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1.
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   

2.
The reaction of 4‐amino‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)‐thione (AMTT, 1 ) with 4‐methoxy benzaldehyde and 3‐methoxybenzaldehyde in methanol led to the iminic derivatives 4‐(4‐methoxybenzylideneamino)‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)thione ( 2 , L1) and 4‐(3‐methoxybenzylideneamino)‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)‐thione ( 3 , L2). The reaction of the latter with [(PPh3)2CuCl] in methanol solution gave the first CuI complex of 3 , [(PPh3)2CuCl(L2)] ( 4 ) and in chloroform solution the complex [(PPh3)2CuCl(L2)]·2CHCl3 ( 5 ). All compounds were characterized by infrared spectroscopy, elemental analyses as well as by X‐ray diffraction studies. Crystal data for 2 at ?80 °C: space group P21/c with a = 1351.3(3), b = 399.4(1), c = 2225.2(5) pm, β = 96.50(2)°, Z = 4, R1 = 0.0667, for 3 at ?80 °C: space group R3c with a = b = 3020.4(2), c = 708.2(1) pm, Z = 18, R1 = 0.0435, for 4 at ?80 °C: space group P21/c with a = 1427.8(1), b = 1129.0(1), c = 2622.8(2) pm, β = 97.19(1)°, Z = 4, R1 = 0.0517 and for 5 at ?80 °C: space group with a = 1280.5(1), b = 1316.1(1), c = 1731.4(1) pm, α = 78.14(1)°, β = 86.06(1)°, γ = 64.69(1)°, Z = 2, R1 = 0.0525.  相似文献   

3.
The reaction of 4‐amino‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)‐thione (AMTT, 1 ) with AgNO3 and triphenylphosphane in a molar ratio 1:1:2 in ethanol led to the dimeric complex {[Ag(AMTT)(PPh3)2]NO3}2·4EtOH ( 2 ). 2 was characterized by elemental analyses, IR, 31P NMR spectroscopy as well as single crystal X‐ray diffraction. Crystal data for 2 at ?80 °C: space group with a = 1265.5(2), b = 1300.9(2), c = 1509.5(2) pm, α = 83.77(2)°, β = 79.22(2)°, γ = 62.89(2)°, Z = 2, R1 = 0.0330.  相似文献   

4.
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   

5.
The reaction of 4‐amino‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)‐thione (AMTT) with 4‐methylbenzaldehyde and 4‐methoxybenzaldehyde in ethanol led to the iminic derivatives ‐4‐(4‐methylbenzylideneamino)‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)thione ( L1 ) and 4‐(4‐methoxybenzyl‐ideneamino)‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)‐thione ( L2 ). The reaction of L1 with CuCl in the presence of triphenylphosphane as co‐ligand in methanol/chloroform solution gave the CuI complex containing L1 , [Cu( L1 )(PPh3)2Cl]·0.5CH3OH·0.25CHCl3 ( 1 ). Treatment of L2 with the same metal salt in a molar ratio of 1:1 in methanol and further addition of a solution of PPh3 in chloroform led to the complex [Cu( L2 )(PPh3)2Cl]·2.5CHCl3 ( 2 ). The complexes and L1 were characterized by IR and NMR spectroscopy as well as by X‐ray diffraction studies. In both complexes, the Schiff base ligand is coordinated to the copper ion through its sulfur atom. The other coordination sites around the copper ion are occupied by two triphenylphosphane molecules and one chloride ion. Therefore, each CuI ion is in a distorted tetrahedral environment. Crystal data for L1 at ?100 °C: space group P21/n with a = 720.5(1), b = 1140.6(1), c = 1426.3(2) pm, β = 91.25(1)°, Z = 4, R1 = 0.03, for 1 at ?120 °C : space group with a = 1286.3(1), b = 1740.3(1), c = 2060.2(1) pm, α = 79.085(6), β = 83.827(5), γ = 76.688(6)°, Z = 4, R1 = 0.0649 and for 2 at ?80 °C : space group with a = 1183.7(2), b = 1370.1(2), c = 1812.1(3) pm, α = 85.69(2), β = 88.52(2), γ = 64.89(2)°, Z = 2, R1 = 0.0488.  相似文献   

6.
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   

7.
The reactions of 4‐amino‐5‐methyl‐2H‐1,2,4‐triazole‐3(4H)‐thione (AMTT, L1 ) with 2‐thiophen carbaldehyde, salicylaldehyde and 2‐nitrobenzaldehyde in methanol led to the corresponding Schiff‐bases ( L1a‐c ). The reaction of L1 with [(PPh3)2Cu]NO3 in ethanol gave the ionic complex [(PPh3)2Cu(L1)]NO3·EtOH ( 2 ) All compounds were characterized by infrared spectroscopy, elemental analyses as well as by X‐ray diffraction studies. Crystal data for L1a at 20 °C: space group P21/n with a = 439.6(2), b = 2074.0(9), c = 1112.8(4) pm, β = 93.51(3)°, Z = 4, R1 = 0.0406, L1b at ?80 °C: space group P21/n with a = 1268.9(2), b = 739.3(1), c = 1272.5(1) pm, β = 117.97(1)°, Z = 4, R1 = 0.0361, L1c at ?80 °C: space group P21/n with a = 847.8(1), b = 1502.9(2), c = 981.5(2) pm, β = 110.34(1)°, Z = 4, R1 = 0.0376 and for 2 at ?80 °C: space group with a = 1247.8(1), b = 1270.3(1), c = 1387.5(1) pm, α = 84.32(1)°, β = 84.71(1)°, γ = 63.12(1)°, Z = 2, R1 = 0.0539.  相似文献   

8.
The reaction of of 4‐amino‐5‐ethyl‐2H‐1,2,4‐triazole‐3(4H)‐thione (AETT, L ) with furfural in methanol led to the corresponding Schiff‐Base ( L1 ). The reaction of L1 with [Cu(PPh3)2]Cl in methanol gave to the neutral compound [( L1 )Cu(PPh3)2Cl] ( 1 ). By recrystallization of 1 from CH3CN the complex [( L1 )Cu(PPh3)2Cl]·CH3CN ( 1a ) was obtained. All compounds were characterized by infrared spectroscopy, elemental analyses as well as by X‐ray diffraction studies. Crystal data for L1 at ?80 °C: space group with a = 788.4(1), b = 830.3(2), c = 928.8(2) pm, α = 84.53(1)°, β = 65.93(1)°, γ = 72.02(1)°, Z = 2, R1 = 0.0323; for 1 at ?100 °C: space group with a = 1166.3(1), b = 1423.8(2), c = 1489.1(2) pm, α = 62.15(1)°, β = 72.04(1)°, γ = 88.82(1)°, Z = 2, R1 = 0.0338 and for 1a at ?100 °C: space group P21/c with a = 1294.1(1), b = 1019.8(2), c = 3316.9(4) pm, β = 94.73(1)°, Z = 4, R1 = 0.0435.  相似文献   

9.
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   

10.
Pyridine Complexes of Rare Earth Element Trichlorides. Syntheses and Crystal Structures of [YCl3(py)4] and [LnCl3(py)4] · 0.5 py with Ln = La and Er The pyridine complexes [YCl3(py)4] ( 1 ), [LaCl3(py)4] · 0.5 py ( 2 · 0.5 py), and [ErCl3(py)4] · 0.5 py ( 3 · 0.5 py) have been prepared from the diacetone‐alcohol complexes [LnCl3(DAA)2] or directly from the metal trichlorides with excess pyridine to give colourless, only sparingly moisture sensitive crystals. They were characterized by IR spectroscopy and by crystal structure determinations. 1 : Space group Pbca, Z = 16, lattice dimensions at –80 °C: a = 1647.4(1), b = 1743.1(1), c = 3190.5(1) pm, R1 = 0.031. 2 · 0,5 Py: Space group P21/n, Z = 4, lattice dimensions at –80 °C: a = 978.9(1), b = 1704.5(1), c = 1589.5(1) pm, β = 103.61(1)°, R1 = 0.0281. 3 · 0,5 Py: Space group P21/n, Z = 4, lattice dimensions at –80 °C: a = 970.1(1), b = 1706.4(1), c = 1566.1(1) pm, β = 103.46(1)°, R1 = 0.0232. All complexes realize monomeric molecular structures with the metal atom in a distorted pentagonal‐bipyramidal coordination. One of the chlorine atoms and the four pyridine molecules are in the equatorial plane.  相似文献   

11.
The reaction of 4‐amino‐1, 2, 4‐triazin‐3(2H)‐thione‐5‐one (ATTO, 1 ) with [Cu(PPh3)2]NO3 in ethanol led to the complex [Cu(PPh3)2(ATTO)]NO3 ( 2 ). 2 was characterized by elemental analyses, IR, 1H NMR and Raman spectroscopy. A single‐crystal X‐ray diffraction of compound 2 revealed that ATTO acts as a bidentate ligand via its nitrogen and sulfur atoms. Crystal data for 2 at 20 °C: space group P21/n with a = 975.7(1), b = 1533.5(2), c = 2504.2(3) pm, β = 92.25(1)°, Z = 4, R1 = 0.0632.  相似文献   

12.
The reaction of 4‐amino‐6‐methyl‐1,2,4‐triazine‐3‐thione‐5‐one, HAMTTO, with silver (I) nitrate in methanol led under deprotonation to the polymeric compound [(AMTTO)Ag]n. The coordination polymer {[Ag(HAMTTO)]ClO4}n ( 1 ) is synthesized from the reaction of the latter polymeric compound with perchloric acid. Both compounds were characterized by elemental analysis and IR spectroscopy. Single‐crystal X‐ray diffraction studies on compound 1 showed that HAMTTO acts as a bidentate ligand and chelates the silver atom via its hydrazine nitrogen atom and its sulfur atom. Crystal data for 1 at ?90 °C: space group P21, Z = 2, a = 629.3(1), b = 748.7(1), c = 1071.7(1) pm, β = 98.28(1)°, R1 = 0.0533.  相似文献   

13.
The complexes cis‐[SnCl4(H2O)2]·2H2O ( 1 ), [Sn2Cl6(OH)2(H2O)2]·4H2O ( 3 ), and [HL][SnCl5(H2O)]·2.5H2O ( 4 ) were isolated from a CH2Cl2 solution of equimolar amounts of SnCl4 and the ligand L (L=3‐acetyl‐5‐benzyl‐1‐phenyl‐4, 5‐dihydro‐1, 2, 4‐triazine‐6‐one oxime, C18H18N4O2) in the presence of moisture. 1 crystallizes in the monoclinic space group Cc with a = 2402.5(1) pm, b = 672.80(4) pm, c = 1162.93(6) pm, β = 93.787(6)° and Z = 8. 4 was found to crystallize monoclinic in the space group P21, with lattice parameters a = 967.38(5) pm, b = 1101.03(6) pm, c = 1258.11(6) pm, β = 98.826(6)° and Z = 2. The cell data for the reinvestigated structures are: [SnCl4(H2O)2]·3H2O ( 2 ): a = 1227.0(2) pm, b = 994.8(1) pm, c = 864.0(1) pm, β = 103.86(1)°, with space group C2/c and Z = 4; 3 : a = 961.54(16) pm, b = 646.29(7) pm, c = 1248.25(20) pm, β = 92.75(1)°, space group P21/c and Z = 4.  相似文献   

14.
The reaction of an ethanolic solution 2,6‐pyridinedicarboxylic acid ( 1 , LH2) with TlNO3 in the presence of triethylamine led to the coordination polymer [Tl(LH)]n ( 2 ). The complex was characterized by elemental analysis, IR spectroscopy and single‐crystal X‐ray diffraction. Crystal data for 2 at –80 °C: monoclinic, space group I2/a, a = 696.1(1), b = 1190.6(2), c = 931.0(2) pm, β = 103.28(1)°, Z = 4, R1 = 0.0256.  相似文献   

15.
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   

16.
Phosphanimine and Phosphoraneiminato Complexes of Beryllium. Crystal Structures of [BeCl2(HNPPh3)2], [BeCl(HNPPh3)2(Py)]Cl, and [Be3Cl2(NPPh3)4] Tetraphenylphosphonium hexachlorodiberyllate, (Ph4P)2[Be2Cl6], reacts with lithium phosphoraneiminate, [LiNPPh3]6, in dichloromethane to give the three‐nuclear beryllium phosphoraneiminate [Be3Cl2(NPPh3)4] ( 3 ). As a by‐product the phosphaneimine complex [BeCl2(HNPPh3)2] ( 1 ) can be isolated, which reacts with pyridine to give the ionic complex [BeCl(HNPPh3)2(Py)]Cl ( 2 ). On the other hand, the silylated phosphanimine Me3SiNP(p‐tolyl)3 ( 5 ) does not react with BeCl2 or (Ph4P)2[Be2Cl6] forming the expected phosphoraneiminates. From CH2Cl2 solutions only the amino‐phosphonium salt [(C7H7)3PNH2]Cl ( 4 ) can be obtained. The compounds 1 ‐ 5 are characterized by single X‐ray analyses and by IR spectroscopy. 1 ·C7H8: Space group C2/c, Z = 4, lattice dimensions at 193 K: a = 1408.9(2), b = 1750.9(2), c = 1633.2(2) pm, β = 106.50(1)°; R1 = 0.0385. 1 forms a molecular structure with short Be—N distances of 169.8(3) pm. 2 ·Py: Space group P1¯, Z = 4, lattice dimensions at 193 K: a = 969.5(1), b = 2077.1(2), c = 2266.4(2) pm, α = 72.24(1)°, β = 87.16(1)°, γ = 77.42(2)°, R1 = 0.0776. 2 forms ion pairs in which the NH atoms of the phosphaneimine ligands act as hydrogen bridges with the chloride ion. The HNPPh3 ligand realizes short Be—N bonds of 169.0(6) pm, the Be—N distance of the pyridine molecule is 182.5(6) pm. 3 ·3CH2Cl2: Space group P1¯, Z = 2, lattice dimensions at 193 K: a = 1333.2(2), b = 1370.2(2), c = 2151.8(3) pm, α = 107.14(1)°, β = 91.39(1)°, γ = 105.15(1)°, R1 = 0.0917. The structure of the three‐nuclear molecule 3 corresponds with a Be2+ ion which is tetrahedrally coordinated by the nitrogen atoms of two {ClBe(NPPh3)2} chelates. 4 ·CH2Cl2: Space group P21/c, Z = 4, lattice dimensions at 193 K: a = 1206.6(2), b = 1798.0(2), c = 1096.2(1) pm, β = 97.65(1)°, R1 = 0.0535. 4 forms dimeric units in which the NH2 groups of the [(C7H7)3PNH2]+ cations act as hydrogen bridges with the chloride ions to give centrosymmetric eight‐membered rings. 5 : Space group P21/n, Z = 4, lattice dimensions at 193 K: a = 1074.3(2), b = 2132.2(3), c = 1075.5(2) pm, β = 110.68(1)°, R1 = 0.0664. 5 forms molecules with distances PN of 154.6(3), SiN of 168.8(3) pm, and bond angle SiNP of 134.4(2)°.  相似文献   

17.
The reaction of solution 2,6‐pyridinedicarboxylic acid and 1,10‐phenanthroline ( 1 ) with CrCl3·6H2O led to the complex [Cr(phen)(pydc)(H2O)][Cr(pydc)2]·4H2O ( 2 ) (phen is 1,10‐phenanthroline and pydcH2 is 2,6‐pyridinedicarboxylic acid). 2 was characterized by elemental analysis, IR spectroscopy and single‐crystal structure determination. Crystal data for 2 at ?80 °C: triclinic, space group , a = 818.5(1), b = 1492.2(1), c = 1533.6(2) pm, α = 76.45(1)°, β = 84.22(1)°, γ = 77.99(1)°, Z = 2, R1 = 0.0416.  相似文献   

18.
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   

19.
Trichloroberyllate Complexes of Dimethyl Cyanamide, Morpholine, and 4,4′‐Bipyridine The trichloroberyllate complexes (Ph4P)[BeCl3(NCNMe2)] ( 1 ), (Ph4P)[BeCl3{HN(CH2)4O}] ( 2 ), and (Ph4P)2[(BeCl3)2(4,4′‐bipy)] ( 3 ) were prepared by reactions of (Ph4P)2[Be2Cl6] with dimethyl cyanamide, trimethylsilylmorpholinate, and 4,4′‐bipyridine, respectively, in dichloromethane solutions. 1 ‐ 3 were characterized by X‐ray crystallography and by IR‐spectroscopy. 1 ·CH2Cl2: Space group P1, Z = 1, lattice dimensions at 173 K: a = 714.2(1), b = 919.5(2), c = 1233.4(2) pm, α = 94.97(1)°, β = 90.86(1)°, γ = 111.90(1)°, R1 = 0.0310. In the complex anion [BeCl3(NCNMe2)]? the dimethyl cyanamide ligand is coordinated via a linear Be–N≡C‐NMe2 arrangement, the CH2Cl2 molecules forming linear chains by hydrogen bridges ···HCH···Cl··· with the chlorine atoms of the {BeCl3?} groups. 2 : Space group , Z = 2, lattice dimensions at 173 K: a = 1050.9(1), b = 1099.7(1), c = 1308.3(2) pm, α = 87.57(1)°, β = 70.97(1)°, γ = 74.58(1)°, R1 = 0.0397. The complex anions are dimerized by centrosymmetric puckered eight‐membered [Be–N–H···Cl]2 rings. 3 ·2CH2Cl2: Space group , Z = 2, lattice dimensions at 173 K: a = 1095.4(1), b = 1559.6(2), c = 1869.8(3) pm, α = 79.12(1)°, β = 73.83(1)°, γ = 78.76(1)°, R1 = 0.0548. The complex contains dianions [Cl3Be(μ‐bipy)BeCl3]2? with Be–N distances of 177.0(6) and 178.5(6) pm. Both {BeCl3}? groups form C–H···Cl hydrogen bridges with the dichloromethane molecules.  相似文献   

20.
The reaction of copper(I) chloride with 6‐aza‐2‐thiothymine (ATT, 1 ) and triphenylphosphane in methanol/chloroform gives [(ATT)CuCl(PPh3)] ( 2 ) as a neutral complex. [(ATT)Ag(NO3)(PPh3)2]·MeOH ( 3 ) can be obtained by the reaction of 1 with silver(I) nitrate and triphenylphosphane in methanol/chloroform in excellent yields and the single crystals of 3 can be obtained from acetonitril solution. 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 I2/a with a = 1859.3(1), b = 1143.2(1), c = 2208.2(1) pm, β = 104.84(1)°, Z = 8, R1 = 0.0355 and for 3 at —80 °C: space group P21/c with a = 1344.1(1), b = 1553.6(1), c = 1977, 3(3) pm, β = 105.26(1)°, Z = 4, R1 = 0.0436.  相似文献   

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