bluuebunny/crossref_metadata_2025_split huggingface dataset:
Reaktive E=C(p-p)π-Systeme, XLIII [1] Darstellung und Charakterisierung P-Phosphino- oder P-Arsino-substituierter Fluorphosphaalkene des Typs R2E-P=C(F)NEt2 (R = Me, CF3, Me2N; E = P, As) / Reactive E=C(p-p)-π Systems XLIII [1] Synthesis and Characterization of P-Phosphino or P-Arsino Substituted Fluorophosphaalkenes of the Type R2E-P=C(F)NEt2 (R= Me, CF3, Me2N; E = P As)
Authors: Grobe Joseph , Van Duc Le , Winnemöller Jost , Krebs Bernt , Läge Mechtild 
Published: February 2015

Abstract
The easily accessible phosphaalkene HP=C(F)NEt2 (lb) reacts with halophosphanes or -arsanes R2EX (X = Cl, I) in the presence of NEt3 to give P-phosphino- or -P-arsino substituted fluorophosphaalkenes of the type RiE-P=C(F)NEti (2 - 6) in high yields (60 - 85 %) [R2E: (CF3)2P (2), Me2N(CF3)P (3), Me2P (4), (CF3)2As (5), Me2As (6)]. The analogous reaction of ib with CF3PI2 (molar ratio 1:2) unexpectedly leads to the triphosphetene Et2N - C=P-PCF3-PCF3 (7). The stability of compounds 2 - 6 as a function of R2E decreases from As to P and from CF3 to Me, respectively.
Compounds 2 - 6 generally show the Z-configuration and have been characterized by thorough spectroscopic investigations (MS,IR; 1H, 19F, 11C, 31PNMR). A single crystal X-ray diffraction study of 2 proves the π-type interaction of the nitrogen lone pair with the P=C bond thus enhancing the stability of the system and the PP bond order
The Stannides EuPdSn and EuPtSn
Authors: Pöttgen Rainer 
Published: February 2015

Abstract
EuPdSn and EuPtSn were prepared from the elements in tantalum tubes at 1070 K and investigated by X-ray diffraction on both powder as well as single crystals. They crystallize with the TiNiSi type structure of space group Pnma and with Z = 4 formula units per cell. Both structures were refined from single-crystal diffractometer data: a = 751.24(9), b = 469.15(6), c = 804.31(9) pm, V = 0.2835(1) nm3 for EuPdSn, and a = 753.38(7), b = 467.72(4), c = 793.08(7) pm, V = 0.2795(1) nnr for EuPtSn. The structures consist of three-dimensional [PdSn] and [PtSn] polyanionic networks in which the europium atoms are embedded. The crystal chemistry of these stannides is briefly discussed
Komplexe eines vierzehngliedrigen Tetraazadibenzo-Makrocyclus. Strukturen des freien und zweifach protonierten Liganden und seiner Nickel(II)-, Kupfer(II)-, Zink(II)- und Palladium(II)-Komplexe / Complexes of a 14-Membered N4 Dibenzo Macrocycle. Crystal Structures of the Free and Diprotonated Ligand and of its Nickel(II), Copper(II), Zink(II) and Palladium (II) Complexes
Authors: Feldhaus Ralf , Köppe Jens , Mattes Rainer 
Published: February 2015

Abstract
The synthesis and structural characterisation of complexes of the 14-membered macrocyclic trans-N4 dibenzo ligand 5,6,7,8,9,14.15,16,17,18-decahydrodibenzo[e,l][1,4, 8,11]-tetraazacyclotetradecine (L2) is described. The crystal structures of six compounds were determined by single crystal X-ray diffraction. The free ligand L2 has a saddle-shaped structure with short intramolecular hydrogen bonds. The N-N distances are 289 pm. The diprotonated species [H2L2]2+ has a different conformation due to intra- and intermolecular hydrogen bonds. The ligand is folded along an N-N axis in c/s-[Ni(L2)(H2O)2]2+, but displays a saddleshaped structure in the Cu(II), Zn(II) and Pd(II) complexes with a more or less planar arrangement of the four N donor atoms. The metal atoms are incorporated within the macrocyclic cavity in [Cu(L2)(CF3SO3)]+ and [Pd(L2)]2+. The metal-to-nitrogen bond lengths herein are rather small. Zn(II) is five-coordinate in [Zn(L2)(Cl)]+. The coordination polyhedron is intermediate between a trigonal bipyramid and a square pyramid. In all complexes the metalto- ligand distances originating at the nitrogen atoms in β-position (with respect to the aromatic ring) are significantly shorter then the donor bonds of the ‘anilinic’ N atoms
Synthesis of Methyl 6-Deoxy-6-diphenylphosphino-α-D-glucopyranoside: Temperature-Dependence of the Primary O-Tosyl Cleavage Mode
Authors: Dahlhoff Wilhelm V. , Radkowski Karin 
Published: February 2015

Abstract
Methyl α-D-glucopyranoside is converted to methyl 6-p-toluenesulfonyl-2,3,4-tris-O-trimethylsilyl- α-D-glucopyranoside 2 and then reacted with lithium diphenylphosphide in THF. When the reaction is carried out at room tem perature and below, S-O cleavage dominates giving methyl 2,3,4-tris-O-trimethylsilyl-α-D-glucopyranoside 3 , whereas at 60°C in THF or at 35°C in diethyl ether, C-O cleavage occurs yielding the title carbohydrate-phosphine 4 in good yield after deprotection
Neue Pnictide mit modifizierten AIB2-Strukturen / New Pnictides with Modified AIB2-Type Structures
Authors: Johrendt Dirk , Miericke Reiner , Mewis Albrecht 
Published: February 2015

Abstract
Nine new compounds AMX with A: Ca, Sr, Ba, M: Pd, Au and X:P, As were prepared by heating mixtures of the elements and investigated by Xray methods. They crystallize in modified AIB2- type structures, for the present examples in the ZrBeSi- and SrPtSb-types, with an ordered distribution of the atoms
Synthese von Heteroanaloga der Penicillsäure / Synthesis of Hetero Analogues of Penicillic Acid
Authors: Stachel Hans-Dietrich , Schachtner Josef 
Published: February 2015

Keywords
Grignard Reaction, Penicillic Acid, Tetramic Acids, Hydroxamic Acids, Thiepin-2,5-dione
N,N′-Dim ethylharnstoff als chelatisierende Lewis-Säure: Synthese und Kristallstrukturen von PPh4[Cl(H2Me2N2CO)] und (PPh4)2[Cl(H2Me2N2CO)]Cl / N.N′-Dimethylurea as a Chelating Lewis Acid: Synthesis and Crystal Structures of PPh4[Cl(H2Me2N2CO)] and (PPh4)2[Cl(H2Me2N2CO)]Cl
Authors: Ghassemzadeh Mitra , Harms Klaus , Dehnicke Kurt 
Published: February 2015

The title compounds have been prepared from tetraphenylphosphonium chloride and N,N′- dimethylurea in acetonitrile using different molar ratios of the educts. Both compounds were characterized by IR spectroscopy and by crystal structure determinations.
PPh4[Cl(H2,Me2,N2,CO)]: Space group P1̅, Z = 4 ,a = 1021.8(2), b = 1192.7(2), c = 2143.9(4) pm, α = 87.21(3)°, β = 85.95(3)°, γ = 74.16(3)° (-50°C).
(PPh4)2[Cl(H2Me2N2CO)]Cl: Space group P21/n, Z = 4, a = 1138.4(2), b = 2855.4(3), c = 1394.0(1) pm, β = 91.19(10)° (-60°C).
In both compounds the N.N′-dimethylurea molecule acts as a chelating Lewis acid via two Cl···H hydrogen bonds forming nearly planar ClH2N2C-six-membered heterocycles.
Die Kristallstrukturen des Diphenylphosphinsäureamids, Ph2P(O)NH2, und seines Cäsiumsalzes [Cs{Ph2P(O)NH}] / Crystal Structures of Diphenylphosphinic Acid Amide, Ph2P(O)NH2, and of its Cesium Salt [Cs{Ph2P(O)NH}]
Authors: Schlecht Sabine , Chitsaz Soheila , Neumüller Bernhard , Dehnicke Kurt 
Published: February 2015

The crystal structures of the monoclinic form of Ph2P(O)NH2 and of its cesium salt, [Cs{Ph2P(O)NH}] have been determined by X-ray methods.
Ph2P(O)NH2: Space group P21/c, Z = 16, lattice dimensions (-80°C): a = 2530.2(3), b = 858.9(2), c = 2135.5(3) pm, β = 110.78(1)°, R , = 0.055. Diphenylphosphinic acid amide forms dimeric molecules via N-H ··· O hydrogen bonds, the dimeric units again are associated via hydrogen bonds to form infinite double chains along the crystallographic c axis.
[Cs{Ph2P(O)NH}]: Space group Pccn, Z = 8 , lattice dimensions (-83°C): a = 1262.8(1), b = 2632.3(2), c = 769.1(1) pm , R1 = 0.024. The compound is associated via Cs-O and Cs-N contacts along the crystallographic [001] axis forming a tubular arrangement. There are no hydrogen bonds.
Reaktivität nitrophenylsubstituierter cyclischer Amine bei Dehydrierungen / The Reactivity of Nitrophenyl Substituted Cyclic Amines with Dehydrogenations
Authors: Möhrle H. , Mehrens J. 
Published: February 2015

Piperidine and perhydroazepine bearing a 1 -(4-nitrophenyl) substituent were inert to mercury-edta, while the a-pipecoline derivative gave an aminoketone with cleavage of the heterocycle. However the corresponding (2-nitrophenyl) compounds reacted to give respectively a piperidin-2-one, an aminopentanal and an aminohexanone.
By an additional substituent in 2′-position the p-nitro compounds underwent dehydrogenation too. With a methyl group resulted a pattern analogous to o-nitro products. A neighbouring hydroxymethyl function enhanced the reaction with formation of benzoxazines and if possible their further oxidized derivatives, the hydroxylactams.
Oligomere Tetraeder-Anionen in Borophosphaten: Darstellung und Kristall­strukturen von NaFe[BP2O7(OH)3] und K2Fe2[B2P4O16(OH)2 ]/Oligomeric Tetrahedral Anions in Borophosphates: Synthesis and Crystal Structures of NaFe[BP2O7(OH)3] and K2Fe2[B2P4O16(OH)2]
Authors: Boy Insan , Cordier Gerhard , Eisenmann Brigitte , Kniep Rüdiger 
Published: February 2015

Abstract
Crystals of the title compounds were grown under hydrothermal conditions. The crystal structures were determined by single crystal data.
NaFe[BP2O7(OH)3] (monoclinic, C 2/c, a = 1042.0(2), b = 821.5(1), c = 921.7(1) pm, β = 116.60(1)°, Z=4): The crystal structure contains isolated anions [BP2O7(OH)3]4-, which correspond to trinuclear units PO1/2O3-BO2/2(OH)2 -PO1/2O2(OH) of corner sharing tetrahedra. Fe3+ is coordinated octahedrally by oxygen, Na+ is 8 -fold coordinated by oxygen forming cubes.
K2Fe2[B2P4O16(OH)2] (triclinic, P1̄, a = 516.7(1), b = 808.9(1), c = 834.0(1) pm, α = 87.06(f), β = 80.21(1), γ = 86.59(1)°, Z = 1): The crystal structure contains isolated anions [B2P4O16(OH)2]8-. Four-membered rings of tetrahedra with two additional terminal phosphate groups are formed by condensation of two trinuclear units P O1/2O3 -BO3/2(OH) -PO2/2O2. Fe3+ is in an octahedral and K+ in an irregularly 10-fold coordination by oxygen.
(Triphenylarsine)gold(I) Complexes: Synthesis of an Oxonium Salt and Redistribution of the Arsine Ligands
Authors: Tripathi Upendra M. , Schier Annette , Schmidbaur Hubert 
Published: February 2015

Abstract
The reaction of [(Ph3As)AuCl] with Ag2O in the presence of NaBF4 in tetrahydrofuran affords three products, identified as [(Ph3As)4Au]BF4 (40.3%), [(Ph3As)2Au]BF4 (16.4%) and {[(Ph3As)Au]3O}BF4 (17.3%). The properties of the main product agree well with recent literature data. The other two compounds are new and have been identified by their analytical, spectroscopic, and crystallographic data. The structures are isomorphous with those of the analogous Ph3P complexes. Variations in the stabilities are discussed in terms of kinetic and thermodynamic effects.
Thermische Zersetzung und Lösungskalorimetrie von Ammoniumneodymchloriden/Thermal Decomposition and Solution Calorimetry of Ammonium Neodymium Chlorides
Authors: Hennig C. , Oppermann H. 
Published: February 2015

Abstract
The thermodynamical data of ammonium neodymium chlorides (NH4)2NdCl5 and NH4Nd2Cl7 were derived by the determination of their decomposition equilibria by total pres­sure measurements. Moreover, solution calorimetry was applied. The enthalpies of formation of these phases were calculated from their heats of solution and from the enthalpies of formation and the heats of solution of NdCl3 and NH4Cl.
Data by total pressure measurement:
ΔH°B((NH4)2NdCl5,f,298) = - 412,5 ± 3,6 kcal/mol;
S°((NH4)2NdCl5 f 298) = 80,1 ± 5,8 cal/K · mol;
ΔH°B(NH4Nd2Cl7,f,298) = -579,5 ± 3,5 kcal/mol;
S°(NH4Nd2Cl7,f,298) 101,8 ± 5,6 cal/K mol.
Data by solution calorimetry:
ΔH°B(NdCl3,f,298) = -251,2 ± 0,7 kcal/mol;
ΔH°B((NH4)2NdCl5,f,298) = -405,5 ± 1,0 kcal/mol;
ΔH°B(NH4Nd2Cl7,f, 298) = -576,8 ± 1,7 kcal/mol.
Photoreactivity of Titanocene Pentasulfide
Authors: Kunkely Horst , Vogler Arnd 
Published: February 2015

Abstract
The electronic spectrum of Cp2TiS5 shows a long-wavelength absorption at λ max = 492 nm which is assigned to the lowest-energy S5
2- → TiIV ligand-to-metal charge transfer (LMCT) transition. The photolysis of the complex in CH2CI2 leads to the formation of Cp2TiCl2 and elemental sulfur. It is suggested that LMCT excitation initiates a reductive elimination with the extrusion of S5 while the reduced titanocene is reoxidized by the solvent.
18-Krone-6 und kleine Carbonsäuren. Bildung und Struktur binärer Addukte mit Ameisen-und Essigsäure sowie ternärer mit Essigsäure und Wasser/18-Crown-6 and Small Carboxylic Acids. Formation and Structure of Binary Adducts with Formic and Acetic Acid, as well as Ternary Ones with Acetic Acid and Water
Authors: Albert Antje , Mootz Dietrich 
Published: February 2015

Abstract
The melting diagrams of the binary systems 18-crown-6/formic acid and 18-crown-6/acetic acid have been set up and the crystal structures of the adducts 18C6 · 2 HCOOH (1, space group P 21/c with Z = 2 formula units per unit cell) and 18C6 · 2 CH3COOH (2, C2/m, Z = 2) determined. Furthermore three ternary phases, 18C6 · CH3COOH · H2O (3, P21/c, Z = 4) and dimorphic 18C6 · 2 CH3COOH · 4 H2O (high temperature form 4, P21/n, Z = 2; low temperature form 5, P21/n, Z = 2) have been characterized in the same way. In each structure the crown ether molecule has the (pseudo) D3d conformation common for many of its complexes. Various aspects of the intermolecular hydrogen bonding are described.
Redoxreaktionen von Molybdänverbindungen mit Bis(2-salicyliden- aniinophenvl Klisulfid. Kristallstruktur von Salicylaldehyd-2-mercapto- anilato(2-)-triphenylphosphanoxid-dioxomolybdän(VI) Redox / Reactions of Molybdenum Compounds with Bis(2-salicylidene-aminophenyl)disulfide. Crystal Structure of Salicylaldehyde-2-mercaptoanilato(2-)– triphenylphosphaneoxide-dioxo- molybdenum(VI)
Authors: Banße Wolfgang , Fliegner Jana , Sawusch Stefan , Schilde Uwe , Uhlemann Erhard 
Published: February 2015

Abstract
The reactions of Mo(CO)6, Mo(acac)2(NO)2, and MoO2(acac)2 with bis(2-salicylideneaminophenyl) disulfide in the presence of triphenylphosphane have been studied. The crystal structure of salicylaldehyde-2-mercaptoanilato(2-)-triphenylphosphaneoxidedioxomolybdenum (VI) was determined by X-ray analysis.
Ag+ als Substituent eines Alkalimetalls in Ag2SrMnV2O8 / Ag+ As Substituent Of An Alkaline Metal In Ag2SrMnV2O8
Authors: Rettich R. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single crystals of Ag2 SrMnV2O8 have been prepared by reactions of metallic silver and a mixture of SrCO3, MnCO3 · H2O and V2O5. X-Ray investigations showed monoclinic symmetry, space group C6
2h -C2/c, a = 9.7022(9), b = 5.5882(5), c = 13.894(1), β = 90.41(1)°, Z = 4. The crystal structure is isotypic to Na2BaCuV2O8 and includes VO4 tetrahedra, MnO6 octahedra as well as irregular AgO8 and SrO10 polyhedra. Ag2SrMnV2O8 is characterized by a [MnV2O8] network incorporating Ag+ and Sr2+ or a [Ag2V28] frame incorporating Mn2+ and Sr2+ ions. Ag+ is able to replace an alkali ion in the cationic part of the crystal structure.
Spectrometric pK Determination of Daphnetin, Chlorogenic Acid and Quercetin
Authors: Sauerwald N. , Schwenk M. , Polster J. , Bengsch E. 
Published: February 2015

Abstract
Daphnetin, Chlorogenic Acid, Quercetin Polyphenols play an important role in the ‘immune system’ of plants. Since their charge is important for their physiological effect it is important to know their pKj values. Therefore, the pKj values of some plant contents such as daphnetin (pK = 7.36), chlorogenic acid (pK ≈ 8.5), and quercetin (pK1 = 7.03, pfro = 9.15) were determined in the pH range 7 -10 using UV/VIS spectroscopy. The decomposition kinetics of quercetin in alkaline solutions was taken into consideration by extrapolating the absorbance time curves to time zero (t = 0). The graphic method of absorbance (A) diagrams was used to determine the pKi values. In the case of quercetin the method of linear regression was also used for the determination.
Dimere und polymere Pnictidostannat(IV)-Anionen -Darstellung und Kristallstrukturen von Na2K3[SnP3], Na2Cs3[SnP3] und Na2K3[SnBi3] / Dimeric and Polymeric Pnictidostannate(IV) Anions -Preparation and Crystal Structures of Na2K3[SnP3], Na2Cs3[SnP3] and Na2K3[SnBi3]
Authors: Asbrand Matthias , Eisenmann Brigitte , Engelhardt Holger , Rößler Ute 
Published: February 2015

Abstract
The metallic lustrous compounds Na2K3[SnP3], Na2Cs3[SnP3], and Na2K3[SnBi3] were prepared from melts of mixtures of the elements. The isotypic compounds Na2K3[SnP3] and Na2Cs3[SnP3] crystallize in the orthorhombic system, space group Cmca (No 64), Z = 8, with lattice constants a = 1996.1 (4)/2047.9(4) pm, b = 669.5(1)/686.5(2) pm, c = 1494.5(2)/1617.8(3) pm. The structure is characterized by dimeric units [Sn2P6] 10- of edge-sharing [SnP4] tetrahe­dra, which are coordinated by the alkali cations. Na2K3[SnBi3] crystallizes in the orthorhombic system, space group Ibca (No 73), Z = 8, with lattice constants a = 718.2(1) pm , b -1692.6(2) pm, c = 2159.5(2) pm. In the anionic partial structure [SnBi4] tetrahedra are connected via common corners to infinite 1
∞[SnBi3]5- Zweier single chains. The sodium and potassium cat­ ions separate the chains from each other. Neglecting the distortions caused by covalent bonding and different radii both structure types can be classified as superstructure defect variants of the Li3Bi structure. Different orderings in the occupation of the tetrahedral voids lead to the variants in the anionic assemblies.
Some Applications of Ultrahigh Resolution 15N NMR Spectroscopy
Authors: Wrackmeyer Bernd , Kupče Ēriks 
Published: February 2015

Abstract
Ultrahigh resolution 15N NMR spectra were measured for two nitroalkanes (MeNO2 la, tBuNO2 1c), two isocyanates (tBuNCO 2c, Me3SiNCO 2d), four isothiocyanates (MeNCS 3a, EtNCS 3b, tBuNCS 3c, Me3SiNCS 3d), one carbodiimide (Me3SiNCNSiMe3 4d), one keteneimine [Me3SiNCC(SiMe3)2 5d], two sulphinyl imides (tBuNSO 6c, Me3SiNSO 6d), and N-tert-butyl-pyrrole 7c, in order to determine coupling constants J(15N ,I3C) and isotope induced chemical shifts 1∆12/13C (15N) at the natural abundance of the isotopes. The values 1∆12/13C (15N) can be separated into two groups, one dealing with NC single and another one with NC double bonds. In each group (with few exceptions), the values 1∆12/13C (15N) become more negative with a decrease in the absolute magnitude of l1J(l5N ,13C)l. The corresponding values 1∆14/15N (13C) show a sim ilar behaviour. However, N-substituted pyrroles appear to be exceptional in this respect.
Metallkomplexe mit biologisch wichtigen Liganden, CIV [1]. ortho-Palladierte Komplexe von N,N-Dimethyl-C-phenyl-glycinmethylester. Synthese von α-Aminosäure-Derivaten durch Insertion von Isocyaniden, CO, Alkenen und Alkinen in die Pd-C-Bindung / Metal Complexes of Biologically Important Ligands, CIV [ 1]. ortho-Palladated Complexes of N,N-Dimethyl-C-phenylglycine-methylester. Synthesis of α-Amino Acid Derivatives by Insertion of Isocyanides, CO, Alkenes, and Alkynes into the Pd-C Bond
Authors: Böhm Andreas , Polborn Kurt , Sünkel Karlheinz , Beck Wolfgang 
Published: February 2015

Abstract
N,N-Dimethyl-C-phenylglycinemethylester reacts with Pd(OAc)2 in acetic acid to give the orthopalladated, acetato bridged complex 1. Treatment of 1 with sodium halide affords the chloro, bromo, and iodo bridged compounds [Me2NC(H)(CO2Me)C6H4PdX]2 (2a -c) (X = halide). From 2a and 1,1′-bis(diphenylphosphino)ferrocene the phosphine bridged trinuclear complex 3 is obtained. Substitution of the amine ligand of 2a by the phosphino group is observed for the reaction of 2a with Ph2PC(Me)C(Me)PPh2. Insertion of 2,6-dimethyl-phenylisocyanide, CO, alkyl-vinyl-ketones, and diphenylacetylene into the Pd-C bond o f 2a -c provides the orthosubstituted organic and organometallic derivatives of phenylglycine 6a -c, 7, 8a -b and 9a -c. The crystal structures of 1, 4a, 6a, 7 and 9a were determined by X-ray diffraction.
Enantioselective Catalysis, 120 [1] New Optically Active Pyrrole-oxazolines
Authors: Brunner Henri , Haßler Bernd 
Published: February 2015

Abstract
14 new optically active pyrrole-oxazolines were synthesised from 2-pyrrole-carbonitrile or methyl 2-pyrrole-carboximidate and chiral amino alcohols. Their use in copper-catalysed enantioselective cyclopropanation reactions gave only low optical yields (3-14%ee).
Untersuchungen an Polyhalogeniden, XXXVI. Zur Kenntnis des Oktaiodid-Ions I8
2-: Darstellung und Kristallstruktur des [(Crypt-2.2.2)H2]l8, des [Ni(phen)3]I8 · 2CHCl3 und der Bis(N-alkylurotropinium) oktaiodide (UrR)2I8 mit R = Methyl und Ethyl / Studies on Polyhalides, XXXVI. On the Octaiodide Ion I8
2-: Preparation and Crystal Structure of [(Crypt-2.2.2)H2]I8, of [Ni(phen)3]I8-2CHCl3 and of the Bis(N-alkylurotropinium)octaiodides (UrR)2I8 with R = methyl and ethyl
Authors: Gräfe-Kavoosian Arista , Nafepour Shida , Nagel Klaus , Tebbe Karl-Friedrich 
Published: February 2015

Abstract
The new compound [(Crypt-2.2.2)H2]I8 has been prepared by the reaction of [(Crypt-2.2.2)H2](I3)2 with iodine in methanol. It crystallizes in the orthorhombic space group Pbcn with a = 11.476 (2), b = 13.589 (2), c = 22.888 (2) Å and Z = 4. The crystal structure has been refined to RF = 0.031 for 1618 reflections. It may be described as a layerlike packing of octaiodide anions I8
2-and diprotonated 2.2.2-Crypt as cations. The non planar octaiodide anion is built up from two triiodide groups and a bridging iodine molecule.
Tris(1, 10-phenanthroline)nickel(II) octaiodide bis(chloroform) crystallizes in the monoclinic space group P21/n with a = 11.683 (8), b = 21.717 (8), c = 20.752 (5) Å, β = 95.03 (5)° and Z = 4 formula units. The crystal structure has been refined to RF = 0.058 for 3894 reflections. The structure consists of two chloroform molecules, octahedrally coordinated complex cations [Ni(phen)3]2+ and nonplanar octaiodide anions I8
2- each composed of two asymmetric triiodide units I3
- weakly associated with an elongated bridging iodine molecule I2.
The already known structure of bis(N-methylurotropinium) octaiodide, (UrMe)2I8, has been verified and more accurate crystal data have been collected. The crystal structure has been refined to RF = 0.045 for 1908 reflections. The compound crystallizes in the monoclinic space group P21/c with a = 11.302 (2), b = 9.850 (2), c = 14.188 (2) Å , β = 92.59 (1)° and Z = 2. The anion has the shape of a stretched Z.
The structure of bis(N-ethylurotropinium) octaiodide (UrEt)2I8 has been determined and a new configuration (I3
-, I5
-) for octaiodide ions between Z (I3
- · I2 ·I3
-) and a “broken” configuration (I3
-, I5
-) has been observed. The compound crystallizes in the triclinic space group P1̄ with a = 9.741 (3), b = 11.815 (3), c = 15.426 (3) Å, α = 91.80 (2), β = 107.14 (2), γ = 90.04 (2)° and Z = 2. The crystal structure has been refined to RF = 0.037 for 3657 reflections.
Francoanellit K3Al5HPO4)6(PO4)2 · 12H2O: Struktur und Synthese durch topochemische Entwässerung von Taranakit / Francoanellite K3Al5HPO4)6(PO4)2 · 12H2O: Structure and Synthesis by Topochemical Dehydration of Taranakite
Authors: Dick Stefan , Zeiske Thomas 
Published: February 2015

Abstract
Single crystals of synthetic francoanellite K3Al5(HPO4)6(PO4)2-12H2O could be obtained for the first time by topochemical dehydration of taranakite crystals. An X-ray structure determination showed francoanellite to be the mineral with the second longest crystallographic axis described hitherto. Crystal data: space group R3c, a = 869.0(2), c = 8227(1)pm, Z = 6 , Rg = 0.042. Francoanellite is a layer structure mineral having six layers of composition [K3Al5(HPO4)6(PO4)2(H2O)12], connected by hydrogen bonds. The rigid layer is formed by columns of corner sharing hydrogen phosphate tetrahedra and AIO6-octahedra which are inter­ connected by additional six-coordinated Al ions. In trigonal holes of the layer orthophosphate ions are situated. The structure of francoanellite is very similar to the structure of taranakite K3H6Al5(PO4) 8 · 18H2O which has planar water interlayers between the Al-phosphate layers. A neutron scattering experiment with subsequent Rietveld refinement of the powder pattern gave the H-atom positions. Hydrogen bonds in francoanellite are formed within the rigid layers and between them.
During the reaction taranakite → francoanellite crystals in an intermediate stage of dehydration could be obtained. From the c-axis of 8858 pm and one-dimensional electron density projections it can be proposed that in these crystals every second water interlayer was lost and a first order staging product of the deintercalation of water from taranakite was formed.