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1.
Summary A new platinum complex of 1-methyl-5-nitroimidazole has been obtained and characterized by elemental analysis, i.r. and n.m.r. spectroscopy. The structure of [PtI2-(C4 H5N3O2)2] has been determined by single-crystal X-ray diffraction. The crystals are triclinic: P1, a = 15.640(3), b = 12.617(2), c = 6.701(1) , = 102.77(5), = 101.15(5), = 100.71(5)°, V = 1228.6(3) 3, Z = 3, Dx = 2.851(6) Mg m–3, (MoK ) = 0.71069 , = 12.85 mm, F(000) = 948, final R = 0.038 for 2859 reflections. The complex consists of monomeric PtI2(1-methyl-5-nitroimidazole)2 units. The coordination geometry is square-planar. The two 1-methyl-5-nitroimidazole ligands are trans coordinated to platinum.  相似文献   

2.
Crystals of the Cs+ Pic (B15C5) complex (Pic=picrate; B15C5=benzo-15-crown-5) (M r =629.3) are yellow prisms which belong to the triclinic space groupP witha=7.377(4),b=11.372(2),c=14.806(2) , =90.31(1), =91.06(2), =108.32(2)0,Z=2,D x =1.77, andD m =1.77 g cm–3. FinalR=0.055 for 3575 observed reflections out of a total of 4004 measured reflections. Cesium forms a 1:1 anion paired complex with B15C5 like sodium rather than a charge separated sandwich structure as found for potassium and expected for cesium in view of the ion-cavity radius concept. The Cs cation is 9-coordinate involving the five crown oxygens (Cs...O, 3.00(1) to 3.24(1) ), the phenoxide (Cs...O, 3.03(1) ) and anortho nitro group oxygen (Cs...O, 3.01(1) ) of the picrate counteranion and, uniquely, with two additional oxygens (Cs...O, 3.17(1) and 3.40(1) ) from apara nitro group of the picrate belonging to the adjacent molecule in the lattice. The Cs+ ion lies 2.07 out of the mean plane formed by the crown oxygens. This system provides the first structural evidence that the interaction stoichiometry of an alkali cation with a cyclic multidentate ligand is not a function of the ion and cavity size alone but also of its Lewis acid strength as modified by the charge neutralizing anion. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82027.  相似文献   

3.
A new compound from the series of alkoxyketoiminates, Cu(II) bis-(2-methoxy-2,6-dimethyl-3-imino-5-heptanonate), has been synthesized and studied by X-ray crystallography. Crystal data for CuO4N2C20H36: a=10.154(1), b=9.921(1), c=11.684(2) , =96.17(1)°, space group P21/c, Z=2, dcalc =1.226 g/cm3, R=0.037. The structure is molecular and built from isolated trans-complexes. The copper atom has a plane square environment of two oxygen atoms (Cu–O 1.93 ) and two nitrogen atoms (Cu–N 1.90 ). The O–Cu–N chelate angle is 91.7°. The complex has an intramolecular hydrogen bond, N–H...O 2.16 , involving the alkoxy oxygen atom. The molecular packing in the crystal is close to that of copper(II) dipivaloylmethanate. The calculated van der Waals intermolecular interaction energies and thermogravimetric characteristics of the complexes are compared.  相似文献   

4.
An X-ray structure analysis of 1-(p-tolyl)-4-[4-(N-naphthalimido)butyl]piperazine (I) was carried out: a=9.551(3), b=13.775(3), á=8.917(4) , =103.96(3), =101.47(4), =92.60(3)°, V=1110.4(7) 3, Z=2,calc=1.279 g/cm3, =0.644 mm, space group P 1, 4239 nonzero reflections, R=0.056. The molecule is linear elongated. The p-tolyl and naphthalimide fragments are almost planar, while the piperazine cycle has a chair conformation. The long well-packed molecules form parallel and antiparallel chains with van der Waals interactions between them.  相似文献   

5.
An integrated Xray diffraction study was performed on polycrystals and single crystals of three new isostructural phases with general formula Ag4A2[M(NO2)4]3 (M = Pd, Pt; A = K, Rb). Data on the crystal structure solution (CAD4 diffractometer, MoK radiation, graphite monochromator = 2–30° are presented. In one crystallographically independent [M(NO2)4]2- complex anion, the planar square coordination of the central atom is completed to 4 + 2 by two oxygen atoms at a distance of 3.02–3.12 in the other anion, it is completed to 4 + 1 + 1 by an oxygen atom at a distance of 3.12–3.30 and an Ag+ cation at a distance of 3.04–3.11 . Part of the Ag+ cations form Ag - Ag dimers with a distance of 3.03–3.07. Crystalchemical analysis of known structures containing [Pd(NO2)4]2- complex anions was performed. It has been established that in none of the cases do any of the possible limiting configurations occur.  相似文献   

6.
This paper describes a new method for the synthesis of the -iminoketonate complex Pt(ktf)2 using 1,1,1-trifluoro-4-iminopentan-2-one as a bidentate ligand. An X-ray study has been performed on the polycrystals and single crystals of the compound. The single crystal X-ray diffraction analysis was carried out on a CAD-4 diffractometer (MoK radiation, /2 scan mode). Crystal data: a = 10.217(2), b = 10.231(2), c = 10.924(2) , = 83.12(3), = 63.38(3), = 70.77(3)°, V = 963.4(3) 3, space group P1, Z = 2, d calc = 1.721 g/cm3. The Pt atom has a distorted planar square environment; the average lengths of Pt–N and Pt–O coordination bonds coincide (1.97 ). The mean value of the chelate angle is 94.2°. The environment of Pt is completed to bipyramid by the hydrogen atoms of the neighboring molecules. The structure of the compound is molecular. The differently oriented molecules of the complex are linked into chains down the x axis with Pt...Pt distances of 5.10 . A comparative crystal-chemical analysis of the structures of Pt(ktf)2 and Pd(ktf)2 and their O,O-chelate analogs — Pt(II) and Pd(II) trifluoroacetylacetonates — has been carried out. An X-ray study of Pt(tfa)2 and Pd(tfa)2 has been accomplished, and crystal data are given.  相似文献   

7.
Synthesis of the complex [Rh(NO2)3(NH3)3] is described. The compound crystallizes as monoclinic colorless plates. Crystal data: a = 7.176(10), b = 10.407(2), c = 10.989(2) , = 93.27°, V = 819.3(2) 3, space group , Z = 4, d calc = 2.367 g/cm3. The structure is molecular and built of neutral complexes having cis-facial configuration. The unit cell of the crystal contains two independent complexes.  相似文献   

8.
Procedures for synthesis of the first nitrochloride complex of nitrosoruthenium(II), fac-K2[RuNO(NO2)2Cl3], are described and the mechanism of its formation is suggested. The compound was investigated by IR spectroscopy and X-ray phase and X-ray diffraction analyses. Crystal data for Cl3N3O5K2Ru: a = 7.050(1), b = 7.524(2), c = 10.125(2) , = 90.44(3), = 103.17(3), = 90.51(3)°, V = 522.9 3, space group , Z = 2, d calc = 2.589 g/cm3. The structure consists of the complex anions fac-[RuNO(NO2)2Cl3]2– and K+ cations. The complex crystallizes as triclinic plates and red orange prisms; it is well soluble in water, not readily soluble in KCl solutions, and insoluble in ethanol and acetone; the complex is stable when stored in air.  相似文献   

9.
The results of structural studies of the synthetic analog of the radtkeite mineral Hg3S2Cl1.00I1.00 are analyzed. The crystal structure of the compound has been refined; the unit cell parameters are a m = 16.827(4) , b m = 9.117(1) , c m = 13.165(5) , = 130.17(2)°, V = 1543.3(8) 3, space group C2/m, Z = 8, R = 0.0527. A possible transition a 0 = a m; b 0 = a m + 2c m; c 0 = –b m to the pseudo-orthorhombic F cell previously determined for radtkeite, where one of the angles ( 0 ) is slightly different from 90° (89.55°), has been found. Each sulfur atom in the structure is bonded to three mercury atoms, forming SHg3 umbrellas with distances 2.240(6) –2.474(8) and angles HgSHg 94.7(2)°–102.9(2)°. The SHg3 fragments are linked through Hg vertices to form corrugated [Hg12S8] layers. The halogen atoms lie inside and between the [Hg12S8] layers; the distances are Hg-Cl and Hg-I 2.783(7) , 2.961(7) , and 3.083(4) –3.311(3) , respectively.Original Russian Text Copyright © 2004 by N. V. Pervukhina, S. V. Borisov, S. A. Magarill, D. Yu. Naumov, V. I. Vasiliev, and B. G. NenashevTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 4, pp. 755–758, July–August, 2004.This revised version was published online in April 2005 with a corrected cover date.  相似文献   

10.
Two crystal modifications (m-1 and m-2) of the mixed-ligand complex ZnPhen(i-PrOCS2)2 have been isolated. Their crystal structures were solved using X-ray diffraction data (CAD-4 diffractometer, MoK radiation, 3141 and 3532 Fhkl, R = 0.0363 and 0.0304). For both modifications, the crystals are monoclinic with unit cell parameters a = 10.543(2), b = 13.494(3), c = 16.875(3) , = 102.08(3)°, V = 2347.6(8) 3, Z = 4, space group P21/n (m-1) and a = 10.931(2), b = 12.996(3), c = 16.288(3) , = 92.69(3)°, V = 2311.3(8) 3, Z = 4, space group P21/n (m-2). The structures basically consist of discrete monomer molecules in which the Zn atom has a tetragonal pyramidal (m-1: ZnN2S3, c.n. 5, bidentate and monodentate i-PrOCS 2 - ligands) or distorted octahedral (m-2: ZnN2S4, c.n. 6, bidentate i-PrOCS 2 - ligands) environment. Molecular packings and their interactions in the structures are discussed.  相似文献   

11.
The reaction products of palladium(II) nitration with sodium nitrite in the presence of rubidium salts are described. The crystal structure of rubidium dinitrodichloropalladoate(II) — trans-Rb2[Pd(NO2)2Cl2] — has been studied (KUMA automatic diffractometer, MoK radiation, graphite monochromator, /2 scan mode for 2 < 30°, 758 experimental reflections, R = 0.030; R = 0.023 for I>2(I)). Crystal data: a = 15.123(3), b = 7.750(2), c = 7.776(2) , V = 911.4(4) 3, space group Cmca, Z = 4, d calc = 3.209 g/cm3. The structure consists of [Pd(NO2)2Cl2]2– complex anions and Rb+ cations. The planar square coordination of the Pd atom is completed to distorted octahedral by the chlorine atoms of the neighboring complexes at Pd...Cl distances of 3.18 . Chains of complexes with alternating orientations are formed. The geometrical characteristics of the complex anions, the coordination polyhedra of the cations, and the heavy atom sublattice are analyzed. The crystal structure of Na2[Pd(NO2)4] has been refined, and refinement data are given.  相似文献   

12.
Piperidine octamolybdate [C5H5NH2]4[Mo8O26]·4H2O (I) has been synthesized and characterized by X-ray diffraction analysis. Crystals I are monoclinic, space group P21/n, a=12.892(3), b=9.283(2), c=19.184(4) , =92.50(3)°, V=2293.7(9) 3, Z=2,calc = 2.317 g/cm3.  相似文献   

13.
Mo2Cl4 Pic 4·CHCl3 (A) (Pic=4-methylpyridine) and Mo2Br4 Pic 4 (B) crystallize in the monoclinic space group.A inC2/c (No. 15) witha=15.175 (4),b=10.847 (2),c=19.946 (6) and =104.52 (2)°;D o=1.71 (2),D c =1.72 gcm–3 forZ=4.B inP2l/n (No. 14) witha=9.270 (3),b=16.614 (5),c=9.305 (3) and =91.96 (5)°;D o=2.03 (3),D c =2.05 gcm–3 forZ=2.Two halogens and 4-methylpyridines of the MoX 2 Pic 2 group are in the trans position. Mo–Mo bond lengths are 2.153 96) forA and 2.150 92) forB. Both molecules are situated on the inversion center resulting in the eclipsed configuration of the ligands around the molybdenum pair. The structure ofB has been refined to the conventionalR factors of 0.08 and 0.098. Disorder on the part of 4-methylpyridines and chloroform molecules stopped the refinement ofA at the endR value of 0.175.Mean Mo–X and Mo–N bonding distances are 2.40 (2), 2.25 (5) forA and 2.53 (3), 2.25 (1) forB.
  相似文献   

14.
Xray structural investigation of the monoammonium salt of 5nitroaminotetrazole was performed. The crystals are orthorhombic: a = 10.077(1), b = 17.009(1), c = 6.6472(6), V = 1139.33(17)3, space group Pbca, Z =8, calc = 1.715 g/cm3. Monodeprotonation of 5nitroaminotetrazole during formation of the salt occurs at the N(4) nitrogen atom of the heterocycle. The anion has an almost flat structure; the bond lengths suggest delocalization of electron density in the molecule. The negative charge is distributed among three nitrogen atoms and two oxygen atoms of the anion. Changes in the geometrical parameters of 5nitroaminotetrazole on monodeprotonation are considered.  相似文献   

15.
The crystal and molecular structures of (trans-3,4-diamino-2,2,6,6-tetramethylpiperidine-1-oxyl-N3, N4)(oxalato-O,O)platinum(II) (C11H20N3O5Pt) are studied by X-ray diffraction analysis. The crystals are monoclinic: a=15.210 , b=7.222 , c=14.520 , =118.14°, Z=4, and space group P21/c. The structure is solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R=0.05 against 3227 independent reflections (CAD4 automated diffractometer, MoK ). A molecule of the complex is mononuclear with two different bidentate ligands. The coordination of the Pt2+ cation is a distorted square. The crystal contains intermolecular hydrogen bonds.Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 3, 2005, pp. 179–182.Original Russian Text Copyright © 2005 by Chekhlov.This revised version was published online in April 2005 with a corrected cover date.This revised version was published online in April 2005 with a corrected cover date.  相似文献   

16.
The binary complex salt [Rh(NH3)5Cl][PtBr6] was synthesized and studied by Xray structural analysis. The crystallographic data are as follows: a = 12.013(2) , b = 8.401(2) , c = 15.999(3) , = 91.13(3)°, V = 1614.3(6) 3, space group P21/m, Z = 4, dx = 3.70 g/cm3, R = 0.086. The thermal decomposition of the salt in a hydrogen atmosphere is shown to produce a Rh0.5Pt0.5 solid solution with an FCC cell [a = 3.864(2) . The thermal decomposition of the salt in a helium atmosphere proceeds via the formation of metallic Pt and RhBr3 and finally results in a mixture of several solid solutions.  相似文献   

17.
The reaction of Ni{(i-C4H9)2PS2}2 with imidazole and 3,5-dimethylpyrazole in ethanol gave paramagnetic (ef = 3.02 and 3.11 BM) mixed-ligand complex compounds [Ni(Im)2{(i-C4H9)2PS2}2] (I) and [Ni(Pyr){(i-C4H9)2PS2}2] (II). Single crystals were grown and the crystal structures of I and II were determined from X-ray diffraction data (CAD-4 diffractometer, Mo radiation, 1483 , R = 0.0344 for I and 2630 , R = 0.0486 for II). The crystals are monoclinic with cell dimensions a = 12.845(2), b = 10.250(1), c = 13.431(1) , = 115.89(1)°, V = 1591(1) 3, Z = 2, d calc = 1.281 g/cm3, space group (for I); a = 11.152(3), b = 12.483(2), c = 23.389(4) , = 100.78(1)°, V = 3199(2) 3, Z = 4, d calc = 1.191 g/cm3, space group (for II). The structures consist of discrete monomer molecules. The coordination polyhedron of the Ni atom is a compressed octahedron NiN2S4 (in I) and a tetragonal pyramid NiNS4 (in II) formed by four S atoms of the two cyclic bidentate ligands i-Bu2 and the N atoms of two monodentate ligands (Im molecules in trans-positions) or the N atom of the monodentate Pyr ligand in complexes I and II, respectively. The character of interaction between molecules I and II and molecular packing modes are considered. The electronic spectra of the complexes are consistent with the symmetry of chromophores found from X-ray data.  相似文献   

18.
Synthesis and X-ray diffraction study of trans-bis-(2-(methylimino)-4-pentanonato)Cu(II), which is methyl-substituted ketoiminate, is reported. Crystal data for CuN2O2C12H20: a = 7.374(1) , b = 9.171(1) , c = 10.823(2) ; = 96.51(1)°, = 106.12(1)°, = 96.81(1)°, space group P , Z = 2, d calc = 1.38 g/cm3, d exp = 1.37 g/cm3, R = 0.037. The structure is molecular and consists of isolated trans-complexes. The coordination polyhedron of the copper atom is intermediate between the square and tetrahedron; the average distances are Cu-O 1.91 and Cu-N 1.95 , the O-Cu-O and N-Cu-N trans bond angles are 145.5° and 150.3°, respectively. The O-Cu-N chelate angle is 94.6°. The calculated energies of van der Waals intermolecular interactions are compared with the thermogravimetric characteristics of the complex with ketoiminate and copper(II) ethylenediamine-bis-acetylacetonate.Original Russian Text Copyright © 2004 by I. A. Baidina, P. A Stabnikov, A. D. Vasiliev, S. A. Gromilov, and I. K. IgumenovTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 4, pp. 706–712, July–August, 2004.This revised version was published online in April 2005 with a corrected cover date.  相似文献   

19.
Summary The title compound [W3C3S4{S2P(OEt)2}3(I)(2 PhCO2)(MeCN)] crystallized in triclinic system with space group P1 and cell dimensiona=11.645(6),b=18.565(2),c=11.292(7)Å, =96.15(3)°, =113.65(3)°, =93.77(3)°, V=2207.6Å3, Z=2, Mr=1588.09, Dc=2.39 g cm–3. MoK radiation, =0.71073 Å, =97.3 cm–1, F(000)=1488, R=0.042 for 5588 observed unique reflections I3(I). There are some distortions in the cubane-like W3CuS4 core, with three W-W bonds and three weak W-Cu bonds. Two W atoms are coordinated by PhCO2 bridge ligand, the other W atom is coordinated to the N atom of MeCN.  相似文献   

20.
The crystal and molecular structure of [Au(C14H22N4)]Br has been determined. Monoclinic crystals, a=12.592(2), b=6.309(1), c=19.628(2) ; =98.00(1)°, V=1544.1(4) 3, Z=4, dcalc=2.251 g/cm3, space group C2/c. The structure consists of virtually planar centrosymmetric [Au(C14H22N4)]+ cations and Br- anions. The coordination sphere of the gold atom involves four nitrogen atoms of the ligands, forming a planar square. The Au–N bond lengths are equal (the mean length is 1.982(7) ). The C–C and C–N bonds inside the -diiminate rings are delocalized. The parameters of the -diiminate rings of the [Au(C14H22N4)]+ cation are compared with the parameters of the related complexes.  相似文献   

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