Complexing and ion selective properties of some acid type phosphoryl podands. The crystal and molecular structures of 1,5-bis(2-dihydroxyphosphoryl-4-ethylphenoxy)-3-oxapentane dihydrate [(HO)2(O)P(C6H3CH2CH3)(OCH2CH2)2O (C6H3CH2CH3)P(O)(OH)2] · 2H2O

The synthesis of 1,5-bis(2-dihydroxyphosphoryl-4-ethylphenoxy)-3-oxapentane [(HO)₂(O)P(C₆H₃CH₂CH₃)(OCH₂CH₂)₂O(C₆H₃CH₂CH₃)P(O)(OH)₂] (H₄K²) and single crystal X-ray diffraction study of H₄K² · 2H₂O (I) are described. The crystals are orthorhombic, a = 33.291(4) Å, b = 8.9374(10) Å, c = 8.1021(9) Å, V = 2410.6(5) ų, Z = 4, space group Cmc2₁, R = 0.0484 for 2566 reflections with I > 2σ(I). In I, the molecules of H₄K² are hydrogen-bonded to two crystallographically independent H₂O molecules to give neutral conglomerates H₄K² · 2H₂O. The electroanalytical characteristics of poly(vinyl chloride) membranes based on H₄K² were tested. Cu²⁺ and Zn²⁺ complexes with H₄K² and Er³⁺, Nd³⁺, and complexes with H₄K², 1,5-bis[2-(dihydroxyphosphoryl-4-methoxy)phenoxy]-3-oxapentane, 1,5-bis[2-(dihydroxyphosphinyl)phenoxy]-3-oxapentane, and 1,8-bis[2-(dihydroxyphosphinyl)phenoxy]-3,6-dioxaoctane were prepared.     

Syntheses and Crystal Structures of (H3O)(C3H5N2)[Mn(OH)6 Mo6O18]·3.5H2O and (H3O)3[Co(OH)6Mo6O18]·7H2O

The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]·3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]·7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 21.5018(9), b = 10.9331(5), c = 11.8667(5)A,β = 95.3570(10)o, V = 2777.5(2)A3, Z = 4, Dc = 2.802 g/cm3, Mr = 1171.80,μ(MoKα) = 3.173 mm-1, F(000) = 223, the final R = 0.0458 and wR = 0.1041 for 2093 observed reflections (I>2σ(I)); Compound 2 crystallizes in monoclinic, space group P21/c with a = 11.4042(12), b = 10.9481(11), c = 11.6722(12)A, β= 99.948(2)o, V = 1435.4(3)A3, Z = 2, Dc = 2.794 g/cm3, Mr = 1207.80,μ(MoKα) = 3.223 mm-1, F(000) = 1160, the final R = 0.0544 and wR = 0.1066 for 1906 observed reflections (I > 2σ(I)). Both compounds 1 and 2 adopt the Anderson structure, in which the anion is of centrosymmetry and formed by six octahedral edge-sharing MoO6 units surrounding the central MO6 (M = Mn or Co) octahedron.     

Crystal structure of Na6[(UO2)3O(OH)3(SeO4)2]2 · 10H2O

The complex Na₆[(UO₂)₃O(OH)₃(SeO₄)₂]₂ · 10H₂O (I) is synthesized and studied by X-ray diffraction. The compound crystallizes in the orthorhombic crystal system with the unit cell parameters: a = 14.2225(7) Å, b = 18.3601(7) Å, c = 16.5406(6) Å, V = 4319.2(3) ų, Z = 4, space group Cmcm, R ₁ = 0.0406. Compound I is found to be a representative of the crystal-chemical group A₃M³M² ₃T³ ₂ (A = UO²⁺ ₂, M³ = O^2?, M² = OH^?, T³ = SeO^2? ₄) of the uranyl complexes; it contains layer uranium-containing groups [(UO₂)₃O(OH)₃(SeO₄)₂]^3?. These layers linked to form a three-dimensional cage through bonds formed by the sodium atoms with the oxygen atoms of the uranyl ions and SeO₄ groups that belong to different layers.     

New 1D and 2D metal oxygen connectivities in Cu(II) succinato and glutarato coordination polymers: [Cu3(H2O)2(OH)2(C4H4O4)2] · 4H2O, [Cu4(H2O)2(OH)4(C4H4O4)2] · 5H2O and [Cu5(OH)6(C5H6O4)2] · 4H2O

Two Cu(II) hydroxo succinates [Cu₃(H₂O)₂(OH)₂(C₄H₄O₄)₂]?·?4H₂O (1) and [Cu₄(H₂O)₂(OH)₄(C₄H₄O₄)₂]?·?5H₂O (2) and one Cu(II) hydroxo glutarate [Cu₅(OH)₆(C₅H₆O₄)₂]?·?4H₂O (3) have been prepared and structurally characterized by single crystal X-ray diffraction methods. They feature 1D and 2D copper oxygen connectivity of elongated {CuO₆} octahedra in “4?+?1?+?1” and “4?+?2” coordination geometries. Within 1, linear trimers of three edge-sharing {CuO₆} octahedra are connected into copper oxygen chains, which are bridged by the anti conformational succinate anions to generate 2D layers with mono terminally coordinating gauche succinate anions on both sides. The layers are assembled into a 3D framework by interlayer hydrogen bonds with lattice H₂O molecules distributed in channels. Different from 1, the principal building units in 2 are linear tetramers of four edge-sharing {CuO₆} octahedra. The tetramers are condensed into copper oxygen chains and the succinate anions interlink them into a 3D framework with triangular channels filled by lattice H₂O molecules. The {CuO₆} octahedra in 3 are edge-shared to form unprecedented 2D inorganic layers with mono terminally coordinating glutarate anions on both sides. Interlayer hydrogen bonding interactions are responsible for supramolecular assembly of the layers into a 3D framework with lattice H₂O molecules in the channels. The inorganic layers in 3 can be described as hexagonal close packing of oxygen atoms with the Cu atoms in the octahedral cavities. The title compounds were further characterized by elemental analyses, IR spectra and thermal analyses.     

Synthesis and crystal structure of Cs2[(UO2)2(C2O4)3] and Cs2[UO2(C3H2O4)2] · H2O

Cs₂[(UO₂)₂(C₂O₄)₃] (I) and Cs₂[UO₂(C₃H₂O₄)₂] · H₂O (II) have been synthesized and studied by X-ray diffraction. The crystals of complexes I and II are monoclinic: a = 8.1453(2) Å, b = 8.9831(2) Å, c = 11.3897(4) Å, β = 104.0950(10)°, V = 808.29(4) ų, space group P2₁/n, Z = 2, and R ₁ = 0.0255 for I and a = 9.6998(2) Å, b = 17.8686(3) Å, c = 8.2074(2) Å, β = 97.5780(10)°, V = 1410.10(5) ų, space group P2₁/c, Z = 4, and R ₁ = 0.0287 for II. The uranium-containing structural units of complexes I and II are [(UO₂)₂(C₂O₄)₃]^2? chains and [UO₂(C₃H₂O₄)₂] ₂ ^4? dimers, which belong to the AK _0.5 ⁰² T¹¹ and AT¹¹B⁰¹ crystallochemical groups (A = UO ₂ ²⁺ , K⁰² and T¹¹ = C₂O ₄ ^2? , T¹¹ and B⁰¹ = C₃H₂O ₄ ^2? ) of uranyl complexes.     

Syntheses and crystal structures of two Cd(II) coordination polymers: one-dimensional chain [Cd(C4H6N2)2(C4H2O4)(H2O)2] n and two-dimensional sheet [Cd(C4H6N2)(H2O)(C4H4O4)] n · n H2O

Two new Cd(II) coordination polymers, [Cd(C₄H₆N₂)₂(C₄H₂O₄)(H₂O)₂] _n (1) (where C₄H₆N₂?=?2-methylimidazole, C₄H₂O₄?=?fumarate), and [Cd(C₄H₆N₂)(H₂O)(C₄H₄O₄)] _n ?·?nH₂O (2), (where C₄H₄O₄?=?succinates), have been prepared and structurally characterized by single crystal X-ray diffraction. Complex 1 crystallizes in the triclinic space group P 1 in a one-dimensional chain structure, in which carboxy is monodentate; a three-dimensional supermolecular network structure was formed through hydrogen bonding. In complex 2, the coordination geometry of the Cd atoms is a pentagonal bipyramid, and a two-dimensional sheet is formed though carboxyl group bridging. In 1 and 2, IR spectra indicate the presence of bridging carboxyl groups, confirmed by structure analyses.     

Synthesis,structure, and properties of a new trinuclear iron cluster, [(MeOH)(H2O)2Fe3(μ3-O)(μ-OOCC6H4OCH2C5H4NH)6] (ClO4)7 · · 8MeOH · 3.5H2O

Reactions of iron(m) salts with a new bidentate ligand, which is potentially capable of forming binuclear iron complexes upon complexation, were studied. Under various conditions, we succeeded in isolating only the trinuclear cationic complex (Fe^III ₃(O₂CR)6(₃-)17+ (1), where RCO₂ is 2-(pyrid-2-ylmethoxy)benzoic acid protonated at the pyridyl moiety. The structure of 1 was established by spectral, magnetic, and X-ray structural studies. Cyclic voltammetry in McCN in the temperature range from -35 to 20 °C demonstrated that 1 undergoes successive Fe^IIIFe^II reduction in three one-electron stages, which is indicative of the electronic interaction between iron atoms in the complex.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 2086–2092, August, 1996.     

Magnetic Properties of (C5H6N)5[Fe13O4F24(OCH3)12] · CH3OH · 4H2O

The static magnetic susceptibility of Fe(III) complex [Fe₁₃O₄F₂₄(OCH₃)₁₂]^5– was measured in the temperature range 2–300 K. The structure of the complex consists of four triangular Fe₃ fragments interacting with a central Fe atom. By disregarding weak exchange interactions through F bridges, an analytical solution of the exchange Hamiltonian was obtained with Nf 1.3 × 10¹⁰ levels. This made it possible to perform quantitative interpretation of the temperature dependence of the magnetic susceptibility. The obtained exchange parameters of the best approximation are –2J ₁ = 43 cm^–1, –2J ₂ 30 cm^–1. The ratio J ₂/J ₁ 0.70 suggests that the Fe₁₃ ground state has the spin of the ground state 23/2 or 15/2.     

Synthesis and crystal structure of [UO2(L)(OH)], (CN3H6)2[(UO2)2CrO4(L)4 · 2H2O and [UO2(H2O)5][(UO2)2Cr2O7(L)4] (where L is picolinate ion)

[[UO₂(L)(OH)] (I), (CN₃H₆)₂[(UO₂)₂CrO₄(L)₄] · 2H₂O (II), and [UO₂(H₂O)₅][(UO₂)₂Cr₂O₇(L)₄] (III) crystals, where L is picolinate ion C₅H₄NCOO^?, have been synthesized and studied by X-ray diffraction and IR spectroscopy. Complex I crystallizes in triclinic system with the unit cell parameters a = 6.2858(5) Å, b = 7.9522(5) Å, c = 8.3598(6) Å, α = 79.527(6)°, β = 87.760(6)°, γ = 79.126(6)°, space group P $\bar 1$ , Z = 2, R = 0.0306, and complexes II and III crystalize in monoclinic system with a = 8.8630(9) Å, b = 13.4540(13) Å, c = 31.266(3) Å, β = 93.118(3)°, space group C2/c, Z = 4, R = 0.0187 (II), and a = 7.3172(4) Å, b = 15.4719(8) Å, c = 16.6534(10) Å, β = 98.943(4)°, space group P2₁/m, Z = 2, R = 0.0588 (III). The structure of complex I is built of electronegative [UO₂(L)(OH)] chains, which belong to the AT¹¹M² crystallochemical group (A = UO ₂ ²⁺ , T¹¹ = L, M² = OH^?) of uranyl complexes. The structure of complexes II and III contains [(UO₂)₂(L′)(L)₄]^2? dimers (L′ = CrO ₄ ^2? or Cr₂O ₇ ^2? ), which belong to the A₂B²B ₄ ⁰¹ group (A = UO ₂ ²⁺ ,B² = L′, B⁰¹ = L). The specifics of intermolecular interactions in the structures of complexes I–III and some their analogues have been considered using molecular Voronoi-Dirichlet polyhedra.     

Synthesis, crystal structure, and IR spectral study of Na[(UO2)(C3H7COO)3] · 0.25H2O and K[(UO2)(C3H7COO)3]

Synthesis, IR spectral study and X-ray diffraction analysis of single crystals of Na[(UO₂)(C₃H₇COO)₃] · 0.25H₂O (I) and K[(UO₂)(C₃H₇COO)₃] (II) were carried out. Compound I is monoclinic, unit cell parameters are: a = 13.5671(15) ?, b = 20.070(2) ?, c = 13.6139(15) ?, ?? = 106.839(2)°, space group P2₁, Z = 8, R = 0.0493. Compound II is orthorhombic, unit cell parameters are: a = 17.1325(9) ?, b = 19.6966(11) ?, c = 21.9686(11) ?, space group P2₁2₁2₁, Z = 16, R = 0.0563. Mononuclear groups [UO₂(C₃H₇COO)₃]^? related to the A ₃ ⁰¹ crystal-chemical group (A = UO ₂ ²⁺ , B ⁰¹ = C₃H₇COO^?) of uranyl complexes are the uranium-containing structural units of crystals I and II. The data of IR spectral study agree well with X-ray diffraction data.     

Crystal and Molecular Structure of Guanidinium Pentamolybdobis (n-amylphosphonate)(CN3H6)4[(n-C5H11P)2Mo5O21]

The crystal structure of guanidinlum pentamolybdobis(n-ainylphcsphonate), which contains the longest carbon chain hitherto known, was determined by single-crystal X-ray diffraction analysis. It belongs to monoclinic, space group C2/c, Z = 4, 0=18.857(2), b=12.170(1), c=18. 294(2) A .β=102.73 (2), V=4095. 2A3.u= 140. 34 cm-1. The intensity data were collected on an Enraf-Nonius CAD4 diffractometer with MoKa radiation. The positions of all molybdenum and phosphorus atoms were determined by the direct method. The other non-hydrogen atoms were revealed by difference Fourier synthesis. The structure was refined by full-matrix least-squares procedure to a final R value of 0. 068. The structure of the anion is similar to [(CH2P)2Mo5O21]4-, [(NH3C2H4P)2Mo6O21]2-, [(n-C3H7As)2Mo5O21]--, and [(C3H5As)2Mo6O21]4-. It consists of a ring of five distorted MoO, octahedra joined by edge-sharing, except for one pair which is joined by corner- sharing. The size of the Mo6O16 ring is close to those of [(CH3P)2Mo5O21]4- a     

Crystal structure of [Pt3S2(P(CH2OH)3)6](PF6)(OH)·H2O

[Pt₃S₂(P(CH₂OH)₃)₆](PF₆)(OH)·H₂O (1) is obtained by a reaction of [Pt₃S₂(P(CH₂OH)₃)₆]Cl₂ with NH₄PF₆. The crystal structure of 1 was determined by a single crystal X-ray diffraction analysis (space group R{ie638-1}c, a = 12.0042(2) Å, c = 52.6879(11) Å, V = 6575.2(2), Z = 6, C₁₈H₅₇F₆O₂₀P₇Pt₃S₂, d _x = 2.385 g/cm³, T = 150 K, R ₁ = 0.044 for 2123 F ₀ > 4δ(F) until 2θ_max = 63°). The cations contain a {Pt₃(μ₃-S)₂}²⁺ core with nonbonding Pt…Pt distances of 3.1536(6) Å. The Pt atoms are in a square planar environment; the Pt-S and Pt-P bond lengths are 2.3586(16) Å and 2.260(2) Å respectively.     

Methyl Propiolate Cluster Complex (Ph4P)2[W6I8(C≡C–C(O)OCH3)6]

Russian Journal of Coordination Chemistry - A new organometallic iodide cluster complex (Bu4N)2[W6I8(C≡C–C(O)OCH3)6] (I), analogous to the previously described...     

Synthesis and X-ray diffraction study of K4[(UO2)2(C2O4)3(NCS)2] · 4H2O

Single crystals of K₄[(UO₂)₂(C₂O₄)₃(NCS)₂] · 4H₂O(I) have been synthesized and studied by X-ray diffraction. The crystals are monoclinic with the unit cell parameters a = 8.0226(7) Å, b = 14.9493(11) Å, c = 11.1670(9) Å, β = 98.299(3)°, space group P2₁/n, Z = 2, V = 1325.26(19) ų, R = 0.0186. The main structural units of the crystals of structure I are discrete binuclear groups [(UO₂)₂(C₂O₄)₃(NCS)₂]^4? belonging to the crystal-chemical group A₂K⁰²B ₂ ⁰¹ M ₂ ¹ (A =UO ₂ ²⁺ , K⁰² =C₂O ₄ ^2? , B⁰¹ =C₂O ₄ ^2? , M¹ = NCS^?) of the uranyl complexes. The uranium-containing complexes are linked into a three-dimensional framework through the potassium ions and a system of hydrogen bonds involving the outer-sphere water molecules.     

Tetranuclear bismuth complexes Bi4(O)2(O2CC6H2F3-3,4,5)8 · 2C6H6 and Bi4(O)2(O2CC6H2F3-3,4,5)8 · 2C6H4Me2-1,4: Synthesis and structures

X-ray diffraction study of tetranuclear organobismuth complexes Bi₄(O)₂(O₂CC₆H₂F₃-3,4,5)₈ · 2⁶-C₆H₆ and Bi₄(O)₂(O₂CC₆H₂F₃-3,4,5)₈ · 2(C₆H₄Me₂-1,4) revealed four Bi atoms connected through the bridging carboxylate ligands and the O atoms. The coordination sphere of the terminal Bi atoms includes the chelate carboxylate ligand and the 6-arene molecule. The bridging O atoms are tricoordinated, the distances between the terminal Bi atom and the center of benzene molecule (1,4-dimethylbenzene) are 3.024 Å(3.131 Å).Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 1, 2005, pp. 4–11.Original Russian Text Copyright © 2005 by Sharutin, Egorova, Sharutina, Ivanenko, Adonin, Starichenko, Pushilin, Gerasimenko.     

Synthesis and Structure of Antimony Complex Compounds [(4-N,N-Me2C6H4)3MeSb]I and [(4-N,N-Me2C6H4)3MeSb]2[Hg2I6]·2DMSO

Russian Journal of General Chemistry - It was first found that the alkylation of tris(4-N,N-dimethylaminophenyl)stibine with methyliodide leads to the formation of...     

新型杂多化合物[(CH3CH2)4N]4H3O· {Na[(HMo2O5)3(HPO4)(H2PO4)3]2}·(H2PO4)2·10H2O的水热合成与晶体结构

杂多化合物在催化、医药、材料及光化学等方面具有广泛的应用前景 [1～ 4 ] ,其中钼磷多金属氧酸盐具有优异的氧化催化性能 [5,6 ] .近年来合成的新奇结构的钼磷多金属氧酸盐中已测定结构的有含帽[7,8] 和非帽[9～ 12 ] 系列 .本文利用水热法合成了未见文献报道的结构新颖的夹心型磷钼多金属氧酸盐[( CH3CH2 ) 4N]4 H3O{Na[( HMo2 O5) 3( HPO4 ) ( H2 PO4 ) 3]2 }· ( H2 PO4 ) 2 · 1 0 H2 O,并测定了其晶体结构 .1　实验与晶体结构分析1 .1　仪器与试剂　元素 Na用美国原子吸收分光光度计测定 ;C,H和 N用 Perkin- Elmer 2 4 0…     

[Ba(18-冠-6)(H2O)(OH)][Fe(NCS)4]的分子和晶体结构

本文用凝胶法培养出18-冠-6钡和硫氰酸铁的配合物单晶, 并用X射线衍射分析了其晶体和分子结构.     

Syntheses and Structures of the Hexacoordinated Antimony Complexes: Ph3(C2H4O2)Sb⋅⋅⋅DMSO, (3-FC6H4)3(C2H4O2)Sb⋅⋅⋅DMSO,and (4-MeC6H4)3(C6H4O2)Sb⋅⋅⋅DMSO

Russian Journal of Coordination Chemistry - Complexes Ph3(C2H4O2)Sb???DMSO (I), (3-FC6H4)3(C2H4O2)Sb???DMSO (II), and...     

Synthesis and structure assignment of vanadyl(iv) citrate [(VO)3(C6H5O7)2]·H2O

Pseudo-crystals of vanadyl(iv) citrate [(VO)₃(C₆H₅O₇)₂]·H₂O have been obtained after addition of V₂O₅ to citric acid solution. Composition of the compound has been established by thermal analysis and confirmed by IR, UV-VIS, Raman and ESR spectra.