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1.
The title compound (C6H8N)2Mo2I6(H2O)2 crystallizes in theP¯1 space group, witha = 8.127(3),b = 8.337(3),c = 10.415(4) Å, = 73.99(2), = 84.35(2), = 73.91(2) ° andZ = 1. The structure was solved by direct methods and refined to the unweighted and weighted residuals of 0.044 and 0.052. The structure is characterized by the eclipsed configuration of the iodide ions and water molecules within Mo2I6(H2O) 2 2– ion and very short Mo-Mo bond distance 2.115(1) Å. Three independent Mo-I distances are 2.784(1), 2.760(2) and 2.797(1) Å. 4-Methylpyridinium ion is planar within 0.02° Å. The compound is isostructural with (C6H8N)2Mo2Br6(H2O)2.Part II, Breni, J. V., Leban, I., and egedin, P. (1976).Z. Anorg. Allg. Chem. 427, 85.  相似文献   

2.
The structures of anionic pyridine-2,6-dicarboxylato (pdc2–) complexes of cobalt, nickel, and copper have been studied. The stoichiometries and structures are very much dependent on whether KOH, Et4NOH, or NaOH is used in the synthesis to deprotonate the H2pdc ligand. Crystallographic results are: (1) K2[Co(pdc)2] · 7H2O, orthorhombic, Pnna, Z = 4, a = 20.637(2)Å, b = 13.480(1)Å, c = 8.200(1)Å (2) K2[Ni(pdc)2] · 7H2O, orthorhombic, Pnna, Z = 4, a = 20.648(1)Å, b = 13.375(1)Å, c = 8.2393(8)Å (3) [Co2(H2O)5(pdc)2] · 2H2O, monoclinic, P21/c, Z = 4, a = 8.3880(6)Å, b = 27.384(2)Å, c = 9.6110(8)Å, = 98.271(6)° (4) [Ni(Hpdc)2] · 3H2O, monoclinic, P21/c, Z = 4, a = 13.679(1)Å, b = 10.0450(9)Å, c = 13.767(2)Å, = 115.184(7)° (5) Na6[Co(H2O)6][Co(pdc)2]4 · 28H2O, monoclinic, P21/n, Z = 2, a = 13.363(1)Å, b = 8.437(1)Å, c = 40.689(3)Å, = 91.288(5)° (6) Na[Ni(Hpdc)(pdc)] · 11.5H2O, monoclinic, C2/m, Z = 4, a = 15.200(2)Å, b = 22.299(2)Å, c = 8.3596(7)Å, = 118.894(7)° (7) Na[Cu(Hpdc)(pdc)] · 3H2O, monoclinic, P21/n, Z = 4, a = 9.516(4)Å, b = 14.917(6)Å, c = 12.247(5)Å, = 92.00(5)°. The potassium and sodium complexes have extensive K+—H2O and Na+—H2O networks. The fact the Et4N+ ion does not appear in any of the complexes is likely due to the fact that it is incapable of forming the intricate cation—water and hydrogen-bonding networks observed in all of the other structures.  相似文献   

3.
A terephthalato-bridged copper(II) complex [Cu2(tpt)(bpy)2(H2O)4][Cu2(tpt)3(bpy)2 (H2O)2] (1) (tpt = terephthalate, bpy =; 2,2'-bipyridine) was synthesized by the reaction of Cu(ClO4)2 6H2O and terephthalic acid in the presence of 2,2'-bipyridine in H2O solution. Crystal structure of 1 was determined by X-ray diffraction analysis in the triclinic space group P , with a = 10.7327(10) Å, b = 11.1658(11) Å, c = 17.3768(16) Å, = 108.063(2), = 91.064(2), = 116.721(2), V = 1737.5(3) Å3, and Z = 2. Both the anion and the countercation in 1 are copper(II) complexes linked by terephthalate bridges in the bis(monodentate) (syn–anti) mode. The anion and the countercation are also linked by two hydrogen bonds between coordinating water molecules and terephthalate ligand.  相似文献   

4.
The syntheses, properties, and structures of N-phenylmaleimidetriazole derivatives are described. Intermediates and by-products are also discussed. 1b. a = 43.997(7) Å, 5.7610(9) Å, 8.245(1) Å, = 99.339(4), C2/c; 2a. a = 13.646(4) Å, b = 7.744(2) Å, c = 10.612(3) Å, = 91.979(6), P21/c. 3a. a = 22.245(1) Å, b = 22.245(1) Å, 10.010(1) Å, P42/n. 3a. a = 11.727(2) Å, b = 14.075(3) Å, c = 16.080(3) Å, = 105.859(3), = 105.331(3), = 98.187(3), P-1. 3b. a = 8.561(3) Å, b = 14.755(5) Å, c = 22.771(7) Å, = 97.006(5), P21/c. 3c. a = 10.500(2) Å, b = 12.189(2) Å, c = 13.040(2) Å, = 109.091(3), = 106.089(3), = 101.022(3), P-1. 8a. a = 16.389(8) Å, b = 5.749(3) Å, c = 19.316(3) Å, = 97.467(9), P21/n. 8b. a = 5.822(2) Å, b = 10.114(3) Å, c = 16.705(4) Å, = 84.681(5), = 82.840(5), = 75.769(4), P-1. 9b. a = 11.251(1) Å, 13.335(3) Å, 13.376(3) Å, = 102.456(4), P21/n. 9c. a = 15.836(3) Å, b = 8.236(2) Å, c = 5.447(3) Å, = 92.551(3), P21/c. 10a. a = 13.177(2) Å, b = 14.597(2) Å, c = 5.5505(8) Å, = 110.979(2), Cc. 11a. a = 14.720(2) Å, b = 13.995(2) Å, c = 38.245(6) Å, = 94.430(3), P21/n. 12b. a = 15.067(5) Å, b = 20.378(6) Å, c = 8.669(5) Å, = 99.16(4), = 99.32(3), = 105.23(3), P-1. 13b. a = 8.2824(6) Å, b = 10.5245(7) Å, c = 15.518(1) Å, = 92.305(1), = 100.473(1), = 100.124(1), P-1. 15a. a = 15.357(3) Å, b = 7.778(2) Å, c = 22.957(2) Å, Pbca. 16b. a = 18.0384(4) Å, b = 12.474(3) Å, c = 20.078(5) Å, Pbca.  相似文献   

5.
The title compounds palladium(II) and platinum(II) tetrakisthiourea dichloride bis(7-hydroxy-5-methyl[1,2,4]triazolo[1,5a]pyrimidine (Hmtpo)) dihydrate solvates, have been synthesized by reacting thecis-[MCl2(Hmtpo)2] (where M=Pt(II), Pd(II)) complexes with an excess of thiourea (tu) and the structure of the palladium compound was solved by X-ray diffraction. Crystals of [Pd(tu)4]Cl2·2Hmtpo·2H2O are triclinic with space groupP and unit cell dimensionsa=7.972(1),b=9.049(1),c=11.808(2)Å, =88.20(1), =75.15(1), =76.54(1)o. The cation [Pd(tu)4]2+ is centrosymmetric involving four sulfur thiourea atoms in a near square planar environment. The triazolopyrimidine molecules, chloride anions and water molecules do not take part in the metal center coordination but interact by hydrogen bonding between them and the thiourea moieties. A comparison between powder diffraction data of palladium(II) and platinum(II) compounds clearly indicates that both compounds are isomorphous.  相似文献   

6.
A one-dimensional chain complex, {[Co(bpm)2(N3)2][Co(bpm)2(H2O)2]} (ClO4)2, (bpm being bis(pyrazol-l-yl)methane), has been synthesized and characterized by X-ray diffraction: triclinic, space group P - 1 with a = 8.805(2) Å, b = 8.902(2) Å, c = 13.621(3) Å, = 84.27(3)°, = 84.63(3)°, = 80.05(3)°, V = 1043.2(4) Å3, Z = 1. Two cobalt atoms have ideal octahedral environments with different coordination atoms. One cobalt atom is six-coordinated with nitrogen atoms from two bpm ligands and two azide ligands, while the other cobalt atom is coordinated by four nitrogen atoms from bpm and two oxygen atoms from water molecules. The complex forms one-dimensional chain through hydrogen bonds.  相似文献   

7.
A novel two-dimensional 4f-3d heterometallic coordination polymer Ce2Co3(EDTA)3(H2O)11·12H2O (EDTA = ethylenediamine-N,N,N,N-tetraacetate) has been synthesized using complex Na[Ce(EDTA)] as ligand. The complex crystallines in the space group C2, with lattice parameters a = 15.974(3) Å, b = 14.676(3) Å, c = 14.773(3) Å, = 116.39(3)°,V = 3102.4(11) Å3, Dx = 1.858 g/m3, Z = 2. It consists of a two-dimensional sheet in which the Ce(III) is ten-coordinated by six carboxylic O atoms from three EDTA molecules and four O atoms of water molecules, forming a distorted bicapped square antiprism, and the Co(II) atom is seven-coordinated by two N, four O atoms from one EDTA molecule and one O atom from the water molecule, giving rise to a monocapped trigonal prism. Each chelated Co(II) atom is connected to two hydrated Ce(III) atoms through tridendate bridging carboxylate groups, while each Ce(III) atom has three Co(II) atoms as neighbors. These sheets are linked into a three-dimensional network by the water molecules between layers through rich hydrogen bonds.  相似文献   

8.
The compound [Fe(C4H6N2)6][C5H4NSO3]2 crystallized in the monoclinic space group, P21/n with unit cell parameters: a = 13.676(3), b = 8.345(2), c = 18.663(4) Å, = 106.40(3)° and Z = 2. The title compound consists of a [Fe(C4H6N2)6]+2 hexacoordinated iron(II) cation and two C5H4NSO 3 anions. In the cation the iron atom is coordinated to six N-methylimidazole imine nitrogen atoms in a distorted octahedral arrangement. The N1,N5,N1i,N5i atoms are coplanar and the iron lies in this plane.  相似文献   

9.
[Mn(H2O)3(phen)(C4H4O4)]·2H2O was obtained by reaction of freshly prepared MnCO3, phen and succinic acid in CH3OH/H2O (1:1 v/v), and its crystal structure has been determined by single crystal X-ray diffraction methods. The title mixed ligand complex crystallizes in the triclinic space group with cell dimensions a = 7.590(1) Å, b = 9.324(1) Å, c = 13.917(1) Å, = 85.64(1)°, = 74.56(1)°, = 77.10(1)°, and D calc = 1.584 g/cm3 for Z = 2. The crystal structure consists of the [Mn(H2O)3(phen)(C4H4O4)] complex molecules and lattice H2O molecules. The Mn atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of three H2O molecules and one succinato ligand with d(Mn—N) = 2.271 and 2.299 Å, and d(Mn—O) = 2.133–2.239 Å. Through intermolecular hydrogen bondings, the complex molecules are interlinked to form 2D layers, which are assembled by – stacking interactions into 3D framework with tunnels occupied by the lattice H2O molecules. Thermal analyses showed that the title compound decomposes in two steps over the range 25–600°C upon heating in flowing Ar.  相似文献   

10.
The complex [Co(L)]Cl2·10H2O (1) (L = 2,13,-bis(2-pyridylmethyl)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane) has been synthesized and structurally characterized. Compound 1 crystallizes in the triclinic system, space group P-1 with a = 9.731(2) Å, b = 9.789(2) Å, c = 11.998(1) Å, = 66.66(1)°, = 76.95(1)°, = 87.99(2)°, V = 1020.4(3) Å3, and Z = 1. The crystal structure of 1 shows that the complex is centrosymmetric and the cobalt(II) ion has a slightly distorted octahedral geometry with four nitrogen atoms of the macrocycle and two nitrogen atoms of the pendent arms at the axial positions. Cyclic voltammetry for 1 undergoes reversible one-electron oxidation to the Co(III) and irreversible one-electron reduction to the Co(I).  相似文献   

11.
The X-ray crystal structure of the title compound, [Co(NCS)2(C6H6N4)2(H2O)2], has been determined. The crystals are monoclinic, space groupC2/c, with cell dimensionsa=15.6901(5),b=7.9248(10),c=16.1278(12) Å,=94.4(8)°V c=1999.44 Å3,M r=479.18,Z=4,D x=1.5918 Mg m3,Cu K radiation (graphite crystal monochromator, =1.54051 Å), (CuK)=39.08 cm–1,F(000)=980.00 andT=290 K. Final conventionalR-factor=0.051, andR w=0.053 for 1430 observed reflections and 141 variables. The structure was solved using the programsPatsys andDirdif. The Co atom is octahedrally coordinated (CoN2O2N2 chromophore), with only the 5-methyl-[1,2,4]-triazolo[1,5-a]pyrimidine (5mtp) ligands in thetrans positions. The triazolo pyrimidine rings are planar and coordinated through their N(3) atoms. The H2O ligands are also H-bond donors to N(4) (intramolecularly) and to the S atoms of the NSC anions (intermolecularly).  相似文献   

12.
The crystal and molecular structure of MgCl2(H2O)2(ethylpropionate)2 has been determined by single crystal X-ray diffraction analysis. The complex crystallizes in the triclinic system, space group (No. 2);a=5.912 (2),b=5.931 (3),c=12.792 (4) Å, =77.15°(3), =86.21°(3), =88.31°(3);Z=1. The metal lies at the center of a slightly distorted octahedron formed by two chlorine atoms and four oxygens, two from water molecules and two from the carbonyl groups of the ethylpropionate ligands in atrans configuration.  相似文献   

13.
The complex [Ni(H2O)3(phen)(C4H2O4)] H2O (1), which was obtained by reaction of phenanthroline, Ni(NO3)2 6H2O, and maleic acid in CH3OH/H2O at pH = 7.05, crystallized in the monoclinic space group P21 (no. 4) with cell dimensions: a = 9.350(1) Å, b = 7.631(1) Å, c = 12.821(1) Å, = 106.25(1), and D calc = 1.607 g/cm3 for Z = 2. The Ni atoms are each octahe drally coordinated by one chelating phen ligand, three H2O molecules and one monodentate maleato ligand to form [Ni(H2O)3(phen)(C4H2O4)] complex molecules with d(Ni–O) = 2.038–2.090 Å, d(Ni–N) = 2.066, 2.089 Å. The formed complex molecules are, via the intermolecular hydrogen bonds, assembled into columnar 1D chains. Interdigitation of the chelating phen ligands of the neighboring chains leads to 2D layers and the crystal H2O molecules are hydrogen bonded to the oxygen atoms of the maleate not coordinated to the Ni atom. However, reaction of NiCO3, phen, and maleic acid in CH3OH/H2O at pH = 6.33 afforded [Ni(H2O)2(phen)(C4H2O4)] 2H2O (2), which crystallized in the triclinic space group (no. 2) with cell dimensions: a = 7.971(1) Å, b = 8.237(1) Å, c = 13.304(1) Å, = 81.005(6)°, = 87.877(8)°, = 78.322(8)°, and D calc = 1.671 g/cm3 for Z = 2. The Ni atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of two H2O molecules and two bis–monodentate maleato ligands with d(Ni–O) = 2.041–2.120 Å and d(Ni–N) = 2.095 Å. The Ni atoms are bridged by the maleato ligands to generate 1D 1 [Ni(H2O)2(phen)(C4H2O4)2/2] chains along [100]. The supramolecular assemblies of the 1D chains via – stacking inter- actions result in thick 2D layers parallel to (001), between which the noncoordinating H2O molecules are sandwiched. The paramagnetic [Ni(H2O)2(phen)(C4H2O4)2/2] 2H2O (2) obeys the Curie–Weiss law m(T-) = 1.139cm3 mol–1 K with the Weiss constant = –0.95 K.  相似文献   

14.
The X-ray crystal structure of [(NH3)5Co(ClO2)][Pd(CN)4]·H2O consists of two discrete complex ions and a water of hydration. The red crystals are triclinic, P , with lattice parameters a = 7.1992(5), b = 9.4873(7), c = 11.7752(8) Å. = 66.680(1), = 75.784(1), = 82.203(1)°, and Z = 2 giving a cell volume of 715.27(9) Å3 and a calculated density of 2.043 g/cm3 at 293°. The chlorite ion is O-bonded to the cobalt atom with amine N—Co distances all equal. The chlorite ion is bent with a O—Cl—O angle of 110.8(2)° and the Cl—O distances being 1.601(3) and 1.558(3) Å, the longer value for the O atom also coordinated to Co. The Pd(CN)–2 4 ions are planar, C-coordinated and stack along the x-axis, separated by 3.599(1) Å and alternatively rotated by 29.9(5)°.  相似文献   

15.
[Na4(H2O)14]SnS4 is obtained by the reaction of Na2S·9H2O with SnCl4·5H2O in aqueous solution at 21°C. It crystallizes in the space group Cc with a = 8.621(2) Å, b = 23.543(5) Å, c = 11.358(2) Å, = 110.58(3)° and V = 2158.2 Å3 with Z = 2. Refinement of 3826 unique reflections from a racemically twinned crystal yielded a final value of R1 = 0.0464 (|F| > 4) and wR2 = 0.104 and a goodness of fit of 1.125. The structure consists of a Na+/H2O network supporting the tetrahedral SnS4 4– anions. Water molecules or sulfide ions octahedrally coordinate each of the four crystallographically independent Na+ ions. The dominant feature of the structure is the existence of zigzag chains of edgeshared Na octahedra. These chains are tied together into a three-dimensional network by bridging Na(H2O)6 octahedra and individual H2O molecules.  相似文献   

16.
The crystal and molecular structure of pyridinium di--oxo-bis(oxodichloroaquomolybdate(V)) monohydrate has been determined from MoK diffractometer data. The compound crystallizes in the monoclinic space groupP2 1/m witha = 7.544(1),b= 17.046(3),c = 7.894(1) Å, = 106.00(1) ° andZ = 2. The structure was solved by the heavy-atom technique and refined by full-matrix least-squares method toR = 0.046, using 1800 reflections for whichF> 4(F). Molybdenum atoms are linked by the double oxygen bridge with an Mo—O distance of 1.943(4) Å and an Mo—O—Mo angle of 83.4(2) °. The Mo—Mo distance is 2.584(1) Å, indicating direct Mo—Mo bonding. The pyridinium and [Mo2O4C14(H2O)2]2- ions are hydrogen bonded through N—H ... O bonds. The N ... O contact is 2.656(8) Å.  相似文献   

17.
Two cadmium(II) complexes of betaine (BET) have been prepared and characterized by X-ray crystallography. [Cd(BET) (–Cl)2] (1), is a one-dimensional polymer in which each cadmium atom is coordinated by two pairs of bridging chlorine atoms [Cd-Cl=2.631(2), 2.614(2) Å] and two oxygen atoms from different bridging carboxylate groups [Cd-O=2.291(6), 2.329(6) Å] in the form of a compressed octahedron. [Cd(BET)(H2O)Cl(–Cl)]2 (2) is a dimer with each cadmium atom in a distorted octahedral coordination environment, being surrounded by a chelating bidentate carboxylate group [2.480(2), 2.332(3) Å], one aqua ligand [2.364(3) Å], two bridging chlorine atoms [2.659(1), 2.557(1) Å], and one terminal chlorine atom [2.480(1) Å].  相似文献   

18.
The luminescent heteroleptic Cd(II) complex bis (-1,2-benzenedithiolato)-1 kS, 1:2 k 2 S 2 kS, 1:2 k 2 S-bis[(1,10-phenanthroline-k 2 N 1, N 1)cadmium], [Cd2(C6H4S2)2(C12H8N2)2], containing benzenedithiolate (bdt) and 1,10-phenanthroline (phen) has been synthesized and found to have the dinuclear formulation [Cd(bdt)(phen)]2. The complex crystallizes in the space group P21/n with a = 10.3400(4), b = 11.5110(4), c = 13.6230(5) Å, and = 106.828(2)°. The dinuclear complex has crystallographically imposed centrosymmetry with one S atom of the bdt ligand bridging the Cd atoms in an asymmetric fashion (Cd–S = 2.5743(5) and 2.6817(5) Å) while the second S atom is bound in a terminal mode (Cd–S = 2.4955(5) Å). The mean interplanar spacing between the phen ligand and the phenyl ring of the bdt ligand is 3.291 Å while that between the phen ligands of adjacent molecules is 3.363 Å, suggesting the presence of both intra- and intermolecular -stacking. The complex is emissive in the solid state at room temperature (em = 569 nm) with a luminecsent lifetime of 369 ns. The unstructured emission is believed to be a ligand-to-ligand –* charge transfer transition.  相似文献   

19.
A novel compound catena-(-CrO4-O,O)[Ni(L1)Ni(L2)] 3H2O (1) (L1 = 3,5,10,12-tetramethyl-1,4,8,11-tetraazacyclotetradecane and L2 = 2,5,9,12-tetramethyl-1,4,8,11-tetraazacyclotetradecane) has been synthesized for the first time and structurally characterized. 1 crystallizes in the triclinic space group P with a = 9.623(1), b = 10.084(1), c = 12.723 (3) Å, = 66.74(2), = 75.20(1), = 72.02(1)°, V = 1066.2(3) Å3, and Z = 2. The coordination environment around the Ni(II) ions is an axially elongated octahedron with the secondary amines of the isomeric ligands and two oxygen atoms of [CrO4]2–.  相似文献   

20.
The copper complex, [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2], has been prepared and its structure determined using X-ray crystallography. The dimer is a di-2-alkoxo complex which is a five-coordinate copper dimer with unsupported alkoxo bridges. The complex crystallizes in the triclinic space group P-1 with a = 11.384(2), b = 14.636(5), c = 9.609(2) Å, = 100.07(2), = 104.33(3), = 72.79(2)°, V = 1471.8(7) Å3, and Z = 2. The structure is comprised of discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the dmpa ligands. The Cu-O and Cu-N distances are in good agreement with those found for other copper(II) aminoalcoholato complexes. The Cu···Cu distance is 2.9765(6) Å. In the crystal, every two dimeric coordination molecules are combined together by the recognition through intermolecular hydrogen-bonding interactions between the apical water molecule and the non-coordinated O atom from the p-chlorobenzoato ligand, forminga tetramer.  相似文献   

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