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1.
A Three Dimensional Network of Iodide Ions and Iodine Molecules in the Crystal Structure of [Pr(Benzo-15-Crown-5)2]I21 Black polyhedra of [Pr(benzo-15-crown-5)2]I21 were grown from an ethanol / dichlormethane solution of PrI3, benzo-15-crown-5 and I2. The crystal structure (orthorhombic, P21cn, a = 1201.1(1), b = 2168.3(1), c = 2571.1(1) pm, Z = 4) is built up from sandwich like cations [Pr(benzo-15-crown-5)2]3+ and polyiodide anions I213-. This unique polyiodide anion exhibits a complex connection pattern of iodide ions and iodine molecules with variable bond lengths forming a complicated network.  相似文献   

2.
Single crystals of [Gd(OH)(H2O)(b18c6)]I(I3)(CH3CN) were obtained from an acetonitrile solution of GdI3, I2 and benzo‐18‐crown‐6. The crystal structure (monoclinic, P21/a (no. 14), Z = 4, a = 1233.8(1) pm, b = 1925.0(2) pm, c = 1252.3(1) pm, β = 104.375(7)°) contains hydroxide bridged cationic dimers and iodide as well as triiodide as anions.  相似文献   

3.
The cyanide building block [FeIII(pzphen)(CN)4] and its four lanthanide complexes [{FeIII(pzphen)(CN)4}2LnIII(H2O)5(DMF)3] · (NO3) · 2(H2O) · (CH3CN) [Ln = Nd ( 1 ), Sm ( 2 ), DMF = dimethyl formamide] and [{FeIII(pzphen)(CN)4}2LnIII(NO3)(H2O)2(DMF)2](CH3CN) [Ln = Gd ( 3 ), Dy ( 4 )] were synthesized and structurally characterized by single‐crystal X‐ray diffraction. Compounds 1 and 2 are ionic salts with two [FeIII(pzphen)(CN)4] cations and one LnIII ion, but compounds 3 and 4 are cyano‐bridged FeIIILnIII heterometallic 3d‐4f complexes exhibiting a trinuclear structure in the same conditions. Magnetic studies show that compound 3 is antiferromagnetic between the central FeIII and GdIII atoms. Furthermore, the trinuclear cyano‐bridged FeIII2DyIII compound 4 displays no single‐molecular magnets (SMMs) behavior by the alternating current magnetic susceptibility measurements.  相似文献   

4.
The reaction of [CpRu(CH3CN)3]PF6 with the bidentate ligands L-L=1,2-bis(diphenylphosphino)ethane, dppe, and (1-diphenylarsino-2-diphenylphosphino)ethane, dpadppe, affords mononuclear or dinuclear complexes of formula [CpRu(η2-L-L)(CH3CN)]PF6, [{CpRu(CH3CN)2}2(μ-η1:1-L-L)](PF6)2 and [{CpRu(CH3CN)}2(μ-η1:1-L-L)2](PF6)2 (L-L=dppe, dpadppe). All of the compounds are characterized by microanalysis and NMR [1H and 31P{1H}] spectroscopy. The crystal structure of [{CpRu(CH3CN)2}2(μ-η1:1-dppe)](PF6)2 has been determined by X-ray diffraction analysis. The complex exhibits a dppe ligand bridging two CpRu(CH3CN)2 fragments.  相似文献   

5.
Three multinuclear complexes, [Co(L)(OAc)Co(CH3CH2OH)2]·H2O, [Zn(L)(OAc)Zn(CH3OH)], and [{Cd(L)(OAc)Cd(CH3OH)}2], containing a single-armed salamo-type bisoxime H3L have been synthesized and characterized structurally. The Co(II) complex forms a dimeric unit by intermolecular hydrogen bond interactions of neighboring dimeric molecules. The Zn(II) complex also forms a dimeric unit by intermolecular hydrogen bond interactions. Interesting features of the crystal structure include O?O short contacts. Meanwhile, self-assembling infinite 1-D, 2-D, and 3-D supramolecular structures are formed by intermolecular hydrogen bond and C–H?π interactions. The Cd(II) complex forms an infinite 2-D supramolecular structure by intermolecular hydrogen bond interactions. The photophysical properties of the Co(II), Zn(II), and Cd(II) complexes have also been discussed.  相似文献   

6.
Reactions of Pd8 strings supported by meso-Ph2PCH2P(Ph)CH2P(Ph)CH2PPh2 (meso-dpmppm) ligands, [Pd8(meso-dpmppm)4(L)2]4+ (L=CH3CN ( 1 ), XylNC ( 2 )) with C60 resulted in the exclusive formation of unprecedented metal-chain-wired C60 bucky balls, [{Pd4(meso-dpmppm)2(L)}2(C60)]4+ (L=CH3CN ( 11 ), XylNC ( 12 )), in which a C60 fullerene is trapped in the central Pd–Pd junction, as unambiguously established by spectroscopic, X-ray crystallographic, and theoretical techniques. The similar reaction of Pd8 strings supported by rac-dpmppm, [Pd8(rac-dpmppm)4(CH3CN)2]4+ ( 3 ) also afforded a racemic mixture of [{Pd4((R*,R*)-dpmppm)2(CH3CN)}2(C60)]4+ ( 13 ) without scrambling the Pd4 fragments with (R,R)- and (S,S)-dpmppm ligands. Consequently, those of enantiopure chiral Pd8 strings, [Pd8((R*,R*)-dpmppm)4(CH3CN)2]4+, certainly afforded chiral bucky balls of [{Pd4((R*,R*)-dpmppm)2(CH3CN)}2(C60)]4+ ( 13 RR and 13 SS ), that exhibit mirror-image circular dichroism spectra. The reactions of 1 and 2 were also applied for trapping a C70 fullerene to give 2 : 1 adducts of [{Pd4(meso-dpmppm)2(L)}2(C70)]4+ (L=CH3CN ( 21 ), XylNC ( 22 )). These results provide useful information for creating a platform to develop dimensionally and chirality controlled metal–carbon nanocomposite materials.  相似文献   

7.
Three new cyano-bridged compounds, viz., [{Cu(en)}{Cu(NH3)(en)}Re4Se4(CN)12]·{5H2O (1), [{Cu(dien)}2Re4Te4(CN)12]·9H2O (2), and [{Cu(trien)}2Re4Se4(CN)12]··5H2O (3), were synthesized by the reactions of the tetrahedral rhenium chalcocyanide cluster complexes K4[Re4Q4(CN)12] ((Q = Se or Te) with copper(II) cations in aqueous solutions containing ethylenediamine (en), diethylenetriamine (dien), or triethylenetetraamine (trien), respectively. Complex 1 has a ladder-tubular-like polymeric structure, in which two infinite chains are linked to each other by Re-CN-Cu bridges, compound 2 has a polymeric chain structure, and compound 3 has a molecular structure. The structures of all complexes were established by X-ray diffraction analysis.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2040–2044, October, 2004.  相似文献   

8.
Crown Ether Complexes of Lead(II). The Crystal Structures of [PbCl(18-Krone-6)][SbCl6], [Pb(18-Krone-6)(CH3CN)3][SbCl6]2 und [Pb(15-Krone-5)2][SbCl6]2 . [PbCl(18-crown-6)][SbCl6] has been prepared in low yield besides [Pb(CH3)2(18-crown-6)][SbCl6]2 by the reaction of Pb(CH3)2Cl2 with antimony pentachloride in acetonitrile solution in the presence of 18-crown-6, forming pale-yellow crystals. The other two title compounds are formed as colourless crystals by the reaction of PbCl2 with antimony pentachloride in acetonitrile solutions in the presence of 18-crown-6 and 15-crown-5, respectively. The complexes were characterized by IR spectroscopy and by crystal structure determinations. [PbCl(18-crown-6)][SbCl6]: Space group P21/c, Z = 8, 5 003 observed unique reflections, R = 0.046. Lattice dimensions at - 80°C: a = 1 386.9; b = 1 642.7; c = 2 172.1 pm, β = 92.95°. The lead atom in the cation [PbCl(18-crown-6)]+ is surrounded in an almost hexagonal-planar construction by the six oxygen atoms of the crown ether and an axially oriented Cl atom. [Pb(18-crown-6)(CH3CN)3][SbCl6]2: Space group P1 , Z = 2, 6 128 observed unique reflections, R = 0.076. Lattice dimensions at - 70°C: a = 1 228.0; b = 1 422.9; c = 1 463.2 pm, α = 69.08°; β = 65.71°; γ = 64.51°. In the cation [Pb(18-crown-6)(CH3CN)3]2+ the lead atom is coordinated by the six oxygen atoms of the crown ether and by the three nitrogen atoms of the acetonitrile molecules. The structure determination is restricted by disorder. [Pb( 15-crown-5)2][SbCI6]2: Space group P63/m, Z = 6, 5 857 observed unique reflections, R = 0.059. Lattice dimensions at -70°C: a = b = 2 198.5; c = 1499.4 pm, α = β = 90°, γ = 120°. In the cation [Pb(l5-crown-5)2]2 the lead atom is sandwich-like coordinated by the ten oxygen atoms of the two crown ether molecules. The structure determination is restricted by disorder.  相似文献   

9.
Di-μ-chlorobis(2-methyl-2-methoxy-3-t-butylthiopropyl)dipalladium(II) reacted with bis(1,3-diphenyl-2-imidazolidinylidene) to afford a new chlorobridged carbene complex [{PdCl(did)}2] (did  1,3-diphenyl-2-imidazolidinyl-idenato,2-C,2′-C) in 46.2% yield, which has a cyclopalladated chelate structure involving a Pd—carbene and a Pd—aryl bond; new carbene complexes, [{PdBr(did)}2], [{Pd(CH3COO)(did)}2], [Pd(acac)(did)], and [PdCl(did)Q] (Q  4-MePy, P[OCHMe2]3) were also prepared from [{PdCl(did)}2].  相似文献   

10.
[Na(15-crown-5)][ReFCl3(NO)(CH3CN)] Synthesis, IR Spectrum, and Crystal Structure The title compound has been prepared by the reaction of [ReCl3(NO)2(CH3CN)] with the equivalent amount of sodium fluoride in the presence of 15-crown-5 in boiling acetonitrile, forming blue crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. Space group P21/n, Z = 4,2117 observed independent reflections, R = 0.037, wR = 0.029. Lattice dimensions at 20°C: a = 834.0(2), b = 1600.0(3), c = 1670.0(3) pm; β = 104.19(3)°. The compound forms an ion pair via one Na F contact of 234.4 pm and one Na Cl contact of 293.4 pm; the nitrosyl ligand ist in trans-position to the F atom of the anion [ReFCl3(NO)(CH3CN)].  相似文献   

11.
On the Reactivity of Alkylthio Bridged 44 CVE Triangular Platinum Clusters: Reactions with Bidentate Phosphine Ligands The 44 cve (cluster valence electrons) triangular platinum clusters [{Pt(PR3)}3(μ‐SMe)3]Cl (PR3 = PPh3, 2a ; P(4‐FC6H4)3, 2b ; P(n‐Bu)3, 2c ) were found to react with PPh2CH2PPh2 (dppm) in a degradation reaction yielding dinuclear platinum(I) complexes [{Pt(PR3)}2(μ‐SMe)(μ‐dppm)]Cl (PR3 = PPh3, 3a ; P(4‐FC6H4)3, 3b ; P(n‐Bu)3; 3e ) and the platinum(II) complex [Pt(SMe)2(dppm)] ( 4 ), whereas the addition of PPh2CH2CH2PPh2 (dppe) to cluster 2a afforded a mixture of degradation products, among others the complexes [Pt(dppe)2] and [Pt(dppe)2]Cl2. On the other hand, the treatment of cluster 2a with PPh2CH2CH2CH2PPh2 (dppp) ended up in the formation of the cationic complex [{Pt(dppp)}2(μ‐SMe)2]Cl2 ( 5 ). Furthermore, the terminal PPh3 ligands in complex 3a proved to be subject to substitution by the stronger donating monodentate phosphine ligands PMePh2 and PMe2Ph yielding the analogous complexes [{Pt(PR3)}2(μ‐SMe)(μ‐dppm)]Cl (PR3 = PMePh2, 3c ; PMe2Ph, 3d ). NMR investigations on complexes 3 showed an inverse correlation of Tolmans electronic parameter ν with the coupling constants 1J(Pt,P) and 1J(Pt,Pt). All compounds were fully characterized by means of NMR and IR spectroscopy. X‐ray diffraction analyses were performed for the complexes [{Pt{P(4‐FC6H4)3}}2(μ‐SMe)(μ‐dppm)]Cl ( 3b ), [Pt(SMe)2(dppm)] ( 4 ), and [{Pt(dppp)}2(μ‐SMe)2]Cl2 ( 5 ).  相似文献   

12.
A series of binuclear complexes [{Cp*Ir(OOCCH2COO)}2(pyrazine)] ( 1 b ), [{Cp*Ir(OOCCH2COO)}2(bpy)] ( 2 b ; bpy=4,4′‐bipyridine), [{Cp*Ir(OOCCH2COO)}2(bpe)] ( 3 b ; bpe=trans‐1,2‐bis(4‐pyridyl)ethylene) and tetranuclear metallamacrocycles [{(Cp*Ir)2(OOC‐C?C‐COO)(pyrazine)}2] ( 1 c ), [{(Cp*Ir)2(OOC‐C?C‐COO)(bpy)}2] ( 2 c ), [{(Cp*Ir)2(OOC‐C?C‐COO)(bpe)}2] ( 3 c ), and [{(Cp*Ir)2[OOC(H3C6)‐N?N‐(C6H3)COO](pyrazine)}2] ( 1 d ), [{(Cp*Ir)2[OOC(H3C6)‐N?N‐(C6H3)COO](bpy)}2] ( 2 d ), [{(Cp*Ir)2[OOC(H3C6)‐N?N‐(C6H3)COO](bpe)}2] ( 3 d ) were formed by reactions of 1 a – 3 a {[(Cp*Ir)2(pyrazine)Cl2] ( 1 a ), [(Cp*Ir)2(bpy)Cl2] ( 2 a ), and [(Cp*Ir)2(bpe)Cl2] ( 3 a )} with malonic acid, fumaric acid, or H2ADB (azobenzene‐4,4′‐chcarboxylic acid), respectively, under mild conditions. The metallamacrocycles were directly self‐assembled by activation of C? H bonds from dicarboxylic acids. Interestingly, after exposure to UV/Vis light, 3 c was converted to [2+2] cycloaddition complex 4 . The molecular structures of 2 b , 1 c , 1 d , and 4 were characterized by single‐crystal x‐ray crystallography. Nanosized tubular channels, which may play important roles for their stability, were also observed in 1 c , 1 d , and 4 . All complexes were well characterized by 1H NMR and IR spectroscopy, as well as elemental analysis.  相似文献   

13.
Three multinuclear Cu (II), Zn (II) and Cd (II) complexes, [Cu2(L)(μ‐OAc)]·CHCl2 ( 1 ), [Zn2(L)(μ‐OAc)(H2O)]·3CHCl3 ( 2 ) and [{Cd2(L)(OAc)(CH3CH2OH)}2]·2CH3CH2OH ( 3 ) with a single‐armed salamo‐like dioxime ligand H3L have been synthesized, and characterized by FT‐IR, UV–vis, X‐ray crystallography and Hirshfeld surfaces analyses. The ligand H3L has a linear structure and C‐H···π interactions between the two molecules. The complex 1 is a dinuclear Cu (II) complex, Cu1 and Cu2 are all five‐coordinate possessing distorted square pyramidal geometries. The complex 2 also forms a dinuclear Zn (II) structure, and Zn1 and Zn2 are all five‐coordinate bearing distorted trigonal bipyramidal geometries. The complex 3 is a symmetrical tetranuclear Cd (II) complex, and Cd1 is a hexa‐coordinate having octahedral configuration and Cd2 is hepta‐coordinate with a pentagonal bipyramidal geometry, and it has π···π interactions inside the molecule. In addition, fluorescence properties of the ligand and its complexes 1 – 3 have also been discussed.  相似文献   

14.
The reaction of K2[PtCl4] with 2-(1-methylbenzyl)pyridine, HL, and 2-benzylpyridine, HL', affords the cyclometallated species [{Pt(L)Cl}2] (1) and [{Pt(L')Cl}2] (2), respectively. The chloride bridge in complex 1 can be split by neutral or anionic species to give the monomeric, [Pt(L)(Ph3P)Cl], as two isomers, trans-P-Pt-C (3) and trans-P-Pt-N, (4), [Pt(L)(py)Cl] (5), [Pt(L)(CO)Cl] (6), [Pt(L)(CNCH2SO2C6H4CH3-4)Cl] (7), [Pt(L)(acac)] (Hacac = 2,4-pentanedione) (8), [Pt(L)(dppm)][BF4] (dppm = bis(diphenyl-phosphino)methane) (9), [Pt(L)(dppe)][BF4] (dppe = bis(diphenylphosphino)ethane) (10) and [Pt(L)(dipy)][BF4](dipy = 2,2'-dipyridine) (11). Similarly, compound 2, by reaction with Ph3P, affords [Pt(L')(Ph3P)Cl], as two isomers, trans-P-Pt-C (12) and trans-P-Pt-N (13). Reaction of compounds 1 or 4 with AgBF4 in acetonitrile affords [Pt(L)(CH3CN)2IBF4] (14) or [Pt(L)(Ph3P)-(CH3CN)][BF4] (15). From these, [Pt(L)(Ph3P)2][BF4] (16), [Pt(L)(Ph3P)(CO)][BF4] (17) and [Pt(L)(Ph3P)(py)][BF4] (18), can be obtained by displacement of the coordinated acetonitrile. The new complexes were characterized by IR, 1H and 31P NMR and FAB-MS spectroscopic techniques. The NMR spectra at room temperature of most of the species derived from HL give evidence for the presence in solution of two diastereomers a and b. The structure of one diastereomer of complex 4 has been solved by single crystal X-ray diffraction, 4b. The platinum atom is in an almost square planar geometry with a P-Pt-N trans arrangement: Pt-N = 2.095(3), Pt-C = 1.998(4), Pt-P = 2.226(1) and Pt-Cl = 2.400(1) Å. The six-membered cyclometallated ring is in a boat conformation, with the CH3 group in an equatorial position, i.e pointing away from the metal. Attempts to obtain [{Pt(L″)Cl}2] (HL″ = 2-(dimethylbenzyl)pyridine), afforded an insoluble product heavily contaminated by platinum metal; treatment of this crude material with Ph3P gave [Pt(L″)(Ph3P)Cl] (19).  相似文献   

15.
Two new 1-D manganese(III) Schiff-base complexes bridged by dicyanamide (dca), [Mn(III)(5-Brsalen)(dca)] ? CH3OH (1) and [Mn(III)(3,5-Brsalen)(dca)] · CH3OH · CH3CN (2) (5-Brsalen = N,N′-ethylenebis(5-bromo salicylaldiminato) dianion; 3,5-Brsalen = N,N′-ethylenebis(3,5-dibromosalicylal diminato) dianion), have been synthesized and characterized. X-ray diffraction analyses reveal that the two complexes have 1-D chain structures constructed by μ 1,5-dca bridge. Magnetic susceptibility measurements exhibit weak antiferromagnetic exchange coupling in the complexes.  相似文献   

16.
The deep blue, paramagnetic Cs2[TcII(NO)F5] is formed during reactions of pertechnetate, acetohydroxamic acid, and CsF in aqueous HF. A reaction of Cs2[Tc(NO)F5] with BF3 · MeOH in acetonitrile gives yellow blocks of the fluorido‐bridged dimer [{TcI(NO)(CH3CN)4}2F](BF4)3. The compound is stable as solid and in acetonitrile solutions. The complex cation contains a bent μ‐F ligand and two linear nitrosyl groups.  相似文献   

17.
The 2-picolylpalladium(II) complex [{Pd(CH2Py)Cl(PPh3)}2] (CH2Py=2-picolyl) (I), prepared from 2-picolyl chloride and [Pd(PPh3)4], was treated with lithium bromide, silver acetate, 4-picoline (pic) and silver perchlorate, thallium acetylacetonate{Tl(acac)}, sodium dimenthyldithiocarbamate-water-(1/2) {Na(dmdc). 2 H2O}, and 1,2-bis(diphenylphospino)ethane (dppe) to yield [{PdBr(CH2Py)(PPh3)}2] (II), [{Pd(CH2Py)OAc(PPh3)}2] (III), [{Pd(Ch2Py)(pic)(PPh3)}2](ClO4)2 (IV), [Pd(CH2Py)(acac)(PPh3)] (V), [Pd(CH2Py)(dmdc)(PPh3)] (VI), and [Pd(Ch2Py)Cl(dppe)] (VII), respectively. Halogen abstraction from VII using silver perchlorate afforded an ionic complex [{Pd(CH2Py)(dppe)}2](ClO4)2 (VIII). It was concluded that the 2-picolyl groups in these eight complexes are σ-bonded to palladium, and that in the dinuclear complexes I, II, III, IV, and VIII, they serve as bridging ligands.  相似文献   

18.
Simple strategies to obtain magnesium complexes with the soft chelating diylidic ligand [Ph2PCHPPh2(fluorenylidene)]? (dppmflu?) were developed to evaluate the influence of the hard acid (cation) and soft base (anion) mismatch on the stability and reactivity of the formed derivatives. Deprotonation of the precursor Ph2PCH2PPh2(flu) (dppmfluH) by an alkylmagnesium derivative or magnesium amide provided access to [{Mg(dppmflu)(μ‐nBu)}2], [Mg(dppmflu){N(SiMe3)2}], and [{Mg(dppmflu)(μMe)}2], which were used as starting materials for further investigations. The reaction of [{Mg(dppmflu)(μ‐nBu)}2] with PhSiH3 in the presence of THF allowed isolation of the magnesium hydride complex [{Mg(dppmflu)(μH)(thf)}2] without a stabilizing nitrogen donor ligand. Prolonged heating enforced ligand redistribution and [{Mg(dppmflu)(μH)(thf)}2] was converted to [Mg(dppmflu)2] and MgH2. The homoleptic derivative [Mg(dppmflu)2], in which the magnesium center is in a very soft ligand environment, can open a THF molecule by frustrated Lewis pair reactivity to give [{Mg(dppmflu)(μOC4H8dppmflu)}2].  相似文献   

19.
The dinuclear hydroxo complex [{Pd(μ-OH)(Phox)}2] (I) (Phox = 2-(2-oxazolinyl)phenyl) reacts in a 1:2 molar ratio with several imidate ligands to yield new cyclometallated palladium complexes [{Pd(μ-NCO)(Phox)}2] containing asymmetric imidate –NCO– bridging units. [–NCO– = succinimidate (succ) (1), phtalimidate (phtal) (2), maleimidate (mal) (3), 2,3-dibromomaleimidate (2,3-diBrmal) (4) and glutarimidate (glut) (5)]. The reaction of these complexes with tertiary phosphines provides novel mononuclear N-bonded imidate derivatives of the general formula [Pd(imidate)(Phox)(PR3)] [R = Ph (a), 4-F–C6H4 (b) or CH2CH2CN (c)]. The new complexes were characterized by partial elemental analyses and spectroscopic methods (IR, FAB, 1H, 13C and 31P). The single-crystal structures of compounds 4, 4a and 5a have been established.  相似文献   

20.
Hydrolysis reactions of di- and trinuclear organotin halides yielded large novel cage compounds containing Sn−O−Sn bridges. The molecular structures of two octanuclear tetraorganodistannoxanes showing double-ladder motifs, viz., [{Me3SiCH2(Cl)SnCH2YCH2Sn(OH)CH2SiMe3}2(μ-O)2]2 [ 1 , Y=p-(Me)2SiC6H4-C6H4Si(Me)2] and [{Me3SiCH2(I)SnCH2YCH2Sn(OH)CH2SiMe3}2(μ-O)2]2 ⋅ 0.48 I2 [ 2⋅ 0.48 I2, Y=p-(Me)2SiC6H4-C6H4Si(Me)2], and the hexanuclear cage-compound 1,3,6-C6H3(p-C6H4Si(Me)2CH2Sn(R)2OSn(R)2CH2Si(Me)2C6H4-p)3C6H3-1,3,6 ( 3 , R=CH2SiMe3) are reported. Of these, the co-crystal 2⋅ 0.48 I2 exhibits the largest spacing of 16.7 Å reported to date for distannoxane-based double ladders. DFT calculations for the hexanuclear cage and a related octanuclear congener accompany the experimental work.  相似文献   

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