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1.
Hsiao‐Fen Wang Kuang‐Hway Yih Weng‐Feng Zeng Shou.‐Ling Huang Gene‐Hsiang Lee 《中国化学会会志》2012,59(8):989-994
Reactions of the thiocarbamoyl‐molybdenum complex [Mo(CO)2(η2‐SCNMe2)(PPh3)2Cl] 1 , and ammonium diethyldithiophosphate, NH4S2P(OEt)2, and potassium tris(pyrazoyl‐1‐yl)borate, KTp, in dichloromethane at room temperature yielded the seven coordinated diethyldithiophosphate thiocarbamoyl‐molybdenum complexe [Mo(CO)2{η2‐S2P(OEt)2}(η2‐SCNMe2)(PPh3)] β‐3 , and tris(pyrazoyl‐1‐yl)borate thiocabamoyl‐molybdenum complex [Mo(CO)2(η3‐Tp)(η2‐SCNMe2)(PPh3)] 4 , respectively. The geometry around the metal atom of compounds β‐3 and 4 are capped octahedrons. The α‐ and β‐isomers are defined to the dithio‐ligand and one of the carbonyl ligands in the trans position in former and two carbonyl ligands in the trans position in later. The thiocabamoyl and diethyldithiophosphate or tris(pyrazoyl‐1‐yl)borate ligands coordinate to the molybdenum metal center through the carbon and sulfur and two sulfur atoms, or three nitrogen atoms, respectively. Complexes β‐3 and 4 are characterized by X‐ray diffraction analyses. 相似文献
2.
Three new triruthenium clusters, Ru3(CO)9(μ‐arphos)AsPh3 ( 1 ), Ru3(CO)9(μ‐arphos)As(m‐C6H4Me)3 ( 2 ), and Ru3(CO)9(μ‐arphos)As(p‐C6H4Me)3 ( 3 ) were synthesized via thermal reactions of Ru3(CO)10(μ‐arphos) with different tertiary arsine ligands [AsPh3, As(m‐C6H4Me)3, As(p‐C6H4Me)3]. All these complexes were fully characterized by elemental analysis, FT‐IR, NMR spectroscopy, and single‐crystal X‐ray diffraction. 相似文献
3.
Single crystals of [Be3(μ3‐O)3(MeCN)6{Be(MeCN)3}3](I)6·4CH3CN ( 1 ·4CH3CN) were obtained in low yield by the reaction of beryllium powder with iodine in acetonitrile suspension, which probably result from traces of beryllium oxide containing the applied beryllium metal. The compound 1 ·4CH3CN forms moisture sensitive, colourless crystal needles, which were characterized by IR spectroscopy and X‐ray diffraction (Space group Pnma, Z = 4, lattice dimensions at 100(2) K: a = 2317.4(1), b = 2491.4(1), c = 1190.6(1) pm, R1 = 0.0315). The hexaiodide complex cation 1 6+consists of a cyclo‐Be3O3 core with slightly distorted chair conformation, stabilized by coordination of two acetonitrile ligands at each of the beryllium atoms and by a {Be(CH3CN)3}2+ cation at each of the oxygen atoms. This unique coordination behaviour results in coplanar OBe3 units with short Be–O distances of 155.0 pm and 153.6 pm on average of bond lengths within the cyclo‐Be3O3 unit and of the peripheric BeO bonds, respectively. Exposure of compound 1 ·4CH3CN to moist air leads to small orange crystal plates of [Be(H2O)4]I2·2CH3CN ( 3 ·2CH3CN). According to the crystal structure determination (Space group C2/c, Z = 4, lattice dimensions at 100(2) K: a = 1220.7(1), b = 735.0(1), c = 1608.5(1) pm, β = 97.97(1)°, R1 = 0.0394), all hydrogen atoms of the dication [Be(H2O)4]2+ are involved to form O–H ··· N and O–H ··· I hydrogen bonds with the acetonitrile molecules and the iodide ions, respectively. Quantum chemical calculations (B3LYP/6‐311+G**) at the model [Be3(μ3‐O)3(HCN)6{Be(HCN)3}3]6+ show that chair and boat conformation are stable and that the distorted chair conformation is stabilized by packing effects. 相似文献
4.
The η2‐thio‐indium complexes [In(η2‐thio)3] (thio = S2CNC5H10, 2 ; SNC4H4, (pyridine‐2‐thionate, pyS, 3 ) and [In(η2‐pyS)2(η2‐acac)], 4 , (acac: acetylacetonate) are prepared by reacting the tris(η2‐acac)indium complex [In(η2‐acac)3], 1 with HS2CNC5H10, pySH, and pySH with ratios of 1:3, 1:3, and 1:2 in dichloromethane at room temperature, respectively. All of these complexes are identified by spectroscopic methods and complexes 2 and 3 are determined by single‐crystal X‐ray diffraction. Crystal data for 2 : space group, C2/c with a = 13.5489(8) Å, b = 12.1821(7) Å, c = 16.0893(10) Å, β = 101.654(1)°, V = 2600.9(3) Å3, and Z = 4. The structure was refined to R = 0.033 and Rw = 0.086; Crystal data for 3 : space group, P21 with a = 8.8064 (6) Å, b = 11.7047 (8) Å, c = 9.4046 (7) Å, β = 114.78 (1)°, V = 880.13(11) Å3, and Z = 2. The structure was refined to R = 0.030 and Rw = 0.061. The geometry around the metal atom of the two complexes is a trigonal prismatic coordination. The piperidinyldithiocarbamate and pyridine‐2‐thionate ligands, respectively, coordinate to the indium metal center through the two sulfur atoms and one sulfur and one nitrogen atoms, respectively. The short C‐N bond length in the range of 1.322(4)–1.381(6) Å in 2 and C‐S bond length in the range of 1.715(2)–1.753(6) Å in 2 and 3 , respectively, indicate considerable partial double bond character. 相似文献
5.
Mohammad Kazem Rofouei Zahra Ghalami Dr. Jafar Attar Gharamaleki Vanik Ghoulipour Giuseppe Bruno Hadi Amiri Rudbari 《无机化学与普通化学杂志》2012,638(5):798-803
The title ligand, [1‐(2‐methoxyphenyl)‐3‐(4‐chlorophenyl)]triazene, H L ( 1 ), was prepared. In a reaction with Hg(NO3)2 it forms the complex [Hg(C26H22Cl2N6O2)], [Hg L 2] ( 2 ). Both compounds were characterized by means of X‐ray crystallography, CHN analysis, FT‐IR, 1H NMR, and 13C NMR spectroscopy. In the structure of compound 1 , two independent fragments are present in the unit cell. They exhibit trans arrangement about the –N=N– double bond. The dihedral angles between two benzene rings in both fragments are 4.36 and 18.79 Å, respectively. Non‐classic C–H ··· N hydrogen bonding and C–H ··· π interactions form a layer structure along the crystallographic ab plane [110]. In compound 2 , the HgII atom is hexacoordinated by two tridentate [1‐(2‐methoxyphenyl)‐3‐(4‐chlorophenyl)]triazenide ligands through a N2O2 set. In addition, in the structure of 2 , monomeric complexes are connected to each other by C–H ··· π stacking interactions, resulting in a 2D architecture. These C–H ··· π edge‐to‐face interactions are present with H ··· π distances of 3.156 and 3.027 Å. The results of studies of the stoichiometry and formation of complex 2 in methanol solution were found to support its solid state stoichiometry. 相似文献
6.
Single crystals of Sr[B(C6H5O7)2](H2O)4 · 3H2O, a new borate‐citrate material, were grown with sizes up to 8 × 6 × 2 mm by slow evaporation of water at room temperature. The structure of Sr[B(C6H5O7)2](H2O)4 · 3H2O was determined by single‐crystal X‐ray diffraction. It crystallizes in the monoclinic space group P21/c, with a = 11.363(3) Å, b = 18.829(4) Å, c = 11.976(3) Å, β = 110.736(3)°, and Z = 4. The SrO8 dodecahedra, BO4 tetrahedra and citrate groups are linked together to form chains. The compound was characterized by IR and UV/Vis/NIR transmittance spectroscopy as well as thermal analysis. 相似文献
7.
Syntheses and Crystal Structures of [μ‐(Me3SiCH2Sb)5–Sb1,Sb3–{W(CO)5}2] and [{(Me3Si)2CHSb}3Fe(CO)4] – Two Cyclic Complexes with Antimony Ligands cyclo‐(Me3SiCH2Sb)5 reacts with [(THF)W(CO)5] (THF = tetrahydrofuran) to form cyclo‐[μ‐(Me3SiCH2Sb)5–Sb1,Sb3–{W(CO)5}2] ( 1 ). The heterocycle cyclo‐ [{(Me3Si)2CHSb}3Fe(CO)4] ( 2 ) is formed by an insertion reaction of cyclo‐[(Me3Si)2CHSb]3 and [Fe2(CO)9]. The crystal structures of 1 and 2 are reported. 相似文献
8.
Christian Fischer Anja König Hans‐Joachim Drexler Prof. Dr. Detlef Heller 《无机化学与普通化学杂志》2012,638(6):905-906
Three new, hitherto unknown, rhodium complexes with aniline and two of its derivatives (2, 6‐dimethylaniline and N‐methylaniline) are presented. All complexes have been characterized by X‐ray analysis. 相似文献
9.
Christian Fischer Carmen Selle Hans‐Joachim Drexler Prof. Dr. Detlef Heller 《无机化学与普通化学杂志》2012,638(6):907-908
Two novel BINAP rhodium complexes containing η6‐coordinated arenes have been disclosed. Both have been characterized by X‐ray analysis and NMR spectroscopy. 相似文献
10.
Yizheng Geng Junyu Chen Haiwei Zhao Hongjian Sun Benjing Xue Xiaoyan Li Olaf Fuhr Dieter Fenske 《无机化学与普通化学杂志》2017,643(11):712-716
Three η4‐(C=C–C=O) coordination cobalt(I) complexes 1 – 3 were synthesized by the reactions of cinnamaldehyde, p‐fluorocinnamaldehyde, and p‐chlorocinnamaldehyde with CoMe(PMe3)4. Complex 4 as η2‐(C=C) coordination was prepared by the reaction of chalcone with Co(PMe3)4. The structures of complexes 1 – 4 were confirmed by single‐crystal X‐ray diffraction. Although the reactions didn't undergo C–H bond activation and decarbonylation, the formation of complexes 1 – 4 deepens our understanding of the reactions between α,β‐unsaturated aldehyde or ketone with low‐valent central cobalt atom. 相似文献
11.
Treatment of Pd(PPh3)4 with 5‐bromo‐pyrimidine [C4H3N2Br] in dichloromethane at ambient temperature cause the oxidative addition reaction to produce the palladium complex [Pd(PPh3)2(η1‐C4H3N2)(Br)], 1 , by substituting two triphenylphosphine ligands. In acetonitrile solution of 1 in refluxing temperature for 1 day, it do not undergo displacement of the triphenylphosphine ligand to form the dipalladium complex [Pd(PPh3)Br]2{μ,η2‐(η1‐C4H3N2)}2, or bromide ligand to form chelating pyrimidine complex [Pd(PPh3)2(η2‐C4H3N2)]Br. Complex 1 reacted with bidentate ligand, NH4S2CNC4H8, and tridentate ligand, KTp {Tp = tris(pyrazoyl‐1‐yl)borate}, to obtain the η2‐dithiocarbamate η1‐pyrimidine complex [Pd(PPh3)(η1‐C4H3N2)(η2‐S2CNC4H8)], 4 and η2‐Tp η1‐pyrimidine complex [Pd(PPh3)(η1‐C4H3N2)(η2‐Tp)], 5 , respectively. Complexes 4 and 5 are characterized by X‐ray diffraction analyses. 相似文献
12.
Coordination Chemistry of P‐rich Phosphanes and Silylphosphanes. XVII [1] [Co(g5‐Me5C5)(g3‐tBu2PPCH–CH3)] from [Co(g5‐Me5C5)(g2‐C2H4)2] and tBu2P–P=P(Me)tBu2 [Co(η5‐Me5C5)(η3‐tBu2PPCH–CH3)] 1 is formed in the reaction of [Co(η5‐Me5C5)(η2‐C2H4)2] 2 with tBu2P–P 4 (generated from tBu2P–P=P(Me)tBu2 3 ) by elimination of one C2H4 ligand and coupling of the phosphinophosphinidene with the second one. The structure of 1 is proven by 31P, 13C, 1H NMR spectra and the X‐ray structure analysis. Within the ligand tBu2P1P2C1H–CH3 in 1 , the angle P1–P2–C1 amounts to 90°. The Co, P1, P2, C1 atoms in 1 look like a „butterfly”︁. The reaction of 2 with a mixture of tBu2P–P=P(Me)tBu2 3 and tBu–C?P 5 yields [Co(η5‐Me5C5){η4‐(tBuCP)2}] 6 and 1 . While 6 is spontaneously formed, 1 appears only after complete consumption of 5 . 相似文献
13.
Tetra(N,N′‐tetramethylurea)‐beryllium‐triiodide, [Be(TMU)4](I3)2 ( 1 ) was prepared from beryllium powder and iodine in N,N′‐tetramethylurea to give orange crystals, which were characterized by X‐ray diffraction and IR spectroscopy. Compound 1 crystallizes monoclinically in the space group C2/c with four formula units per unit cell. Lattice dimensions at 100(2) K: a = 1906.6(1), b = 1185.7(1), c = 1895.0(1) pm, β = 113.60(1) °, R1 = 0.0291. The structure of 1 consists of distorted tetrahedral cations [Be(TMU)4]2+ with Be–O bond lengths of 162.5(5) and 160.8(5) pm and triiodide ions without site symmetry. 相似文献
14.
15.
Adina Rotar Markus Schürmann Richard A. Varga Cristian Silvestru Klaus Jurkschat Prof. Dr. 《无机化学与普通化学杂志》2008,634(9):1533-1536
Single‐crystal X‐ray diffraction analysis of [2,6‐(Me2NCH2)2C6H3]2SnF2 reveals that only one of the two dimethylaminomethyl groups of each pincer‐type ligands [2,6‐(CH2NMe2)2C6H3]? is coordinated to the tin atom at Sn‐N distances of 2.576(2) and 2.470(2) Å, inducing chirality of the latter. The tin atom exhibits a distorted octahedral trans(C,C)cis(N,N)cis(F,F) configuration. Extensive intra‐ and intermolecular C‐H···F hydrogen bonding is observed with the latter giving rise to formation of polymeric chains. 相似文献
16.
The synthesis and structural characterization of two azirine rhodium(III ) complexes are described. The stabilization, N‐coordination and phenylgroup π‐stacking of the highly reactive and strained 3‐phenyl‐2H‐azirine by transition metal coordination is observed. The reaction of the dimeric complex [(η5‐C5Me5)RhCl2]2 with 3‐phenyl‐2H‐azirine (az) in CH2Cl2 at room temperature in a 1:2 molar ratio afforded the neutral mono‐azirine complex [(η5‐C5Me5)RhCl2(az)]. The subsequent reaction of [(η5‐C5Me5)RhCl2]2 with six equivalents of az and 4 equivalents of AgOTf yielded the cationic tris‐azirine complex [(η5‐C5Me5)Rh(az)3](OTf)2. After purification, all complexes have been fully characterized. The molecular structures of the novel rhodium(III ) complexes exhibit slightly distorted octahedral coordination geometries around the metal atoms. 相似文献
17.
π‐Allyl (η3‐C3H5), a four‐electron donor, was used as a ligand model to replace η5‐C5Me4SiMe3 in DFT calculations on the tetranuclear yttrium polyhydrido complex (η5‐C5Me4SiMe3)4Y4H8 containing a Y4H8 tetrahedral core structure, which may separate the four π‐allyl groups and hence suppress the allyl ligand coupling during the computation. In terms of the calculated core geometry, isomerization energy barrier, charge population, and frontier orbital features of the complex, the η3‐C3H5 ligand model is comparable to η5‐C5H5. © 2006 Wiley Periodicals, Inc. Int J Quantum Chem, 2007 相似文献
18.
The mononuclear complex, [NiCl2 (trzCH2CH2COPh)4]·6H2O (trz =1,2,4‐triazole), was synthesized and its structure was determined by single crystal X‐ray determination. It crystallizes in the monoclinic system, space group P21/c, with lattice parameters: a = 0.80391(2) nm, b = 1.08215(2) tun, c = 2.90133(2) nm, β = 94.792 (1)° and Z = 2. Each nickel atom is coordinated by four N atoms of triazole from four β‐(1,2,4‐triazole‐1‐yl)propiophenone ligands and two chloride anions in trans arrangement with octahedral coordination geometry. In addition to the coordinating nickel complex, there are six uncoordinated water molecules. The Ni‐Cl distance is 0.24865(8) nm and the Ni‐N distances are in the range of 0.2072(2) to 0.2099(2) nm, respectively. In the solid state, the title compound forms three dimensional network structure through hydrogen bonds. The intermolecular hydrogen bonds connect the [NiCl2(C2H2N3CH2CH2COPh)4] and H2O moieties. The deep green crystals were also examined by elemental analysis, FT‐IR and UV spectra, which are in agreement with the structural data. 相似文献
19.
The reaction of the thiocarbamoyl‐molybdenum complex [Mo(CO)2(η2‐SCNMe2)(PPh3)2Cl] 1 , with EtOCS2K and C4H8NCS2NH4 in dichloromethane at room temperature yielded the seven coordinated ethyldithiocarbonate thiocarbamoyl‐molybdenum complex [Mo(CO)2(η2‐S2COEt)(η2‐SCNMe2)(PPh3)] 2 , and the dithiocarbamate thiocarbamoyl‐molybdenum complex [Mo(CO)2(η2‐S2CNC4H8)(η2‐SCNMe2)(PPh3)] 3 . The geometry around the metal atom of compounds 2 and 3 are capped octahedrons as revealed by X‐ray diffraction analyses. The thiocarbamoyl and ethyldithiocarbonate or pyrrolidinyldithiocarbamate ligands coordinate to the molybdenum metal center through the carbon and sulfur and two sulfur atoms, respectively. Structure parameters, NMR, IR and Mass spectra are in agreement with the crystal chemistry of the two compounds. 相似文献
20.
Dr. Eberhardt Herdtweck Tobias Kornprobst Roland Sieber Leo Straver Johann Plank 《无机化学与普通化学杂志》2011,637(6):655-659
From hydrothermal synthesis needle‐shaped crystals of [Ca3(C6H5O7)2(H2O)2] · 2H2O were obtained. The crystal structure was determined by single‐crystal X‐ray experiments and confirmed by powder data (P$\bar{1}$ (no. 2) a = 5.9466(4), b = 10.2247(8), c = 16.6496(13) Å, α = 72.213(7)°, β = 79.718(7)°, γ = 89.791(6)°, V = 947.06(13) Å3, Z = 2, R1 = 0.0426, wR2 = 0.1037). The structure was obtained from pseudo merohedrically polysynthetic twinned crystals using a combined data collection approach and refinement processes. The observed three‐dimensional network is dominated by eightfold coordinated Ca2+ cations linked by citrate anions and hydrogen bonds between two non‐coordinating crystal water molecules and two coordinating water molecules. 相似文献