Structural Features of a Sulfur-Containing Group 4 Metalla[11]-crown-4 Derivative

2003 ◽  
Vol 58 (9) ◽  
pp. 838-842 ◽  
Author(s):  
Alexander Snell ◽  
Gerald Kehr ◽  
Birgit Wibbeling ◽  
Roland Frönlich ◽  
Gerhard Erker
Keyword(s):  
Structural Features ◽  
Crystal Structure Analysis ◽  
Octahedral Structure ◽  
X Ray ◽  
Ligand System ◽  
Group 4 ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Analogous Complex ◽  
Sulfur Containing

Treatment of the ligand system (ο-C6H4OH)-S-CH2-CH2-S-(ο-C6H4-OH) (2a) with TiCl4 gave the metalla-crown ether derivative [(-S-CH2-CH2-S-)(ο-C6H4O)2]TiCl2 (5a). Complex 5a was characterized by an X-ray crystal structure analysis. It showed a pseudo-octahedral structure with both sulfur atoms being cis-coordinated to the metal center. The chloride ligands are also cispositioned, whereas the remaining two Ti−oxygen bonds are trans to each other to complete the distorted octahedral coordination geometry. The reaction of 2a with ZrCl4 gave the analogous complex 5c. The related ligand system (ο-C6H4OH)-O-CH2-CH2-O-(ο-C6H4OH) (2b) was doubly deprotonated by treatment with butyl lithium and then reacted with TiCl4 to yield the complex [(-O-CH2-CH2-O-)(ο-C6H4O)2]TiCl2 (5b).

The crystal structure of Bis[2-(pyridin-2-ylamino)-4-(pyridin-2-yl)thiazole]iron(II) Bis(tetrafluoroborate) trihydrate

1984 ◽  
Vol 37 (2) ◽  
pp. 443 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin ◽  
AD Rae
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Octahedral Structure ◽  
Space Group ◽  
X Ray ◽  
Disordered Structure ◽  
Distorted Octahedral ◽  
A Cell

The crystal structure of an iron(II) complex of 2-(pyridin-2-ylamino)-4-(pyridin-2-yl)tliazoe (paptH) has been determined by single-crystal X-ray diffractometry. [Fe(paptH)2] [BF4]2.3H2O is monoclinic, space group P21/c, with Z = 4 in a cell of dimensions a 8.968(6), b 9.038(4), c 41.15(2)�, β 94.81(2)�. The disordered structure was refined to a residual R 0.0826 for 2549 observed reflections. The ligands and anions are orientationally disordered, and the waters of crystallization are positionally disordered. Comprehensive constrained refinement, with 220 parameters for 139 atom positions, produced reliable geometry. The complex cation has a distorted octahedral structure of meridional configuration with both paptH ligands functioning as tridentates.

The Crystal Structure of [2,6-Bis(1-methyl-4-methylthio-5-thia-2,3-diazahexa-1,3-dienyl)-pyridine]dithiocyanatonickel(II), a Complex of a Potentially Pentadentate N3S2 Ligand, and a Comparison with Complexes of an N3O2 Ligand

1979 ◽  
Vol 32 (6) ◽  
pp. 1199 ◽  
Author(s):  
W Choong ◽  
NC Stephenson ◽  
MA Ali ◽  
MA Malik ◽  
DJ Phillips
Keyword(s):  
Crystal Structure ◽  
Data Structure ◽  
Pyridine Ring ◽  
Structure Refinement ◽  
Three Dimensional ◽  
Octahedral Structure ◽  
Potential Donor ◽  
X Ray ◽  
Distorted Octahedral ◽  
R Value

The crystal structure of Ni(dapsm)(NCS)2 [dapsm is 2,6-bis(1-methyl-4-methylthio-5-thia-2,3-diazahexa-1,3-dienyl)pyridinel has been determined from three-dimensional single-crystal diffractometer X-ray data. Structure refinement was carried out by least-squares methods to a final R value of 0.059. The ligand dapsm is a potential N3S2 pentadentate, but it coordinates as a tetradentate, giving a planar N3S donor grouping. Rotation occurs about an N-N bond in dapsm, moving a potential donor sulfur atom away from the nickel(II) ion. The pyridine ring of the ligand, and the N3S donor grouping, are approximately coplanar. Two thiocyanate groups are coordinated to the nickel, giving a distorted octahedral structure. The structure and electronic spectrum of Ni(dapsm)- (NCS)2 are compared with those for seven-coordinate complexes with the related N3O2 ligand, 2,6-diacetylpyridine bissemicarbazone.

Poly[[μ-(1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonato)]sodium]: a powder X-ray diffraction study

2013 ◽  
Vol 69 (8) ◽  
pp. 815-818 ◽  
Author(s):  
Mwaffak Rukiah ◽  
Thaer Assaad
Keyword(s):  
Hydrogen Bonding ◽  
Rietveld Method ◽  
Three Dimensional ◽  
Coordination Geometry ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

The title two-dimensional coordination polymer, [Na(C2H8NO6P2)]n, was characterized using powder X-ray diffraction data and its structure refined using the Rietveld method. The asymmetric unit contains one Na+cation and one (1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonate) anion. The central Na+cation exhibits distorted octahedral coordination geometry involving two deprotonated O atoms, two hydroxy O atoms and two double-bonded O atoms of the bisphosphonate anion. Pairs of sodium-centred octahedra share edges and the pairs are in turn connected to each other by the biphosphonate anion to form a two-dimensional network parallel to the (001) plane. The polymeric layers are connected by strong O—H...O hydrogen bonding between the hydroxy group and one of the free O atoms of the bisphosphonate anion to generate a three-dimensional network. Further stabilization of the crystal structure is achived by N—H...O and O—H...O hydrogen bonding.<!?tpb=18.7pt>

A new three-dimensional CdIIsupramolecular framework constructed from the 1-[(1H-tetrazol-5-yl)methyl]-1,4-diazoniabicyclo[2.2.2]octane ligand

2015 ◽  
Vol 71 (2) ◽  
pp. 93-96 ◽  
Author(s):  
Qiang Li ◽  
Hui-Ting Wang ◽  
Lin Zhou
Keyword(s):  
Crystal Packing ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Cl Atoms

A new tetrazole–metal supramolecular compound, di-μ-chlorido-bis(trichlorido{1-[(1H-tetrazol-5-yl-κN2)methyl]-1,4-diazoniabicyclo[2.2.2]octane}cadmium(II)), [Cd2(C8H16N6)2Cl8], has been synthesized and structurally characterized by single-crystal X-ray diffraction. In the structure, each CdIIcation is coordinated by five Cl atoms (two bridging and three terminal) and by one N atom from the 1-[(1H-tetrazol-5-yl)methyl]-1,4-diazoniabicyclo[2.2.2]octane ligand, adopting a slightly distorted octahedral coordination geometry. The bridging bicyclo[2.2.2]octane and chloride ligands link the CdIIcations into one-dimensional ribbon-like N—H...Cl hydrogen-bonded chains along thebaxis. An extensive hydrogen-bonding network formed by N—H...Cl and C—H...Cl hydrogen bonds, and interchain π–π stacking interactions between adjacent tetrazole rings, consolidate the crystal packing, linking the poymeric chains into a three-dimensional supramolecular network.

Synthesis, crystal structure and fluorescence spectrum of a cadmium(II) sulfaquinoxaline complex

2013 ◽  
Vol 69 (11) ◽  
pp. 1332-1335 ◽  
Author(s):  
Xiu-Hua Zhao ◽  
Ya-Yun Zhao ◽  
Jie Zhang ◽  
Jian-Guo Pan ◽  
Xing Li
Keyword(s):  
Thermal Analysis ◽  
Single Crystal ◽  
Fluorescence Spectrum ◽  
Chain Structure ◽  
Zigzag Chain ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

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.

Structure and redox properties of the molybdenum(IV) metal cluster K5[Mo3S4(CN)9].7H2O

1983 ◽  
Vol 36 (2) ◽  
pp. 377 ◽  
Author(s):  
NC Howlader ◽  
Jr GP Haight ◽  
TW Hambley ◽  
GA Lawrance ◽  
KM Rahmoeller ◽  
...  
Keyword(s):  
Equilateral Triangle ◽  
Metal Cluster ◽  
Saturated Calomel Electrode ◽  
Crystal Structure Analysis ◽  
Single Step ◽  
Redox Properties ◽  
Triclinic Space Group ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral

The anionic molybdenum(IV) cluster [Mo3S4(CN)9]5- has been subjected to X-ray crystal structure analysis. The potassium salt crystallized in the triclinic space group P1, a 10.634(1), b 11.888(3), c 24.892(2) �, α 89.56(2), β 79.86(1), γ 76.53(2)�, Z 4. The three MoIV atoms in each unit of approximately CSL3v symmetry are situated at the corners of an equilateral triangle with Mo-Mo distance 2.765(7) �. There are three S2- ligands bridging between pairs of Mo atoms, and a unique S2- ligand located uniformly above the plane of the equilateral triangle. Distorted octahedral coordination of each MoIV is completed by three CN- ligands to each of the three metal centres. The ion is structurally similar to the [MO3S(S2)6]2- precursor, and to [Mo3O4X9]n- analogues. In dimethyl sulfoxide, the cluster is irreversibly reduced in a single step near -2 V (v. saturated calomel electrode), but exhibits a quasi-reversible oxidation at + 0.51 V. On the coulometric time scale, the complex is irreversibly oxidized to MoV monomer.

Preparation and structure of mer-trichloro(acetonitrile)bis-(triphenylphosphine)osmium(III)

1980 ◽  
Vol 58 (10) ◽  
pp. 1042-1045 ◽  
Author(s):  
R. L. Parkes ◽  
N. C. Payne ◽  
E. O. Sherman
Keyword(s):  
Three Dimensional ◽  
Phosphine Ligands ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
The Mean ◽  
Bond Trans

An air-stable, red, crystalline, N-bonded acetonitrile complex of Os(III), OsCl3(NCCH3)(P(C6H5)3)2, has been prepared and characterized by elemental analysis, magnetic susceptibility, and a single crystal X-ray structure determination. Crystals are monoclinic, space group P21/c, cell dimensions a = 10.029(2), b = 15.233(2), c = 25.246(4) Å, β = 113.65(1)°, and Z = 4. Three dimensional X-ray diffraction intensity data were collected on an automatic four circle diffractometer using Cu radiation. Full-matrix least-squares refinement on F converged at R = 0.038 for 4384 unique observations. The Os atom has a slightly distorted octahedral coordination geometry, with trans phosphine ligands, mean Os—P 2.406(2) Å. The acetonitrile ligand is σ-bonded through the N atom, Os—N 2.038(6) Å. The bond trans to the acetonitrile ligand. Os—Cl(1) 2.364(2) Å, is not significantly different from the mean of the cisOs—Cl bonds, 2.361(2) Å.

The 125Te Mössbauer Absorption Spectra of Tellurium Complexes with Sulfur-Containing Ligands

1975 ◽  
Vol 53 (13) ◽  
pp. 1855-1860 ◽  
Author(s):  
Robert Michael Cheyne ◽  
Colin Henry Wilson Jones ◽  
Steinar Husebye
Keyword(s):  
Crystal Structure ◽  
Absorption Spectra ◽  
Structure Data ◽  
Mössbauer Spectra ◽  
Crystal Structure Data ◽  
X Ray ◽  
Mossbauer Spectra ◽  
Distorted Octahedral ◽  
Sulfur Containing ◽  
Bonding Scheme

The 125Te Mössbauer spectra of a number of Te(II) and Te(IV) complexes with sulfur-containing ligands have been measured. The Te(II) compounds exhibit large quadrupole splittings of 12.4 to 15.2 mm s−1 and isomer shifts (125I/Cu) of + 0.33 to + 0.91 mm s−1. These data are interpreted as evidence for the incorporation of some 5s character in the bonding scheme for several of the compounds, consistent with the interpretation of X-ray crystal structure data. For the Te(IV) compounds 6, 7, and 8 coordinate molecules have been studied containing tellurium in distorted octahedral, pentagonal bipyramidal, and dodecahedral coordination.

Synthesis, Crystal Structure and Luminescence Property on Cabazoly-Based Zinc Metal Organic Frameworks

2017 ◽  
Vol 727 ◽  
pp. 628-634
Author(s):  
Ying Jie Zhang ◽  
Li Xian Sun ◽  
Fen Xu
Keyword(s):  
Crystal Structure ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Zinc Metal ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
1D Chain ◽  
Metal Organic ◽  
Metal Charge Transfer

A novel zinc metal organic frameworks, named ZnL(2,2′-bpy), has been successfully synthesized, serving 3,6-dicarboxylic-9-ethylcarbazole acid (H2L) as ligand. This kind of ZnMOFs was characterized by FI-IR, elemental analysis, SEM, powder X-ray diffraction and single crystal X-ray diffraction to illustrate the structures. TG analysis was applied to investigate the thermostability. Structural analysis demonstrates that ZnMOFs possess triclinic crystal structure which is a 1D chain that occurs distorted-octahedral coordination geometry. Furthermore, the luminescent performance of ZnMOFs is performed and discussed in detail. The results show that ZnMOFs can emit blue luminescence originating, which is assigned to the ligand-to-metal charge transfer (LMCT).

Iron(II) and Nickel(II) Complexes of 4,4′-Bithiazole: Spectral, Magnetic and Structural Studies

1985 ◽  
Vol 38 (6) ◽  
pp. 851 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Bond Length ◽  
Least Squares ◽  
State Transitions ◽  
Structural Studies ◽  
Octahedral Structure ◽  
Thermally Induced ◽  
X Ray ◽  
Distorted Octahedral

Iron(II) and nickel(II) complexes of 4,4′-bithiazole (L) have been prepared. Salts of [FeL3]2+ undergo thermally induced spin-state transitions, in the solid state and in solution. The structures of both [FeL3] [ClO4]2 and [NiL3] [ClO4]2 have been determined by single-crystal X-ray diffractometry . The compounds are isomorphous : monoclinic with space group C2/c, with four molecules in a unit cell of dimensions (Fe, Ni): a 17.250(3), 17.379(3); b 9.8168(9), 9.685(1); c 16.867(3), 17.135(3) Ǻ; β 105.943(7), 104.860(7)°. The structures were refined by least-squares methods to residuals of 0.033 (Fe) and 0.033 (Ni) for 1917 (Fe) and 2017 (Ni) observed reflections. The cations have a distorted octahedral structure with the average Ni-N bond length being 0.11 Ǻ longer than the average Fe-N bond length.

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