Syntheses and Crystal Structures of Silver(I) Organosulfur Polymers as One-Dimensional Chains

2003 ◽  
Vol 56 (11) ◽  
pp. 1167 ◽  
Author(s):  
Ruihu Wang ◽  
Maochun Hong ◽  
Weiping Su ◽  
Rong Cao ◽  
Yingjun Zhao ◽  
...  

Two silver(I) organosulfur coordination polymers, {[Ag2(mbpsq).dmf](NO3)2}n (1) and {[Ag3(bpsp)2(CH3CN)]-(BF4)3.2 H2O}n (2), were prepared by self-assembly of silver(I) with the chelating heterocyclic ligands mbpsq and bpsp (mbpsq = 2,3-bis[2-(4-methylpyrimidinyl)methylsulfanyl]-quinoxaline; bpsp = 2,6-bis[(2-pyrimidinyl)-methylsulfanyl]-pyridine). Single-crystal X-ray diffraction analysis reveals that (1) crystallizes in the triclinic space group P1– with a 10.1937(8), b 11.2160(9), c 13.8445(11) Å, α 103.0620(10), β 106.4850(10), γ; 96.2720(10)°, V 1452.8(2) Å3, Z 2. Each mbpsq molecule acts as a hexadentate ligand, in which two nitrogen atoms of the quinoxaline ring and adjacent sulfur atoms form two stable five-membered rings and two nitrogen atoms from different methylpyrimidine rings bridge two silver(I) centers to form a one-dimensional chain structure. Complex (2) crystallizes also in the triclinic space group P1– with a 12.8119(3), b 13.8902(4), c 15.4534(5) Å, α 70.6980(10), β 68.7570(10), γ; 85.3380(10)°, V 2416.83(12) Å3, Z 2. The bpsq molecules act as tridentate and tetradentate ligands ligating three silver(I) centres of different coordination environments to form a one-dimensional zigzag chain.

2013 ◽  
Vol 69 (11) ◽  
pp. 1332-1335 ◽  
Author(s):  
Xiu-Hua Zhao ◽  
Ya-Yun Zhao ◽  
Jie Zhang ◽  
Jian-Guo Pan ◽  
Xing Li

catena-Poly[[[4-amino-N-(quinoxalin-2-yl)benzenesulfonamidato]aquacadmium(II)]-μ-4-amino-N-(quinoxalin-2-yl)benzenesulfonamidato], [Cd(C14H11N4O2S)2(H2O)], has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction, elemental analysis, fluorescence, IR and thermal analysis. Single-crystal X-ray analysis reveals that the complex is a one-dimensional zigzag chain structure, and the CdIIcation has a distorted octahedral coordination geometry formed by five N atoms from three different sulfaquinoxaline ligands and one O atom from a water molecule. The fluorescence spectrum reveals that the complex emits strong blue fluorescence and thermal analysis shows that the complex has high thermal stability.


2008 ◽  
Vol 63 (2) ◽  
pp. 139-142 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
Orhan Büyükgüngör

Two new complexes [Ag(sac)(aepip)] (1) and [Ag(sac)(hepip)] (2) have been obtained by the reaction of AgNO3 with Na(sac)・2H2O (sac = saccharinate) in the presence of N-(2-aminoethyl)piperidine (aepip) and N-(2-hydroxyethyl)piperidine (hepip), and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group C2 and triclinic space group P1, respectively. In both complexes, silver( I) is tricoordinated. The sac ligand is N-coordinated, while aepip and hepip behave as N-N and N-O bidentate chelating ligands, respectively. The pip rings of both aepip amd hepip ligands adopt typical ‘chair’ conformation. The individual molecules are linked into one-dimensional chains by two N-H···O hydrogen bonds in 1, and one O-H···O hydrogen bond in 2. TG-DTG curves illustrated that the endothermic elimination of aepip and hepip ligands takes place in the early stages of thermal decomposition, while that of the sac moiety occurs exothermically at higher temperatures to give metallic silver


2019 ◽  
Vol 75 (4) ◽  
pp. 462-468 ◽  
Author(s):  
Jayaraman Selvakumar ◽  
Meredith H. Miles ◽  
David A. Grossie ◽  
Kuppuswamy Arumugam

Diffraction-quality single crystals of two gold(I) complexes, namely bis(1,3-dimesityl-4,5-naphthoquinoimidazol-2-ylidene)gold(I) chloride benzene monosolvate, [Au(C29H26N2O2)2]Cl·C6H6or [(NQMes)2Au]Cl·C6H6,2, and bis(1,3-dimesityl-4,5-naphthoquinoimidazol-2-ylidene)gold(I) dichloridoaurate(I) dichloromethane disolvate, [Au(C29H26N2O2)2][AuCl2]·2CH2Cl2or [(NQMes)2Au][AuCl2]·2CH2Cl2,4, were isolated and studied with the aid of single-crystal X-ray diffraction analysis. Compound2crystallizes in a monoclinic space groupC2/cwith eight molecules in the unit cell, while compound4crystallizes in the triclinic space groupP\overline{1} with two molecules in the unit cell. The crystal lattice of compound2reveals C—H...Cl−interactions that are present throughout the entire structure representing head-to-tail contacts between the aromatic (C—H) hydrogens of naphthoquinone and Cl−counter-ions. Compound4stacks with the aid of short interactions between a naphthoquinone O atom of one molecule and the mesityl methyl group of another molecule along theaaxis, leading to a one-dimensional strand that is held together by strong π–η2interactions between the imidazolium backbone and the [AuCl2]−counter-ion. The bond angles defined by the AuIatom and two carbene C atoms [C(carbene)—Au—C(carbene)] in compounds2and4are nearly rectilinear, with an average value of ∼174.1 [2]°. Though2and4share the same cation, they differ in their counter-anion, which alters the crystal lattice of the two compounds. The knowledge gleaned from these studies is expected to be useful in understanding the molecular interactions of2and4under physiological conditions.


2012 ◽  
Vol 554-556 ◽  
pp. 268-272
Author(s):  
Jia Gui Li ◽  
Wan Ren Zhu ◽  
Shu Hong Ding ◽  
Yuan Chen ◽  
Yu Lin Zhu ◽  
...  

A new one-dimensional [CuC16H18N4O4S]n(1) was synthesized by the self-assembly of a ligand 2,5-thiophenediformates, 3,5-dimethylpyrazole and copper(II), and characterized by elemental analysis, IR and single-crystal X-ray diffraction. 1 crystallizes in monoclinic, space group C2/c with unit cell parameters, a=18.6156(4), b=5.96110(10), c= 18.1598(4)Å, =115.467(2)°, Z=4, V=1819.37(7)Å3, Mr = 425.94, Dc = 1.555g/cm3, μ=1.345mm-1, and F(000)= 876. The final R and wR are 0.0328 and 0.0816 for 7611 observed reflections with I>2σ(I). 1 shows an infinite 1-D polymeric chain structure based on the repeated basic units Cu(II)(3,5-dimethylpyrazole)2(2,5-thiophene diformate). The Cu(II)center acts as the joint of the unit, and is coordinated in a slightly distorted octahedral geometry comprised of four O atoms from two different 2,5-thiophenediformate ligands and two N atoms of two trans 3,5-dimethylpyrazole ligands.


2001 ◽  
Vol 79 (5-6) ◽  
pp. 964-976 ◽  
Author(s):  
Kamaluddin Abdur-Rashid ◽  
Alan J Lough ◽  
Robert H Morris

The hexahydridobis(phosphine)rhenate anions, [ReH6(PR3)2]- (PR3 = PCy3, P-i-Pr3, PPh3, PMe3) were generated by potassium hydride deprotonation of the neutral heptahydride conjugate acids (ReH7(PR3)2), isolated as their [K(18-crown-6)]+ and [K(1,10-diaza-18-crown-6)]+ salts, and characterized by NMR and IR spectroscopy and elemental analyses. Structures from single crystal X-ray diffraction were obtained for the [K(1,10-diaza-18-crown-6)]+salts and these indicate the presence of short protonic—hydridic bonds involving the hydrides of the anions and the proton donor NH moieties of the cations. The structure of [K(1,10-diaza-18-crown-6)][ReH6(P-i-Pr3)2] adopts a one-dimensional zigzag chain with alternating cations and anions connected and held together by inter-ion N-H···Hx-Re interactions (x = 1 or 2). Short distances between the NH protons of the cations and hydrides of the anion ranging from 1.6 to 1.9 Å are estimated for this complex. A different kind of chain structure is observed for [K(1,10-diaza-18-crown-6)][ReH6(PMe3)2] in which the combined effects of inter-ion protonic—hydridic bonding (N-H···Hx-Re) and inter-ion electrostatic interactions (ReH-x···K+···H-xRe), result in one-dimensional networks of alternating cations and anions, with the metals and hydrides occupying the interior and the organic moieties of the phosphine ligands and crown ether lining the exterior of cylindrical supramolecular assemblies. A combination of intra- and inter-ion protonic-hydridic and intra-ion-pair electrostatic interactions in [K(1,10-diaza-18-crown-6)][ReH6(PPh3)2] result in the formation of discrete two-dimensional {[K(1,10-diaza-18-crown-6)][ReH6(PPh3)2]}4 tetramers. The PCy3 salt is disordered but appears to consist of isolated 1:1 ion pairs containing strong intra-ion-pair NH···HRe bonding. The solid-state IR spectra of the [K(1,10-diaza-18-crown-6)]+ salts show low-frequency shifts for the NH bands relative to [K(1,10-diaza-18-crown-6)][BPh4], and perturbed Re-H bands relative to those in the [K(18-crown-6)]+ salts. The magnitude of ΔνNH is related to the basicity of the anion as indicated by the pKαTHF of the conjugate acid form (ReH7(PR3)2), which increases as PPh3 < < PMe3 < P-i-Pr3 < PCy3. Solution 1H NMR, NOE, and T1 relaxation measurements of [K(1,10-diaza-18-crown-6)][ReH6(PPh3)2] indicate that these interactions also persist in toluene solutions of this compound.Key words: rhenium, hydride, phosphine, hydrogen bonding, self-assembly.


2019 ◽  
Vol 75 (3) ◽  
pp. 294-303 ◽  
Author(s):  
Syed Raza Shah ◽  
Zarbad Shah ◽  
Najeeb Ullah ◽  
Javid Hussain ◽  
Rashid Al-Harrasi ◽  
...  

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-κ2 N,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-κ2 N,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-κ2 N,N′)magnesium]-μ-2-(3,4-dichlorophenyl)acetato-κ2 O: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\overline{1} 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\overline{1} 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.


2003 ◽  
Vol 56 (7) ◽  
pp. 671 ◽  
Author(s):  
Hong-Bo Liu ◽  
Shu-Yan Yu ◽  
Hui Huang ◽  
Zhong-Xing Zhang

Two infinite complexes {[Cu2(O2CCH3)4](3-tpt)(CH3OH)2}∞ (1) and {[Cu2(O2CPh)4](3-tpt)(C6H6)1.5}∞ (2) were obtained by reactions of 2,4,6-tris(3′-pyridyl)-1,3,5-triazine (3-tpt) with Cu2(O2CCH3)4 and Cu2(O2CPh)4, respectively, which have been structurally established by single-crystal X-ray diffraction. Complex (1) consists of one-dimensional zig-zag chains in its solid state, which can encapsulate methanol molecules; complex (2) consists of one-dimensional helical chains in its solid state, providing large channels which can selectively enclathrate benzene molecules. (1) crystallizes in the monoclinic space group P21/c with a 8.2892(4), b 22.8479(8), c 16.9258(10) Å, β 99.1480(10)°, V 3164.8(3) Å3, and Z 4; (2) crystallizes in the triclinic space group P1 with a 10.7641(8), b 12.0908(8), c 18.9039(12) Å, α 82.514(3)°, β 85.268(2)°, γ 79.746(4)°, V 2395.9(3) Å3, and Z 2. The inclusion selectivity toward aromatic molecules was discussed.


2021 ◽  
Author(s):  
Heyi Zhang ◽  
Fangyuan He ◽  
Xiaonan Li ◽  
Zhi-Hui Wang ◽  
Hong Zhang

Through the self-assembly of 1,1'-bis(3-cyanobenzyl)-[4,4'-bipyridine] dichloride ligand, m-H2BDC and Zn(NO3)2·6H2O, a novel one-dimensional chain structure multifunctional coordination polymer was successfully synthesized. Due to electron transfer during irradiation and heating to...


2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.


1998 ◽  
Vol 53 (11) ◽  
pp. 1329-1334 ◽  
Author(s):  
L. Homolya ◽  
S. Strueß ◽  
W. Preetz

The crystal structures of cis-(n-Bu4N)2[ReCl4(NCS)2] (triclinic, space group P1̅, a = 11,245( 1), b = 20.174(3), c = 21.320(8) Å, a =109.06(2), β = 96.46(2), γ = 98.22(5)°, Z = 4) and cis-(Ph4P)2[ReCl4(NCSe)2]·2CH2Cl2 (triclinic, space group P1̅, a = 10.341(2), b = 13.436(3), c = 19.616(4) Å, α = 92.70(2), β = 92.02(2), γ = 89.99( 1)°, Z= 2) have been determined by single crystal X-ray diffraction analysis. Both ambidentate ligands NCS and NCSe are bonded via the N atom. Using the molecular parameters of the X-ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis based on a modified valence force field. The valence force constants fd(ReN) are 1,78(NCS) and 1,79(NCSe) mdyn/ Å.


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