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1.
The Influence of Phosphoryl Substituents on the Properties of P‐Substituted 2‐Methylimidazolium Ions and 2‐Methyleneimidazolines [1] The imidazolines ImCHP(E)Ph2 [ 6 , E = S ( a ), Se ( b )] are obtained from ImCHPPh2 ( 4 ) and sulfur or selenium. HBF4 reaction yields the corresponding imidazolium salts [ImCH2P(E)Ph2][BF4] [ 5 , E = S ( a ), Se ( b )]. 1, 3, 4, 5‐Tetramethyl‐2‐methylenimidazoline ( 1 , ImCH2) reacts with Ph2P(O)Cl to give the corresponding phosphane salt [ImCH2P(O)Ph2]Cl ( 7 ) from which the vinyl compound ImCHP(O)Ph2 ( 8 ) is formed through deprotonation. 8 reacts with excess HBF4 to give the phosphine oxide BF3 adduct [ImCH2P(O)Ph2 · BF3][BF4] ( 9 ). The crystal structures of 5a , 5b , 6b , 7 · CH2Cl2 and 9 · H2O as well as preliminary data of 8 are reported and discussed on comparison with the phosphanes [ImCH2PPh2][BF4] ( 3b ) and ImCHPPh2 ( 4 ). From structural data, π‐electron delocalisation is concluded for 6b and 8 . 相似文献
2.
Red crystals of [NMeEt3]2n[TeBr6(Se2Br2)3]n ( 1 ) were isolated when selenium and bromine (1:1) were allowed to react in acetonitrile solution in the presence of tellurium(IV) bromide and methyltriethylammonium bromide (1:2). The salt 1 crystallizes in the monoclinic space group C2/c with the cell dimensions a = 27.676(6) Å, b = 9.665(2) Å, c = 18.796(4) Å and ß = 124.96(3)° (120 K). The [TeBr6(Se2Br2)3]2— anions contain nearly regular octahedral [TeBr6]2— ions which are incorporated into a polymeric chain by bonding contacts between 3 facial bromo ligands and 3 Se2Br2 molecules, one of which is situated on the twofold symmetry axis. The distances between the μBr ligands and the SeI atoms of the Se2Br2 molecules are observed in the range 3.308(2) — 3.408(2) Å and can tentatively be interpreted as donor‐acceptor bonds with μBr as donors and Se2Br2 as acceptors. The TeIV—Br distances are in the range 2.669(1) — 2.687(1) Å. The bond lengths in the connecting Se2Br2 molecules are: SeI—SeI = 2.267(2) and 2.281(2) Å, SeI—Br = 2.340(1), 2.353(1) and 2.337(1) Å. 相似文献
3.
Colourless block‐shaped crystals of [(NH4)2(2.2.2‐cryptand)2][P2S8] ( 1 ) and [(NH4)2(18‐crown‐6)2][P2S8]·H2O ( 2 ) could be obtained by the reaction of an aqueous solution of ammonium hexathiohypodiphosphate, (NH4)4P2S6·2 H2O, with sulfur and 2.2.2‐cryptand or 18‐crown‐6. The crystal structures of both compounds have been determined by single‐crystal X‐Ray diffraction analysis. Compound 1 crystallizes in the monoclinic space group C2/c with a = 2032.7(2), b = 1243.6(2), c = 2244.6(2) pm, β = 98.64(1)°, and Z = 8, whereas compound 2 crystallizes also monoclinic in the space group P21/c with a = 2121.3(2), b = 865.5(1), c = 2345.4(2) pm, β = 91.96(1)°, and Z = 4. It could be established that the title compounds contain a new type of six‐membered [1,2‐P2S4] ring with P – P bond and three S – S linkages. The tetrahedral environment of each phosphorus is completed by a (formally) single and double bonded sulfur atom attached externally to the [1,2‐P2S4] ring. These terminal PS2 units are mesomerically stabilized according to their P – S distances. FT‐IR and FT‐Raman spectra of the title compounds are recorded and interpreted. 相似文献
4.
Thesynthesisofcrystallinezirconiumphosphateswasfirstreportedinl964byClearfieldandStynes['J,whodeterminedtheformulaasZr(HPO,),.H,O(a-ZrP)basedonchemicalcomposition,dehydrationandion-exchangebe-haviour'Sincethen,manyothercrystallinezirconiumphosphate,suchasZr(HPO,)(g-ZrP),Zr(HPO'),.H,O(Y-ZrP),havebeenprepared['.'1.Thesephosphatesconsistedofalternate,cross-linkedlayersofZrO,octahedraandPO'tetrahedrawithwatermoleculesaccommodatedininterlamellarfashion.a-Zirco-niumphosphate,Zr(HPO'),.… 相似文献
5.
The tris‐bidentate complex [Ni(C12H8N2)2(CO3)] was synthesized by the reaction of Na2CO3, 1,10‐phenanthroline (phen = C12H8N2) and NiSO4 · 6 H2O in the presence of succinic acid in a CH3OH–H2O solution. The compound crystallizes as heptahydrate. The crystal structure (monoclinic, P21/c (no. 14), a = 9.897(1), b = 26.384(2), c = 10.582(1) Å, β = 105.87(1)°, Z = 4, R = 0.0505, wR2 = 0.1029 for 3166 observed reflections (F ≥ 2σ(F ) out of 6100 unique reflections) consists of hydrogen bonded water molecules and [Ni(phen)2(CO3)] complex molecules. The Ni atoms are sixfold octahedrally coordinated by the four N atoms of two bidentate chelating phen ligands and by two O atoms of the bidentate chelating carbonate group with d(Ni–N) = 2.092–2.100 Å, d(Ni–O) = 2.051, 2.079 Å. The complex molecules are stacked into 2D corrugated layers parallel to (010) via two types of intermolecular π‐π stacking interactions. One occurs between two quinoline rings of neighboring phen ligands at the distance of 3.63 Å in [010] direction and the other results from 1D π‐π stacking interactions through partially covered phen rings at alternative distances of 3.26 Å and 3.33 Å in [001] direction. The water molecules are sandwiched between 2D layers. 相似文献
6.
Brown crystals of [PMePh3]2[TeBr6(SeBr2)2] ( 1 ) were obtained when selenium and bromine (1:1) react in acetonitrile solution in the presence of tellurium(IV) bromide and methyltriphenylphosphonium bromide. The salt 1 crystallizes in the triclinic space group P1¯ with the cell dimensions a = 10.3630(14)Å, b = 11.5140(12)Å, c = 11.7605(17)Å, α = 108.643(9)°, β = 106.171(10)° and γ = 99.077(9)° (296 K). In the solid state the [TeBr6(SeBr2)2]2— anion contains a nearly regular [TeBr6] octahedron where the four equatorial bromo ligands each have developed a bond to the SeII atom of a SeBr2 molecule. The contacts between the bridging bromo and the SeII atoms of the SeBr2 molecules are observed in the range 3.11—3.21Å, and can be interpreted as bonds of the donor‐acceptor type with the bridging bromo ligands as donors and the SeBr2 molecules as acceptors. The TeIV—Br distances are in the range 2.67—2.72Å, and the SeII—Br bond lengths in coordinated SeBr2 molecules in the range 2.33—2.34Å. 相似文献
7.
The X‐ray structure of 2‐Chloro‐1, 3‐diisopropyl‐4, 5‐dimethylimidazolium dichlorophosphate ( 2 ) (obtained from 2‐chloro‐1, 3‐diisopropyl‐4, 5‐dimethylimidazolium chloride 1 and POCl3 in the presence of water) is reported. 相似文献
8.
Novel Halogenochalcogeno(IV) Acids: [H3O(Benzo‐18‐Crown‐6)]2[Te2Br10] and [H5O2(Dibenzo‐24‐Crown‐8)]2[Te2Br10] Systematic studies on halogenochalcogeno(IV) acids containing tellurium and bromine led to the new crystalline phases [H3O(Benzo‐18‐Crown‐6)]2[Te2Br10] ( 1 ) and [H5O2(Dibenzo‐24‐Crown‐8)]2[Te2Br10] ( 2 ). The [Te2Br10]2‐ anions consists of two edge‐sharing distorted TeBr6 octahedra, the oxonium cations are stabilized by crownether. ( 1 ) crystallizes in the monoclinic space group P21/n with a = 14.520(5) Å, b = 22.259(6) Å, c = 16.053(5) Å, β = 97.76(3)° and Z = 4, whereas ( 2 ) crystallizes in the triclinic space group with a = 11.005(4) Å, b = 12.103(5) Å, c = 14.951(6) Å, α = 71.61(3)°, β = 69.17(3)°, γ = 68.40(3)° and Z = 1. 相似文献
9.
Single crystals of [Cu(ATSC)]NH2SO3 ( 1 ) (ATSC –4‐allylthiosemicarbazide) were obtained by electrochemical synthesis using alternating current. Compound ( 1 ) crystallizes in P212121 sp. gr., a = 6.8284(2), b = 9.3054(3), c = 16.1576(11) Å, Z = 4. ATSC moiety acts as tetradentate ligand, chelating two symmetrically related copper atoms. The Cu atom possesses trigonal pyramidal coordination, formed by two sulphur atoms (one of them at the apical position), nitrogen atom and C=C bond. Sulfamate anion is associated via hydrogen bonds. By slow hydrolysis of 1 crystals of [Cu2(ATSC)2]SO4 ( 2 ) were obtained: P 1 sp. gr., a = 9.526(2), b = 12.687(2), c = 14.7340(10) Å, α = 95.119(10), β = 89.903(12), γ = 109.113(14)°, Z = 4. The asymmetric unit of 2 contains two formula units, which are related by pseudosymmetry via a glide plane a. One half of four ATSC molecules act as in 1 , the rest as tridentate ligands, which coordinate the two copper atoms in apical positions with sulfate anions. This Cu–S coordination was to date unknown. The structure of the ATSC ligands contributes to the unexpected competitiveness of C=bond in the coordination sphere of CuI inspite of strong donor atoms. 相似文献
10.
Crystals of the zwitterionic copper(I) π‐complex [(HC≡CCH2NH3)Cu2Br3] have been synthesized by interaction of CuBr with [HC≡CCH2NH3]Br in aqueous solution (pH < 1) and X‐ray studied. The crystals are monoclinic: space group P21/n, a = 6.722(4), b = 12.818(8), c = 9.907(3) Å, β = 100.25(4)°, V = 840.0(8) Å3, Z = 4, R = 0.0592 for 3015 reflections. The crystal structure of the π‐complex contains isolated [(HC≡CCH2NH3)+(Cu2Br3)?]2 units which are incorporated into a framework by strong hydrogen N–H···Br and C≡C–H···Br bonds. The length of π‐coordinated propargylammonium C≡C bond is equal 1.216(8) Å and Cu(I)–(C≡C) distance equals 1.958(5) Å. 相似文献
11.
ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option. 相似文献
12.
Single crystals of Li4(PO2NH)4 · 4 H2O were obtained by dissolving LiOH and H4(PO2NH)4 · 2 H2O in water and subsequent precipitation with acetone and ethanol followed by slow evaporation of the solvents. The structure of Li4(PO2NH)4 · 4 H2O was solved by single‐crystal X‐ray methods ( (No. 2), a = 489.2(2), b = 853.2(2), c = 880.5(2) pm, α = 101.71(3), β = 102.39(3), γ = 94.88(3)°, Z = 1). The structure is composed of LiO4 tetrahedra and (PO2NH)44? ions. The P4N4 rings of the anions exhibit a slightly distorted chair–1 conformation, which is supported by IR data and has been described by torsion angles, displacement asymmetry parameters and puckering parameters. Via Li+ ions and hydrogen bonds, the tetrametaphosphimate anions are connected forming a three‐dimensional network. 相似文献
13.
Tetrafluorobo‐Synthesis and Deprotonation of a Phosphinomethylimidazolium Salt. On the π‐Electron Delocalization im Aminovinyl Phosphanes [1] The ylidic olefin 1, 3, 4, 5‐tetramethyl‐2‐methyleneimidazoline ( 1 , Im=CH2) reacts with chlorodiphenylphosphane to give the phosphane salt [(Im‐CH2)PPh2]Cl ( 6 ) from which the vinylphosphane Im=CHPPh2 ( 8 ) is obtained by deprotonation. 8 reacts with HBF4 etherate to give the tetrafluoroborate salt [(Im‐CH2)‐PPh2] BF4 ( 7 ). The crystal structures of 7 and 8 are determined and discussed. In 8 , π‐electron delocalisation is indicated both by structural data and temperature dependent n.m.r. spectroscopy 相似文献
14.
Yong‐Qin Wei Ke‐Chen Wu Bo‐Tao Zhuang Zhang‐Feng Zhou Ming‐Xin Zhang Cai‐Ping Liu 《无机化学与普通化学杂志》2005,631(8):1532-1535
The silver complex Ag(PPh3)2(H2TMT) ( 1 )(H3TMT = 2,4,6‐trimercapto‐1,3,5‐triazine) has been synthesized and characterized. The ligand trimercaptotriazine exhibits a novel coordination mode and the complex shows a special hydrogen bonding linkage in the crystal packing. The colorless crystals of 1 exhibit broad emission in the visible region at room temperature. TDDFT calculation indicated that the π–π attraction is crucial for fluorescence of the title complex. 相似文献
15.
The compound [NH4(NH3)4][Co(C2B9H11)2] · 2 NH3 ( 1 ) was prepared by the reaction of Na[Co(C2B9H11)2] with a proton‐charged ion‐exchange resin in liquid ammonia. The ammoniate 1 was characterized by low temperature single‐crystal X‐ray structure analysis. The anionic part of the structure consists of [Co(C2B9H11)2]‐ complexes, which are connected via C‐H···H‐B dihydrogen bonds. Furthermore, 1 contains an infinite equation/tex2gif-stack-2.gif[{NH4(NH3)4}+(μ‐NH3)2] cationic chain, which is formed by [NH4(NH3)4]+ ions linked by two ammonia molecules. The N‐H···N hydrogen bonds range from 1.92 to 2.71Å (DHA = Donor···Acceptor angles: 136‐176°). Additional N‐H···H‐B dihydrogen bonds are observed (H···H: 2.3‐2.4Å). 相似文献
16.
Molecular Structure of Bis[salicylaldehyde-2-hydroxyanilato(2—)]vanadium(IV) By the reaction of tris(acetylacetonato)vanadium(III) with salicylaldehyde-2-hydroxyanil the non-oxo vanadium(IV) complex of this ligand was prepared. Bis[salicylaldehyde-2-hydroxyanilato(2—)]vanadium(IV) has a distorted octahedral structure. Crystallographic data see “Inhaltsübersicht”. 相似文献
17.
[Cu(C12H8N2)(C4H4O4)(H2O)]2 · C4H6O4 was prepared by the reaction of succinic acid, CuCl2 · 2 H2O, 1,10‐phenanthroline (phen = C12H8N2), and Na2CO3 in a CH3OH–H2O solution. The crystal structure (triclinic, P 1 (no. 2), a = 7.493(1), b = 9.758(1), c = 13.517(1) Å; α = 68.89(1)°, β = 88.89(1)°, γ = 73.32(1)°, Z = 1, R = 0.0308, wR2 = 0.0799 for 3530 observed reflections (F ≥ 2σ(F ) out of 3946 unique reflections) consists of hydrogen bonded succinic acid molecules and succinato bridged 1 D zipperlike supramolecular [Cu(phen)(C4H4O4)2/2(H2O)]2 double chains based on 1 D π‐π stacking interactions between the chelating phen systems at distances of 3.71 Å and 3.79 Å. The Cu atoms are fivefold trigonal bipyramidally coordinated by two N atoms of the bidentate chelating phen ligand and three O atoms of one water molecule and two bidentate bridging succinate ligands. The water O atom and one phen N atom are at the apical positions (equatorial: d(Cu–O) = 1.945, 2.254(2) Å, d(Cu–N) = 2.034(2) Å; axial: d(Cu–O) = 1.971(2) Å, d(Cu–N) = 1.995 Å). 相似文献
18.
Phase‐pure ammonium catena‐polyphosphate IV [NH4PO3]x was synthesized by heating NH4H2PO4 in a tube furnace under an ammonia gas flow. The product contained single crystals of [NH4PO3]x IV appropriate for an X‐ray structure determination enabling structure refinement of this compound. The pseudo‐merohedrally twinned crystals of [NH4PO3]x crystallize in the monoclinic crystal system (P21/c, no. 14, a = 2270.3(5), b = 458.14(9), c = 1445.1(3) pm, β = 108.56(3)°, Z = 4, 2264 data, R1 = 0.076). In the unit cell the catena‐polyphosphate chain anions run parallel [010] with a chain‐periodicity P = 2 and a stretching factor fs = 0.94. The chain anions are interconnected through extensive hydrogen bonding towards the ammonium ions. Due to ‘chemical twinning’ a novel catena‐polyphosphate structure type is realized in [NH4PO3]x IV. The vibrational spectra of [NH4PO3]x IV are reported as well. 相似文献
19.
Srinivasan Natarajan Wilhelm Klein Jürgen Nuss Leo van Wüllen Martin Jansen 《无机化学与普通化学杂志》2003,629(2):339-343
A one‐dimensional aluminum phosphate, [NH3(CH2)2NH2(CH2)3NH3]3+ [Al(PO4)2]3—, has been synthesized hydrothermally in the presence of N‐(2‐Aminoethyl‐)1, 3‐diaminopropane (AEDAP) and its structure determined by single crystal X‐ray diffraction. Crystal data: space group = Pbca (no. 61), a = 16.850(2), b = 8.832(1), c = 17.688(4)Å, V = 2632.4(2)Å3, Z = 8, R1 = 0.0389 [5663 observed reflections with I > 2σ(I)]. The structure consists of anionic [Al(PO4)2]3— chains built up from AlO4 and PO4 tetrahedra, in which all the AlO4 vertices are shared and each PO4 tetrahedron possesses two terminal P=O linkages. The cations, which balances the negative charge of the chains, are located in between the chains and interact with the oxygen atoms through strong N—H···O hydrogen bonds. Additional characterization of the compound by powder XRD and MAS‐NMR has also been performed and described. 相似文献
20.
Synthesis and Crystal Structure of [Cr(NH3)6][Cr(NH3)2F4][BF4]2 The action of ammonium fluoride on a mixture of boron and chromium in a sealed Monel ampoule at 300 °C yields single crystals of [Cr(NH3)6][Cr(NH3)2F4][BF4]2. The crystal structure (tetragonal, P4/mbm, Z = 2, a = 1056.0(1), c = 781.7(1) pm; R1 = 0.0414; wR2 = 0.1087 for 411 reflections with I0 > 2σ(I)) contains [Cr(NH3)6]3+ and [Cr(NH3)2F4]– octahedra and twice as many [BF4]– tetrahedra that are arranged in a quadrupled super‐structure of the CsCl‐type of structure. 相似文献