Crystal and molecular structure of di-μ-chlorobis[2-[[[(2-hydroxy-1-naphthyl)methyl]imino]-ethanolato]N,O,O′]di-copper(II) hemihydrate

The structure of the title compound [Cu₂Cl₂(C₁₃H₁₂NO₂)₂]·1/2 H₂O has been determined from single crystal X-ray diffraction data by direct methods. Full-matrix least-squares refinement of the structural parameters led to conventionalR factor of 0.037 for 4367 intensities above 3(I). The compound forms a dinuclear complex with distorted tetragonal-pyramidal geometry at each copper center. The unsymmetrical dimers are formed by weak axial coordination to one copper center by chloride ligands which are in the base plane of the adjacent copper atom. The apical Cu1-C12 and Cu2-C11 distances are 2.788(1) and 3.130(1) Å, respectively. The Cu1-Cu2 separation is 3.4995(3) Å in the dimers. A disorder of one five-membered chelate ring has been observed. Two alternative positionsa andb of the C26 atom were found and refined with constrained bond lengths. The geometry of the ligand and hydrogen bonds is discussed.     

Crystal and molecular structure of di-μ-chlorobis[2-[[[(2-hydroxy-1-naphthyl)methyl]-imino]ethanolato]N,O,O′]di-copper(II) dihydrate

The crystal structure of the title compound has been determined from three-dimensional, single crystal X-ray diffraction data. [Cu₂Cl₂(C₁₃H₁₂NO₂)₂]·2H₂O crystallizes in the orthorhombic space group P2₁2₁2₁ with lattice constants,a=11.866(2),b=13.555(3),c=17.380(3) Å. Final full-matrix least-squares refinement of 3735 unique reflections yieldedR=0.054. The structure consists of dimeric C₂₆H₂₄Cl₂Cu₂N₂O₄ molecules and water molecules connected with the dimeric molecules by a hydrogen bond system. Both of the copper(II) centers are five-coordinated by twotrans oxygen atoms and one nitrogen atom from one ligand molecule and two chloride ions. The geometry at each copper(II) center is best described as distorted tetragonal pyramidal. The apical Cu1–Cl2 and Cu2–C11 distances are 2.747(2) and 2.938(3)Å, respectively. The Cu...Cu separation is 3.496(1)Å. The comparison with previously reported crystal structure of [Cu₂Cl₂ (C₁₃H₁₂NO₂)₂]·1/2H₂O is given.     

Structure of the adduct of bis(O,O′-diisopropyldithiophosphato) metal with pyridine: Ni[(iPrO)2PS2]2(py)2 and Cd[(iPrO)2PS2]2 (py)2(py = pyridine)

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.     

Reactions of [Mn2(μ-pyS)2(CO)6] with bidentate phosphines: X-ray structure of [Mn(η2-pyS) (η2-dppp)(CO)2] [dppp = Ph2P(CH2)3PPh2, pySH = pyridine-2-thiol]

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) ų, 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.     

The properties,crystal, and molecular structure of catena-[(μ-acetato-) (μ-phthalazine)silver(I)dihydrate]: {[Ag(μ-O2CCH3) (μ-PHZ) (H2O)2]2}n

The crystal and molecular structure of catena-[(-acetato) (-phthalazine)-silver(I)dihydrate], {[Ag(O₂CCH₃) (C₈H₆N₂)(H₂O)₂]₂}_n, has been determined by single crystal X-ray analysis: the space group is P2₁/n,a=16.150(8) Å,b=3.886(5) Å,c=18.716(9) Å, =96.02(5)°,V=1168 ų. Phthalazine (PHZ) bridges the silver atoms to form {Ag--PHZ]₂ dimeric subunits. These dimeric subunits are planar and stack by bridging acetates to form a polymeric lattice. The acetates also form an asymrnetric chelate ring with the silver atoms which result in a distorted, square pyramidal configuration. The complex is further characterized by its IR and thermal properties.     

Structure of bis(O,O′-diisopropyldithiophosphato-S,S′) (1,10-phenanthroline-N1,N10)zinc(II) complex, [Zn(phen)(S2P(OiPr)2)2]

The crystal and molecular structure of [Zn(phen)(S₂P(OiPr)₂)₂] (Phen = 1,10-phenanthroline) has been determined by X-ray crystallography. It crystallizes in the Monoclinic system, space group C2/c, with lattice parameters a = 19.315(4), b = 10.438(2), c = 16.567(3)Å, = 102.89 (3)°, and Z = 4. The complex has C₂ symmetry. The coordination geometry of each Zn atom, by two S atoms from two (O,O-diisopropyldithiophosphato) anions and by two N atoms from phenanthroline ligand, is that of a slightly distorted tetrahedron [Zn—S 2.2914(8)Å Zn—N 2.111(2)Å]. The Zn···S distances to the noncoordinated S atoms are long: 3.5276 Å, which are indicated that there are much weaker interactions between them.     

Synthesis,Structure, and Properties of the Tris(ethylendiamine)nickel(II) Dichloride Dihydrate [Ni(H2NCH2CH2NH2)3]Cl2 ⋅ 2H2O Crystals

Crystallography Reports - The conditions for synthesis of [Ni(H2NCH2CH2NH2)3]Cl2 ⋅ 2H2O ([Ni(en)3]Cl2 ⋅ 2H2O) crystals from aqueous solutions have been considered. The synthesized...     

Synthesis, crystal structure, and properties of the adduct of bis(O,O′-diisopropyl dithiophosphato)nickel(II) with pyridine [Ni(i-Pr2dtp)2(py)2]

A new adduct bis(pyridine)-bis(O,O-diisopropyl dithiophosphato-S,S)nickel(II), [Ni(i-Pr₂dtp)₂(py)₂] (dtp = dithiophosphate, py = pyridine) has been obtained by re-crystallization from CH₃COCH₃. The crystal and molecular structure of the title complex has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group P2₁/c, with lattice parameters a = 6.4890(13) Å, b = 16.386(3) Å, c = 14.830(3) Å, = 99.74(3)°, V = 1554.1(5) ų, and Z = 2. The crystal structure consists of discrete molecules of [Ni(i-Pr₂dtp)₂(py)₂], which displays a slightly distorted octahedral geometry for the NiS₄N₂ chromophore. Two O,O-diisopropyl dithiophosphate ions act as bidentate ligands with their S atoms coordinated to Ni atom. Each forms a four-membered chelate ring in the equatorial plane. The N atoms from two pyridine ligands are axially coordinated to the Ni atom. The Ni S bond distances are 2.4492(8) Å and 2.5711(9) Å, and the Ni bond distances are 2.127(3) Å. Thermal analyses show that the thermal decomposition of this adduct is so unstable that loss of two pyridine ligands begins at about 65°C. Electronic and IR spectra data is in agreement with the structural data.     

Catena-Poly[[[2,4-dichloro-6-{[(2-hydroxyethyl)imino]methyl}phenolato-κ3N,O,O']-copper(II)]-μ-chlorido]monohydrate]: Synthesis,structural, spectroscopic and luminescent properties

A new chloride bridged polymeric Cu(II) complex, [Cu(HL)(μ-Cl).H₂O]_n, 1, (H₂L = 2,4-dichloro-6-{[(2-hydroxyethyl)imino]methyl}phenol) has been synthesized and characterized by elemental-spectral analysis, crystal structure analysis and photoluminescence measurements. The Copper(II) atom is five-coordinate in a slightly distorted square-pyramidal geometry (τ = 0.085), with one N and two O atoms of the Schiff base ligand and one Cl atom defining the basal plane and a symmetry-related Cl atom occupying the apical position. The bridging Cl atom lies in apical position for one Cu(II) ion and basal for the other, and it makes this structural arrangement unusual. The linked moieties form polymeric zigzag chains running along the c axis. This zigzag chains connect each other with intramolecular and intermolecular O–H···O hydrogen bonds, which form 3D structure through π?π interactions. Furthermore, the photoluminescence properties of H₂L and 1 were investigated, they exhibit unique bright green visible emissions in the solid state, under the excitation of 349 nm UV light. The strong luminescence emission of them makes 1 a potentially useful photoactive material in photo-physical chemistry.     

A dinuclear cyanide-bridged complex, [(DMF)4(H2O)3LuCo(CN)6]·H2O

The crystal structure of the bimetallic cyanide bridged complex [(DMF)₄(H₂O)₃LuCo(CN)₆]·H₂O (1) was obtained by single-crystal X-ray diffraction. The central lutetium(III) ion is eight coordinate arranged in a square antiprism while the cobalt(III) ion is six coordinate, oriented octahedrally. Molecules in the crystal lattice are held together by a network of hydrogen bonding. Crystallization of 1 occurs in the centrosymmetric monoclinic space group P2₁/c (No. 14) with a = 13.875(2), b = 8.8352(9), c = 24.633(2) Å = 96.392(8)° and Z = 4.     

Structure of bis[α-(1,2,4-triazole-1-yl)-acetophenone] dichorozinc(II) complex [ZnCl2(C2H2N3CH2COPh)2]

The crystal and molecular structure of [ZnCl₂(N⁴-trzCH₂COPh)₂] (trz = 1,2,4-triazole) has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group C2/c, with lattice parameters a = 26.7892(4) Å, b = 4.9392(2) Å, c = 20.7872(1) Å, = 127.517 (1), and z = 4. The complex has C ₂ symmetry. The coordination geometry of each Zn atom is distorted tetrahedral formed by two Cl atoms and two tertiary N atoms of the -(1,2,4-triazole-1-yl)-acetophenone ligands. The two equivalent Zn–Cl and Zn–N bonds form bond angles around the Zn(II) atom in the range 101.4(1)–120.8(1). C–H O intermolecular interactions link the molecules in infinite chains in the [101] direction.     

Synthesis and crystal structure of trans-bis(O, O′-diisopropylthiophosphoryl-1H-imidazole-N3) bis(O,O′-diisopropyldithiophosphato) nickel(II) complex: Ni[N3-ImSP(OiPr)2]2[S2P(OiPr)2]2 (Im = imidazole; iPr = isopropyl)

The mononuclear complex, Ni[N³-ImSP(OiPr)₂]₂[S₂P(OiPr)₂]₂ (Im = imidazole; iPr = isopropyl), was unexpectedly obtained in a reaction of bis(O,O-diisopropyl-dithiophosphato) nickel(II) complex with imidazole ligand, and its structure was determined by X-ray crystallography. It crystallizes in the triclinic system, space group P , with lattice parameters a = 12.437(3) Å, b = 13.181(3) Å, c = 8.4580(17) Å, = 93.16(3)°, = 101.93(3)°, = 65.26(3)°, and Z = 1. The Ni atom has almost perfect octahedral coordination geometry and is coordinated by two N atoms of imidazole from two O,O-diisopropylthiophosphoryl-1H-imidazole ligands in axial positions and four S atoms from two (O,O-diisopropyldithiophosphato) anions which act as bidentate ligands forming a four-membered chelate ring in the equatorial plane. The Ni—S bond distances are 2.469(1) and 2.507(1) Å, and the Ni—N bond distances are 2.097(2) Å. The IR spectra data are in agreement with the structural data.     

Molecular and crystal structure of [NO2Py]2[Ni(mnt)2](NO2Py=1-(4-nitrobenzyl)pyridinium, mnt2−=maleonitriledithiolate)

The structure of [NO₂Py]₂[Ni(mnt)₂], as determined by x-ray single crystal analysis, consists of two 1-(4-nitrobenzyl)pyridinium cations and one [Ni(mnt)₂]^2– anion. The crystallographic data for the complex:monoclinic P2₁/n, a = 9.913(2) Å, b = 11.968(2) Å, c = 14.566(3) Å, = 100.36(3)°, V = 1699.9(6) ų, Z = 2. The [Ni(mnt)₂]^2– anion has a crystallographically imposed center of symmetry and exhibits a relatively planar structure. The cation, [NO₂Py]⁺, adopts a conformation where both the aromatic rings are twisted to the C11-C10-N3 reference plane. The anions (A) and the cations (C) consist of alternating layers (i.e., of type ···C₁A₁C₂A₂C₁A₁C₂···) along the c axis of the crystallographic unit cell.     

Crystal structure of triaquamaleatostrontium(II) monohydrate, [Sr(C4H2O4)(OH2)3]·H2O

[Sr(C₄H₂O₄)(OH₂)₃]·H₂O is monoclinic, P2₁/n, witha=11.476(2),b=7.027(1),c=12.344(2) Å, =115.74(3)°,V=896.67 ų,Z=4. The Sr atom is surrounded by nine oxygen atoms which come from four different maleate anions and three water molecules. The Sr–O distances range from 2.546(2) to 2.808(2) Å. The C–O distances are equal within the standard deviation 1.263(3) to 1.258(3) Å). In the maleate anion, the planes that contain the carboxylate groups form an angle of 74.44(9)°. Both carboxylate groups deviate significantly from planarity. The different coordination modes of the carboxylate group and the extensive hydrogen bonding present are responsible for the polymeric nature of the structure.     

Metal-pyrimidine interaction: synthesis and crystal structure of a cadmium complex of trimethoprim ([CdBr2(TMP)2(H2O)2]·H2O, TMP = trimethoprim)

The crystal structure of a cadmium complex of trimethoprim ([CdBr₂(TMP)₂(H₂O)₂] · H₂O, TMP = trimethoprim) has been determined from X-ray diffraction data using MoK radiation. The crystals are monoclinic, C2/c, with a = 7.7811(11), b = 15.439(3) c = 29.645(6)Å, = 97.23(2)° and Z = 4. Trimethoprim (2,3-diamino(3,4,5trimethoxybenzyl)pyrimidine) acts as a monodentate ligand. Cadmium is coordinated to N(1) atoms of two trimethoprim moieties. The octahetral coordination geometry around cadmium is completed by two Br-ions and two water molecules. The complex has a two-fold axis coinciding with a crystallographic two-fold axis. There is an interligand hydrogen bond between the bromide ion and the 2-amino group of the pyrimidine.     

Crystal and molecular structure of (3aR,8bS,5′R)3-[(2,5-dihydro-3-methyl-2-oxo-5-furanyl)oxymethylene]-3,3a,4,8b-tetrahydroindeno[1,2-b]furan-2-one

The stereogeometry and absolute configuration of the title compound has been proved by an X-ray diffraction analysis. Crystal data: monoclinic, C2,a=20.2528(4),b=6.7254(2),c=10.6748(2) Å, =94.699(3),Z=4. The crystal structure has been solved by vector search methods and refined toR ₁=0.053 for 2043 observed reflections.     

配合物[Co(SCN)2(HSCN)2(dabco)2]的合成、晶体结构与表征

以SCN-和三乙撑二胺(dabco)为配体,以钴为中心离子采用自组装的方法合成了配合物[Co(SCN)2(HSCN)2(dabco)2],采用单晶X射线衍射、红外光谱、热重分析和元素分析等方法对其进行了晶体结构的解析和表征.它属于单斜晶系,P21/n空间群,晶胞参数分别为a＝0.71964(11)nm,b＝1.12716(17)nm,c＝1.4454(2)nm,β＝96.629(2)°,V＝1.1646(3)nm3,Dc＝1.470 g/cm3,Z＝2,F(000)＝534,μ＝1.115mm-1.热重分析表明,该配合物在530 K以下稳定.     

Crystal structure of triethanolammonium bis(1-hydroxyethane-1,1-diphosphonato)diaquazincate pentahydrate, [(OHCH2CH2)3NH][Zn(H2O)2(H2.5 L)2] ⋅ 5H2O

The crystal structure of [(HOCH₂CH₂)₃NH][Zn(H₂O)₂(H_2.5 L)₂] ? 5H₂O, where H₄ L is 1-hydroxyethane-1,1-diphosphonic acid, was determined by X-ray diffraction. The anionic complex has a cis-octahedral structure. The zinc atom is coordinated by four O atoms of two bidentate chelate H_2.5 L ^1.5? ligands and two O atoms of water molecules. The Zn-O(L) bond lengths range between 2.050 and 2.175 Å, and the Zn-O(H₂O) bond lengths are 2.105 and 2.133 Å. The anionic complexes, triethanolammonium cations, and molecules of crystallization water are interlinked by an extensive network of hydrogen bonds. The crystallographic data for isostructural complexes of cobalt and nickel are given.     

Reaction of trimethylaluminum and trimethylgallium with bifunctional amines: Syntheses and molecular structures of [Me2Al−N(CH2CH2)2−C−(OCH2)2]2 and [Me2Ga−N(Si(H)Me2)2]2

The crystalline products [Me₂Al–N(CH₂CH₂)₂–C–(OCH₂)₂]₂ (I) and [Me₂Ga–N(Si(H)Me₂)₂]₂ (II) were prepared from reactions of trimethylaluminum and trimethylgallium with 1,4-dioxa-8-azaspiro[4.5]-decane and 1,1,3,3-tetramethyldisilazane, respectively, in toluene. The organoaluminum dimer crystallizes in the monoclinic space groupP2₁/c with unit cell parametersa=8.970(2) ,b=9.683(2) ,c=12.833(3) , =103.18(2)°,V=1085.3(3) ³, andD _calcd=1.22 g cm^–3 forZ=2. Least-squares refinement based on 935 observed reflectionsI>3(I) in the range 3.5°<2<45.0° led to a finalR factor of 0.033 (R _w =0.041). The dimeric organosilazagallium crystallizes in the triclinic space group with unit cell parametersa=7.636(2) ,b=9.168(2) ,c=9.466(3), =72.81(2)°, =87.94(2)°, =69.90(2)°,V=593.0(3) ³, andD _calcd=1.30 g cm^–3 forZ=1. Least-squares refinement based on 1661 observed reflectionsI>3(I) in the range 3.5°<2<48.0° led to a finalR factor of 0.055 (R _w =0.070). Both compoundsI andII reside about a crystallographic center of symmetry and contain a planar M₂N₂ (M=Al forI, Ga forII) four-membered ring withI having an Al...Al contact of 2.801 .