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1.
Brian J. Grimmond Joyce Y. Corey Nigam P. Rath 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(1):53-55
The first title metallocene, 1,3‐bis(dichlorotitanocene)‐1,1,3,3‐tetramethyldisiloxane dichloromethane solvate, [(η5‐C5H5)TiCl2(η5‐C5H4SiMe2)]2O·CH2Cl2, (I), crystallizes in space group P21/c. Compound (I) represents the first crystal structure of a bimetallic siloxy‐bridged titanocene. The geometric parameters of (I) are similar to those of the parent titanocene; however, the disiloxane substituents adopt an unexpected eclipsed conformation. The second title metallocene, 1,3‐bis[(pentamethylcyclopentadienyl)(cyclopentadienyl)titanium dichloride]‐1,1,3,3‐tetramethyldisiloxane, [(η5‐C5‐Me5)TiCl2(η5‐C5H4SiMe2)]2O, (II), represents the second crystal structure of a bimetallic siloxy‐bridged titanocene and crystallizes in the space group P21/n. Compound (I) possesses non‐crystallographic twofold molecular symmetry and both metal centers adopt pseudo‐tetrahedral geometries. The geometric parameters of (II) are similar to those of the mixed titanocene Cp*CpTiCl2 (Cp* = C5Me5) and the disiloxane substituents adopt a staggered conformation. 相似文献
2.
Ansa‐Complexes of [Mn(η5‐C5H5)(η6‐C6H6)]: Preparation,Characterization, and Reactivity of [n]Manganoarenophanes (n=1, 2, 3) 下载免费PDF全文
Prof. Dr. Holger Braunschweig Dr. Alexander Damme Dr. Klaus Dück Dr. Marco Fuß Dr. Christian Hörl Dr. Thomas Kramer Dr. Ivo Krummenacher Dr. Thomas Kupfer Valerie Paprocki Christoph Schneider 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(42):14797-14803
We report the synthesis of [n]manganoarenophanes (n=1, 2) featuring boron, silicon, germanium, and tin as ansa‐bridging elements. Their preparation was achieved by salt‐elimination reactions of the dilithiated precursor [Mn(η5‐C5H4Li)(η6‐C6H5Li)]?pmdta (pmdta=N,N,N′,N′,N′′‐pentamethyldiethylenetriamine) with corresponding element dichlorides. Besides characterization by multinuclear NMR spectroscopy and elemental analysis, the identity of two single‐atom‐bridged derivatives, [Mn(η5‐C5H4)(η6‐C6H5)SntBu2] and [Mn(η5‐C5H4)(η6‐C6H5)SiPh2], could also be determined by X‐ray structural analysis. We investigated for the first time the reactivity of these ansa‐cyclopentadienyl–benzene manganese compounds. The reaction of the distannyl‐bridged complex [Mn(η5‐C5H4)(η6‐C6H5)Sn2tBu4] with elemental sulfur was shown to proceed through the expected oxidative addition of the Sn?Sn bond to give a triatomic ansa‐bridge. The investigation of the ring‐opening polymerization (ROP) capability of [Mn(η5‐C5H4)(η6‐C6H5)SntBu2] with [Pt(PEt3)3] showed that an unexpected, unselective insertion into the Cipso?Sn bonds of [Mn(η5‐C5H4)(η6‐C6H5)SntBu2] had occurred. 相似文献
3.
Xia Li Ying‐Quan Zou Hai‐Bin Song 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(3):m110-m111
Each La3+ ion in the title complex, tetra‐μ‐2‐fluorobenzoato‐κ10O:O′;O:O,O′;O:O′;O,O′:O′‐bis[aqua(4,4′‐bipyridine‐κN)(2‐fluorobenzoato‐κO)lanthanum(II)], [La(C7H4FO2)6(C10H8N2)2(H2O)2], is coordinated by six O atoms from the carboxylate groups of five 2‐fluorobenzoate ligands, one O atom from a water molecule and one N atom from a 4,4′‐bipyridine molecule, thus forming a dimeric molecule. An infinite one‐dimensional dimeric supramolecular chain is formed via intermolecular hydrogen bonds. 相似文献
4.
Reijo Sillanp Jordi Llop Clara Vias Francecs Teixidor Raikko Kiveks 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(8):900-901
In the title compound, (η5‐2,5‐dimethylpyrrolyl)[(7,8,9,10,11‐η)‐7‐methyl‐7,8‐dicarba‐nido‐undecaborato]cobalt(III), [3‐Co{η5‐[2,5‐(CH3)2‐NC4H2]}‐1‐CH3‐1,2‐C2B9H10] or [Co(C3H13B9)(C6H8N)], the CoIII atom is sandwiched between the pentagonal faces of the pyrrolyl and dicarbollide ligands, resulting in a neutral molecule. The C—C distance in the dicarbollide cage is 1.649 (3) Å. 相似文献
5.
Zoran D. Tomi
eljko K. Jaimovi Vukadin M. Leovac Valeria I. eljevi 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(7):777-779
The title compound, bis(μ‐4‐acetyl‐3‐amino‐5‐methylpyrazolato‐N1:N2)bis[(acetato‐O)(4‐acetyl‐3‐amino‐5‐methylpyrazole‐N2)zinc(II)], [Zn2(C6H8N3O)2(C2H3O2)2(C6H9N3O)2], ex‐ists as a centrosymmetric binuclear molecule with two tetrahedrally coordinated Zn atoms bridged by two pyrazolate anions. The geometry of the terminal and bridging pyrazole ligands are slightly different as a consequence of their differing modes of coordination. 相似文献
6.
Frank J. Feher Richard K. Baldwin Joseph W. Ziller 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(6):633-634
The crystal structure of the title complex, (η6‐hexamethylbenzene)bis(trifluoromethanesulfonato‐O)(2,4,6‐trimethylaniline‐N)ruthenium(II), [Ru(CF3O3S)2(C12H18)(C9H13N)], is described. The complex has the classic three‐legged piano‐stool structure with a planar arene 1.667 Å from the metal, two monodentate O‐bound trifluoromethanesulfonate ligands [Ru—O 2.169 (2) and 2.174 (2) Å] and one N‐bound mesidine ligand [Ru—N 2.198 (2) Å]. The Ru—N distance is relatively long and the average Ru—O distance is relatively short when compared with previously characterized RuII complexes. 相似文献
7.
1,2-Diphenyl-1,2-dimethyldisilanylene-bridged bis-cyclopentadienyl complex[η~5,η~5-C_5H_4PhMeSiSiMePh-C_5H_4]Fe_2(CO)_2(μ-CO)_2(1)was synthesized by a modified procedure,from which the trans-isomer 1b that was pre-viously difficult to obtain has been isolated for the first time.More interestingly,two new regio-isomers[η~5,η~5C_5H_4SiMe(SiMePh_2)C_5H_4]Fe_2(CO)_2(μ-CO)_2(2)and [η~5,η~5-C_5H_4Me_2SiSiPh_2C_5H_4]Fe_2(CO)_2(μ-CO)_2(3)were occa-sionally obtained during above process,the novel structures of which opened up new options for further study ofthis type of Si—Si bond-containing transition metal complexes.The molecular structure of 2 has been determinedby the X-ray diffraction method. 相似文献
8.
Ana María Atria María Teresa Garland Ricardo Baggio Piedad Corts 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(7):m297-m302
Two new oxo complexes, namely hexa‐μ2‐acetato‐acetatoaquabis(di‐3‐pyridylamine)di‐μ3‐oxo‐tetrairon(III) chloride monohydrate ethanol 1.25‐solvate, [Fe4(C2H3O2)7O2(C10H9N3)2(H2O)]Cl·1.25C2H6O·H2O, (I), containing a tetranuclear [Fe4(μ3‐O)2]8+ unit, and 2‐methylimidazolium hexa‐μ2‐acetato‐acetatodiaqua‐μ3‐oxo‐triiron(III) chloride dihydrate, (C4H7N2)[Fe3(C2H3O2)7O(H2O)2]Cl·2H2O, (II), with a trinuclear [Fe3(μ3‐O)]7+ unit, are presented. Both structures are formed by two well differentiated entities, viz. a compact isolated cluster composed of FeIII ions coordinated to O2− and CH3CO2− anions, and an external group formed by a central Cl− ion surrounded by different solvent groups to which the anion is bound through hydrogen bonding. In the case of (I), charge balance cannot be achieved within the groups, so the structure is macroscopically ionic; in the case of (II), in contrast, each group is locally neutral owing to the internal compensation of charges. The trinuclear complex crystallizes with the metal cluster, chloride anion and 2‐methylimidazolium cation bisected by a crystallographic mirror plane. 相似文献
9.
Hong‐Yu Chen Qi Fang Gang Xue Wen‐Tao Yu 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(12):m535-m537
In the title compound, {[K2Ni(C5O5)2(H2O)2]·4H2O}n, the Ni atom lies on an inversion centre. Two inversion‐related croconate [4,5‐dihydroxy‐4‐cyclopentene‐1,2,3‐trionate(2−)] ligands and an NiII ion form a near‐planar symmetrical [Ni(C5O5)2]2− moiety. The near‐square coordination centre of the moiety is then extended to an octahedral core by vertically bonding two water molecules in the [Ni(C5O5)2(H2O)2]2− coordination anion. The crystal structure is characterized by a three‐dimensional network, involving strong K⋯O⋯K binding, K⋯O—Ni binding and hydrogen bonding. 相似文献
10.
Cengiz Arici Filiz Ercan Raif Kurtaran Orhan Atakol 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(7):812-814
In the title compounds, {2,2′‐[2,2‐dimethyl‐1,3‐propanediylbis(nitrilomethylidyne)]diphenolato‐κ4N,N′,O,O′}nickel(II), [Ni(C19H20N2O2)], and {2,2′‐[2,2‐dimethyl‐1,3‐propanediylbis(nitrilomethylidyne)]diphenolato‐κ4N,N′,O,O′}copper(II), [Cu(C19H20N2O2)], the NiII and CuII atoms are coordinated by two iminic N and two phenolic O atoms of the N,N′‐bis(salicylidene)‐2,2‐dimethyl‐1,3‐propanediaminate (SALPD2?, C17H16N2O22?) ligand. The geometry of the coordination sphere is planar in the case of the NiII complex and distorted towards tetrahedral for the CuII complex. Both complexes have a cis configuration imposed by the chelate ligand. The dihedral angles between the N/Ni/O and N/Cu/O coordination planes are 17.20 (6) and 35.13 (7)°, respectively. 相似文献
11.
Jie Chen Ning‐Hai Hu Jie Zhan Yue‐Sheng Li 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(7):m337-m338
A new polynuclear titanium(IV) complex, dichlorodeca‐μ2‐oxo‐hexakis(pentamethylcyclopentadienyl)hexatitanium(IV), [Ti6(C10H15)6Cl2O10], has been synthesized by hydrolysis of a titanium complex bearing an N‐(2‐hydroxy‐3,5‐dimethylbenzyl)diethanolamine Mannich ligand. The molecule has two O‐bridged Ti3O3 rings linked to two similar rings through a tetrahedrally O‐coordinated Ti atom. All Ti atoms except the central one are coordinated to pentamethylcyclopentadienyl (Cp*) ligands. The Cp* ligands are arranged with approximate symmetry with respect to the Ti/O/Cl core. 相似文献
12.
Ramn Macías Simon A. Barrett Jonathan Bould Udo Drfler Josef Holub John D. Kennedy Mark Thornton‐Pett Bohumil tíbr 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(5):520-522
Neutral 8‐(5‐iodo‐n‐pentyl)‐3‐(η5‐pentamethylcyclopentadienyl)‐arachno‐3‐rhoda‐7,8‐dithiaundecaborane, [Rh(C5H19B8IS2)(C10H15)], obtained from the [arachno‐7,8‐S2B9H10]? anion by treatment with I(CH2)5I followed by [Rh(C5Me5)Cl2]2 and N,N,N′,N′‐tetramethyl‐1,8‐diaminonaphthalene, has the 11‐vertex cluster geometry of [arachno‐7,8‐S2B9H10]?, but with an {Rh(C5Me5)} unit in the 3‐position instead of a {BH} unit, and with a –(CH2)5I chain attached exo to an S atom. 相似文献
13.
Lan Yang Changwen Hu Haruo Naruke Toshihiro Yamase 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(7):799-801
The title compound, poly[[[diaqua(μ‐4,4′‐bipyridyl)dinickel(II)]‐bis(μ‐4,4′‐bipyridyl)‐di‐μ‐hexaoxodivanadate(2?)] 2.5‐hydrate], [Ni2(V2O6)2(C10H8N2)3(H2O)2]·2.5H2O, has been prepared hydrothermally and characterized by elemental analyses, IR spectroscopy and single‐crystal X‐ray diffraction. The structure consists of [V2O6], [Ni(4,4′‐bipy)4O2] and [Ni(H2O)2(4,4′‐bipy)2O2] polyhedra, and water of crystallization. The Ni atoms and one bipyridyl group lie on centres of symmetry. 相似文献
14.
Tim Kemmitt Graeme J. Gainsford Hana Robson‐Marsden 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(5):m310-m312
The title compound, bis(2,2′‐methyliminodiethanolato)‐1κ3O,N,O′;3κ3O,N,O′‐di‐μ3‐propane‐1,3‐diolato‐1:2:3κ8O:O,O′:O′‐μ‐propane‐1,3‐diolato‐1:3κ2O:O′‐propane‐1,3‐diolato‐2κ2O,O′‐trititanium(IV), [Ti3(C5H11NO2)2(C3H6O2)4], has four 1,3‐propanediolate ligands binding in three different modes. Two ligands chelate adjacent Ti atoms with normal μ3‐O bridges, giving typical edge‐sharing of the Ti distorted octahedra, one chelating to the central Ti atom with no μ‐bridging, and the other spanning the cluster, binding only to the outermost Ti atoms. The two methyliminodiethanolate ligands each coordinate to the outer Ti atoms via their N and two O atoms. The Ti—O bond lengths range, in a self‐consistent fashion, from 1.816 (2) to 2.082 (2) Å, while the average Ti—N distance is 2.391 (3) Å. 相似文献
15.
John Bacsa Hanhua Zhao Kim R. Dunbar 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(12):m561-m564
Two new iron–oxo clusters, viz. di‐μ‐trifluoroacetato‐μ‐oxo‐bis[(2,2′‐bipyridine‐κ2N,N′)(trifluoroacetato‐κO)iron(III)], [Fe2O(CF3CO2)4(C10H8N2)2], and bis(2,2′‐bipyridine)di‐μ3‐oxo‐hexa‐μ‐trifluoroacetato‐bis(trifluoroacetato)tetrairon(III) trifluoroacetic acid solvate, [Fe4O2(CF3CO2)8(C10H8N2)2]·CF3CO2H, contain dinuclear and tetranuclear FeIII cores, respectively. The FeIII atoms are in distorted octahedral environments in both compounds and are linked by oxide and trifluoroacetate ions. The trifluoroacetate ions are either bridging (bidentate) or coordinated to the FeIII atoms via one O atom only. The fluorinated peripheries enhance the solubility of these compounds. Formal charges for all the Fe centers were assigned by summing valences of the chemical bonds to the FeIII atom. 相似文献
16.
Reactions of one or two equiv. of cyclohexyl isocyanide in THF at room temperature with Mo?Mo triply bonded complexes [Mo(CO)2(η5‐C5H4R)]2 (R=COCH3, CO2CH3) gave the isocyanide coordinated Mo? Mo singly bonded complexes with functionally substituted cyclopentadienyl ligands, [Mo(CO)2(η5‐C5H4R)]2(μ‐η2‐CNC6H11) ( 1a , R=COCH3; 1b , R=CO2CH3) and [Mo(CO)2(η5‐C5H4R)(CNC6H11)]2 ( 2a , R=COCH3; 2b , R=CO2CH3), respectively. Complexes 1a , 1b and 2a , 2b could be more conveniently prepared by thermal decarbonylation of Mo? Mo singly bonded complexes [Mo(CO)3(η5‐C5H4R)]2 (R=COCH3, CO2CH3) in toluene at reflux, followed by treatment of the resulting Mo?Mo triply bonded complexes [Mo(CO)2(η5‐C5H4R)]2 (R=COCH3, CO2CH3) in situ with cyclohexyl isocyanide. While 1a , 1b and 2a , 2b were characterized by elemental analysis and spectroscopy, 1b was further characterized by X‐ray crystallography. 相似文献
17.
Syntheses, Structure and Reactivity of η3‐1,2‐Diphosphaallyl Complexes and [{(η5‐C5H5)(CO)2W–Co(CO)3}{μ‐AsCH(SiMe3)2}(μ‐CO)] Reaction of ClP=C(SiMe2iPr)2 ( 3 ) with Na[Mo(CO)3(η5‐C5H5)] afforded the phosphavinylidene complex [(η5‐C5H5)(CO)2Mo=P=C(SiMe2iPr)2] ( 4 ) which in situ was converted into the η1‐1,2‐diphosphaallyl complex [η5‐(C5H5)(CO)2Mo{η3‐tBuPPC(SiMe2iPr)2] ( 6 ) by treatment with the phosphaalkene tBuP=C(NMe2)2. The chloroarsanyl complexes [(η5‐C5H5)(CO)3M–As(Cl)CH(SiMe3)2] [where M = Mo ( 9 ); M = W ( 10 )] resulted from the reaction of Na[M(CO)3(η5‐C5H5)] (M = Mo, W) with Cl2AsCH(SiMe3)2. The tungsten derivative 10 and Na[Co(CO)4] underwent reaction to give the dinuclear μ‐arsinidene complex [(η5‐C5H5)(CO)2W–Co(CO)3{μ‐AsCH(SiMe3)2}(μ‐CO)] ( 11 ). Treatment of [(η5‐C5H5)(CO)2Mo{η3‐tBuPPC(SiMe3)2}] ( 1 ) with an equimolar amount of ethereal HBF4 gave rise to a 85/15 mixture of the saline complexes [(η5‐C5H5)(CO)2Mo{η2‐tBu(H)P–P(F)CH(SiMe3)2}]BF4 ( 18 ) and [Cp(CO)2Mo{F2PCH(SiMe3)2}(tBuPH2)]BF4 ( 19 ) by HF‐addition to the PC bond of the η3‐diphosphaallyl ligand and subsequent protonation ( 18 ) and/or scission of the PP bond by the acid ( 19 ). Consistently 19 was the sole product when 1 was allowed to react with an excess of ethereal HBF4. The products 6 , 9 , 10 , 11 , 18 and 19 were characterized by means of spectroscopy (IR, 1H‐, 13C{1H}‐, 31P{1H}‐NMR, MS). Moreover, the molecular structures of 6 , 11 and 18 were determined by X‐ray diffraction analysis. 相似文献
18.
The o‐substituted hybrid phenylphosphines, PPh2(o‐C6H4NH2) and PPh2(o‐C6H4OH), could be deprotonated with LDA or n‐BuLi to yield PPh2(o‐C6H4NHLi) and PPh2(o‐C6H4OLi), respectively. When added to a solution of (η5‐C5H5)Fe(CO)2I at room temperature, these two lithiated reagents produce a chelated neutral complex 1 (η5‐C5H5)Fe(CO)[C(O)NH(o‐C6H4)PPh2‐C,P‐η2] for the former and mainly a zwitterionic complex 2 , (η5‐C5H5)Fe+(CO)2[PPh2(o‐C6H4O?)] for the latter. Complex 1 could easily be protonated and then decarbonylated to give 4 [(η5‐C5H5)Fe(CO){NH2(o‐C6H4)PPh2‐N,P‐η2}+]. Complexes 1 and 4‐I have been crystallographically characterized with X‐ray diffraction. 相似文献
19.
Graeme J. Gainsford Tim Kemmitt 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(3):m136-m138
In the title compound, [Na4(C8H16BO4)4(C4H10O2)]n, there are two coordination types for the four independent Na+ cations: two Na+ cations bond to six diolate O atoms [Na—O = 2.305 (2)–2.609 (2) Å], while the other two are five‐coordinate via one 1,4‐butanediol [2.289 (2) and 2.349 (3) Å] and four diolate O atoms [2.295 (2)–2.408 (2) Å]. Corresponding to this, there are three‐ and four‐coordinate diolate O atoms, the latter bridging Na atoms. The 1,4‐butanediol molecules lie on inversion centres. The boron stereochemistry shows minor local perturbations from its usual tetrahedral state [B—O = 1.457 (4)–1.503 (4) Å]. The resulting polymer packs as sheets parallel to the (10) plane crosslinked by the butanediol molecules. The structure was solved using data from a multiple crystal. 相似文献
20.
Frank Seela Helmut Rosemeyer Alexander Melenewski Eva‐Maria Heithoff Henning Eickmeier Hans Reuter 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(3):o142-o144
In the monohydrate of 2‐amino‐8‐(2‐deoxy‐α‐d ‐erythro‐pentofuranosyl)‐8H‐imidazo[1,2‐a][1,3,5]triazin‐4‐one, C10H13N5O4·H2O, denoted (I) or αZd, the conformation of the N‐glycosylic bond is in the high‐anti range [χ = 87.5 (3)°]. The 2′‐deoxyribofuranose moiety adopts a C2′‐endo,C3′‐exo(2′T3′) sugar puckering (S‐type sugar) and the conformation at the C4′—C5′ bond is ?sc (trans). 相似文献