Synthesis and crystal structure of (18-crown-6)(perchlorato-O)(triphenylphosphine oxide)potassium

A new complex, (18-crown-6)(perchlorato-O)(triphenylphosphine oxide)potassium, was synthesized and its structure was studied by X-ray diffraction. The crystals are trigonal: a = 14.419,c = 13.895 Å, Z = 3, space group R3m; the structure was solved by the direct method and refined by the anisotropic full-matrix least-squares method, R = 0.079 on 1930 independent reflections, CAD-4 automated diffractometer, λMoK _α . The structure contains a highly symmetric host-guest complex molecule [K(ClO₄)(18-crown-6)(Ph₃PO)] in position 3m (with three Ph rings of the Ph₃PO ligand and all the O atoms of a crown ligand lying in three m planes). The coordination polyhedron of the K⁺ cation is a distorted hexagonal bipyramid with six O atom of the 18-crown-6 ligand in a base and the O atom of the Ph₃PO ligand and disordered O atom of the ClO ₄ ^? ligand in the axial vertices.     

(18-Crown-6)(nitrato-<Emphasis Type="Italic">O,O</Emphasis>′)potassium and (18-crown-6)(nitrato-O,O′)potassium<Subscript>(0.91)</Subscript>silver<Subscript>(0.09)</Subscript>: Synthesis and crystal structures

Two complexes with similar compositions are synthesized: (18-crown-6)(nitrato-O,O′)potassium (I) and (18-crown-6)(nitrato-O,O′)potassium_(0.91)silver_(0.09) (II). Their isomorphic orthorhombic crystals (space group P2₁2₁2₁, Z = 4) are studied by X-ray diffraction analysis. Structure I (a = 8.553 Å, b = 11.967 Å, c = 17.871 Å) and structure II (a = 8.540 Å, b = 11.956 Å, c = 17.867 Å) are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.044 (I) and 0.055 (II) for all 2385 (I) and 2379 (II) measured independent reflections. Complex molecules [K(NO₃)(18-crown-6)] in structure I and [K_0.91Ag_0.09(NO₃)(18-crown-6)] in compound II are of the host-guest type and rather similar in structure. Their 18-crown-6 and NO ₃ ^? ligands are disordered over two orientations. The K⁺ cation in complex I and the mixed cation (K_0.91Ag_0.09)⁺ in complex II reside in the cavity of the disordered 18-crown-6 ligand and is coordinated by its six O atoms and by two disordered O atoms of the NO ₃ ^? . ligand. The coordination polyhedron (CN = 8) of the K⁺ cation in complex I and that of (K_0.91Ag_0.09)⁺ cation in complex II is a distorted hexagonal pyramid with a base of six O atoms of the 18-crown-6 ligand and a split vertex at two O atoms of the NO ₃ ^? ligand.     

Syntheses and crystal structures of hydrated complexes of strontium and barium bromides with 18-crown-6

Two complexes, namely, triaqua(18-crown-6)strontium dibromide monohydrate (I) and diaquabromo(18-crown-6)barium bromide (II), are synthesized. Their crystal structures are determined by X-ray diffraction analyses. For complex I, space group C2/c, a = 17.547 Å, b = 10.246 Å, c = 14.786 Å, β = 123.08°, Z = 4. For complex II, space group Pnma, a = 17.753 Å, b = 17.465 Å, c = 6.629 Å, Z = 4. The structures are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.056 (I) and 0.042 (II) for 2696 (I) and 2440 (II) independent reflections (CAD-4 automated diffractometer, λMoK _α radiation). Both complex cations—randomly disordered [Sr(18C6)(H₂O)₃]²⁺ in complex I and [BaBr(18C6)(H₂O)₂]⁺ in complex II—are of the host-guest type. The Sr²⁺ (Ba²⁺) cation resides in the cavity of the 18-crown-6 ligand and coordinated by all six O atoms. In the structures complexes I and II, the coordination polyhedra of the Sr²⁺ and Ba²⁺ cations (coordination number 9) can be described as distorted hexagonal bipyramids with one apex at the O atom of the water molecule in complex I or at the Br^? ligand in complex II and the other split apex at the O atoms of two water molecules.     

(18-Crown-6)sodium tribromide and (18-crown-6)potassium triiodide (with an admixture of bromodiiodide): Synthesis and crystal structure

Two crystalline host-guest complexes are synthesized and studied using X-ray diffraction analysis: (18-crown-6)sodium tribromide [Na(18-crown-6)]⁺ · Br ₃ ^? (I) and (18-crown-6)potassium tribromide (with an admixture of bromodiiodide) [K(18-crown-6)]⁺ · (Br_0.25I_2.75)^? (II). The structures of compound I (space group P2₁/_{n, a} = 8.957 Å, b = 8.288 Å, c = 14.054 Å, β = 104.80°, Z = 2) and compound II (space group Cc, a = 8.417 Å, b = 15.147 Å, c = 17.445 Å, β = 99.01°, Z = 4) are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.098 (I) and 0.036 (II) for all 2311 (I) and 2678 (II) independent measured reflections on a CAD-4 automated diffractometer (λMoK _α). Similar crystalline complexes I and II exist as infinite chains of alternating complex cations and trihalide anions linked to each other through weak Na-Br or K-I coordination bonds. In [Na(18-crown-6)]⁺ and [K(18-crown-6)]⁺ complex cations, the Na⁺ or K⁺ cation (coordination number is eight) is located in the center of the cavity of the 18-crown-6 ligand and coordinated by the six O atoms and two terminal Br or I atoms of two trihalide anions lying on opposite sides of the rms plane of the crown ligand.     

Synthesis and crystal structure of bis(μ-periodato-<Emphasis Type="Italic">O,O′,O″</Emphasis>)bis(18-crown-6)dirubidium

A new binuclear complex, bis(μ-periodato-O,O′,O″)bis(18-crown-6)dirubidium [Rb₂(IO₄)₂(18-crown-6)₂] (I), is synthesized. Its crystal structure is studied by single-crystal X-ray diffraction analysis (space group P2₁/n, a = 11.942 Å, b = 8.394 Å, c = 19.664 Å, β = 101.08°, Z = 4, direct method, anisotropic full-matrix least-squares approximation, R = 0.030 for 2823 independent reflections, CAD-4 automated diffractometer, λMoK _α radiation). Complex I is binuclear and centrosymmetric, consisting of two cationic monomers [Rb(18-crown-6)]⁺ of the host-guest type linked through two tridentate IO ₄ ^? bridging ligands. The coordination polyhedron of the Rb⁺ cation (coordination number 9) can be described as a distorted hexagonal pyramid with a base of six O atoms of one 18-crown-6 ligand and one threefold vertex at three O atoms of the two IO ₄ ^? bridging ligands. The 18-crown-6 ligand has a usual crown conformation.     

Ammonium (18-Crown-6)(Triphenylphosphine Oxide) Perchlorate: Synthesis and Crystal Structure

A new compound, ammonium (18-crown-6)(triphenylphosphine oxide) perchlorate (I), is synthesized, and its crystal structure is studied using X-ray diffraction analysis (space group R3m, a = 14.432 Å, c = 14.034 Å, Z = 3, direct method, full-matrix least-squares method in the anisotropic approximation, R = 0.064 for 1945 independent reflections, CAD4 automated diffractometer, λMoKα radiation). In the structure, the NH ₄ ⁺ cation resides in the 18-crown-6 macrocycle cavity and is hydrogen-bonded with three symmetrically equivalent O atoms of the 18-crown-6 molecule and with the phosphoryl O atom of the Ph₃PO molecule. The P=O H-N and Cl atoms occupy the partial position 3m. The oxygen atoms of the ClO ₄ ^? anion are disordered over the 3m position.     

Synthesis and crystal structure of 18-crown-6 <Emphasis Type="Italic">E</Emphasis>-2-phenylethenylphosphonic acid diaqua(18-crown-6)sodium <Emphasis Type="Italic">E</Emphasis>-2-phenylethenylphosphonate

New complex compound, diaqua(18-crown-6)sodium E-2-phenylethenylphosphonate 18-crown-6 E-2-phenylethenylphosphonic acid, [Na(18-crown-6)(H₂O)₂]⁺·HO ₃ ^? PCH=CHPh·18-crown-6·H₂O₃PCH=CHPh, was obtained and its crystal and molecular structures were studied by the X-ray structural analysis. In this structure the complex cation [Na(18-crown-6)(H₂O)₂]⁺ is of guest-host type. The coordination polyhedron of its Na⁺ cation is a slightly screwed hexagonal bipyramid with the base consisting of all 6 O atoms of 18-crown-6 ligand and with two opposite apexes at two O atoms of two ligand water molecules. In the studied crystal structure the alternating complex cations and 18-crown-6 molecules as well as the molecules of acid and its anion HO ₃ ^? PCH=CHPh form by means of hydrogen bonds the infinite chains of two different types.     

Tetrakis(isothiocyanato)manganese(II) bis[aqua(18-crown-6)potassium] (18-crown-6)(thiocyanato)potassium

A new complex compound, i.e., tetrakis(isothiocyanato)manganese(II) bis[aqua(18-crown-6)potassium] (18-crown-6)(thiocyanato)potassium, was synthesized and its crystal structure was studied by X-ray diffraction (space group P2₁/m, a = 13.377, b = 14.690, c = 17.499 Å, β = 108.96°, Z = 2) and refined by the least-squares method in anisotropic approximation to R = 0.060 for 4715 independent reflections (CAD-4 automated diffractometer, λMoK _α). In the crystal, infinite chains are formed through the coordination bonds between its components. The monomer fragment of a chain [Mn(NCS)₅K₃(18-crown-6)₃(H₂O)₂] lies in plane m; three of the five SCN^? ligands and one of the two water molecules behave as bridges. The [Mn(NCS)₄]^2? anion has the tetrahedral structure. The coordination polyhedron of each of the three K⁺ cations is a distorted hexagonal bipyramid with six O atom of the corresponding crown ligand in a base. Three 18-crown-6 ligands have standard crown conformation.     

Synthesis,crystal structure,and vibrational spectrum of lithium <Emphasis Type="Italic">N</Emphasis>-(4′-benzo-15-crown-5)-5-bromo-2-hydroxyphenylaldiminatozinc perchlorate dihydrate

The synthesis, the IR absorption spectrum, and X-ray diffraction analysis of the complex [ZnLi(L¹)₂(H₂O)](ClO₄) · H₂O (I) (HL¹ = N-(4′-benzo-15-crown-5)-5-bromo-2-hydroxyphenylaldimine) are described. The crystals of I are monoclinic, a = 19.840(4) Å, b = 13.947(3) Å, c = 19.956(4) Å, β = 117.06(3)°, V = 4917.4(17) ų, Z = 4, space group P2₁/n, R = 0.0609 for 1409 reflections with I > 2σ(I). In the complex cation [ZnLi(L¹)₂(H₂O)]⁺, the Zn atom is bound to a distorted tetrahedral array of two N atoms (av. Zn-N, 2.027(10) Å) and two O atoms (av. Zn-O, 1.8968(8) Å) of two deprotonated L¹ ligands. The Li atom linked to the five ether oxygen atoms (av. Li-O_ether, 2.254(3) Å) sits atop the benzo-15-crown-5 (B15C5) macrocyclic plane of one coordinated L¹ ligand. The Li coordination is completed by water oxygen (Li-O(w1), 1.83(5) Å). The B15C5 cavity of the second coordinated ligand L¹ is vacant.     

Reactions of triphenylbenzylphosphonium and tetraphenylstibonium chlorides with potassium tetrachloroplatinates in dimethylsulfoxide

Platinum complexes [Ph₃PhCH₂P]⁺[(Me₂S=O)PtCl₃]^? I and cis-Cl₂(Ph₃Sb)(Me₂S=O)Pt II were synthesized by reaction of triphenylbenzylphosphonium and tetraphenylstibonium chlorides with potassium tetrachloroplatinate in DMSO. Crystal I is formed by triphenylbenzylphosphonium tetrahedral cations [P-C_Ph 1.791(4)-1.795(4) Å, P-C_Alk 1.811(4) Å; CPC 107.57(18)°-111.46(17)°] and by square anions [(Me₂S=O)PtCl₃]^? [Pt-Cl 2.3236(11), 2.2981(12), 2.2977(11) Å; Pt-S 2.1950(10) Å; trans-angles SPtCl 177.51(4)°, ClPtCl 178.74(4)°]. In a square-planar complex II [trans-angles SPtCl 178.01(6)°, ClPtSb 177.96(4)°] with central platinum atom the chlorine atoms [Pt-Cl 2.308(1), 2.350(1) Å], triphenylstibine [Pt-Sb 2.5118(4) Å] and dimethyl sulfoxide [Pt-S 2.195(1) Å] molecules are coordinated. Compound II is a first example of mixed ligand complex of platinum(II), where in the coordination sphere of central atom the tertiary stibine is present along with DMSO ligand.     

Synthesis and crystal structures of binuclear complexes of cobalt(II) and cadmium(II) diisobutyldithiophosphinates with hexamethylenetetramine

Heteroligand complexes [Co₂(HMTA)(iso-Bu₂PS₂)₄] (I) (μ_eff = 4.67 μB) and [Cd₂(HMTA)(iso-Bu₂PS₂)₄] (II) have been synthesized. Single crystals of compounds I and II have been obtained. The crystals are monoclinic: a = 32.622(2) Å, b = 9.4891(6) Å, c = 21.7570(13) Å, β = 125.774(1)^o, V = 5464.3(6) Å,³, Z = 4, ρ_calcd = 1.331 g/cm³ for I; a = 34.6092(7) Å, b = 9.5595(2) Å, c = 22.3473(5) Å, β = 127.144(1)^o, V = 5893.5(2) Å, Z = 4, ρ_calcd = 1.355 g/cm³ for II; space group for both complexes C2/c. Structures I and II are based on discrete binuclear molecules. The coordination polyhedra of the Co and Cd atoms are distorted tetragonal pyramids NS₄, with the bases formed by four S atoms of two bidentate chelating ligand iso-Bu₂PS ₂ ^? and the axial vertices occupied by N atoms of bidentate bridging HMTA ligand. The character of interaction of the molecules in structures I and II is considered.     

<Emphasis Type="Italic">catena</Emphasis>-(μ<Subscript>3</Subscript>-Bromo)di(μ<Subscript>2</Subscript>-bromo)bromo(18-crown-6)dilead(II): Synthesis and crystal structure

A new polymeric complex, catena-(μ₃-bromo)di(μ₂-bromo)bromo(18-crown-6)dilead(II), [Pb₂Br(μ₂-Br)₂(μ₃-Br)(18-crown-6)] _n (I), is synthesized, and its crystal structure is studied using X-ray diffraction analysis (space group P \(\bar 1\), a = 7.970, b = 16.048, c = 19.153 Å, α = 72.75°, β = 88.57°, γ = 87.92°, Z = 4, direct method, full-matrix least-squares method in the anisotropic approximation, R = 0.076 for 6093 independent reflections, CAD4 automated diffractometer, λMoK_α radiation). The crystal structure of complex I contains infinite chains of the PbBr₆ octahedra along the x axis with the bridging Br^? anions as common edges. The [PbBr(18-crown-6)]⁺ host-guest complex fragments are attached through weak Pb-Br bonds to these chains on the side. In two independent terminal fragments, the coordination polyhedra of the Pb²⁺ cations are distorted hexagonal bipyramids with bases of six O atoms of the crown ligand and two Br^? anions in the axial vertices. Two Pb²⁺ cations from the [PbBr₃] _n ^? infinite polymer chain have a distorted octahedral coordination.     

Rosenmund-Braun Reaction Products 4′,5′-Dicyanobenzo-15-crown-5 and 4′,5′-Dicyanobenzo-15-crown-5,4′-cyano-5′-cyano(bromo)benzo-15-crown-5 Hydrates: Spectroscopic Properties and Crystal Structure

The products of 4′,5′-dibromobenzo-15-crown-5 (I) cyanation by the Rosenmund-Braun reaction are studied by the ¹H NMR and IR spectroscopy methods. X-ray diffraction analysis of two isolated products, i.e., di(4′,5′-dicyanobenzo-15-crown-5) 1.6 hydrate {(CN)₂B15C5}₂ · 1.6H₂O (IIa) and 4′,5′-dicyanobenzo-15-crown-5,4′-cyano-5′-cyano(bromo)benzo-15-crown-5 dihydrate (CN)_3.85Br_0.15(B15C5)₂ · 2H₂O (III) is performed. Crystals IIa are monoclinic, a = 15.882(2) Å, b = 11.412(2) Å, c = 18.484(3) Å, β = 100.717(3)°, V = 3291.7(9) ų, Z = 4, space group P2₁/c, R = 0.0746 for 4775 reflections with I > 2σ(I). Crystals III are monoclinic, a = 15.956(3) Å, b = 11.425(2) Å, c = 18.865(4) Å, β = 99.32(3)°, V = 3394(1) ų, Z = 4, space group _P2₁/_{c, R} = 0.0692 for 2070 reflections with I > 2σ(I). Compounds IIa and III have similar structures with two crystallographically independent molecules in each (A and B in IIa; C and D in III). Four of the five O atoms of a macrocycle in molecules A and C form hydrogen bonds with the water molecules. The latter molecules lie above and below the cycle plane at a distance of ～2 Å from this plane. The A and C molecules have identical conformations (TTG TTG TTG TTG TTC) that differ from those of molecules B (TTG TGG STT SSG TTC) and D (TTC TSG STT SSG TTC).     

Crystal Structure of Mononuclear Non-Heme Nikel(II) Octahedral Complex: [Ni(bqenH<Subscript>2</Subscript>)(bpy)](ClO<Subscript>4</Subscript>)<Subscript>2</Subscript>·0.125H<Subscript>2</Subscript>O

The crystal structure of a mononuclear Ni(II) complex [Ni(bqenH₂)(bpy)](ClO₄)₂·0.125H₂O 1 (where bqenH₂ is N,N′-bis(8-quinolyl)ethane-1,2-diamine, bpy = 2,2′-bipyridine) is reported here. The crystallographic data for 1 are as follows: monoclinic crystal system, P2_1/n space group, a = 17.3255(11), b = 10.6110(7), c = 34.328(2) Å, α = 90°, β = 93.9480(13)°, γ = 90°, V = 6295.8(7) ų, Z = 4, d_x = 1.541 mg/m³. The nickel(II) ion coordinates four N atoms of the tetradentate ligand bqenH₂ and two N atoms of the auxiliary bidentate 2,2′-bipyridine ligand, resulting in a slightly distorted NiN6 octahedron with two perchlorates serving as charge balancing counter anions. The overall structure of 1 is stabilized by the presence of water of crystallization in the crystal lattice. The crystal structure shows two symmetrically identical octahedral NiN6 units in its asymmetric unit. The extensive hydrogen bonding network resulting in a supramolecular architecture is observed due to the N–H?O, O–H?O, O–H?Cl, and N–H?Cl interactions.     

Aquabis(dibenzo-18-crown-6)(tetrabromocuprato(II))dipotassium: Synthesis and crystal structure

The novel complex [K(Db18C6)(H₂O)]⁺[K(Db1)] ⁺(CuBr₄)^2? (I) was obtained. Its crystal structure (space group P2₁/c, a = 17.970 Å, b = 29.838 Å, c = 9.074 Å, β = 103.11°, Z = 4) was studied by X-ray diffraction analysis, solved by the direct method, and refined by the least-squares method in the anisotropic approximation to R = 0.098 from 6220 independent reflections (CAD-4 automated diffractometer, λMo Kα). In both “guest-host” complex ions, the K⁺ cation is in the cavity of the crown ligand Db18C6 and is coordinated by all its O atoms, as well as by a Br atom of the complex anion [CuBr₄]^2? or the water O atom. The coordination of either K⁺ cation is extended to a hexagonal bipyramid by a weak K⁺ → π\((C\dddot ---C)\) bond to two C atoms of the benzene ring of the adjacent ligand Db18C6. In the crystal, the complex anions and cations are united into infinite double chains through the above contacts and the interion hydrogen bonds O-H…Br.     

Synthesis and structure of <Emphasis Type="Italic">cis</Emphasis>-dichloro(triphenylstibine)(dimethylsulfoxide)platinum(II)

The platinum molecular complex cis-Cl₂(Ph₃Sb)(Me₂S=O)Pt (I) was synthesized by the reaction of tetraphenylstibonium chloride with potassium tetrachloroplatinate in dimethyl sulfoxide. The crystal structure of square-planar complex I was determined by X-ray crystallography. The complex contains, in addition to chlorine atoms, triphenylstibine and DMSO molecules coordinated to the central atom. The bond lengths Pt-Cl, Pt-S, and Pt-Sb are 2.308(1), 2.350(1), 2.195(1), and 2.5118(4) Å, respectively. The compound is the first example of mixed-ligand platinum(II) complex in which the coordination sphere of the central atom contains, along with dimethyl sulfoxide ligand, a tertiary stibine ligand.     

Synthesis and structural determination of a novel complex [Yb<Superscript>III</Superscript>(HEgta)] · 4H<Subscript>2</Subscript>O in comparison with [Yb<Superscript>III</Superscript>(HEgta)] · 2H<Subscript>2</Subscript>O

One novel ytterbium complex [Yb^III(HEgta)] · 4H₂O (I), where H₄Egta = ethylene glycol-bis(2-aminoethylether)-N,N,N′,N′-tetraacetic acid, has successfully been synthesized by the reaction of Yb₂O₃ with H₄Egta in an aqueous solution after refluxing for 18 h. The crystal and molecular structures were determined by the infrared spectrum and X-ray crystallography. The crystal structural analysis reveals that central Yb(III) in I is eight-coordinated in a geometry of pseudo-square antiprismatic polyhedron by two amine N atoms, two ethylene glycol O atoms, and four carboxyl O atoms from one HEgta ligand and crystallizes in the orthorhombic crystal system with P2₁2₁2₁ space group. The crystal data are as follows: a = 9.4927(8), b = 12.2627(13), c = 18.3657(17) Å, V=2137.9(4) ų, Z = 4, ρ_calcd = 1.934 mg/m³, μ = 4.448 mm^?1, F(000) = 1236, R = 0.0291, and wR = 0.0714 for 8850 observed reflections with I ≥ 2σ(I). In addition, there is a protonated coordinated carboxyl O atom (O(5)) in the [Yb^III(HEgta)] moiety.     

(18-Crown-6)(hydrogennitrato)potassium: Synthesis and crystal structure

A new complex, [K(18-crown-6)(NO₃)(HNO₃)] (I), is synthesized, and its crystal structure is studied using X-ray diffraction analysis: space group P \(\bar 1\), a = 8.253 Å, b = 9.277 Å, c = 13.903 Å, α = 95.89°, β = 104.30°, γ = 91.89°, Z = 2. The triclinic structure of compound I was solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.059 for all 3573 independent reflections (CAD4 automated diffractometer, γMoK _α radiation). The structure of compound I contains two independent halves of two centrosymmetric complex molecules with different coordination modes of the K⁺ cations. Two NO ₃ ^? and HNO₃ ligands are randomly disordered relative to the symmetry center and are presented by two average independent H_0.5N ₃ ^1/2? , ligands, which are also orientationally disordered.     

Crystal structure of adducts of copper(II) acetylacetonate and hexafluoroacetylacetonate with 4-aminopyridine

Single crystal X-ray diffraction is used to investigate two synthesized β-diketonate complexes of copper(II) with aminopyridine: Cu(4-NH₂Py)(aa)₂ (I) and Cu(4-NH₂Py)(hfa)₂ (II). The crystals of I and II have a monoclinic system; the unit cell parameters of I are: P2₁/n space group, a = 8.2921(3) Å, b = 14.7243(5) Å, c = 13.4970(4) Å, β = 102.426(1)°, V = 1609.32(9) ų, Z = 4; for II: C2/c space group, a = 23.5704(5) Å, b = 11.4977(2) Å, c = 16.0285(3) Å, β = 109.265(1)°, V = 4100.6(1) ų, Z = 8. The structures of I and II are molecular; they are composed of isolated molecules. The coordination polyhedron of the copper atom is formed by the O atoms of two acetylacetonate ligands (Cu-O 1.940(2)–2.171(2) I and the O atoms of two hexafluoroacetylacetonate ligands (Cu-O 1.940(2)–2.215(3) Å) in II. The molecules of 4-NH₂Py are bonded to the copper atom via the nitrogen atom of the aromatic ring (Cu-N 2.008(2) Å in I and Cu-N 1.978(3) Å in II). Noncoordinated amino groups join the molecules of the complexes together by means of N-H…O hydrogen bonds.     

Synthesis,crystal structures,and antimicrobial activity of copper(II) and zinc(II) complexes derived from 2-bromo-4-chloro-6-[(2-morpholin-4-ylethylimino)methyl]phenol

An end-to-end azido-bridged dinuclear copper(II) complex [Cu₂L₂(μ_1,3-N₃)](NO₃) (I) and a mononuclear zinc(II) complex [ZnCl₂(HL)] ? CH₃OH (II), where L is 2-brom-4-chloro-6-[(2-morpholin- 4-ylethylimino)methyl]phenolate, have been prepared and characterized by elemental analyses, IR, and single crystal X-ray crystallographic determination (CIF files CCDC nos. 1415217 (I), 1415218 for (II)). The crystal of I is monoclinic: space group C2/c, a = 28.684(2), b = 7.1787(5), c = 18.292(1) Å, β = 117.887(3)°, V = 3329.1(4) ų, Z = 4. The crystal of II is monoclinic: space group P2₁/c, a = 10.8207(9), b = 12.3398(7), c = 14.9477(7) Å, β = 93.473(3)°, V = 1992.2(2) ų, Z = 4. The Schiff base ligand in I coordinates to the Cu atom through the phenolate O, imine N, and morpholine N atoms, while the Schiff base ligand in II coordinates to the Zn atom through the phenolate O and imine N atoms, with the morpholine N atom protonated. The effect of these complexes on the antimicrobial activity against Staphylococcus aureus, Escherichia coli, and Candida albicans was studied.