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).     

Synthesis and X-ray diffraction study of (Cs0.5Ba0.25)[UO2(CH3COO)3] and Ba0.5[UO2(CH3COO)3]

Uranyl triacetate complexes (Cs_0.5Ba_0.25)[UO₂(CH₃COO)₃] (I) and Ba_0.5[UO₂(CH₃COO)₃] (II) are synthesized for the first time and their structures are determined by X-ray diffraction. Both compounds crystallize in the cubic crystal system. The crystal data are as follows: a = 17.3289(7) ?, V = 5203.7(4) ?³, space group I2₁3 and Z = 16 (I); a = 17.0515(8)?, V = 4957.8(4) ?³, space group I $ \bar 4 $ \bar 4 3d, and Z = 16 (II). In I and II, as in all uranyl triacetates studied earlier, the coordination polyhedron of the uranium atom is a hexagonal bipyramid whose vertices are occupied by the oxygen atoms of the uranyl and three acetate groups. The uranium-containing group belongs to the AB ₃⁰¹ (A = UO₂²⁺, B ⁰¹ = CH₃COO⁻) crystal chemical group of uranyl complexes. It was found that compound II is isostructural to the (Rb_0.50Ba_0.25)[UO₂(CH₃COO)₃] studied earlier.     

Crystal structure of R[UO2(CH3COO)3] (R = NH 4+ , K+, or Cs+)

The single crystal structure of NH₄[UO₂(CH₃COO)₃] (I), K[UO₂(CH₃COO)₃] (II), and Cs[UO₂(CH₃COO)₃] (III) is studied by X-ray diffraction. I and II crystallize in the tetragonal crystal system. The crystal data are as follows: a = 13.6985(3) and c = 27.5678(14) ?, V = 5173.1(3) ?³, space group I4₁/a, Z = 16, and R = 0.023 for I; a = 13.8890(5) and c = 26.0839(18) ?, V = 5031.7(4) ?³, space group I4₁/a, Z = 16, and R = 0.037 for II. Crystals III are orthorhombic, a = 18.176(2), b = 13.119(2), and c = 22.088(4) ?, V = 5267(1)?³, space group Pbca, Z = 16, and R = 0.0424. In structures I–III, the uranium-containing structural units are represented by discrete mononuclear [UO₂(CH₃COO)₃]⁻ groups, which belong to the AB ₃⁰¹ (A = UO₂²⁺, B ⁰¹=CH₃COO⁻) crystal chemical group of uranyl complexes.     

Crystal structure of M4[(UO2)2C2O4(SO4)2(NCS)2] ( M = K+, Rh+) and K4[(UO2)2C2O4(SeO4)2(NCS)2]

Three heteroacidoligand uranyl complexes M ₄[(UO₂)₂C₂O₄(SO₄)₂(NCS)₂] (M = K⁺ (I), Rb⁺ (II)) and K₄[(UO₂)₂C₂O₄(SeO₄)₂(NCS)₂] (III) have been synthesized and their crystal structure has been determined by X-ray diffraction analysis. The compounds I–III are isostructural and crystallized in the monoclinic system, sp. gr. P2₁/c, Z = 2, a = 11.5548(3) ?, b = 7.0847(1) ?, c = 13.5172(3) ?, β = 93.130(1)°, V = 1104.90(4), R = 0.015 (I); a = 11.5854(9) ?, b = 7.3841(6) ?, c = 13.9072(9) ?, β = 95.754(3)°, V = 1183.74(15), R = 0.0235 (II); a = 11.6715(3) ?, b = 7.1418(2) ?, c = 13.8546(1) ?, β = 93.539(1)°, V = 1152.66(5), R = 0.0126 (III). Basic structural units of these crystals are [(UO₂)₂C₂O₄(XO₄)₂(NCS)₂]⁴⁻ chains, which belong to the crystallochemical group A ₂ K ⁰² B ₂² M ₂¹ (A = UO₂²⁺, K ⁰² = C₂O₂₋⁴, B ² = SO₄²⁻ or SeO₄²⁻, M ¹ = NCS⁻) of uranyl complexes. Uranium-containing chains are connected into a 3D framework via a system of electrostatic interactions with potassium or rubidium cations from outer spheres. Original Russian Text ? I.V. Medrish, E.V. Peresypkina, A.V. Virovets, L.B. Serezhkina, 2008, published in Kristallografiya, 2008, Vol. 53, No. 3, pp. 495–498.     

Synthesis, characterization and crystal structure of [Ni(DACH)2](H2O)2(CH3COO)2 (DACH = 1,4-diazacycloheptane): a three-dimensional (3-D) hydrogen-bonded network embodying 1-D water chains

The mononuclear complex [Ni(DACH)₂](H₂O)₂(CH₃COO)₂ (DACH = 1,4-diazacyclo-heptane) has been synthesized and characterized by IR, UV-Vis, elemental analysis and single crystal X-ray diffraction. The complex crystallizes in monoclinic system, P2₁/n space group with a=7.500(3) ?, b=8.788(3) ?, c=16.429(6) ?, β=93.395(5)°, D _c =1.269 g cm⁻³, μ=0.930 mm⁻¹, V=1080.9(6) ?³, Z=2. The central Ni^II atom is in a square-planar coordination geometry formed by four N atoms of two DACH chelated ligands. The notable feature of the title compound resides in the formation of a three-dimensional network through hydrogen bonds between the [Ni(DACH)₂]²⁺ cations, the CH₃COO⁻ counter anions and the guest water molecules trapped in the crystal lattice.     

The isomorphous substitution of 2H+ for the Cu2+ cation in the complex of bis(aminoguanidine)copper(II): Crystal structures of (Cu0.61H0.78Agu2)B12H12 and (HAgu)2B12H12

An X-ray diffraction study of the (Cu_0.61H_0.78 Agu ₂)B₁₂H₁₂ (I) mixed crystal and one of its components (HAgu)₂B₁₂H₁₂ (II) is performed at 160 K (R = 0.0312 and 0.0345, respectively). Crystals I and II are isostructural. In I, two H⁺ ions partially substitute the Cu²⁺ cation, resulting in a combination of [CuAgu ₂]²⁺ and (HAgu ₂)₂₊ cations in the structure. The cations and polyhedral B₁₂H₁₂²⁻ anions have centrosymmetric structures. A square planar environment for the Cu atom is formed by four N atoms of two Agu molecules, which close five-membered chelate cycles [Cu-N, 1.9702(13) and 2.0261(10) ?]. The distant apical vertices are occupied by H atoms of the B₁₂H₁₂²⁻ anions [Cu…H, 2.805(14) ?]. In the dimeric (HAgu ₂)²⁺ cations, the proton that substitutes for the Cu²⁺ cation forms a three-center N(1)-H…N(4),N(4)′ hydrogen bond which consists of intramolecular and an intermolecular components. In crystal II, the N(1)…N(4) and N(1)…N(4)′ distances [2.685(1) and 3.111(1) ?] are longer than in I [2.610(2) and 3.027(2) ?]. In I, the Cu…H interactions connect [CuAgu ₂]²⁺ cations and B₁₂H₁₂²⁻ anions into chains. In the cells that contain the (HAgu ₂)²⁺ dimeric cation, the chains are retained due to the secondary N-H…(B-H) interactions. Numerous weak secondary interactions between the cations and anions form three-dimensional frameworks in structures I and II.     

Syntheses, Characterizations and Crystal Structures of Two Copper Coordination Polymers Both Having Cu2Cl2 Bridging Subunit [CuI(bipy)1/2Cl]n(1) and {[(CuII)4(phen)4(SSA)2Cl2](H2O)2(DMF)2}n(2)

Abstract  

Two copper coordination polymers [Cu^I(bipy)_1/2Cl] _n (1) and {[(Cu^II)₄(phen)₄(SSA)₂Cl₂] (H₂O)₂(DMF)₂} _n (2)(bipy = 4,4′-bipyridine, phen = 1,10-phenanthroline, H₃SSA = 5-sulfosalicylic acid, DMF = N,N-dimethylformamide) have been prepared and characterized by X-ray diffraction, elemental analysis, IR spectrum and 2 was also studied by cyclic voltammetric method. X-ray analysis indicates that both of them have Cu₂Cl₂ bridging subunit. Complex 1 is a two dimensional network structure. While 2 shows a one dimensional zigzag chain. Electrochemistry studies reveal that complex 2 undergo a quasi reversible one-electron metal-centered redox process at E _1/2 = +0.062 V.     

Synthesis and crystal structure of oxonitrate complexes Cs[VO2(NO3)2], Cs[MoO2(NO3)3], and MoO2(NO3)2

Cs[VO₂(NO₃)₂] (I), MoO₂(NO₃)₂ (II), and Cs[MoO₂(NO₃)₃] (III) complexes have been obtained by crystallization from nitric solutions and studied by single-crystal X-ray diffraction. Complexes I and II contain infinite zigzag chains of similar compositions, [VO₂(NO₃)₂]⁻ and [MoO₂(NO₃)₂], in which V and Mo atoms form, respectively, trigonal- and pentagonal-bipyramidal polyhedra. Each of these polyhedrons also contains one terminal and two bridge O atoms and two terminal NO₃ groups which are monodentate and bidentate in complexes I and II, respectively. Complex III has an island structure and consists of Cs⁺ cations and [MoO₂(NO₃)₃]⁻ anions, in which the Mo atom is surrounded by one bidentate NO₃ group and two monodentate NO₃ groups and two terminal O atoms in the cis-positions; oxygen atoms form a polyhedron in the form of distorted octahedron. According to the ab initio calculation of isolated MoO₂(NO₃)₂ molecules in the gas phase and solution, the coordination environment of the Mo atom, similarly to the Cr(VI) atom in CrO₂(NO₃)₂, is formed by two bidentate nitrate groups and two terminal O atoms (polyhedron- twisted trigonal prism).     

Reactions of triosmium clusters with indole: X-ray structures of [Os3(CO)10(μ-OH)(μ-OMeCO)] and [Os3(μ-H)(CO)10(μ-1, 2-η2-NC8H6)]

Treatment of [Os₃(CO)₁₂] with indole in presence of a methanolic solution of Me₃NO⋅2H₂O at 60^∘C afforded the previously reported compounds [(μ-H)Os₃(CO)₁₀(μ-OMe)] 2, [(μ-H)Os₃(CO)₁₀(μ-OH)] 3 and [Os₃(CO)₁₀(μ-OH)(μ-OMeCO)] 4 in 10, 5 and 20% yields, respectively. The reaction of [Os₃(CO)₁₀(MeCN)₂] with indole at room temperature gave [(μ-H)Os₃(CO)₁₀(μ-1,2-η²-NC₈H₆)] 5 in 40% yield. Compounds 4 and 5 have been characterized by single crystal X-ray diffraction studies. Compound 4 crystallizes in the monoclinic space group P2(1)/c with a = 23.1239(3), b = 9.8087(4), c = 16.9017(6) ?, β = 92.6998(14)^∘, Z = 8 and V = 3829.3(2) ?³ and 5 crystallizes in the monoclinic space group P2(1)/c with a = 9.009(3), b = 9.764(4), c = 24.906(6) ?, β = 93.452(14)^∘, Z = 4 and V = 2186.9(13) ?³. Compound 4 consists of an open cluster of three osmium atoms with the hydroxy and methoxycarbonyl ligands bridging the open Os–Os edge. Compound 5 consists of an isosceles triangle of osmium atoms with one elongated Os–Os edge which is bridged by the hydride and the indolyl ligands.     

Crystal structure of a new basic nitrate of neodymium(III), [Nd6O(OH)8(H2O)14(NO3)6](NO3)2 · 2H2O

A new basic Nd³⁺ nitrate, [Nd₆O(OH)₈(H₂O)₁₄(NO₃)₆](NO₃)₂ · 2H₂O (I), is isolated in the crystal form and studied. Compound I differs from the basic Ln nitrates containing [Ln ₆O(OH)₈] clusters in that it involves a larger number of water molecules. The incorporation of additional water molecules is accompanied by changes in the coordination environment of one of the three crystallographically independent Nd³⁺ cations. Two cations have coordination polyhedra in the form of a monocapped tetragonal antiprism with a coordination number of 9, and the third cation has a polyhedron in the form of a bicapped tetragonal antiprism with a coordination number of 10. Original Russian Text ? I.A. Charushnikova, C. Den Auwer, 2007, published in Kristallografiya, 2007, Vol. 52, No. 2, pp. 248–251.     

Synthesis and structure of (NH4)4[(DMF)2Mo8O26]· 2CH3CH2OH·2H2O (DMF= N , N -dimethylformamide)

A new organic-inorganic hybrid γ-octamolybdate complex, (NH₄)₄[(C₃H₇NO)₂Mo₈O₂₆]·2CH₃CH₂OH·2H₂O was synthesized from the mixture of ethanol, DMF, 4-aminobenzoic acid, (NH₄)₆Mo₇O₂₄·4H₂O, HCl and H₂O. The structure was determined by X-ray crystallography. It crystallizes in monoclinic P2₁/n space group with the crystal cell parameters of a = 8.8825(4), b = 21.1608(10), c = 11.1343(6) ?, β = 104.7720(10)°, V = 2023.64(17) ?³ and Z = 2. The crystal X-ray analysis shows that two DMF molecules are bound to γ-octamolybdate anion. The molecular structure is stabilized by the complex hydrogen bonding.     

Palladium (II) compounds with diaminocarboxylic acids: Crystal structures of [Pd(H2Cdta)] · H2O, [Pd(H3Edtp)Cl] · 2H2O, and (H6Edtp)[PdCl4] · 4H2O

The crystal structures of three Pd(II) compounds with diamine tetracarboxylates in different protonation states are determined, namely, [Pd(H₂ Cdta)] · H₂O (I), [Pd(H₃ EdtpCl] · 2H₂O (II), and (H₆ Edtp)[PdCl₄] · 4H₂O (III) (R ₁ = 0.0230, 0.0313, and 0.0277 for 3040, 3377, and 3809 reflections with I > 2σ(I) for I–III, respectively). Crystals I and II are built of neutral complexes [Pd(H₂ Cdta)] and [Pd(H₃ Edtp)Cl], respectively, and crystallization water molecules. Crystal III consists of [PdCl₄]²⁻ anionic complexes, H₆ Edtp ²⁺ cations, and water molecules. In I, one of the protonated acetate groups of the H₂ Cdta ²⁻ ligand forms a very weak additional Pd-O bond [2.968(2) Å] over the 2N + 2O coordination square. In II and III, the protonated propionate groups of the H₃ Edtp ⁻ ligand and the H₆ Edtp ²⁺ cation are not involved in Pd coordination and the coordination squares consist of the 2N + O + Cl and 4Cl atoms, respectively. __________ Translated from Kristallografiya, Vol. 48, No. 2, 2003, pp. 278–282. Original Russian Text Copyright ? 2003 by Polyakova, Poznyak, Sergienko.     

Synthesis and X-ray structural investigation of K2(H5O2)[UO2(C2O4)2(HSeO3)]

The synthesis and X-ray diffraction analysis of K₂(H₅O₂)[UO₂(C₂O₄)₂(HSeO₃)] single crystals have been performed. This compound crystallizes in the triclinic system with the unit-cell parameters a = 6.7665(4) ?, b = 8.8850(4) ?, c = 12.3147(7) ?, α = 94.73°, β = 90.16°, γ = 92.11°, sp. gr. P[`1]P\bar 1, Z = 2, and R = 0.019. The basic structural units are island [UO₂(C₂O₄)₂(HSeO₃)]³⁻ groups, which belong to the AB ₂⁰¹ M ¹ crystallochemical group of uranyl complexes (A = UO₂²⁺, B ⁰¹ = C₂O₄²⁻, and M ₁ = HSeO₃⁻). Uraniumcontaining complexes are linked through K⁺ and H₅O₂⁺ ions and via a system of hydrogen bonds with the participation of oxonium hydrogen atoms in this structure.     

A Novel Three Dimensional Organic–Inorganic Hybrid Based Porous Phase: Synthesis and Characterization of Reduced Oxovanadium pyromellitate, [VIV2O2(H2O)2(C6H2(COO)4)]

The hydrothermal reaction of a mixture of VOSO₄ · xH₂O, 1,2,4,5-benzenetetracarboxylic acid (pyromellitic acid) and 0.1 M H₂SO₄ for 72 h at 160 °C gives blue needle like crystals of [V^IV ₂O₂(H₂O)₂(C₆H₂(COO)₄)] in 30% yield. The compound has a porous 3-D extended network structure having a rigid architecture which is held together by the multidentate functionalities of 1,2,4,5-benzenetetracarboxylate ligand. Crystal data for the compound: monoclinic space group C 2/c (No:15), a = 11.756(5) ?, b = 9.645(3) ?, c = 11.822(7) ?, β = 107.10(4)°, Z = 8. The compound constitutes the first example of a fully reduced oxovanadium based solid incorporating the organic ligand. This article consists of synthesis, crystal structure and characterization of [V^IV ₂O₂(H₂O)₂(C₆H₂(COO)₄)].     

Solvothermal Syntheses and Crystal Structures of Neodymium Thiostannates [Nd(dien)3]2[(Sn2S6)Cl2] and [Nd(dien)3]2[(Sn2S6)(SH)2]

Abstract  

Two neodymium thiostannates [Nd(dien)₃]₂[(Sn₂S₆)Cl₂] (1) and [Nd(dien)₃]₂[(Sn₂S₆)(SH)₂] (2) (dien = diethylenetriamine) were synthesized by the reaction of tin and sulfur in the presence of NdCl₃ and Nd₂O₃, respectively under solvothermal conditions. Compounds 1 and 2 crystallize in monoclinic space group P2₁/n. Crystallographic data for 1: a = 11.6722(16), b = 15.119(2), c = 14.1566(19) ?, β = 96.213(3)°, V = 2483.6(6) ?³, Z = 4. For 2: a = 11.7190(14), b = 15.2168(19), c = 14.2209(18) ?, β = 95.775(4)°, V = 2523.1(5) ?³, Z = 4. The nine-coordinate [Nd(trien)₃]³⁺ complex cation formed in situ acts as the counter ion to the [Sn₂S₆]⁴⁻ anion. The [Nd(dien)₃]³⁺, [Sn₂S₆]⁴⁻ and Cl^– (or SH^–) ions form a 3-dimensional network structure through the N–H···S and N–H···Cl hydrogen bonds.     

Synthesis, structure and supramolecular assembly in the crystalline state of a bifunctionalized arylimido derivative of hexamolybdate [n-Bu4N]2[Mo6O17(o,p-(MeO)2C6H3N)2]

A novel bifunctionalized arylimido derivative of hexamolybdate [n-Bu₄N]₂[Mo₆O₁₇(o,p-(MeO)₂C₆H₃N)₂] (1) was synthesized by self-assembled metathesis of α-type octamolybdate ion and 2,4-dimethoxyaniline and structurally characterized by crystal X-ray diffraction. Crystallographic data for1: monoclinic system, space group:C2/c,a = 17.319(4),b = 18.087(4),c = 21.357(5) ?, β = 106.486(4),V = 6415(2) ?³, andZ = 4,D_c = 1.693 g/cm³,R₁ = 0.0439. The complex has a short Mo–N bond length of 1.735(5) ? and an imido (Mo–N–C) bond angle of 177.8(4)^∘. The complex has also been characterized by¹H NMR, IR, and UV–vis spectroscopy.     

Synthesis, Spectroscopic Characterization and Crystal Structure of a New Acetyl phosphorylamidate P(O)[NHC(O)C6H4(4-NO2)][N(CH(CH3)2)(CH2C6H5)]2

Abstract  

A new acetyl phosphorylamidate P(O)[NHC(O)C₆H₄(4-NO₂)][N(CH(CH₃)₂)(CH₂C₆H₅)]₂ has been synthesized and characterized by elemental analysis, ¹H, ¹³C and ³¹P NMR, IR and single crystal X-ray diffraction. Single crystal X-ray analysis shows that it belongs to triclinic system, space group P[`1] P\bar{1} , with a = 10.5868(16) Å, b = 11.8058(18) Å, c = 12.4364(19) Å, α = 65.410(3)°, β = 67.492(4)°, γ = 85.879(3)°, V = 1,298.6(3) Å³, and Z = 2. The intermolecular PO···HN hydrogen bond makes H-bonded dimer of molecule with Ci symmetry. In the crystal network, the dimers are aggregated in the chain arrays through π-stacking between p-NO₂–C₆H₄–C(O)–NH– moieties. Moreover, weak C–H···O and C–H···π interactions exist in the crystal network.     

Synthesis and Crystal Structure of Copper II and Silver I Complex with 1,4-diazabicyclo[2.2.2]octane[Cu(CBC)2(Dabco)(H2O)] n (1) and [Ag2(HBC)2(Dabco)] n (2)

Two 1D polymeric complex, [Cu(CBC)₂(Dabco)(H₂O)] _n (1) and [Ag₂(HBC)₂(Dabco)] _n (2) have been synthesized and characterized by X-ray single crystal analysis, where CBCH is p-chlorobenzoic acid, HBCH 2 is 2-hydroxybenzoic acid and Dabco is 1,4-diazabicyclo[2.2.2]octane. Complex 1 has been obtained in high yield by hydrothermal synthesis from CuO and CBCH and Dabco, and complex 2 has been obtain by evaporation of the solvent from silver salicylate and Dabco, 1 crystallizes in the orthorhombic space group Pmn2 ₁ with a = 24.3310(5) ?, b = 6.9050(6) ?, c = 5.9980(5) ?, Z = 2, V = 1007.70(4) ?³ and Dx = 1.657 g cm⁻³, 2 crystallizes in the monoclinic space group P2 ₁ /m with a = 10.292(3) ?, b = 6.913(2) ?, c = 14.417(4) ?, β = 95.660(5), Z = 2, V = 1020.8(5) ?³ and Dx = 1.959 g cm⁻³. The final R value is 0.0302 for 1323 measured reflections for 1 and the final R value is 0.0684 for 1545 measured reflections for 2. The atomic arrangement is built by infinite one-dimensional polymeric chain in both complexes. These chains are cross-linked by hydrogen bonds involving the coordinated water molecules to form a two-dimensional framework in complex 1.     

Crystal structure of bis[diethylenetriamine-N′-(3-propionato)-N, N′,N″,O,O′]dicopper(II) Diperchlorate, [Cu2(4-Dtmp)2](ClO4)2

A complex of copper(II) with the diethylenetriaminemonopripionate ligand [Cu₂(4-Dtmp)₂](ClO₄)₂ (I) is synthesized and characterized using X-ray diffraction. The crystals of compound I are monoclinic, a = 7.740(2) Å, b = 19.199(3) Å, c = 8.449(2) Å, β = 91.61(2)°, Z = 2, and space group P2₁/n. The structural units of crystal I are centrosymmetric dimeric cations and statistically disordered ClO ₄ ⁻ anions. In the cation, the copper atom is coordinated by three N atoms [mean Cu-N, 2.01(1) Å] and two O atoms [Cu-O, 2.134(6) Å and 1.958(7) Å] of the pentadentate bridging-chelate Dtmp ligand, which occupy vertices of the trigonal bipyramid. The binuclear cations are linked via centrosymmetric pairs of hydrogen bonds into ribbons aligned parallel to the a axis of the crystal. The ClO ₄ ⁻ anions form columns in the same direction. In the crystal, the cationic ribbons and anionic columns alternate in a chessboard fashion. __________ Translated from Kristallografiya, Vol. 50, No. 3, 2005, pp. 450–454. Original Russian Text Copyright ? 2005 by Antsyshkina, Sadikov, Poznyak, Sergienko.     

Structures of mixed-ligand Manganese(II) compounds [Mn(Heida)(Phen)]2 · 7H2O and [Mn2(Edta)(Phen)] · 4H2O

The crystal structures of [Mn(Heida)(Phen)]₂ · 7H₂O (I) and [Mn₂(Edta)(Phen)] · 4H2O (II) are studied by X-ray diffraction [R ₁ = 0.0375 (0.0283) and wR ₂ = 0.0954 (0.0662) for 5449 (3176) observed reflections in I (II), respectively]. Structure I contains mononuclear mixed-ligand complexes [Mn(Heida)(Phen)] and [Mn(Heida)(Phen)(H₂O)]. In structure II, the [Mn(Edta)]²⁻ anionic complexes and the [Mn(Phen)(H₂O)₂]²⁺ cationic complexes are linked by the bridging carboxyl groups into the tetramers with C ₂ symmetry. In both compounds, two independent Mn atoms have different coordination numbers (6 and 7). __________ Translated from Kristallografiya, Vol. 47, No. 2, 2002, pp. 280–285. Original Russian Text Copyright ? 2002 by Polyakova, Sergienko, Poznyak.