Structural Characterization of Nickel(II) Tetraphenylporphyrin

1996 ◽  
Vol 49 (12) ◽  
pp. 1273 ◽  
Author(s):  
AL Maclean ◽  
GJ Foran ◽  
BJ Kennedy ◽  
P Turner ◽  
TW Hambley
Keyword(s):  
Synchrotron Radiation ◽  
Single Crystal ◽  
Bond Length ◽  
Diffraction Pattern ◽  
Structural Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Single Crystal Analysis

The structure of 5,10,15,20-tetraphenylporphinatonickel(II) ([Ni( tpp )]) has been studied by both X-ray diffraction (powder and single-crystal methods) and EXAFS. The bond lengths obtained from analysis of the EXAFS agree, within standard deviations, with those obtained from the X-ray diffraction studies. The Ni-N bond length of 1.93(1) Ǻ agrees especially well with the value of 1.931(2) Ǻ obtained from the single-crystal analysis. The powder X-ray diffraction pattern, collected by using synchrotron radiation, is presented.

The dinuclear scandium(III) cyclooctatetraenyl chloride complex di-μ-chlorido-bis[(η8-cyclooctatetraene)(tetrahydrofuran-κO)scandium(III)]

2017 ◽  
Vol 73 (5) ◽  
pp. 420-423 ◽  
Author(s):  
Zheng Zhou ◽  
Joshua Greenough ◽  
Zheng Wei ◽  
Marina A. Petrukhina
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Bond Length ◽  
Metal Ion ◽  
Chloride Complex ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Bond Lengths

Only a few cyclooctatetraene dianion (COT) π-complexes of lanthanides have been crystallographically characterized. This first single-crystal X-ray diffraction characterization of a scandium(III) COT chloride complex, namely di-μ-chlorido-bis[(η8-cyclooctatetraene)(tetrahydrofuran-κO)scandium(III)], [Sc2(C8H8)2Cl2(C4H8O)2] or [Sc(COT)Cl(THF)]2 (THF is tetrahydrofuran), (1), reveals a dimeric molecular structure with symmetric chloride bridges [average Sc—Cl = 2.5972 (7) Å] and a η8-bound COT ligand. The COT ring is planar, with an average C—C bond length of 1.399 (3) Å. The Sc—C bond lengths range from 2.417 (2) to 2.438 (2) Å [average 2.427 (2) Å]. Direct comparison of (1) with the known lanthanide (Ln) analogues (La, Ce, Pr, Nd, and Sm) illustrates the effect of metal-ion (M) size on molecular structure. Overall, the M—Cl, M—O, and M—C bond lengths in (1) are the shortest in the series. In addition, only one THF molecule completes the coordination environment of the small ScIII ion, in contrast to the previously reported dinuclear Ln–COT–Cl complexes, which all have two bound THF molecules per metal atom.

Synthesis and structural characterization of two copper(II) complexes with 3-(4-(1H-benzo[d]imidazol-1-yl)-4-methoxyphenyl)-1-phenylprop- 2-en-1-one ligands

2015 ◽  
Vol 70 (3) ◽  
pp. 165-169 ◽  
Author(s):  
Gao-Feng Wang
Keyword(s):  
Infrared Spectroscopy ◽  
Single Crystal ◽  
Structural Characterization ◽  
X Ray Diffraction ◽  
Distorted Octahedral Environment ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Elemental Analyses

AbstractThe synthesis of two new copper(II) complexes with benzimidazole type ligands, Cu(tta)2(L1)2 (1) and Cu(tta)2(L1) (2) (where L1 is 3-(4-(1H-benzo[d]imidazol-1-yl)-4-methoxy phenyl)-1-phenylprop-2-en-1-one; tta is 2-thenoyltrifluoroacetonate), are reported. Their structures have been characterized by infrared spectroscopy, elemental analyses and single-crystal X-ray diffraction. The copper(II) ion of 1 is in a distorted octahedral environment, while that of 2 is in a distorted square-pyramidal environment. In both cases, the donor atoms are provided by oxygen atoms of the tta ligands and nitrogen atoms of the L1 ligands.

Synthesis and Structural Characterization of Palladium Dicarbene Complexes Bearing Labile Co-Ligands

2009 ◽  
Vol 62 (9) ◽  
pp. 983 ◽  
Author(s):  
Han Vinh Huynh ◽  
Hui Xian Seow
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Metathesis Reaction ◽  
X Ray ◽  
Low Activity

Dicarbene complexes [Pd(OAc)2(diNHC)] (2), [Pd(O2CCF3)2(diNHC)] (3), and [Pd(CNCH3)2(diNHC)](SO3CF3)2 (4) bearing labile acetato, fluoroacetato, and acetonitrile co-ligands have been synthesized via metathesis reaction of the respective precursor [PdBr2(diNHC)] (1) with Ag-salts. All complexes are stable towards air and moisture and have been fully characterized by spectroscopic and spectrometric methods. Notably and in comparison to diphosphine analogues, they resist ligand disproportionation in solution. Their molecular structures have also been determined by single crystal X-ray diffraction. A preliminary catalytic study showed low activity in the hydroamination reaction, but revealed an interesting co-ligand influence.

Energetic Materials: The Preparation and Structural Characterization of Three Biguanidinium Dinitramides

1997 ◽  
Vol 53 (3) ◽  
pp. 504-512 ◽  
Author(s):  
A. Martin ◽  
A. A. Pinkerton ◽  
R. D. Gilardi ◽  
J. C. Bottaro
Keyword(s):  
Hydrogen Bonding ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Energetic Materials ◽  
Room Temperature ◽  
Asymmetric Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

Three biguanidinium salts of the energetic dinitramide anion have been prepared and structurally characterized from room-temperature X-ray diffraction data. Biguanidinium mono-dinitramide, (BIGH)(DN), triclinic, P\overline 1, a = 4.3686 (4), b = 9.404 (2), c = 10.742 (1) Å, \alpha = 83.54 (1), \beta = 80.386 (9), \gamma = 79.93 (1)°, V = 426.8 (1) Å3, Z = 2, D x = 1.62 g cm−3. Biguanidinium bis-dinitramide, (BIGH2)(DN)2, monoclinic, C2/c, a = 11.892 (2), b = 8.131 (1), c = 13.038 (2) Å, \beta = 115.79 (1)°, V = 1135.1 (3) Å3, Z = 4, D x = 1.84 g cm−3. Biguanidinium bis-dinitramide monohydrate, (BIGH2)(DN)2.H2O, orthorhombic, P212121, a = 6.4201 (6), b = 13.408 (1), c = 14.584 (2) Å, V = 1255.4 (4) Å3, Z = 4, D x = 1.76 g cm−3. All three structures are characterized by extensive hydrogen bonding. Both the mono- and diprotontated cations consist of two planar halves twisted with respect to each other. The dinitramide anion has a surprisingly variable and asymmetric structure. The two halves of the anion are twisted with respect to each other; however, the twist varies from 5.1 to 28.9°. In addition, the two ends of the anion have significantly different geometries, e.g. the `equivalent' N—N bond lengths differ by up to 0.045 Å.

scholarly journals STRUCTURAL CHARACTERIZATION OF 2-AMINO-2-OXOACETIC ACID BY X-RAY POWDER DIFFRACTION AND QUANTUM CHEMISTRY

2019 ◽  
Vol 16 (33) ◽  
pp. 516-523
Author(s):  
G. E. DELGADO ◽  
L. M. BELANDRIA ◽  
M. GUILLEN ◽  
A.. J. MORA ◽  
L. E. SEIJAS
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Structural Study ◽  
Powder Diffraction ◽  
Structural Characterization ◽  
Structure Determination ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
X Ray

2-amino-2-oxoacetic acid, carbamoyl formic acid, or oxamic acid is an active pharmaceutical ingredient (API) of great importance mainly because is an inhibitor of lactic dehydrogenase (LDH). It acts as an inhibitor to the metabolic pathways of the tumor cells and exhibited significant anticancer activity against nasopharyngeal carcinoma (NPC) cells in vitro and can be considered as a potential drug for the treatment of type 2 diabetes. Also, this compound could be used as a building block in the design of supramolecular architectures based on hydrogen bonds through the complimentary hydrogen-bond functionalities of the carbonyl and amide functional groups present. Single-crystal X-ray diffraction is the most powerful technique for crystal structure determination of small molecules. However, for several materials, including oxamic acid, it could be complicated to grow single crystals of suitable size and quality that make them appropriated to structure analysis. For this reason, the structural study was conducted with powder X-ray diffraction which is a process significantly more challenging than structure determination from single-crystal data. Oxamic acid has been characterized by FT-IR and NMR spectroscopic techniques, thermal TGA-DSC analysis, semi-empirical PM7 calculations, and X-ray powder diffraction. The title compound crystallizes in the monoclinic system with space group Cc, Z=4, and unit cell parameters a= 9.4994(4) Å, b= 5.4380(2) Å, c= 6.8636(3) Å, b= 107.149(2)°, V= 338.79(2) Å3. The molecule has a trans conformation. The molecular structure and crystal packing are stabilized mainly by intra- and intermolecular O--H···O and N--H···O hydrogen bonds. The structural characterization of this type of API compound is important to understand its mechanisms of action due to its considerable biological effects. In particular, for oxamic acid, this structural study would allow subsequent examination of its medicinal properties as an antitumor and antidiabetic agent.

Lewis-Base Adducts of Group-11 Metal(I) Compounds. XXXI. Reaction of 2,6-Bis[1-phenyl-1-(pyridin-2-Yl)ethyl]pyridine (L), and Copper(I) Halides in Acetonitrile: Structural Characterization of Salts of the [(MeCN)Cu(meso-L)]+ Cation

1987 ◽  
Vol 40 (11) ◽  
pp. 1881 ◽  
Author(s):  
AJ Canty ◽  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
NJ Minchin ◽  
...  
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Lewis Base ◽  
Tridentate Ligand ◽  
Acetonitrile Solution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ligand Conformation

Reaction of 2,6-bis[l-phenyl-1-(pyridin-2-yl)ethyl]pyridine, L, with copper(1) chloride, bromide, and iodide in acetonitrile solution has been shown to yield salts, structurally characterized by single-crystal X-ray diffraction methods as [( MeCN ) CuL ]+ [ ClCuCl ]-, (1), [( MeCN ) CuL ]+2 [XCuX2CuX]2-, X = Br (2), I (3) (both isomorphous ), all as yellow needles, and a form of (3), orange blocks, as the hemiacetonitrile solvate, (4), [( MeCN ) CuL ]+2 [IcuI2Cul]2-. MeCN . The same cation is common to all four species, containing four-coordinate copper(r), with L as meso -tridentate ligand; in (4), the most precisely defined example, Cu-N( MeCN ) is 1.919(5) �, the shortest copper(1) acetonitrile distance known, while Cu-N(L) are 2.065(5)-2.073(5) �. The reason for non-formation of species of the type [ LCuX ] appears to lie in the tridentate ligand conformation which permits coordination of acetonitrile but not larger halide species.

Synthesis and Structural Characterization of a Gallium(III) Bis(selenoureato) Complex

2013 ◽  
Vol 68 (1) ◽  
pp. 91-94 ◽  
Author(s):  
Anja Molter ◽  
Fabian Mohr
Keyword(s):  
Metal Complex ◽  
Single Crystal ◽  
Structural Characterization ◽  
Crystalline Compound ◽  
X Ray Diffraction ◽  
X Ray

In an attempt to prepare the tris(selenoureato)gallium(III) complex [Ga(4-O2NC6H4C(O)NC(Se)NEt2)3] from the reaction of the nitro-substituted acylselenourea 4-O2NC6H4C(O)NHC(Se)NEt2 with [Ga(NO3)3] in EtOH we obtained a crystalline compound from a CH2Cl2 solution which was identified as the bis(selenoureato)gallium(III)chlorido complex [GaCl(4- O2NC6H4C(O)NC(Se)NEt2)2] by single-crystal X-ray diffraction. This compound is a rare example of a metal complex containing chelating selenoureato ligands in a trans arrangement.

scholarly journals Synthesis and structural characterization of new polyether complexes of germanium(II) and tin(II)

2018 ◽  
Vol 96 (6) ◽  
pp. 570-577 ◽  
Author(s):  
Alina M. Secara ◽  
Justin F. Binder ◽  
Ala’aeddeen Swidan ◽  
Charles L.B. Macdonald
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Water Molecule ◽  
Single Crystal ◽  
Structural Characterization ◽  
X Ray Diffraction ◽  
X Ray

A series of germanium(II) and tin(II) bromide polyether complexes have been synthesized. Specifically, [GeBr([15]crown-5)][GeBr3], [GeBr([18]crown-6)][GeBr3], [GeBr(triglyme)][GeBr3], [GeBr(tetraglyme)][GeBr3], [SnBr([18]crown-6)][SnBr3], [Sn([15]crown-5)2][SnBr3]2, [SnBr(triglyme)][SnBr3], and [SnBr(tetraglyme)][SnBr3] have been fully characterized including by single crystal X-ray diffraction. The synthesis of [GeBr(dibenzo[24]crown-8)][GeBr3] and [GeCl(dibenzo[24]crown-8)][GeCl3] are also reported, along with the crystal structure of the latter’s water adduct, which features a water molecule adjacent to the GeCl+ ion within the cavity of the crown ether.

Synthesis and structural characterization of a Ni(II) coordination polymer with a tripodal 4-imidazolyl-functional ligand

2019 ◽  
Vol 74 (11-12) ◽  
pp. 857-860
Author(s):  
Hai-Wei Kuai ◽  
Xiao-Hong Zhu ◽  
Ding-Yun Jiang ◽  
Xiao-Chun Cheng ◽  
Deng-Hao Li
Keyword(s):  
Infrared Spectroscopy ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Network Structure ◽  
Structural Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
X Ray

Abstract1,3,5-Tri(1H-imidazol-4-yl)benzene (H3L) reacts with Ni(ClO4)2 · 6H2O under hydrothermal conditions at T = 100°C to yield a new complex: [Ni(H2L)2] · 5.5H2O (1). The product is characterized by single crystal and powder X-ray diffraction, infrared spectroscopy, and elemental and thermogravimetric analyses. Complex 1 crystallizes in the monoclinic space group C2/c and exhibits a binodal (3,6)-connected 2D kgd network structure with (43)2(46.66.83) topology.

Structural Characterization of a [Cl3CuL]- (L=Nitrogen Base) Species. A Novel Coordination Environment for Copper(II)

1985 ◽  
Vol 38 (5) ◽  
pp. 669 ◽  
Author(s):  
PC Healy ◽  
C Pakawatchai ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Structural Characterization ◽  
The Other ◽  
X Ray Diffraction ◽  
Nitrogen Base ◽  
Coordination Environment ◽  
X Ray

The crystal structure of [C13H10N] [CuCl3(C13H9N)].H2O(C13H9N ≡ acridine ) has been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to a residual of 0.037 for 1942 independent 'observed' reflections. Crystals are triclinic, Pī , a 16.27(2), b 10.080(8), c 7.236(5) Ǻ, α 88.85(6), β 82.68(8), γ 81.12(9)°, Z 2. The metal atom stereochemistry is unusual, being of pseudo-m symmetry; one of the chlorine atoms is coplanar with the copper and the acridine [Cu- Cl 2.237(2) Ǻ, N-Cu- Cl 143.5(1)°], with the other two disposed to either side of that plane [Cu- Cl 2.252(3), 2.243(2) Ǻ; Cl-Cu-Cl 145.62(7)°]. Cu-N is 2.018(5) Ǻ.

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