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1.
A new ruthenium(II) complex [Ru(NO2)4(CO)(H2O)]Cl2 · 2H2O has been prepared and characterized structurally. The compound crystallizes in monoclinic space group C2 /m, with the unit cell parameters a = 12.913(2), b = 14.605(2), c = 7.4494(1)Å, ß =121.49(2)°; V = 1198.0(3)Å3, Z = 4, Dc = 2.429 Mgm—3; μ = 1.83 mm—1; R = 0.0455, wR = 0.1552. The complex contains four neutral NO2 ligands. The ruthenium atom is six‐coordinated to four nitrogen atoms of nitrogen dioxide, one carbon atom from carbon monoxide and one oxygen atom from water molecule, forming slightly distorted octahedral coordination. The preparation procedure has been discussed.  相似文献   

2.
The yellow‐orange crystals of [Pt(Hmimt)4](NO3)2 [Hmimt = 1‐methyl‐2(3H)‐imidazolinethione] are monoclinic [P21, a = 8.136(3), b = 13.978(4), c = 12.150(9)Å, β = 96.89(5)°]. They consist of [Pt(Hmimt)4]2+ cations and nitrate anions. In the cation the Pt atom is coordinated by four S atoms [Pt‐S: 2.291(5)‐2.357(5)Å] in a slightly distorted square planar arrangement.  相似文献   

3.
Crystalline NO[Mn(NO3)3] ( I ) and (NO)2[Co(NO3)4] ( II ) were synthesized by reaction of the corresponding metal and a liquid N2O4/ethylacetate mixture. I is orthorhombic, Pca21, a = 9.414(2), b = 15.929(3), c = 10.180(2) Å, Z = 4, R1 = 0.0286. II is monoclinic, C2/c, a = 14.463(3), b = 19.154(4), c = 13.724(3) Å, β = 120.90(3), Z = 12, R1 = 0.0890. Structure I consists of [Mn(NO3)3] sheets with NO+ cations between them. Two types of Mn atoms have CNMn = 7 and 8. Structure II is ionic containing isolated [Co(NO3)4]‐anions and NO+ cations with CNCo = 8. Crystals of Mn(NO3)2 ( III ) and Co(NO3)2 ( IV ) were obtained by concentration of metal nitrate hydrate solutions in 100% HNO3 in a desiccator with P2O5. III is cubic, Pa 3, a = 7.527(2) Å, Z = 4, R1 = 0.0987. IV is trigonal, R 3, a = 10.500(2), c = 12.837(3) Å, Z = 12, R1 = 0.0354. The three dimensional structure III is isotypic to the strontium and barium dinitrates. Structure IV contains a three dimensional network of interconnected Co(NO3)6/3 units with a distorted octahedral coordination environment of Co atoms. General correlations between central atom coordination and coordination modes of NO3 groups are discussed.  相似文献   

4.
The reaction of PhN3(H)C6H4N3(H)Ph with Hg(NO3)2 in THF in the presence of triethylamine yields {Hg[PhN3C6H4N3(H)Ph](NO3)} as a yellow powder that can be recrystallized from THF/acetone. The crystals belong to the monoclinic system, space group P21 with the cell dimensions a = 9.639(2), b = 5.412(1), c = 19.675(4) Å, β= 97.47(3)°, V = 1017.7 (4) Å3, Z = 2. The crystal structure determination (2668 unique reflections with [I>2σ(I)], 262 parameters, R1 = 0.0393) shows that the structure consists of mononuclear complexes. Hg atoms are linearly coordinated by one Nα atom of the triazenide unit of the planar ligand [Hg‐N(1) = 2.101(8) Å] and an O atom of the NO3 ion [Hg‐O(1) = 2.11(1) Å]. Additional weak Hg‐N contacts [Hg‐N(4) = 2.662(9) and Hg‐N(3) = 2.851(9) Å] and an intramolecular hydrogen bond between the triazenide hydrogen and an O atom of the nitrate group are observed [N(6)‐H(6)···O(2) = 2.92(2) Å]. The complexes are stacked to infinite chains by metal‐arene π‐interactions. Each Hg atom is coordinated by the terminal phenyl rings of two neighboring complexes [Hg‐C from 3.40(1) to 4.10(1) Å] in a η2 fashion.  相似文献   

5.
Four Schiff base complexes, [Cu2(L1)2(μ‐NCS)2] ( 1 ), [Cu2(L2)2(μ‐N3)2] ( 2 ), Cu[Cu(CH3COO)(L3)]2 ( 3 ), and [Zn{Zn(C3H4N2)(L3)}2(NO3)](NO3) ( 4 ) (where L1 = 2‐[(pyridin‐2‐ylmethylimino)methyl]phenol, L2 = 1‐[(pyridin‐2‐ylmethylimino)methyl]naphthalen‐2‐ol, and L3 = bis(salicylidene)‐1, 3‐propanediamine), were synthesized and characterized by elemental analyses, infrared spectroscopy, and single crystal X‐ray determinations. Both 1 and 2 are structurally similar di‐nuclear complexes, which are located at crystallographic inversion centers (with the center of the central Cu2N2 ring). In 1 , each copper atom has a slightly distorted square pyramidal configuration, coordinated by two nitrogen atoms and one oxygen atom from L1 and another two terminal nitrogen atoms from two bridging thiocyanate anions. The Cu···Cu separation is 3.466(3) Å. The structure of 2 is similar to that of 1 , with Cu···Cu separation of 3.368(2) Å. Both 3 and 4 are linear tri‐nuclear complexes. In 3 , the central Cu2+ ion is located on an inversion centre and has a distorted octahedral coordination involving four bridging O atoms from two Schiff base ligands (L3) in the equatorial plane and one O atom from each bridging acetate group in the axial positions. The coordination around the terminal Cu2+ ions is irregular‐square pyramidal, with two O and two N atoms of L3 in the basal plane and one O atom from an acetate group in the apical position. The acetate bridges linking the central and terminal Cu2+ ions are mutually trans. The Cu···Cu separation is 3.009(3) Å. In 4 , the coordination configuration of the central and the terminal zinc atoms are similar to that of the 3 , with Zn···Zn separation of 3.153(4) Å. The three Schiff bases and the corresponding three copper complexes exhibit good antibacterial properties, while the zinc complex 4 has nearly no.  相似文献   

6.
The title salt, methyl (1R,2R,3S,5S,8S)‐3‐benzoyl­oxy‐8‐methyl‐8‐aza­bicyclo­[3.2.1]octane‐2‐carboxyl­ate tetra­chloro­aurate(III), (C17H22NO4)[AuCl4], has its protonated N atom intra­molecularly hydrogen bonded to the O atom of the methoxy­carbonyl group [N⋯O = 2.755 (6) Å and N—H⋯O = 136°]. Two close inter­molecular C—H⋯O contacts exist, as well as five C—H⋯Cl close contacts. The [AuCl4] anion was found to be distorted square planar.  相似文献   

7.
The complexes [Cu(dpp)Br2] ( 1 ) and [Cu(dpp)2][CuBr2] ( 2 ) (dpp = 2,9‐diphenyl‐1,10‐phenanthroline) were synthesized and characterized by single‐crystal X‐ray diffraction methods. Reaction of copper(II) bromide with the dpp ligand in dichloromethane at room temperature afforded 1 , which is a rare example of non‐square planar four‐coordinate copper(II) complexes. Complex 1 crystallizes in the monoclinic space group C2/c with a = 15.352(3), b = 13.192(3), c = 11.358(2) Å, β = 120.61(3)°, V = 1979.6(7) Å3, Z = 4, Dcalc = 1.865 g cm?3. The coordination geometry about the copper center is distorted about halfway between square planar and tetrahedral. The Cu‐N distance is 2.032(2) Å and the Cu‐Br distance 2.3521(5) Å. Heating a CH2Cl2 or acetone solution of 1 resulted in complex 2 , which consists of a slightly distorted tetrahedral [Cu(dpp)2]+ cation and a linear two‐coordinate [CuBr2]? anion. 2 crystallizes in the triclinic space group with a = 10.445(2), b = 11.009(2), c = 18.458(4) Å, α = 104.72(3), β = 94.71(3), γ = 103.50(3)°, V = 1973.3(7) Å3, Z = 2, Dcalc = 1.602 g cm?3. The four Cu(1)‐N distances are between 2.042(3) and 2.067(3) Å, the distance of Cu(2)‐Br(1) 2.2268(8) Å, and the disordered Cu(3)‐Br(2) distances are 2.139(7) and 2.237(4) Å, respectively. Complex 2 could also be prepared by directly reacting CuBr with dpp in CH2Cl2.  相似文献   

8.
The β‐diketone 3‐(4‐cyano­phenyl)­pentane‐2,4‐dione crystallizes as the enol tautomer 4‐(2‐hydroxy‐4‐oxopent‐2‐en‐3‐yl)­benzo­nitrile, C12H11NO2, (I), with an intramolecular O—H⋯O hydrogen bond [O⋯O = 2.456 (2) Å]. Reaction of (I) with copper acetate monohydrate in the presence of triethyl­amine leads to the formation of the copper(II) complexbis­[3‐(4‐cyano­phenyl)­pentane‐2,4‐dionato‐κ2O,O]copper(II), [Cu(C12H10NO2)2], (II). In the structure of (II), the Cu atom is coordinated by four β‐diketonate O atoms in a slightly distorted square‐planar geometry, with Cu—O distances in the range 1.8946 (11)–1.9092 (11) Å. The nitrile moieties in (II) make it a candidate for reaction with other metal ions to produce supramolecular structures.  相似文献   

9.
Two first uranyl chromate nitrates, K[(UO2)(CrO4)(NO3)] ( 1 ) and Rb[(UO2)(CrO4)(NO3)] ( 2 ), were prepared by solid‐state reactions and characterized by electron microprobe analysis and single‐crystal X‐ray diffraction. The compounds are isotypic [ 1 : monoclinic, P21/c, a = 9.881(5), b = 7.215(4), c = 14.226(6) Å, β = 124.85(3)°, V = 832.3(7) Å3; 2 : monoclinic, P21/c, a = 9.804(1), b = 7.359(1), c = 14.269(1) Å, β = 122.048(4), V = 872.6(1) Å3]. The structures of 1 and 2 are based upon the complex [(UO2)(CrO4)(NO3)] layers with unprecedented structural topology, which consist of the UrO3NO3 units linked through CrO4 tetrahedra. The resulted kinked layer can be divided into chains arranged in the ladder fashion. The layers are parallel to (100) and are linked by A+ (A = K, Rb) cations located between the layers.  相似文献   

10.
In the title compound, 4‐iodoanilinium 2‐carboxy‐6‐nitrobenzoate, C6H7IN+·C8H4NO6, the anions are linked by an O—H...O hydrogen bond [H...O = 1.78 Å, O...O = 2.614 (3) Å and O—H...O = 171°] into C(7) chains, and these chains are linked by two two‐centre N—H...O hydrogen bonds [H...O = 1.86 and 1.92 Å, N...O = 2.700 (3) and 2.786 (3) Å, and N—H...O = 153 and 158°] and one three‐centre N—H...(O)2 hydrogen bond [H...O = 2.02 and 2.41 Å, N...O = 2.896 (3) and 2.789 (3) Å, N—H...O = 162 and 105°, and O...H...O = 92°], thus forming sheets con­taining R(6), R(8), R(13) and R(18) rings.  相似文献   

11.
The phosphorus‐sulfur ligand 1‐(methylthio)‐3‐(diphenylphosphino)‐propane (S‐P3) has been synthesized and characterized by 1H NMR and 13C NMR. Reactions of S‐P3 with [PdCl2(PhCN)2] afforded the complexes [PdCl2(S‐P3)] ( I ) and [PdCl2(S‐P3)2] ( II ), in which S‐P3 acts as a bidentate and monodentate ligand, respectively. Compound I crystallizes in monoclinic space group P21/n (No. 14) with cell dimensions: a = 8.589(3), b = 15.051(3), c = 17.100(3)Å, β = 102.91(2)°, V = 2154.7(9)Å3, Z = 4. Likewise, compound II crystallizes in monoclinic space group P21/n (No. 14) with a = 9.993(5), b = 8.613(4), c = 18.721(5)Å, β = 90.18(3)°, V = 1611.3(12)Å3, Z = 2. Compound II has a trans square planar configuration with only the P‐site of the ligand bonded to the palladium atom.  相似文献   

12.
In bis­[1‐(3‐pyridyl)butane‐1,3‐dionato]copper(II) (the Cu atom occupies a centre of inversion), [Cu(C9H8NO2)2], (I), and bis­[1‐(4‐pyridyl)butane‐1,3‐dionato]copper(II) methanol solvate, [Cu(C9H8NO2)2]·CH3OH, (II), the O,O′‐chelating diketonate ligands support square‐planar coordination of the metal ions [Cu—O = 1.948 (1)–1.965 (1) Å]. Weaker Cu⋯N inter­actions [2.405 (2)–2.499 (2) Å], at both axial sides, occur between symmetry‐related bis­(1‐pyridylbutane‐1,3‐dion­ato)copper(II) mol­ecules. This causes their self‐organization into two‐dimensional square‐grid frameworks, with uniform [6.48 Å for (I)] or alternating [4.72 and 6.66 Å for (II)] inter­layer separations. Guest methanol mol­ecules in (II) reside between the distal layers and form weak hydrogen bonds to coordinated O atoms [O⋯O = 3.018 (4) Å].  相似文献   

13.
The self‐assembly of 4 ‐ MTPP [ 4 ‐ MTPP = 2‐(methylthio)‐4‐(pyridin‐4‐yl)pyrimidine] with Cu(NO3)2 and AgNO3 was structurally investigated. For Cu(NO3)2, a discrete mononuclear CuII coordination compound, [Cu( 4 ‐ MTPP )2(NO3)2] ( 1 ), resulted that is exclusively based on Cu–N coordination. For AgNO3, a unique one‐dimensional double‐chain structure ( 2 ) was obtained with the Ag–N distances varying from 2.181(9) to 2.223(9) Å, and the average Ag–S distance being 2.98 Å. Compared to zero‐dimensional 1 , the extension to one‐dimensional 2 is considered to result from the specific affinity between Ag+ and the ligand 4 ‐ MTPP that is attributed to the strong coordinating tendency of silver for aromatic nitrogen and thioether sulfur atoms.  相似文献   

14.
Single crystals of γ‐K(UO2)(NO3)3 were prepared from aqueous solutions by evaporation. The crystal structure [orthorhombic, Pbca (61), a = 9.2559(3) Å, b = 12.1753(3) Å, c = 15.8076(5) Å, V = 1781.41(9) Å3, Z = 8] was determined by direct methods and refined to R1 = 0.0267 on the basis of 3657 unique observed reflections. The structure is composed of isolated anionic uranyl trinitrate units, [(UO2)(NO3)3], that are linked through eleven‐coordinated K+ cations. Both known polymorphs of K(UO2)(NO3)3 (α‐ and γ‐phases) can be considered as based upon sheets of isolated complex [(UO2)(NO3)3] ions separated by K+ cations. The existence of polymorphism in the two K[UO2(NO3)3] polymorphs is due to the different packing modes of uranyl trinitrate clusters that adopt the same two‐dimensional but different three‐dimensional arrangements.  相似文献   

15.

The complex [Cu(l-Leu)(phen)(H2O)]NO3 has been synthesized and characterized by elemental analysis, molar conductivity, spectroscopic and X-ray diffraction methods, where phen = 1,10-phenanthroline and l-Leu = l-leucinate. The complex crystallizes in the triclinic space group Pī with two molecules in a unit cell of dimensions a = 7.288(4) Å, b = 11.588(7) Å, c = 12.349(3) Å, α = 86.388(10)o, β = 76.175(11)°, γ = 72.132(3)°, V = 963.8(10) Å3, Z = 2, D c = 1.564 g/cm3, μ = 1.177 mm?1, F(000) = 470, R 1 = 0.0611, and wR 2 = 0.0711. The copper(II) is ligated in a distorted square-pyramidal geometry by the two nitrogen atoms of phen and the amino nitrogen atom and one carboxylate oxygen atom from each independent l-Leu moiety in the basal plane, and one water oxygen at the apical position. A supramolecular configuration is formed from strong phen-phen stacking interactions between neighboring [Cu(l-leu)(phen)(H2O)]+cations in the crystal.  相似文献   

16.
A novel coordination compound tris[(2.2.2-cryptand)(nitrato-O,O′)lead(II)] pentakis(nitrato-O, O′)lead(II), 3[Pb(NO3)(Crypt-222)]+·[Pb(NO3)5]3? (I) has been prepared and studied by the single crystal X-ray diffraction technique. The crystals of I are monoclinic: space group Pc, a = 25.944 Å, b = 18.389 Å, c = 17.145 Å, β = 93.33°, Z = 4. The structure of I has been solved by the direct and heavy atom methods and refined in a full-matrix anisotropic-isotropic approximation to R = 0.122 for the total of 11145 measured reflections (automated diffractometer CAD-4, λMoK α). The structure of I includes six independent host-guest complex cations [Pb(NO3)(Crypt-222)]+ and two independent complex anions [Pb(NO3)5]3?. Coordination number of the cation Pb2+ equals ten in all these complex ions, and its coordination polyhedron in the first of them is a strongly distorted “hexagonal bipyramid” with two forked vertices, while for the latter ones it is a strongly distorted “square pyramid” with all five vertices forked.  相似文献   

17.
Single crystals of the hitherto unknown compound Hg2(OH)(NO3)·HgO were obtained unintentionally during hydrothermal phase formation experiments in the system Ag—Hg— As—O. Hg2(OH)(NO3)·HgO (orthorhombic, Pbca, Z = 8, a = 6.4352(8), b = 11.3609(14), c = 15.958(2) Å, 1693 structure factors, 83 parameters, R1[F2 > 2σ(F2)] = 0.0431) adopts a new structure type and is composed of two types of mercury‐oxygen zig‐zag‐chains running perpendicular to each other and of intermediate nitrate groups. One type of chains runs parallel [010] and consists of (Hg—Hg—OH) units with a typical Hg—Hg distance of 2.5143(10) Å for the mercury dumbbell, whereas the other type of chains runs parallel [100] and is made up of (O—Hg—O) units with short Hg—O distances of about 2.02Å. Both types of chains are concatenated by a common O atom with a slightly longer Hg—O distance of 2.25Å. The three‐dimensional assembly is completed by nitrate groups whose O atoms show Hg—O distances > 2.80Å. Weak hydrogen bonding between the OH group and one oxygen atom belonging to the nitrate group stabilizes this arrangement. Hg2(OH)(NO3)·HgO decomposes above 200 °C to HgO.  相似文献   

18.
In catena‐poly­[[(di‐2‐pyridyl­amine‐κ2N,N′)silver(I)]‐μ‐nico­tinato‐κ2N:O], [Ag(C6H4NO2)(C10H9N3)]n, the AgI atom is tetracoordinated by two N atoms from the di‐2‐pyridyl­amine (BPA) ligand [Ag—N = 2.3785 (18) and 2.3298 (18) Å] and by one N atom and one carboxyl­ate O atom from nicotinate ligands [Ag—N = 2.2827 (15) Å and Ag—O = 2.3636 (14) Å]. Bridging by nicotinate N and O atoms generates a polymeric chain structure, which extends along [100]. The carboxyl O atom not bonded to the Ag atom takes part in an intrachain C—H⋯O hydrogen bond, further stabilizing the chain. Pairs of chains are linked by N—H⋯O hydrogen bonds to generate ribbons. There are no π–π interactions in this complex. In catena‐poly­[[(di‐2‐pyridyl­amine‐κ2N,N′)silver(I)]‐μ‐2,6‐di­hydroxy­benzoato‐κ2O1:O2], [Ag(C7H5O4)(C10H9N3)]n, the AgI atom has a distorted tetrahedral coordination, with three strong bonds to two pyridine N atoms from the BPA ligand [Ag—N = 2.286 (5) and 2.320 (5) Å] and to one carboxyl­ate O atom from the 2,6‐di­hydroxy­benzoate ligand [Ag—O = 2.222 (4) Å]; the fourth, weaker, Ag‐atom coordination is to one of the phenol O atoms [Ag⋯O = 2.703 (4) Å] of an adjacent moiety, and this interaction generates a polymeric chain along [100]. Pairs of chains are linked about inversion centers by N—H⋯O hydrogen bonds to form ribbons, within which there are π–π interactions. The ribbons are linked about inversion centers by pairs of C—H⋯O hydrogen bonds and additional π–π interactions between inversion‐related pairs of 2,6‐di­hydroxy­benzoate ligands to generate a three‐dimensional network.  相似文献   

19.
The self‐assembly of 1, 0‐phenanthroline (phen) and 1,2,4,5‐benzenetetracarboxylic acid(H4btc) with Ca(NO3)2 gives rise to a two‐dimensional network structure coordination polymer, [Ca(phen)(btc)0.5(H2O)] ( 1 ), which was characterized by elemental analysis, IR spectroscopy, and single‐crystal X‐ray diffraction. This compound is monoclinic, space group C2/c, with Z = 8 in a unit cell with dimensions a = 21.744(3) Å, b = 10.0151(12) Å, c = 14.7122(17) Å, β = 110.2850(10)°. The structure contains one crystallographic unique CaII atom, one phen coordinated molecule and a half of btc4– anion. The phen molecule acts as a didentate ligand chelating with a CaII atom, whereas the btc4– anion acts as a μ6‐bridge linking six different CaII atoms to form a two‐dimensional network with (4, 4) topological structure. The three dimensional stacking structures are formed by C–H ··· O hydrogen bonding and π–π interaction. The thermal stability and fluorescent properties of 1 were investigated. Calcite particles are produced by calcination of compound 1 at 580 °C. The obtained calcite was characterized by XRD and SEM analyses.  相似文献   

20.
A novel La( III )‐Cu( II ) heterometallic coordination polymer {[LaCu2(NTA)2(4,4′‐bpy)(H2O)3]NO3·5H2O]n, where H3NTA denotes nitrilotriacetic acid and 4,4′‐bpy denotes 4, 4‐bipyridine, was synthesized and characterized by IR spectrum, elemental analysis and X‐ray diffraction. The complex crystallizes in the triclinic space group Pi with cell parameters a = 1.33710(10) nm, b = 1,44530(10) nm, c =1.0949(2) nm, α = 71.905(7)°, β = 74.327(7)°, γ = 64.427(9)°, V = 1.7912(4) nm3and Z = 2. It consists of heterometallic units, in which each La( II ) ion is coordinated in a distorted monocapped square antiprism by three oxygen atoms from water molecules and six carboxyl oxygen atoms from five NTA3? ions, and each Cu( I ) ion is coordinated by one nitrogen atom from 4,4′‐bpy and one nitrogen atom, three oxygen atoms from NTA3?. In the title complex, La( I ) ions and Cu( II ) ions are connected by the heterometallic bridging of NTA3?, constructing a two‐dimensional network structure along the [110]. And it is extended into an infinite three‐dimensional network structure by the formation of homometallic bridging of Cu‐4, 4′‐bpy‐Cu, exhibiting a certain inclusion ability.  相似文献   

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