Organolanthanoids. XXI Synthesis of Bis- and Tris-(diphenylphosphinocyclopenta- dienyl)lanthanoid Compounds and the X-Ray Crystal Structures of [Ln(C5H4PPh2)3(OPPh3)]·(thf)1

1997 ◽  
Vol 50 (10) ◽  
pp. 959 ◽  
Author(s):  
Glen B. Deacon ◽  
Craig M. Forsyth ◽  
Bryan M. Gatehouse ◽  
Anna Philosof ◽  
Brian W. Skelton ◽  
...  
Keyword(s):  
Oxygen Atom ◽  
Single Crystal ◽  
Crystal Structures ◽  
Room Temperature ◽  
Central Metal ◽  
Metal Oxidation ◽  
X Ray

Redox transmetallation ofTl(C5H4PPh2)with an excess of Sm in refluxing thf (thf = tetrahydrofuran) or Eu indme (dme = 1,2-dimethoxyethane) at room temperature gave thelanthanoid(II) compounds[Sm(C5H4PPh2)2](1) and[Eu(C5H4PPh2)2(dme)](2). Crystallization of (1) or[Yb(C5H4PPh2)2(dme)]with OPPh3 in dme yielded[Sm(C5H4PPh2)2(OPPh3)2](3) and[Yb(C5H4PPh2)2(OPPh3)2](4). Room-temperature transmetallation ofTl(C5H4PPh2)with Nd gave the lanthanoid(III) compound[Nd(C5H4PPh2)3(thf)](5), but analogous reactions with La, Pr, Er, Gd and Y in refluxing thfgenerally gave intractable oils, although in one instance impure[La(C5H4PPh2)3(thf)]·(thf)0 · 5,namely(6)·(thf)0 · 5, wasisolated. This complex was also obtained at room temperature by usingLaI3-activated La metal. Oxidation of (1) with 1 equiv.ofTl(C5H4PPh2)in toluene yielded solvent-freeSm(C5H4PPh2)3(7). Addition of OPPh3 to these systems allowed theisolation of[Ln(C5H4PPh2)3(OPPh3)]·(thf)x(x = 0-1 · 5; Ln = La (8), Pr (9),Nd (10), Sm (11), Er (12), Y (13)). Single-crystal X-ray structuredetermination of(10)·(thf)1 · 5,(11)·(thf)1 · 5 and(12)·(thf)1 · 5revealed formally 10-coordinate complexes with an O-bondedOPPh3, threeη5-C5H4PPh2ligands and lattice thf. The centroids of the C5 ringsand the oxygen atom surround the central metal in a distorted tetrahedralarray.

Synthesis, Crystal Structure and Antimicrobial Activity of Poly [bis-and#181;-3,5-dinitro-2-oxidobenzoato) (py) Cu II]

2020 ◽  
Vol 42 (6) ◽  
pp. 928-928
Author(s):  
Fouzia Chang Fouzia Chang ◽  
Najma Memon Najma Memon ◽  
Shahabuddin Memon Shahabuddin Memon ◽  
Muhammad Naeem Ahmed Muhammad Naeem Ahmed ◽  
Muhammad Nawaz Tahir Muhammad Nawaz Tahir ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Room Temperature ◽  
Central Metal Atom ◽  
Central Metal ◽  
Single Crystal Xrd ◽  
Monoclinic System ◽  
X Ray ◽  
Pyramidal Geometry ◽  
Square Pyramidal Geometry

A novel Poly [bis-and#181;-3,5-dinitro-2-oxidobenzoato) (py) Cu II]/(C12H7CuN3O7) was synthesized by a self assemble method at room temperature. The molecular structure was determined by single-crystal X-ray analysis. The compound crystallizes in the monoclinic system, space group P 2 1/c with lattice parameters of a = 10.2143, b = 5.1651 and c = 26.608, α = 90, β = 99.720, γ = 90, Z = 4, V = 1383.60 (18) and#197;3.Pore size depicted from single crystal XRD data was 47and#197;. The central metal atom Cu (II) is coordinated with oxygen of carboxylates group and nitrogen atom of pyridine. The coordination polyhedron posses square pyramidal geometry is manifested by the N— Cu—O angle of 90o. The structure is composed of monomeric coordination units with the central copper (II) ion is not occupying a centre of symmetry.

Temperature dependence of the AV3O7 (A = Ca, Sr) structure

2007 ◽  
Vol 63 (6) ◽  
pp. 836-842 ◽  
Author(s):  
Sebastian Prinz ◽  
Karine M. Sparta ◽  
Georg Roth
Keyword(s):  
Single Crystal ◽  
Temperature Dependence ◽  
Crystal Structures ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Space Groups ◽  
Temperature Ranges ◽  
First Time

The V4+ (spin ½) oxovanadates AV3O7 (A = Ca, Sr) were synthesized and studied by means of single-crystal X-ray diffraction. The room-temperature structures of both compounds are orthorhombic and their respective space groups are Pnma and Pmmn. The previously assumed structure of SrV3O7 has been revised and the temperature dependence of both crystal structures in the temperature ranges 297–100 K and 315–100 K, respectively, is discussed for the first time.

Crystal structures of the simple monoclinic and orthorhombic polytypes of tripotassium hexacyanoferrate(III)

1978 ◽  
Vol 31 (6) ◽  
pp. 1195 ◽  
Author(s):  
BN Figgis ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Room Temperature ◽  
Potassium Ferricyanide ◽  
X Ray Diffraction ◽  
X Ray ◽  
Monoclinic Form

The room-temperature (295 K) crystal structures of potassium ferricyanide, K3[Fe(CN)6], have been determined for the simplest monoclinic (a reinvestigation) and orthorhombic polytypes by single- crystal X-ray diffraction. The monoclinic form is P21/c, a 7.047(3), b 10.400(3), c 8.384(3) Ǻ, β 107.29(3)°, Z 2. The iron atoms lie on special positions with symmetry 1. In the orthorhombic form, Pnca, a 13.422(6), b 10.396(4), 8.381(4) Ǻ, Z4, the iron atoms now lie on special positions with symmetry 2 (parallel to c). Residuals are 0.036 and 0.048 for 1232 and 855 'observed' reflections respectively.

High-pressure syntheses and crystal structures of orthorhombic DyGaO3 and trigonal GaBO3

2015 ◽  
Vol 70 (4) ◽  
pp. 207-214 ◽  
Author(s):  
Daniela Vitzthum ◽  
Stefanie A. Hering ◽  
Lukas Perfler ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
High Pressure High Temperature

AbstractOrthorhombic dysprosium orthogallate DyGaO3 and trigonal gallium orthoborate GaBO3 were synthesized in a Walker-type multianvil apparatus under high-pressure/high-temperature conditions of 8.5 GPa/1350 °C and 8 GPa/700 °C, respectively. Both crystal structures could be determined by single-crystal X-ray diffraction data collected at room temperature. The orthorhombic dysprosium orthogallate crystallizes in the space group Pnma (Z = 4) with the parameters a = 552.6(2), b = 754.5(2), c = 527.7(2) pm, V = 0.22002(8) nm3, R1 = 0.0309, and wR2 = 0.0662 (all data) and the trigonal compound GaBO3 in the space group R3̅c (Z = 6) with the parameters a = 457.10(6), c = 1419.2(3) pm, V = 0.25681(7) nm3, R1 = 0.0147, and wR2 = 0.0356 (all data).

scholarly journals Single crystal structures and theoretical calculations of uranium endohedral metallofullerenes (U@C2n, 2n = 74, 82) show cage isomer dependent oxidation states for U

2017 ◽  
Vol 8 (8) ◽  
pp. 5282-5290 ◽  
Author(s):  
Wenting Cai ◽  
Roser Morales-Martínez ◽  
Xingxing Zhang ◽  
Daniel Najera ◽  
Elkin L. Romero ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Oxidation State ◽  
Theoretical Calculations ◽  
State Dependence ◽  
Oxidation States ◽  
Metal Oxidation ◽  
X Ray ◽  
Endohedral Metallofullerenes ◽  
Single Crystal Structures

First X-ray structures and metal oxidation state dependence on cage isomerism for U-EMFs.

Synthesis, characterization and reactivity of trans-dihydroxy platinum(IV) porphyrins

2016 ◽  
Vol 20 (07) ◽  
pp. 785-792 ◽  
Author(s):  
Yingying Ning ◽  
Yi Yu ◽  
Yi-Wei Liu ◽  
Jing Zhang ◽  
Hao-Ling Sun ◽  
...  
Keyword(s):  
Oxygen Atom ◽  
Single Crystal ◽  
Crystal Structures ◽  
Oxidation State ◽  
Photoelectron Spectroscopy ◽  
Catalytic Reactions ◽  
X Ray ◽  
Single Crystal Structures

Synthesis of two trans-dihydroxy platinum(IV) porphyrins (TPP, tetraphenylporphyrin and F[Formula: see text]TPP, tetrakispentafluorophenylporphyrin) by dimethyl dioxirane (DMD) oxidation of their Pt[Formula: see text] porphyrin precursors have been described. The oxidation state of Pt cation in such complexes was assessed by X-ray photoelectron spectroscopy and shown to be [Formula: see text]4. More importantly, proton was found to promote the formation and stabilization of the trans-dihydroxy platinum(IV) porphyrins, as revealed by UV-vis spectroscopic results and single crystal structures. In addition, these trans-dihydroxy Pt[Formula: see text] porphyrins were much easier to be reduced than their Pt(II) counterparts and capable to transfer oxygen atom to triphenylphosphine and thioanisol, which is important for further application of Pt(IV) complexes in catalytic reactions.

Reaction between Yttrium Nitrate and 2,2':6',2"-Terpyridine (terpy) in MeCN: Preparation, Crystal Structures and Spectroscopic Characterization of [Y (NO3)3(terpy)(H2O )] and [Y(NO3)3(terpy)(H2O )] · terpy · 3 MeCN

2001 ◽  
Vol 56 (2) ◽  
pp. 122-128 ◽  
Author(s):  
Athanassios K. Boudalis ◽  
Vassilios Nastopoulos ◽  
Aris Terzis ◽  
Catherine P. Raptopoulou ◽  
Spyros P. Perlepes
Keyword(s):  
Oxygen Atom ◽  
Single Crystal ◽  
Crystal Structures ◽  
Spectroscopic Characterization ◽  
Yttrium Nitrate ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Tricapped Trigonal Prism

Abstract The reaction of Y(NO3)3 · 5H2O and 2,2':6',2"-terpyridine (terpy) in MeCN leads to [Y(N03 )3(terpy)(H2O )] (1) and [Y(N03 )3(terpy)(H2O )] terpy-3MeCN (2) in good yields depending on the isolation conditions. The structures of both complexes were determined by single-crystal X-ray crystallography. The YIII atom in 1 is 9-coordinate and ligation is provided by one terdentate terpy molecule, two chelating nitrates, one monodentate nitrate and one terminal H2O molecule; the coordination polyhedron about the metal may be viewed as a tricapped trigonal prism. The YIII atom in 2 is 10-coordinate and its coordination sphere consists of three nitrogen atoms from the terdentate terpy, six oxygen atoms from the three chelating nitrates (one of them being “anisobidentate”) and one oxygen atom from a terminal H2O molecule; the polyhedron about the metal may be viewed as a distorted sphenocorona. The interstitial terpy is strongly hydrogen-bonded to the O atom of the coordinated H2O molecule to form [Y(NO3 )3(terpy)(H20)] ··· terpy pairs. The new complexes were characterized by IR and 1H NMR spectroscopies. The YIII/NO3-/terpy chemistry is compared to the already well-developed LnIII/NO3-/terpy chemistry (Ln = lanthanide).

scholarly journals Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh3)(Br)]2(μ,η2-C4H3N2)2, [Pd(Br)]2(μ,η2-Hdppa)2, and [{Pd(PPh3)(CH3CN)}2(μ,η2-C4H3N2)2][BF4]2

Molecules ◽  
2020 ◽  
Vol 25 (9) ◽  
pp. 2035
Author(s):  
Hsiao-Fen Wang ◽  
Kuang-Hway Yih ◽  
Gene-Hsiang Lee
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Room Temperature ◽  
Palladium Complex ◽  
Chloroform Solution ◽  
Bidentate Ligand ◽  
Tridentate Ligand ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray

In a refluxing chloroform solution, the η1-pyrimidinyl {pyrimidinyl = C4H3N2} palladium complex [Pd(PPh3)2(η1-C4H3N2)(Br)], 1 exhibited intermolecular displacement of two triphenylphosphine ligands to form the doubly bridged η2-pyrimidinyl Dipalladium complex [Pd(PPh3)(Br)]2(μ,η2-C4H3N2)2, 3. The treatment of 1 with Hdppa {Hdppa = N,N-bisdiphenyl phosphinoamine} in refluxing dichloromethane yielded the doubly bridged Hdppa dipalladium complex [Pd(Br)]2(μ,η2-Hdppa)2, 4. Complex 1 reacted with the bidentate ligand, NH4S2CNC4H8 and, NaS2COEt, and the tridentate ligand, KTp {Tp = tris(pyrazoyl-1-yl)borate}, to form the η2-dithio η1-pyrimidinyl complex [Pd(PPh3)(η1-C4H3N2)(η2-SS)], (5: SS = S2CNC4H8; 6: SS = S2COEt) and η2-Tp η1-pyrimidinyl complex [Pd(PPh3)(η1-C4H3N2)(η2-Tp)], 7, respectively. Treatment of 1 with AgBF4 in acetonitrile at room temperature resulted in the formation of the doubly bridged η2-pyrimidinyl dipalladium complex [{Pd(PPh3)(CH3CN)}2(μ,η2-C4H3N2)2][BF4]2, 8. All of the complexes were identified using spectroscopic methods, and complexes 3, 4, and 8 were determined using single-crystal X-ray diffraction analyses.

Hydrogen bonding in hydroxypyridium salts

2018 ◽  
Vol 233 (7) ◽  
pp. 501-506
Author(s):  
Andrei V. Mironov ◽  
Victor A. Tafeenko ◽  
Dmitrii Yu. Grebenkin ◽  
Alexander E. Oblezov
Keyword(s):  
Hydrogen Bonding ◽  
Oxygen Atom ◽  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Nitrate Anion ◽  
Single Crystal Diffraction ◽  
Space Group ◽  
X Ray ◽  
Unit Cells

Abstract The crystal structures of 6-methyl-2-ethyl-3-hydroxypyridiniun nitrate (C8H12NO)NO3 (I) and fumarate (C8H12NO)2C4H2O4 (II) were solved and refined from X-ray single crystal diffraction data (CuKα, (I) a=4.6477(2), b=14.5906(9), c=14.5551(8) Å, β=99.100(4)°, space group P21/c, Z=4, Rp/Rwp=0.033/0.047; (II) a=8.8293(3), b=13.4268(5), c=8.3893(3) Å, β=96.303(3)°, space group P21/c, Z=2, Rp/Rwp= 0.034/0.049). Both structures are built of infinite chains along ac diagonal of the unit cells formed by hydrogen bonding between the hydroxypyridium cation and the corresponding anion. Each fumarate anion is linked to four hydroxypyridium cations while nitrate anion is connected with two hydroxypyridium cations only leaving one oxygen atom in the nitrogen group isolated.

Crystal structures of Dimeric O-ethylxanthato-quinolin-8-olato-lead(II) and of tetraethylammonium Tris-(O-ethylxanthato)plumbate(II)

1982 ◽  
Vol 35 (12) ◽  
pp. 2423 ◽  
Author(s):  
SG Hardin ◽  
PC Healy ◽  
WG Mumme ◽  
AH White ◽  
G Winter
Keyword(s):  
Nitrogen Atom ◽  
Oxygen Atom ◽  
Single Crystal ◽  
Crystal Structures ◽  
Lead Atom ◽  
X Ray Diffraction ◽  
X Ray

The crystal structures of the title compounds have been carried out by single-crystal X-ray diffraction methods at 295 K. For (1), [(EtOCS2)Pb(C9H6NO)2Pb(S2COEt)], crystals are triclinic, P1, a 11.600(6), b 8.9739, c 6.863(4) �, α 96.79(5), β 90.19(5), γ 101.54(4)�, with one dimer in the cell. R was 0.038 for 3109 'observed' reflections. The lead atom is coordinated by two sulfur atoms from the xanthate ligand [Pb-S 2.705(3), 3.173(3) �], the quinolin-8-olato nitrogen atom [Pb-N 2.479(6) �] and the oxygen atom which bridges two centrosymmetrically related lead atoms [Pb-O 2.296(5), 2.548(4) �]. For (2), (Et4N) [Pb(S2COEt)3], crystals are monoclinic, P21/c, a 10.827(3), b 18.889(6), c 14.292(5) �, β 111.05(2)�, Z 4. R was 0.050 for 3657 'observed' reflections. The lead atom is surrounded by the six sulfur atoms [Pb-S 2.754(4)-3.126(3) �], with close approaches from the two sulfur atoms of one of the ligands of a centrosymmetrically related anion [Pb.. .S 3.545(4), 3.555(4) �], in a similar manner to that observed in the 'isoelectronic' tris(N,N-diethyldithiocarbamato)bismuth(III) complex.

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