Synthese, Eigenschaften und Kristallstruktur von (NH4)NbOBr4/ Synthesis, Properties and Crystal Structure of (NH4)NbOBr4

1988 ◽  
Vol 43 (8) ◽  
pp. 981-984 ◽  
Author(s):  
Manfredo Hörner ◽  
Wolfgang Hiller ◽  
Joachim Strähle ◽  
George M. Sheldrick

Abstract (NH4)NbOBr4 is obtained as air sensitive, light red crystals from NH4Br and NbBr 5 in a sealed glass ampoule at 420 °C, whereby the oxygen presumably originates from the glass surface. The compound crystallizes in the monoclinic space group C2/m with a = 1269.9(1), b = 1384.7(2). c = 773.0(2) pm, β = 114.44(2)° and Z = 6. The structure is built up by NH4+ cations and polymeric NbOBr4 anions. Symmetrical linear oxo bridges with Nb-O = 199 pm connect square planar NbBr4 units to form endless chains arranged in planes parallel (010). Neighbouring NbBr4 units are in eclipsed as well as staggered orientations. The NH4+ cations are located between the planes of parallel NbOBr4 - chains. The vibrational frequencies of the IR and Raman spectrum are assigned.

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.


1977 ◽  
Vol 32 (7) ◽  
pp. 741-744 ◽  
Author(s):  
Walther Werner ◽  
Joachim Strähle

AgAuCl4 crystallizes in the monoclinic space group I2/c with Zi = 4. The crystal structure is built up by Ag+ cations and square planar AuCl4⁻ anions with Au-Cl bond length of 228 pm. The Ag+ ions have an octahedral coordination of Cl atoms. AgAuCl4 is topologically related to RbAuCl4.


1978 ◽  
Vol 33 (3) ◽  
pp. 265-267 ◽  
Author(s):  
Bernhard Nuber ◽  
Johannes Weiss ◽  
Karl Wieghardt

Abstract cis-Dioxo-dipicolinato-vanadate(V), Crystal Structure, IR, Raman The crystal structure of Cs[V(O)2(dipic)]·H2O (dipic = pyridine-2,6-dicarboxylate) has been determined by single crystal x-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/a, with cell constants a =737.8(3), 6=1917.5(5), c = 792.9(3) pm, β= 94.87(6)°, and Z = 4. The geometry about vanadium is a distorted trigonal bipyramid containing a cis-dioxo moiety (∢ O-V-O 109.9(3)°, V=O bond lengths 161.0(6) and 161.5(6) pm). Vibrational absorptions νs(V - 0) and νas(V=O) were found at 956 and 947 cm-1 in the IR and Raman spectrum, resp.


2011 ◽  
Vol 66 (8) ◽  
pp. 871-872
Author(s):  
Florian Kraus

The crystal structure of caesium tetrachlorido aurate(III), CsAuCl4, is presented. The compound crystallizes in the form of orange, needle-shaped single crystals in the monoclinic space group C2/c with a = 12.923(2), b = 6.1715(9), c = 96512(13) Å , β = 105.049(13)°, V = 743.34(19) Å3, and Z = 4. As expected, the compound consists of isolated Cs+ cations and square planar AuCl4- anions


1991 ◽  
Vol 46 (2) ◽  
pp. 147-156 ◽  
Author(s):  
Hans-F. Klein ◽  
Herbert Beck ◽  
Birgit Hammerschmitt ◽  
Udo Koch ◽  
Susanne Koppert ◽  
...  

Dinitrogen bridged cobalt(I) hydride compounds (L3CoH)2 N 2 (1: L = PMe3, 2: 3L = CH3C(CH2PMe2)3 have been synthesized by protonation of dinitrogen cobaltates. 1 crystallizes in the monoclinic space group C 2/m . a = 965, b = 1653, c = 1148 pm ,β = 106.88°, Z = 2. In solution 1 takes up N 2 reversibly forming CoH(N2)(PMe3)3 (1 a) . Infrared data including isotope labeling (15N , 2H) and assignment of vN = N and vCoH bands are presented. 1 reacts with aryl alkynes to give dialkynylcobalt(III) complexes CoH(C2,R1)(C2,R2)(PMe3)3 (5: R 1 = R 2 = C6H5; 6 : R 1 = R 2 = 4 -CH3C6H4; 7: R 1 = R 2 = 4-C lC 6 H 4; 8 : R 1 = C 6 H 5, R 2 = 4-ClC6H4) that are also obtained in a more convenient synthesis involving cobalt(I) intermediates Co(C2R1)(PMe3)4 (10: R 1 = 4 -CH3C6H4, 11: R 1 = 4-ClC6H4). Three metastable isomers of 5 have been characterized, the stable configuration is mer-trans as shown by a crystal structure determination: Space group P 21, a = 933.5(5), b = 1636.7(6), c = 901.1(3) pm, β = 97.4(1)°, Z = 2.


1989 ◽  
Vol 44 (12) ◽  
pp. 1483-1487 ◽  
Author(s):  
Hans Georg Stammler ◽  
Johannes Weiss

(S4N3)2Se2Cl10, (S4N3)2Se2Cl6 and [(S4N3)SeCl5]n are formed by the reaction of S4N4, Se2Cl2, and SOCl2. The structures of the three compounds where determined by X-ray diffraction. The yellow crystals of (S4N3)2Se2Cl,10 are monoclinic, space group P21/a, a = 817.5(2) pm, b = 1790.4(5) pm, c = 843.1(6) pm, β = 104.31(4)°, Z = 2. The Se2Cl,102- anion consists of 2 Cl-bridged distorted octahedra. (S4N3)2Se2Cl6 forms red monoclinic crystals, space group P21/c, a = 1036.5(3) pm, b = 1376.5(5) pm, c = 1400.4(4) pm, β = 100.65(2)°, Ζ = 4. In the Se2Cl62- anion the Se atoms have a square planar environment. The yellow crystals of (S4N3)SeCl5 are orthorhombic, space group P212121, a = 734.2(3) pm, b = 989.4(4) pm, c = 1627.4(6) pm, Z = 4. In the SeCl5- anion the Se atom has an octahedral environment of chlorine atoms, thus forming a polymeric structure.


1993 ◽  
Vol 48 (4) ◽  
pp. 425-430 ◽  
Author(s):  
K. Wurst ◽  
J. Strähle

Whereas (COD)PtCl2 usually reacts with bidentate phosphine ligands under substitution of the COD ligand, the reaction with the newly synthesized 1,4-bis-[di(t-butylphosphino)] butane results in the insertion of COD into one Pt-P bond affording [(t-Bu)2P(CH2)4 P(t-Bu)2-(C8H12)-PtCl]+Cl- (1). 1 crystallizes in the monoclinic space group C2/c with a = 3912.8(8), b = 1765.6(3), c = 3851.3(4) pm, β = 118.36(2)°, Ζ = 24. In the cation of 1 the second C=C bond remains coordinated to the central Pt2+ ion. The square-planar coordination of Pt2+ ion is completed by a Cl ligand and the second P atom of the phosphine ligand. The inserted C-C bond is elongated to 149(5) pm with respect to the coordinating C=C bond of 133(6) pm.


1997 ◽  
Vol 52 (2) ◽  
pp. 157-161 ◽  
Author(s):  
Ayhan Elmali ◽  
Yalcin Elerman ◽  
Ingrid Svoboda ◽  
Hartmut Fuess ◽  
Klaus Griesar ◽  
...  

Abstract [Cu2L] (L=N-2-hydroxy-4-methylphenyl-4-oxo-2-pentalketimine) was synthesized and its crystal structure determined. C24H26Cu2N2O4 monoclinic space group P21/n with a= 10.978(2), 17.045(3), c= 11.958(2) Å, β = 101.89(1)°, V = 2189.6(7) Å3,Z = 4. Two copper(II) atoms in a distorted square-planar coordination are bridged by two oxygen atoms to form a dinuclear unit. The copper(II) centers are separated by 3.025(1) Å and antiferromagnetically coupled (J =-222.3 cm-1 ), which follows from temperature-dependent magnetic susceptibility measurements in the range 4.2 to 300 K.


1989 ◽  
Vol 67 (11) ◽  
pp. 2041-2046 ◽  
Author(s):  
John Fawcett ◽  
John H. Holloway ◽  
David R. Russell ◽  
Anthony J. Edwards ◽  
Khalaf I. Khallow

3SbF3•4SbF5 has been prepared from the reaction of SbF3 with a large excess of SbF5 and from the reaction of WF5 with SbF5 in Genetron 113. An X-ray structure determination has shown that the compound crystallizes in the monoclinic space group P21/c with a = 8.547(10), b = 13.521(8), c = 19.551(12) Å, β = 100.3(1)°,Z = 4with the final residual indices of R = 0.0486 and Rw = 0.0526 for 4274 unique reflections. If only Sb—F distances of less than 2.1 Å are considered the structure can be viewed in terms of the arrangement (SbF2+)(SbF2+)(SbF6−)4. A Raman spectrum from single crystals of the compound is reported. Keywords: X-ray, structure, antimony, fluoride, Raman.


2013 ◽  
Vol 68 (5-6) ◽  
pp. 605-610 ◽  
Author(s):  
Christian Näther ◽  
Nicola Herzberg ◽  
Wolfgang Bensch

The new compound [Mn(dien)2][Mn(dien)SbS4]2 (dien=diethylenetriamine) was synthesized under solvothermal conditions. It crystallizes in the non-centrosymmetric monoclinic space group P21 with a=7.5736(5), b=19.1081(16), c=13.1174(11) Å, b =90:022(9) , V =1898.3(3) Å3, and Z =2. The crystal structure is composed of one [Mn(dien)2]2+ cation and an anionic chain composed of [SbS4]3- anions and [Mn(dien)2]2+ cations. The [SbS4]3- anions connect [Mn(dien)2]2+ ions in a μ2-fashion to form an undulated {[Mn(dien)SbS4]}-2 chain running along [001]. The Mn2+ ions in the chain are in a rare distorted rectangular pyramidal coordination environment with 3 N and 1 S atom forming the base and one S atom being located at the apex of the pyramid. The anionic chains and the cations alternate along [010]. Several relatively strong intra- and inter-chain N-H-S bonding interactions are observed. From the Raman spectrum the reduction of the ideal Td symmetry of the [SbS4]3- anions is obvious because more resonances occur than expected for the undistorted geometry


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