Complexes of cobalt(II), nickel(II) and copper(II) with a pentadentate Bis(β-amino ketone); Crystal and molecular structure of Aqua(4,4,12,12-tetramethyl-5,8,11-triazapentadecane-2,14-dione)cobalt(II) perchlorate hydrate

1982 ◽  
Vol 35 (6) ◽  
pp. 1105 ◽  
Author(s):  
KR Morgan ◽  
GJ Gainsford ◽  
NF Curtis
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Complex Cation ◽  
Carbonyl Oxygen ◽  
Amino Ketone ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
Imine Ligands ◽  
Pentadentate Ligand

The diperchlorate salts of the mono(β-amino ketone) 10-amino-4,4-dimethyl-5,8-diazadecan-2-one and of the bis(β-amino ketone) 4,4,12,12-tetramethyl-5,8,11-triazapentadecane-2,14-dione, ttp, have been prepared by reaction of the diperchlorate of 3-azapentane-1,5-diamine with acetone. The salt [ttpH2] (ClO4)2 has been used to prepare the six-coordinate complexes [Cu(ttp)(H2O)] (ClO4)2,1.5H2O and [Ni(ttp)(H2O)] (ClO4)2,H2O, and the five-coordinate [Cu(ttp)] (CIO,),. The complex [Cu(ttp)] (ClO4), reacts with ammonia, methylamine and ethylamine to form complexes of pentadentate β-amino ketone β-amino imine ligands. The structure of [Co(ttp)(H2O)] (ClO4)2,1.5H2O has been determined by X-ray diffractometry [space group P21/c, Z 4, a 797.5(2), b 1632.8(3), c 2236.4(3) pm, β 97.504(2)�, R 0.0749, Rw 0.0765 for 1678 reflections]. The complex cation has the bis(β-amino ketone) ttp acting as a pentadentate ligand, with the three nitrogen and one carbonyl oxygen atoms coplanar, and with oxygen of a water molecule completing distorted octahedral coordination about the cobalt(II) ion.

Phenylimido complexes of tungsten(VI) and tungsten(V). The crystal and molecular structure of Trichloro(phenylimido)bis(trimethylphosphine)tungsten(V)

1983 ◽  
Vol 36 (2) ◽  
pp. 243 ◽  
Author(s):  
AJ Nielson ◽  
JM Waters
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Multiple Bond ◽  
Coordination Geometry ◽  
Fourier Methods ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Tetrahydrofuran Solution

Tetrachloro(phenylimido)tungsten(VI) is reduced by trimethylphosphine in tetrahydrofuran solution to give the tungsten(V) complex PhNWCl3(Pme3)2 in which the phenylimido multiple bond remains intact. The complex reacts with oxygen to form the phosphine oxide complex PhNWCl3 (OPMe3)2. Pyridine and alkyl cyanides do not reduce tetrachloro(phenylimido)tungsten(V1) but give the adducts PhNWCl4.L (L = py, MeCN, EtCN). The crystal and molecular structure of the title complex has been determined from single-crystal X-ray diffractometer data. The crystals are monoclinic with a 14.903, b 10.221, c 14.380Š β 116.05�, space group P21/c, Z 4. The structure has been solved by Patterson and Fourier methods and refined to R 0.030 for the 1566 observed data. Distorted octahedral coordination geometry is found with two trans trimethylphosphine and two trans chloride ligands; a third chloride is trans to the phenylimido group. The W-N(imido) bond length is 1.731 �.

Synthesis, IR and X-Ray Studies of Tetra(N,N′-tetraethyl-N″-benzoyl- phosphorictriamide)-tetra(μ-3-methoxo)-tetra(methanol)tetra-NickeI(II)

1998 ◽  
Vol 53 (8) ◽  
pp. 836-840 ◽  
Author(s):  
Vladimir A. Ovchynnikov ◽  
Vladimir M. Amirkhanov ◽  
Anatoliy A. Kapshuk ◽  
Tatyana Yu. Sliva ◽  
Tadeusz Glowiak ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Oxygen Atom ◽  
Metal Ion ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Methoxy Groups ◽  
Oxygen Atoms

Abstract A new nickel(II) complex with N,N′-tetraethyl-N″-benzoylphosphortriamide (HL = C6H5C(O)N(H)P(O)(NEt2)2) of composition Ni4L4(OCH3)4·(HOCH3)4 (1) has been synthe­ sized. The crystal and molecular structure of 1 has been determined from the X-Ray diffraction data (tetragonal, space group P4̄21c with a = 17.000(2) Å, c = 15.338(3) Å, Z = 2; R = 0.0399 for 1412 unique reflections). The structure is made up of cubane-like tetramers. In the corners of a cube there are 4 atoms of nickel and 4 atoms of oxygen of methoxy groups. The nickel atoms are characterized by a slightly distorted octahedral environment, which consists of three oxygen atoms of methoxy groups, carbonylic and phosphorylic oxygen atoms of the ligand L-, and an oxygen atom of a methanol molecule. The ligands L- coordinate to the metal ion forming a chelate via the oxygen atoms of carbonylic and phosphorylic groups.

scholarly journals cis-Bromidobis(1,2-diaminoethane-κ2 N,N′)(ethylamine-κN)cobalt(III) dibromide

IUCrData ◽  
2018 ◽  
Vol 3 (6) ◽  
Author(s):  
S. Manimaran ◽  
M. Manjunathan ◽  
E. Govindan ◽  
K. Sambathkumar ◽  
K. Anbalagan
Keyword(s):  
Hydrogen Bonds ◽  
Complex Cation ◽  
Three Dimensional ◽  
Title Complex ◽  
Coordination Environment ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Dimensional Network ◽  
Distorted Octahedral ◽  
Distorted Octahedral Coordination Environment

In the title complex, [CoBr(C2H7N)(C2H8N2)2]Br2, the CoIII centre has a distorted octahedral coordination environment, and is surrounded by four N atoms in the equatorial plane, with an additional N atom and the Br atom occupying the axial positions. The complex is isostructural with the Cl compound for which the X-ray structure has also been reported [Anbalagan, Mahalakshmi & Ganeshraja (2011). J. Mol. Struct. 1005, 45–52]. In the crystal, the complex cation and the two counter-anions are linked via N—H...Br hydrogen bonds, forming a three-dimensional network.

scholarly journals Crystal structure of cis-(1,4,8,11-tetraazacyclotetradecane-κ4 N)bis(thiocyanato-κN)chromium(III) bromide from synchrotron X-ray diffraction data

2021 ◽  
Vol 77 (3) ◽  
pp. 222-225
Author(s):  
Dohyun Moon ◽  
Jong-Ha Choi
Keyword(s):  
Crystal Structure ◽  
Complex Cation ◽  
Title Complex ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Bromide Anion ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral

The crystal structure of the title complex, cis-[Cr(NCS)2(cyclam)]Br (cyclam = 1,4,8,11-tetraazacyclotetradecane, C10H24N4), has been determined from synchrotron X-ray data. The asymmetric unit contains one [Cr(NCS)2(cyclam)]+ cation and one bromide anion. The CrIII ion of the complex cation is coordinated by the four N atoms of the cyclam ligand and by two N-coordinating NCS groups in a cis arrangement, displaying a distorted octahedral coordination sphere. The Cr—N(cyclam) bond lengths are in the range 2.075 (3) to 2.081 (3) Å while the average Cr—N(NCS) bond length is 1.996 (16) Å. The macrocyclic cyclam moiety adopts the most stable cis-V conformation. The crystal structure is stabilized by intermolecular hydrogen bonds involving the cyclam N—H groups as donor groups, and the bromide anion and the S atom of one of the NCS ligands as acceptor groups.

Crystal and Molecular Structure of Di-μ-phenoxido-bis-[N-{(2-hydroxybenzyl)-(S)-alaninato-κ3-O,O',N}copper(II)]. A Simple Homodimetallic Model for N-terminal Tyrosine Coordination with (S)-Alanine as a Second Amino Acid Residue

1998 ◽  
Vol 63 (3) ◽  
pp. 356-362 ◽  
Author(s):  
Svetlana Pakhomova ◽  
Jan Ondráček ◽  
František Jursík
Keyword(s):  
Molecular Structure ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Carbonyl Oxygen ◽  
Antiferromagnetic Coupling ◽  
X Ray Diffraction ◽  
Apical Position ◽  
X Ray ◽  
Pyramidal Geometry ◽  
Square Pyramidal Geometry

Single-crystal X-ray diffraction study established the dimeric [Cu2(ohb-(S)-Ala)2] structure (ohb-(S)-Ala = N-(2-hydroxybenzyl-(S)-alaninate). The complex crystallizes in the tetragonal space group P43212 with a = b = 8.849(1) Å, c = 24.913(2) Å, V = 1950.8(3) Å3, Z = 8. The Cu(II) ion has distorted square-pyramidal geometry with the equatorial positions occupied by three oxygen and one nitrogen atom. Each copper atom is weakly coordinated at the apical position by carbonyl oxygen atom of the neighbouring molecule at the distance 2.329(2) Å. The Cu-Cu separation 3.0204(7) Å and the Cu-O3-Cu angle 100.8(1)° lead to antiferromagnetic coupling (at room temperature μeff = 1.35 μB). The O1-Cu-O3 angle (154.9(1)°) indicates distortion of the square pyramid toward a trigonal bipyramid (t = 0.23).

Octahedral Complexes of Fe(III) with Phosphorylic Ligands Closely Related to β-Diketones

2002 ◽  
Vol 57 (7) ◽  
pp. 746-750 ◽  
Author(s):  
Elizaveta A Trush ◽  
Vladimir A Ovchynnikov ◽  
Konstantin V Domasevitch ◽  
Jolanta Swiatek-Kozlowska ◽  
Vera Ya Zub ◽  
...  
Keyword(s):  
Molecular Structure ◽  
General Formula ◽  
Coordination Compounds ◽  
Esr Spectroscopy ◽  
Carbonyl Oxygen ◽  
X Ray ◽  
Distorted Octahedral ◽  
Chelate Rings

Iron(III) coordination compounds of the general formula FeL3 (where L1 = {CCl3C(O)NP(O)-[N(C2H5)2]2-}-N,N'-tetraethyl-N''-trichloroacetylphosphorictriamide anion, and L2 = {CCl3- C(O)NP(O)[N(CH2CH2)2O]2}--dimorpholido-N-trichloroacetylphosphoricamide anion) have been synthesized and characterized by means of IR, UV-VIS, ESR spectroscopy, and X-ray analysis. The complexes have a molecular structure with the phosphoryl ligands coordinated to the metal ioninabidentatemanner via phosphoryl and carbonyl oxygen atomswith formation of six membered chelate rings. The coordination around the Fe(III) atoms is distorted octahedral, to give fac-isomers in both structures.

Preparation and crystal and molecular structure of (η3-nonamethylcyclotetraphosphazanium-P,P,P)tricarbonylmolybdenum(0) iodide – acetonitrile (1:1), [(η3-Me(MeNPMe)4)Mo(CO)3]I•MeCN

1984 ◽  
Vol 62 (9) ◽  
pp. 1869-1873 ◽  
Author(s):  
Keith D. Gallicano ◽  
Norman L. Paddock ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Mirror Symmetry ◽  
Crystal And Molecular Structure ◽  
Complex Cation ◽  
Neutral Species ◽  
Full Matrix ◽  
Carbonyl Ligands ◽  
Fourier Techniques ◽  
Distorted Octahedral ◽  
Solvent Molecules

The synthesis and physical properties of [(η3-Me(MeNPMe)4)Mo(CO)3]l are reported. Crystals of (η3-nonamethylcyclotetraphosphazanium-P,P,P)tricarbonylmolybdenum(0) iodide – acetonitrile (1:1) are orthorhombic, a = 13.1938(4), b = 13.7847(5), c = 29.281(2) Å, Z = 8, space group Pcab. The structure was solved by Patterson and Fourier techniques and was refined by full-matrix least-squares procedures to R = 0.030 and Rw = 0.034 for 2388 reflections with I ≥ 3σ(I). The structure consists of discrete cations, anions, and solvent molecules. The complex cation has approximate mirror symmetry in the solid state, the Mo atom being coordinated to three phosphazane P atoms and three carbonyl ligands in a distorted octahedral arrangement. Important bond lengths (corrected for libration) are: Mo—P = 2.483(2), 2.439(2), and 2.474(2), mean Mo—C = 1.984(3), mean P—N = 1.710(11) for coordinated P and 1.669(5) Å for quaternized P. The stronger bonding of the cationic ligand to the metal relative to that of the neutral species (CH3NPCH3)4Mo(CO)3, and the strengthening of the ring bonds in both molecules relative to (CH3NPCH3)4, are discussed in terms of d-orbital contraction.

The crystal and molecular structure of gold tris(fluorosulfate)

1991 ◽  
Vol 69 (3) ◽  
pp. 391-396 ◽  
Author(s):  
H. Willner ◽  
S. J. Rettig ◽  
J. Trotter ◽  
F. Aubke
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Gold Atom ◽  
Coordination Geometry ◽  
Full Matrix ◽  
Distorted Octahedral Coordination ◽  
Square Planar ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

Single crystals of gold(III) tris(fluorosulfate) are obtained by recrystallization from bis(fluorosulfuryl) peroxide, S2O6F2, under O2 pressure. The crystals of [Au(SO3F)3]2 are monoclinic, a = 9.700(4), b = 9.222(2), c = 10.810(4)Å, β = 94.43(3)°, Z = 2, space group P21/a. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures, R(F) = 0.038 and Rw(F) = 0.050 for 1491 reflections with I ≥ 3σ(I). The structure consists of centrosymmetric [Au(SO3F)3]2 dimers containing two bidentate, symmetrically bridging and four monodentate, terminal SO3F ligands. The Au(III) ions have square-planar coordination geometry with bridging Au—O = 2.020(7) and 2.016(6) Å, and terminal Au—O = 1.959(7) and 1.956(9) Å. The dimeric [Au(SO3F)3]2 units are linked in the solid state by weak Au—O interactions (2.757(8) and 2.960(7) Å), resulting in a distorted octahedral coordination geometry about each gold atom. Key words: gold(III) tris(fluorosulfate), crystal structure.

Crystal and molecular structure of bis(perchlorato)(γ-C-meso-5,5,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)copper(II)

1978 ◽  
Vol 56 (3) ◽  
pp. 267-272 ◽  
Author(s):  
Ei-Ichiro Ochiai ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Macrocyclic Ligand ◽  
Coordination Geometry ◽  
Full Matrix ◽  
Bond Lengths ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

Crystals of bis(perchlorato) (γ-C-meso-5,5,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)copper(II) are monoclinic, a = 14.061(1), b = 8.908(1), c = 19.710(1) Å, β = 90.912(5)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to a final R of 0.054 and Rw of 0.069 for 2945 reflections with I ≥ 3σ(I). The copper(II) ion has tetragonally distorted octahedral coordination geometry. The four nitrogen atoms of the macrocyclic ligand occupy the equatorial sites and two perchlorate oxygen atoms are in the axial positions. Bond lengths (corrected for libration) are: Cu—N, 2.024(4)–2.051(4), Cu—O, 2.657(5) and 2.697(5), Cl—O, 1.420(4)–1.473(6), N—C, 1.463(6)–1.508(6), and C—C, 1.498(8)–1.542(8) Å.

Crystal structure – reactivity correlations in the solid state photochemistry of N-(tert-butyl)succinimide

1994 ◽  
Vol 72 (9) ◽  
pp. 1952-1960 ◽  
Author(s):  
Tai Y. Fu ◽  
John R. Scheffer ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Solid State ◽  
Crystalline State ◽  
Crystal And Molecular Structure ◽  
Carbonyl Oxygen ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Tert Butyl ◽  
Close Contacts

In order to provide experimental evidence on the stereoelectronic requirements for intramolecular hydrogen atom abstraction by carbonyl oxygen, N-(tert-butyl)succinimide, 1, was investigated by the crystal structure – reactivity correlation method. In this method, the success or failure of a given reaction in the crystalline state is correlated with the geometric parameters associated with the process as determined by X-ray crystallography. In the case of N-(tert-butyl)succinimide, the crystal and molecular structure shows that the molecule adopts a conformation in which there are very close contacts (d = 2.17–2.24 Å) between the carbonyl oxygen atoms and certain γ-hydrogen atoms on the tert-butyl group. In accord with these close contacts, ultraviolet irradiation of N-(tert-butyl)succinimide in the crystalline state leads to transfer of one of the γ-hydrogen atoms from carbon to oxygen. This produces a 1,4-biradical which closes to form a cyclobutanol, and the cyclobutanol undergoes ring opening to afford the final stable product, tetrahydro-1H-azepine-2,5-dione, 2. The crystal and molecular structure of photoproduct 2 is also reported. In contrast to many solid state transformations, there was no discernable melting of the crystals during reaction, and complete conversions of 1 into 2 could be achieved. The isolated chemical yield of photoproduct 2 from the solid state reaction (79%) is in fact considerably higher than that reported by Kanaoka and Hatanaka for the corresponding solution phase process (49%). This permitted the solid state reaction to be followed to 100% conversion by X-ray powder diffractometry, which showed that the process is a single crystal-to-polycrystalline transformation involving a regular and progressive conversion of 1 into 2 with no obvious diffraction peaks that might be attributable to the intermediate cyclobutanol.

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