Chemistry of subvalent main group metals with dithiolates. Part 2. X-Ray structural, thermal, and theoretical investigations on the novel one-dimensional stacking structure K2[Pb{S2CC(CN)2}2]·2H2O

1989 ◽  
pp. 627-630 ◽  
Author(s):  
Hans-Ulrich Hummel ◽  
Hermann Meske
Keyword(s):  
Main Group ◽  
The Novel ◽  
One Dimensional ◽  
X Ray ◽  
Main Group Metals ◽  
Theoretical Investigations ◽  
Stacking Structure

Synthesis and Structural Systematics of Nitrogen Base Adducts of Group 2 Salts. VII. Some Complexes of Group 2 Metal Halides With Aromatic N,N'-Bidentate Ligands

1996 ◽  
Vol 49 (1) ◽  
pp. 99 ◽  
Author(s):  
BW Skelton ◽  
AF Waters ◽  
AH White
Keyword(s):  
Room Temperature ◽  
The Novel ◽  
Bidentate Ligands ◽  
Nitrogen Base ◽  
One Dimensional ◽  
X Ray ◽  
L System ◽  
L Systems ◽  
Group 2 ◽  
Structural Characterizations

Syntheses and room-temperature single-crystal X-ray structural characterizations are recorded for a number of adducts of Group 2 halides with the aromatic N,N′- bidentate ligands L = 2,2'-bipyridine ( bpy ) and 1,10-phenanthroline ( phen ). One adduct of 1 : 1 MX2/L stoichiometry is recorded: [( bpy )Ca(μ-Br)(4/2)](∞ ׀ ∞) (1) is monoclinic, C 2/c, a l7.102(5), b 9.845(1), c 7.600(2) Ǻ, β 107.65(2)°, Z = 4 f.u .; conventional R on #1472; F ׀ at convergence was 0.057 for No 817 independent 'observed' ( I > 3σ(I)) reflections, the compound being a one-dimensional polymer… CaL (μ-Br)2CaL(μ-Br)2…, with six-coordinate calcium, cis-CaN2(μ-Br)4, on a twofold axis. 1 : 2 MX2/L systems have been described for two types of array: [( bpy )2CaI2] (2), orthorhombic, Pnca, a 16.914(4), b 13.80(1), c 9.290(4) Ǻ, Z = 4 f.u .; R 0.039 for No 1738, is discrete mononuclear, containing cis-CaN4I2 six-coordinate calcium, whereas the barium analogue is an infinite one-dimensional polymer, [( bpy )2Ba(μ-I)(4/2)](∞׀ ∞) (3), triclinic, Pī, a 11.318(2), b 11.078(2), c 9.206(4) Ǻ, α 80.87(2), β 77.52(2), γ 87.53(1)°, Z = 2 f.u .; R 0.032 for No 4154, with eight-coordinate (N2)2Ba(μ-I)4. The perchlorate analogue, [( bpy )2Ba(μ-OClO2O)(4/2)](∞ ׀ ∞) (4), although of similar stoichiometry, has a trans-rather than a cis-linked chain; it is monoclinic, P 21/c, a 6.606(2), b 18.661(7), c 19.440(8) Ǻ, β 109.45(4)°, Z = 4 f.u .; R 0.044 for No 4060, with μ-I replaced by O,O'-ClO4 bridging units and eight-coordinate barium, (N2)2BaO4. The 1 : 3 MX2/L system is represented (as its hemi( bipyridine ) 'solvate') by mononuclear [( bpy )3SrI2].0.5bpy (5), monoclinic, P 21/c, a 20.834(8), b 9.735(4), c 18.460(7) Ǻ, β 114.87(3)°, Z = 4 f.u .; R 0.039 for No 3711, containing eight-coordinate strontium, [(N2)3SrI2]; there is also an isomorphous calcium/ perchlorate analogue [( bpy )3Ca(OClO3)2].0.5bpy (6), a 21.413(6), b 9.813(4), c 18.659(2) Ǻ, β 115.67(2)°, R 0.057 for No 3090, in which unidentate O-ClO4 ligands replace the iodine about the metal atom. A 1 : 4 adduct is obtained with CaI2/phen; ionic [Ca( phen )4] I2 (7), triclinic, Pī , a 14.703(3), b 13.292(3), c 11.38(1) Ǻ, α 92.78(4), β 96.15(4), γ 105.22(2)°, Z = 2 f.u ., R 0.053 for No 3658, contains eight-coordinate Ca(N2)4 arrays, while the novel 1 : 5 adduct [ Ba ( phen )4] I2.MeCN (8) is triclinic, Pī , a 12.170(6), b 13.760(7), c 18 254(8) Ǻ, α 77.05(9), ,β 71.96(4), γ 70.83(9)°, Z = 2 f.u ., R 0.040 for No 4447, containing 10-coordinate barium, [ Ba (N2)5]. A 1 : 4 adduct formed with BaBr2 is [ BrBa( phen )4] Br.MeOH (9), triclinic, Pī , a 17.748(4), b 17.418(2), c 15.535(7) Ǻ, α 91.63(2), β 100.53(3), γ 115.39(1)°, Z = 4 f.u ., R 0.062 for No 4092, containing nine-coordinate barium, [ BrBa (N2)4].

Synthesis, Crystal Structure and Magnetic Properties of Novel Complex [μ-(NC)-Fe(CN)3(NO)-μ-(CN)-Cu(ept)]n·4nH2O (ept = N-(2-Aminoethyl)propane-1,3-diamine)

2001 ◽  
Vol 66 (10) ◽  
pp. 1490-1498 ◽  
Author(s):  
Zdeněk Smékal ◽  
Jiří Kameníček ◽  
Ingrid Svoboda ◽  
Albert Escuer
Keyword(s):  
Crystal Structure ◽  
Magnetic Measurement ◽  
Antiferromagnetic Interaction ◽  
Title Complex ◽  
The Novel ◽  
One Dimensional ◽  
X Ray ◽  
Magnetic Investigation ◽  
Novel Complex ◽  
Cyanide Ligands

The novel complex [μ-(NC)-Fe(CN)3(NO)-μ-(CN)-Cu(ept)]n·4nH2O (ept = N-(2-aminoethyl)- propane-1,3-diamine) was obtained by the reaction of Cu(ClO4)2·6H2O with N-(2-amino- ethyl)propane-1,3-diamine and Na2[Fe(CN)5NO]·2H2O in water. This compound was characterized by IR, UV-VIS and EPR spectroscopies and magnetic measurement. Single-crystal X-ray structure analysis revealed that the title complex has a one-dimensional polymeric structure containing hexacoordinate iron(II) with five cyanide ligands (two of them, in trans position, bridging) and one nitrosyl group, and pentacoordinate copper(II) with N-(2-aminoethyl)propane-1,3-diamine and two sites occupied by bridging cyanide ligands. Magnetic investigation revealed a very weak antiferromagnetic interaction between the copper atoms (superexchange interaction parameter J = -1.7(1) cm-1; H = -JSiSi+1) within the chain through the diamagnetic [Fe(CN)5NO]2- ions.

scholarly journals Zur Koordination unterschiedlicher Hauptgruppenmetalle mit einem speziellen, chelatisierenden Silazan / On the Coordination of Different Main Group Metals with a Special, Chelating Silazane

1988 ◽  
Vol 43 (7) ◽  
pp. 846-856 ◽  
Author(s):  
M. Veith ◽  
F. Goffing ◽  
V. Huch
Keyword(s):  
Nmr Spectra ◽  
Main Group ◽  
High Symmetry ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Main Group Metals ◽  
H Nmr ◽  
Structure Determinations ◽  
Cis Isomer

Abstract The cis-isomer of the silazane H2L (1) (L = [NtBu][Me]Si(NtBu)2Si[Me][NtBu]) has been used as a ligand to main group metals. By displacing the hydrogen atoms of 1 the compounds L(MgMe)2 (4), L(MgCl)2 (5) and L(Li)(InMe2) (6) have been obtained. According to the 1H NMR spectra the structures of 4-6 are very similar: a polycyclic, cubane-like Si2N4M2 framework results from the special atomic arrangements and from intramolecular Lewis acid-base interactions between the metals M and the nitrogen atoms. Divalent metals and metal-centered groups can also be incorporated into 1. In the latter case a seco norcubane-like polycycle Si2N4M is produced as confirmed by X-ray structure determinations of LGaMe (8) and LSb+ InCl4- (11). LInMe (7) and LSn (9) seem to adopt the same tricyclic structure as 8, although the 1H NMR spectra are not consistent with a rigid molecule (low symmetry), but rather with a fluxional behaviour (high symmetry). When 5 is allowed to react with sodium/naphthalene in THF part of the magnesium is reduced and LMg(THF)2 (12) is formed. An X-ray structure determination of 12 reveals the compound to be only bicyclic with the magnesium atom coordinated by two nitrogen and two THF oxygen atoms.

scholarly journals Connecting Main-Group Metals (Al, Ga, In) and Tungsten(0) Carbonyls via the N2S2 Metallo-Ligand Strategy

Inorganics ◽  
2019 ◽  
Vol 7 (9) ◽  
pp. 115
Author(s):  
Xuemei Yang ◽  
Allen Lunsford ◽  
Marcetta Y. Darensbourg
Keyword(s):  
Transition Metals ◽  
Mass Spectra ◽  
Main Group ◽  
Bimetallic Complexes ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Group Iii ◽  
Main Group Metals ◽  
Square Planar

Tetradentate N2S2 ligands (such as bismercaptoethanediazacycloheptane in this study) have seen extensive use in combination with transition metals. Well-oriented N2S2 binding sites are ideal for d8 transition metals with square planar preferences, especially NiII, but also as a square pyramidal base for those metals with pentacoordinate preferences, such as [V≡O]2+, [Fe(NO)]2+, and [Co(NO)]2+. Further reactivity at the thiolate sulfurs generates diverse bi, tri, and tetra/heterometallic compounds. Few N2S2 ligands have been explored to investigate the possibility of binding to main group metals, especially group III (MIII) metals, and their utility as synthons for main group/transition metal bimetallic complexes. To open up this area of chemistry, we synthesized three new five-coordinate main group XMN2S2 complexes with methyl as the fifth binding ligand for M = Al, and chloride for M = Ga and In. The seven-membered diazacycle, dach, was engaged as a rigid stabilized connector between the terminal thiolate sulfurs. The pentacoordinate XMN2S2 complexes were characterized by 1H-NMR, 13C-NMR, +ESI-Mass spectra, and X-ray diffraction. Their stabilities and reactivities were probed by adding NiII sources and W(CO)5(THF). The former replaces the main group metals in all cases in the N2S2 coordination environment, demonstrating the weak coordinate bonds of MIII–N/S. The reaction of XMN2S2 (XM = ClGaIII or ClInIII) with the labile ligand W(0) complex W(CO)5(THF) resulted in Ga/In–W bimetallic complexes with a thiolate S-bridge. The synthesis of XMN2S2 complexes provide examples of MIII–S coordination, especially Al–S, which is relatively rare. The bimetallic Ga/In–S–W complex formation indicates that the nucleophilic ability of sulfur is retained in MIII–S–R, resulting in the ability of main group MIII–N2S2 complexes to serve as metalloligands.

A one-dimensional coordination polymer createdvia in situligand synthesis involving C—N bond formation

2013 ◽  
Vol 69 (11) ◽  
pp. 1307-1310 ◽  
Author(s):  
Hua Cai ◽  
Ying Guo ◽  
Jian-Gang Li
Keyword(s):  
Addition Reaction ◽  
Bond Formation ◽  
Three Dimensional ◽  
Cadmium Complex ◽  
Stacking Interactions ◽  
The Novel ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
The One

The novel cadmium complexcatena-poly[cadmium(II)-μ3-{2-[3-(pyridin-2-yl)-1H-pyrazol-1-yl]butanedioato}], [Cd(C12H9N3O4)]n, has been prepared by the conjugate addition reaction of 2-(1H-pyrazol-3-yl)pyridine to fumaric acid in the presence of Cd(OAc)2·3H2O (OAc is acetate) at 413 K. Single-crystal X-ray diffraction analysis reveals that the complex consists of one-dimensional ladders constructed from [Cd2(COO)2] dimeric subunits. A combination of hydrogen bonding and π–π stacking interactions extend the one-dimensional ladders into a three-dimensional supramolecular architecture.

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

X-ray Crystallographic Study of Alkylammonium Anthracene-9-carboxylates as a Model for Fibrous Structure of Binary Anthracene Salt Gels

2004 ◽  
Vol 69 (6) ◽  
pp. 1292-1300 ◽  
Author(s):  
Tahahiro Tani ◽  
Kazuki Sada ◽  
Masatsugu Ayabe ◽  
Yuya Iwashita ◽  
Takanori Kishida ◽  
...  
Keyword(s):  
Alkyl Chain ◽  
Columnar Structure ◽  
Hydrogen Bond Network ◽  
One Dimensional ◽  
X Ray ◽  
Crystallographic Study ◽  
Alkylammonium Salts ◽  
Bond Network ◽  
Fibrous Assemblies ◽  
Long Alkyl Chain

Crystal structure of hexylammonium anthracene-9-carboxylate was investigated. The salt was arranged by a one-dimensional hydrogen bond network to form a columnar structure in the crystalline state. This columnar structure should be the model of fibrous assemblies in the organogels of anthracene-9-carboxylate alkylammonium salts having a long alkyl chain.

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