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1.
Mitra Ghassemzadeh Forough Adhami Majid M. Heravi Abas Taeb Soheila Chitsaz Bernhard Neumüller 《无机化学与普通化学杂志》2002,628(13):2887-2893
The complexes [Cu(AMTTO)Cl2] ( 2 ), [Cu(AMTTO)2]Cl ( 3 ), and [Cu(AMTTO)(PPh3)2Cl] ( 4 ) have been prepared and characterized by IR spectroscopy and elemental analyses. Also single‐crystal X‐ray diffraction studies on compound 2 , 3 and 4 revealed that AMTTO acts in 2 as a bidentate ligand via nitrogen and sulfur atoms, in 3 and 4 as a monodentate via sulfur atoms. Complex 3 was already mentioned in literature, but the structure was not described in detail. The molecules in 2 form infinite chains through additional weak Cu—S interactions along [010] indicating the Jahn‐Teller distortion of the d9 ion Cu2+. The infinite chains are connected by hydrogen bonding along [100]. Crystal data for 2 at —80°C: monoclinic, space group P21/m, a = 666.7(1), b = 609.4(1), c = 1132.6(2) pm, b = 95.46(2)°, Z = 2, R1 = 0.0365; for 3 at —80°C: orthorhombic, space group Pbcn, a = 1291.2(2), b = 1146.5(1), c = 1000.5(1) pm, Z = 4, R1 = 0.0315; for 4 at —80°C: monoclinic, space group, P21/n, a = 879.4(1), b = 1849.3(2), c = 2293.8(3) pm, β = 92.38(1)°, Z = 4, R1 = 0.0688. 相似文献
2.
The reaction of [(AMTTO)PdCl2] ( 1 ) (AMTTO = 4-Amino-6-methyl-1,2,4-triazine-3(2H)-thione-5-one) with triphenylphosphane and sodium thiocyanate led to the air-stable crystalline complexes [(AMTTO)Pd(PPh3)Cl]Cl · MeOH ( 2 ) and [(AMTTO)Pd(SCN)2] · MeCN ( 3 ) in excellent yields. 2 and 3 have been characterized by IR and 31P NMR spectroscopy, elemental analyses as well as X-ray diffraction studies. Crystal data for 2 at –83 °C: monoclinic, space group P21/n, with a = 974.4(1), b = 988.6(1), c = 2750.7(2) pm, β = 98.16(1)°, Z = 4, R1 = 0.0241 and for 3 at –80 °C: orthorhombic, space group P212121, with a = 972.0(3), b = 1168.1(4), c = 1316.6(1) pm, Z = 4, R1 = 0.0817. 相似文献
3.
Mitra Ghassemzadeh Kioumars Aghapoor Majid M. Heravi Bernhard Neumüller 《无机化学与普通化学杂志》1998,624(12):1969-1972
The reaction of 4-amino-6-methyl-1,2,4-triazine-3(2H)-thione-5-one (AMTTO, 1 ) with palladium(II) chloride in acetonitrile/methanol leads to the N,S-coordinated complex [Pd(η2-AMTTO-N,S)Cl2] · CH3OH ( 2 ). 2 has been characterized by IR and MS techniques. The ligand 1 and the complex 2 were also investigated by X-ray structure determinations. 1 crystallizes in the space group P1¯ with the lattice dimensions at –70 °C: a = 419.6(1), b = 598.2(1), c = 1351.3(1) pm, α = 92.23(1), β = 91.20(1), γ = 100.51(1)°, Z = 2, R1 = 0.0441. 2 crystallizes in the space group P21/c with the lattice dimensions at 20 °C: a = 683.3(1), b = 1323.0(1), c = 1254.2(1) pm, β = 92.61(1)°, Z = 4, R1 = 0.0361. According to the structure analysis 1 consists of planar C,N-heterocycles connected by hydrogen bridges forming an infinite chain along [110]. The basic heterocyclic skeleton of 2 is essentially planar and linked three-dimensionally through hydrogen bridges. 相似文献
4.
Mitra Ghassemzadeh Samira Bahemmat Javad Malakootikhah Bernhard Neumüller Alexander Rothenberger 《无机化学与普通化学杂志》2007,633(8):1178-1182
The reactions of AMTTO = 4‐amino‐6‐methyl‐1,2,4‐triazine‐thione‐5‐one (AMTTO, 1 ) with 2‐hydroxybenzaldehyde (salicylaldehyde) and 4‐hydroxybenzaldehyde in methanol under reflux conditions led to the corresponding Schiff‐bases ( H2L1 and H2L2 ). The reaction of H2L1 with palladium acetate in ethanol and additional recrystallization from toluene gave the tetrameric complex [Pd(L)]4·2C7H8 ( 2 ). All compounds were characterized by infrared spectroscopy, elemental analyses as well as by X‐ray diffraction studies. Crystal data for H2L1 at ?80 °C: space group P21/c with a = 1285.4(1), b = 707.7(1), c = 1348.2(1) pm, β = 109.32(1)°, Z = 4, R1 = 0.0328, H2L2 at ?80 °C: space group P43212 with a = 762.5(1), b = 762.5(1), c = 4038.9(2) pm, Z = 8, R1 = 0.025 and for 2 at ?103 °C: space group C2/c with a = 2862.5(6), b = 2847.6(6), c = 1727.8(4) pm, β = 105.18(3)°, Z = 8, R1 = 0.0704. 相似文献
5.
Mitra Ghassemzadeh Forough Adhami Majid M. Heravi Abas Taeb Soheila Chitsaz Bernhard Neumüller 《无机化学与普通化学杂志》2001,627(5):815-819
The reaction of [(Ph3P)2CuCl]2 with 4‐amino‐6‐methyl‐1,2,4‐triazine‐thione‐5‐one (AMTTO, 1 ) in methanol and further recrystallization from methanol/acetone solution gives [(C4H4N3SON(=CMe2)Cu(PPh3)2Cl] ( 2 ) as a neutral complex. [(C4H4N3SON(=CMe2)Ag(PPh3)2]NO3 ( 4 ) can be obtained in excellent yield by the reaction of [(AMTTO)2Ag]NO3 ( 3 ) with triphenylphosphane in methanol/acetone. Both complexes were characterized by infrared spectroscopy, elemental analyses as well as by X‐ray diffraction studies. Crystal data for 2 at –80 °C: space group P1 with a = 1233.8(1), b = 1389.7(1), c = 1417.1(1) pm, α = 89.36(1)°; β = 65.10(1)°, γ = 65.95(1)°, Z = 2, R1 = 0.0582 and for 4 at –80 °C: space group P1, with a = 1193.3(1), b = 1308.5(1), c = 1385.3(1) pm, α = 94.69(1)°, β = 109.14(1)°, γ = 93.42(1)°, Z = 2, R1 = 0.0716. 相似文献
6.
Mitra Ghassemzadeh Masoomeh Tabatabaee Mostafa M. Pooramini Majid M. Heravi Abbas Eslami Bernhard Neumüller 《无机化学与普通化学杂志》2006,632(5):786-792
The reaction of 4‐amino‐6‐methyl‐1,2,4‐triazin‐thione‐5‐one (H2AMTTO, 1 ) with 4‐chlorobenzaldhyde led to the corresponding iminic compound {(4‐[(4‐chloro‐benzylidene)‐amino]‐6‐methyl‐3‐thioxo[1,2,4]‐triazin‐3,4‐dihydro(2H)‐5‐one), CAMTTO ( 2 ). Treatment of 2 with copper(I) chloride in chloroform gave the dimeric complex [{(CAMTTO)2CuCl}2]·2CHCl3 ( 3 ). Treatment of 2 with copper(I) chloride and silver(I) nitrate in the presence of the co‐ligand triphenylphophane gave the complexes [(CAMTTO)CuCl(PPh3)2] ( 4 ) and [(CAMTTO)Ag(PPh3)2]NO3·2CHCl3 ( 5 ). All compounds have been characterized by elemental analyses, 1H NMR spectroscopy, IR spectroscopy, and partly by mass spectrometry and X‐ray diffraction studies. In addition 4 and 5 have been characterized by 31P{1H} NMR spectroscopy. Crystal data for 2 at ?80 °C: monoclinic, space group P21/c, a = 1370.3(1), b = 767.8(1), c = 1268.7(1) pm, β = 107.12(1)°, Z = 4, R1 = 0.0379; for 3 at ?80 °C: monoclinic, space group P21/c, a = 1442.6(2), b = 878.8(1), c = 2558.7(3) pm, β = 95.31(1)°, Z = 2, R1 = 0.0746; for 4 at ?80 °C: triclinic, space group , a = 1287.9(1), b = 1291.7(1), c = 1359.5(1) pm, α = 90.44(1)°, β = 94.81(1)°, γ = 107.54(1)°, Z = 2, R1 = 0.0359 and for 5 at ?80 °C: triclinic, space group , a = 1060.5(1), b = 1578.2(2), c = 1689.6(2) pm, α = 87.70(1)°, β = 86.66(1)°, γ = 76.84(1)°, Z = 2, R1 = 0.0487. 相似文献
7.
Mitra Ghassemzadeh Majid M. Heravi Rahim Hekmat‐Shoar Bernhard Neumüller 《无机化学与普通化学杂志》2003,629(14):2438-2439
The reaction of 4‐Amino‐6‐methyl‐1, 2, 4‐triazine‐3(2H)‐thione‐5‐one (HAMTTO) with n‐butyl lithium in dimethoxyethane (DME) gives the complex [Li(DME)(AMTTO)] ( 1 ). 1 was characterized by elemental analysis, IR‐ and mass‐spectrometry and an X‐ray structure analysis [space group P21/n, Z = 4, lattice dimensions at —80 °C: a = 867.6(1), b = 1721.5(2), c = 931.8(1) pm, β = 112.81(1)°, R1 = 0.0315. The complex is a coordination polymer along [001] with a zig‐zag arrangement. 相似文献
8.
Forogh Adhami Masomeh Tabatabaee Mitra Gassemzadeh Bernhard Neumüller 《无机化学与普通化学杂志》2008,634(9):1466-1468
Reaction of 4‐amino‐6‐methyl‐1,2,4‐triazine‐3‐thione‐5‐on (AMTTO) as a bidentate ligand with silver nitrate and triphenyl phosphine as the co‐ligand make the centrosymmetric dimeric complex {[(AMTTO)Ag(PPh3)2]NO3}2·0.5CH3OH·0.5H2O ( 1 ). 1 was characterized by elemental analyses, IR‐ and NMR spectroscopy as well as X‐ray diffraction studies. The silver atom in 1 has distorted tetrahedral coordination. 1 crystallizes in triclinic space group . Crystal data for 1 at −80 °C: a = 1185.8(1), b = 1314.6(1), c = 1385.3(1) pm, α = 97.78(1)°, β = 111.38(1)°, γ = 92.41(1)°, Z = 2, R1 = 0.0377. 相似文献
9.
Mitra Ghassemzadeh Masomeh Tabatabaee Zohreh Mirrokni Bernhard Neumüller 《无机化学与普通化学杂志》2005,631(5):832-834
The reaction of 4‐Amino‐6‐methyl‐1, 2, 4‐triazine‐3(2H)‐thione‐5‐one (AMTTO, 1 ) with silver nitrate in methanol led to the dimeric complex {[(AMTTO)2Ag]NO3}2 ( 2 ). 2 was characterized by elemental analyses and IR spectroscopy as well as by X‐ray structure analysis. Crystal data for 2 at ?80 °C: crystal system orthorhombic, space group P212121 with a = 1043.6(1), b = 1329.6(1), c = 2358.4(1) pm, Z = 8 and R1 = 0.037. The cation possesses a highly distorted linear coordination sphere in the solid state. 相似文献
10.
S. Chitsaz H. Folkerts J. Grebe T. Grb K. Harms W. Hiller M. Krieger W. Massa J. Merle M. Mhlen B. Neumüller K. Dehnicke 《无机化学与普通化学杂志》2000,626(3):775-783
Crystal Structures of a Series of Compounds with Cations of the Type [R3PNH2]+, [R3PN(H)SiMe3]+, and [R3PN(SiMe3)2]+ The crystal structures of a series of compounds with cations of the type [R3PNH2]+, [R3PN(H)SiMe3]+, and [R3PN(SiMe3)2]+, in which R represents various organic residues, are determined by means of X‐ray structure analyses at single crystals. The disilylated compounds [Me3PN(SiMe3)2]+I–, [Et3PN(SiMe3)2]+I–, and [Ph3PN(SiMe3)2]+I3– are prepared from the corresponding silylated phosphaneimines R3PNSiMe3 with Me3SiI. [Me3PNH2]Cl (1): Space group P21/n, Z = 4, lattice dimensions at –71 °C: a = 686.6(1), b = 938.8(1), c = 1124.3(1) pm; β = 103.31(1)°; R = 0.0239. [Et3PNH2]Cl (2): Space group Pbca, Z = 8, lattice dimensions at –50 °C: a = 1272.0(2), b = 1147.2(2), c = 1302.0(3) pm; R = 0.0419. [Et3PNH2]I (3): Space group P212121, Z = 4, lattice dimensions at –50 °C: a = 712.1(1), b = 1233.3(2), c = 1257.1(2) pm; R = 0.0576. [Et3PNH2]2[B10H10] (4): Space group P21/n, Z = 4, lattice dimensions at –50 °C: a = 809.3(1), b = 1703.6(1), c = 1800.1(1) pm; β = 96.34(1)°; R = 0.0533. [Ph3PNH2]ICl2 (5): Space group P1, Z = 2, lattice dimensions at –60 °C: a = 825.3(3), b = 1086.4(3), c = 1241.2(4) pm; α = 114.12(2)°, β = 104.50(2)°, γ = 93.21(2)°; R = 0.0644. In the compounds 1–5 the cations are connected with their anions via hydrogen bonds of the NH2 groups with 1–3 forming zigzag chains. [Me3PN(H)SiMe3][O3S–CF3] (6): Space group P21/c, Z = 8, lattice dimensions at –83 °C: a = 1777.1(1), b = 1173.6(1), c = 1611.4(1) pm; β = 115.389(6)°; R = 0.0332. [Et3PN(H)SiMe3]I (7): Space group P21/n, Z = 4, lattice dimensions at –70 °C: a = 1360.2(1), b = 874.2(1), c = 1462.1(1) pm; β = 115.19(1)°; R = 0.066. In 6 and 7 the cations form ion pairs with their anions via NH … X hydrogen bonds. [Me3PN(SiMe3)2]I (8): Space group P21/c, Z = 8, lattice dimensions at –60 °C: a = 1925.4(9), b = 1269.1(1), c = 1507.3(4); β = 111.79(3)°; R = 0.0581. [Et3PN(SiMe3)2]I (9): Space group Pbcn, Z = 8, lattice dimensions at –50 °C: a = 2554.0(2), b = 1322.3(1), c = 1165.3(2) pm; R = 0.037. [Ph3PN(SiMe3)2]I3 (10): Space group P21, Z = 2, lattice dimensions at –50 °C: a = 947.7(1), b = 1047.6(1), c = 1601.6(4) pm; β = 105.96(1)°; R = 0.0334. 8 to 10 are built up from separated ions. 相似文献
11.
New Phosphorus-bridged Transition Metal Carbonyl Complexes. The Crystal Structures of [Re2(CO)7(PtBu)3], [Co4(CO)10(PtBu)2], [Ir4(CO)6(PtBu)6], and [Ni4(CO)10(PiPr)6], (PtBu)3 reacts with [Mn2(CO)10], [Re2(CO)10], [Co2(CO)8] and [Ir4(CO)12] to form the multinuclear complexes [M2(CO)7(PtBu)3] (M = Re ( 1 ), Mn ( 5 )), [Co4(CO)10(PtBu)2] ( 2 ) and [Ir4(CO)6(PtBu)6] ( 3 ). The reaction of (PiPr)3 with [Ni(CO)4] leads to the tetranuclear cluster [Ni4(CO)10(PiPr)6] ( 4 ). The complex structures were obtained by X-ray single crystal structure analysis: ( 1 : space group P1 (Nr. 2), Z = 2, a = 917.8(3) pm, b = 926.4(3) pm, c = 1 705.6(7) pm, α = 79.75(3)°, β = 85.21(3)°, γ = 66.33(2)°; 2 : space group C2/c (Nr. 15), Z = 4, a = 1 347.7(6) pm, b = 1 032.0(3) pm, c = 1 935.6(8) pm, β = 105.67(2)°; 3 : space group P1 (Nr. 2), Z = 4, a = 1 096.7(4)pm, b = 1 889.8(10)pm, c = 2 485.1(12) pm, α = 75.79(3)°, β = 84.29(3)°, γ = 74.96(3)°; 4 : space group P21/c (Nr. 14), Z = 4, a = 2 002.8(5) pm, b = 1 137.2(8) pm, c = 1 872.5(5) pm, β = 95.52(2)°). 相似文献
12.
Protonation and Methylation of 1, 1-Dicyanoethylene-2, 2-dithiolate Dianion. Preparative and Structural Investigations Protonation of alkaline metal salts of [S2C = C(CN)2]2? ( I ) in water yields a product of composition H2S2C4N2 ( II ). The species has to be formulated as dimere and crystallizes with two moles DMSO from DMSO solution with space group C2/c and a = 20.611(3), b = 4.800(1), c = 20.638(3) Å, β = 103.3(1)°, Z = 4. The X-ray structural analysis shows II to be a centrosymmetric 1, 3-Dithiacyclobutane system. On methylation of I with CH3I in the molar ratio 1:1, the monomethylated anion III can be isolated as AsPh4 salt. The compound crystallizes in the monoclinic space group P21/c, with a = 23.632(2), b = 14.304(1), c = 7.989(1) Å, β = 100.1(8)° and Z = 4. There are nearly planar anions [MeS(S)C?C(CN)2]? with an anti-conformation of the MeS group. 相似文献
13.
Diacetone Alcohol as Complex Ligand. Crystal Structures of [MnBr2{O=C(Me)CH2–C(Me)2OH}2] and [M{O=C(Me)CH2–C(Me)2OH}2][MCl4] with M = Fe, Co, and Zn The metal halides MnBr2 and MCl2 (M = Fe, Co, Zn) react with diacetone alcohol (4-hydroxy-4-methyl-2-pentanon) forming the title compounds, which are characterized by IR spectroscopy and crystal structure analyses. [MnBr2{O=C(Me)CH2–C(Me2)OH}2] ( 1 ): Space group C2/c, Z = 4, lattice dimensions at 293 K: a = 1189.2(4), b = 1317.2(3), c = 1200.0(3) pm, β = 102.25(3)°, R1 = 0.0256. In 1 the manganese atom is coordinated in a distorted octahedral fashion by the two cis bromine atoms and by the four oxygen atoms of the two diacetone alcohol chelating molecules. The distances Mn–[OH] (223.8 pm) and Mn–[O=C] (222.1 pm) are only slightly different. [M{O=C(Me)CH2–C(Me)2OH}2][MCl4] [M = Fe ( 2 ), Co ( 3 ), Zn ( 4 )]: 2 and 3 crystallize isotypically with each other in the space group Pc, Z = 4. Lattice dimensions for 2 at 293 K: a = 865.8(3), b = 926.3(2), c = 1401.5(1) pm, β = 104.19(2)°, R1 = 0.0421. Lattice dimensions for 3 at 293 K: a = 872.3(1), b = 925.7(1), c = 1394.2(3) pm, β = 104.79(2)°, R1 = 0.0481. As in 1 , the metal atoms of the [M{O=C(Me)CH2–C(Me)2OH}2]2+ ions in 2 and 3 are chelated in a distorted octahedral fashion by two diacetone alcohol molecules and associated cis via two μ-Cl atoms of the [MCl4]2– anions to form strands. [Zn{O=C(Me)CH2–C(Me)2OH}2][ZnCl4] ( 4 ): Space group C2/c, Z = 4. Lattice dimensions at 213 K: a = 1582.27(13), b = 1356.15(13), c = 941.93(7) pm, β = 107.283(10)°, R1 = 0.0328. The zinc atom of the dication in 4 is associated in a distorted octahedral fashion by the two diacetone alcohol chelating molecules in the equatorial positions and trans by two μ-Cl atoms of the [ZnCl4]2– ions to form strands. 相似文献
14.
Mohammad Yazdanbakhsh Mohammad Hakimi Majid M. Heravi Mitra Ghassemzadeh Bernhard Neumüller 《无机化学与普通化学杂志》2005,631(5):924-927
The reaction of 4‐amino‐1,2,4‐Δ2‐triazoline‐5‐thione (ATT, 1 ) with AgNO3 in methanol led to the complex [Ag(ATT)2]NO3 ( 2 ). 2 was characterized by elemental analyses, 1H NMR, IR, and Raman spectroscopy as well as single‐crystal X‐ray diffraction. The molecular structure of 1 was also determined by single crystal X‐ray analysis. Crystal data for 1 at ?80 C: space group C2/c with a = 2107.4(2), b = 1425.1(1), c = 688.4(1) pm, β = 104.55(1)°, Z = 16, R1 = 0.0514, crystal data for 2 at ?80 °C: space group P21/c with a = 675.7(1), b = 1321.1(1), c = 1311.2(1) pm, β = 90.03(1)°, Z = 4, R1 = 0.0437. 相似文献
15.
Pyridinium Chlorometallates of Lanthanoid Elements. Crystal Structures of [HPy]2[LnCl5(Py)] mit Ln = Eu, Er, Yb und von [H(Py)2][YbCl4(Py)2] · Py The pyridinium chlorometallates [HPy]2[LnCl5(Py)] with Ln = Eu, Er and Yb, as well as [H(Py)2][YbCl4(Py)2]·Py have been obtained by the reaction of diacetone alcohol with solutions of the corresponding metal trichlorides in pyridine at 100 °C. According to the crystal structure determinations the anions [LnCl5(Py)]2— are linked by bifurcated Cl···H···Cl bridges with the protons of the [HPy]+ cations forming chains along [001]. The anions of [H(Py)2][YbCl4(Py)2]·Py form discrete octahedrons with trans‐positions of the pyridine ligands. [HPy]2[EuCl5(Py)] ( 1a ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1874.4(2), b = 1490.2(2), c = 741.5(1) pm, R1 = 0.0466. [HPy]2[ErCl5(Py)] ( 1b ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1864.3(1), b = 1480.7(2), c = 739.7(1) pm, R1 = 0.0314. [HPy]2[YbCl5(Py)] ( 1c ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1858.9(2), b = 1479.0(1), c = 736.8(1) pm, R1 = 0.0306. [H(Py)2][YbCl4(Py)2]·Py ( 2 ·Py): Space group Ia, Z = 4, lattice dimensions at —80 °C: a = 1865.5(1), b = 827.5(1), c = 1873.4(1) pm, ß = 103.97(1)°, R1 = 0.0258. 相似文献
16.
Colorless single crystals of Cd[AlCl4]2 grow from the melt of CdCl2 and AlCl3 upon slow cooling from 250°C. The crystal structure [monoclinic, P1a1, Z = 2, a = 1288.7(2), b = 660.2(1), c = 705.1(1) pm, β = 92.89(1)º] may be derived from hexagonally closest packed layers of Cl?. Octahedral and tetrahedral holes are filled with Cd2+ and Al3+ in a 1:2 ratio between all layers stacked in the [104] direction. Cd[GaCl4]2 and Cd[AlBr4]2 are isotypic. Reduction of Cd[AlCl4]2 with excess cadmium shot and slow cooling from 350°C yields plate-like very moisture-sensitive, colorless single crystals of Cd2[AlCl4]2. The crystal structure [triclinic, C1 , Z = 2, a = 655.47(3), b = 1135.26(1), c = 935.23(6) pm, α = 89.70(2)º, β = 103.61(1)º, γ = 90.455(1)º] is built from slabs stacked in the [100] direction consisting of ethane-like [Cd2Cl6] units with a Cd? Cd distance of 256.1 pm sharing common vertices with [AlCl4] tetrahedra. 相似文献
17.
Halomercurates: Syntheses and Crystal Structures of [Cu(en)2][Hg2Cl6], [Cu(en)2][Hg2Br6], and [Cu(en)2][HgBr4] Crystals of [Cu(en)2][Hg2Cl6] ( 1 ) have been obtained by layering a solution of Hg(NO3)2 and NaCl with a solution of [Cu(en)2]SO4. An analogous procedure, using NaBr instead of NaCl, gave crystals of [Cu(en)2][HgBr4] ( 3 ). Crystals of [Cu(en)2][Hg2Br6] ( 2 ) were obtained by gel crystallization using the same starting materials as for 3 . The complexes show very low solubility. The dinuclear anions of 1 consist of two nearly planar HgCl3 units related by a center of symmetry. In 2 infinite anionic chains are present, made up of parallel HgBr3 units. These units are packed in such a way as to produce a trigonal bipyramidal configuration around the Hg atoms. 3 contains mononuclear deformed tetrahedral [HgBr4]2– anions. In all three complexes the packing of the ions is such that halogen atoms of halomercurate anions complete a tetragonal bipyramidal coordination at Cu. The resulting Cu–Halogen distances are 2.924 Å for 1 , 3.036 Å for 2 and 3.085 and 3.119 Å for 3 . 1 : Space group P 1, Z = 1, lattice constants at 20 °C: a = 7.000(2), b = 7.526(2), c = 8.239(2) Å; α = 88.39(2), β = 86.06(2), γ = 86.10(3)°; R1 = 0.040. 2 : Space group P21/c, Z = 2, lattice constants at –50 °C: a = 7.185(1), b = 16.338(2), c = 7.814(1) Å; β = 94.88(2)°; R1 = 0.033. 3 : Space group P21/n, Z = 4, lattice constants at 20 °C: a = 8.055(3), b = 13.101(3), c = 13.814(3) Å; β = 91.24(3)°; R1 = 0.092. 相似文献
18.
Preparation, Crystal Structures, Vibrational Spectra, and Normal Coordinate Analysis of Four Linkage Isomeric Tetrachlorodirhodanoosmates(IV) By treatment of cis- or trans-[OsCl4I2]2? with (SCN)2 in dichloromethane the linkage isomers cis-[OsCl4(NCS)2]2? ( 1 ), trans-[OsCl4(NCS)(SCN)]2? ( 2 ), cis-[OsCl4(NCS)(SCN)]2? ( 3 ) and trans-[OsCl4(SCN)2]2? ( 4 ) are formed which have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The X-Ray structure determinations on single crystals of cis-(Ph4As)2[OsCl4(NCS)2] (triclinic, space group P1 , a = 10.019(5), b = 11.702(5), c = 21.922(5) Å, α = 83.602(5)°, β = 85.718(5)°, γ = 73.300(5)°, Z = 2), trans-(Ph4As)2[OsCl4 · (NCS)(SCN)] (monoclinic, space group P21/c, a = 18.025(5), b = 11.445(5), c = 23.437(5) Å, β = 94.208(5)°, Z = 4), cis-(Ph4As)2[OsCl4(NCS)(SCN)] (triclinic, space group P1 , a = 10.579(5), b = 11.682(5), c = 22.557(5) Å, α = 81.073(5)°, β = 85.807(5)°, γ = 87.677(5)°, Z = 2) and trans-(Ph4As)2 · [OsCl4(SCN)2] (triclinic, space group P1 , a = 10.615(5), b = 11.691(5), c = 11.907(5) Å, α = 111.314(5)°, β = 96.718(5)°, γ = 91.446(5)°, Z = 1) reveal the complete ordering of the complex anions. The via N or S coordinated thiocyanate groups are located nearly direct above one of the cis-positioned Cl ligands with Os? N? C angles of 171.2° and 174.3° ( 1 ), 162.3° ( 2 ), 172° ( 3 ) and Os? S? C angles of 108.3° ( 2 ), 105.7° ( 3 ) and 105.5° ( 4 ). Using the molecular parameters of the X-Ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts of all four linkage isomers are assigned by normal coordinate analyses based on a modified valence force field. The valence force constants are fd(OsN) = 1.59 ( 1 ), 1.67 ( 2 ), 1.60 ( 3 ) and fd(OsS) = 1.27 ( 2 ), 1.31 ( 3 ) and 1.32 mdyn Å?1 ( 4 ). Taking into account increments of the trans influence a good agreement between observed and calculated frequencies is achieved. 相似文献
19.
Treatment of the ligand 6‐aza‐2‐thiothymine (ATT, HL, 1 ) with palladium chloride in methanol forms the ionic complex [(HL)4Pd]Cl2·8MeOH ( 2 ), while its reaction with palladium iodide in same solvent produces the neutral complex trans‐[(HL)2PdI2]·2MeOH ( 3 ) in high yields. The reaction of 1 with Na2[PdCl4] in the presence of sodium acetate in a molar ratio of 2:1:2 and with platinum(II) chloride in presence of sodium acetate led to the dimer tetranuclear complexes [(L4Pd2)NaCl]2·8MeOH ( 4 ) and [L4Pt2Cl2]·6MeOH·H2O ( 5 ). The latter is the first PtIII complex of the ligand. All complexes were characterized by elemental analyses and IR spectroscopy and the crystal structures of 2 , 3 , 4 and 5 are determined by single‐crystal X‐ray diffraction. Crystal data for 2 at ?80 °C: triclinic space group , a = 1006.6(1), b = 1006.9(1), c = 1158.1(1) pm, α = 85.20(1)°, β = 83.84(1)°, γ = 88.91(1)°, Z = 1, R1 = 0.0278; for 3 at ?80 °C: triclinic space group , a = 490.5(1), b = 977.2(2), c = 1116.8(2) pm, α = 90.26(1)°, β = 102.33(1)°, γ = 96.08(1)°, Z = 1, R1 = 0.0394; for 4 at ?80 °C: orthorhombic space group Ccca, a = 1791.7(2), b = 1874.1(2), c = 2044.0(1) pm, Z = 4, R1 = 0.0341 and for 5 at ?80 °C: monoclinic space group P21/c, a = 1464.3(1), b = 2003.7(1), c = 1368.5(1) pm, β = 95.66(1)°, Z = 4, R1 = 0.0429. 相似文献
20.
Synthesis and Crystal Structures of the Samarium Complexes [SmI2(DME)3] and [Sm2I(NPPh3)5(DME)] When treated with ultrasound, the reaction of samarium metal with N-iodine-triphenylphosphaneimine in 1,2-dimethoxyethane (DME) leads to the two samarium complexes [SmI2(DME)3] ( 1 ) and [Sm2I(NPPh3)5(DME)] ( 2 ), which are separated from each other by fractional crystallization. 1 could be isolated in two different crystallographic forms, namely as brownish black crystals ( 1 a ) and as violet-black crystals ( 1 b ), both of them are characterized by crystal structure analyses. 1 a : Space group P21/c, Z = 4, lattice dimensions at –80 °C: a = 1459.4(1), b = 1314.4(1), c = 2293.6(2) pm, β = 99.245(8)°, R = 0.0344. The structure of 1 a holds two crystallographically independent molecules [SmI2(DME)3], in which the samarium atoms have coordination number eight. The two individuals differ from each other particularly in their I–Sm–I bond angles, which are 157.94 and 178.45°. 1 b : Space group P21, Z = 2, lattice dimensions at –80 °C: a = 849.4(3), b = 1060.1(3), c = 1235.1(6) pm, b = 93.86(5)°, R = 0.0251. 1 b has a molecular structure similar to that of 1a with a bond angle I–Sm–I of 158.40°. The phosphoraneiminato complex [Sm2I(NPPh3)5(DME)] ( 2 ) forms colourless, moisture sensitive crystals which contain two molecules DME per formula unit. 2 · 2 DME: Space group P1, Z = 2, lattice dimensions at –80 °C: a = 1405.0(4), b = 1656.5(3), c = 2208.3(7) pm, α = 89.60(3)°, β = 72.96(4)°, γ = 78.70(3)°, R = 0.0408. In 2 the two samarium atoms are linked via the μ-N atoms of two phosphoraneiminato ligands to form a planar Sm2N2 four-membered ring. One of the Sm atoms is terminally coordinated by the N atoms of two (NPPh3)– groups, thus achieving a distorted tetrahedral surrounding. The second Sm atom is coordinated by the N atom of one (NPPh3)– group, by the terminally bonded iodine atom, and by the O atoms of the DME chelate, thus achieving a distorted octahedral surrounding. 相似文献