bluuebunny/crossref_metadata_2025_split huggingface dataset:
Zur Kenntnis der Tief-und Hochtemperaturform eines Oxidarsenats des Zinks: ZnOZn3(AsO4)2
Authors: Frerichs D. , Park C.H. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single crystals of the low (t-) and high (h-) temperature form of ZnOZn3(AsO4)2 have been prepared by flux and by CO2-LASER techniques respectively. Both compounds crystal­lizes monoclinic, space group C5
2h-P21/n with the lattice parameters t-ZnOZn3(AsO4)2: a = 9.807(3), b = 8.180(2), c = 9.967(2) Å , β = 116.53(2)°, Z = 4 and h -ZnOZn3(AsO4)2: a = 9.743(3), b = 8.163(8), c = 17.933(2) Å , β = 91.55(2)°, Z = 8. Similarities and differences of the crystal structures will be discussed.
Photoredox Decomposition of [Cobalamin-μ-NC-FenII(CN)5]3- Induced by Metal-to-Metal Charge Transfer Excitation
Authors: Kunkely H. , Vogler A. 
Published: February 2015

Abstract
In the presence of oxygen aqueous solutions of the binuclear complex [cobalamin-μ-NC-Fe(CN)5]3- undergo a redox photolysis (ø ~ 2 x 10-3 at λirr = 405 nm) which yields aquocoba-lamin and [Fe(CN)6]3- It is suggested that this photoreaction is induced by direct metal-to-metal charge transfer (MMCT) excitation. On the contrary, [cobalamin-μ-NC-Ru(CN)5]3- is photo-inert because a reactive MMCT state is not accessible.
Quaternary Thorium Transition Metal Pnictide Oxides: ThCu1-xPO, ThCuAsO, and Th2Ni3-xP3O
Authors: Albering Jörg H. , Jeitschko Wolfgang 
Published: February 2015

Abstract
The new compounds ThCu1-xPO and ThCuAsO with ZrCuSiAs-type structure were pre­pared in well crystallized form by chemical vapor transport reactions. Th2Ni3-xP3O with a new structure type was obtained by reaction of ThO2 with the other elemental components in an alumina crucible at high temperatures. The crystal structures of the three compounds were determined from single-crystal X-ray data. ThCu1-xPO: P4/nmm, a = 389.43(4), c -828.3(1) pm, R = 0.024 for 13 variable parameters and 338 structure factors; ThCuAsO: P4/ nmm, a = 396.14(5), c = 844.0(1) pm, R = 0.028 (13 variables and 379 F values); Th2Ni3-xP3O : P4/nmm, a = 394.62(4), c = 1723.2(3) pm, R = 0.018 (27 variables and 374 F values). The refinement of the occupancy parameters revealed significant deviations from the ideal values for the transition metal sites for two compounds resulting in the exact compositions ThCu0.938(4)PO and Th2Ni2.45(1)P3O . Magnetic susceptibility measurements indicate Pauli paramagnetism for ThCu1-xPO . The crystal structures of these compounds are closely related. They belong to a large family of tetragonal structures of which the ThCr2Si2-and the PbFCl-type structures are well known examples.
Die Kristallstruktur von [Mn(CH3CN)6][MnI4]
Authors: Weller Frank , Mai Hans-Joachim , Dehnicke Kurt 
Published: February 2015

Abstract
[Mn(CH3CN)6][MnI4] crystallizes from acetonitrile solutions of Mnl2 as yellow single crystals which were characterized by their IR spectrum and by a crystal-structure analysis. Space group P21/n, Z = 4, structure solution with 3742 observed unique reflections with Fo >5σ(Fo), R = 0.050. Lattice dim ensions at 20°C: a = 1258.0(5), b = 1244.7(2), c = 1753.3(6) pm, β = 92.22(3)°. The compound forms octahedral cations [Mn(CH3CN)6]2+ with site symmetry Ci with average Mn-N bond lengths of 222.3 pm and te­trahedral anions [Mnl4]2- without symmetry with average bond lengths MnI of 271.3 pm.
Structure of Chloro(cyclopentadienone)- (cyclopentadienyl)ruthenium and its Cytotoxic Activity
Authors: Yamazaki Yoshimitsu , Goto Midori , Kageyama Yu-ichi , Tomohiro Takenori , Okuno Hiroaki 
Published: February 2015

Abstract
The structure of Ru(cpO)(cp)Cl complex (3), which was precipitated from aqueous solutions of Ru(cp)2Cl+PF6
- (1), was determined by X-ray crystallographic analysis. The Ru-halogen bond distance was shorter and the dihedral angle be­ tween the rings was larger than the values re­ ported for the corresponding Br analogue, Ru(cpO)(cp)Br (4). The complex 3 (IC50 109 μM) was more cytotoxic than 1 (IC50 163 μM) against mouse sarcoma S180 cells, but less toxic than 4 (IC50 72 μM).
Pb6(AsO4)[B(AsO4)4] - ein neuartiger Kristallstrukturtyp im System PbO/B2O3/As2O5 mit einem Beitrag über Pb(BAsO5)/Pb6(AsO4)[B(AsO4)4] - a New Crystal Structure Type in the System PbO/B2O3/As2O5 with Remarks about Pb(BAsO5)
Authors: Park Cheong-Hwa , Bluhm Karsten 
Published: February 2015

Abstract
Single crystals of Pb6(AsO4)[B(AsO4)4] (I) and Pb(BAsO5) (II) were obtained by melting B2O3, As2O5 and PbO at 800 °C. X-ray investigation led to the space group (I): S4
1 -P4̄ (Nr. 81) with a = 715.4(1), c = 976.2(3) pm, Z = 1 and (II): C3
2 -P31 (Nr. 144) with a = 712.2(1), c = 693.5(2) pm, Z = 3. While (II) is isotypic to the Stillwellite structure, Pb6(AsO4)[B(AsO4)4] represents a completely novel type of crystal structure. Boron and arsenic are tetrahedrally coordinated by oxygen. These polyhedra form two kinds of isolated anions: AsO4
3- and B(AsO4)4
9-. Lead is eightfold coordinated by oxygen.
Zur Synthese und Kristallstruktur von Dibariumkaliumtrizinkborat Ba2KZn3(B3O6)(B6O13)/Synthesis and Crystal Structure of Di-barium Potassium Tri-zinc Borate Ba2KZn3(B3O6)(B6O13)
Authors: Busche Silke , Bluhm Karsten 
Published: February 2015

Abstract
Single crystals of the new compound Ba2KZn3(B3O6)(B6O13) were obtained by using a B2O3 flux technique; they crystallize in an as yet unknown structure type. X-ray investigations led to the space group Ci
1-P1̄ (Nr.2) with lattice parameters a = 705.2(2), b = 712.5(2), c = 1880.3(6), a = 93.43(3)°, β = 90.72(2)°, γ = 119.57(2)°, Z = 2. The structure contains (B3O6)3--rings and a new discrete (B6O13)8- anion, which is composed of two BO4 and two B2O5 units. Zn2+ is tetrahedrally coordinated by oxygen and two out of three tenfold coordinated Ba-sites are statistically occupied by Ba2+ and K+.
Zur Kenntnis zweier Formen des Zinkorthoarsenates: α-Zn3(AsO4)2 und β-Zn3(AsO4)2/On Two Forms of Zinc Orthoarsenate: α -Zn3(AsO4)2 and β-Zn3(AsO4)2
Authors: Frerichs D. , Park C. H. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single crystals of two forms of zinc orthoarsenate (α-Zn3(AsO4)2 (I) and β-Zn3(AsO4)2 (II)) have been prepared by flux techniques. Both compounds crystallize monoclinically, space groups (I): C2h
5-P21/c, (II): C2h
5-P21/n, with the lattice parameters (I): a = 6.306(2), b = 8.652(2), c =1.321(4) Å, β = 92.25(5) °, Z = 4 and (II): a = 5.281(1), b = 8.494(2), c = 7.726(3) Å, β = 96.39(3)°, Z = 2. α-Zn3(AsO4)2 is isotypic to I-Cu3(AsO4)2 and β-Zn3(AsO4)2 to γ-Zn3(PO4)2. Similarities and differences of the crystal structures are discussed.
Notizen:1,3-Dimethoxy-6H- benzo[b]naphtho[1,2-d]pyran-6-thione, a Thionolactone-Bridged Axially Prostereogenic Biaryl
Authors: Peters Karl , Peters Eva-Maria , Bringmann Gerhard , Schupp Olaf 
Published: February 2015

Abstract
The title compound was prepared from the cor­responding “ordinary” oxolactone bridged biaryl using Lawesson’s reagent. It crystallizes from dichloromethane / petroleum ether in the mono­clinic system, space group P21/a; a = 1115.7(2),b = 1383.9(2), c = 1042.0(1) pm and β = 106.67(1)°.
Weitere Verbindungen mit isolierten quadratischen PdO4-Polygonen: BaPdLn2O5 (Ln=Eu, Gd, Dy, Ho) / Compounds Containing Isolated Square Planar PdO4 Polygons: BaPdLn2O5 (Ln=Eu, Gd, Dy, Ho)
Authors: Müller-Buschbaum Hk. , Wulff L. 
Published: February 2015

Abstract
New compounds of the composition BaPdLn2O5 (Ln = Eu, Gd, Dy, Ho) have been prepared by crystallization from flux. They crystallize isotypic to BaPtLn2O5, space group D5
4h-P4/ mbm. Eu: a = 6.6359(6), c = 5.885(3) Å ; Gd: a = 6.608(3), c = 5.873(3) Å ; Dy: a = 6.5431(7), c = 5.8574(8) Å ; Ho: a = 6.522(4), c = 5.855(5) A , Z = 2. The crystal structure is characterized by isolated planar PdO4 polygons incorporated into a framework of edge-and corner-sharing doubly capped BaO8 cubes and edge-and face-sharing LnO6 prisms.
Mit Bor besetzte kondensierte Cluster in Ta5G e3By (y ≈ 0,7) / Boron Occupied Condensed Clusters in Ta5Ge3By (y ≈ 0.7)
Authors: Peters E. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Tantalum, Germanium, Cluster Bronze coloured, rod-shaped crystals of Ta5Ge3By have been prepared by CO2-LASER-techniques. X-ray-methods confirm the well known hexagonal Mn5Si3 type, space-group D3
6h-P63/mcm, a = 7.6276(6) and c = 5.2781(9) Å . The Ta6-clusters are centred by boron atoms.
Zur Kenntnis des ersten Alkalimetall-Cadmium-Halogeno-Oxovanadats: K4CdV5O15Cl / On the First Alkaline-Cadmium-Vanadium Oxide Halide: K4CdV5O15Cl
Authors: Münchau S. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single crystals of K4CdV5O15Cl have been prepared by crystallization from melts. The yellow crystals show tetragonal symmetry, space group C1
4-P4, a = 9.097(1), c = 5.331(2) Å, Z = 1. K4CdV5O15Cl belongs to the K4CuV5O3Cl type. V (l) forms V2O7 double tetrahedra connected by square V(2)O5 pyramids and CdO4Cl2 octahedra. The crystal structure is dis­cussed with respect to the isotypic compound K4CuV5O15Cl considering a short V(2)-O distance indicative of a vanadinyl group.
1.3.5.7-Tetra-tert-butyl-3.7-dichlor-2.4.6.8.9-pentaaza-1.3.5.7- tetrasilabicyclo[3.3.1.]nonan - Synthese und Kristallstruktur / 1.3.5.7-Tetra-tert-butyl-3.7-dichloro-2.4.6.8.9-pentaaza-1.3.5.7- tetrasilabicyclo[3.3.1.]nonane - Syntheses und Crystal Structure
Authors: Rakebrandt Hans-J. , Klingebiel Uwe , Noltemeyer Mathias , Zak Zdirad 
Published: February 2015

Abstract
The reaction of tert-butyltrichlorosilane with an excess of ammonia leads to the formation of a tetrasilabicyclo[3.3.1.]nonane, an NH-bridged cyclotetrasilazane. The crystal structure of the compound (Me3CSi)4Cl2(NH)5 is described.
New Preparative Methods for the Halides of Titanium(II) and Vanadium(II): Reduction of Titanium(IV) Halides with Sodium and Oxidation of Bis(mesitylene)vanadium(0)
Authors: Calderazzo Fausto , Benedetto Giuseppe E. De , Engler Ulli , Ferri Isabella , Pampaloni Guido , Wagner Trixie 
Published: February 2015

Abstract
TiCl4(THF)2 reacts with two equivalents of sodium in THF to afford the soluble TiCl2(THF)n (1), which has been characterized analytically and by spectroscopic and magnetic measurements. By redox reactions. TiCl2(THF)n gives TiCl2(9,10-C10H8O2) (2), or TiCl2(benzoate)2 .(3), with 9,10-phenanthrenequinone or dibenzoylperoxide in toluene, respectively. By operating in 1,2-dimethoxyethane (DME), Na(DME)1.5[TiCl4(DME)] (4), or NaTiCl3(DME)2 have been isolated from the reaction of TiCl4(DME) with one or two equivalents of sodium, respectively. From 4, by cation exchange, PPN[TiCl4(DME)] [PPN = bis(triphenylphosphine)iminium] (5), has been obtained and characterized analytically, spectroscopically and by X-ray diffraction methods. Crystal data: C40HCl4NO2P2Ti. MW = 818.4, space group: Pna21 (N° 33). a = 14.445(2), b = 15.690(2), c = 17.544(2) Å . V = 3976(2) Å3, Z = 4, F(000) = 1692, R = 0.041, Rw = 0.0420. The titanium(III) atom in the anion has the expected cis-octahedral, slightly distorted, geometry. By reaction of TiBr4(DME)0.5 with sodium in DME, TiBr3(DME)1.5 .1.5 DM E (7), is the product. Bis(mesitylene)vanadium(0), Vmes2, reacts with two equivalents of CPh3Cl in DME, to give VCl2(DME)n.
Die Kristallstrukturen der Dysprosium-Komplexe [DyCl3(DME)2] und [DyCl2(THF)5]+[DyCl4(THF)2]- / Crystal Structures of the Dysprosium Complexes [DyCl3(DME)2] and [DyCl2(THF)5]+[DyCl4(THF)2]-
Authors: Anfang Stefan , Dehnicke Kurt , Magull Jörg 
Published: February 2015

Abstract
[DyCl3(DME)2] (DME = 1,2-dimethoxyethane) has been prepared from the known tetrahy-drofuran complex [Dy2Cl6(THF)7] in boiling DME. Both complexes were characterized by structure determinations. [DyCl3(DME)2]: Space group P21/c, Z = 4, lattice dimensions at -70 °C: a = 1141.9(6), b = 884.2(4), c = 1558.3(6) pm, β = 104.83(4)°. The complex has a molecular structure with a distorted pentagonal bipyramidal geometry in which the oxygen atoms of the chelating DME molecules and one chlorine atom occupy the pentagonal plane. [DyCl2(THF)5]+[DyCl4(THF)2]-: Space group C2/c, Z = 4, lattice dimensions at -70 °C: a -1241.4(9), b = 1139.4(6), c = 2735.1(19) pm, β = 91.19(4)°. The complex contains a seven-coordinate cation with axial chloride ligands in a pentagonal bipyramidal structure and a six-coordinate anion with a trans octahedral geometry.
Darstellung, Schwingungsspektren und Normalkoordinatenanalyse der 10B-und 11B-Isotopomeren von [B2(NCS)6]2- sowie Kristallstruktur von (Ph3P=N=PPh3)2[B2(NCS)6] / Preparation, Vibrational Spectra and Normal Coordinate Analysis of the 10B and 11B Isotopomers of [B2(NCS)6]2- and Crystal Structure of (Ph3P=N=PPh3)2[B2(NCS)6]
Authors: Preetz W. , Steuer B. 
Published: February 2015

Abstract
By reaction of [B6H6]2- with a solution of (SCN)2 in dichloromethane in the presence of solid KOH the hexaisothiocyanatodiborate anion [B2(NCS)6]2- is formed and can be isolated by fractionated crystallization. The crystal structure of (PNP)2[B2(NCS)6] has been determined by single crystal X-ray diffraction analysis; triclinic space group P1̄ with a=12,282(5), b=12,416(5), c=14,155(5)Å, a=68,36(5), β=70,59(5), γ=80,93(5)°.The [B2(NCS)6]2- anion reveals a staggered conformation with nearly local D3d symmetry and a B-B bond length of 1,73(2) Å. Using the crystallographic data a normal coordinate analysis has been performed. With a set of 12 force constants (e.g. fd(BB)=3,62, fd(BN)=4,21 mdyn/Å) a good agreement between observed and calculated frequencies for the 10B and 11B isotopomers has been achieved. The potential energy distribution on the force constants reveals strong vibrational couplings within the B2N6 framework.
Metallkomplexe mit biologisch wichtigen Liganden, LXXXIII [1]. Palladium(II)-und Platin(II)-Komplexe mit 2-Hydroxyiminocarboxylaten und ihren Derivaten / Metal Complexes of Biologically Im portant Ligands, LXXXIII [1], Palladium(II) and Platinum (II) Complexes of 2-Hydroxyiminocarboxylates and their Derivatives
Authors: Lampeka Rostislav , Wanje Herbert , Bec Wolfgang 
Published: February 2015

Abstract
Palladium(II), Platinum(II), 2-Hydroxyiminocarboxylate, Oximes of Pyruvoyl a-Amino Acids The synthesis and spectroscopic properties of palladium(II) and platinum (II) chelate com­ plexes with carboxylates of 2-hydroxyiminopropionic, 2-hydroxyimino-3-phenylpropionic acids, with the amide and N-methylamide of 2-hydroxyiminopropionic acid, and with oximes of pyruvoylglycine and pyruvoyl-L-phenylalanine are reported.
Metallkomplexe mit biologisch wichtigen Liganden, LXXXY [1] Koordinationsverbindungen von Cobalt(III), Iridium(III), Ruthenium(II) und Palladium(II) mit Isoxazol-und Isoxazolin-3-carboxylaten / Metal Complexes of Biologically Important Ligands, LXXXV [1] Coordination Compounds of Cobalt(III), Iridium (III), Ruthenium (II) and Palladium(II) with Isoxazole-and Isoxazoline-3-carboxylates
Authors: Lampeka Rostislav , Mihan Shahram , Beck Wolfgang 
Published: February 2015

Abstract
Chelate complexes of 5-phenyl-isoxazole-3-carboxylate (L1) and 5-phenyl-isoxazoline-3-carboxylate (L2) ligands were prepared: Pd(L1)2. Cp*(Cl)Ir(L1), (p-cymene)(Cl)Ru(L1), Pd(L2)2, (Et3P)(Cl)Pd(L2),

, Cp*(I)Co(L2), Cp*(Cl)Ir(L2) (10), and (p-cymene)(Cl)Ru(L2) (Cp* = C5Me5). The structure of 10 was determined by X-ray diffraction.
Die Kristallstruktur von [(THF)2Li(μ2-Cl)2TiCl2(THF)2] / Crystal Structure of [(THF)2Li(μ2-Cl)2TiCl2(THF)2]
Authors: Neumüller Bernhard , Heshmatpou Felora , Dehnicke Kurt 
Published: February 2015

Abstract
The crystal structure of the title com pound has been determined by X-ray methods. Space group C2/c, Z = 4, lattice dimensions at -80 °C: a = 1343.8(2), b = 1031.6(1), c = 1669.4(1) pm, β = 96.47(1)°. The compound forms an ion pair in which the lithium atom is coordinated in a distorted tetrahedral geometry by two THF molecules and by two chlorine atoms. The halide atoms have a μ2-bridging function, coordinating the lithium and the titanium center. The titanium atom possesses a distorted octahedral environment with two THF ligands in trans-position.
Hochdruckreaktionen quaternärer Chalkogenide mit Schichtstruktur / High-Pressure Reactions of Quaternary Layered Chalcogenides
Authors: Berand N. , Haeuseler H. , Range K.-J. 
Published: February 2015

Abstract
The layered chalcogenides CoGa1.7Ti0.3S4, CoGa1.7V0.3, CoGa1.6Cr0.4S4, CoGaInS4, MnGa1.5Cr0.5S4, MnGa1.4Sc0.6S4, MnGa0.8In1.2S4, MnIn2S1.6Se2.4 and CdIn2S2.1 Se1.9 have been investigated under high-pressure - high-temperature conditions (p ≤ 60 kbar, T ≤ 1600°C). MnIn2S1.6Se2.4 and CdIn2S2.1,S1.9 show a phase transition to spinel-type compounds (a = 11.022(2) and a = 11.059(1) Å, respectively). MnGa0.8In1.2S4 forms a high-pressure polymorph with an olivine-type structure (a = 12. 856(3), b = 7.500(3), c = 6.128(2)Å. All other compounds decompose under the conditions applied. The results of a Rietveld structure refinement for the two high-pressure spinels are presented
Ligand Influences on the Supramolecular Chemistry of Simple Gold(I) Complexes: Mononuclear (Isonitrile)gold(I) Complexes
Authors: Schneider Wolfgang , Angermaier Klaus , Sladek Alexander , Schmidbaur Hubert 
Published: February 2015

Abstract
A series of (isonitrile)gold(I) complexes has been synthesized: (MeNC)AuX (X = Cl la, I lc), (t-BuNC)AuBr 2b. (PhNC)AuX (X = Cl 3a. Br 3b. I 3c. SCN 3d), (MesNC)AuCl 4a [mes=mesityl], and (MeOC(O)CH2NC)AuX (X = Cl 5a. Br 5b. I 5c. SCN 5d). The chlorides were prepared by the reaction of (Me2S)AuCl with equimolar amounts (or with an excess) of the corresponding isonitrile. The bromides, iodides and thiocyanates were obtained from the reaction of (RNC)AuCl with K+X- (X = Br, I, SCN) in the two-phase system H2O/CH2CI2. The molecular and crystal structures of la. 2b. 3a-c, 4a, and 5a-c have been determined by X-ray diffraction methods. In the solid state the molecules are aggregated through short Au-Au contacts into dimers (4a and 5c), chains (la, 2b and 3a-c) or sheets (5a and 5b). The influence of the isonitrile and halide ligands on the type and strength of the intermolecular Au-A u contacts is discussed
Synthesis of Pentaalkyl-6-bromo-2,3,4,5-tetracarba-nido-hexaboranes(6)
Authors: Wrackmeyer Bernd , Glöckle Alexandra 
Published: February 2015

Abstract
Peralkylated 2,3,4,5-tetracarba-mdo-hexaboranes(6) 1 react with boron tribromide, BBr3, via selective exchange of the alkyl substituent in 6-position to give the corresponding new 6- bromo derivatives 2 in quantitative yield. The 6-iodo derivatives 2(1) can be prepared in the same way using BI3. Treatment of the carbaboranes 2 with Li Et3BH leads to the 1,2,3,4,5- pentaalkyl-2,3,4,5-tetracarba-inido-hexaboranes(6) 3. 1,3,4,6-Tetraethyl-2,3,4,5-tetracarbaw do-hexaborane(6) 4 reacts with BBr3 via degradation of the carbaborane cage to give EtBBr2, and (Z)-1,4-bis [bis(dibromoboryl)]-3-hexene 5. A new bis(diethylboryl)-substituted dialkenyl(bromo)borane 8 was prepared, but attem pts failed to convert it into a 1-bromo- or 6-bromo-mdo-C4B2-carbaborane. Treatment of 1,1-dialkyl-3-diethylboryl-4-ethylstannoles 9 with a large excess of BBr3 also affords 5, whereas 6-bromo-l,3,4-triethyl-2,3,4.5-tetracarbamdo- hexaborane(6) 11 was isolated in low yield (<5%) from the reaction between 9 and BBr3 (slight excess)
Halogenierungs- und Dissoziationsstufen eines Diphosphonio-1,2,4- triphosphoiids / Stages of Halogenation and Dissociation of a Diphosphonio-1,2,4-triphospholide
Authors: Schrödel Hans-Peter , Schmidpeter Alfred , Nöth Heinrich , Schmidt Martin 
Published: February 2015

Reductive condensation of Ph3P=C(SiMe3)2 and PCl3 or PBr3 yields the ionic halides of the 3,5-bis(triphenylphosphonio)-1,2,4-triphospholide cation 5. The compounds can take up two moles of halogen X2. In the first step bis(triphenylphosphoranediyl)trihalo-1,2,4-triphos- pholanes 6 are formed. Low temperature 31P NMR spectroscopy shows them to exist in two conformeric forms. In polar solvents heterolytic dissociation of the phosphorus-halogen bond in the 4-position occurs.
The molecular structure of 5 demonstrates a cyclic delocalized bonding system. Chlorination or bromination (to give 6) effects little structural change with exception of a large increase of the PP bond length. The phosphorus-halogen bonds in 6 are very long and rather different in length. The overall situation as well as the structural details can be rationalized to result from a negative hyperconjugation between the ylidic carbon atoms and the phosphorus-halogen bonds.
Zwei Metasilicate mit Vierer-Einfach-Ketten: Hochdrucksynthese und Strukturverfeinerung von Sr2(VO)2Si4O12 (Haradait) und Sr2(TiO)2Si4O12 / Two Metasilicates with Vierer Single Chains: High-Pressure Synthesis and Structure Refinement of Sr2(VO)2Si4O12 (Haradaite) and Sr2(TiO )2Si4O12
Authors: Berger Thomas , Range Klaus-Jürgen 
Published: February 2015

Single crystals of Sr2(VO)2Si4O12 could be obtained by high-pressure high-temperature reaction of a SrSiO3/SiO2/V2O5 mixture in a modified Belt-type apparatus. The green crystals are orthorhombic, space group Cmcm, with a = 5.3139(3), b = 14.6281(7), c = 7.0329(4) Å and Z = 2. The structure comprises vierer single chains of SiO4 tetrahedra, the resulting Si4O12 units being connected by VO5 square pyramids. There is one short distance (V - O = 1.61 (1) Å) within the square pyramid, giving definite evidence to a (VO)2+ group with a V = O double bond.
The crystal structure of microcrystalline Sr2(TiO)2Si4O12, obtained by high-pressure hightemperature reaction of a SrSiO3/SiO2/TiO2 mixture, was refined by the Rietveld technique. The compound (Cmcm, a = 5.3530(2), b = 14.4864(7), c = 7.0817(3) Å, Z = 2) is isostructural with the vanadium compound.
Iodbenzol als Lewis-Säure: Synthese und Kristallstrukturen von PPh4[Cl-I-C6H5] und PPh4[Br-I-C6H5] / Iodobenzene as Lewis-Acid: Synthesis and Crystal Structures of PPh4[Cl-I-C6H5] and PPh4[Br-I-C6H 5]
Authors: Ghassemzadeh Mitra , Magull Jörg , Fenske Dieter , Dehnicke Kurt 
Published: February 2015

The donor-acceptor complexes [X-I-C6H5]− with X− = Cl− and Br− have been prepared as tetraphenylphosphonium salts from iodobenzene and PPh4X in acetonitrile solutions. They form colourless single crystals, which were characterized by crystal structure determinations.
PPh4[Cl-I-C6H5]: Space group P21/c, Z = 4. Lattice dimensions at -70°C: a = 1301.1(5), b= 1457.0(5), c = 1478.8(5) pm, β = 114.17(3)°.
PPh4[Br-I-C6H5]: Space group P21/n, Z = 4. Lattice dimensions at 20°C: a = 1354.9(1), b= 1480.1(2), c = 1375.5(1) pm, β = 106.13(2)°.
The halide ions are coordinate at the iodine atom of the iodobenzene molecule in a linear arrangement [X-I-C6H5]− with bond lengths Cl-I of 327.9 and Br-I of 347.2 pm.
Kristallstruktur von MgSO3·H2O/Crystal Structure of Mg SO3·H2O
Authors: Buchmeier Willi , Engelen Bernward , Müller Holger 
Published: February 2015

Abstract
The crystal structure of MgSO3·H2O , space group P21 /ln, Z = 4, Dx = 2.415 g·cm-3 , a = 4.699(1), b = 12.751(3), c = 5.618(1) Å, β = 90.49(3)°, was determined by single crystal X-ray diffraction. MgSO3·H2O crystallizes in the MnSO3·H2O type. The structure consists of buckled trans layers ∞[MgSO3·H2O], which are built up from strongly distorted MgO5(H2O) octahedra sharing four equatorial vertices, and of trigonal pyramidal SO3
2- ions. It is close­ly related to the structures of orthorhombic MnSeO3·D2O and monoclinic ZnSeO3·H2O . The Mg-O distances range from 2.051(3) to 2.175(4) Å. The S-O distances (1.543(3), 1.547(3) and 1.493(3) Å) and the O-S-O angles (98.4(2) and 2x 106.0(2)°) correspond to those in MnSO3·H2O . The distortion of the MO5(H2O) octahedra (M = Mg, Mn) and of the SO3
2- ions is smaller in MgSO3·H2O , but with greater deviations from m symmetry. The distances between the H-connected ∞
2[MSO3·H2O] layers are greater in MgSO3·H2O , indicating weaker inter-layer hydrogen bonds. The lateral arrangement of the ∞
2[MSO3·H2O] layers is nearly the same in both sulfite monohydrates.