共查询到20条相似文献,搜索用时 15 毫秒
1.
Haijun Hao Herbert W. Roesky Chunming Cui Hans‐Georg Schmidt Mathias Noltemeyer Peihua Yu Guangcai Bai 《无机化学与普通化学杂志》2000,626(2):368-373
Treating [Cp*V(μ‐Cl)2]3 (Cp* = C5Me5) and [(2,6‐i‐Pr2C6H3N)2MoMe2], respectively, with Me3SnF afforded the title compounds [Cp*V(μ‐F)2]4 ( 1 ) and [(2,6‐i‐Pr2C6H3N)2MoF2] · THF ( 2 ). 1 has a tetrameric structure, in which four V atoms can be regarded as being arranged at the vertices of a distorted tetrahedron, with four long edges bridged by one F atom and each of the other two short edges bridged by two F atoms with a mean V–F bond length of 2.00 Å. A hydrolyzed product of 2 , [(2,6‐i‐Pr2C6H3N)6Mo4(μ3‐F)2Me2(μ‐O)4] ( 3 ) was characterized by elemental analyses and X‐ray single crystal study. The X‐ray diffraction analysis reveals that 3 has a unique tetranuclear structure, containing two five and two six coordinated Mo atoms connecting each other by four μ‐O and two μ3‐F atoms. The geometries around the two Mo atoms can be described having distorted trigonal bipyramidal and distorted octahedral coordination spheres, respectively. The Mo–(μ‐O) bond lengths are 1.813 Å (average) for five coordinated Mo atoms and 2.030 Å (average) for those of six coordinated, respectively, indicating an additional π bonding between five coordinated Mo atoms and the μ‐O atoms. The Mo–(μ3‐F) distances range from 2.291 to 2.352 Å. 相似文献
2.
Crystal Structure of the Molybdenum(V) Complex [MoCl3(NtBu)(H2NtBu)]2 · 1/2 C7H8 Green moisture sensitive single crystals of [MoCl3(NtBu)(H2NtBu)]2 ( 1 · 1/2 C7H8) have been prepared from molybdenum pentachloride with Me2Si(HNtBu)2 in toluene solution; they were suitable for a crystal structure determination. 1 · 1/2 C7H8: Space group P 1, Z = 2, lattice dimensions at –83 °C: a = 696.9(1), b = 1470.9(2), c = 1579.0(2) pm, α = 96.673(13)°, β = 92.014(14)°, γ = 94.852(14)°, R = 0.0321. 1 forms centrosymmetric molecules in which the molybdenum atoms are linked by two μ‐Cl‐bridges with MoCl bond lengths of 245.7 and 270.2 pm in average of the two crystallographically independent individuals. The longer MoCl bond is in trans‐position to the nitrogen atom of the imido ligand (MoN distance 169.0 pm, MoNC bond angle 167.0° in average). 相似文献
3.
1, 3‐Diaminobenzene reacts readily with PPh2Cl to give N, N, N′, N′‐tetrakis(diphenylphosphanyl)‐1, 3‐diaminobenzene ( 1 ) in excellent yield. The dinuclear complex [1, 3‐{cis‐Mo(CO)4(PPh2)2N}2C6H4] ( 2 ) is obtained in high yield from 1 and cis‐[Mo(CO)4(NCEt)2]. Compounds 1 and 2 were characterized by NMR spectroscopy (1H, 13C, 31P) and by crystal structure determination. The latter shows the formation of a bis‐chelate complex with Mo‐P‐N‐P four‐membered rings. 相似文献
4.
Matthias Stender Hannes Oesen Steffen Blaurock Evamarie Hey‐Hawkins 《无机化学与普通化学杂志》2001,627(5):980-984
Synthesis and Molecular Structure of [{Cp′(μ‐η1 : η5‐C5H3Me)Mo(μ‐AlRH)}2] (Cp′ = C5H4Me, R = iBu, Et) [Cp′2MoH2] reacts with HAlR2 to give [{Cp′(μ‐η1 : η5‐C5H3Me)Mo(μ‐AlRH)}2] (Cp′ = C5H4Me, R = iBu ( 1 ), Et ( 2 )). Crystal structure determinations were carried out on [Cp′2MoH2] and 1 . 1 exhibits a direct Mo–Al bond (2.636(2) Å). 相似文献
5.
Molecular and Crystal Structure of Bis[chloro(μ‐phenylimido)(η5‐pentamethylcyclopentadienyl)tantalum(IV)](Ta–Ta), [{TaCl(μ‐NPh)Cp*}2] Despite the steric hindrance of the central atom in [TaCl2(NPh)Cp*] (Ph = C6H5, Cp* = η5‐C5(CH3)5), caused by the Cp* ligand, the imido‐ligand takes a change in bond structure when this educt is reduced to the binuclear complex [{TaCl(μ‐NPh)Cp*}2] in which tantalum is stabilized in the unusual oxidation state +4. 相似文献
6.
The complexes [Ag(η2‐N∧S)2](PF6), N∧S = 1‐methyl‐2‐(methylthiomethyl)‐1H‐benzimidazole, mmb (complex 1 ) or 1‐methyl‐2‐(tert‐butylthiomethyl)‐1H‐benzimidazole, mtb (complex 2 ), and [Ag(μ,η2‐mmb)(μ,η2‐O2PF2)] (complex 3 ) were synthesized and characterized by X‐ray crystallography. Long Ag–S (ca. 2.70 Å) and shorter Ag–N bonds (ca. 2.23 Å) are part of characteristically distorted tetrahedral coordination arrangements at the silver(I) ions in 1 and 2 . Unexpectedly, the comparison with the copper analogue [Cu(η2‐mmb)2](PF6) reveals a more tetrahedral and less linear coordination arrangement for the corresponding silver species. Compound 3 as obtained by hydrolysis of the PF6 ion or by the use of AgPO2F2 exhibits bridging mmb and η2‐difluorophosphate ligands in a chain‐type structure. 相似文献
7.
Tungsten and molybdenum complexes [M(CO)2(dpphen)(dbf)2] (M = W 1 or Mo 2 ; dpphen = 4,7‐diphenyl‐1,10‐phenanthroline; dbf = dibutylfumarate) have been synthesized and structurally characterized by X‐ray diffraction analysis. In both complexes which have similar structure, the metal atom co‐ordination is distorted octahedral with dpphen and two CO groups in the equatorial plane and the metal atom binds in an η2‐fashion to the C–C bonds of two dbf ligands. The two C–C bonds are almost mutually orthogonal. The two complexes are different in conformation which result from face selection of the two dbf ligands for coordination to the metal atom. 相似文献
8.
Two manganese(II) bipyridine carboxylate complexes, [(bipy)2MnII(μ‐C2H5CO2)2MnII(bipy)2}2](ClO4)2 ( 1 ), and [MnII(ClCH2CO2)(H2O)(bipy)2]ClO4 · H2O ( 2 ) were prepared. 1 crystallizes in the triclinic space group P 1 with a = 8.604(3), b = 12.062(3), c = 13.471(3) Å, α = 112.47(2), β = 93.86(2), γ = 92.87(3)°, V = 1211.1(6) Å3 and Z = 1. In the dimeric, cationic complex with a crystallographic center of symmetry two 2,2′‐bipyridine molecules chelate each manganese atom. These two metal fragments are then bridged by two propionato groups in a syn‐anti conformation. The Mn…Mn distance is 4.653 Å. 2 crystallizes in the monoclinic space group P21/c with a = 9.042(1), b = 13.891(1), c = 21.022(3) Å, β = 102.00(1)°, V = 2569.3(5) Å3 and Z = 4. 2 is a monomeric cationic complex in which two bipyridine ligands chelate the manganese atom in a cis fashion. A chloroacetato and an aqua ligand complete the six‐coordination. Only in 2 is the intermolecular packing controlled by weak π‐stacking besides C–H…π contacts between the bipyridine ligands. 相似文献
9.
Unexpected Reduction of [Cp*TaCl4(PH2R)] (R = But, Cy, Ad, Ph, 2,4,6‐Me3C6H2; Cp* = C5Me5) by Reaction with DBU – Molecular Structure of [(DBU)H][Cp*TaCl4] (DBU = 1,8‐diazabicyclo[5.4.0]undec‐7‐ene) [Cp*TaCl4(PH2R)] (R = But, Cy, Ad, Ph, 2,4,6‐Me3C6H2 (Mes); Cp* = C5Me5) react with DBU in an internal redox reaction with formation of [(DBU)H][Cp*TaCl4] ( 1 ) (DBU = 1,8‐diazabicyclo[5.4.0]undec‐7‐ene) and the corresponding diphosphane (P2H2R2) or decomposition products thereof. 1 was characterised spectroscopically and by crystal structure determination. In the solid state, hydrogen bonding between the (DBU)H cation and one chloro ligand of the anion is observed. 相似文献
10.
Barbara Becker Anna Doga Antoni Konitz Lech Swinder Wiesaw Wojnowski 《无机化学与普通化学杂志》2001,627(2):280-286
[Zn{SSi(OBut)3}2(NH3)]2 ( 1 ) reacts with 2‐picoline or 2,4‐lutidine (L) without elimination of ammonia giving stable monometallic complexes [Zn{SSi(OBut)3}2(NH3)L] ( 3 and 4 ), with two different nitrogen ligands bonded to the metal center. Reaction of (ButO)3SiSH with zinc di(acetylacetonate) in ammonia atmosphere leads to the complex with two ammine ligands [Zn{SSi(OBut)3}2(NH3)2] · MeCN ( 5 ). Molecular and crystal structures of 3 , 4 and 5 have been determined by the single crystal X‐ray structural analysis. All have distorted tetrahedral geometry. The presence of ammonia gives rise to hydrogen bonds, different in all three cases. 3 , 4 , and 5 are the first examples of structurally characterized ammine ligated zinc thiolates. 相似文献
11.
New Azido Complexes of Tantalum(V). Synthesis and Molecular Structure of the Dinuclear Compounds [Cp*TaCl(N3)(μ‐N3)]2(μ‐O) and [Cp*Ta(N3)3(μ‐N3)]2 (Cp* = Pentamethylcyclopentadienyl) The reaction of Cp*TaCl4 ( 1 ) with an excess of trimethylsilyl azide (Me3Si–N3) leads to azide‐rich dinuclear complexes which contain both terminal and bridging azido ligands. The oxo complex [Cp*TaCl(N3)(μ‐N3)]2(μ‐O) ( 4 ) was formed in dichloromethane in the presence of traces of water, whereas [Cp*Ta(N3)3(μ‐N3)]2 ( 5 ) was obtained from boiling toluene after several days. According to the X‐ray structure determinations the Ta…Ta distance in 4 (314,5 pm) is considerably shorter than in 5 (382,2 pm). 相似文献
12.
[Mo2(O2C–CH3)4 · 1/2 {(CH2)6N4} · 1/2 CH2Cl2] – a Donor‐Acceptor Complex with Supramolecular Structure Yellow single crystals of [Mo2(O2C–CH3)4 · 1/2 {(CH2)6N4} · 1/2 CH2Cl2] ( 1 ) have been obtained by the reaction of the silylated phosphaneimine Me3SiNPEt3 with [Mo2(O2C–CH3)4] in dichloromethane solution. 1 forms a three‐dimensional network with linear N–Mo:Mo–N and tetrahedral (CH2)6N4Mo4 moieties, which is topologically related with the PtS type. Space group P42/nnm, Z = 4, lattice dimensions at –70 °C: a = b = 1121.7(1), c = 1395.0(3) pm, R1 = 0.0413. 相似文献
13.
The reaction of CpMo(CO)3X (X = Cl, I) with SbF5 in toluene leads to the cationic, halogen bridged compounds [{CpMo(CO)3}2X]SbF6 ( 1 , 2 ). CpW(CO)3Cl reacts with SbF5 to yield [{CpW(CO)3}2Cl]SbF6 ( 3 ), whereas with SbCl5, the oxidative substitution product [{CpW(CO)2Cl2}2Cl]SbCl6 ( 4 ) is formed, which decomposes in solution to yield the trichloride CpW(CO)2Cl3 ( 5 ). The strong Lewis acid SbF5 separates the halide from CpM(CO)3X (M = Mo, W), and the resulting cationic fragment “CpM(CO)3+” reacts with a further CpM(CO)3X forming a halonium bridge ( 1 – 3 ). The exclusive formation of SbF6– can be explained by the oxidizing power of SbF5. The IR, MS and NMR spectra of the compounds 1 – 5 as well as the X‐ray structure analysis of 5 are reported and discussed. 相似文献
14.
The reaction of ammonium heptamolybdate with hydrazine sulfate in an aqueous solution of glycine at room temperature yielded colorless crystals of (NH4)4[(NH3CH2CO)2(Mo8O28)] · 2 H2O. The crystal is monoclinic, space group C2/c (no. 15), a = 17.234 Å, b = 10.6892 Å, c = 18.598 Å, β = 108.280°, V = 3253.2 Å3, Z = 4. The crystal structure contains ammonium cations and isolated octamolybdate(4–) anions, [(NH3CH2CO)2(Mo8O28)]4–, with two zwitterionic glycine molecules as ligands. 相似文献
15.
Mononuclear [MoO2LD], and dinuclear [MoO2L]2 or [MoO2L]2 · D dixomolybdenum(VI) complexes have been prepared by the reaction of tridentate Schiff‐base ligands L with [MoO2(acac)2]. The Schiff‐base ligands have been synthesized from salicylaldehyde ( 1 , 1a , 1c , 1d ), 2‐hydroxy‐1‐naphthaldehyde ( 2 , 2c ) and 2‐hydroxy‐3‐methoxybenzaldehyde ( 3a , 3b , 3c , 3d , 3e ) with 2‐amino‐p‐cresol. All prepared complexes consist of cis‐MoO22+core coordinated by Schiff‐base ligand through two deprotonated hydroxyl groups and one imino nitrogen atom. The usual octahedral coordination around the molybdenum atoms is completed by the neutral ligand D (methanol, ethanol, dimethyl sulfoxide, imidazole or 4, 4′‐bipyridine). All compounds were characterized by elemental analyses, IR spectroscopy and some of them by X‐ray crystallography ( 1a , 2c , 3a , 3b , 3c and 3e ). 相似文献
16.
(NH4)2[Mo6Cl14] · H2O ( 1 ) was prepared from reactions of MoCl2 in ethanol with aqueous NH4Cl solution. It crystallizes in the monoclinic space group I2/a (no. 15), Z = 4 with a = 912.3(1), b = 1491.2(2), c = 1724.8(2) pm, β = 92.25(1)°; R1 = 0.023 (based on F values) and wR2 = 0.059 (based on F2 values), for all measured X‐ray reflections. The structure of the cluster anion can be given as [(Mo6Cl)Cl]2– (i = inner, a = outer ligands). Thermal stability studies show that 1 loses crystal water followed by the loss of NH4Cl above 350 °C to yield MoCl2. The water‐free compound (NH4)2[Mo6Cl14] ( 2 ) was synthesized by solid state reaction of MoCl2 and NH4Cl in a sealed quartz ampoule at 270 °C. No single‐crystals could be obtained. Decompositions of 1 and 2 under nitrogen and argon exhibited the loss of NH4Cl at about 350 °C. Decomposition under NH3 resulted in the formation of MoN and Mo2N at 540 °C and 720 °C, respectively. 相似文献
17.
18.
O. J. Scherer J. Meiers M. Regitz M. A. Hofmann K. Karaghiosoff G. Wolmershuser 《无机化学与普通化学杂志》2001,627(7):1532-1536
[CpR(OC)Mo(μ‐η2:2‐P2)2FeCpR′] as Educt for Heterobimetallic Dinuclear Clusters with P2 and CnRnP4‐n Ligands (n = 1, 2) The cothermolysis of [CpR(OC)Mo(μ‐η2:2‐P2)2FeCpR′] ( 1 ) and tBuC≡P ( 2 ) as well as PhC≡CPh ( 3 ) affords the heterobimetallic triple‐decker like dinuclear clusters [(Cp'''Mo)(Cp*′Fe)(P3CtBu)(P2)] ( 4 ), Cp''' = C5H2tBu3‐1,2,4, Cp*′ = C5Me4Et, and [(Cp*Mo)(Cp*Fe)(P2C2Ph2)(P2)] ( 5 ) with a bridging tri‐ and diphosphabutadiendiyl ligand. 4 and 5 have been characterized additionally by X‐ray crystallography. 相似文献
19.
Synthesis, Structure, and Properties of Some Selenidostannates. II. [(C2H5)3NH]2Sn3Se7 · 0,25 H2O and [(C3H7)2NH2]4Sn4Se10 · 4 H2O The new selenidostannate hydrates [(C2H5)3NH]2Sn3Se7 · 0.25 H2O ( I ) and [(C3H7)2NH2]4Sn4Se10 · 4 H2O ( II ) were synthesized from an aqueous suspension of triethylammonium (tripropylammonium), tin, selenium I and in addition sulfur II at 130 °C. I crystallizes at ambient temperature in the monoclinic space group P21/n (a = 2069,3(4) pm, b = 1396,6(3) pm, c = 2342,8(5) pm, β = 114,68(3)°, Z = 8) and is characterized by two different anions, chains from edge‐sharing [Se3Se7]2– units and nets from trigonal SnSe5 bipyramids. II crystallizes at ambient temperature in the tetragonal space group I41/amd (a = 2150,0(3) pm, c = 1174,4(2) pm, Z = 4) and contains adamantane like [Sn4Se10]4–‐cages. The UV‐VIS spectra of the selenidostannates demonstrate that the absorption edges red shift as the dimensionality of the compounds is increased. 相似文献
20.
The reactions of 4‐amino‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)‐thione (AMTT, L1 ) with 2‐thiophen carbaldehyde, salicylaldehyde and 2‐nitrobenzaldehyde in methanol led to the corresponding Schiff‐bases ( L1a‐c ). The reaction of L1 with [(PPh3)2Cu]NO3 in ethanol gave the ionic complex [(PPh3)2Cu(L1)]NO3·EtOH ( 2 ) All compounds were characterized by infrared spectroscopy, elemental analyses as well as by X‐ray diffraction studies. Crystal data for L1a at 20 °C: space group P21/n with a = 439.6(2), b = 2074.0(9), c = 1112.8(4) pm, β = 93.51(3)°, Z = 4, R1 = 0.0406, L1b at ?80 °C: space group P21/n with a = 1268.9(2), b = 739.3(1), c = 1272.5(1) pm, β = 117.97(1)°, Z = 4, R1 = 0.0361, L1c at ?80 °C: space group P21/n with a = 847.8(1), b = 1502.9(2), c = 981.5(2) pm, β = 110.34(1)°, Z = 4, R1 = 0.0376 and for 2 at ?80 °C: space group with a = 1247.8(1), b = 1270.3(1), c = 1387.5(1) pm, α = 84.32(1)°, β = 84.71(1)°, γ = 63.12(1)°, Z = 2, R1 = 0.0539. 相似文献