Nickel(II) and iron(II) complexes of 4-(Pyridin-2-yl)thiazole: Spectral, magnetic and structural studies

1984 ◽  
Vol 37 (12) ◽  
pp. 2431 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin ◽  
AD Rae
Keyword(s):  
Solid State ◽  
Electronic Spectrum ◽  
Spin Transition ◽  
Monoclinic Space Group ◽  
Structural Studies ◽  
Octahedral Structure ◽  
Coordination Environment ◽  
Disordered Structure ◽  
Distorted Octahedral ◽  
Symmetric Ligands

Iron(II) and nickel(II) complexes of 4-(pyridin-2-yl)thiazole (L) have been prepared. The electronic spectrum of [NiL3] [ClO2,]2 is similar to that of the corresponding complex of 2,2'-bipyridine (bpy) but indicates that the thiazole provides the weaker field, the actual value of Dq(Ni2+) being within the range which suggests the likely appearance of a spin transition in iron(III). The iron(II) complexes [FeL3] X2 (X = ClO4, BF4) are, however, low-spin both in the solid state and in solution. The structure of [NiL3] [ClO4]2.3H2O has been determined, and this reveals a close similarity in the coordination environment to that in [Ni(bpy),] SO4.7.5H2O. The compound is monoclinic, space group P21/c, with four molecules in a unit cell of dimensions a 9.404(4), b 29.169(8), c 17.900(8)ź, β 137.76(1)�. The disordered structure was refined to a residual R 0.087 for 2307 observed reflections. The pseudo-symmetric ligands are orientationally disordered and one anion was also disordered. Restrained refinement with 194 parameters for 85 atomic positions produced a reliable geometry. The ligands function as bidentates, giving the cation a distorted octahedral structure.

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.

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.

The 119Sn Mössbauer and solid-state NMR and the crystal and molecular structure of tin(II) bisfluorosulfate, Sn(OSO2F)2

1991 ◽  
Vol 69 (12) ◽  
pp. 2122-2126 ◽  
Author(s):  
David C. Adams ◽  
Thomas Birchall ◽  
Romolo Faggiani ◽  
Ronald J. Gillespie ◽  
John E. Vekris
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Three Dimensional ◽  
Lone Pair ◽  
Monoclinic Space Group ◽  
Bridging Ligands ◽  
Nmr Spectrum ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
The Mean

The reaction of tin(II) fluoride with fluorosulfuric acid has been shown to produce tin(II) bisfluorosulfate. Crystals of Sn(OSO2F)2 are monoclinic, space group P21/c with a = 5.195(1), b = 9.709(1), c = 13.861(1) Å, β = 110.12(1)°, Z = 4, R = 0.029, and Rw = 0.030 for 1461 unique reflections. The structure consists of a three-dimensional framework of fluorosulfate groups linked by O—Sn—O bridges with the two crystallographically independent fluorosulfates acting as tridentate bridging ligands between tin atoms. There are four short bonds (Sn—O = 2.338(3), 2.350(3), 2.398(4), and 2.427(3) Å) and two longer ones (Sn—O = 2.695(3) and 2.702(3) Å) around tin. The four short bonds have a disphenoidal, AX4E, primary geometry with the lone pair occupying an equatorial site. If the two longer interactions are also considered the geometry is distorted octahedral, AX4Y2E. Two more non-bonding contacts of 3.420(4) and 3.319(4) Å complete an approximately dodecahedral arrangement of oxygen atoms around the tin. The fluorosulfate groups deviate significantly from C3υ symmetry and have the mean dimensions, S(1)—O = 1.419(4), S(1)—F = 1.541(4), S(2)—O = 1.435(3), S(2)—F = 1.539(3) Å, O—S(1)—O = 114.3(2)°, F—S(1)—O = 104.1(3)°, O—S(2)—O = 114.2(2)°, and F—S(2)—O = 104.1(2)°, respectively. The solid-state 119Sn nmr spectrum shows only one single resonance with a shift of −1534 ppm which is substantially different from that of a solution in HSO3F. The 119Sn Mössbauer spectrum shows an unresolved quadrupole splitting as a result of a distorted environment around tin, produced by the stereochemically active non-bonding electron pair. Key words: tin(II) bisfluorosulfate, 119Sn Mössbauer, solid-state nmr, X-ray crystallography

Cs2.91Na1.34Fe3+0.25[Fe3O(SO4)6(H2O)3]·5H2O, a member of the Maus's salt family

2013 ◽  
Vol 69 (10) ◽  
pp. 1085-1090 ◽  
Author(s):  
Kurt Mereiter
Keyword(s):  
Three Dimensions ◽  
Octahedral Coordination ◽  
Monoclinic Space Group ◽  
Coordination Environment ◽  
Clear Cut ◽  
Cation Disorder ◽  
Distorted Octahedral ◽  
The Family ◽  
Set Up ◽  
Cation Sites

The title compound, tricaesium sodium iron(III) μ3-oxido-hexa-μ2-sulfato-tris[aquairon(III)] pentahydrate, Cs2.91Na1.34Fe3+0.25[Fe3O(SO4)6(H2O)3]·5H2O, belongs to the family of Maus's salts, K5[Fe3O(SO4)6(H2O)3]·6H2O, which is based on the triaqua-μ3-oxido-hexa-μ-sulfato-triferrate(III) anion, [Fe3O(SO4)6(H2O)3]5−, with Fe in a characteristically distorted octahedral coordination environment, sharing a common cornerviaan oxide O atom. Cs in four different cation sites, Na in three different cation sites and five water molecules link the anions in three dimensions and set up a crystal structure in which those parts parallel to (001) and within 0.05 <z< 0.95 have a distinct trigonal pseudosymmetry, whereas the cation arrangement and bonding nearz∼ 0 generate a clear-cut noncentrosymmetric polar edifice with the monoclinic space groupC2. The structure shows some cation disorder in the region nearz ∼ {1\over 2}, where one Na atom in octahedral coordination is partly substituted by Fe3+, and a Cs atom is substituted by small amounts of Na on a separate nearby site. One Na atom, located on a twofold axis atz= 0 and tetrahedrally coordinated by four sulfate O atoms of two [Fe3O(SO4)6(H2O)3]5−units, plays a key role in generating the noncentrosymmetric structure. Three of the seven different cation sites are on twofold axes (one Na+site and two Cs+sites), and all other atoms of the structure are in general positions.

Synthesis, Characterisation and Structural Studies of [Zn(phen)3][Fe(CN)5(NO)]·2H2O·0.25MeOH and [(bipy)2(H2O)Zn(μ-NC)Fe(CN)4(NO)]·0.5H2O

2003 ◽  
Vol 58 (9) ◽  
pp. 916-921 ◽  
Author(s):  
Amitabha Datta ◽  
Samiran Mitra ◽  
Georgina Rosair
Keyword(s):  
Infrared Spectroscopy ◽  
Thermogravimetric Analysis ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Structural Studies ◽  
Crystal Lattices ◽  
X Ray ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Solvent Molecules

Two new bimetallic complexes [Zn(phen)3][Fe(CN)5(NO)] · 2 H2O · 0.25 MeOH, (1) and [(bipy)2(H2O)Zn(μ-NC)Fe(CN)4(NO)] · 0.5 H2O, (2), have been isolated (where phen = 1,10-phenanthroline and bipy = bipyridyl) and characterised by X-ray crystallography [as the 2 H2O · 0.25 CH3OH solvate for (1) and hemihydrate for (2)] infrared spectroscopy and thermogravimetric analysis. Substitution of phenanthroline for bipyridyl resulted in a cyano-bridged bimetallic species rather than two discrete mononuclear metal complexes. The bond angles of Fe-N-O were shown to be practically linear for both 1 [179.2(7)°] and 2 [178.3(3)°], and the Zn atoms have distorted octahedral geometry. The solvent molecules in both crystal lattices take part in forming hydrogen-bonded networks.

Structural studies of oriented zirconium bis(phosphonoacetic acid) using solid-state phosphorus-31 and carbon-13 NMR

1992 ◽  
Vol 114 (11) ◽  
pp. 4144-4150 ◽  
Author(s):  
David A. Burwell ◽  
Kathleen G. Valentine ◽  
Jozef H. Timmermans ◽  
Mark E. Thompson
Keyword(s):  
Solid State ◽  
Structural Studies ◽  
Phosphonoacetic Acid

Comparative Structural Studies on Three-Coordinate Copper(I) Halide Complexes With Tertiary Phosphines. Crystal Structures of [(PPh2Mes)CuX]2 and [(PPhMes2)CuX]2 (Mes = Mesityl X = Cl, Br, I)

1992 ◽  
Vol 45 (7) ◽  
pp. 1155 ◽  
Author(s):  
GA Bowmaker ◽  
D Camp ◽  
RD Hart ◽  
PC Healy ◽  
BW Skelton ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Copper Atom ◽  
Structural Studies ◽  
Coordination Environment ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Structure Determinations ◽  
Halide Complexes ◽  
The Subject

The 1 : 1 complexes of the substituted triphenylphosphine ligands mesityldiphenylphosphine and dimesitylphenylphosphine with copper(1) chloride, bromide and iodide have been the subject of single-crystal X-ray structure determinations at 295 K. All six complexes crystallize as air-stable dimeric molecules, [(PPh2Mes)CuX]2 and [ (PPhMes2)CUX]2 with each copper atom in a distorted trigonal PCuX2. coordination environment. Crystals of [(PPh2Mes)CuCl]2 (1) are monoclinic, P21/n, a 9.961(3), b 18.687(6), c 11.009(7) Ǻ, β 114.63(4)°; R was 0.049 for 2450 'observed' reflections. [(PPh2Mes)CuBrI2 (2) is monoclinic, P21/n, a 9.939(2), b 18.832(6), c 11.238(6) Ǻ, β 115.36(3)°; R was 0.046 for 1803 'observed' reflections. [(PPh2Mes)CuI]2.4/3 C6H6 (3) is rhornbohedral, R3, a 36.877(8), c 9.047(5) A; R was 0.039 for 2537 'observed' reflections. Crystals of [(PPhMes2)CuCl]2.2MeCN (4) are triclinic, Pi, a 15.783(7), b 9.570(4), c 8.914(4) Ǻ, α 72.43(3), β 76.37(3), γ 74.03(3)°; R was 0.045 for 3341 'observed' reflections. [(PPhMes2)CuBr]2.3C6H6 (5) is monoclinic, C2/c, a 9.694(6), b 30.15(2), c 20.66(2) Ǻ, β 98.00(7)°; R was 0.047 for 2117 'observed' reflections. [(PPhMes2)CuI]2.2MeCN (6) is orthorhombic, PP1nb, a 11.694(8), b 14.77(1), c 29.76(3) Ǻ; R was 0.049 for 3447 'observed' reflections. Cu-P bond lengths are: 2.196(2) A (1); 2.198(3) Ǻ (2); 2.222(5) and 2.226(5) Ǻ (3); 2.202(1) Ǻ (4); 2.197(3) A (5); 2.201(4) and 2.264(5) Ǻ (6). The geometries of the LCuX2 and CuX2Cu units are compared with data reported for other monomeric and dimeric compounds for both phosphorus- and nitrogen-based ligands L.

(Acetylacetonato-κ2O,O′)[1-(4-bromophenyl-κC2)-3-methylimidazol-2-ylidene-κC2]platinum(II)

2012 ◽  
Vol 68 (8) ◽  
pp. m203-m205 ◽  
Author(s):  
Mario Tenne ◽  
Yvonne Unger ◽  
Thomas Strassner
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Intermolecular Hydrogen Bonding ◽  
Coordination Environment ◽  
Π Interactions ◽  
New Class ◽  
Square Planar ◽  
Parallel Fashion

The title platinum(II) complex, [Pt(C10H8BrN2)(C5H7O2)], has a bidentate cyclometallated phenylimidazolylidene ligand and an acetylacetonate spectator ligand, which form a distorted square-planar coordination environment around the PtIIcentre. In the solid state, the molecules are oriented in a parallel fashion by intermolecular hydrogen bonding and π–π and C—H...π interactions, while close Pt...Pt contacts are not observed. The structure is only the second example for this new class of compounds.

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