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The enantiomeric pure TADDOLate complexes of the heavier group 4 metals [(η5‐C5H5)2M{(S,S)‐TADDOLate}] (M = Zr, Hf) were prepared by treatment of (S,S)‐TADDOL with 2.5 equivalents of n‐butyl lithium followed by reaction with zirconocene and hafnocene dichloride, respectively. The new complexes have been characterized by standard analytical/spectroscopic techniques and the solid‐state structures of both compounds were established by single crystal X‐ray diffraction. The title compounds are the first fully characterized TADDOLate complexes of zirconium and hafnium. 相似文献
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《无机化学与普通化学杂志》2018,644(18):1091-1095
Five new heteroleptic zirconium and hafnium complexes were synthesized. The complexes carry chloro ligands as well as differently substituted phenoxy benzoxazole ligands [ HL1 = 2‐(2′‐hydroxyphenyl)benzoxazole, HL2 = 2‐(2′‐hydroxynaphthyl)benzoxa‐zole, HL3 = 2‐(2′‐hydroxy‐3′,5′‐di‐tert‐butylphenyl)benzoxazole]. They were characterized by 1H and 13C{1H} NMR spectroscopy as well as by elemental analyses and X‐ray diffraction experiments. The molecular structures in the crystals show distorted octahedral or capped trigonal prismatic coordination spheres. The intermolecular interactions influencing the packing patterns are mainly H ··· Cl contacts. For the hafnium complex [Cl2Hf( L3 )2] a dynamic behavior in solution was examined using temperature dependent 1H NMR spectroscopy. The photo‐physical data show that in all cases fluorescence arises from a short‐lived excited state, the emission maxima being located in the blue spectral region. 相似文献
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Gerhard Erker 《Angewandte Chemie (International ed. in English)》1989,28(4):397-412
The structure and creativity spectrum of transition-metal carbene complexes has been widened significantly by the bent metallocenes of titanium, zirconium, and hafnium. Proceeding from metal carbonyls and reactive (butadiene)-, (aryne)-, or (olefin) MCp2 complexes, many new Fischer-type metaloxycarbene complexes of Zr, Hf, V, Nb, Cr, Mo, W, Mn, Re, Fe, Ru, Os, Co, Ni, and Rh have been synthesized. The incorporation of titanocene, zirconocene, or hafnocene fragments allows new types of carbene complexes to be prepared. For the (alkylidenamido)metallocene complexes , metallocene ylides , and binuclear (μ-alkynyl)metallocene compounds, some metalligand π bonding is indicated. Metallocene complexes with metallaoxirane units, , show similar chemical behavior to that of binuclear (μ-methylene)complexes . The methylene groups of zirconaoxirane complexes, which are derived from carbon monoxide, may be expelled as ethylene by thermally induced CC coupling. With metal hydrides, CH2 transfer with insertion into the metal–hydride bond occurs. In one case, methylene insertion into a metal–carbon bond can even be observed. These reactions of Ti-group metallaoxiranes could be models for postulated intermediates in the Fischer–Tropsch synthesis. 相似文献
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Werner Fischer B. Deierling H. Heitsch G. Otto H.-P. Pohlmann K. Reinhardt 《Angewandte Chemie (International ed. in English)》1966,5(1):15-23
The partition equilibria of zirconium and hafnium thiocyanates between water and methyl isobutyl ketone have been studied under various conditions. Since the system shows extremely marked deviations from Nernst's distribution law, the two elements cannot be prepared in a very pure state by a simple multi-stage partition. By the use of suitable additives and a new scheme of material flow, however, a continuous process using 23 mixer settlers has been developed, by means of which ZrO2 containing less than 10 p.p.m. of HfO2 and HfO2 containing only 0.3% of ZrO2 can be obtained from a zirconium-hafnium mixture (hafnium content: 1 to 2%). 相似文献
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Dorothea Wolff von Gudenberg Hak-Chul Kang Werner Massa Kurt Dehnicke Ccilia Maichle-Mssmer Joachim Strhle 《无机化学与普通化学杂志》1994,620(10):1719-1724
Silanolato Complexes of Titanium and Zirconium. The Crystal Structures of Cp2TiCl(OSiPh3) and Cp2ZrCl(OSiPh3) The title compounds have been prepared by the reaction of Cp2MCl2 (M = Ti, Zr) with triphenylsilanole in diethylether in the presence of piperidine. They form only sparingly moisture sensitive orange (Ti) or colourless (Zr) crystal needles, which were characterized by X-ray crystallography. Cp2TiCl(OSiPh3): Space group P21/n, Z = 4, structure solution with 3961 observed unique reflections, R = 0.057. Lattice dimensions at 20°C: a = 1029.6, b = 1719.3, c = 1388.9 pm, β = 100.69°. The compound forms monomeric molecules with bond lengths TiO of 184.2 pm, SiO of 161.5 pm, and a TiOSi bonding angle of 164.5°. Cp2ZrCl(OSiPh3): Space group P3 , Z = 18, structure solution with 2799 observed unique reflections, R = 0.047. Lattice dimensions at ?20°C: a = b = 3518, c = 1058.3 pm. The structure consists of three symmetry-independent monomeric molecules, which differ only slightly. The bond lengths are (in average): ZrO 196.4 pm, SiO 162.1 pm, the ZrOSi bond angle is 173.7°. 相似文献
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Synthesis and Structure of Ag7M6F31 (M = Zr, Hf, Ce) Colorless single crystals of Ag7Zr6F31 have been obtainend by heating up a mixture of AgF and ZrF4 in a closed goldtube (T = 450 °C, t ∼ 2 d). The compound crystallizes trigonal, space group R3‐C (No. 148) with a = 1400,9(3) pm, c = 979,0(2) pm, Z = 3. Also prepared were the isotypic compounds Ag7Hf6F31 with a = 1393,8(2) pm, c = 978,7(2) pm, and Ag7Ce6F31 with a = 1469,8(1) pm, c = 998,5(1) pm. 相似文献
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H. Schwarz 《Fresenius' Journal of Analytical Chemistry》1966,215(6):445-446
Ohne Zusammenfassung 相似文献
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Synthesis and Structure of RbHfF5, Rb2Zr3F12O and Rb2Hf3F12O — two Oxydefluorides with Central Trigonal‐plane [M3O] Group Colorless RbHfF5 crystallizes isotypic with (NH4)ZrF5 and TlHfF5 monoclinic, space group P21/c ‐ C2h (No. 14) with a = 776.6, b = 789.6, c = 789.8 pm, and β = 120.52°. Also colorless Rb2Zr3F12O crystallizes trigonal, space group R3¯m — D3d (No. 166), with a = 771.9 and c = 2963.0 pm, isotypic is Rb2Hf3F12O with a = 769.2 pm and c = 2986.1 pm. Both compounds are isotypic with Tl2Zr3F12O. 相似文献
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Christine Schließburg Karl‐Heinz Thiele Birgit Lindner Wolfgang Brüser 《无机化学与普通化学杂志》2000,626(3):741-746
Synthesis and Properties of Metallocene and Half Sandwich Complexes with Pyridine‐containing Bridges or Side Chains 2,6‐Bis(chlormethyl)pyridine ( 1 ) reacts with 4 equivalents of indenyllithium with formation of 2,6bis(methylenindenyl)pyridine‐dilitihium ( 2 ) from which with MCl4 · 2 thf (M = Zr, Hf) the corresponding metallocene dichlorides 3 and 4 can be obtained. At reaction of 1 with 2 equivalents of C5H5Na only one Cl atom is replaced by a C5H5Na unit. Following reactions with indenyl lithium and ZrCl4 · 2 thf give the unsymmetric complex [C5H3N–2,6‐CH2‐(2‐C5H4)–(6‐C9H6)ZrCl2] ( 7 ). – Picolylcyclopentadiene ( 8 ) and 1‐(picolyl)‐indene ( 9 ) are synthesized from 2‐chlomethyl‐pyridinium chloride and C5H5Na or indenyl lithium respectively, which are transferred in the half sandwich complexes (C5H4N–CH2C5H4)MCl3 (M = Ti 10 , Zr 11 ) and (C5H4–CH2C9H6)ZrCl3 ( 12) . The compounds were characterized by elemental analysis, 1H n.m.r., ms, ir, and raman spectra. N → M interactions are discussed. 相似文献
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