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Giancarlo Pelizzi 《Transition Metal Chemistry》1979,4(3):199-204
Summary The structures of the title compounds were both solved from diffractometer data by direct methods and refined by full-matrix least-squares toR=4.63% for 3069 independent reflections for the nickel compound [triclinic,a=10.499(7),b=13.295(8),c=10.182(7) Å, =92.13(8), =103.58(7), =68.79(7)°;Z=2. Space group P1] and toR=7.98% for 772 independent reflections for the copper compound [tetragonal,a=12.939(6),c=14.991(7) Å;Z=4. Space group P4/ncc]. In the first compound two chemically equivalent, crystallographically independent molecules are present, in which each nickel atom attains an octahedral coordination involving four N(ring)-bonded isoxazole molecules and two isothiocyanate groups. In the copper compound, the metal atom shows square-pyramidal fivecoordination with the four symmetry-related organic molecules bondedvia N(ring) in the square plane and one bromide ion (the other is not coordinated) in the apical position. 相似文献
4.
Martina Schfer Ehmke Pohl Karen Schmidt-Bse George M. Sheldrick Rolf Hermann Adriano Malabarba Marino Nebuloni Giancarlo Pelizzi 《Helvetica chimica acta》1996,79(7):1916-1924
The crystal structure of a glycopeptide antibiotic A–40926 aglycone was investigated by X-ray analysis at ?120°. A-40926 crystallises in the orthorhombic space group P212121 with two monomers in the asymmetric unit, a = 21.774(4), b = 28.603(7), c = 29.757(4) Å. ‘Conventional’ direct methods approach failed to solve the structure, but a novel iterative real/reciprocal space procedure was successful. Refinement against 11248 F2 data led to R1 = 13.3% for 6770 F > 4σ (F). The two monomers of A-40926 have similar conformations and are bound by antiparallel H-bonds to form a ‘chain’ structure of connecting dimers. The antibiotic molecule possesses a ‘binding pocket’ for the C-terminal carboxy group of the cell-wall protein, which is consisten with suggestions based on NMR data and the recently reported crystal structure of ureido-balhimycin. In A-40926 the monomers are polymerically linked by H-bonds, quite unlike the tight dimer formation observed in ureido-balhimycin. 相似文献
5.
Di-2-pyridylketone semicarbazone as ligand in metal complexes: synthesis and X-ray crystal structure
Luigi P. Battaglia Pier Giovanni Berzolla Anna Bonamartini Corradi Corrado Pelizzi 《Journal of chemical crystallography》1993,23(12):973-979
A series of complexes of di-2-pyridylketone semicarbazone (Hdips) and Mn(II), Co(II), Co(III), Ni(II) and Cu(II) nitrates were synthesized and characterized by means of IR spectroscopy and for cobalt and nickel by X-ray crystal structures. The results are in agreement with the formulae: Mn(Hdips)2(NO3)2·2H2O, [Co(Hdips)2](NO3)2·H2O (I), [Ni(Hdips)2](NO3)2·H2O (II), Cu(Hdips)(NO3)2·2H2O, [Co(dips)2](NO3)·2H2O (III). The structure of I and II are monoclinic, space groupP21/c, with, I,a=15.980(4),b=11.531(2),c=16.170(2)Å;=104.20(2)°,Z=4,R=0.032; II,a=16.109(5),b=11.480(3),c=16.135(6)Å;=104.15(2)°,Z=4,R=0.069. Compound III is also monoclinic, space groupP21/c witha=12.173(5),b=15.619(5),c=15.338(8)Å;=111.40(4)°,Z=4,R=0.059. In these complexes the ligand is tridentate via carbonylic oxygen, semicarbazone and pyridine nitrogens forming each two five membered chelate rings with the metal in a distorted octahedral geometry. 相似文献
6.
Leandro Coghi Maurizio Lanfranchi Giancarlo Pelizzi Pieralberto Tarasconi 《Transition Metal Chemistry》1978,3(1):69-76
Summary Crystals of the title compounds are both monoclinic, with unit cell dimensions:a = 9.293(5),b = 10.122(5),c = 16.737(7) Å. = 103.44(3)°,Z = 4, space groupP21/c for the cobalt derivative;a = 13.1ß5(7),b = 17.546(ß),c = 6.871(3) Å, = 107.01(4)°Z = 4, space groupP21/n for the copper derivative. The structures were solved from diffractometer data by the heavy-atom technique for the first compound and by direct methods for the second compound. Refinement by block diagonal least-squares gaveR = 5.9% for 3511 independent reflections andR = 8.8% for 2885 independent reflections for the cobalt and copper compound respectively. In both compounds the biguanide moiety behaves as a bidentate chelating ligand in a symmetrical tautomeric form, but it is deprotonated in the octahedral cobalt compound and neutral in the square planar copper compound. 相似文献
7.
Paolo Domiano Amos Musatti Mario Nardelli Corrado Pelizzi Giovanni Predieri 《Transition Metal Chemistry》1979,4(6):351-354
Summary The x-ray crystal structure of the title complex is described Crystals are monoclinic, space groupP21/n, with unit-cell dimensions:a=18.070(2),b=13.471(2),c=6.788(2) Å,=94.70(1),Z=4. The structure was solved from diffractometer data by Patterson and Fourier methods and refined by least-squares techniques toR=5.0% for 2451 independent reflections. It consists of complex molecules, in which the copper atom square planar coordination comprises the chlorine atom, Cu-Cl=2.240(3) Å, and the organic ligand which acts as terdentate through the oxygen atom [Cu-O=1.948(3) Å] and a nitrogen atom, [Cu-N=1.933(5) Å] from the hydrazidic chain and the oxygen atom, [Cu-O = 1.894(4) Å] from the pyridoxal group. 相似文献
8.
Bacchi Alessia Pelizzi Giancarlo Minardi Giovannina Pistuddi Angelo M. Solinas Costantino Chelucci Giorgio 《Transition Metal Chemistry》2002,27(3):274-278
Metal complexes of general formula M(L)X2 and M(L)X3 [L = (4S,5S)-2,2-dimethyl-4,5-bis{6-[(4,5-dihydro-4-(S)-(1-methylethyl)oxazol-2-yl)pyridin-2-yl]}-1,3-dioxolane] were obtained by reacting, respectively, CoII, CuII, NiII, and ZnII nitrate salts and the RhIII chloride salt, with a chiral C2-symmetric bis(oxazolinylpyridinyl)dioxolane (L) ligand, in MeOH/CHCl3 solution. A single crystal X-ray analysis was carried out on [Ni(L)(OH2)2](NO3)2 · 2H2O and the molecular structure of L was also determined. In the free ligand the two symmetric arms are essentially planar and oriented nearly perpendicular to the dioxolane average plane. In the Ni complex one seven-membered and two five-membered chelation rings are formed. The metal atom also lies on the C2 axis, and two symmetry-related water molecules complete the octahedral coordination environment. Both compounds crystallize in chiral space groups; the ligand crystallizes in orthorhombic system, space group C 2 2 21, Z = 4; the nickel complex crystallizes in tetragonal system, space group P 43 21 2, Z = 4. 相似文献
9.
Albertin G Antoniutti S Bacchi A Bordignon E Miani F Pelizzi G 《Inorganic chemistry》2000,39(15):3283-3293
Depending on experimental conditions and the nature of the hydrazine, the reactions of ReCl3P3 [P = PPh(OEt)2] with RNHNH2 (R = H, CH3, tBu) afford the bis(dinitrogen) [Re(N2)2P4]+ (2+), dinitrogen ReClN2P4 (3), and methyldiazenido [ReCl(CH3N2)(CH3NHNH2)P3]+ (1+) derivatives. In contrast, reactions of ReCl3P3 [P = PPh(OEt)2, PPh2OEt] with arylhydrazines ArNHNH2 (Ar = Ph, p-tolyl) give the aryldiazenido cations [ReCl(ArN2)(ArNHNH2)P3]+ (4+) and [ReCl(ArN2)P4]+ (7+) and the bis(aryldiazenido) cations [Re(ArN2)2P3]+ (5+, 6+). These complexes were characterized spectroscopically (IR; 1H and 31P NMR), and the BPh4 complexes 1, 2, and 7 were characterized crystallographically. The methyldiazenido derivative [ReCl(CH3N2)(CH3NHNH2)(PPh(OEt)2)3][BPh4] (1) crystallizes in space group P1 with a = 15.396(5) A, b = 16.986(5) A, c = 11.560(5) A, alpha = 93.96(5) degrees, beta = 93.99(5) degrees, gamma = 93.09(5) degrees, and Z = 2 and contains a singly bent CH3N2, group bonded to an octahedral central metal. One methylhydrazine ligand, one Cl- trans to the CH3N2, and three PPh(OEt)2 ligands complete the coordination. The complex [Re(N2)2(PPh(OEt)2)4][BPh4] (2) crystallizes in space group Pbaa with a = 23.008(5) A, b = 23.367(5) A, c = 12.863(3) A, and Z = 4. The structure displays octahedral coordination with two end-on N2 ligands in mutually trans positions. [ReCl(PhN2)(PPh(OEt)2)4][BPh4] (7) crystallizes in space group P2(1)/n with a = 19.613(5) A, b = 20.101(5) A, c = 19.918(5) A, beta = 115.12(2) degrees, and Z = 4. The structure shows a singly bent phenyldiazenido group trans to the Cl- ligand in an octahedral environment. The dinitrogen complex ReClN2P4 (3) reacts with CF3SO3CH3 to give the unstable methyldiazenido derivative [ReCl(CH3N2)P4][BPh4]. Reaction of the methylhydrazine complex [ReCl(CH3N2)(CH3NHNH2)P3][BPh4] (1) with Pb(OAc)4 at -30 degrees C results in selective oxidation of the hydrazine, affording the corresponding methyldiazene derivative [ReCl(CH3N=NH)(CH3N2)P3][BPh4] (8). In contrast, treatment with Pb(OAc)4 of the related arylhydrazines [ReCl(ArN2)(ArNHNH2)P3][BPh4] (4) [P = PPh(OEt)2] gives the bis(aryldiazenido) complexes [Re(ArN2)2P3][BPh4] (5). Possible protonation reactions of Br?nsted acids HX with all diazenides, 1, 4, 5, 6, and 8, were investigated and found to proceed only in the cases of the bis(aryldiazenido) complexes 5 and 6, affording, with HCl, the octahedral [ReCl(ArN=NH)(ArN2)P3][BPh4] or [ReCl(Ar(H)NN)(ArN2)P3][BPh4] (10) (Ar = Ph; P = PPh2OEt) derivative. 相似文献
10.
Vesna Radulovi? Alessia Bacchi Giancarlo Pelizzi Du?an Sladi? Ilija Br?eski Katarina Andjelkovi? 《Monatshefte für Chemie / Chemical Monthly》2006,23(3):681-691
Complexes of Pt(II), Pd(II), and Ni(II) with the condensation derivative of 2-(diphenylphosphino)benzaldehyde and semioxamazide
were synthesized, characterized, and their antimicrobial activity was evaluated. The ligand and the complexes were characterized
by spectroscopic methods with the particular accent on NMR spectral analysis. For the palladium(II) complex, the crystal structure
was determined by X-ray analysis. In all the complexes the ligand is coordinated as a tridentate via a P, N, O donor set. The Pd(II) and Pt(II) complexes have a square planar geometry, whereas the geometry of the Ni(II) complex
is tetrahedral. The ligand showed antibacterial and antifungal activity, which was enhanced upon complexation. 相似文献