Synthesis and structure of tin tetrachloride adducts with crown ether: Crystal structure of [Sn(H2O)2Cl4] · 18C6 and [Sn(H2O)2Cl4] · 18C6 · 2H2O

Tin coordination compounds [Sn(H₂O)₂Cl₄] · 18C6 (I) and [Sn(H₂O)₂Cl₄] · 18C6 · 2H₂O (II) were synthesized and identified by IR spectroscopy, CH analysis, and X-ray powder diffraction. The crystal structures of compounds I and II were determined. The crystals of I and II are orthorhombic; a = 16.871(1) ?, b = 7.7305(7) ?, c = 16.939(1) ?, Z = 4, space group Cmca for I; a = 14.206(2) ?, b = 20.376(3) ?, c = 8.319(1) A, Z = 4, space group Pna21 for II. The structural units of I and II are [Sn(H₂O)₂Cl₄] · 18C6 complex molecules (in II, also water molecules of crystallization). The coordinated water molecules in I are trans and those in II are cis to each other. The structural units in the crystals of I and II are combined only by hydrogen bonds between water molecules and the crown-ether oxygen atoms with the formation of the chain structure. Complex I was tested as the precursor of tin dioxide in a chemical vapor deposition (CVD) process. The morphology of the obtained film was studied by atomic force microscopy (AFM) and scanning electron microscopy (SEM), and the composition was studied by laser mass spectrometry for elemental analysis.     

Isomerization of [In(H2O)3Cl3] · 18C6. Crystal structure of [ mer -In(H2O)3Cl3] · 18C6 and [ fac -In(H2O)3Cl3] · 18C6 · 2H2O

The complex [mer-In(H₂O)₃Cl₃] · 18C6 (I) was isolated from the InCl₃-H₂O-Solv-18C6 solutions (Solv = MeOH, EtOH, THF). The second crystallization from mother solutions resulted in [fac-In(H₂O)₃Cl₃] · 18C6 · 2H₂O (II). The crystal and molecular structures of isomers I, II were identified by the powder X-ray diffraction, IR, and X-ray diffraction methods. Although complexes I, II have different compositions, they have the chain structure. The thermal decomposition of complexes I, II was studied. Original Russian Text ? A.B. Ilykhin, Zh.V. Dobrokhotova, S.P. Petrosyants, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 9, pp. 651–656.     

Crystal structure of [Pd(NH3)4]3[Ir(NO2)6]2·H2O

A single crystal of [Pd(NH₃)₄]₃[Ir(NO₂)₆]₂·H₂O double complex salt is studied by X-ray diffraction. Crystallographic characteristics are as follows: a = 21.0335(5) ?, b = 8.0592(2) ?, c = 21.3452(5) ?, β = 91.254(1)°, V = 3617.43(15) ?³, P2₁/c space group, Z = 4, d _x = 2.714 g/cm³. Single-layer pseudohexagonal packing of complex anions is determined along the [−1 0 1] direction in the structure. Complex cations and crystallization water molecules are located between the mentioned layers.     

Synthesis, structure, and thermal decomposition of [H2(4,4′-Bipy)][In(H2O)2(NCS)4]2 and [HUr]2[In(H2O)(NCS)5] · 2H2O

The reaction of indium thiocyanate with bipyridine (4,4-Bipy) and urotropine (Ur) gave [H₂(4,4′-Bipy)][In(H₂O)₂(NCS)₄]₂ (I) and [HUr]₂[In(H₂O)(NCS)₅] · 2H₂O (II), which were identified using elemental analysis, IR spectra, and thermogravimetric analysis. The thermal decomposition of compound I and II ends at 650 and 640°C, respectively, and gives In₂O₃. X-Ray diffraction analysis of compound I showed that complex anions in the crystal form chains through O-H…S hydrogen bonds. The anion chains form a close packing of columns with bipyridine cations located in the voids. Original Russian Text ? S.P. Petrosyants, A.B. Ilyukhin, V.A. Ketsko, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 6, pp. 951–955.     

Structural determination of new eight-coordinate NH4[EuIII(Cydta)(H2O)2]·4.5H2O and K2[Eu 2III (pdta)2(H2O)2]·6H2O complexes

The NH₄[Eu^III(Cydta)(H₂O)₂]·4.5H₂O (I) (H₄Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid) and K₂[Eu₂^III(pdta)₂(H₂O)₂]·6H₂O (II) (H₄pdta = propylenediamine-N,N,N′,N′-tetraacetic acid) complexes are prepared by heat-refluxing and acidity-adjusting methods respectively, and their composition and structures are determined by elemental analyses and single crystal X-ray diffraction techniques. The complex I has a mononuclear structure, crystallizes in the triclinic crystal system with the P[`1]P\bar 1 space group; the central Eu^III ion is eight-coordinated by a hexadentate Cydta ligand and two water molecules. The crystal data are as follows: a = 8.653(4) ?, b = 10.041(4) ?, c = 14.405(6) ?, α = 88.469(6)°, β = 74.892(6)°, γ = 88.256(7)°, V = 1207.5(9) ?³, Z = 1, D _c = 1.731 g/cm³, μ = 2.669 mm⁻¹, F(000) = 638, R = 0.0257, and wR = 0.0667 for 3807 observed reflections with I ≥ 2σ(I). The EuN₂O₆ part in the [Eu^III(Cydta)(H₂O)₂]⁻ complex anion forms a pseudo-square antiprismatic polyhedron. The complex II is eight-coordinate as well; it is a binuclear structure that crystallizes in the monoclinic crystal system with the C ₂/c space group; half of the central Eu^III ion is coordinated by two nitrogen atoms from one hexadentate pdta ligand and six oxygen atoms from the same pdta ligand, one water molecule and carboxylic group from the neighboring pdta ligand respectively. The crystal data are as follows: a = 19.866(3) ?, b = 9.1017(12) ?, c = 21.010(3) ?, β = 104.972(2)°, V = 3670.1(9) ?³, Z = 8, D _c = 2.046 g/cm³, μ = 3.710 mm⁻¹, F(000) = 2240, R = 0.0213 and wR = 0.0460 for 4183 observed reflections with I ≥ 2σ(I). Otherwise, the two EuN₂O₆ parts in the [Eu₂^III(pdta)₂(H₂O)₂]²⁻ complex anion form a pseudo-square antiprismatic polyhedron.     

Crystal structures of barium bis(iminodiacetato)cobaltates(III): [Ba(H2O)6][Co(Ida)2]2 · H2O and Ba4(H2O)14][Co(Ida)2]5(ClO4)3 · 5.46H2O · 2CH3OH

The structures of the crystals of Ba₄[trans(N)-Co(Ida)₂]₃[cis-(N)-Co(Ida)₂]₂(ClO₄)₃ · 19.46H₂O · 2CH₃OH (I) and Ba[trans-(N)-Co(Ida)₂]₂ · 7H₂O (II) (H₂Ida is iminodiacetic acid) were determin by X-ray diffraction. The crystals of I containing two geometric isomers of the complex anions [Co(Ida)₂]⁻ were obtained by a slow cooling of a hot solution, which contained initially only the cis-isomer. One Ba atom in I interacts with the trans-complex and with two cis-complexes to give a three-dimensional framework in crystal I. The positive charge of the last framework is compensated by one more trans-complex and by the perchlorate ions, one of which acts as a bidentate ligand with respect to the Ba atom. The crystals of II are built of the chains with the alternating Ba atoms and the trans-(N)-[Co(Ida)₂]⁻ anions. The other anions of the same structure are each “suspended” to the Ba atoms of the chain. Original Russian Text ? M. Zabel, A.I. Poznyak, V.I. Pawlowskii, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 11, pp. 831–836.     

Crystal structures of the octahedral rhenium cluster compexes Cs4[Re6S8(OH)6]·6H2O and Cs4[Re6Se8(OH)6]·8H2O

The salts Cs₄[Re₆S₈(OH)₆]·6H₂O (1) and Cs₄[Re₆Se₈(OH)₆]·8H₂O (2) were obtained by the reactions of Re₆S₈Br₂ and Re₆Se₈Br₂ with a CsOH melt with further solution of the products in water and crystallization of 1 and 2 from the aqueous solutions. The structure of the compounds was established by X-ray single crystal diffraction analysis. Compound 1 crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 14.175(2) Å, b = 11.321(2) Å, c = 17.503(2) Å, V = 2808.5(7) ų, Z = 4, d _calc = 5.003 g/cm³; compound 2 crystallizes in the triclinic space group with unit cell parameters a = 9.020(4) Å, b = 9.127(4) Å, c = 10.289(4) Å, α = 79.589(7)°, β = 75.829(7)°, γ = 72.186(7)°, V = 776.8(6) ų, Z = 1, d _calc = 5.402 g/cm³. Original Russian Text Copyright ? 2007 by K. A. Brylev, Yu. V. Mironov, S.-J. Kim, and V. E. Fedorov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 6, pp. 1183–1188, November–December, 2007.     

Synthesis, thermogravimetric analysis, IR spectrum, and the crystal structure of sodium hexatunstomanganate [Na2(H2O)10][Na(H2O)3]2[MnW6O18(OH)6] · 6H2O

The complex [Na₂(H₂O)₁₀][Na(H₂O)₃]₂[MnW₆O₁₈(OH)₆] · 6H₂O was synthesized and studied by mass spectrometry, thermogravimetry, IR spectroscopy, X-ray diffraction. The crystals are monoclinic, space group P2₁/n, a = 11.698(2), b = 11.670(2), c = 14.652(3) ?, β = 102.52(3)°, V = 1952.7(7) ?³, ρ(calcd.)= 3.45 g/cm³, Z = 2.     

[Gd2(Gly)6(H2O)4](ClO4)6(H2O)5的合成、晶体结构与热化学研究

利用微波技术合成了配合物[Gd₂(Gly)₆(H₂O)₄](ClO₄)₆(H₂O)₅, 进行了化学成分分析、红外表征和热重分析. 应用X衍射仪测定其晶体结构, 该晶体为一维链结构, 属三斜晶系, P 空间群, 晶胞参数: a＝1.1569(17) nm, b＝1.4138(2) nm, c＝1.5642(2) nm, α＝96.910(2)°, β＝102.735(2)°, γ＝105.512(2)°, V＝2.3606(6) nm³, Z＝2, D_c＝2.144 g•cm^－3. 采用精密溶解-反应量热计, 通过设计热化学循环, 计算出了该配合物的标准摩尔生成焓为 －(7960.73±3.23) kJ•mol^－1.     

Synthesis and crystal structure of the octahedral cyano-bridged cluster complex β-[{Ni(NH3)5}2{Re6Te8(CN)6}]·4H2O

The rhenium cyano-bridged cluster complex with a composition of β-[{Ni(NH₃)₅}₂{Re₆Te₈(CN)₆}]−4H₂O is obtained and structurally characterized. The compound pound crystallizes in the P $ P\bar 1 $ P\bar 1 triclinic space group with the unit cell parameters: a = 9.997(2) ?, b = 10.423(2) ?, c = 11.714(2) ?, α = 100.92(3)°, β = 111.87(3)°, γ = 98.05(3)°, V = 1082.1(4) ?³, Z = 1, d _calc = 4.072 g/cm³. The rhenium atoms of the {Re₆Te₈} cluster core are coordinated by CN ligands to form the [Re₆Te₈(CN)₆]⁴⁻ cluster; two nitrogen atoms of CN ligands trans-positioned with respect to each other are coordinated to Ni atoms in the {Ni(NH₃)₅}²⁺ fragments to form the molecular complexes of [{Ni(NH₃)₅}₂}Re₆Te₈(CN)₆}]. The crystal structure is the H-bonded packing of these molecular complexes and crystallization water molecules.     

A new organic-inorganic composite sandwich-type phosphotungstate: Synthesis, crystal structure and properties of [Ni(phen)3]2H6[Ni4(H2O)2(B-α-PW9O34)2] · 4H2O

A new organic-inorganic composite sandwich-type phosphotungstate [Ni(phen)₃]₂H₆[Ni₄(H₂O)₂(B-α-PW₉O₃₄)₂] · 4H₂O (I) (phen = 1,10-phenanthroline) has been synthesized by hydrothermal method and characterized by elemental analysis, IR spectrum, thermogravimetry (TG) analysis, X-ray photoelectron spectroscopy (XPS) and X-ray single crystal diffraction. The structural analysis indicates that each structure unit of the compound III consists of two isolated [Ni(phen)₃]²⁺ cations, six protons, one tetra-Ni^II-substituted sandwich-type [Ni₄(H₂O)₂(B-α-PW₉O₃₄)₂]¹⁰⁻ anion and four crystallization water molecules. In the compound III the cations and the polyanion were linked together through electrostatic interactions and intermolecular forces. XPS measurement indicates that the oxidation state of W and Ni atoms in the compound III are +6 and +2, respectively. TG analysis of the compound III shows two steps of weight loss.     

Syntheses of the eight-coordinate NH4[ErIII(Cydta)(H2O)2] · 4.5H2O and (NH4)2[Er 2III (Pdta)2(H2O)2] · 2H2O complexes and their structural investigation

In this work, the title complexes, NH₄[Er^III(Cydta)(H₂O)₂] · 4.5H₂O (I) (H₄Cydta = trans-1,2-cyclo-hexanediamine-N,N,N′,N′-tetraacetic acid) and (NH₄)₂[Er₂^III(Pdta)₂(H₂O)₂] · 2H₂O (II) (H₄Pdta= propylene-diamine-N,N,N′,N′-tetraacetic acid), were prepared, respectively, and their composition and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques. Complex I selects a mononu-clear structure with pseudosquare antiprismatic geometry crystallized in the triclinic crystal system with space group $ P\bar 1 $ P\bar 1 and the central Er³⁺ ion is eight-coordinated by the hexadentate Cydta ligand and two water molecules. The crystal data are as follows: a = 8.568(3), b = 10.024(3), c = 14.377(4) ?, α = 88.404(4)°, β = 75.411(4)°, γ = 88.332(4)°, V = 1194.2(6) ?³, Z = 1, ρ _c = 1.793 g/cm³, μ = 3.586 mm⁻¹, F(000) = 648, R = 0.0257, and wR = 0.0667 for 4169 observed reflections with I ≥ 2σ(I). Complex II is eight-coordinated as well, which selects a binuclear structure with two pseudosquare antiprismatic geometry and crystallizes in the monoclinic crystal system with space group P2₁/n. The central Er³⁺ ion is coordinated by two nitrogens and four oxygens from one hexadentate Pdta ligand. Besides, two oxygens come from one carboxylic group of the neighboring Pdta ligand and one water molecule, respectively. The crystal data are as follows: a = 12.7576(8), b = 9.3151(6), c = 14.3278(9) ?, β = 96.1380(10)°, V = 1692.93(19) ?³, Z = 4, ρ _c = 2.054 g/cm³, μ = 5.015 mm⁻¹, F(000) = 1028, R= 0.0228, and wR = 0.0534 for 2984 observed reflections with I ≥ 2σ(I).     

Crystal structure of K2[Mo3(PdPPh3)S4(C2O4)3(H2O)3]·0.5H2O

By the reaction of [Mo₃S₄(C₂O₄)₃(H₂O)₃]²⁻ with PdCl₂ and NH₄H₂PO₂ as a reducing agent, followed by the addition of PPh₃, a new oxalate cuboidal cluster complex [Mo₃(PdPPh₃)S₄(C₂O₄)₃(H₂O)₃]²⁻ is obtained. It was isolated and structurally characterized as K₂[Mo₃(PdPPh₃)S₄(C₂O₄)₃(H₂O)₃]·0.5H₂O. Original Russian Text Copyright ? 2008 by A. L. Gushchin, M. N. Sokolov, D. Yu. Naumov, and V. P. Fedin __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 4, pp. 775–778, May–June, 2008.     

X-ray structure of KCs[Pd(NO3)4]·0.5H2O

A new Pd nitrate complex KCs[Pd(NO₃)₄]·0.5H₂O is synthetized. Its crystal structure contains isolated complex anions [Pd(NO₃)₄]²⁻, cations K⁺, Cs⁺, and crystallization water. Square-planar coordination around Pd is achieved by oxygen atoms of monodentate nitrate ligands. The coordinated nitrate ligands are all oriented in the same way, in a “basket”-like arrangement. The coordination around Pd is completed to 4+1 by forming Pd...Pd contacts of 3.564 ?. Original Russian Text Copyright ? 2009 by S. P. Khranenko, I. A. Baidina, N. V. Kuratieva, and S. A. Gromilov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 173–176, January–February, 2009.     

Formation of Co nanoparticles in the process of thermal decomposition of the cobalt complex with hexamethylenetetramine (NO3)2Co(H2O)6(HMTA)2 · 4(H2O)

The thermal decomposition of the cobalt complex with hexamethylenetetramine (NO₃)₂Co(H₂O)₆(HMTA)₂ · 4(H₂O) was studied by the methods of differential thermal analysis, thermogravimetry, mass spectrometry, X-ray diffraction analysis, and by the magnetic method. It was established that the thermal decomposition of the complex in a current of an inert gas is accompanied by a pronounced exothermic process and formation of Co nanoparticles. It was shown that the kinetics of this process and the chemical nature of the decomposition products depend on the initial density of the sample under study.     

配合物Fe(pda)2(H2O)4和[FeCo(pda)4(H2O)4]n的合成与晶体结构

采用水热法合成了2个3-(3-吡啶基)丙烯酸的配合物:Fe(pda)2(H2O)4(1)和[FeCo(pda)4(H2O)4]n(2)(pda=3-(3-吡啶基)丙烯酸),用红外光谱、元素分析、热重-差热以及X-射线衍射单晶结构分析进行了表征.2个配合物都属于单斜晶系,配合物1的空间群为P21/n,配合物2的为P21/c.配合物1是一个pda配体中仅吡啶基氮原子参与配位、而羧基上的氧原子未参与配位的单核结构,通过大量的氢键作用形成三维超分子体系.2是pda配体桥联Fe和Co的异核二维层状配位聚合物;配体吡啶基上的氮原子和羧基上的氧原子都参与了配位,其中羧基采用单齿配位模式.     

[Bi2Cl10(H2-Norf)4(H2O)8](H-Norf是诺氟沙星)(英)

The crystal structure of [Bi2Cl10(H2-Norf)4(H2O)8] (1) comprises [H2-Norf]^ cations and [Bi2Cl10]4^- anions, that are loosely associated via H-bonding interactions, as well as water molecules that also participate in H-bonding interactions. Strong blue-fluorescent emission of 1 at solid state is observed at the room temperature. CCDC:238237.     

Crystal structure of a tetrahedral cluster complex [Zn2(NH3)6(μ-OH)][Zn(NH3)4]0.5[Re4Te4(CN)12]·5H2O

A cluster complex of the composition [Zn₂(NH₃)₆(μ-OH)][Zn(NH₃)₄]_0.5[Re₄Te₄(CN)₁₂]·5H₂O is obtained by the interaction of an aqueous solution of K₄[Re₄Te₄(CN)₁₂]·5H₂O with an aqueous ammonia solution of ZnCl₂. The compound crystallizes in the C2/m (12) monoclinic space group with unit cell parameters a = 23.233(2) ?, b = 14.5906(16) ?, c = 14.3825(15) ?, β = 125.169(1)°, V = 3985.5(7) ?³, Z = 4, d _x = 3.290 g/cm³. The structure is built from cluster [Re₄Te₄(CN)₁₂]⁴⁻ anions and complex [Zn₂(NH₃)₆(μ-OH)]³⁺ and [Zn(NH₃)₄]²⁺ cations; the latter is disordered over two positions.     

Synthesis and crystal structure of sodium isopolyvanadate [Na2(H2O)8]2H2[V10O28] · 4H2O

The sodium hydrogen oxovanadate [Na₂(H₂O)₈] ₂H₂[V₁₀O₂₈] · 4H₂O was synthesized and studied by TGA, X-ray diffraction, and NMR and IR spectroscopy. The crystals are triclinic, space group P $ \bar 1 $ \bar 1 , a = 8.545(7) ?, b = 10.827(2) ?, c = 11.627(2) ?, α = 105.48(3)°, β = 99.38(3)°, γ = 101.29(3)°, V = 989.9(3) ?³, ρ(calcd) = 2,381 g/cm³, Z= 1.     

Synthesis and structures of Cs4[(UO2)2(C2O4)(SO4)2(NCS)2] · 4H2O and (NH4)4[(UO2)2(C2O4)(SO4)2(NCS)2] · 6H2O

Single crystals of Cs₄[(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂] · 4H₂O (I) and (NH₄)₄[(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂] · 6H₂O (II) have been synthesized and studied by X-ray diffraction. The crystals of both compounds are orthorhombic with the space group Pbam, Z = 2, and unit cell parameters a = 12.0177(3) ?, b = 18.6182(5) ?, c = 6.7573(10) ?, R = 0.0376 (I); a = 11.6539(9) ?, b = 18.3791(13) ?, c = 6.7216(5) ?, R = 0.0179 (II). The main structural units of crystals I and II are [(UO₂)₂(C₂O₄)(SO₄)₂(NCS)₂]⁴⁻ chains belonging to the crystal-chemical group A₂K⁰²B₂²M₂¹ (A = UO₂²⁺, K⁰² = C₂O₄²⁻, B² = SO₄²⁻, M¹ = NCS⁻) of the uranyl complexes. The uranium-containing chains are joined into a three-dimensional framework due to a system of electrostatic interactions with the cesium or ammonium ions in the structure of I. In the structure of II, this framework is additionally stabilized by hydrogen bonds involving the outer-sphere water molecules and ammonium ions. Original Russian Text ? I.V. Medrish, A.V. Virovets, E.V. Peresypkina, L.B. Serezhkina, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 7, pp. 1115–1120.