A novel complex, namely [RuII(PPh3)(CO)(H)(Hbpdc)]·2MeOH ( 1 ) (H2bpdc = 2,2′‐bipyridyl‐5,5′‐dicarboxylic acid), has been synthesized from the reaction of H2bpdc with [RuII(PPh3)3(CO)(H)2] in methanol under mild condition and characterized by elemental analysis, IR spectrum, ESI mass spectrometry, and single crystal X‐ray diffraction. The structure shows that the complex crystallizes in the monoclinic space group P21/c with unit cell parameters a = 11.8984(13) Å, b = 16.5180(18) Å, c = 25.5322(19) Å, β = 115.302(4)°, V = 4536.6(8) Å3, Z = 4. This compound features a 1‐D supramolecular chain constructed via hydrogen bonds. Its photophysical properties have been investigated in MeOH solution and in the solid state at room temperature. 相似文献
The structure of the title complexes [Cu(AFO)2(H2O)2](ClO4)2.2(AFO).2H2O (AFO = 4,5‐Diazafluoren‐9‐one)has been established by single‐crystal X‐ray diffraction. The complex crystallizes in the triclinic space group P‐1 with cell constants a = 7.659(3) Å, b = 11.066(3) Å, c = 14.203(5) Å, alpha = 75.16(3)°, β = 79.87(3)°, gamma = 85.71(3)°, Z = 1. The structure was solved by direct methods and refined to R1 = 0.0595 (wR2 = 0.1164). The X‐ray analysis reveals that a pair of AFO ligands chelate to a Cu(II) atom in an asymmetric fashion with one Cu‐N bond being much longer than the other, the Cu(II) atom is further coordinated by a pair of aqua ligands to form an elongated octahedral geometry. In the crystal of the complex, the mononuclear complex cations [Cu(AFO)2(H2O)2]2+, uncoordinated AFO molecules, lattice water molecules and perchlorate anions are assembled into 3‐D structure via hydrogen bonds and π‐π stacking interaction. 相似文献
The crystal structure of Li2MgSiO4 was established by single-crystal X-ray diffraction analysis. The crystals are monoclinic, a = 4.9924(7) Å, b = 10.681(2) Å, c = 6.2889(5) Å, β = 90.46(1)°, Z = 4, sp. gr. P21/n, V = 335.54 Å3, R = 0.062. In a Li2MgSiO4 crystal, four types of independent T(1–4) tetrahedra share vertices to form a three-dimensional framework. Three of these tetrahedra are occupied simultaneously by Li and Mg cations, which corresponds to the crystallochemical formula (Li0.98Mg0.02)(Li0.80Mg0.20) · (Li0.22Mg0.78)SiO4. In slightly distorted SiO4 tetrahedra denoted as T(1), the average Si-O distance is 1.635(2) Å. The distortions of other tetrahedra and the average (LixMg1 ? x)-O distances increase with an increase in lithium content. These distances in the T(2), T(3), and T(4) tetrahedra are 1.955(2), 1.971(4), and 2.019(6) Å, respectively. The structure of the new compound is compared with the crystal structures of other Li2M2+SiO4 compounds and the luminescence spectra of Cr4+: Li2MgSiO4. 相似文献
(I) Mg2C20H24O18 monoclinic,PT,a=10.760(2) Å,b=11.052(2) Å,c=12.822(3) Å, α=105.31(3)o, β=98.18(3)o, γ=91.59(3)o,Z=2. (II) MgC10H14O10, monoclinic,C2/c,a=30.817(6)Å,b=10.499(2)Å,c=9.000(2)Å, β=91.31(3)o,Z=8. Magnesium in complexes with furoic acids reveals two ways of coordination: direct, when furoic anions are bonded to Mg2+ in an ionic fashion and outer-sphere, when cations bind water in the first coordination sphere and furancarboxylic ligands are hydrogen bonded to the water molecules. This results in the formation of three bridging systems: ?Mg?Ocarboxyl?C?Ocarboxyl?Mg?, ?Mg?Owater ?Ocarboxyl?C?Ocarboxyl?C?Ocarboxyl?Mg?, and ?Mg?Owater?Ocarboxyl?C?Ocarboxyl?Owater?Mg?. Magnesium 2-furancarboxylate (I) is dimeric, while magnesium 3-furancarboxylate (II) exhibits a polymeric structure. 相似文献
The title compound has been synthesized and its crystal structure determined at room temperature. Cd2(Sacch)4(Im)4 F.W. = 1225.83, monoclinic. Space group: C2/c, Z = 4, a = 20.065(3) Å, b = 11.164(4) Å, c = 20.697(6) Å, β = 94.69(5)°, The coordination polyhedron of Cd(II) correspond to a five-coordinate trigonal-bipyramid. In the title complex, two of the saccharin groups act as monodentate ligands. The other two act as bidentate ligands. The two Cd(II) ions are bridged by the two bidentate saccharin groups and the distance is 4.75 Å. 相似文献
Series of mixed valence monophosphates AFe3‐xMgx(PO4)3 [A = Sr(x = 0), Ba(x = 0.6), Pb(x = 0.6)] were synthesized by mild hydrothermal treatment at 210 °C. Refinements of single crystal X‐ray diffraction datas show all these compounds are isostructural. The attempts to make AFe3(PO4)3 (A = Ba, Pb) hydrothermally in the experiment were unsuccessful. However, the Mg‐doped homologues AFe2.4Mg0.6(PO4)3 (A = Ba, Pb) were synthesized with the addition of MgCO3 in the reactants as mineralizer. EDS and single crystal X‐ray data refinement indicated that the Mg2+ cations were doped in the Fe2+ sites of AFe2.4Mg0.6(PO4)3 (A = Ba, Pb). The influence of the Mg‐doping on the structure and the reason why the Mg doped in the Fe(II) site instead of A site was discussed from the point of view of the bond valence model. 相似文献
Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate was synthesized from ethyl 6-(4-bromophenyl)-4-(4-fluorophenyl)-2-oxocyclohex-3-ene-1-carboxylate and ammonium acetate in glacial acetic acid. The synthesized compound was characterized by elemental analysis, FT-IR, thermogravimetric analysis (TGA), differential thermal analysis (DTA), UV-Visible, and single-crystal X-ray diffraction. The title compound, ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate, C21H2OFNO2, crystallizes in the orthorhombic space group Pbca with the following unit-cell parameters: a = 17.417(2), b = 9.7287(9), c = 21.014(2) Å, and Z = 8. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0644 for 1616 observed reflections. An intramolecular N–H…O hydrogen bond generates an S(6) graph-set motif. In the crystal, molecules are linked by N–H…O hydrogen bonds, forming a two-dimensional network. 相似文献
Trans‐bis(ethanolamine)bis(saccharinato)mercury(II), [Hg(ea)2(sac)2], where ea and sac denote the ethanolamine molecule and the saccharinate anion, respectively, crystallizes in the triclinic space group P (No. 2) with a = 9.4651 (5), b = 10.4365 (5), c = 11.9314 (6) Å, α = 84.402 (1)° β = 78.313 (1)°, γ = 75.307 (1)°, Z = 2, V = 1115.11 (10) Å3. The structure consists of isolated [Hg(ea)2(sac)2] units in which the Hg(II) ion is octahedrally coordinated by two nitrogen and two oxygen atoms of two neutral ea ligands, and two nitrogen atoms of two sac ligands. The ea acts as a bidentate N‐ and O‐donor ligand and occupies the trans positions of the equatorial plane of the coordination octahedron forming a fivemembered chelate ring, while sac behaves as a monodentate N‐donor ligand occupying the axial positions. The average Hg‐Nsac and Hg‐Nea bond distances are 2.739 (3) and 2.114 (7) Å, respectively. The crystal exhibits extensive hydrogen bonds between the hydroxyl and amine hydrogen atoms of the ea ligands and the sulfonyl, carbonyl and amine groups of the sac ligands. 相似文献
A new complex phosphate Li5Cu2Al(PO4)4 has been obtained by the flux method in the Cs-Li-Cu-V-P-O system. Its crystal structure has been determined by X-ray diffraction (R1 = 2.74%) to be as follows: sp. gr. $P\bar 1$, a = 4.860(5) Å, b = 7.788(5) Å, c = 8.324(5) Å, α = 69.542(5)°, β = 90.016(5)°, γ = 75.318(5)°, Z = 1, and V = 284.2(4) Å3. The compound under study has a dense structure and a three-dimensional framework build up of [LiO5], [AlO6], [Cu/LiO5], and [CuO4] polyhedra and [PO4] tetrahedra. A comparative crystal-chemical analysis of two isotypic compounds with a general formula Li5Cu2M(PO4)4 (M = Fe, Al) has been performed. Topological relations between the Na2Mg5(PO4)4 and Li5Cu2M(PO4)4 crystal structures, which are characterized by different cationic compositions, are revealed. 相似文献
The title compound is (μ-H)Ru3(CO)7(μ-As(C6H5)CH2As(C6H5)2)((C6H5)2 AsCH2As(C6H5)2)·CH2C12. Crystal data: monoclinic,P21/n, cell parameters (X-ray)a=12.82(2) Å,b=22.91(2) Å,c=17.83(2) Å, β=99.1(3)°; (neutron)a=12.94(1) Å, β=22.95(2)Å,c=17.93(3)Å,β=99.55(5)°. The structure was solved from X-ray data. FinalR indices areR(F)=0.051,Rw(F)=0.049 (X-ray);R(F)=0.064,Rw(F)=0.048,R(F2)=0.072,Rw(F2)=0.088 (neutron). The complex is derived from Ru3(CO)8(dpam)2 through reaction with hydrogen. The structure consists of a triangular array of metal atoms involving three metal-metal bonds[Ru(1)?Ru(2)=2.912(7)Å;Ru(1)?Ru(3)=2.829(3) A; Ru(2)?Ru(3)=2.845(6) Å]. The metal-metal edge Ru(1)?Ru(2) is supported by a bridging bis(diphenylarsino)methane ligand which lies in the equatorial plane. Activation of the second dpam ligand has generated the new face-bridging ligand unit μ-As(C6H5)CH2As(C6H5)2. In this unit, the bridgehead As atom spans over the Ru(1)?Ru(2) bond, while the second As atom is only bonded to Ru(3). The metal environment is achieved by CO ligands. The hydride ligand is bridging the Ru(1)?Ru(2) vector [Ru(1)?H=1.791(10) Å; Ru(2)?H=1.818(8) Å]. Geometric features of the dibridged Ru(μ-H)(μ-As)Ru bond are discussed. 相似文献
Treatment of [Fe2(CO)6(μ-S2C3H6)] (1) with triphenylstibine in a 1:1 molar ratio at room temperature in presence of Me3NO resulted compound [Fe2(CO)5(SbPh3)(μ-S2C3H6)] (2) in 88% yield as red crystals. When the reaction was carried out under a 1:5 molar ratio in presence of Me3NO, it resulted a monosubstituted compound [Fe2(CO)5(SbPh3)(μ-S2C3H6)] (2) in 63% yield along with a disubstituted compound [Fe2(CO)4(SbPh3)2(μ-S2C3H6)] (3) in low yield (8%) as red crystals. Reaction of 2 with triphenylstibine in a 1:5 molar ratio under same condition resulted 3 in moderate yield (46%). Compounds 2 and 3 were characterized by elemental analyses, IR, 1H NMR and 13C NMR spectroscopic data. Crystal structures of the compounds were unambiguously determined by single crystal X-Ray diffraction studies. Compound 2 crystalized as monoclinic crystal system with the space group P21/c, a?=?9.464(4) Å, b?=?16.902(7) Å, c?=?17.081(7) Å, β?=?101.216(13)° and Z?=?4. Compound 3 was triclinic, space group P-1, a?=?9.552(3) Å, b?=?13.985(5) Å, c?=?16.487(6) Å, α?=?78.372(16)°, β?=?89.976(14)°, γ?=?71.638(11)° and Z?=?2.
Graphic Abstract
Two new diiron propane-1,3-dithiolate complexes, [Fe2(CO)5(SbPh3)(μ-S2C3H6)] (2) and [Fe2(CO)4(SbPh3)2(μ-S2C3H6)] (3), were synthesized by the displacement of carbonyl groups from [Fe2(CO)6(μ-S2C3H6)] (1) with triphenylstibine, and the resulting complexes were structurally characterized.
Solid state molecular structure of compound 2 (left) and compound 3 (right)