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1.
Crystal structures were determined for two new derivatives of heteroligand complexes of Cu(C5HF6O2)2 with nitroxyl radicals derived from 3-imidazoline: Cu(C5HF6O2)2(C13H18N3O) (I) and Cu(C5HF6O2)2(C8H15N2O) (II). The unit cell parameters for I are as follows: a=10.555(3), b=15.505(5), c=18.509(6) Å, V = 3029(1) Å3, Z=4, dcalc=1.57 g/cm3, space group P212121. The unit cell parameters for II are as follows: a=16.018(3), b=15.886(3), c=19.665(4) Å, V = 5004(1)Å3, Z=8, dcalc=1.68 g/cm3, dexp=1.68 g/cm3, space group P212121. The structure of I is molecular. The coordination of the copper ion is a trigonal bipyramid formed by two oxygen atoms of the (hfac) ions and the nitrogen atom of the imidazoline heterocycle in the equatorial plane [Cu–O, 1.91(7), 2.242(7) Å, Cu–N, 2.010(7) Å] and the other oxygen atoms of the (hfac) anion in the axial positions [Cu–O, 1.940(6), 1.963(6) Å]. Complex II is polymeric. The two crystallographically independent Cu(hfac)2 fragments are linked in a chain by means of two L2 ligands. The coordination of the copper ions is a square bipyramid, whose equatorial plane is formed by the oxygen atoms of the (hfac) anion [Cu–O, 1.89(1)–2.03(1) Å]. The axial positions are occupied by nitrogen atoms [Cu–N, 2.52(1), 2.40(1) Å] and an oxygen atom of the NO fragment [Cu–O, 2.96(1), 2.67(1) Å] of different L2 ligands. The ...Cu(hfac)2–L2–Cu(hfac)2–L2... chains in the unit cell are located at two levels (x1/4 and 3/4).Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences. Translated from Zhurnal Strukturnoi Khimii, Vol. 34, No. 2, pp. 126–133, March–April, 1993. 相似文献
2.
Skorik Yu. A. Romanenko G. V. Neudachina L. K. Vshivkov A. A. 《Russian Journal of Coordination Chemistry》2001,27(11):796-802
Crystals of [Cu(o-Andp)(H2O)2] · 2H2O (where o-Andp2–is -anisidine-N,N-di-3-propionate) were synthesized and studied using X-ray diffraction analysis. The crystals are triclinic: a= 12.063(1) Å, b= 12.483(3) Å, c= 13.586(2) Å, = 91.29(1)°, = 111.67(1)°, = 104.00(1)°, V= 1830.5(5) Å3, space group P
, Z= 2, and R= 0.0528 for 5965 reflections with I2(I). The two crystallographically independent complexes are isostructural. The tetragonal–bipyramidal coordination of copper(III) involves three O atoms, the N atom of the tetradentate ligand o-Andp2–, and two O atoms from water. The aminodipropionate group of the ligand (average Cu–O 1.939 Å and Cu–N 2.051 Å) and one of the coordinated water molecules (Cu–O(w) 1.991 Å) lie in the equatorial plane. The second water molecule (Cu–O(w) 2.32 Å) and the methoxy O atom of o-Andp2–(Cu–O 2.37 Å) are in the apical positions of the bipyramid. 相似文献
3.
Tong Ming-Liang Chen Xiao-Ming Sun Zi-Ming Hendrickson David N. 《Transition Metal Chemistry》2001,26(1-2):195-197
The synthesis and characterization of the oxo-centered carboxylato-bridged trinuclear iron(III) complex, triaquahexakis(2-betaine)(3-oxo)triiron(III) perchlorate heptahydrate are described. X-ray crystallography shows that the FeIII atom in the complex has a slightly distorted octahedral geometry, coordinated by four oxygen atoms from different betaine ligands [Fe—;O = 2.009(3) 2.034(3) Å], one aqua ligand [Fe—O = 2.028(4) and 2.031(3) Å] and the central 3-oxo atom [Fe—O = 1.917(2) and 1.917(3) Å]. The central oxygen is ideally coplanar with the plane of the three metal atoms. Magnetic susceptibility data (4–320 K) show the presence of an antiferromagnetic exchange interaction with a coupling constant of J = –20.2 cm–1. 相似文献
4.
Novel tetranuclear copper complexes, Cu4(OH)2(ClO4)3 (HA)·H2O (1) and Cu4(ClO4)5(H3B)·3H2O (2), were synthesized by reacting 1,5-bis(1-phenyl-3-methyl-5-pyrazolone-4)-1 ,5-pentanedione with 1,3-propanediamine and 2-hydroxyl-1,3-propanediamine in the presence of a template reagent copper ion. New [2+2] type open cyclic multidentate ligands are also obtained from the reaction (H4A and H6B stand for new compounds from 1,3-propanediamine and 2-hydroxyl-1,3-propanediamine, respectively). They each contain five C = O, three C = N and one NH2 groups. The complexes were characterized by elemental analyses, conductivity, FT-i.r. (micro-i.r., deconvolution technique), FAB-MS, e.s.r., electronic spectra and extended X-ray absorption fine structure (EXAFS). Copper ions in (1) are basically four coordinate with tetragonal geometry. The average coordination bond distances of Cu–N and Cu–O are 1.91 Å and 2.05 Å. In (2), copper ions are primarily five coordinate with square-based pyramidal geometry. The average coordination bond distances of Cu–N and Cu–O are 1.93Å and 2.08Å. Four copper atoms in molecules may be arranged tetragonally. Both the ligand field and the coordination bonds in complex (1) are stronger than those in (2). Investigations on variable temperature susceptibilities show that some antiferromagnetic exchange interaction exist in the complexes. The plots of –1 versus T obey the Curie-Weiss law only at low temperature. Preliminary results of a bioassay indicate that the two complexes have some antitumour activity in vitro. 相似文献
5.
Chan-Chen Su Hwei-Lien Tsai Shiou-Rong Li Sne-Lein Wang Chih-Yi Cheng 《Transition Metal Chemistry》1990,15(6):454-458
Summary The x-ray crystal structure of tris(N-methylformamide) (N, N, N', N'-tetramethylethylenediamine)copper(II) perchlorate has been determined using three-dimensional x-ray diffraction data. The complex crystallizes in space group P21/c with Z=4. The cell dimensions are=8.255(3),b=17.951(6),c=16.541(4) Å, and =91.03(2)°. Least-squares refinement of the structure has yielded a final R value of 4.52% for 2108 independent reflect ions. The square pyramidal structure consists ofN, N, N', N'-tetramethylethylenediamine and twoN-methylformamide ligands forming a basal square plane with Cu–N bond lengths of 2.029(5) and 2.033(5) and Cu–O 1.981(4) and 1.985(4) Å, and a thirdN-methylformamide on the apex with a Cu–O distance of 2.181(4)Å. Each of the molecular plances of the three N-methylformamides lies nearly coplanar with thexy, yz andxz molecular coordination planes. The bonding properties of the title compound and its i.r. and uv-vis spectra are discussed with reference to the structure. 相似文献
6.
Novitskii G. Shova S. Voronkova V. K. Korobchenko L. Gdanec M. Simonov Yu. A. Turte K. 《Russian Journal of Coordination Chemistry》2001,27(11):791-795
A new copper carboxylate polymer with cyanoacetate anion as a ligand was synthesized and studied using X-ray diffraction, IR, and EPR spectroscopy. The crystal is tetragonal: a= 14.702(2) Å, c= 13.470(3) Å, Z= 8, space group I41/a, and R= 0.0634. The copper atoms in the centrosymmetric dimeric fragment have a square-pyramidal surrounding with the CuO4N coordination core and are joined through four bidentate bridging anions of cyanoacetic acid Cu(1)"–O(1A) 1.931(4) Å, Cu(1)"–O(1B) 1.926(4) Å, Cu(1)–O(2B) 2.018(3) Å, Cu(1)–O(2A) 2.036(4) Å, and Cu(1)–N(1A)" 2.206(5) Å). The Cu···Cu" distance in the dimer is 2.709 Å. The copper atom is extended from the mean equatorial plane toward the axial nitrogen atom by 0.23 Å. EPR data confirm strong antiferromagnetic interaction (2J –275 cm–1) between the copper(II) ions of the dimeric fragment, whereas the interaction between the dimers is significantly weaker (J< 0.3 cm–1). 相似文献
7.
Rajendiran Thekkel M. Kannappan Ramu Mahalakshmi Rajaram Venkatesan Rangarajan Sambasiva Rao Pillutla Govindaswamy Lakshmanan Velmurugan Devadasan 《Transition Metal Chemistry》2003,28(6):644-649
The synthesis, X-ray and e.p.r. spectral studies of a 3d–4f couple are described here. The crystal structure of [Cu(salbn)Gd(NO3)3·H2O], (2), salbn = N,N-butylenebis(salicylideaminato), has been determined by X-ray crystallography. Compound (2) crystallizes in the monoclinic system, space group p21/n, with a = 9.025(1), b = 22.912(1), c = 12.790(1) Å, = 99.36(1), Z = 4. The deviations of the four coordinating atoms (O(1)O(2)N(1) and N(2) of salbn and the copper atom is displaced from the plane in spite of the lack of any apical ligand. The gadolinium(III) ion is nine-coordinated by the two oxygen atoms of the salbn moiety, three bidentate nitrate ions and one water molecule. The geometry of GdIII can be described as a square antiprism, in which compound CuII and GdIII are bridged by the two phenolic oxygens of salbn. The CuII–GdIII distance is 3.269(1) Å. The bridging core CuO2Gd is a butterfly shape. Significant distortion was observed for the complex having the larger diamino string. The title compound exhibits seven e.s.r. transitions with |D| = 0.0467 cm–1, which demonstrates the existence of zero field splitting. This outcome indicates that compound (2) consists of a perfectly isolated dinuclear Cu–Gd core and steric bulk alters the dihedral angle in the Cu–O–Gd bridge. 相似文献
8.
Solov'ev L. A. Vasil'ev A. D. Golovnev N. N. 《Russian Journal of Coordination Chemistry》2002,28(8):587-592
The complex salt [Cu4(SCN2H4)7(NO3)](NO3)(SO4) · 3.3H2O was synthesized via reaction of aqueous solutions of thiourea with copper nitrate at 80°C and studied using X-ray diffraction analysis. The conditions and reasons for the partial oxidation of thiourea to sulfate ions were established. The crystals are monoclinic: a = 12.6072(7) Å, b = 15.4265(8) Å, c = 22.108(1) Å, = 120.133(6)°, space group P21/c, Z = 4. The crystal structure consists of [Cu4(SCN2H4)7(NO3)]3+ complex cations, SO4
2–, and NO3
– anions, and molecules of the water of crystallization. Three types of coordination of the Cu atom were distinguished in the structure: trigonal (Cu–S 2.213–2.279 Å), tetrahedral (Cu–S 2.315–2.459 Å), and trigonal–pyramidal (3+1) (Cu–S 2.26–2.288, Cu–O 2.68 Å). The NO3 ligand was found to be orientationally disordered. 相似文献
9.
Murphy Brian Aljabri Moza Light Mark Hursthouse Michael B. 《Transition Metal Chemistry》2004,29(4):394-399
The crystal structure of bis(2,2-bipyridyl)monobenzoatocopper(II) nitrate hydrate, [Cu(bipy)2(O2CPh)][NO3]· H2O, (1) has been determined. The [Cu(bipy)2(O2CPh)]+ cation chromophore is basically five-coordinate, but with O(1), the second oxygen atom of the benzoato ligand, occupying the sixth coordinate position at a distance 2.696(2)Å, from the copper. This suggests a (4 + 1 + 1*) coordination, involving a distorted stereochemistry, with a CuN4OO chromophore. O(2) is located at a distance 2.009(2)Å from the copper. The two oxygens, O(1) and O(2), therefore occupy cis positions of the distorted octahedral coordination sphere and the coordinated benzoate is a highly asymmetric, bidentate ligand with O = 0.687(2)Å and Cu—OMEAN= 2.353(2)Å. The two nitrogens, N(1) and N(3), located in positions trans to the oxygen sites, at distances Cu—N(1)= 2.148(2)Å and Cu—N(3)= 2.058(2)Å[Cu—Nmean/in= 2.103(2)Å, N1,3= 0.090(2)Å] are slightly longer than the bonds to the two mutually trans related 'axial' nitrogens, Cu—N(2)= 1.987(2)Å and Cu—N(4)= 1.977(2)Å. The 'equatorial' angles
1,
2 and
3 have values 147.34(8), 93.29(9) and 105.39(9) respectively. The back-angle,
3, of 105.39(9)° is unique for a bipy complex, containing a carbonyl-containing oxoanion in such series. The asymmetric nature of the benzoato ligand is further evidence of the static nature of such complexes. The complex also involves a hydrogen bonding network, linking the O(6) of the nitrate to H(2)W of the water molecule at a distance 2.052(6)Å and H(1)W to the long-bonded O(1) of the benzoato ligand, at a distance of 1.804(12)Å. 相似文献
10.
Summary The crystal and molecular structure of bis(1-methylimidazole)bis(perchlorato)bis(pyridineN-oxide)copper(II) have been determined using three-dimensional x-ray diffraction data. The complex crystallizes in space group P21/c with Z=2. The cell dimensions area=9.355(3),b=14.363(4),c=9.698(4) Å, and =106.40(3)o. Least-squares refinement of the structure has yielded a final R value of 0.049 for 1235 independent reflections. The centrosymmetric structure consists oftrans pairs of 1-methylimidazole and pyridineN-oxide figands forming a square planar geometry with Cu–N and Cu–O bond lengths of 1.963(4) Å and 1.948(4) Å, respectively. The two perchlorate ions are located above and below the square plane with Cu–O distances of 2.590(5) Å. The uv-vis and i.r. spectra and bonding properties of the title compound are discussed with reference to the structure. 相似文献
11.
Andreas Roodt Johann G. Leipoldt Stephen S. Basson Izak M. Potgieter 《Transition Metal Chemistry》1990,15(6):439-442
The crystal structure of (Me4N)3[WO(CN)4(NCS)]·NaNCS was determined from three-dimensional x-ray diffraction data. The dark blue crystals are monoclinic, space group C2/m, with cell dimensions a=13.105(4), b=12.688(2), c=18.871(3) Å, =100.4(8)°, z=4 and D=1.46 g cm–3. Anisotropic refinement of 1333 observed reflections converged to R=0.068. The [WO(CN)4(NCS)]3– ion is a distorted octahedron with the tungsten atom displaced by 0.35 Å out of the plane formed by the four cyano ligands, towards the oxo ligand. The coordinated thiocyanate ligand is bonded to the tungsten atomvia the nitrogen atomtrans to the oxo ligand. Bond distances found: W–CNav=2.14(3), W–O=1.61(2) and W–NCS=2.23(2) Å. The compound crystallizes as an adduct with an additional thiocyanate anion, ionically bonded to a severely disordered sodium cation. The results correlate with available data from similar complexes. 相似文献
12.
Lobana Tarlok S. Mahajan Ranjana Castineiras Alfonso 《Transition Metal Chemistry》2001,26(4-5):440-444
Complexes of CuI with tertiary phosphine chalcogenides are described. CuI reacts with Ph3PS in MeCN/CH2Cl2 to form {CuI(Ph3PS)(MeCN)} and CuCl reacts with 1,2-ethylene-bis(tertiary phosphine selenide) {dpeSe2} in MeCN to yield {CuCl(dpeSe2)}. Both compounds exist as halogen-bridged centrosymmetric dimers: [Cu2(-I)2-(Ph3PS)2(MeCN)2] (1) and [Cu2(-Cl)2(dpeSe2)2] (2) respectively. Compound (1) has almost symmetric Cu—I bonds, d(Cu—I) = 2.6503(8) Å and d(Cu—I) = 2.7196(9) Å, and each Cu is further bonded to a S atom [d(Cu—S) = 2.3444(13) Å] from Ph3PS and to a N atom [d(Cu—N) = 2.030(5) Å] from MeCN. Compound (2) has unequal Cu—Cl bonds, 2.6390(19) and 2.2806(18) Å and nearly equal Cu—Se bonds [2.4042(11) and 2.4060(11) Å]. The geometry about each Cu center in both cases is distorted tetrahedral. The Cu—Cu bond distance in (2) is 3.249(2) Å as compared with 3.4141(16) Å in (1). MeCN is bonded strongly to CuI as the excess of Ph3PS failed to remove it from the coordination sphere. Compound (2) represents the first structurally characterised example of copper(I) with a bis(tertiary phosphine selenide) (dpeSe2) acting as a bridging ligand. 相似文献
13.
Absract—Diaqua(2.2.2-Cryptand)strontium dichloride trihydrate [Sr(2.2.2-Crypt)(H2O)2]2+ · 2Cl– · 3H2O (I) was prepared and studied by X-ray diffraction. The triclinic structure of I (space group P
, a = 9.152 Å, b = 10.140 Å, c = 15.219 Å, = 88.84°, = 88.19°, = 87.62°, Z = 2) was solved by the direct method and refined by full-matrix least-squares calculations in the anisotropic approximation to R = 0.050 for 4188 independent reflections (CAD4 automated diffractometer, CuK
radiation). The structure contains the [Sr(2.2.2-Crypt)(H2O)2]2+ host–guest cation. The Sr2+ cation resides in the 2.2.2-cryptand cavity and is coordinated by all eight heteroatoms (6O + 2N) of the cryptand ligand and by two O atoms of water molecules. The Sr2+ coordination polyhedron (C.N. 10) is a highly distorted dibase-centered two-cap trigonal prism. The crystal structure of I contains a branched system of ion–ion (intermolecular) hydrogen bonds O(w)–H···Cl–, which connect the complex cations, the Cl– anions, and the crystal water molecules to form infinite thick layers parallel to the yz plane. 相似文献
14.
The diaqua(1,10-diaza-18-crown-6)(tetrafluorosuccinato-O)barium complex [Ba(DA18C6)(C4F4O4)(H2O)2] (I) is synthesized and studied using X-ray diffraction analysis: space group P21/n, a = 16.342 Å, b = 8.989 Å, c = 17.087 Å, = 107.09°, Z = 4. The structure was solved by the direct method and refined by the full-matrix least squares method in anisotropic approximation to R = 0.075 for all 3515 unique reflections (CAD4 automated diffractometer, MoK
). Complex I exists in the crystal as individual host–guest molecules of the aforementioned composition. The Ba2+ cation (coordination number 9) is located in the void of the DA18C6 macrocycle and is coordinated by its six O and N heteroatoms. It is also coordinated by the O atom of the tetrafluorosuccinate ligand and the O atom of the water molecule on one side of the macrocycle and by the O atom of the second water molecule on the other macrocycle side. The DA18C6 ligand has a crown conformation with approximate D
3d
symmetry. The complex molecules in the crystal are combined into infinite two-dimensional layers by intermolecular hydrogen bonds. 相似文献
15.
Stephen S. Basson Johann G. Leipoldt Andreas Roodt Walter Purcell 《Transition Metal Chemistry》1987,12(1):82-84
Summary The structure of [S(CH2CH2)3S]2[Re2O3(CN)8]·4H2O has been determined from three-dimensional x-ray diffraction data. The blue crystals are monoclinic, space group P21/c, with cell dimensionsa=9.431(2),b=10.879(2),c=16.217(3)Å, =110.84(2)°,Z=2 andD
m=2.11 gcm–3. Anisotropic refinement by least-squares methods of 2483 observed reflections converged toR=0.050.The centrosymmetric binuclear anion has a linear O=Re–O–Re=O grouping with an eclipsed configuration for the cyano ligands. Bond distances: Re–O (terminal)=1.69(1), Re–O (bridging)=1.921(1) and Re–Cav=2.12(2)Å. Each Re atom is displaced by 0.11(2)Å towards the terminal oxygen atom giving a slight square-pyramidal distortion of the octahedral environment. The ring-constrained cation has C–Sav=1.82(2)Å with averaged bond angles C–S–C=101(1) and S–C–C=113(1)°. 相似文献
16.
Summary From a survey of spectroscopic and structural data of six corresponding 2-hydroxybenzamides and 2-hydroxythiobenzamides (amide, N-methylamide, N,N-dimethylamide, piperidide, morpholide, 2,6-dimethylpiperidide) remarkable similarities between O(N)-H ... O and O(N)-H ... S hydrogen-bonds are obtained, concerning both, hydrogen-bond patterns and hydrogen-bond strengths. In dilute solution the OH groups of all compounds are intramolecularly associated to the (thio)carbonyl O (S) atoms with distinctly larger hydrogen-bond strengths for primary and secondary amides [
(O-H)=2950–3020 cm–1, (OH)=12.16–11.99 ppm] and thioamides [
(O-H)=2960–3000 cm–1, (OH)=11.65–11.13 ppm], than for tertiary amides [
(O-H)=3200–3250 cm–1, (OH)=9.95–8.95 ppm] and thioamides [
(O-H)=3245–3330 cm–1, (OH)=8.09–7.06 ppm]. In the solid state, the OH groups of the primary and secondary (thio)amides are also engaged in rather strong intramolecular O-H ... O=C [O ... O=2.51 Å,
(O-H)=2700–2750 cm–1] and O-H ... S=C [O ... S=2.90–2.94 Å,
(O-H)=2700–2840 cm–1] hydrogen-bonds; thetrans-NH groups of the primary (thio)amides and the NH groups of the secondary (thio)amides connect the molecules to N-H ... O-H [N ... O=2.93–3.10 Å,
(N-H)=3319–3407 cm–1] hydrogen-bonded chains; the remainingcis-NH groups of the primary (thio)amides give rise to eight-membered cyclic dimers via N-H ... O=C [N ... O=2.93 Å,
(N-H)=3226 cm–1] and N-H ... S=C [N ... S=3.46–3.47 Å,
(N-H)=3233–3277 cm–1] hydrogen-bonds. Contrary, the OH groups of the tertiary (thio)amides are intermolecular associated in the solid state and link the molecules to O-H ... O=C [O ... O=2.63–2.75 Å,
(O-H)=3075–3135 cm–1] and O-H ... S=C [O ... S=3.18–3.26 Å,
(O-H)=3130–3190 cm–1] hydrogen-bonded chains.
O-H ... O(S)-Wasserstoffbrückenbindungen in 2-Hydroxy(thio)benzamiden. Ein Überblick über spektroskopische und strukturelle Daten
Zusammenfassung Aus einer Zusammenstellung von spektroskopischen und strukturellen Daten von sechs entsprechenden 2-Hydroxybenzamiden und 2-Hydroxythiobenzamiden (Amid, N-Methylamid, N,N-Dimethylamid, Piperidid, Morpholid, 2,6-Dimethylpiperidid) ergeben sich bemerkenswerte Analogien zwischen O(N)-H ... O und O(N)-H ... S H-Brücken, die sowohl die H-Brücken-Muster als auch die H-Brücken-Stärken betreffen. In verdünnter Lösung sind die OH-Gruppen aller Verbindungen intramolekular mit den O(S)-Atomen der (Thio)Carbonylgruppen assoziiert, wobei die H-Brücken bei den primären und sekundären Amiden [ (O-H)=2950–3020 cm–1, (OH)=12.16–11.99 ppm] und Thioamiden [ (O-H)=2960–3060 cm–1, (OH)=11.65–11.13 ppm] deutlich stärker sind, als bei den tertiären Amiden [ (O-H)=3200–3250 cm–1, (OH)=9.95–8.95 ppm] und Thioamiden [ (O-H)=3245–3330 cm–1, (OH)=8.09–7.06 ppm]. Im Festkörper weisen die primären und sekundären (Thio)Amide ebenfalls sehr starke intramolekulare O-H ... O=C [O ... O=2.51 Å, (O-H)=2700–2750 cm–1] und O-H ... S=C [O ... S=2.90–2.94 Å, (O-H)=2700–2840 cm–1] H-Brücken auf; dietrans-NH-Gruppen der primären (Thio)Amide und die NH-Gruppen der sekundären (Thio)Amide verknüpfen die Moleküle über N-H ... O-H H-Brücken [N ... O=2.93–3.10 Å, (N-H)=3318–3407 cm–1] zu Ketten; die verbleibendencis-NH-Gruppen der primären (Thio)Amide bilden zyklische, über N-H ... O=C [N ... O=2.93 Å, (N-H)=3226 cm–1] und N-H ... S=C [N ... S=3.46–3.47 Å, (N-H)=3233–3277 cm–1] H-Brücken gebundene, 8-Ring-Dimere. Im Gegensatz dazu sind die OH-Gruppen der tertiären (Thio)Amide im Festkörper intermolekular assoziiert und verknüpfen die Moleküle über O-H ... O=C [O ... O=2.63–2.75 Å, (O-H)=3075–3135 cm–1] und O-H ... S=C [O ... S=3.18–3.26 Å, (O-H)=3130–3190 cm–1] H-Brücken zu Ketten.相似文献
17.
Hsiu-Ju Chiu Chan-Cheng Su Sue-Lein Wang Fen-Lin Liao 《Transition Metal Chemistry》1994,19(4):413-417
Summary Mixed ligand diglycinatocopper(II) complexes of the Cu(glygly)L·nH2O type, where glygly stands for [NH2-CH2 CONCH2CO2]2– and L for imidazole (n = 1.5), N-methylimidazole (n = 1), 2-methylimidazole (n = 2), 4-methylimidazole (n = 2), 4-phenylimidazole (n = 2), N-acetylhistamine (n = 2) and NH3 (n = 2), were prepared and characterized by elemental analyses, i.r., vis. and e.p.r. spectroscopic measurements. The molecular structure of [Cu(glygly)(achmH)]·2H2O (achmH = acetylhistamine) was determined using three dimensional XRD data. The structure consists of distorted square planar [Cu(glygly)-(achmH)] units interconnected via the peptide oxygen at the apex to complete a square pyramidal structure, Cu—O-(peptide) 2.477(2) Å. The H2O molecules, not binding directly to the copper ion, involve in intermolecular hydrogen bonding with the copper units. The dianionic glygly ligand and the imidazole ring bind strongly to the central copper ion with Cu—N(amino) 2.045(6) Å, Cu—N-(peptide) 1.891(5) Å, Cu—O(carboxylate) 2.001(4) Å and Cu—N(imidazole) 1.956(5) Å. The dihedral angle between the imidazole nucleus and the CuN3O xy plane is 6.0°. Similar structures with a CuN3O coordination plane are proposed for the imidazole complexes, based on spectroscopic data. The bonding properties of the glygly ligand and the unidentate imidazole ligands are elucidated and discussed with reference to the electronic structures of the complexes deduced from Gaussian analyses. 相似文献
18.
A new macrocyclic ligand, 1,4,7,10-tetrakisbenzyl-1,4,7,10-tetraazacyclododecane (L) and its three new divalent metal complexes of general formula: M(NO3)2(L)nH2O [M = Co(1), Ni(2), n = 0; M = Cu(3), n = 1.5] have been synthesized and characterized by elemental analysis, i.r., EI mass spectra and molecular conductance. Complex (2) has been characterized by X-ray diffraction. In complex (2), the central NiII atom coordinatively bonds to four nitrogen atoms of the macrocyclic ligand and two oxygen atoms of nitrate anion, to form a distorted octahedron. X-ray diffraction indicated that the bonds Ni–N(1), Ni–N(2), Ni–N(3) and Ni–N(4) are of almost equal length, i.e. 2.11(1), 2.12(1), 2.10(1) and 2.17(1)Å, respectively. Bond lengths of Ni–O(1) and Ni– O(2) are 2.11(1) and 2.10(1)Å. Preliminary pharmacological tests show that these complexes have high antitumor activity towards HL-60 tumor cell lines. 相似文献
19.
Bezrukavnikova I. M. Polynova T. N. Poznyak A. L. Stopolyanskaya L. V. 《Russian Journal of Coordination Chemistry》2002,28(3):212-216
The cobalt(III) complexes with tridentate ethylenediamine-N,N"-diacetate ions (Edda2–) and additional ligands, namely, diethylenetriamine (Dien) or ethylenediamine (En) and cyanide ions, were synthesized. As follows from X-ray diffraction analysis of [Co(Edda)(Dien)]ClO4· H2O (monoclinic crystals with a = 9.243 (2) Å, b = 14.167 (4) Å, c = 13.046 (3) Å, = 91.19 (2)°, Z = 4, space group P21/c), the secondary N atom of the Dien ligand occupies the trans-position relative to the N atom of the Edda2– ligand, which contains a free acetate group. Two fac-isomers of [Co(Edda)(En)(CN)] with the CN– ion in the cis- and trans-positions relative to the oxygen atom of the carboxyl group were isolated, and the structure of the trans-(O,CN)-[Co(Edda)(En)(CN)]· 2H2O was determined: monoclinic crystals with a = 9.136 (3) Å, b = 15.484 (3) Å, c = 10.564 (3) Å, = 110.67 (5)°, Z = 4, space group P21/c. 相似文献
20.
The reaction of AsPh4[TcNX4] (X=Cl or Br) with naked F– in MeCN solution has been shown by e.p.r. spectroscopy to result in the facile substitution of the halo ligands by fluoride. Addition of six equivalents of NBu4F·3H2O has provided, for the first time, direct evidence for the formation of the six-coordinate [TcNF5]2– in solution. An e.p.r. study of ligand exchange of Cs2[TcNCl5] (4 × 10–2 – 5 × 10–4 mol dm–3) in 28.6 mol dm–3 aqueous HF has shown that the distribution of the five [TcNFnCl4–n]– (n = ;0–4) species is concentration dependent, with the formation of [TcNF4]– being favoured by dilution. 相似文献