Crystal structure of C17H20FN3O 32+ ·CuBr 42? ·H2O

A new compound C₁₇H₂₀FN₃O₃²⁺·CuBr₄²⁻·H₂O is synthesized in the crystal form, where C₁₇H₁₈FN₃O₃ (CfH, ciprofloxacin) is 4-oxo-7-(1-piperazinyl)-6-fluoro-1-cyclopropyl-1,4-dihydroquinoline-3-carboxylic acid. Crystallographic data of ciprofloxacinium tetrabromocuprate(II) monohydrate, C₁₇H₂₂Br₄CuFN₃O₄: a = 8.214(1) ?, b = 10.781(2) ?, c = 13.703(2) ?, α = 85.144(2)°, β = 79.119(2)°, γ = 84.018(2)°, V = 1182.5(4) ?³, P [`1]\bar 1 space group, Z = 2. Supramolecular architecture of the crystal differs from that established for C₁₇H₂₀FN₃O₃²⁺·CuCl₄²⁻·H₂O by the absence of π-π interactions of the aromatic rings of CfH₃²⁺ ions and also the structural motifs formed by intermolecular hydrogen bonds.     

Structure of the C17H20FN3O 32+ ·2HSO 4? · H2O compound

A new compound of C₁₇H₂₀FN₃O₃²⁺ · 2HSO₄⁻·H₂O [ciprofloxacindi-um bis(hydrosulfate) monohydrate], C₁₇H₁₈FN₃O₃ 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid (CfH, ciprofloxacin) is obtained and its crystal structure is determined. The crystal contains CfH₃²⁺ and HSO₄⁻ ions and crystallization water molecules. Hydrogen (H3), which forms an intramolecular hydrogen bond with oxygen O2 of the carboxyl group, is attached to the carbonyl O1 atom. Hydrogen H4 of the carboxyl group is hydrogen bonded to the crystallization water molecule which links CfH₃²⁺ with two HSO₄⁻ groups by hydrogen bonds. Both H atoms at N3 of the piperazine ring form hydrogen bonds with two oxygen atoms of other HSO₄⁻ anions. Intramolecular hydrogen bonds of two types are present in the CfH₃²⁺ cation. One of them forms a six-membered ring, bonding O1 and O2 atoms, while the other, also enclosing a six-membered ring, links fluorine and carbon C14 atoms. Original Russian Text Copyright ? 2009 by A. D. Vasiliev, N. N. Golovnev, and I. A. Baidina __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 165–168, January–February, 2009.     

Synthesis and structure of C17H22FN3O 32+ ?CuCl 42-

A new compound C₁₇H₂₂FN₃O₃ ²⁺ • CuCl₄ ^2- [pefloxacindium tetrachlorocuprate(II)], C₁₇H₂₀FN₃O₃ — 1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(4-methyl-1-piperazinyl)-3-quinoline carboxylic acid (pefloxacin, PefH) is synthesized and characterized by single crystal X-ray diffraction technique. The crystal structure of the compound contains one PefH₃ ²⁺ cation and one CuCl₄ ^2- anion. The supramolecular architecture of the crystal is determined.     

Crystal structure of pefloxancindium tetrabromidozinkate C17H22FN3O 32+ · ZnBr 42?

A new compound, namely pefloxancindium tetrabromidozincateC₁₇H₂₂FN₃O₃²⁺ · ZnBr₄²⁺ where C₁₇H₂₀FN₃O₃ is 1-ethyl-N-methyl-6-fluoro-1,4-dihydro-4-oxo-7-(4-methyl-1-piperazinyl)-3-quinoline carboxylic acid (PefH, pefloxacin), has been synthesized and its crystal and molecular structure has been solved. It contains PefH₃²⁺ and ZnBr₄²⁻ ions. The latter is a slightly distorted tetrahedron. The supramolecular architecture of a crystal has been analyzed.     

Molecular and crystal structures of [FeCl(HMPA)3(H2O)2]2+(FeCl4) 2? · 3HMPA

IR and single-crystal X-ray diffraction study are carried out for compound, C₃₆H₁₁₂Cl₉Fe₃N₁₈O₈P₆(I). It crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 14.2992(3), b = 21.4351(4), c = 25.5407(5) ?, V = 7828.3(3) ?³, ρ_calcd = 1.553 g/cm³, Z = 4. The FeCl fragment is coordinated with chlorine atom of two water molecules and three HMPA molecules to form a cation, with a distorted octahedral coordinate geometry. In the crystal I, the cation is linked with HMPA by the O-H…O hydrogen bond. The chiral crystal is formed through self-assembly even from achiral molecules.     

Ionophoretische Trennung von ReCl62?, ReBr62? und ReO4?

Zusammenfassung Es wurde die ionophoretische Trennung von ReCl₆ ^2–, ReBr₆ ^2– und ReO₄ ^– unter Verwendung verschiedener Papiersorten untersucht. Am geeignetsten erwies sich das Papier 2045 b Gl von Schl. & Sch.

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Summary The ionophoretic separation of ReCl₆ ^2–, ReBr₆ ^2–, and ReO₄ ^– has been examined using different kinds of paper. Best results have been obtained with the paper 2045 b Gl from Schleicher & Schüll.

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Herrn Prof. G. Brauer danke ich für Förderung. Für die Überlassung von Rheniumverbindungen bin ich der Fa. W. C. Heraeus, Hanau, verpflichtet. Die Neutronenaktivierung wurde freundlicherweise von den Herren Dr. Marth und Dr. Köhler von der Reaktorstation in Garching bei München vorgenommen. Das Bundesministerium für Atomkernenergie und Wasserwirtschaft unterstützte die Untersuchung durch eine Sachbeihilfe.     

Structure and thermal properties of [RhPy4Cl2]X complex salts (X = Cl?, ReO 4? , ClO 4? )

[RhPy₄Cl₂]Cl·4H₂O (I), [RhPy₄Cl₂]ReO₄ (II), [RhPy₄Cl₂]ClO₄ (III), and [RhPy₄Cl₂]ReO₄·2H₂O complex salts were synthesized. The crystal structure of compounds II (P4/ncc, a = 25.5655(3) ?, c = 14.3521(4) ?), III (P2₁/n, a = 13.5308(3) ?, b = 15.1044(5) ?, c = 23.3457(8) ?, β = 93.327°), and dyhydrate of II (Pbcm, a = 10.6199(9) ?, b = 10.4964(9) ?, c = 22.9834(16)?) was determined by X-ray diffraction analysis. The thermal transformations of the complexes were studied by differential thermal analysis. The substances were characterized by IR spectroscopy, XRPA, and element analysis Original Russian Text Copyright ? 2009 by D. B. Vasilchenko, I. A. Baidina, E. Yu. Filatov, and S. V. Korenev __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 349–356, March–April, 2009.     

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 levofloxacindium cadmium tetrabromide dihydrate C18H22FN3O 42+ ·[CdBr4]2?·2H2O

A new compound C₁₈H₂₂FN₃O₄²⁺·[CdBr₄]²⁻·2H₂O, C₁₈H₂₀FN₃O₄-levofloxacin (LevoH) is synthesized and its crystal and molecular structure is determined. Crystallographic data for levofloxacindi-um cadmium tetrabromide dihydrate C₁₈H₂₆CdBr₄FN₃O₆ are as follows: a = 8.3815(8) ?, b = 27.318(3) ?, c = 12.066(1) ?, β = 107.105(1)°, V = 2640.5(4) ?³, P2₁ space group, Z = 4. Hydrogen bonds form a branched threedimensional network linking LevoH₃²⁺, CdBr₄²⁻, and water molecules. The structure is also stabilized by the π-π interaction of LevoH₃²⁺ aromatic rings.     

Synthesis and structure of cobalt complexes [Me3EtN] 2+ [CoI4]2? and [Me3BuN] 2+ [CoI4]2?

Complexes [Me₃EtN]₂⁺[CoI₄]²⁻ (I) and [Me₃EtN]₂⁺[CoI₄]²⁻ (II) were synthesized by reacting trimethylalkylammonium iodide with cobalt(II) iodide in acetone. According to X-ray diffraction data, complexes I and II consist of tetrahedral tetraalkylammonium cations (for I, N-C is 1.481(5)–1.590(8) CNC is 107.3(3)°–111.6(3)°; for II, N-C is 1.485(8)–1.506(10) ? and CNC is 106.9(7)°–111.7(5)°) and [CoI₄]²⁻ anions (for I, Co-I is 2.5951(5)–2.6127(5) ? and ICoI is 104.67(2)°–113.23(2)°; for II, Co-I is 2.5914(8)–2.5943(9) ? and ICoI is 107.05(2)°–114.42(5)°).     

Complex salts trans-[Rh(β-Pic)4Cl2]X (X = Cl?, ReO 4? , and ClO 4? ): Synthesis, crystal structures, and thermal properties

Three novel complex salts containing the cation trans-[Rh(β-Pic)₄Cl₂]⁺ with the anions Cl⁻ (I), ReO₄⁻ (II), and ClO₄⁻ (III) were obtained and characterized by elemental analysis, X-ray diffraction, NMR spectroscopy, and IR spectroscopy. The complex trans-[Rh(β-Pic)₄Cl₂]ReO₄ crystallizes from DMF as a solvate in which solvent molecules fill the channels formed by the cations and anions. The thermal properties of complexes I, II, and II · DMF were examined by DTA. Final and some intermediate products of the thermolysis were isolated and characterized by physicochemical methods.     

Synthesis and structure of cobalt complexes [Ph3(n-Pr)P 2+ [CoI4]2? and [Ph3(n-Am)P 2+ [CoI4]2?

Complexes Ph₃(n-Pr)P₂⁺[CoI₄]²⁻ (I) and [Ph₃(n-Am)P]₂⁺ [CoI₄]²⁻ (II) were synthesized by reactions of triphenyl(alkyl)phosphonium iodide with cobalt(II) iodide in acetone. According to the X-ray diffraction data, complexes I and II consist of tetrahedral triphenyl(alkyl)phosphonium cations (for I, P-C is 1.787(4)–1.804(4) ? and CPC is 106.73(18)°–111.4(18)°; for II P-C is 1.786(6)–1.802(6) ? and CPC is 107.6(3)°–111.7(3)°) and [CoI₄]²⁻ anions (Co-I 2.5923(6)–2.6189(6) ?, ICoI 101.86(2)°–113.25(2)° for I; Co-I 2.5899(9)–2.6171(9) 107.01(3)°–110.47(3)° for II).     

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.     

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.     

Unusual ion UO4? formed upon collision induced dissociation of [UO2(NO3)3]?, [UO2(ClO4)3]?, [UO2(CH3COO)3]? ions

The following ions [UO₂(NO₃)₃]⁻, [UO₂(ClO₄)₃]⁻, [UO₂(CH₃COO)₃]⁻ were generated from respective salts (UO₂(NO₃)₂, UO₂(ClO₄)₃, UO₂(CH3COO)2) by laser desorption/ionization (LDI). Collision induced dissociation of the ions has led, among others, to the formation of UO₄ ⁻ ion (m/z 302). The undertaken quantum mechanical calculations showed this ion is most likely to possess square planar geometry as suggested by MP2 results or strongly deformed geometry in between tetrahedral and square planar as indicated by DFT results. Interestingly, geometrical parameters and analysis of electron density suggest it is an U^VI compound, in which oxygen atoms bear unpaired electron and negative charge.     

Phase formation in the ZrO(NO3)2-H3PO4-RbF-H2O system: the PO 43? /Zr = 0.5 section

We studied phase formation in the ZrO(NO₃)₂-H₃PO₄-RbF-H₂O system along PO₄³⁻/Zr = 0.5 (mol/mol) and RbF/Zr = 1–5 (mol/mol) sections with 2–10 wt % ZrO₂ in the starting solution. We recovered amorphous rubidium oxofluorophosphatozirconate Rb₂Zr₃OF₆(PO₄)₂ · 2H₂O and the following fluorophosphatonitratozirconates: Rb₂ZrF₄(PO₄)_0.33NO₃, which forms large cubic system crystals; weakly crystallized RbZr₃OF₃(PO₄)₂(NO₃)₂ · 5H₂O; and amorphous Zr₃OF₃(PO₄)₂NO₃ · (7–8) H₂O. A shown by its IR spectrum, Rb₂ZrF₄(PO₄)_0.33NO₃ contains NO₃- and PO₄ groups that are not coordinated to zirconium, meaning that this is a triple salt ZrF₄ · Rb(PO₄)_0.33 · RbNO₃. The formula units of the RbZr₃OF₃(PO₄)₂(NO₃)₂ · 5H₂O and Zr₃OF₃(PO₄)₂NO₃ · (7–8)H₂O phases are only conventional. All compounds have been recovered for the first time.     

Crystal structures of seven-coordinate (NH4)2[MnII(edta)(H2O)]·3H2O, (NH4)2[MnII(cydta)(H2O)]·4H2O and K2[MNII(hdtpa)]·3.5H2O complexes

The title compounds, (NH₄)₂[Mn^II(edta)(H₂O)]·3H₂O (H₄edta = ethylenediamine-N,N,N′,N′-tetraacetic acid), (NH₄)₂[Mn^II(cydta)(H₂O)]·4H₂O (H₄cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid) and K₂[Mn^II(Hdtpa)]·3.5H₂O (H₅dtpa = diethylenetriamine-N,N,N′,N″,N″-pentaacetic acid), were prepared; their compositions and structures were determined by elemental analysis and single-crystal X-ray diffraction technique. In these three complexes, the Mn²⁺ ions are all seven-coordinated and have a pseudomonocapped trigonal prismatic configuration. All the three complexes crystallize in triclinic system in P-1 space group. Crystal data: (NH₄)₂[Mn^II(edta)(H₂O)]·3H₂O complex, a = 8.774(3) ?, b = 9.007(3) ?, c = 13.483(4) ?, α = 80.095(4)°, β = 80.708(4)°, γ = 68.770(4)°, V = 972.6(5) ?³, Z = 2, D _c = 1.541 g/cm³, μ = 0.745 mm⁻¹, R = 0.033 and wR = 0.099 for 3406 observed reflections with I ≥ 2σ(I); (NH₄)₂[Mn^II(cydta)(H₂O)]·4H₂O complex, a = 8.9720(18) ?, b = 9.4380(19) ?, c = 14.931(3) ?, α = 76.99(3)°, β = 83.27(3)°, γ = 75.62(3)°, V = 1190.8(4)?³, Z = 2, D _c = 1.426 g/cm³, μ = 0.625 mm⁻¹, R = 0.061 and wR = 0.197 for 3240 observed reflections with I ≥ 2σ(I); K₂[Mn^II(Hdtpa)]·3.5H₂O complex, a = 8.672(3) ?, b = 9.059(3) ?, c = 15.074(6) ?, α = 95.813(6)°, β = 96.665(6)°, γ = 99.212(6)°, V = 1152.4(7) ?³, Z = 2, D _c = 1.687 g/cm³, μ = 1.006 mm⁻¹, R = 0.037 and wR = 0.090 for 4654 observed reflections with I ≥ 2σ(I). Original Russian Text Copyright ? 2008 by X. F. Wang, J. Gao, J. Wang, Zh. H. Zhang, Y. F. Wang, L. J. Chen, W. Sun, and X. D. Zhang The text was submitted by the authors in English. Zhurnal Strukturnoi Khimii, Vol. 49, No. 4, pp. 753–759, July–August, 2008.     

［Mn2(CHZ)4(H2O)2］(PA)4·10H2O的制备和分子结构研究

本文论述了苦味酸(PA,三硝基苯酚)锰与碳酰肼(CHZ, NH₂NHCONHNH₂)反应制备目标配合物的方法及该配合物的晶体结构。该配合物的结构式为［O,O′-μ-Mn₂(CHZ)₄(H₂O₂)］(PA)₄·10H₂O。晶体属三斜晶系,P1 空间群。晶体学参数为：a=0.8269(1) nm, b=1.2812(1) nm, c=1.5915(1) nm; α=109.58(1)°, β=95.19(1)°, γ=92.76(1)°, V=1.5765(2)nm³; Z=1, Dc=1.580 g·cm^-3, μ(Mo K_α)=520 m^-1。晶体结构经全矩阵最小二乘法修正,最终偏离因子R=0.0557。该化合物为具有中心对称的双核配合物,以两个碳酰肼分子中羰基氧为桥原子将两个锰离子结合起来,与锰离子形成配位键的原子是碳酰肼分子第一、五氮原子,羰基氧原子和水分子中的氧原子,锰离子的配位数为七。若味酸根作为外界离子以库伦力和氢键与内界离子结合成配合物分子。