Preparation, Crystal Structure and Spectroscopic Properties of Dimeric [Zn(2-bromobenzoato)2(phenazone)]2 and Monomeric [Zn(2-bromobenzoato)2(thiourea)2]·2H2O

Abstract  

The binuclear zinc complex bis(2-bromobenzoato-O)-bis(μ ₂ -2-bromobenzoato-O,O′)-bis(phenazone-O)-dizinc(II) (I) and the mononuclear dihydrate bis(2-bromobenzoato-O)-bis(thiourea-S)-zinc(II) (II) have been synthesized and characterized by means of elemental analysis and spectroscopic methods (IR, ¹H and ¹³C NMR, EDS). The solid state structures of both compounds were determined by single-crystal X-ray diffractometry. Compound [Zn(2-BrC₆H₄COO)₂(phen)]₂ (phen—phenazone) (I) crystallized as a dimeric compound with a triclinic lattice (space group P − 1), where both zinc atoms, interconnected by two carboxylate groups, possess a distorted tetrahedral coordination environment. The crystallographic data of complex I: a = 9.9410(3) ?, b = 10.7309(3) ?, c = 12.9237(4) ?, α = 93.6004(17)°, β = 92.5898(11)°, γ = 116.2192(16)°, V = 1230.26(6) ?³, Z = 1. Complex [Zn(2-BrC₆H₄COO)₂(tu)₂]·2H₂O (tu—thiourea) (II) crystallized with an orthorhombic lattice (space group Aba2) as a monomeric compound, where the coordination environment of the central zinc atom is a distorted tetrahedron. The crystallographic data of complex II are: a = 9.8595(3) ?, b = 19.7052(5) ?, c = 12.5908(3) ?, V = 2446.18(11) ?³, Z = 4. The modes of the carboxylate binding were assigned from the IR spectra using the magnitude of the separation between the carboxylate stretches (Δ), which correlated well with the crystal structures. The computed theoretical IR spectrum agreed well with the experimental data.     

Synthesis, Crystal Structure and Fluorescence Property of a Binuclear Zn(II) Complex: [Zn2(μ-N3)2(N3)2(L)2] [L?=?1-(1,10-phenanthrolin-2-yl)-2-pyridone]

Abstract  Hydrated zinc perchlorate reacted with sodium azide and 1-(1,10-phenanthrolin-2-yl)-2-pyridone (L) in methanol solution and resulted in the formation of a new binuclear complex: [Zn₂(μ-N₃)₂(N₃)₂(L)₂]. The complex has been characterized by elemental analysis and IR spectrum, and its crystal structure determined by X-ray crystallography and the complex crystallizes in the monoclinic system with space group P2₁/c and a = 11.409(2), b = 8.0733(15), c = 18.163(3) Ǻ, β = 99.095(3)°. In the complex two azide anions act as bridge ligand and another two azide anion and two 1-(1,10-phenanthrolin-2-yl)-2-pyridone function as terminal ligands, and Zn(II) ion lies in a distorted triangle bipyramid geometry. Index Abstract  The title binuclear Zn(II) complex was synthesized by zinc perchlorate, sodium azide and 1-(1,10-phenanthrolin-2-yl)-2-pyridone and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that azide anion function as both bridge ligand and terminal ligand, and 1-(1,10-phenanthrolin-2-yl)-2-pyridone only acts as a terminal ligand.      

Crystal Structure of a Trinuclear Mercury(II) Cyanide Complex of Tetramethylthiourea, [{(Tetramethylthiourea)2Hg(CN)2}2·Hg(CN)2]

Abstract  

The title compound was prepared by reacting mercury(II) cyanide and tetramethylthiourea (Tmtu) in the molar ratio of 1:1.75. It was characterized by IR and NMR (¹H and ¹³C) spectroscopy, and X-ray crystallography. The appearance of a band around 2,200 cm⁻¹ in IR and a resonance around 145 ppm in ¹³C NMR indicated the binding of cyanide to mercury(II). The crystal structure of the title complex, [{(tetramethylthiourea)₂Hg(CN)₂}₂·Hg(CN)₂] (1) consists of two independent [(Tmtu)₂Hg(CN)₂] moieties bridged by a Hg(CN)₂ unit. The mercury atom in [(Tmtu)₂Hg(CN)₂] unit is coordinated to two thione sulfur atoms of Tmtu and to two cyanide carbon atoms in a distorted tetrahedral mode.     

The Synthesis of Zinc(II) and Cadmium(II) 2,4-Dichlorophenoxyacetates in Water–Methanol Environment. Structure and Properties of Polymeric [Zn(2,4-D)2(MeOH)2]n and [Cd(2,4-D)2(H2O)2]n

Abstract  

The zinc(II) and cadmium(II) 2,4-dichlorophenoxyacetate salts were synthesized in mixed water–methanol environment and characterized by elemental analysis, IR spectrometry and thermal analysis coupled with mass spectrometry. The crystal structures were determined by X-ray crystallography (compound 1, [C₁₈H₁₈Cl₄O₈Zn] _n : monoclinic, P2₁/c, a = 19.094, b = 7.378, c = 8.008, α = 90.00, β = 101.134, γ = 90.00, V = 1106.95; compound 2, [C₁₆H₁₄Cl₄O₈Cd] _n : monoclinic, P2₁/c, a = 17.730, b = 7.293, c = 8.060, α = 90.00, β = 95.18, γ = 90.00, V = 1037.9). The structural and some thermal data about the presented cadmium salt were previously reported (Song et al. Acta Crystallogr E 62:m2397, 2006; Kobylecka et al. Thermochim Acta 482:49, 2009).     

Synthesis, Crystal Structure and Magnetic Property of a Cyano-Bridged Two-Dimensional Heterometallic Assembly [Mn(salen)]2[Fe(CN)5NO]·2H2O

Abstract  

A cyano-bridged bimetallic assembly, [Mn^III(salen)]₂[Fe^II(CN)₅NO]·2H₂O [salen = N,N′-1,2-ethylenebis(salicylideneiminato)dianion], has been prepared and characterized structurally and magnetically. It crystallizes in the tetragonal space group P4/ncc with a = b = 14.813(2) ?, c = 17.093(5) ?, V = 3750.6(13) ?³, Z = 4. In this complex, each [Fe(CN)₅NO]²⁻ unit connects four [Mn(salen)]⁺ units with its four co-planar cyanide groups, and each [Mn(salen)]⁺ unit is linked to two [Fe(CN)₅NO]²⁻ ions in trans-form, which results in a two-dimensional (2-D) network consisting of pillow-like octanuclear [–Fe^II–CN–Mn^III–NC–]₄ units with dimensions: Fe–C = 1.943(3) ?, C≡N– = 1.139(4) ?, Mn–N = 2.326(3) ?, Fe–C≡N = 178.0(3)°, Mn–N≡C = 161.7(3)°. The NO group of [Fe(CN)₅NO]²⁻ remains monodentate and the bond angle of Fe–N–O is linear (180.0°). The variable temperature magnetic susceptibilities, measured in the 1.8–300 K range, show a weak Mn^III···Mn^III antiferromagnetic interaction through the diamagnetic –NC–Fe^II–CN– bridges.     

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.     

Crystal Structure and Magnetic Properties of the Dinuclear MnII Compound [Mn2(bpy)4(2-ClC6H4COO)2](ClO4)2·2EtOH

Abstract  

The synthesis and crystal structure of the dinuclear manganese (II) compound [Mn₂(bpy)₄(2-ClC₆H₄COO)₂](ClO₄)₂·2EtOH is described. The complex crystallizes in the monoclinic system, space group P2₁/n with a = 12.2067(18), b = 17.335(3), c = 13.706(3) ? and β = 92.606(8)°. In this structure, two manganese ions are bridged by two 2-chlorobenzoate ligands in a syn–anti mode. The hexa-coordination of each manganese is completed by two 2,2′-bipyridine ligands. Two perchlorate anions and two molecules of ethanol complete the packing. In order to check the magnetic properties previously reported from a powder sample, new magnetic studies have been carried out from a crystal sample, obtaining J = −1.79 cm⁻¹ and g = 2.00 (H = −JS ₁ ·S ₂ ).     

Synthesis and structure of K2[(UO2)4(O)2(OH)2(C2O4)(CH3COO)2(H2O)2]·2H2O

Single crystals of the compound K₂[(UO₂)₄(O)₂(OH)₂(C₂O₄)(CH₃COO)₂(H₂O)₂]·2H₂O (I) are synthesized, and their structure is investigated using X-ray diffraction. Crystals of compound I belong to the triclinic system with the unit cell parameters a = 7.6777(6) ?, b = 7.9149(7) ?, c = 10.8729(9) ?, α = 72.379(2)°, β = 86.430(3)°, γ = 87.635(2)°, V = 628.33(9) ?³, space group P , Z = 1, and R ₁ = 0.0323. The main structural units of the crystals are [(UO₂)₄(O)₂(OH)₂(C₂O₄)(CH₃COO)₂(H₂O)₂]²⁻ chains, which belong to the crystal-chemical group A ₄ M ₂³ M ₂² K ⁰² B ₂⁰¹ M ₂¹ (A = UO₂²⁺, M ³ = O²⁻, M ² = OH⁻, K ⁰² = C₂O₄²⁻, B ⁰¹ = CH₃COO⁻, M ¹ = H₂O) of the uranyl complexes. The chains are formed by linking the centrosymmetric tetramers of the composition (UO₂)₄(O)₂(OH)₂(CH₃COO)₂(H₂O)₂ via tetradentate bridging oxalate ions. The uranium-containing groups are joined into a three-dimensional framework through the electrostatic interaction with potassium cations and a system of hydrogen bonds, which are formed with the participation of atoms involved in the composition of the water molecules, hydroxide ions, and uranyl ions. Original Russian Text ? L.B. Serezhkina, A.V. Vologzhanina, N.A. Neklyudova, V.N. Serezhkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 3, pp. 483–487.     

Structure, thermal, and infrared analyses of [NH3(CH2)3NH3]2[Ni(HP2O7)2(H2O)2] ? 4H2O

[NH₃(CH₂)₃NH₃]₂[Ni(HP₂O₇)₂(H₂O)₂] 4H₂O (NiDAP) is a new diphosphate of transition metallic and organic cations obtained from a mixture of H₄P₂O₇, 2NiCO₃ Ni(OH)₂ 4H₂O and NH₂(CH₂)₃NH₂ in a 1:1/6:1 molar ratio. This mixed organo-mineral compound crystallizes in the triclinic system, P¯, with the unit cell dimensions: a = 7.3678(3)~Å, b = 7.8018(5)Å, c = 11.1958(7)Å, = 76.914(4), = 81.052(4), = 85.46(1), V = 618.57(6)ų and Z = 1. The crystal structure of NiDAP consists of a complex anion, [Ni(HP₂O₇)₂(H₂O)₂]^4– and a diammoniumpropane cation. The complex anion is built up from two neutral water molecules (OW1) and two diphosphosphoric anions coordinated to Ni(II) in a bidentate chelating manner. (OW1) molecules link anionic complexes, [Ni(HP₂O₇)₂(H₂O)₂]^4– to create a thick bidimensional layers parallel to the (a, b) plane. These layers are interconnected in three dimensions through hydrogen bonds established between organic cations, the remaining water molecules OW2, OW3, and some external oxygen atoms of the anionic complex arrays. NiDAP was also characterized by IR spectroscopy, TG-DTA, and DSC analyses.     

Crystal structure of (μ5-decahydro- closo -decaborato) (μ2- O -dimethylformamide)disilver(I) [Ag2(B10H10)(DMF)]

The compound [Ag₂(B₁₀H₁₀)(DMF)] is synthesized, and its crystal structure is studied (R = 0.0699 for 2836 observed reflections). The coordination number of each of the four independent Ag atoms is 4 + 2. The nearest environment of the Ag(1) and Ag(4) atoms consists of two O atoms of the DMF molecules and two BH groups, and that of the Ag(2) and Ag(3) atoms consists of four BH groups. All the Ag atoms additionally form weak bonds with two BH groups. The Ag-O and Ag-B bonds lie in the ranges 2.319–2.465(9) and 2.46–2.70(1) ?, respectively, and the Ag⋯B distances are 2.89–3.25(1) ?. Due to the binding of each polyhedral anion to five Ag atoms, layers are formed. Bridging DMF molecules link layers into the three-dimensional framework. Original Russian Text ? I.N. Polyakova, E.A. Malinina, V.V. Drozdova, N.T. Kuznetsov, 2008, published in Kristallografiya, 2008, Vol. 53, No. 2, pp. 279–282.     

Synthesis and X-ray structural investigation of K8[(UO2)2(C2O4)2(SeO4)4] · 2H2O

Single crystals of the compound K₈[(UO₂)₂(C₂O₄)₂(SeO₄)4] · 2H₂O (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 = 14.9290(4) ?, b = 7.2800(2) ?, c = 15.3165(4) ?, β = 109.188(1)°, V = 1572.17(7) ?³, space group P2₁/n, Z = 2, and R = 0.0297. The uranium-containing structural units of crystals I are dimers of the composition [(UO ₂)₂(C₂O₄)₂(SeO₄)₄]⁸⁻, which belong to the crystal-chemical group AB ⁰¹ B ² M ¹ (A = UO₂²⁺, B ⁰¹ = C₂O₄²⁻, B ² = SeO₄²⁻, M ¹ = SeO₄²⁻) of the uranyl complexes. The [(UO₂)₂(C₂O₄)₂(SeO₄)₄]⁸⁻ dimers are joined into a three-dimensional framework through electrostatic interactions with the outer-sphere potassium cations. Original Russian Text ? L.B. Serezhkina, E.V. Peresypkina, A.V. Virovets, A.G. Verevkin, D.V. Pushkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 1, pp. 68–71.     

Investigations of 2-Thiazoline-2-thiol as a Ligand: Synthesis and X-ray Structures of [Mn2(CO)7(μ-NS2C3H4)2] and [Mn(CO)3(PPh3)(κ2-NS2C3H4)]

Abstract  Treatment of Mn₂(CO)₁₀ with 2-thiazoline-2-thiol in the presence of Me₃NO at room temperature afforded the dimanganese complexes [Mn₂(CO)₇(μ-NS₂C₃H₄)₂] (1) and [Mn₂(CO)₆(μ-NS₂C₃H₄)₂] (2) in 51 and 34% yields, respectively. Compound 1 was quantitatively converted into 2 when reacted with one equiv of Me₃NO. Reaction of 1 with triphenylphosphine at room temperature furnished the mononuclear complex [Mn(CO)₃(PPh₃)(κ ²-NS₂C₃H₄)] (3) in 66% yield. All three new complexes have been characterized by elemental analyzes and spectroscopic data together with single crystal X-ray diffraction studies for 1 and 3. Compound 1 crystallizes in the orthorhombic space group Pbca with a = 12.4147(2), b = 16.2416(3), c = 19.0841(4) ?, β = 90°, Z = 8 and V = 3848.01(12) ?³ and 3 crystallizes in the monoclinic space group P 2₁/n with a = 10.41730(10), b = 14.7710(2), c = 14.9209(2) ?, β = 91.1760(10)°, Z = 4 and V = 2295.45(5) ?³. Graphical Abstract  Two new dimanganese complexes [Mn₂(CO)₇(μ-NS₂C₃H₄)₂] (1) and [Mn₂(CO)₆(μ-NS₂C₃H₄)₂] (2) were formed when [Mn₂(CO)₁₀] was treated with 2-thiazoline-2-thiol in the presence of Me₃NO. Compound 2 reacts with PPh₃ to give the monomeric complex [Mn(CO)₃(PPh₃ )(κ ²-NS₂C₃H₄)]. The structures of 1 and 3 were established by crystallography. Shishir Ghosh, Faruque Ahmed, Rafique Al-Mamun, Daniel T. Haworth, Sergey V. Lindeman, Tasneem A. Siddiquee, Dennis W. Bennett, Shariff E. Kabir Investigations of 2-thiazoline-2-thiol as a ligand: Synthesis and X-ray structures of [Mn₂(CO)₇(μ-NS₂C₃H₄)₂] and [Mn(CO)₃ (PPh3)(κ ²-NS₂C₃H₄)].      

A Novel Keggin-Type Aluminotungstate Dimeric Compound: H3.5[Ni(2,2′-bipy)3]3{[AlW 10VI W 2V O40Ni(2,2′-bipy)2(H2O)]2Na0.5}

Abstract  A novel dimeric compound H_3.5[Ni(2,2′-bipy)₃]₃{[AlW₁₂O₄₀Ni(2,2′-bipy)₂(H₂O)]₂Na_0.5} prepared by the hydrothermal method consists of a {[AlW₁₂O₄₀Ni(2,2′-bipy)₂(H₂O)]₂Na_0.5}^9.5− heteropolyanion, and in the anion, two reduced Keggin heteropolyanions [AlW^VI ₁₀W₂^VO₄₀]⁷⁻ are bridged via Na coordination ion by means of an O–Na1–O linkage (O atoms from the surface bridging oxygen atoms of [AlW^VI ₁₀W₂^VO₄₀]⁷⁻) and two Ni coordination ions are linked to the Na1 square planar moiety by making use of Ni–Ow–Na1–Ow–Ni bridges. The crystal belongs to the monoclinic-space group C2/c, a = 46.592(9), b = 14.306(3), c = 25.967(5) ?, β = 90.14(3)°, V = 17308(6) ?³, Z = 4, D _c  = 3.116 Mg/m³. Index Abstract  A novel dimeric compound H_3.5[Ni(2,2′-bipy)₃]₃{[AlW₁₂O₄₀Ni(2,2′-bipy)₂(H₂O)]₂Na_0.5} prepared by the hydrothermal method consists of a {[AlW₁₂O₄₀Ni(2,2′-bipy)₂(H₂O)]₂Na_0.5}^9.5− heteropolyanion, and in the anion, two reduced Keggin heterpolyanions [AlW^VI ₁₀W^V ₂O₄₀]⁷⁻ are bridged via Na coordination ion by means of an O–Na1–O linkage (O atoms from the surface bridging oxygen atoms of [AlW^VI ₁₀W^V ₂O₄₀]⁷⁻) and two Ni coordination ions are linked to the Na1 square planar moiety by making use of Ni7–Ow7–Na17–Ow7–Ni bridges.      

Reactivity of [Re2(CO)8(MeCN)2] With 1-vinylimidazole: X-ray Structures of [Re2(CO)8{η1-NC3H3N(CH=CH2)}2] and [ReCl2(CO)2{η1-NC3H3N(CH=CH2)}2]

Abstract  Treatment of [Re₂(CO)₈(MeCN)₂] with excess 1-vinylimidazole in refluxing benzene gives three new compounds [Re₂(CO)₉{η ¹-NC₃H₃N(CH=CH₂)}] (1), [Re₂(CO)₈{η ¹-NC₃H₃N(CH=CH₂)}₂] (2) and [ReCl₂(CO)₂{η ¹-NC₃H₃N(CH=CH₂)}₂] (3) in 11, 32 and 2% yields, respectively. The solid-state structures of complexes 2 and 3 have been determined by single crystal X-ray diffraction studies. Compound 2 crystallizes in the monoclinic space group C2/c, with lattice parameters a = 13.8378(5) ?, b = 11.8909(5) ?, c = 14.4591(6) ?, β = 116.6470(10)°, Z = 4 and V = 2131.99(15) ?³. Compound 3 crystallizes in the monoclinic space group C2/c, with lattice parameters a = 10.1028(3) ?, b = 13.5640(5) ?, c = 12.5398(4) ?, β = 109.637(2)°, Z = 4 and V = 1618.4(9) ?³. The disubstituted dinuclear compound 2 contains two 1-vinylimidazole ligands coordinated through the imino nitrogen atoms at the equatorial sites, whereas the mononuclear compound 3 contains two carbonyl ligands, two N coordinated η ¹-1-vinylimidazole ligands and two terminal Cl ligands. Graphical Abstract  Two dinuclear complesxes [Re₂(CO)₉{η ¹-NC₃H₃N(CH=CH₂)}] (1) and [Re₂(CO)₈{η ¹-NC₃H₃N(CH=CH₂)}₂] (2) and the mononuclear [ReCl₂(CO)₂{η ¹-NC₃H₃N(CH=CH₂)}₂] (3) were obtained from the reaction of [Re₂(CO)₈(MeCN)₂] with excess 1-vinylimidazole at 80 °C. The X-ray structrures of 2 and 3 are described.      

Synthesis and structure of {NH2(C2H5)2}2[(UO2)2(C2O4)(CH3COO)4] · 2H2O

Single crystals of the compound {NH₂(C₂H₅)₂}₂[(UO₂)₂C₂O₄(CH₃COO)₄] · 2H₂O (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 = 9.210(2) ?, b = 14.321(3) ?, c = 12.659(3) ?, β = 105.465(13)°, V = 1609.2(6) ?³, space group P2₁/c, Z = 2, and R = 0.0198. The structural units of crystals I are binuclear groups of the composition [(UO₂)₂C₂O₄(CH₃COO)₄]²⁻ with an island structure, which belong to the crystal-chemical group A ₂ K ⁰² B ₄⁰¹ (A = UO₂²⁺, K ⁰² = C₂O₄²⁻, B ⁰¹ = CH₃COO⁻) of the uranyl complexes, diethylammonium cations, and water molecules. The uranium-containing groups are joined into a three-dimensional framework through electrostatic interactions with diethylammonium cations and a system of hydrogen bonds, which are formed with the participation of the atoms involved in the composition of the water molecules, oxalate ions, acetate ions, and diethylammonium cations. Original Russian Text ? L.B. Serezhkina, A.V. Vologzhanina, N.A. Neklyudova, V.N. Serezhkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 1, pp. 65–67.     

Synthesis, Characterization and Crystal Structure of a New One-Dimensional Heterobimetallic Coordination Polymer Based on [(Tp)Fe(CN)3]?

Abstract  

By using a pre-designed anionic precursor [TpFe^III(CN)₃]⁻ (Tp = hydrotris(pyrazolyl)borate) as a structural building block, a new cyanide-bridged one-dimensional heterobimetallic coordination polymer, [(Tp)₂Fe₂^III(CN)₆Zn·2H₂O] _n (I) has been prepared and characterized by X-ray single crystal diffraction, M?ssbauer and magnetic experiments. Complex I crystallizes in the orthorhombic Ibam space group with a = 14.4094(8) ?, b = 18.3003(10) ?, c = 12.9855(7) ? and consists of rhombic chains, in which the [TpFe^III(CN)₃]⁻ unit acts as a bridging bidentate ligand toward two Zn²⁺ atoms through two of its three cyanide groups.     

Synthesis and X-ray structural investigation of (C3N6H7)4(CN3H6)2[UO2(CrO4)4] · 4H2O and (H3O)6[UO2(CrO4)4]

Single crystals of the compounds (C₃N₆ H₇)₄(CN₃H₆)₂[UO₂(CrO₄)₄] · 4H₂O (I) and (H₃O)₆[UO₂(CrO₄)₄] (II) are synthesized, and their structures are investigated using X-ray diffraction. Compound I crystallizes in the triclinic system with the unit cell parameters a = 6.3951(8) ?, b = 10.8187(16) ?, c = 16.9709(18) ?, α = 93.674(4)°, β = 97.127(4)°, γ = 92.020(4)°, space group, P Z = 1, V = 1161.6(3) ?³, and R = 0.0470. Crystals of compound II belong to the monoclinic system with the unit cell parameters a = 14.3158(4) ?, b = 11.7477(3) ?, c = 13.1351(4) ?, β= 105.836(1)°, space group C2/c, Z = 4, V = 2125.2(1) ?³, and R = 0.0213. The uranium-containing structural units of crystals I and II are mononuclear anionic complexes of the composition [UO₂(CrO₄)₄]⁶⁻ with an island structure, which belong to the crystal-chemical group Am ₁⁴ (A = UO₂₊², M ¹ = CrO₂₋⁴) of the uranyl complexes. The [UO₂(CrO₄)₄]⁶⁻ anionic complexes are joined into a three-dimensional framework through the electrostatic interactions with outer-sphere cations and a system of hydrogen bonds. Original Russian Text ? L.B. Serezhkina, E.V. Peresypkina, A.V. Virovets, A.G. Verevkin, D.V. Pushkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 2, pp. 284–290.     

Sandwich-Type Manganese-Substituted Polyoxometalate, [(α-B-ZnW9O34)2W2Mn2(H2O)2]8?

Abstract  

The novel dimeric manganese-substituted polyoxotungstate Na₁₀[(α-B-ZnW₉O₃₄)₂W₂Mn₂(H₂O)₂](OH)₂·34H₂O (1) has been designed and synthesized from the hydrothermal reaction of Na₂WO₄·2H₂O, MnCl₂·4H₂O, and ZnCl₂ in a Teflon-lined stainless steel autoclave at 140°. X-ray diffraction analysis results reveal that compound (1) crystallizes in the monoclinic system, space group P2(1)/n, with a = 13.0901(3) ?, b = 17.8242(4) ?, c = 21.2401(5) ?, β = 93.6380(10)°, Z = 1, V = 4945.8(2) ?³, F(000) = 5244, Dc = 3.974 g/cm⁻³, μ(Mo-Kα) = 2.4037 cm⁻¹, λ(Mo-Kα) = 0.71073 ?. The structure was refined to R = 0.0631 and wR = 0.1532. The polyoxoanion of [(α-B-ZnW₉O₃₄)₂W₂Mn₂(H₂O)₂]⁸⁻ consist of two Keggin lacunary α-B-ZnW₉O₃₄ ¹²⁻ moieties linked via a rhomblike W₂Mn₂O₁₆ group leading to a sandwich-type structure.     

Synthesis and Crystal Structure of Bis(μ3-4-Oxapentan-2-onato)-Tetrakis(μ2-4-Oxapentan-2-onato)-Tetra-Magnesium Dichloride Dichloromethane

Abstract  

A new magnesium alkoxide which posses centrosymmetric tetranuclear structure derived from 1-methoxy-2-propanol, a functionalized alcohol containing asymmetric carbon. X-ray analysis of single crystal shows an open dicubane-like structure with triple-bridging alkoxo groups between alternating five- and six-coordinated magnesium atoms. There are six alkoxo bridging groups in which two of them bridge three metal centers and the other four bridge two. All of the etheric-oxygens are coordinated to magnesium and provide a rigid structure. Two chlorine atoms are bonded to five-coordinated magnesium. This compound crystallizes in the monoclinic system with a = 10.040(6) Ǻ, b = 14.004(9) Ǻ, c = 15.344(5) Ǻ, β = 95.55(9)˚, Z = 2 and V = 2147 Ǻ³ in the space group of P2₁/n.     

Synthesis and Structure of a Silver(I) Complex {[Ag5(L)2(NO3)4](NO3)(CHCl3)2}n [L?=?2,3-bis(pyrimidine-2-thiomethyl)quinoxaline]

Abstract  The reaction of the dithioether ligand, 2,3-bis(pyrimidine-2-thiomethyl)quinoxaline (L) with AgNO₃, leads to the formation of a novel complex {[Ag₅(L)₂(NO₃)₄](NO₃)(CHCl₃)₂}n 1, which has been characterized by single-crystal X-ray diffraction analysis: monoclinic, space group C2/c, with a = 34.741(7), b = 9.930(2), c = 17.004(4) ?, β = 106.497(6)° and V = 5625(2) ?³.Complex 1 consists of 2D {[Ag₅(L)₂(NO₃)₄]⁺}n cations, uncoordinated anions and CHCl₃ solvent molecules. In 1, there exist three crystallographic independent Ag^I centers, which adopt different coordination geometries. There exist π–π stacking interactions in the complex and these weak interactions further stabilize the crystal structure in the solid state. The coordination feature of the ligand has been investigated by DFT calculations. Index Abstract  Synthesis and Structure of a Silver(I) Complex {[Ag₅(L)₂(NO₃)₄](NO₃)(CHCl₃)₂}_n [L = 2,3-bis(pyrimidine-2-thiomethyl)quinoxaline] Chao-Yan Zhang, Qian Gao, Ya-Bo Xie*, and Jian-Bo Feng The crystal structure of complex {[Ag₅(L)₂(NO₃)₄](NO₃)(CHCl₃)₂}n (L = 2,3-bis(pyrimidine-2-thiomethyl)quinoxaline) consists of 2D {[Ag₅(L)₂(NO₃)₄]⁺}n cations, uncoordinated anions and CHCl₃ solvent molecules. There exist three crystallographic independent Ag^I centers, which adopt different coordination geometries. The coordination feature of the ligand has been investigated by DFT calculations.