A stable organometallic Pd (Ⅱ) compound Pd(ptac-C,N)(acac-O,O) (Hacac = acetyl acetone, Hptac = 3-(2-pyridinethioxy)-acac, formula: C15H17NO4SPd, Mr = 413.76) 1 has been synthesized and its crystal structure was dete...A stable organometallic Pd (Ⅱ) compound Pd(ptac-C,N)(acac-O,O) (Hacac = acetyl acetone, Hptac = 3-(2-pyridinethioxy)-acac, formula: C15H17NO4SPd, Mr = 413.76) 1 has been synthesized and its crystal structure was determined by X-ray crystallography. The crystal is of monoclinic with space group C2/c, a = 17.9342(3), b = 17.7791(4), c = 13.1800(1) ? b = 128.400(1), V = 3293.5(1) 3, Z = 8, Dc = 1.669 g/cm3, F(000) = 1664, m = 1.269 mm-1, R = 0.0261 and wR = 0.0710 for 2653 observed reflections (I > 2s(I)). There exist two Pd rings in the title compound, C(14)O(4)PdO(3)C(12)C(13) and C(1)NPdC(8)S, with the palladium atom taking a square-planar coordination. Two oxygen atoms from the acetyl acetone ligand (PdO, 1.991(2) and 2.036(2) ), one N atom (PdN 2.019 ? and the g-carbon atom (PdC 2.067(3) ? from the ptac ligand are coordinated to Pd.展开更多
A new lanthanide coordination polymer, [Dy(OAc)(BDC)]n 1 (OAc = acetate, BDC = 1,4-benzenediacarboxylate), has been synthesized under hydrothermal conditions. Single-crystal X-ray diffraction analysis reveals th...A new lanthanide coordination polymer, [Dy(OAc)(BDC)]n 1 (OAc = acetate, BDC = 1,4-benzenediacarboxylate), has been synthesized under hydrothermal conditions. Single-crystal X-ray diffraction analysis reveals that complex 1 has infinite zigzag Dy-OAc chains, which are further connected by BDC to form a 3D metal-organic framework. According to topology analysis, this framework can be characterized as (4,6)-connected (3.4.54)(32.4.56.66) net that has never been reported before. Crystal structure for 1: space group Pbca, a = 13.314(3), b = 8.0269(18), c = 20.275(5)A, V= 2166.8(9)A3, C10H7O6Dy, Mr = 385.66, Z= 8, Dc = 2.364 g/cm^3, μ= 6.910 mm^-1, F(000) = 1448, the final R = 0.0181 and wR = 0.0520.展开更多
The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (phen = 1,10-phe-nan throline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crys...The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (phen = 1,10-phe-nan throline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1^- with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10) A, α = 80.6830(10), β = 66.6480(10), γ = 64.048000)°, V = 1554.63(4) A^3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm^3,μ = 0.845 mm^-1, F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (1 〉 2σ(I)). The compound contains a six-coordinated copper(Ⅱ) center, which is surround by four N atoms of two phen ligands (Cu-N distances in the range of 1.997(2)- 2.225(2) A), one sulfate O atom (Cu-O = 2.0037(17) A) and one water O atom (Cu-O(Sw) = 2.719(2) A,) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.展开更多
One new coordination polymer, namely {[Zn(HL)(Hbipy)]2·3H2O}n(bipy = 4,4A-bipyridine, H4 L = 6-(3',4'-dicarboxyl-phenoxy) isophthalic acid), has been synthesized through a hydrothermal method and charac...One new coordination polymer, namely {[Zn(HL)(Hbipy)]2·3H2O}n(bipy = 4,4A-bipyridine, H4 L = 6-(3',4'-dicarboxyl-phenoxy) isophthalic acid), has been synthesized through a hydrothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectra(IR), and thermogravimetric(TG) analysis. The crystal structure is of monoclinic, space group P21/n with a = 9.6435(3), b = 19.8515(7), c = 12.9731(5) A, β = 103.023(4)o, V = 2419.67(15) A3, C52H38Zn2N4O21, Mr = 1185.6, Z = 2, Dc = 1.619 g/cm^3, F(000) = 1200, μ = 1.083 mm-1, the final R = 0.0443 and w R = 0.1079 for 4269 observed reflections(I 2σ(I). The compound features a two-dimensional(2D) framework and stabilizes itself by interlayer π···π interactions and innerlayer hydrogen bonds. The 2D layer presents a simple 3-connected 63 topology. Moreover, the thermal dynamic stability and luminescent property of the compound have also been discussed in detail.展开更多
The title compound {Cu2(pdc)2(4,4?-bipy)(H2O)3H2O}2 1 (H2pdc = pyridine-2,6- dicarboxylic acid, also known as dipicolinic acid; 4,4?-bipy = 4,4?-bipyridine) has been synthesized by the hydrothermal reaction and its st...The title compound {Cu2(pdc)2(4,4?-bipy)(H2O)3H2O}2 1 (H2pdc = pyridine-2,6- dicarboxylic acid, also known as dipicolinic acid; 4,4?-bipy = 4,4?-bipyridine) has been synthesized by the hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pi with a = 7.2278(3), b = 10.6259(4), c = 17.7614(6) ? a = 79.5990(10), = 83.6300(10), ? = 71.8280(10)o, V = 1272.60(8) ?, C48H44Cu4N8O24, Mr = 1371.07, Z = 1, Dc = 1.789 g/cm3, = 1.747 mm-1, F(000) = 696, R = 0.0397 and wR = 0.1137 for 3938 observed reflections (I > 2s(I)). There are two kinds of Cu coordination environments, and each central copper(II) atom is five-coordinated in a distorted square-based pyramidal coordination geo- metry. Four copper(II) atoms are linked by four pdc and two 4,4?-bipy ligands to form an annular rectangle structure. Extensive hydrogen-bonding interactions involving carboxylate O atoms as well as coordinated and free water molecules lead to the formation of a three-dimensional network struc- ture.展开更多
A supramolecular complex of Cd(II) with 1D water tapes as pillars[Cd2(dpa)2(phen)2(H2O)2]·6H2O 1 (H2dpa = diphenic acid, phen = phenanthroline), has been synthesized and characterized by elemental analy...A supramolecular complex of Cd(II) with 1D water tapes as pillars[Cd2(dpa)2(phen)2(H2O)2]·6H2O 1 (H2dpa = diphenic acid, phen = phenanthroline), has been synthesized and characterized by elemental analysis, IR spectroscopy, and single-crystal X-ray diffraction analysis. The crystal is of triclinic, space group P1^- with a = 9.7029(4), b = 11.9601(5), c = 12.1788(4) A, α = 71.6990(10), β = 71.8740(10), γ = 74.4680(10)°, V = 1252.39(8) A^3, C52H48Cd2N4O16, Mr = 1209.76, Z= 1, Dc = 1.604 g/cm^3,μ = 0.925 mm^-1, F(000) = 612, R = 0.0679 and wR = 0.2514 for 3870 observed reflections (I 〉 2σ(I)). Two intramolecular Cd(II) centers of this complex are encircled by two dpa^2- ligands forming an 18-membered ring, which is further assembled into a pillared three-dimensional (3D) supramolecular architecture through the synergetic effect of intermolecular face-to-face π…π stacking and weak O-H…O hydrogen-bonding interactions. Moreover, this complex exhibits photoluminescence with the main emission bands located at about 456 nm upon excitation at 355 nm in the solid state at room temperature.展开更多
A cluster compound, Mo3S4(DTP)3(IN)(Py)·EtOH I (DTP = diethyl dithiophosphate, IN = isonicotinate) has been rationally synthesized and characterized by single-crystal X-ray diffraction. The crystal belong...A cluster compound, Mo3S4(DTP)3(IN)(Py)·EtOH I (DTP = diethyl dithiophosphate, IN = isonicotinate) has been rationally synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 13.6345(2), b = 13.7805(2), c = 14.5400(1)A, α = 107.078(1), β = 113.380(1), γ = 96.310(1)°, C25H45Mo3- N2O9P3S10, Mr = 1218.96, V = 2315.75(5) A^3, Z = 2, Dc = 1.748 g/cm^3, μ = 1.399, F(000) = 1224, R = 0.0425 and wR = 0.1144 for 6335 observed reflections (I 〉 2σ(I)). 31^P NMR spectrum has been measured with the resonance 110.050 and 108.783 (2:1).展开更多
A new cobalt compound,{[Co(H2btec)(2,2'-bipy)(H2O)3]·H2O}n (1,H4btec=1,2,4,5-benzenetetracarboxylic acid,2,2'-bipy=2,2'-bipyridine),has been synthesized and charac-terized by single-crystal X-ray diffr...A new cobalt compound,{[Co(H2btec)(2,2'-bipy)(H2O)3]·H2O}n (1,H4btec=1,2,4,5-benzenetetracarboxylic acid,2,2'-bipy=2,2'-bipyridine),has been synthesized and charac-terized by single-crystal X-ray diffraction,elemental analysis,IR and X-ray powder diffraction.The crystal belongs to the triclinic system,space group P1,with a=7.230(3),b=11.626(5),c=14.001(6),α=108.12(0)°,β=95.85(0)°,V=1095.33(157)3,C20H20CoN2O12,Mr=539.31,Z= 2,Dc=1.635 g/cm3,μ=0.855 mm-1,F(000)=554,R=0.0427 and wR=0.1042 for 3883 observed reflections (I 〉 2σ(I)).The title compound features a discrete molecular structure,which is connected with each other through extensive O-H…O hydrogen bonds into an intricate 3D supramolecular network.Additionally,two different patterns of π-π stacking interactions further consolidate the framework.展开更多
基金the State Key Basic Research and Development Plan of China (001CB108906), the NNSF of China (No. 29733090 and No. 20173063), Key Project in KIP of CAS (KJCX2-H3) and the NSF of Fujian province (E0020001)
文摘A stable organometallic Pd (Ⅱ) compound Pd(ptac-C,N)(acac-O,O) (Hacac = acetyl acetone, Hptac = 3-(2-pyridinethioxy)-acac, formula: C15H17NO4SPd, Mr = 413.76) 1 has been synthesized and its crystal structure was determined by X-ray crystallography. The crystal is of monoclinic with space group C2/c, a = 17.9342(3), b = 17.7791(4), c = 13.1800(1) ? b = 128.400(1), V = 3293.5(1) 3, Z = 8, Dc = 1.669 g/cm3, F(000) = 1664, m = 1.269 mm-1, R = 0.0261 and wR = 0.0710 for 2653 observed reflections (I > 2s(I)). There exist two Pd rings in the title compound, C(14)O(4)PdO(3)C(12)C(13) and C(1)NPdC(8)S, with the palladium atom taking a square-planar coordination. Two oxygen atoms from the acetyl acetone ligand (PdO, 1.991(2) and 2.036(2) ), one N atom (PdN 2.019 ? and the g-carbon atom (PdC 2.067(3) ? from the ptac ligand are coordinated to Pd.
基金the State Key Basic Research and Development Plan of China (2007CB815302)the Chinese Academy of Sciences (KJCX2-YW-M05)+3 种基金the NSF (E0620005) of Fujian Provincethe Major Special Foundation of Fujian Province (2005HZ1027, 2005HZ01-1)the Fund of Fujian Key Laboratory of Nanomaterials (2006L2005)the Knowledge Innovation Program of the Chinese Academy of Sciences
文摘A new lanthanide coordination polymer, [Dy(OAc)(BDC)]n 1 (OAc = acetate, BDC = 1,4-benzenediacarboxylate), has been synthesized under hydrothermal conditions. Single-crystal X-ray diffraction analysis reveals that complex 1 has infinite zigzag Dy-OAc chains, which are further connected by BDC to form a 3D metal-organic framework. According to topology analysis, this framework can be characterized as (4,6)-connected (3.4.54)(32.4.56.66) net that has never been reported before. Crystal structure for 1: space group Pbca, a = 13.314(3), b = 8.0269(18), c = 20.275(5)A, V= 2166.8(9)A3, C10H7O6Dy, Mr = 385.66, Z= 8, Dc = 2.364 g/cm^3, μ= 6.910 mm^-1, F(000) = 1448, the final R = 0.0181 and wR = 0.0520.
文摘The title compound, [Cu(phen)2(SO4)(H2O)]·0.5C4H4O4·7H2O (phen = 1,10-phe-nan throline and C4H4O4 = fumaric acid), has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1^- with a = 11.4827(2), b = 11.9086(2), c = 13.77350(10) A, α = 80.6830(10), β = 66.6480(10), γ = 64.048000)°, V = 1554.63(4) A^3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm^3,μ = 0.845 mm^-1, F(000) = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections (1 〉 2σ(I)). The compound contains a six-coordinated copper(Ⅱ) center, which is surround by four N atoms of two phen ligands (Cu-N distances in the range of 1.997(2)- 2.225(2) A), one sulfate O atom (Cu-O = 2.0037(17) A) and one water O atom (Cu-O(Sw) = 2.719(2) A,) in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.
基金supported by 973 Program of China(2011CBA00505)National Key Technology R&D Program(2012BAE06B08)+1 种基金the Chinese Academy of Sciences(KJCX2-YW-H30)the Science Foundation of Fujian Province(2009HZ0005-1)
文摘One new coordination polymer, namely {[Zn(HL)(Hbipy)]2·3H2O}n(bipy = 4,4A-bipyridine, H4 L = 6-(3',4'-dicarboxyl-phenoxy) isophthalic acid), has been synthesized through a hydrothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectra(IR), and thermogravimetric(TG) analysis. The crystal structure is of monoclinic, space group P21/n with a = 9.6435(3), b = 19.8515(7), c = 12.9731(5) A, β = 103.023(4)o, V = 2419.67(15) A3, C52H38Zn2N4O21, Mr = 1185.6, Z = 2, Dc = 1.619 g/cm^3, F(000) = 1200, μ = 1.083 mm-1, the final R = 0.0443 and w R = 0.1079 for 4269 observed reflections(I 2σ(I). The compound features a two-dimensional(2D) framework and stabilizes itself by interlayer π···π interactions and innerlayer hydrogen bonds. The 2D layer presents a simple 3-connected 63 topology. Moreover, the thermal dynamic stability and luminescent property of the compound have also been discussed in detail.
基金This work was financially supported by the NNSFC (No. 20173063) the State Key Basic Research and Development Plan of China (001CB108906) and the NSF of Fujian Province (E0020001)
文摘The title compound {Cu2(pdc)2(4,4?-bipy)(H2O)3H2O}2 1 (H2pdc = pyridine-2,6- dicarboxylic acid, also known as dipicolinic acid; 4,4?-bipy = 4,4?-bipyridine) has been synthesized by the hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pi with a = 7.2278(3), b = 10.6259(4), c = 17.7614(6) ? a = 79.5990(10), = 83.6300(10), ? = 71.8280(10)o, V = 1272.60(8) ?, C48H44Cu4N8O24, Mr = 1371.07, Z = 1, Dc = 1.789 g/cm3, = 1.747 mm-1, F(000) = 696, R = 0.0397 and wR = 0.1137 for 3938 observed reflections (I > 2s(I)). There are two kinds of Cu coordination environments, and each central copper(II) atom is five-coordinated in a distorted square-based pyramidal coordination geo- metry. Four copper(II) atoms are linked by four pdc and two 4,4?-bipy ligands to form an annular rectangle structure. Extensive hydrogen-bonding interactions involving carboxylate O atoms as well as coordinated and free water molecules lead to the formation of a three-dimensional network struc- ture.
基金the State Key Basic Research and Development Plan of China (001CB108906)the Knowledge Innovation Program of the Chinese Academy of Sciences, the NSF (2006J0015)the Major Special Foundation of Fujian Province (2005HZ1027, 2005HZ01-1)
文摘A supramolecular complex of Cd(II) with 1D water tapes as pillars[Cd2(dpa)2(phen)2(H2O)2]·6H2O 1 (H2dpa = diphenic acid, phen = phenanthroline), has been synthesized and characterized by elemental analysis, IR spectroscopy, and single-crystal X-ray diffraction analysis. The crystal is of triclinic, space group P1^- with a = 9.7029(4), b = 11.9601(5), c = 12.1788(4) A, α = 71.6990(10), β = 71.8740(10), γ = 74.4680(10)°, V = 1252.39(8) A^3, C52H48Cd2N4O16, Mr = 1209.76, Z= 1, Dc = 1.604 g/cm^3,μ = 0.925 mm^-1, F(000) = 612, R = 0.0679 and wR = 0.2514 for 3870 observed reflections (I 〉 2σ(I)). Two intramolecular Cd(II) centers of this complex are encircled by two dpa^2- ligands forming an 18-membered ring, which is further assembled into a pillared three-dimensional (3D) supramolecular architecture through the synergetic effect of intermolecular face-to-face π…π stacking and weak O-H…O hydrogen-bonding interactions. Moreover, this complex exhibits photoluminescence with the main emission bands located at about 456 nm upon excitation at 355 nm in the solid state at room temperature.
基金This work was supported by the State Key Basic Research and Development Plan of China (001CB108906)the YIF (2005J060) and NSF (2006J0015) of Fujian Provincethe Major Special Foundation of Fujian Province (2005HZ1027 and 2005HZ01-1)
文摘A cluster compound, Mo3S4(DTP)3(IN)(Py)·EtOH I (DTP = diethyl dithiophosphate, IN = isonicotinate) has been rationally synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 13.6345(2), b = 13.7805(2), c = 14.5400(1)A, α = 107.078(1), β = 113.380(1), γ = 96.310(1)°, C25H45Mo3- N2O9P3S10, Mr = 1218.96, V = 2315.75(5) A^3, Z = 2, Dc = 1.748 g/cm^3, μ = 1.399, F(000) = 1224, R = 0.0425 and wR = 0.1144 for 6335 observed reflections (I 〉 2σ(I)). 31^P NMR spectrum has been measured with the resonance 110.050 and 108.783 (2:1).
基金supported by 973 Program (2007CB815302,2009CB939803)Chinese Academy of Sciences (KJCX2.YW.319,KJCX2.YW.M10,KJCX2-YW-M05)the Knowledge Innovation Program of Chinese Academy of Science,and Fujian Key Laboratory of Nanomaterials (2006L2005)
文摘A new cobalt compound,{[Co(H2btec)(2,2'-bipy)(H2O)3]·H2O}n (1,H4btec=1,2,4,5-benzenetetracarboxylic acid,2,2'-bipy=2,2'-bipyridine),has been synthesized and charac-terized by single-crystal X-ray diffraction,elemental analysis,IR and X-ray powder diffraction.The crystal belongs to the triclinic system,space group P1,with a=7.230(3),b=11.626(5),c=14.001(6),α=108.12(0)°,β=95.85(0)°,V=1095.33(157)3,C20H20CoN2O12,Mr=539.31,Z= 2,Dc=1.635 g/cm3,μ=0.855 mm-1,F(000)=554,R=0.0427 and wR=0.1042 for 3883 observed reflections (I 〉 2σ(I)).The title compound features a discrete molecular structure,which is connected with each other through extensive O-H…O hydrogen bonds into an intricate 3D supramolecular network.Additionally,two different patterns of π-π stacking interactions further consolidate the framework.