N-Octadecyl-N1-maleoyl-L-phenylalanine (ODMA-L-Phe) was synthesized through the condensation, deprotection and acid- ylation reaction of BOC-L-phenylalanine, octadecylamine and maleic anhydride. ODMA-L-Phe can self-...N-Octadecyl-N1-maleoyl-L-phenylalanine (ODMA-L-Phe) was synthesized through the condensation, deprotection and acid- ylation reaction of BOC-L-phenylalanine, octadecylamine and maleic anhydride. ODMA-L-Phe can self-assemble in some organic solvents and turned them into thermally reversible physical supramolecular organogels. The morphology of ODMA-L-Phe aggregates was characterized by polarized optical microscopy (POM) and field emission scanning electron microscope (FE-SEM). The aggregates of ODMA-L-Phe were needle-like fibrils with diameters of approximately 100-200 nm. The mechanism of ODMA- L-Phe self-assembly in organic solvents was investigated using XH NMR and circular dichroism (CD). The results indicated that hydrogen bonding was one of the main driving forces for the self-assembly of ODMA-L-Phe.展开更多
The hydrothermal reactions of CuI, KI and bidentate amines [ 1,10 phenanthroline (phen) or ethylenediamine (en)] gave the three copper(I) halide compounds, Cu3I3(phen)2 (1), CuI(phen)2 (2) and 2 (3), which were stru...The hydrothermal reactions of CuI, KI and bidentate amines [ 1,10 phenanthroline (phen) or ethylenediamine (en)] gave the three copper(I) halide compounds, Cu3I3(phen)2 (1), CuI(phen)2 (2) and 2 (3), which were structurally characterized via singlecrystal Xray diffraction studies. Hydrogen bonds and ππ interactions are the most remarkable structural features of the title compounds. All can be described as higherdimensional supramolecular compounds connected via these secondary bondings. Moreover, the title compounds were characterized by elemental analyses, IR spectra and TGA analyses. The thirdorder nonlinear optical properties of the title compounds were also investigated and all exhibit nicer nonlinear absorption and selffocusing performance.Keywords copper(I) halide, hydrothermal synthesis, the thirdorder nonlinear optical property, supramolecular structure展开更多
Making use of N-P-acetamidobenzenesulfonyl-glycine acid (abbreviated as abglyH2),two transitional metal complexes [Zn(abglyH)(phen)2]ClO4·H2O (1) and Co(abglyH)2(bipy)2(H2O)2 (2) (phen = 1,10-phe...Making use of N-P-acetamidobenzenesulfonyl-glycine acid (abbreviated as abglyH2),two transitional metal complexes [Zn(abglyH)(phen)2]ClO4·H2O (1) and Co(abglyH)2(bipy)2(H2O)2 (2) (phen = 1,10-phenanthroline,bipy = 4,4'-bipyridine) have been synthesized under mild conditions and characterized by IR,elemental analysis and X-ray diffraction analysis. Complex 1 is a monomeric compound which is further assembled by intermolecular hydrogen bonds and π-π interaction into a 2-D supramolecular network. Complex 2 is also a monomeric compound and further connected by intermolecular hydrogen bonds to form a 2-D supramolecular network. Fluorescent analysis shows that complex 1 has an emissive maximum at 364 nm in the solution state at room temperature.展开更多
A new complex [Pb(phen)2(4-NBA)]2·2(NO3)·H2O(phen = 1,10-phenanthroline,4-NBA = 4-nitrobenzoate) has been hydrothermally synthesized and structurally determined by single-crystal X-ray diffraction,el...A new complex [Pb(phen)2(4-NBA)]2·2(NO3)·H2O(phen = 1,10-phenanthroline,4-NBA = 4-nitrobenzoate) has been hydrothermally synthesized and structurally determined by single-crystal X-ray diffraction,elemental analyses and IR spectroscopy.The complex crystallizes in monoclinic,space group P21/c with a = 13.416(3),b = 14.065(3),c = 16.845(3)(A°) ,β = 110.55(3)o,V = 2976.5(10)(A°)^3,Z = 2,Dc = 1.796 g/cm^3,F(000) = 1564,GOOF = 0.962,the final R = 0.0686 and wR = 0.1746.The crystal structure shows that the lead ion is coordinated with two carboxylate O atoms from the 4-NBA anion,and four N atoms from two phen molecules,forming a slightly distorted pentagonalbipyramidal coordination geometry.It is further extended by various supramo-lecular interactions to form a three-dimensional supramolecular network.The TG analysis result shows that this complex begins decomposing at 30 ℃ and decompounding completely at 733 ℃.展开更多
Two homochiral enantiomorphic 3D coordination polymers: (D-HAPA)2[Cd2Cs(D- HAPA)(m-BDC)4]'(EtOH) (1D) and (L-HAPA)2[Cd2Cs(L-HAPA)(m-BDC)a]'(EtOH) (1L) (APA = 2-amino-l-propanol, m-H2BDC = 1,3-b...Two homochiral enantiomorphic 3D coordination polymers: (D-HAPA)2[Cd2Cs(D- HAPA)(m-BDC)4]'(EtOH) (1D) and (L-HAPA)2[Cd2Cs(L-HAPA)(m-BDC)a]'(EtOH) (1L) (APA = 2-amino-l-propanol, m-H2BDC = 1,3-benzenedicarboxylate), have been assembled solvothermally respectively with the induction of enantiomorphic organic small molecules (D,L-APA). 1L and 1I) crystallize in chiral space group P21 with Flack parameters of-0.012(13) and -0.07(3), respectively, and have been characterized by satisfactory elemental analysis, FT-IR spectra, CD-spectra and single-crystal X-ray diffraction. They both exhibit sqp topological net, purple fluorescence and SHG activity.展开更多
One-pot solvothermal reaction of transition metal Cd(II ) salt with (2E,2′E)-3,3′- ((propane-1,3-diylbis(oxy))bis(2,1-phenylene))diacrylic acid (H2ppa) and 1,10-phenanthroline (phen) generates a meso...One-pot solvothermal reaction of transition metal Cd(II ) salt with (2E,2′E)-3,3′- ((propane-1,3-diylbis(oxy))bis(2,1-phenylene))diacrylic acid (H2ppa) and 1,10-phenanthroline (phen) generates a meso-helicate, [Cd(ppa)(phen)(H2O)]2, and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent property. The complex crys- tallizes in monoclinic, space group P21/c with a = 13.4622(7), b = 24.8452(12), c = 8.9314(4) A, β = 97.564(1)°, V = 2961.3(2) A3, C66H56N4O14Cd2, Mr = 1353.97, Dc = 1.518 g/cm3, μ(MoKa) = 0.789 mm-1, F(000) = 1376, Z = 2, the final R = 0.0248 and wR = 0.0667 for 4673 observed reflections (I 〉 2σ(I)). The I-D supramolecular chain is built up from the complex by π-π stacking interactions, and inter-chain hydrogen bonds prompt the I-D chains into a 2-D layer. The title compound shows strong photoluminescence with emission maximum at 2 = 445 nm upon λEx, max = 240 nm.展开更多
A novel supramolecular structural inorganic-organic hybrid [(4-bromoanilimiun)([18]crown-6)]3[PMo(12)O40]·CH3 CN has been synthesized through standard solvent evaporated method. The structure of the title c...A novel supramolecular structural inorganic-organic hybrid [(4-bromoanilimiun)([18]crown-6)]3[PMo(12)O40]·CH3 CN has been synthesized through standard solvent evaporated method. The structure of the title compound was determined through single-crystal X-ray diffraction analysis. It crystallizes in monoclinic system with P21/n space group. The crystal data are a = 18.9529(4), b = 26.4444(5), c = 19.0985(4) A, β = 90.132(6)o, V = 9572.1(3) A^3, Z = 4, Dc= 2.203 g·cm^(–1), μ = 14.956 mm^(–1), F(000) = 6192, S = 1.098, the final R = 0.0859 and w R(I 〉 2σ(I)) = 0.2100. Supramolecular cations are constructed through strong N–H…O hydrogen bonding interaction between the six oxygen atoms of [18]crown-6 molecule and nitrogen atom of(4-bromoanilimiun) cation. Three kinds of different arranged supramolecular cations exist in the title compound, which are filled into the large space formed by [PMo(12)O40] polyoxoanions. Thermogravimentic differential thermal analysis revealed that hydrogen bonding interaction and intermolecular interaction play an important role in maintaining the stability of the title compound.展开更多
A novel organic-inorganic hybrid, Na2(Hmorph)2[MosO26]·2H2O (1, Hmorph = morpholine), has been synthesized by convenient aqueous solution method and structurally characterized by single-crystal X-ray diffract...A novel organic-inorganic hybrid, Na2(Hmorph)2[MosO26]·2H2O (1, Hmorph = morpholine), has been synthesized by convenient aqueous solution method and structurally characterized by single-crystal X-ray diffraction, IR, UV/Vis spectrum, elemental analysis and thermogravimetric analysis (TGA). Single-crystal X-ray analysis reveals that the title compound crystallizes in the monoclinic system, space group P21/c with a = 8.0194(4), b = 16.1398(8), c = 12.5893(6) A, fl = 92.824(4)°, V = 1627.47(14) A3, Mr = 1439.78, Z = 2, Dc = 2.938 g/cm3, p = 3.116 mm-1, F(000) = 1364, the final R = 0.0250, wR = 0.0628 and S = 1.027 for 3209 observed reflections with I 〉 2σ(/). In compound 1, the polyanions are stacked through electrostatic interactions, coordination of Na+ ions and hydrogen bonds to form a novel 3-D extended supramolecular "host" network with 1-D channels encapsulating organic "guests".展开更多
The crystal structure of one novel Mn(II) complex, [Mn(pmta)_3]_2[Mn(H_2O)_6]·4H_2O(1), is reported(Hpmta = 5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid). In the title compound, the asymmetric ...The crystal structure of one novel Mn(II) complex, [Mn(pmta)_3]_2[Mn(H_2O)_6]·4H_2O(1), is reported(Hpmta = 5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid). In the title compound, the asymmetric unit consists of a [Mn(pmta_)3]ˉ anion, half [Mn(H_2O)_6]^(2+) counter cation and two lattice H_2O molecules, and the intra- and intermolecular hydrogen bonds connect the complex into a supramolecular structure. The liquid-state fluorescence spectra of complex 1 have been determined. Hirshfeld surface analysis was also studied. The main intermolecular interactions in the complex are O···H and H···H contacts.展开更多
One-pot solvothermal reaction of Iransition metal Znn salt with 4,4-bipyddyl (bpy) and 1,4-benzenediacrylic add (H2L) in the presence of Et3N generates a three-dimensional (3-D) supramolecular network with 1-D c...One-pot solvothermal reaction of Iransition metal Znn salt with 4,4-bipyddyl (bpy) and 1,4-benzenediacrylic add (H2L) in the presence of Et3N generates a three-dimensional (3-D) supramolecular network with 1-D cation metal-organic coordination polymer, [Zn(H20)a(bpy)]-L 1, and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent property. The complex crystallizes in triclinic, space group P1 with a = 7.1291(2), b = 7.3784(3), c = 10.5042(3)A, α = 95.049(2), β = 102.162(2), 7 = 97.027(3)0, V= 532.38(3)A3, C22H24N2O8Zn, Mr = 509.82, De= 1.590 g/cm3, p(MoKa)= 1.207 ram-l, F(000) = 264, Z = 1,the finalR=O.0438and wR=O.lOll for 1589 observed reflections (I 〉 2σ(I)). In the crystal structure, the second building unit composed of [Zn(H2O)4].L constructs two distinct 2-D supramolecular sheets and a neutral 3-D architecture. The title compound 1 shows strong photoluminescence with emission maximum at 2 = 455 nm upon λex.max = 355 nm.展开更多
Two mononuclear metal-organic complexes, [Co(Hmpdc)2(H2O)4]·4H2O 1 and [Ni(Hfmpdc)2(H2O)4]·6H2O 2, were prepared from 2,6-dimethylpyridine-3,5-dicarboxylic acid (Hzmpdc) and 4-furyl-2,6-dimethylpyr...Two mononuclear metal-organic complexes, [Co(Hmpdc)2(H2O)4]·4H2O 1 and [Ni(Hfmpdc)2(H2O)4]·6H2O 2, were prepared from 2,6-dimethylpyridine-3,5-dicarboxylic acid (Hzmpdc) and 4-furyl-2,6-dimethylpyridine-3,5-dicarboxylic acid (H2fmpdc) with M(NO3)2 salts, respectively, and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent measurement. Complex 1 crystallizes in triclinic, space group P1 with a = 7.634(5), b = 8.695(5), c = 10.757(6)A, α = 69.647(7), β = 69.957(8), γ = 83.733(7)°, V = 628.9(7)A^3, Dc = 1. 561 g/cm^3,μ(MoKa) = 0.763 mm^-1, F(000) = 309, Z = 1, the final R = 0.0553 and wR = 0.1469 for 1909 observed reflections (Ⅰ 〉 2σ(Ⅰ)). Complex 2 crystallizes in monoclinic, space group P21/n with a = 9.5934(16), b = 12.422(2), c = 14.826(3) A, β = 105.201(2)°, V = 1705.0(5)A3, Dc = 1. 479 g/cm^3,μ(MoKa) = 0.655 mm^-1, F(000) = 796, Z = 2, the final R= 0.0351 and wR = 0.0889 for 2387 obsevved reflections (Ⅰ 〉 2σ(Ⅰ)). In the crystal structures of 1 and 2, diverse supramolecular motifs from 1-D chains/ladders to 3-D networks are constructed from corresponding distinct [M^Ⅱ(H2O)8] ion clusters as the second building units, respectively. The solid state compounds of 1 and 2 show similar photoluminescent spectra with emission maximum at ca.展开更多
Melanins represent one of the most ancient and important group of natural macromolecular pigments.They have multiple biological roles in almost all organisms across the Phyla,examples being photoprotection,anti-oxidat...Melanins represent one of the most ancient and important group of natural macromolecular pigments.They have multiple biological roles in almost all organisms across the Phyla,examples being photoprotection,anti-oxidative action,radical scavenger activity,and heavy metal removal.From the biomedical point of view,melanocytes are involved in the origin of melanoma tumors,and the main therapeutic advances for their treatment have been revised in Part 1 of this review.The chemical structure of eumelanin is a biological concern of great importance,and therefore,exploring theoretical molecular models and synthesis mechanisms will be here described,as well as molecular orbital features and supramolecular organization,which are responsible for the key properties that make these biological pigments so important,and so fascinating.Ultimately,this updated overview is devoted to describe present structural models and physico-chemical characteristics of eumelanin,in order to explain and utilize melanin properties on which new photothermal and ultrasonic protocols for melanoma treatment can be devised and applied.展开更多
Tungsten dioxo complex WO 2(C 9H 6NO) 2 was obtained via the low temperature solid-state reaction of(NH 4) 2WS 4, 8-hydroxyquinoline(8-hq) and(CH 3) 4NI, and it was characterized by means of elemental analyse...Tungsten dioxo complex WO 2(C 9H 6NO) 2 was obtained via the low temperature solid-state reaction of(NH 4) 2WS 4, 8-hydroxyquinoline(8-hq) and(CH 3) 4NI, and it was characterized by means of elemental analyses, IR spectroscopy and X-ray diffraction analysis. The crystal of the title compound belongs to monoclinic, space group C2/c, with the crystal cell parameters: a=1.3316(3) nm, b=0.94444(19) nm, c=1.3485(3) nm, β=109.66(3)°, V=1.5970(6) nm 3, Z=6. The title compound possesses a supramolecular structure formed through hydrogen bonds and π-π stacking interactions. The third-order non-linear optical(NLO) properties of the title compound were also investigated. The third-order non-linear absorption coefficient α 2 and refractive index n 2 are 0.85×10 -11 m/W -1 and -1.5×10 -19 m 2/W, respectively. The third-order non-linear susceptibility χ (3) is 3.03×10 -13 esu for 3.8×10 -5 mol/L sample concentration.展开更多
The dual ligand system of V-shaped 5-(4-carboxy-2-nitrophenoxy)-isophthalic acid(Hcn-H2ipa) and dipyridy-type molecules produces two new coordination polymers: {[Ni(cn-Hipa)(bpa)(H2O)3]·1.5H2O}n 1 and ...The dual ligand system of V-shaped 5-(4-carboxy-2-nitrophenoxy)-isophthalic acid(Hcn-H2ipa) and dipyridy-type molecules produces two new coordination polymers: {[Ni(cn-Hipa)(bpa)(H2O)3]·1.5H2O}n 1 and {[Cu(Hcn-ipa)(ppe)2]}n 2(bpa = 1,2-bis(4-pyridyl)ethane, and ppe = trans-1-(2-pyridyl)-2-(4-pyridyl)ethylene). Two complexes have been characterized by single-crystal X-ray diffraction, elemental analysis, IR, and thermogravimetric analysis(TGA). Complex 1 is of monoclinic system, space group C2 with a = 25.936(3), b = 7.6100(10), c = 16.558(2), β = 105.9470(10)°, V = 3142.4(7) A3, Dc = 1.415 g/cm3, Mr = 669.23, Z = 4, F(000) = 1388, μ = 0.687 mm-1, the final R = 0.0397 and w R = 0.0967 for 12070 observed reflections with I 〉 2σ(I). Complex 2 belongs to the triclinic system, space group P1 with a = 10.165(5), b = 14.946(7), c = 15.506(11) A, α = 106.461(7), β = 102.454(8), γ = 107.861(5)°, V = 2029(2) A3, Dc = 1.266 g/cm3, Mr = 773.20, Z = 2, F(000) = 794, μ = 0.595 mm-1, the final R = 0.0538 and w R = 0.1378 for 15488 observed reflections with I 〉 2σ(I). Two complexes show that the 1D polymeric chains are cohered together by extensive H-bonds to complete stable supramolecular microporous frameworks.展开更多
A binicotinic biscarbohydrazone compound,2,2'-bipyridyl-3,3'-bis(N,N'-disali- cylidene)-formyhydrazone,1 has been prepared and characterized by elemental analysis,FT-IR,1H- NMR,ESI-MS and single-crystal X-ray dif...A binicotinic biscarbohydrazone compound,2,2'-bipyridyl-3,3'-bis(N,N'-disali- cylidene)-formyhydrazone,1 has been prepared and characterized by elemental analysis,FT-IR,1H- NMR,ESI-MS and single-crystal X-ray diffraction analysis. The crystal belongs to triclinic,space group P1 with a = 9.419(3),b = 11.745(4),c = 12.035(5)A,V = 1178.8(7)A^3,Z = 2,Dc = 1.354 g/cm^3,μ = 0.095 mm^-1,F(000) = 500,λ(MoKα) = 0.71073 ,C26H20N6O4,Mr = 480.48,the final R = 0.0480 and wR = 0.1084 for 3634 observed reflections with I 〉 2σ(I). Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 1 has been constructed by multiply intermolecular N–H···N and O–H···O H-bonding interactions. Besides,compound 1 exhibits a strong green-light emission in the solid state at room temperature.展开更多
Two new organic supramolecular cocrystal complexes C18H18O4·C10H8N2(I) and C18H18O4·C12H10N2(II)(C18H18O4 = 2,3,6,7-tetrahydroxyl-9,10-dimethyl-9,10-dihydro-9,10-ethanoanthracene(LH4), C10H8N2 = 4,4'...Two new organic supramolecular cocrystal complexes C18H18O4·C10H8N2(I) and C18H18O4·C12H10N2(II)(C18H18O4 = 2,3,6,7-tetrahydroxyl-9,10-dimethyl-9,10-dihydro-9,10-ethanoanthracene(LH4), C10H8N2 = 4,4'-bipyridine(bpy) and C12H10N2 = 4,4'-bipyridinylethane(bpe)) have been obtained by mixing LH4 with corresponding bpy or bpe ligand. The two complexes have been determined by X-ray crystal structure analysis, elemental analysis and IR analysis. Compound I crystallizes in the orthorhombic Pnma with a = 9.7078(4), b = 22.4974(10), c = 20.6272(9) V = 4505.0(3)3, Mr = 454.51, Dc. = 1.340 g·cm^-3, μ = 0.09 mm-1, F(000) = 1920, Z = 8, R = 0.0503 and wR = 0.1360. Compound II crystallizes in monoclinic C2/c with a = 29.944(6), b = 9.820(2), c = 22.643(5) , V = 5048.4(18)3, Mr = 480.54, Dc. = 1.265 g cm^–3, μ = 0.084 mm^–1, F(000) = 2032, Z = 8, R = 0.0548 and wR = 0.1600. X-ray single-crystal structure analysis shows that two-dimensional(2D) layer supramolecular structures are formed through hydrogen bonds and π-π interactions in the two complexes. IR analysis also indicates that there are only associated hydroxyl groups in the two complexes.展开更多
A novel Cd(Ⅱ) coordination polymer, [CdCI(Hpc)H2O]n (1, H2pc = 1H-pyrazole-3- carboxylic acid), was synthesized by the reaction of CdCl2·2.5H2O with H2pc, and structurally characterized by IR spectrum, UV-...A novel Cd(Ⅱ) coordination polymer, [CdCI(Hpc)H2O]n (1, H2pc = 1H-pyrazole-3- carboxylic acid), was synthesized by the reaction of CdCl2·2.5H2O with H2pc, and structurally characterized by IR spectrum, UV-Vis spectrum, elemental analysis, single-crystal X-ray diffraction, as well as thermal analysis. Compound 1 crystallizes in monoclinic, P21/n space group with α = 7.0304(3), b = 10.3047(3), c = 10.6446(4) A, β= 107.174(4)°, F = 736.78(5) A^3, Z = 4, C4HsCdClN2O3, Mr = 276.95, Dc = 2.497 g/cm%3, F(000) = 528.0,μ= 3.281 mm^-1, R = 0.0169 and wR = 0.0387. The central metals adopt distorted octahedral geometry. Carboxyl groups of the ligand connect Cd(Ⅱ) into a one-dimensional chain, which further constructs a two-dimensional network by halogen bridging. Such two-dimensional structures are finally connected into a three-dimensional supramolecular architecture due to the hydrogen bonds and intermolecular π…π interactions. In addition, complex 1 has high thermal stability.展开更多
Two crystals of receptor 1, C(42)H(52)N(10)O4S2(anthracene-9,10-dicarbaldehyde bis-(phenyl-semithiocarbazone)) and-1-H2PO4, C(68)H(114)N(10)O(10)P2S2 were obtained at room temperature successfully, a...Two crystals of receptor 1, C(42)H(52)N(10)O4S2(anthracene-9,10-dicarbaldehyde bis-(phenyl-semithiocarbazone)) and-1-H2PO4, C(68)H(114)N(10)O(10)P2S2 were obtained at room temperature successfully, and their structures were characterized by X-ray crystallography diffraction. X-ray diffraction reveals that, receptor 1 crystallizes in monoclinic, space group P21/c, with a = 9.487(3),b = 20.674(6), c = 11.821(4)A, β = 113.416(8)o, Mr = 825.06, V = 2127.5(12) A^3, Z = 2, Dc = 1.288g/cm^3, μ = 0.18 mm^-1, F(000) = 876, MoK α radiation(λ = 0.71073 A), the final R = 0.0472 and wR = 0.0930. A total of 3758 unique reflections were collected, of which 3313 with I 〉 2σ(I) were observed. Compound 1-H2PO4^-crystallizes in triclinic, space group P21/n, with a = 8.767(1), b =13.6190(15), c = 16.615(2) ?, α = 98.727(14), β = 103.061(14), γ = 91.382(16)°, Mr = 1357.75, V =1906.6(4) A^3, Z = 1, Dc = 1.183 g/cm^3, μ = 0.17 mm-(-1), F(000) = 734, MoK α radiation(λ = 0.71073?), the final R = 0.0769 and wR = 0.1884. A total of 6699 unique reflections were collected, of which 2989 with I 〉 2σ(I) were observed. As it was observed in the crystal structure of 1-H2PO4^-, 1bound H2PO4^-at a 1:2 ratio by intermolecular interaction of N-H···O hydrogen bond obviously.Another interesting feature was that H2PO4--groups assembled chains themselves via intramolecular hydrogen bond O-H···O and connected the 1 molecules together through the interaction of H-bonds,which improved the planarity of 1 and increased the stability of the entire structure.展开更多
A novel bimetallic porphyrin complex salt, { [MnTPP(CHaOH)2]3Fe(CN)6}·13H2O (TPP = tetraphenylporphyrin), has been synthesized and structurally characterized by X-ray diffraction analysis. The crystal is of...A novel bimetallic porphyrin complex salt, { [MnTPP(CHaOH)2]3Fe(CN)6}·13H2O (TPP = tetraphenylporphyrin), has been synthesized and structurally characterized by X-ray diffraction analysis. The crystal is of trigonal, space group R-3 with a = b = 31.0618(10), c = 11.8366(8)A, Z = 3, V = 9890.3(8)A^3, C144H134FeMn3N18O19, Mr = 2641.36, Dc = 1.330 g/cm^3, μ(MoKa) = 0.463 mm^-1, F(000) = 4131, R= 0.0525 and wR = 0.1382 for 3045 observed reflections (I 〉 2σ(I)). The title complex is composed of one [Fe(CN)6]^3- anion, three [MnTPP(CH3OH)2]^+ cations and thirteen water molecules, which are connected by multiform hydrogen bonds leading to a 3D supramolecular network structure.展开更多
基金the National Natural Science Foundation of China(No.20474022)for financial support.
文摘N-Octadecyl-N1-maleoyl-L-phenylalanine (ODMA-L-Phe) was synthesized through the condensation, deprotection and acid- ylation reaction of BOC-L-phenylalanine, octadecylamine and maleic anhydride. ODMA-L-Phe can self-assemble in some organic solvents and turned them into thermally reversible physical supramolecular organogels. The morphology of ODMA-L-Phe aggregates was characterized by polarized optical microscopy (POM) and field emission scanning electron microscope (FE-SEM). The aggregates of ODMA-L-Phe were needle-like fibrils with diameters of approximately 100-200 nm. The mechanism of ODMA- L-Phe self-assembly in organic solvents was investigated using XH NMR and circular dichroism (CD). The results indicated that hydrogen bonding was one of the main driving forces for the self-assembly of ODMA-L-Phe.
基金theNationalNaturalScienceFoundationofChina (No .2 97330 90 )theDoctoralProgramofHigherEducation(No.19990 18310 )
文摘The hydrothermal reactions of CuI, KI and bidentate amines [ 1,10 phenanthroline (phen) or ethylenediamine (en)] gave the three copper(I) halide compounds, Cu3I3(phen)2 (1), CuI(phen)2 (2) and 2 (3), which were structurally characterized via singlecrystal Xray diffraction studies. Hydrogen bonds and ππ interactions are the most remarkable structural features of the title compounds. All can be described as higherdimensional supramolecular compounds connected via these secondary bondings. Moreover, the title compounds were characterized by elemental analyses, IR spectra and TGA analyses. The thirdorder nonlinear optical properties of the title compounds were also investigated and all exhibit nicer nonlinear absorption and selffocusing performance.Keywords copper(I) halide, hydrothermal synthesis, the thirdorder nonlinear optical property, supramolecular structure
基金supported by the National Natural Science Foundation of China (Nos. 20771054 and 20471026) Henan Tackle Key Problem of Science and Technology (Nos. 072102270030 and 072102270034)
文摘Making use of N-P-acetamidobenzenesulfonyl-glycine acid (abbreviated as abglyH2),two transitional metal complexes [Zn(abglyH)(phen)2]ClO4·H2O (1) and Co(abglyH)2(bipy)2(H2O)2 (2) (phen = 1,10-phenanthroline,bipy = 4,4'-bipyridine) have been synthesized under mild conditions and characterized by IR,elemental analysis and X-ray diffraction analysis. Complex 1 is a monomeric compound which is further assembled by intermolecular hydrogen bonds and π-π interaction into a 2-D supramolecular network. Complex 2 is also a monomeric compound and further connected by intermolecular hydrogen bonds to form a 2-D supramolecular network. Fluorescent analysis shows that complex 1 has an emissive maximum at 364 nm in the solution state at room temperature.
基金Supported by the National Natural Science Foundation of China (Nos. 20971065, 20721002)National Basic Research Program of China (2007CB925103,2010CB923303)
文摘Four cobalt supramolecular architectures with Hmtyaa(2-(5-methyl-1,3,4-thiadiazol-2-ylthio)acetic acid) ligand have been synthesized.[Co(mtyaa)2(H2O)4]·4(H2O)(1):triclinic,space group P1 with a = 6.7537(18),b = 8.591(2),c = 10.615(3) ,α = 96.495(4),β = 99.955(5),γ = 103.615(5)°,V = 581.9(3) 3,Z = 1,Mr = 581.52,Dc = 1.659 g/m3,μ = 1.158 mm-1,F(000) = 301,Rint = 0.0557,R = 0.0377 and wR = 0.1056 for 1854 observed reflections with Ⅰ 〉 2σ(Ⅰ);{[Co(4,4'-bipy)(H2O)4]·2(mtyaa)·2(H2O)}n(2):triclinic,space group P1 with a = 7.669(2),b = 8.840(3),c = 11.521(4) ,α = 79.912(5),β = 73.954(5),γ = 86.612(6)°,V = 738.9(4) 3,Z = 1,Mr = 701.67,Dc = 1.577 g/m3,μ = 0.924 mm-1,F(000) = 363,Rint = 0.0636,R = 0.0498 and wR = 0.1311 for 2155 observed reflections with Ⅰ 〉 2σ(Ⅰ);{[Co(4,4'-bipy)(mtyaa)(H2O)3](mtyaa)·2(H2O)}(3):monoclinic,space group Pc with a = 7.7832(17),b = 11.527(3),c = 31.483(7) ,β = 91.952(4)°,V = 2822.9(11) 3,Z = 4,Mr = 683.65,Dc = 1.609 g/m3,μ = 0.963 mm-1,F(000) = 1412,Rint = 0.0758,R = 0.0609 and wR = 0.1095 for 5841 observed reflections with I 〉 2σ(I);{[Co(bpe)(mtyaa)2(H2O)2]}n(4):monoclinic,space group C2/c with a = 19.290(11),b = 12.027(7),c = 14.865(8) ,β = 125.648(8)°,V = 2802(3)3,Z = 4,Mr = 657.66,Dc = 1.559 g/m3,μ = 0.959 mm-1,F(000) = 1356,Rint = 0.0456,R = 0.0332 and wR = 0.0985 for 2299 observed reflections with Ⅰ 〉 2σ(Ⅰ).
基金supported by the National Natural Science Foundation of China (No. 20947003)China Postdoctoral Science Foundation (No. 20090461066)
文摘A new complex [Pb(phen)2(4-NBA)]2·2(NO3)·H2O(phen = 1,10-phenanthroline,4-NBA = 4-nitrobenzoate) has been hydrothermally synthesized and structurally determined by single-crystal X-ray diffraction,elemental analyses and IR spectroscopy.The complex crystallizes in monoclinic,space group P21/c with a = 13.416(3),b = 14.065(3),c = 16.845(3)(A°) ,β = 110.55(3)o,V = 2976.5(10)(A°)^3,Z = 2,Dc = 1.796 g/cm^3,F(000) = 1564,GOOF = 0.962,the final R = 0.0686 and wR = 0.1746.The crystal structure shows that the lead ion is coordinated with two carboxylate O atoms from the 4-NBA anion,and four N atoms from two phen molecules,forming a slightly distorted pentagonalbipyramidal coordination geometry.It is further extended by various supramo-lecular interactions to form a three-dimensional supramolecular network.The TG analysis result shows that this complex begins decomposing at 30 ℃ and decompounding completely at 733 ℃.
基金supported by the National Basic Research Program of China(973 Program,2012CB821702)the National Natural Science Foundation of China(21233009 and 21173221)
文摘Two homochiral enantiomorphic 3D coordination polymers: (D-HAPA)2[Cd2Cs(D- HAPA)(m-BDC)4]'(EtOH) (1D) and (L-HAPA)2[Cd2Cs(L-HAPA)(m-BDC)a]'(EtOH) (1L) (APA = 2-amino-l-propanol, m-H2BDC = 1,3-benzenedicarboxylate), have been assembled solvothermally respectively with the induction of enantiomorphic organic small molecules (D,L-APA). 1L and 1I) crystallize in chiral space group P21 with Flack parameters of-0.012(13) and -0.07(3), respectively, and have been characterized by satisfactory elemental analysis, FT-IR spectra, CD-spectra and single-crystal X-ray diffraction. They both exhibit sqp topological net, purple fluorescence and SHG activity.
基金Supported by the Science and Technology Projects of Chongqing Municipal Education Commission(KJ120632)Scientific Research Foundation Project of Chongqing Normal University (2011XLS30, 10XLZ005)
文摘One-pot solvothermal reaction of transition metal Cd(II ) salt with (2E,2′E)-3,3′- ((propane-1,3-diylbis(oxy))bis(2,1-phenylene))diacrylic acid (H2ppa) and 1,10-phenanthroline (phen) generates a meso-helicate, [Cd(ppa)(phen)(H2O)]2, and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent property. The complex crys- tallizes in monoclinic, space group P21/c with a = 13.4622(7), b = 24.8452(12), c = 8.9314(4) A, β = 97.564(1)°, V = 2961.3(2) A3, C66H56N4O14Cd2, Mr = 1353.97, Dc = 1.518 g/cm3, μ(MoKa) = 0.789 mm-1, F(000) = 1376, Z = 2, the final R = 0.0248 and wR = 0.0667 for 4673 observed reflections (I 〉 2σ(I)). The I-D supramolecular chain is built up from the complex by π-π stacking interactions, and inter-chain hydrogen bonds prompt the I-D chains into a 2-D layer. The title compound shows strong photoluminescence with emission maximum at 2 = 445 nm upon λEx, max = 240 nm.
基金thank the foundation of Wuhan Textile University(No.165002)Hubei Key Laboratory of Biomass Fibers and Eco-dyeing&Finishing for supporting this work
文摘A novel supramolecular structural inorganic-organic hybrid [(4-bromoanilimiun)([18]crown-6)]3[PMo(12)O40]·CH3 CN has been synthesized through standard solvent evaporated method. The structure of the title compound was determined through single-crystal X-ray diffraction analysis. It crystallizes in monoclinic system with P21/n space group. The crystal data are a = 18.9529(4), b = 26.4444(5), c = 19.0985(4) A, β = 90.132(6)o, V = 9572.1(3) A^3, Z = 4, Dc= 2.203 g·cm^(–1), μ = 14.956 mm^(–1), F(000) = 6192, S = 1.098, the final R = 0.0859 and w R(I 〉 2σ(I)) = 0.2100. Supramolecular cations are constructed through strong N–H…O hydrogen bonding interaction between the six oxygen atoms of [18]crown-6 molecule and nitrogen atom of(4-bromoanilimiun) cation. Three kinds of different arranged supramolecular cations exist in the title compound, which are filled into the large space formed by [PMo(12)O40] polyoxoanions. Thermogravimentic differential thermal analysis revealed that hydrogen bonding interaction and intermolecular interaction play an important role in maintaining the stability of the title compound.
基金supported by the Science and Technology Development Foundation of Jilin Province(201201105,201215171)
文摘A novel organic-inorganic hybrid, Na2(Hmorph)2[MosO26]·2H2O (1, Hmorph = morpholine), has been synthesized by convenient aqueous solution method and structurally characterized by single-crystal X-ray diffraction, IR, UV/Vis spectrum, elemental analysis and thermogravimetric analysis (TGA). Single-crystal X-ray analysis reveals that the title compound crystallizes in the monoclinic system, space group P21/c with a = 8.0194(4), b = 16.1398(8), c = 12.5893(6) A, fl = 92.824(4)°, V = 1627.47(14) A3, Mr = 1439.78, Z = 2, Dc = 2.938 g/cm3, p = 3.116 mm-1, F(000) = 1364, the final R = 0.0250, wR = 0.0628 and S = 1.027 for 3209 observed reflections with I 〉 2σ(/). In compound 1, the polyanions are stacked through electrostatic interactions, coordination of Na+ ions and hydrogen bonds to form a novel 3-D extended supramolecular "host" network with 1-D channels encapsulating organic "guests".
基金supported by the National Natural Science Foundation of China(No.20801012)New Energy Technology Co.Ltd.of Ai Naji of Jiangsu Province(No.8507040091)
文摘The crystal structure of one novel Mn(II) complex, [Mn(pmta)_3]_2[Mn(H_2O)_6]·4H_2O(1), is reported(Hpmta = 5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid). In the title compound, the asymmetric unit consists of a [Mn(pmta_)3]ˉ anion, half [Mn(H_2O)_6]^(2+) counter cation and two lattice H_2O molecules, and the intra- and intermolecular hydrogen bonds connect the complex into a supramolecular structure. The liquid-state fluorescence spectra of complex 1 have been determined. Hirshfeld surface analysis was also studied. The main intermolecular interactions in the complex are O···H and H···H contacts.
基金supported by the NNSFC (No. 20701041)the Key Project of Chinese Ministry of Education (No. 208116)+1 种基金the Natural Science Foundation of CQ CSTC (No. 2007BB5228)the Scientific and Technological Project of CQEC (No. KJ080829)
文摘One-pot solvothermal reaction of Iransition metal Znn salt with 4,4-bipyddyl (bpy) and 1,4-benzenediacrylic add (H2L) in the presence of Et3N generates a three-dimensional (3-D) supramolecular network with 1-D cation metal-organic coordination polymer, [Zn(H20)a(bpy)]-L 1, and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent property. The complex crystallizes in triclinic, space group P1 with a = 7.1291(2), b = 7.3784(3), c = 10.5042(3)A, α = 95.049(2), β = 102.162(2), 7 = 97.027(3)0, V= 532.38(3)A3, C22H24N2O8Zn, Mr = 509.82, De= 1.590 g/cm3, p(MoKa)= 1.207 ram-l, F(000) = 264, Z = 1,the finalR=O.0438and wR=O.lOll for 1589 observed reflections (I 〉 2σ(I)). In the crystal structure, the second building unit composed of [Zn(H2O)4].L constructs two distinct 2-D supramolecular sheets and a neutral 3-D architecture. The title compound 1 shows strong photoluminescence with emission maximum at 2 = 455 nm upon λex.max = 355 nm.
基金supported by the NNSFC (No. 20701041)the Key Project of Chinese Ministry of Education (No. 208116)+1 种基金the Natural Science Foundation of CQ CSTC (No. 2007BB5228)the Scientific and Technological Project of CQEC (No. KJ080829).
文摘Two mononuclear metal-organic complexes, [Co(Hmpdc)2(H2O)4]·4H2O 1 and [Ni(Hfmpdc)2(H2O)4]·6H2O 2, were prepared from 2,6-dimethylpyridine-3,5-dicarboxylic acid (Hzmpdc) and 4-furyl-2,6-dimethylpyridine-3,5-dicarboxylic acid (H2fmpdc) with M(NO3)2 salts, respectively, and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent measurement. Complex 1 crystallizes in triclinic, space group P1 with a = 7.634(5), b = 8.695(5), c = 10.757(6)A, α = 69.647(7), β = 69.957(8), γ = 83.733(7)°, V = 628.9(7)A^3, Dc = 1. 561 g/cm^3,μ(MoKa) = 0.763 mm^-1, F(000) = 309, Z = 1, the final R = 0.0553 and wR = 0.1469 for 1909 observed reflections (Ⅰ 〉 2σ(Ⅰ)). Complex 2 crystallizes in monoclinic, space group P21/n with a = 9.5934(16), b = 12.422(2), c = 14.826(3) A, β = 105.201(2)°, V = 1705.0(5)A3, Dc = 1. 479 g/cm^3,μ(MoKa) = 0.655 mm^-1, F(000) = 796, Z = 2, the final R= 0.0351 and wR = 0.0889 for 2387 obsevved reflections (Ⅰ 〉 2σ(Ⅰ)). In the crystal structures of 1 and 2, diverse supramolecular motifs from 1-D chains/ladders to 3-D networks are constructed from corresponding distinct [M^Ⅱ(H2O)8] ion clusters as the second building units, respectively. The solid state compounds of 1 and 2 show similar photoluminescent spectra with emission maximum at ca.
文摘Melanins represent one of the most ancient and important group of natural macromolecular pigments.They have multiple biological roles in almost all organisms across the Phyla,examples being photoprotection,anti-oxidative action,radical scavenger activity,and heavy metal removal.From the biomedical point of view,melanocytes are involved in the origin of melanoma tumors,and the main therapeutic advances for their treatment have been revised in Part 1 of this review.The chemical structure of eumelanin is a biological concern of great importance,and therefore,exploring theoretical molecular models and synthesis mechanisms will be here described,as well as molecular orbital features and supramolecular organization,which are responsible for the key properties that make these biological pigments so important,and so fascinating.Ultimately,this updated overview is devoted to describe present structural models and physico-chemical characteristics of eumelanin,in order to explain and utilize melanin properties on which new photothermal and ultrasonic protocols for melanoma treatment can be devised and applied.
基金the National Natural Science Foundation of China(No.2 0 2 710 2 1)
文摘Tungsten dioxo complex WO 2(C 9H 6NO) 2 was obtained via the low temperature solid-state reaction of(NH 4) 2WS 4, 8-hydroxyquinoline(8-hq) and(CH 3) 4NI, and it was characterized by means of elemental analyses, IR spectroscopy and X-ray diffraction analysis. The crystal of the title compound belongs to monoclinic, space group C2/c, with the crystal cell parameters: a=1.3316(3) nm, b=0.94444(19) nm, c=1.3485(3) nm, β=109.66(3)°, V=1.5970(6) nm 3, Z=6. The title compound possesses a supramolecular structure formed through hydrogen bonds and π-π stacking interactions. The third-order non-linear optical(NLO) properties of the title compound were also investigated. The third-order non-linear absorption coefficient α 2 and refractive index n 2 are 0.85×10 -11 m/W -1 and -1.5×10 -19 m 2/W, respectively. The third-order non-linear susceptibility χ (3) is 3.03×10 -13 esu for 3.8×10 -5 mol/L sample concentration.
基金supported by the National Natural Science Foundation of China(No.21271098)the Foundation of Education Committee of Henan Province(No.142300410301)
文摘The dual ligand system of V-shaped 5-(4-carboxy-2-nitrophenoxy)-isophthalic acid(Hcn-H2ipa) and dipyridy-type molecules produces two new coordination polymers: {[Ni(cn-Hipa)(bpa)(H2O)3]·1.5H2O}n 1 and {[Cu(Hcn-ipa)(ppe)2]}n 2(bpa = 1,2-bis(4-pyridyl)ethane, and ppe = trans-1-(2-pyridyl)-2-(4-pyridyl)ethylene). Two complexes have been characterized by single-crystal X-ray diffraction, elemental analysis, IR, and thermogravimetric analysis(TGA). Complex 1 is of monoclinic system, space group C2 with a = 25.936(3), b = 7.6100(10), c = 16.558(2), β = 105.9470(10)°, V = 3142.4(7) A3, Dc = 1.415 g/cm3, Mr = 669.23, Z = 4, F(000) = 1388, μ = 0.687 mm-1, the final R = 0.0397 and w R = 0.0967 for 12070 observed reflections with I 〉 2σ(I). Complex 2 belongs to the triclinic system, space group P1 with a = 10.165(5), b = 14.946(7), c = 15.506(11) A, α = 106.461(7), β = 102.454(8), γ = 107.861(5)°, V = 2029(2) A3, Dc = 1.266 g/cm3, Mr = 773.20, Z = 2, F(000) = 794, μ = 0.595 mm-1, the final R = 0.0538 and w R = 0.1378 for 15488 observed reflections with I 〉 2σ(I). Two complexes show that the 1D polymeric chains are cohered together by extensive H-bonds to complete stable supramolecular microporous frameworks.
文摘A binicotinic biscarbohydrazone compound,2,2'-bipyridyl-3,3'-bis(N,N'-disali- cylidene)-formyhydrazone,1 has been prepared and characterized by elemental analysis,FT-IR,1H- NMR,ESI-MS and single-crystal X-ray diffraction analysis. The crystal belongs to triclinic,space group P1 with a = 9.419(3),b = 11.745(4),c = 12.035(5)A,V = 1178.8(7)A^3,Z = 2,Dc = 1.354 g/cm^3,μ = 0.095 mm^-1,F(000) = 500,λ(MoKα) = 0.71073 ,C26H20N6O4,Mr = 480.48,the final R = 0.0480 and wR = 0.1084 for 3634 observed reflections with I 〉 2σ(I). Single-crystal X-ray diffraction analysis reveals that a 1D supramolecular structure of 1 has been constructed by multiply intermolecular N–H···N and O–H···O H-bonding interactions. Besides,compound 1 exhibits a strong green-light emission in the solid state at room temperature.
基金supported by the National Natural Science Foundation of China(No.21176246)Jiangsu Qinglan Project
文摘Two new organic supramolecular cocrystal complexes C18H18O4·C10H8N2(I) and C18H18O4·C12H10N2(II)(C18H18O4 = 2,3,6,7-tetrahydroxyl-9,10-dimethyl-9,10-dihydro-9,10-ethanoanthracene(LH4), C10H8N2 = 4,4'-bipyridine(bpy) and C12H10N2 = 4,4'-bipyridinylethane(bpe)) have been obtained by mixing LH4 with corresponding bpy or bpe ligand. The two complexes have been determined by X-ray crystal structure analysis, elemental analysis and IR analysis. Compound I crystallizes in the orthorhombic Pnma with a = 9.7078(4), b = 22.4974(10), c = 20.6272(9) V = 4505.0(3)3, Mr = 454.51, Dc. = 1.340 g·cm^-3, μ = 0.09 mm-1, F(000) = 1920, Z = 8, R = 0.0503 and wR = 0.1360. Compound II crystallizes in monoclinic C2/c with a = 29.944(6), b = 9.820(2), c = 22.643(5) , V = 5048.4(18)3, Mr = 480.54, Dc. = 1.265 g cm^–3, μ = 0.084 mm^–1, F(000) = 2032, Z = 8, R = 0.0548 and wR = 0.1600. X-ray single-crystal structure analysis shows that two-dimensional(2D) layer supramolecular structures are formed through hydrogen bonds and π-π interactions in the two complexes. IR analysis also indicates that there are only associated hydroxyl groups in the two complexes.
基金supported by the National Natural Science Foundation of China(No.20801012)New Energy Technology Co.Ltd.of Ai Naji of Jiangsu Province(No.8507040091)
文摘A novel Cd(Ⅱ) coordination polymer, [CdCI(Hpc)H2O]n (1, H2pc = 1H-pyrazole-3- carboxylic acid), was synthesized by the reaction of CdCl2·2.5H2O with H2pc, and structurally characterized by IR spectrum, UV-Vis spectrum, elemental analysis, single-crystal X-ray diffraction, as well as thermal analysis. Compound 1 crystallizes in monoclinic, P21/n space group with α = 7.0304(3), b = 10.3047(3), c = 10.6446(4) A, β= 107.174(4)°, F = 736.78(5) A^3, Z = 4, C4HsCdClN2O3, Mr = 276.95, Dc = 2.497 g/cm%3, F(000) = 528.0,μ= 3.281 mm^-1, R = 0.0169 and wR = 0.0387. The central metals adopt distorted octahedral geometry. Carboxyl groups of the ligand connect Cd(Ⅱ) into a one-dimensional chain, which further constructs a two-dimensional network by halogen bridging. Such two-dimensional structures are finally connected into a three-dimensional supramolecular architecture due to the hydrogen bonds and intermolecular π…π interactions. In addition, complex 1 has high thermal stability.
基金supported by the China Postdoctoral Science Foundation(No.2014M551053)Natural Science Foundation of Hebei Province(No.B2015203124)Key Laboratory of Advanced Energy Materials Chemistry(Ministry of Education),Nankai University
文摘Two crystals of receptor 1, C(42)H(52)N(10)O4S2(anthracene-9,10-dicarbaldehyde bis-(phenyl-semithiocarbazone)) and-1-H2PO4, C(68)H(114)N(10)O(10)P2S2 were obtained at room temperature successfully, and their structures were characterized by X-ray crystallography diffraction. X-ray diffraction reveals that, receptor 1 crystallizes in monoclinic, space group P21/c, with a = 9.487(3),b = 20.674(6), c = 11.821(4)A, β = 113.416(8)o, Mr = 825.06, V = 2127.5(12) A^3, Z = 2, Dc = 1.288g/cm^3, μ = 0.18 mm^-1, F(000) = 876, MoK α radiation(λ = 0.71073 A), the final R = 0.0472 and wR = 0.0930. A total of 3758 unique reflections were collected, of which 3313 with I 〉 2σ(I) were observed. Compound 1-H2PO4^-crystallizes in triclinic, space group P21/n, with a = 8.767(1), b =13.6190(15), c = 16.615(2) ?, α = 98.727(14), β = 103.061(14), γ = 91.382(16)°, Mr = 1357.75, V =1906.6(4) A^3, Z = 1, Dc = 1.183 g/cm^3, μ = 0.17 mm-(-1), F(000) = 734, MoK α radiation(λ = 0.71073?), the final R = 0.0769 and wR = 0.1884. A total of 6699 unique reflections were collected, of which 2989 with I 〉 2σ(I) were observed. As it was observed in the crystal structure of 1-H2PO4^-, 1bound H2PO4^-at a 1:2 ratio by intermolecular interaction of N-H···O hydrogen bond obviously.Another interesting feature was that H2PO4--groups assembled chains themselves via intramolecular hydrogen bond O-H···O and connected the 1 molecules together through the interaction of H-bonds,which improved the planarity of 1 and increased the stability of the entire structure.
基金the Natural Science Foundation of Gansu Province (3ZS041-A25-008)
文摘A novel bimetallic porphyrin complex salt, { [MnTPP(CHaOH)2]3Fe(CN)6}·13H2O (TPP = tetraphenylporphyrin), has been synthesized and structurally characterized by X-ray diffraction analysis. The crystal is of trigonal, space group R-3 with a = b = 31.0618(10), c = 11.8366(8)A, Z = 3, V = 9890.3(8)A^3, C144H134FeMn3N18O19, Mr = 2641.36, Dc = 1.330 g/cm^3, μ(MoKa) = 0.463 mm^-1, F(000) = 4131, R= 0.0525 and wR = 0.1382 for 3045 observed reflections (I 〉 2σ(I)). The title complex is composed of one [Fe(CN)6]^3- anion, three [MnTPP(CH3OH)2]^+ cations and thirteen water molecules, which are connected by multiform hydrogen bonds leading to a 3D supramolecular network structure.