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1.
The structure of the title compound, poly[(dihydrogenphosphato‐κO)(μ3‐hydrogenphosphato)di‐μ‐oxido‐(1,10‐phenanthroline)copper(II)vanadium(V)], [CuV(HPO4)(H2PO4)O2(C12H8N2)]n, is defined by [(phen)Cu–μ‐(κ2O:O′‐VP2O10H3)2–Cu(phen)] units (phen is 1,10‐phenanthroline), which are connected to neighbouring units through vanadyl bridges. Neighbouring chains have no covalent bonds between them, although they interdigitate through the phen groups viaπ–π interactions.  相似文献   

2.
Two copper‐containing compounds based on MoO42–, [Cu4(phen)42‐OH)23‐OH)2(H2O)2][MoO4]2 · 10H2O ( 1 ) and [Cu(phen)2Mo2O7(phen)] · 8H2O ( 2 ) (phen = 1,10‐phenanthroline), were hydrothermally synthesized. In the crystal lattices of 1 and 2 , discrete octameric water cycles and 2D layer water clusters were observed. The cyclic water octamer clusters exist stably in the channels constructed by [Cu4(phen)4(OH)4(H2O)2]2+ and MoO42– by hydrogen bonds in 1 at low temperature and 2D layer water clusters are formed by (H2O)16 units in 2 .  相似文献   

3.
New heteroatom polyoxovanadates (POVs) were synthesized by applying a water‐soluble high‐nuclearity cluster as new synthon. The [V15Sb6O42]6? cluster shell exhibiting D3 symmetry was in situ transformed into completely different cluster shells, namely, the α‐[V14Sb8O42]4? isomer with D2d and the β‐[V14Sb8O42]4? isomer with D2h symmetry. The solvothermal reaction of {Ni(en)3}3[V15Sb6O42(H2O)x] ? 15 H2O (x=0 or 1; en=ethylenediamine) in water led to the crystallization of [{Ni(en)2}2V14Sb8O42] ? 5.5 H2O containing the β‐isomer. The addition of [Ni(phen)3](ClO4)2 ? 0.5 H2O (phen=1,10‐phenanthroline) to the reaction slurry gave the new compound {Ni(phen)3}2[V14Sb8O42] ? phen ? 12 H2O with the α‐isomer. Both transformation reactions are complex due the change of symmetry, the chemical composition, and rearrangement of the VO5 square pyramids and Sb2O5 handle‐like moieties.  相似文献   

4.
Two novel polymers exhibiting metal–organic frameworks (MOFs) have been synthesized by the combination of a metal ion with a benzene‐1,3,5‐tricarboxylate ligand (BTC) and 1,10‐phenanthroline (phen) under hydrothermal conditions. The first compound, poly[[(μ4‐benzene‐1,3,5‐tricarboxylato‐κ4O:O′:O′′:O′′′)(μ‐hydroxido‐κ2O:O)bis(1,10‐phenanthroline‐κ2N,N′)dizinc(II)] 0.32‐hydrate], {[Zn2(C9H3O6)(OH)(C12H8N2)2]·0.32H2O}n, denoted Zn–MOF, forms a two‐dimensional network in which a binuclear Zn2 cluster serves as a 3‐connecting node; the BTC trianion also acts as a 3‐connecting centre. The overall topology is that of a 63 net. The phen ligands serve as appendages to the network and interdigitate with phen ligands belonging to adjacent parallel sheets. The second compound, poly[[(μ6‐benzene‐1,3,5‐tricarboxylato‐κ7O1,O1′:O1:O3:O3′:O5:O5′)(μ3‐hydroxido‐κ2O:O:O)(1,10‐phenanthroline‐κ2N,N′)dimanganese(II)] 1.26‐hydrate], {[Mn2(C9H3O6)(OH)(C12H8N2)]·1.26H2O}n, denoted Mn–MOF, exists as a three‐dimensional network in which an Mn4 cluster serves as a 6‐connecting unit, while the BTC trianion again plays the role of a 3‐connecting centre. The overall topology is that of the rutile net. Phen ligands act as appendages to the network and form the `S‐shaped' packing mode.  相似文献   

5.
The title complex, poly[di‐μ3‐oxo‐hepta‐μ2‐oxo‐tetra­oxo­bis(1,10‐phenanthroline)‐μ4‐terephthalato‐dicopper(II)­tetra­molybdate(VI)], [Cu2Mo4(C8H4O4)O13(C12H8N2)2], represents a novel two‐dimensional copper–molybdate compound with mixed ligands. Tetra­nuclear molybdenum oxide clusters are joined through corner‐sharing into a ribbon‐like chain, with [Cu(phen)]2+ (phen is 1,10‐phenanthroline) complexes grafted onto either side. The terephthalate ligand lies about an inversion centre and links these chains to form a layer via Cu—O and Mo—O bonds. Face‐to‐face π–π stacking inter­actions between adjacent phen ligands stabilize the structure.  相似文献   

6.
The X‐ray structure analysis of the title compound, chloro[1‐cyclopropyl‐6‐fluoro‐1,4‐dihydro‐4‐oxo‐7‐(piperazin‐4‐ium‐1‐yl)‐3‐quinolinecarboxylate‐κ2O3,O4](1,10‐phenanthroline‐κ2N,N′)copper chloride dihydrate, [CuCl(C17H18FN3O3)(C12H8N2)]Cl·2H2O or [CuCl(cfH)(phen)]Cl·2H2O, where cfH is 1‐cyclopropyl‐6‐fluoro‐1,4‐dihydro‐4‐oxo‐7‐(piperazin‐4‐ium‐1‐yl)‐3‐quinolinecarboxylate and phen is 1,10‐phenanthroline, shows that the geometry around the Cu ion is a slightly distorted square pyramid. Two O atoms of the carbonyl and carboxyl groups of ciprofloxacin and two N atoms of 1,10‐phenanthroline are coordinated to the metal centre in the equatorial plane, and a Cl ion is coordinated at the apical position. Extensive intermolecular hydrogen bonding produces a supramolecular structure that consists of alternating six‐ and 12‐membered rings.  相似文献   

7.
Reaction of O,O′‐diisopropylthiophosphoric acid isothiocyanate (iPrO)2P(S)NCS with 1,10‐diaza‐18‐crown‐6, 1,7‐diaza‐18‐crown‐6, or 1,7‐diaza‐15‐crown‐5 leads to the N‐thiophosphorylated bis‐thioureas N,N′‐bis[C(S)NHP(S)(OiPr)2]‐1,10‐diaza‐18‐crown‐6 ( H2LI ), N,N′‐bis[C(S)NHP(S)(OiPr)2]‐1,7‐diaza‐18‐crown‐6 ( H2LII ) and N,N′‐bis[C(S)NHP(S)(OiPr)2]‐1,7‐diaza‐15‐crown‐5 ( H2LIII ). Reaction of the potassium salts of H2LI–III with a mixture of CuI and 2,2′‐bipyridine ( bpy ) or 1,10‐phenanthroline ( phen ) in aqueous EtOH/CH2Cl2 leads to the dinuclear complexes [Cu2(bpy)2LI–III] and [Cu2(phen)2LI–III] . The structures of these compounds were investigated by 1H, 31P{1H} NMR spectroscopy, and elemental analysis. The crystal structures of H2LI and [Cu2(phen)2LI] were determined by single‐crystal X‐ray diffraction. Extraction capacities of the obtained compounds in comparison to the related compounds 1,10‐diaza‐18‐crown‐6, N,N′‐bis[C(=CMe2)CH2P(O)(OiPr)2]‐1,10‐diaza‐18‐crown‐6, N,N′‐bis[C(S)NHP(O)(OiPr)2]‐1,10‐diaza‐18‐crown‐6 towards the picrate salts LiPic, NaPic, KPic. and NH4Pic were also studied.  相似文献   

8.
Two cobalt phosphonates, [Co2(2,2′‐bpy)2(H2O)(pbtcH)] ( 1 ) and [Co2(H2O)(pbtcH)(phen)2] ( 2 ; pbtcH5=5‐phosphonatophenyl‐1,2,4‐tricarboxylic acid, 2,2′‐bpy=2,2′‐bipyridine, phen=1,10‐phenanthroline), with layer structures are reported. Compound 1 contains O‐C‐O and O‐P‐O bridged tetramers of Co4, which are further connected by pbtcH4? units to form a layer. In compound 2 , the cobalt tetramers made up of water‐bridged Co2 dimers and O‐P‐O linkages are connected into a layer by pbtcH4? units. Upon dehydration, compounds 1 and 2 experience single‐crystal‐to‐single‐crystal (SC–SC) structural transformations to form [Co2(2,2′‐bpy)2(pbtcH)] ( 1 a ) and [Co2(pbtcH)(phen)2] ( 2 a ), respectively. The process is reversible in each case. Notably, a breathing effect is observed for 1 , accompanied by pore opening and closing due to the reorientation of the coordinated 2,2′‐bpy molecules. The transformation was also monitored by in situ IR measurements. Magnetic studies reveal that antiferromagnetic interactions are mediated between the magnetic centers in compounds 1 and 1 a , whereas ferromagnetic interactions are dominant in compound 2 .  相似文献   

9.
The title compound, [CoCl(C12H8N2)2(H2O)]Cl·[CoCl2(C12H8N2)2]·6H2O, is the first example of a new 1:1 cocrystal of the octahedral [CoCl2(phen)2] and [CoCl(phen)2(H2O)]+·Cl complexes (phen is 1,10‐phenanthroline). The latter form heterochiral dimers held by strong π–π stacking interactions via their phenathroline ligands, which confirms that π stacking is an important and reliable synthon in supramolecular design. In addition, the crystal structure is networked by H2O...H2O, H2O...Cl and H2O...Cl hydrogen bonds, which interconnect the different units of the cobalt complexes.  相似文献   

10.
The α‐[P2W18O62]6–‐based coordination polymer [Cu2(phen)3(H2O)3(P2W18O62)][Cu(phen)2(H2O)] · 5H2O ( 1 ) (phen = phenanthroline), was hydrothermally synthesized and characterized by single‐crystal and powder X‐ray diffraction, IR and UV/Vis diffuse reflection spectroscopy, and elemental analysis. Structural studies reveal that compound 1 exhibits a three‐dimensional (3D) supramolecular structure based on π–π and hydrogen bonding interactions. In addition, visible light driven photocatalytic experiments of compound 1 were also studied.  相似文献   

11.
The blue tetranuclear CuII complexes {[Cu(bpy)(OH)]4Cl2}Cl2 · 6 H2O ( 1 ) and {[Cu(phen)(OH)]4(H2O)2}Cl4 · 4 H2O ( 2 ) were synthesized and characterized by single crystal X‐ray diffraction. ( 1 ): P 1 (no. 2), a = 9.240(1) Å, b = 10.366(2) Å, c = 12.973(2) Å, α = 85.76(1)°, β = 75.94(1)°, γ = 72.94(1)°, V = 1152.2(4) Å3, Z = 1; ( 2 ): P 1 (no. 2), a = 9.770(3) Å, b = 10.118(3) Å, c = 14.258(4) Å, α = 83.72(2)°, β = 70.31(1)°, γ = 70.63(1)°, V = 1252.0(9) Å3, Z = 1. The building units are centrosymmetric tetranuclear {[Cu(bpy)(OH)]4Cl2}2+ and {[Cu(phen)(OH)]4(H2O)2}4+ complex cations formed by condensation of four elongated square pyramids CuN2(OH)2Lap with the apical ligands Lap = Cl, H2O, OH. The resulting [Cu42‐OH)23‐OH)2] core has the shape of a zigzag band of three Cu2(OH)2 squares. The cations exhibit intramolecular and intermolecular π‐π stacking interactions and the latter form 2D layers with the non‐bonded Cl anions and H2O molecules in between (bond lengths: Cu–N = 1.995–2.038 Å; Cu–O = 1.927–1.982 Å; Cu–Clap = 2.563; Cu–Oap(OH) = 2.334–2.369 Å; Cu–Oap(H2O) = 2.256 Å). The Cu…Cu distances of about 2.93 Å do not indicate direct interactions, but the strongly reduced magnetic moment of about 2.74 B.M. corresponds with only two unpaired electrons per formula unit of 1 (1.37 B.M./Cu) and obviously results from intramolecular spin couplings (χm(T‐θ) = 0.933 cm3 · mol–1 · K with θ = –0.7 K).  相似文献   

12.
The title dinuclear complex, (aqua‐1κO)tetrakis(μ‐2,3‐diphenylprop‐2‐enoato‐1:2κ2O:O′)bis(2,3‐diphenylprop‐2‐enoato)‐1κO;2κO‐(ethanol‐2κO)bis(1,10‐phenanthroline)‐1κ2N,N′;2κ2N,N′‐dilanthanum(III), [La2(C15H11O2)6(C12H8N2)2(C2H5OH)(H2O)], contains two similar LaIII centres with distorted [LaO6N2] bicapped triganol–prismatic coordination polyhedra formed by six phenylcinnamate (PCA or 2,3‐diphenylprop‐2‐enoate) ligands, two 1,10‐phenanthroline (phen) ligands, a coordinating ethanol molecule and a coordinating water molecule. The two metal centres are bridged by four μ‐PCA ligands, with the remaining two PCA ligands coordinated in a monodentate fashion. The noncoordinated carboxylate O atoms on the terminal PCA ligands form O—H...O hydrogen bonds with the coordinated solvent molecules. Each La centre is also coordinated by a bidentate phen ligand. The PCA ligands all adopt synsyn orientations, with the two phenyl rings presenting dihedral angles of about 70°. The compound displays photochromic behaviour both in solution and in the solid state.  相似文献   

13.
《化学:亚洲杂志》2017,12(18):2441-2446
A flexible one‐pot strategy with pyramidal SeIV heteroatoms was employed for the assembly of the praseodymium‐containing gly‐decorated polyoxotungstate [{Pr3(H2O)10[Se2W22O76(gly)2]}2(Se2W7O30H2)]18− ( 1 a ), which is constructed from one {Se2W7O30H2} unit and two identical {Pr3(H2O)10[Se2W22O76(gly)2]} units. Furthermore, the catalytic performance of Cs2Na4H12[{Pr3(H2O)10[Se2W22O76(gly)2]}2(Se2W7O30H2)] ⋅ 25 H2O ( 1 ) for alkene epoxidation with hydrogen peroxide was investigated under mild reaction conditions, and the experimental results suggested that compound 1 exhibits good catalytic performance for the epoxidation of cyclooctene.  相似文献   

14.
The triply bridged title dinuclear copper(II) compound, [Cu2(C2H3O2)(OH)(C12H8N2)2(H2O)](NO3)2·H2O, (I), consists of a [Cu22‐CH3COO)(μ2‐OH)(phen)22‐OH2)]2+ cation (phen is 1,10‐phenanthroline), two uncoordinated nitrate anions and one water molecule. The title cation contains a distorted square‐pyramidal arrangement around each metal centre with a CuN2O3 chromophore. In the dinuclear unit, both CuII ions are linked through a hydroxide bridge and a triatomic bridging carboxylate group, and at the axial positions through a water molecule. The phenanthroline groups in neighbouring dinuclear units interdigitate along the [010] direction, generating several π–π contacts which give rise to planar arrays parallel to (001). These are in turn connected by hydrogen bonds involving the aqua and hydroxide groups as donors with the nitrate anions as acceptors. Comparisons are made with isostructural compounds having similar cationic units but different counter‐ions; the role of hydrogen bonding in the overall three‐dimensional structure and its ultimate effect on the cell dimensions are discussed.  相似文献   

15.
A Tri‐µ‐O‐S‐O coordinative manganese dimer: [Mn2(SO4)2(phen)4]·CH3OH (phen1,10‐phenanthroline) ( 1 ) was yielded by the reaction of 1,10‐phenanthroline and MnSO4·H2O in a mixed solvent of methanol and acetonitrile under room temperature and was structurally characterized. Single crystal analysis shows that complex 1 has polymeric structure based on binuclear Mn(II) units bridged by O‐S‐O groups of two SO42− anion. The UV spectrum of the complex clarifies that each metal‐organic building unit parallels with each other through the Π‐Π interactions of face‐to‐face separations of two 1,10‐phen planes among the complex, forming a layered structure. And the electronic paramagnetic resonance (EPR) signal clearly indicates that those manganese atoms in complex 1 are in +2 oxidation states.  相似文献   

16.
The title compound, {[Zn4(C8H4O4)3(OH)2(C12H6N2O2)2]·2H2O}n, has been prepared hydrothermally by the reaction of Zn(NO3)2·6H2O with benzene‐1,4‐dicarboxylic acid (H2bdc) and 1,10‐phenanthroline‐5,6‐dione (pdon) in H2O. In the crystal structure, a tetranuclear Zn4(OH)2 fragment is located on a crystallographic inversion centre which relates two subunits, each containing a [ZnN2O4] octahedron and a [ZnO4] tetrahedron bridged by a μ3‐OH group. The pdon ligand chelates to zinc through its two N atoms to form part of the [ZnN2O4] octahedron. The two crystallographically independent bdc2− ligands are fully deprotonated and adopt μ3‐κOO′:κO′′ and μ4‐κOO′:κO′′:κO′′′ coordination modes, bridging three or four ZnII cations, respectively, from two Zn4(OH)2 units. The Zn4(OH)2 fragment connects six neighbouring tetranuclear units through four μ3‐bdc2− and two μ4‐bdc2− ligands, forming a three‐dimensional framework with uninodal 6‐connected α‐Po topology, in which the tetranuclear Zn4(OH)2 units are considered as 6‐connected nodes and the bdc2− ligands act as linkers. The uncoordinated water molecules are located on opposite sides of the Zn4(OH)2 unit and are connected to it through hydrogen‐bonding interactions involving hydroxide and carboxylate groups. The structure is further stabilized by extensive π–π interactions between the pdon and μ4‐bdc2− ligands.  相似文献   

17.
The title coordination complex, [Ni(C14H14O2PS2)2(C12H8N2)] or [Ni(pMePh‐dtp)2(phen)] (phen is 1,10‐phenanthroline; dtp is di­aryl­di­thio­phosphate), has a non‐crystallographic twofold axis of symmetry through the Ni atom and the phen moiety. Two O,O‐di‐p‐tolyl­di­thio­phosphate (dtp) ions act as bidentate ligands. The central metal atom is coordinated by four S atoms from two dtp groups and two N atoms from the phen ligand. The title compound displays distorted octahedral geometry around the central Ni atom.  相似文献   

18.
Reactions of 1,10‐phenanthroline (phen) and 2‐(3,4‐dichlorophenyl)acetic acid (dcaH) with Mn(CO3) (M = LiI, NaI and MgII; n = 1 and 2) in MeOH yield the mononuclear lithium complex aqua[2‐(3,4‐dichlorophenyl)acetato‐κO](1,10‐phenanthroline‐κ2N,N′)lithium(I), [Li(C8H5Cl2O2)(C12H8N2)(H2O)] or [Li(dca)(phen)(H2O)] ( 1 ), the dinuclear sodium complex di‐μ‐aqua‐bis{[2‐(3,4‐dichlorophenyl)acetato‐κO](1,10‐phenanthroline‐κ2N,N′)sodium(I)}, [Na2(C8H5Cl2O2)2(C12H8N2)2(H2O)2] or [Na2(dca)2(phen)2(H2O)2] ( 2 ), and the one‐dimensional chain magnesium complex catena‐poly[[[diaqua(1,10‐phenanthroline‐κ2N,N′)magnesium]‐μ‐2‐(3,4‐dichlorophenyl)acetato‐κ2O:O′] 2‐(3,4‐dichlorophenyl)acetate monohydrate], {[Mg(C8H5Cl2O2)(C12H8N2)(H2O)2](C8H5Cl2O2)·H2O}n or {[Mg(dca)(phen)(H2O)2](dca)·H2O}n ( 3 ). In these complexes, phen binds via an N,N′‐chelate pocket, while the deprotonated dca? ligands coordinate either in a monodentate (in 1 and 2 ) or bidentate (in 3 ) fashion. The remaining coordination sites around the metal ions are occupied by water molecules in all three complexes. Complex 1 crystallizes in the triclinic space group P with one molecule in the asymmetric unit. The Li+ ion adopts a four‐coordinated distorted seesaw geometry comprising an [N2O2] donor set. Complex 2 crystallizes in the triclinic space group P with half a molecule in the asymmetric unit, in which the Na+ ion adopts a five‐coordinated distorted spherical square‐pyramidal geometry, with an [N2O3] donor set. Complex 3 crystallizes in the orthorhombic space group P212121, with one Mg2+ ion, one phen ligand, two dca? ligands and three water molecules in the asymmetric unit. Both dcaH ligands are deprotonated, however, one dca? anion is not coordinated, whereas the second dca? anion coordinates in a bidentate fashion bridging two Mg2+ ions, resulting in a one‐dimensional chain structure for 3 . The Mg2+ ion adopts a distorted octahedral geometry, with an [N2O4] donor set. Complexes 1 – 3 were evaluated against urease and α‐glucosidase enzymes for their inhibition potential and were found to be inactive.  相似文献   

19.
The title bimetallic compound, [Yb43‐OH)4(C6H13NO2)7(H2O)7][ZnCl4][ZnCl3(OH)]Cl4·8H2O, was synthesized at near physiological pH (6.0). The compound exhibits some novel structural features, including an asymmetric [Yb43‐OH)4(l ‐leucine)7(H2O)7]8+ complex cation in which four OH groups act as bridging ligands, linking four Yb3+ cations into a Yb4O4 structural unit. Each pair of adjacent Yb3+ ions is further bridged by one carboxy group from a leucine ligand. Water mol­ecules and a monodentate leucine ligand also coordinate to Yb3+ ions, completing their eight‐coordinate square‐antiprismatic coordination. The Yb43‐OH)4(l ‐leu­cine)7(H2O)7]8+ cation, the [ZnCl4]2−, [ZnCl3OH]2− and Cl anions, and the lattice water mol­ecules are linked via hydrogen bonds.  相似文献   

20.
Metalat Ions [Al(OR)4] as Chelating Ligands for Transition Metal Cations Waterfree CoCl2 can be reacted with [{Li(Diglyme)}{Al(OtBu)4}] in THF to the complex [Li(THF)4][{CoCl2}{Al(OtBu)4}]. Addition of diglyme to the reaction mixtures gives the blue compound [Li(diglyme)2][{CoCl2}{Al(OtBu)4}] ( 1 ). According to this procedure the FeII complex [Li(Diglyme)2][{FeCl2}2{Al(OtBu)4}] ( 2 ) was formed by treatment of FeCl2 with Li[Al(OtBu)4]. [{Li(diglyme)}{Al(OtBu)4}] in THF/diglyme can be used as alkoxide transfer reagent on TiCl4 to give the neutral complex [TiCl2(OtBu)2(diglyme)] ( 3 ). The sky‐blue salt [Li(THF)4]2[{CoCl2}3{Al(OCH2Ph)4}2] ( 4 ) was obtained by reaction of Li[Al(OCH2Ph)4] with CoCl2 in THF. By treatment of 4 with diglyme ligand redistribution was observed giving the sky‐blue compound [Li(Diglyme)2]2[{CoCl2}3{Al(OCH2Ph)4}2] ( 5 ) and the violet salt [Li(Diglyme)2]2[Co2Cl5(OCH2Ph)] ( 6 ). A similar salt can be synthesized also directly from Li[Al(OtBu)4] and CoCl2 in diglyme to give [Li(Diglyme)2]2[Co2Cl5(OtBu)] ( 7 ). 1 — 7 were characterized by IR spectroscopy, partly by mass spectrometry and X‐ray analyses. UV‐VIS spectra were recorded from 1 and 5 . According to the X‐ray analyses the MII ions as well as the AlIII ions are coordinated distorted tedrahedrally. In 1 , 2 , 4 und 5 the unit [Al(OR)4] acts a chelating ligand as desired.  相似文献   

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