dianions are predominantly ordered. As the main structural motif the structures of compounds 1a, 1b and 1c contain pseudo-hexagonal layers of [C60]2− dianions. Compound 1c contains a rare example of a Cs+ sequestering [2.2.2]crypt molecule. The packing of the ionic units in compound 2 also shows layers of distorted hexagons formed by [C60]2− dianions which arranged in pairs with short contacts of 10.3 Å between their centers of gravity.
Two New Iridoid Glucosides from Verbascum salviifolium Boiss.
Authors: Akdemir Zeliha S , Tatli I. Irem , Bedir Erdal , Khan Ikhlas A.
Published: August 2018

From the aerial parts of the plant Verbascum salviifolium, two new iridoid glucosides, 6-O- β-D-glucopyranosylcatalpol (1) and 6-O-(6″-O-trans-p-hydroxycinnamoyl)- β -D-glucopyranosylaucubin (2) along with five known iridoid glycosides, 6-O- β -D-glucopyranosylaucubin (3), 6-O-α-L-rhamnopyranosylcatalpol (4), verbaspinoside [= 6-O-(2″-O-trans-cinnamoyl)-α-L-rhamnopyranosylcatalpol] (5), pulverulentoside I [= 6-O-(2″-O-trans-p-methoxycinnamoyl-3″ -O-acetyl)-α-L-rhamnopyranosylcatalpol] (6), and buddlejoside A8 [= 6-O-(4″-O-trans-3,4-dimethoxycinnamoyl)- α-L-rhamnopyranosylcatalpol] (7) were isolated. The structures of the new compounds were established on the basis of spectroscopic evidence.