Fluctuations between square-planar and tetrahedral coordination geometry with bis(2-benzimidazolyl)alkane ligands. Synthesis, spectroscopic properties and X-ray crystal structure of four representative examples

1999 ◽  
Vol 290 (1) ◽  
pp. 105-112 ◽  
Author(s):  
Gerard A. van Albada ◽  
Wilberth J.J. Smeets ◽  
Nora Veldman ◽  
Anthony L. Spek ◽  
Jan Reedijk
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Properties ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
X Ray ◽  
Square Planar

Synthesis and X-ray crystal structure of the novel Mo—Cu complex, (Ph2PCH2CH2PPh2)2Cu+[(HBpz″3)Mo(CO)3]2Cu−(where pz″ = 3,5-dimethylpyrazolyl, N2C5H7)

1988 ◽  
Vol 66 (9) ◽  
pp. 2194-2199 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
The Novel ◽  
Tetrahedral Coordination ◽  
X Ray ◽  
Carbonyl Ligands ◽  
Cu Complex ◽  
Anionic Ligand ◽  
Average Bond

The novel complex, (Ph2PCH2CH2PPh2)2Cu+[(HBpz″3)Mo(CO)3]2Cu− (where pz″ = 3,5-dimethylpyrazolyl), has been synthesized by reacting the (HBpz″3)Mo(CO)3− anionic ligand with CuI in the presence of a stoichiometric amount of Ph2PCH2CH2PPh2. Crystals of (Ph2PCH2CH2PPh2)2Cu+[(HBpz″3)Mo(CO)3]2Cu−•3.5C6H6•CH2Cl2 are triclinic, a = 13.421(1), b = 14.931(3), c = 28.523(5) Å, α = 90.41(2), β = 90.19(1), γ = 104.65(1)°, Z = 2, space group [Formula: see text] The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.047 and Rw = 0.049 for 8779 reflections with I ≥ 3σ(I). The crystal structure consists of (Ph2PCH2CH2PPh2)2Cu+ cations having irregular tetrahedral coordination geometry about the copper atom (Cu—P = 2.263(2)–2.304(2) Å and P—Cu—P = 88.30(7)–134.62(8)°) and novel [(HBpz″3)Mo(CO)3]2Cu− anions having exact Ci and approximate D3d symmetry. The central Cu atom of the anion is bonded to two Mo atoms in a linear fashion and also interacts with six semi-bridging carbonyl ligands, three from each (HBpz″3)Mo(CO)3− ligand. Average bond lengths and angles for the anion are Mo–Cu = 2.565, Mo—C = 1.955, Mo—N = 2.256, Cu—C = 2.309, C—O = 1.174 Å, Mo—C—O = 171.7° and Cu—C—O = 114.7°.

scholarly journals Crystal structure of a new mixed-metal coordination polymer consisting of NiII piperidine-dithiocarbamate and pentanuclear CuI—I cluster units

2018 ◽  
Vol 74 (2) ◽  
pp. 233-236
Author(s):  
Kento Himoto ◽  
Toshiya Horii ◽  
Shoki Oda ◽  
Shimpei Suzuki ◽  
Kunihisa Sugimoto ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Coordination Polymer ◽  
Chain Structure ◽  
Mirror Plane ◽  
Zigzag Chain ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Square Planar ◽  
Cluster Unit ◽  
Distorted Tetrahedral Coordination

A new heterometallic CuI–NiII coordination polymer, poly[[tetra-μ3-iodido-μ2-iodido-bis(μ3-piperidine-1-dithiocarbamato)propionitrilepentacopper(I)nickel(II)] chloroform monosolvate], {[CuI 5NiIII5(C6H10NS2)2(C3H5N)]·CHCl3} n , has been synthesized and structurally characterized. This coordination polymer consists of an NiII mononuclear unit of NiII(Pip-dtc)2 (Pip-dtc− is piperidine-1-dithiocarbamate) and a pentanuclear copper(I) cluster unit of Cu5I5(CH3CH2CN). The NiII ion, which lies on an inversion centre, is surrounded by four S atoms in a square-planar coordination geometry while all CuI ions have distorted tetrahedral coordination geometries. In the pentanuclear copper(I) cluster unit, a mirror plane passes through one CuI ion and three I ions. All the S atoms in NiII(Pip-dtc) are also coordinated by the CuI ions, forming an infinite zigzag chain structure along the b-axis direction. The chains are weakly connected by solvent CHCl3 molecules via Cl...I [3.653 (1) Å] and Cl...S [3.4370 (1) Å] short-contact interactions.

scholarly journals Crystal structure of bis(tetramethylthiourea-κS)bis(thiocyanato-κN)nickel(II)

2020 ◽  
Vol 76 (12) ◽  
pp. 1841-1845
Author(s):  
Aleksej Jochim ◽  
Rastko Radulovic ◽  
Inke Jess ◽  
Christian Näther
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Rotational Axis ◽  
Coordination Geometry ◽  
Asymmetric Unit ◽  
Hydrogen Atoms ◽  
Thiourea Derivatives ◽  
X Ray ◽  
Square Planar

In the course of our investigations regarding transition-metal thiocyanates with thiourea derivatives, the title compound, [Ni(NCS)2(C5H12N2S)2], was obtained. The asymmetric unit consists of one thiocyanate anion and one tetramethylthiourea molecule on general positions, as well as one NiII cation that is located on a twofold rotational axis. In this compound, discrete complexes are formed in which the NiII cations are surrounded by two trans-N-bonding thiocyanate anions as well as two trans-S-bonding tetramethylthiourea molecules within a distorted square-planar coordination geometry. The discrete complexes are linked by pairs of weak C—H...S hydrogen bonds between the thiocyanate S and one of the tetramethylthiourea methyl hydrogen atoms into chains along the crystallographic a- and c-axis directions, which are combined into layers parallel to the ac plane. X-ray powder diffraction proves that a pure crystalline phase was obtained and measurements using thermogravimetry and differential thermoanalysis reveal that the compound decomposes at about 408 K, where all tetramethylthiourea molecules are lost.

Systhesis, Characterization and Spectroscopic Properties of (2E,6E)-2,6-Bis(2,3,4-tri-methoxy-benzylidene)cyclohexanone

2011 ◽  
Vol 396-398 ◽  
pp. 2338-2341
Author(s):  
Xing Chuan Wei ◽  
Zhi Li Liu ◽  
Kun Zhang ◽  
Zhi Yun Du ◽  
Xi Zheng
Keyword(s):  
Crystal Structure ◽  
Acetic Acid ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Spectroscopic Properties ◽  
Spectral Studies ◽  
Double Bonds ◽  
X Ray ◽  
Π Interactions ◽  
X Ray Crystallography

In this paper, (2E,6E)-2,6-Bis(2,3,4-tri-methoxy -benzylidene)cyclohexanone (omitted as tmbcho) (1) was obtained by the reaction of acetic acid, tetrahydrofuran, cyclohexanone and 2,3,4-tri-methoxy-benzaldehyde. Three non-classic hydrogen bonds were observed in the compound. X-ray crystallography shows that the crystal structure is stabilized by intermolecular C-H•••π interactions and it contains plenty of conjugated double bonds. The title compound was characterized by UV-vis and fluorescent spectral studies.

Crystal Structure, Spectroscopic and Redox Properties of Copper(II) Bis{2-[(2,6-dimethylphenyl)iminomethyl-3-methoxyphenolate]}

2007 ◽  
Vol 62 (9) ◽  
pp. 1133-1138 ◽  
Author(s):  
Veli T. Kasumov ◽  
Ibrahim Uçar ◽  
Ahmet Bulut ◽  
Fevzi Kösal
Keyword(s):  
Crystal Structure ◽  
Title Complex ◽  
Redox Properties ◽  
Orthorhombic Space Group ◽  
Long Distance ◽  
X Ray ◽  
X Ray Crystallography ◽  
Square Planar ◽  
Planar Molecules ◽  
Exchange Interaction Parameter

The coordination chemistry of N-(2,6-di-methylphenyl)-2-hydroxy-3-methoxybenzaldimine (1) with Cu(II) has been investigated by X-ray crystallography, electronic and EPR spectroscopies, as well as by electro- and magnetochemistry. The title complex 2 crystallizes in the orthorhombic space group P212121 (a = 8.1538, b = 17.7466, c =19.8507 Å). The mononuclear square-planar molecules 2 featuring trans-N2O2 coordination are connected via weak intermolecular C-H· · ·π interactions into infinite chains parallel to the a axis. Although the intermolecular Cu· · ·Cu separations within individual chains and between chains are very long (8.154 and 9.726 Å ), the exchange interaction parameter G = 2.03 < 4, estimated from solid state EPR spectra, suggests the existence of long-distance superexchange pathways between adjacent Cu(II) centers. The electronic and electrochemical features of the compound are also discussed.

The molecular and crystal structure of [Pt(diethylenetriamine)(guanosine)](ClO4)2

1979 ◽  
Vol 57 (1) ◽  
pp. 57-61 ◽  
Author(s):  
R. Melanson ◽  
F. D. Rochon
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Least Squares ◽  
Platinum Atom ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
R Factor ◽  
Square Planar ◽  
Coordination Plane

The crystal structure of [Pt(diethylenetriamine)(guanosine)](ClO4)2 has been determined by X-ray diffraction. The crystals are orthorhombic, space group P212121, with a = 12.486(6), b = 13.444(7), c = 14.678(11) Å, and Z = 4. The structure was refined by block-diagonal least-squares analysis to a conventional R factor of 0.050 and a weighted Rw = 0.045.The coordination around the platinum atom is square planar. Guanosine is bonded to platinum through N(7). The purine planar ring makes an angle of 62.7° with the platinum coordination plane. The structure is stabilized by hydrogen bonding.

scholarly journals Comparison of molecular structures of cis-bis[8-(dimethylphosphanyl)quinoline]nickel(II) and -platinum(II) complex cations

2020 ◽  
Vol 76 (12) ◽  
pp. 1813-1817
Author(s):  
Masatoshi Mori ◽  
Takayoshi Suzuki
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Steric Hindrance ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Donor Group ◽  
Bending Deformation ◽  
Bond Lengths ◽  
Square Planar ◽  
Chelate Ligands

The crystal structures of the complexes (SP-4-2)-cis-bis[8-(dimethylphosphanyl)quinoline-κ2 N,P]nickel(II) bis(perchlorate) nitromethane monosolvate, [Ni(C11H12NP)2](ClO4)2·CH3NO2 (1), and (SP-4-2)-cis-bis[8-(dimethylphosphanyl)quinoline-κ2 N,P]platinum(II) bis(tetrafluoroborate) acetonitrile monosolvate, [Pt(C11H12NP)2](BF4)2·C2H3N (2), are reported. In both complex cations, two phosphanylquinolines act as bidentate P,N-donating chelate ligands and form the mutually cis configuration in the square-planar coordination geometry. The strong trans influence of the dimethylphosphanyl donor group is confirmed by the Ni—N bond lengths in 1, 1.970 (2) and 1.982 (2) Å and, the Pt—N bond lengths of 2, 2.123 (4) and 2.132 (4) Å, which are relatively long as compared to those in the analogous 8-(diphenylphosphanyl)quinoline complexes. Mutually cis-positioned quinoline donor groups would give a severe steric hindrance between their ortho-H atoms. In order to reduce such a steric congestion, the NiII complex in 1 shows a tetrahedral distortion of the coordination geometry, as parameterized by τ4 = 0.199 (1)°, while the PtII complex in 2 exhibits a typical square-planar coordination geometry [τ4 = 0.014 (1)°] with a large bending deformation of the ideally planar Me2Pqn chelate planes. In the crystal structure of 2, three F atoms of one of the BF4 − anions are disordered over two sets of positions with refined occupancies of 0.573 (10) and 0.427 (10).

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