| 1 | Author
| T. J. Bastow | Requires cookie* | | Title
| 47,49jj NMR in Metals, Inorganics, and Gels  | | | Abstract
| Some recent progress in solid state 47,49 Ti NMR is described and reviewed. The metallic-state work described covers metals such as hep titanium, TiB 2 , a number of intermetallics such as TiAl 2 and TiAl 3 . The inorganic work covers the various titanium oxide based materials including the Ti0 2 polymorphs, anatase, rutile and brookite. The gel work covers the evolution of crystalline titania from gels formed by hydrolysis of titanium isopropoxide. Some complementary data from 17 0 and 13 C NMR and powder X-ray diffraction is also included. | | |
Reference
| Z. Naturforsch. 55a, 291—297 (2000); received September 11 1999 | | |
Published
| 2000 | | |
Keywords
| Titanium, NMR, Metals, Oxides, Gels | | |
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| default:Reihe_A/55/ZNA-2000-55a-0291.pdf | | | Identifier
| ZNA-2000-55a-0291 | | | Volume
| 55 | |
3 | Author
| DietrichW. Wabner, Rainer Huss, Fritz Hindelang, HeinzP. Fritz, Detlef Missol | Requires cookie* | | Title
| Bleidioxid-Verbundelektroden für die Elektrosynthese, II Vorbehandlung von Titan für die Bleidioxidabscheidung 1 Lead Dioxide Electrodes for Electrosynthesis, II Pretreatment of Titanium for the Deposition of Lead Dioxide  | | | Abstract
| A novel method enables the production of lead dioxide-coated electrodes with life times of several thousand hours in certain electrooxidations. The most important step of this technique is described as an adsorption of Ti(IV)-oxalate at the titanium surface. By potential-time plots and by potentiodynamic investigation it is shown, that by Ti(IV)-adsorption the titanium surface is lifted to a higher (more noble) potential and in this way is protected against further dissolution or oxidation. | | |
Reference
| (Z. Naturforsch. 31b, 45—50 [1976]; eingegangen am 16. September 1975) | | |
Published
| 1976 | | |
Keywords
| Lead Dioxide Electrodes, Electrosynthesis, Titanium | | |
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| default:Reihe_B/31/ZNB-1976-31b-0045.pdf | | | Identifier
| ZNB-1976-31b-0045 | | | Volume
| 31 | |
4 | Author
| J. Schmachtel, Hk, Müller-Buschbaum | Requires cookie* | | Title
| Oxotitanate mit gemischter Valenz, II Zur Kenntnis von Sr2Ti6013 Oxotitanates with Mixed Valence, II About Sr2Ti60i3  | | | Abstract
| Single crystals of Sr2TieOi3 were prepared by heating a mixture of SrO • Ti203 • 2 TiOo in a vacuum furnace to 1800 °C for 6 hours. X-ray investigations show monoclinic sym-metry (a = 1525,0, b = 376,9, c = 916,4 pm; ß = 99,15°, space group Cgh-C2/m). Sr2Ti60i3 is isotypic with Ba2Ti60i3. | | |
Reference
| (Z. Naturforsch. 35b, 4—6 [1980]; eingegangen am 9. Oktober 1979) | | |
Published
| 1980 | | |
Keywords
| Strontium, Titanium, Oxygen, Crystal Structure | | |
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| default:Reihe_B/35/ZNB-1980-35b-0004.pdf | | | Identifier
| ZNB-1980-35b-0004 | | | Volume
| 35 | |
5 | Author
| Amal Haoudi-M, Ahmed Azzah, Hans-Georg Mazzah, M. Schmidt, H. Athias Noltemeyer, W. Erbert, Roesky | Requires cookie* | | Title
| Synthese und Struktur von achtgliedrigen Titan-und Zirkon-haltigen Siloxanringen Synthesis and Structure of Eight-Membered Titanium and Zirconium Containing Siloxane Rings  | | | Abstract
| Reaction o f (fBu)2Si(OH)2 with TiCl4, TiBr4, T il4, and ZrCl4 affords eight-membered rings | | |
Reference
| Z. Naturforsch. 46b, 587—5 (1991); eingegangen am 23. Juli 1990 | | |
Published
| 1991 | | |
Keywords
| Titanium, Zirconium, Siloxane, Heterocycles | | |
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| default:Reihe_B/46/ZNB-1991-46b-0587.pdf | | | Identifier
| ZNB-1991-46b-0587 | | | Volume
| 46 | |
6 | Author
| E. Peters, Hk Müller-Buschbaum | Requires cookie* | | Title
| Ein Titan-Tantaloxid mit Ti11: Ti0 ,3 3 Ta0 ,6 7O2 (TiTa20 6)  | | | Abstract
| Black single crystals o f Tio^Tao 670 2 have been prepared by C 0 2-LA SER techniques heating a mixture of TiO and Ta20 5 to T > 2000 °C. The titanium tantalum oxide crystallizes with tetragonaj symmetry, space group D 4 h -P 4 2/mnm, lattice constants a = 4.7344(6) A, c = 3.0504(2) A , Z = 2. Ti().33Ta0.67O 2 represents the compound TiTa20 6 with rutile structure because of the statistical distribution of Ti2+ and Ta5+. The composition of rutile-type com pounds is discussed in more general terms. | | |
Reference
| Z. Naturforsch. 50b, 1167—1170 (1995); eingegangen am 16. Januar 1995 | | |
Published
| 1995 | | |
Keywords
| Titanium, Tantalum, Oxide, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-1167.pdf | | | Identifier
| ZNB-1995-50b-1167 | | | Volume
| 50 | |
7 | Author
| E. Peters, Hk Müller-Buschbaum | Requires cookie* | | Title
| Über ein niedervalentes Titan-Wolframoxid: Ti0 ,54W 0,46^2 On a Low Valent Titanium Tungsten Oxide: Ti0 54W 0 .46^2  | | | Abstract
| Single crystals of Ti0 .54W0. 460 2 have been prepared by C 0 2-LASER techniques. This phase crystallizes with a non-distorted rutile structure, space group D4h-P42/mnm, a = 4.6862(4), c = 2.9039(3) A, Z = 2. Split positions of the statistically distributed metal ions show the existence of W-W pair formation as reported for pure W 0 2. | | |
Reference
| (Z. Naturforsch. 51b, 29—31 [1996]; eingegangen am 27. Juli 1995) | | |
Published
| 1996 | | |
Keywords
| Titanium, Tungsten-Pairs, Rutile-Type | | |
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| default:Reihe_B/51/ZNB-1996-51b-0029.pdf | | | Identifier
| ZNB-1996-51b-0029 | | | Volume
| 51 | |
8 | Author
| A. N. Ägele3, E. A. Nokhinab, J. Sitarb, H.-JM. Eyer3, A. Lachgarb | Requires cookie* | | Title
| Synthesis and Crystal Structures of ATi[Nb6Cli8] Compounds (A = K, Rb, Cs, In, Tl)  | | | Abstract
| New quaternary niobium cluster chlorides corresponding to the general formula ATi[Nb6Clis] (A = K, Rb, Cs, In, Tl) have been synthesized in sealed quartz tubes at 720 °C, starting from stoichiometric amounts of NbCls, niobium metal, TiCb, and AC1 (A = K, Rb, Cs), or In or Tl metals. The structures of RbTi[Nb6Clis] and CsTifNböClis] were determined using single crystal X-ray diffraction. RbTifNböClis] crystallizes in the rhombohedral crystal system, space group R3 (no. 148), Z = 3, with lattice parameters: a = 9.163(4), c = 25.014(14) A (hexagonal setting). The structure refinement converged to R] = 0.044 and wRi = 0.058 for all data. In this structure, discrete [NböClig]4-cluster units are linked by Rb+ and Ti3+ cations, located in a 12-coordinated anticubeoctahedral and octahedral chloride coordination environment, respectively. In contrast, CsTifNböClis] crystallizes in the trigonal crystal system, space group P31c (no. 163), Z = 2. The lattice parameters were determined to be a -9.1075(6), c = 17.0017(8) A. The structure refinement gives the reliability factors Ri = 0.029 and wRa = 0.063 for all data. The structure is built up of discrete octahedral [N bödis]4-cluster units, linked by Cs+ and Ti3+ cations which are located in a distorted hexagonal antiprismatic and octahedral chloride coordination environment, respectively. The structures of the compounds ATifNböClis] (A = K, In, Tl) were found to be isotypic with RbTi[NböCli8], and their unit cell parameters were refined using X-ray powder diffraction analysis. In tro d u ctio n | | |
Reference
| Z. Naturforsch. 55b, 139—144 (2000); received September 13 1999 | | |
Published
| 2000 | | |
Keywords
| Niobium, Titanium, Cluster, Chlorides, Synthesis | | |
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| default:Reihe_B/55/ZNB-2000-55b-0139.pdf | | | Identifier
| ZNB-2000-55b-0139 | | | Volume
| 55 | |
9 | Author
| J. Schmachtel, Hk Müller-Buschbaum | Requires cookie* | | Title
| Oxotitanate mit gemischter Valenz, III Zur Kenntnis von BaTi8016 Oxotitanates with Mixed Valence. III About BaTisOie  | | | Abstract
| The hitherto unknown compound BaTisOi6 was prepared by heating a mixture of Ba0:Ti02 = 1:4 in a vacuum furnace to 1400 °C (Ti crucible). Single crystal X-ray investigations show monoclinic symmetry (a — 1420,9, b = 297,1, c — 998,1 pm, ß = 133,50°; space group C|-C2). The crystal structure was found to be isotypic to a-Mn02. | | |
Reference
| Z. Naturforsch. 35b, 332—334 (1980); eingegangen am 14. Dezember 1979 | | |
Published
| 1980 | | |
Keywords
| Barium, Titanium, Oxide, Crystal Structure, a-Mn02-Type | | |
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| default:Reihe_B/35/ZNB-1980-35b-0332.pdf | | | Identifier
| ZNB-1980-35b-0332 | | | Volume
| 35 | |
10 | Author
| Yüniu Bai, M. Athias Noltemeyer, H. Erbert, W. Roesky | Requires cookie* | | Title
| Synthese und Strukturen von Monoalkylamiden und -imiden des Titans Synthesis and Structures o f M onoalkylam ides and -imides of Titanium  | | | Abstract
| A new method for the preparation o f m onoalkylam ides o f com position Cp'TiCl2N H R is reported. M e3SnN H R (R = /Bu l a , CH/Pr-, lb) reacts with Cp'TiCl3 with elimination o f M e3SnCl to yield Cp'TiCLNHR (2) (2a: Cp' = C 5H 5, R = /Bu, 2b: Cp' = M e3SiC5H 4, R = t Bu, 2c: Cp' = (M e3Si)?C 5H 3, R = /Bu, 2d: Cp' = M e4C5H, R = /Bu, 2e: Cp' = M e5C5, R = t Bu, 2f: Cp' = C5H 5, R = CH/Pr2, 2g: Cp' = M e3SiC5H 4, R = CH/Pr2, 2h: Cp' = (M e3Si)2C5H3, R = CH/Pr2, 2i: Cp' = M e4C5H , R = CH/Pr2, 2j: Cp' = M e5C5, R = CH/Pr2). Compounds 2 a -2 j are stable and eliminate HC1 only in the presence o f a strong base to form (C5H 5T iC lN /B u)2 (3a) or (M e3SiC5H4T iC lN /B u)2 (3b) from 2 a and 2b, respectively. In 3a the chlorine atom s are substituted by N H /B u groups in boiling T H F by means o f L iN H /Bu to give (C5H 5T iN H /B uN /B u)2 (4). The reactions o f 2 e and 2b with L iN (SiM e3)2-Et20 in the presence o f pyridine yield M e5C5T iC lN /B u • Py (5 a) (Py = pyridine) and M e3SiC5H4T iC lN /B u P y (5 b), respectively. Com pounds 2 e and 5 a have been characterized by X-ray crystal structural analysis. | | |
Reference
| Z. Naturforsch. 46b, 1357 (1991); eingegangen am 22. März 1991 | | |
Published
| 1991 | | |
Keywords
| X -Ray, Synthesis, Titanium, Amides, Imides | | |
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| default:Reihe_B/46/ZNB-1991-46b-1357.pdf | | | Identifier
| ZNB-1991-46b-1357 | | | Volume
| 46 | |
11 | Author
| S. Möhr, Hk Müller-Buschbaum | Requires cookie* | | Title
| Ein gemischtvalentes Oxometallat mit Cr3+ anstelle von Ti3+: Ba2Ti4+Cr20 13  | | | Abstract
| Single crystals of Ba2Ti4+C r20 13 w ere p rep a red by C 0 2-L A S E R h igh te m p era tu re r ea ctio n s and in v estig a te d by X -ra y w o rk . T h e c o m p o u n d c ry sta llize s w ith m o n o c li nic sym m etry, a = 15.0 1 8 5 , b = 3 .9 4 1 9 , c -9 .0 7 6 4 Ä , ß = 9 8 .1 3 7 °, Z = 2. B a 2T i4Cr20 13 is iso ty p ic to N a 2T i60 13. T h e crystal stru ctu re is d isc u sse d w ith r e sp e ct to o rd ered or d iso rd ered d istrib u tio n s o f T i4+ and C r3+ u sin g c a lc u la tio n s o f C o u lo m b term s o f la ttice energy. It is sh o w n , th at th e sta b ility o f th is stru ctu re ty p e w ill b e d e c r e ased by rep la ce m en t o f N a + by io n s w ith h ig h er o x id a tio n sta tes. | | |
Reference
| Z. Naturforsch. 49b, 911 (1994); eingegangen am 17. Februar 1994 | | |
Published
| 1994 | | |
Keywords
| Barium, Titanium, Chromium, Oxide, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0911.pdf | | | Identifier
| ZNB-1994-49b-0911 | | | Volume
| 49 | |
12 | Author
| S. Trojanov, A. Stiewe, E. Kemnitz | Requires cookie* | | Title
| Synthese und Struktur saurer Ubergangsmetallsulfate - Ti(H50 2)(S 0 4)2(H20 ) 2 und Zr(H30 ) 2(S 0 4)3 Synthesis and Structure of Acid Transition Metal Sulfates - Ti(H50 2)(S 0 4)2(H20 )2 and Zr(H30 ) 2(S 0 4)3  | | | Abstract
| From the ternary system Mn(S 0 4)n/2 / S 0 3 / H20 (Mn+ = Zr4+, Ti3+) two new acid metal sulfates, Ti(H50 2)(S 0 4)2(H20)2 and Zr(H30) 2(S 0 4)3, have been synthesized and structurally characterized. Ti(H50 2)(S 0 4)2(H->0)i crystallizes in the orthorhombic space group Pnma with cell parameters a = 9.858(5), b = 18.32(2), c = 5.437(7)Ä (Z = 4); Zr(H30) 2(S 0 4)3 crystallizes in the triclinic space group PI with cell parameters a = 5.092(2), b = 8.533(3), c = 12.388(6)A, a = 92.95(3)°, ß = 90.89(3)°, 7 = 94.35(3)° (Z= 2). In the titanium compound there are slightly distorted T i0 6 octahedra with T i-0 distances between 1.99 and 2.09 A which are sharing corners with S 0 4 tetrahedra. Through hydrogen bonds layers are formed perpendicular to the 6-axis. These layers are connected by H30 + ions only. The structure of Zr(H30) 2(S 0 4)3 consists of three different S 0 4 tetrahedra and distorted Zr07 polyhedra which are connected via common corners and edges to form columns parallel to the a-axis. The Z r-0 distances vary from 2.13o to 2.18A for equatorial positions, significantly longer than the axial Zr-O distances with 2.05A. | | |
Reference
| (Z. Naturforsch. 51b, 19—24 [1996]; eingegangen am 13. Juni 1995) | | |
Published
| 1996 | | |
Keywords
| Synthesis, Crystal Structure, Titanium, Zirconium, Hydrogen Sulfates | | |
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| default:Reihe_B/51/ZNB-1996-51b-0019.pdf | | | Identifier
| ZNB-1996-51b-0019 | | | Volume
| 51 | |
13 | Author
| HkM. Üller-Buschbaum, B. M. Ertens | Requires cookie* | | Title
| Single Crystal X-Ray Analysis of Ba3Ce R  | | | Abstract
| Single crystals of (I) Ba3C eRu20 9, (II) Ba3SmRu20 9, (III) Ba3D yR u20 9, (IV) Ba3ErRu20 9 and (V) Ba3Ti24Ru0.6O 9 have been prepared by high temperature solid state reactions. The compounds were exam ined by X-ray techniques. They crystallize with hexagonal symmetry, | | |
Reference
| (Z. Naturforsch. 51b, 79 [1996]; eingegangen am 18. Mai 1995) | | |
Published
| 1996 | | |
Keywords
| Barium, Rare Earth, Ruthenium Oxide, Titanium, Crystal Structure | | |
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| default:Reihe_B/51/ZNB-1996-51b-0079.pdf | | | Identifier
| ZNB-1996-51b-0079 | | | Volume
| 51 | |
14 | Author
| Bernd Schwarze, Wolfgang Milius, Wolfgang Schnick | Requires cookie* | | Title
| Synthese und Kristallstruktur von [(CXjSi^N^TiC^ -ein perchloriertes N-Silyl-titanamid Synthesis and Crystal Structure of [(Cl3Si)2N]2TiCl2 -a Fully Chlorinated N-Silyl Titanium Amide  | | | Abstract
| The chlorinated titanium amides [(Cl3Si)2N]2TiCl2 (1) and (Cl3Si)2NTiCl3 have been syn thesized selectively from hexachlorodisilazane lithium and TiCl4. The crystal structure of 1 was determined by single crystal X-ray methods at room temperature (P2|2j 2 |, a = 1232.4(2), b = 1265.5(2), c -1469.1(2) pm, Z = 4). The central titanium atom of 1 is bound to two nitrogen atoms and two Cl atoms and is weakly coordinated further by two Cl atoms of the trichlorosilyl groups. | | |
Reference
| Z. Naturforsch. 52b, 819—822 (1997); eingegangen am 1. April 1997 | | |
Published
| 1997 | | |
Keywords
| N-Silyl Titanium Amides, Trichlorosilyl Groups, Crystal Structure, Titanium | | |
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| default:Reihe_B/52/ZNB-1997-52b-0819.pdf | | | Identifier
| ZNB-1997-52b-0819 | | | Volume
| 52 | |
15 | Author
| Thomas Miekisch, Klaus Harms, Sigrid Wocadlo, Werner Massa, Bernhard Neumüller, Christoph Frommen, Kurt Dehnicke, Herrn Prof, J. Dr, Lorberth | Requires cookie* | | Title
| [TiJv Cl8(NPMe3)3]Cl und [Vnw vCl4(NPPh3)3] Crystal Structures of the Phosphoraneiminato Complexes [Ti3v Cl8(NPMe3)3]Cl and [vl"/IVCl4(NPPh3)3]  | | | Abstract
| [Ti3Cl8(NPMe3)3]Cl has been prepared by the reaction of TiCl3(THF)3 with Me3SiNPMe3 in dichloromethane forming green moisture sensitive crystals. According to the crystal structure determination the titanium atoms of the cation [Ti3Cl8(NPMe3)3]+ are linked by two /x3-N atoms of two NPMe3~ groups forming a distorted trigonal-bipyramidal arrangement. The third NPMe3_ group and two of the chlorine atoms have /i2-bridging functions. The mixed-valence complex [V2Cl4(NPPh3)3] is formed as dark green moisture sensitive crystals by the reaction of vanadium trichloride with Me3SiNPPh3 in boiling toluene. According to the crystal structure determination the vanadium atoms are linked by two /z2-N atoms of two NPPh3_ groups forming a nonplanar V2N2 four-membered ring with a V-V distance of 266.8(1) pm which corresponds to a (a, 1/27r) bond type. This is confirmed by the measurement of the magnetic susceptibility which leads to a magnetic moment of 1.45(5) B. M., corresponding to the remaining d 1 -electron. | | |
Reference
| Z. Naturforsch. 52b, 1484—1490 (1997); eingegangen am 8. September 1997 | | |
Published
| 1997 | | |
Keywords
| Phosphoraneiminato Complexes, Titanium, Vanadium, Crystal Structure | | |
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| default:Reihe_B/52/ZNB-1997-52b-1484.pdf | | | Identifier
| ZNB-1997-52b-1484 | | | Volume
| 52 | |
16 | Author
| Regina Bettenhausen, Wolfgang Milius, Wolfgang Schnick | Requires cookie* | | Title
| Synthese und Kristallstruktur von [H2NMe2]+[(Me2 NH)2 TiCl4 ]_ Synthesis and Crystal Structure of [H2NMe2]+[(Me2NH)2TiCl4]~  | | | Abstract
| The title compound has been synthesized as a green solid by the reaction of M eCl2 SiNHSiM e3 and Ti(NM e2)4 in CH2C12. The crystal structure was determined by single crystal X-ray methods at room temperature (C2/c, a = 1825,7(4), b = 909,9(2), c = 1116,1(2) pm, ß = 125,09(3)°, Z = A,R\= 0,047, wR2 = 0,147) to be an ionic salt [H2NMe2]+[(Me2NH)2TiCl4]" . The central titanium(III) atom of the anion is bound to four Cl atoms and weakly coordinated by two Me2NH ligands. | | |
Reference
| Z. Naturforsch. 53b, 239—241 (1998); eingegangen am 20. November 1997 | | |
Published
| 1998 | | |
Keywords
| N-Silyl Amides, Crystal Structure, Titanium | | |
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| default:Reihe_B/53/ZNB-1998-53b-0239.pdf | | | Identifier
| ZNB-1998-53b-0239 | | | Volume
| 53 | |
17 | Author
| Andreas Mommertz, Roland Leo, Werner Massa, Kurt Dehnicke | Requires cookie* | | Title
| Uber die Reaktion von Bis(f-butylamino)dimethylsilan mit Titantetrachlorid. Kristallstrukturen des Imido-Komplexes [TiCl2 (N-CMe3 )(H2 N-CMe3 )(CH3CN)]2 und des Ketimido-Komplexes [TiCl3 {NC(Me)N(H)CMe3}(CH3CN)2 ]  | | | Abstract
| On the Reaction of Bis(f-butylamino)dimethylsilane with Titanium Tetrachloride. Crystal Structures of the Imido Complex [TiCl->(N-CMe3)(H-,N-CMe3)(CH3CN)]2 and of the Ketimido Complex [TiCl3{NC(Me)N(H)CMe3}(CH3CN)2] The reaction of bis(f-butylamino)dimethylsilane with titanium tetrachloride in dichloro methane solution leads to a mixture of compounds from which the imido complex (H3N-CMe3)2[TiCl3(N-CMe3)]2 (1) and by extraction of the residue with acetonitrile the imido complex [TiCl2(N-CMe3)(H2N-CMe3)(CH3CN)]2 (2) can be isolated. 1 reacts with acetonitrile to give the ketimido complex [TiCl3{NC(Me)N(H)CMe3}(CH3CN)2] (3). According to crystal structure determinations 2 consists of centrosymmetric dimeric molecules containing TiCl2Ti bridges, the N-CMe3~ ligands being in equatorial positions with TiN bond lengths of 168.8(4) pm which corresponds to double bonds. In the monomeric complex 3 the chloro ligands are in meridional positions of the distorted octahedrally coordinated titanium atom with a TiN bond length of 175.7(2) pm of the ketimido ligand. | | |
Reference
| Z. Naturforsch. 53b, 887—892 (1998); eingegangen am 27. April 1998 | | |
Published
| 1998 | | |
Keywords
| Titanium, Imido Complex, Ketimido Complex, Crystal Structure | | |
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| default:Reihe_B/53/ZNB-1998-53b-0887.pdf | | | Identifier
| ZNB-1998-53b-0887 | | | Volume
| 53 | |
18 | Author
| K. Urt, O. Klepp | Requires cookie* | | Title
| Preparation and Crystal Structure of Na4TiSe4. A Selenotitanate with Discrete Tetrahedral Anions  | | | Abstract
| 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) A, (3 = 104.52(2)°, Z = 16. Its crystal structure was determined from diffractometer data (AgK a-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, [TiSe,*]4" , which are arranged in slabs parallel to (100). The average Ti-Se bond length is 2.385(1) A. The Na+ cations are in different chalcogen environments with distorted octahedral, square pyramidal or planar configurations, respectively. | | |
Reference
| (Z. Naturforsch. 55b, 39—44 [2000]; received September 28 1999) | | |
Published
| 2000 | | |
Keywords
| Crystal Structure, Chalcogenides, Titanium, Sodium, Selenium | | |
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| default:Reihe_B/55/ZNB-2000-55b-0039.pdf | | | Identifier
| ZNB-2000-55b-0039 | | | Volume
| 55 | |
19 | Author
| ;.M = Ti, ZrDieter Fenske, Eva Hartmann, Kurt Dehnicke | Requires cookie* | | Title
| N,N'-Bis(trimethylsilyl)benzamidinato-Koniplexe von Titan und Zirkon. Die Kristallstrukturen von [C 6 H 5 -C(NSiMe3) 2 MCl 3 ] 2 ; M = Ti, Zr N,N'-Bis(trimethylsilyl)benzamidinato Complexes of Titanium and Zirconium. The Crystal Structures of [C 6 H 5 -C(NSiMe 3 ) 2 MCl 3 ]  | | | Abstract
| The N,N'-bis(trimethylsilyl)benzamidinato complexes [C 6 H 5 -C(NSiMe 3) 2 MCl 3 ] 2 (M = Ti. Zr) have been prepared by the reactions of N,N,N'-tris(trimethylsilyl)benzamidine, [C 6 H 5 — C(NSiMe 3)N(SiMe 3) 2 ] with titanium tetrachloride, and zirconium tetrachloride, respec-tively. The compounds form moisture sensitive, dark red (Ti) and white (Zr) crystals, which were characterized by crystal structure determinations. [C 6 H 5 —C(NSiMe 3) 2 TiCl 3 ] 2 : space group P2,/rc. Z = 2, 4373 observed independent reflexions, R = 0.034. Lattice dimensions (-90 °C): a — 959.0(8); b = 1196.5(8); c = 1770.9(11) pm; ß = 93.79(4)°. [C 6 H 5 -C(NSiMe 3) 2 ZrCl 3 ] 2 : space group P2,/«. Z = 2, 3160 observed independent reflexions, R = 0.031. Lattice dimensions (-90 °C): a = 971.6(7); b = 1222.2(9); c = 1792.9(10) pm; ß = 93.51(5)°. Both complexes crystallize isotypically, forming centrosymmetric dimeric molecules via chloro bridges with bond lengths of 242.0 and 253.8 pm (Ti), and of 253.7 and 264.9 pm (Zr). The metal atoms complete their distorted octahedral surroundings with two chlorine ligands and the nitrogen atoms of the chelating amidinato ligand. The N atoms of the amidinato group are in equatorial and axial positions. This accounts for the different metal-nitrogen bond lengths of 207 pm (ax) and 199 pm (eq) in the titanium compound and 219 pm (ax) and 214 pm (eq) in the zirconium complex. | | |
Reference
| Z. Naturforsch. 43b, 1611—1615 (1988); eingegangen am 22. Juni 1988 | | |
Published
| 1988 | | |
Keywords
| N, N'-Bis(trimethylsilyl)benzamidinato Complexes, Titanium, Zirconium, Syntheses, IR Spectra | | |
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| default:Reihe_B/43/ZNB-1988-43b-1611.pdf | | | Identifier
| ZNB-1988-43b-1611 | | | Volume
| 43 | |
20 | Author
| Fausto Calderazzo, Guido Pam, M. Artin Sperrlea, Ulli Englertb | Requires cookie* | | Title
| Electron-and Ligand-Transfer Reactions Involving N,N-Dialkylcarbamates. Synthesis and Molecular Structure of V jIf^ -C C sH ^ yC ^ C N t^ H ^ h  | | | Abstract
| Electron-and ligand-transfer reactions o f low-valent organom etallic com pounds o f titanium and vanadium with N,N-dialkylcarbam ates o f titanium(IV) are reported. The reaction o f VCp2 (Cp = ^-cyclopentadienyl) with T i(0 2C N E t2)4 affords, inter alia, the dimeric vana-dium(III) N ,N-diethylcarbam ato derivative V2Cp2(0 2C N E t2)4 which has been studied by X-ray diffraction methods. Crystal data; triclinic, space group P i; a = 10.802(2), b = 11.004(1), c = 8.960(1) Ä; a = 112.879(9), ß = 102.66(1), y = 102.42(1)°; V = 902.3(6) A 3; Z = 1; F(000) = 368, gcalc = 1.282 g em -3; n = 5.47 cm -1. It consists o f a centrosymmetric dimer, the two vanadium atom s being surrounded by four oxygen atom s o f the bridging N,N-diethylcar-bamato groups and by the cyclopentadienyl ligand. The metal atom exhibits a distorted square-pyramidal coordination geometry with the oxygen atom s occupying the basal plane. The reaction o f TiCp2(CO)2 or Vmes2 (mes = //6-l,3 ,5 -M e3C6H 3) with T i(0 2C N E t2)4 affords Ti(III) and V(III) N,N-diethylcarbam ato derivatives by a simultaneous ligand-and electron-transfer reaction. M agnesium N ,N-diisopropylcarbam ate, M g (0 2CNPr'2)2, has been obtained by a ligand-transfer reaction between M gCp2 and T i(0 2CNPr'2)3. | | |
Reference
| Z. Naturforsch. 47b, 389 (1992); received A ugust 9 / October 16 1991 | | |
Published
| 1992 | | |
Keywords
| N, N-D ialkylcarbam ates, Vanadium, Titanium, Cyclopentadienyl, Electron Transfer | | |
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| default:Reihe_B/47/ZNB-1992-47b-0389.pdf | | | Identifier
| ZNB-1992-47b-0389 | | | Volume
| 47 | |
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