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1.
Walter Mier Keith A.N Graham Susanne Krämer Michael Eisenhut 《Tetrahedron letters》2004,45(28):5453-5455
The clinical impact of peptides that accumulate in tumours is determined by the number of particle emitting or paramagnetic isotopes attached. Therefore, attempts should be made to increase the cargo capacity of the peptide carriers. A general synthetic route to conjugates is described that allows insertion of multiple DOTA (1,4,7,10-tetraazacyclododecane-N′,N″,N?,N?-tetraacetic acid) moieties at the N-terminal end of the cyclic peptide Tyr3-octreotate. The peptide moiety was assembled by Fmoc solid phase synthesis and oxidised to form the cyclic disulfide. Subsequently, the required number of DOTA-tris tert-butyl ester chelating units were attached to the side chains of lysines. The conjugates were purified and thoroughly studied by RP-HPLC, size exclusion HPLC and mass spectrometry. The labelling of the novel conjugates and of DOTA0-Tyr3-octreotate (DOTATATE) was exemplified for 90Y and 111In. The methodology described here allows the versatile introduction of multiple DOTA chelates into a peptide sequence, thus, introducing a new scope to the receptor affine peptides that can be synthesised using solid phase synthesis. 相似文献
2.
[CoCl2{N,N′-Te2(NtBu)4}] (1) was obtained in good yields by the reaction of equimolar amounts of (tBu)NTe(μ-NtBu)2TeN(tBu) and CoCl2 in toluene under an argon atmosphere. The crystal structure of 1·CH2Cl2 showed that the dimeric tellurium diimide ligand is N,N′-chelated to cobalt. The related reaction of Se(NtBu)2 and CoCl2 affords a green product tentatively identified as a 1:1 adduct [CoCl2{N,N′-Se(NtBu)2}] (CHN analysis). However, recrystallization from thf produces the ion-separated complex [Co2(μ-Cl)3{N,N′-Se(NtBu)2}2(thf)2][CoCl3{NH2(tBu)}]·1½thf (2·1½thf), in which the monomeric selenium diimide ligand is N,N′-chelated to cobalt in the cation. A pathway for the formation of 2 from [CoCl2{N,N′-Se(NtBu)2}] in thf is proposed. 相似文献
3.
Almudena García-Fernández Josefina Díez Ángel Manteca Jesús Sánchez M. Pilar Gamasa Elena Lastra 《Polyhedron》2008
A series of half-sandwich ruthenium(II) complexes containing κ3(N,N,N)-hydridotris(pyrazolyl)borate (κ3(N,N,N)-Tp) and the water-soluble phosphane 1,3,5-triaza-7-phosphaadamantane (PTA) [RuX{κ3(N,N,N)-Tp}(PPh3)2−n(PTA)n] (n = 2, X = Cl (1), n = 1, X = Cl (2), I (3), NCS (4), H (5)) and [Ru{κ3(N,N,N)-Tp}(PPh3)(PTA)L][PF6] (L = NCMe (6), PTA (7)) have been synthesized. Complexes containing 1-methyl-3,5-diaza-1-azonia-7-phosphaadamantane(m-PTA) triflate [RuCl{κ3(N,N,N)-Tp}(m-PTA)2][CF3SO3]2 (8) and [RuX{κ3(N,N,N)-Tp}(PPh3)(m-PTA)][CF3SO3] (X = Cl (9), H (10)) have been obtained by treatment, respectively, of complexes 1, 2 and 5 with methyl triflate. Single crystal X-ray diffraction analysis for complexes 1, 2 and 4 have been carried out. DNA binding properties by using a mobility shift assay and antimicrobial activity of selected complexes have been evaluated. 相似文献
4.
《Journal of organometallic chemistry》2007,692(1-3):208-216
The reaction of [Cp1CoI2]2 (1b) with 2 equiv of NaNCNH affords the 16-membered macrocyclic NCNH-bridged tetracobalt(III) complex [Cp1CoI(μ2-NCNH-N,N′)]4 (2b), while that with 2 equiv of Na2NCN yields the C3-elongated cubane-like NCN-bridged tetracobalt(III) complex [Cp1Co(μ3-NCN-N,N,N′)3(CoCp1)3(μ3-NCN-N,N,N)] (4b). Treatment of [Cp1RhCl2]2 (1c) with 2 equiv of NaNCNH gives the C3-elongated cubane-like tetrarhodium(III) complex [Cp1Rh(μ3-NCN-N,N,N′)3(RhCp1)3(μ3-NCN-N,N,N)] (4c) via the macrocyclic complex [Cp1RhCl(μ2-NCNH-N,N′)]4 (2c). On the other hand, the reaction of [Cp1CoCl]2 (7) with Na2NCN affords the anionic bis(NCN)-capped tricobalt(II) complex Na[(Cp1Co)3(μ3-NCN-N,N,N)2] (6). The molecular structures of complexes 2b · CH2Cl2 and 4c · 2C6H6 have been confirmed by X-ray analyses. The electrochemical properties of these types of NCN-bridged group 9 metal complexes have also been examined. 相似文献
5.
Dra Lakk-Bogth Natalija Pantalon Juraj Bashdar I. Meena Berislav Peri Sreko I. Kirin Jzsef Kaizer 《Molecules (Basel, Switzerland)》2021,26(11)
Heme and nonheme-type flavone synthase enzymes, FS I and FS II are responsible for the synthesis of flavones, which play an important role in various biological processes, and have a wide range of biomedicinal properties including antitumor, antimalarial, and antioxidant activities. To get more insight into the mechanism of this curious enzyme reaction, nonheme structural and functional models were carried out by the use of mononuclear iron, [FeII(CDA-BPA*)]2+ (6) [CDA-BPA = N,N,N’,N’-tetrakis-(2-pyridylmethyl)-cyclohexanediamine], [FeII(CDA-BQA*)]2+ (5) [CDA-BQA = N,N,N’,N’-tetrakis-(2-quinolilmethyl)-cyclohexanediamine], [FeII(Bn-TPEN)(CH3CN)]2+ (3) [Bn-TPEN = N-benzyl-N,N’,N’-tris(2-pyridylmethyl)-1,2-diaminoethane], [FeIV(O)(Bn-TPEN)]2+ (9), and manganese, [MnII(N4Py*)(CH3CN)]2+ (2) [N4Py* = N,N-bis(2-pyridylmethyl)-1,2-di(2-pyridyl)ethylamine)], [MnII(Bn-TPEN)(CH3CN)]2+ (4) complexes as catalysts, where the possible reactive intermediates, high-valent FeIV(O) and MnIV(O) are known and well characterised. The results of the catalytic and stoichiometric reactions showed that the ligand framework and the nature of the metal cofactor significantly influenced the reactivity of the catalyst and its intermediate. Comparing the reactions of [FeIV(O)(Bn-TPEN)]2+ (9) and [MnIV(O)(Bn-TPEN)]2+ (10) towards flavanone under the same conditions, a 3.5-fold difference in reaction rate was observed in favor of iron, and this value is three orders of magnitude higher than was observed for the previously published [FeIV(O)(N2Py2Q*)]2+ [N,N-bis(2-quinolylmethyl)-1,2-di(2-pyridyl)ethylamine] species. 相似文献
6.
Wen-Yan Dan Jing-Tao Chen You-Ying Di Qiang Wang Wei-Wei Yang Yu-Xia Kong Da-Qi Wang 《The Journal of chemical thermodynamics》2011,43(2):161-166
A novel complex, bis(trans-bis(N,N-dimethyl-(1-(R)-phenyl-2-(S)-methyl-2-aminoethoxy-N,O))-copper(II)) heptahydrate (abbreviated as Cu2(C11H16NO)4·7H2O(cr)), was synthesized by the method of liquid phase reflux. The composition and structure of the complex were characterized by chemical analysis, elemental analysis, FTIR, and X-ray crystallography. A reasonable thermochemical cycle was designed based on the preparation reaction of the coordination compound, and standard molar enthalpies of dissolution of reactants and products were measured by an isoperibol solution-reaction calorimeter. Finally, the standard molar enthalpy of formation of the complex Cu2(C11H16NO)4·7H2O(cr) was determined to be ?(4525.22 ± 13.71) kJ · mol?1 in accordance with Hess’s law. 相似文献
7.
Fang-Yuan Lee Yu-Ju Chen Gene-Hsiang Lee Jih Ru Hwu 《Journal of organometallic chemistry》2005,690(2):441-449
The reaction of Os3(CO)12 with an excess of 1-hydroxypyridine-2-thione and Me3NO gives three mononuclear osmium complexes Os(CO)2(η2-SC5H4N(O))2 (1), Os(CO)2(η2-SC5H4N(O))(η2-SC5H4N) (2), and Os(CO)2(η2-SC5H4N)2 (3). The results of single-crystal X-ray analyses reveal that complex 1 contains two O,S-chelate pyridine-2-thione N-oxide (PyOS) ligands, whereas complex 2 contains one O,S-chelate PyOS and one N,S-chelate pyridine-2-thiolate group. The unique structure of 2 provides evidence of the pathway for this transformation. When this reaction was monitored by 1H NMR spectroscopy the triosmium complexes Os3(CO)10(μ-H)(μ-η1-S-C5H4N(O)) (4) and Os3(CO)9(μ-H)(μ-η1:η2-SC5H4N(O)) (5) were identified as intermediates in the formation of the mononuclear final products 1-3. The proposed pathway is further supported by the observation of several dinuclear osmium intermediates by electrospray ionization mass spectrometry. In addition, the reaction of Os3(CO)12 with 1-hydroxypyridine-2-thione in the absence of Me3NO at 90 °C generated mononuclear complex 2 as the major product along with smaller amounts of complexes 1 and 3. These results suggest that the N-oxide facilitates the decarbonylation reaction. Crystal data for 1: monoclinic, space group C2/c, a = 26.9990(5) Å, b = 7.6230(7) Å, c = 14.2980(13) Å, β = 101.620(2)°, V = 2882.4(4) Å3, Z = 8. Crystal data for 2: monoclinic, space group C2/c, a = 5.7884(3) Å, b = 13.9667(7) Å, c = 17.2575(9) Å, β = 96.686(1)°, V = 1385.69(12) Å3, Z = 4. 相似文献
8.
Density functional calculations with the B3LYP functional were carried out for the [Ru(NO)Cl5]2−, [Ru(NO)(NH3)5]3+, [Ru(NO)(CN)5]2−, [Ru(NO)(CN)5]3−, [Ru(NO)(hedta)]q (hedta = N-(hydroxyethyl)ethylenediaminetriacetate triple-charged anion; q = 0, −1, −2), Rh2(O2CR)4, Rh2(O2CR)4(NO)2, Ru2(O2CR)4, Ru2(O2CR)4(NO)2, Ru2(dpf)4, and Ru2(dpf)4(NO)2 (dpf = N,N′-diphenylformamidinate ion; R = H, CH3, CF3) complexes. The electronic structure was analyzed in terms of Mayer and Wiberg bond order indices. The technique of bond order indices decomposition into σ-, π-, and δ-contributions was proposed. 相似文献
9.
Kwong-Chak Cheung Ming-Him So Kam-Piu Ho Kam-Han Lee Zhong-Yuan Zhou 《Journal of organometallic chemistry》2009,694(17):2842-85
A dipyridylamine ligand with a pendant pyrrole (N-(3-N,N′-bis(2-pyridyl)propylamino)pyrrole, PPP) and its corresponding rhenium(I) complex, Re(CO)3(κ2-N,N-PPP)Cl, were synthesized. The structure of Re(CO)3(κ2-N,N-PPP)Cl was determined by X-ray crystallography. Electrochemical polymerization of the pyrrole moiety resulted in the immobilization of poly[Re(CO)3(κ2-N,N-PPP)Cl] film onto a glassy carbon electrode, which exhibited electrocatalytic activity for the reduction of CO2 to CO. 相似文献
10.
Microwave-assisted synthesis of phthalocyanine-porphyrin complex and its photoelectric conversion properties 总被引:1,自引:0,他引:1
A soluble phthalocyanine-porphyrin complex (Lu(TBPor)Pc) has been rapidly synthesized from a lutetium porphyrin (Lu(TBPor)OAc) and a metal-free phthalocyanine (H2(TBPc)) under microwave irradiation. Its photoelectric conversion properties have also been investigated. The experimental results reveal that Lu(TBPor)Pc exhibits better photoelectric conversion effect than Lu(TBPor)OAc, H2(TBPc), and Lu(TBPor)OAc/H2(TBPc) blend. Furthermore, we have also introduced a n-type photoconductor (N,N′-bis(1,5-dimethylhexyl)-3,4:9,10-perylenebis(dicarboximide)(PDHEP)) and TiO2 into Lu(TBPor)Pc photoelectric cell to fabricate a SnO2/Lu(TBPor)Pc + PDHEP + TiO2/Al photoelectric cell, exhibiting the largest short-circuit photocurrent (691.3μA/cm2) among all of lab-made cells under illumination of white light (1.2 mW/cm2). 相似文献
11.
《Journal of organometallic chemistry》2006,691(24-25):5423-5430
The reaction of (SPY-5-34)-dichloro-(κ2(C,O)-2-formylbenzylidene)(H2IMes)ruthenium (H2IMes=1,3-bis(2,4,6-trimethylphenyl)-4,5-dihydroimidazol-2-ylidene) with potassium hydridotris(pyrazolyl)borate (KTp) in dichloromethane yielded an unusual ruthenium complex chloro(κ3(N,N,N)-chlorotris(pyrazolyl)borate)(κ2(C,C)-1-(2,4,6-trimethylphenyl)-3-(4,6-dimethylphenyl-2-methylidene)-4,5-dihydroimidazol-2-ylidene)ruthenium (2). In 2, a chlorotris(pyrazolyl)borate ligand, which had been created during this reaction, binds in κ3(N,N,N)-mode to the central ruthenium atom. Additionally, a double C–H activation of a methyl group of the H2IMes resulted in the formation of a chelating N-heterocyclic biscarbene ligand and liberation of the former 2-formylbenzylidene as 2-methylbenzaldehyde. Formally, a double hydrogen transfer from a methyl group of the H2IMes to the initial carbene carbon occurred. 2 was characterized by NMR spectroscopy, elemental analysis and single crystal X-ray structure determination. The reaction of KTp with (SPY-5-34)-dichloro(κ2(C,O)-2-ethoxycarbonylbenzylidene)(H2IMes)ruthenium, on the other hand, gave the expected product chloro(κ3(N,N,N)-hydridotris(pyrazolyl)borate)(H2IMes)(2-ethoxycarbonylbenzylidene)ruthenium (6). Compound 6 was characterized by NMR spectroscopy, elemental analysis and single crystal X-ray structure determination. Investigations of the relative activities of these complexes in model ring opening metathesis polymerizations showed a pronounced thermal latency. Polymerizations proceeded at temperatures above 100 °C in case of 6 and 130 °C in case of 2. 相似文献
12.
Treatment of the uranium(IV) complexes [{ML1(py)}2UIV] (M = Cu, Zn; L1 = N,N′-bis(3-hydroxysalicylidene)-1,3-propanediamine) with silver nitrate in pyridine led to the formation of the corresponding cationic uranium(V) species which were found to be thermally unstable and were converted back into the parent UIV complexes; no electron transfer was observed in solution between the UIV and UV compounds. In the crystals of [{ML1(py)}2UIV][{ML1(py)}2UV][NO3], the neutral UIV and cationic UV species are clearly identified by the distinct U–O distances. Similar reaction of [{ZnL2(py)}2UIV] [L2 = N,N′-bis(3-hydroxysalicylidene)-1,4-butanediamine] with AgNO3 gave crystals of [{ZnL2(py)}UV{ZnL2(py)2}][NO3] but the copper counterpart was not isolated. Crystals of [{ZnL1(py)}2UV][OTf] · THF (OTf = OSO2CF3) were obtained fortuitously from the reaction of [Zn(H2L1)] and U(OTf)3. 相似文献
13.
The family of hydroxymonophosphates of generic formula AMIII(PO3(OH))2 has been revisited using hydrothermal techniques. Four new phases have been synthesized: CsIn(PO3(OH))2, RbFe(PO3(OH))2, RbGa(PO3(OH))2 and RbAl(PO3(OH))2. Single crystal diffraction studies show that they exhibit two different structural types from previously observed other phases with A=H3O, NH4, Rb and M=Al, V, Fe. The “Cs-In” and “Rb-Fe” phosphates crystallize in the triclinic space group , with the cell parameters a=7.4146(3) Å, b=9.0915(3) Å, c=9.7849(3) Å, α=65.525(3)°, β=70.201(3)°, γ=69.556(3)° and V=547.77(4) Å3 (Z=3) for CsIn(PO3(OH))2 and a=7.2025(4) Å, b=8.8329(8) Å, c=9.4540(8) Å, α=65.149(8)°, β=70.045(6)°, γ=69.591(6)° and V=497.44(8) Å3 (Z=3) for α-RbFe(PO3(OH))2. The “Rb-Al” and “Rb-Ga” phosphates crystallize in the Rc space group, with a=8.0581(18) Å and c=51.081(12) Å (V=2872.5(11) Å3 and Z=18) for RbAl(PO3(OH))2 and a=8.1188(15) Å and c=51.943(4) Å (V=2965(8) Å and Z=18) for RbGa(PO3(OH))2. These two structural types are closely related. Both are built up from MIIIO6 octahedra sharing their apices with PO3(OH) tetrahedra to form [M3(PO3OH)6] units, but the latter exhibits a different configuration of their tetrahedra. The three-dimensional host-lattices result from the connection of the [M3(PO3OH)6] units and they present numerous intersecting tunnels containing the monovalent cations. 相似文献
14.
A series of vanadium(V) complexes with unsymmetrical tridentate Schiff base ligands, obtained by the single condensation of R(−)-1,2-diaminopropane with salicylaldehyde and its derivatives, 2-hydroxy-1-naphthaldehyde, 2-hydroxyacetophenone, 1-hydroxy-2-acetonaphthone and 2-hydroxybenzophenone, were prepared. The complexes were characterized by elemental analysis and by their IR, CD, UV–Vis, 1D (1H, 51V) and 2D (COSY, NOESY, gHSQC) NMR spectra. Crystal structures of the mononuclear complex {R(−)-2-amino-1-N-[(2′-oxido-κO-4′,6′-dimethoxyphenyl)methylene]aminopropane-κ2N}dioxidovanadium(V), VO2(C12H17N2O3), 4, and of the dinuclear complex, di-μ-oxido-bis({R(−)-2-[1-(2-aminopropylimino)ethyl]-4-methylphenolato-κ3N,N′,O}oxidovanadium(V)), V2O4(C11H15N2O)2, 5, have been obtained by X-ray diffraction studies. The structure of 4 was revealed to be a distorted trigonal–bipyramidal coordination geometry, rarely encountered in VO2(tridentate Schiff base) complexes. Complexes 2 and 3 have the ability to catalyze the oxidation of prochiral sulfide substrates PhSR (R = Me, Bz) utilizing hydrogen peroxide or cumene hydroperoxide (CHPO) as the oxidant. 相似文献
15.
Two novel assembling systems 3 and 4, with the structures of C6F5CF2−?H+N(Me)2CH2CH2(Me2)N+H?−CF2C6F5 and C6F5CF2I?N(Me)2CH2CH2(Me)2N?ICF2C6F5, respectively, have been generated from the solution of heptafluorobenzyl iodide 1 and N,N,N′,N′-tetramethylethylenediamine 2 in dichloromethane. Their structures have been characterized by X-ray diffraction analysis, NMR and IR spectroscopy. Intermolecular N?I halogen bond and F?H hydrogen bond are revealed to be the driving forces for their formation. 相似文献
16.
Reactions of (1R,2R)-N1,N2-bis(pyridinylmethyl)cyclohexane-1,2-diamine derivatives, (1R,2R)-2-bpcd and (1R,2R)-3-bpcd [(1R,2R)-2-bpcd = (1R,2R)-N1,N2-bis(pyridin-2-ylmethyl)cyclohexane-1,2-diamine, (1R,2R)-3-bpcd = (1R,2R)-N1,N2-bis(pyridin-3-ylmethyl)cyclohexane-1,2-diamine], with CdI2 in an analogous way led to the formation of a chiral discrete mononuclear complex and a chiral one-dimensional polymeric chain, respectively, which may be attributed to the positional isomerism of the ligands. The chiral organic ligands and complexes display luminescent properties indicating that they may have a potential application as optical materials. Powder second-harmonic generation (SHG) efficiency measurement shows that the SHG efficiency of the complexes is approximately 0.3 and 0.45 times that of KDP, respectively. 相似文献
17.
The synthesis of tricyclic compounds on functionalized cyclam core is described. The addition of four methyl acrylate molecules and consecutive condensation of this derivative with ethylenediamine resulted in formation of 1,4,8,11-tetrakis(2-(N-(2-aminoethyl)carbamoyl)ethyl)-1,4,8,11-tetraazacyclotetradecane (3). Compound 3 was the substrate for further condensation with dialdehydes: iso-phthaldialdehyde and 2,6-pyridinedicarbaldehyde, resulting in spontaneous macrocycle ring closure to give tricyclic derivatives: 1,11:4,8-bis(benzene-1,3-diyl-bis(2-(N-(2-formidoylethylene)carbamoyl)ethylene))-1,4,8,11-tetraazacyclotetradecane (4) in the reaction of 3 with iso-phthaldialdehyde and three isomers: 1,4:8,11-bis(pyridine-2,6-diyl-bis(2-(N-(2-formidoylethylene)carbamoyl)ethylene))-1,4,8,11-tetraazacyclotetradecane (5A), 1,11:4,8-bis(pyridine-2,6-diyl-bis(2-(N-(2-formidoylethylene)carbamoyl)ethylene))-1,4,8,11-tetraazacyclotetradecane (5B), and 1,8:4,11-bis(pyridine-2,6-diyl-bis(2-(N-(2-formidoylethylene)carbamoyl)ethylene))-1,4,8,11-tetraazacyclotetradecane (5C) when 2,6-pyridinedicarbaldehyde was used. The compounds 4, 5B, and 5C were identified crystallographically. The isolated 5A converted in solution into the mixture of 5B and 5C as monitored by the 1H NMR spectroscopy. The tricycle 5 is able to accept two manganese(II) metal ions by reacting with manganese(II) dichloride with simultaneous diprotonation of 5. Structure of the resulting Mn2(5BH2)Cl6·(CH3OH)2(H2O)2 was determined crystallographically. 相似文献
18.
Junying Chen Heejung Yoon Yong-Min Lee Mi Sook Seo Ritimukta Sarangi Shunichi Fukuzumi Wonwoo Nam 《Chemical science》2015,6(6):3624-3632
Triflic acid (HOTf)-bound nonheme Mn(iv)-oxo complexes, [(L)MnIV(O)]2+–(HOTf)2 (L = N4Py and Bn-TPEN; N4Py = N,N-bis(2-pyridylmethyl)-N-bis(2-pyridyl)methylamine and Bn-TPEN = N-benzyl-N,N′,N′-tris(2-pyridylmethyl)ethane-1,2-diamine), were synthesized by adding HOTf to the solutions of the [(L)MnIV(O)]2+ complexes and were characterized by various spectroscopies. The one-electron reduction potentials of the MnIV(O) complexes exhibited a significant positive shift upon binding of HOTf. The driving force dependences of electron transfer (ET) from electron donors to the MnIV(O) and MnIV(O)–(HOTf)2 complexes were examined and evaluated in light of the Marcus theory of ET to determine the reorganization energies of ET. The smaller reorganization energies and much more positive reduction potentials of the [(L)MnIV(O)]2+–(HOTf)2 complexes resulted in greatly enhanced oxidation capacity towards one-electron reductants and para-X-substituted-thioanisoles. The reactivities of the Mn(iv)-oxo complexes were markedly enhanced by binding of HOTf, such as a 6.4 × 105-fold increase in the oxygen atom transfer (OAT) reaction (i.e., sulfoxidation). Such a remarkable acceleration in the OAT reaction results from the enhancement of ET from para-X-substituted-thioanisoles to the MnIV(O) complexes as revealed by the unified ET driving force dependence of the rate constants of OAT and ET reactions of [(L)MnIV(O)]2+–(HOTf)2. In contrast, deceleration was observed in the rate of H-atom transfer (HAT) reaction of [(L)MnIV(O)]2+–(HOTf)2 complexes with 1,4-cyclohexadiene as compared with those of the [(L)MnIV(O)]2+ complexes. Thus, the binding of two HOTf molecules to the MnIV(O) moiety resulted in remarkable acceleration of the ET rate when the ET is thermodynamically feasible. When the ET reaction is highly endergonic, the rate of the HAT reaction is decelerated due to the steric effect of the counter anion of HOTf. 相似文献
19.
《Solid State Sciences》2004,6(6):593-598
The solution-mediated syntheses and single crystal structures of C6N2H10·Zn(HPO3)2 (I) and (C6N2H8)0.5·ZnHPO3 (II) are reported. Slight variation of the synthesis conditions led to two quite different phases. I contains infinite chains of ZnO4 and HPO3 groups with the protonated organic moiety acting as a template and interacting with the chains by NH⋯O hydrogen bonds and possible CH⋯O interactions. In II, the neutral 1,4-diamino benzene molecule bonds to Zn (as a ligand) and an unusual composite, “pillared”, structure results, with the organic species bridging 63 polyhedral sheets, although NH⋯O bonds are also present. Similarities and differences to other zinc phosphites and phosphates are briefly discussed for I and II. Crystal data: C6N2H10·Zn(HPO3)2, Mr=335.48, monoclinic, C2/c (No. 15), a=17.2471 (14) Å, b=9.0720 (8) Å, c=7.6529 (6) Å, β=103.752 (2)°, V=1163.09 (7) Å3, Z=4, R(F)=0.038, wR(F2)=0.084. (C6N2H8)0.5·ZnHPO3, Mr=199.42, orthorhombic, Pbca (No. 61), a=8.0314 (16) Å, b=8.1299 (16) Å, c=18.830 (4) Å, V=1229.5 (4) Å3, Z=8, R(F)=0.026, wR(F2)=0.055. 相似文献
20.
Three new N,N′-dialkylimidazolium salts of cadmium-thiocyanate, [EtMeIm]2[Cd2(SCN)6] (2), [C6H4(CH2ImMe)2][Cd(SCN)4] (3), [C6Me3(CH2ImMe)3][CdBr3(SCN)](NO3) (4) have been prepared, and their crystal structures have been determined by X-ray diffraction. Crystal data: 2, monoclinic, C2/c, a=18.349(4) Å, b=7.8667(18) Å, c=21.399(5) Å, β=110.346(4)°, V=2896.1(11) Å3, Z=4, and R1=0.0561; 3, monoclinic, C2/c, a=20.347(7) Å, b=14.029(5) Å, c=9.380(3) Å, β=112.034(6)°, V=2482.1(15) Å3, Z=4, and R1=0.0397; 4, hexagonal, P63, a=b=10.7634(8) Å, c=16.0315(17) Å, V=1608.4(2) Å3, Z=2, and R1=0.0569. Compound 2 consists of triply bridged infinite one-dimensional cadmium-thiocyanate chains, and two independent cadmium atoms are octahedrally coordinated in 2N4S and 4N2S geometry, respectively. In 3, the cadmium atom is octahedrally coordinated with two cis N-bonded monodentate NCS− ligands and four bridging SCN− in a S trans to S, and N trans to N coordination fashion, and thus form doubly bridged infinite one-dimensional chains. Whereas 4 is mononuclear, consisting of a discrete [C6Me3(CH2ImMe)3]3+ cation, a nitrate, and [CdBr3(SCN)]− ion, and each cadmium(II) ion is coordinated to three bromide and one nitrogen atom of SCN− ion. The structures of these compounds are dictated by the imidazolium cations. 相似文献