Notizen: Eine neue bicyclische Zinn-Selen-Verbindung. Synthese und Kristallstruktur von [{Cp(CO)2Fe}3ClSn3Se4] / A New Bicyclic Tin Selenium Compound. Synthesis and Crystal Structure of [{Cp(CO)2Fe}3ClSn3Se4]

1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.

1985 ◽  
Vol 40 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Kay Jansen ◽  
Kurt Dehnicke ◽  
Dieter Fenske

The syntheses and IR spectra of the complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, CI, Br and the counter ion PPh4⊕ are reported. The azido and the bromo complexes are obtained from a solution of [Mo2(O2CPh)4] with PPh4N3 in pyridine or by reaction with PPh4Br in CH2Br2, respectively. When (PPh4)2[Mo2(O2CPh)4(N3)2] is dissolved in CH2Cl2, nitrogen is evolved and the complex with X = CI is obtained. The crystal structure of (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 was determined from X-ray diffraction data (5676 observed independent reflexions, R = 0.042). It crystallizes in the monoclinic space group P21/n with four formula units per unit cell; the lattice constants are a = 1549, b = 1400, c = 1648 pm, β = 94.6°. The centrosymmetric [Mo2(O2CPh)4Cl2]2⊖ ion has a rather short Mo-Mo bond of 213 pm, whereas the MoCl bonds are very long (288 pm)


1994 ◽  
Vol 49 (3) ◽  
pp. 430-433 ◽  
Author(s):  
Hans-Dieter Hausen ◽  
Jochen Tödtmann ◽  
Johann Weidlein

AbstractN-M ethyl-2-dimethylaluminium pyrrolide, (CH3)2Al -C4H3NCH3, crystallizes in the triclinic space group P1̄ with the lattice constants a = 700.5(1), b = 725.9(1), c = 886.8(1) pm, α = 67.69(1)°, β = 70.99(1)°, γ = 88.48(1)°, and Z = 2. This compound is isotypic with the gallium homologue [1], the shortest metal-ring contact between the two molecules of one unit cell decreases to 228.6 pm. N-dimethylgallium tetramethylpyrrolide has been synthesized from Li-N (CCH3)4 and (CH3)2GaCl. This “π-associate” crystallizes in the monoclinic space group P21/c with the lattice parameters a = 989.9(2), b = 1305.4(3), c = 878.3(2) pm, β - 112.73(1)° and 4 units per cell. Again two centrosymmetrically orientated molecules form a dimer by short (224.0 pm) intermolecular “Ga - πC ” contacts but the structure differs significant from the structure of the indium homologue [1].


1988 ◽  
Vol 43 (2) ◽  
pp. 135-137 ◽  
Author(s):  
H.-Jürgen Meyer ◽  
Joachim Pickardt

Ca2[Fe(CN)6] · C6H12N4 · 6H2O crystallizes in the monoclinic space group B2/b with a = 1130,2(4), b = 1373,5(4), c = 1353,0(4) pm and γ = 97,17°. The X-ray single crystal structure determination converged at R = 0.055 (2057 reflections). Each of the four Fe(CN)6 octahedra (Z = 4) in the unit cell is coordinated by six Ca atoms with mean NCYAN - Ca distances of 253.5(3) pm. The Ca atoms are bridged by hexamethylenetetramine and water molecules


2000 ◽  
Vol 55 (6) ◽  
pp. 484-486 ◽  
Author(s):  
B. v. Malottki ◽  
W. Preetz

By reaction of (n-Bu4N)2[ReBr6] with pyridine and (n-Bu4N)BH4 in dichloromethane various bromo-pyridine-rhenium(III) complexes are formed which can be separated by chromatography. Electrochemical oxidation of (n-Bu4N)2[ReBr5Py] leads to (n-Bu4N)[ReBr5Py]. X-ray structure determination on a single crystal has been performed of (n-Bu4N)[ReBr5Py] (monoclinic, space group P21/n a = 11,248(5), b = 17,192(5), c = 15,206(5) Å, β = 97,600(5)°, Z = 4).


Author(s):  
P. BHYRAPPA ◽  
K. S. SUSLICK

The synthesis, characterization and crystal structure of the octanitro-substituted porphyrin 5,10,15,20-tetrakis(3,5-dinitrophenyl)porphyrin, H 2 T (3,5- DNP ) P , are described. The solid state structure has two porphyrins in the unit cell with eight pyridine solvates and is made up from columnar arrays of the porphyrins. X-ray crystal structure data: monoclinic, space group P1 21/n1, a = 14.9996(9) Å, b = 8.2489(5) Å, c = 24.818(2) Å, α = 90 °, β = 104.172(1) °, γ = 90 °, V = 2977.3(3) Å3, dcalc = 1.440 g m-3, Z = 2.


1991 ◽  
Vol 46 (3) ◽  
pp. 307-314 ◽  
Author(s):  
Evamarie Hey-Hawkins ◽  
Hans Georg von Schnering

NaSi reacts with MoCl5 and 15-crown-5 in toluene with reduction of Mo(V) to Mo(IV). Work-up in DME yields MoCl4(DME)· 15-crown-5 (1). MoCl4(DME) (2) is prepared more conveniently from MoCl5/DME. 1 and 2 were characterized spectroscopically and by X-ray structure determination. Crystal data: 1, space group P212121 (No. 19), Z = 4, 2765 observed independent reflexions, R = 0.026, cell dimensions (110 K): a = 16.292(4), b = 12.884(3), c = 10.452(2) Å. 2, space group I4̄2d (No. 122), Z = 8, 558 observed independent reflexions, R = 0.037, cell dimensions (292 K): a = b = 9.562(2), c = 23.777(6)Å. The MoCl4(DME) molecule of 1 and 2 forms a distorted octahedron. There are four non-coordinating 15-crown-5 molecules present in the unit cell of 1. The UV/VIS spectrum and the magnetic properties of 2 are discussed.


1978 ◽  
Vol 33 (3) ◽  
pp. 261-264 ◽  
Author(s):  
Erich Sepp ◽  
Albert Pürzer ◽  
Gerhard Thiele ◽  
Helmut Behrens

Abstract The crystal structure of the [C7H7Fe(CO)3]- anion stabilized with the [(C6H5)4As]+ cation has been determinated by X-ray diffraction. The crystals are monoclinic, space group P21/n. The unit cell with lattice constants a = 1607.9 pm, b = 1386.8 pm, c = 1249.1 pm and β - 91.52° includes four formula units. The Fe(CO)3 group is bonded to the allyl anion part of the C7H7 ring system, while the diene part is unco-ordinated.


1998 ◽  
Vol 53 (11) ◽  
pp. 1335-1337 ◽  
Author(s):  
S. Kolf ◽  
W. Preetz

By reaction of K3[Os(NCS)3(SCN)3] with pyridine and glycerine the complex mer- [Os(NCS)3Py3] is formed. The X-ray structure determination on a single crystal (monoclinic, space group C2/c, a = 18.6156(12), b = 15.9448(7), c = 19.555(2) Å, β = 94.657(7)°, Z = 8) reveals that the nearly linear thiocyanate groups are exclusively bonded via the N atoms with Os-N-C angles ranging from 169.9° to 177.7°.


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


1982 ◽  
Vol 37 (11) ◽  
pp. 1361-1368 ◽  
Author(s):  
H.-J. Schweizer ◽  
Reginald Gruehn

By using chemical transport reactions with various transporting agents (HgCl2, NbCl5, Nb3O7Cl) a slightly substoiehiometric NbO2-phase, β-NbO2, was obtained from samples with O/Nb ∼ 1.5 (source; T > 1373 K) and with deposition temperatures > 1273 K (sink). The rango of composition of β-NbO2 was found to exist from NbO1.990 to NbO1.998.The structure of the tetragonal, column-shaped black crystals was determined by X-ray diffraction. It crystallizes tetragonally in the space group I41 with lattice constants a = 9.693(3) Å, c = 5.985(1) Å and Z = 10 formula units.The crystal structure of β-NbO2 is shown to be a deformed rutile type. As in α-NbO2 the Nb-atoms are grouped in pairs. However, both oxides are different with respect to their long-range order.


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