Brahim El Bali

New hybrid diphosphates Ln2(NH2(CH2)2NH2)(HP2O7)2 · 4 H2O(Ln = Eu, Tb, Er): synthesis, single crystal and powder X-ray crystal structure

Crystals of lanthanide ethylenediamine diphos phates Ln2(NH2(CH2)2NH2)(HP2O7)2 · 4 H2O (Ln = Eu (1), Tb (2), Er (2)) have been synthesized and investigated by single crystal X-ray diffractometry (Eu and Tb phases) and by powder X-ray diffractometry (Er phase). The three structures resulted to be isostructural within triclinic space group P-1, with unit cell parameters of a = 6.5050(6) Å; b = 6.9990(2) Å; c = 9.8450(9) Å; α = 81.548(5)°; β = 80.631(19)°; γ = 88.369(9)°; V = 437.44(6) Å3(1), a = 6.4360(7) Å; b = 6.9480(12) Å; c = 9.816(4) Å; α = 81.987(19)°; β = 80.595(16)°; γ = 88.591(13)°; V = 428.82(19) Å3(2), a = 6.39658(2) Å; b = 6.86682(2) Å; c = 9.78849(3) Å; α = 81.6811(4)°; β = 80.2304(3)°; γ = 88.3812(3)°; V = 419.255(3) Å3(3).The three-dimensional network is built up by the repetition of ab-parallel layers of LnO8 polyhedra corner-sharing with (HP2O7) groups; ethylenediamine molecules lie between such layers, acting both as receptors and donors in strong hydrogen bonds which assure the stabilizing of the entire framework.

New isostructural ethylenediammonium diphosphates (NH3(CH2)2NH3)2[Me(HP2O7)2 · 2 H2O] [Me = Co, Ni] : X-ray crystal structure and vibrational spectroscopy

Abstract New ethylenediammonium diphosphates (NH3(CH2)2NH3)2[Me(HP2O7)2 · 2 H2O] [Me = Co (1), Ni (2)] have been synthesized and investigated by single-crystal X-ray diffractometry. The two structures resulted to be isostructural within triclinic space group P-1. The unit-cell parameters are: a = 7.5211(6) Å, b = 7.5574(3) Å, c = 9.7689(7) Å, α = 103.6(1)°, β = 111.14(1)°, γ = 98.04(1)°, V = 486.9(1) Å3 (1) and a = 7.4631(15) Å, b = 7.5274(12) Å, c = 9.743(3) Å, α = 104.28(2)°, β = 110.75(2)°, γ = 97.50(2)°, V = 481.4(2) Å3 (2). The three-dimensional network is built up by discrete Me(HP2O7)2 · 2 H2O moieties, which, via strong O—H … O bonds, form layers parallel to ab plane. Ethylenediammonium groups are located between such layers, stabilizing the framework via N—H … O bonds. The hydrogendiphosphate group presents bent eclipsed conformation, while the Me ion lies on inversion centre. The structural data, as the bent POP configuration, have been confirmed by the Raman and infrared spectra of the title compounds. In particular, the non-coincidence between the infrared and Raman bands supports the centrosymmetric structure of the investigated crystals.

Isolation and X-ray Crystal Structure of Tetrahydroisoquinoline Alkaloids from Calycotome Villosa Subsp. intermedias

Two tetrahydroisoquinoline alkaloids were extracted from the alkaloid fraction of a methanol extract of the seeds of Calycotome Villosa Subsp. intermedia. Their structures were established as (R)-1-hydroxymethyl-7-8-dimethoxy-1,2,3,4-tetrahydro- isoquinoline (1) and (S)-7-hydroxymethyl-2-3-dimethoxy-7,8,9,10-tetrahydroisoquinoline chloride (2) by spectroscopic techniques and X-ray diffraction analysis.

Tetragonal form of barium cobalt disilicate, Ba2CoSi2O7

The structure of Ba2CoSi2O7 consists of layers made from corner-sharing of [SiO4] and [CoO4] polyhedra. These layers, lying parallel to (001), are linked by Ba⋯O interactions. Co2+ forms flattened CoO4 tetrahedra (point symmetry overline 4), which are isolated in the structure. The blue color of the solid might be explained by the coordination mode of the Co atoms.

Reinvestigation of NH4[Co(H2O)6]PO4 based on single-crystal data

The structure of the title compound, ammonium hexaxadaquaxadcobalt(II) orthophosphate, known from powder data, has been refined based on single-crystal data. The compound crystallizes in the struvite [NH4Mg(H2O)6PO4] structure type and is isotypic with the homologous nickel phase. The framework is built of NH4+, [Co(H2O)6]2+ and PO43− ions stacked in two kinds of ribbons parallel to (010). CoII atoms are well separated in the framework, with the shortest Co⋯Co distance being over 6u2005A.

3-Nitro­so-2-phenyl­imidazo­[1,2-a]­pyrimidine

Institut fu¨rAnorganische Chemie, J. W. Goethe-Universita¨tFrankfurt, Marie-Curie-Strase 11, 60439Frankfurt/Main, GermanyCorrespondence e-mail:bolte@chemie.uni-frankfurt.deKey indicatorsSingle-crystal X-ray studyT = 173 KMean ˙(C–C) = 0.004 A˚R factor = 0.054wR factor = 0.140Data-to-parameter ratio = 11.9For details of how these key indicators wereautomatically derived from the article, seehttp://journals.iucr.org/e.# 2004 International Union of CrystallographyPrinted in Great Britain – all rights reserved

Synthesis, crystal structure and vibrational spectra of a new di­ammonium zinc(II) di­hydrogendiphosphate dihydrate, (NH4)2Zn(H2P2O7)2·2H2O

(NH4)2Zn(H2P2O7)2·2H2O is isostructural with its manganese homologue. Isolated almost-regular ZnO6 octahedra form a layered structure. The IR and Raman spectra show bands characteristic of H2P2O7 groups.

(2Z)-2-(Hydro­ximino)-3-methoxy-3-phenyl-2,3-di­hydro-1H-imidazo­[1,2-a]­pyrimidin-4-ium perchlorate

The title salt, C13H13N4O2+·ClO4−, contains an imidazoxad[1,2-a]xadpyrimidinium moiety carrying a hydroxyxadimine group, a methoxy group and a phenyl ring. The charge is balanced by a perchlorate anion. The 2-hydroxadximinoxadimidazoxad[1,2-a]xadpyrimidinium moiety is essentially planar and the hydroxyxadimine group is cis to the N atom of the heterocycle.

Dipotassium cobalt(II) bis­(hydrogenphosphite) dihydrate, K2Co(HPO3)2·2H2O

K2Co(HPO3)2·2H2O is a new phosphite within the K–T–H3PO3 system (T = divalent transition metal cation). Its structure can be described as a three-dimensional network made up of KO6 and HPO3 polyhedra, which share corners and edges. In the cavities of this framework, Co2+ ions are located in an almost regular octahedral oxyxadgen coordination. An IR study has confirmed the presence of HPO3 hydrogenphosphite groups.

3-(Anthracen-9-yl­methyl­ene)-2,4-di­methyl-3H-benzo­[1,5]­diazepine

The title compound, C26H20N2, crystallizes with two almost identical molxadecules in the asymmetric unit. The diazepine ring adopts a boat conformation.