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1.
Two ethylenediamine derivatives—N-(2-ammoniumethyl)carbamate HN(COO?)CH2CH2N+H3 (I) and tetraacetylethylenediamine (H3CC(O))2NCH2CH2N(C(O)CH3)2 (II) (synthesized for the first time)—have been synthesized and characterized by X-ray crystallography. Compounds I and II are isolated as minor admixtures upon an attempt to synthesize ethylenediamine complexes of lanthanum and neodymium nitrates, respectively. The crystals of I and II are monoclinic: a = 7.778 Å, b = 8.060 Å, c = 7.568 Å, β = 95.73°, Z = 4, space group P21/c (I); a = 5.946, b = 10.255, c = 9.343 Å, β = 95.72°, Z = 2, space group P21/c (II). The bond lengths and bond angles lie within the corresponding standard values. Compounds I and II have different conformations of the N-C-C-N ethylenediamine moiety: gauche in I and trans in II, and the corresponding torsion angles are equal to 66.6° and 180°, respectively.  相似文献   

2.
The (DienH3)[AuCl4]3 · H2O (I) and (DienH3)2[AuCl4]Cl5 (II) compounds were obtained by the reaction of HAuCl4 with diethylenetriamine trihydrochloride (DienH3Cl3) in hydrochloric acid. The compounds were characterized by elemental analysis, X-ray diffraction, thermogravimetry, and IR spectroscopy. Crystals of I and II are monoclinic with space group P21/n. For I, a = 12.2314(3) Å, b = 14.6077(5) Å, c = 13.2680(5) Å, β = 106.7350(10)°, V = 2270.22(13) Å3, Z = 8. For II, a = 6.62990(10) Å, b = 17.9026(5) Å, c = 10.3661(3) Å, β = 101.9230(10)°, V = 1203.83(5) Å3, Z = 2. Both structures are ionic. The gold atoms in I and II have a 4 + 2 coordination environment. The Au-Cl bond lengths are within 2.276–2.294 Å, and the axial Au…Cl contacts are within 3.315–3.405 Å. The diethylenetriammonium cation in I and II has different conformations.  相似文献   

3.
Single crystal X-ray diffraction is used to investigate two synthesized β-diketonate complexes of copper(II) with aminopyridine: Cu(4-NH2Py)(aa)2 (I) and Cu(4-NH2Py)(hfa)2 (II). The crystals of I and II have a monoclinic system; the unit cell parameters of I are: P21/n space group, a = 8.2921(3) Å, b = 14.7243(5) Å, c = 13.4970(4) Å, β = 102.426(1)°, V = 1609.32(9) Å3, Z = 4; for II: C2/c space group, a = 23.5704(5) Å, b = 11.4977(2) Å, c = 16.0285(3) Å, β = 109.265(1)°, V = 4100.6(1) Å3, Z = 8. The structures of I and II are molecular; they are composed of isolated molecules. The coordination polyhedron of the copper atom is formed by the O atoms of two acetylacetonate ligands (Cu-O 1.940(2)–2.171(2) I and the O atoms of two hexafluoroacetylacetonate ligands (Cu-O 1.940(2)–2.215(3) Å) in II. The molecules of 4-NH2Py are bonded to the copper atom via the nitrogen atom of the aromatic ring (Cu-N 2.008(2) Å in I and Cu-N 1.978(3) Å in II). Noncoordinated amino groups join the molecules of the complexes together by means of N-H…O hydrogen bonds.  相似文献   

4.
The phenolic azide bridged dinuclear nickel(II) complex, [Ni2(L1)2(N3)(H2O)(μ1,1-N3)] · EtOH (I), and the thiocyanate bridged dinuclear copper(II) complex, [Cu2(L2)21,1-NCS)2] (II), where L1 and L2 are the deprotonated forms of 2-mothoxy-6-[(2-piperidin-1-ylethylimino)methyl]phenol and 2,4-dichloro-6-[(2-methylaminoethylimino)methyl]phenol, respectively, were synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal of I is orthorhombic: space group Pbca, a = 12.172(1), b = 20.953(1), c = 29.779(2) Å, V = 7594.8(9) Å3, Z = 8. The crystal of II is monoclinic: space group P21/n, a = 8.7615(11), b = 19.672(2), c = 16.568(2) Å, β = 99.449(2)°, V = 2816.9(6) Å3, Z = 4. The Ni atoms in I are in octahedral coordinations, and the Cu atoms in II are in square-pyramidal coordinations.  相似文献   

5.
Zinc(II) and manganese(II) complexes of 2-(diphenylacetyl)indandione-1,3 (HL) were synthesized. Crystals of [M(DMSO)2L2] · CHCl3, where M= Zn(II) (I) and Mn(II) (II), obtained from chloroform plus dimethyl sulfoxide (DMSO) mixture were found to be isostructural based on the similarity of their unit cell parameters and unit cell volumes. The crystals are triclinic, Z = 2, space group P \(\bar 1\); a = 10.422(1) Å, b = 11.929(1) Å, c = 20.429(1) Å, α = 73.616(1)°, β = 85.095(1)°, γ = 77.586(1)° for complex I; a = 10.436(1) Å, b = 12.297(1) Å, c = 19.924(2) Å, α = 78.138(2)°, β = 87.625(2)°, γ = 82.048(2)° for complex II. X-ray structural analysis of complex I was carried out. For complex II, the structure was not refined because all of its atoms are each disordered over three to five positions. The two DMSO molecules in complex I coordinate the central metal atoms in the monodentate mode via their donor oxygen atoms to occupy an axial position and an equatorial position in an octahedral polyhedron. The other four positions are occupied by the four oxygen atoms of the two deprotonated ligands L? coordinated in the bidentate-cyclic mode. The outer sphere of complex I contains the solvating chloroform molecule.  相似文献   

6.
Heteroligand complexes [Co2(HMTA)(iso-Bu2PS2)4] (I) (μeff = 4.67 μB) and [Cd2(HMTA)(iso-Bu2PS2)4] (II) have been synthesized. Single crystals of compounds I and II have been obtained. The crystals are monoclinic: a = 32.622(2) Å, b = 9.4891(6) Å, c = 21.7570(13) Å, β = 125.774(1)o, V = 5464.3(6) Å,3, Z = 4, ρcalcd = 1.331 g/cm3 for I; a = 34.6092(7) Å, b = 9.5595(2) Å, c = 22.3473(5) Å, β = 127.144(1)o, V = 5893.5(2) Å, Z = 4, ρcalcd = 1.355 g/cm3 for II; space group for both complexes C2/c. Structures I and II are based on discrete binuclear molecules. The coordination polyhedra of the Co and Cd atoms are distorted tetragonal pyramids NS4, with the bases formed by four S atoms of two bidentate chelating ligand iso-Bu2PS 2 ? and the axial vertices occupied by N atoms of bidentate bridging HMTA ligand. The character of interaction of the molecules in structures I and II is considered.  相似文献   

7.
Reactions of bis(acetylacetonato)oxovanadium(IV) with N′-[2-hydroxy-4-diethylaminobenzylidene)]-2-methylbenzohydrazide (H2HMB) and N′-[5-bromo-2-hydroxy-3-methoxybenzylidene)]-2-methylbenzohydrazide (H2BMB), respectively, produce two oxovanadium(V) species with the formulas [VO(OMe)(HMB)]2 (I) and [VO(OMe)(HOMe)(BMB)] (II). The complexes have been characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal of I is triclinic: space group P \(\bar 1\), a = 8.843(1), b = 9.937(1), c = 12.327(2) Å, α = 96.500(2)°, β = 110.070(2)°, γ = 104.220(2)°, V = 962.8(2) Å3, Z = 1. The crystal of II is monoclinic: space group P21/c, a = 9.908(2), b = 19.968(3), c = 11.065(3), β = 109.362(3)°, V = 2065.3(8) Å3, Z = 4. Compound I is the methoxide-bridged dimeric oxovanadium(V) complex, and II is the mononuclear oxovanadium(V) complex. Each V atom in the complexes is in an octahedral coordination.  相似文献   

8.
Hexaamminecadmium hydrogen hexamolybdocobaltate(III) and hydrogen hexamolybdochromate(III) of compositions [Cd(NH3)6] · H[CoMo6O18(OH)6] · 6H2O (I) and [Cd(NH3)6] · H[CrMo6O18(OH)6] · 6H2O (II), respectively, were synthesized and studied by mass spectroscopy, thermo-gravimetry, X-ray powder diffraction, and IR spectroscopy. Crystals of I and II are monoclinic. For I: a = 10.79 Å, b = 3.70 Å, c = 11.95 Å, β = 91.05°, V = 470.12 Å3, ρcalc = 2.37 g/cm3, Z = 2; and for II: a = 10.80 Å, b = 3.68 Å, c = 11.97 Å, β = 91.07°, V = 468.98 Å3, ρcalc = 2.36 g/cm3, Z = 2.  相似文献   

9.
The crystal structures of compounds of the composition [Rh(H2O)6]2(SO4)3·5H2O (I) and [Rh(H2O)6]PO4 (II) are determined. Crystallographic data for I: a = 7.272(9) Å, b = 27.047(1) Å, c = 12.464(9) Å, β = 97.038(10)°, P21 space group, Z = 4, d x = 2.184 g/cm3; for II: a = 9.746(6)Å, b = 6.877(7) Å, c = 23.623(6) Å, β = 100.601(10)°, C2/c space group, Z = 8, d x = 2.611 g/cm3. Compounds are analyzed by IR spectroscopy and powder XRD. Crystalline phase I is well soluble in water, whereas II is almost insoluble.  相似文献   

10.
An end-to-end azido-bridged dinuclear copper(II) complex [Cu2L21,3-N3)](NO3) (I) and a mononuclear zinc(II) complex [ZnCl2(HL)] ? CH3OH (II), where L is 2-brom-4-chloro-6-[(2-morpholin- 4-ylethylimino)methyl]phenolate, have been prepared and characterized by elemental analyses, IR, and single crystal X-ray crystallographic determination (CIF files CCDC nos. 1415217 (I), 1415218 for (II)). The crystal of I is monoclinic: space group C2/c, a = 28.684(2), b = 7.1787(5), c = 18.292(1) Å, β = 117.887(3)°, V = 3329.1(4) Å3, Z = 4. The crystal of II is monoclinic: space group P21/c, a = 10.8207(9), b = 12.3398(7), c = 14.9477(7) Å, β = 93.473(3)°, V = 1992.2(2) Å3, Z = 4. The Schiff base ligand in I coordinates to the Cu atom through the phenolate O, imine N, and morpholine N atoms, while the Schiff base ligand in II coordinates to the Zn atom through the phenolate O and imine N atoms, with the morpholine N atom protonated. The effect of these complexes on the antimicrobial activity against Staphylococcus aureus, Escherichia coli, and Candida albicans was studied.  相似文献   

11.
Iron(III) and aluminum(III) complexes with 2-diphenylacetyl-1,3-indandione (HL) have been synthesized. The structures of the obtained compounds FeL3(I) and AlL3(II) were studied. The isostructural crystals are monoclinic, I: Z = 8, space group P21/c, a = 16.061(3) Å, b = 16.658(3) Å, c = 22.015(4) Å, β = 111.41(3)°; II: Z = 8, space group P21/c, a = 16.115(14) Å, b = 16.476(8) Å, c = 21.949(20) Å, β = 111.04(11)°. The structural units of crystals I and II are neutral molecules in which each ligand is bidentately coordinated to a central metal atom through the oxygen atom of the acyl keto group and an oxygen atom of the indandione fragment to form a six-membered chelate ring. In the crystals, neutral molecules I and II form pseudodimers due to stacking of indandione moieties of two adjacent coordination spheres and additional C-H…O contacts. Each pseudodimer is in contact with six neighboring dimers also through hydrogen bonds C-H…O to form an infinite framework.  相似文献   

12.
New double complexes [Co(DMSO)6][SiF6] ? 2H2O (I) and [Co(DMF)3(H2O)3][SiF6] ? DMF (II) have been synthesized and studied by IR spectroscopy and X-ray diffraction. Crystals of complex I belong to the tetragonal symmetry system, space group R3?, Z = 3, a = 11.8232(3) Å, c = 18.4699(5) Å, V = 2235.97(10) Å3, ρcalc = 1.573 g/cm3. Crystals of complex II are triclinic, space group P1?, Z = 2, a = 8.6264(4) Å, b = 10.1419(4) Å, c = 13.9657(6) Å, α = 100.847(2)°, β = 98.549(2)°, γ = 93.479(2)°, V = 1181.71(9) Å3, ρcalc = 1.539 g/cm3.  相似文献   

13.
Two Mn(II) coordination polymers, {[Mn3 (Pfca)6(Phen)2] · 2DMF} n (I) and [Mn(Pfca)2(Phen)(H2O)] n (II) (HPfca = 4-fluorocinnamic acid, Phen = 1,10-phenanthroline), were synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and singlecrystal X-ray diffraction (CIF files CCDC nos. 967513 (I), 1542972 (II)). Complex I crystallizes in the triclinic crystal system, space group Pī with a = 11.0821(11), b = 12.2632(12), c = 15.0288(15) Å, α = 87.3760(10)°, β = 88.4610(10)°, γ = 81.2220(10)°, V = 2016.0(3) Å3, ρc = 1.369 g/cm3, M r = 1662.25, Z = 1, F(000) = 853, μ = 0.543 mm–1, the final R = 0.0592 and wR = 0.1681 for 15498 observed reflections with I > 2σ(I). Complex II is of monoclinic system, space group P21/c with a = 18.0539(19), b = 8.5806(9), c = 18.758(2) Å, β = 116.5700(10)°, V = 2599.0(5) Å3, ρc = 1.491 g/cm3, M r = 583.44, Z = 4, F(000) = 1196, μ = 0.567 mm–1, the final R = 0.0337 and wR = 0.0853 for 18139 observed reflections with I > 2σ(I). Complex I features linear Mn(II)-trinuclear units, which form 1D chain structure through F···F weak interactions, and complex II is 1D polymeric Mn(II)-chains. Antiferromagnetic coupling interactions exist within Mn(II)- carboxylate trinuclear in I (J =–0.40 cm–1) and Mn(II)-carboxylate chain in II (J =–0.45 cm–1).  相似文献   

14.
Two new mononuclear complexes, [NiL1] · CH3OH (I) and [NiL2] (II), have been prepared from the tetradentate Schiff bases N,N'-bis(5-methylsalicylidene)ethylenediamine (H2L1) and N,N'-bis(5-methylsalicylidene)- o-phenylenediamine (H2L2), respectively. The complexes have been characterized by physico-chemical and spectroscopic methods, as well as single-crystal X-ray determination (CIF files nos. 1428969 (I), 1428968 (II)). Complex I crystallizes in the triclinic space group P1 with a = 6.7387(14), b = 10.7010(17), c = 12.681(2) Å, α = 87.059(2)°, β = 88.828(2)°, γ = 89.901(2)°, V = 913.0(3) Å3, Z = 2. Complex II crystallizes in the monoclinic space group P21/n with a = 12.1437(11), b = 8.0537(8), c = 18.4545(18) Å, β = 105.088(2)°, V = 1742.7(3) Å3, Z = 4. The nickel atoms in the complexes are coordinated by two phenolate O and two imine N atoms of the tetradentate Schiff base ligands, forming square planar coordination. The complexes and the Schiff base compounds were assayed for antibacterial activities against three Gram-positive bacterial strains (B. subtilis, S. aureus, and St. faecalis) and three Gram-negative bacterial strains (E. coli, P. aeruginosa, and E. cloacae) by MTT method. As a result, the complexes showed effective antimicrobial activity against the microorganisms tested.  相似文献   

15.
Single crystal X-ray diffraction at a temperature of 150(2) K is used to determine the structures of two magnesium complexes with trifluoroacetylacetone: [Mg(tfac)2]3I and [Mg(H2O)2(tfac)2]·H2O II. Crystallographic data for I: space group P21/n, a = 12.5226(10) Å, b = 13.0591(7) Å, c = 12.6034(13) Å, β = 95.243(2)°, V = 2052.5(3) Å3, Z = 2; for II: space group P21/c, a = 10.826(2) Å, b = 7.0742(13) Å, c = 21.858(4) Å, β = 102.712(5)°, V = 1632.9(5) Å3, Z = 4. The isle structure of I is formed by linear trimeric molecules; in the structure of II the molecules of the complex and crystallization water form a layered framework using hydrogen bondings; the coordinated water molecules are in a trans position. The magnesium atoms have a distorted octahedral coordination environment, the Mg–O distances are 1.991(4)- 2.146(4) Å and 2.040(5)-2.073(5) Å in molecules of I and II respectively.  相似文献   

16.
The complexes [AgL2(NO3)] (I) and [AgL2(CH3SO3)] · H2O (II) (L is 2-methylquinoline, C10H9N) have been synthesized and structurally characterized by single-crystal X-ray diffraction. Crystals of I are monoclinic, space group P21/n, a = 9.296(1) Å, b = 13.495(1) Å, c = 14.931(1) Å, β = 95.06(1)°, V = 1865.8(3) Å3, ρcalc = 1.624 g/cm3, Z = 4. Crystals of II are monoclinic, space group P21/n, a = 13.147(1) Å, b = 11.767(1) Å, c = 13.814(1) Å, β = 96.06(1)°, V = 2124.3(3) Å3, ρcalc = 1.599 g/cm3, Z = 4. Compounds I and II are composed of discrete complexes of similar structure but with different orientation of the methyl groups of ligand L (trans and cis arrangement, respectively). Both anions, NO 3 - and CH3SO 3 - function as a chelating weakly bound ligand for the Ag+ ion. The presence of water molecules in II is favorable for the formation of dimeric supramolecular moieties between the centrosymmetrically arranged Ag+ complexes with 2-methylquinoline. The luminescence spectra of solid complexes I and II showed a bathochromic shift as compared to the spectrum of L in acetonitrile. Complexes I and II have been characterized by 1H and 13C{H} NMR spectra in CD3CN.  相似文献   

17.
Two new mononuclear Schiff base zinc(II) complexes, [ZnCl2(L1)] ? MeOH (I) and [Zn(L2)2] (II) (L1 = 2-bromo-4-chloro-6-[(2-ethylammonioethylimino)methyl]phenolate; L2 = 2-bromo-4-chloro-6-(isopropyliminomethyl)phenolate), have been prepared and characterized by elemental analyses, infrared and UV-Vis spectroscopy, and single-cyrstal X-ray diffraction (CIF files CCDC nos. 1408962 (I), 1408961 (II)). Complex I crystallizes in the triclinic space group \(P\overline 1\) with unit cell dimensions a = 9.859(1), b = 13.015(2), c = 19.817(3) Å, α = 73.591(2)°, β = 76.032(2)°, γ = 82.966(2)°, V = 2363.0(5) Å3, Z = 4, R 1 = 0.0925, and wR 2 = 0.2257. Complex II crystallizes in the monoclinic space group P21/c with unit cell dimensions a = 7.6387(7), b = 22.307(2), c = 21.443(2) Å, β = 96.216(3)°, V = 3632.4(6) Å3, Z = 8, R 1 = 0.0651, and wR 2 = 0.1100. The both Zn atoms in I is four-coordinated in a tetrahedral geometry by the NO donor set of the Schiff base ligand, and two Cl ligands. The Zn atom in II is in a tetrahedral geometry by two N and two O atoms from two Schiff base ligands. Crystals of the complexes are stabilized by hydrogen bonds and weak π…π interactions. Fluorescence property of the complexes have been determined.  相似文献   

18.
Two new isostructural zinc(II) complexes, [ZnCl2(L)] (I) and [ZnBr2(L)] (II), derived from the Schiff base ligand (1-pyridin-2-ylethylidene)pyridin-2-ylmethylamine (L), have been prepared and characterized by physicochemical methods and single-crystal X-ray crystallography. The crystal of I is monoclinic: space group P21/c, a = 11.699(3) Å, b = 8.460(2) Å, c = 14.766(3) Å, β = 99.686(3)°, V = 1440.6(6) Å3, Z = 4. The crystal of II is monoclinic: space group P21/n, a = 8.166(2) Å, b = 15.153(3) Å, c = 11.966(2) Å, β = 96.964(2)°, V = 1469.7(5) Å3, Z = 4. The geometry of the pentacoordinated zinc atoms in both complexes is best described as a square pyramid.  相似文献   

19.
Two complexes, namely, triaqua(18-crown-6)strontium dibromide monohydrate (I) and diaquabromo(18-crown-6)barium bromide (II), are synthesized. Their crystal structures are determined by X-ray diffraction analyses. For complex I, space group C2/c, a = 17.547 Å, b = 10.246 Å, c = 14.786 Å, β = 123.08°, Z = 4. For complex II, space group Pnma, a = 17.753 Å, b = 17.465 Å, c = 6.629 Å, Z = 4. The structures are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.056 (I) and 0.042 (II) for 2696 (I) and 2440 (II) independent reflections (CAD-4 automated diffractometer, λMoK α radiation). Both complex cations—randomly disordered [Sr(18C6)(H2O)3]2+ in complex I and [BaBr(18C6)(H2O)2]+ in complex II—are of the host-guest type. The Sr2+ (Ba2+) cation resides in the cavity of the 18-crown-6 ligand and coordinated by all six O atoms. In the structures complexes I and II, the coordination polyhedra of the Sr2+ and Ba2+ cations (coordination number 9) can be described as distorted hexagonal bipyramids with one apex at the O atom of the water molecule in complex I or at the Br? ligand in complex II and the other split apex at the O atoms of two water molecules.  相似文献   

20.
A new mononuclear cobalt(III) complex, [CoL2(N3)]2 · CH3OH (I), and a new mononuclear zinc(II) complex, [ZnLCl(CH3OH)] (II) (HL = 4-chloro-2-[(2-morpholin-4-ylethylimino)methyl]phenol), were prepared and structurally characterized by elemental analyses, infrared spectroscopy, and single- crystal X-ray diffraction. The crystal of I is monoclinic: space group P21/c, a = 18.742(2) Å, b = 15.197(2) Å, c = 25.646(2) Å, β = 125.996(3)°, V = 5909.8(11) Å3, Z = 4. The crystal of II is monoclinic: space group P21/c, a = 7.257(1) Å, b = 24.707(2) Å, c = 9.637(1) Å, β = 101.557(2)°, V = 1692.9(3) Å3, Z = 4. The Co atom in I is in an octahedral coordination, and the Zn atom in II is in a trigonal-bipyramidal coordination. The urease inhibitory test shows that complex I has strong urease inhibitory activity, while complex II has no activity.  相似文献   

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