The title complex (enH2){NH4[Co(en)3][Mo2O7(C2O4)]}22H2O (C18H70Co2Mo4- N16O24, Mr = 1396.52) was obtained under hydrothermal conditions and its crystal structure has been determined by single-crystal X-ray diffractio...The title complex (enH2){NH4[Co(en)3][Mo2O7(C2O4)]}22H2O (C18H70Co2Mo4- N16O24, Mr = 1396.52) was obtained under hydrothermal conditions and its crystal structure has been determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 17.8023(8), b = 7.7527(4), c = 16.9781(4) ? b = 103.878(7), V = 2274.8(2) 3, Dc = 2.039 g/cm3, Z = 2, m(MoKa) = 1.878 mm-1 and F(000) = 1408. The final R = 0.0410 and wR = 0.1070 for 4065 observed reflections with I≥2s(I). The crystal structure is composed of bi- nuclear [Mo2O7(C2O4)]4- anions, complex [Co(en)3]2+ cations, protonated ethylenediamine cations, ammonium cations and crystal water molecules, which are held together into a three-dimensional network via hydrogen-bonding interactions. The binuclear structure of [Mo2O7(C2O4)]4- consist of one MoO4 and one MoO6 octahedra through sharing a bridging oxygen atom, where the oxalate ligand acts as a bidentate ligand coordinating to the octahedral molybdenum atom though two deprotonated corboxylate groups.展开更多
[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15c...[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .展开更多
The crystal and molecular structures of molybdenum complex, Mo [ o- NHCOCH3- m-NO2C6H3COOH]2O2Cl2.PhCl are reported. The crystal belongs to space group Cc of monoclinic system with unit cell parameters:α= 11. 214 (3)...The crystal and molecular structures of molybdenum complex, Mo [ o- NHCOCH3- m-NO2C6H3COOH]2O2Cl2.PhCl are reported. The crystal belongs to space group Cc of monoclinic system with unit cell parameters:α= 11. 214 (3) A .b= 19. 544 (4 ) A . c = 14. 091 (6) A .β=94.06(3)°,V'=3080.3 A3 and Z=4. The structure was refined to R=0. 061.The coordination number for the Mo atom Is six. The coordination polyhedron formed by four O atoms and two Cl atoms around the Mo atom is a distorted octahedron. Four O atoms and one Mo atom construct a plane. Two benzyl planes in coordinate groups and the benzyl plane of solvent are almost parallel. The quantum-chemical calculations were carried out. There are hydrogen bonds in the Complex. The EHMO calculations and the existence of hydrogen bonds prove that the O atoms are stronger coordinated atoms in the carbonyls than in the carboxyls.展开更多
The deprotonated derivative pyridine-2-thiolato （PyS<sup>-</sup>） of pyridine-2-thione （PySH）is a potentially amibidentate or multi-functional donor which coordinates toward transitionmetals with eithe...The deprotonated derivative pyridine-2-thiolato （PyS<sup>-</sup>） of pyridine-2-thione （PySH）is a potentially amibidentate or multi-functional donor which coordinates toward transitionmetals with either the exocyclic S or heterocyclic N atom or both atoms to form differentcoordination modes. We have recently reported the synthesis and crystal structure ofthe first dinuclear molybdenum complex with doubly-bridging PyS ligands [Mo<sub>2</sub>（CO）<sub>4</sub>（μ-PyS）<sub>2</sub>（PPh<sub>3</sub>）<sub>2</sub>]which was obtained from the reaction of [Mo（CO）<sub>3</sub>（CH<sub>3</sub>CN）<sub>3</sub>]展开更多
A di-molybdenum carbonyl compound containing thiolate and dithiocarbamate ligands, [Bu4N][（CO）4Mo（μ-SC6H5）2Mo（C5H10dtc）（CO）2] 1 （CsH10dtc = S2CNC5H10）, has been prepared by reaction of [Mo2（SC6H5）2（CO）8...A di-molybdenum carbonyl compound containing thiolate and dithiocarbamate ligands, [Bu4N][（CO）4Mo（μ-SC6H5）2Mo（C5H10dtc）（CO）2] 1 （CsH10dtc = S2CNC5H10）, has been prepared by reaction of [Mo2（SC6H5）2（CO）8] with C5H10dtcNa and [NBu4]Br in acetone. It crystallizes in monoclinic, space group P21/n with a = 13.162（3）, b = 17.466（2）, c = 20.453（4） A,β= 100.77（1）°, Z = 4, V= 4619（2）A^3, C40H56Mo2N2O6S4, Mr = 980.95, De= 1.389 g/cm^3,μ = 7.66 cm^-1, F（000） = 1988 and R = 0.0746 for 5161 observed reflections with I 〉 2σ（I）. The complex contains a [Mo2S2]^2- planar core in which one Mo atom is chelated by a C5H10dtc ligand, leading to different coordination environments of the two Mo atoms. 95Mo NMR measurement indicates that the two Mo atoms are in different oxidation states.展开更多
A new copper（II） complex 3, Cu（C17H13F3O3）2·C5H5N, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 17.8511（7）, b = 17.413...A new copper（II） complex 3, Cu（C17H13F3O3）2·C5H5N, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 17.8511（7）, b = 17.4136（7）, c = 13.9425（7） A, β = 124.4830（10）°, V = 3572.5（3） A^3, Z = 4, C39H29CuF6NO6, Mr = 785.17,/7（000） = 1604, T = 292（2） K, Dc = 1.460 g/cm^3 and p = 0.691 mm^-1. The structure was refined to R = 0.0477 and wR = 0.1110 for 2935 observed reflections with I 〉 2σ（I）. For the title compound, X-ray analysis reveals that the copper（II） is penta-coordinated by four oxygen atoms from the corresponding 1-（4-（benzyloxy）phenyl）-4,4,4-trifluorobutane-1,3-dione ligands and one nitrogen atom of pyridine, forming a distorted square pyramidal geometry. It is found that the trifluoromethyl group, F（1）/F（1＇）, F（2）/F（2＇） and F（3）/F（3＇））, is disordered over two orientations in an approximate 3：1 ratio.展开更多
A new cobalt(Ⅱ) complex [Co(-phth)(imi)2]n (phth = o-phthalato, imi = imidazole) has been synthesized by the reaction of CoCl2 with disodium o-phthalate and imidazole. The crystal structure of the compound has been d...A new cobalt(Ⅱ) complex [Co(-phth)(imi)2]n (phth = o-phthalato, imi = imidazole) has been synthesized by the reaction of CoCl2 with disodium o-phthalate and imidazole. The crystal structure of the compound has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group Pn with a = 8.405(1), b = 9.995(1), c = 9.996(2) ? b = 104.479(2), V = 813.0(2) ?, Dc = 1.467 g/cm3, C14H12N4O4Co, Mr = 359.21, F(000) = 366, m = 1.079 mm-1, Z = 2, R = 0.0483 and wR = 0.1209 for 1583 observed reflections (I > 2s(I)). In the title complex, the Co(Ⅱ) ions are bridged by o-phthalate ligands in a bidentate mode, producing a zigzag infinite chain structure. Each four-coordinated cobalt(Ⅱ) center was coordinated by two oxygen atoms and two nitrogen atoms to give a distorted tetrahedral geometry. The chains are linked by hydrogen bonds between oxygen atoms belonging to carboxylate groups and hydrogen atoms of imidazole molecules, forming an unusual two-dimensional coordination polymer.展开更多
A Cupro-8-thioquinoline coordination polymer, [Cu I(C_9H_6NS)]_n, was synthesized by methano-thermal reaction of CuCl and 8,8′-dithiodiquinoline (dtdq) in a molar ratio of 2∶1 at 160 ℃ for 7 d. X-Ray single crysta...A Cupro-8-thioquinoline coordination polymer, [Cu I(C_9H_6NS)]_n, was synthesized by methano-thermal reaction of CuCl and 8,8′-dithiodiquinoline (dtdq) in a molar ratio of 2∶1 at 160 ℃ for 7 d. X-Ray single crystal structure determination revealed the formation of a one-dimensional structure belonging to monoclinic crystal system, space group P2_1/c with cell parameters a=0.8043(1) nm, b=1.8949(3) nm, c=1.1048(1) nm, β=110.109(4)°, V=1.5810(4) nm 3 and Z=4. The crystal was found to be stable up to approximately 300 ℃ by thermal analysis and have an energy gap (E_g) of 2.0 eV exhibited by UV-Vis-NIR reflectance spectrum.展开更多
Reaction of bis（4,6-dimethyl-2-pyrimidinethiolato）methane（bpytm） with CuCl2·4H2O in a mixed methanol/dichloromethane solution gave a one-dimensional coordina-tion polymer [CuCl2（μ-bpytm）]n which was charac...Reaction of bis（4,6-dimethyl-2-pyrimidinethiolato）methane（bpytm） with CuCl2·4H2O in a mixed methanol/dichloromethane solution gave a one-dimensional coordina-tion polymer [CuCl2（μ-bpytm）]n which was characterized by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group P21/c with a=16.9433（5）,b=13.6986（4）,c=7.8434（2）,β=100.371（2）°,V=1790.71（9）3,Z=4,Mr=426.86,Dc=1.583 g/cm3,μ（MoKα）=1.751mm-1,F（000）=868,S=1.025,the final R=0.0399 and wR=0.0924 for 2538 observed reflections with Ⅰ〉2σ（I） and 206 variables. The neutral coordination polymer is constructed by the bidentate thioether ligands to link adjacent copper atoms. Each copper atom is bridged by two adjacent nitrogen atoms of bpytm ligands and terminally bonded by two chloride atoms to form a squareplanar coordination geometry. The average Cu-N and Cu-CI bond lengths are 2.025（2） and 2.234（1） A, respectively.展开更多
Crystal structure of the title complex was determined by X-ray diffraction method. It crystallizes in space group P21/n with cell dimensions:α=10. 041(5) , b=10. 719(4) , c= 1. 5671(6) nm, β=104. 36(3)°. The st...Crystal structure of the title complex was determined by X-ray diffraction method. It crystallizes in space group P21/n with cell dimensions:α=10. 041(5) , b=10. 719(4) , c= 1. 5671(6) nm, β=104. 36(3)°. The structure was solved by Patterson method. The final residual factor is R=0. 050.展开更多
A new 2D coordination polymer, {[Cd5(BTC)2(L)4(H2O)2]n·2H2O}n(1, H3BTC = 1,3,5-benzenetricarboxylic acid, HL = 3-(2-pyridyl)pyrazole) was synthesized under hydrothermal conditions and characterized by single-crys...A new 2D coordination polymer, {[Cd5(BTC)2(L)4(H2O)2]n·2H2O}n(1, H3BTC = 1,3,5-benzenetricarboxylic acid, HL = 3-(2-pyridyl)pyrazole) was synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, powder XRD, IR, TGA, fluorescence spectrum and elemental analysis techniques. Complex 1 belongs to the monoclinic system, P21/c space group, with a = 8.8732(4), b = 17.5179(7), c = 17.8123(7) ?, β = 103.1830(10)°, V = 2695.77(19) ?3 and Z = 2. It features a 2D network constructed by BTC and L ligand. In addition, we analyzed Natural Bond Orbital(NBO) by using the PBE0/LANL2DZ method built in Gaussian 09 Program. The calculation results indicated obvious covalent interactions between the coordinated atoms and Cd(Ⅱ) ion.展开更多
基金the Natural Science Foundation of Fujian province
文摘The title complex (enH2){NH4[Co(en)3][Mo2O7(C2O4)]}22H2O (C18H70Co2Mo4- N16O24, Mr = 1396.52) was obtained under hydrothermal conditions and its crystal structure has been determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 17.8023(8), b = 7.7527(4), c = 16.9781(4) ? b = 103.878(7), V = 2274.8(2) 3, Dc = 2.039 g/cm3, Z = 2, m(MoKa) = 1.878 mm-1 and F(000) = 1408. The final R = 0.0410 and wR = 0.1070 for 4065 observed reflections with I≥2s(I). The crystal structure is composed of bi- nuclear [Mo2O7(C2O4)]4- anions, complex [Co(en)3]2+ cations, protonated ethylenediamine cations, ammonium cations and crystal water molecules, which are held together into a three-dimensional network via hydrogen-bonding interactions. The binuclear structure of [Mo2O7(C2O4)]4- consist of one MoO4 and one MoO6 octahedra through sharing a bridging oxygen atom, where the oxalate ligand acts as a bidentate ligand coordinating to the octahedral molybdenum atom though two deprotonated corboxylate groups.
基金Project supported by the National Natural Science Foundation of China
文摘[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .
文摘The crystal and molecular structures of molybdenum complex, Mo [ o- NHCOCH3- m-NO2C6H3COOH]2O2Cl2.PhCl are reported. The crystal belongs to space group Cc of monoclinic system with unit cell parameters:α= 11. 214 (3) A .b= 19. 544 (4 ) A . c = 14. 091 (6) A .β=94.06(3)°,V'=3080.3 A3 and Z=4. The structure was refined to R=0. 061.The coordination number for the Mo atom Is six. The coordination polyhedron formed by four O atoms and two Cl atoms around the Mo atom is a distorted octahedron. Four O atoms and one Mo atom construct a plane. Two benzyl planes in coordinate groups and the benzyl plane of solvent are almost parallel. The quantum-chemical calculations were carried out. There are hydrogen bonds in the Complex. The EHMO calculations and the existence of hydrogen bonds prove that the O atoms are stronger coordinated atoms in the carbonyls than in the carboxyls.
文摘The deprotonated derivative pyridine-2-thiolato （PyS<sup>-</sup>） of pyridine-2-thione （PySH）is a potentially amibidentate or multi-functional donor which coordinates toward transitionmetals with either the exocyclic S or heterocyclic N atom or both atoms to form differentcoordination modes. We have recently reported the synthesis and crystal structure ofthe first dinuclear molybdenum complex with doubly-bridging PyS ligands [Mo<sub>2</sub>（CO）<sub>4</sub>（μ-PyS）<sub>2</sub>（PPh<sub>3</sub>）<sub>2</sub>]which was obtained from the reaction of [Mo（CO）<sub>3</sub>（CH<sub>3</sub>CN）<sub>3</sub>]
文摘A di-molybdenum carbonyl compound containing thiolate and dithiocarbamate ligands, [Bu4N][（CO）4Mo（μ-SC6H5）2Mo（C5H10dtc）（CO）2] 1 （CsH10dtc = S2CNC5H10）, has been prepared by reaction of [Mo2（SC6H5）2（CO）8] with C5H10dtcNa and [NBu4]Br in acetone. It crystallizes in monoclinic, space group P21/n with a = 13.162（3）, b = 17.466（2）, c = 20.453（4） A,β= 100.77（1）°, Z = 4, V= 4619（2）A^3, C40H56Mo2N2O6S4, Mr = 980.95, De= 1.389 g/cm^3,μ = 7.66 cm^-1, F（000） = 1988 and R = 0.0746 for 5161 observed reflections with I 〉 2σ（I）. The complex contains a [Mo2S2]^2- planar core in which one Mo atom is chelated by a C5H10dtc ligand, leading to different coordination environments of the two Mo atoms. 95Mo NMR measurement indicates that the two Mo atoms are in different oxidation states.
基金supported by the Natural Science Foundation of the Educational Commission of Hubei Province (No. Q20082202)
文摘A new copper（II） complex 3, Cu（C17H13F3O3）2·C5H5N, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 17.8511（7）, b = 17.4136（7）, c = 13.9425（7） A, β = 124.4830（10）°, V = 3572.5（3） A^3, Z = 4, C39H29CuF6NO6, Mr = 785.17,/7（000） = 1604, T = 292（2） K, Dc = 1.460 g/cm^3 and p = 0.691 mm^-1. The structure was refined to R = 0.0477 and wR = 0.1110 for 2935 observed reflections with I 〉 2σ（I）. For the title compound, X-ray analysis reveals that the copper（II） is penta-coordinated by four oxygen atoms from the corresponding 1-（4-（benzyloxy）phenyl）-4,4,4-trifluorobutane-1,3-dione ligands and one nitrogen atom of pyridine, forming a distorted square pyramidal geometry. It is found that the trifluoromethyl group, F（1）/F（1＇）, F（2）/F（2＇） and F（3）/F（3＇））, is disordered over two orientations in an approximate 3：1 ratio.
基金Supported by the National Natural Science Foundation of China (29872037)the Natural Science Foundation of Fujian province (C0120002)
文摘A new cobalt(Ⅱ) complex [Co(-phth)(imi)2]n (phth = o-phthalato, imi = imidazole) has been synthesized by the reaction of CoCl2 with disodium o-phthalate and imidazole. The crystal structure of the compound has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group Pn with a = 8.405(1), b = 9.995(1), c = 9.996(2) ? b = 104.479(2), V = 813.0(2) ?, Dc = 1.467 g/cm3, C14H12N4O4Co, Mr = 359.21, F(000) = 366, m = 1.079 mm-1, Z = 2, R = 0.0483 and wR = 0.1209 for 1583 observed reflections (I > 2s(I)). In the title complex, the Co(Ⅱ) ions are bridged by o-phthalate ligands in a bidentate mode, producing a zigzag infinite chain structure. Each four-coordinated cobalt(Ⅱ) center was coordinated by two oxygen atoms and two nitrogen atoms to give a distorted tetrahedral geometry. The chains are linked by hydrogen bonds between oxygen atoms belonging to carboxylate groups and hydrogen atoms of imidazole molecules, forming an unusual two-dimensional coordination polymer.
基金ProjectsupportedbytheNationalNaturalScienceFoundationofChina (No .2 96730 0 4)andtheStateKeyLaboratoryforStructuralChemistryofUnstableandStableSpecies ,China
文摘A Cupro-8-thioquinoline coordination polymer, [Cu I(C_9H_6NS)]_n, was synthesized by methano-thermal reaction of CuCl and 8,8′-dithiodiquinoline (dtdq) in a molar ratio of 2∶1 at 160 ℃ for 7 d. X-Ray single crystal structure determination revealed the formation of a one-dimensional structure belonging to monoclinic crystal system, space group P2_1/c with cell parameters a=0.8043(1) nm, b=1.8949(3) nm, c=1.1048(1) nm, β=110.109(4)°, V=1.5810(4) nm 3 and Z=4. The crystal was found to be stable up to approximately 300 ℃ by thermal analysis and have an energy gap (E_g) of 2.0 eV exhibited by UV-Vis-NIR reflectance spectrum.
基金supported by the Natural Science Foundation of the Education Bureau of Anhui Provincethe Program for New Century Excellent Talents in University (2006kj035a and NCET-06-0556)
文摘Reaction of bis（4,6-dimethyl-2-pyrimidinethiolato）methane（bpytm） with CuCl2·4H2O in a mixed methanol/dichloromethane solution gave a one-dimensional coordina-tion polymer [CuCl2（μ-bpytm）]n which was characterized by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group P21/c with a=16.9433（5）,b=13.6986（4）,c=7.8434（2）,β=100.371（2）°,V=1790.71（9）3,Z=4,Mr=426.86,Dc=1.583 g/cm3,μ（MoKα）=1.751mm-1,F（000）=868,S=1.025,the final R=0.0399 and wR=0.0924 for 2538 observed reflections with Ⅰ〉2σ（I） and 206 variables. The neutral coordination polymer is constructed by the bidentate thioether ligands to link adjacent copper atoms. Each copper atom is bridged by two adjacent nitrogen atoms of bpytm ligands and terminally bonded by two chloride atoms to form a squareplanar coordination geometry. The average Cu-N and Cu-CI bond lengths are 2.025（2） and 2.234（1） A, respectively.
文摘Crystal structure of the title complex was determined by X-ray diffraction method. It crystallizes in space group P21/n with cell dimensions:α=10. 041(5) , b=10. 719(4) , c= 1. 5671(6) nm, β=104. 36(3)°. The structure was solved by Patterson method. The final residual factor is R=0. 050.
基金supported by the Science and Technology development plan of Jilin Province(2015052006JH)
文摘A new 2D coordination polymer, {[Cd5(BTC)2(L)4(H2O)2]n·2H2O}n(1, H3BTC = 1,3,5-benzenetricarboxylic acid, HL = 3-(2-pyridyl)pyrazole) was synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, powder XRD, IR, TGA, fluorescence spectrum and elemental analysis techniques. Complex 1 belongs to the monoclinic system, P21/c space group, with a = 8.8732(4), b = 17.5179(7), c = 17.8123(7) ?, β = 103.1830(10)°, V = 2695.77(19) ?3 and Z = 2. It features a 2D network constructed by BTC and L ligand. In addition, we analyzed Natural Bond Orbital(NBO) by using the PBE0/LANL2DZ method built in Gaussian 09 Program. The calculation results indicated obvious covalent interactions between the coordinated atoms and Cd(Ⅱ) ion.
