Crystal Structure and Infrared Spectroscopy of
trans-[Cr(NCS)2(Me2tn)2][Cr(NCS)4(Me2tn)] Moiety

A novel double complex, trans-[Cr(NCS)2(Me2tn)2][Cr(NCS)4(Me2tn)]·NaSCN·i-PrOH, (1) (Me2tn = 2,2-dimethyl-1,3-propanediamine, C5H14N2; i-PrOH = isopropyl alcohol), was prepared and its structure was determined by single-crystal X-ray diffraction at 95 K. The complex 1 crystallized in the space group P1 of the triclinic system with two nuclear formula units in a cell of dimensions a = 13.220(3), b = 13.699(3), c = 15.087(3) Å and α = 116.193(3), β = 102.73(3) and γ = 104.48(3)°. X-ray structural analysis revealed two crystallo-graphically independent Cr(III) complex cations in the complex 1. The asymmetric unit contains two halves of trans-[Cr(NCS)2(Me2tn)2]+ cations (2 and 3), one cis-[Cr(NCS)4(Me2tn)]− anion (4), one NaSCN salt and one isopropyl alcohol molecule. In two independent complex cations, the chromium(III) ions are coordinated by four N atoms of two chelating Me2tn and two NCS groups in a distorted octahedral geometry while the chromium(III) ion in cis-[Cr(NCS)4(Me2tn)]- has a distorted octahedral coordination with two N atoms of one Me2tn and four NCS groups. The two six-membered rings in trans-[Cr(NCS)2(Me2tn)2]+ cations adopt both anti chair-chair conformations. The Cr–N(Me2tn) bond lengths range from 2.0624(18) to 2.0877(16) Å, while the Cr–N(NCS) bond lengths range from 2.0718(16) to 2.0428 (16) Å. The crystal lattice is stabilized by hydrogen bonding interactions among the NH groups of the Me2tn ligand, OH group of i-PrOH and the S atoms of the NCS groups. The infrared spectral properties are also described.

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The crystal and molecular structures of the bispyridine and 1,10-phenanthroline adducts of Bis(ethyl 3-mercaptobut-2-enoato)nickel(II)

Australian Journal of Chemistry ◽

10.1071/ch9820331 ◽

1982 ◽

Vol 35 (2) ◽

pp. 331 ◽

Cited By ~ 7

Author(s):

J Sachinidis ◽

MF Mackay ◽

MW Grant

Keyword(s):

Thermodynamic Data ◽

Molecular Structures ◽

Space Group ◽

X Ray ◽

Bond Lengths ◽

Crystal And Molecular Structures ◽

Distorted Octahedral ◽

In Cis ◽

Oxygen Atoms

X-ray analyses of monoclinic crystals of the bispyridine and 1,10-phenanthroline adducts of the monothioacetylacetonate complex bis(ethyl 3-mercaptobut-2-enoato)nickel(n), Ni(eosm)2,* have defined their structures. Crystals of the bispyridine adduct Ni(eosm)2,py2, C22H28N2NiO4S2, belong to the space group P21/c with a 8.865(6), b 15.758(4), c 9.136(3)Ǻ, β 109.18(4)°, Z 2. Crystals of the 1,10-phenanthroline adduct Ni(eosm)2,phen, C24H26N2NiO4S2, belong to the space group P21c with a 12.451(2), b 16.949(1), c 15 5921(2) Ǻ, β 130.97(1)°, Z 4. The structures were refined with diffractometer data measured with Cu Ka radiation to R 0.047 (1962 terms) for the bispyridine adduct and R 0.061 (3115 terms) for the phenanthroline adduct. The geometry about the nickel in each complex is distorted octahedral. The molecule of the bispyridine adduct has exact rn symmetry with the two sulfur atoms cis-equatorial and the nitrogen atoms axial. In the phenan- throline adduct, pairs of sulfur, nitrogen and oxygen atoms are in cis configurations. In the bis-pyridine adduct, the Ni-N bond lengths, 2.153(3) and 2.182(4) Ǻ, are significantly longer than those in other bispyridine adducts of nickel(II) species. It is suggested that the long Ni-N distances reflect the relative instability of the bispyridine adduct, and thermodynamic data are presented to support this.

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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

Zeitschrift für Naturforschung B ◽

10.1515/znb-2003-0913 ◽

2003 ◽

Vol 58 (9) ◽

pp. 916-921 ◽

Cited By ~ 3

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.

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Structure cristalline et moléculaire du cis-dithiocyanatobis(phénanthroline-1,10)mercure(II), Hg(SCN)2(C12H8N2)2

Canadian Journal of Chemistry ◽

10.1139/v74-426 ◽

1974 ◽

Vol 52 (16) ◽

pp. 2923-2927 ◽

Cited By ~ 7

Author(s):

André L. Beauchamp ◽

Bernard Saperas ◽

Roland Rivest

Keyword(s):

Heavy Atom ◽

Octahedral Geometry ◽

Van Der Waals Interactions ◽

Distorted Octahedral Geometry ◽

Triclinic Space Group ◽

Bond Lengths ◽

R Factor ◽

Distorted Octahedral ◽

Phenanthroline Ligands ◽

Heavy Atom Method

The compound cis-Hg(SCN)2(Phen)2 belongs to the triclinic space group [Formula: see text] with a = 13.252(5), b = 11.077(4), c = 8.443(3) Å, α = 105.20(3), β = 83.25 (3), γ = 90.92(3)°, and Z = 2. The structure was solved by the heavy atom method and refined on 1718 independent reflections to an R factor of 0.069. The crystal contains discrete molecules, in which mercury is coordinated to four nitrogen atoms from two phenanthroline molecules and to two sulfur atoms from thiocyanate groups. These donor atoms define a distorted octahedral geometry around mercury. The Hg—N bond lengths are in the range 2.42(2)–2.52(2) Å, whereas the Hg—S bonds are equal to 2.622(8) and 2.582(8) Å. The molecules are packed in layers parallel to the (110) planes and the layers are held together by normal van der Waals interactions. Within the layers, the packing of the complex is characterized by parallel stacking of phenanthroline ligands at distances of ∼3.4 Å. The terminal nitrogen atoms of the thiocyanate groups are uncoordinated.

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Synthesis and crystal structures of bis(imidazolidine-2-thione-κS)bis(thiocyanato-κS)mercury(II) and bis(cyanido)bis(μ2-imidazolidine-2-thione-κS)mercury(II).Hg(CN)2

Zeitschrift für Naturforschung B ◽

10.1515/znb-2017-0080 ◽

2017 ◽

Vol 72 (9) ◽

pp. 671-676 ◽

Cited By ~ 1

Author(s):

Muhammad Ashraf Shaheen ◽

Muhammad Nawaz Tahir ◽

Sarwat Sabir ◽

Aneela Anwar ◽

Anvarhusein A. Isab ◽

...

Keyword(s):

Rotation Axis ◽

Mercury Atom ◽

Distorted Octahedral Geometry ◽

Weakly Bound ◽

X Ray ◽

X Ray Crystallography ◽

Hydrogen Bonding Interactions ◽

Ir And Nmr Spectroscopy ◽

Distorted Octahedral ◽

Cyanide Ligands

AbstractTwo mercury(II) complexes containing imidazolidine-2-thione (Imt) and thiocyanate or cyanide ligands, [Hg(Imt)2(SCN)2] (1) and [Hg(Imt)2(CN)2].Hg(CN)2(2), have been prepared and characterized by IR and NMR spectroscopy and X-ray crystallography. In compound1, the mercury atom is located on a two-fold rotation axis and is coordinated to two thione sulfur atoms of imidazolidine-2-thione (Imt) and to two sulfur atoms of thiocyanate in a distorted tetrahedral mode with the S-Hg-S bond angles in the range of 98.96(3)–148.65(6)°. In2, the mercury atom is hexa-coordinated having a distorted octahedral geometry composed of two cyanide C atoms [Hg-C=2.055(5) Å] and four weakly bound thione S atoms of imidazolidine-2-thione (Imt) [Hg-S=3.1301(13) and 3.1280(13) Å]. One free Hg(CN)2molecule is also present in the crystal. In both complexes, the molecular structure is stabilized by N-H…N and N-H…S hydrogen bonding interactions.

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The Crystal Structure of KIO3.HIO3

Canadian Journal of Chemistry ◽

10.1139/v71-072 ◽

1971 ◽

Vol 49 (3) ◽

pp. 468-476 ◽

Cited By ~ 12

Author(s):

Lilian Y. Y. Chan ◽

F. W. B. Einstein

Keyword(s):

Crystal Structure ◽

Three Dimensional ◽

Monoclinic Space Group ◽

X Ray ◽

R Factor ◽

Octahedral Environment ◽

Distorted Octahedral ◽

Potassium Hydrogen ◽

A Cell ◽

Least Squares Techniques

The crystal structure of potassium hydrogen di-iodate (bi-iodate) KIO3.HIO3 was determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.0 % for the 1392 observed reflexions. The salt crystallizes in the monoclinic space group P21/c with eight formula units in a cell of dimension a = 7.028(1) Å, b = 8.203(1) Å, c = 21.841(3) Å, β = 98.03(1)°.The iodate units are all basically pyramidal; weak interionic I—O contacts complete a very distorted octahedral environment around three iodine atoms. There is a capped octahedral (7-coordinate) environment around the remaining iodine atom. The I—O bonds are in the range 1.75–1.82 Å and the I—OH bonds are 1.91 and 1.95 Å, variations in length can be correlated with differences in the degree of involvement in (a) hydrogen bonding and (b) interaction with adjacent iodine atoms.

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Crystal structure of the coordination compound of triiodidomethyltin(IV) with 2,2′-bipyridine, MeSnI3·bipy

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989015022975 ◽

2016 ◽

Vol 72 (1) ◽

pp. 17-20

Author(s):

Hans Reuter ◽

Martin Reichelt

Keyword(s):

Chelate Ring ◽

Octahedral Geometry ◽

Distorted Octahedral Geometry ◽

Orthorhombic Space Group ◽

Methyl Group ◽

Bond Lengths ◽

Distorted Octahedral ◽

Bipyridine Ligand ◽

Twisting Angle ◽

Van Der Waals Contacts

The title compound, (2,2′-bipyridine-κ2N,N′)triiodidomethyltin(IV), [Sn(CH3)I3(C10H8N2)], crystallizing in the non-centrosymmetric orthorhombic space groupPca21as an inversion twin, represents one of the few structurally characterized coordination compounds of an organotin(IV) trihalide with 2,2′-biypridine. Its distorted octahedral geometry shows a meridional arrangement of the I atoms and the methyl group is in-plane with the five-membered chelate ring. Asymmetric bonding of the biypridine ligand to the tin(IV) atom is reflected by different Sn—N bond lengths [2.268 (4) Åversus2.293 (4) Å] and caused by the statictranseffect of the methyl group. Sn—I bond lengths show some differences with respect to their orientation to the methyl group or the bipyridine ligand, respectively. Angular distortions in the coordination sphere of the SnIVatom mainly arise from the large I atoms. Distortion of the 2,2′-bipyridine ligand as a result of its coordination to the SnIVatom are described by the twisting angle of 2.5 (2)° between the least-squares planes of the two pyridine rings, as well as by the angle of 6.2 (2)° between the two lines through the pyridine-connecting C atoms and thepara-orientated C atoms. Directional intermolecular interactions are restricted to weak I...H van der Waals contacts.

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Synthesis and Structure of cis-Dioxobis(pyrimidine-2-thiolato-N,S)molybdenum(VI)

Australian Journal of Chemistry ◽

10.1071/ch9921933 ◽

1992 ◽

Vol 45 (11) ◽

pp. 1933 ◽

Cited By ~ 4

Author(s):

PR Traill ◽

AG Wedd ◽

ERT Tiekink

Keyword(s):

Least Squares ◽

Octahedral Geometry ◽

Distorted Octahedral Geometry ◽

Monoclinic Space Group ◽

Full Matrix ◽

X Ray ◽

Distorted Octahedral ◽

Cell Dimensions ◽

Unit Cell Dimensions

The characterization of two MoVI complexes, cis -[MoO2(2-pymS)2] and cis -[MoO2(2-pyS)2] (where 2-pymSH is pyrimidine-2-thiol and 2-pySH is pyridine-2-thiol), and their reaction with Ph3P are reported. The X-ray structure of cis -[MoO2(2-pymS)2] shows the molybdenum atom to exist in a distorted octahedral geometry defined by two mutually cis oxygen atoms and two chelating 2-pymS ligands so that the two sulfur atoms occupy approximate trans positions. Crystals of cis -[MoO2(2-pymS)2] are monoclinic, space group P 21/n, with unit cell dimensions: a 9.301(3), b 12.121(2), c 11.303(3) �, β 112.62(3)�, V 1176.3 �3, Z 4. The structure was refined by a full-matrix least-squares procedure to R 0.067 for 1858 reflections with I ≥ 2.5 (I).

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Dichlorido(η6-p-cymene)[tris(2-cyanoethyl)phosphine]ruthenium(II)

Molbank ◽

10.3390/m1025 ◽

2018 ◽

Vol 2018 (4) ◽

pp. M1025

Author(s):

William Henderson ◽

Ashwin Nair ◽

Nathan Halcovich ◽

Edward Tiekink

Keyword(s):

Mass Spectrometry ◽

Negative Ions ◽

Chloride Ion ◽

Distorted Octahedral Geometry ◽

X Ray ◽

X Ray Crystallography ◽

Mass Spectrometry Study ◽

Ruthenium Atom ◽

Distorted Octahedral ◽

Esi Mass Spectrometry

The tris(2-cyanoethyl)phosphine (tcep) complex [RuCl2{P(CH2CH2CN)3}(η6-p-cymene)] (p-cymene = p-CH3C6H4iPr) was synthesised by the bridge-splitting reaction of the chlorido-dimer [RuCl2(η6-p-cymene)]2 with tcep. The complex was characterised by a single-crystal X-ray structure determination as well as NMR spectroscopy, ESI mass spectrometry, and microelemental analysis. X-ray crystallography shows the ruthenium atom is coordinated by p-cymene in a η6-fashion, two chlorides and the phosphorus atom of the tcep ligand with the donor set defining a distorted octahedral geometry. The ESI mass spectrometry study reveals that the complex readily forms negative ions [M + Cl]− and [2M + Cl]− by association with a chloride ion.

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Reaction of 2-[(2-aminoethyl)amino]ethanol with pyridine-2-carbaldehyde and complexation of the products with CuII and CdII along with docking studies

Acta Crystallographica Section C Structural Chemistry ◽

10.1107/s2053229619008258 ◽

2019 ◽

Vol 75 (7) ◽

pp. 951-959 ◽

Cited By ~ 1

Author(s):

Zahra Mardani ◽

Mohammad Hakimi ◽

Keyvan Moeini ◽

Fabian Mohr

Keyword(s):

Crystal Packing ◽

Docking Studies ◽

Molar Ratio ◽

Distorted Octahedral Geometry ◽

X Ray Diffraction ◽

Donor Ligand ◽

X Ray ◽

H Nmr ◽

Distorted Octahedral ◽

Ft Ir

The reaction between 2-[2-(aminoethyl)amino]ethanol and pyridine-2-carbaldehyde in a 1:2 molar ratio affords a mixture containing 2-({2-[(pyridin-2-ylmethylidene)amino]ethyl}amino)ethanol (PMAE) and 2-[2-(pyridin-2-yl)oxazolidin-3-yl]-N-(pyridin-2-ylmethylidene)ethanamine (POPME). Treatment of this mixture with copper(II) chloride or cadmium(II) chloride gave trichlorido[(2-hydroxyethyl)({2-[(pyridin-2-ylmethylidene)amino]ethyl})azanium]copper(II) monohydrate, [Cu(C10H16N3O)Cl3]·H2O or [Cu(HPMAE)Cl3]·H2O, 1, and dichlorido{2-[2-(pyridin-2-yl)oxazolidin-3-yl]-N-(pyridin-2-ylmethylidene)ethanamine}cadmium(II), [CdCl2(C16H18N4O)] or [CdCl2(POPME)], 2, which were characterized by elemental analysis, FT–IR, Raman and 1H NMR spectroscopy and single-crystal X-ray diffraction. PMAE is potentially a tetradentate N3O-donor ligand but coordinates to copper here as an N2 donor. In the structure of 1, the geometry around the Cu atom is distorted square pyramidal. In 2, the Cd atom has a distorted octahedral geometry. In addition to the hydrogen bonds, there are π–π stacking interactions between the pyridine rings in the crystal packing of 1 and 2. The ability of PMAE, POPME and 1 to interact with ten selected biomolecules (BRAF kinase, CatB, DNA gyrase, HDAC7, rHA, RNR, TrxR, TS, Top II and B-DNA) was investigated by docking studies and compared with doxorubicin.

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Quinquedentate Coordination of 6-Methyl-1,11-dithia-4,8-diazacyclotetradecan-6-amine to Cobalt(III). X-Ray Crystal Structure of the [Co(N3S2)(OOCCH3)] (ClO4)2.H2O Complex

Australian Journal of Chemistry ◽

10.1071/ch9910113 ◽

1991 ◽

Vol 44 (1) ◽

pp. 113 ◽

Cited By ~ 8

Author(s):

GA Lawrance ◽

M Martinez ◽

BW Skelton ◽

AH White

Keyword(s):

Crystal Structure ◽

Metal Ion ◽

Crystal Structure Analysis ◽

Base Hydrolysis ◽

Distorted Octahedral Geometry ◽

Chloro Complex ◽

X Ray ◽

Group A ◽

Nitrogen Donors ◽

In Cis

The pendant arm macrocycle 6-methyl-1,11-dithia-4,8-diazacyclotetradecan-6-amine (7) can coordinate to cobalt(III) as a quinquedentate N3S2 ligand . Spectroscopy indicated a geometry with the macrocycle folded and the pendant amine and the unidentate donor in cis dispositions for the [Co(7) Cl ]2+ and [Co(7)(OOCCH3)]2+ products isolated. An X-ray crystal structure analysis of [Co(7)(OOCCH3)](ClO4)2.H2O characterized the cis stereochemistry. The complex crystallized in the Pbca space group, a 10.620(9), b 13.926(9), c 32.35(2)Ǻ, and analysis defined a distorted octahedral geometry with the primary and two secondary nitrogen donors occupying an octahedral face with relatively short Co-N bonds [1.937(7)-1.950(7)Ǻ], the acetate ion [Co-O 1.905(6)Ǻ] trans to one of the secondary amine donors and thioether donors [Co-S 2.223(3), 2.227(3)Ǻ] trans to the other nitrogen donors. Significant angle distortions occur around the metal ion. Base hydrolysis of the chloro complex is slow and stereoretentive , with a rate constant of 1.08×103 dm3 mol-1 s-1 at 25°C, 15-fold faster than for the pentaaza analogue.

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