Synthesis,characterization, and X-ray crystal structure of tris(1,10-phenanthroline)nickel(II) perchlorate hemihydrate

The title compound was synthesized and characterized by conventional methods and its X-ray crystal structure was determined. The complex crystallizes in the monoclinic space group C2/c with eight formula units in a cell of dimensions:a=36.714(4),b=15.746(2),c=12.337(2) Å; =102.9(1)°. The structure is built up by alternate layers of octahedral [Ni(phen)₃]²⁺ cations and perchlorate anions with water molecules which run in the direction of thea axis nearly parallel to thebc plane.     

Crystal structure of dinitro(2,9-dimethyl-1,10-phenanthroline)-palladium(II)

Dinitro(2,9-dimethyl-1,10-phenanthroline)-palladium(II) crystallizes in the orthorhombic system, space groupP2₁ nb, with cell dimensionsa = 6·790,b = 19·807,c = 10·625 Å andZ = 4. The structure was determined from three-dimensional Fourier syntheses and refined by full-matrix least squares, the finalR for 1155 measured reflexions being 0·07.     

3-D polymeric structure formed by hydrogen bonds of copper (II) complex

A new copper complex trans-Dichlorobis[4-methoxypyridine]copper(II) (1) was synthesized and its crystal structure determined by X-ray diffraction. The close Cu···Cl contacts between the molecular units form bi-bridged dimers. The Copper(II) ion completes its 4 + 2 coordination via interaction with the Cu···Cl close contact. The complex has a polymeric structure of infinite one-dimensional (1D) bi-bridged chains, consisting of six-coordinate copper(II) units. C–H···C l intermolecular interaction connect the 1D-chains in the structure of 1 which form to 3D structure. The π ··· π interactions between the aromatic rings are also observed in the hydrogen bonded assembly of 1.     

Mercury(II) halide complexes with N-donor organic ligands: crystal and molecular structure of HgI2R, R = 1,10-phenanthroline, 2,9-dimethyl-1,10-phenanthroline, bipyridine

The synthesis, characterization and single crystal X-ray structure of three compounds of general formula HgI₂R (R = phen[1], dmph [2] and bpy[3]) are presented. The crystal data for the three compounds are: [1], triclinic, space group P (#2) a = 7.902(2), b = 9.479(2), c = 10.002(2) Å, = 91.45(2), = 111.34(2), = 100.82(2)° [2]: monoclinic, space group C2/c (#15) a = 15.670(3), b = 11.640(2), c = 9.730(2) Å, = 114.57(3)° [3]: triclinic, space group P1¯ (#2) a = 9.472(1), b = 9.507(1), c = 9.023(1) Å, = 98.46(1), = 102.89(1), = 119.62(1)°. Compounds [1] and [2] are monomers, with highly distorted tetrahedral environments around Hg. In [3], instead, there is a significant intermolecular I···Hg interaction leading to the formation of softly bound dimers linking two pentacoordinated cations. The structure is compared with related ones in the literature.     

Synthesis and crystal structure of a new dysprosium(III) complex with 2-fluorobenzoato and 1,10-phenanthroline

The dysprosium complex with 2-fluorobenzoato (2-FBA) and 1,10-phenanthroline (phen) was synthesized and characterized by X-ray diffraction. The complex crystallizes in the triclinic system with space group , lattice parameters: a = 11.233(7)  Å, b = 12.598(8)  Å, c = 22.718(14)  Å, α = 81.045(13)°, β = 78.213(12)°, γ = 80.506(11)°, V = 3079(3) ų, Z= 2, Dcalc = 1.689 Mg/m³. The complex contains two independent binuclear molecules, namely, [Dy(2-FBA)₃·phen·CH₃CH₂OH]₂ (I) and [Dy(2-FBA)₃·phen]₂ (II). In molecule (I), Dy1³⁺ ion is coordinated by eight atoms, five O atoms from five 2-FBA groups, one O atom from an ethanol molecule and two N atoms from the phen ligand. The 2-FBA groups adopt monodentate and bridging two-coordination modes. In molecule (II), the Dy2³⁺ ion is coordinated by nine atoms, seven O atoms from five 2-FBA groups and two N atoms from the phen ligand. The 2-FBA groups adopt chelating, bridging and chelating-bridging three-coordination modes.Supplementary material CCDC-257186 for the compound contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from CCDC, 12 Union Road, Cambridge, CB2 1EZ, UK; fax: (44(0) 1223-336033; email: deposit@ccdc.cam.ac.uk.     

Crystal structure of an unusual four-coordinated copper(II) complex containing 1,10-o-phenanthroline and salicyclic acid crystal structure containing Cu(II) o-phen and salicyclic acid

We have synthesized a multi-ligand chelate copper(II) complex [Cu · (C₇H₅O₃] · (C₁₂H₈N₂) · H₂O₁ · (C₇H₆O₃)· NO₃, and determined its structure by X-ray diffraction method. The space group of the title compound is P2₁/a. It is monoclinic, with a = 14.227(4), b = 9.627(4), c = 19.008(7) Å, β = 102.06(3)·, Z = 4. The two salicyclic acid molecules in the cell are in different environments, one inner, the other outer. The geometry around Cu(II) is a four-coordinated distorted plane square. The two coordinating atoms are two nitrogen atoms from phenanthroline, one oxygen atom from salicyclic acid, one oxygen atom from water.     

X-ray crystal structure oftrans-dichlorobis(2,4,6-collidine)-copper(II)

The X-ray crystal structure oftrans-dichlorobis(2,4,6-collidine)copper(II) has been determined. Dark blue crystals of the complex crystallize in the monoclinic space group P2₁/c, with cell dimensionsa=7.527(3),b=14.732(4),c=7.951(4)Å and=92.79(9)°;V=880.6(6)ų andZ=2. 949 unique reflections withI _net>3(I) on refinement afforded values ofR=0.041 andR _w =0.048.     

X-ray crystal structure oftrans-dichlorobis(2,6-lutidine)palladium(II)

The X-ray structure oftrans-(2,6-lutidine)₂PdCl₂ has been determined. Golden orange crystals of the complex crystallize in the triclinic space group , with cell dimensionsa=7.6950(8),b=7.9705(10),c=8.0485(8)Å, =116.967(9), =113.343(8), and =93.836(9)°;V=385.18(7)ų andZ=2. 1336 unique reflections withI _net>3 (I) on refinement afforded values ofR=0.018 andR _w=0.023.     

X-ray crystal structure and spectroscopy of a pseudo-square pyramidal Cu(II) complex, trans-dinitratotetrakis (trans-4-styrylpyridine)copper(II)

Single crystals of the title Cu(II) complex, [Cu(stpy)₄(ONO₂)(ONO₂)] [stpy = trans-4-styryl-pyridine] have been prepared and characterized by elemental and thermal analyses, IR, electronic and EPR spectral measurements, and X-ray crystal structure determination. The complex crystallizes in the monoclinic space group P2₁/c with unit-cell parameters, a = 12.985(2), b = 22.865(8), c = 17.024(10) Å, = 112.29(3)°, and Z = 4. The structure consists of discrete monomeric units of [Cu(stpy)₄(ONO₂)(ONO₂)]. The equatorial positions of the Cu(II) polyhedron are occupied by nitrogen atoms of the four stpy ligands and the axial positions by the oxygens of two unidentate nitrate anions. One of these oxygens is at rather longer distance [2.609(3) Å] and may be considered to be semicoordinated. If this semibond is ignored, the coordination geometry lies closer to an idealized square pyramid than to the trigonal bipyramid geometry. IR spectra reveal nitrogen coordination from stpy and asymmetry in the monodentate oxygen binding of the two nitrate ligands. The optical reflectance band at 600 nm suggests pseudo-square-based pyramidal geometry around Cu(II). Well-resolved Cu(II) hyperfine features in the EPR spectra reveal the absence of exchange interactions between adjacent copper centers. Optical and EPR spectra of a methanolic solution of the complex indicate solvent interactions. Thermogravimetric analysis shows the complex to be stable up to 175°C.     

X-ray crystal structure of tetraaquabis (xanthosinato)nickel(II) hexahydrate

The complex [Ni(XsH_–1)₂(H₂O)₄]·6H₂O (XsH_–1: xanthosinate) was isolated from the reaction of nickel carbonate with xanthosine in aqueous solution. The octahedral coordination is supported by the reflectance measurements. Single-crystal X-ray diffraction studies show that the crystals belong to the triclinic P1 space group, with a = 7.152(1), b = 8.830(1),c = 13.783(1) Å, = 82.024(1)°, = 86.155(1)°, = 70.900(1)°, and D = 1.643 mg/m³, forZ = 1. Nickel is six coordinate with four water molecules, and two N7 atoms from xanthosinato ligands. A complicated hydrogen-bonding network is present, all possible donors taking part in it.     

Synthesis and crystal structure of thiosemicarbazide complexes of nickel(II) and copper(II)

Thiosemicarbazide complexes of nickel(II) [Ni(TSC)₂](HSal)₂ (I) and copper(II) [Cu(TSC)₂](HSal)₂ (Ia) (TSC is thiosemicarbazide and HSal is a salycilate anion), as well as complexes [Ni(TSC)₂](SO₄) · 2H₂O (II) and [Ni(TSC)₃]Cl₂ · H₂O (III), are synthesized and characterized by IR spectroscopy and X-ray diffraction. Monoclinic crystals I and Ia are isostructural; space group P2₁/n, Z = 2. Crystals II are monoclinic, space group P2₁/m, Z = 2. Crystals III are orthorhombic, space group Pbca, Z = 8. In I and Ia, two planar salycilate anions sandwich a planar centrosymmetric [Ni(TSC)₂]²⁺ cation to form a supermolecule. The cation and anions are additionally bound by hydrogen bonds. Other hydrogen bonds connect supermolecules into planar layers. In structure II, centrosymmetric [Ni(TSC)₂]²⁺ cations are connected by ??-stacking interactions into supramolecular ensembles of a specific type. The ensembles, water molecules, and (SO₄)^2? anions are bound in the crystal via hydrogen bonds. In the [Ni(TSC)₃]²⁺ cation of structure III, ligands coordinate the Ni atom by the bidentate chelate pattern with the formation of five-membered metallocycles. These metallocycles have an envelope conformation unlike those in I and II, which are planar. In III (unlike in analogous complexes), a meridional isomer of the coordination octahedron of the Ni atom is formed. Together with Cl1^? and Cl2^? anions, cations form supermolecules, which are packed into planar layers with a square-cellular structure. The layers are linked by hydrogen bonds formed by crystallization water molecules that are located between the layers.     

Dinuclear complex of rhodium(III) with an amine-phenol ligand: synthesis and X-ray crystal structure

A new rhodium(III) complex of an amine-phenol ligand N,NN-bis-(2-hydroxybenzyl)1,3-diaminopropane was synthesized and characterized by X-ray diffraction studies. Diffraction data were collected by the-2 scan method using MoK. radiation. The structure was solved by conventional methods resulting in a final R factor of 0.037 for 1954 independent reflections (F _o >2(F _o )). The structure consists of a dinuclear complex with two -hydroxy bridges between the two Rh atoms. The overall charge of the molecule is neutral due to deprotonation of all phenolic groups. Crystal data: triclinic, space groupP¯1,a=7.308(3)Å;b=9.586(3)Å,c=12.686(5)Å, =87.51(2), =88.28(2), =71.70(3)°,V=866.6(6)ų;Z=2.     

Two novel two-dimensional frameworks with channels built from hydrogen bonds: Structures and properties study on copper(II) and nickle (II) complexes of the macrocyclic ligand 1,4,7-triazacyclodecane (tacd)

Two novel supramolecular complexes [Cu(tacd)₂](C₄H₃O₄)₂ (1) and [Ni(tacd)₂]Cl₂·4H₂O (2) were synthesized and their structures were characterized by elemental analysis, IR spectrum, TGA and single-crystal X-ray analysis. The results indicated that the complexes 1 and 2 assemble into different 2D supramolecular net-work structures with channels via hydrogen bonds interaction. TGA curves showed the steps of weight-loss for 1 and 2.     

Synthesis and crystal structure of a new two-dimensional chromium(III) network through hydrogen bonds

A new chromium(III) complex, [Cr(ox)(bdmpza)(H₂O)], (ox = oxalate dianion and bdmpza = bis(3,5-dimethylpyrazol-1-yl)acetate, respectively), has been synthesized and characterized by X-ray crystallography. This compound crystallizes in the monoclinic space group P2₁/c, with a = 7.008(3) Å, b = 14.229(5) Å, c = 16.497(7) Å, = 101.588(7)°, V = 1611.5(11) ų, Z = 4. The chromium atom has a distorted octahedral environment with different coordination atoms. Bis(3,5-dimethylpyrazol-1-yl)acetate anion is a tridentate ligand, and the oxalate group acts as a chelating bidentate ligand. This compound also forms an infinite two-dimensional network through O–H O hydrogen bonds. The lengths of the hydrogen bonds are 2.765(5) and 2.733(5) Å, respectively.     

Synthesis and crystal structure of a macrocyclic azidotetraamine copper(II) complex

The complex [Cu(L)N₃](H₂O)(ClO₄) (1) (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^1.18, 0^7.12]docosane) has been prepared and characterized by X-ray crystallography. 1 crystallizes in the monoclinic space group P2₁/c, with a = 8.907(5), b = 20.036(3), c = 14.773(2) Å, = 103.78(2)°, V = 2560.6(15) ų, and Z = 4. The coordination geometry around the Cu(II) ion is a distorted square-pyramidal with four nitrogen atoms of the macrocycle and one nitrogen atom of the axial azido group.     

X-ray crystal structure of trans-bis(monoethanolamine) bis(saccharinato)nickel(II)

The crystal structure of trans-bis(monoethanolamine)bis(saccharinato)nickel(II), [Ni(C₇H₄NO₃S)₂(C₂H₇NO)₂], has been determined from X-ray diffraction data. The metal complex is monoclinic, with a = 11.0555(5), b = 8.9103(4), c = 11.3890(5) Å, = 105.0230(10)°, Z = 2, and space group P2_1/c . The structure consists of individual molecules. Two monoethanolamine molecules and two saccharinate anions coordinate the nickel atom forming a distorted octahedron. The monoethanolamine molecules act as a bidentate ligand and form five-membered trans chelate rings, which constitute the plane of the coordination octahedron, while two saccharinate ions behave as a monodentate ligand occupying the axial positions. Intermolecular hydrogen bonds link the molecules to form a three-dimensional infinite structure.     

Synthesis and structure of a hexaazamacrocyclic copper(II) complex with maleato ligand

A hexaazamacrocyclic copper(II) complex Cu(L)(H₂O) (O₂CCH = CHCO₂)⋅H₂O (1) (L = 3,10-bis(2-hydroxyethyl)-1,3,5,8,10,12-hexaazacyclotetradecane) was prepared and structurally characterized by a combination of analytical, spectroscopic, and crystallographic methods. In complex 1, the coordination geometry about the copper(II) ion is six-coordinate with four equatorial nitrogen atoms from the macrocycle and two oxygen atoms from the axial maleato and aqua ligands. In 1, the one end of the maleato ligand coordinates to the central copper atom, while the other end is not bonded. The macrocycle and the axial ligands are highly involved in multiple types of hydrogen bonding interactions, resulting in the stabilization of the maleato ligand as a “coordinated ligand counter anion.”     

Synthesis and the crystal and molecular structure of two modifications of bis(1,10-phenanthroline)trinitratoerbium(III) Er(NO3)3(Phen)2

Two crystalline modifications (I and II) of the phenanthroline complex of erbium nitrate with the same chemical composition, Er(NO₃)₃(Phen)₂, are synthesized by a procedure similar to that used for preparing the phenanthroline complexes of europium nitrate. The crystal structures of these modifications are determined using X-ray diffraction. Crystals of compound I belong to the isostructural family Ln(NO₃)₃(Phen)₂ (Ln = La-Lu). Crystals of compound II are isostructural to those of modification II (new phase) of the Eu(NO₃)₃(Phen)₂ compound. Crystals of I and II are monoclinic, space group C2/c, and Z = 4. The unit cell parameters are as follows: a = 11.126 Å, b = 17.815 Å, c = 12.976 Å, β = 100.45°, and V = 2529 ų for modification I and a = 9.459 Å, b = 15.463 Å, c = 17.076 Å, β = 93.52°, and V = 2493 ų for modification II. The molecular complexes in the structures of compounds I and II are nearly identical. The mean lengths of the Er-N and Er-O bonds are equal to 2.500 and 2.466 Å in compound I and 2.508 and 2.457 Å in compound II, respectively. The difference between the structures of compounds I and II is associated with the difference between intermolecular interactions in the unit cell.