Synthesis of complexes（η;-CH;C;H;）M（CO）;NO（M=Mo,I;M=W,II）and clusters（η;-CH;C;H;）M（μ;-NH）(μ;-NO) （μ;-CO）Fe;（CO）;（M=Mo,III:M=W,IV）,based on the reaction of （η;-C5;）M（CO）;Cl with Na[Fe（CO）;NO...Synthesis of complexes（η;-CH;C;H;）M（CO）;NO（M=Mo,I;M=W,II）and clusters（η;-CH;C;H;）M（μ;-NH）(μ;-NO) （μ;-CO）Fe;（CO）;（M=Mo,III:M=W,IV）,based on the reaction of （η;-C5;）M（CO）;Cl with Na[Fe（CO）;NO] at room tem-perature,have been demonstrated,The crystal structures of II and IV arealso presented.展开更多
The crystal structure of a new type arylarsonic polytungstate[C(NH_)_]_4[p-NH_3C_6H_4As)_2- W_6O_(25)]·4H_O was determined by single-crystal X-ray diffraction analysis.It belongs to triclinic,space group P,with c...The crystal structure of a new type arylarsonic polytungstate[C(NH_)_]_4[p-NH_3C_6H_4As)_2- W_6O_(25)]·4H_O was determined by single-crystal X-ray diffraction analysis.It belongs to triclinic,space group P,with cell dimensions a=12.863(3),b=18.912(3),c=21.383(4)α=91.14(2)°,β= 93.65(3)°,γ=92.25(3)°,V=5185.9~3,Z=4,D_c=2.753g/cm^3.The intensity data were collected on an Enraf-Nonius CAD4 diffractometer with Mo Kα radiation.The positions of all tungsten and arsenic atoms were determined by direct method.The other non-hydrogen atoms were revealed by difference Fourier synthesis.The structure was refined by fullmatrix least-squares procedure to a final R value of 0.070.The crystal structure contains two similar but nonidentical molecules.Two similar anions consist of a ring of six WO_6 octahedra,which are connected with one face-sharing,two corner-sharings and three edge-sharings,and two p-aminophenylarsonic tetrahedra capped above and below the ring. In each WO_6 ring,four tungsten atoms,which are joined with edge-sharing oxygen atoms,are almost coplanar,while the two others,which are joined with face-sharing oxygen atoms,protrude out of the ring towards the same side.The two arsenic atoms in each anion are not equivalent in their bonding manner.In each anion,all non-hydrogen atoms of each organic group are in the same plane.Each molecule contains one anion,four C(NH_2)_3^+ cations and four water molecules.There are many hydrogen bonds between cations and anions throughout the whole crystal.The amino groups can accept protons,so that the charge of the resulting anion decreases and[(RAs)_2W_6O_(25)]^(4-)type complexes are formed.展开更多
This paper reported an efficient and economical method for preparation of anhydrous LaBr3 for scintillation crystal growth. High purity anhydrous LaBr3 powders in large quantities were successfully obtained by stepped...This paper reported an efficient and economical method for preparation of anhydrous LaBr3 for scintillation crystal growth. High purity anhydrous LaBr3 powders in large quantities were successfully obtained by stepped dehydration of LaBr3-7H2O using NH4Br as additive. Experiments revealed that adding proper amount of NHaBr could effectively restrain the hydrolysis of LaBr3 during dehydration and thus decreased the yield of deleterious impurity of LaOBr. Optimum preparation conditions, including the amount of NH4Br in use, the dehydration temperature and atmosphere, were investigated by DTA/TG and water/oxygen analysis. The Raman characterization of the as-prepared anhydrous LaBr3 was also presented.展开更多
文摘Synthesis of complexes（η;-CH;C;H;）M（CO）;NO（M=Mo,I;M=W,II）and clusters（η;-CH;C;H;）M（μ;-NH）(μ;-NO) （μ;-CO）Fe;（CO）;（M=Mo,III:M=W,IV）,based on the reaction of （η;-C5;）M（CO）;Cl with Na[Fe（CO）;NO] at room tem-perature,have been demonstrated,The crystal structures of II and IV arealso presented.
文摘The crystal structure of a new type arylarsonic polytungstate[C(NH_)_]_4[p-NH_3C_6H_4As)_2- W_6O_(25)]·4H_O was determined by single-crystal X-ray diffraction analysis.It belongs to triclinic,space group P,with cell dimensions a=12.863(3),b=18.912(3),c=21.383(4)α=91.14(2)°,β= 93.65(3)°,γ=92.25(3)°,V=5185.9~3,Z=4,D_c=2.753g/cm^3.The intensity data were collected on an Enraf-Nonius CAD4 diffractometer with Mo Kα radiation.The positions of all tungsten and arsenic atoms were determined by direct method.The other non-hydrogen atoms were revealed by difference Fourier synthesis.The structure was refined by fullmatrix least-squares procedure to a final R value of 0.070.The crystal structure contains two similar but nonidentical molecules.Two similar anions consist of a ring of six WO_6 octahedra,which are connected with one face-sharing,two corner-sharings and three edge-sharings,and two p-aminophenylarsonic tetrahedra capped above and below the ring. In each WO_6 ring,four tungsten atoms,which are joined with edge-sharing oxygen atoms,are almost coplanar,while the two others,which are joined with face-sharing oxygen atoms,protrude out of the ring towards the same side.The two arsenic atoms in each anion are not equivalent in their bonding manner.In each anion,all non-hydrogen atoms of each organic group are in the same plane.Each molecule contains one anion,four C(NH_2)_3^+ cations and four water molecules.There are many hydrogen bonds between cations and anions throughout the whole crystal.The amino groups can accept protons,so that the charge of the resulting anion decreases and[(RAs)_2W_6O_(25)]^(4-)type complexes are formed.
基金Project supported by National Basic Research Program of China (2012CBA01207)
文摘This paper reported an efficient and economical method for preparation of anhydrous LaBr3 for scintillation crystal growth. High purity anhydrous LaBr3 powders in large quantities were successfully obtained by stepped dehydration of LaBr3-7H2O using NH4Br as additive. Experiments revealed that adding proper amount of NHaBr could effectively restrain the hydrolysis of LaBr3 during dehydration and thus decreased the yield of deleterious impurity of LaOBr. Optimum preparation conditions, including the amount of NH4Br in use, the dehydration temperature and atmosphere, were investigated by DTA/TG and water/oxygen analysis. The Raman characterization of the as-prepared anhydrous LaBr3 was also presented.
