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1.
The molecular structure of trans-W2(CO)6(PPh2H)2(2-PPh2)2 was determined by X-ray diffraction analysis. The two tungsten centers, bridged by two diphenylphosphido ligands, are separated by 3.0667(6) Å with W–P–W angles of 77.10(5) and 77.08(5). Average tungsten–phosphorus bond distances are 2.461(17) and 2.4576(21) Å for bridging and terminal phosphorus groups, respectively, with a range of 0.037 Å for the former and 0.001 Å for the latter. The complex crystallizes in the monoclinic space group P21/c with a = 19.282(4) Å, b = 12.158(2) Å, c = 21.294(9) Å, = 92.821(4), and Z = 4.  相似文献   

2.
In aqueous solution, [M(chelate)Cl2]x (chelate = 2,2-bipyridine, 1,10-phenanthroline) complexes can disproportionate to produce M(chelate)2 n+ species that contain two chelating ligands. After extraction with organic solvent,Co(phen)2(-Cl)2CoCl2(1) has been characterized by X-ray diffraction (monoclinic, C2/c, a = 10.278(2)Å, b = 22.026(5)Å, c = 12.941(3)Å, = 103.959(4)°, Z = 4, 2414 reflections [I 2 (I)], R 1 = 0.0321, wR 2 = 0.0864). However, addition of [M(chelate)Cl2]x starting materials to dimethyl sulfoxide produces complexes that retain a single chelate ligand. The pentacoordinate complex Co(bpy)Cl2DMSO (2) has been structurally characterized (triclinic, P , a = 7.824(2)Å, b = 9.570(4)Å, c = 10.025(2)Å, = 83.24(3)°, = 87.14(2)°, = 83.35(3)°, Z = 2, 2455 reflections [I 2 (I)], R 1 = 0.0278, wR 2 = 0.0747). In the case of nickel, two different geometric isomers are observed, depending on the chelate identity: trans-(DMSO)2Ni(bpy)Cl2 DMSO (3) (monoclinic, P21/c, a = 10.9149(8)Å, b = 12.1287(9)Å, c = 17.0044(13)Å, = 98.610(1)°, Z = 4,3519 reflections [I 2 (I)], R 1 = 0.0209, wR 2 = 0.0560) and cis-(DMSO)2Ni(phen)Cl2 (4) (monoclinic, P21/c, a = 8.404(2)Å, b = 14.051(4)Å, c = 16.710(4)Å, = 92.44(3)°, Z = 4, 3069 reflections [I 2 (I)], R 1 = 0.0691, wR 2 = 0.1782).  相似文献   

3.
The crystal and molecular structures of the complex of [Ni{(iPrO)2dtp}2(py)2] and [Cd{(iPrO)2dtp}2(py)2] (dtp = dithiophosphate, py = pyridine) have been determined by X-ray crystallography. They are isomorphous. The crystal structures are very similar and consist of discrete molecules of [Ni{(iPrO)2dtp}2(py)2] and [Cd{(iPrO)2dtp}2(py)2], respectively. They both crystallize in the monoclinic system, space group P21/c, the former with lattice parameters a = 6.489(1) Å, b = 14.830(3) Å, c = 16.386(3) Å, = 99.74(3), and Z = 2; the latter with a = 6.461(3) Å, b = 14.583(4) Å, c = 17.433(4) Å, = 99.55(3)°, and Z = 2. They all display distorted octahedral geometry around the central metal atom. In the complexes, two O,O-diisopropyl dithiophosphate ions act as bidentate ligands with their S atoms coordinated to metal. Each forms a four-membered chelate ring in the equatorial plane. The N atoms from two pyridine ligands are axially coordinated to the metal atom. The Ni–S bond distances are 2.5137(10) and 2.5386(9) Å, and the Ni–N bond distances are 2.127(3) Å. The Cd–S(1) and Cd–S(2) bond distance are 2.694(1) and 2.704(1) Å, respectively, and the Cd–N bond distances are 2.399(3) Å. The IR spectra data is in agreement with the structural data.  相似文献   

4.
Treatment of the diphosphine ligand 1,2-bis(diphenylphosphino)cyclobutenedione (bpcbd) with the THF adduct fac-BrRe(CO)3(THF)2 at room temperature furnishes the new dirhenium compound [BrRe(CO)3]2(bpcbd) instead of the expected mononuclear compound fac-BrRe(CO)3(bpcbd). [BrRe(CO)3]2(bpcbd) was characterized in solution by IR spectroscopy, and the solid-state structure was solved by X-ray crystallography. [BrRe(CO)3]2(bpcbd), as the CH2Cl2 solvate, crystallizes in the space group P , a = 11.173(1), b = 13.362(1), c = 15.250(1) Å, = 108.973(7)°, = 99.477(8)°, = 110.466(7)°, V = 1915.0(3) Å3, Z = 2, and d calc = 2.143 g-cm–3. The structure of [BrRe(CO)3]2(bpcbd) consists of two rhenium centers that are six-coordinate and possess nearly ideal octahedral geometry. The two Re(CO)3 units are linked together by the bridging diphosphine ligand and two bridging bromide groups.  相似文献   

5.
The salt triethylentetraammonium bis monohydrogen-monophosphate dihydrate is orthorhombic Pbca with unit cell dimensions a = 8.963(2), b = 10.326(2), c = 17.381(4)Å; Z = 4; Dm = 1.540 g cm–3; D x = 1.562 g cm–3. The examination of the structure shows a layer arrangement parallel to the axis: planes of [HPO4]2– tetrahedra alternate with planes of [(NH3(CH2)2NH2CH2)2]4+. The [HPO4]2– tetrahedra are connected through O(W)s--H···O hydrogen bonds, so that infinite chains of the composition [HPO4(H2O)]n 2n– are formed in the structure parallel to the axis. The structure of this compound is built from [HPO4]2– anions, [(NH3(CH2)2NH2CH2)2]4+ cations and zeolitic water molecules connected by hydrogen bonds.  相似文献   

6.
The dimeric complex [Mn2(-pyS)2(CO)6] (1) reacted with 2 M equivalents of both PPh3 and PHPh2 to give the respective monomeric phosphine complexes [Mn(pyS)(L)(CO)3][L = PPh3 (2) and PHPh2 (3)]; with 4 M equivalents of dppm, it yielded the complex [Mn(pyS)(1-dppm)2(CO)2](4). An X-ray structure determination of 4 shows that it crystallizes in the monoclinic space group P21/n with a = 11.027(3), b = 24.984(7), c = 18.379(5) Å, = 99.870(8)°, V = 4988(2) Å3, and Z = 4. The complex has an octahedral geometry with the chelating pyS ligand and two CO groups occupying the equatorial sites and the two monodentate dppm ligands lying in the trans positions.  相似文献   

7.
The crystal structures of the anhydrous and monohydrated (dabcoH2)CuCl4nH2O salts (n = 0,1) have been determined and a comparison of their crystal structures has been reported. The anhydrous salt is monoclinic P21/c with a = 9.045(2) Å, b = 6.9270(10) Å, c = 18.767(4) Å and = 90.07(3)° with V = 1175.8(4) Å3. The hydrated salt is also monoclinic P21/c with a = 9.266(2) Å, b = 9.395(2) Å, c = 14.386(3) Å and = 93.32(3)° with V = 1250.3(5) Å3. The structures of the two salts are closely related. Both compounds contain isolated distorted (compressed) tetrahedral CuCl4 2– anions, diprotonated dabco cations, and in the case of the hydrated salt, lattice H2O molecules. In the anhydrous salt, each of the two N–H+ groups of the dabcoH2 2+ dications form bifurcated hydrogen bonds to chloride ions on adjacent CuCl4 2– anions along the c axis, thus forming chains running parallel to the c axis. In the hydrated salt, a water molecule is inserted into one of the pair of bifurcated hydrogen bonds, forming instead N–H O–H CuCl4 2– linkages. The chains thus formed are cross-linked by O–H Cl hydrogen bonds between the chains. Because of this additional hydrogen bonding, the CuCl4 2– anions in the hydrated salt are distorted further from tetrahedral geometry.  相似文献   

8.
The reaction of equal millimolar quantities of CdBr2 and 2-hydroxyethyl sulfide in 31 CH3CNCH3OH produced [Cd(OH2)2(Br)4 (Cd(2-hydroxy ethyl sulfide) (-Br))2]n. The compound crystallizes as a bromide-bridged polymer with hydrogen bonding interactions between the polymeric chains. Each of the two unique metal centers has a distorted octahedral geometry. The thioether ligand is bidentate to one cadmium position with one alcoholic terminus uncoordinated. The uncoordinated portion of the molecule is disordered with each conformation participating in slightly different hydrogen bonding environments. The other unique cadmium center is coordinated to four bridging bromides and twotrans water molecules.  相似文献   

9.
The title compound crystallizes in the monoclinic spacegroup P21/m with a = 6.796(9), b = 12.145(14), c = 7.749(8)Å, = 101.86(1)°, and Z = 2. The crystal structure consists of molecules of [MoCl(CO)2(NCMe)2(3-C3H4Me-2)] with crystallographically imposed Cs symmetry and has a pseudo-octahedral geometry, with the -allyl group trans- to the chloro group and the two cis-carbonyl and acetonitrile groups occupying the equatorial plane.  相似文献   

10.
Treatment of (μ-SCH2CH2CH2S-μ)Fe2(CO)6 with equimolar 2-C5H4NPPh2 in the presence of Me3NO·2H2O in CH2Cl2/MeCN solutions gave the title complex (μ-SCH2CH2CH2S-μ)Fe2(CO)5(2-C5H4NPPh2) in 76% yield. The title complex was characterized by spectroscopy as well as by single crystal X-ray diffraction analysis. The molecular structure consists of a butterfly [Fe2S2] cluster with propane, five carbonyls, and 2-C5H4NPPh2. In the crystal packing diagram, intermolecular C–H···O hydrogen bonds between phenyl and carbonyl groups stabilize the solid state.  相似文献   

11.
The title compound was obtained from a CS2 solution of bis(2,2-dipyridylamido)copper(II), by insertion of solvent into this complex. In the structure of the dithiocarbamate the metal atom is approximately square-planar coordinated by four S atoms from two chelating ligands. Considering the long interactions between the metal center and the S(2) atom from a centrosymmetrically related complex [Cu(1)...S(2)=3.230 Å], double bridged dimers are formed with the copper atoms in an elongated square-pyramidal coordination. The crystals are monoclinic, space groupP2 1/n witha=14.549(3),b=11.662(3)c=15.329(4) Å and =114.79(2)°.  相似文献   

12.
Compound (I) is 2-methyl-3-(2-methyl-2-nitrovinyl)indole, C12H12N2O2,M r=216.24, monoclinic,P21/n,a=16.710(1),b=7.627(1),c=17.646(1) Å,=104.8(1)°,V=2174.7(1) Å3,Z=8.D x=1.321 g cm–3, MoK, =0.71073 Å,=0.858 cm–1,F(OOO)=912, room temperature,R=0.061 for 1956 observed reflections. Compound (II) is 3-(2-nitrovinyl)indole, C10H8N2O2,M r=188.18, monoclinic,P21/n,a=10.178(1),b=10.608(1),c=8.411(1) Å,=105.5(2)°,V=875.0(1) Å3,Z=4,D x=1.4284 g cm–3, CuK, =1.5418 Å,=8.068 cm–1,F(000)=392, room temperature,R=0.040 for 1330 observed reflections. Compounds (I) and (II) have a similar geometry, the only significant difference lying in the rotation of the nitrovinyl chain. This feature could be responsible for the difference in biological activity. In both compounds, the molecules are associated, forming charge-transfer complexes.  相似文献   

13.
The title compound has been prepared by the addition of fluoroboric acid to 18-crown-6 in toluene. The compound crystallizes in the triclinic space group P¯1 witha=7.341(2),b=8.364(2),c=10.631(3)Å,=71.48(2),=67.91(2), =67.94(2)°, andD c =1.44 g cm–3 forZ=1. The final conventionalR value was 0.079 based on 1575 observed reflections. The molecule resides on a center of inversion. The (H2O·HBF4) moieties are best viewed as fluoroboric acid monohydrate molecules hydrogen bonded to the crown ether, one above and one below the plane of the crown. The FO(water) hydrogen bond separation is 2.474(5)Å, and the O(crown)O(water) separations are 2.834(5) and 2.841(6) Å. The oxygen atoms of the crown ether are planar to 0.23 Å.  相似文献   

14.
The title compound has been synthesized, and characterized by means of X-ray, magnetic, and IR-spectroscopic measurements.The crystals of Cu(DPhP)2(H2O)2(DPhP=diphenylphosphate) are monoclinic, space groupI2/c witha=24.126(6),b=8.510(2),c=12.333(3) Å,=90.73(5)° andZ=4. The structure was solved by the heavy-atom technique, and refined by full-matrix least-squares calculations to a finalR of 0.040 for 1494 reflections.The complex is centrosymmetric, and the Cu atom at a center of symmetry is four-fold coordinated with two oxygen atoms from two phosphate groups and two water molecules. The coordination about the Cu atom is square-planar, with Cu-O and Cu-O(W) distances 1.926(3) and 1.912(3) Å, respectively.The O(2) phosphate oxygen is an acceptor of two H bonds; one of them is an intramolecular O(W)-H(2)O(2) of 2.714(4) Å, and the other is an intermolecularO(W)-H(1)O(2i) of 2.667(4) Å. Their presence is also deduced from the IR spectrum of this compound at 3250 and 3000 cm–1, respectively.The calculated magnetic moment value of 1.92 B.M. corresponds to that of the monomeric copper(II) complexes including those of some alkyl phosphates.  相似文献   

15.
The dimeric complex [Mn2(-pyS)2(CO)6] (1) reacted with 2 molar equivalents of Ph2P(CH2)3PPh2 (dppp) and Ph2P(CH2)2PPh2 (dppe) to give the respective monomeric chelate complexes [Mn(2-pyS)(2-dppp)(CO)2] (2) and [Mn(2-pyS)(2-dppe)(CO)2] (3). In contrast, with 2 molar equivalents of Ph2P(CH2)5PPh2 (dpppe), 1 gave the highly insoluble polymeric complex [Mn(2-pyS)(-dpppe)(CO)2]n (4). An X-ray structure determination shows that 2 crystallizes in the monoclinic space group P21/n with a = 10.721(2) Å, b = 19.712(5) Å, c = 14.846(4) Å, = 109.06(2)°, V = 2965.5(14) Å3, and Z = 4. The complex has a distorted octahedral geometry with the dppp ligand, one CO group and the N atom of the chelating pyS ligand occupying equatorial sites, and one CO group and the S atom of the pyS ligand lying in the axial positions.  相似文献   

16.
The crystal structures of threo(RR,SS) diethyl ester of 2-hydroxy-1,2-diphenylethylphosphonic acid (1) and of (±)diethyl ester of (1-hydroxycyclopentyl)(2-methylphenyl)methylphosphonic acid (2) have been solved by X-ray methods. They are built up in a similar way to centrosymmetric dimers of hydrogen-bonded molecules. The orientation of the substituents around the central C-C bond in both molecules fulfills the requirement for the least spatial hindrance. The observed shift of the oh stretching frequencies from 3312(1), 3346 (2) cm–1 in solid to 3408(1), 3450(2), in diluted (10–3 M) tetrachloromethane solution, indicates the formation of intramolecular hydrogen-bonded species.  相似文献   

17.
The structure of the new tetranucleating ligand 2,3,-dihydroxy benzenemethanimine -(2-hydroxymethyl)phenyl has been determined by X-ray diffraction techniques. C14H13NO3 is monoclinic, space groupP21/a, with cell dimensionsa=10.382(2),b=19.147(1),c=12.799(1) Å,=113.08(1)°,V=2340.6(3) Å3,Z=8,M=243.04,D o=1.36,D x=1.38 mg/m3,F(000)=1024,T=293 K,R=0.041 for 2640 observed reflections. There are two molecules in the asymmetric unit and both have a similar geometry. The molecules are parallel to each other, the distance between them being 3.7 Å and the dihedral angle between mean planes 7.8°. There is a pseudocenter between molecule A and (1–x, 1–y, 1–z) of molecule B. The structure is stabilized by intramolecular O-HN and intermolecular O-HO as well as by C-HO hydrogen bonds.NCL Communication No. 5332.  相似文献   

18.
The salt triethylentetraammonium bis monohydrogenmonophosphate dihydrate is monoclinic with the following unit cell dimensions: a = 8.462(1), b = 10.500(1), c = 9.520 Å, = 99.297(1)°, space group P21/n with Z = 2. The structure was solved by the Patterson method and refined to final R value of 0.043 for 1590 independent reflections. The structure consists of infinite parallel two-dimensional [ 01] planes built of mutually connected ions and water molecules by strong O—H···O and N—H···O hydrogen bonding.  相似文献   

19.
The structure of an important intermediate, IUPAC name: 2-(2-nitrophenyl) acrylonitrile has been studied by X-ray crystallography. C9H6N2O2 is monoclinic, space groupP21/c with cell dimensionsa=7.045(1),b=10.011(1),c=12.016(1) Å,=97.88(1)°,V=839.5(2) Å3,Z=4,M r =174.30,D 0=1-38(1),D x =1.39(1) g cm–3,F(000)=360,T=293 K, (CuK)=1.5418 Å,=8.00 cm–1,R=0.034 for 987 observed reflections. The aromatic ring is nearly planar. The Nitro group is rotated out of the aromatic plane by 26.5(1)°. There are three C-HO[3.469(3), 3.245(3), and 3.440(3) Å] and one C-HN[3.561(3) Å] intermolecular interaction.N.C.L. Communication No. 4847.  相似文献   

20.
The spectroscopic and X-ray investigation of the N-(2-phenylethyl) amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid are reported. The1H NMR spectra for the title structure and for the N-(p-methoxybenzyl) amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid are given. The N-(2-phenylethyl)amide of -(1,1-ethylenedioxy)-ethyl--hydroxybutyric acid, C16H23O4N, crustallizes in the monoclinic space groupP2 1/c witha=21.547(5),b=6.333(2),c=11.822(3) Å and =101.01(2)°. The dioxolane ring has a half-chair conformation with C2(O3)=2.4° and ||av=18.2°. The inconsiderable deviations from planarity of the six atoms of the amide group are caused mainly by twist around the C4–N1 bond and out-of-plane bending at the N1 atom ((C4–N1)=4°, XN =7°, Xc =0.4° ). The amide group plane is nearly coplanar with the phenyl ring. The molecules are connected by two intermolecular hydrogen bonds.  相似文献   

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