K2TiS3, ein neues Thiotitanat(IV) mit fünffach koordiniertem Titan / K2TiS3, A New Thiotitanate(IV) with Pentacoordinate Titanium

1992 ◽  
Vol 47 (2) ◽  
pp. 201-204 ◽  
Author(s):  
Kurt O. Klepp

Fibrous red crystals of the new compound K2TiS3 were obtained by reacting K2S, Ti and S at 1070 K. K2TiS3 is monoclinic, space group C 2/c with a = 11.667(6) Å, b = 8.325(4) Å, c = 6.494(4) Å, β = 9 i.81(4)°, Z = 4. The crystal structure was refined to a conventional residual of 0.070. The atomic arrangement is characterized by pseudo-one-dimensional -∞-[TiS3]2− chains formed by distorted TiS5 square pyramids sharing opposite edges of their basal planes. The structure - though closely related to that of Cs2TiS3 - is of a new type.

2000 ◽  
Vol 55 (1) ◽  
pp. 39-44 ◽  
Author(s):  
Kurt O. Klepp

Red crystals of Na4TiSe4 were obtained by reacting an intimate mixture of Na2Se, Ti and Se at 750°C. Na4TiSe4 is monoclinic, space group I2/a with a = 24.027(6), b = 7.346(4), c = 21.572(6) Å, (β = 104.52(2)°, Z = 16. Its crystal structure was determined from diffractometer data (AgK α-radiation) and refined to a conventional R of 0.036 for 2673 F0′s and 158 variables. The crystal structure is of a new type, characterized by the presence of discrete tetrahedral complex anions, [TiSe4]4- , which are arranged in slabs parallel to (100). The average Ti-Se bond length is 2.385(1) Å. The Na+ cations are in different chalcogen environments with distorted octahedral, square pyramidal or planar configurations, respectively


1992 ◽  
Vol 47 (7) ◽  
pp. 937-941 ◽  
Author(s):  
Kurt O. Klepp

Transparent single crystals of Na4Ga2S5 were obtained from a melt of Na2S, Ga and S. Na4Ga2S5 is monoclinic, space group P21/c with a = 7.967(1), b = 6.133(2), c = 19.852(9) Å, β = 91.61(2)°, Ζ = 4. Its crystal structure was refined to a conventional R of 0.033 for 1150 observed reflections.The structure of Na4Ga2S5 is of a new type. It is characterized by infinite ribbon like thiogallate anions, -, which are built up by GaS4-tetrahedra (mean Ga-S bond length 2.28 A) sharing apices and edges. The four crystallographically independent alkali cations are coordinated to six sulphur atoms in distorted octahedral configurations.


1988 ◽  
Vol 43 (2) ◽  
pp. 149-152 ◽  
Author(s):  
Karl-Friedrich Tebbe ◽  
Norbert Krauß

The new compound K[I(CN)2] can be prepared by addition of one formula unit of iodine to a concentrated aqueous solution of two mole equivalents of potassium cyanide. It crystallizes in the monoclinic space group C2/m with a = 736.4, b = 451.4, c = 908.0 pm, β = 92.56° and Z = 2. The crystal structure has been refined to Rf = 0.020 for 301 observed reflections.The structure may be described as a layer-like package of cations K+ and trihalide-analogous anions [I(CN)2]-. The anions are strictly linear at the I atoms (symmetry 2/m) and nearly linear at the C atoms with φ (I-C-N) = 178.6° and d(I-C) = 229.8, d(C-N) = 112.9 pm. The cation is surrounded by a slightly distorted octahedron of nitrogen atoms with d(K···N) = 284.8,292.6 pm


2014 ◽  
Vol 700 ◽  
pp. 156-160
Author(s):  
Yan Xu

A novel O-P-O bridged [Mn (3-MeOsalen)·H2O] (3-MeOsalen = N,N'-ethylenebis (3-methoxysalicylideneiminato) dianion) chain compound, namely [Mn2(3-MeOsalen)2(O2PPh2)(H2O)2] [Mn (3-MeOsalen)(H2O)2]·(ClO4)2·(H2O)4 (1) is successfully synthesized and structurally characterized. Compound 1 crystallized in monoclinic, space group P21/c. This compound consists of two fragments, the dinuclear cationic unit [Mn2(3-MeOsalen)2(O2PPh2)(H2O)2]+, which is resulted from O-P-O bridged cationic unit [Mn (3-MeOsalen)·H2O]+, and mononuclear unit [Mn (3-MeOsalen)(H2O)2]+, forming an one-dimensional chain by intermolecular hydrogen bonding and strong π-π stacking.


Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group


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.


1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.


1993 ◽  
Vol 48 (12) ◽  
pp. 1727-1731 ◽  
Author(s):  
A. Franken ◽  
W. Preetz ◽  
M. Rath ◽  
K.-F. Hesse

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and the base DBU in dichloromethane solution mononitropentahydrohexaborate [B6H5(NO2)]2- ions are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of the K and Cs salt were determined from single crystal X-ray diffraction analyses. K2[B6H5(NO2)] is monoclinic, space group P21/m with a = 5.953(1), b = 8.059(4), c = 8.906(1) Å, β = 109.553(9)°; Cs2[B6H5(NO2)] is monoclinic, space group P21/a with a = 9.438(6), b = 9.644(7), c = 11.138(9) Å, β = 101.44(9)°. The B6 octahedron is compressed in the direction of the B—NO2 bond by about 5%, with bond lengths between 1.67 and 1.77 A.


1996 ◽  
Vol 51 (2) ◽  
pp. 277-285
Author(s):  
Rolf Minkwitz ◽  
Ulrike Lohmann ◽  
Hans Preut

Abstract The synthesis of salts of the type RnSH3-n+MF6- (R = C2H5, i-C3H7; n = 1, 2; M = As, Sb) by protonation of the corresponding thiols and sulfides in the superacid systems HF/MF5 is reported. The salts have been characterized by vibrational and NMR spectroscopic methods. Isopropylsulfonium hexafluoroantimonate is the first known example of a sulfonium salt, for which a SH bond distance has been determined by a crystal structure analysis, i-C3H7SH2+SbF6- crystallizes in the monoclinic space group P21/m with a = 568.0(4), b = 801.1(6), c = 1019.7(8) pm, β = 82.63(6) °, with two formula units per unit cell.


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