Compound [Co 3(BTC)(HBTC)(H 2BTC)(C 2H 4O 2) 3]·3(DMF)·6(H 3O) was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure ...Compound [Co 3(BTC)(HBTC)(H 2BTC)(C 2H 4O 2) 3]·3(DMF)·6(H 3O) was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure was solved by direct method and refined by full-matrix least-square method. The crystal is monoclinic and belongs to space group Cc with a=2.645 3(5) nm, b= 1.670 4(3) nm, c=1\^821 6(4) nm, β=128.16(3) °, V=6.329(2) nm 3, Z=2 , D c=20.200 Mg/m 3, M r= 1 314.744, μ=10.274 mm -1, F(000) =38 226, GOF=0.99, R=0.094 1, ωR=0.257 3.展开更多
Two new Gd Ⅲ complexes with nitrilotriacetic acid(nta) and trans-1,2-cyclohexanediaminetetraacetic acid(Cydta) ligands were synthesized. Their crystal structures were determined by single-crystal X-ray structure anal...Two new Gd Ⅲ complexes with nitrilotriacetic acid(nta) and trans-1,2-cyclohexanediaminetetraacetic acid(Cydta) ligands were synthesized. Their crystal structures were determined by single-crystal X-ray structure analyses. The crystal data are as follows: K 3[Gd Ⅲ(nta) 2·(H 2O)]·6H 2O, monoclinic system, C2/c space group, a=1.534 81(15) nm, b=1.292 05(12) nm, c=2.610 8(3) nm, β=96.244(2)°, V=5.146 7(9) nm 3, Z=8, M=776.87, D c=2.005 g/cm 3, μ= 3.149 mm -1 and \{F(000)=\}3 080, R=0.024 5, wR=0.064 3 for 4 455 unique reflections and R= 0.028 9, wR=0.067 2 for all 10 305 reflections. The Gd ⅢN 2O 7 part in the [Gd Ⅲ(nta) 2(H 2O)] 3- anion is a pseudo-monocapped square antiprismatic nine-coordination structure.(NH 4)[Gd Ⅲ(Cydta)(H 2O) 2]·5H 2O, triclinic system, P1 space group, a=0.866 2(3) nm, b=1.006 7(3) nm, c= 1.444 8(5) nm, α= 88.282(5)°, β=75\^190(5)°, γ=88.317(4)°, V=1.217 2(7) nm 3, Z=2, M=643.69, D c=1.756 g/cm 3, μ=2.798 mm -1 and F(000)=650, R=0.030 3, wR=0.080 9 for 4 273 unique reflections and R=0.033 2, wR=0.082 5 for all 5 062 reflections. The Gd ⅢN 2O 6 part in the [Gd Ⅲ(Cydta)(H 2O) 2] - anion has a pseudo-square antiprismatic eight-coordination structure.展开更多
The title compound H2SiW12O40·(CH3)2NH was synthesized in mixed solvent of aqueous and acetonitrile, and its crystal structure had been determined using single crystal X ray diffraction. The crystal belongs to mo...The title compound H2SiW12O40·(CH3)2NH was synthesized in mixed solvent of aqueous and acetonitrile, and its crystal structure had been determined using single crystal X ray diffraction. The crystal belongs to monoclinic, space group C2/m, a=2.0654(4)nm, b=1.3306(3)nm, c=1.3194(3)nm, β=119.59(3)°, V=3.1531(11)nm3, Dc=3.606Mg·m-3, Z=2, R=0.0462, Rw=0.0836. The title compound comprises of a 2+ unit, a polyanion and a free (CH3)2NH molecule. The ESR spectrum of the title compound shows that charge transfer between organic groups and polyanion takes place under irradiation of the sunlight in solid state. The TG study of the title compound shows that it had four stages of the weight loss, and the increase of the decomposition temperature for the polyanion shows that the stability of the polyanion was enhanced due to the influence of Zn2+ ion. CCDC:175866.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 mixed-valence trinuclear oxo-centered manganese complex Mn3O(O2CCC l3)6(py)2(H2O) was prepared by the reaction of NnBu4MnO4 with Mn(OAc)2·4H2O, t richloroacetic acid and pyridine in absolute EtOH. The cryst...A new mixed-valence trinuclear oxo-centered manganese complex Mn3O(O2CCC l3)6(py)2(H2O) was prepared by the reaction of NnBu4MnO4 with Mn(OAc)2·4H2O, t richloroacetic acid and pyridine in absolute EtOH. The crystal structure was det ermined. The complex crystallizes in monoclinic, space group P21/c, unit cell pa rameters, a=14.951(1), b=20.791(2), c=17.882(1),á=?=90a=102.67(1)展开更多
A new compound 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] has been hydrothermally synthesized. Single crystal X-ray analysis indicates that this compound crystallizes in a monoclinic system, space group P2 1/n with a=1.438 5...A new compound 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] has been hydrothermally synthesized. Single crystal X-ray analysis indicates that this compound crystallizes in a monoclinic system, space group P2 1/n with a=1.438 5(3) nm, b=1.012 2(2) nm, c=1.832 5(4) nm, β=90.21°, V=2\^668 2(9) nm 3, Z=2, D c=2.112 g/cm 3, R=0.055, wR=0.149 7, S=1.037. The structure of 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] is characterized by P-V-O layers constructed by [(VO) 4(OH) 2(PO 4) 4] 6- non-symmetric units. The P-V-O layers are pillared by [Co(H 2O) 2] 2+ group, resulting in the channels within which the protonated diaminoethane and H 3O + are located.展开更多
文摘Compound [Co 3(BTC)(HBTC)(H 2BTC)(C 2H 4O 2) 3]·3(DMF)·6(H 3O) was synthesized under mild conditions and its crystal structure was determined by using single crystal X-ray diffraction. The crystal structure was solved by direct method and refined by full-matrix least-square method. The crystal is monoclinic and belongs to space group Cc with a=2.645 3(5) nm, b= 1.670 4(3) nm, c=1\^821 6(4) nm, β=128.16(3) °, V=6.329(2) nm 3, Z=2 , D c=20.200 Mg/m 3, M r= 1 314.744, μ=10.274 mm -1, F(000) =38 226, GOF=0.99, R=0.094 1, ωR=0.257 3.
文摘Two new Gd Ⅲ complexes with nitrilotriacetic acid(nta) and trans-1,2-cyclohexanediaminetetraacetic acid(Cydta) ligands were synthesized. Their crystal structures were determined by single-crystal X-ray structure analyses. The crystal data are as follows: K 3[Gd Ⅲ(nta) 2·(H 2O)]·6H 2O, monoclinic system, C2/c space group, a=1.534 81(15) nm, b=1.292 05(12) nm, c=2.610 8(3) nm, β=96.244(2)°, V=5.146 7(9) nm 3, Z=8, M=776.87, D c=2.005 g/cm 3, μ= 3.149 mm -1 and \{F(000)=\}3 080, R=0.024 5, wR=0.064 3 for 4 455 unique reflections and R= 0.028 9, wR=0.067 2 for all 10 305 reflections. The Gd ⅢN 2O 7 part in the [Gd Ⅲ(nta) 2(H 2O)] 3- anion is a pseudo-monocapped square antiprismatic nine-coordination structure.(NH 4)[Gd Ⅲ(Cydta)(H 2O) 2]·5H 2O, triclinic system, P1 space group, a=0.866 2(3) nm, b=1.006 7(3) nm, c= 1.444 8(5) nm, α= 88.282(5)°, β=75\^190(5)°, γ=88.317(4)°, V=1.217 2(7) nm 3, Z=2, M=643.69, D c=1.756 g/cm 3, μ=2.798 mm -1 and F(000)=650, R=0.030 3, wR=0.080 9 for 4 273 unique reflections and R=0.033 2, wR=0.082 5 for all 5 062 reflections. The Gd ⅢN 2O 6 part in the [Gd Ⅲ(Cydta)(H 2O) 2] - anion has a pseudo-square antiprismatic eight-coordination structure.
文摘The title compound H2SiW12O40·(CH3)2NH was synthesized in mixed solvent of aqueous and acetonitrile, and its crystal structure had been determined using single crystal X ray diffraction. The crystal belongs to monoclinic, space group C2/m, a=2.0654(4)nm, b=1.3306(3)nm, c=1.3194(3)nm, β=119.59(3)°, V=3.1531(11)nm3, Dc=3.606Mg·m-3, Z=2, R=0.0462, Rw=0.0836. The title compound comprises of a 2+ unit, a polyanion and a free (CH3)2NH molecule. The ESR spectrum of the title compound shows that charge transfer between organic groups and polyanion takes place under irradiation of the sunlight in solid state. The TG study of the title compound shows that it had four stages of the weight loss, and the increase of the decomposition temperature for the polyanion shows that the stability of the polyanion was enhanced due to the influence of Zn2+ ion. CCDC:175866.
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 mixed-valence trinuclear oxo-centered manganese complex Mn3O(O2CCC l3)6(py)2(H2O) was prepared by the reaction of NnBu4MnO4 with Mn(OAc)2·4H2O, t richloroacetic acid and pyridine in absolute EtOH. The crystal structure was det ermined. The complex crystallizes in monoclinic, space group P21/c, unit cell pa rameters, a=14.951(1), b=20.791(2), c=17.882(1),á=?=90a=102.67(1)
文摘A new compound 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] has been hydrothermally synthesized. Single crystal X-ray analysis indicates that this compound crystallizes in a monoclinic system, space group P2 1/n with a=1.438 5(3) nm, b=1.012 2(2) nm, c=1.832 5(4) nm, β=90.21°, V=2\^668 2(9) nm 3, Z=2, D c=2.112 g/cm 3, R=0.055, wR=0.149 7, S=1.037. The structure of 2 6[Co(H 2O) 2(VO) 8(OH) 4(PO 4) 8] is characterized by P-V-O layers constructed by [(VO) 4(OH) 2(PO 4) 4] 6- non-symmetric units. The P-V-O layers are pillared by [Co(H 2O) 2] 2+ group, resulting in the channels within which the protonated diaminoethane and H 3O + are located.
