Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds

Autores
Rius, Jordi; Vallcorba, Oriol; Crespi, Anna; Colombo, Fernando
Año de publicación
2017
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
Successful phasing of synchrotron through-the-substrate microdiffraction data by δ-recycling direct-methods largely depends on the number of missing intensities caused by the limited sample rotation range [J. Rius, Direct phasing from Patterson syntheses by δ recycling. Acta Cryst. A 2012, 68, 77–81]. Particularly, for the unfavorable triclinic system, dataset completeness resulting from a single series of consecutive ϕ-scans covering a total ϕ interval of ±35° is around 41%. This value is not enough for the routinary solution of a crystal structure by δ-recycling but can be increased by ~29% by applying the orthogonal χ strategy consisting of merging the information of two series of orthogonal ϕ-scans collected at the same microvolume of the polished thin section. Test calculations using simulated and experimental tts-data of the triclinic mineral axinite confirm that, with the help of the orthogonal χ strategy, crystal structures can be solved routinely. Since data in the ±35 ϕ-interval are normally accessible even for relatively thick glass-substrates (1–1.5 mm), a crystal structure can be determined from a single microvolume. For high-symmetry phases, due to the Laue symmetry redundancy, a single series of ϕ-scans normally suffices for the application of δ-recycling. However, when for experimental causes this series is incomplete, the orthogonal χ strategy also provides a simple way to increase the completeness which besides allowing solving the structure, is also beneficial for the subsequent refinement.
Fil: Rius, Jordi. Consejo Superior de Investigaciones Científicas. Instituto de Ciencia de los Materiales de Barcelona; España
Fil: Vallcorba, Oriol. ALBA Synchrotron Light Source; España
Fil: Crespi, Anna. Consejo Superior de Investigaciones Científicas. Instituto de Ciencia de los Materiales de Barcelona; España
Fil: Colombo, Fernando. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Centro de Investigaciones en Ciencias de la Tierra. Universidad Nacional de Córdoba. Facultad de Ciencias Exactas Físicas y Naturales. Centro de Investigaciones en Ciencias de la Tierra; Argentina
Materia
Recycling Phasing
Polished Thin Sections
Structure Solution
X-Ray Data Completeness
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/44906
Acceder
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oai_identifier_str oai:ri.conicet.gov.ar:11336/44906
network_acronym_str CONICETDig
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network_name_str CONICET Digital (CONICET)
spelling Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compoundsRius, JordiVallcorba, OriolCrespi, AnnaColombo, FernandoRecycling PhasingPolished Thin SectionsStructure SolutionX-Ray Data Completenesshttps://purl.org/becyt/ford/1.5https://purl.org/becyt/ford/1Successful phasing of synchrotron through-the-substrate microdiffraction data by δ-recycling direct-methods largely depends on the number of missing intensities caused by the limited sample rotation range [J. Rius, Direct phasing from Patterson syntheses by δ recycling. Acta Cryst. A 2012, 68, 77–81]. Particularly, for the unfavorable triclinic system, dataset completeness resulting from a single series of consecutive ϕ-scans covering a total ϕ interval of ±35° is around 41%. This value is not enough for the routinary solution of a crystal structure by δ-recycling but can be increased by ~29% by applying the orthogonal χ strategy consisting of merging the information of two series of orthogonal ϕ-scans collected at the same microvolume of the polished thin section. Test calculations using simulated and experimental tts-data of the triclinic mineral axinite confirm that, with the help of the orthogonal χ strategy, crystal structures can be solved routinely. Since data in the ±35 ϕ-interval are normally accessible even for relatively thick glass-substrates (1–1.5 mm), a crystal structure can be determined from a single microvolume. For high-symmetry phases, due to the Laue symmetry redundancy, a single series of ϕ-scans normally suffices for the application of δ-recycling. However, when for experimental causes this series is incomplete, the orthogonal χ strategy also provides a simple way to increase the completeness which besides allowing solving the structure, is also beneficial for the subsequent refinement.Fil: Rius, Jordi. Consejo Superior de Investigaciones Científicas. Instituto de Ciencia de los Materiales de Barcelona; EspañaFil: Vallcorba, Oriol. ALBA Synchrotron Light Source; EspañaFil: Crespi, Anna. Consejo Superior de Investigaciones Científicas. Instituto de Ciencia de los Materiales de Barcelona; EspañaFil: Colombo, Fernando. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Centro de Investigaciones en Ciencias de la Tierra. Universidad Nacional de Córdoba. Facultad de Ciencias Exactas Físicas y Naturales. Centro de Investigaciones en Ciencias de la Tierra; ArgentinaDe Gruyter2017-01info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/44906Rius, Jordi; Vallcorba, Oriol; Crespi, Anna; Colombo, Fernando; Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds; De Gruyter; Zeitschrift für Kristallographie Crystalline Materials; 232; 12; 1-2017; 827–8342194-49462196-7105CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/url/https://www.degruyter.com/view/j/zkri.ahead-of-print/zkri-2017-2064/zkri-2017-2064.xmlinfo:eu-repo/semantics/altIdentifier/doi/10.1515/zkri-2017-2064info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-sa/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-29T09:32:54Zoai:ri.conicet.gov.ar:11336/44906instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-09-29 09:32:55.214CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds
title Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds
spellingShingle Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds
Rius, Jordi
Recycling Phasing
Polished Thin Sections
Structure Solution
X-Ray Data Completeness
title_short Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds
title_full Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds
title_fullStr Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds
title_full_unstemmed Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds
title_sort Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds
dc.creator.none.fl_str_mv Rius, Jordi
Vallcorba, Oriol
Crespi, Anna
Colombo, Fernando
author Rius, Jordi
author_facet Rius, Jordi
Vallcorba, Oriol
Crespi, Anna
Colombo, Fernando
author_role author
author2 Vallcorba, Oriol
Crespi, Anna
Colombo, Fernando
author2_role author
author
author
dc.subject.none.fl_str_mv Recycling Phasing
Polished Thin Sections
Structure Solution
X-Ray Data Completeness
topic Recycling Phasing
Polished Thin Sections
Structure Solution
X-Ray Data Completeness
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.5
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv Successful phasing of synchrotron through-the-substrate microdiffraction data by δ-recycling direct-methods largely depends on the number of missing intensities caused by the limited sample rotation range [J. Rius, Direct phasing from Patterson syntheses by δ recycling. Acta Cryst. A 2012, 68, 77–81]. Particularly, for the unfavorable triclinic system, dataset completeness resulting from a single series of consecutive ϕ-scans covering a total ϕ interval of ±35° is around 41%. This value is not enough for the routinary solution of a crystal structure by δ-recycling but can be increased by ~29% by applying the orthogonal χ strategy consisting of merging the information of two series of orthogonal ϕ-scans collected at the same microvolume of the polished thin section. Test calculations using simulated and experimental tts-data of the triclinic mineral axinite confirm that, with the help of the orthogonal χ strategy, crystal structures can be solved routinely. Since data in the ±35 ϕ-interval are normally accessible even for relatively thick glass-substrates (1–1.5 mm), a crystal structure can be determined from a single microvolume. For high-symmetry phases, due to the Laue symmetry redundancy, a single series of ϕ-scans normally suffices for the application of δ-recycling. However, when for experimental causes this series is incomplete, the orthogonal χ strategy also provides a simple way to increase the completeness which besides allowing solving the structure, is also beneficial for the subsequent refinement.
Fil: Rius, Jordi. Consejo Superior de Investigaciones Científicas. Instituto de Ciencia de los Materiales de Barcelona; España
Fil: Vallcorba, Oriol. ALBA Synchrotron Light Source; España
Fil: Crespi, Anna. Consejo Superior de Investigaciones Científicas. Instituto de Ciencia de los Materiales de Barcelona; España
Fil: Colombo, Fernando. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Centro de Investigaciones en Ciencias de la Tierra. Universidad Nacional de Córdoba. Facultad de Ciencias Exactas Físicas y Naturales. Centro de Investigaciones en Ciencias de la Tierra; Argentina
description Successful phasing of synchrotron through-the-substrate microdiffraction data by δ-recycling direct-methods largely depends on the number of missing intensities caused by the limited sample rotation range [J. Rius, Direct phasing from Patterson syntheses by δ recycling. Acta Cryst. A 2012, 68, 77–81]. Particularly, for the unfavorable triclinic system, dataset completeness resulting from a single series of consecutive ϕ-scans covering a total ϕ interval of ±35° is around 41%. This value is not enough for the routinary solution of a crystal structure by δ-recycling but can be increased by ~29% by applying the orthogonal χ strategy consisting of merging the information of two series of orthogonal ϕ-scans collected at the same microvolume of the polished thin section. Test calculations using simulated and experimental tts-data of the triclinic mineral axinite confirm that, with the help of the orthogonal χ strategy, crystal structures can be solved routinely. Since data in the ±35 ϕ-interval are normally accessible even for relatively thick glass-substrates (1–1.5 mm), a crystal structure can be determined from a single microvolume. For high-symmetry phases, due to the Laue symmetry redundancy, a single series of ϕ-scans normally suffices for the application of δ-recycling. However, when for experimental causes this series is incomplete, the orthogonal χ strategy also provides a simple way to increase the completeness which besides allowing solving the structure, is also beneficial for the subsequent refinement.
publishDate 2017
dc.date.none.fl_str_mv 2017-01
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/11336/44906
Rius, Jordi; Vallcorba, Oriol; Crespi, Anna; Colombo, Fernando; Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds; De Gruyter; Zeitschrift für Kristallographie Crystalline Materials; 232; 12; 1-2017; 827–834
2194-4946
2196-7105
CONICET Digital
CONICET
url http://hdl.handle.net/11336/44906
identifier_str_mv Rius, Jordi; Vallcorba, Oriol; Crespi, Anna; Colombo, Fernando; Increasing data completeness in synchrotron tts-microdiffraction experiments for δ-recycling phasing of low-symmetry compounds; De Gruyter; Zeitschrift für Kristallographie Crystalline Materials; 232; 12; 1-2017; 827–834
2194-4946
2196-7105
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/https://www.degruyter.com/view/j/zkri.ahead-of-print/zkri-2017-2064/zkri-2017-2064.xml
info:eu-repo/semantics/altIdentifier/doi/10.1515/zkri-2017-2064
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv De Gruyter
publisher.none.fl_str_mv De Gruyter
dc.source.none.fl_str_mv reponame:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
collection CONICET Digital (CONICET)
instname_str Consejo Nacional de Investigaciones Científicas y Técnicas
repository.name.fl_str_mv CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas
repository.mail.fl_str_mv dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar
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score 13.070432

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