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1.
A reaction of the potassium salts of RC(S)NHP(S)(OiPr)2 (R = PhNH, HL I; Ph, HL II) with a mixture of AgNO3 and Ph2P(CH2)1 − 3PPh2 or Ph2P(C5H4FeC5H4)PPh2 in aqueous EtOH/CH2Cl2 leads to [Ag2(Ph2PCH2PPh2)2LINO3] ( 1 ), [Ag{Ph2P (CH2)2PPh2}LI,II] ( 2, 6 ), [Ag{Ph2P(CH2)3PPh2}LI,II] ( 3, 7 ), [Ag{Ph2P(C5H4FeC5H4)PPh2}LI,II] ( 4, 8 ), and [Ag2(Ph2PCH2PPh2)LII2] ( 5 ) complexes. The structures of these compounds were investigated by 1H and 31P{1H} NMR spectroscopy and elemental analyses. It was established that the binuclear complexes 1 and 5 are luminescent in the solid state at ambient conditions. © 2010 Wiley Periodicals, Inc. Heteroatom Chem 21:386–391, 2010; View this article online at wileyonlinelibrary.com . DOI 10.1002/hc.20627 相似文献
2.
Jian‐Long Du Xiao‐Long Zhu Pei Li 《Acta Crystallographica. Section C, Structural Chemistry》2012,68(10):m281-m283
Yellow needle‐shaped crystals of the title compound, {[Ag(C30H22N4)][Ag(NO3)2]}n, were obtained by the reaction of AgNO3 and 9,10‐bis(benzimidazol‐1‐ylmethyl)anthracene (L) in a 2:1 ratio. The asymmetric unit consists of two AgI cations, one half L ligand and one nitrate anion. One AgI cation occupies a crystallographic inversion centre and links two N‐atom donors of two distinct L ligands to form an infinite one‐dimensional coordination polymer. The second AgI cation lies on a crystallographic twofold axis and is coordinated by two O‐atom donors of two nitrate anions to form an [Ag(NO3)2]− counter‐ion. The polymeric chains are linked into a supramolecular framework via weak Ag...O [3.124 (5) Å] and Ag...π (2.982 Å) interactions (π is the centroid of an outer anthracene benzene ring). The π interactions contain two short Ag...C contacts [2.727 (6) and 2.765 (6) Å], which can be considered to define Ag–η2‐anthracene bonding interactions. In comparison with a previously reported binuclear AgI complex [Du, Hu, Zhang, Zeng & Bu (2008). CrystEngComm, 10 , 1866–1874], this new one‐dimensional coordination polymer was obtained by changing the metal–ligand ratio during the synthesis. 相似文献
3.
CpFe(CO)I(η1-Ph2PCH2P(O)Ph2) 2 was obtained in small yield from reaction of [CpFe(CO)]2[μ-(Ph2P)2CH2] with diiodine in benzene, or prepared in 82% yield on treating CpFe(CO)I(η1-Ph2PCH2PPh2) 1 with H2O2. Compound 2 crystallizes in the space group P21/n, with a = 8.441(2) Å, b = 10.054(2) Å, c = 33.343(8) Å, β = 92.33(2)°, Z = 4, V = 2827(1) Å3, RF = 0.057, and Rw = 0.056. 相似文献
4.
Mao-Chun Hong Zhi-Ying Huang Xin-Jian Lei Bei-Sheng Kang Fei-Long Jiang Han-Qin Liu 《中国化学》1991,9(5):425-429
Co4(μ3-S)8(Ph2PCH2sP(O)Ph2)6, MW = 3012.5, space group R3 , has the hexagonal parameters, a = 26.764 (10), c = 16.979 (10) Å, V = 10532.8 Å3, Z = 3. Mo Ka radiation, λ = 0.71069 Å, Dc = 1.425 g/cm3, μ = 9.94 cm?3, F(000) = 4650, R = 0.073 and Rw = 0.077 for 1965 observed unique reflections with I > 3σ (I). The molecular structure consists of a distorted octahedral Co4—core. The Co—Co and Co—S distances fall in the range of 2.805—2.838 and 2.213—2.253 Å, respectively. 相似文献
5.
Przemysaw J. Malinowski Daniel Himmel Ingo Krossing 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2016,128(32):9408-9412
The synergistic Ag+/X2 system (X=Cl, Br, I) is a very strong, but ill‐defined oxidant—more powerful than X2 or Ag+ alone. Intermediates for its action may include [Agm(X2)n]m+ complexes. Here, we report on an unexpectedly variable coordination chemistry of diiodine towards this direction: ( A )Ag‐I2‐Ag( A ), [Ag2(I2)4]2+( A −)2 and [Ag2(I2)6]2+( A −)2⋅(I2)x≈0.65 form by reaction of Ag( A ) ( A =Al(ORF)4; RF=C(CF3)3) with diiodine (single crystal/powder XRD, Raman spectra and quantum‐mechanical calculations). The molecular ( A )Ag‐I2‐Ag( A ) is ideally set up to act as a 2 e− oxidant with stoichiometric formation of 2 AgI and 2 A −. Preliminary reactivity tests proved this ( A )Ag‐I2‐Ag( A ) starting material to oxidize n‐C5H12, C3H8, CH2Cl2, P4 or S8 at room temperature. A rough estimate of its electron affinity places it amongst very strong oxidizers like MF6 (M=4d metals). This suggests that ( A )Ag‐I2‐Ag( A ) will serve as an easily in bulk accessible, well‐defined, and very potent oxidant with multiple applications. 相似文献
6.
Yu. V. Kokunov Yu. E. Gorbunova V. V. Kovalev 《Russian Journal of Coordination Chemistry》2012,38(4):245-248
The complex [Ag(2-MePyz)ReO4] (I) is synthesized, and its structure is determined. The crystals are monoclinic, space group P 21/c, a = 7.234(1), b = 15.451(1), c = 8.036(3) Å, β = 92.56(1)°, V = 897.3(2) Å3, ρcalcd = 3.347 g/cm3, Z = 4. Structure I consists of cationic polymer chains [Ag(2-MePyz)] ∞ + . Anions ReO 4 ? are weakly bound to Ag+ (Ag...Oaverage 2.693 Å) and join the latter into a supramolecular framework. The Ag+ ion has a linear coordination (NAgN 177.9(2)°, distances Ag-N 2.223(5) and 2.242(5) Å). 相似文献
7.
The reaction of Ag2SO4 and bpp (bpp = 1,3‐bis(4‐pyridyl)propane) in H2O afforded the complex [Ag2(bpp)2(SO4) · 6.5H2O·CH3OH]n, 1. The IR and TGA have been recorded and the structure has been determined. Crystal data for 1: Space group C2/c, a = 17.885(4), b = 25.230(6), c = 8.832(2) Å, β = 105.437(4)°. V = 3841(1) Å3, Z = 8 with final residuals R1 = 0.0710 and wR2 = 0.1620. The complex shows a three‐dimensional supramoleclar structure constructed with two‐dimensional infinite [Ag2(bpp)2]n sheetlike layers pillared by Ag‐Ag interactions and Ag····O (SO4) interactions in the solid state. 相似文献
8.
Ming‐Liang Tong Xiao‐Ming Chen Seik Weng Ng 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(9):m481-m482
In the title compound {alternative name: poly[silver(I)‐μ‐(3‐amino‐2‐chloropyridine)‐μ‐nitrato]}, [Ag(NO3)(C5H5ClN2)]n the AgI atom is in an irregular AgN2O3 geometry, surrounded by one pyridyl N atom [Ag—N 2.283 (5) Å], one amine N atom [Ag—N 2.364 (6) Å] and three O atoms from different nitrate ions [Ag—O 2.510 (6)–2.707 (6) Å]. The Ag ions are bridged by the 3‐amino‐2‐chloropyridine ligands into helical chains. Adjacent uniform chiral chains are further interlinked through the NO3 bridges into an interesting two‐dimensional coordination network in the solid. 相似文献
9.
Il'ya A. Gural'skiy Pavlo V. Solntsev Konstantin V. Domasevitch Eduard B. Rusanov Alexander N. Chernega 《Acta Crystallographica. Section C, Structural Chemistry》2007,63(6):m259-m263
Poly[[μ4‐4,4′‐bipyridazine‐μ5‐sulfato‐disilver(I)] monohydrate], {[Ag2(SO4)(C8H6N4)]·H2O}n, (I), and poly[[aqua‐μ4‐pyridazino[4,5‐d]pyridazine‐μ3‐sulfato‐disilver(I)] monohydrate], {[Ag2(SO4)(C6H4N4)(H2O)]·H2O}n, (II), possess three‐ and two‐dimensional polymeric structures, respectively, supported by N‐tetradentate coordination of the organic ligands [Ag—N = 2.208 (3)–2.384 (3) Å] and O‐pentadentate coordination of the sulfate anions [Ag—O = 2.284 (3)–2.700 (2) Å]. Compound (I) is the first structurally examined complex of the new ligand 4,4′‐bipyridazine; it is based upon unprecedented centrosymmetric silver–pyridazine tetramers with tetrahedral AgN2O2 and trigonal–bipyramidal AgN2O3 coordination of two independent AgI ions. Compound (II) adopts a typical dimeric silver–pyridazine motif incorporating two kinds of square‐pyramidal AgN2O3 AgI ions. The structure exhibits short anion–π interactions involving noncoordinated sulfate O atoms [O...π = 3.041 (3) Å]. 相似文献
10.
Konstantinos Chondroudis Debojit Chakrabarty Enos A. Axtell Mercouri G. Kanatzidis 《无机化学与普通化学杂志》1998,624(6):975-979
The reaction of one equivalent of In with a molten flux of (Ph4P)2Se5 and P2Se5 (1 : 2), at 250 °C gave the (Ph4P)[In(P2Se6)] ( I ). Stoichiometric elemental synthesis at 750 °C produced the Cs5In(P2Se6)2 ( II ). The thin, yellow crystals of ( I ), and the irregular, dark orange crystals of ( II ), appear to be air- and water-stable. Compound ( I ) crystallizes in the monoclinic space group C2/c (no. 15) and at 23 °C: a = 23.127(7) Å, b = 6.564(1) Å, c = 19.083(3) Å, β = 97.42(2)°, V = 2873(1) Å3, Z = 4, final R/Rw = 4.4/5.2%. Compound ( II ) crystallizes in the tetragonal space group P42/m (no. 84) and at 23 °C: a = b = 13.886(1) Å, c = 7.597(2) Å, V = 1464.9(3) Å3, Z = 2, final R/Rw = 3.9/5.1%. Compound ( I ) contains infinite [In(P2Se6)]nn– with a structure related to that of K2FeP2Se6. Compound ( II ) contains the discrete [In(P2Se6)2]5– which can be viewed as a fragment of the [In(P2Se6)]nn– chain. 相似文献
11.
The reaction of Ag2O and 2-amino-6-methylpyridine (AMP) with nicotinic acid (HNA) and isonicotinic acid (HINA), respectively, afforded two silver(I) complexes, [Ag2(NA)2(AMP)2] n (I) and [Ag2(INA)2(AMP)2] n (II). Both complexes were characterized by elemental analyses and X-ray single-crystal diffraction. Complex I is a pyridine-3-carboxylate bridged polynuclear silver(I) complex, in which the Ag atom is in a tetrahedral geometry, while complex II is a pyridine-4-carboxylate bridged polynuclear silver(I) complex, in which the Ag atom is in a distorted T-shaped geometry. The crystal of I is monoclinic: space group P21/c, a = 8.079(2), b = 17.150(3), c = 8.912(2) Å, β = 98.106(2)°, V = 1222.5(5) Å3, Z = 4. The crystal of II is monoclinic: space group P21/c, a = 7.225(1), b = 12.049(1), c = 15.053(2) Å, β = 102.050(1)°, V = 1281.6(3) Å3, Z = 4. 相似文献
12.
《Polyhedron》1988,7(14):1289-1298
The following adducts of Group III trialkyls with phosphines have been prepared, either by direct reaction in hydrocarbon solution or by displacement of ether from the metal trialkyl etherate: Me3M·PPh3 (M = Ga, In); Me3In·P(2-MeC6H4)3; (R3M)2·(Ph2PCH2)2 (R = Me, M = Al, Ga, In; R = Et, M = Ga, In; R = Bui, M = Al); (Me3M)3·(Ph2PCH2CH2)2PPh (M = Al, Ga, In) and (Me3M)4·(Ph2PCH2CH2PPhCH2)2 (M = Al, Ga, In). The compounds were analysed by 1H and 31P NMR spectra of (Me3M)2·(Ph2PCH2)2 (M = Ga, In) showed little change between 193 K and room temperature. Thermal dissociation of the adducts in vacuo gave the free metal trialkyl with no detectable contamination by the respective phosphine. Crystals of (Me3M)2·(Ph2PCH2)2 (M = Al, Ga, In) are iso-structural and the molecules contain two distorted tetrahedral metals bridged by the (Ph2PCH2)2; the MP distances are 2.544(4), 2.546(4) and 2.755(4) Å, respectively. The X-ray crystal structure of (Me3Al)3·(Ph2PCH2CH2)2PPh shows the molecule to contain distorted tetrahedral aluminium atoms bonded to each of the three phosphorus atoms, with AlP distances of 2.536(9) and 2.510(9) Å for the terminal and central moieties, respectively; the unit cell contains two such molecules plus one benzene molecule (the crystallizing solvent). 相似文献
13.
Olof Kristiansson 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(2):165-167
The bis(4‐aminopyridine)silver(I) cation in [Ag(C5H6N2)2]NO3 has the Ag atom on a twofold axis and displays an N—Ag—N angle of 174.43 (15)° and an Ag—N distance of 2.122 (3) Å. The two ligands are planar and the angle between the two ligand planes is 79.45 (9)°. The pyridine rings are stacked in piles with an interplanar distance of 3.614 (5) Å, a distance that strongly suggests that pyridine π–π interactions have an appreciable importance with respect to the non‐bonded crystal organization. The tris(2,6‐diaminopyridine)silver(I) cation in [Ag(C5H7N3)3]NO3 has Ag—N distances of 2.243 (2), 2.2613 (17) and 2.4278 (18) Å, and N—Ag—N angles of 114.33 (7), 134.91 (7) and 114.33 (7)°. The Ag+ ion is situated 0.1531 (2) Å from the plane defined by the three pyridine N atoms. 相似文献
14.
Yu. V. Kokunov Yu. E. Gorbunova V. V. Kovalev L. D. Popov S. A. Borodkin G. A. Razgonyaeva S. A. Kozyukhin 《Russian Journal of Inorganic Chemistry》2016,61(11):1397-1402
The coordination compound [Ag2L2(H2O)2] · 2H2O (I), L = C12H10NO2S has been synthesized by the reaction of AgNO3 with 4-methyl-2-quinolylthioacetic acid (HL) preliminarily neutralized with an equimolar amount of NBu4OH. Its crystal structure has been determined, and luminescence properties have been studied. Crystals of I are monoclinic, space group C2/c, a = 31.239(6) Å, b = 12.056(2) Å, c = 16.846(3) Å, β = 122.17(3)°, V = 5370.4(2) Å3, ρcalc = 1.861 g/cm3, Z = 16. The structure is formed by two crystallographically nonequivalent silver atoms Ag(1) and Ag(2) and two tridentate bridging ligands L coordinated through the S, N, and O atoms. These atoms, together with water molecules, form the coordination environments of the metal atoms with CN = 5 and 4, respectively. The Ag+ ions and the tridentate ligands form infinite [Ag4L4]n bands extended in the [001] direction. The presence of outer-sphere water molecules involved in O–H···O hydrogen bonding is responsible for the formation of a supramolecular framework structure. The photoluminescence spectrum of compound I shows two bands at ~450 and ~485 nm corresponding to the blue spectral range. 相似文献
15.
Osman Serindag Raymond D. W. Kemmitt John Fawcett David R. Russell 《Transition Metal Chemistry》1995,20(6):548-551
Summary Aminoalkanesulphonic acids H2N(CH2)
n
SO3H, (n = 1, 2 or 3) react with phosphonium salts [R2P(CH2OH)2]Cl (R = Ph or Cy, Cy = cyclohexyl) in the presence of Et3N to give the sulphonated aminomethylphosphines [Et3NH] [(R2PCH2)2N(CH2)
n
SO3] (R = Ph, n = 1, 2 or 3; R = Cy, n = 1). The single crystal X-ray structure of [Et3NH] [(Ph2PCH2)2N(CH2)2SO3] has been determined. Some NiII, PdII, PtII and RhI complexes of the phosphines have been prepared. 相似文献
16.
Gwo-Wei Tseng Maw-Cherng Suen Jhy-Der Chen Jiunn-Jer Hwang Yui Whei Chen-Yang Tai-Chiun Keng Ju-Chun Wang 《中国化学会会志》1999,46(4):545-550
The red complex trans-Mo2(O2CCH3)2(μ-dppa)2(BF4)2, 1 , was prepared by reaction of [Mo2(O2CCH3)2(CH3CN)6][BF4]2 with dppa (dppa = Ph2PN(H)PPh2) in THF. The reactions of Mo2(O2C(CH2)nCH3)4 with dppa and (CH3)3SiX (X = Cl or Br) afforded the complexes trans-Mo2X2(O2C(CH2)nCH3)2(μ-dppa)2 (X = Cl, n = 2, 2; X = Br, n = 2, 3; X = Cl, n = 10, 4 ; X = Cl, n = 12, 5 ). Their UV-vis, IR and 31P{1H}-NMR spectra have been recorded and the structures of 1, 2 and 3 have been determined. Crystal data for 1 : space group P21/n, a = 12.243(1) Å, b = 17.222(1) Å, c = 13.266(1) Å, β = 95.529(1)°, V = 2784.1(6) Å3, Z = 2, with final residuals R = 0.0509 and Rw = 0.0582. Crystal data for 24CH3Cl2: space group P21/n, a = 13.438(1) Å, b = 19.276(1) Å, c = 14.182(1) Å, β = 111.464(1)°, V = 3418.9(6) Å3, Z = 2, with final residuals R = 0.0492 and Rw = 0.0695. Crystal data for 3·4CH2Cl2: space group P21/n, a= 13.579(1) Å, b = 19.425(1) Å, c = 14.199(1) Å, β = 111.881(2)°, V = 3475.6(7) Å3, Z = 2, with final residuals R = 0.0703 and Rw = 0.0851. Comparison of the structural data shows that the effect of the axial ligand on weakening the Mo-Mo bond strength is X? > CH3CN > BF4?. The Tm values are 121.7 °C for 2 , 111.1 °C for 3 and 91.5 °C for 5 , respectively. 相似文献
17.
Coordination Chemistry of Diiodine and Implications for the Oxidation Capacity of the Synergistic Ag+/X2 (X=Cl,Br, I) System
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Dr. Przemysław J. Malinowski Dr. Daniel Himmel Prof. Dr. Ingo Krossing 《Angewandte Chemie (International ed. in English)》2016,55(32):9262-9266
The synergistic Ag+/X2 system (X=Cl, Br, I) is a very strong, but ill‐defined oxidant—more powerful than X2 or Ag+ alone. Intermediates for its action may include [Agm(X2)n]m+ complexes. Here, we report on an unexpectedly variable coordination chemistry of diiodine towards this direction: ( A )Ag‐I2‐Ag( A ), [Ag2(I2)4]2+( A ?)2 and [Ag2(I2)6]2+( A ?)2?(I2)x≈0.65 form by reaction of Ag( A ) ( A =Al(ORF)4; RF=C(CF3)3) with diiodine (single crystal/powder XRD, Raman spectra and quantum‐mechanical calculations). The molecular ( A )Ag‐I2‐Ag( A ) is ideally set up to act as a 2 e? oxidant with stoichiometric formation of 2 AgI and 2 A ?. Preliminary reactivity tests proved this ( A )Ag‐I2‐Ag( A ) starting material to oxidize n‐C5H12, C3H8, CH2Cl2, P4 or S8 at room temperature. A rough estimate of its electron affinity places it amongst very strong oxidizers like MF6 (M=4d metals). This suggests that ( A )Ag‐I2‐Ag( A ) will serve as an easily in bulk accessible, well‐defined, and very potent oxidant with multiple applications. 相似文献
18.
The title compounds, Mo(CO)2(Ph2PCH2PPh2)(Ph2PCH2CH2PPh2), Mo(CO)2(dppm)(dppe) 1, and Mo(CO)2(Ph2PCH2CH2PPh2)(Ph2PCH = CHPPh2), Mo(CO)2(dppe)(cis-vpp) 2, were prepared from Mo(CO)6 and the corresponding bidentate diphosphine ligands in n-decane under nitrogen atomosphere. Crystals of 1 are monoclinic, space group P 21/c, with a = 19.072(3), b = 11.348(3), c = 23.57(1) Å, β = 99.64(3)°, Z = 4, and the final residual R(F) = 0.044 for 4810 observed reflections; data of 2 are triclinic, space group P 1, with a = 12.091(3), b = 12.186(8), c = 18.934(5) Å, α = 96.93(4),β = 108.15(2), γ = 107.08(4)deg;, Z = 2, and the final residual R(F) = 0.058 for 4570 observed reflections. The distortion of compound 1 is more pronounced than that of compound 2, The two Mo-P lengths in the same bidentate chelate ligand for both compounds are different. Among them, the two larger Mo-P bond lengths for compound 2 are similar, but significantly different for 1. 相似文献
19.
The crystal structure of the title compound has been determined from 6049 X-ray diffractometric intensities with I > 3σ(I), and refined by a least-squares procedure to R = 0.050. The crystals are monoclinic, space group P21/n, a = 13.702(2) b = 14.255(2), c = 39.556(6) Å, β = 94.75(1)°, Z = 4. The structure of the cation displays two different coordination modes of the Ph2PCH2PPh2 ligands. Two of these are bidentate, bridging the Pt-Pt bond [2.769(1)Å] to form a Pt2(μ-Ph2PCH2PPh2)2 nucleus, while the third acts as a monodentate two-electron donor. The hydrido ligand was not located, but its position is inferred from the coordination geometry of the platinum atom to which it is bonded. The metalligand distances are: Pt-P(trans to P) 2.248(3)–2.289(4) and Pt—P(trans to Pt) 2.347(4) Å. 相似文献
20.
Di Sun Na Zhang Rong‐Bin Huang Lan‐Sun Zheng 《Acta Crystallographica. Section C, Structural Chemistry》2010,66(7):m174-m176
The asymmetric unit of the title compound, [Ag(NH3)2][Ag(C7H5N2O4)2], comprises half an [Ag(NH3)2]+ cation and half an [Ag(anbz)2]− anion (anbz is 2‐amino‐5‐nitrobenzoate). Both AgI ions are located on inversion centres. The cation has a linear coordination geometry with two symmetry‐related ammine ligands. The AgI cation in the anionic part shows a rare four‐coordinate planar geometry completed by two chelating symmetry‐related anbz ligands. Intra‐ and intermolecular N—H...O hydrogen bonds create a slightly undulating two‐dimensional supramolecular sheet. Adjacent sheets are only ca 3.3 Å apart. Ag...O, Ag...N and π–π stacking interactions consolidate the packing of the molecules in the solid state. 相似文献