M<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from Routine
Single crystals of Sn<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> have been grown over a period of more than a decade in hermetically sealed flasks of various triorganotin(IV)-trihydrides in toluene/<i>N</i>,<i>N</i>-dimethylformamide and thos...
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| Format: | Article |
| Language: | English |
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MDPI AG
2023-04-01
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| Series: | Crystals |
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| Online Access: | https://www.mdpi.com/2073-4352/13/5/739 |
| _version_ | 1797600574622924800 |
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| author | Hans Reuter Dirk Schröder Kristina Peckskamp |
| author_facet | Hans Reuter Dirk Schröder Kristina Peckskamp |
| author_sort | Hans Reuter |
| collection | DOAJ |
| description | Single crystals of Sn<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> have been grown over a period of more than a decade in hermetically sealed flasks of various triorganotin(IV)-trihydrides in toluene/<i>N</i>,<i>N</i>-dimethylformamide and those of Pb<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> on a petri dish within some days from the reaction of Pb(ClO<sub>4</sub>)<sub>2</sub> with Sr(OH)<sub>2</sub>·8H<sub>2</sub>O. High-resolution X-ray diffraction data of the tetragonally crystallizing compounds have been collected conventionally at 100 K. Crystal structure determinations have been performed in space groups <i>P</i>4/<i>mnc</i> and <i>P</i><inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mover accent="true"><mn>4</mn><mo>¯</mo></mover></semantics></math></inline-formula>2<sub>1</sub><i>c</i> with different structure models because of a pretended specific systematic extinction condition. Its violation was routinely overseen because of the very low intensities of the respective reflections, an effect reinforced by crystal size. The non-existence of this systematic extinction was experimentally confirmed by studying the datasets in more detail, including the simulation of layer photographs. The importance of additional information obtained from dataset analysis tools and structure validation programs to assess the different structure models is demonstrated. Structures of both molecules are analyzed with respect to the molecules as a whole as well as to their constructive building units: two crystallographic different prototypes of {MO<sub>4</sub>} coordination polyhedra with a bent seesaw conformation, one μ<sub>3</sub>-OH- and one μ<sub>3</sub>-O- group, each trigonal-pyramidally coordinated. |
| first_indexed | 2024-03-11T03:49:43Z |
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| id | doaj.art-6ebdd8b54dca4c0680cdf89432a2c761 |
| institution | Directory Open Access Journal |
| issn | 2073-4352 |
| language | English |
| last_indexed | 2024-03-11T03:49:43Z |
| publishDate | 2023-04-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Crystals |
| spelling | doaj.art-6ebdd8b54dca4c0680cdf89432a2c7612023-11-18T00:59:13ZengMDPI AGCrystals2073-43522023-04-0113573910.3390/cryst13050739M<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from RoutineHans Reuter0Dirk Schröder1Kristina Peckskamp2Chemistry, Department of Biology/Chemistry, Osnabrück University, Barbarastr. 7, D-49069 Osnabrück, GermanyChemistry, Department of Biology/Chemistry, Osnabrück University, Barbarastr. 7, D-49069 Osnabrück, GermanyChemistry, Department of Biology/Chemistry, Osnabrück University, Barbarastr. 7, D-49069 Osnabrück, GermanySingle crystals of Sn<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> have been grown over a period of more than a decade in hermetically sealed flasks of various triorganotin(IV)-trihydrides in toluene/<i>N</i>,<i>N</i>-dimethylformamide and those of Pb<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> on a petri dish within some days from the reaction of Pb(ClO<sub>4</sub>)<sub>2</sub> with Sr(OH)<sub>2</sub>·8H<sub>2</sub>O. High-resolution X-ray diffraction data of the tetragonally crystallizing compounds have been collected conventionally at 100 K. Crystal structure determinations have been performed in space groups <i>P</i>4/<i>mnc</i> and <i>P</i><inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mover accent="true"><mn>4</mn><mo>¯</mo></mover></semantics></math></inline-formula>2<sub>1</sub><i>c</i> with different structure models because of a pretended specific systematic extinction condition. Its violation was routinely overseen because of the very low intensities of the respective reflections, an effect reinforced by crystal size. The non-existence of this systematic extinction was experimentally confirmed by studying the datasets in more detail, including the simulation of layer photographs. The importance of additional information obtained from dataset analysis tools and structure validation programs to assess the different structure models is demonstrated. Structures of both molecules are analyzed with respect to the molecules as a whole as well as to their constructive building units: two crystallographic different prototypes of {MO<sub>4</sub>} coordination polyhedra with a bent seesaw conformation, one μ<sub>3</sub>-OH- and one μ<sub>3</sub>-O- group, each trigonal-pyramidally coordinated.https://www.mdpi.com/2073-4352/13/5/739crystal growthsystematic extinction conditionspace group determinationrefinement strategiesstructure validationbuilding units |
| spellingShingle | Hans Reuter Dirk Schröder Kristina Peckskamp M<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from Routine Crystals crystal growth systematic extinction condition space group determination refinement strategies structure validation building units |
| title | M<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from Routine |
| title_full | M<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from Routine |
| title_fullStr | M<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from Routine |
| title_full_unstemmed | M<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from Routine |
| title_short | M<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub> of M = Sn, Pb: Single Crystal Growth and Crystal Structure Determinations Far Away from Routine |
| title_sort | m sub 6 sub o sub 4 sub oh sub 4 sub of m sn pb single crystal growth and crystal structure determinations far away from routine |
| topic | crystal growth systematic extinction condition space group determination refinement strategies structure validation building units |
| url | https://www.mdpi.com/2073-4352/13/5/739 |
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