bluuebunny/crossref_metadata_2025_split huggingface dataset:
Phosphanimin-Komplexe von Mangan(II)halogeniden. Die Kristallstrukturen von [MnCl2(Me3SiNPEt3)]2, [Mnl2(Me3SiNPEt3)2] und [MnI2(Me2Si(NPEt3)2)] / Phosphaneimine Complexes of Manganese(II)halides. The Crystal Structures of [MnCl2(Me3SiNPEt3)]2, [Mnl2(Me3SiNPEt3)2] and [MnI2(Me2Si(NPEt3)2)]
Authors: Mai Hans-Joachim , Wocadlo Sigrid , Massa Werner , Weller Frank , Dehnicke Kurt , Maichle-Mössmer Cäcilia , Strähle Joachim 
Published: February 2015

The phosphaneimine complexes [MnCl2(Me3SiNPEt3)]2 (1) and [MnI2(Me3SiNPEt3)2] (2) have been prepared by the reaction of Me3SiNPEt3 with MnCl2 and Mnl2, respectively. Thermal decomposition of 2 leads to the chelate complex [MnI2(Me2Si(NPEt3)2)] (3) by cleaving SiMe4. The complexes are characterized by IR spectroscopy and by crystal structure determinations.
1: Space group P21/c, Z = 4, structure solution with 5062 observed unique reflections, R = 0.047. Lattice dimensions at -55 °C: a = 1175.8(5), b = 1634.5(2), c = 1740.2(8), β = 99.58(2)°. 1 forms dimeric molecules via chloro bridges and a cis-arrangement of the Me3SiNPEt3 donor molecules with Mn-N bond lengths of 210.4(5) and 208.2(4) pm.
2: Space group P 41212, Z = 4, structure refinement with 1633 independent reflections, 1072 observed unique reflections, R = 0.053. Lattice dimensions at -60 °C: a = b = 949.5(1), c = 3345.2(7) pm. 2 forms monomeric molecules with tetrahedrally coordinated Mn atoms and Mn-N bond lengths of 220.7(13) pm.
3: Space group P21/c, Z = 4, structure refinement with 8419 independent reflections, 4584 observed unique reflections, R = 0.047. Lattice dimensions at 20 °C: a = 1343.3(1), b = 2508.2(2), c = 1535.1(1) pm, β = 91.742(5)°. 3 forms monomeric molecules with the [Me2Si(NPEt3)2] ligand bound in a chelating fashion with Mn-N bond lengths of 212.9 pm in average.
Ubergangsmetallkomplexe mit Schwefelliganden, CIX. Synthese und Reaktivität von meso-[Ru(L)('buS5')]-Komplexen mit L = NO+, CO, PR3 (R = Me, Ph, Cy), pyr, CN-, N2H4, NH2NHR (R = Me, Ph), NH2NMe2, NH3, NH2Ph, NHEt2 ('buS5' - H2 = 2,2'-Bis(2-mercapto-3,5-di-t-butylphenylthio)di-ethylsulfid) / Transition Metal Complexes with Sulfur Ligands, CIX. Synthesis and Reactivity of meso-[Ru(L)('buS5')] Complexes with L = NO+, CO, PR3 (R = Me, Ph, Cy), pyr, CN-, N2H4, NH2NHR (R = Me, Ph), NH2NMe2, NH3, NH2Ph, NHEt2 ( 'buS5' - H2 = 2,2'-Bis(2-mercapto-3,5-di-t-butylphenylthio)diethylsulfide)
Authors: Sellmann Dieter , Rohm Christine , Moll Matthias , Knoch Falk 
Published: February 2015

In a search of transition metal complexes with sulfur dominated coordination spheres and free coordination sites for the binding of small molecules, [Ru(L)('buS5')] complexes with the sterically demanding pentadentate thioether-thiolate ligand 'buS5'2- ( 'buS5'2- = 2,2'-Bis(2-mercapto-3,5-di-t-butylphenylthio)diethylsulfide(2-)) have been synthesized.
Reaction of [RuCl3(NO)(PPh3)2] with 3,5-di(t-butyl)benzene-1,2-dithiolate, ′buS2'2-, yields the 16 electron complex [Ru(NO )('buS2')2]- which is isolated as the NBu4
+-salt, 1. According to the NMR spectra, 1 contains a two-fold axis or a mirror plane. Alkylation of 1 with bis(β-bromethyl)sulfide under reflux leads stereoselectively to meso-[Ru(NO)('buS5')]Br, [2]Br. Reaction of [2]Br with LiBEt3H yields the barely soluble binuclear complex [Ru('buS5')]2, 3, with [Ru('buS5')Ru(NO)('buS2')('buS2'- C2H4SH)], 4, as a by-product. 4 ·THF, 4a, has been characterized by X-ray structure analysis.
Reactions of 3 with σ-π- and σ-ligands yield mononuclear meso-[Ru(L)('buS5')] complexes which have been isolated and characterized with L = CO, PMe3, PPh3, PCy3, pyr, CN-, 5 - 10, NH2NHPh, NH2NHMe, NH2NMe2, NH2Ph und NHEt2, 13-17. Complexes 5 -10 are stable compounds. Complexes 13-17, however, are sensitive towards oxidation and/or substitution. Coordination of L = N2H4 and NH3 to 3 leads to insoluble [Ru(L)('buS5')]x complexes.
Koordinationschemie π-gebundener Cyclopentadienyl-Chalcogeno-Ether, II. Palladium(II)- und Platin(II)-Komplexe von [C5(SMe)5]Mn(CO)3, [C5Cl2(SMe)3]Mn(CO)3 und [C5Cl2(SMe)2(PPh2)]Mn(CO)3./ Coordination Chemistry of π-Bonded Cyclopentadienyl Chalcogeno Ethers, II. Palladium(II) and Platinum(II) Complexes of [C5(SMe)5]Mn(CO)3, [C5Cl2(SMe)3]Mn(CO)3 and [C5Cl2(SMe)2(PPh2)]Mn(CO)3
Authors: Sünkel Karlheinz , Blum Adrian 
Published: February 2015

Abstract
Treatment of the cymantrene thioether [C5(SMe)5]Mn(CO)3 (IIb) with Na2PdCl4 or K2PtCl4 yields the bimetallic chelate complexes [C5(SMe)5]Mn(CO)3*MCl2 (M = Pd (2) or Pt (3)). Similarly, the S,P-chelate complexes [C5Cl2(SR)2(PPh2)]Mn(CO)3*PdCl2 (R = Me (4a), Ph (4b)) can be obtained from the corresponding mononuclear cymantrene derivatives and Na2PdCl4 or (PhCN)2PdCl2. Analysis of the 1H NMR spectra only allows for the Pt complex the identification of one meso form, which seems to be favoured by 2:1, together with the D,L forms. The crystal structures of [C5Cl2(SMe)3]Mn(CO)3*PdCl2(1, C11H9Cl4MnO3PdS3, triclinic, P1̄, a = 7.617(3) Å , b = 10.528(4) Å ,c = 12.473(5) Å , α = 72.95(3)°, β = 84.94(3)°, γ = 88.75(3)°, V = 952.6(6) Å3, Z = 2), 2 (C13H15Cl2MnO3PdS5, orthorhombic, Pn21/c, a = 12.739(5) Å , b = 9.992(3) Å , c = 16.884(5) Å , V = 2149(1) Å, Z = 4), and 4 (C23H18Cl6MnO3PPdS2, monoclinic, P21/c, a = 13.199(4) Å , b = 29.198(11) Å , c = 15.921(7) , β - 101.41(3)°, V = 6015(4) Å3, Z = 8) are reported and compared with each other and other bimetallic metallocene phosphine and thioether derivatives.
Synthese dreizähniger Phosphanliganden RP[(CH2)n]2 (Y = OR′ oder CO2R′, n = 1 oder 2) sowie einiger zweizähniger chiraler Phosphane R2PCH(CH3)CO2Me / Synthesis of Tridentate Phosphine Ligands RP[(CH2)nY]2 (Y = OR′ or CO2R′, n = 1 or 2) and Some Bidentate Chiral Phosphines R2PCH(CH3)CO2Me
Authors: Wolfsberger Werner , Bank Jürgen , Werner Helmut 
Published: February 2015

Abstract
The bis(γ-alkoxypropyl)phosphines RP(CH2CH2OR′)2 1-4 were prepared by the reaction of RPLi2 (generated by lithiation of RPH2 with n-BuLi) with ClCH2CH2OR′. Deprotonation of the alkyl group R of RPH2 by n-BuLi and other side reactions leading preferably to diphosphines of the formula R [R′O(CH2)2]PP[(CH2)2OR′]R are responsible for the low yields of 1-4. The bis(propionate) analogues PhP(CH2CH2CO2R′)2 5 and 6 were readily accessible by hydrophosphination of methyl and ethyl acrylate with phenylphosphine, whereas the corresponding compounds RP(CH2CO2R′)2 7 -14 were best prepared by desilylation of RP(SiMe3)2 with C1CH2CO2R′. A similar reaction between R2PSiMe3 and the commercially available R - (+) - ClCH(CH3)CO2Me resulted in the formation of the chiral phosphinoesters R2PCH(CH3)CO 2Me 15-17. In the case of 15 and 16 partial racemation took place during the preparation, whereas 17 could be isolated in an enantiomerically pure form.
Two Modifications of Hg5Re2O10
Authors: Schriewer-Pöttgen Marietta S. , Jeitschko Wolfgang 
Published: February 2015

Abstract
The previously reported mercury perrhenate Hg5Re2O10, prepared hydrothermally, has now been obtained by reaction of HgO with the mercury(II) metaperrhenate Hg(ReO4)2 in sealed silica tubes. A second modification of this compound can be obtained by reaction of elemental mercury with Hg(ReO 4)2 also in sealed silica tubes. Its crystal structure has been determined from single-crystal X-ray data: P21/c, a - 861.5(1), b = 1200.9(2), c = 1203.9(2) pm, β = 97.15(1)°, Z = 4, R = 0.024 for 1733 structure factors and 105 variables. Both modifications may be represented by the formula Hg2+-2Hg2O - 2ReO4-, indicating that mercury occurs in oxidation states I and II. In both modifications the mercury and some oxygen atoms form two-dimensionally infinte, puckered, cationic nets of the composition (Hg2+-2Hg2O)n , which are separated by the ReO4- tetrahedra. In the modification reported earlier the mercury oxygen nets consist of condensed 16-membered rings, while the nets of the present modification contain 10- and 22-membered rings.
Synthese eines Pyrochlors mit TiII: (Ta0.67TiII
0.33)2Sm2O7/ Synthesis of a Pyrochlore Containing TiII: (Ta0.67TiII
0.33)2Sm2O7
Authors: Peters E. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
High temperature reactions using a CO2-LASER led to a TiII containing phase of the composition (Ta0.67TiII
0.33Sm2O7, space group O7
h - Fd3̄m (No. 227), a = 10.385(2) Å . The oxidation state TiII which is stabilized by incorporation into the cubic pyrochlore structure was proved by the statistical occupation of the 16c point position by a Ta:Ti ratio of 2:1.
Reindarstellung und Kristallstruktur von Lithiumnitriddibromid, Li5NBr2 / Preparation and Crystal Structure of Lithium Nitride Dibromide, Li5NBr2
Authors: Marx Rupert , Mayer Hans Michael 
Published: February 2015

Abstract
Single phase Li5NBr2 was prepared by the reaction of Li3N and dry, OH-free LiBr under inert gas at 430 °C. In the quasi-binary system Li3-2xN1-xBrx, Li5NBr2 is the second most nitride rich compound after Li10N3Br. Following unit cell indexing using laboratory X-ray powder data the previously unknown structure of Li5NBr2 was solved from neutron powder diffraction data recorded at the flat-cone and powder diffractometer E2 at the rebuilt reactor BERII in Berlin. The title compound crystallizes in the orthorhombic space group Immm (No. 71), a = 603.79(4), b = 1181.3(1), c = 390.14(3) pm with two formula units per unit cell. The L i-N -sublattice comprises linear chains of vertex sharing Li6N-octahedra which are aligned along the short c-axis and are separated by chains of bromine atoms. The N-Br arrangement may be regarded as an ordered AX2 variant of a cubic close packing involving two kinds of atoms. Lithium atoms occupy the tetrahedral holes formed by one nitrogen and three bromine atoms, as well as the N - N edges of the N2Br2 tetrahedra.
Synthese und Struktur des Au12Pd-Clusters [(Ph3PAu)8(AuCl)4Pd] / Synthesis and Structure of the Au12Pd Cluster [(Ph3PAu)8(AuCl)4Pd]
Authors: Laupp Martin , Strähle Joachim 
Published: February 2015

Abstract
Photolysis of a mixture of (Ph3P)2Pd(N3)2, Ph3PAuN3 and PhsPAuCI yields [(Ph3PAu)8(AuCl)4Pd] after chromatographic separation. The cluster crystallizes in the triclinic space group P1̄ with a = 1675.45(8), b = 1870.57(6), c = 2673,15(9) pm, α = 82.30(3)°, β = 75.90(3)°, γ = 73.02(3)°, Z = 2. The twelve gold atoms form an icosahedron with the Pd atom in its center, and distances Pd-Au between 271.0(3) and 278.2(4) pm. The Au-Au distances range from 277.1(2) to 298.3(2) pm.
Die Synthese und Struktur von Clusteraziden: A4[Nb6Cl12(N3)6](H2O)2 mit A=Rb. Cs / Synthesis and Structure of the Cluster Azides: A4Nb6Cl12(N3)6](H2O)2 with A=Rb, Cs
Authors: Reckeweg Olaf , Meyer H.-Jürgen 
Published: February 2015

Abstract
The new compounds A4[Nb6Cl12(N3)6](H2O)2 (A = Rb, Cs) were synthesized from In4[Nb6Cl12Cl6] by substituting six terminal Cl ligands and the In+ ions in methanolic solution. An X-ray structure refinement was performed on single-crystal data of Rb4[Nb6Cl12(N3)6](H2O)2 (1) (space group P1̄, Z = 1, a = 912.5(1) pm, b = 937.2(1) pm, c = 1062.0(1) pm, α = 96.88(2)°, β = 101.89(1)°, γ = 101.44(2)°) and Cs4[Nb6Cl12(N3)6](H2O)2 (2) (space group PI, Z = 1, a = 920.9(5) pm, b = 947.9(7) pm, c = 1091.8(7) pm, α = 96.89(6)°, β = 103.35(5)°, γ = 101.60(5)°. Each of the centrosymmetric [Nb6Cl12(N3)6]4- ions of the isotypic compounds contains six terminal azide groups at the corners of the octahedral niobium cluster (d̄Nb-N = 226(1) pm (1), 225(1) pm (2), bond angles Nb-N-N 120-127°). The [Nb6Cl12(N3)6]4- ions are linked via Rb-N and Rb-Cl interactions of the Rb+ ions to form a three-dimensional structure. Crystals of the compounds react explosively on heating or mechanical pressure.
Notizen: Darstellung und Kristallstruktur von Cs3ClO / Preparation and Crystal Structure of Cs3ClO
Authors: Feldmann Claus , Jansen Martin 
Published: February 2015

Abstract
The preparation and crystal structure of Cs3ClO (a = 9,442(6), b = 4,452(2), c = 16,344(10) Å ) is reported. In contrast to other compounds M3XO (M = alkali metal; X = halide, auride) Cs3ClO does not crystalize as an anti perovskite or a related structure, but in the anti-NH4CdCl3 type of structure.
Notizen: Zur Struktur des Diazadimethylstannetidinderivats [(CH3)2Sn(NC(CH3)3)2GaCH3]2/ The Structure of the Diazadimethylstannetidine Derivative [(CH3)2Sn(NC(CH3)3)2GaCH3]2
Authors: Hausen Hans-Dieter , Kuhnle Rainer , Weidlein Johann 
Published: February 2015

Abstract
The title compound Me2Sn(NtBu)2GaMe (Me = CH3, tBu = C(CH3)3) is formed in only low yield by the reaction of diazadistannetidine [Me2SnNtBu]2 with galliumtrimethyl. It is dimeric in the solid state and crystallizes in the monoclinic space group P21/n with the cell parameters a = 923.4(1), b = 1832.8(2), c = 972.9(1) pm, β = 111.24(1)°, and Z = 2. The centrosymmetric dimer (point symmetry Q ) consists of three consecutive edge-sharing four-membered rings; the central Ga2N2 unit is formed by two Ga ← N donor-acceptor bonds of 203.7 pm. The two SnN2Ga rings and the central ring form angles of ± 113.7°. The compound is very similar to, but not isotypic with the homologous In/Si compound [Me2Si(NtBu)2InMe]2 [5],
Notizen: New Colchicine and Homoaporphine- N-Oxide Alkaloids from Colchicum Ritchii: The First Homoaporphine TV-Oxide Found in Nature
Authors: Abu Zarga Musa H. , Al-Qawasmeh Raed A. , Sabri Salim S. , Al-Tel Taleb H. , Voelter Wolfgang 
Published: February 2015

Abstract
From Colchicum ritchii R.Br (Liliaceae) of Jordanian origin, the new colchicine-type alkaloid (-)-O -methylspeciosine (1), the known alkaloid (-)-speciosine (2) and two new homoaporphine- N-oxides are isolated and characterized: (+)-kreysigine-N-oxide (5) and (+)-szovitsamine-N-oxide (6). Additinally, two photoisomers of the cholchicine alkaloids are identified after their isolation and their 1H and 13C NMR data reinvistigated: β-lumicornigerine (3) and β-lumidemecolcine (4).
Ubergangsmetallkomplexe mit Schwefelliganden, CXVI. Carbonylkomplexe mit [MoS4]-Zentren in mittleren und hohen Oxidationsstufen / Transition Metal Complexes with Sulfur Ligands, CXVI. Carbonyl Complexes with [MoS4] Centers in Medium and High Oxidation States
Authors: Sellmann Dieter , Kremitzl Hans-Jörg , Knoch Falk , Moll Matthias 
Published: February 2015

In the quest of suitable precursors for the synthesis of Mo(IV) carbonyl complexes the compounds [Mo(CO)2(PCy3)(′buS4′)] (3) and [Mo(CO)2(PCy3)(′S4′)] (4) [′buS4′2- = 1,2-bis(2-mercapto-3,5-di-t-butyl-phenylthio)ethane(2-); ′S4′2- = 1,2-bis(2-mercaptophenylthio)ethane(2-)] were synthesized via CO substitution from [Mo(CO)3(′buS4′)] (13) and [Mo(CO)3(′S4′)](14). 4 was characterized by X -ray structure analysis and exhibits, due to the sterically demanding PCy3, a strongly compressed [Mo(′S4′)] core.
Intramolecular redox reactions of 3, 4 and, in addition, [Mo(CO)2(PMe3)(′S4′)] (15) leading to thioether dealkylation via loss of C2H4 from the ′RS4′2- ligands and Mo(II)→ Mo(IV) oxidation yielded the Mo(IV) complexes [Mo(CO)(PCy3)(′buS2′)2] (6), [Mo(CO)-(PCy3)(′S2′)2] (7) and [Mo(CO)(PMe3)(′S2′)2] (8) [′buS2′)2]= 3,5-di-t-butyl-1,2-benzenedithiolate(2-), ′S2′2- = 1,2-benzenedithiolate(2-)]. Depending on the nature of the phosphines and the R substituents of the ′RS4′2- ligands, the syntheses required very specific reaction conditions ranging from thermolysis in vacuo to heating in boiling THF. For instance, [Mo(CO)2(PCy3)(′S4′)] (4) decomposes in CH2Cl2 solution even at ambient temperature yielding the binuclear Mo(II) complex [Mo(CO)(μ-′S4′)]2 (10), which was characterized by an X-ray structure determination. Thermolysis of 4 in vacuo at 80 °C , however, results in the formation of the Mo(IV) complex 7. By optimizing the reaction conditions preparative amounts of the prototype [Mo(CO)2(′buS2′)2] (1) have now also become accessible.
These findings can be rationalized in part on the basis of results obtained from cyclic voltammetry. The redox potentials of the Mo(IV) complexes are drastically shifted by about -0.5 V per substitution of CO by PR3, and the substitution of ′S2′2- by ′buS2′2- ligands causes a negative shift in the range from 0.03 V to 0.18 V.
The results of IR spectroscopical m onitoring the substitution of CO by PMe3 in [Mo(CO)(PMe3)(′RS2′)2] yielding [Mo(PMe3)2(′RS2′)2] suggested an associative substitution mechanism via the intermediate [Mo(CO)(PMe3)2(′RS2′)2]. The formation of [Mo(CO)-(PMe3)(′buS2′)2] (12) from [Mo(PMe3)2(′buS2′)2] (9) and CO under standard conditions further shows that the direct coordination of CO to Mo(IV ) centers is also possible if these centers are surrounded by thiolate donors. The results are discussed with respect to the reactivity of the Mo centers of the FeMo cofactors in nitrogenases.
Ba2Na(CN2)(CN)3, ein neues Cyanamid-cyanid mit interpenetrierenden Teilstrukturen / Ba2Na(CN2)(CN)3, a Novel Cyanamide Cyanide with Interpenetrating Substructures
Authors: Berger Ute , Schnick Wolfgang 
Published: February 2015

Abstract
Ba2Na(CN2)(CN)3 was obtained by the reaction of Ba2N with melamine and NaCN at 700 °C. The compound was structurally characterized by single-crystal X-ray investigations (Fd3̄m, a = 1518.8(3) pm, Z = 16). In the crystal structure the Ba2+ ions form a cubic close packed arrangement, the Na+ and the CN2-
2 ions occupy the octahedral interstices. The CN-ions are located within the close packed Ba2+ layers. The unit cell of Ba2Na(CN2)(CN)3 contains two interpenetrating substructures of the zinc-blende structure type, building up a variant of NaTl. A reversible phase transition has been observed during cooling of the compound. Whereas the Ba2(CN2)(CN)3 sublattice remains nearly unaffected in this process, the Na+ ions of the low-temperature phase are statistically distributed on two crystallographic positions.
Synthese und Struktur von Zn(HSO4)2(H2SO4)2 und Cd(HSO4)2 / Synthesis and Structure of Zn(HSO4)2(H2SO4)2 und Cd(HSO4)2
Authors: Kemnitz E. , Werner C. , Stiewe A. , Worzala H. , Trojanov S. 
Published: February 2015

Abstract
From the binary systems M2SO4/H2SO4 (M = Zn, Cd), two new hydrogen sulfates, (Zn(HSO4)2(H2SO4)2 and Cd(HSO4)2, have been synthesized and structurally characterized. Both compounds crystallize in the monoclinic space group P21/c with cell parameters a = 5.047(2), b = 15.430(4), c = 7.958(3) Å and β = 104.16(4)° (Z= 2) for Zn(HSO4)2(H2SO4)2 and a = 5.339(1), b = 13.351(3), c = 8.508(2) Å and β = 92.22(3)° (Z = 4) for Cd(HSO4)2. In the zinc compound there are slightly distorted centrosymmetric ZnO6 octahedra with Zn-O distances of 2.05-2.13 A which are sharing corners with SO4 tetrahedra. HSO4 and H2SO4 tetrahedra are linked via hydrogen bonds to form layers perpendicular to the c-axis. In the crystal structure of Cd(HSO4)2 there exist two crystallographically different HSO4 tetrahedra. The CdO6 octahedra with Cd-O distances between 2.24 and 2.31 A are strongly angle-distorted. Besides hydrogen bonds of medium strength (do···o = 2.66 Å) there are also much more weaker ones (do···o = 3.04 Å). Considering these latter ones zigzag chains in z-direction can be recognized.
The relatively low stability of Cd(HSO4)2 in comparison with other metal-II-hydrogen sulfates is discussed with respect to its structural pecularities.
Methanolothermale Synthese und Kristallstruktur von Tetraselenidoarsenaten( V) und -antimonaten(V) des Rubidiums und Cäsiums / Methanolothermal Synthesis and Crystal Structure of Tetraselenidoarsenates(V) and -antimonates(V) of Rubidium and Cesium
Authors: Wachhold Michael , Sheldrick William S. 
Published: February 2015

Abstract
Tetraselenidoarsenates(V) and -antimonates(V), Rubidium, Cesium, Methanolothermal Synthesis, Crystal Structure Methanolothermal reaction of M2CO3 (M = Rb, Cs) with E2Se3 (E = As, Sb) and Se at temperatures in the range 180 -200°C leads to the formation of tetraselenidoarsenates(V) and -antimonates(V) M3ESe4 in moderate to quantitative yields. All four compounds crystallize in the (NH4)3AsS4 structure type (space group Pnma) and contain isolated slightly distorted tetrahedral ESe3-
4 anions with crystallographic CS symmetry. Both of the independent cations are coordinated in an irregular manner by seven Se atoms.
Preparation and Crystal Structure of the Mercury(I) Dimolybdate(VI) Hg2Mo2O7
Authors: Wessels Annemarie L. , Jeitschko Wolfgang 
Published: February 2015

Abstract
Crystal Structure, Magnetic Susceptibility, Mercury Molybdates(VI) Yellow, flat, needle-shaped, diamagnetic crystals of Hg2Mo2O7 were obtained by decomposition of Hg2MoO4 in evacuated, sealed silica tubes at 550 °C. Their crystal structure was determined from four-circle diffractometer data: P1̄, a = 709.7(2), b -714.4(2), c = 803.8(2) pm, α = 64.89(1)°, β = 66.09(1)°, γ = 66.45(1)°, Z = 2, R = 0.030 for 3165 structure factors and 66 variables. The molybdenum atoms are coordinated by four oxygen atoms at 171 to 195 pm in a very distorted tetrahedral arrangement. These tetrahedra are linked via a common oxygen atom, thus forming Mo2O7 groups. The tetrahedral oxygen coordination of each molybdenum atom is augmented by two additional oxygen atoms at 218 to 231 pm, which leads to a distorted octahedral coordination for the molybdenum atoms. These MoO6 octahedra are connected via common corners and edges and in this way they form two-dimensionally infinite sheets, which are separated by the Hg2 pairs (Hg-HG distance: 252.2 pm).
The Oxidation of Partially Acylated Myoinositols
Authors: Kurzer Frederick , Chapman Dennis 
Published: February 2015

Abstract
1,3,4,6-Tetrakis-and 1,3,4,5,6-pentakis-acylmyoinositols are obtained by the controlled catalyzed acylation of myoinositol. The extent of the substitution depends both on the reaction conditions and the structure of the acylating agent, including steric factors. Chromic acid oxidation converts the acylmyoinositols into the corresponding 2-ketones. Under electron impact, the compounds undergo stepwise deacylation.
Methansulfinylchlorid-Lewissäure-Addukte CH3S(Cl)OMF5 (M = As, Sb) und Kristallstruktur von CH3S(Cl)OSbCl5 [1] / Methanesulfinylchloride Lewis Acid Adducts CH3S(Cl)OMF5 (M = As, Sb) and Crystal Structure of CH3S(Cl)OSbCl5 [1]
Authors: Minkwitz Rolf , Lohmann Ulrike , Preut Hans 
Published: February 2015

Abstract
CH3S(0)C1 reacts in HF as solvent with MF5 (M = As, Sb) to give products CH3S(Cl)OMF5 (M = As, Sb). The new compounds are stable below 253 K and were charac­ terized by Raman and NMR spectroscopy.
In addition, the crystal structure of CH3S(Cl)OSbCl5 has been determinated. The complex crystallizes in the monoclinic space group P21/n with a = 644.3(5), b = 1905.9(14), c = 900.0(7) pm, β = 99.27(6)° with four formula units per unit cell.
Zwischenmolekulare Wechselwirkungen bei RSbCl2 und die Bildung cyclischer Organoantimon(III)-chalkogenide, (RSbE)n [R = (Me3Si)2CH, E = S, Se, Te] / Intermolecular Interactions of RSbCl2 and Formation of Cyclic Organoantimony(III) Chalcogenides, (RSbE)n [R = (Me3Si)2CH, E = S, Se, Te]
Authors: Mohammed Mohammed A. , Ebert Klaus H. , Breunig Hans Joachim 
Published: February 2015

Abstract
Alkylantimony Dichloride, Cyclostibane Chalcogenides The crystal structure of the compound (Me3Si)2CHSbCl2 (1) has been determined as obtained from the melt. It contains dimers with in­ termolecular Sb···Cl distances of 351.8 (1) pm. Reactions of 1 with the corresponding sodium chalcogenides yield the products (RSbS)n (2), (RSbSe)n (3) and (RSbTe)n (4) [R = (Me3Si)2CH], The mass spectra of 2-4 give peaks for the dimers, trimers and tetramers, while the NM R spectra of solutions of 2-4 in CDCl3 show that the trimers are the most abundant species in ring-ring-equilibria.