Crystal Structures of (PPh3)2Pd(N3)2, (AsPh3)2Pd(N3)2, (2-Chloropyridine)2Pd(N3)2, [(AsPh4)2][Pd2(N3)4Cl2], [(PNP)2][Pd(N3)4], [(AsPh4)2][Pt(N3)4] · 2 H2O, and [(AsPh4)2][Pt(N3)6]

Beck, Wolfgang; Fehlhammer, Wolf Peter; Feldl, Klaus; Klapötke, Thomas M.; Kramer, Gernot; Mayer, Péter; Piotrowski, Holger; Pöllmann, P.; Ponikwar, Werner; Schütt, Thomas; Schuierer, Erich; Vogt, Martin

doi:10.1002/1521-3749(200108)627:8<1751::aid-zaac1751>3.0.co;2-5

Cited by 20 publications

(22 citation statements)

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“…This phenomenon typically caused by the close proximity of heavy and light atoms was also reported, e.g. for SbCl(N 3 ) 2 63, NBu n 4 [Ir(N 3 )pc(acac)] (pc = phthalocyaninate(2‐))64, [IrCp*(N 3 )bipy]PF 6 65, (AsPh 4 ) 2 [Pd 2 (N 3 ) 4 Cl 2 ]58, [N(PPh 3 ) 2 ] 2 [Pd(N 3 ) 4 ]58, [Me 3 PtN 3 ] 4 66, trans ‐[Pt(Me)N 3 (PPr i 3 ) 2 ]62, (AsPh 4 ) 2 [Pt(N 3 ) 4 ]67, (AsPh 4 ) 2 [Pt(N 3 ) 6 ]58,67, (PPh 4 ) 2 [Pt(N 3 ) 6 ], (AsPh 4 ) 2 [Pt(N 3 )Cl 5 ]HCONMe 2 68, and Au(N 3 )(PPh 3 )59b.…”

Section: Homoleptic Azido Complexessupporting

confidence: 60%

“…1 was shown to exist in solution (CDCl 3 , 303 K) predominantly as the trans isomer. [154] The same configuration has been proposed for the solid state of 1 as well as of Pd(N 3 ) 2 (AsPh 3 ) 2 and Pd(N 3 ) 2 (2‐chloropyridine) 2 on the basis of IR and Raman spectroscopy, [2, 155, 156] and recently confirmed by X‐ray crystallography 58. X‐ray data proving trans geometry are now available for a whole bunch of further Pd(N 3 ) 2 L 2 complexes with L = PBzl 3 , [157] py, [158] quinoline, [156] phenyl‐3‐methylpyrazole, [159] and isonicotinamide (isn).…”

Section: Heteroleptic Azido Complexesmentioning

confidence: 56%

“…Of several d‐metals homoleptic azido complexes have been obtained in more than one oxidation state, e.g., [Pt II (N 3 ) 4 ] 2– /[Pt IV (N 3 ) 6 ] 2– or [Au I (N 3 ) 2 ] – /[Au III (N 3 ) 4 ] – 2. Some of the early complexes – [N(PPh 3 ) 2 ] 2 [Pd(N 3 ) 4 ]58, (AsPh 4 ) 2 [Pt(N 3 ) 4 ] · 2H 2 O58, AsPh 4 [Au(N 3 ) 4 ]59 – together with newly prepared variants thereof, e.g. [Pd(NH 3 ) 4 ][Pd(N 3 ) 4 ]60, have meanwhile been characterized by X‐ray and found to possess the ‘wind wheel'‐like structure (cf.…”

Section: Homoleptic Azido Complexesmentioning

confidence: 99%

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Azide Chemistry – An Inorganic Perspective, Part I Metal Azides: Overview, General Trends and Recent Developments

Fehlhammer

Beck

2013

Zeitschrift anorg allge chemie

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With Sharpless' and Meldal's discovery of the immensely supportive effect that metal catalysis has on Huisgen's classical 1, 3‐dipolar cycloaddition, azides (RN3) – long underappreciated in organic synthesis – suddenly got in the focus of attention as most crucial players in sensational ‘click chemistry'. Less noisy though with the same commitment and even a much broader scope of scientific topics and objectives, the inorganic azide chemistry has made just as great strides in the last few decades. This review (Part I) gives an introductory survey of the most important results, and informs about modern developments and general trends. Particular emphasis is placed on the recent successful approaches to highly unstable homoleptic azido metal complexes of the main group and early transition elements, as well as on the enormous structural versatility caused by the ‘flexidentate' N3– ligand with its unsurpassed bridging capacities. The presentation in this paper of selected compounds and reactions is meant, in a way, as a prelude to the [3+2]‐cycloadditions of metal azides and related species which will be covered in‐depths in Part II. A large part of the comments finally deals with applications in fields such as catalysis, high explosive performance or magnetism of metal compounds containing azide, today certainly one of the most attractive research areas world‐wide.

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Section: Homoleptic Azido Complexessupporting

confidence: 60%

Section: Heteroleptic Azido Complexesmentioning

confidence: 56%

Section: Homoleptic Azido Complexesmentioning

confidence: 99%

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Azide Chemistry – An Inorganic Perspective, Part I Metal Azides: Overview, General Trends and Recent Developments

Fehlhammer

Beck

2013

Zeitschrift anorg allge chemie

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“…[1][2][3][4] In particular, the complex [Pd(NCO)2(PPh3)2] was firstly prepared by Norbury and Sinha 5 in 1967 by the displacement of pyridine from [Pd(NCO)2(py)2] by 2 equivalents of PPh3. However, the formulation of this compound was based only on infrared evidence.…”

mentioning

confidence: 91%

Molecular and Crystal Structure of trans-(Dicyanato)-bis(triphenylphosphine)palladium(II)

et al. 2008

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The molecular and crystal structures of square-planar complexes of general formulae [PdX2(PPh3)2] (X = halide or pseudohalide, PPh3 = triphenylphosphine) have been determined by many authors. [1][2][3][4] In particular, the complex [Pd(NCO)2(PPh3)2] was firstly prepared by Norbury and Sinha 5 in 1967 by the displacement of pyridine from [Pd(NCO)2(py)2] by 2 equivalents of PPh3. However, the formulation of this compound was based only on infrared evidence. Focusing our interest on the coordination and supramolecular chemistry of Pd(II) compounds bearing halides and pseudohalides, 6,7 we describe in this work the synthesis and X-ray structural study of the complex trans-(di cyanato)bis(triphenylphosphine)palladium(II) (Fig. 1).Triphenylphosphine (202 mg; 0.77 mmol) in 7 mL of CHCl3 was added to a deep-orange solution of [PdCl2(MeCN)2] (100 mg; 0.38 mmol) in 20 mL of CHCl3. After stirring the resulting orange solution for 5 min, KNCO (62.5 mg; 0.77 mmol) in 2 mL of CH3OH/H2O (1:1) was added and the solution became yellow. Slow evaporation of the solution gave yellow crystals in high yield and of good quality for X-ray diffraction studies. Yield, 65%; M.p., 205˚C (dec.).Anal. Calcd. for C38H30N2O2P2Pd(%): C, 63.83; N, 3.92; H, 4.23. Found: C, 63.72; N, 3.86; H, 4.20 . The complex was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The title compound was crystallized in a triclinic system, space group P1 with a = 9.213(3)Å, b = 9.781 (7)

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“…6 The Pd-N(azide) bond length (mean value of 2.061 Å) is in agreement with those found for trans-[Pd(N3)2(PPh3)2] (2.022 Å). 7 Another structural parameter of interest is the quasilinearity of the azido groups coordinated to palladium atoms [N-N-N average angle 175.3(6)˚] as well their asymmetry with the long N-N bonds being between the a and the g nitrogen atoms [Na-Nb average length, 1.119(5)Å; Nb-Ng average length, 1.198(6)Å]. 8 The crystal packing of [Pd2(N3)4(PPh3)2(m-ted)] is depicted in Fig.…”

mentioning

confidence: 99%

Crystal and Molecular Structure of Dinuclear Palladium(II) Complex Containing Nitrogen and Phosphorus Donor Ligands, [Pd2(N3)4(PPh3)2(.MU.-ted)]

et al. 2008

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Triethylenediamine (ted) is a bidentade ligand that can bind to metallic centers through two nitrogen atoms.1 Such coordination behavior is very attractive, since the triethylenediamine can be used as linear building block for constructing sophisticated metallosupramolecular architectures.2 Moreover, in environmental and military applications, ted has been impregnated on various supports in order to adsorb toxic gases, such as HCN, CNCl, SO2 and CH3I, or as a sensor to detect these gases. The pseudohalide azide (NNN -) is known to coordinate to metals in both terminal and bridging modes.Besides, 1,3-dipolar cycloaddition of multiply-bonded molecules (e.g. CS2) to coordinated azide in metal compounds is an effective method for obtaining metal-bonded heterocycles, many of which are otherwise inaccessible. 4 In the medical area, Pd(II) azido compounds have shown remarkable antitumor activity against some human cancer cell lines. 5 Focusing our interest on the coordination and supramolecular chemistry of palladium-based compounds, 6 we describe herein the synthesis and single-crystal X-ray structure of [Pd2(N3)4(PPh3)2(m-ted)] (Fig. 1). To the best of our knowledge, this is the first complex containing the ted ligand coordinated to the palladium(II) center. This compound was prepared by adding ted, PPh3 and NaN3 to an acetone solution of [PdCl2(CH3CN)2] in 1:2:4:2 molar ratio. After 1 h of stirring, the orange suspension formed was filtered off and the mother liquor was left to evaporate, yielding orange single-crystals suitable for X-ray diffraction measurements.The structure of the title compound, C42H42N14P2Pd2, was determined by single-crystal X-ray diffraction. It was solved from 8358 independent reflections [R(int) = 0.0389] and refined by full-matrix least-squares of the non-H atoms to an R1 value of 0.0339 for 7178 reflections with Fo > 4s(Fo). The H-atoms were positioned stereochemically and refined with the riding model. The locations of the methylenic hydrogen atoms were optimized during the refinement by treating them as rigid

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Crystal Structures of (PPh3)2Pd(N3)2, (AsPh3)2Pd(N3)2, (2-Chloropyridine)2Pd(N3)2, [(AsPh4)2][Pd2(N3)4Cl2], [(PNP)2][Pd(N3)4], [(AsPh4)2][Pt(N3)4] · 2 H2O, and [(AsPh4)2][Pt(N3)6]

Abstract: -011Crystal Structures of (PPh 3 ) 2 Pd(N 3 ) 2 (I), (-As revealed by single crystal XRD, compounds (PPh

Cited by 20 publications

References 17 publications

Azide Chemistry – An Inorganic Perspective, Part I Metal Azides: Overview, General Trends and Recent Developments

Azide Chemistry – An Inorganic Perspective, Part I Metal Azides: Overview, General Trends and Recent Developments

Molecular and Crystal Structure of trans-(Dicyanato)-bis(triphenylphosphine)palladium(II)

Crystal and Molecular Structure of Dinuclear Palladium(II) Complex Containing Nitrogen and Phosphorus Donor Ligands, [Pd2(N3)4(PPh3)2(.MU.-ted)]

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Crystal Structures of (PPh3)2Pd(N3)2, (AsPh3)2Pd(N3)2, (2-Chloropyridine)2Pd(N3)2, [(AsPh4)2][Pd2(N3)4Cl2], [(PNP)2][Pd(N3)4], [(AsPh4)2][Pt(N3)4] · 2 H2O, and [(AsPh4)2][Pt(N3)6]

Abstract: -011Crystal Structures of (PPh 3 ) 2 Pd(N 3 ) 2 (I), (-As revealed by single crystal XRD, compounds (PPh

Cited by 20 publications

References 17 publications

Azide Chemistry – An Inorganic Perspective, Part I Metal ­Azides: Overview, General Trends and Recent Developments

Azide Chemistry – An Inorganic Perspective, Part I Metal ­Azides: Overview, General Trends and Recent Developments

Molecular and Crystal Structure of trans-(Dicyanato)-bis(triphenylphosphine)palladium(II)

Crystal and Molecular Structure of Dinuclear Palladium(II) Complex Containing Nitrogen and Phosphorus Donor Ligands, [Pd2(N3)4(PPh3)2(.MU.-ted)]

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Azide Chemistry – An Inorganic Perspective, Part I Metal Azides: Overview, General Trends and Recent Developments

Azide Chemistry – An Inorganic Perspective, Part I Metal Azides: Overview, General Trends and Recent Developments