Darstellung und Kristallstruktur des Niob-(triphenylphosphinimino)tetrachlorids, Nb [NP (C6 H5 )3] Cl4, einer Verbindung mit einer Niob-Stickstoff-Mehrfachbindung /Preparation and Crystal Structure of Niobium(triphenyl-phosphineimino)tetrachloride, Nb[NP(C6H5)3]Cl4, a Compound with a Niobium Nitrogen Multiple Bond

1979 ◽  
Vol 34 (9) ◽  
pp. 1199-1202 ◽  
Author(s):  
Hans Bezier ◽  
Joachim Strahle

AbstractNb[NPPh3]Cl4 can be prepared by reacting NbCl4N3 with PPh3 in 1,2 dichloro ethane. The crystalline, yellow compound crystallizes in the monoclinic space group C2/c. The crystal structure consists of eight molecules, which are linked together via bridging chlorine atoms to centrosymmetric dimers. Thereby the niobium atoms obtain a sixfold coordination by one N and five Cl atoms. The triphenyl phosphine imine ligand is bound to niobium by its N atom. The approximate linearity of the resulting Nb-N-P group (angle Nb-N-P = 171°) and the distances Nb-N - 178 pm and N-P =164 pm can be interpreted by an sp hybridized N atom and double bonds to both the Nb and P atom.

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.


1991 ◽  
Vol 46 (2) ◽  
pp. 183-186

(TeCl3)(MoOCl4) is obtained by the reaction of TeCl4 and MoOCl3 in a sealed ampoule at 180 °C. It forms yellow-green moisture sensitive crystals. The crystal structure determination (lattice constants a = 734.8(1), b = 1281.5(3), c = 1172.2(2) pm, β = 94.62(2)°, monoclinic space group P 21/c, 2808 unique reflections for 92 parameters, final R = 0.029) shows that (TeCl3)(MoOCl4) consists of square pyramidal (MoOCl4-) anions and (TeCl3+) cations. The (MoOCl4-) anions are linked by asymmetric chlorine bridges and form centrosymmetric dimers (MoOCl4-)22- with the oxygen atoms located in the trans positions of the chlorine bridges. The coordination sphere for the Mo atom is a deformed octahedron of one oxygen and five chlorine atoms. Each trigonal pyramidal (TeCl3+) cation is connected by chlorine bridges to two neighboured (MoOCl4)22- anions resulting in a strongly deformed octahedral environment of six chlorine atoms for the Te atom. The MoOCl5 and TeCl6 octahedra are linked by edges and corners and form layers parallel to the be plane. Alternatively the structure can be regarded as a close packing of Cl and O atoms with the layer sequence ABAC, A ··· and Mo and Te atoms located in one quater of the octahedral holes.


1989 ◽  
Vol 44 (9) ◽  
pp. 1151-1154 ◽  
Author(s):  
André du Bois ◽  
Walter Abriel

Using 293 K diffractometer intensity data, the structure of [H3N(CH2)3NH3]SbCl5 has been determined by single crystal X-ray technique and refined to a final Rw of 0.026. The colorless crystals are monoclinic (space group P21/c) with a = 10.1338(5), b = 11.4623(7), c = 11.3668(6) Å, β = 113.52(5)° and Ζ = 4. The structure contains ψ-octahedral SbCl52- anions. A center of symmetry connects two anions forming a (Sb2Cl10)4- unit with rather long Sb—Cl distances for the bridging Cl-atoms (2.92 and 3.68 A, respectively).


1983 ◽  
Vol 38 (3) ◽  
pp. 317-320 ◽  
Author(s):  
Hans Bezler ◽  
Joachim Strähle

[TaCl4N3]2 reacts easily with PPh3 yielding TaCl4(NPPh3 ) , TaCl4(NPPh3)(NHPPh3) and TaCl5 . The latter are supposed to be products of the reaction of primarily formed TaCl4(NPPh3)2-TaCl4+ with the solvent ClCH2-CH2Cl. TaCl4(NPPh3) crystallizes in the monoclinic system with the space group P21/c. The crystal structure shows centrosymmetric dimers, in which the Ta atoms are linked together by asymmetric Cl bridges. The phosphinimino ligand is coordinated trans to the Cl bridge and causes a strong trans effect. A linear P = N = Ta group with double bonds of P = N = 159.3 and Ta = N = 180,1 pm is observed.


1988 ◽  
Vol 43 (10) ◽  
pp. 873-884 ◽  
Author(s):  
Stefanie Brummer

Abstract The 35Cl NQR spectra of 2,4,4,6-tetrachloro-3,5-dimethyl-cyclohexadiene-2,5-one-l and 2,4,4,6- tetrachloro-cyclohexadiene-2,5-one-l were studied from 77 K up to the decomposition temperature, their crystal structure having been determined by single crystal X-ray diffraction. The first com­pound crystallizes in the monoclinic space group C22h -P21/m with two molecules in the unit cell. The lattice constants are a = 887.2 (3) pm, b = 704.8 (3) pm, c = 824.0 (3) pm, β = 96.10(1)°. The sec­ond compound crystallizes orthorhombic, space group D182h - Cmca, with 8 molecules in the unit cell which has the dimensions a = 711.2(2) pm, b = 1388.4(3) pm, c = 1729.8(4) pm. The structures deter­mined belong to the stable phases of the title compounds as seen from the NQR spectra as a function of temperature which show no sign for a phase transition between the melting point and 77 K. In both title compounds the molecules are planar. Their symmetry is compared with other chloro- cyclohexadiene-2,5-ones-1 and chloro-cyclohexadiene-2,5-diones-1.4. The intramolecular distances d(C-Cl) of the sp2 carbon atoms and the 35Cl NQR frequencies assigned to the corresponding Cl atoms correlate quite well according to the theory: ν(35Cl) ~ (d(c-cl))-3 The relation is ν(35Cl)/MHz = 2 + 174 · 106 -(d/pm)-3.


1990 ◽  
Vol 45 (5) ◽  
pp. 603-606 ◽  
Author(s):  
Petra Runge ◽  
Mathias Schulze ◽  
Werner Urland

(CH3NH3)3PrCl6 · 2 H2O has been prepared as light green, air sensitive crystals by the reaction of PrCl3·xH2O with [CH3NH3]Cl in ethanol. The compound was characterized by crystal structure determination. Crystal data: monoclinic space group I 2/a, Z = 8. Lattice constants: a = 1963.3(4), b = 925.9(3), c = 1954.3(4) pm, β = 90.56(1)°. The compound forms [PrCl4(H2O)2]--chains where two Pr3+-ions are connected via two chlorine atoms. The magnetic behaviour of (CH3NH3)3PrCl6· 2H2O has been studied.


2022 ◽  
Vol 0 (0) ◽  
Author(s):  
Adrienne Ndiolene ◽  
Tidiane Diop ◽  
Ndiak Ndiaye ◽  
Mouhamadou Sembene Boye ◽  
François Michaud ◽  
...  

Abstract Two novel zinc(II) complexes containing 4-methoxybenzylidene moieties namely, Zn(L)Cl2 (L = N, N′-bis(4-methoxybenzylidene)ethane-1, 2-diamine (1) or N-(4-methoxybenzylidene)-ethane-1, 2-diamine (2)) have been synthesized and characterized by infrared spectroscopy and single-crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic space group P21/c with a = 9.2315(4); b = 12.0449(4); c = 18.2164(7) Å; β = 98.472(4)°, V = 1278.9(4) Å3 and Z = 4. Complex 2 crystallizes in the monoclinic space group P21/n with a = 6.5733 (2), b = 13.6595(5), c = 15.1615(5) Å; β = 101.846(4)°, V = 1332.33(8) Å3 and Z = 4. The environment of each Zn(II) atom is distorted tetrahedral with coordination of two terminal Cl atoms and two N atoms of the N,N′ – bis(4-methoxybenzylidene)ethane-1,2-diamine (1) or N-(4-methoxybenzylidene)ethane-1,2-diamine (2) ligand. The stability of the crystalline structure is ensured by the existence of intra- and intermolecular hydrogen bonds of the type C–H…Cl (1) and N–H…Cl (2) leading to supramolecular topologies.


2009 ◽  
Vol 65 (6) ◽  
pp. o1207-o1208 ◽  
Author(s):  
Abid Hussain ◽  
Shahid Hameed ◽  
Helen Stoeckli-Evans

The title compound, C17H16N2O5S, crystallized in the chiral monoclinic space groupP21, with two enantiomeric molecules (AandB) in the asymmetric unit. It is composed of a methylimidazolidine-2,4-dione unit substituted with a phenyl group and a 4-methoxyphenylsulfonyl group. The benzene ring mean planes are inclined to one another by 22.20 (14)° in moleculeAand by 15.82 (13)° in moleculeB. In the crystal structure, theAandBmolecules are linked by N—H...O hydrogen bonds, forming centrosymmetric dimers. A number of C—H...O interactions are also present in the crystal structure, leading to the formation of a three-dimensinoal network.


1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2


2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.


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