Hydro(solvo)thermal in situ ligand syntheses

Zhang, Xian‐Ming

doi:10.1016/j.ccr.2005.01.004

Cited by 551 publications

(80 citation statements)

References 62 publications

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“…In thetitle crystal structure, each Fe of adimer is coordinated in a distortedo ctahedronb yt wo oxygen atoms from oxalate, three oxygen atomsfrom Ph 3 PO (triphenylphosphine oxide) and one chlorine atom.T he asymmetric unit contains half of ad imer, which is one Fe, half oxalate, one chlorine and three Ph 3 PO molecules, andthere is oneneutral molecule perunitcell. Thebond angles ÐO3-Fe1-O5 are less than 90°and ÐCl-Fe-O are more than9 0°.T he three Ph 3 …”

Section: Discussionmentioning

confidence: 97%

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Crystal structure of (μ-oxalato)bis[chlorotris(triphenylphosphine oxide- O)iron(III)] tetrachloroferrate(III), [FeCl(C18H15PO)3][C2O4][FeCl4]

Zhang¹

2011

Zeitschrift Für Kristallographie - New Crystal Structures

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C 110 H 90 Cl 10 Fe 4 O 10 P 6 ,triclinic, P1 (no. 2), a =10.672(7) Å, b =15.74(1) Å, c =16.71(1) Å, a =78.803(8)°, b =85.771(9)°, g =81.857(9)°, V =2722.4 Å 3 , Z =1, Source of materialStarting materials and solvents for synthesis were purchased commercially and used as received. Experimental detailsAllHatoms on Catoms were generated geometrically andrefined as riding with d(C-H) =0.95 Åand U iso (H) =1.2 U eq (O). Three Cl atomso ft he FeCl 4 are disordered over two equivalent positions. DiscussionThe preparation of inorganic-organic hybrid coordination complexes has received much attention due to their potential applications as functional materials [1,2]. Solvo(hydro)thermal synthesis has rapidly developed over the past several years due to its effectiveness,s implicity and environmental friendliness [3]. In order to synthetize new inorganic-organic hybrid material, we synthetized the title complex by hydrothermalmethod and report here. In thetitle crystal structure, each Fe of adimer is coordinated in a distortedo ctahedronb yt wo oxygen atoms from oxalate, three oxygen atomsfrom Ph 3 PO (triphenylphosphine oxide) and one chlorine atom.T he asymmetric unit contains half of ad imer, which is one Fe, half oxalate, one chlorine and three Ph 3 PO molecules, andthere is oneneutral molecule perunitcell. Thebond angles ÐO3-Fe1-O5 are less than 90°and ÐCl-Fe-O are more than9 0°.T he three Ph 3 PO molecules bind to the Fe from the direction nearly perpendicular to the FeOCl plane with the bond angles ÐO-Fe-O (Ph 3 PO) being less than 90°and ÐCl-Fe-O (Ph 3 PO) more than 90°.

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Section: Discussionmentioning

confidence: 97%

“…Solvo(hydro)thermal synthesis has rapidly developed over the past several years due to its effectiveness,s implicity and environmental friendliness [3]. In order to synthetize new inorganic-organic hybrid material, we synthetized the title complex by hydrothermalmethod and report here.…”

Section: Discussionmentioning

confidence: 99%

Crystal structure of (μ-oxalato)bis[chlorotris(triphenylphosphine oxide- O)iron(III)] tetrachloroferrate(III), [FeCl(C18H15PO)3][C2O4][FeCl4]

Zhang¹

2011

Zeitschrift Für Kristallographie - New Crystal Structures

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“…The in situ reduction of Cu II to Cu I was broadly confirmed by the solvothermal reactions. [13] The infrared spectrum of 2 shows bands at ñ = 2100 cm À1 , which is attributed to the stretch vibration of C=N. In fact, many other Cu I complexes based on HL or related ligands contain in situ-formed cyanide anions from methanol and NH 3 ·H 2 O under solvothermal conditions, which will be reported in further publications.…”

Section: Introductionmentioning

confidence: 96%

Polymerizing Cluster Helicates into High‐Connectivity Networks

Zhan

Hou

et al. 2008

Chemistry A European J

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Solvothermal reactions of CuII salts and 3,5-bis(4-pyridyl)pyrazole (HL) under various conditions gave three different types of crystalline compound, namely [Cu2(Cu5L6)]BF(4).5 H2O (1 a), [Cu2(Cu5L6)]ClO(4).5 H2O (1 b), and [Cu7(CN)2(Cu5L6)2][BF4]3 (2). 1 a and b were obtained in ethanol and NH3.H2O, whereas 2 was obtained in methanol and NH3.H2O. The three complexes were constructed by incorporating new pentanuclear copper(I) pyrazolate bis(triple helical) cluster helicates (Cu5L6) as the second building units (SBUs), in which as many as twelve 4-pyridyl N atoms are available for further coordination and construction of high-connectivity topological networks. In 1 a and b, seven 4-pyridyl N atoms are linked to three three-coordinated CuI atoms and four four-coordinated CuI atoms, which results in 3,4,7-connected networks. In 2, as many as eleven 4-pyridyl N atoms coordinate to eleven CuI atoms, which results in a 4,10-connected topological network. The increasing connectivity of the cluster nodes in 2 is closely related to the in situ-formed CN- anion bridge around the periphery of the pentanuclear cluster helicates. The luminescenct properties of these compounds were also investigated.

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“…An important feature of 1Y is the simultaneous "capture" of isomeric ic and mc ligands that originate from the in situ pyrolysis of H 3 L. [4] In situ ligand synthesis under hydro(solvo)thermal conditions has received intense interest in the past years. [5] Like 1Y, one compound capturing two in situ generated ligands from the same precursor was rarely reported in the literature. [6] The vinyl bonds of the ic and mc ligands have lengths of 1.296 (7) and 1.316(3) , respectively, which are comparable to those reported in the literature.…”

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confidence: 98%

“…[8] Furthermore, these bilayers are cross-bridged by 4,4'-bipy ligands through the N41 and N42 atoms to generate a 3D Archimedean-type network with a 4 2 6 6 8 2 topology built upon five-connected Cd II metal centers (Figure 2 c,d). The long topological (OKeeffe) vertex symbol of this 4 2 6 6 8 2 net is 4.4.6.6.6 3 .6 3 .6 3 .6 3 .8 4 .8 5 . [9] To the best of our knowledge, this structural topology has not Supporting information for this article is available on the WWW under http://www.angewandte.org or from the author.…”

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confidence: 99%

Photochromism of a 3D Cd^II Complex with Two Captured Ligand Isomers Generated In Situ from the Same Precursor

et al. 2008

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Photochromic compounds have gained intense interest owing to their novel photochemical and photophysical reactions as well as their various potential applications such as in sunglasses and optical memories.[1] An appreciable number of photochromic families have been reported to date; [2] however, those based on an electron-transfer (redox) chemical process, especially for metal-organic compounds, are rare.[3] We present herein a hydrothermally synthesized 3D complex [Cd 2 (ic)(mc)(4,4'-bipy) 3 ] n ·4n H 2 O (1Y; ic= itaconate, mc = mesaconate) which exhibits reversible radicalbased redox photochromic behavior. This compound also merits attention for its unusual five-connected Archimedeantype topological structure and unexpected "capture" of isomeric ic and mc ligands that are generated in situ from trans-propene-1,2,3-tricarboxylic acid (H 3 L, Scheme 1).Yellow prismatic crystals of 1Y accompanied by a few colorless block crystals of [Cd 3 L 2 (H 2 O) 6 ] n (2; Figure S1 in the Supporting Information) were obtained by the hydrothermal reaction of CdCO 3 , 4,4'-bipy, H 3 L, and deionized water in a molar ratio of 1:1:1:1111 at 120 8C for 12 h. Powder X-ray diffraction (PXRD) verified the purity of a mechanically separated sample of 1Y ( Figure S2 in the Supporting Information). Thermal analysis and PXRD data show that compound 1Y still keeps its metal-organic framework at 200 8C after the elimination of lattice water molecules ( Figure S2 and S3 in the Supporting Information).A single-crystal X-ray diffraction study of 1Y revealed a 3D structure based on a network of seven-coordinated Cd II centers linked by three kinds of bridging ligands. As shown in Figure 1, the central Cd1 atom is located in a pentagonalbipyramidal coordination environment with N41 and N42 atoms of crystallographically independent 4,4'-bipy ligands acting as the two pyramidal apexes. An important feature of 1Y is the simultaneous "capture" of isomeric ic and mc ligands that originate from the in situ pyrolysis of H 3 L. [4]

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Hydro(solvo)thermal in situ ligand syntheses

Cited by 551 publications

References 62 publications

Crystal structure of (μ-oxalato)bis[chlorotris(triphenylphosphine oxide- O)iron(III)] tetrachloroferrate(III), [FeCl(C18H15PO)3][C2O4][FeCl4]

Crystal structure of (μ-oxalato)bis[chlorotris(triphenylphosphine oxide- O)iron(III)] tetrachloroferrate(III), [FeCl(C18H15PO)3][C2O4][FeCl4]

Polymerizing Cluster Helicates into High‐Connectivity Networks

Photochromism of a 3D Cd^II Complex with Two Captured Ligand Isomers Generated In Situ from the Same Precursor

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Hydro(solvo)thermal in situ ligand syntheses

Cited by 551 publications

References 62 publications

Crystal structure of (μ-oxalato)bis[chlorotris(triphenylphosphine oxide- O)iron(III)] tetrachloroferrate(III), [FeCl(C18H15PO)3][C2O4][FeCl4]

Crystal structure of (μ-oxalato)bis[chlorotris(triphenylphosphine oxide- O)iron(III)] tetrachloroferrate(III), [FeCl(C18H15PO)3][C2O4][FeCl4]

Polymerizing Cluster Helicates into High‐Connectivity Networks

Photochromism of a 3D CdII Complex with Two Captured Ligand Isomers Generated In Situ from the Same Precursor

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Photochromism of a 3D Cd^II Complex with Two Captured Ligand Isomers Generated In Situ from the Same Precursor