Structure of bis(1,1,1,5,5,5-hexafluoro-2,4-pentanedionato)(2,5,8,11,14-pentaoxapentadecane)barium(II)

Sluis, P. van der; Spek, A. L.; Timmer, K.; Meinema, H.A.

doi:10.1107/s0108270190004188

Cited by 38 publications

(17 citation statements)

References 1 publication

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“…These occupancies were obtained by constraining the isotropic U's to be equal. The fluorine atoms of C (10) do not reside on the mirror plane and were, therefore, assigned occupancies of 50%. The -CF3 groups were refined with C-F and F-F distances constrained to 1.34 and 2.19 Å, respectively.…”

Section: Methodsmentioning

confidence: 99%

“…Group 2 species that have been primarily studied as precursors to group 2 element-containing films are the β-diketonate derivatives. 2,[5][6][7][8][9][10][11] These derivatives contain the most volatile group 2 species discovered to date and have lead to the successful deposition of group 2 containing films, such as MF 2 12 and MTiO 3 . [13][14][15][16][17][18][19] However, in the case of deposition of metal titanate and other metal oxide films, water 6,[14][15][16]18,[20][21][22] is often added as a reagent in an attempt to remove cleanly the β-diketonate ligand by hydrolysis, according to the equation of reaction 1.…”

Section: Introductionmentioning

confidence: 99%

“…by chemical vapor deposition, CVD). − In the case of the group 2 compounds, the synthesis of precursors with properties suitable for CVD (volatility and reactivity) is extremely challenging because of the large size of the lower group 2 elements and the resulting tendency for oligomerization and, therefore, a decrease in volatility. Group 2 species that have been primarily studied as precursors to group 2 element-containing films are the β-diketonate derivatives. ,− These derivatives contain the most volatile group 2 species discovered to date and have lead to the successful deposition of group 2 containing films, such as MF 2 12 and MTiO 3 . − However, in the case of deposition of metal titanate and other metal oxide films, water 6,14-16,18,20-22 is often added as a reagent in an attempt to remove cleanly the β-diketonate ligand by hydrolysis, according to the equation of reaction 1 …”

Section: Introductionmentioning

confidence: 99%

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Synthesis, Characterization, and Thermal Behavior of Polydentate Ligand Adducts of Barium Trifluoroacetate

1998

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The reaction of BaH 2 with polydentate ligands and CF 3 COOH in THF at -40 °C in 1:1:2 stoichiometries leads to compounds of general formula [Ba(O 2 CCF 3 ) 2 ] m L n (L ) 12-crown-4 (1), triglyme (2), 2-(hydroxymethyl)-15crown-5 (15-crown-5CH 2 OH) (3), cryptand(222) (4), 18-crown-6‚C 5 H 5 N (5), 2-(hydroxymethyl)-18-crown-6 (18crown-6CH 2 OH) (6)). A sulfonate compound, Ba(O 3 SCF 3 ) 2 (tetraglyme) (7), was also prepared by a similar reaction. The polydentate ligands of 1-6 are coordinated to the barium atoms through all of their donating atoms, and the trifluoroacetate ligands are found in four distinct types of bonding modes. The compounds were characterized by spectroscopic and analytical methods, and 1-6 are among the first examples of group 2 trifluoroacetate compounds with mononuclear or dinuclear structures in the solid state as determined by single-crystal X-ray diffraction. Ba 2 (O 2 CCF 3 ) 4 (12-crown-4) 2 (1) crystallizes from ethanol in monoclinic space group P2 1 /n with a ) 11.014(1) Å, b ) 12.016(1) Å, c ) 15.269(1) Å, β ) 104.47(1)°, and Z ) 4. Ba 2 (O 2 CCF 3 ) 4 (triglyme) 2 (2) crystallizes from ethanol in monoclinic space group P2 1 /n with a ) 11.203(1) Å, b ) 12.220(1) Å, c ) 15.451(1) Å, β ) 107.61(1)°, and Z ) 4. Ba 2 (O 2 CCF 3 ) 4 (15-crown-5CH 2 OH) 2 (3) crystallizes from ethanol in monoclinic space group P2 1 /c with a ) 12.445(2) Å, b ) 12.499(3) Å, c ) 15.615(2) Å, β ) 111.11 (1)°, and Z ) 4. Ba(O 2 CCF 3 ) 2 (cryptand( 222)) ( 4) crystallizes from toluene in the tetragonal space group P4 3 2 1 2 with a ) b ) 9.263(2) Å, c ) 35.897(7) Å, and Z ) 4. Ba(O 2 CCF 3 ) 2 (18-crown-6)(py) (5) crystallizes from pyridine in orthorhombic space group Pnma with a ) 27.178(3) Å, b ) 11.417(1) Å, c ) 9.133(1) Å, and Z ) 4. Ba(O 2 -CCF 3 ) 2 (18-crown-6CH 2 OH) (6) crystallizes from ethanol in monoclinic space group Pn with a ) 8.279(1) Å, b ) 11.410(1) Å, c ) 13.661(2) Å, β ) 98.41(1)°, and Z ) 2. Infrared spectroscopy on 1-6 supplied information on the relationships among ν asym (CO 2 ), bonding mode of the trifluoroacetate ligand, and donating ability of the polydentate ligand. Thermogravimetric analysis of 1-7 shows loss of the organic supporting ligands in the temperature range 250-600 °C with formation of BaF 2 .

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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Synthesis, Characterization, and Thermal Behavior of Polydentate Ligand Adducts of Barium Trifluoroacetate

1998

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“…Finally, it is worth noting in this section that a number of groups have investigated the use of neutral cyclic and acyclic polyether ligands including crown ethers to control metal ion coordination environments in metal-organic precursors. These studies have resulted in formation of soluble and sometimes volatile complexes including Ba(2,5,8,11,14-pentaoxapentadecane)(hfac) 2,200 Ba(hfac)(18-crown-6),201 andPb(OAc)2 (18-crown-6). 202 In some cases, such ether complexes react with the metal center to form olefin complexes, or with cleavage of a C-0 bond resulting in formation of an alkoxide species.…”

Section: Metal Alkoxide Compounds With Multidentate Ligandsmentioning

confidence: 99%

Chemical aspects of solution routes to perovskite-phase mixed-metal oxides from metal-organic precursors

Chandler¹,

Roger²,

1993

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“…Polyether complexes of barium β-diketonates and related derivatives are well-known and have been used as precursors for the chemical vapor deposition (CVD) of Ba-containing materials. − Fluorinated β-diketonate derivatives have been studied as a result of their lower tendency to dissociate their polyether ligand compared to non-fluorinated derivatives. However, where the deposition pathway involves the thermal decomposition of the β-diketonate ligand, these compounds often lead to the deposition of impure films due to the lack of a suitable mechanism to remove the organic byproducts.…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Characterization of Polyether Adducts of Barium and Strontium Carboxylates and Their Use in the Formation of MTiO₃ Films

et al. 1996

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The synthesis, characterization, and reactivity of new polyether adducts of strontium and barium carboxylates of general composition M(O(2)CCF(3))(n)()(L) (M = Ba, L = 15-crown-5, (1); M = Ba (2), Sr (3), respectively, with L = tetraglyme are reported. The compounds were synthesized by reaction of BaCO(3) or MH(2) (M = Sr or Ba) with organic acids in the presence of the polyether ligands. These compounds have been characterized by IR and (13)C and (1)H NMR spectroscopies, elemental analyses, and thermogravimetric analysis. The species Ba(2)(O(2)CCF(3))(4)(15-crown-5)(2) (1) and [Ba(2)(O(2)CCF(3))(4)(tetraglyme)](infinity) (2), were also characterized by single-crystal X-ray diffraction. Ba(2)(O(2)CCF(3))(4)(15-crown-5)(2) (1) crystallizes in the orthorhombic space group Cccm with cell dimensions of a = 13.949(1) Å, b = 19.376(2) Å, c = 16.029(1) Å, and Z = 8. [Ba(2)(O(2)CCF(3))(4)(tetraglyme)](infinity) (2) crystallizes in the monoclinic space group C2/c with cell dimensions of a = 12.8673(12) Å, b = 16.6981(13) Å, c = 15.1191(12) Å, beta = 99.049(8) degrees, and Z = 4. Compounds 1-3 thermally decompose at high temperatures in the solid state to give MF(2). However, solutions of compounds 1-3 dissolved in ethanol with Ti(O-i-Pr)(4) give crystalline perovskite phase MTiO(3) films, or in the case of mixtures of 2 and 3, Ba(1)(-)(x)()Sr(x)()TiO(3) films below 600 degrees C when spin coated onto silicon substrates and thermally treated. The crystallinity, purity, and elemental composition of the films was determined by glancing angle X-ray diffraction and Auger electron spectroscopy.

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Structure of bis(1,1,1,5,5,5-hexafluoro-2,4-pentanedionato)(2,5,8,11,14-pentaoxapentadecane)barium(II)

Cited by 38 publications

References 1 publication

Synthesis, Characterization, and Thermal Behavior of Polydentate Ligand Adducts of Barium Trifluoroacetate

Synthesis, Characterization, and Thermal Behavior of Polydentate Ligand Adducts of Barium Trifluoroacetate

Chemical aspects of solution routes to perovskite-phase mixed-metal oxides from metal-organic precursors

Synthesis and Characterization of Polyether Adducts of Barium and Strontium Carboxylates and Their Use in the Formation of MTiO₃ Films

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Structure of bis(1,1,1,5,5,5-hexafluoro-2,4-pentanedionato)(2,5,8,11,14-pentaoxapentadecane)barium(II)

Cited by 38 publications

References 1 publication

Synthesis, Characterization, and Thermal Behavior of Polydentate Ligand Adducts of Barium Trifluoroacetate

Synthesis, Characterization, and Thermal Behavior of Polydentate Ligand Adducts of Barium Trifluoroacetate

Chemical aspects of solution routes to perovskite-phase mixed-metal oxides from metal-organic precursors

Synthesis and Characterization of Polyether Adducts of Barium and Strontium Carboxylates and Their Use in the Formation of MTiO3 Films

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Synthesis and Characterization of Polyether Adducts of Barium and Strontium Carboxylates and Their Use in the Formation of MTiO₃ Films