bluuebunny/crossref_metadata_2025_split huggingface dataset:
1,1-Organoboration of Trimethyl-l-propynyltin Using Diorganoboryl-Substituted Ferrocenes
Authors: Wrackmeyer Bernd , Dörfler Udo , Milius Wolfgang , Herberhold Max 
Published: February 2015

Abstract
The reactions of various diorganoborylferrocenes, Fc -BR2 [1, R = Me (a), Et (b), iPr (c), tBu (d), Ph (f), R2B = 9-borabicyclo[3.3.1]nonyl (e)] and 1,1′-bis(9-borabicyclo[3.3.1]nonyl)- ferrocene (2) with trimethyl-l-propynyltin (3) were studied, and the products of the 1,1- organoboration were characterized as the alkenyltin compounds 4 -6 by 1H, 11B, 13C and 119Sn NMR. In the cases of 1a - 1d and If, there is competition between the transfer of a ferrocenyl group and the other organyl groups R from boron to carbon, whereas in the case of the 9-borabicyclo[3.3.1]nonane derivatives 1e and 2, the enlargement of the bicyclic system takes place selectively (compounds 4e and 6). The molecular structure of the product 6, obtained from the reaction between the 1,1′-diborylated ferrocene 2 and two equivalents of 3, was determined by single crystal X-ray analysis (space group P21/c monoclinic; Z = 4, a = 958.3(2), b = 1610.4(3), c = 2405.3(5) pm and β = 90.33(3)°)
Preparation and Structure of Poly(gold)telluronium Salts
Authors: Angermaier Klaus , Schmidbaur Hubert 
Published: February 2015

Abstract
Tris[(triphenylphosphine)gold(I)]telluronium tetrafluoroborate (1) was prepared from the corresponding oxonium salt and bis(t-butyldimethylsilyl)tellurium in dichloromethane at -78°C. The product forms yellow crystals, thermally stable to 125°C. It was identified by standard analytical and spectroscopic techniques, including a single crystal X-ray diffraction study. In the crystal lattice, the cations form tellurium-capped triangles of gold, which are associated into dimers through short intermolecular Au -Au contacts, resembling those in the corresponding sulfur and selenium compounds. - The reaction of (t-BuMe2Si)2Te with four equivalents of [(Ph3P)Au]BF4 in tetrahydrofuran at -78°C gives a tetranuclear compound, {[(Ph3P)Au]4Te}2+ 2 BF4
- (2) which differs from 1 in its analytical and spectroscopic data. Its structure could not be determined, but it is assumed that the dications have a square pyramidal geometry
Synthese und Kristallstruktur von Pb2LnAl3O8 (Ln = Eu, Gd) / Synthesis and Crystal Structure of Pb2LnAl3O8 (Ln = Eu, Gd)
Authors: Werner J.-P. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single Crystals of Pb2LnAl3O8 (Ln = Eu, Gd) have been prepared by flux techniques. The compounds crystallize with cubic symmetry, space group Oh-Pn3̅m, a(Eu) = 9.4578(5), a(Gd) = 9.4448(7) Å, Z = 4. The crystal structure is characterized by heterocubane units of the type Pb4O4 and hexagonal bipyramids of oxygen around the rare earth ions. These components form a network made of macro polyhedra of the type Pb4O4- LnO6- Pb4O4
, der erste einzähnig koordinierte Aziridin-Komplex / , the First Mono-Coordinate Aziridine Complex
Authors: Beckerath Stephan von , Lorenz Ingo-Peter , Fawzi Riad , Steimann Manfred 
Published: February 2015

The photolytically induced CO-substitution reaction of CpMn(CO)3 with N-benzyl-aziridine leads to the first mono coordinate aziridine complex,

. It is stable against thermal C2H4 elimination up to 135°C. No nitrene complexes {Cp(CO)2Mn}nNBz (n = 1, 2) were detected.
The X-ray structure analysis of

shows the intact three-membered ring ligand and the pyramidal configuration of the nitrogen atom.
Titan- und Vanadiumkomplexe mit 4-[1-(N′-Benzoylhydrazino)-l-phenylmethyliden]- 3-methyl-1-phenyl-pyrazol-5-on. Röntgenkristallstruktur von 4-[1-(N′-Benzoylhydrazino)-1-phenyl-methyliden]-3-methyl-1-phenyl- pyrazol-5-on / Titanium- and Vanadium Complexes of 4-[1-(N′-Benzoylhydrazino)-1-phenylmethylidene]-3-methyl-1-phenyl-pyrazol-5-one. Structure of 4-[1-(N′-Benzoylhydrazino)-1-phenyl-methylidene]-3-methyl-1-phenyl-pyrazol-5-one
Authors: Kraudelt Heide , Schilde Uwe , Hefele Heike , Ludwig Eberhard , Ludwig Erhard 
Published: February 2015

By reaction of 1-phenyl-3-methyl-4-benzoyl-pyrazol-5-one with benzoylhydrazine the tridentate diacidic ligand 4-[1-(N′-benzoylhydrazino)-1-phenyl-m ethylidene]-3-m ethyl-lphenyl-1-pyrazol-5-one (H2L) is formed which gives complexes ML2 with tetravalent titanium and vanadium ions. The ligand and its complexes were characterized by mass spectroscopy. The vanadium(IV) complex can be oxidised and reduced electrochemicallv. The chemical bonding in the titanium(IV) complex and in the ligand was studied by IR and 13C NMR spectroscopy.
The molecular structure of 4-[1-(N′-benzoylhydrazino)-1-phenyl-methylidenel-3-m ethyl-lphenyl- pyrazol-5-one was determined by X-ray analysis. Crystal data: a = 9.159(3) Å, b = 11.014(4) Å, c = 11.136(5) Å, a = 90.11 (2)°, β = 101.84(3)°, γ = 113.01 (2)°; space group P1̄, Z = 2.
Synthese und Kristallstruktur der (p-Brombenzyl)triphenylphosphonium-bromide: [(p-Br-C6H4-CH2)P(C6H5)3]+B-;[(p-Br-C6H4-CH2)P(C6H5)3]+Br2
- und [(p-Br-C6H4-CH2)P(C6H5)3]+Br3
-/ Synthesis and Crystal Structures of (p-Bromobenzyl)triphenylphosphonium Bromides, [(p-Br-C6H4-CH2)P(C6H5)3]+Br-;[(p-Br-C6H4-CH2)P(C6H5)3]+Br- and [(p-Br-C6H4-CH2)P(C6H5)3]+Br3-
Authors: Vogt H. , Wulff-Molder D. , Meisel M. 
Published: February 2015

(p-Bromobenzyl)triphenylphosphonium Bromide,
[(p-Br-C6H4-CH2)P(C6H5)3]+Br- · (CH2Cl2)2.5 (1) has been prepared by the reaction of triphenylphosphine with p-bromobenzylbromide and its structure determined (triclinic, space group P1̅, Z = 2, a = 1198.03(12), b = 1245.80(11), c = 1258.42(12)pm, a = 100.170(8), β = 103.543(9), γ = 1 18.158(7)°. The compound exists as Br- anions and [(p-Br-C6H4- CH2)P(C2H5)3]+ cations, with weak interactions between the chlorine atoms of the CH2Cl2 molecules and the bromine bonded in the cation.
[p-Br-C6H4-CH2)P(C6H5)3]Br2 (2) and [(p-Br-C6H4-CH2)P(C6H5)3]Br3·(CH2Cl2)1.5 (3) have been obtained by reactions of the corresponding amounts of bromine with 1 in methylenechloride solution. The yellow-red crystals of 2 are orthorhombic, space group Pccn, Z = 8, a = 2060.8(3), b = 1223.6(4), c = 1860.8(3) pm. Compound 2 exists as [p-Br-C6H4-CH2)P(C6HO5)3]+ cations and linear Br2-
4 units with a bromide-bromine distance of 297.3(4) pm. The red crystals of (3) are triclinic, space group P1̅, Z = 2, a = 1 171.16(7), b = 1260.97(8), c = 1270.35(7)pm, α = 65.510(5), β = 75.811(5), γ = 62.320(5)°, and contain [(p-Br-C6H4-CH2)P(C6H5)3]+ cations and linear, slightly asymmetrical Br-
3 anions. In all cases the cation has a slightly irregular tetrahedral geometry around the P atom.
N-Iod-triphenylphosphanimin. Synthese und Kristallstrukturen von [Me3SiNPPh3· ICl] und Ph3PNI / N -Iodo-triphenylphosphaneimine. Synthesis and Crystal Structures of [Me3SiNPPh3 · ICl] and Ph3PNI
Authors: Grebe Jutta , Weller Frank , Dehnicke Kurt 
Published: February 2015

N-Iodo-triphenylphosphaneimine, Ph3PNI, has been prepared by thermolysis of the donor acceptor complex [Me3SiNPPh3·ICl] in boiling acetonitrile in the presence of potassium fluoride. Both compounds have been characterized by IR spectroscopy and by crystal structure determinations.
[Me3SiNPPh3 · ICl]: Space group P1̄, Z = 2, a = 888.3(1), b = 1070.7( 1), c = 1310.2( 1) pm, α = 95.15( 1)°, β = 108.67( 1)°, γ = 97.78( 1)° at 20°C. The complex has a molecular structure in which the N atom of the phosphaneimine is connected with the iodine atom of the ICI molecule in a linear arrangement N-I-Cl with bond lengths N-I = 232.7 pm, I-Cl = 255.37 pm. \
Ph3PNI: Space group P21/n, Z = 4, a = 952.8(1), b = 1800.8(2), c = 1003.6(1) pm, β = 110.25(1)° at -50°C. The compound forms monomeric molecules with bond lengths PN = 159.1 pm, I-N = 205.6 pm and an INP bond angle of 113.3°.
Synthese und Kristallstruktur des Lanthan-Titanat-Tellurats LaTi(Ti0,25Te0,75)O6 und seine Verwandtschaft mit PbSb2O6 und Sr(MnTe)O6/Synthesis and Crystal Structure of the Lanthanum Titanate Tellurate LaTi(Ti0.25Te0.75)O6 and its Relationship to PbSb2O6 and Sr(MnTe)O6
Authors: Wulff L. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single crystals of LaTi(Ti0.25Te0.75)O6 have been prepared by solid state reactions. X-ray investigations led to trigonal symmetry, space group C3
1-P3 , a = 5.141(10), c = 5.218(10) Å, Z = 1. The compound is characterized by a predominantly ordered distribution of Ti4+ and Te6+. Typical features of the crystal structure are staggered layers containing edge connected TiO6 and (Ti,Te)O6 octahedra. The layers are connected by La3+ ions receiving an octahedral coordination by the surrounding oxygen ions. The relationships to the PbSb2O6 type and the recently described compound Sr(MnTe)O6 are discussed.
Oxochlorierung von Übergangsmetall-Komplexen mit Thionylchlorid/Oxochlorination of Transition Metal Complexes with Thionyl Chloride
Authors: Stoll Carola , Lorenz Ingo-Peter , Nöth Heinrich , Seifert Thomas 
Published: February 2015

Abstract
The reaction of the transition metal complexes CpV(CO)4 and [CpMo(CO)3]2 with thionyl chloride affords the oxodichlorides CpM(O)Cl2 (M = V, Mo) by oxidative decarbonylation. The X-ray structure analysis of CpV (O)Cl2 shows the pseudo tetrahedral “piano-stool” configuration for the central vanadium atom.
Ag2Cs[B15O24]: Ein wasserfreies quaternäres Silber(I)-Borat mit einem neuartigen Boratanion mit helixartigem Aufbau / Ag2Cs[B15O24]: An Anhydrous Quaternary Silver(I)-Borate with a New Helical Borate Anion
Authors: Wiesch A. , Bluhm K. 
Published: February 2015

Abstract
Single crystals of Ag2Cs[B15O24] were prepared by using a B2O3 flux technique with Ag2CO3 and Cs2CO3 in a closed silver tube at 650 °C. X-Ray investigations led to a new crystal structure in the space group P 21212 (Nr. 18) with lattice parameters a = 1778.7 (4); b = 2219.2 (4); c = 512.2 (1) pm, Z = 4. The silver atoms are part of distorted AgO4 tetrahedra and planar AgO3 units while the caesium atoms are eightfold coordinated by oxygen. The compound contains an as yet unknown borate anion [B15O24] with twelve BO3- and three BO4 units per formula. The BO3 units are connected to eight cords twisted to helices which are combined via BO4 tetrahedra to a three dimensional framework with large tunnels occupied by the cations.
Zum Chemischen Transport von Rhenium und Rheniumoxiden/On the Chemical Transport of Rhenium and Rhenium Oxides
Authors: Feller J. , Oppermann H. , Binnewies M. , Milke E. 
Published: February 2015

Abstract
Synthesis and single crystal growth by chemical transport reactions of rhenium and rhenium oxides is reported. Several transport agents like the mercury halides HgCl2, HgBr2, HgI2, tellurium tetrachloride and iodine have been employed the transport of the rhenium compounds. Mass spectrometric experiments gave informations about the composition of the gas phase. The transport reactions were traced by calculations based on the knowledge of the gas phase species and their thermodynamical data.
Darstellung und Schwingungsspektren von cis- und trans-[OsXY(acac)2], X ≠ Y = Cl, Br, I sowie Normalkoordinatenanalyse von trans-[OsClBr(acac)2]/Synthesis and Vibrational Spectra of cis- and trans-[OsXY(acac)2], X ≠ Y = Cl, Br, I, and Normal Coordinate Analysis of trans-[OsClBr(acac)2]
Authors: Dallmann K. , Preetz W. 
Published: February 2015

Abstract
In the reaction of K2[OsX3 Y3] with boiling water/acetylacetone (1:1) the six mixed com­plexes cis-and trans-[OsX2 (acac)2] (X ≠ Y = Cl, Br, I) are formed, which have been purified by column chromatography with toluene on silica gel. The IR and Raman spectra (10K) show the intraligand vibrations of the acac groups with nearly constant frequencies and the stretching vibrations of OsO in the range 460-696, of OsCl at 315-345, of OsBr at 210-225, and of Osl at 160-175 cm-1 . A normal coordinate analysis based on a modified valence force field was performed for trans-[OsClBr(acac)2] and the vibrational modes have been assigned. With a set of 32 force constants, taking into account the intraligand vibrations, a good agreement between observed and calculated frequencies has been achieved. The valence force constants are fd (OsCl•) = 1.75, fd(OsBr′) = 1.63 and fd (OsO) = 3.27 mdyn/Å.
Interaction of the Vanadyl(IV) Cation with L-Ascorbic Acid and Related Systems
Authors: Ferrer E. G. , Williams P. A . M. , Baran E. J. 
Published: February 2015

Abstract
The interaction of VO2+ with L-ascorbic acid and dehydroascorbic acid was investigated by electronic spectroscopy in solution at different pH values. In the case of ascorbic acid, two different solid complexes containing one or two monodeprotonated ascorbate ligands could be isolated and characterized. With dehydroascorbic acid, interaction begins at pH = 4 but at higher pH values the ligand is hydrolysed irreversibly, generating 2,3-diketogulonic acid. A solid complex containing this ligand could be precipitated at pH = 7. Its spectroscopic behavior confirms the interaction of the cation with an enolised form of the acid.
Isolierte trigonale SrO6 – Prismen verknüpfen Kagome-Netze im Strontium-Manganat(IV)-Tellurat(VI): SrMnTeO6 / Kagomé Layers Connected by Isolated Trigonal SrO6 Prisms in the Strontium Manganate(IV) Tellurate(VI): SrMnTeO6 L
Authors: Wulff L. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single crystals of the hitherto unknown compound SrMnTeO6 have been prepared from Sr(OH)2 ·8H2O , MnCO3(aq) and TeO2 in air by crystallization below the melt range. X-ray investigations showed hexagonal symmetry, space group D3
3h -P6̅2m, lattice constants a = 5.143( 1), c = 5.384(2) A, Z = 1. SrMnTeO6 is characterized by staggered [(Mn/Te)6O18] Kagome layers along [001]. These layers are connected by Sr2+ ions, resulting in SrO6 prisms isolated from each other. The structure is discussed with respect to the connection of Kagome nets in the quaternary oxides of the Ba3Ln4O9 type.
Kristallstruktur von [Mo(Co)3(Ncme)(Srbu)]2 / Crystal Structure of [Mo(CO)3(NCMe)(S'Bu)]2
Authors: Kopp Mike R. , Neumüller Bernhard 
Published: February 2015

Abstract
Single crystals of [Mo(CO)3(NCMe)(S′Bu)]2 (1) and [{Mo(CO)3}2{Mo(CO)2}{S′Bu}4] (2) were obtained by the reaction of [Mo(CO)3(NCMe)3] with [(PhCH2)2GaS′Bu]2 in 1,4-dio-xane. The X-ray structure determination of 1 showed the presence of a Mo2S2 four-membe-red ring with a Mo-Mo bond length of 296,7(1) pm. Space group Pbca, Z = 4, lattice dimen­sions at -80°C: a = 1588,2(3), b = 905,8(1), c = 1676,0(1) pm, R1 = 0,0555.
Experimental and Computational Studies on Aminoguanidine Free Base, Monocation and Dication. Part III: Proton Affinities of Guanidine, Aminoguanidine and Glyoxal Bis(amidinohydrazone)
Authors: Koskinen Jere T. 
Published: February 2015

Abstract
The structures of glyoxal bis(amidinohydrazone) (GBG) free base and glyoxal bis(amidi-nohydrazonium) monocation and dication were calculated quantum chemically by using the density functional hybrid method B3-LYP with the standard basis set 6 -31 G (d). Proton affinities calculated from these data are 246.4 kcal/mol for the free base and 176.0 kcal/mol for the monocation. The proton affinities of guanidine free base (246.2 kcal/mol), aminogua­nidine free base (242.9 kcal/mol), aminoguanidinium monocation (88.6 kcal/mol) were calcu­lated for reference. The B3-LYP functional overestimates the proton affinities for all the species studied. For example, for guanidine the proton affinity at the M P2/6-31G (d) level is 238.3 kcal/mol, the experimental reference value being 233 kcal/mol. However, from the B3-LYP values it can be concluded that in the gas phase all the three bases are nearly equally basic. On the other hand, it is known that in aqueous solution guanidine is a much stronger base than aminoguanidine and glyoxal bis(amidinohydrazone). The results are discussed from the point of view of molecular size, shape and symmetry, and hydrogen bonding in solution.
Synthesis and Structure of Benzyltriethylammonium Trichlorogermanate(II)
Authors: Wegner Gerald L , Jockisch Alexander , Schmidbaur Hubert 
Published: February 2015

Abstract
The reaction of equimolar quantities of GeCl2 · dioxane with [BzEt3N]+ Cl- in tetrahydro-naphthaline gives high yields of [BzEt3N]+ [GeCl3]-. The asymmetric unit of the monoclinic single crystals (from CH2CI2 , space group P21/c, Z = 8) are comprising two pairs of crystallographically independent cations and anions, each with very similar molecular dimensions. The isolated [GeCl3]-anions have a trigonal pyramidal structure with narrow Cl-Ge-Cl angles in the range from 93.41(5) to 98.27(5)° and Ge-Cl distances between 2.293(2) and 2.305(2) Å. This structure is thus very similar to that of the isoelectronic AsCl3 molecule and of the [SeCl3]+ cation.
Untersuchungen An Natriumtrifluormethylsulfonat. Kristallstruktur von Natriumtrifluormethylsulfonat- Trifluormethylsulfonsäure (1/3) / Studies on Sodium Trifluoromethanesulfonate. Crystal Structure of Sodium Trifluoromethanesulfonate-Trifluoromethanesulfonic Acid (1/3)
Authors: Korus Gabriele , Jansen Martin 
Published: February 2015

Abstract
Single crystals of sodium trifluoromethanesulfonate-trifluoromethanesulfonic acid (1/3) (NaSO3CF3 · 3 HSO3CF3) have been prepared by reaction of sodium trifluoromethanesulfonate with anhydrous trifluoromethanesulfonic acid at 60 °C. NaSO3CF3 · 3 HSO3CF3 crystallizes in space group I213 (No. 199) with a = 16.210(1) Å, Z = 8. Sodium is coordinated by six oxygen atoms from six different trifluoromethanesulfonic acid molecules, each acid molecu­le connecting two sodium ions. The 3-dimensional network resulting from the edge sharing octahedra corresponds to the cubic (10, 3) net, not realised otherwise, so far. The trifluorome­thanesulfonate anion is bonded to three trifluoromethanesulfonic acid molecules by hydrogen bonds.
Carbacylamidophosphates: Synthesis, Properties, and Structure of Dimorfolido-N-trichloroacetylphosphorylamide
Authors: Ovchynnikov Vladimir A , Amirkhanov Vladimir M , Timoshenko Taras P , Glowiak Tadeusz , Kozlowskib Henryk 
Published: February 2015

Abstract
Dimorpholido-N-trichloroacetylphosphorylamide: CCl3C(O)NHP(O)[N(CH2CH2)2O]2 [HL] and its sodium [NaL] and morpholine [HN(CH2-CH2)2O•HL] salts were synthesized for the first time. The compounds were studied by IR spectroscopy and assignments of the characteristic IR bands have been made. The structure of [HL] was determined by X-ray diffraction. Crystals are monoclinic, a = 11.412(2) Å, b = 16.056(3) Å, c = 9.622(2) Å, β = 108.55(3)°, space group P21/c; Z = 4. The refinement of the structure converged at R = 0.066. The molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups.
The Partial Oxidation of Methane to Methanol with Nitrite and Nitrate Melts
Authors: Lee Bor-Jih , Kitsukawa Shigeo , Nakagawa Hidemoto , Asakura Shukuji , Fukuda Kenzo 
Published: February 2015

Abstract
The effect of reduced oxygen species on the partial oxidation of methane to methanol was examined with nitrite melts. The experimental results support the suggestion that the formation of methanol or C2 compounds depends on different reduced oxygen species, as observed in our previous work using nitrate melts. It has been suggested that the partial oxidation of methane proceeds to CH3OH or C2 compounds via parallel pathways. This suggestion was verified by increasing the oxygen concentration to carry out the partial oxidation of methane in 25 mol% NaNCO3 -75 mol% KNO3 melts. A methanol selectivity of 8.2% and a methanol yield of 0.43% were observed with CH4/O2 = 15/1 at 575 °C, whereas with CH4/O2 = 7/1 methanol selectivity and yield increased to 23.7% and 1.1%, respectively. The results further confirm the contribution of the superoxide ion O2
- on methanol formation.
Dioxomolybdän(VI)-Komplexe mit dreizähnigen diaciden Liganden / Dioxomolybdenum(VI) Complexes with Tridentate Diacidic Ligands
Authors: Banße Wolfgang , Fliegner Jana , Sawusch Stefan , Schilde Uwe , Uhlemann Erhard 
Published: February 2015

Abstract
Dioxomolybdenum(VI) complexes have been synthesized by ligand exchange reactions of Mo(CO)6, Mo(NO)2(acac)2 and MoO2(acac)2 with tridentate diacidic ligands. X-ray structure analyses were performed on single crystals. The complexes salicylaldehyde-2-hydroxyanilato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (1b) and 2,2'-dihydroxy-azobenzenato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (2) are isomorphous. In all chelates the Mo atom is in a distorted octahedral environment.
Structural data: Salicylaldehyde-2-hydroxyanilato(2-)-tetrahydrofurane-dioxomolybdenum (VI) (1a): a = 23.381(6) Å, b = 6.756(2) Å, c = 28.380(8) Å, β = 124.47(2)°; Salicylaldehyde-2-hydroxyanilato(2-)-triphenylphosphaneoxide-dioxomolybdenum (VI) (1b): a = 9.4208(14) Å, b = 30.550(5) Å, c = 10.461(2) Å, β = 111.005(17)°; 2,2′-Dihydroxy-azobenzenato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (2): a = 9.392(2) Å, b = 31.012(13) Å, c = 10.350(2) Å, β = 110.968(17)°; Salicylaldehyde-salicylhydrazonato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (3): a = 9.321(2) Å, b = 12.048(2) Å, c - 13.858(3) Å, α = 101.90(2)°, β = 94.94(2)°, γ = 105.479(17)°.
Synthesis, Spectroscopic Studies, and Crystal Structure of Diethylchlorotin Dimethylphosphinate Et2ClSnO2PMe2
Authors: Shihada Abdel-Fattah , Weller Frank 
Published: February 2015

Abstract
Diethylchlorotin dimethylphosphinate has been synthesized by treating (Et2ClSn)2O with HO2PMe2 in toluene. Single crystal X-ray analysis shows that O2PMe2 groups behave as bidentate bridge ligands between Et2ClSn units leading to a polymeric chain structure in which the tin atoms exhibit a distorted trigonal bipyramidal geometry with the oxygen atoms in the axial positions. The Sn-Cl bond lies on a C2 axis of symmetry in the (C2v) OCClSnCO unit. Et2ClSnO2PMe2 crystallizes in the monoclinic space group C2/c (a = 877.9 (2), b = 1907.8 (4), c = 695.5 (1) pm, β= 106.72 (2)°, Z = 4 and R = 0.043). The characteristic IR bands of Et2ClSnO2PMe2 are assigned and the mass spectrum is reported and discussed.
Studies on Tetramethylammonium Selenate(VI) and Chromate(VI)
Authors: Malchus Michael , Jansen Martin 
Published: February 2015

Abstract
[N(CH3)4]2SeO4 and [N(CH3)4]2CrO4 have been investigated by Infrared and Raman spectroscopy, coupled thermogravimetric and differential thermal analysis combined with mass spectroscopy of the evolved gases and temperature dependent X-ray diffraction. The crystal structure of [N(CH3)4]2SeO4 has been determined from single crystal data (cubic, Fm3̄m. a -11.1077(7) Å, Z = 4) and reveals [N(CH3)4]+ cations and SeO4
2- anions to be arranged in a Li2O -type of structure. While the cation framework of regular tetrahedra is orientationally fixed, the selenate anions are disordered. Powder diffraction data show [N(CH3)4]2CrO4 to be isostructural (cubic, Fm3̄m, a = 11,039(1) Å, Z = 4).
Polysulfonylamine, CV. Die ersten N,N-disulfonylierten Sulfinsäureamide: Synthese und Kristallstrukturen von RS(O)-N(SO2Me)2 (R = Me, CCl3) / Polysulfonylamines, C V. The First N,N -Disulfonylated Sulfinic Amides: Synthesis and Crystal Stru ctures of RS(O)-N(SO2Me)2 (R = Me, CCl3)
Authors: Näveke Martina , Blaschette Armand , Jones Peter G. 
Published: February 2015

Abstract
The novel sulfinamides RS(O) -N(SO2Me)2, where R = Me (1a) or CCl3 (1b), were obtained by treating the corresponding sulfinyl chlorides with Me3SiN(SO2Me)2 or AgN-(SO2Me)2, respectively. A presumedly ionic 1:1 adduct of 1b with 4-dimethylaminopyridine was isolated and analytically characterized. In the crystals of 1a (monoclinic, space group P21/c) and 1b (monoclinic, P21/c) , the molecules feature approximately planar NS3 moieties, unusually long S(O) -N bonds and, in the case of 1b, an extremely long S(O) -C bond [for la and 1b, in order: sum of bond angles at nitrogen 359.5 and 357.1°, S(O) -N 178.2(2) and 173.6(2) pm, S(O) -C 178.8(2) and 194.1(2) pm]. In both molecular structures, an attractive S(O) ··· O 1,4-interaction leads to a 7.3° discrepancy in the S(O) -N -SO2 angles. The crystal packing of 1a displays a tape (double-chain) motif generated by two prominent intermolecular C -H ··· O interactions involving one MeSO2 group and the sulfinyl oxygen atoms of two adjacent molecules, whereas in 1b the molecules are associated into parallel chains via a bonding Cl ⋯ O(sulfonyl) interaction.