Crystal structure and triboluminescence of the [Tb(BTFA)2(NO3)(TPPO)2] complex

The crystal structure of the [Tb(BTFA)₂(NO₃)(TPPO)₂] complex (TPPO is triphenylphosphine oxide, BTFA is benzoyltrifluoracetone), which exhibits strong triboluminescence, has been established by X-ray crystallography. The crystals are triclinic: a = 11.668(3) Å, b = 11.700(3) Å, c = 12.512(3) Å, α = 65.161(4°), β = 79.120(4)°, γ = 61.860(4)°, space group P1, Z = 1. The central terbium(III) atom coordinates two oxygen atoms from two triphenylphosphine oxide molecules (Tb-O, 2.264(3) and 2.273(3) Å), two oxygen atoms from the nitrate group (Tb-O, 2.460(3) and 2.476(3) Å), and four oxygen atoms from two benzoyltrifluoroacetonate groups (Tb-O, 2.329(3), 2.399(3), 2.351(3), and 2.367(3) Å). The coordination polyhedron of the Tb(III) atom is a distorted dodecahedron. The photoluminescence and triboluminescence spectra of the [Tb(BTFA)₂(NO₃)(TPPO)₂] complex are identical and caused by the f-f luminescence of Tb³⁺.     

Crystal structure of [Pb<Subscript>3</Subscript>(OH)<Subscript>4</Subscript>Co(NO<Subscript>2</Subscript>)<Subscript>3</Subscript>](NO<Subscript>3</Subscript>)(NO<Subscript>2</Subscript>)·2H<Subscript>2</Subscript>O

The structure of [Pb₃(OH)₄Co(NO₂)₃](NO₃)(NO₂)·2H₂O is determined by single crystal X-ray diffraction. The crystallographic characteristics are as follows: a = 8.9414(4) Å, b = 14.5330(5) Å, c = 24.9383(9) Å, V = 3240.6(2) ų, space group Pbca, Z = 8. The Co(III) atoms have a slightly distorted octahedral coordination formed by three nitrogen atoms belonging to nitro groups (Co–N_av is 1.91 Å) and three oxygen atoms belonging to hydroxyl groups (Co–O_av is 1.93 Å). The hydroxyl groups act as μ₃-bridges between the metal atoms. The geometric characteristics are analyzed and the packing motif is determined.     

A new 3s–3d heterometallic polymer containing N‐methyliminodiacetic acid: synthesis,structure and characterization

A new complex {[Na₂(H₂O)₃(µ‐L)₂Cu]₄}_∞ (L = N‐methyliminodiacetic acid) has been synthesized and structurally characterized. The complex crystallizes in the monoclinic, space group C2/c, with the unit cell parameters a = 16.556(3) Å, b = 8.0622(13) Å, c = 12.671(2) Å, α = 90°, β = 95.849(2)°, γ = 90°. The central metal Cu (II) ion is coordinated with two nitrogen atoms and four oxygen atoms belonging to two ligands. Simultaneously, the sodium is six‐coordinated with oxygen atoms coming from the ligand and water molecule; the sodium atoms related are bridged by oxygen atoms, forming a sodium chain. The structure consists of CuL₂ moieties linked by sodium chain via the exo oxygen atoms of two ligands, forming a novel three‐dimensional structure. Moreover, elemental analysis, IR, UV‐vis, ESR spectroscopy and thermal stability were determined. Copyright © 2007 John Wiley & Sons, Ltd.     

Coordination compounds of cobalt(II) and cadmium(II) with 2-amino-4-methylpyrimidine: Synthesis, crystal structure, and luminescent properties

The coordination compounds [CoL₂Cl₂] (I) and [CdL₂(H₂O)₂(NO₃)₂] (II) have been synthesized by the reaction of CoCl₂ · 6H₂O and Cd(NO₃)₂ · 4H₂O with L = 2-amino-4-methylpyrimidine (Ampym, C₅H₇N₃), and their structures have been solved. The crystals of complex I are triclinic, space group $P\bar 1$ , a = 5.627(1) Å, b = 11.191(1) Å, c = 12.445(1) Å, α = 81.00(1)°, β = 77.21(1)°, γ = 76.18(1)°, V = 737.7(2) ų, ρ_calcd = 1.567 g/cm³, Z = 2. The crystals of complex II are monoclinic, space group P2₁/c, a = 10.390(1) Å, b = 11.982(1) Å, c = 7.624(1) Å, β = 102.61(1)°, V = 926.1(2) ų, ρ_calcd = 1.760 g/cm³, Z = 2. Discrete [CoL₂Cl₂] moieties are realized in the structure of complex I. The cobalt atom is tetrahedrally coordinated to the two nitrogen atoms of crystallographically nonequivalent ligands L and two chlorine atoms (Co(1)-N_avg, 2.051(4)Å; Co(1)-Cl(1), 2.241(1) Å; Co(1)-Cl(2), 2.263 Å; bond angles at the cobalt atom lie within a range of 102.1°–118.6°). The complexes are linked into supramolecular zigzag chains by N-H...N(Cl) hydrogen bonds. In the structure of complex II, the Cd²⁺ ion (at the inversion center) is coordinated in pairs to the nitrogen atoms of ligand L and the O(NO₃) and O(H₂O) oxygen atoms. The coordination of the Cd²⁺ ion is distorted octahedral (Cd(1)-N(1), 2.341Å; Cd(1)-O(1), 2.340(4) Å; Cd(1)-O(4), 2.327(3) Å; bond angles at the cadmium atom lie within a range of 79.1°–100.9°). N-H...N hydrogen bonds link the complexes into supramolecular chains. These chains are linked into a supramolecular framework by the O-H...O hydrogen bonds between water molecules and NO₃ groups.     

Synthesis and crystal structure of a supramolecular adduct of the aqua nitrato complex of gadolinium [Gd(NO<Subscript>3</Subscript>)(H<Subscript>2</Subscript>O)<Subscript>7</Subscript>]<Superscript>2+</Superscript> with macrocyclic cavitand cucurbit[6]uril

A supramolecular adduct of gadolinium aqua nitrato complex and cucurbit[6]uril { [Gd(NO₃)(H₂O)₇](C₅H₅N)@(C₃₆H₃₆N₂₄O₁₂)}(NO₃)₂·10H₂O is obtained by slow diffusion of methanol into an aqueous solution containing gadolinium nitrate, pyridine, and cucurbit[6]uril. According to single crystal X-ray diffraction data, water molecules coordinated to metal atom make hydrogen bonds to polarized carbonyl groups of the macrocycle. The heptaaquanitratogadolinium(III) [Gd(NO₃)(H₂O)₇]²⁺ cation is structurally characterized for the first time. Crystal system is triclinic, space group \(P\overline 1 \), a = 12.3137(4) Å, b = 14.2334(5) Å, c = 19.5629(6) Å; α = 80.850(1)°, β = 86.879(1)°, γ = 68.855(1)°; V = 3157.15(18) ų, Z = 2. Oriented hydrogen-bonded chains of alternating cucurbit[6]uril molecules and gadolinium aqua cations form in the crystal structure.     

Synthesis and crystal structure of Isotrithionedithiolato-bis(phenanthroline)zinc(II)

The synthesis of a mixed-ligand complex 1,3-dithiole-2-thione-4,5-dithiolato-bis(1,10-phenanthroline)zinc(II), [Zn(Dmit)(Phen)₂], is described. The crystals are monoclinic, space group P2₁/n, a = 11.868(2) Å, b = 13.122(3) Å, c = 17.010(3) Å, β = 102.01(3)°, Z = 4. The coordination polyhedron of the Zn(II) atom is an octahedron formed by two sulfur atoms of the Dmit ligand and four nitrogen atoms of the two Phen ligands. The complex is studied by IR and UV spectroscopy.     

Complexes of acetic acid α-(N-benzoxazolin-2-one) with Zn(II), Cu(II), and Co(II): Syntheses and crystal structures

The results of syntheses and X-ray diffraction analyses of mononuclear complexes [ML₂(H₂O)₄] (M = Co²⁺(I), Cu²⁺(II), and Zn²⁺(III)) containing water molecules and anions of acetic acid α-(N-benzoxazolin-2-one) (L = C₉H₆O₄) are presented. The crystals of complexes I–III are isostructural (space group P2₁/n, Z = 2) and are built of discrete neutral complex molecules. The crystallographic data are as follows: for complex I, a = 6.1470(5), b = 5.3310(3), c = 30.5894(17) Å, β = 95.056(6)°, V = 998.50(11) ų; for complex II, a = 5.9661(6) Å, b = 5.1414(4) Å, c = 32.672(2) Å, β = 92.395(6)°, V = 1001.33(14) ų; and for complex III, a = 6.1404(3) Å, b = 5.3476(2) Å, c = 30.5865(12) Å, β = 94.708(4)°, V = 1000.96(7) ų. The metal atoms (M) of the complexing agents are localized in the crystallographic symmetry centers and have a distorted octahedral environment due to two oxygen atoms of the carboxy groups of two monodentate ligands (L) and four water molecules. The M-O(1w)(H₂O) and M-O(2w)(H₂O) bond lengths for the indicated complexes are 2.088(3) and 2.118(3), 2.446(3) and 1.971(3), and 2.113(4) and 2.093(3) Å for M = Co²⁺, Cu²⁺, and Zn²⁺, respectively. The crystal structures are formed due to packing of chains built of inter-molecular hydrogen bonds O-H…O.     

A novel copper(II) complex with schiff base derived from o-vanillin and L-methionine: Syntheses and crystal structures

A new Schiff base copper(II) complex, {[CuL(H₂O)₂][CuL(H₂O)]₃ · 4H₂O · C₃H₇NO} _n (H₂L = (Z)-2-(2-hydroxy-3-methoxybenzylideneamino)-4-(methylthio)butanoic acid), was synthesized and characterized by IR, UV, and X-ray diffraction single-crystal analysis. The crystal belongs to the triclinic crystal system, space group with cell parameters a = 5.2027(5) Å, b = 16.6916(16) Å, c = 20.237(2) Å, α = 88.895(10)°, β = 84.127(1)°, γ = 83.577(10)°, V = 1737.2(3) ų, Z = 1, F(000) = 848, S = 1.042, ρ_calcd = 1.561 g cm^?3, μ = 1.411 mm^?1, the final R ₁ = 0.0760 and wR ₂ = 0.2318 for 6030 observed reflections (I > 2σ(I)). The crystal structure of the complex contains two independent units with different coordination environments. In independent unit 1, the Cu(1) is five-coordinated by one nitrogen atom and two oxygen atoms from the Schiff base ligand and two oxygen atoms from two water molecules to form a distorted square pyramid geometry. On the other hand, in independent unit 2, the Cu(2) is five-coordinated and possesses a slightly distorted square-pyramidal coordination geometry, defined by one nitrogen atom, one hydroxyl oxygen atom, two carboxylate oxygen atoms in two different ligands, and one oxygen atom of the water molecule. The complex forms a one-dimensional chain polymer in the xy plane through carboxyl oxygen atoms in the Schiff base ligands.     

Synthesis and crystal structure of divaleratobis(nicotinamide)copper(II)

A copper(II) valerate complex with nicotinamide (L) [CuL₂(C₄H₉COO)₂] (I) has been synthesized and studied by IR spectroscopy and thermogravimetry. The crystal structure has been determined. The crystals of 1 are monoclinic, a = 11.297(1) Å, b = 6.666(1) Å, c = 16.873(2) Å, b = 108.50(1)°, V = 1204.9(3) ų, Z = 2, space group P2₁/c. The structural units of the crystal of I are centrosymmetric tetragonal bipyramidal (4+2) complex molecules. The equatorial positions of the bipyramid are occupied by trans-arranged pairs of O (Cu-O, 1.973 Å) and N (Cu-N, 2.006 Å) atoms, and the axial positions are occupied by the second O atoms of the valerate anions located at longer distances (Cu-O, 2.506 Å). The supramolecular associates formed in the crystal are layers of hydrogen-bonded complexes. The disordered hydrocarbon “tails” of the valerate groups point toward the interlayer space.     

Crystal structure and triboluminescence of the [Eu(TTA)2(NO3)(TPPO)2] complex

The crystal structure of [Eu(TTA)₂(NO₃)(TPPO)₂] (I) (TTA = thenoyltrifluoroacetone, TPPO = triphenylphosphine oxide) possessing intense triboluminescence was established by X-ray crystallography. The crystals are triclinic, noncentrocymmetrical: a = 11.047(3) Å, b = 11.794(3) Å, c = 12.537(3) Å; α = 102.635 (4)°, β = 102.088(4)°,γ = 117.765(3)°; space group P1, Z = 1. The central Eu(III) atom coordinates two oxygen atoms of two TPPO molecules at distances of 2.271 Å and 2.282 Å, two oxygen atoms of the nitrate group at distances of 2.478 Å and 2.481 Å, four oxygen atoms of two TTA ions at distances of 2.365 Å, 2.381 Å, and 2.363 Å, 2.371 Å (coordination number is 8). The coordination polyhedron of the Eu(III) atom is a distorted dodecahedron. Possible reasons for spectral differences in the Stark structure of photo-and triboluminescence of I are discussed.     

Synthesis and structure of a new molecular octahedral cluster complex Mo<Subscript>6</Subscript>Se<Subscript>8</Subscript>(Ph<Subscript>3</Subscript>P)<Subscript>6</Subscript>·2H<Subscript>2</Subscript>O

Mo₆Se₈(Ph₃P)₆·2H₂O cluster complex has been synthesized and its structure has been defined. The compound is triclinic, space group P1ˉ, with unit cell parameters a = 14.3356(5) Å, b = 15.7882(4) Å, c = 25.3949(8) Å, = 95.9750(10)°, β = 91.1030(10)°, γ= 112.2570(10)°, V = 5279.8(3) ų, Z = 2, ρ_calc = 1.772 g/cm³. The complex has a molecular structure. The molybdenum atoms of the {Mo₆Se₈} cluster nucleus are coordinated by the phosphorus atoms of triphenylphosphine molecules. Original Russian Text Copyright ? 2007 by Yu. V. Mironov, Zh. S. Kozhomuratova, D. Yu. Naumov, and V. E. Fedorov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 389–393, March–April, 2007.     

Synthesis, crystal structure, and luminescent properties of a silver(I) perrhenate complex with phenazine

The silver complex with phenazine [Ag(Phz)₂(H₂O)]ReO₄ (Phz is C₁₂H₈N₂) has been synthesized, and its crystal structure has been determined. The crystals are triclinic: space group $P\bar 1$ , a = 9.587(1) Å, b = 10.875(1) Å, c = 11.668(1) Å, α = 104.98(1)°, β = 103.87(1)°, γ = 92.94(1)°, V = 1132.6(2) ų, Z = 2, ρ_calc = 2.160 g/cm³. The structure is composed of the [Ag(Phz)₂(H₂O)]⁺ silver cationic complexes and ReO ₄ ^? anions. The Ag⁺ ion is coordinated by two nitrogen atoms of independent phenazine molecules and the water oxygen atoms and has a T-shaped coordination (Ag-N_av 2.223 Å, Ag-O_w 2.498(8) Å). Phenazine, being an electron-donor ligand, forms columns due to π-π stacking interaction between the aromatic groups. The water molecules form hydrogen bonds with the oxygen atoms of water molecules of neighboring complexes and with oxygen atoms of the ReO ₄ ^? anions.     

Heteroligand zinc(II) and copper(II) complexes with naphthylacetic acid and monoethanolamine: Syntheses and crystal structures

New heteroligand Cu(II) and Zn(II) complexes with the α-naphthylacetic acid anion (NAA) and monoethanolamine (MEA), [M(NAA)₂(MEA)₂] (M = Cu²⁺, (I), Zn²⁺ (II)), are synthesized. The crystal structures of the obtained complexes are determined by X-ray diffraction analysis (CIF files CCDC 984097 (I) and 930946 (II)). The crystals are monoclinic, for I: a = 18.8140(9) Å, b = 4.82500(14) Å, c = 16.0360(7) Å, β = 115.135(6)°, V = 1317.87(11) ų, space group P2₁/c, Z = 2; for II: a = 32.9760(14) Å, b = 5.0911(3) Å, c = 15.7994(10) Å, β = 94.418(5)°, V = 2644.6(3) ų, space group C2/c, Z = 4. In the structure of complex I, the Cu²⁺ ion arranged in the symmetry center is coordinated at the vertices of the distorted octahedron by the oxygen atoms of two NAA molecules (Cu-O(2) 2.019(4) Å) and two MEA molecules. The latter is the bidentate-chelating ligand and coordinates the metal through the O and N atoms to form the five-membered metallocycle (Cu-O(3) 2.457(5), Cu-N(1) 1.986(5) Å). In complex II, the Zn atom (on axis 2) is coordinated at the vertices of the distorted tetrahedron by the oxygen atoms of two NAA molecules (Zn-O(2) 1.976(4) Å) and the nitrogen atoms of two MEA molecules (Zn-N 2.034(6) Å). The character of the interaction of coordinated NAA and MEA ligands and methods for packing complexes I and II are considered on the basis of the structural data.     

A complex of cadmium(II) iodide with 4-cyanopyridine: Synthesis,crystal structure,and luminescent properties

The complex [CdI₂(4-CNPy)₂] (I) was obtained by a reaction of CdI₂ with 4-cyanopyridine (4-CNPy, C₆H₄N₂) and structurally characterized (CIF file CCDC no. 983377). The crystals of complex I are monoclinic, space group C2, a = 24.698(5) Å, b = 4.127(1) Å, c = 7.597(2) Å, β = 96.05(1)°, V = 770.0(3) ų, ρ_calcd = 2.477 g/cm³, Z = 2. In structure I, iodine atoms serve to unite complex molecules into the polymer chains [CdI₂(4-CNPy)₂]_∞ along the direction [010]. The Cd(1) atom lying on a twofold axis has a slightly distorted octahedral environment made up of four bridging iodine atoms and two nitrogen atoms of two ligands 4-CNPy (Cd-I_av, 2.947(2) and Cd-N(1), 2.410(6) Å). Within each chain, cadmium atoms are spaced apart at 4.13 Å. Complex I exhibits photoluminescence.     

Crystal and molecular structures of bis(2,2,6,6-tetramethyl-3-methylaminoheptan-5-onate) copper(II) and nickel(II)

Two bis-chelates M(tmih)₂ (M = Cu(II), Ni(II), tmih = (CH₃)₃C(NCH₃)CHCOC(CH₃)₃)^? are synthesized and their crystal structures are determined using XRD (Bruker APEX-II diffractometer with a CCD detector, λMoK _α, λCuK _α, graphite monochromator, T = 240(2) K and 296(2) K): Cu(tmih)₂ (I) (space group P2₁/c, a = 12.9670(8) Å, b = 18.4921(9) Å, c = 11.0422(6) Å, β = 93.408(4)°, V = 2643.1(3) ų, Z = 4) and Ni(tmih)₂ (II) (space group P2₁/c, a = 12.810(2) Å, b = 18.529(2) Å, c = 11.243(2) Å, β = 91.959(7)°, V = 2667.1(6) ų, Z = 4). The complexes are isostructural; the coordination polyhedron of metal atoms is a flattened tetrahedron formed from two O atoms (Cu-O of 1.901(2) Å, 1.892(2) Å, Ni-O of 1.845(2) Å, 1.833(2) Å) and two N atoms (Cu-N of 1.976(3) Å, 1.972(3) Å, Ni-N of 1.911(2) Å, 1.920(2) Å) of the ligand; the chelate OMN angles (M = Cu(II), Ni(II)) are in the 87.4–93.1° range; the OMO and NMN angles are 162.2° and 167.2° in I, 171.1° and 173.2° in II. The complexes have the molecular structures formed from isolated molecules bonded by van der Waals interactions. Using a quantum chemical hybrid M06 method, the structures of copper(II) chelates with the H, CH₃, CH₂CH₃, CH(CH₃)₂, and C(CH₃)₃ substituents at the nitrogen atom are calculated. Found that with a bulky substituent at the nitrogen atom, the formation of chelates is hindered due to the intraligand repulsion between the atoms of this substituent and the tert-butyl group.     

Cadmium(II) iodide molecular coordination compounds with 4-methylpyridine and 4-methylquinoline

The coordination compounds [CdI₂(4-MePy)₂] (I) and [CdI₂(4-MeQuin)₂] (II) where Quin is quinoline have been synthesized, and their structure has been solved. Crystals of complex I are monoclinic, space group C2/c, a = 13.353(1) Å, b = 16.653(1) Å, c = 14.380 (1) Å, β = 103.17(1)°, V = 3113.5(4) ų, ρ_calcd = 2.425 g/cm³, Z = 8. Crystals of complex II are monoclinic, space group P2₁/c, a = 10.647(1) Å, b = 25.264(1) Å, c = 8.610(1) Å, β = 113.73(1)°, V = 2120.1(3) ų, ρ_calcd = 2.044 g/cm³, Z = 4. Polymer [CdI₂(4-MePy)₂]_∞ chains running in the direction [001] are formed in the structure of complex I. Each of the two crystallographically nonequivalent Cd(1) and Cd(2) atoms are octahedrally surrounded by the four iodine and two nitrogen atoms of the 4-MePy ligand. The Cd(1)?Cd(2) distance in a chain is 4.33 Å. The structure of complex II is built of [CdI₂(4-MeQuin)₂] discrete neutral clusters. The two iodine and two nitrogen atoms of the 4-MeQuin ligand participate in the coordination of the Cd²⁺ ion. The cadmium coordination polyhedron is a distorted tetrahedron (Cd-I_avg, 2.72 Å; Cd-N_avg, 2.30 Å; angles N(I)CdN(I), 98.3–121.8°). The minimum and maximum values correspond to the ICdI angle and NCdN angle, respectively. Complex I is photoluminescent in the solid state at room temperature.     

Synthesis and crystal and molecular structure of the mixed-ligand coordination compound ZnPhen(n-C4H9OCS2)2

A mixed-ligand complex ZnPhen(n-BuOCS₂)₂ has been synthesized. The structure of the compound was solved by X-ray diffractometry (X8 APEX diffractometer, MoK _α radiation, 4254 F _hkl , R = 0.0448). Triclinic crystals with the parameters a = 9.4464(3) Å, b = 11.0279(4) Å, c = 13.6528(6) Å;α = 106.940(1)°, β = 98.382(1)°, γ = 106.347(1)°; V = 1264.72(8) ų; Z = 2, space group 1. P1ˉ. The structure consists of discrete mononuclear molecules. The polyhedron of the Zn atom is a trigonal bipyramid N₂S₃ formed by coordination of the N atoms of the bidentate Phen molecules and the sulfur atoms of the monodentate and cyclic bidentate xanthate ligands. Dimer assemblies are formed in the structure due to π-π interactions of Phen molecules. Original Russian Text Copyright ? 2006 by R. F. Klevtsova, T. G. Leonova, L. A. Glinskaya, and S. V. Larionov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 6, pp. 1189–1194, November–December, 2006.     

Synthesis and crystal structure of zinc(II) and manganese(II) complexes of 2-(diphenylacetyl)indandione-1,3

Zinc(II) and manganese(II) complexes of 2-(diphenylacetyl)indandione-1,3 (HL) were synthesized. Crystals of [M(DMSO)₂L₂] · CHCl₃, where M= Zn^(II) (I) and Mn^(II) (II), obtained from chloroform plus dimethyl sulfoxide (DMSO) mixture were found to be isostructural based on the similarity of their unit cell parameters and unit cell volumes. The crystals are triclinic, Z = 2, space group P \(\bar 1\); a = 10.422(1) Å, b = 11.929(1) Å, c = 20.429(1) Å, α = 73.616(1)°, β = 85.095(1)°, γ = 77.586(1)° for complex I; a = 10.436(1) Å, b = 12.297(1) Å, c = 19.924(2) Å, α = 78.138(2)°, β = 87.625(2)°, γ = 82.048(2)° for complex II. X-ray structural analysis of complex I was carried out. For complex II, the structure was not refined because all of its atoms are each disordered over three to five positions. The two DMSO molecules in complex I coordinate the central metal atoms in the monodentate mode via their donor oxygen atoms to occupy an axial position and an equatorial position in an octahedral polyhedron. The other four positions are occupied by the four oxygen atoms of the two deprotonated ligands L^? coordinated in the bidentate-cyclic mode. The outer sphere of complex I contains the solvating chloroform molecule.     

Synthesis and crystal structure of diaquadibenzoatobis(nicotinamide)nickel(II)

A coordination compound of nickel(II) benzoate with nicotinamide [Ni(C₆H₅COO)₂(L)₂(H₂O)₂] (I) (L is nicotinic acid amide) is synthesized and studied by IR spectroscopy. Its crystal structure is solved by X-ray crystallography. The crystals of compound I are monoclinic: a = 7.152 Å, b = 18.266 Å, c = 10.341 Å, β = 109.24°, V = 1275.4 ų, Z = 2, space group P2₁/c. Structural units of a crystal of I are centrosymmetric octahedral complex molecules. The coordination environment of the Ni atom contains two O atoms (Ni-O(1) 2.066(2) Å) and two N atoms (Ni-N(1) 2.091(2) Å) of the monodentate-coordinated benzoate anions and nicotinamide molecules, respectively, as well as two O atoms of the H₂O molecules (Ni-O(1w) 2.110(2) Å).     

Crystal structure of barium α-(Ethylenediamine-N,N-diacetato)malonatocobaltate(III) perchlorate pentahydrate Ba[Co(Edda)(Mal)(ClO4) · 5H2O

The crystal structure of [Co (Edda)(Mal)](ClO₄) · 5H₂O is determined by X-ray diffraction analysis (the crystals are triclinic: a = 10.1363(12) Å, b = 11.0801(13) Å, c = 11.3173(13) Å, α = 101.129(13)°, β = 108.594(13)°, γ = 112.883(13)°, Z = 2, space group P $\overline 1 $ ). The Co³⁺ ion coordinates two O atoms of the malonate ion, as well as two N atoms and two trans-O atoms of the ethylene-N,N-diacetate ion. The [(H₂O)₄Ba(ClO₄)]⁺ subunits interact with the [Co(Edda)(Mal)]^? complexes to form infinite ribbons, and each complex is bonded with three Ba atoms through the O atoms of the carboxyl groups. The coordination number of the Ba atom is nine (four O atoms of the water molecule, one O atom of the perchlorate ion, and four O atoms of three adjacent complexes).