The formation constants of Co￣(2+), Ni￣(2+), Cu￣(2+) and Zn￣(2+) complexes with humic acid (HA) and fulvicacid (FA) in red soil were determined by the potentiometric titration method. The constants as a functionof...The formation constants of Co￣(2+), Ni￣(2+), Cu￣(2+) and Zn￣(2+) complexes with humic acid (HA) and fulvicacid (FA) in red soil were determined by the potentiometric titration method. The constants as a functionof composition of the complexation solutions were obtained by two graphical approaches respectively Theformation constants decreased with increasing concentration of metal in the solution. The results provideunambiguous evidence for the heterogeneity of the function groups of humic substances. The formationconstants of FA were much smaller than those of HA, and the formation constants of Cu￣(2+) were muchgreater than those of Co￣(2+) , Ni￣(2+) and Zn￣(2+) . The potentiometric titration method for determining formationconstants are also discussed in the article.展开更多
Three new nickel(Ⅱ) binuclear complexes, namely,[Ni_2(CTPHA)(Phen)_4](ClO_4)2·4H_2O (complex 1 ), [Ni_2(CTPHA) (Nphen)_4](ClO_4)_2·2H_2O(complex 2 ) and [Ni2 (CTPHA)(Bpy)4] (ClO4)2 (complex 3 ). (CTPHA = 2-...Three new nickel(Ⅱ) binuclear complexes, namely,[Ni_2(CTPHA)(Phen)_4](ClO_4)2·4H_2O (complex 1 ), [Ni_2(CTPHA) (Nphen)_4](ClO_4)_2·2H_2O(complex 2 ) and [Ni2 (CTPHA)(Bpy)4] (ClO4)2 (complex 3 ). (CTPHA = 2-chloroterephthalate . Phen=1, 10-phenanthroline, Nphen=5-nitro-1, 10-phenanthroline, Bpy=2, 2-bipyridyl), have been synthesized and characterized by elemental analysis, IR, molar conductance and electronic spectra. These complexes are proposed tohave extended Z-chloroterephthalato-bridged structure and to consist of two nickel(Ⅱ). The variable-temperature magnetic susceptibilities of complex 1 were measuredover 4. 2～300 K and the data were fitted by least-squares to a susceptibility equationderived from the Hamiltonian operator, giving the exchange integral ZJ=1. 6 cm-1, which indicate a very weak antiferromagnetic interaction between nickelf (Ⅱ) ions.展开更多
The nickel(Ⅱ) complex with the new ligand of S-benzyl-b-N-[10-ethyl- phenothiazine-3-methylene]dithiocarbazate(HL) crystallizes in the triclinic system, space group P?with a = 7.516(1), b = 11.322(1), c = 13.366(1) ,...The nickel(Ⅱ) complex with the new ligand of S-benzyl-b-N-[10-ethyl- phenothiazine-3-methylene]dithiocarbazate(HL) crystallizes in the triclinic system, space group P?with a = 7.516(1), b = 11.322(1), c = 13.366(1) , a = 84.818(1), b = 81.688(1), g = 76.037(1), V = 1090.26(3) 3, Z = 1, Dc = 1.413 g/cm3, F(000) = 482, m(MoKa) = 0.774 mm-1 (l = 0.7103 ?, R = 0.0573 and wR = 0.1375 for 3357 observed reflections with I ≥ 2s(I). The HL has lost a proton from its tautomeric thiol form and acts as a single negatively charged bidentate ligand coordinating to the nickel ion via the mercapto sulfur and b-nitrogen atoms. The geometry around Ni(Ⅱ) is almost square-planar with two equivalent NiN and NiS bonds. The nonlinear absorption of HL and NiL2 solutions (in DMF) was measured by open-aperture Z-scan technique at the wavelength of 532 nm.展开更多
The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characteriz...The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characterized by X ray diffraction study, IR and UV Vis spectroscopy. Crystallographic data : space group: P2 1/n, a=11.843(2), b=11 079(1), c = 15.404(1) , β=110.33(1)°, V = 1895.1 3, Z=2, D c =1.62 g/cm 3 , μ =17.6 cm -1 , F (000)=956, R=0.052, R w =0.061. In the structure of the title complex, the tto (tto=tetrathioxalato) ligand in bridging form is chelated to two nickel atoms and dmit (dmit=1,3 dithiole 2 thione 4,5 dithiolate) ligands coordinated to nickel atoms.展开更多
The title compound, [Ni(acac)2(Im)2] (acac = acetylacetone), has been obtained by the reaction of Ni(acac)2 with imidazole ligand in the ethanol solvent. The blue crystal is of triclinic, space group Pi with a = 7.472...The title compound, [Ni(acac)2(Im)2] (acac = acetylacetone), has been obtained by the reaction of Ni(acac)2 with imidazole ligand in the ethanol solvent. The blue crystal is of triclinic, space group Pi with a = 7.472(2), b = 9.456(2), c = 13.823(3) ? a = 85.55(3), = 89.03(3), ? = 80.63(3)o, C16H22N4NiO4, Mr = 393.09, V = 960.7(3) 3, Z = 2, Dc = 1.359 g/cm3, F(000) = 412, = 1.036 mm-1, R = 0.0549 and wR = 0.1615. The crystal structure consists of two disconnected structural units. Each Ni atom coordinated by two N atoms from two imidazole ligands and four O atoms from two acetylactone ligands adopts a slightly distorted octahedron. The structure characterization was performed by means of IR, UV, TG, elemental analysis and single-crystal X-ray analysis. The thermal gravity (TG) data indicate that thermal decomposition of the title compound takes place in two steps, and the residue is NiO.展开更多
The ligand azobis(2-pyridine) L was used in the synthesis of two new organic-inorganic coordination complexes: [Ni(L)2(NCS)2] 1 and [Co(L)2(NCS)2] 2. Crystal data for 1: monoclinic, space group C2/c, a = 13.361(18), b...The ligand azobis(2-pyridine) L was used in the synthesis of two new organic-inorganic coordination complexes: [Ni(L)2(NCS)2] 1 and [Co(L)2(NCS)2] 2. Crystal data for 1: monoclinic, space group C2/c, a = 13.361(18), b = 10.731(15), c = 18.14(2) ? β = 109.86(2)? V = 2446(6) 3, Z = 4, Mr = 543.25, Dc = 1.410 g/cm3, μ = 0.993 mm-1, F(000) = 1064, T = 298(2) K, R = 0.0454 and wR = 0.1010 for 1288 observed reflections with I > 2s(I); and those for 2: monoclinic, space group C2/c, a = 13.35(2), b = 10.806(15), c = 18.06(2) , β = 110.34(2)? Z = 4, Mr = 543.49, Dc = 1.413 g/cm3, μ = 0.902 mm-1, F(000) = 1060, T = 298(2) K, R = 0.0699 and wR = 0.1354 for 728 observed reflections with I > 2s(I). Single-crystal X-ray diffraction studies revealed that 1 and 2 have similar structures, in which each Ni(II) or Co(II) cation is coordinated by two L ligands and two terminal thiocynates (NCS-).展开更多
An ion-pair compound, [HL]2[Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphen...An ion-pair compound, [HL]2[Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphenyl)-1,5,9-triazacyclododecan-2-one) in aqueous solution, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.380(1), b = 9.9637(8), c = 17.087(1) ? ?= 105.947(2)? V = 2026.6(3) ?, Rint = 0.0509, Z = 2, Dc = 1.297 g/cm3, C34H56O8N10Ni, Mr = 791.60, F(000) = 844, m(MoKa) = 0.538 mm1, S = 1.030, the final R = 0.0644 and wR = 0.1299 for 2023 observed reflections with I ≥ 2(I). The title compound 1 contains one anion of [Ni(CN)4]2, two cations of [HL]+ and four packing water molecules, which are held together by the NH···O and OH···O hydrogen bonds to form a three- dimensional framework.展开更多
The crystal structure of [Ni(C5H2N2O4)(2, 2?bipy)(H2O)2]?H2O 1 has been determined by X-ray diffraction. Crystal data: triclinic system, space group P with a = 7.9424(3), b = 9.9417(3), c = 12.1867(3) ? a = 84.771(1),...The crystal structure of [Ni(C5H2N2O4)(2, 2?bipy)(H2O)2]?H2O 1 has been determined by X-ray diffraction. Crystal data: triclinic system, space group P with a = 7.9424(3), b = 9.9417(3), c = 12.1867(3) ? a = 84.771(1), b = 77.375(2), g = 68.993(2)? C15H18N4O8Ni, Mr = 440.7, V = 876.16(5) 3, Z = 2, Dc = 1.672 g/cm3, F(000) = 456, m(MoKa) = 1.162 mm-1, the final R = 0.0464 and wR = 0.1055 for 3026 observed reflections with I > 2s(I). In the title compound, the nickel ion is coordinated by a nitrogen atom and an oxygen atom from the orotate ligand, two nitrogen atoms from 2, 2?bipy and two oxygen atoms from the coordinated water molecules in a distorted octahedral geometry. The presence of intermolecular hydrogen bonding and p-p stacking interaction of aromatic rings from 2, 2?bipy results in a 3D structure.展开更多
A novel two-dimensional compound [Ni0.5(H2O)1.5{Ni(en)2}3V18O42(Cl)]3.5H2O 1 has been hydrothermally synthesized and characterized by IR, elemental analysis, and single-crystal X-ray diffraction analysis. Crystal data...A novel two-dimensional compound [Ni0.5(H2O)1.5{Ni(en)2}3V18O42(Cl)]3.5H2O 1 has been hydrothermally synthesized and characterized by IR, elemental analysis, and single-crystal X-ray diffraction analysis. Crystal data for 1: monoclinic, space group C2/c with a = 12.824(3), b = 27.873(6), c = 21.092(4) , b = 92.93(3), V = 7529(3) 3, Z = 4, Dc = 2.012 g/cm3, Mr = 2280.56, F(000) = 4476 and m = 3.092 mm-1. The final R and wR are 0.0769 and 0.1783, respectively for 4203 observed reflections with I>2s(I). The structure consists of [V18O42(Cl)]7- clusters linked by trans- {Ni(en)2} groups into linear chains, while cis-{Ni(en)2} groups provide the cross-linking adjacent chains to form a two-dimensional structure.展开更多
A new series of dimeric Cu（II） and Ni（II） complexes with some aroylhydrazones of a-pyridoin were synthesized and characterized using different physical techniques. Their chemical formulae were based on their micro...A new series of dimeric Cu（II） and Ni（II） complexes with some aroylhydrazones of a-pyridoin were synthesized and characterized using different physical techniques. Their chemical formulae were based on their microanalysis and IR data. The structures of the solid complexes were determined from the electronic, IR and ESR spectral studies as well as their magnetic susceptibility measurements. The ligands acted as bi-, tri- and tetra-dentate forming different dinuclear complexes with different structures. The assumed molecular structures based on the experimental results were also confirmed by the molecular mechanics calculations. The extraction ability of the hydrazones has been investigated by liquid-liquid extraction for Cu（II） and Ni（II）.展开更多
The title compound [Ni(bipy)3][(-oxo)Fe2Cl6] (bipy = 2, 2?bispyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group P2l/c with unit c...The title compound [Ni(bipy)3][(-oxo)Fe2Cl6] (bipy = 2, 2?bispyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group P2l/c with unit cell parameters: a = 9.7085(7),b = 26.409(2), c = 14.014(1) ,?= 100.237(3), V = 3535.9(2) 3,Z = 4,C30H24Cl6Fe2N6NiO,Mr = 867.66, Dc = 1.630 g/cm3,F(000) = 1744, (MoK? = 1.824 mm-1, the final R = 0.0394 and wR = 0.0475 for 2750 observed reflections with I ≥ 2(I). The title compound contains cation of [Ni(bipy)3]2+ and anion of [(-oxo)Fe2Cl6] 2- which consists of two [FeCl3] fragments connected by an oxo bridge with the bond distances of Fe(2)O(1) 1.752(2) and Fe(1)O(1) 1.763(2) , and the bond angle of Fe(2)O(1)Fe(1) 148.6(2)? In the [Fe2(-oxo)Cl6]2- complex, the two iron(Ⅲ) centers exhibit a tetrahedral coordination with the distorted tetrahedron formed by three Cl atoms and one oxo bridge.展开更多
The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-dien...The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-diene and mnt2- = cis-1, 2-dicyano-1,2-ethylenedithiolato. Its crystal structure has been determined by X-raycrystallography analysis with 4827 independent reflections (Fo>4σ(F0). The bimetallic complex salt [Ni (trans [14] diene )] [Ni (mnt )2] (C24 H32N8Ni2S4, Mr = 678. 24 )crystallizes in the triclinic system with space group P1, a = 9. 2911 (9), b= 11. 7075(12), c=15. 799(2) A, α=68. 384(7), β=79. 324(7), γ=67. 581(6)°, V=1474. 9(3) A3, Dc=1. 527 Mg/m3, Z=2, λ=0. 71073 A, μ=1. 589mm-1, F(000) =704,R=0. 0367. The structure consists of slightly distorted Square planar units [Ni(trans[14]diene)]2+ and [Ni(mnt)2]2-.展开更多
文摘The formation constants of Co￣(2+), Ni￣(2+), Cu￣(2+) and Zn￣(2+) complexes with humic acid (HA) and fulvicacid (FA) in red soil were determined by the potentiometric titration method. The constants as a functionof composition of the complexation solutions were obtained by two graphical approaches respectively Theformation constants decreased with increasing concentration of metal in the solution. The results provideunambiguous evidence for the heterogeneity of the function groups of humic substances. The formationconstants of FA were much smaller than those of HA, and the formation constants of Cu￣(2+) were muchgreater than those of Co￣(2+) , Ni￣(2+) and Zn￣(2+) . The potentiometric titration method for determining formationconstants are also discussed in the article.
文摘Three new nickel(Ⅱ) binuclear complexes, namely,[Ni_2(CTPHA)(Phen)_4](ClO_4)2·4H_2O (complex 1 ), [Ni_2(CTPHA) (Nphen)_4](ClO_4)_2·2H_2O(complex 2 ) and [Ni2 (CTPHA)(Bpy)4] (ClO4)2 (complex 3 ). (CTPHA = 2-chloroterephthalate . Phen=1, 10-phenanthroline, Nphen=5-nitro-1, 10-phenanthroline, Bpy=2, 2-bipyridyl), have been synthesized and characterized by elemental analysis, IR, molar conductance and electronic spectra. These complexes are proposed tohave extended Z-chloroterephthalato-bridged structure and to consist of two nickel(Ⅱ). The variable-temperature magnetic susceptibilities of complex 1 were measuredover 4. 2～300 K and the data were fitted by least-squares to a susceptibility equationderived from the Hamiltonian operator, giving the exchange integral ZJ=1. 6 cm-1, which indicate a very weak antiferromagnetic interaction between nickelf (Ⅱ) ions.
基金Supported by a grant for the State Key Program of China (G1998061402) the National Natural Science Foundation of China (29871001, 20071001, and 50272001)
文摘The nickel(Ⅱ) complex with the new ligand of S-benzyl-b-N-[10-ethyl- phenothiazine-3-methylene]dithiocarbazate(HL) crystallizes in the triclinic system, space group P?with a = 7.516(1), b = 11.322(1), c = 13.366(1) , a = 84.818(1), b = 81.688(1), g = 76.037(1), V = 1090.26(3) 3, Z = 1, Dc = 1.413 g/cm3, F(000) = 482, m(MoKa) = 0.774 mm-1 (l = 0.7103 ?, R = 0.0573 and wR = 0.1375 for 3357 observed reflections with I ≥ 2s(I). The HL has lost a proton from its tautomeric thiol form and acts as a single negatively charged bidentate ligand coordinating to the nickel ion via the mercapto sulfur and b-nitrogen atoms. The geometry around Ni(Ⅱ) is almost square-planar with two equivalent NiN and NiS bonds. The nonlinear absorption of HL and NiL2 solutions (in DMF) was measured by open-aperture Z-scan technique at the wavelength of 532 nm.
文摘The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characterized by X ray diffraction study, IR and UV Vis spectroscopy. Crystallographic data : space group: P2 1/n, a=11.843(2), b=11 079(1), c = 15.404(1) , β=110.33(1)°, V = 1895.1 3, Z=2, D c =1.62 g/cm 3 , μ =17.6 cm -1 , F (000)=956, R=0.052, R w =0.061. In the structure of the title complex, the tto (tto=tetrathioxalato) ligand in bridging form is chelated to two nickel atoms and dmit (dmit=1,3 dithiole 2 thione 4,5 dithiolate) ligands coordinated to nickel atoms.
基金This work was supported bythe Natural Science Foundation of Shandong Province (No. Y2002B06) and Science Research Foundation of Qingdao University of Science and Technology (No. 03Z08)
文摘The title compound, [Ni(acac)2(Im)2] (acac = acetylacetone), has been obtained by the reaction of Ni(acac)2 with imidazole ligand in the ethanol solvent. The blue crystal is of triclinic, space group Pi with a = 7.472(2), b = 9.456(2), c = 13.823(3) ? a = 85.55(3), = 89.03(3), ? = 80.63(3)o, C16H22N4NiO4, Mr = 393.09, V = 960.7(3) 3, Z = 2, Dc = 1.359 g/cm3, F(000) = 412, = 1.036 mm-1, R = 0.0549 and wR = 0.1615. The crystal structure consists of two disconnected structural units. Each Ni atom coordinated by two N atoms from two imidazole ligands and four O atoms from two acetylactone ligands adopts a slightly distorted octahedron. The structure characterization was performed by means of IR, UV, TG, elemental analysis and single-crystal X-ray analysis. The thermal gravity (TG) data indicate that thermal decomposition of the title compound takes place in two steps, and the residue is NiO.
基金NNSFC (No 20361004)and NSF of Yunnan Province (No 2003E0012M and2003RC13) and Yunnan University (No 2002Z001GC)
文摘The ligand azobis(2-pyridine) L was used in the synthesis of two new organic-inorganic coordination complexes: [Ni(L)2(NCS)2] 1 and [Co(L)2(NCS)2] 2. Crystal data for 1: monoclinic, space group C2/c, a = 13.361(18), b = 10.731(15), c = 18.14(2) ? β = 109.86(2)? V = 2446(6) 3, Z = 4, Mr = 543.25, Dc = 1.410 g/cm3, μ = 0.993 mm-1, F(000) = 1064, T = 298(2) K, R = 0.0454 and wR = 0.1010 for 1288 observed reflections with I > 2s(I); and those for 2: monoclinic, space group C2/c, a = 13.35(2), b = 10.806(15), c = 18.06(2) , β = 110.34(2)? Z = 4, Mr = 543.49, Dc = 1.413 g/cm3, μ = 0.902 mm-1, F(000) = 1060, T = 298(2) K, R = 0.0699 and wR = 0.1354 for 728 observed reflections with I > 2s(I). Single-crystal X-ray diffraction studies revealed that 1 and 2 have similar structures, in which each Ni(II) or Co(II) cation is coordinated by two L ligands and two terminal thiocynates (NCS-).
文摘An ion-pair compound, [HL]2[Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphenyl)-1,5,9-triazacyclododecan-2-one) in aqueous solution, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.380(1), b = 9.9637(8), c = 17.087(1) ? ?= 105.947(2)? V = 2026.6(3) ?, Rint = 0.0509, Z = 2, Dc = 1.297 g/cm3, C34H56O8N10Ni, Mr = 791.60, F(000) = 844, m(MoKa) = 0.538 mm1, S = 1.030, the final R = 0.0644 and wR = 0.1299 for 2023 observed reflections with I ≥ 2(I). The title compound 1 contains one anion of [Ni(CN)4]2, two cations of [HL]+ and four packing water molecules, which are held together by the NH···O and OH···O hydrogen bonds to form a three- dimensional framework.
基金This project was supported by the Natural Science Foundation of China and Chinese Academy of Sciences
文摘The crystal structure of [Ni(C5H2N2O4)(2, 2?bipy)(H2O)2]?H2O 1 has been determined by X-ray diffraction. Crystal data: triclinic system, space group P with a = 7.9424(3), b = 9.9417(3), c = 12.1867(3) ? a = 84.771(1), b = 77.375(2), g = 68.993(2)? C15H18N4O8Ni, Mr = 440.7, V = 876.16(5) 3, Z = 2, Dc = 1.672 g/cm3, F(000) = 456, m(MoKa) = 1.162 mm-1, the final R = 0.0464 and wR = 0.1055 for 3026 observed reflections with I > 2s(I). In the title compound, the nickel ion is coordinated by a nitrogen atom and an oxygen atom from the orotate ligand, two nitrogen atoms from 2, 2?bipy and two oxygen atoms from the coordinated water molecules in a distorted octahedral geometry. The presence of intermolecular hydrogen bonding and p-p stacking interaction of aromatic rings from 2, 2?bipy results in a 3D structure.
基金This work was supported by NNSFC (No. 20271050 and 20171045) the Educational Ministry of China the Talents Program of the Chinese Academy of Sciences and NSF of Fujian province (E0210029)
文摘A novel two-dimensional compound [Ni0.5(H2O)1.5{Ni(en)2}3V18O42(Cl)]3.5H2O 1 has been hydrothermally synthesized and characterized by IR, elemental analysis, and single-crystal X-ray diffraction analysis. Crystal data for 1: monoclinic, space group C2/c with a = 12.824(3), b = 27.873(6), c = 21.092(4) , b = 92.93(3), V = 7529(3) 3, Z = 4, Dc = 2.012 g/cm3, Mr = 2280.56, F(000) = 4476 and m = 3.092 mm-1. The final R and wR are 0.0769 and 0.1783, respectively for 4203 observed reflections with I>2s(I). The structure consists of [V18O42(Cl)]7- clusters linked by trans- {Ni(en)2} groups into linear chains, while cis-{Ni(en)2} groups provide the cross-linking adjacent chains to form a two-dimensional structure.
文摘A new series of dimeric Cu（II） and Ni（II） complexes with some aroylhydrazones of a-pyridoin were synthesized and characterized using different physical techniques. Their chemical formulae were based on their microanalysis and IR data. The structures of the solid complexes were determined from the electronic, IR and ESR spectral studies as well as their magnetic susceptibility measurements. The ligands acted as bi-, tri- and tetra-dentate forming different dinuclear complexes with different structures. The assumed molecular structures based on the experimental results were also confirmed by the molecular mechanics calculations. The extraction ability of the hydrazones has been investigated by liquid-liquid extraction for Cu（II） and Ni（II）.
基金Supported by the foundation of Education Committee of Fujian Province (JB01045)
文摘The title compound [Ni(bipy)3][(-oxo)Fe2Cl6] (bipy = 2, 2?bispyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group P2l/c with unit cell parameters: a = 9.7085(7),b = 26.409(2), c = 14.014(1) ,?= 100.237(3), V = 3535.9(2) 3,Z = 4,C30H24Cl6Fe2N6NiO,Mr = 867.66, Dc = 1.630 g/cm3,F(000) = 1744, (MoK? = 1.824 mm-1, the final R = 0.0394 and wR = 0.0475 for 2750 observed reflections with I ≥ 2(I). The title compound contains cation of [Ni(bipy)3]2+ and anion of [(-oxo)Fe2Cl6] 2- which consists of two [FeCl3] fragments connected by an oxo bridge with the bond distances of Fe(2)O(1) 1.752(2) and Fe(1)O(1) 1.763(2) , and the bond angle of Fe(2)O(1)Fe(1) 148.6(2)? In the [Fe2(-oxo)Cl6]2- complex, the two iron(Ⅲ) centers exhibit a tetrahedral coordination with the distorted tetrahedron formed by three Cl atoms and one oxo bridge.
文摘The title compound has been synthesized by the reaction of [Ni(trans[14]diene)]I2 with Na[Ni(mnt)2] in water and THF, where [trans[14]diene]= 5, 7,7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradeca-4, 11-diene and mnt2- = cis-1, 2-dicyano-1,2-ethylenedithiolato. Its crystal structure has been determined by X-raycrystallography analysis with 4827 independent reflections (Fo>4σ(F0). The bimetallic complex salt [Ni (trans [14] diene )] [Ni (mnt )2] (C24 H32N8Ni2S4, Mr = 678. 24 )crystallizes in the triclinic system with space group P1, a = 9. 2911 (9), b= 11. 7075(12), c=15. 799(2) A, α=68. 384(7), β=79. 324(7), γ=67. 581(6)°, V=1474. 9(3) A3, Dc=1. 527 Mg/m3, Z=2, λ=0. 71073 A, μ=1. 589mm-1, F(000) =704,R=0. 0367. The structure consists of slightly distorted Square planar units [Ni(trans[14]diene)]2+ and [Ni(mnt)2]2-.
