The Influence of the Amine Concentration onto Product Formation: Crystal Structures, Thermal Stability and Spectroscopic Properties of Two New Manganese Thiostannates Obtained under Solvothermal Conditions

2008 ◽  
Vol 63 (11) ◽  
pp. 1243-1251 ◽  
Author(s):  
Nicole Pienack ◽  
Christian Näther ◽  
Wolfgang Bensch
Keyword(s):  
Coordination Polymer ◽  
Spectroscopic Properties ◽  
Product Formation ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
Hydrogen Bonding Interactions ◽  
Solvothermal Conditions

Abstract Two new thiostannates with Mn2+ ions were obtained under solvothermal conditions applying different amine concentrations. [Mn(C6H14N2)2(H2O)]2Sn2S6 (1) (C6H14N2 = 1,2-diaminocyclohexane, 1,2-dach) crystallizes in the monoclinic space group C2/c (with a = 23.7500(18), b = 15.5655(16), c = 12.1072(9) Å , β = 113.532(8)°, Z = 8). The second compound, [Mn(C6H14N2)2]- Sn2S6 ・2 C6H15N2 (2), crystallizes in the triclinic space group P¯1 with a = 7.3019(6), b = 11.1798(9), c = 13.2837(11) Å , α = 76.877(10), β = 74.719(9), γ = 82.972(10)°, Z = 1. Both structures feature [Sn2S6]4− anions acting as bidentate ligands and joining the octahedrally coordinated Mn2+ cations, but in 1 a molecular complex is formed, whereas in 2 a one-dimensional coordination polymer is observed. In 1 the Mn2+ cation has bonds to four N atoms of two 1,2-dach ligands, to one H2O molecule, and to one S atom of the [Sn2S6]4− anion. The [Sn2S6]4− anion is located on a center of inversion joining two symmetry related complexes. In 2 Mn2+ is surrounded by four N atoms of two 1,2-dach ligands and by two S atoms of two neighboring [Sn2S6]4− anions. In contrast to 1 a negatively charged coordination polymer is formed with [Sn2S6]4− anions acting as linkers and the Mn2+ centered complexes being the nodes. The co-crystallized 1,2-dach molecules are protonated, and they are located between the chains. The first compound was obtained from diluted aqueous solutions of 1,2-dach, and 2 crystallized from solutions containing < 25% H2O. In both compounds several short S···H distances indicate weak hydrogen bonding interactions. Compound 1 is stable up to 121 °C and 2 up to 220 °C. In the Raman spectra of 1 and 2 resonances which are typical for [Sn2S6]4− units could be observed. The band gaps are found to be 2.6 eV (477 nm) and 3.1 eV (400 nm) for 1 and 2, respectively.

One-dimensional ribbons of solvated Ag sulfonates

1999 ◽  
Vol 77 (3) ◽  
pp. 313-318 ◽  
Author(s):  
George KH Shimizu ◽  
Gary D Enright ◽  
Gabriela S Rego ◽  
John A Ripmeester
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
The Other ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Structure Determinations

Single crystal X-ray structure determinations of two solvated silver sulfonates have been obtained and these compounds have been shown to adopt infinite one-dimensional motifs. {AgOTs(MeCN)}[Formula: see text] (OTs = p-toluenesulfonate) crystallizes in the monoclinic space group, P21, a = 8.4278(5) Å, b = 5.7413(3) Å, c = 12.1057(7) Å, β = 109.24(1)°. {Ag(NDSA)(MeCN)2(H3O)(H2O)2}[Formula: see text] (NDSA = 1,5-naphthalenedisulfonate) crystallizes in the triclinic space group, P[Formula: see text], a = 8.3407(4) Å, b = 10.4374(5) Å, c = 12.3399(6) Å, α = 101.941(8)°, β = 109.24(1)°, γ = 102.190(8)°. Despite one compound containing a monosulfonate and the other a disulfonate, both complexes form infinite one-dimensional arrays.Key words: silver, sulfonates, coordination polymer.

Synthesis and structural characterization of donor-stabilized disubstituted diphenyldithiophosphates of nickel(II)

2014 ◽  
Vol 70 (4) ◽  
pp. 761-767 ◽  
Author(s):  
Sandeep Kumar ◽  
Ruchi Khajuria ◽  
Amanpreet Kaur Jassal ◽  
Geeta Hundal ◽  
Maninder S. Hundal ◽  
...  
Keyword(s):  
Single Crystal ◽  
Chelate Ring ◽  
Donor Ligands ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Donor-stabilized addition complexes of nickel(II) with disubstituted diphenyldithiophosphates, [{(ArO)2PS2}2NiL2] {Ar = 2,4-(CH3)2C6H3[(1), (5)], 2,5-(CH3)2C6H3[(2), (6)], 3,4-(CH3)2C6H3[(3), (7)] and 3,5-(CH3)2C6H3[(4), (8)];L= C5H5N [(1)–(4)] and C7H9N [(5)–(8)]}, were successfully isolated and characterized by elemental analysis, magnetic moment, IR spectroscopy and single-crystal X-ray analysis. Compound (4) crystallizes in the monoclinic space groupP21/nwhereas compounds (7) and (8) crystallize in the triclinic space group P\bar 1. The single-crystal X-ray diffraction analysis of (4), (7) and (8) reveals a six-coordinated octahedral geometry for the NiS4N2chromophore. Two diphenyldithiophosphate ions act as bidentate ligands with their S atoms coordinated to the Ni centre. Each of them forms a four-membered chelate ring in the equatorial plane. The N atoms from two donor ligands are axially coordinated to the Ni atom.

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

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.

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.

Supramoleküle aus Kronenethern und geminalen Sulfonen: Synthese von vier binären Komplexen und Kristallstruktur von (CH2CH2O)4·2H 2C(SO2C2H5)2/Supramolecules of Crown Ethers with Geminal Sulfones: Synthesis of Four Binary Complexes and Crystal Structure of (CH2CH2O )4·2H2C(SO2C2H5)2

1995 ◽  
Vol 50 (7) ◽  
pp. 1018-1024 ◽  
Author(s):  
Axel Michalides ◽  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Binary Complexes ◽  
Cyclic Polyethers ◽  
Adjacent Unit ◽  
Methylene Group

In a systematic search for supramolecular complexes involving all combinations of the cyclic polyethers 12-crown-4 (12C4), 15-crown-5 (15C 5), 18-crown-6 (18C 6) and dibenzo- 18-crown-6 (DB -18C6), and the geminal di- or trisulfones H2C(SO 2Me)2, H2C (SO2Et)2 and HC (SO2Me)3-n (SO2Et)n (n = 0 -3 ) , only the following four complexes could be isolated and unequivocally characterized by elemental analysis and 1H NMR spectroscopy: [(12C4){H2C (SO2Et)2}2] (3), [(18C6){H2C (S O2Me)2}] (4), [(DB -18C 6){H2C (SO2Et)2}] (5) and [(D B -18C 6)2{HC (SO2Me )(SO2Et)2}3] (6). The structure of 3 (triclinic, space group P1̄) consists of crystallographically centrosymmetric formula units, in which the disulfone molecules are bonded on each side of the ring by two C -H ··· O(crown) interactions originating from the central methylene group (H···O 213 pm) and from the methylene group of one EtSO2 moiety ( H ··· O 237 pm). Formula units related by translation are connected into parallel strands by a third type of reciprocal C -H ···O bond (H ···O 232 pm) between the second H atom of the central methylene group and a sulfonyl oxygen atom of the adjacent unit. The structure of 4 (monoclinic, space group C2/c) showed severe disorder of the crown ether and could not be refined satisfactorily. Compounds 5 and 6 crystallized as long and extremely thin fibres, indicative of linear-polymeric supramolecular structures; single crystals for X-ray crystallography were not available.

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.

Zur Umsetzung von ReO2I(PPh3)2 mit PhNCO. Synthese und Kristallstrukturen von ReO2I(PPh3)2 · CHCl3, [ORe(OCONPh)I(PPh3)]3, Re(NPh)(NH2Ph)I2(PPh3)(OCONHPh) und Re(NPh)(NH2Ph)I2(PPh3) ( OReO3) / On the Reaction of ReO2I(PPh3)2 with PhNCO. Synthesis and Crystal Structures of ReO2I(PPh3)2 · CHCl3, [ORe(OCONPh)I(PPh3)]3, Re(NPh)(NH2Ph)I2(PPh3)(OCONHPh) and Re(NPh)(NH2Ph)I2(PPh3) ( OReO3)

1991 ◽  
Vol 46 (2) ◽  
pp. 235-244 ◽  
Author(s):  
S. Schmid ◽  
J. Strähle
Keyword(s):  
Hydrolysis Product ◽  
Phosphine Ligands ◽  
Partial Hydrolysis ◽  
Monoclinic Space Group ◽  
Linear Arrangement ◽  
Triclinic Space Group ◽  
Metal Centers ◽  
Space Group ◽  
Trimeric Complex ◽  
Oxo Ligand

PhNCO reacts with oxo ligands at metal centers to form phenyl nitrene complexes. As an intermediate of this reaction we obtained with ReO2I(PPh3)2 (1) the trimeric complex [ORe(OCONPh)I(PPh3)]3 (2) in which the PhNCO moiety was added to an oxo ligand to form an N -phenyl carbamato group. This group acts as a bridging ligand chelating one Re atom via its N and one O atom and coordinating an other Re atom by its second O atom . 2 crystallizes as 2 · 2 CHCl3 in the triclinic space group P1̄ with a = 1423.1(5), b = 2443.3(7), c = 1403.8(6) pm , α = 92.31(3), β = 94.76(3), γ = 81.48(3)°, and Z = 2. From the mother liquor of 2 after a few days Re(NPh)(NH2Ph)I2(PPh3)(OCONHPh) (3) is formed as a partial hydrolysis product. 3 is monoclinic with the space group P21/n and a = 1163.0(4), b = 2527.0(3), c = 1243.9(5) pm, β = 98.04°, Z = 4. The Re atom exhibits an octahedral coordination w ith the two I atom s in a ?ra«s-arrangem ent and the phenyl nitrene ligand trans to the m onodentate PhN HCO2 group. The coordination is completed by a phosphine and an aniline ligand. Reaction of 2 with excess PPh3 yields 1. It crystallizes from CHCl3 as 1 · CHCl3 in the monoclinic space group P21/n with a = 975.9(3), b = 2731(1), c = 1417.3(6) pm , β = 93.35° and Z = 4. In 1 the Re atom is pentacoordinated in form of a trigonal bipyram id with the two phosphine ligands in axial positions. A solution of 2 in THF forms Re(NPh)(NH2Ph)I2(PPh3) (OReO3) (4) upon exposure to air at room temperature. 4 is obtained as orthorhombic crystals with the space group Pca21 and a = 1727(1), b = 1064.2(4), c = 1765.7(9) pm , Z = 4, and is an analogue of 3 from which it can be derived by substituting the carbamato ligand by a perrhenat ion. In 3 and 4 the phenyl nitrene ligand is bound by a Re = N triple bond of 172 pm in a linear arrangement Re = N - Ph .

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.

Stabilisierung des reaktiven Methylcarbonat-Ions im Kronenether- Komplex [Cs(18-Krone-6)(CH3CO3)] und dessen Hydrolyseprodukt / Stabilization of the Reactive Methylcarbonate Ion in the Crown Ether Complex [Cs(18-crown-6)(CH3CO3)], and its Hydrolysis Product

2008 ◽  
Vol 63 (9) ◽  
pp. 1101-1106
Author(s):  
Adelė Jonušaite ◽  
Arnold Adam
Keyword(s):  
Crown Ether ◽  
Hydrolysis Product ◽  
Starting Material ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
Space Group ◽  
Methyl Carbonate ◽  
Hydrolysis Of ◽  
Ether Complex ◽  
Oxygen Atoms

[Cs(18-crown-6)(CH3CO3)] (1) has been obtained by the reaction of CsOCH3 with 18-crown-6 (1,4,7,10,13,16-hexaoxacyclooctadecane) in methanol in a CO2 atmosphere. The compound crystallizes in the monoclinic space group P21/n (no. 14) with a = 12.141(3), b = 8.610(1), c = 17.985(4) Å , β = 91.17(2)° and V = 1879.6(7) Å3. Cs is tenfold coordinated by six oxygen atoms of the crown ether and four oxygen atoms of two methyl carbonate anions which act as bidentate ligands. The slow hydrolysis of the methylcarbonate results in the hydrogencarbonate complex {Cs2(18-crown- 6)2 · [H2(CO3)2] · H2O · CH3OH} (2), the basic structural constitution of the starting material being retained. This new compound crystallizes in the monoclinic space group P21/c with a = 8.657 (7), b = 22.601 (2), c = 19.619 (15) Å, β = 92.09 (6)° and V = 3836.5 (6) Å3.

Sign in / Sign up

Export Citation Format

Share Document