A chainlike coordination polymer [Gd（dca）3（phen）2（H2O）], （dca=dicyanamide, phen=1,10-phenanthroline） has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The c...A chainlike coordination polymer [Gd（dca）3（phen）2（H2O）], （dca=dicyanamide, phen=1,10-phenanthroline） has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a=10.6581（13）, b=15.6129（16）, c=17.733（3）A°,β=90.499（5）°, V=2950.8（7）A°^3, Z= , C3oH18GdN13O, Mr=733.82, De= 1.652 g/cm^3, F（000）=1444, λ（MoKα）=0.71073A°,μ=2.297 mm^-1, R=0.0258 and wR=0.0616 for 4570 observed reflections （I〉 2σ（I））. In this complex, the gadolinium atom is nine-coordinated by four dca anions, two chelated phen ligands and one H2O molecule in a distorted tricapped trigonal prism. Two bridging dca anions connect the Gd（Ⅲ） ions yielding chainlike polymers that are linked by hydrogen bonds and π-π interactions to form a three-dimensional network.展开更多
The crystal structure of the title complex[Li (dme)3] [(t-BuC_5H_4)_2Gd (NPh_2)_2]·1/2dme,C56H81O7N2LiGd(M,r=1058. 63), has been determined by single-crystal X-ray diffraction. The crystal is triclinic with space...The crystal structure of the title complex[Li (dme)3] [(t-BuC_5H_4)_2Gd (NPh_2)_2]·1/2dme,C56H81O7N2LiGd(M,r=1058. 63), has been determined by single-crystal X-ray diffraction. The crystal is triclinic with space group P1, a=12. 741 (3),b =13. 353(3), c=16. 843(4) A, a=94. 70(2), β=91. 57(2)', r=92. 03(2), V=2852. 7(1) A3, Dc= 1.23g/cm3, F(000)=1038, u=12. 5 cm-1, Z=2, and finalR=0. 050 and Rw=0. 045 for 5829 reflections (I≥3d(I)). The structure analysis re-vealed that the complex consists of disconnected ion pairs of (Li (dine)3 ]+ and [(t-BuC5H4),Gd (NPh2)2]-. The Gd atom is connected to two n5-bonded t-butylcy-clopentadienyl groups and two a bonded diphenylamidos in a distorted tetrahedral ar-rangement. The Li atom is coordinated by six O atoms from three dimethoxyethane lig-ands forming an octahedron structure.展开更多
Crystals of a new lanthanide orthosilicate, Gd_3Br(SiO_4)_2 (M_r=735.82) were prepared by solid state reaction from the GdOBr/V/NH_4Br system at 900℃. The ammonium bromide served as transport gas. The title compound ...Crystals of a new lanthanide orthosilicate, Gd_3Br(SiO_4)_2 (M_r=735.82) were prepared by solid state reaction from the GdOBr/V/NH_4Br system at 900℃. The ammonium bromide served as transport gas. The title compound crystallizes on orthorhombic, space group Imma with a=6.960(3), b=18. 176(6), c=6. 284(2) A ; V=794. 9(5) A￣3; Z=4; D_c=6. 12 g/cm￣3 F(000)=1276; μ(MoKα)=301.63cm￣(-1). A full-matrix least-squares structure factors refined with the 484 observed reflections with I>3. 0σ (I) and anisotropic thermal parameters for the Gd atoms gave R=0.061 and R_w=0. 064 respectively. The gadolinium atoms are in two sites and 8-coordinated as GdO_6Br_2 and GdO_7Br bicapped trigonal prism. The Gd(2) atom is disordered and distributed systematically among two I-lattice related(81) positions, the distance between these positions is 1.599 A. The presence of the bromine atoms causes some long Gd - O bonds. The silicon atoms were extracted from the quartz tube.展开更多
The hydrothermal reaction of pyridine-3,4-dicarboxylic acid(pydcH2),4,4'-bipyridine and GdCl3.6H2O yield a novel gadolinium coordination polymer {[Gd2(pydc)2(μ3-OH)2(H2O)2].H2O}n(1).The compound was chara-cterize...The hydrothermal reaction of pyridine-3,4-dicarboxylic acid(pydcH2),4,4'-bipyridine and GdCl3.6H2O yield a novel gadolinium coordination polymer {[Gd2(pydc)2(μ3-OH)2(H2O)2].H2O}n(1).The compound was chara-cterized by elemental analysis,thermal analysis,IR spectra and single-crystal X-ray structure analysis.The crystal of the Gd(Ⅲ) complex belongs to triclinic system,space group P1 with:a=0.796 25(16) nm,b=0.944 46(19) nm,c=1.262 1(3) nm,α=76.50(3)°,β=84.95(3)°,γ=83.04(3)°,Z=2,V=0.914 4(3) nm3,Dc=2.669 g.cm-1,μ=7.269 mm-1,F(000)=692,and R1=0.033 3,wR2=0.062 3.The crystal structure revealed that compound 1 has a 2D layer structure incorporating 1D Gd-O-Gd double chain,and hydrogen bonding interactions result in the former of 3D supramolecular network structure.CCDC:669079.展开更多
基金Supported by the National Natural Science Foundation of China (20201008, 50272034)
文摘A chainlike coordination polymer [Gd（dca）3（phen）2（H2O）], （dca=dicyanamide, phen=1,10-phenanthroline） has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a=10.6581（13）, b=15.6129（16）, c=17.733（3）A°,β=90.499（5）°, V=2950.8（7）A°^3, Z= , C3oH18GdN13O, Mr=733.82, De= 1.652 g/cm^3, F（000）=1444, λ（MoKα）=0.71073A°,μ=2.297 mm^-1, R=0.0258 and wR=0.0616 for 4570 observed reflections （I〉 2σ（I））. In this complex, the gadolinium atom is nine-coordinated by four dca anions, two chelated phen ligands and one H2O molecule in a distorted tricapped trigonal prism. Two bridging dca anions connect the Gd（Ⅲ） ions yielding chainlike polymers that are linked by hydrogen bonds and π-π interactions to form a three-dimensional network.
文摘The crystal structure of the title complex[Li (dme)3] [(t-BuC_5H_4)_2Gd (NPh_2)_2]·1/2dme,C56H81O7N2LiGd(M,r=1058. 63), has been determined by single-crystal X-ray diffraction. The crystal is triclinic with space group P1, a=12. 741 (3),b =13. 353(3), c=16. 843(4) A, a=94. 70(2), β=91. 57(2)', r=92. 03(2), V=2852. 7(1) A3, Dc= 1.23g/cm3, F(000)=1038, u=12. 5 cm-1, Z=2, and finalR=0. 050 and Rw=0. 045 for 5829 reflections (I≥3d(I)). The structure analysis re-vealed that the complex consists of disconnected ion pairs of (Li (dine)3 ]+ and [(t-BuC5H4),Gd (NPh2)2]-. The Gd atom is connected to two n5-bonded t-butylcy-clopentadienyl groups and two a bonded diphenylamidos in a distorted tetrahedral ar-rangement. The Li atom is coordinated by six O atoms from three dimethoxyethane lig-ands forming an octahedron structure.
文摘Crystals of a new lanthanide orthosilicate, Gd_3Br(SiO_4)_2 (M_r=735.82) were prepared by solid state reaction from the GdOBr/V/NH_4Br system at 900℃. The ammonium bromide served as transport gas. The title compound crystallizes on orthorhombic, space group Imma with a=6.960(3), b=18. 176(6), c=6. 284(2) A ; V=794. 9(5) A￣3; Z=4; D_c=6. 12 g/cm￣3 F(000)=1276; μ(MoKα)=301.63cm￣(-1). A full-matrix least-squares structure factors refined with the 484 observed reflections with I>3. 0σ (I) and anisotropic thermal parameters for the Gd atoms gave R=0.061 and R_w=0. 064 respectively. The gadolinium atoms are in two sites and 8-coordinated as GdO_6Br_2 and GdO_7Br bicapped trigonal prism. The Gd(2) atom is disordered and distributed systematically among two I-lattice related(81) positions, the distance between these positions is 1.599 A. The presence of the bromine atoms causes some long Gd - O bonds. The silicon atoms were extracted from the quartz tube.
文摘The hydrothermal reaction of pyridine-3,4-dicarboxylic acid(pydcH2),4,4'-bipyridine and GdCl3.6H2O yield a novel gadolinium coordination polymer {[Gd2(pydc)2(μ3-OH)2(H2O)2].H2O}n(1).The compound was chara-cterized by elemental analysis,thermal analysis,IR spectra and single-crystal X-ray structure analysis.The crystal of the Gd(Ⅲ) complex belongs to triclinic system,space group P1 with:a=0.796 25(16) nm,b=0.944 46(19) nm,c=1.262 1(3) nm,α=76.50(3)°,β=84.95(3)°,γ=83.04(3)°,Z=2,V=0.914 4(3) nm3,Dc=2.669 g.cm-1,μ=7.269 mm-1,F(000)=692,and R1=0.033 3,wR2=0.062 3.The crystal structure revealed that compound 1 has a 2D layer structure incorporating 1D Gd-O-Gd double chain,and hydrogen bonding interactions result in the former of 3D supramolecular network structure.CCDC:669079.
