An inorganic-organic hybrid thioantimonate（Ⅲ） [CH3（CH2）3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system, space group P1 with a = 7.0124（11）, b ...An inorganic-organic hybrid thioantimonate（Ⅲ） [CH3（CH2）3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system, space group P1 with a = 7.0124（11）, b = 11.919（2）, c =14.879（3）A, α = 108.791（3）, β= 102.441（3）, γ = 92.846（2）°, V= 1140.1（3）A3, Mr = 859.71, Z= 2, Do = 2.504 g/cm^3 ,μ = 5.324 mm^-1, F（000） = 804, S = 1.013, the Final R = 0.0297 and wR = 0.0618 for 3534 observed reflections with Ⅰ 〉 2 σ（Ⅰ）. 1 consists of [C4HgNH3]＋ cations and two-dimensional [Sb4ST]n^2n- anion which is composed of three SbS3 trigonal pyranaids and one SbS4 unit joined by sharing common comers. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]^＋ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.展开更多
A new polyborate containing ehiral metal-complex Zn（en）3 B5O7（OH）3, where en = ethylenediamine, was synthesizedunder solvothermal conditions and structurally characterized by means of X-ray diffraction analysis. C...A new polyborate containing ehiral metal-complex Zn（en）3 B5O7（OH）3, where en = ethylenediamine, was synthesizedunder solvothermal conditions and structurally characterized by means of X-ray diffraction analysis. Crystal data： Zn（en）3 B5O7（OH）3, monoclinic, space group P21/c, a =0.8532（72） nm, b =2.3340（5） nm, c = 0.9526（92） nm, β =107. 04（3）°, Z=4, V=1.8140（6） nm^3, Dc =1.694 g/cm^3, p=1.416 mm^-1, F（000） = 960, GOF = 1. 020, R =0. 0276, Rw =0. 0828. There is a chiral Zn（en）3^2＋ complex cation and an isolated B5O7（OH）3^2- group in a Zn（en）3 B5O7（OH）3 molecule. The enantiomer of the chiral complex cation is separated orderly as ,4 and A configurations in the compound and the borate group consists of two B303 cycles linked through a bridging boron atom.展开更多
A new selenidoarsenate [Co（en）3]2As2Se5 1 （en = ethylenediamine） was synthesized by a reaction of AsCI3, CoCl2-6H2O and Se in en under mild solvothermal conditions, and the structure was determined by single-cryst...A new selenidoarsenate [Co（en）3]2As2Se5 1 （en = ethylenediamine） was synthesized by a reaction of AsCI3, CoCl2-6H2O and Se in en under mild solvothermal conditions, and the structure was determined by single-crystal X-ray diffraction. 1 crystallizes in the orthorhombic system, space group Pbca with a = 15.5092（12）, b = 11.5756（9）, c = 17.8138（14） A, V = 3198.1（4） A^3, Mr= 1023.12, Z = 4, D, = 2.125 g/cm^3,μ = 8.807 mm^-1, F（000） = 1976, S = 1.171, the final R = 0.0591 and wR = 0.1067 for 3170 observed reflections with 1 〉 2σ（I）. 1 consists of isolated dimeric [As2Se5]^4- anion constructed by two corner-sharing AsSe3 trigonal pyramids and transition metal [Co（en）3]^2＋ cations. The optical absorption property and thermal stability of 1 are reported.展开更多
Two new borate compounds, C4H10N2·B6O8（OH）2 and （NH3CH2CH2NH3）B5O8 （OH）2, have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction, IR, elemental analysis and...Two new borate compounds, C4H10N2·B6O8（OH）2 and （NH3CH2CH2NH3）B5O8 （OH）2, have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction, IR, elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system, space group P21/c, with a = 8.3318（17）, b = 6.2118（12）, c = 12.479（3） A, β = 108.96（3）°, V = 610.8（2） A^3, Mr = 313.02, Z = 2, 13,.= 1.702 g/cm^,/J = 0.150 mm^-1, F（000） = 320, R = 0.0387 and wR = 0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system, which are built up from alternative B6O8（OH）2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic, space group Co, with a = 6.7207（13）, b = 11.481 （2）, c = 12.564（3）A,β = 95.25（3）°, V = 965.4（3） A^3, Mr = 261.18, Z = 4, Dc = 1.797 g/cm^3,/t = 0.164 mm^-1, F（000） = 536, R = 0.0396 and wR = 0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.展开更多
A novel ternary borate, sodium strontium pentaborate, NaSrB5O9, has been prepared by solid-state reaction below 800 ℃. The single-crystal X-ray structural analysis showed that NaSrB5O9 crystallizes in monoclinic, spa...A novel ternary borate, sodium strontium pentaborate, NaSrB5O9, has been prepared by solid-state reaction below 800 ℃. The single-crystal X-ray structural analysis showed that NaSrB5O9 crystallizes in monoclinic, space group P21/c with a = 6.499（2）, b = 13.979（3）, c = 8.045（2）A, β = 106.92（2）°, V = 699.2（3）A^3, Z = 4, Mr = 308.66, Dc = 2.932 g/cm^3, μ = 7.804 mm^-1, F（000） = 584, R = 0.0264 and wR = 0.0621 for 2426 observed reflections and 146 variables. NaSrB5O9 is a layered compound containing double ring B5O11 building units composed of two BO4 tetrahedra and three BO3 triangles. Each B5O11 unit is connected to four other equivalent units through exocyclic oxygen atoms to form a two-dimensional ∞^2 [B5O9]^3- layer. Symmetry-center related layers are stacked along the b axis and held together by Na^＋ and Sr^2＋ cations via electrostatic interactions.展开更多
Two new nonmetal borates, [（C2H10N2）]2[B14O20（OH）6] 1 and [C8H22N4][B5O6（OH）4]2 2, have been synthesized under mild conditions and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis and ...Two new nonmetal borates, [（C2H10N2）]2[B14O20（OH）6] 1 and [C8H22N4][B5O6（OH）4]2 2, have been synthesized under mild conditions and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis and thermogravimetric analysis. Crystal data for compound 1： triclinic, space group P^-1, a = 8.4979（17）, b = 8.8498（18）, c = 10.065（2）A^°, α = 95.01（3）, β = 96.99（3）, γ = 116.82（3）°, V= 661.8（3）A^°^3, Z= 1, Mr = 697.63, Dc = 1.751 g/cm^3,μ = 0.163 mm^-1, F（000） = 356, the final R = 0.0372 and wR = 0.0968 （I 〉 2σ（I））; and those for compound 2： monoclinic, space group P21/c, a = 9.1867（18）, b= 14.118（3）, c = 10.334（2）A^°, β = 91.48（3）°, V = 1339.8（5）A^°^3, Z = 2, Mr = 610.46, Dc = 1.513 g/cm^3,μ = 0.135 mm^-1, F（000） = 632, the final R = 0.0350 and wR = 0.0912 （I 〉 2σ（I））. For both 1 and 2, the anionic units are interlinked via O-H…O hydrogen bonds to form a 3D supramolecular network, while the protonated cations are located in the free space of the inorganic borate framework and interact with the anions by electrostatic attraction and extensive N-H…O hydrogen bonds.展开更多
Solvothermal reaction of Pb（NO3）2·6H2O with rigid linear ligand terephthalic acid（H2pta） in N,N-dimethylformamide（DMF） produced a new three-dimensional（3D） lead（Ⅱ）coordination polymer[Pb2（pta）1.5（μ...Solvothermal reaction of Pb（NO3）2·6H2O with rigid linear ligand terephthalic acid（H2pta） in N,N-dimethylformamide（DMF） produced a new three-dimensional（3D） lead（Ⅱ）coordination polymer[Pb2（pta）1.5（μ4-OH）（DMF）]n 1,and its structure was characterized by single-crystal X-ray diffraction analyses.In polymer 1,the μ4-OH bridges the nearby lead（Ⅱ） ions into an infinite one-dimensional（1D） chain,and then the organic ligand pta^2- joins the neighbored chains into a 3D structure by two similar connection modes in different configurations.The solid-state photoluminescent studies revealed that 1 exhibits a strong greenish emission mainly originating from ligand-to-metal charge transfer between the delocalized π bonds of the aromatic carboxylate ligand pta^2- and the p orbitals of the Pb^2＋ centers.展开更多
A novel imide nickel complex [Ni（CH3CONCOCH3）2·2（H2O）] was synthesized by the solvothermal reaction of nickel acetate tetrahydrate and acetonitrile.What amazed us is that acetonitrile had changed into acetyl ...A novel imide nickel complex [Ni（CH3CONCOCH3）2·2（H2O）] was synthesized by the solvothermal reaction of nickel acetate tetrahydrate and acetonitrile.What amazed us is that acetonitrile had changed into acetyl imide in enol form during the formation process of the title complex.The complex was characterized by elemental analysis,IR spectrum and X-ray single-crystal diffraction analysis.It crystallizes in the orthorhombic system,space group Pbca with a = 7.4503（7）,b = 13.1089（12）,c = 14.1303（14）,V = 1380.0（2）3,Dc = 1.420 g/cm3,Mr = 294.94,Z = 4,F（000） = 616,μ = 1.422 mm-1,the final R = 0.0487 and wR = 0.1482.The four-coordinated nickel（II） center is surrounded by 4O atoms from two imide ligands and has a distorted square planar geometry.The complex is connected to form a supramolecule with an infinite three-dimensional network through intramolecular and intermolecular hydrogen bonds.Antimicrobial activity was investigated by agar diffusion method,and the result showed that the complex was active against coli bacillus,staphylococcus aureus and bacillus subtilis.The thermal stability of the title complex was also studied by TG-DTA method.展开更多
An inorganic-organic hybrid lanthanide selenidostannate [{Tb（en）3}2（μ-OH）2]Sn2Se6（1） was synthesized by the solvothermal method.1 crystallizes in the monoclinic system,space group P21/n with a=10.120（2）,b=11....An inorganic-organic hybrid lanthanide selenidostannate [{Tb（en）3}2（μ-OH）2]Sn2Se6（1） was synthesized by the solvothermal method.1 crystallizes in the monoclinic system,space group P21/n with a=10.120（2）,b=11.781（3）,c=15.403（3）,β=99.534（5）°,V=1811.1（7）3,Mr=1423.62,Z=2,Dc=2.611 g/cm3,μ=11.281 mm-1,F（000）=1312,S=1.101,the final R= 0.0400 and wR=0.0853 for 3242 observed reflections with Ⅰ 〉2σ（Ⅰ）.1 consists of a [Sn2Se6]4-and a [{Tb（en）3}2（μ-OH）2]4＋ ions.The [Sn2Se6]4-anion is constructed by two SnSe4 tetrahedra sharing a common edge.The binuclear [{Tb（en）3}2（μ-OH）2]4＋ complex is composed of two [Tb（en）3]3＋ ions joined by two μ-OH bridging ligands.The Tb3＋ ion lies in an eight-coordinated bicapped trigonal prism.In 1,the [Sn2Se6]4-and [{Tb（en）3}2（μ-OH）2]4＋ moieties are connected into a 3-D network via N-H···Se and O-H···Se H-bonds.展开更多
One organic-decorated quanternaery [TM（1,2-dap）3]Hg Sb2Se5（1,2-dap = 1,2-dianinopropane, TM = Co（1）, Fe（2）） compound has been solvothermally synthesized. The compounds crystallize in triclinic space group P 1,...One organic-decorated quanternaery [TM（1,2-dap）3]Hg Sb2Se5（1,2-dap = 1,2-dianinopropane, TM = Co（1）, Fe（2）） compound has been solvothermally synthesized. The compounds crystallize in triclinic space group P 1, with a = 11.248（6）, b = 11.542（7）, c = 12.180（12） A, V =1268.7（16） A^3, Z = 2, F（000） = 1010 for 1 and a = 11.311（5）, b = 11.558（5）, c = 12.180（9） A, V =1276.5（12） A^3, Z = 2, F（000） = 1008 for 2. The crystal structure consists of one-dimensional anionics chains composed of Hg Se4 tetrahedra and SbSe3 trigonal pyramids sharing corners and[TM（dap）3]^2＋ cations. The [HgSb2Se＋5^2-]∞ anionic chains run along the [001] direction, and are surrounded by the [TM（dap）3]^2＋ cations. Meanwhile, 8-ring [Hg2Sb2Se4] and 6-ring [HgSb2Se2] are alternately found. The compounds were structurally characterized by elemental analysis,thermogravimetric analysis, infrared spectroscopy and UV-Vis diffuse reflectance spectroscopy.展开更多
A compound （NH3 CH2 CH2 NH3 ）HgSnS4 with a column structure was synthesized solvothermally and characterized by X-ray single-crystal diffraction. This compound crystallizes in the monoclinic space group C2/c with a ...A compound （NH3 CH2 CH2 NH3 ）HgSnS4 with a column structure was synthesized solvothermally and characterized by X-ray single-crystal diffraction. This compound crystallizes in the monoclinic space group C2/c with a = 1. 3863 （6） nm, b = 0. 6640 （ 3 ） nm, c = 2. 3198 （10） nm, β = 106. 168 （ 7 ）° and Z = 8. It consists of anionic columns of [ HgSnS4 ]^2- that are interrupted by cationic columns of [ EnH2 ]^2＋ . Its thermal and optical properties were studied.展开更多
The solvothermal reaction of H3dhpmc (H3dhpmc = 2, 4-dihydroxypyrimidine- 5-carboxylic acid), CuCl2稨2O and NaVO3 results in the formation of a discrete mononuclear Cu(Ⅱ) complex [Cu(H2dhpmc)2]?H2O. It crystallizes i...The solvothermal reaction of H3dhpmc (H3dhpmc = 2, 4-dihydroxypyrimidine- 5-carboxylic acid), CuCl2稨2O and NaVO3 results in the formation of a discrete mononuclear Cu(Ⅱ) complex [Cu(H2dhpmc)2]?H2O. It crystallizes in monoclinic system, space group P21/c with a = 5.0497(9), b = 10.0196(6), c = 13.715(2) ? b = 96.237(1)? V = 689.8(2) 3, Z = 2, Dc = 1.973 g/cm3, ?= 1.654 mm-1, F(000) = 414, R = 0.0736 and wR = 0.1351. Each Cu(Ⅱ) is coordinated to four oxygen atoms of two 2, 4-dihydroxypyrimidine-5-carboxylic acid ligands in the equatorial position and two oxygen atoms of two water molecules in the axial position to form an axially elongated octahedral geometry. The title complex is further linked into a three-dimensional structure through the weak interactions of hydrogen bonds between the oxygen atoms and the nitrogen atoms.展开更多
A magnesium metal organic framework, [N-H2（CH3）2][-N（CH3）4][Mgs（bpdc）3（O2CH）6]· 3H2O （1, bpdcH2 = 4,4＇-biphenyldicarboxylic acid）, has been solvothermally synthesized and structurally characterized. 1 ...A magnesium metal organic framework, [N-H2（CH3）2][-N（CH3）4][Mgs（bpdc）3（O2CH）6]· 3H2O （1, bpdcH2 = 4,4＇-biphenyldicarboxylic acid）, has been solvothermally synthesized and structurally characterized. 1 crystallizes in the trigonal system, space group R-3, with a = 11.3427（3）, c = 41.5662（18） A, V = 4631.3（3） A^3, Z = 3 and the final R = 0.0457. Its structure features a pillared-layered three-dimensional network with 8.21 A cavities, in which cationic [NH2（CH3）2]^＋ or [N（CH3）4]^＋ and lattice water molecules are located. Thermal stability of the title compound has also been investigated.展开更多
A novel inorganic organic hybrid material, Fe 2O(OH)(C 5H 4 ~NCOO)SO 4 was synthesized via solvothermal route using a reaction of FeCl 3·6H 2O, KCNS, and 4 cyanopyridine in aqueous solution of H 2O 2...A novel inorganic organic hybrid material, Fe 2O(OH)(C 5H 4 ~NCOO)SO 4 was synthesized via solvothermal route using a reaction of FeCl 3·6H 2O, KCNS, and 4 cyanopyridine in aqueous solution of H 2O 2 and ethanol at 130 ℃ for 3 d. The compound crystallized in monoclinic space group P 2 1, with cell parameters a =0 73850(15) nm, b =0 65100(13) nm, c =1 0546(2) nm, β =90 36(3)°, V =0 50700(18) nm 3 and Z =2. The structure is constructed with inorganic layered [Fe 2O(OH)SO 4] + cations linked by organic (C 5H 4NCOO) - anions. The compound is thermally stable up to approximately 240 ℃.展开更多
A Fe-based metal-organic framework, [Fe(INAIP)(DMF)]_(n)·0.5nDMF(1), has been synthesized by the reaction of 5-(isonicotinamido)isophthalic acid(H_(2)INAIP) with FeSO_(4)·7H_(2)O under DMF reaction solvent. ...A Fe-based metal-organic framework, [Fe(INAIP)(DMF)]_(n)·0.5nDMF(1), has been synthesized by the reaction of 5-(isonicotinamido)isophthalic acid(H_(2)INAIP) with FeSO_(4)·7H_(2)O under DMF reaction solvent. Single-crystal X-ray diffraction analysis indicates that complex 1 displays a two-fold interpenetrated three-dimensional(3D) framework with sra topology. The TG, magnetic and adsorption properties of the complex were also studied.展开更多
The title compound (H3NCH2CH2NH3)4[(VO)6(B10O22)2]·(H3O)7 1 has been synthe- sized by the hydrothermal method and determined by X-ray crystallography. Crystallographic data: monoclinic, space group C2/c, a = 20.2...The title compound (H3NCH2CH2NH3)4[(VO)6(B10O22)2]·(H3O)7 1 has been synthe- sized by the hydrothermal method and determined by X-ray crystallography. Crystallographic data: monoclinic, space group C2/c, a = 20.250(4), b = 13.448(3), c = 21.655(4) ?, β = 97.05(3)°, Mr = 851.74 (C4H30.5B10N4O28.5V3), V = 5852(2) ?3, Z = 8, Dc = 1.933 g/cm3, μ = 1.057 mm-1, F(000) = 3436, R = 0.0500 and wR = 0.1442 for 4511 observed reflections with I > 2σ(I). The structure con- sists of [(VO)6(B10O22)2]15- cluster anions that have a central band of six trans-edge-sharing VO5 square pyramids capped by two [B10O22]14- polyborate ligands. Other characterizations are also describ- ed by elemental analysis, IR spectrum and thermal analysis.展开更多
New hydrated potassium hexaborate K2[B6O9（OH）2] has been synthesized under mild solvothermal conditions. The structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR, Rarnan sp...New hydrated potassium hexaborate K2[B6O9（OH）2] has been synthesized under mild solvothermal conditions. The structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR, Rarnan spectra and DTA-TG. It crystallizes in the monoclinic system with space group P21/n, a=0.9036（2） nm, b=0.66052（18） nm, c=1.5997（4） nm, β=91.862（4）°, V=0.9543（4） nm^3 and Z=4. Its crystal structure consists of K-O polyhedra and 1-D stepped polyborate chains constructed by new [B6O9（OH）2]2- fundamental building blocks. 1-D polyborate chains contain 3,8-membered boron rings. Adjacent chains are further linked via H-bonding interactions into 2-D layers. The K^＋ cations reside not only between the layers but also in the 8-membered boron rings of the chains, compensating the negative charges of the borate chains and holding the layers together into the 3-D structure through bonding with oxygen atoms of the chains.展开更多
A new hydrated lithium borate, Li4[B8O13（OH）2]·3H2O, has been hydrothermally synthesized and characterized by single crystal X-ray diffraction, FT-IR spectroscopy, simultaneous TGA-DTA and chemical analysis. It...A new hydrated lithium borate, Li4[B8O13（OH）2]·3H2O, has been hydrothermally synthesized and characterized by single crystal X-ray diffraction, FT-IR spectroscopy, simultaneous TGA-DTA and chemical analysis. It crystal- lizes in the triclinic, space group P]-, a=8.4578（5） A, b=8.7877（5） A, c= 10.8058（7） A, a=87.740（3）°, β= 71.819（3）°, γ=61.569（3）°, Z=2, V=665.26（7） A3, Dc=2.043 g/cm3. Its crystal structure features polyborate ani- onic layers with the larger odd 13-membered boron rings constructed by [B8O13（OH）2]4- FBBs. Through designing the thermochemical cycle, the standard molar enthalpy of formation of this borate was determined to be -（7953.8 ± 6.6） kJ·mol-1 by using a heat conduction microcalorimeter.展开更多
A new coordination polymer with sulfide moieties, [Co(ptmb)2]·0.25H2O (ptmb=4-(4-pyridylthiomethyl)-benzoate), was synthesized by self-assembly of Co(NO3)2·6H2O with Hptmb under solvothermal conditions. X-ra...A new coordination polymer with sulfide moieties, [Co(ptmb)2]·0.25H2O (ptmb=4-(4-pyridylthiomethyl)-benzoate), was synthesized by self-assembly of Co(NO3)2·6H2O with Hptmb under solvothermal conditions. X-ray single crystal diffraction study shows that it is a 2D layer structure consisting of puckered rhombus grid with di-mensions 1.175 nm×1.110 nm.展开更多
A new Nd（Ⅲ） coordination polymer [Nd（pidc）（H2O）4]·pidc-·7H2O（1,pidc2-= 2-py-ridyl-4,5-imidazoledicarboxylate） has been synthesized by solvothermal reaction at 120 ℃ and structurally characterized.T...A new Nd（Ⅲ） coordination polymer [Nd（pidc）（H2O）4]·pidc-·7H2O（1,pidc2-= 2-py-ridyl-4,5-imidazoledicarboxylate） has been synthesized by solvothermal reaction at 120 ℃ and structurally characterized.The complex belongs to triclinic,space group P with a = 9.022（2）,b = 13.731（3）,c = 13.782（3） ,α = 70.87（3）,β = 71.71（3）,γ = 71.71（3）,V = 1488.6（7） 3,Z = 2,Dc = 1.798 g/cm3,S = 1.04,μ = 1.839 mm-1,F（000） = 814,Mr = 805.76,Rint = 0.081 and wR = 0.1644 for 5242 observed reflections（I 〉 2（I））.Each Nd3＋ ion is nine-coordinated by five O atoms from three pidc ligands,and four O atoms from lattice water molecules.Each pidc is coordinated to three Nd3＋ ions with a μ3-κO：κO＇：κO＂,κO＇＂-μ2 coordination mode into 1D chains,which can be further built into a 3D framework through intermolecular N-H···O and O-H···O hydrogen bonds.Photolu-minescent studies have shown that 1 exhibits emission at 439 nm（λex = 395 nm）.展开更多
基金the Natural Science Foundation of Universities of Jiangsu Province (No. 05KJB150110)
文摘An inorganic-organic hybrid thioantimonate（Ⅲ） [CH3（CH2）3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system, space group P1 with a = 7.0124（11）, b = 11.919（2）, c =14.879（3）A, α = 108.791（3）, β= 102.441（3）, γ = 92.846（2）°, V= 1140.1（3）A3, Mr = 859.71, Z= 2, Do = 2.504 g/cm^3 ,μ = 5.324 mm^-1, F（000） = 804, S = 1.013, the Final R = 0.0297 and wR = 0.0618 for 3534 observed reflections with Ⅰ 〉 2 σ（Ⅰ）. 1 consists of [C4HgNH3]＋ cations and two-dimensional [Sb4ST]n^2n- anion which is composed of three SbS3 trigonal pyranaids and one SbS4 unit joined by sharing common comers. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]^＋ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.
文摘A new polyborate containing ehiral metal-complex Zn（en）3 B5O7（OH）3, where en = ethylenediamine, was synthesizedunder solvothermal conditions and structurally characterized by means of X-ray diffraction analysis. Crystal data： Zn（en）3 B5O7（OH）3, monoclinic, space group P21/c, a =0.8532（72） nm, b =2.3340（5） nm, c = 0.9526（92） nm, β =107. 04（3）°, Z=4, V=1.8140（6） nm^3, Dc =1.694 g/cm^3, p=1.416 mm^-1, F（000） = 960, GOF = 1. 020, R =0. 0276, Rw =0. 0828. There is a chiral Zn（en）3^2＋ complex cation and an isolated B5O7（OH）3^2- group in a Zn（en）3 B5O7（OH）3 molecule. The enantiomer of the chiral complex cation is separated orderly as ,4 and A configurations in the compound and the borate group consists of two B303 cycles linked through a bridging boron atom.
基金Supported by the Natural Science Foundation of Universities of Jiangsu Province (05KJB150110)
文摘A new selenidoarsenate [Co（en）3]2As2Se5 1 （en = ethylenediamine） was synthesized by a reaction of AsCI3, CoCl2-6H2O and Se in en under mild solvothermal conditions, and the structure was determined by single-crystal X-ray diffraction. 1 crystallizes in the orthorhombic system, space group Pbca with a = 15.5092（12）, b = 11.5756（9）, c = 17.8138（14） A, V = 3198.1（4） A^3, Mr= 1023.12, Z = 4, D, = 2.125 g/cm^3,μ = 8.807 mm^-1, F（000） = 1976, S = 1.171, the final R = 0.0591 and wR = 0.1067 for 3170 observed reflections with 1 〉 2σ（I）. 1 consists of isolated dimeric [As2Se5]^4- anion constructed by two corner-sharing AsSe3 trigonal pyramids and transition metal [Co（en）3]^2＋ cations. The optical absorption property and thermal stability of 1 are reported.
基金the Natural Science Foundation of Henan Province (0611021600, 0311050500)the Key Discipline Foundation of Zhoukou Normal University
文摘Two new borate compounds, C4H10N2·B6O8（OH）2 and （NH3CH2CH2NH3）B5O8 （OH）2, have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction, IR, elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system, space group P21/c, with a = 8.3318（17）, b = 6.2118（12）, c = 12.479（3） A, β = 108.96（3）°, V = 610.8（2） A^3, Mr = 313.02, Z = 2, 13,.= 1.702 g/cm^,/J = 0.150 mm^-1, F（000） = 320, R = 0.0387 and wR = 0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system, which are built up from alternative B6O8（OH）2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic, space group Co, with a = 6.7207（13）, b = 11.481 （2）, c = 12.564（3）A,β = 95.25（3）°, V = 965.4（3） A^3, Mr = 261.18, Z = 4, Dc = 1.797 g/cm^3,/t = 0.164 mm^-1, F（000） = 536, R = 0.0396 and wR = 0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.
基金Supported by the Talent Training Funds of Beijing (20051D0501501)the Funding Project for Academic Human Resources Development in Institutions of Higher Learning under the Jurisdiction of Beijing Municipality, and the Natural Science Foundation of Beijing (No. 2073021)
文摘A novel ternary borate, sodium strontium pentaborate, NaSrB5O9, has been prepared by solid-state reaction below 800 ℃. The single-crystal X-ray structural analysis showed that NaSrB5O9 crystallizes in monoclinic, space group P21/c with a = 6.499（2）, b = 13.979（3）, c = 8.045（2）A, β = 106.92（2）°, V = 699.2（3）A^3, Z = 4, Mr = 308.66, Dc = 2.932 g/cm^3, μ = 7.804 mm^-1, F（000） = 584, R = 0.0264 and wR = 0.0621 for 2426 observed reflections and 146 variables. NaSrB5O9 is a layered compound containing double ring B5O11 building units composed of two BO4 tetrahedra and three BO3 triangles. Each B5O11 unit is connected to four other equivalent units through exocyclic oxygen atoms to form a two-dimensional ∞^2 [B5O9]^3- layer. Symmetry-center related layers are stacked along the b axis and held together by Na^＋ and Sr^2＋ cations via electrostatic interactions.
基金supported by the Natural Science Foundation of Ningbo City (2007A610022) K. C. Wong Magna Fund in Ningbo University
文摘Two new nonmetal borates, [（C2H10N2）]2[B14O20（OH）6] 1 and [C8H22N4][B5O6（OH）4]2 2, have been synthesized under mild conditions and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis and thermogravimetric analysis. Crystal data for compound 1： triclinic, space group P^-1, a = 8.4979（17）, b = 8.8498（18）, c = 10.065（2）A^°, α = 95.01（3）, β = 96.99（3）, γ = 116.82（3）°, V= 661.8（3）A^°^3, Z= 1, Mr = 697.63, Dc = 1.751 g/cm^3,μ = 0.163 mm^-1, F（000） = 356, the final R = 0.0372 and wR = 0.0968 （I 〉 2σ（I））; and those for compound 2： monoclinic, space group P21/c, a = 9.1867（18）, b= 14.118（3）, c = 10.334（2）A^°, β = 91.48（3）°, V = 1339.8（5）A^°^3, Z = 2, Mr = 610.46, Dc = 1.513 g/cm^3,μ = 0.135 mm^-1, F（000） = 632, the final R = 0.0350 and wR = 0.0912 （I 〉 2σ（I））. For both 1 and 2, the anionic units are interlinked via O-H…O hydrogen bonds to form a 3D supramolecular network, while the protonated cations are located in the free space of the inorganic borate framework and interact with the anions by electrostatic attraction and extensive N-H…O hydrogen bonds.
基金supported by the Natural Science Foundation of Fujian province(2015J01033)Industry-University Cooperation Key Project of Science and Technology of Fujian Province(2012H6002)
文摘Solvothermal reaction of Pb（NO3）2·6H2O with rigid linear ligand terephthalic acid（H2pta） in N,N-dimethylformamide（DMF） produced a new three-dimensional（3D） lead（Ⅱ）coordination polymer[Pb2（pta）1.5（μ4-OH）（DMF）]n 1,and its structure was characterized by single-crystal X-ray diffraction analyses.In polymer 1,the μ4-OH bridges the nearby lead（Ⅱ） ions into an infinite one-dimensional（1D） chain,and then the organic ligand pta^2- joins the neighbored chains into a 3D structure by two similar connection modes in different configurations.The solid-state photoluminescent studies revealed that 1 exhibits a strong greenish emission mainly originating from ligand-to-metal charge transfer between the delocalized π bonds of the aromatic carboxylate ligand pta^2- and the p orbitals of the Pb^2＋ centers.
基金supported by the Natural Science Foundation of Jiangsu Province (No. BK2005045) and Key Marine Biotechnology Lab.of HHIT
文摘A novel imide nickel complex [Ni（CH3CONCOCH3）2·2（H2O）] was synthesized by the solvothermal reaction of nickel acetate tetrahydrate and acetonitrile.What amazed us is that acetonitrile had changed into acetyl imide in enol form during the formation process of the title complex.The complex was characterized by elemental analysis,IR spectrum and X-ray single-crystal diffraction analysis.It crystallizes in the orthorhombic system,space group Pbca with a = 7.4503（7）,b = 13.1089（12）,c = 14.1303（14）,V = 1380.0（2）3,Dc = 1.420 g/cm3,Mr = 294.94,Z = 4,F（000） = 616,μ = 1.422 mm-1,the final R = 0.0487 and wR = 0.1482.The four-coordinated nickel（II） center is surrounded by 4O atoms from two imide ligands and has a distorted square planar geometry.The complex is connected to form a supramolecule with an infinite three-dimensional network through intramolecular and intermolecular hydrogen bonds.Antimicrobial activity was investigated by agar diffusion method,and the result showed that the complex was active against coli bacillus,staphylococcus aureus and bacillus subtilis.The thermal stability of the title complex was also studied by TG-DTA method.
基金Supported by the National Natural Science Foundation of China (No. 20771077)
文摘An inorganic-organic hybrid lanthanide selenidostannate [{Tb（en）3}2（μ-OH）2]Sn2Se6（1） was synthesized by the solvothermal method.1 crystallizes in the monoclinic system,space group P21/n with a=10.120（2）,b=11.781（3）,c=15.403（3）,β=99.534（5）°,V=1811.1（7）3,Mr=1423.62,Z=2,Dc=2.611 g/cm3,μ=11.281 mm-1,F（000）=1312,S=1.101,the final R= 0.0400 and wR=0.0853 for 3242 observed reflections with Ⅰ 〉2σ（Ⅰ）.1 consists of a [Sn2Se6]4-and a [{Tb（en）3}2（μ-OH）2]4＋ ions.The [Sn2Se6]4-anion is constructed by two SnSe4 tetrahedra sharing a common edge.The binuclear [{Tb（en）3}2（μ-OH）2]4＋ complex is composed of two [Tb（en）3]3＋ ions joined by two μ-OH bridging ligands.The Tb3＋ ion lies in an eight-coordinated bicapped trigonal prism.In 1,the [Sn2Se6]4-and [{Tb（en）3}2（μ-OH）2]4＋ moieties are connected into a 3-D network via N-H···Se and O-H···Se H-bonds.
基金supported by the National Natural Science Foundation of China(No.21461019)
文摘One organic-decorated quanternaery [TM（1,2-dap）3]Hg Sb2Se5（1,2-dap = 1,2-dianinopropane, TM = Co（1）, Fe（2）） compound has been solvothermally synthesized. The compounds crystallize in triclinic space group P 1, with a = 11.248（6）, b = 11.542（7）, c = 12.180（12） A, V =1268.7（16） A^3, Z = 2, F（000） = 1010 for 1 and a = 11.311（5）, b = 11.558（5）, c = 12.180（9） A, V =1276.5（12） A^3, Z = 2, F（000） = 1008 for 2. The crystal structure consists of one-dimensional anionics chains composed of Hg Se4 tetrahedra and SbSe3 trigonal pyramids sharing corners and[TM（dap）3]^2＋ cations. The [HgSb2Se＋5^2-]∞ anionic chains run along the [001] direction, and are surrounded by the [TM（dap）3]^2＋ cations. Meanwhile, 8-ring [Hg2Sb2Se4] and 6-ring [HgSb2Se2] are alternately found. The compounds were structurally characterized by elemental analysis,thermogravimetric analysis, infrared spectroscopy and UV-Vis diffuse reflectance spectroscopy.
基金Supported by the National Natural Science Foundation of China(No. 20071006)
文摘A compound （NH3 CH2 CH2 NH3 ）HgSnS4 with a column structure was synthesized solvothermally and characterized by X-ray single-crystal diffraction. This compound crystallizes in the monoclinic space group C2/c with a = 1. 3863 （6） nm, b = 0. 6640 （ 3 ） nm, c = 2. 3198 （10） nm, β = 106. 168 （ 7 ）° and Z = 8. It consists of anionic columns of [ HgSnS4 ]^2- that are interrupted by cationic columns of [ EnH2 ]^2＋ . Its thermal and optical properties were studied.
基金This work was supported by the National Natural Science Foundation of China
文摘The solvothermal reaction of H3dhpmc (H3dhpmc = 2, 4-dihydroxypyrimidine- 5-carboxylic acid), CuCl2稨2O and NaVO3 results in the formation of a discrete mononuclear Cu(Ⅱ) complex [Cu(H2dhpmc)2]?H2O. It crystallizes in monoclinic system, space group P21/c with a = 5.0497(9), b = 10.0196(6), c = 13.715(2) ? b = 96.237(1)? V = 689.8(2) 3, Z = 2, Dc = 1.973 g/cm3, ?= 1.654 mm-1, F(000) = 414, R = 0.0736 and wR = 0.1351. Each Cu(Ⅱ) is coordinated to four oxygen atoms of two 2, 4-dihydroxypyrimidine-5-carboxylic acid ligands in the equatorial position and two oxygen atoms of two water molecules in the axial position to form an axially elongated octahedral geometry. The title complex is further linked into a three-dimensional structure through the weak interactions of hydrogen bonds between the oxygen atoms and the nitrogen atoms.
基金supported by the NNSFC (No. 20873149)the Knowledge Innovation Program of the Chinese Academy of Sciences (KJCX2-XW-H21)
文摘A magnesium metal organic framework, [N-H2（CH3）2][-N（CH3）4][Mgs（bpdc）3（O2CH）6]· 3H2O （1, bpdcH2 = 4,4＇-biphenyldicarboxylic acid）, has been solvothermally synthesized and structurally characterized. 1 crystallizes in the trigonal system, space group R-3, with a = 11.3427（3）, c = 41.5662（18） A, V = 4631.3（3） A^3, Z = 3 and the final R = 0.0457. Its structure features a pillared-layered three-dimensional network with 8.21 A cavities, in which cationic [NH2（CH3）2]^＋ or [N（CH3）4]^＋ and lattice water molecules are located. Thermal stability of the title compound has also been investigated.
文摘A novel inorganic organic hybrid material, Fe 2O(OH)(C 5H 4 ~NCOO)SO 4 was synthesized via solvothermal route using a reaction of FeCl 3·6H 2O, KCNS, and 4 cyanopyridine in aqueous solution of H 2O 2 and ethanol at 130 ℃ for 3 d. The compound crystallized in monoclinic space group P 2 1, with cell parameters a =0 73850(15) nm, b =0 65100(13) nm, c =1 0546(2) nm, β =90 36(3)°, V =0 50700(18) nm 3 and Z =2. The structure is constructed with inorganic layered [Fe 2O(OH)SO 4] + cations linked by organic (C 5H 4NCOO) - anions. The compound is thermally stable up to approximately 240 ℃.
基金supported by the Natural Science Foundation of Hunan Province(2020JJ4148)the Scientific Research Fund of Hunan Provincial Education Department(18A328)+1 种基金the Foundation of Key Laboratory of Functional Organometallic Materials,University of Hunan Province(GN19K03)the Center for the Functionalization of Metal-organic Frameworks Materials Studies(KYJG1802)。
文摘A Fe-based metal-organic framework, [Fe(INAIP)(DMF)]_(n)·0.5nDMF(1), has been synthesized by the reaction of 5-(isonicotinamido)isophthalic acid(H_(2)INAIP) with FeSO_(4)·7H_(2)O under DMF reaction solvent. Single-crystal X-ray diffraction analysis indicates that complex 1 displays a two-fold interpenetrated three-dimensional(3D) framework with sra topology. The TG, magnetic and adsorption properties of the complex were also studied.
基金This work was supported by the Natural Science Foundation of Fujian Province (E0110013 and K02028)
文摘The title compound (H3NCH2CH2NH3)4[(VO)6(B10O22)2]·(H3O)7 1 has been synthe- sized by the hydrothermal method and determined by X-ray crystallography. Crystallographic data: monoclinic, space group C2/c, a = 20.250(4), b = 13.448(3), c = 21.655(4) ?, β = 97.05(3)°, Mr = 851.74 (C4H30.5B10N4O28.5V3), V = 5852(2) ?3, Z = 8, Dc = 1.933 g/cm3, μ = 1.057 mm-1, F(000) = 3436, R = 0.0500 and wR = 0.1442 for 4511 observed reflections with I > 2σ(I). The structure con- sists of [(VO)6(B10O22)2]15- cluster anions that have a central band of six trans-edge-sharing VO5 square pyramids capped by two [B10O22]14- polyborate ligands. Other characterizations are also describ- ed by elemental analysis, IR spectrum and thermal analysis.
文摘New hydrated potassium hexaborate K2[B6O9（OH）2] has been synthesized under mild solvothermal conditions. The structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR, Rarnan spectra and DTA-TG. It crystallizes in the monoclinic system with space group P21/n, a=0.9036（2） nm, b=0.66052（18） nm, c=1.5997（4） nm, β=91.862（4）°, V=0.9543（4） nm^3 and Z=4. Its crystal structure consists of K-O polyhedra and 1-D stepped polyborate chains constructed by new [B6O9（OH）2]2- fundamental building blocks. 1-D polyborate chains contain 3,8-membered boron rings. Adjacent chains are further linked via H-bonding interactions into 2-D layers. The K^＋ cations reside not only between the layers but also in the 8-membered boron rings of the chains, compensating the negative charges of the borate chains and holding the layers together into the 3-D structure through bonding with oxygen atoms of the chains.
文摘A new hydrated lithium borate, Li4[B8O13（OH）2]·3H2O, has been hydrothermally synthesized and characterized by single crystal X-ray diffraction, FT-IR spectroscopy, simultaneous TGA-DTA and chemical analysis. It crystal- lizes in the triclinic, space group P]-, a=8.4578（5） A, b=8.7877（5） A, c= 10.8058（7） A, a=87.740（3）°, β= 71.819（3）°, γ=61.569（3）°, Z=2, V=665.26（7） A3, Dc=2.043 g/cm3. Its crystal structure features polyborate ani- onic layers with the larger odd 13-membered boron rings constructed by [B8O13（OH）2]4- FBBs. Through designing the thermochemical cycle, the standard molar enthalpy of formation of this borate was determined to be -（7953.8 ± 6.6） kJ·mol-1 by using a heat conduction microcalorimeter.
基金the National Natural Science Foundation of China (No. 20231020), the Natural Science Foundation of Fujian Province and Chinese Academy of Sciences.
文摘A new coordination polymer with sulfide moieties, [Co(ptmb)2]·0.25H2O (ptmb=4-(4-pyridylthiomethyl)-benzoate), was synthesized by self-assembly of Co(NO3)2·6H2O with Hptmb under solvothermal conditions. X-ray single crystal diffraction study shows that it is a 2D layer structure consisting of puckered rhombus grid with di-mensions 1.175 nm×1.110 nm.
基金Funded by the National Natural Science Foundation of China (No.21101035)Natural Science Foundation of Guangxi Province (2010GXNSFF013001)+1 种基金State Key Laboratory of Cultivation Base for the Chemistry and Molecular Engineering of Medicinal Resources,Ministry of Science and Technology of China (CMEMR2011-23)the Natural Science Foundation of the Education Committee of Guangxi Province (No.201010LX074)
文摘A new Nd（Ⅲ） coordination polymer [Nd（pidc）（H2O）4]·pidc-·7H2O（1,pidc2-= 2-py-ridyl-4,5-imidazoledicarboxylate） has been synthesized by solvothermal reaction at 120 ℃ and structurally characterized.The complex belongs to triclinic,space group P with a = 9.022（2）,b = 13.731（3）,c = 13.782（3） ,α = 70.87（3）,β = 71.71（3）,γ = 71.71（3）,V = 1488.6（7） 3,Z = 2,Dc = 1.798 g/cm3,S = 1.04,μ = 1.839 mm-1,F（000） = 814,Mr = 805.76,Rint = 0.081 and wR = 0.1644 for 5242 observed reflections（I 〉 2（I））.Each Nd3＋ ion is nine-coordinated by five O atoms from three pidc ligands,and four O atoms from lattice water molecules.Each pidc is coordinated to three Nd3＋ ions with a μ3-κO：κO＇：κO＂,κO＇＂-μ2 coordination mode into 1D chains,which can be further built into a 3D framework through intermolecular N-H···O and O-H···O hydrogen bonds.Photolu-minescent studies have shown that 1 exhibits emission at 439 nm（λex = 395 nm）.
