Structure of the new mineral sarrabusite, Pb5CuCl4(SeO3)4, solved by manual electron-diffraction tomography

Gemmi, Mauro; Campostrini, Italo; Demartin, Francesco; Gorelik, Tatiana E.; Gramaccioli, C. M.

doi:10.1107/s010876811104688x

Cited by 41 publications

(24 citation statements)

References 48 publications

(51 reference statements)

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“…The interest has also been stimulated by the attempts to understand purely fundamental reasons for structural diversity in selenites and its underlying crystal chemical mechanisms [10][11][12]. In this regard, copper selenite chlorides are of particular importance, due to their natural occurrences as minerals [13][14][15][16][17] and the structures featuring 'scissor'-type disruption of a bonding network induced by the well-localized stereochemically active but chemicall inactive lone electron pairs [18][19][20][21][22].…”

Section: Introductionmentioning

confidence: 99%

[NaCl][Cu(HSeO₃)₂], NaCl-intercalated Cu(HSeO₃)₂: synthesis, crystal structure and comparison with related compounds

Kovrugin¹,

Krivovichev²,

Mentré

et al. 2015

Zeitschrift Für Kristallographie - Crystalline Materials

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NaCl][Cu(HSeO 3 ) 2 ], NaCl-intercalated Cu(HSeO 3 ) 2 : synthesis, crystal structure and comparison with related compounds Abstract: Single crystals of [NaCl][Cu(HSeO 3 ) 2 ] have been prepared by the chemical vapor transport reactions. Its crystal structure (monoclinic, C2/c, a = 13.9874(7), b = 7.2594(4), c = 9.0421(5) Å, β = 127.046(2)°, V = 732.81(7) Å 3 ) is based upon electroneutral [Cu(HSeO 3 ) 2 ] sheets formed by corner sharing between the [CuO 4 ] squares and (HSeO 3 ) groups that are parallel to the (100) plane. Each (SeO 2 OH) -group forms the O h 1 ... O2 hydrogen bond to an adjacent hydroselenite group to constitute a [(SeO 2 OH) 2 ] 2-dimer that provides additional stabilization of the copper diselenite sheet. The [Cu(HSeO 3 ) 2 ] sheets alternate with the sheets consisting of zigzag-Na-Cl-Na-Cl-chains formed by Cl atoms and disordered Na sites. The chains are parallel to the c axis. The linkage between the alternating electroneutral [Cu(HSeO 3 ) 2 ] and [NaCl] sheets is provided by the Cu-Cl and Na-O bonds. The coordination of Na is fivefold and consists of three O and two Cl atoms. [NaCl][Cu(HSeO 3 ) 2 ] is a new member of the group of compounds based upon the M(HSeO 3 ) 2 layers (M 2+ = Cu, Co, Cd). The prototype structure for this group is [Cu(HSeO 3 ) 2 ] that does not have any chemical species separating the copper hydroselenite layers. In other compounds, the interlayer space between the [Cu(HSeO 3 ) 2 ] 0 layers is occupied by structural units of different complexity. [NaCl][Cu(HSeO 3 ) 2 ] can be considered as [Cu(HSeO 3 ) 2 ] intercalated with the NaCl layers consisting of one-dimensional-Na-Cl-Na-Cl-chains.

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Section: Introductionmentioning

confidence: 99%

[NaCl][Cu(HSeO₃)₂], NaCl-intercalated Cu(HSeO₃)₂: synthesis, crystal structure and comparison with related compounds

Kovrugin¹,

Krivovichev²,

Mentré

et al. 2015

Zeitschrift Für Kristallographie - Crystalline Materials

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“…The success of ADT has encouraged other groups to develop their own systems for tomographic acquisition of electron diffraction data (Palatinus et al 2011;Gemmi et al 2012;Fan et al 2013;Cora et al 2014). A promising alternative experimental setting was proposed with the rotation electron diffraction (RED) method, where mechanical sample tilt is supplemented by beam tilt for a finer reciprocal space sampling (Zhang et al 2010).…”

Section: Discussionmentioning

confidence: 99%

“…It is anyway possible to perform ADT without any specific acquisition software, eventually collecting data in selected area electron diffraction (SAED) and using TEM imaging for crystal tracking (see, e.g., Palatinus et al 2011;Gemmi et al 2012). This procedure normally implies a longer beam exposure and eventually a more pronounced sample degradation due to beam damage.…”

Section: Introductionmentioning

confidence: 99%

Single nano crystal analysis using automated electron diffraction tomography

Mugnaioli

2014

Rend. Fis. Acc. Lincei

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Most of hitherto unknown natural phases and many new synthetic compounds can grow only in the form of nanocrystals. X-ray powder diffraction is the most widespread technique for the structural characterization of nanomaterials, but its use is limited by two main restrictions: structural information is projected in one dimension and data come from the whole sample and not from a specific single crystallite. On the other hand, crystallographic methods based on the scattering of accelerated electrons are able to obtain 3-D structural data from single volumes of few tens of nanometers. Automated diffraction tomography is a recently developed method able to record more kinematical and complete electron diffraction data. This method consists in the acquisition of a series of electron diffraction patterns while the sample is rotated around an arbitrary tilt axis by sequential mechanical steps, within the full tilt range of the microscope goniometer. Data collection can be performed on highly beam sensitive materials, as no time is required for orienting the crystal along specific crystallographic orientations and mild illumination conditions are used. In the last years many nanocrystalline materials belonging to different material classes have been characterized by automated diffraction tomography. This review describes the different experimental and analytical approaches used for the determination of inorganic and organic phases and points out the advantages offered by automated diffraction tomography for the characterization of minor phases available only in polyphasic nanomixtures and for the description of domain arrangement in polycrystalline nanocomposites.

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“…In principle, ADT can be implemented on any microscope (see, for example, Gorelik et al, 2011;Palatinus et al, 2011;Gemmi et al, 2012). Until now, most of the structures determined by this strategy have been done in Mainz thanks to the development of an acquisition routine that permits collecting nano electron diffraction (NED) patterns and tracking the crystal position in scanning transmission electron microscopy (STEM) mode.…”

Section: Introductionmentioning

confidence: 99%

Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes

et al. 2013

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δ Recycling is a simple procedure for directly extracting phase information from Patterson-type functions [Rius (2012). Acta Cryst. A68, 399-400]. This new phasing method has a clear theoretical basis and was developed with ideal single-crystal X-ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507-513]. When combined with precession electron diffraction, it delivers quasi-kinematical intensity data even for complex inorganic compounds, so that single-crystal diffraction data of nanometric volumes are now available for structure determination by direct methods. To check the tolerance of δ recycling to missing data-collection corrections and to deviations from kinematical behaviour of ADT intensities, δ recycling has been applied to differently shaped nanocrystals of various inorganic materials. The results confirm that it can phase ADT data very efficiently. In some cases even more complete structure models than those derived from conventional direct methods and least-squares refinement have been found. During this study it has been demonstrated that the Wilson-plot scaling procedure is largely insensitive to sample thickness variations and missing absorption corrections affecting electron ADT intensities.

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Structure of the new mineral sarrabusite, Pb₅CuCl₄(SeO₃)₄, solved by manual electron-diffraction tomography

Cited by 41 publications

References 48 publications

[NaCl][Cu(HSeO₃)₂], NaCl-intercalated Cu(HSeO₃)₂: synthesis, crystal structure and comparison with related compounds

[NaCl][Cu(HSeO₃)₂], NaCl-intercalated Cu(HSeO₃)₂: synthesis, crystal structure and comparison with related compounds

Single nano crystal analysis using automated electron diffraction tomography

Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes

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Structure of the new mineral sarrabusite, Pb5CuCl4(SeO3)4, solved by manual electron-diffraction tomography

Cited by 41 publications

References 48 publications

[NaCl][Cu(HSeO3)2], NaCl-intercalated Cu(HSeO3)2: synthesis, crystal structure and comparison with related compounds

[NaCl][Cu(HSeO3)2], NaCl-intercalated Cu(HSeO3)2: synthesis, crystal structure and comparison with related compounds

Single nano crystal analysis using automated electron diffraction tomography

Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes

Contact Info

Product

Resources

About

Structure of the new mineral sarrabusite, Pb₅CuCl₄(SeO₃)₄, solved by manual electron-diffraction tomography

[NaCl][Cu(HSeO₃)₂], NaCl-intercalated Cu(HSeO₃)₂: synthesis, crystal structure and comparison with related compounds

[NaCl][Cu(HSeO₃)₂], NaCl-intercalated Cu(HSeO₃)₂: synthesis, crystal structure and comparison with related compounds