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1.
The synthesis of new dihaloheptasilanes X2Si[SiMe(SiMe3)2]2 (X=Cl: 2, Br: 3, I: 4) was performed by treating dihydridoheptasilane 1 (X=H) with CCl4, HCBr3 or HCI3. Difluoroheptasilane 6 (X=F) was prepared from either diphenylheptasilane 5 (X=Ph), triflic acid (HOTf), and LiF with concomitant isolation of heptasilanes 7 (X2=Ph and OTf), 8 (X2=F and Ph), and 9 (X2=F and OTf), or by halogen exchange from 2 using ZnF2. Crystal structures of 2, 3, 4, and 5 are reported.
The reduction of 2 with Li, Na or KC8 resulted in the instantaneous formation of various cyclotrisilanes, while the reduction of 3 gave exclusively the unsymmetrical cyclotrisilane (E)-1-methyl-2,3,3-tris[methylbis(trimethylsilyl)silyl]-1,2-bis(trimethylsilyl)cyclotrisilane 10, which was characterized by X-ray crystallography. A mechanism for the formation of cyclotrisilanes via a silylsilylene-to-disilene
rearrangement is proposed.
Attempts to prepare the tetradekasilane [(Me3Si)2MeSi]2SiH–SiH[SiMe(SiMe3)2]2 (by reductive dehalogenation of either HClSi[SiMe(SiMe3)2]2
13 or HISi[SiMe(SiMe3)2]2
18), or the tetradekasilane [(Me3Si)2MeSi]2SiPh–SiPh[SiMe(SiMe3)2]2 (by reductive dehalogenation of either PhClSi[SiMe(SiMe3)2]2
14 or PhISi[SiMe(SiMe3)2]2
19) as precursors for the disilene [(Me3Si)2MeSi]2Si=Si[SiMe(SiMe3)2]2 failed. 14 was characterized by X-ray crystallography. All compounds described were also characterized by multinuclear NMR spectroscopy
and elemental analysis. 相似文献
2.
《Journal of Coordination Chemistry》2012,65(20):3565-3575
Three supramolecular complexes [Zn(HL1 )2(H2O)2(ZnCl4)2] (1), [Cu(L2 )2Cl2] (2), and [Zn(L3 )Cl2] (3) have been synthesized and characterized by single crystal X-ray diffraction analysis (L1 = 3,5-di(2-pyridyl)-4-amino-1,2,4-triazole, L2 = 3,5-di(2-pyridyl)-1,2,4-triazole, and L3 = 2-pyridinecarboxylic acid (pyridin-2-ylmethylene)-hydrazide). In 1, anion–π interactions between Cl? and the π-systems of L1 are observed and anion–π, hydrogen bonding and π–π stacking interactions link the two complex units of [Zn(HL1 )2(H2O)2]4+ and [ZnCl4]2? to form a 3-D supramolecular network. In 2, π–π stacking interactions between aromatic rings of 1,2,4-triazole and pyridine rings are observed; in 3, hydrogen bonding of Cl ··· H–N and π–π stacking interactions between parallel pyridine rings of L 3 are observed. The mechanisms of rearrangement reactions of L to L1 –L3 are discussed. The fluorescent properties for solid 1 and 3 are also investigated. 相似文献
3.
Chang-Jiu Wang Wen-Fang Xu Bi-Hai Tong Ai-Quan Jia 《Journal of Coordination Chemistry》2017,70(10):1617-1631
Eight substituted bidentate Schiff base ligands HOC6H4CH=N-R (HL) (HL1: R = 4-ClC6H4, HL2: R = 2-ClC6H4, HL3: R = 4-NO2C6H4, HL4: R = 4-MeC6H4, HL5: R = 2,6-Me2C6H3, HL6: R = 2,46-Me3C6H2, HL7: R = CH2C6H5, and HL8: R = n-Pr) were synthesized by the typical condensation reaction. Interaction of cis-[Ru(bpy)2Cl2]?2H2O (bpy = 2,2′-bipyridine) with one equivalent of HL ligand in the presence of KPF6 afforded the cationic ruthenium(II) complexes of the type [Ru(bpy)2(L)](PF6) (1–8). The reaction of cis-[Ru(phen)2Cl2]?2H2O (phen = 1,10-phenanthroline) and HL1 under similar condition gave complex [(phen)2Ru(L)](PF6) (1a). Treatment of cis-[Ru(phen)2Cl2]?2H2O with two equivalents of HL in the presence of KPF6 resulted in isolation of the cationic ruthenium(III) complexes of the type [Ru(phen)(L)2](PF6) (9-16). All complexes have been spectroscopically characterized. The structures of 1a?CH2Cl2, 2?½CH2Cl2, 3?CH3CN, 5?½H2O, 6, 12?½HOCH2CH2OH, 13?CH3CN, 15?H2O, and 16 have been determined by single-crystal X-ray diffraction. 相似文献
4.
Huiyeong Ju So Young Lee Eunji Lee Seulgi Kim In-Hyeok Park 《Supramolecular chemistry》2017,29(10):723-729
AbstractA comparative study on the exo-coordination-based networking of 15-membered O2S2-macrocycle isomers (L1 and L2) induced by interdonor distances is reported. In copper(I) bromide complexation, the isomer L1 incorporating a shorter sulfur-to-sulfur separation yielded a discrete dimer complex [(μ-Cu2Br2)(L1)2] (1) in which two macrocycles are bridged by a Cu2Br2 square cluster. While, the reaction of copper(I) bromide with the isomer L2 incorporating a longer sulfur-to-sulfur separation afforded a double-stranded one-dimensional (1D) coordination polymer {[(μ4-Cu2Br2)(L2)2]·CH2Cl2}n (2) as a kinetic product which converted to [(μ4-Cu2Br2)(L2)2]n (3) with different 1D connectivity pattern as a thermodynamic product. The results indicate as examples of programmed self-assembly that the proposed interdonor distances and the ligand isomerism play decisive roles cooperatively in the topologies of the supramolecular products via different coordination modes. 相似文献
5.
Jin-Hua Wang Ting-Xiao Qin Yue-Zhi Cui Seik Weng Ng 《Journal of Coordination Chemistry》2017,70(7):1168-1189
Five new coordination complexes, [CdI2(3-PyBim)](H2O)3 (1), [Cd(SO4)(3-PyBim)(H2O)4] (2), [CdCl2(4-PyBim)2(H2O)2] (3), [CdBr2(4-PyBim)2(H2O)2] (4) and [CdI2(4-PyBim)2(H2O)2] (5) [3-PyBim=2-Pyridin-3-yl-1H-benzoimidazole, 4-PyBim=2-Pyridin-4-yl-1H-benzoimidazole], were obtained under hydrothermal conditions and characterized by single crystal X-ray diffraction, IR, elemental analysis, and powder X-ray diffraction. All of the complexes have mononuclear structures. Among the crystal structures of these complexes, there exist a variety of intermolecular hydrogen bonding interactions and π?π interactions, which further extend to a 3-D supramolecular architecture. The solid state photoluminescent properties of 1–5 vary with the electronegativity of the coordination anion. Additionally, the thermogravimetric analyses of these complexes are discussed. 相似文献
6.
《Journal of Coordination Chemistry》2012,65(24):4430-4440
Reaction of Ln(NO3)3?·?6H2O with H2napn (H2napn?=?N,N′-ethylenebis(2-hydroxy-1-naphthylideneiminato)) and KSCN produces seven new coordination polymers, [La(H2napn)(SCN)(C2H5OH)2(NO3)2] n (1), [La(H2napn)2(SCN)(NO3)2] n (2), and [Ln(H2napn)1.5(NO3)3] n [Ln?=?La(3), Sm(4), Eu(5), Dy(6), Er(7)]. Crystal structure analysis reveals that H2napn functions as a bridging ligand, forming a 1-D chain polymer (1) and 2-D open-frameworks (2–7) with lanthanides. Each metal center of 1–7 is nine-coordinate. Lanthanide contraction is observed in 3–7. 相似文献
7.
X-ray crystallographic studies of cobalt(III) complexes of 5-methyl-3-formylpyrazole-N(4)-diethylthiosemicarbazone (HMPzNEt2), [Co(MP
z
NEt
2
)
2
]Br·2H
2
O, 5-methyl-3-formylpyrazole-N(4)-dipropylthiosemicarbazone (HMPzNPr
2
), [Co(MP
z
NPr
2
)
2
]Br·2H
2
O and 5-methyl-3formylpyrazole-N(4)-dibutylthiosemicarbazone (HMPzNBu
2
), [Co(MP
z
NBu
2
)
2
]Br·H
2
O, have been reported. In all the three complex species, X-ray crystallography has authenticated a CoN4S2 octahedral coordination with the pair of orthogonally coordinated NNS tridentate ligands in the monodeprotonated form of
the ligand. The two azomethine nitrogen atoms are trans to each other, while the pyrazolyl ring nitrogens and the thiolato sulfurs are in cis positions. A gradual decrease in the dihedral angle between the coordinating ligands has been observed with increase in the
bulkiness of the aliphatic side chains of the substituent on the thiosemicarbazone moieties. In all the three complexes, intraligand
C–H···S contacts appear to arrest the free rotation of the side chains about the C(6)–N(5) single bond.
†Deceased 相似文献
8.
《Journal of Coordination Chemistry》2012,65(6):1063-1070
Transition metal complexes [Fe(HL)2]Cl3 ? 1.5H2O (1), [Co(L)2] ? ClO4 ? H2O (2), Ni(HL)2(ClO4)2 ? 2H2O (3), Zn(HL)L ? BF4 ? 2H2O (4), and Cd(HL)2(ClO4)2 ? 2H2O (5), where HL = C7H9N5S, 2-acetylpyrazine thiosemicarbazone, have been synthesized. Complex 2 was characterized by elemental analysis, infrared spectra, mass spectra, and single-crystal X-ray diffraction. Preliminary in vitro screening showed that 1, 4, and 5 exhibit higher antitumor activity than 2 and 3 against K562 leucocythemia cancer cell line. 相似文献
9.
利用3-(2-吡啶基)-1,2,4-三唑配体(HL)和不同的金属盐设计合成了5个配合物[Co(HL)2(H2O)2](NO3)2(1)、[Cu2(L)2(NO3)2(H2O)4](2)、[Cu2(L)2(AcO)2(H2O)2]·6H2O(3)、[Cu2(L)2(HL)2(ClO4)2]·2CH3CN(4)和[Cd2(L)2(HL)2(NO3)2]·2H2O(5),并通过X射线单晶衍射、红外、元素分析、X射线粉末衍射和热重对配合物结构进行了表征。测试结果表明配合物1具有单核结构,并且可以通过氢键的相互作用形成二维超分子结构。配合物2~5为双核结构。配合物2和5可以通过氢键的相互作用形成二维超分子结构。配合物3通过氢键的相互作用形成三维超分子结构。研究了配合物中HL配体的配位模式。此外,研究了配体HL和配合物2和5的固态荧光性质及荧光寿命。 相似文献
10.
《Journal of Coordination Chemistry》2012,65(22):4032-4051
Ten new complexes, [Cu2(L1)(NO3)2]·2H2O (1), [Cu4(L1)2]·4ClO4·H2O (2), [Cu2(L1)(H2O)2]·(adipate) (3), [Cu6(L1)2(m-bdc)4]·2DMF·5H2O (4), [Cu2(L1)(Hbtc)]·5H2O (5), [Cu2(L1)(H2O)2]·(ntc)·3H2O (6), [Co2(L2)]·[Co(MeOH)4(H2O)2] (7), [Co3(L2)(EtOH)(H2O)] (8), [Ni6(L2)2(H2O)4]·H2O (9) and [Zn4(L2)(OAc)2]·0.5H2O (10), have been synthesized. 1 displays a [Cu2(L1)(NO3)2] monomolecular structure. 2 shows a supramolecular chain including [Cu2L1]2+. In 3, two Cu(II) ions are connected by L1 to form a [Cu2(L1)(H2O)2]2+ cation. In 4, the m-bdc anions bridge Cu(II) ions and L1 anions to form a layer. Both 5 and 6 display 3-D supramolecular structures. 7 consists of both [Co2L2]2? and [Co(MeOH)4(H2O)2]2+ units. 8 and 9 show infinite chain structures. In 10, Zn(II) dimers are linked by L2 to generate a 3-D framework. The magnetic properties for 4 and 8 and the luminescent property for 10 have been studied. 相似文献
11.
《Journal of Coordination Chemistry》2012,65(8):1234-1243
New biferrocenylpropane derivatives FcC(CH3)2Fc′-C≡C–R [Fc?=?C5H5FeC5H4; Fc′?=?C5H5FeC5H3, R?=?C6H5 (L 1 ), Fc (L 2 )] and their complexes [FcC(CH3)2Fc′-C≡C–R][Co2(CO)6] [R?=?C6H5 (1); R?=?Fc (2)] have been synthesized by the Castro-Stephens coupling reaction and the reactions of ligands L 1 , L 2 with Co2(CO)8. Compounds L 1 , L 2 , 1 and 2 were characterized by elemental analysis, IR, 1H (13C) NMR and MS, and the molecular structures of ligands L 1 , L 2 were determined by X-ray single crystal analysis. The electrochemical properties of L 1 , L 2 , 1 and 2 demonstrate two or three resolved one-electron redox processes. 相似文献
12.
A. Okruszek J. G. Verkade 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3):235-240
Abstract The syntheses of the P(III) analogues of cyclophosphamide, isophosphamide and triphosphamide are reported. These compounds (4–6, respectively) polymerize easily at room temperature but are sufficiently stable in solution to react with Cl2Pt(NCPh)2, forming cis-Cl2Pt(4)2, cis-Cl2Pt(5)2 and cis-Cl2Pt(6)2 (complexes 9–11, respectively). Complex 10 can also be made by condensing cis-Cl2Pt[ClPN(CH2CH2Cl)CH2CH2CHO]2 with ClCH2CH2NH2, while an alternate route to 9 and 11 is afforded by the condensation of cis-Cl2Pt[Cl2PN(CH2CH2Cl)2]2 with H2NCH2CH2CH2OH and ClCH2CH2NHCH2CH2CH2OH, respectively. Complexes 9–11 exist in two diastereomeric configurations and these can be separated in the cases of 9 and 11 by column chromatography. 31P NMR spectral data for the complexes are discussed and the results of NCl antitumor screening are presented. 相似文献
13.
《Journal of Coordination Chemistry》2012,65(17):3006-3015
Three disulfoxide uranyl complexes [UO2(DBSOB)(NO3)2] n (1), [UO2(DBM)2]2(DBSOB) (2), and [UO2(PMBP)2]2(DBSOB) (3) (DBSOB = 1,4-di(butylsulfinyl)butane, HDBM = dibenzoylmethane, HPMBP = 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone) were synthesized and characterized. The [UO2(NO3)2] groups are connected by bridging disulfoxide ligands DBSOB to form a 1-D zigzag chain in 1. Two [UO2(DBM)2] or [UO2(PMBP)2] groups are connected by a bridging DBSOB to form the dimeric structures of 2 or 3, respectively. Complexes 1, 2, and 3 are the first structurally characterized disulfoxide–actinide compounds. Thermal stabilities of 1, 2, and 3 were investigated. 相似文献
14.
利用3-(2-吡啶基)-1,2,4-三唑配体(HL)和不同的金属盐设计合成了5个配合物[Co(HL)2(H2O)2](NO3)2(1)、[Cu2(L)2(NO3)2(H2O)4] (2)、[Cu2(L)2(AcO)2(H2O)2]·6H2O (3)、[Cu2(L)2(HL)2(ClO4)2]·2CH3CN (4)和[Cd2(L)2(HL)2(NO3)2]·2H2O (5),并通过X射线单晶衍射、红外、元素分析、X射线粉末衍射和热重对配合物结构进行了表征。测试结果表明配合物1具有单核结构,并且可以通过氢键的相互作用形成二维超分子结构。配合物2~5为双核结构。配合物2和5可以通过氢键的相互作用形成二维超分子结构。配合物3通过氢键的相互作用形成三维超分子结构。研究了配合物中HL配体的配位模式。此外,研究了配体HL和配合物1和5的固态荧光性质及荧光寿命。 相似文献
15.
Shan-Shan Zhao Peng Wang Li-Na Wang Lin Fu Xiao-Meng Han 《Journal of Coordination Chemistry》2017,70(5):885-897
The multidentate Schiff-base ligand N′-(1-(pyrazin-2-yl)ethylidene)isonicotinohydrazide (HL) has been prepared. Reaction with zinc, copper, and silver nitrate afford three complexes, [Zn(HL′)2](NO3)2·3H2O (1), {[Cu2(L)2(NO3)(H2O)2]·NO3}n (2) and {[Ag2(L)2]·3H2O}n (3). These complexes have been characterized by elemental analysis, IR spectroscopy, and single-crystal X-ray diffraction. In 1, HL is a neutral tridentate ligand, whereas in 2 and 3, HL is a deprotonated tetradentate ligand. The hydrogen bonding interactions between NO3? and the host framework result in various supramolecular polymeric structures: a 2-D layer for 1 and 3-D network for 2 and 3. The antibacterial activities of these complexes have been investigated and the results indicate that 3 showed good antibacterial activities. 相似文献
16.
《Journal of Coordination Chemistry》2012,65(15):2657-2670
Four alkaline earth metal-organic frameworks, [Mg(H2O)6]?·?(pmtz)2 (1), [Ca(pmtz) 2(H2O)3]?·?H2O (2), [Sr(pmtz)2(H2O)4] (3), and [Ba(pmtz)2(H2O)2]?·?4H2O (4) [pmtz?=?5-(pyrimidyl)tetrazole anion], were synthesized and characterized by elemental analysis, IR spectroscopy, and X-ray crystallography. The crystal structures reveal that 1–3 are mononuclear while 4 displays a 2-D layer structure by bis(bidentate) bridging pmtz?. The luminescence properties of 1–4 were investigated in the solid state at room temperature. 相似文献
17.
A. G. Shipov E. P. Kramarova S. A. Pogozhikh Vad. V. Negrebetskii L. S. Smirnova O. B. Artamkina S. Yu. Bylikin Yu. E. Ovchinnikov Yu. I. Baukov 《Russian Chemical Bulletin》2007,56(3):461-474
New mono-and bis-chelate hypercoordinate silicon complexes containing the monoanionic C,O-chelating 2,2-dimethyl-2,3-dihydrobenzo-1,3-oxazin-3-ylmethyl
(BonCH2) ligand were synthesized starting from 2,2-dimethyl-2,3-dihydrobenzo-1,3-oxazin-4-one (1) through its TMS derivative 2. The reactions of compound 2 with the chlorosilylmethylating agents ClCH2SiMe2Cl, ClCH2SiMeCl2, and (ClCH2)2SiCl2 followed by the transformations of the initially formed chlorosilanes BonCH2SiMe2Cl (3), BonCH2SiMeCl2 (6), and [(BonCH2)2Si(Cl)]+Cl− (8), respectively, into the target products afforded neutral monochelates, viz., monofluoride BonCH2SiMe2F (5) and difluoride BonCH2SiMeF2 (7), and the bis-chelate disiloxane cation-anion complexes {[(BonCH2)2Si]2O}2+·Cl−·ClHCl− (9) and {[(BonCH2)2Si]2O}2+·2TfO− (10). The reaction of ditriflate 10 with boron trifluoride etherate produced fluoride triflate (BonCH2)2Si(F)OTf (11). The X-ray diffraction study of compounds 5, 7, 9, 10, and 11, as well as of NH-heterocycle 1 and disiloxane (BonCH2SiMe2)2O (4) studied earlier, demonstrated that the Si atoms in complexes 5, 7, 9, and 10 are pentacoordinate through the formation of an intramolecular O→Si bond. The coordination of silicon in fluoride triflate
11 can be described as 5+1. In disiloxane 4, one of two Si atoms is pentacoordinate. Dinuclear cation-anion complexes 9 and 10 contain the diastereomeric bis-silylium ions {[(BonCH2)2Si]2O}2+, which differ in the configuration of the chiral bis-chelate fragments (BonCH2)2Si. In complex 9, these fragments have opposite configurations (ΛΔ); in ditriflate 10, the same configurations (ΛΛ).
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 446–458, March, 2007. 相似文献
18.
《Journal of Coordination Chemistry》2012,65(18):3042-3053
We report the synthesis and structures of three copper(I) complexes, [Cu4(μ3-Cl)2(μ2-Cl)2{μ2-(2,6-Me2C6H3N(PPh2)2)}2] (2), [Cu4(μ3-Cl)2(μ2-Cl)2{μ2-(Ph2POPPh2)}2] (4), and [Cu2(μ2-Cl)2(μ2-PPh2OPPh2)(η1-Ph2PP(=O)Ph2)(PPh3)] (5), and one cobalt complex, [(CoCl2){μ2-2,6-Me2C6H3N(PPh2)2}2][CoCl3NH2(2,6-Me2Ph)] (3). Tetra-nuclear copper complex 2 was prepared in good yield by the reaction of bis(diphenylphosphino)-2,6-dimethylaniline [2,6-Me2C6H3N(PPh2)2] (1) with copper(I) chloride along with triphenylphosphine in methanol. Adding a calculated amount of water and dichloromethane mixture (1?:?10) to 2 produced a second tetra-nuclear copper(I) complex, 4, with a P–O–P backbone, along with a small amount of the unsymmetrical copper(I) complex 5. The cobalt complex 3 was obtained by reaction of 1 with cobalt(II) chloride. The solid-state structures of 2–5 were established by single-crystal X-ray diffraction analysis. In the solid state, both 2 and 4 form a tetra-nuclear copper core. In the 31P{1H} NMR study, we observed the conversion of 2, with P–N–P backbone, to 4, with P–O–P backbone. 相似文献
19.
《Journal of Coordination Chemistry》2012,65(22):3556-3567
Three vanadium polymers [V2(µ-OH)2(H2O)2(Hpdc)2] n (1), {[Na2(µ-H2O)2][V2O2(pdc)2]} n (2) and {[K2(µ-H2O)][V2O2(pdc)2]} n (3) (H3pdc?=?3,5-pyrazoledicarboxylate acid) have been hydrothermally synthesized and characterized by spectroscopic methods, magnetic susceptibility measurements and X-ray crystallography. The structure of 1 consists of infinite double-stranded chains. Both 2 and 3 are 3D coordination polymers, featuring ladder-like moieties, made up of [V2O2(pdc)2] subunits, interconnected by pairs of alkali ion chains. Variable-temperature magnetic behavior reveals the existence of antiferromagnetic interactions in 1 and dominant ferromagnetic interactions in 2 and 3. 相似文献
20.
《Journal of Coordination Chemistry》2012,65(6):1077-1083
Reaction of (μ 3-S)FeCo2(CO)9 with N-substituted bis(diphenylphosphanyl)amine Ph2PN(R)PPh2 (R?=?CH2CH2CH3, A; CH2Ph, B) at room temperature in CH2Cl2 afforded dicobalt–iron cluster complexes (μ 3-S)FeCo2(CO)7[Ph2PN(R)PPh2] (R?=?CH2CH2CH3, 1; CH2Ph, 2) in 75% and 66% yields, respectively. 1 and 2 were characterized by elemental analysis and spectroscopy. In addition, the molecular structures of A, 1, and 2 were determined by single crystal X-ray diffraction analysis. 相似文献