scholarly journals Synthesis and molecular structure of biologically significant bis(1,3-dimesityl-4,5-naphthoquinoimidazol-2-ylidene)gold(I) complexes with chloride and dichloridoaurate counter-ions

2019 ◽  
Vol 75 (4) ◽  
pp. 462-468 ◽  
Author(s):  
Jayaraman Selvakumar ◽  
Meredith H. Miles ◽  
David A. Grossie ◽  
Kuppuswamy Arumugam
Keyword(s):  
Crystal Lattice ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Counter Anion ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
Average Value ◽  
Counter Ions

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.

One-dimensionally Hydrogen-bonded Silver(I) Saccharinate Complexes with N-(2-Aminoethyl)piperidine and N-(2-Hydroxyethyl)piperidine: Synthesis, Crystal Structures, FTIR and Thermal Studies

2008 ◽  
Vol 63 (2) ◽  
pp. 139-142 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
Orhan Büyükgüngör
Keyword(s):  
Thermal Studies ◽  
Chair Conformation ◽  
Metallic Silver ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
The Individual

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

Enclathrating Benzene in a Neutral Dicopper(II) Coordination Framework

2003 ◽  
Vol 56 (7) ◽  
pp. 671 ◽  
Author(s):  
Hong-Bo Liu ◽  
Shu-Yan Yu ◽  
Hui Huang ◽  
Zhong-Xing Zhang
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Aromatic Molecules ◽  
Coordination Framework

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.

Studies of Some Cadmium(II) and Mercury(II) Complexes With Dicyclohexylphosphino-N-Phenylthioformamide, LH: Crystal and Molecular-Structures of [Cdl2(LH)]2, ([HgCl2(LH)]2.CH2Cl2) And HgCl2(LH)2

1986 ◽  
Vol 39 (4) ◽  
pp. 547 ◽  
Author(s):  
SW Cowan ◽  
D Dakternieks ◽  
RW Gable ◽  
BF Hoskins ◽  
CL Rolls ◽  
...  
Keyword(s):  
Unit Cell ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Space Group ◽  
Mercury Compounds ◽  
Crystal And Molecular Structures ◽  
Tetrahedral Environment

The crystal and molecular structures of the title compounds, [CdI2(LH)]2, (1), [HgCl2(LH)]2.CH2Cl2(2), and HgCl2(LH)2(3)[where LH = dicyclohexylphosphino-N-phenyl-thioformamide,* (c-C6H11)2PC(S)N(H)Ph] have been determined by single-crystal X-ray diffraction techniques. Crystals of (1) are monoclinic, space group P21/n, a 13.051(2), b 10.183(1), c 18.106(1)Ǻ and β 101.55(8)° with Z 2; R and Rw were 0.047 and 0.044 respectively for 2320 unique, observed reflections. The unit cell contains two equivalent centrosymmetric, halogen-bridged cadmium dimers. Crystals of (2) are triclinic, space group Pī, with a 10.668(4), b 14.978(3), c 16.838(4)Ǻ, and α 111.80(2), β 101.03(2), γ 92.06(2)° with Z 2; R and Rw were 0.069 and 0.067 respectively for 3379 unique observed reflections. The structure shows two independent centrosymmetric halogen-bridged dimers within the unit cell. Crystals of (3) are monoclinic, space group C2/c, a 24.719(6), b 12.247(3), c 26.818(6) Ǻ, and β 94.62(2)° with Z 8; R and Rw were 0.075 and 0.071 respectively for 2698 unique, observed reflections. The structure shows the complex to be monomeric. In all three compounds the metal atom is in an approximately tetrahedral environment with the potentially multidentate ligand, LH, coordinating only through the phosphorus atom. The mercury compounds show a much larger deviation from ideal tetrahedral geometry than does the cadmium compound.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

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.

Polysulfonylamine, LXIII [1] / Polysulfonylamines, LXIII [1]

1995 ◽  
Vol 50 (1) ◽  
pp. 128-138 ◽  
Author(s):  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Hydrogen Bond ◽  
Phenyl Group ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
Amine Molecule ◽  
Chain Sequence ◽  
O 193 ◽  
Oxygen Atoms

Complexes of Uncharged Molecules, Crystal StructureThe thermally labile ternary complexes 18C6 · 2MeOH · 2 HN(SO2Ph)2 (2a), 18C6 · 2MeOH · 2HN(SO2–C6H4-4-Cl)2 (2b) and 18C6 · 3 MeOH · HN(SO2Me)(SO2Ph) (3) were obtained by co-crystallization of 18-crown-6 (18C6) and the appropriate di(organosulfonyl)amine from methanolic solutions and characterized by low-temperature X-ray diffraction. The crystal structures of 2a (monoclinic, space group P21/n) and 2b (triclinic, space group P1̄) consist of monomeric, centrosymmetric formula units. Each di(arenesulfonyl)-amine molecule is connected to a methanol molecule by an N-Η ··· O hydrogen bond (H ··· O 203 pm in 2a, 190 pm in 2b). The methanol molecules are linked to three alternate crown oxygen atoms via one O-Η ··· O(crown) hydrogen-bond and two weaker C-Η ··· O(crown) interactions (OH ··· O 201 pm in 2a, 186 pm in 2b; CH ··· O 236 and 247 pm in 2a, 240 and 254 pm in 2b); two symmetry-related oxygen atoms of the crown are involved in O-Η ··· O and the other four in C-Η ··· O interactions. The structure of complex 3 (monoclinic, space group P21) is built of infinite chains parallel to [101]. The methyl group of the di(organosulfonyl)amine is bonded by C-Η ··· O(crown) interactions to a set of three alternate oxygen atoms of the cyclic polyether (H ··· O 228, 245 and 247 pm). Starting from the acidic NH function, a sequence of three methanol molecules catenated by hydrogen bonds curves around the bulky phenyl group and links with its terminal MeOH through one O-H ··· O(crown) and two C-Η ··· O(crown) bonds to the second set of alternate oxygen atoms in the adjacent symmetry-equivalent crown (OH ··· O 193 pm, CH ··· O 248 and 250 pm). Within the chain sequence N-H ··· O′(Me)H′ ··· O″(Me)H″ ··· O‴(Me)H, the H ··· O distances are H ··· O′ 184, H′ ··· O″ 189 and H″··· O‴ 183 pm. In the structures of 2a, 2b and 3, the crown rings adopt the frequently observed D3d pseudosymmetry.

Anionische Komplexe [Mo2(O2CPh)4X2]2⊖ mit X = N3, Cl, Br. Die Kristallstruktur von (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 / Anionic Complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, Cl, Br. The Crystal Structure of (PPh4)2[Mo2(O2C-Ph)4Cl2] · 2CH2Cl2

1985 ◽  
Vol 40 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Kay Jansen ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Diffraction Data ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Anionic Complexes

The syntheses and IR spectra of the complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, CI, Br and the counter ion PPh4⊕ are reported. The azido and the bromo complexes are obtained from a solution of [Mo2(O2CPh)4] with PPh4N3 in pyridine or by reaction with PPh4Br in CH2Br2, respectively. When (PPh4)2[Mo2(O2CPh)4(N3)2] is dissolved in CH2Cl2, nitrogen is evolved and the complex with X = CI is obtained. The crystal structure of (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 was determined from X-ray diffraction data (5676 observed independent reflexions, R = 0.042). It crystallizes in the monoclinic space group P21/n with four formula units per unit cell; the lattice constants are a = 1549, b = 1400, c = 1648 pm, β = 94.6°. The centrosymmetric [Mo2(O2CPh)4Cl2]2⊖ ion has a rather short Mo-Mo bond of 213 pm, whereas the MoCl bonds are very long (288 pm)

Structural Systematics of Metal Acetylide Complexes: X-Ray Studies of Some 'Extended-Chain' Gold σ-Acetylide Complexes

1997 ◽  
Vol 50 (10) ◽  
pp. 991 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Ground State ◽  
Structural Data ◽  
Monoclinic Space Group ◽  
Confidence Limits ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Back Bonding ◽  
Ground State Geometry

The structures of Au(4-C≡CC6H4XYC6H4-4′-NO2)(PPh3) (XY = (E )-CH=CH (1), (Z)-CH=CH (2), C≡C (3), N=CH (4)) have been determined by single-crystal X-ray diffraction analyses, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a8·847(1), b 17·870(4), c 19·705(3) Å, α116·25(1), β 93·33(1), γ 92·64(2)˚, Z 4, 6747 unique reflections (703 parameters), converging at R 0·025 and Rw 0·029. For (2), crystals are monoclinic, space group P 21/a, with a 10·718(6), b 19·398(5), c14·469(3) Å, β 108·96(2)˚, Z 4, 3295 unique reflections (352 parameters), converging atR 0·040 and Rw 0·034. For (3), crystals are triclinic, space group P-1, with a 10·671(4), b 17·599(7), c 18·220(8) Å, α 116·31(3), β 105·00(4), γ 95·08(4)˚, Z 4, 4828 unique reflections (703 parameters), converging at R 0·043 and Rw 0·030. For (4), crystals are triclinic, space group P-1, with a 8·8314(6), b 17·834(2), c 20·001(2) Å, α 115·249(7), β 90·930(7), γ 94·082(7)˚, Z 4, 4724 unique reflections (703 parameters), converging at R 0·035 and Rw 0·034. Despite the [ligated metal donor]-bridge-[nitro acceptor] composition of these complexes, Au–C and C≡C distances are normal and consistent with minimal allenylidene contribution to the ground-state geometry. Within the 3σ confidence limits, the structural data do not provide evidence for π*-back-bonding in these complexes

Supramolecular assembly of two copper(II) coordination compounds of topiroxostat with dialkylformamide ligands

2019 ◽  
Vol 74 (6) ◽  
pp. 479-484 ◽  
Author(s):  
Li-Ting Jiang ◽  
Xiang Chang ◽  
Sheng-Chun Chen ◽  
Xue-Jun Feng ◽  
Qun Chen
Keyword(s):  
Coordination Compounds ◽  
Supramolecular Assembly ◽  
Oxidase Inhibitor ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Thermal Stabilities ◽  
Xanthine Oxidase Inhibitor ◽  
Triclinic Space Group ◽  
Space Group ◽  
Supramolecular Coordination

AbstractA well-known selective xanthine oxidase inhibitor topiroxostat, 4-[3-(4-pyridinyl)-1H-1,2,4-triazol-5-yl]-2-pyridinecarbonitrile (ptpc), was selected to react with Cu(NO3)2 · 3H2O in dialkylformamide solvents, affording two novel supramolecular coordination compounds [Cu(ptpc)2(NO3)(DMF)2] · NO3 (1) and Cu(ptpc)2(NO3)2(DEF)2 (2). Single-crystal X-ray diffraction revealed that compound 1 crystallizes in the monoclinic space group C2/c. The components are assembled to a 3D supramolecular framework through hydrogen-bonding interactions between the large [Cu(ptpc)2(NO3)(DMF)2]+ cationic moieties and the nitrate anions. Compound 2 crystallizes in the triclinic space group P1̅ and shows a 2D hydrogen-bonded network structure. The results clearly indicate that dialkylformamide solvents with different sizes have an important influence on the structures of the complexes. The luminescence properties of 1 and 2 in the solid state and their thermal stabilities were also investigated.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

Synthese von zweikernigen Triazenido- und Pentaazadienidokomplexen des einwertigen Silbers. Kristallstruktur von [Ag(MeOC6H4N3C6H4OM e)]2· 2/3 Py, [Ag(MeOC6H4N5C6H4OMe)]2 und [Ag(EtOC6H4N5C6H4OEt)]2 · Py / Dimeric Triazenido and Pentaazadienido Complexes of Monovalent Silver. Synthesis and Structure of [Ag(MeOC6H4N3C6H4OM e)]2· 2/3 Pyridine, [Ag(MeOC6H4N5C6H4OMe)]2 und [Ag(EtOC6H4N5C6H4OEt)]2 · Pyridine

1989 ◽  
Vol 44 (7) ◽  
pp. 778-785 ◽  
Author(s):  
Edmund Hartmann ◽  
Raimund Schmid ◽  
Joachim Strähle
Keyword(s):  
Unit Cell ◽  
Dinuclear Complexes ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Bridging Ligand ◽  
Orange Yellow ◽  
Ag Contact ◽  
Saturated Solutions

[Ag(MeOC6H4N3C6H4OMe)]2 (1) is formed in THF from AgNO3 , and the triazenide anion, as obtained from the corresponding triazene and Na. 1 crystallizes from pyridine in the form of orange-yellow , air stable crystals with the com position 1·2/3 C5H5N: space group P 1̅ with a = 1468.0(5), b = 1514.1(6), c - 1316.1(3) pm, a = 113.45(3)°, β = 1 1 4 .8 1 (2 )°, γ = 66.78(3)°, Z - 3. The triazenide ion functions as a bridging ligand forming planar (AgN3)2 heterocycles. The unit cell contains two symmetry-independent dinuclear complexes, one of which is centrosymmetrical. The short Ag -Ag distances of 268.0 and 269.8 pm suggest Ag -Ag bonding. The pentaazadienido complexes Ag(RN5R) with R = p -MeO - C6H4 (2), p -EtO - C6H4 (3), p-Cl -C6H4 (4), p -F -C6H4 (5), are obtained from saturated solutions of the pentaazadiene in conc. NH3 and AgNO3 , as explosive, red precipitates which are stable in air. Crystals of 2 and 3 · C5H5N are obtained from pyridine. 2 crystallizes in the monoclinic space group P21/c: a - 583.7(6), b = 1705.1(9), c = 1489.6(9) pm. β = 96.2(1)°, Z = 2; 3 · C5H5N is triclinic (space group P 1̅) with a = 1160.4(4). b = 1671.0(6), c = 509.0(1) pm. a = 97.51(2)°, β = 97.36(2)°, γ = 81.51(3)°, Z = 1. The complexes 2 and 3 are dinuclear with the pentaazadienide ion as a (N1)-η1,(N5)-η1 bridging ligand in 2 and a (N1)-η1, (N3)-η1 bridging ligand in 3. The bridging mode in 3 results in a short Ag -Ag contact of 283.44 pm. The Ag -N distances range from 210.8 to 215.7 pm in 1 and from 215.0 to 220 pm in (2) and (3).

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