Synthesis of molybdenum complexes containing η3-bonded trans-butadienyl ligands: crystal structure of[Mo(2,2′-bipyridine)(CO)2-

Reaction of Ph₄P[Mo(2,2′-bipyridine)Cl(CO₃] with 1,4-dichlorobut-2-yne in the presence of primary or secondary aliphatic amines gives high yields of neutral molybdenum complexes containing 2-substituted η³-bonded trans-butadienyl ligands. The crystal structure of the perfluorocarboxylate derivative [Mo(2,2′-bipyridine)(CO)₂(η³-CH₂C(CONHMe)CCH₂) (O₂CC₃F₇] has been determined.     

Synthesis,characterization, and crystal structure determination of two mercury(II) dimer complexes with 4,7-diphenyl-1,10-phenanthroline, 5,5′-dimethyl-2,2′-bipyridine and bromide

Mercury(II) complexes, {[Hg(Ph₂phen)(μ-Br)]₂Br₂} · CH₃CN (1) and {[Hg(dmbpy)(µ-Br)]₂Br₂}(2) (where Ph₂phen is 4,7-diphenyl-1,10-phenanthroline and dmbpy is 5,5′-dimethyl-2,2′-bipyridine), were synthesized from reaction of HgBr₂ with Ph₂phen and dmbpy in CH₃CN and CH₃OH. Both complexes were thoroughly characterized by elemental analysis, infrared, ¹H and ¹³C NMR spectroscopy and single-crystal X-ray diffraction. Complexes 1 and 2 crystallize in the space group P2₁/n of the monoclinic and P 1 of the triclinic systems and contain four and one molecules per unit cell, respectively. The unit cell dimensions for 1 are: a = 20.422(4) Å, b = 11.384(2) Å, c = 20.665(4) Å, and β = 109.94(3)° and for 2 are: a = 8.7470(17) Å, b = 8.8328(18) Å, c = 9.4950(19) Å and α = 75.47(3)°, β = 82.21(3)°, γ = 85.56(3)°. According to X-ray structure determination both complexes are five coordinate with three bromides and one bidentate ligand; one bromide is set at a semi-bridging position.     

Synthesis and crystal structure of dinuclear nickel (Ⅱ) complex

The crystal structure of Ni(Ⅱ) complex with 3-hydroxyl-1, 5-diazacycloheptane-N, N'-diacetate was determined by X-ray diffraction method. Crystal data for Ni2 (C9H14N2O5)2·2H2O: monoclinic, space group P21/n, a = 1.1717(5), b = 0.9794(3), c = 1.2971(2) nm, β= 96.62(3), V= 1.4786(7) nm3, Dc = 1.377 g/cm3, Z = 2,μ=13.321 cm-1 (Mo-Kα), F(000)=640. The final R and Rw are 0.075 and 0.089 respectively. The Ni(Ⅱ) ion forms 2:2 complex with ligand. Two ligands are bridged by two Ni(Ⅱ) atoms which are bridged by two O atoms. Every Ni(Ⅱ) is coordinated by two N atoms and four 0 atoms. The coordination polyhedron of the Ni(Ⅱ) ion is a distorted octahedron.     

Synthesis and structure of the first molybdenum compound of N,O,N-hydroxybis(2-pyridyl)methanolato (η 3-dpkO,OH). The structure of [Mo(O)2(μ-O)(η 3-dpkO,OH)]2 · 2dmso

When di-2-pyridyl ketone (dpk) was allowed to react with [Mo(CO)₆] in toluene under reflux in air [Mo(O)₂(μ-O)(η ³-dpkO,OH)]₂ where η ³-dpkO,OH is N,O,N-hydroxybis(2-pyridyl)methanolato was isolated. Infrared and ¹H-NMR spectral data measured on solutions of the isolated compound indicate the absence of the carbonyl groups and the presence of coordinated η ³-dpkO,OH, terminal and bridging oxo-groups and elemental analysis confirmed the formulation of the product as [Mo(O)₂(μ-O)(η ³-dpkO,OH)]₂. Crystals of [Mo(O)₂(μ-O)(η ³-dpkO,OH)]₂·2dmso obtained from a dimethyl sulfoxide (dmso) solution of [Mo(O)₂(μ-O)(η ³-dpkO,OH)]₂ are in the monoclinic P2₁/c space group. X-ray structural analysis confirmed the identity of [Mo(O)₂(μ-O)(η ³-dpkO,OH)]₂ and shows a dioxomolybdenum oxo-bridged dimer with two terminal oxygen atoms and one tridentate N,O,N-dpkO,OH occupying the coordination sites of the high-valent molybdenum(VI) in a pseudo-octahedral coordination geometry. The molecular packing shows parallel stacks of [Mo(O)₂(μ-O) (η ³-dpkO,OH)]₂·2dmso and disclose an extensive network of non-covalent interactions within each stack.     

Synthesis and crystal structure of [(η3-C3H5)(CO)2Mo(μ-S2CPCy3)-Mo(η3-CH2CMeCH2)(CO)2]

A novel dimolybdenum complex [(³-C₃H₅)(CO)₂Mo(-S₂CPCy₃)Mo(³-CH₂CMeCH₂)(CO)₂], obtained by reacting the [(CO)₂(³-C₃H₅)Mo(-S₂CPCy₃)Mo(CO)₃]^– anion with an excess of ClCH₂CMe=CH₂, has been characterized by i.r., ³¹P{¹H}, ¹H- and ¹³C-n.m.r. spectroscopy and by elemental analysis. The crystal structure of the complex, determined by X-ray diffraction, shows a definite preference for the central carbon of the S₂CPCy₃ bridge to bind to the Mo(2) atom coordinated by ³-2-methylallyl, rather than the Mo(1) atom attached to unsubstituted ³-allyl ligand.     

Synthesis and characterisation of [AgL(μ-PR2)M(CO)5], L= 1,10-phenanthroline or tricyclohexylphosphine; M = Cr,Mo, W

The new heterobimetallic phosphide-bridged compounds [AgL(μ-PR₂)M(CO)₅], (L = 1,10-phenanthroline or tricyclohexylphosphine: M = Cr, M, W) have been prepared from AgO₃SCF₃, M(CO)₅PR₂H and the ligand L in the presence of Et₂NH or MeO⁻ as base, and characterized by ³¹P NMR spectroscopy.     

Synthesis, Structure and DFT Investigation into a Copper(Ⅱ) Compound Consisting of 4,7-diphenyl-1,10-phentheanthroline

The copper(Ⅱ) DPP adduct Cu(DPP)(DMF)2(H2O)·(ClO4)2 1 (DPP = 4,7-diphenyl-1, 10-phentheanthroline, DMF = N,N'-dimethyl formamide) has been prepared by a direct synthetic method and structurally characterized. It presents a mononuclear structure and crystallizes in triclinic, space group P with a = 9.8717(2), b = 12.579, c = 14.7574(2)(A), α = 67.976(6), β = 82.031(9), γ = 80.343(9)o, V = 1668.96(9) (A)3, Z = 1, Dc = 1.495 g/cm3, μ(MoKα) = 0.877 mm-1, F(000) = 774, C60H64Cl4Cu2N8O21, Mr = 1502.09, the final R1 = 0.0643 and Wr2 = 0.1799 for 6153 observed reflections with I > 2σσI). Structure analysis shows that copper atom presents an unusual five- coordination of square pyramid geometry. The whole structure is stabilized by π-π stacking inter- actions and static attractive forces from [ClO4]- anions. Based on crystal data, quantum chemistry calculation on DFT/B3LPY level was used to reveal the electronic structure of 1.     

Synthesis and crystal structure of a heterodinuclear complex with a bridged ethenyl ligand FeCo(CO)7(μ-CH=CPhH)

[Fe₂(CO)₆(μ-CO)(μ-CHCPhH)]⁻ reacts with Co₂(CO)₈ at room temperature to give the neutral heterodinuclear complex FeCo(CO)₇(μ-CHCPhH), which has been characterized by elemental analysis and spectroscopic (mass, IR and ¹H NMR) methods and by determination of its structure by X-ray diffraction.     

Synthesis,crystal structure,and characterization of energetic complex Pb(ATZ)(phen)2 · 3H2O

A new energetic complex, Pb(ATZ)(phen)₂·3H₂O (1) (ATZ = 5,5′-azotetrazolate), was synthesized and characterized by single crystal X-ray diffraction. Crystal data: monoclinic, P2(1)/n space group, a = 8.4545(1) Å, b = 25.846(2)Å, c = 13.096(2)Å, and β = 102.873(2)°. In addition, elemental analysis, IR, and thermogravimetric analysis are presented. Furthermore, the complex was also explored as an additive to promote thermal decomposition of ammonium perchlorate.     

Synthesis and crystal structure of (E)-[(2-cyclohexenyl) vinyl]triaryltin

(E)-[(2-Cyclohexenyl)vinyl]triaryltin (aryl=phenyl, p-tolyl) were synthesized and characterized by elemental analysis, IR, 1H NMR spectroscopy. The crystal structure of (E)-[(2-cyclohexenyl)vinyl]triphenyltin was also determined by the X-ray diffraction. Experiments show that this compound has the conjugated system, which makes it have possible bioactivity and anti-tumor activity.     

Synthesis, Structure and DFT Investigation into a Copper(II) Compound Consisting of 4,7-diphenyl-1,10-phentheanthroline

1 INTRODUCTION terested in the unique effects associated with substituents at 4- and 7-positions of the phenan- The coordination chemistry of 1,l0-phenanthroline throline ring. Thus, when phenyl groups are present, and its derivatives has captured the attention of che- the absorptivities of the CT transitions are increased mists for years. The reports on biological importance[1~4], markedly due to the extension of the dipole moment supramolecular chemistry[5], electronic spectra[6], conne…     

Novel di-μ-chloro-bis[chloro(4,7-dimethyl-1,10-phenanthroline)cadmium(II)] dimer complex: synthesis, spectral, thermal, and crystal structure studies

A novel di-μ-chloro-bis[chloro(4,7-dimethyl-1,10-phenanthroline)cadmium(II)] dimer complex has been prepared by reacting CdCl₂·2.5H₂O with 4,7-dimethyl-1,10-phenanthroline (dmphen) ligand. The complex was characterized on the basis of elemental analysis, FAB-MS, IR, UV–visible, ¹H, and ¹³C NMR spectroscopy, TG/DTA, and X-ray single-crystal diffraction studies. The Cd(II) ions in [CdCl₂(C₁₄H₁₂N₂)]₂ are coordinated to three Cl atoms with the centrosymmetric dimer bridged through the Cl atoms and two N atoms in a slightly distorted square-pyramidal disposition. Several hydrogen bonds formed between the terminal Cl atoms and H-Me/H-Ph groups may stabilize the structure in the dimer form.     

A novel interpenetrating 2-D brush-like structure: hydrothermal synthesis and crystal structure of [Cu(phen)V4O10]∞ (phen=1,10-phenanthroline)

A novel vanadium oxide, [Cu(phen)V₄O₁₀]_∞ (1), has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, IR, EPR spectroscopy and thermal analysis. The compound crystallizes in monoclinic structure of P2₁/m with a=7.4169(10) Å, b=10.0460(13) Å, c=11.0845(15) Å, β=102.520(2)°, V=806.27(19) Å³ and Z=2.     

Synthesis,crystal structure and magnetic properties of [1-(4′-bromobenzyl)-4-methylquinolinium] [Ni(mnt)2] complex (mnt2 − =maleonitriledithiolate)

A new ion-pair complex, [BrBzMeQl][Ni(mnt)₂] (1) ([BrBzMeQl]⁺?=?1-(4′-bromobenzyl)-2-methylquinolinium; mnt^2??=?maleonitriledithiolate), has been prepared and characterized. X-ray diffraction analysis shows that the Ni(mnt)₂ anion and [BrBzMeQl]⁺ cations of 1 form completely segregated stacking columns, with the Ni?···?Ni distances alternating between 3.717 and 4.466?Å?in the Ni(mnt)₂ stacking column. The variable-temperature magnetic susceptibilities of 1 have been measured over the range 75–300?K and the results reveal that the complex exhibits antiferromagnetic behavior.     

Synthesis, crystal structure, and spectral studies of the molecular complex of [60]fullerene with chloro(triphenylphosphine)gold(I), C60·2[(Ph3P)AuCl]

The molecular complex C₆₀·2[(Ph₃P)AuCl] (1) was synthesized. The crystal and molecular structure of1 was established by X-ray diffraction analysis. At room temperature, the [60]fullerene molecules in complex1 are ordered due to π—π interactions between C₆₀ and the phenyl rings of the chloro(triphenylphosphine)gold(1) molecules. The satellite structure, which accompanies the Cls photoelectron peak of complex1, is indicative of a partial suppression of a channel of losses due to π→π transition in the phenyl ring. The 1R spectral data indicate that either a charge is absent or the charge transfer to the fullerene molecule is negligible. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 365–369, February, 2000.     

Effects of Processing Temperature on the Oxygen Quenching Behavior of Tris(4,7′-diphenyl-1,10′-phenanthroline) Ruthenium (II) Sequestered Within Sol-Gel-Derived Xerogel Films

Sol-gel processing methods offer novel pathways for tailoring glasses. Amongst the issues that have received the least attention are the effects of the curing temperature on the behavior and photophysics of a dopant molecule sequestered within a sol-gel-derived xerogel. Of particular interest to our group are the effects of processing variables on the ability of a dopant molecule, that is sequestered within a xerogel glass, to be accessed by an analyte and the distribution of the dopant sites within the xerogel. The thermal stability of the luminophore tris(4,7-diphenyl-1,10-phenanthroline) ruthenium (II) ([Ru(dpp)₃]²⁺) provides a convenient way to address these issues and develop an understanding of how one might best exploit curing temperature to construct improved chemical sensors. This paper focuses on quantifying how the film curing temperature affects the spectroscopy and O₂ quenching of ([Ru(dpp)₃]²⁺) sequestered within sol-gel-derived xerogel thin films. Our quenching data on films once they have been cured demonstrate that there is a dramatic increase in the sensitivity of the ([Ru(dpp)₃]²⁺) molecules to O₂ quenching when the films have been cured at elevated temperatures. This arises primarily because there are two main types of ([Ru(dpp)₃]²⁺) microenvironments within the glass and higher temperature curing leads to an increase in the bimolecular quenching rate between O₂ and ([Ru(dpp)₃]²⁺). This is accomplished as follows. Below a curing temperature of 100–150°C, 15% of the xerogel-doped ([Ru(dpp)₃]²⁺) molecules are not accessed to any detectable degree by the O₂ molecules during the ([Ru(dpp)₃]²⁺) excited-state luminescence lifetime. However, as the xerogel is cured at or above 150°C, residual silanol-bound waters (or other impurities) dissociate from the xerogel and those ([Ru(dpp)₃]²⁺) molecules that were initially inaccessible become accessible to O₂. The dissociation of these water molecules, plus other events, also causes the originally inaccessible ([Ru(dpp)₃]²⁺) population to ultimately exhibit a quenching rate that is greater than the fraction of initially accessible ([Ru(dpp)₃]²⁺) molecules that were formed under ambient curing conditions.     

Synthesis,crystal structure,and magnetic properties of a new end-to-end thiocyanato-bridged dicobalt(II) complex CoII(dien)(H2O)(NCS)(μ1,3-NCS)CoII(dien)(NCS)2 (dien = diethylenetriamine)

Synthesis, characterization, crystal structure, and magnetic properties of the first single µ_1,3-thiocyanato-bridged dicobalt(II) compound, [Co^II(dien)(H₂O)(NCS)(µ_1,3-NCS)Co^II(dien)(NCS)₂] (1; dien = diethylenetriamine), are described. In 1, cobalt(II) is six coordinate with distorted-octahedral geometry. The Co(1) ··· Co(2) distance is 5.99 Å. The magnetic properties of 1 have been investigated by variable-temperature magnetic susceptibility measurements. The metal centers are coupled by weak ferromagnetic interaction (J = 1.14 cm^?1). The structure and magnetic properties are compared with related thiocyanate-bridged compounds.     

Unexpected preparation and X-ray crystal structure of the dinuclear complex Mo2(μ-P(O)(OCH3)2)2(CO)4(P(OCH3)3)2(CF3COO)2

Prolonged reaction of CF₃COOH with Mo(CO)₃(P(OCH₃)₃)₃ in CH₂Cl₂ yields the dimer [Mo(CO)₂(μ(O)P(OCH₃)₂)P(OCH₃)₃CF₃COO]₂ in low yield. The complex has been characterized by the usual spectroscopic methods and by an X-ray crystal structure determination. The molybdenum atoms are linked by two OP bridges, the six-membered dimetallacycle adopting a twisted-boat conformation. Each molybdenum is seven-coordinated and has a capped trigonal prism geometry, the capping position being occupied by an oxygen atom of the bridging OP(OCH₃)₂ group. A mechanism similar to the well-known Michaelis-Arbuzov rearrangement is proposed and substantiated by the concomitant apparition of CF₃COOCH₃ during the reaction.     

Carbene complexes of molybdenum and tungsten Et3E-CH=M(NAr)(OR)2 (M = Mo, W; E = Si, Ge) and π-complex of molybdenum (RO)2(ArN)Mo(CH2=CH-GeEt3). Synthesis and catalytic properties

The heteroelement-containing alkylidene imide complexes with molybdenum and tungsten Et₃SiCH=Mo(NAr)(OR)₂ (I), Et₃ ECH=W(NAr)(OR)₂ (E = Si (II), Ge (III); Ar = 2,6-i-Pr₂C₆H₃; R=CMe₂ CF₃) and π-complex (RO)₂(ArN)Mo(CH₂=CH-GeEt₃) (IV) were synthesized by the reaction of Alkyl-CH=M(NAr) (OR)₂ (M=Mo, W; Alkyl = t-Bu, PhMe₂C) with organosilicon and organogermanium vinyl reagents Et₃ECH=CH₂ (E = Si, Ge). The structure of compounds I–III was determined by X-ray diffraction (XRD). The complexes I–IV are active initiators of metathesis polymerization of cycloolefins.     

Crystal Structure of 〔Aqua(oxalato)(1,10-phenanthroline)(H_2O)〕copper(Ⅱ) Monohydrate

1INTRODUCTIONThemixeda,a'-diimineandoxygendonorligandsofcopper(n)complexesareknowntobepossiblemodelsforenzyme~metalion-substrateandundernumerousin-vestigationst".Themixedoxalato2,2'-bipyridylcomplexesofcopper(I)havebeenwellcharacterizedL2j.Herebywereportthecrystalstructureofits1,lO-phenanthro-lineanalogue.2EXPERIMENTALThetitlecomplexwaspreparedbymixingCuCl,.2H,O,1,lO-phenanthrolineandH,C,o'inmethanol-water(1:lv/v)intheratio1:1:l.Afewdropsoftri-ethylaminewereaddedandtheresultingmi…