Radiation decay - a new tool in macromolecular crystallography

Otwinowski, Zbyszek; Borek, Dominika; Minor, W.

doi:10.1107/s010876730209459x

Cited by 12 publications

(15 citation statements)

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“…[38] Refinement and data reduction were performed using the HKL DENZO and SCALEPACK software and a multiscan absorption correction was applied (SCALEPACK). [39] Transmission coefficients were calculated using SHELXL-2012.…”

Section: Synthesis Of Bis(boryl)ferrocene 5 Cmentioning

confidence: 99%

Chiral Bora[1]ferrocenophanes: Syntheses, Mechanistic Insights, and Ring‐Opening Polymerizations

Sadeh

Bhattacharjee

Sarbisheh

et al. 2014

Chemistry A European J

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A series of new boron-bridged [1]ferrocenophanes ([1]FCPs) was prepared by salt-metathesis reactions between enantiomerically pure dilithioferrocenes and amino(dichloro)boranes (Et2 NBCl2 , iPr2 NBCl2 , or tBu(Me3 Si)NBCl2 ). The dilithioferrocenes were prepared in situ by lithium-bromine exchange from the respective planar-chiral dibromides (Sp ,Sp )-[1-Br-2-(HR2 C)H3 C5 ]2 Fe (R=Me or Et). In most of the cases, mixtures of the targeted [1]FCPs 4 and the unwanted 1,1'-bis(boryl)ferrocenes 5 were formed. The product ratio depends on the bulkiness of the amino group, the speed of addition of the amino(dichloro)borane, the alkyl group on Cp rings, and in particular on the reaction temperature. The formation of strained [1]FCPs is strongly favored by increased reaction temperatures. Secondly, CHEt2 groups at Cp rings favored the formation of the targeted [1]FCPs stronger than CHMe2 groups. These discoveries open up new possibilities to further suppress the formation of unwanted byproducts by a careful choice of the reaction temperature and through tailoring the bulkiness of CHR2 groups on ferrocene. Thermal ring-opening polymerizations of selected boron-bridged [1]FCPs gave metallopolymers with a Mw of 10 kDa (GPC).

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Section: Synthesis Of Bis(boryl)ferrocene 5 Cmentioning

confidence: 99%

Chiral Bora[1]ferrocenophanes: Syntheses, Mechanistic Insights, and Ring‐Opening Polymerizations

Sadeh

Bhattacharjee

Sarbisheh

et al. 2014

Chemistry A European J

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“…[57] An absorption correction was applied with a multiscan method using SCALEPACK. [58] The figures were created with SHELXTL [59] and DIAMOND (release 2.1e, 2001). Selected crystallographic data are presented in Tables 1 and 2.…”

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confidence: 99%

Polynuclear Bismuth‐Oxo Clusters: Insight into the Formation Process of a Metal Oxide

Mehring

Mansfeld

Paalasmaa

et al. 2006

Chemistry A European J

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The reaction of the bismuth silanolates [Bi(OSiR2R')3] (R = R' = Me, Et, iPr; R = Me, R' = tBu) with water has been studied. Partial hydrolysis gave polynuclear bismuth-oxo clusters whereas amorphous bismuth-oxo(hydroxy) silanolates were obtained when an excess of water was used in the hydrolysis reaction. The metathesis reaction of BiCl3 with NaOSiMe3 provided mixtures of heterobimetallic silanolates. The molecular structures of [Bi18Na4O20(OSiMe3)18] (2), [Bi33NaO38(OSiMe3)24].3 C7H8 (3.3 C7H8), [Bi50Na2O64(OH)2(OSiMe3)22].2 C7H8.2H2O (4.2 C7H8.2 H2O), [Bi4O2(OSiEt3)8] (5), [Bi9O7(OSiMe3)13].0.5 C7H8 (6. 0.5C7H8), [Bi18O18(OSiMe3)18)].2C7H8 (7. 2C7H8) and [Bi20O18(OSiMe3)24].3C7H8 (8.3C7H8) are presented and compared with the solid-state structures of [Bi22O26(OSiMe2tBu)14] (9) and beta-Bi2O3. Compound 2 crystallises in the triclinic space group P1 with the lattice constants a = 17.0337(9), b = 19.5750(14), c = 26.6799(16) A, alpha = 72.691(4), beta = 73.113(4) and gamma = 70.985(4) degrees ; compound 3.3C7H8 crystallises in the monoclinic space group P2(1)/n with the lattice constants a = 20.488(4), b = 22.539(5), c = 26.154(5) A and beta = 100.79(3) degrees ; compound 4.2C7H82 H2O crystallises in the monoclinic space group P2(1)/n with the lattice constants a = 20.0518(12), b = 24.1010(15), c = 27.4976(14) A and beta = 103.973(3) degrees ; compound 5 crystallises in the monoclinic space group P2(1)/c with the lattice constants a = 25.256(5), b = 15.372(3), c = 21.306(4) A and beta = 113.96(3) degrees ; compound 6.0.5C7H8 crystallises in the triclinic space group P1 with the lattice constants a = 15.1916(9), b = 15.2439(13), c = 22.487(5) A, alpha = 79.686(3), beta = 74.540(5) and gamma = 66.020(4) degrees ; compound 7.2C7H8 crystallises in the triclinic space group P1 with the lattice constants a = 14.8295(12), b = 16.1523(13), c = 18.4166(17) A, alpha = 75.960(4), beta = 79.112(4) and gamma = 63.789(4) degrees ; and compound 8.3C7H8 crystallises in the triclinic space group P1 with the lattice constants a = 17.2915(14), b = 18.383(2), c = 18.4014(18) A, alpha = 95.120(5), beta = 115.995(5) and gamma = 106.813(5) degrees . The molecular structures of the bismuth-rich compounds are related to the CaF2-type structure. Formally, the hexanuclear [Bi6O8]2+ fragment might be described as the central building unit, which is composed of bismuth atoms placed at the vertices of an octahedron and oxygen atoms capping the trigonal faces. Depending on the reaction conditions and the identity of R, the thermal decomposition of the hydrolysis products [Bi(n)O(l)(OH)(m-)(OSiR3)(3n-(2l-m))] gives alpha-Bi2O3, beta-Bi2O3, Bi12SiO20 or Bi4Si3O12.

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“…Die . Nach der Mittelung der symmetrieäquivalenten Reflexe und der Korrektur der Lorentz-, Polarisations-und Absorptionseffekte mit dem Programm SCALEPACK [27] (T min = 0.346, T max = 0.164) wurde ein interner R-Wert von 0.069 erhalten. Zwei SiMe 2 tBu-Gruppen (C21-C36) und zwei tBu-Gruppen (C65, C66, C73-C76) wurden isotrop verfeinert.…”

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Ein monomeres Bismutsilanolat zur Synthese des Bismutoxoclusters [Bi₂₂O₂₆(OSiMe₂tBu)₁₄]

2004

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Radiation decay - a new tool in macromolecular crystallography

Cited by 12 publications

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Chiral Bora[1]ferrocenophanes: Syntheses, Mechanistic Insights, and Ring‐Opening Polymerizations

Chiral Bora[1]ferrocenophanes: Syntheses, Mechanistic Insights, and Ring‐Opening Polymerizations

Polynuclear Bismuth‐Oxo Clusters: Insight into the Formation Process of a Metal Oxide

Ein monomeres Bismutsilanolat zur Synthese des Bismutoxoclusters [Bi₂₂O₂₆(OSiMe₂tBu)₁₄]

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Radiation decay - a new tool in macromolecular crystallography

Cited by 12 publications

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Chiral Bora[1]ferrocenophanes: Syntheses, Mechanistic Insights, and Ring‐Opening Polymerizations

Chiral Bora[1]ferrocenophanes: Syntheses, Mechanistic Insights, and Ring‐Opening Polymerizations

Polynuclear Bismuth‐Oxo Clusters: Insight into the Formation Process of a Metal Oxide

Ein monomeres Bismutsilanolat zur Synthese des Bismutoxoclusters [Bi22O26(OSiMe2tBu)14]

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Ein monomeres Bismutsilanolat zur Synthese des Bismutoxoclusters [Bi₂₂O₂₆(OSiMe₂tBu)₁₄]