A chiral salency complex,[Mn(Salency)(H2O)2](PF6)·2H2O 1(Salency =(R,R)-N,N'-bis(salicylidene)-1,2-cyclohexanediamine),has been prepared by the reaction of Mn(CH3COO)3·2H2O with Salency and NH4PF6,and was established by X-ray diffraction techniques.The complex crystallizes in triclinic,space group P1 with a=9.299(8),b=10.012(8),c=13.461(11),α=92.037(15),β=92.974(12),γ=93.530(18)°,V=1248.3(18)3,C20H28F6MnN2O6P,Mr = 592.35,Z=2,Dc=1.038 g/cm3,F(000)=608,μ=0.676 mm-1,the final R=0.0651 and wR=0.1880 for 5260 observed reflections with I > 2σ(I).
A new thiostannate,[tmdpH2]Sn3S7 1(tmdp = 4,4'-trimethylenedipiperidine),has been synthesized under solvothermal conditions and characterized by elemental analysis,IR spectroscopy,and single-crystal X-ray diffraction analysis.In 1,the Sn3S4 secondary incomplete cubane-like building units are bridged by μ2-S atoms to form Sn12S12 rings which are then joined parallelly to the [001] plane,giving the final 2D(Sn3S72-)n layer of(6,3) network.The layers are stacked along the c axis so that 24-membered ring channels are generated,in which the organic cations are accommodated.The compound crystallizes in monoclinic,space group C2/c,with a=23.052(3),b=13.4039(12),c=18.412(2),β=120.112(4)°,V=4921.3(9)3,C13H28N2S7Sn3,Mr=792.86,Z=8,Dc=2.140 g/cm3,F(000)=3056,μ=3.619 mm-1,the final R=0.0488 and wR=0.1125 for 4607 observed reflections with I>2σ(I).
Solvothermal reaction of lanthanide(Ⅲ) salts with fluorescein (2-(6-hydroxy3-oxo-3H-xanthen-9-yl)benzoic acid) led to a series of new coordination polymers {[Ln(C 20 H 11 O 5)(C 20 H 10 O 5)(H 2 O)]·DMF} n (Ln=Er,Eu,Gd,Tb,Tm,Yb).The PXRD patterns of the complexes indicate they are isomorphous.The structure of complex {[Er(C 20 H 11 O 5)(C 20 H 10 O 5)(H 2 O)]·DMF} n has been determined by single-crystal X-ray diffraction,revealing a 2D framework in which DMF molecules were filled between the layers.The crystal structure belongs to the triclinic system,space group P1,with a=12.107(4),b=12.232(4),c=13.273(4),α=68.005(7),β=88.024(11),γ=77.451(8)°,V=1776.7(9) 3,Z=2,D c=1.720 g/cm 3,μ=2.434 mm-1,F(000)=918,R int=0.0584,T=293(2) K,the final R=0.0621 and wR=0.1501.
A new tetranuclear cyanide-bridged complex [PPh4]2[NiⅡ(CN)4CuⅠ(PPh3)2]2·2CH3OH ([PPh4]+ = tetraphenylphosphine cation, PPh3 = triphenylphosphine) 1 has been synthesized and characterized by IR spectroscopy, elemental analysis, electronic absorption spectra and single-crystal X-ray diffraction. This complex crystallizes in triclinic, space group Pí with a = 10.910(5), b = 15.777(7), c = 18.275(8), α = 68.752(12), β = 79.776(13), γ = 81.400(14)°, NiCuC65H50N4OP3, Mr = 1122.25, V = 2873(2)3 , Z = 2, Dc = 1.293 g/cm3, F(000) = 1156, μ = 0.826 mm-1, the final R = 0.0755 and wR = 0.2155 for 7324 observed reflections (I > 2σ(I)). The title compound exhibits a discrete square tetranuclear structure and a cubic order NLO property.
Two new transition-metal organic coordination polymers [M(mna)2](M = Cd(1),Zn(2);mna = 2-mercaptonicotinic anion) have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction along with IR and elemental analyses.Compound 1 is generally a one-dimensional linear structure bridged through the sulfur donor of mna ligand,while 2 is a one-dimensional zigzag chain ligated via the oxygen donor of mna ligand.These compounds further result in three-dimensional structures via intermolecular π...π stacking interactions and/or hydrogen bonding interactions.The two compounds were structurally determined by single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic space group P21/c with a = 3.730(3),b = 13.973(12),c = 12.380(11) ,β = 97.953(18)°,V = 639.0(10) 3,Z = 2,CdC12H8O4N2S2,Mr = 420.72,Dc = 2.187 g/cm3,F(000) = 412,Rint = 0.0252,T = 293(2) K,μ = 2.052 mm?1,the final R = 0.0269 and wR = 0.0586 for 1377 observed reflections with I > 2σ(I).Complex 2 belongs to monoclinic space group P21/c with a = 13.376(2),b = 12.8429(14),c = 7.4856(10) ,β = 96.190(10)°,V = 1278.5(3) 3,Z = 4,ZnC12H8O4N2S2,Mr = 373.69,Dc = 1.941 g/cm3,F(000) = 752,Rint = 0.0414,T = 293(2) K,μ = 2.264 mm?1,the final R = 0.0418 and wR = 0.0966 for 2396 observed reflections with I > 2σ(I).
A new tri-nuclear mixed metal thiolate complex [Ag(PPh3)2]2[Ni(edtO2)2] 1 has been synthesized and structurally characterized by single-crystal diffraction.The molecule has a crystallographic inversion centre occupied in the central Ni(II) atom and the two silver(I) atoms are related by the inversion centre.The unique structural feature is that one of thiolates of each edt ligand has been oxidized to sulfinate from the precursor [Ni(edt)2]2-to the neutral linear trinuclear complex.The crystal structure belongs to the monoclinic system,space group P21/n with a = 13.581(11),b = 12.239(9),c = 22.316(17) ,β = 103.08(2)o,V = 3613(5) 3,Z = 2,Mr = 1571.87,Dc = 1.445 g/cm3,μ = 1.046 mm-1,F(000) = 1604,T = 293(2) K,the final R = 0.0652 and wR = 0.1499 for 6776 observed reflections with I > 2σ(I).
Two cyanide bridged trinuclear compounds [Fe(bpy)2(CN)2]·[Cu(Cyclam)]2- (ClO4)4·DMF 1 and [Fe(Phen)2(CN)2]·[Cu(Cyclam)]2(ClO4)4·2CH3CN·4H2O 2 (Bpy = 2,2'- bipyridine, Phen = 1,10-phenanthroline, Cyclam = 1,4,8,11-tetraaza-cyclotetradecane, and DMF = N,N-dimethylformamide) have been synthesized by using mononuclear [Fe(Phen)2(CN)2]·2H2O and [Fe(bpy)2(CN)2]·3H2O as precursors. These two complexes crystallize in monoclinic space groups P21/c and C2/c, respectively. For 1, a = 25.164(2), b = 12.0405(11), c = 20.4433(15) , β = 91.948(3)o, V = 6190.5(9) 3, Z = 4, Mr = 1418.90, Dc = 1.522 g/cm3, F(000) = 2936, μ = 1.161 mm-1, the final R = 0.0722 and wR = 0.2011 for 10779 observed reflections (I > 2σ(I)). For 2, a = 43.5945(0), b = 11.8447(0), c = 29.5637(2), β = 120.430(11)o, V = 13162.76(9) 3, Z = 8, Mr = 1518.48, Dc = 1.533 g/cm3, F(000) = 6288, μ = 1.101 mm-1, the final R = 0.0711 and wR = 0.1783 for 11262 observed reflections (I > 2σ(I)).
