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1.
In this work, we determine the crystal structure of dimethoxo(meso-tetra(4-methoxyphenylporphyrinato))tin(IV), Sn(tmpp)(OMe)2 (1). Experimental results indicate that the tin atom has an octahedral geometry. The geometry around the tin center has Sn(1)–O(5) = 2.020(6), Sn(1)–O(6) = 2.003(7) Å and an average Sn(1)–N = 2.10(1) Å. The two methoxo groups are unidentately coordinated to the tin(IV) atom. Two-stage hydrolysis of Sn(tmpp)(OMe)2 in CDCl3 was observed by 1H and 13C NMR spectroscopy. Compound (1) crystallizes in the space group P21/n with a = 14.7492(1), b = 19.2022(3), c = 16.0806(2) Å, = 94.104(1)°, and Z = 4.  相似文献   

2.

Abstract  

Hydrothermal synthesis and the structural characterization of V(IV) complex of 2-pyrazinecarboxylate (pzc), is reported. The vanadium is in a distorted octahedral environment. Pairs of pyrazine-2-carboxylate ligands are always cis to each other. The pzc ligands do not link adjacent vanadium atom directly. The remainder of the three-dimensional network is completed by intense hydrogen bonding of uncoordinated water molecules to aqua and pzc ligands. Cis-[VIVO(pzc)2(H2O)]·2H2O, 1, was characterized by means of elemental analysis (CHNS), TGA, FT-IR, manganometric titration, bond valance sum calculations and single crystal X-ray diffraction methods. Crystal data for 1: monoclinic space group P2 1 /c and unit-cell parameters are a = 9.1142(5), b = 16.5822(10), c = 12.8936(7) ?, β = 131.625(3)° and Z = 4. To the best of our knowledge, cis-[VIVO(pzc)2(H2O)] is reported without single crystal structure by Eugenio Garribba and his colleagues in year 2006. Herein we complete full characterization of the title complex with single crystal structure and also 1 will be the first reported example of solid vanadium complex of 2-pyrazinecarboxylates involving intense hydrogen bonding.  相似文献   

3.
Abstract  Grandiflorenic acid [(−)-kaura-9(11)-16-dien-19-oic acid] methyl ester (2), C21H30O2, was synthesized from grandiflorenic acid, isolated from the plant Montanoa tomentosa. Compound (2) was formerly described as an oily derivative. X-ray diffraction analysis of (2) demonstrated that it consists of four rings, three six-membered rings (I, II and III) and one five-membered ring (IV). I, II and III rings occur in chair, twist, and envelope conformations, respectively. Ring IV occurs in a conformation between envelope and half-chair. The crystal of grandiflorenic acid methyl ester is in monoclinic crystal system with space group P21, lattice constants: a = 7.2170(10), b = 11.4170(10), c = 11.2850(10) ?, β = 98.700(10)°, V = 919.1(2) ?3 and Z = 2. Index Abstract  Grandiflorenic acid [(−)-kaura-9(11)-16-dien-19-oic acid] methyl ester (2) was synthesized. This compound was formerly considered as an oily derivative. The crystal structure of (2) was obtained by determination of X-ray diffraction from suitable single crystals.   相似文献   

4.

Abstract  

The title compound (C5Me5)2U(OtBu)(SePh) (1) was synthesized and characterized by NMR spectroscopy, elemental analysis, and X-ray crystallography. This system represents a unique example of an actinide complex with two different group 16 elements coordinated to the metal center and the first mixed-ligand actinide alkoxide-selenide complex. The complex crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 17.830(7) ?, b = 14.973(6) ?, c = 21.254(8) ?, V = 5674(4) ?3, Z = 8, D calc = 1.727 Mg/m3. The uranium(IV) mixed-ligand alkoxide-selenide complex adopts a pseudo-tetrahedral geometry, with the tert-butoxide and phenylselenide ligands occupying the plane bisecting the metallocene unit. Structural comparisons of the complex (C5Me5)2U(OtBu)(SePh) (1) are made with related selenide and alkoxide uranium(IV) complexes.  相似文献   

5.

Abstract  

Two newly synthesized coordination compounds copper(II) bromide with the ligand 7-isobutyl-5-methyl[1,2,4]triazolo[1,5-a]pyrimidine (abbreviated as ibmtp) are presented, together with their 3D crystal structure and spectroscopic and magnetic properties. The compounds are CuBr2(ibmtp)2 (1) (red crystals) and [CuBr(ibmtp)4]Br(H2O)3 (2) (blue crystals). In (1) the Cu(ii) ion is present in a distorted tetrahedral environment, while in (2) the Cu(ii) ion has a square pyramidal geometry. These crystal structures are also the first ones reported with the ligand ibmtp.  相似文献   

6.
Abstract (4-Methylpiperidine-dithiocarbamato-S,S′)triphenyltin(IV) derivative of 4-methyl-1-piperidine carbodithioic acid (4-MePCDTA) have been synthesized and characterized by elemental, IR, multinuclear NMR (1H and 13C) and mass spectrometric studies. The crystal structure of the complex has been determined by X-ray single crystal analysis, which shows unsymmetrical nature of the ligand towards coordination to tin. It crystallizes in monoclinic P21/c space group with the crystal cell parameters: a = 10.1863(10) ?, b = 21.200(2) ?, c = 11.7332(11) ?, β = 111.2020(10)°, Z = 4 and V = 2,362.2(4) ?3. The tin atom is coordinated to the two sulfur atoms of the dithiocarbamate ligand and three carbon atoms of the phenyl groups are in distorted trigonal bipyramid geometry. This complex was tested for its antimicrobial activity against six different plant and human pathogens. The screening results show that the complex exhibit higher antibacterial and antifungal activity than the free ligand. Index abstract Synthesis, Spectroscopy, in vitro Biological Activity and X-Ray Structure of (4-Methylpiperidine-dithiocarbamato-S,S′)triphenyltin(IV) Saira Shahzadi, Saqib Ali and Mohammmed Fettouhi 4-Methyl-1-piperidine carbodithioic acid behaves as anisobidentate ligand and chelates the tin atom by means of sulfur atoms giving cis-trigonal bipyramid geometry around the tin atom. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.  相似文献   

7.

Abstract  

Two compounds [Zn(Hdpa)2(2,2′-bipy)]2 (1) and [Mn(dpa)(4,4′-bipy)] n (2) (H2dpa=2,2′-biphenyldicarboxylate, bipy=dipyridine) are synthesized by hydrothermal reactions and structurally characterized by Single crystal X-ray diffraction analyses. Compound 1 is a dual-core molecular structure of two Zn ions in the same coordination environment, we studied the fluorescence of compound 1. Compound 2 is a layer structure based on the one-dimensional chains bridged by 4,4-bipy, it displays weak antiferromagnetic interactions between the inter-chain Mn2+ ions.  相似文献   

8.
The cerium(IV) -diketonate compounds [Ce(-diket)4] [where -diket = tmhd (2,2,6,6-tetramethylheptane-3,5-dionate) 1, pmhd (1-phenyl-5-methylhexane-1,3-dionate) 2] were prepared by reacting cerium(IV) ammonium nitrate [CAN; Ce(NH4)2(NO3)6] with the respective Na(-diket) compound in ethanol, and structurally characterized by single crystal X-ray diffraction. Compound 1 crystallizes in the triclinic space group with a = 12.472(4), b = 19.972(5), c = 21.436(3) Å, = 97.05(7), = 90.16(2), = 106.55(3)°, V = 5076(2) Å3, Z = 4, T = 150(2) K. Compound 2 crystallizes in the monoclinic space group P21/n. with a = 14.817(6), b = 17.123(6), c = 19.146(3) Å, = 105.46(4)°, V = 4682(3) Å3, Z = 4, T = 150(2) K. Crystals of 1 contain two independent [Ce(tmhd)4] molecules, with four chelating tmhd ligands bonded to each metal in a distorted dodecahedral arrangement; the cerium atom in 2 is also bonded to four chelating pmhd ligands but in this case the coordination geometry is closer to square antiprism. Both complexes are air and moisture stable. Sublimation studies reveal that 1 sublimes almost quantitatively, while 2 is comparatively involatile.  相似文献   

9.

Abstract  

A mononuclear fragment [Cu(L)Cl]ClO4 (1) and a cyano-bridged CuII–NiII binuclear complex [CuL][Ni(CN)4]·0.25H2O (2) (L = 1,3,6,8,11,14-hexaazatricyclo[12.2.1.18,11]-octadecane), have been prepared and characterized. X-ray single crystal analyses indicate that the both complexes crystallize in the monoclinic crystalline system. The complex of 1 in P1n1 space group with unit cell constants a = 6.1176(6) ?, b = 11.9147(10) ?, c = 12.2041(12) ?, β = 98.816(5)° and 2 in the P21/n space group with unit cell constants a = 8.1419(13) ?, b = 14.695(2) ?, c = 16.863(3) ?, β = 98.375(2)° have been revealed. The complex 2 assumes a binuclear structure in which the nickel(II) ion is in a square planar environment and the copper(II) is in a square-prism geometry environment.  相似文献   

10.

Abstract  

The reaction of [Ni(L)]Cl2·2H2O (L = 3.14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane) with malonic (H2mal) acid yields a one-dimensional coordination polymer [Ni(L)(mal)2]n (1). The structure was characterized by X-ray crystallography, spectroscopic and magnetic susceptibility. Each nickel(II) ion has a distorted octahedral coordination environment with the four secondary amines of the macrocycle in which two carboxylate anions of the malonate ligand have assembled around each nickel center. The compound crystallizes in the monoclinic system C2/c with a = 19.487(4), b = 8.4143(12), c = 14.6036(18) ?, β = 102.232(11)°, V = 2340.2(6) ?3, Z = 4. Electronic spectrum of 1 exhibits a high-spin octahedral environment. The magnetic behavior of 1 reveals a weak intramolecular antiferromagnetic interaction with J values of −1.91(1) cm−1.  相似文献   

11.

Abstract  

Cadmium(II) complexes, dibromidobis(N,N′-dimethylthiourea-S)cadmium(II), [Cd(Dmtu)2Br2] (1) and diiodidobis(N,N′-dimethylthiourea-S)cadmium(II), [Cd(Dmtu)2I2] (2), have been prepared and their structures have been determined by X-ray crystal structure analysis. Compound 1 crystallized in the monoclinic space group C2/c, and the metal ion is situated on a twofold rotation axis. Compound 2 also crystallized in a monoclinic space group, P21/c, but here the molecules have no crystallographic symmetry. In both compounds the cadmium atom is bonded to two halide ions and to two dimethylthiourea molecules through the sulfur atoms in a tetrahedral environment. The molecules are linked via N–H⋯Halide hydrogen bonds to form infinite one-dimensional chains in 1 and infinite two dimensional networks in 2. The complexes were also characterized by IR and NMR spectroscopy and the data are consistent with the structures of the compounds.  相似文献   

12.
The square-planar complex [Cu(MIMH)(CH3CO2)](ClO4) (1) (MIMH = [(4-methylimidazol-5-yl)methylene]histamine) was prepared and structurally characterized. Complex 1 crystallizes in the monoclinic space group P21/n with a = 10.5331(10), b = 12.6177(10), c = 12.9773(10) Å, = 107.710(10)°, V = 1643.0(2) Å3, and Z = 4. Single-crystal X-ray analysis reveals that the copper(II) atom in 1 has a distorted square-planar environment defined by three nitrogen atoms from the Schiff base ligand and one oxygen atom from the acetate group. The Cu—N bond lengths range from 1.950(3) to 2.015(3) Å and the Cu—O(1) bond length is 1.952(2) Å. The electronic spectra of 1 in aqueous solutions indicates that 1 forms adducts of square-pyramidal geometry with H2O. Cyclic voltammetry of 1 in DMF solution shows that there is some degradation of 1 upon reduction.  相似文献   

13.
Two new nickel(II)(cyclen) coordination polymers, {[Ni(cyclen)·(bipy)]·(ClO4)2}n (1) and [Ni(cyclen)]2·(squa)·(ClO4)2 (2) have been synthesized and characterized structurally, where cyclen is 1,4,7,10-tetraazadodecane. Compound 1 crystallizes in the monoclinic system, space group C2/c, with a = 10.5339(17) ?, b = 14.565(2) ?, c = 16.133(3) ?, β = 102.799(2)°, V = 2413.4(7) ?3. Compound 2 crystallizes in the orthorhombic system, space group P nm a with a = 25.722(3) ?, b = 11.1168(12) ?, c = 11.4580(13) ?, V = 3276.3(6) ?3. In both compounds, each NiII center is in a distorted octahedral coordinated environment with four Ncyclen atoms and two Npyridine atoms from 4,4′-bipyridine linker for 1 and two Oaqueou atoms from the coordinated water for 2, respectively. The complex 1 exhibits infinite zigzag 1D chains by linking of 4,4′-bipyridine coordinated. In complex 2, 2D sheet supramolecule generated through self-assembling by hydrogen bond.  相似文献   

14.
Using the new ligand, 2,2-bis-(4-pyridylethynyl)tolane we have synthesized five new coordination polymers: HgBr2[2,2-bis-(4-pyridylethynyl)tolane] (1), HgI2[2,2-bis-(4-pyridylethynyl)tolane] (2), Ni(acetylacetonate)2[2,2-bis-(4-pyridylethynyl)tolane] (3), Zn(acetylacetonate)2[2,2-bis-(4-pyridylethynyl)tolane] (4), and Cu(hexafluoro acetylacetonate)2[2,2-bis-(4-pyridylethynyl)tolane]CHCl3 (5). 2,2-Bis-(4-pyridyl ethynyl)tolane is a rigid ligand with a Z-shape that promotes the formation of zig-zag chains. Compounds 15 were characterized by single crystal X-ray diffraction; and compounds 13 were additionally characterized by IR, elemental analysis, and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic space group C2/c with a = 29.761(3) Å, b = 5.0531(5) Å, c = 16.7823(15) Å, = 104.090(2), V = 2447.9(4) Å3, Z = 4. Each mercury is bound to two tolane ligands and two bromine anions, resulting in a tetrahedral coordination environment. Compound 2 crystallizes in the monoclinic space group P2/c, with a = 20.3061(17) Å, b = 5.6303(5) Å, c = 24.5459(19) Å, = 110.338(2), V = 2631.4(4) Å3, Z = 4. Here also, each mercury is bound to two tolane ligands and two iodine anions in a tetrahedral coordination environment. The ligand orientation differs in compounds 1 and 2 being trans oriented in 1 and cis oriented in 2. Compound 3 crystallizes in the monoclinic space group P21/c with a = 14.5947(14) Å, b = 6.3082(6) Å, c = 18.3939(18) Å, = 112.112(2), V = 1568.9(3) Å3, Z = 2. Each nickel is bound to two tolane ligands and two bidentate AcAc anions, resulting in an octahedral coordination environment. Compound 4, which is isostructural with 3, also crystallizes in the monoclinic space group P21/c with a = 14.6990(9) Å, b = 6.2724(4) Å, c = 18.6433(11) Å, = 112.8610(10), V = 1583.86(17) Å3, Z = 2. Compound 5 crystallizes in the triclinic space group P-1 with a = 6.5487(4) Å, b = 11.6471(7) Å, c = 14.3225(9) Å, = 70.1360(10), = 89.3990(10), = 88.7680(10), V = 1027.18(11) Å3, Z = 1. Each copper in 5 is bound to two tolane ligands and two bidentate hfAcAc anions, resulting in an octahedral coordination environment identical to that found in 3 and 4.  相似文献   

15.
The title compound, aefh-tetrachloro-cg,db-bis{-[(1-methyl-3-piperidinyl)methanethiolato]--S,N}-diplatinum(II, IV) crystallizes in the monoclinic system, space group P 21/a , with the following crystal data: a = 13.502(2) Å, b = 12.323(2) Å, c = 13.720(3) Å and = 105.92(2)°. It is a dinuclear Pt(II)–Pt(IV) mixed-valence thiolato complex and represents the first chelate compound of 3-mercaptomethyl-1-methyl piperidine. Each ligand is terdentate and simultaneously S,N-chelating and -bridging. The metal environment is approximately square-planar and octahedral for Pt(II) and Pt(IV), respectively, both S2PtNCl planes generating a dihedral angle of approximately 156°. There is no metal–metal bonding.  相似文献   

16.
The dinuclear copper(II) complex {[Cu(pmea)Cl][Cu(H2O)3Cl]}(Cl)·H2O (1) (pmea =bis(2-pyridylmethyl)amino-2-ethanoic acid) has been synthesized and characterized. It crystallizes in the monoclinic system P21/c, a = 9.0057(11), b = 28.031(3), c = 8.5669(10) Å, β = 104.267(2)°, V = 2095.9(4) Å3, Z = 4. Crystal structure of 1 reveals a syn-anti carboxylate-bridged dinuclear complex, in which the coordination environment around each copper atom exhibits a distorted square-pyramid. Magnetic susceptibility measurement for 1 exhibits a weak intermolecular antiferromagnetic exchange interaction with 2J = −1.17(9) cm−1. The cyclic voltammogram of 1 gives one oxidation and two reduction processes.  相似文献   

17.
The mono(dpa)copper(II) complex [Cu(dpa)Cl2] (1) (dpa = di-(2-picolyl)amine) has been synthesized and structurally characterized. It crystallizes in the monoclinic system P21/n with a = 8.155(1), b = 12.560(1), c = 12.817(2) Å, = 91.64(2)°, V = 1312.3(2) Å3, Z = 4. The copper atom is coordinated by three nitrogen atoms from the dpa ligand and two chlorides in a distorted square-pyramidal environment. Cyclic voltammetric data show that 1 undergoes the reversible one-electron oxidation to the Cu(III) and the reversible one-electron reduction to the Cu(I) state.  相似文献   

18.
Two new complexes of [Mn(2-MPyzCI)2Cl2].H2O (1) and [Mn(2-MPyzCI)2(H2O)2](NO3)2 (2) were synthesized from the reaction of MnX2.4H2O (X=Cl? and NO3?) with 2-cyanopyrazine in methanolic solution. The chelating methyl pyrazine-2-carboximidate (2-MPyzCI) ligand is formed via the methanolysis of 2-cyanopyrazine. Although coordination environment around manganes(II) ions is similar, but these complexes are different in geometrical position of 2-MPyzCI ligands. As both compounds are synthesized under the same reaction conditions, the only difference between these two complexes are counter ions and changing of geometrical position of ligands can be considered as a result of influence of the counter-anions on the molecular structures.  相似文献   

19.
Three Sr2+ compounds with the Edta 4− and H2 Edta 2− ligands—Sr2(Edta) · 5H2O (I), Sr2(H2 Edta)(HCO3)2 · 4H2O (II), and Sr2(H2 Edta)Cl2 · 5H2O (III)—are synthesized, and their crystal structures are studied. In I, the Sr(1) atom is coordinated by the hexadentate Edta 4− ligand following the 2N + 4O pattern and by two O atoms of the neighboring ligands, which affords the formation of zigzag chains. The Sr(2) atom forms bonds with O atoms of five water molecules and attaches itself to a chain via bonds with three O atoms of the Edta 4− ligands. The Sr(1)-O and Sr(2)-O bond lengths fall in the ranges 2.520(2)–2.656(3) and 2.527(3)–2.683(2) ?, respectively. The Sr(1)-N bonds are 2.702(3) and 2.743(3) ? long. In II and III, the H2 Edta 2− anions have a centrosymmetric structure with the trans configuration of the planar ethylenediamine fragment. The N atoms are blocked by acid protons. In II, the environment of the Sr atom is formed by six O atoms of three H2 Edta ligands, two O atoms of water molecules, and an O atom of the bicarbonate ion, which is disordered over two positions. In III, the environment of the Sr atom includes six O atoms of four H2 Edta 2− ligands and three O atoms of water molecules. The coordination number of the Sr atoms is equal to 8 + 1. In II and III, the main bonds fall in the ranges 2.534(3)–2.732(2) and 2.482(2)–2.746(3) ?, whereas the ninth bond is elongated to 2.937(3) and 3.055(3) ?, respectively. In II, all the structural elements are linked into wavy layers. The O-H…O interactions contribute to the stabilization of the layer and link neighboring layers. In III, hydrated Sr2+ cations and H2 Edta anions form a three-dimensional [Sr2(H2 Edta)(H2O)3] n 2n+ framework. The Cl anions are fixed in channels of the framework by hydrogen bonds with four water molecules. In II and III, the N-H groups form four-center N-H…O3 hydrogen bonds, which include one intermolecular and two intramolecular components. PACS numbers: 61.66.Hq Original Russian Text ? I.N. Polyakova, A.L. Poznyak, V.S. Sergienko, 2009, published in Kristallografiya, 2009, Vol. 54, No. 2, pp. 262–267.  相似文献   

20.
Abstract The tridentate Schiff base carboxylate-containing ligand 2-pyridylmethylamino-3-butyric acid (Hpaba) reacts with copper(II) perchlorate to give the one-dimensional chain complex {[Cu(μ-paba)](ClO4)·H2O} n (1). The coordination geometry of each copper(II) ion is best described as a square-plane with two nitrogen atoms and one carboxylate oxygen atom of the ligand, and one carboxylate oxygen atom belong to another ligand. It crystallizes in the monoclinic system P21/c with a = 12.717(2), b = 7.9163(15), c = 14.981(2) ?, β = 111.14(1)°, V = 1406.8(4) ?3, Z = 4. Cyclic voltammogram of 1 undergoes the reversible one-electron oxidation to the Cu(III) and the reversible one-electron reduction to the Cu(I) state. Graphical Abstract Crystal structure of 1 reveals a syn-anti carboxylate-bridged one dimensional chain complex in which the coordination environment around each copper(II) ion exhibits a distorted square plane.   相似文献   

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