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1.
Reaction of the N-(2-pyridyl)carbonylaniline ligand (L) with Cu(NO3)2, Cu(ClO4)2, Zn(ClO4)2, Ni(NO3)2 and PdCl2 gives complexes with stoichiometry [Cu(L)2(H2O)2](NO3)2, [Cu(L)2(H2O)2](ClO4)2, [Zn(L)2(H2O)2] (ClO4)2, [Ni(L)2(H2O)Cl](NO3) and PdLCl2. The new complexes were characterized by elemental analyses and infrared spectra. The crystal structures of [Cu(L)2(H2O)2](NO3)2, [Cu(L)2(H2O)2](ClO4)2, and [Zn(L)2(H2O)2](ClO4)2 were determined by X-ray crystallography. The cation complexes [M(L)2(H2O)2] contain copper(II) and zinc(II) with distorted octahedral geometry with two N-(2-pyridyl)carbonylaniline (L) ligands occupying the equatorial sites. The hexa-coordinated metal atoms are bonded to two pyridinic nitrogens, two carbonyl oxygens and two water molecules occupying the axial sites. Both the coordinated water molecules and uncoordinated amide NH groups of the N-(2-pyridyl)carbonylaniline (L) ligands are involved in hydrogen bonding, resulting in infinite hydrogen-bonded chains running in one and two-dimensions.  相似文献   

2.
The complexes cis-Mo(CO)2(Ph2P(CH2)nPPh2)2 (n = 1, 2, 3) are synthesized by heating benzene solutions of cis-dicarbonylbis(norbornadiene)molybdenum and the corresponding diphosphines. The X-ray structural analysis of cis-Mo(CO)2(Ph2P(CH2)3PPh2)2 is reported, with the following crystal data: C56H52MoO2P4·2CH2Cl2·0.5C6H14, mol wt. 1189.81, monoclinic, space group P21/n, a 15.643(2), b 21.453(7), c 17.105(3) Å, β 100.75(1)°, V 5639.59 Å3, Z = 4, Dc 1.39, Dm 1.36 g/cm3.  相似文献   

3.
Treatment of [Rh2Cl2(CO)2 {μ-(PhO)2PN(Et)P(OPh)2}2] with various reducing agents gives a number of products, the type depending on the conditions employed. The products isolated include [Rh2(CO)2{μ-(PhO)2PN(Et)P(OPh)2}2], [Rh2(CO)3{μ-(PhO)2PN(Et)P(OPh)2}2],and [Rh2HgCl(μ-H)(CO)2{μ-(PhO)2PN(Et)P(OPh)2}2]; the structure of the last complex was determined by X-ray diffraction.  相似文献   

4.
Diamino-di-tert-butylsilanes - Building Blocks for Cyclic (SiN)2, (SiNBN)2, (SiN2Sn), and Spirocyclic (SiN2)2Si, (SiN2Sn)2S Compounds The aminochlorosilanes (Me3C)2SiClNHR ( 1 : R?H, 2 : R?Me) are obtained by the ammonolysis ( 1 ) respectively aminolysis ( 2 ) of di-tert-butyldichlorosilane in the n-hexane. The dilithium derivative of diamino-di-tert-butylsilane reacts with FSiMe2R′ ( 3 : R′?Me, 4 : R′?F) in a molar ratio 1 : 2 to give the 1,3,5-trisilazanes 3 and 4 , (Me3C)2SiNHSiMe2R′, in a molar ratio 1 : 1 with F3SiN(SiMe3)2 to give the 1,3-diaza-2,4-disilacyclobutane 5 , (Me3C)2Si(NH)2SiFN(SiMe3)2, and with F2BN(SiMe3)2 to give the 1,3,5,7-tetraaza-2,6-dibora-4,8-disilacyclooctane 6 , [(Me3C)2SiNH-BN(SiMe3)2-NH]2. The dilithium derivative of di-tert-butyl-bis(methylamino)silane reacts with SiF4 with formation of the 1,3,5-trisilazane 7 , (Me3C)2Si(NMeSiF3)2, and the spirocycic compound 8 , [(Me3C)2Si(NMe)2]2Si, with SnCl2 the cyclosilazane 9 , (Me3C)2SiNMe2 is obtained. The dilithium derivative of 3 reacts with SnCl2 to give the cyclo-1,3-diaza-2-sila-4-stannylen 10 , (Me3C)2Si(NSiMe3)2Sn. The oxidation of 10 with elemental sulfur leads to the formation of the spirocyclus 11 , [(Me3C)2Si(NSiMe3)2SnS]2.  相似文献   

5.
(Hg2)Hg(OH)2(ClO4)2: The First Mixed Valent Mercury Perchlorate Colorless single crystals of (Hg2)Hg(OH)2(ClO4)2 (C2/c, Z = 4, a = 1847.7(5), b = 490.8(1), c = 1086.2(3) pm, β = 93.80(2)°, Rall = 0.0610) were obtained as a side product during the dehydration of Hg2(ClO4)2 · 2H2O. The crystal structure consists of infinite zig‐zag chains {∞1[(Hg2)1/2(OH)Hg1/2]+}2 which are separated by the ClO4— ions.  相似文献   

6.
《Polyhedron》1987,6(6):1351-1360
Interaction of trans-VCl2(dmpe)2 with sodium amalgam in tetrahydrofuran under CO gives trans-V(CO)2(dmpe)2. The latter is oxidized by Ag+ in acetonitrile to give [cis-V(CO)2(dmpe)2(CH3CN)]+, isolated as the tetraphenylborate. Interactions with acids (HX) gives neutral complexes of the type V(CO)2(dmpe)2X (X = Cl, MeCO2, EtCO2, CF3CO2, PhPO2H or NH2SO3); the chloride can be exchanged with N3− or CN− in methanol. X-ray structural studies confirm the trans stereochemistry for V(CO)2(dmpe)2 and the seven-coordination of VI in both [V(CO)2(dmpe)2(CH3CN)][BPh4] and V(CO)2(dmpe)2(O2CEt), which have a pseudo octahedral geometry with the two carbonyls occupying a “split” axial site. 51V NMR and other spectra are reported.  相似文献   

7.
In the title compound, (2-chloro­benzyl)­tris­(pyridine-2-thiol­ato)-κ2N,S;κ2N,S;κS-tin(IV), [Sn(C7H6Cl)(C5H4NS)3], two of the three pyridine-2-thiol­ato ligands (SPy) are bidentate and one is monodentate. The bonding C atom of the 2-chloro­benzyl group, the S atom of the monodentate SPy and the S and N atoms of the two bidentate SPy ligands form a distorted octahedron around the Sn atom. The three S atoms and the N atom of one of the bidentate SPy ligands occupy the equatorial positions, while the N atom of the second bidentate SPy ligand and the C(CH2) atom are axial. The axial N—Sn—C angle of 157.9 (1)° demonstrates the heavy distortion of the octahedron.  相似文献   

8.
Four copper(II) complexes and one copper(I) complex with pyridine-containing pyridylalkylamide ligands N-(pyridin-2-ylmethyl)pyrazine-2-carboxamide (HLpz) and N-(2-(pyridin-2-yl)ethyl)pyrazine-2-carboxamide (HLpz?) were synthesized and characterized. The X-ray crystal structures of [Cu2(Lpz)2(4,4?-bipy)(OTf)2] (1, OTf?=?trifluoromethanesulfonate, 4,4?-bipy?=?4,4?-bipyridine) and [Cu(Lpz)(py)2]OTf·H2O (2, py?=?pyridine) revealed binuclear and mononuclear molecular species, respectively, while [Cu(Lpz)(μ2-1,1-N3)]n (3), [Cu(Lpz?)(μ2-1,3-N3)]n (4), and [Cu(HLpz)Cl]n (5) are coordination polymer 1-D chains in the solid state.  相似文献   

9.
Two new complexes, [Co2(CH2=C(CH3)CO2)4(phen)2(H2O)2] (1) and [Pb2(CH2=C(CH3)CO2)4(phen)2] (phen = 1,10-phenanthroline) (2), have been synthesized and structurally characterized by single crystal X-ray diffraction methods. There are two cocrystallized conformers of [Co(CH2=C(CH3)CO2)2(phen)(H2O)] in the asymmetric unit of 1 with the Co atoms displaying similar coordination modes. In the asymmetric unit of 2, there exist two crystallographically independent [Pb(CH2=C(CH3)CO2)2(phen)] molecules with the Pb atoms showing completely different coordination geometries. Weak intermolecular interactions such as hydrogen bonding and π–π stacking are responsible for the supramolecular assembly and stabilization of the crystal structures of 1 and 2. The complexes are characterized by elemental analysis, IR spectra, and UV–Vis spectra. The fluorescent properties of 2 are also discussed.  相似文献   

10.
Normal Coordinate Analysis of (CH3)2SO2, (CH3)2SO(NH), and (CH3)2S(NH)2 using the Method of Stepwise Coupling The qualitative assignment of the vibrational spectra of (CH3)2SO2 ( 1 ), (CH3)2SO(NH) ( 2 a ), and (CH3)2S(NH)2 ( 3 a ) and of the C and N deuterated derivatives of 2 a and 3 a is used in a normal coordinate analysis by the method of stepwise coupling. The force constants and the energy distributions are calculated in symmetry coordinates using a generalized valence force field.  相似文献   

11.
Synthesis and Structure of the Platinum(0) Compounds [(dipb)Pt]2(COD) and (dipb)3Pt2 and of the Cluster Hg6[Pt(dipb)]4 (dipb = (i-Pr)2P(CH2)4P(i-Pr)2) The reduction of (dipb)PtCl2 with Na/Hg yields (dipb)Pt as an intermediate which reacts with the amalgam to form the cluster Hg6[Pt(dipb)]4 ( 3 ) or decomposes to (dipb)3Pt2 ( 2 ) and Pt. In the presence of COD [(dipb)Pt]2(COD) ( 1 ) is obtained. 1 crystallizes monoclinicly in the space group P21/c with a = 1596.1(4), b = 996.5(2), c = 1550.4(3) pm, β = 113.65(2)°, Z = 2. In the dinuclear complex two (dipb)Pt units are bridged by a 1,2-η2-5,6-η2 bonded COD ligand. Whereby the C = C double bonds are lengthened to 145 pm. 2 forms triclinic crystals with the space group P1 and a = 1002.0(2), b = 1635.9(3), c = 868.2(2) pm, α = 94.70(2)°, β = 94.45(2)°, σ = 87.95(1)°, Z = 1. In 2 two (dipb)Pt moieties are connected by a μ-dipb ligand in a centrosymmetrical arrangement. 3 is monoclinic with the space group C2/c and a = 1273.8(3), b = 4869.2(6), c = 1660.2(3) pm, β = 95.16(2)°, Z = 4. The clusters Hg6[Pt(dipb)]4 have the symmetry C2. Central unit is a Hg6 octahedron of which four faces are occupied by Pt(dipb) groups. The bonding in the cluster is discussed on the basis of eight Pt? Hg two center bonds of 267.6 pm and two Pt? Hg? Pt three center bonds with Pt? Hg = 288.0 pm.  相似文献   

12.
The magnetic and spectroscopic (UV, visible-IR and electron paramagnetic resonance spectra) properties of the molecular complexes [Co(AGlH)2py2][Cr(NH3)2(NCS)4] and [Co(AGlH)2py2][Co(NH3)2(NO2)4] (where AGlH2 is diaminoglyoxime) have been examined in solid state. The molecular structure of the complexes and the nature of the interaction in the crystals has been considered.  相似文献   

13.
Synthesis and Crystal Structures of the Zinc Amido Complexes [Zn(NPh2)2]2 and [Zn(NPh2)2(THF)2] Zinc diphenylamide is prepared from Zn[N(SiMe3)2]2 and diphenylamine by transamination reaction. The compound is characterized by a crystal structure analysis. According to it [Zn(NPh2)2]2 forms centrosymmetric dimeric molecules with Zn–N distances of 185.9 pm for the terminally bonded NPh2– ligand and Zn–N distances of 204.0 and 202.6 pm in the four-membered ring. From tetrahydrofuran solutions [Zn(NPh2)2(THF)2] crystallizes as monomeric molecular complex with Zn–N bond lengths of 192.2 pm in average.  相似文献   

14.
Synthesis, Crystal Structure and Spectroscopic Characterization of [Au12(PPh)2(P2Ph2)2(dppm)4Cl2]Cl2 The reaction of [(AuCl)2dppm] (dppm = Ph2PCH2PPh2) with P(Ph)(SiMe3)2 in CHCl3 results in the formation of [Au12(PPh)2(P2Ph2)2(dppm)4Cl2]Cl2 ( 1 ), the crystal structure of which was determined by single crystal X‐ray analysis (space group P21/c, a = 1425.3(3) pm, b = 2803.7(6) pm, c = 2255.0(5) pm, β = 95.00(3)°, V = 8977(3)·106 pm3, Z = 2). The dication in 1 consists of two Au6P3 units built by highly distorted Au3P and Au2P2 heterotetrahedra, connected via four bidentate phosphine ligands. Additionally, the compound was characterized by IR‐, UV‐ and NMR spectroscopy. The 31P{1H} NMR spectrum is discussed in detail.  相似文献   

15.
Synthesis of [Cu(m-HBH)2(OH2)2](NO3)2·2H2O, where m-HBH = C7H8O2N2 (3-hydroxybenzoylhydrazine), is described. The structure of the compound was studied by X-ray phase analysis and IR spectroscopy; crystal data are a = 57.415(6) Å, b = 19.760(2) Å, c = 7.586(2) Å; Fdd 2, Z = 16, R(F) = 0.053. The compound consists of [Cu(m-HBH)2(OH2)2]2+ complex cations, NO 3 ? anions, and two water molecules. The similarity between the IR spectra of Cu(m-HBH)2(NO3)2·nH2O and Co(m-HBH)2(NO3)2·5H2O, element analysis data, and crystal data obtained at the first stage of X-ray analysis show that the structures and compositions of these compounds are identical relative to the type of surroundings of the central atom. In contrast to the cobalt compound [Co(m-HBH)2(OH2)2](NO3)2·3H2O, in which the cobalt atom has a nearly regular octahedron as a coordination polyhedron, the copper(II) compound has a square bipyramid around the copper atom; c.n. is 6 = 4 + 2 (planar distances: 2.013(2) Å, 2.021(2) Å, 2.033(3) Å, 2.087(3) Å; axial distances: 2.367(3) Å, 2.374(3) Å) and lacks one crystallization water molecule.  相似文献   

16.
Molybdenum(VI) and tungsten(VI) dioxodiazide, MO2(N3)2 (M=Mo, W), were prepared through fluoride–azide exchange reactions between MO2F2 and Me3SiN3 in SO2 solution. In acetonitrile solution, the fluoride–azide exchange resulted in the isolation of the adducts MO2(N3)2⋅2 CH3CN. The subsequent reaction of MO2(N3)2 with 2,2′‐bipyridine (bipy) gave the bipyridine adducts (bipy)MO2(N3)2. The hydrolysis of (bipy)MoO2(N3)2 resulted in the formation and isolation of [(bipy)MoO2N3]2O. The tetraazido anions [MO2(N3)4]2− were obtained by the reaction of MO2(N3)2 with two equivalents of ionic azide. Most molybdenum(VI) and tungsten(VI) dioxoazides were fully characterized by their vibrational spectra, impact, friction, and thermal sensitivity data and, in the case of (bipy)MoO2(N3)2, (bipy)WO2(N3)2, [PPh4]2[MoO2(N3)4], [PPh4]2[WO2(N3)4], and [(bipy)MoO2N3]2O by their X‐ray crystal structures.  相似文献   

17.
Complexes Containing Antimony Ligands: [tBu2(Cl)SbW(CO)5], [tBu2(OH)SbW(CO)5], O[SbPh2W(CO)5]2, E[SbMe2W(CO)5]2 (E = Se, Te), cis‐[(Me2SbSeSbMe2)2Cr(CO)4] Syntheses of [tBu2(Cl)SbW(CO)5] ( 1 ), [tBu2(OH)SbW(CO)5] ( 2 ), O[SbPh2W(CO)5]2 ( 3 ), Se[SbMe2W(CO)5]2 ( 4 ), cis‐[(Me2SbSeSbMe2)2Cr(CO)4] ( 5 ) Te[SbMe2W(CO)5]2 ( 6 ) and crystal structures of 1 – 5 are reported.  相似文献   

18.
Abstract

Two isomalononitrile dithiolato complexes, (Bu4N)2Zn(i-mnt)2 (1) and (Et4N)2Pd(i-mnt)2 (2) were synthesized and characterized by elemental analysis, IR and electronic spectroscopy. Their structures have been crystallographically determined. The reaction of (Et4N)2Pd(i-mnt)2 (2) with (Et4N)2WS4 gives (Et4N)2WS4Pd(i-mnt).  相似文献   

19.
Reaction of O,O′-diisopropylphosphoric acid isothiocyanate (iPrO)2P(O)NCS with NH2(CH2)nNH2 (n = 3, 2) leads to the N-phosphorylated bis-thioureas [(iPrO)2C(S)NHP(O) NH]2Z (Z = —(CH2)3—, H2LI ; —(CH2)2—, H2LII ). Reaction of the potassium salt of H2LI with Co(II) and Zn(II) in aqueous EtOH leads to complexes of formula M2(L-O,S)2. The metal cation in both complexes is coordinated by two deprotonated ligands through the sulfur atoms of the thiocarbonyl groups and the oxygen atoms of the phosphoryl groups. Reaction of K2LI with Ni(II) and Pd(II) in the same conditions leads to M2(L-N,S)2 complexes. In both compounds, the metal center is found in a square-planar N2S2 environment formed by the C=S sulfur atoms and the P—N nitrogen atoms of two deprotonated ligands LI . Reaction of H2LII with KOH leads to a product of heterocyclization, in which one of the thiourea fragments is retained. Compounds obtained were investigated by IR, UV-Vis, 1H and 31P NMR spectroscopy, and microanalysis.  相似文献   

20.
Contributions on Crystal Structures and Thermal Behaviour of Anhydrous Phosphates. XXIII. Preparation, Crystal Structure, and Thermal Behaviour of the Mercury(I) Phosphates α-(Hg2)3(PO4)2, β-(Hg2)3(PO4)2, and (Hg2)2P2O7 Light-yellow single crystals of (Hg2)2P2O7 have been obtained via chemical vapour transport in a temperature gradient (500 °C → 450 °C, 23 d) using Hg2Cl2 as transport agent. Characteristic feature of the crystal structure (P2/n, Z = 2, a = 9,186(1), b = 4,902(1), c = 9,484(1) Å, β = 98,82(2)°, 1228 independent of 5004 reflections, R(F) = 0,066 for 61 variables, 7 atoms in the asymmetric unit) are Hg22+-units with d(Hg1–Hg1) = 2,508 Å and d(Hg2–Hg2) = 2,519 Å. The dumbbells Hg22+ are coordinated by oxygen, thus forming polyhedra [(Hg12)O4] and [(Hg22)O6]. These polyhedra share some oxygen atoms. In addition they are linked by the diphosphate anion P2O74– (ecliptic conformation; ∠(P,O,P) = 129°) to built up the 3-dimensional structure. Under hydrothermal conditions (T = 400 °C) orange single crystals of the mercury(I) orthophosphates α-(Hg2)3(PO4)2 and β-(Hg2)3(PO4)2 have been obtained from (Hg2)2P2O7 and H3PO4 (c = 1%). The crystal structures of both modifications have been refined from X-ray single crystal data [α-form (β-form): P21/c (P21/n), Z = 2 (2), a = 8,576(3) (7,869(3)), b = 4,956(1) (8,059(3)), c = 15,436(3) (9,217(4)) Å, β = 128,16(3) (108,76(4))°, 1218 (1602) independent reflections of 4339 (6358) reflections, R(F) = 0,039 (0,048) for 74 (74) variables, 8 (8) atoms in the asymmetric unit]. In the structure of α-(Hg2)3(PO4)2 three crystallographically independent mercury atoms, located in two independent dumbbells, are coordinated by three oxygen atoms each. Thus, [(Hg2)O6] dimers with a strongly distorted tetrahedral coordination of all mercury atoms are formed. Such dimers are present besides [(Hg2)O5]-polyhedra in the less dense crystal structure of β-(Hg2)3(PO4)2 (d(Hg–Hg) = 2,518 Å). The mercury(I) phosphates are thermally labile and disproportionate between 200 °C (β-(Hg2)3(PO4)2) and 480 °C (α-(Hg2)3(PO4)2) to elemental mercury and the corresponding mercury(II) phosphate.  相似文献   

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