The crystal structure of the compound was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P21/n, a=1.136 1(3)nm, b=0.709 8(2) nm, c=1.459 7(4) nm, β=107.538(4...The crystal structure of the compound was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P21/n, a=1.136 1(3)nm, b=0.709 8(2) nm, c=1.459 7(4) nm, β=107.538(4)°, V=1.122 4(6) nm3, Dc=1.858 g·cm-1, Z=4, F(000)=648, R1=0.0264, wR2=0.0665. CCDC: 224880.展开更多
A new compound, \[Ni(en)\-3\]\-2\[Ni(en)\-2(H\-2O)\-2\]\[As\-6V\-\{15\}O\-\{42\}\]·4H\-2O, was first prepared by hydrothermal synthesis and characterized by elemental analysis, IR, TGA\|DSC, ESR and single crysta...A new compound, \[Ni(en)\-3\]\-2\[Ni(en)\-2(H\-2O)\-2\]\[As\-6V\-\{15\}O\-\{42\}\]·4H\-2O, was first prepared by hydrothermal synthesis and characterized by elemental analysis, IR, TGA\|DSC, ESR and single crystal X\|ray diffraction. Crystal data: monoclinic, space group \%C\-c, a\%=1\^523 6(3) nm, \%b\%=2\^051 8(4) nm, \%c\%=2\^395 9(5) nm, \%β=97\^41(3)°, V\%=7\^427(3) nm\+3, \%Z=4, R=0\^057 0, wR\-2=0\^135 7\%. The polyanion consists of six AsO\-3 pyramids and fifteen VO\-5 pyramids. Counterions are complex ions with octahedral structure, which consist of NH\-2CH\-2CH\-2NH\-2 and Ni\+\{2+\}.展开更多
A new two dimensional 8 ring network nickle phosphate Ni 3(PO 4) 2·8H 2O was synthesized hydrothermally and its structure was determined by means of single crystal X ray diffraction. The Ni 3(PO 4) 2·8H 2O c...A new two dimensional 8 ring network nickle phosphate Ni 3(PO 4) 2·8H 2O was synthesized hydrothermally and its structure was determined by means of single crystal X ray diffraction. The Ni 3(PO 4) 2·8H 2O crystal crystallizes in the monoclinic system, space group C2/m , with M=128.13, a =0\^994 7(2) nm, b =1.321 7(3) nm; c =0.463 6(1) nm; β=104.80(3)°, V =0.589 3(2) nm 3, Z=2, R=0.027 2 and wR =0.057 5. The network structure consists of vertex sharing which results in the formation of undulating 4 ring chains and 8 ring sheets.展开更多
Additive reactions of Ni[(C 4H 9O) 2PS 2] 2 with ethylamine,diethylamine and triethylamine were studied by spectrophotometric methods in ethanol at several tempertures.With ethylamine,the adduct formation of NiL 2...Additive reactions of Ni[(C 4H 9O) 2PS 2] 2 with ethylamine,diethylamine and triethylamine were studied by spectrophotometric methods in ethanol at several tempertures.With ethylamine,the adduct formation of NiL 2·B and NiL 2·B 2 was established.For diethylamine and triethylamine,being of their steric hindrance effect,the formation of NiL 2·B only was concluded.Their additive equilibrium constants(lg β n)and additive molecular number(n) were discussed.Thermodynamic parameters △ r H m and △ r S m were found by the least square method.The additive equilibrium constants in the range 278 0～303 0K were described by empirical equation.展开更多
A Hydrothermal reaction of MoO 3, NiCl 2·6H 2O, WO 3 and H 2O with a molar ratio of 1∶0.6∶1∶83.3 gives a rhombic-shaped black crystal [NiMo 12O 40H 10{Ni(H 2O) 3} 4]. It crystallizes in a tetragonal system wit...A Hydrothermal reaction of MoO 3, NiCl 2·6H 2O, WO 3 and H 2O with a molar ratio of 1∶0.6∶1∶83.3 gives a rhombic-shaped black crystal [NiMo 12O 40H 10{Ni(H 2O) 3} 4]. It crystallizes in a tetragonal system with space group I4 1/amd and unit cell parameters a=b=1.518 4(2) nm, c=3.082 9(6) nm, Z=4, V=7.108(2) nm 3, R=0.067 1, wR=0.217 8. The compound possesses a four-capped Keggin structure. The structure of the Keggin- [NiMo 12O 40H 10] 8- consists of twelve MoO 6 octahedrons and a NiO 4 tetrahedron on the center. Four [Ni(H 2O) 3] 2+ at the cap positions are linked to Keggin-structure by three μ 3-O, respectively. The calculation of bond valence shows that the oxidation state of Mo in the compound is +5.展开更多
Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3...Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.展开更多
The structure of single crystal of the polyoxotungstate salt Na10{(PW9O34)2Ni4（H2O）2}·26H2O ( Na10Ni4O96P2W18H56, Mr=5371.96) has been determined by X-ray diffraction (MoK（）. Crystal data: P21/n, a=11.898（2...The structure of single crystal of the polyoxotungstate salt Na10{(PW9O34)2Ni4（H2O）2}·26H2O ( Na10Ni4O96P2W18H56, Mr=5371.96) has been determined by X-ray diffraction (MoK（）. Crystal data: P21/n, a=11.898（2）, b=16.629（4）, c=21.413（4） ?, ( = 100.59（1）o, V= 4164.5（1） ?3, Z=2, Dc = 4.284g/cm3, F（000） = 4704, ( =2.5847cm-1, final R = 0.0344, and wR= 0.0804 for 5830 independent reflections. Two B-(-PW9O349- units in the compound are linked via a set of four coplanar Ni2+ atoms, which also carry H2O ligands. The NiO6 octahedra in each centrosymmetric anion are all tetragonally elongated with their long axes parallel.展开更多
文摘The crystal structure of the compound was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P21/n, a=1.136 1(3)nm, b=0.709 8(2) nm, c=1.459 7(4) nm, β=107.538(4)°, V=1.122 4(6) nm3, Dc=1.858 g·cm-1, Z=4, F(000)=648, R1=0.0264, wR2=0.0665. CCDC: 224880.
文摘A new compound, \[Ni(en)\-3\]\-2\[Ni(en)\-2(H\-2O)\-2\]\[As\-6V\-\{15\}O\-\{42\}\]·4H\-2O, was first prepared by hydrothermal synthesis and characterized by elemental analysis, IR, TGA\|DSC, ESR and single crystal X\|ray diffraction. Crystal data: monoclinic, space group \%C\-c, a\%=1\^523 6(3) nm, \%b\%=2\^051 8(4) nm, \%c\%=2\^395 9(5) nm, \%β=97\^41(3)°, V\%=7\^427(3) nm\+3, \%Z=4, R=0\^057 0, wR\-2=0\^135 7\%. The polyanion consists of six AsO\-3 pyramids and fifteen VO\-5 pyramids. Counterions are complex ions with octahedral structure, which consist of NH\-2CH\-2CH\-2NH\-2 and Ni\+\{2+\}.
文摘A new two dimensional 8 ring network nickle phosphate Ni 3(PO 4) 2·8H 2O was synthesized hydrothermally and its structure was determined by means of single crystal X ray diffraction. The Ni 3(PO 4) 2·8H 2O crystal crystallizes in the monoclinic system, space group C2/m , with M=128.13, a =0\^994 7(2) nm, b =1.321 7(3) nm; c =0.463 6(1) nm; β=104.80(3)°, V =0.589 3(2) nm 3, Z=2, R=0.027 2 and wR =0.057 5. The network structure consists of vertex sharing which results in the formation of undulating 4 ring chains and 8 ring sheets.
文摘Additive reactions of Ni[(C 4H 9O) 2PS 2] 2 with ethylamine,diethylamine and triethylamine were studied by spectrophotometric methods in ethanol at several tempertures.With ethylamine,the adduct formation of NiL 2·B and NiL 2·B 2 was established.For diethylamine and triethylamine,being of their steric hindrance effect,the formation of NiL 2·B only was concluded.Their additive equilibrium constants(lg β n)and additive molecular number(n) were discussed.Thermodynamic parameters △ r H m and △ r S m were found by the least square method.The additive equilibrium constants in the range 278 0～303 0K were described by empirical equation.
文摘A Hydrothermal reaction of MoO 3, NiCl 2·6H 2O, WO 3 and H 2O with a molar ratio of 1∶0.6∶1∶83.3 gives a rhombic-shaped black crystal [NiMo 12O 40H 10{Ni(H 2O) 3} 4]. It crystallizes in a tetragonal system with space group I4 1/amd and unit cell parameters a=b=1.518 4(2) nm, c=3.082 9(6) nm, Z=4, V=7.108(2) nm 3, R=0.067 1, wR=0.217 8. The compound possesses a four-capped Keggin structure. The structure of the Keggin- [NiMo 12O 40H 10] 8- consists of twelve MoO 6 octahedrons and a NiO 4 tetrahedron on the center. Four [Ni(H 2O) 3] 2+ at the cap positions are linked to Keggin-structure by three μ 3-O, respectively. The calculation of bond valence shows that the oxidation state of Mo in the compound is +5.
基金Project supported by China National Climbing plan and National Nature Science Foundation
文摘Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the mole ratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10) 2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and the structure was determined by four-circle diffractometer. Data showed that the crystal is in space group C2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A^3. The structure was solved by a combination of Patterson method and Fourier technique. The final R value is 0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form an essentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atoms are five-coordinate.
基金grants from the State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, CAS, the
文摘The structure of single crystal of the polyoxotungstate salt Na10{(PW9O34)2Ni4（H2O）2}·26H2O ( Na10Ni4O96P2W18H56, Mr=5371.96) has been determined by X-ray diffraction (MoK（）. Crystal data: P21/n, a=11.898（2）, b=16.629（4）, c=21.413（4） ?, ( = 100.59（1）o, V= 4164.5（1） ?3, Z=2, Dc = 4.284g/cm3, F（000） = 4704, ( =2.5847cm-1, final R = 0.0344, and wR= 0.0804 for 5830 independent reflections. Two B-(-PW9O349- units in the compound are linked via a set of four coplanar Ni2+ atoms, which also carry H2O ligands. The NiO6 octahedra in each centrosymmetric anion are all tetragonally elongated with their long axes parallel.
