Diaquabis(phen)Ni(II) Complex with Vitamin B13 Counter-ions

Abstract The synthesis and crystal structure of a new Ni(II) complex of stoichiometry [Ni(phen)₂(H₂O)₂](H₂Or)₂ · 2H₂O, where phen is phenanthroline and H₂Or is oratate monoanion, are reported. The complex [Ni(phen)₂(H₂O)₂](H₂Or)₂ · 2H₂O crystallizes in the monoclinic system with space group C2/c and cell parameters a = 16.1661(8) ?, b = 12.5669(7) ? and c = 16.4752(7) ?. The coordination around Ni(II) is a distorted octahedron with two phen ligands perpendicular to each other and two aqua ligands in cis- position. Orotate ions locate themselves out of the coordination sphere and bridge the [Ni(phen)₂(H₂O)₂]²⁺ moieties through hydogen bonding with aqua ligands. The FT-IR spectrum of the complex and thermal decomposition behaviour are also briefly discussed. Graphical Abstract Diaquabis(phen)Ni(II) Complex with Vitamin B13 Counter-ions Dursun Ali K?se, Birgül Zümreoglu-Karan, Başak Koşar, Orhan Büyükgüng?r A new complex where Vitamin B13 monoanions act as counter ions and bridge the [Ni(phen)₂(H₂O)₂]²⁺ units by hydrogen bonds is described CCDC deposition number is 606339.     

Crystal structures of polymeric complexes of zinc(II) bromide and perchlorate with 1,4-diazoniabicyclo [2.2.2]octane-1,4-diacetate

Two zinc(II) complexes containing a flexible double betaine, namely [{Zn(L)Br₂}_n]·nH₂O (1) and [{Zn(L)₂(H₂O)₂}_n](ClO₄)_2n·4nH₂O (2) [L=1,4-diazoniabicyclo [2.2.2]octane-1,4-diacetate,⁻O₂CCH₂N⁺(CH₂CH₂)₃N⁺CH₂CO₂ ⁻], have been prepared and shown to have polymeric structures by single-crystal X-ray analysis. Complex (1) exhibits an infinite zigzag chain in which each zinc(II) atom is coordinated by two unidentate carboxylate oxygen atoms and two bromide ligands in a distorted tetrahedral geometry. Complex (2) consists of an assembly of catonic Zn(L)₂(H₂O)₂ ²⁺ moieties and discrete perchlorate anions as well as lattice water molecules. In (2) each zinc(II) atom is coordinated by two pairs of unidentate carboxylate oxygen atoms and two aqua ligands in a distorted octahedral geometry and cross-linked by skeletons of double betaine ligands to form a corrugated layer structure corresponding to the plane (100).     

Metal-betaine interactions. II. Crystal structures of catena-dichloro(betaine)cadmium(II) and dimeric diaquabis(betaine)tetrachlorodicadmium(II)

Two cadmium(II) complexes of betaine (BET) have been prepared and characterized by X-ray crystallography. [Cd(BET) (–Cl)₂] (1), is a one-dimensional polymer in which each cadmium atom is coordinated by two pairs of bridging chlorine atoms [Cd-Cl=2.631(2), 2.614(2) Å] and two oxygen atoms from different bridging carboxylate groups [Cd-O=2.291(6), 2.329(6) Å] in the form of a compressed octahedron. [Cd(BET)(H₂O)Cl(–Cl)]₂ (2) is a dimer with each cadmium atom in a distorted octahedral coordination environment, being surrounded by a chelating bidentate carboxylate group [2.480(2), 2.332(3) Å], one aqua ligand [2.364(3) Å], two bridging chlorine atoms [2.659(1), 2.557(1) Å], and one terminal chlorine atom [2.480(1) Å].     

Metal-betaine interactions. I. Crystal structure of polymeric trans-diaquabis(pyridine betaine)manganese(II) dichloride

A new polymeric betaine complex of manganese(II), of stoichiometry [Mn(C₅H₅NCH₂COO)₂ (H₂O)₂]C1₂, has been prepared and characterized by infrared spectroscopy and X-ray crystallography. The complex exhibits strong carboxylate absorptions at 1624, 1396, 1384, and 715 cm^–1. The crystal structure has been refined toR _F =0.057 for 2342 observed (F ₀>6F ₀) MoK data. The complex consists of a packing ofsyn-anti carboxylate-bridged, one-dimensional polymeric chains running parallel to thea axis. Each Mn(II) atom is located at an inversion center, with aqua ligands occupying the trans positions in a slightly distorted octahedron. The chloride ions and aqua ligands are alternately linked by O-HCl hydrogen bonds into a (Cl^–·H₂O) zigzag chain also running parallel to thea axis.     

Synthesis and crystal structures of quadruply carboxylate-bridged dimeric lanthanide(III) complexes of betaine

Three dimeric lanthanide(III) complexes, [Eu₂(bet)₈(H₂O)₄](CIO₄)₆ (1), [Tb₂(bet)₈(H₂O)₄](ClO₄)₆ (2), and [Eu₂(bet)₄(H₂O)₈] Cl₆·6H₂O (3) (bet = Me₃N⁺CH₂COO^–, trimethyl-aminoacetate), have been prepared and structurally characterized by X-ray crystallography. Complex 1 crystallizes in the monoclinic space group P2₁/c, with a = 11.7807(8), b = 27.757(5), c = 11.7980(8) Å, = 99.500(4)°, V = 3805.1(8) ų, and Z = 2. Complex 2 is isomorphous to complex 1, crystallizing in the monoclinic space group P2₁/c, with a = 11.7769(14), b = 27.725(3), c = 11.795(5) Å, = 99.668(14)°, V = 3797(2) ų, and Z = 2. Complex 3 crystallizes in the orthorhombic space group Pbca, with a = 12.5664(8), b = 17.8645(9), c = 22.2573(8) Å, V = 4996.6(4) ų and Z = 4. Both complexes 1 and 2 comprise quadruply carboxylate-O,O-bridged [M₂(bet)₄]⁶⁺ dimeric cores (M = Eu, Tb), and each metal ion is further coordinated by two terminal aqua ligands and two monodentate bet carboxylates to form a distorted square-antiprismatic coordination geometry. Complex 3 also has a [Eu₂(bet)₄]⁶⁺ core, in which two bet ligands act in the ¹:¹:₂ bridging fashion, and the other two bet ligands in the less common ²:¹:₂ bridging fashion, namely bridging-chelate mode. Each europium(III) ion in complex 3 is further coordinated by four water molecules to complete a monocapped square antiprism.     

Self-Assembly of Two Isomorphous Thiocyanate Complexes of Co(II) and Ni(II) with 3-Hydroxypicolinamide

Abstract  

The synthesis, thermal and spectral characterization, and crystal structure of isomorphous thiocyanate cobalt(II) and nickel(II) complexes with 3-hydroxypicolinamide (3-OHpia), [M(C₆H₆N₂O₂)₂(NCS)₂]·2H₂O, are reported. The metal(II) ions are chelated by two cis-oriented 3-OHpia and two thiocyanate ligands in distorted octahedral geometry. The distortion within the coordination sphere is mainly imposed by formation of the chelate rings. The compounds crystallize in monoclinic space group P2/c with two symmetrically independent molecules and a = 14.4945(2) ?, b = 8.5906(1) ?, c = 16.3865(3) ?, β = 105.987(2)°, Z = 4 (1) and a = 14.4927(5) ?, b = 8.5912(3) ?, c = 16.2712(6) ?, β = 105.740(4)°, Z = 4 (2). Commonly observed supramolecular amide synthons are not robust enough to accommodate thiocyanate ions and H₂O molecules. But instead, neutral complexes are linked through hydrogen bonds leading to two different hydrogen bonding ribbon motifs involving amide moieties and H₂O molecules [C(8)R ₂²(12) along c axis] and amide moieties and thiocyanate ions [C(8)R ₂²(16) along b axis] for symmetrically related molecules labelled as 1 [Co1 (1) and Ni1 (2)] and 2 [Co2 (1) and Ni2 (2)], respectively.     

Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane

Abstract The title complex [Co₂(bte)₃(NCS)₄(H₂O)₂] _n (bte = 1,2-bis(triazol-1-yl)ethane) has been prepared. Single-crystal X-ray analysis reveals that the complex crystallizes in space group P ī with a = 7.7962(2), b = 8.3407(4), c = 14.7735(5) ?, α = 86.835(2), β = 76.2031(9), γ = 80.583(3)°. The crystal consists of two discrete complexes, [Co(bte)(NCS)₂(H₂O)₂] and [Co(bte)₂(NCS)₂]. The structure of [Co(bte)(NCS)₂(H₂O)₂] consists of neutral chain containing Co(II) bridged by bte molecules. The six-co-ordination of Co²⁺ is achieved by means of two trans NCS⁻ ions and water molecules. The structure of [Co(bte)₂(NCS)₂] demonstrates a one-dimensional neutral chain through bte-bridge, in which the Co(II) atom is in a distorted octahedral environment formed by four nitrogen atoms of the triazoles and two nitrogen atoms from two trans thiocyanato liagnds. Index abstract Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane This paper reports the synthesis and crystal structure of complex [Co₂(bte)₃(NCS)₄(H₂O)₂]_n (bte = 1,2-bis(triazol-1-yl)ethane), which consists two different neutral chains containing Co(II) bridged by bte molecules.      

Crystal structures of polymeric complexes of zinc(II) bromide and perchlorate with 1,4-diazoniabicyclo [2.2.2]octane-1,4-diacetate

Two zinc(II) complexes containing a flexible double betaine, namely [{Zn(L)Br₂}_n]·nH₂O (1) and [{Zn(L)₂(H₂O)₂}_n](ClO₄)_2n·4nH₂O (2) [L=1,4-diazoniabicyclo [2.2.2]octane-1,4-diacetate,^?O₂CCH₂N⁺(CH₂CH₂)₃N⁺CH₂CO₂ ^?], have been prepared and shown to have polymeric structures by single-crystal X-ray analysis. Complex (1) exhibits an infinite zigzag chain in which each zinc(II) atom is coordinated by two unidentate carboxylate oxygen atoms and two bromide ligands in a distorted tetrahedral geometry. Complex (2) consists of an assembly of catonic Zn(L)₂(H₂O)₂ ²⁺ moieties and discrete perchlorate anions as well as lattice water molecules. In (2) each zinc(II) atom is coordinated by two pairs of unidentate carboxylate oxygen atoms and two aqua ligands in a distorted octahedral geometry and cross-linked by skeletons of double betaine ligands to form a corrugated layer structure corresponding to the plane (100).     

Nickel(II) and Cobalt(II) Complexes with Symmetrical Four-Dentate Ligands: Crystal Structures,Characterization, and Initial DNA Binding Mechanism Research

Abstract  

Four new nickel(II) and cobalt(II) complexes of Schiff base ligands: [Ni(L)Cl₂]·2H₂O (I), [Ni(L)(H₂O)₂] (NO₃)₂ (II), [Ni(L)(H₂O)₂] (ClO₄)₂ (III), and [Co(L) (H₂O)₂] (NO₃)₂ (IV) (L = 1,3-[bis(pyridine-2-imino)]propane) have been synthesized. The four complexes have been fully characterized by elemental analysis, IR, absorption spectra, emission spectra, and single-crystal X-ray diffraction analysis. The binding of the four complexes to calf thymus DNA (CT DNA) has been investigated by absorption spectra and emission spectra. The results of the two methods indicate that the action mode of complex I with DNA is intercalative mainly, and the action mode of complexes II, III, IV with DNA cannot be concluded, it should be sustained by other experimental measurements.     

A Unique Example of a Co-crystal of [Co(AMTTO)2(H2O)2](NO3)2 and [Co(AMTTO)2(CH3CN)2](NO3)2 (AMTTO = 4-amino-5-methyl-1,2,4-triazol-3(2H)-thione)

A co-crystal of cobalt(II) complexes, Co(AMTTO)₂(CH₃CN)₂]²⁺(NO₃)₂. [Co(AMTTO)₂(H₂O)₂]²⁺(NO₃)₂, compound (1) was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine (AMTTO) in acetonitrile as solvent. Isolated crystals were characterized by elemental analyses, IR spectroscopy as well as X-ray diffraction studies. Crystal data for 1 at 95 K revealed a monoclinic space group P2₁/n, a?=?11.7903(5), b?=?12.1279(5), c?=?14.1443(6) Å, β?=?99.244(4)°, Z?=?2, R₁?=?0.0339. Compound 1 consists of two co-crystallized Co(II) complexes [Co(AMTTO)₂(CH₃CN)₂]²⁺ and [Co(AMTTO)₂(H₂O)₂]²⁺ and four nitrate counter anions In both complexes, cobalt(II) ions are in an octahedral arrangement. Two S, N bidentate AMTTO ligands are coordinated to both Co(II) ions. The coordination sphere of Co1 is completed by two acetonitrile molecules, and these positions are occupied by water molecules for Co2.

Graphic Abstract

A co-crystal of cobalt(II) compound was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine in acetonitrile as solvent.

     

Nickel(II) complexes with N,N,O-donor Schiff bases. Self-assembly to two-dimensional network via hydrogen bonding

The syntheses, characterization and crystal structures of two mononuclear nickel(II) complexes are described. Reactions of Ni(O₂CCH₃)₂⋅4H₂O with the Schiff bases derived from 2-pyridinecarbaldehyde and ortho-aminophenol (Hpaap) and 2-pyridinecarbaldehyde and ortho-aminobenzoic acid (Hpaab) in methanolic media afford the complexes in good yields. The elemental analysis, magnetic moments, and spectral features of the complexes are consistent with the formulae [Ni(paap)₂]⋅CH₃COOH⋅H₂O and [Ni(paab)₂]⋅2H₂O. Crystal data for [Ni(paap)₂]⋅CH₃COOH⋅H₂O: monoclinic, P2₁/c, a = 9.675(2) Å, b = 17.109(5) Å, c = 14.403(4) Å, β = 92.903(11)^∘, V = 2381.1(11) ų, and Z = 4 and for [Ni(paab)₂]⋅2H₂O: triclinic, P 1, a = 9.834(3) Å, b = 11.319(3) Å, c = 13.130(4) Å, α = 84.68(3), β = 67.54(3), γ = 85.49(2)^∘, V = 1343.4(6) ų, and Z = 2. In each complex, two tridentate monoanionic meridionally spanning ligands form a distorted octahedral N₄O₂ coordination sphere around the metal ion. In [Ni(paap)₂]⋅CH₃COOH⋅H₂O, two metal coordinated phenolate-O atoms are hydrogen bonded to CH₃COOH and H₂O, respectively. Intramolecular C–H⋅ < eqid1 > ⋅O interactions involving the water molecule and the C–H from azomethine and aromatic fragments lead to a two-dimensional network of [Ni(paap)₂]⋅CH₃COOH⋅H₂O in the crystal lattice. An uncoordinated carboxylate O-atom in [Ni(paab)₂]⋅2H₂O is hydrogen bonded to both water molecules. One of the water molecules is again hydrogen bonded to the corresponding symmetry related water molecule forming a dimer. The azomethine groups and the metal coordinated carboxylate-O atoms in [Ni(paab)₂] are involved in intermolecular C–H⋅ < eqid2 > ⋅O interactions forming a chain-like arrangement of the molecules. The water dimers act as bridges between these chains and a two-dimensional network of [Ni(paab)₂]⋅2H₂O is formed.     

1D Supramolecules Self-Assembled by Nickel(II) Macrocycles with Carboxylate Ligands

Abstract  

Three new macrocyclic nickel(II) supramolecules, {[Ni(L1)(Hmal)₂]} _n (1), {[Ni(L1)(Hdipic)₂]·(H₂O)₂·DMF} _n (2) and {[Ni(L1)(Hisoph)₂]·2DMF} _n (3) (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo [14,4,0^1.18,0^7.12]docosane, mal = maleate, dipic = 2,6-pyridinedicarboxylate, isoph = isophthalate), have been synthesized and characterized by analytical, spectroscopic and X-ray diffraction methods. The complexes 1–3 show that the central nickel(II) ions are coordinated axially by two monodentate carboxylate ligands, respectively. The structures of 1–3 extend their mononuclear structures to form 1D supramolecules through hydrogen bonds. In 3, each 1D chain interacts together to form a 2D layer through hydrogen bonds between the Hisoph ligands.     

Influence of the spectator cation on the structure of anionic pyridine-2,6-dicarboxylato complexes of cobalt(II), nickel(II), and copper(II)

The structures of anionic pyridine-2,6-dicarboxylato (pdc^2–) complexes of cobalt, nickel, and copper have been studied. The stoichiometries and structures are very much dependent on whether KOH, Et₄NOH, or NaOH is used in the synthesis to deprotonate the H₂pdc ligand. Crystallographic results are: (1) K₂[Co(pdc)₂] · 7H₂O, orthorhombic, Pnna, Z = 4, a = 20.637(2)Å, b = 13.480(1)Å, c = 8.200(1)Å (2) K₂[Ni(pdc)₂] · 7H₂O, orthorhombic, Pnna, Z = 4, a = 20.648(1)Å, b = 13.375(1)Å, c = 8.2393(8)Å (3) [Co₂(H₂O)₅(pdc)₂] · 2H₂O, monoclinic, P2₁/c, Z = 4, a = 8.3880(6)Å, b = 27.384(2)Å, c = 9.6110(8)Å, = 98.271(6)° (4) [Ni(Hpdc)₂] · 3H₂O, monoclinic, P2₁/c, Z = 4, a = 13.679(1)Å, b = 10.0450(9)Å, c = 13.767(2)Å, = 115.184(7)° (5) Na₆[Co(H₂O)₆][Co(pdc)₂]₄ · 28H₂O, monoclinic, P2₁/n, Z = 2, a = 13.363(1)Å, b = 8.437(1)Å, c = 40.689(3)Å, = 91.288(5)° (6) Na[Ni(Hpdc)(pdc)] · 11.5H₂O, monoclinic, C2/m, Z = 4, a = 15.200(2)Å, b = 22.299(2)Å, c = 8.3596(7)Å, = 118.894(7)° (7) Na[Cu(Hpdc)(pdc)] · 3H₂O, monoclinic, P2₁/n, Z = 4, a = 9.516(4)Å, b = 14.917(6)Å, c = 12.247(5)Å, = 92.00(5)°. The potassium and sodium complexes have extensive K⁺—H₂O and Na⁺—H₂O networks. The fact the Et₄N⁺ ion does not appear in any of the complexes is likely due to the fact that it is incapable of forming the intricate cation—water and hydrogen-bonding networks observed in all of the other structures.     

Three‐Dimensional Structure Constructed via Hydrogen Bonds and π‐π Stacking Interaction. Crystal Structure of [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)

The structure of the title complexes [Cu(AFO)₂(H₂O)₂](ClO₄)₂.2(AFO).2H₂O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R₁ = 0.0595 (wR₂ = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)₂(H₂O)₂]²⁺, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction.     

Syntheses,Crystal Structures and Physical Properties of Cd(II) and Mn(II) Complexes with <Emphasis Type="Italic">Trans</Emphasis>-1,2-di(4-pyrindyl)ethylene and <Emphasis Type="Italic">P</Emphasis>-(carboxyl-methyloxy)-benzenecarboxylic Acid

Abstract  

Two complexes [Cd₂(dpe)₃(H₂O)₈]·(dpe)·(hssal)₂·(H₂O)₂ 1, [Mn(dpe)₂(Hpcmb)₂·(H₂O)₂] 2, (dpe = trans-1,2-di(4-pyrindyl)ethylene; H₂hssal = sulphosalicylic acid; H₂pcmb = p-(carboxyl-methyloxy)-benzenecarboxylic acid) has been prepared, and was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. Structure indicates in complex 1 that Cd(II) is a distorted octahedral coordination geometry. The hssal²⁻ anions are localized between 2-D sheets {[Cd(dpe)₂(H₂O)₄]²⁺(dpe)}n and {{[Cd(dpe)₂(H₂O)₄]²⁺}n as count anions and bridge to further connect these 2-D sheets through hydrogen bond O–H···O to form 3-D structure. The complex 2 is a single molecule structure. In 2, Each Mn(II) atom is six-coordinated with a distorted octahedral coordination geometry. The single molecule units are extended into three-dimensional structure via π–π, hydrogen bonding interactions. The thermogravimetric behavior and luminescent property of complex 1 were investigated.     

Crystal structure of PbUO2(CH3COO)4(H2O)3

Single crystals of PbUO₂(CH₃COO)₄(H₂O)₃ have been investigated by X-ray diffraction (R = 0.029 for 3175 reflections). The structure of this compound is formed by [Pb(CH₃COO)(H₂O)₃]⁺ chains, which are oriented along the [100] axis and limited by one-core complexes [UO2(CH₃COO)₃]⁻. The coordination numbers of the Pb(II) and U(VI) atoms are 8, and the coordination polyhedron of uranium is a hexagonal bipyramid whose vertices contain oxygen atoms of three bidentate cyclic acetate groups and the uranyl group. Taking into account the different crystallographic roles of acetate ions, the crystal-chemical formula of [PbUO₂(CH₃COO)₄(H₂O)₃] chains can be written as AA′B ²¹ B ¹¹(B ⁰¹)₂ M ₃¹, where A = Pb; A′ = UO₂²⁺; M ¹ = H₂O; and B ²¹, B ¹¹, and B ⁰¹ are CH₃COO⁻ groups.     

Metal-betaine interactions. XXI. Crystal structures of lithium 3-carboxy-1-pyridinioacetate monohydrate and sodium 3-carboxy-1-pyridinioacetate tetrahydrate

Two hydrated alkali-metal salts of the betaine derivative 3-carboxy-1-pyridinioacetate, C₅H₄ (COOH)N⁺CH₂COO^–, have been prepared and investigated by X-ray crystallography. Lithium 3-carboxy-1-pyridinioacetate monohydrate (R _F =0.041 for 1144 observed MoK data) has a one-dimensional polymeric structure based on a centrosymmetric Li₂(acetato--O,O)2 dimeric unit with the Li ion coordinated additionally by an intra-dimer acetate oxygen atom and an aqua ligand molecule in a slightly distorted tetrahedral LiO₄ geometry [Li-O=1.908 (4)-1.976(4)Å]. Sodium 3-carboxy-1-pyridinioacetate tetrahydrate (R _F =0.054 for 1812 observed data) features parallel columns of edge-sharing NaO₆ octahedra linked into a layer by bridging aqua ligands and betaine ligands whose acetato and carboxylato groups function in the unidentate and-O modes, respectively, with Na-O distances ranging from 2.351(2) to 2.608(2)Å. All the water molecules and uncoordinated carboxy oxygen atoms are involved in hydrogen bonding in both crystal structures.     

Synthesis and Crystal Structures of pH-Dependent Ni(II) Coordination Polymers with 3-Pyrid-3-ylbenzoic Acid

Abstract  

Two pyridinecarboxylato-bridged coordination polymers[Ni(pbc)₂(H₂O)₂]_n(1) and {[Ni(pbc) ₂ (H₂O)]·H₂O}_n (2)(Hpbc = 3-Pyrid-3-ylbenzoic acid) have been synthesized by the hydrothermal method and characterized by elemental analysis, IR spectrum and single crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P2₁/c with a = 9.519(5) ?, b = 9.417(5) ?, c = 11.701?, β = 98.086(5)°, V = 1038.5(9) ?³, Z = 2. Compound 2 crystallizes in monoclinic, space group P2₁/c with a = 10.490(2) ?, b = 12.920(3) ?, c = 16.074?, β = 95.97(3)°, V = 2166.7(8) ?³, Z = 4. X-ray diffraction analysis reveals that all pbc⁻ ligands act as diconnectors to link two Ni(II) centers and adopt one coordination mode: μ₂−N, O in compound 1 and the ligands adopt two coordination modes: μ ₂ −N, O and μ ₃ − N, O, O in compound 2.     

Crystal Structures of Two Aromatic Zinc(II) Carboxylates: [Zn(4-Chlorosalicylato)2(H2O)4]·2theophylline·(H2O)2 and Unique [Zn(5-Chlorosalicylato)2(isonicotinamide)2(H2O)]

Abstract  

The crystal structures of two zinc(II) 4-chloro- and 5-chlorosalicylate complexes, [Zn(4-ClC₆H₃-2-(OH)COO)₂(H₂O)₄]·2tph·(H₂O)₂ (I) and [Zn(5-ClC₆H₃-2-(OH)COO)₂(ina)₂(H₂O)] (II), where tph is theophylline and ina is isonicotinamide, have been determined using X-ray diffraction methods. Crystals of both (I) and (II) are triclinic, space group P-1, with Z = 1 in a cell with a = 7.2220(3), b = 8.59700(10), c = 16.0210(5) ?, α = 75.990(2), β = 83.959(2), γ = 68.455(2)°, V = 897.54(5) ?³ (I) and with Z = 2 in a cell with a = 11.4148(11), b = 11.5327(10), c = 12.0685(13) ?, α = 63.458(6), β = 87.547(8), γ = 89.387(7)°, V = 1419.9(2) ?³ (II). The coordination environment of the zinc(II) atom of compound (I) consists of two unidentate carboxylate oxygen atoms and four oxygen atoms of aqua ligands, forming a distorted octahedral configuration. Two theophylline molecules and the remaining water molecules are bound only by hydrogen bonds. The Zn atom of compound (II) is pentacoordinated with two unidentate carboxylate oxygen atoms, two pyridine nitrogen atoms of isonicotinamide ligands, and the oxygen atom of the aqua ligand, forming a distorted configuration between square pyramid and trigonal bipyramid. In both complexes intramolecular O–H···O hydrogen-bonding interactions are present. In the crystal structures, molecules are linked by intermolecular O–H···O and N–H···O hydrogen bonds. The structures are analyzed and compared to the similar Zn(II) complexes, with the chromophores ZnO₆ and ZnO₃N₂.     

Synthesis and crystal structure of (NH4)3[UO2(CH3COO)3]2[UO2(CH3COO)(NCS)2(H2O)]

Single crystals of the compound (NH₄)₃[UO₂(CH₃COO)₃]₂[UO₂(CH₃COO)(NCS)₂(H₂O)] (I) are synthesized, and their structure is investigated using X-ray diffraction. Compound I crystallizes in the monoclinic system with the unit cell parameters a = 18.3414(6) ?, b = 16.3858(7) ?, c = 12.4183(5) ?, β = 92.992(1)°, space group C2/c, Z = 4, V = 3727.1(3) ?³, and R = 0.0253. The uranium-containing structural units of crystals I are mononuclear complexes of two types with an island structure, i.e., the [UO₂(CH₃COO)₃]⁻ anionic complexes belonging to the crystal-chemical group (AB ₃⁰¹ = UO₂²⁺, B ⁰¹ = CH₃COO⁻) of the uranyl complexes and the [UO₂(CH₃COO)(NCS)₂(H₂O)]⁻ anionic complexes belonging to the crystal-chemical group AB ⁰¹M₃¹ (A = UO₂²⁺, B ⁰¹ = CH₃COO⁻, M ¹ = NCS⁻ or H₂O).