bluuebunny/crossref_metadata_2025_split huggingface dataset:
Darstellung, 11B-NMR- und Schwingungsspektren von cis-Monocyanomononitrotetrahydro-closo-hexaborat(2-) , as-[B6H4(CN)(NO2)]2- und cis-μ-Nitroso-bis(monocyanotetrahydro-closo-hexaborat)(3-), cis-[(CN)B6H4(NO)B6H4(CN)]3– sowie Kristallstruktur von [As(C6H5)4]2-cis-[B6H4(CN)(NO2)] / Preparation, n=11B-NMR and Vibrational Spectra of cis-Monocyanomononitrotetrahydro-closo-hexaborate(2-) , cis-[B6H4(CN)(NO2)]2-,cis -μ-Nitroso-bis(monocyanotetrahydro-hexaborate)(3-), cis-[(CN)B6H4(NO)B6H4(CN)]3– and the Crystal Structure of [As(C6H5)4]2-cis-[B6H4(CN)(NO2)]
Authors: Franken A. , Preetz W. 
Published: February 2015

Abstract
By electrochemical oxidation of [B6H5(CN)]2- in the presence of nitrite ions and of the base DBU in dichloromethane solution cis-[B6H4(CN)(NO2)]2- and cis- [(CN)B6H4(NO)B6H4(CN)]3- are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of the tetraphenylarsonium salt has been determined by single crystal X-ray diffraction analysis.
[As(C6H5)4]2-cis-[B6H4(CN)(NO2)] is monoclinic, space group P21/a with a = 20.343(5), b = 10.896(2), c = 21.572(5) A and β = 107.30(2)°. The 11B NMR spectra are consistent with disubstituted octahedral B6 cages with local C2v symmetry. The IR and Raman spectra exhibit characteristic NO2, NO, CN, BH, and B6 vibrations.
Synthese und Struktur saurer Ubergangsmetallsulfate - Ti(H5O2)(SO4)2(H2O)2 und Zr(H3O)2(SO4)3 / Synthesis and Structure of Acid Transition Metal Sulfates - Ti(H5O2)(SO4)2(H2O)2 und Zr(H3O)2(SO4)3
Authors: Trojanov S. , Stiewe A. , Kemnitz E. 
Published: February 2015

Abstract
From the ternary system Mn(SO4)n/2 / SO3 / H2O (Mn+ = Zr4+, Ti3+) two new acid metal sulfates, Ti(H5O2)(SO4)2(H2O)2 and Zr(H3O) 2(SO4)3, have been synthesized and structurally characterized. Ti(H5O2)(SO4)2(H2O)2 crystallizes in the orthorhombic space group Pnma with cell parameters a = 9.858(5), b = 18.32(2), c = 5.437(7)Å (Z = 4); Zr(H3O)2(SO4)3 crystallizes in the triclinic space group P1 with cell parameters a = 5.092(2), b = 8.533(3), c = 12.388(6)A, α = 92.95(3)°, β = 90.89(3)°, γ = 94.35(3)° (Z= 2). In the titanium compound there are slightly distorted TiO6 octahedra with Ti-O distances between 1.99 and 2.09 Å which are sharing corners with SO4 tetrahedra. Through hydrogen bonds layers are formed perpendicular to the b-axis. These layers are connected by H3O+ ions only. The structure of Zr(H3O)2(SO4)3 consists of three different SO4 tetrahedra and distorted ZrO7 polyhedra which are connected via common corners and edges to form columns parallel to the a-axis. The Zr-O distances vary from 2.13 to 2.18Å for equatorial positions, significantly longer than the axial Zr-O distances with 2.05Å.
Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumchlorid [P(NH2)4]Cl / Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Chloride [P(NH2)4]Cl
Authors: Horstmann Stefan , Schnick Wolfgang 
Published: February 2015

Abstract
[P(NH2)4]Cl has been prepared by ammonolysis of phosphorus pentachloride in liquid ammonia. The product was purified by reacting the byproduct, ammonium chloride, with diethylamine and removing the diethylamine hydrochloride. Suitable single crystals were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. The crystal structure of [P(NH2)4]Cl has been determined by single crystal X-ray methods (Pbcn, a = 470.8(2), b = 1622.3(3), c = 756.3(2) pm, Z = 4). In the solid, [P(NH2)4]+ and Cl- ions are found, resembling a TlI-analogous structure.
The N-H···Cl distances indicate N-H···Cl hydrogen bonding interactions. The distortion of the P-N sceleton of the cation and the very short P-NH2 distances (mean value: 161.2 pm) have been confirmed by ab initio calculations, which show a generalized anomeric effect of the electron pairs at nitrogen and pπdπ bonding.
Hochdrucksynthese und Strukturverfeinerung von Strontium-Danburit, SrB2Si2O8
Authors: Berger Thomas , Range Klaus-Jürgen 
Published: February 2015

Abstract
Single crystals of strontium danburite, SrB2Si2O8, were found after high-pressure treatment of SrSiO3/SiO2/Al2O3 mixtures at 40 kbar and 1400°C, obviously formed by an unwanted side reaction with the boron oxide-containing boron nitride capsules used. The crystals are orthorhombic, space group Pnma, with a = 8.1891 (5), b = 7.9311 (6), c = 8.9284(5) Å and Z = 4. The structure was refined to R = 0.031, Rw = 0.028 for 590 independent, absorption-corrected reflections. SrB2Si2O8 is isostructural with danburite (CaB2Si2O8). The structure comprises a tetrahedral framework of ordered B2O7 and Si2O7 groups which contains Sr in irregular coordination.
Metallkomplexe mit biologisch wichtigen Liganden, LXXXIV [1] Halbsandwich-Komplexe von Rhodium(III), Iridium(III), Cobalt(III), Ruthenium(II), Ruthenium(III) und Chrom(III) mit Aminosäureester-Liganden Metal Complexes with Biologically Important Ligands, LXXXIV [1] Half-Sandwich Complexes o f Rhodium(III), Iridium(III), Cobalt(III), Ruthenium(II), Ruthenium(III) and Chromium(III) with Amino Acid Ester Ligands
Authors: Bergs Ralph , Krämer Roland , Maurus Michael , Schreiner Bernhard , Urban Reinhold , Missling Christopher , Polbom Kurt , Sünkel Karlheinz , Beck Wolfgang 
Published: February 2015

Abstract
A series of cyclopentadienyl and pentamethylcyclopentadienyl complexes of cobalt, rhodium, iridium, ruthenium and chromium with a-amino-acid esters (L) as ligands was prepared and characterized: Cp*(Cl)2M(L) (1, 2: M = Rh, Ir), Cp(I)2Co(L) (4), [Cp(Ph3P)2Ru(L)]+BF- (6), [Cp(OC)(Ph3P)Ru]+BF- (7) and the paramagnetic compounds Cp*(Cl)2Ru(L) (8) and Cp(Br)2Cr(L) (9). AlaOMe and HisOMe form N ,O and N,N chelate complexes [Cp*(Cl)M(alaOMe)]+BF-
4 (3: M = Rh, Ir), [Cp(I)Co(hisOMe)]+BF4. Cp*Co(CO)I2 and GlyOMe gave the N,O-dipeptide ester complex Cp*(I)Co(glyglyOMe)]+BF-
4 (5). The crystal structures of Cp(I)2Co(glyOEt) and Cp*(Cl)2Ru(alaOMe) were determined by X-ray diffrac­tion. The complexes 1 and 2 undergo ester exchange reactions with CD3OD. [Cp*MCl2]2 (M = Rh, Ir) catalyze the exchange of the ethoxy group in Me2NCH2CO2Et by CD3OD.
Chemie polyfunktioneller Moleküle, 120 [1] Synthesen und Kristallstrukturanalysen von Tris(imido-tetraphenyl- diphosphinato-0,0')eisen(III) und des PP-verknüpften Phosphazens Ph2P-N=PPh2-PPh2=N-PPh2
Authors: Ellermann Jochen , Gabold Peter , Knoch Falk A. , Moll Matthias , Schmidt Astrid , Schütz Martin 
Published: February 2015

Abstract
While the reaction of anhydrous iron(III) chloride with the chelate ligand [(C6H5)2P(O)]2NH (6) is an efficient way to synthesize the new tricyclic compound imido-tetraphenyl-diphosphinato-O,O′iron(III), [Fe{O-P(Ph2)=N-P(Ph2)=O}3] (4), treatment of [(C6H5)2P]2NLi (1) with anhydrous iron(III) fluoride in THF represents a simple route to obtain the phosphorus-phosphorus connected species Ph2P-N=PPh2-PPh2=N-PPh2(7). Both compounds were charac­terized by X-ray crystallography, 1H ,31P {1H}, 13C {1H} NMR, IR, Raman and mass spectra.
Uber ein neues Oxoiridat(V) vom Sr4PtO6-Typ: NaSr3IrO6
Authors: Frenzen S. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single crystals of NaSr3IrO6 have been prepared by heating mixtures of Na2O2, SrO and iridium in closed silver tubes and were investigated by X-ray techniques, NaSr3IrO6 crystal­lizes with trigonal (rhombohedral) symmetry in the space group D6
3d-R3̄ c , a = 9.636(2), c = 11.556(3) Å , Z = 6, and is isotypic to compounds of the Sr4PtO6 type. The substitution of Sr2+ by Na+ in NaSr3IrO6 led to an ordered metal distribution and an increase of the oxida­tion state from IrIV to Irv.
The Crystal Structure and Low Temperature 13C NMR Spectrum of the Seven-Coordinate Complex of Tungsten(II), [WI2(CO)3(NCPh)2]
Authors: Baker Paul K. , Muldoona David J. , Hursthouseb Michael B. , Colesb Simon J. , Laveryc Aidan J. , Shawcross Andrew 
Published: February 2015

Abstract
The crystal structure of [WI2(CO)3(NCPh)2] (1) has been determined by X-ray methods. The crystals are orthorhombic, space group Pnam, a = 7.815(3), b = 13.839(5), c = 18.475(3) Å, Z = 8, R = 0.0346 for 1497 observed data. The complex [WI2(CO)3(NCPh)2] has a seven-coordinate geometry, which may be described as a distorted capped octahedron, with the two iodo-ligands mutually trans, while each nitrile is trans to a carbonyl group. The capped octahedral geometry consists of a capping carbonyl (C(10)} on the face defined by I(1), C(20) and C(20)#. However, the geom etry may also be described as a capped trigonal prism, which has one triangular face occupied by three carbonyl groups and the second triangular face occupied by N(1) , N (1)# and I(1) atoms, respectively. The iodide I(2) occupies the capping position on the rectangular face defined by the atoms C(20), C(20)#, N (1), and N (1)# . The low temperature 13C NMR spectrum (203 K, CD2Cl2) of 1 shows a single carbonyl resonance at 219.27 ppm which indicates that the complex is undergoing a rapid fluxional process in solution at 203 K.
Synthese und röntgenographische Charakterisierung von zwei neuen Verbindungen des Ludwigit-Strukturtyps: Co5Sn(BO3)2O4 und Co5Mn(BO3 )2O4/Synthesis and X -Ray Characterization of Two New Compounds with Ludwigite-Structure: Co5Sn(BO3)2O4 and Co5Mn(BO3)2O4
Authors: Utzolino Anne , Bluhm Karsten 
Published: February 2015

Abstract
The compounds Co5Sn(BO3)2O4 (I) and Co5Mn(BO3)2O4 (II) were prepared by using a B2O3 flux technique. Single crystals were investigated by X-ray diffraction and showed orthorhombic symmetry, space group D2h
9-Pbam (No. 55), I a = 944.4; b = 1233.8; c = 310.5 pm; Z = 2 and II a = 925.07; b = 1241.67; c = 305.24 pm; Z = 2. Both compounds are isotypic to the mineral Ludwigite. All metal point positions show an octahedral oxygen coordination. Co2+ and M4+ (M = Sn or Mn) occupy one point position statistically. Both structures contain isolated, trigonal planar BO3 units and oxygen atoms that are not coordinated to boron.
Synthese und Kristallstruktur von Dibariumzink-bis(cyclotriborat) Ba2Zn(B3O6)2/Synthesis and Crystal Structure of Di-barium Zinc Bis-cyclotriborate Ba2Zn(B3O6)2
Authors: Busche Silke , Bluhm Karsten 
Published: February 2015

Abstract
Single crystals of the new compound Ba2Zn(B3O6)2 were obtained by using a B2O3 flux technique. They crystallize in an as yet unknown structure type. X-ray investigations led to space group Ci
1-P1̄
(Nr.2) with lattice parameters a = 715.5(2), b = 720.5(2), c = 1178.9(4), a = 78.96(2)°, β = 85.45(2)°, γ = 60.12(1)°, Z = 2. The structure is characterized by iso­lated (B3O6)3--rings and contains two ninefold coordinated Ba-sites. Zn2+ is tetrahedrally coordinated by oxygen. The relation to the crystal structures of high-temperature BaB2O4 and Ba2Ca(B3O6)2 is discussed.
InIII -Phthalocyanine: Darstellung, Eigenschaften und Kristallstruktur von b-Bis(triphenylphosphin)iminium-cis-di(cyanato(N))phthalocyaninato- (2-)indat(III)/ InIII Phthalocyanines: Synthesis, Properties and Crystal Structure of b-Bis(triphenylphosphine)iminium cis-Di(cyanato(N ))phthalocyaninato(2-)indate(III)
Authors: Aβmann Barbara , Franken Andreas , Homborg Heiner 
Published: February 2015

Abstract
[In(Cl)Pc2-] reacts with bis(triphenylphosphine)iminium cyanate ((PNP)OCN) in dichloromethane to yield green-blue b(PNP) cis[In(NCO)2Pc2-] · CH2Cl2, which crystallizes in the triclinic space group P1̄ (No. 2) with Z = 2. The two cyanato(N) ligands are in a mutually cis coordination (∠ (NNCO-In -NNCO) = 84.2(3)°). The In atom is displaced out of the plane of the four Niso atoms towards the two cyanato(N) ligands (d(In-Ct(Niso)4) = 0.988 Å). The average In-NNC0 and In-Niso bond distances are 2.16(1) and 2.216(8) Å, respectively. The NNCO-In -NNCO moiety deviates by ~ 4° from the staggered conformation relative to the In-(Niso)4 sceleton. Though the cyanato(N) ligands are essentially linear, there are different In-N -C angles (164.4(9) and 147.1(8)°) probably due to crystal packing effects. The Pc2- ligand is distorted in an asymmetrically convex manner. The PNP cation adopts the bent conformation (∠(P-N(K)-P) = 143.5(6)°). The cyclic voltammogram shows three electrode processes, which are assigned to the redox pairs: Pc3-/Pc2- (-0.87 V) < InI/InIII (-0.63 V) < Pc2- /Pc- (0.69 V).The UV-VIS-NIR spectra and the vibrational spectra are discussed.
Eine neue Verbindung im System Ba/Ln/Zn/Pt/O: Ba4Sm4Zn3PtO15/On a New Com pound in the System Ba/Ln/Zn/Pt/O : Ba4Sm4Zn3PtO15
Authors: Sfreddo O. , Rabbow Ch. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Reactions of mixtures of BaCO3, ZnO, Sm2O3 (3:5:1) heated in platinum crucibles up to 1250 °C led to big black single crystals of Ba4Sm4Zn3PtO15. The new compound crystallizes with hexagonal symmetry, space group C6v
4mc, a = 11.657, c = 6,789 Å , Z = 2. It is isotypic with Ba6Nd2Al4O15 but shows an ordered Pt4+ and Zn2+ distribution over the aluminium positions. The octahedrally coordinated barium sites of the Ba6Nd2Al4O15 type are occupied by Sm3+. In comparison to compounds of the composition Ba6Ln2M4O15 (M = Al, Fe, Co), Ba4Sm4Zn3PtO15 is the first example containing different oxidation states at the M3+ positions.
Darstellung, 11B-, 13C-, 1H-NMR - und Schwingungsspektren von μ-Pentamethylen-bis-hexahydro-closo-hexaborat, [B6H6(CH2)5B6H6]2-, und μ-Hexamethylen-bis-hexahydro-closo-hexaborat, [B6H6(CH2)6B6H6]2/Preparation, 11B, 13C, 1H NMR and Vibrational Spectra of μ-Pentamethylene-bis-hexahydro-closo-hexaborate, [B6H6(CH2)5 B6H6 ]2-, and μ-Hexamethylene-bis-hexahydro-closo-hexaborate, [B6H6(CH2)6B6H6]2-
Authors: Lübbe W. , Preetz W. 
Published: February 2015

Abstract
In the reaction of [B6H6]2- with diiodopentane or diiodohexane in dichloromethane μ-pentamethylene-bis-hexahydro-closo-hexaborate, [B6H6(CH2)5B6H6]2- (I), and μ-hexamethylene-bishexahydro-closo-hexaborate, [B6H6(CH2)6B6H6]2- (II), are formed, respectively. The products were separated from excess [B6H6]2- by ion exchange chromatography on diethylaminoethyl cellulose and have been identified and characterized by 11B, 13C, 1H NMR and vibrational spectroscopy.
2,5,8,11-Tetra-tert-butyl-peri-xanthenoxanthene and its Dication Spectroelectrochemistry and Model Calculations on a Dioxa-22-π-system
Authors: Frenking Gernot , Rieker Anton , Salbeck Josef , Speiser Bernd 
Published: February 2015

Abstract
Spectroelectrochemistry of 2,5,8,1 1-tetra-tert-butyl-peri-xanthenoxanthene 1 yields the UV/VIS spectra of the corresponding radical cation 1+ and dication 12+. The bathochromic shift for the dication 12+ relative to 1 and to the isoelectronic hydrocarbon anthanthrene (2) can be understood by quantum mechanical calculations (ab initio, AM1) of model structures.
Electroreduction of Organic Compounds, 27 Electrochemical Dehalogenation of Endosulfane
Authors: Gassmann J. , Voss J. , Adiwidjaja G. 
Published: February 2015

Abstract
Partial dechlorination takes place if Endosulfane® is electrolysed in methanol solution at lead cathodes. The products are detected and identified by GC/MS, IR and NMR spectroscopy. The structure of the product 2 is confirmed by an X-ray structural analysis.
Novel Enantiomerically Pure Ferrocenes
Authors: Zeijden Adolphus A . H. van der , Sieler J. , Hovestreydt E. 
Published: February 2015

Abstract
A chiral ferrocene (CpE
2Fe) was synthesized by reaction of CpELi with FeCl2(THF)1.5 The cyclopentadienyl ligand CpE contains a dimethylamino group that is separated from the Cp backbone by two stereogenic carbon centres. Reaction of CpE
2Fe with excess Mel affords the ammonium salt CpE
2Fe.2MeI. Its solid state structure was determined by X-ray diffraction methods.
Strukturverfeinerung von Kalium - periodat bei 297 und 150 K/Structure Refinement of Potassium Periodate at 297 and 150 K
Authors: Waal Danita de , Range Klaus-Jürgen 
Published: February 2015

Abstract
The scheelitetype structure of potassium perio­date, KIO4, has been confirmed and refined from single-crystal X-ray data at two temperatures. The compound crystallizes tetragonally, space group I41/a, with a = 5.726(1), c = 12.607(4) Å at 297(1) K, and a = 5.704(3), c = 12.478(8) Å at 150(1) K, respectively. Except for a significant decrease in the anisotropic displacement factors, the changes in the structural parameters at low temperature are rather small.
Geordnete Metallverteilung in KBaVO4 und KSrVO4 mit β-K2SO4-Struktur / Ordered Metal Distribution in KBaVO4and KSrVO4 Showing β -K2SO4 Structure
Authors: Schrandt O. , Müller-Buschbaum Hk. 
Published: February 2015

Abstract
Single crystals of KBaVO4(I) and KSrVO4(II) have been prepared by crystallization from V2O5 flux. The yellowish crystals show orthorhombic symmetry, space group D16
2h-Pnma with (I): a = 7.774(2), b = 5.899(1), c = 10.375(2) Å , (II): a = 7.400(2), b = 5.812(1), c -9.961(1), Z = 4. Both compounds show an ordered distribution of K+ and Ba2+ and Sr2+ respectively. The different sizes of the KO10 and BaO9 (SrO9) polyhedra are discussed with respect to those of the β-K2SO4 structure, considering the calculations of the Coulomb terms of lattice energy.
Metallkomplexe mit funktionalisierten Schwefelliganden, X [1] Ruthenium(II)-und Platin(II)-1-alkin-1-thiolato-Komplexe. Kristallstrukturanalyse von trans-(Ph3P)2Pt[S-C≡C-C(CH3)3]2 / Metal Complexes of Functionalized Sulfur Containing Ligands, X [1] Synthesis of Ruthenium (II) and Platinum(II) 1-Alkyne-1-thiolato Complexes. X-Ray Structure Analysis of trans-( Ph3P)2Pt[C-C≡C-C(CH3)3]2
Authors: Weigand Wolfgang , Weishäupl Michael , Robl Christian 
Published: February 2015

Abstract
The 1-alkyne-1-thiolates R-C ≡C-SLi [1a: R = C(CH3)3, 1b: R = C6H11 ] react with L2PtCl2 (L = PPh3, 1/2 dppe) and CpRu(PPh3)2Cl, respectively to give the complexes trans-(Ph3P)2Pt[S-C ≡C-C(CH3)3]2 (2a), cis-dppePt[S-C≡C-C(CH3)3]2 (2b), and CpRu(PPh3)2-(S-C ≡ C-R) [3a: R = C(CH3)3, 3b: R = C6H11]. 2a has been characterized by 31P CP/MAS NM R spectroscopy and its crystal structure determined by X-ray diffraction.
The Crystal Structure of Diammonium trans-Tetraammindisulfitonithenate(II)Tetrahydrate,trans-(NH4)2[Ru(SO3)2(NH3)4]·4H2O,and the Tuning of the trans-Influence of the Sulfite Ligand
Authors: Breitinger Dietrich K. , Breiter Roman 
Published: February 2015

Abstract
trans-(NH4)2[Ru(SO3)2(NH3)4]·4H2O(1) (monoclinic, P21/n; a = 629.8(3), b = 1000.6(2), c = 1345.7(5) pm, β = 112.25(4)°, Z = 2; R = 0.021; Rw = 0.017) is obtained as pale greenish-yellow crystals by reaction of trans-[Ru(SO3H)2(NH3)4] (2) with aqueous ammonia, and crystallization at +5 °C. The compound, when isolated, is stable at room temperature for only a few days even under inert gas, but persists under the mother liquor. In the centrosymmetric anion trans-[Ru(SO3)2(NH3)4]2- the bonds Ru-S = 230.5(1) pm are significantly longer than in the neutral complex 2 (227.6(1) pm), whereas the Ru-N bonds are the same in both com­plexes within experimental error (averages 214.1 and 214.0 pm). Hence, the mutual trans-influence of the sulfite ligands is weakened on protonation; the bonding of the co-ligands in cis-position is not affected. The internal structure of the sulfite ligand in 1 with long S-O bonds (average 151.2(5) pm) and small angles O-S-O (average 106.1(6)°) and the weakened Ru-S bond are a good match. The structure of 1 is held together by a complex network of hydrogen bonds, in which all potential hydrogen-bond donors (OH2, NH4
+, NH3) and acceptors (H2O ,SO3) are involved. The structural findings are reflected in the vibrational spectra.
Über die Darstellung, spektroskopische Charakterisierung und Kristallstruktur von Trifluormethylazosulfbn-N,N-dimethylamid (CH3)2NS(O)2NNCF3 / On the Preparation, Spectroscopic Characterization and Crystal Structure of Trifluoromethylazosulfon-N,N-dimethylamid (CH3)2NS(O)2NNCF3
Authors: Minkwitz Rolf , Jakob Jens , Kornath Andreas , Preut Hans 
Published: February 2015

Abstract
The reaction of Trifluoronitrosomethan with (CH3)2NS(O)2NH2 in THF and Na2CO3 as
Syntheses and Properties of Cerium Diphthalocyanines in High Oxidation States; Crystal Structure of [Ce(Pc)2](BF4) 0.33
Authors: Ostendorp G. , Rotter H. W. , Homborg H. 
Published: February 2015

Abstract
Ring oxidized green Cerium(IV)diphthalocyanines, [Ce(Pc)2]X (X = (poly)halide, NO3
-) are prepared by chemical oxidation of (nBu4N)[Ce(Pc2-)2] with the corresponding halogen in solution or of solid [Ce(Pc2-)2] with aqueous HNO3 Electrochemical oxidation of (nBu4N)[Ce(Pc2-)2] in solution in the presence of (nBu4N)BF4 yields [Ce(Pc)2](BF4)0.33, which crystallizes in the tetragonal space group P4/nnc (a, b = 19.643(3) Å, c = 6.525(3) A, Z = 2). The CeIV ion is eightfold coordinated by the isoindole N atoms (Niso) of the two staggered (ca. 41°), slightly distorted Pc ligands. The “[Ce(Pc)2]0.33+” subunits are arranged in infinite columns along [001] with the Ce atoms statistically disordered over two positions and Ce - Niso bond lengths of 2.45(1) and 2.69(1) A, respectively The UV-VIS spectrum is dominated by the transitions of the Pc2- ligand at ca. 15,000 (B band), 30,000 and 36,000 cm -1 (Q, N region). A low energy (“metallic”) band at ca. 2800 cm -1 typical for partially oxidized systems is present. The UV-VIS-NIR spectrum of [Ce(Pc)2]NO3 indicates a cofacial Pc2- - P c- complex. In addition to the π-π’ transitions of the Pc2- moiety at ca. 14,000, 30,000 and 36,000 cm-1, the Ch transition of the Pc- ring is observed at ca. 19,200 cm -1 and the typical NIR band at 6380 cm -1. Oxidation of a thin film of (PNP)[Ce(Pc2-)2] with dry Br2/ N2 gas yields purple [Ce(Pc-)2]Brx, whose UV-VIS-NIR spectrum shows the diagnostic features of dimeric Pc- radicals with intense bands at ca. 14,000 and 18,000 cm -1 assigned as B and Q1 bands, respectively. At ca. 9000 cm-1 the typical QD absorption is observed. The vibrational spectra are dominated by the transitions of the Pc- ligand at 1305/1445 cm -1 (IR) and 560/1120/1172/1591 cm-1 (resonance Raman). Excitation with 1064 nm strongly enhances the sym. C e-N stretch at 163 c m -1.
Tieftemperatur-Kristallstruktur der Einschlußverbindung {[N(CH3)4]+Cl]2
-} · CH3CN · H2O / Low-Temperature Crystal Structure of the Inclusion Compound {[N(CH3)4]+Cl]2
-} · CH3CN · H2O
Authors: Minkwitz Rolf , Bröchler Raimund , Preut Hans 
Published: February 2015

Abstract
The crystal structure of {[N(CH3)4
+Cl]2}·CH3CN · H2O is reported. Crystalls are orthorhombic, space group Pnma, with a = 1622.9(15), b = 671.3(6), c = 1511.2(11) pm, V = 1646(2) 106 pm3 and Z = 4.
Metallkomplexe von N-(Pyrrol-l-yl)salicylaldiminen und deren Strukturbestimmung mittels Röntgendiffraktometrie und Röntgenabsorptionsspektroskopie (XANES) / Metal Chelates of N -(Pyrrol-l-yl)salicylaldim ines and their Structure D eterm ination by X-Ray Structure Analysis and X -R ay Absorption Spectroscopy (XANES)
Authors: Bach A. , Beyer L. , Gelbrich T. , Hallmeier K. H. , Hennig C. , Möbius M. , Richter R. , Szargan R. , Fernandez V. , Losada J. 
Published: February 2015

Abstract
A series of three N-(pyrrol-l-yl)salicylaldim ines 1-3 has been prepared an d characterized. Their metal chelate complexes with Cu, Ni and Co are described. The molecular structures of bis[N-(pyrrol-l-yl)salicylaldim inato]copper(lI) la, bis{N-[3-(pyrrol-l-yl)propyl]- salicylaldiminato}nickel(II) 2b and tris{N-[3-(pyrrol-l-yl)propyl]salicylaldiminato}cobalt(III) 2d were determined by X-ray structure analysis. The chelates with tetracoordinated copper and nickel show a square planar coordination with the characteristic trans configuration. The chelate with hexacoordinated cobalt has a meridional coordination sphere. The complexes have also been investigated by X-ray absorption spectroscopy (X̲-ray A̲bsorption N̲ear E̲dge S̲tructure, XANES) at the K edges of the 3d metals. Analyzing the relative intensities of the Is → 3d prepeak and the K edges of the line shape, it was possible to distinguish between planar, tetrahedral and octahedral coordination of the chelates