Synthesis and Liquid Crystal Properties of Transition Metal Complexes of Mesotetra （4-n-myristyloxyphenyl） porphyrin

Transition metal complexes of meso-tetra (4-myristyloxyphenyl)porphyrin TMPPM′ [M′=Mn, Fe, Co, Ni, Cu, Zn ; TMPP=mesotetra (4-myristyloxyphenyl)porphyrin] have been synthesized and characterized by means of elemental analyses, UV-Vis spectra, infrared photoacoustic spectra, ^1H NMR spectra, molar conductance and differential scanning calorimetry(DSC). The ligand and the Zn complex show liquid crystalline behavior. According to the DSC thermogram of the Zn complex, it exhibits a lower phase transition temperature -7. 453℃ and a wide mesophase temperature span, 77℃.     

Synthesis, Characterization and Structure of 3d Metal Nitrate Complexes with 1,8-Naphthyridine-N-Oxide

The complexes of 3d metal(Cr, Mn, Fe, Co, Ni, Cu, Zn) nitrates with 1 , 8-naphthyridine-N-oxide (NAPYO) were synthesized. The melting points and solubilities of the new complexes were determined and all the complexes were characterized by elemental analyses, IR spectra, UV spectra and molar conductance. The structures of both nickel complex and copper complex were determined by X-ray single crystal diffraction analyses.     

Metal Complexes of Donor-functionalized Fluorinated β-Ketoiminates – Synthesis,Structure, and CVD Application

Six alkali metal complexes of partly-fluorinated, donor-functionalized β-ketoiminate ligands [L¹Li ( 1 ), L¹Na ( 2 ), L¹K ( 3 ), L¹Cs ( 4 ), L¹ = OC(CF₃)CHC(CH₃)NCH₂CH₂OCH₃; L²Li ( 5 ), L²Na ( 6 ), L² = OC(CF₃)CHC(CH₃)NCH₂CH₂N(CH₃)₂] were prepared and structurally characterized. Reactions of L¹Li with PtCl₂ gave the homoleptic Pt complex L¹₂Pt ( 7 ), which was characterized spectroscopically and by single-crystal X-ray diffraction and whose promising application as CVD precursor (chemical vapor deposition) is shown. Polycrystalline, pure Pt films were grown at 500 °C on SiO₂@Si(100) substrates at 10^–3 mbar and characterized by XRD, SEM, AFM, EDX and XPS.     

Synthesis and Crystal Structure of [K(18-Crown-6)]3P11·2en

The undecaphosphide anion in ethylenediamine/18-crown-6 solution is isolated as [K(18-crown-6)]3P11·2en 1.The crystal structure has been determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21 with a = 13.4731(7),b = 16.1123(6),c =16.5117(9) (A),β = 112.133(2)°,V = 3320.3(3) (A)3,Dc= 1.371 g/cm3,C40H88K3N4O18P11,Mr=1371.11,F(000) = 1444,μ = 0.532 mm-1,Z = 2,R = 0.0544 and wR = 0.1326 for 11423 observed reflections (I ＞ 2σ(I)).The "naked" P11 3- ion is stabilized by two partly sequestered potassiums.The third partly sequestered potassium does not interact with the P atom (P(6)) but with two solvent molecules.     

Synthesis and Crystal Structure of [K(18-Crown-6)]_3P_(11)·2en

1 INTRODUCTIONSince the first report on the reduction of lead by sodium to a green solution in 1891 by Johannis, polyanionic clusters of post-transition metals known as Zintl ions have attracted much attention in chemistry due to their beautiful molecules, diverse reactivity and potential applications[1, 2]. Polyphos- phide anions represent one of the most important classes of zintl ions. The binary alkali-metal poly- phosphides, such as MI4P6 (M = K, Rb, Cs)[3～5], MI3P7 (M = Li-Cs)…     

Synthesis,Structure and Oxidation Reaction of Tetrakis-pyridino-cobalt(Ⅱ) Dichromate

The title compound was prepared from the mixture of cobalt ( Ⅱ ) acetate, chromium trioxide and pyridine in an aqueous solution, and its structure was determined by X-ray single crystal diffraction method. A number of alcohols, benzyl halides and benzy-lamines can be oxidized by this oxidant to the corresponding aldehydes in high yields.     

Synthesis,Crystal Structure and Band Structure of Tb3Co4Sn（13）

A new intermetallic compound,Tb3Co4Sn13,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.Tb3Co4Sn13 crystallizes in cubic,space group Pm3n(No.223) with a = 9.5072(2) ,V = 859.33(3) 3,Z = 2,Mr = 2255.45,Dc = 8.717 g/cm3,μ = 34.369 mm-1,F(000) = 1906,and the final R = 0.0140 and wR = 0.0312 for 199 observed reflections with I > 2σ(I).The structure of Tb3Co4Sn13 belongs to the Yb3Rh4Sn13 type.It is isostructural with RE3Co4Sn13(RE = La,Ce),featuring a 3D [Co4Sn12] framework based on [CoSn6] trigonal prisms.The [CoSn6] trigonal prisms are interconnected via corner-sharing and Sn-Sn bonds to form a 3D [Co4Sn12] framework.The other Sn and Tb atoms are located in the spacers of the 3D framework.Band structure calculations indicate that Tb3Co4Sn13 is metallic.     

Synthesis and Crystal Structure of a Sandwiched Trinuclear Complex [Tl2(18-Crown-6)2Pt(CN)4]·2H2O

The trinuclear complex bis(18-crown-6)thallium tetracyanoplatinate [Tl2(18-crown- 6)2Pt(CN)4]·2H2O was prepared and its structure was determined by X-ray diffraction analysis. The compound (C28H52N4O14PtTl2, Mr = 1272.57) crystallizes in monoclinic, space group P21/n with a = 10.5180(10), b = 8.6162(8), c = 21.118(2) (A), β = 92.577(2)°, V = 1911.9(3) (A)3, Z = 2, Dc = 2.211 g/cm3, F(000) = 1200, μ = 12.123 mm-1, R = 0.0181 and wR = 0.0427. The linearly arranged three metals are sandwiched by two 18-crown-6 molecules.     

Synthesis and Crystal Structure of (C6N3H18)2Ti4O4(C2O4)7·4H2O

The title compound (C6N3H18)2Ti4O4(C2O4)7(4H2O 1 (C13H22N3O18Ti2, Mr = 604.14) was synthesized by the reaction of Ti(SO4)2, H2C2O4(2H2O and N-(2-ammonioethyl)- piperazinium (AEPP) in aqueous solution. The single-crystal X-ray analysis has revealed that 1 crystallizes in the triclinic system, space group Pī with a = 9.1437(6), b = 11.4991(10), c = 11.6975(8)A, α = 96.2915(18), β = 107.998(3), γ = 104.276(4)°, V = 1110.35(14)A3, Z = 2, Dc = 1.807 g/cm3, F(000) = 618, μ = 0.815 mm－1, the final R = 0.0463 and wR = 0.1264 for 3718 observed reflections with I > 2σ(I). X-ray crystal-structure analysis suggests that compound 1 consists of [Ti4O4(C2O4)7]6－ anion and two protonated N-(2-ammonioethyl)piperazinium cations. The anions are linked into an infinite chain through Ti4O4(C2O4)8 by sharing the oxalates as bridging ligands.     

Synthesis and Crystal Structure of a New Lanthanum(III) 4-Cyanobenzoate Complex

A new dinuclear La(III) complex [La2(4-cba)4[H(4-cba)2]2(phen)2(H2O)4] (4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline) 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single- crystal X-ray diffraction. Crystallographic data: C88H58La2N12O20, Mr = 1881.28, triclinic P1, a = 7.518(3), b = 17.033(6), c = 17.551(6), α = 115.333(4), β = 92.9910(10), γ = 99.366(5)°, V = 1985.3(12)3, Z = 1, Dc = 1.574 g/cm3, F(000) = 944 μ = 1.145 mm–1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with I > 2σ(I). In 1, two nine-coordinated La(III) ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La(III) ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.     

Synthesis, Characterization and Crystal Structure of the First Tri-nuclear MFe2（M = Cu and Ni） Complexes Based on Nitroprusside

IntroductionSince 184 8,whenPlayfairpublishedthefirstpaperrelatedtonitroprussides ,1thetransitionmetalpenta cyanonitrosylmetallatehydrateshavebeenwidelystudiedbecauseoftheirimportantrolesinmolecularsieves ,cationexchangers,electronscavengersandradionuclidesor bents .2 4 Thenitroprussides ,regardlessofthecationicmetal,arecurrentlyemployedasreversibleinhibitorsofagroupofenzymesknownassuperoxidedismutases .5Recently ,using [Fe(CN ) 5(NO) ]2 - asabuildingblock ,somenitroprusside bridgedpolymeri…     

Synthesis and Crystal Structure of Complexes of Lanthanide Picrates With N,N ′-Dimethyl-N,N ′-Diphenyl-1,2-PhenylenediOxydiacetamide

Lanthanide picrate complexes with the ligand N,N'-dimethyl-N,N'-diphenyl-1,2-phenylenedioxydiacetamide (L) [Ln(Pic)₃L] (Ln=La,Gd,Er,Y) have been prepared in nonaqueous medium and characterized by elemental analysis, IR and ¹H spectra. The Gd(III) complex [Gd(Pic)₃L]·3CH₃CN is triclinic, space group P&1macr;, with a=14.292(1), b=14.967(2), c=16.571(2)Å, α=97.855(9), γ=113.070(9)°, ν=28706(6)ų, D _c=1.584g/cm³ for Z=2. The structure was refined to R=0.0318 based on 8409 observed reflections.     

Synthesis,Structure and Photophysical Properties of a New Class of Inherently Chiral Boron(III) Chelates—The tert-Leucine Complexes

A new family of boron(III) chelates is introduced whereby molecular chirality, confirmed by circular dichroism, is imported during synthesis such that isolation of the diastereoisomers does not require separation procedures. The photophysical properties of two members of the family have been examined: the N,O,O-salicylaldehyde-based derivative shows pronounced intramolecular charge-transfer character in fluid solution and is weakly fluorescent, with a large Stokes shift. The corresponding 2-methylamino-benzaldehyde-derived N,N,O-chelate absorbs and fluoresces in the visible region with a much smaller Stokes shift. Orange fluorescence is also observed for this compound as a cast film. Temperature-dependence studies show that decay of the fluorescent state is weakly activated but emission is less than quantitative at 77 K. Quite rare for boron(III)-based chelates, this derivative undergoes intersystem crossing to form a meta-stable triplet-excited state. X-ray crystal structures are reported for both compounds, along with simulated ECD spectra.     

Synthesis and Crystal Structure of a Sandwiched Trinuclear Complex [Tl_2(18-Crown-6)_2Pt(CN)_4]·2H_2O

1 INTRODUCTION Tetracyanoplatinate ion often forms one-dimen- sional chain compounds, and the Pt–Pt spacings are often only 0.01~0.3 ? longer than those in Pt metal (2.78 ?). The studies of room-temperature electrical conductivities of these complexes indicate that the shorter the Pt–Pt separations in the chains are, the higher the electrical conductivity is[1~3]. Tetracyano- platinate ion may also stack with suitable planar cations into one-dimensional materials such as [Pt- (CNR)4]…     

Synthesis and X-Ray Crystal Structure of Two Novel Complexes: [M II(phen)3]2V4O12·phen·22H2O(M II=Co, Ni; phen=phenanthroline)

Summary. Two novel compounds, [Co(phen)₃]₂V₄O₁₂·phen·22H₂O (1) and [Ni(phen)₃]₂ V₄O₁₂·phen·22H₂O (2), were prepared from KVO₃–1,10-phenanthroline (phen)–Co(NO₃)₂, resp. NiCl₂–H₂O reaction systems. The compounds 1 and 2 are isomorphous and crystallize in triclinic system, space group P-1. Their crystal structures are formed by two types of layers parallel to 001: a cationic one consisting of [M^II(phen)₃]²⁺ ions and an anionic one containing the cyclic V₄O₁₂ ^4– anions. The solvate phenanthroline and crystal water molecules are located in the cationic and anionic layers, respectively. The IR spectra of 1 and 2 are consistent with the presence of the cyclic V₄O₁₂ ^4– anions in the complexes.Received November 13, 2002; accepted (revised) February 3, 2003 Published online June 2, 2003     

Crystal Structure of the Bis(Picrato-O,O")Tetraaquacalcium Complex with 18-Crown-6, [Ca(Pic)2(H2O)4] · 18C6

The crystal structure of the bis(picrato-O,O")tetraaquacalcium complex with 18-crown-6, [Ca(Pic)₂(H₂O)₄] · 18C6 (I), was studied using X-ray diffraction analysis: space group C2/c, a= 20.446 Å, b= 14.985 Å, c= 16.163 Å, = 135. 41°, Z= 4. The structure of Iwas solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R= 0.047 over all 3044 measured independent reflections (CAD4 automated diffractometer, MoK radiation). In the crystal, Iis not a guest–host complex but exists as individual [Ca(Pic)₂(H₂O)₄] and 18C6 molecules joined by intermolecular hydrogen bonds and van der Waals interactions. The Ca²⁺cation (CN 8) is located on a twofold crystallographic axis, its coordination polyhedron being a distorted square antiprism. The centrosymmetrical 18C6 molecule has a crown conformation with approximate D _3d symmetry and has six neighboring water molecules (three on each side of its mean plane), which form eight hydrogen bonds involving all six O atoms of 18C6.     

Synthesis, Crystal Structure, and Properties of Inorganic-organic Hybrid M(Ⅱ)-Nb(Ⅴ)(M = Co, Cu)Oxyfluorides

T Two isostructural inorganic-organic hybrid M(Ⅱ)-Nb(Ⅴ)oxyfluorides, namely,M(H<,2>O)<,2>(pyz)NbOF<,5>(M = Co 1, Cu 2; pyz = pyrazine)have been hydrothermally synthesized and structurally characterized. Both compounds possess two-dimensional layer structure constructed by neutral M(H<,2>0)<,2>NbOF<,5> chains inter-connected via bridging pyrazine ligands. The structure is further extended into three-dimensional supramolecular architecture through inter-layer H-bonding interactions between the coordinated water molecules and fluorine ions. The luminescent properties and thermal stability of both compounds have been investigated.     

Synthesis and Crystal Structure of Cu( Ⅱ ) Adduct with N-(4-Chlorophenyl)aza 15-Crown-5

The title compound C18 H25 NC4ClBr2Cu crystallizes in space group P 1 with a = 1.0105(2)nm b=1.0821(1) nm, c=1. 1007(2) nm, a=80. 00(1)°,β=80. 26(1)° γ=77. 83(1)°. Z=2, D = 1. 831 g/cm3, μ=62. 658 cm-1(Mok(?)). The final refinement converged to R=0. 031 for 2547 independent observed reflections. The complex molecule consists of two cationic moieties (HL)+ and an anion which appears as a bromide-bridged copper dimer (Cu2Br6)2-. This structural characterization seems to be rare in metal complexes with crown-ether.     

Two-dimensional Network Crown Ether Complex. Synthesis and Crystal Structure of 18-Crown-6 Complex: [K(18-C-6)]_2[Cd-(mnt)_2]

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Synthesis and Properties of Uranosilicates M[HSiUO6] · nH2O (M = NH4+, Li,Na, K,Rb, Cs)

A complete set of uranosilicates M[HSiUO₆] · nH₂O of alkali metals and ammonium was obtained under hydrothermal conditions. The functional and phase similarity of the compounds was proved by X-ray phase analysis and IR spectroscopy. The effect of water molecules on the structures of hydrated and anhydrous uranosilicates and the nature of water in these compounds were elucidated by studying hydration-dehydration processes. The dependence of the X-ray and thermal properties of the compounds on the nature of interlayer atoms was considered.