Fatma Tugce Senberber Dumanli, Sibel Kavci Karaagac, A. Kipcak, E. Moroydor Derun
Abstract The copper borate of CuB2O4 in tetragonal form was successfully synthesized as a single-phase by using a solid-state method without using any modifying agent. For the designed experimental procedure, the optimized reaction conditions were estimated as a reaction temperature of 950 °C, reaction time of 240 min, argon atmosphere and Cu:B ratio of 1:5. The possible reaction mechanism estimated for both boron sources of boric acid and boron oxide. In both sets, the lower ratios of Cu:B supported CuB2O4 formation. In the use of boric acid as a boron source, higher reaction yield percentages (98 %) and lower particle sizes were determined. The micron-scale rounded particles were observed in morphological analyses and the particles were shaped in homogeneity in the use of boron oxide as a boron source. The specific FT-IR peaks were observed at the band values of 1190, 1035, 988, 945, 890, 695, 631, 540 and 479 cm−1. The experimental results highlighted the probable use of solid-state in the copper borate synthesis.
{"title":"Effect of different boron sources on the copper borates in solid-state synthesis","authors":"Fatma Tugce Senberber Dumanli, Sibel Kavci Karaagac, A. Kipcak, E. Moroydor Derun","doi":"10.1515/zkri-2023-0023","DOIUrl":"https://doi.org/10.1515/zkri-2023-0023","url":null,"abstract":"Abstract The copper borate of CuB2O4 in tetragonal form was successfully synthesized as a single-phase by using a solid-state method without using any modifying agent. For the designed experimental procedure, the optimized reaction conditions were estimated as a reaction temperature of 950 °C, reaction time of 240 min, argon atmosphere and Cu:B ratio of 1:5. The possible reaction mechanism estimated for both boron sources of boric acid and boron oxide. In both sets, the lower ratios of Cu:B supported CuB2O4 formation. In the use of boric acid as a boron source, higher reaction yield percentages (98 %) and lower particle sizes were determined. The micron-scale rounded particles were observed in morphological analyses and the particles were shaped in homogeneity in the use of boron oxide as a boron source. The specific FT-IR peaks were observed at the band values of 1190, 1035, 988, 945, 890, 695, 631, 540 and 479 cm−1. The experimental results highlighted the probable use of solid-state in the copper borate synthesis.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-08-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48662542","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-08-22eCollection Date: 2023-06-01DOI: 10.1515/iss-2023-0006
Carl Meißner, Frank Meyer, Karsten Ridwelski
Objectives: For years, many efforts have been invested to prepare patients, in particular, those with reduced physical and psychic status, much better to provide and finally achieve better outocme if there is time available to provide several beneficial measures.
Methods: Therefore, the objective was to illustrate the concept and various single elements of a complex prehabilitation concept based on (i) selective references from the medical literature and (ii) own clinical experiences from clinical practice in general and abdominal surgery.
Results: Prehabiliation can be considered the solution of the efforts to improve preoperative status for patients in a disadvantageous status for almost all types of surgery and all other operative and/or interventional procedures. It is the targeted process to improve individual functionality and organ function before a planned (elective) surgical intervention; P. comprises basically nutritional, physical and psychological measures; P. focusses especially onto the elderly, frail and malnourished patients before a planned surgical intervention; the overall aim is to significantly improve final outcome characterized by shorter length of stay, lower complication rate and mortality as well as cost efficiency; P. is especially important in cancer surgery, in which the beneficial effects can be particularly implemented; P. programs and/or "Standard Operating Protocols" (SOP) may help to establish and materialize its single aspects and enhanced recovery after surgery (ERAS). There is still further potential to reliably establish and to utilize the options of prehabilitation measures as listed above.
Conclusions: Prehabiliation is an indispensable aspect in today's preparation for elective surgery, which needs to become obligatory part of the preparation measures to planned surgical interventions, which can further contribute to a better final outcome and ERAS as well as, in addtion, needs to be further developed and accomplished.
{"title":"Prehabilitation in elective surgical interventions - what must the general and abdominal surgeon know.","authors":"Carl Meißner, Frank Meyer, Karsten Ridwelski","doi":"10.1515/iss-2023-0006","DOIUrl":"10.1515/iss-2023-0006","url":null,"abstract":"<p><strong>Objectives: </strong>For years, many efforts have been invested to prepare patients, in particular, those with reduced physical and psychic status, much better to provide and finally achieve better outocme if there is time available to provide several beneficial measures.</p><p><strong>Methods: </strong>Therefore, the objective was to illustrate the concept and various single elements of a complex prehabilitation concept based on (i) selective references from the medical literature and (ii) own clinical experiences from clinical practice in general and abdominal surgery.</p><p><strong>Results: </strong>Prehabiliation can be considered the solution of the efforts to improve preoperative status for patients in a disadvantageous status for almost all types of surgery and all other operative and/or interventional procedures. It is the targeted process to improve individual functionality and organ function before a planned (elective) surgical intervention; P. comprises basically nutritional, physical and psychological measures; P. focusses especially onto the elderly, frail and malnourished patients before a planned surgical intervention; the overall aim is to significantly improve final outcome characterized by shorter length of stay, lower complication rate and mortality as well as cost efficiency; P. is especially important in cancer surgery, in which the beneficial effects can be particularly implemented; P. programs and/or \"Standard Operating Protocols\" (SOP) may help to establish and materialize its single aspects and enhanced recovery after surgery (ERAS). There is still further potential to reliably establish and to utilize the options of prehabilitation measures as listed above.</p><p><strong>Conclusions: </strong>Prehabiliation is an indispensable aspect in today's preparation for elective surgery, which needs to become obligatory part of the preparation measures to planned surgical interventions, which can further contribute to a better final outcome and ERAS as well as, in addtion, needs to be further developed and accomplished.</p>","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"215 1","pages":"93-101"},"PeriodicalIF":1.3,"publicationDate":"2023-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10696941/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89334034","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
S. Stefanovich, B. Lazoryak, A. Antipin, A. Volkov, Andrei I. Evdokimov, O. A. Gurbanova, O. Dimitrova, D. Deyneko
Abstract Large-scale single crystals of Ca9Mg(PO4)6(PO3OH), Ca9Zn(PO4)6(PO3OH), and Ca9Co(PO4)6(PO3OH) were synthesized using hydrothermal technique, and turned out to be similar to natural bone whitlockite. The hexagonal single crystals about 1 mm with high-quality were obtained with this method for the first time. The crystals were of sufficiently good quality for the precision X-ray structural investigation. The compounds crystallize in usual for this structural type trigonal space group R3c. Presence of hydrogen atom in the structure was confirmed by means of infra-red (IR) spectroscopy, differential scanning calorimetry (DSC) and differential thermogravimetry (DTG) methods. Based on the analysis of the local bond valence sum (BVS), a conclusion on the localization of H atoms was made. The formation of O–H groups and hydrogen bonds H⋯O in vicinity of PO4 tetrahedra was shown and similar to bone whitlockite. This research provides new data on possibility of using hydrothermal technique for obtaining doped bone whitlockites. Hydrogen-containing doped whitlockites can combine bioactive properties and improve biocompatibility due to similarity to natural bond. New structural data are useful for finding the ways to better biocompatibility of whitlockite-based materials.
{"title":"Crystal structures of biocompatible Mg-, Zn-, and Co-whitlockites synthesized via one-step hydrothermal reaction","authors":"S. Stefanovich, B. Lazoryak, A. Antipin, A. Volkov, Andrei I. Evdokimov, O. A. Gurbanova, O. Dimitrova, D. Deyneko","doi":"10.1515/zkri-2023-0016","DOIUrl":"https://doi.org/10.1515/zkri-2023-0016","url":null,"abstract":"Abstract Large-scale single crystals of Ca9Mg(PO4)6(PO3OH), Ca9Zn(PO4)6(PO3OH), and Ca9Co(PO4)6(PO3OH) were synthesized using hydrothermal technique, and turned out to be similar to natural bone whitlockite. The hexagonal single crystals about 1 mm with high-quality were obtained with this method for the first time. The crystals were of sufficiently good quality for the precision X-ray structural investigation. The compounds crystallize in usual for this structural type trigonal space group R3c. Presence of hydrogen atom in the structure was confirmed by means of infra-red (IR) spectroscopy, differential scanning calorimetry (DSC) and differential thermogravimetry (DTG) methods. Based on the analysis of the local bond valence sum (BVS), a conclusion on the localization of H atoms was made. The formation of O–H groups and hydrogen bonds H⋯O in vicinity of PO4 tetrahedra was shown and similar to bone whitlockite. This research provides new data on possibility of using hydrothermal technique for obtaining doped bone whitlockites. Hydrogen-containing doped whitlockites can combine bioactive properties and improve biocompatibility due to similarity to natural bond. New structural data are useful for finding the ways to better biocompatibility of whitlockite-based materials.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"0 1","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-08-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"66887776","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Systematization of the vast number of known crystal structures of intermetallic phases is a challenge. One previously proposed group is referred to here as vacancy variants of the W-type structure. Members of this group, may, however, not be easily recognized because of the structural irregularity introduced by the vacancies. Descriptions of the experimentally observed crystal structures of Ni3Sn4 and FeAl2 in terms of vacancy variants of the W-type structure are, respectively, derived by establishing a lattice correspondence with the W-type structure, allowing, in particular, identification of the vacant sites. In both cases only small deviatoric strains are required to obtain the experimentally encountered lattice parameters, and generally small atomic displacements occur from the ideal positions, thus demonstrating significance of the lattice correspondence. The lattice correspondences allow, for both Ni3Sn4 and FeAl2, relating reported microstructure evidence (directions/planes occurring in orientation relationships and crystal habits but also on twinning and slip) with such typical for metals and solid solutions with W-type (“bcc”) structures. This demonstrates that the established lattice correspondences have a significance going beyond a descriptive one, but the underlying W-type structures reveal themselves in the materials’ behavior.
{"title":"Ni3Sn4 and FeAl2 as vacancy variants of the W-type (“bcc”) structure","authors":"A. Leineweber","doi":"10.1515/zkri-2023-0021","DOIUrl":"https://doi.org/10.1515/zkri-2023-0021","url":null,"abstract":"Abstract Systematization of the vast number of known crystal structures of intermetallic phases is a challenge. One previously proposed group is referred to here as vacancy variants of the W-type structure. Members of this group, may, however, not be easily recognized because of the structural irregularity introduced by the vacancies. Descriptions of the experimentally observed crystal structures of Ni3Sn4 and FeAl2 in terms of vacancy variants of the W-type structure are, respectively, derived by establishing a lattice correspondence with the W-type structure, allowing, in particular, identification of the vacant sites. In both cases only small deviatoric strains are required to obtain the experimentally encountered lattice parameters, and generally small atomic displacements occur from the ideal positions, thus demonstrating significance of the lattice correspondence. The lattice correspondences allow, for both Ni3Sn4 and FeAl2, relating reported microstructure evidence (directions/planes occurring in orientation relationships and crystal habits but also on twinning and slip) with such typical for metals and solid solutions with W-type (“bcc”) structures. This demonstrates that the established lattice correspondences have a significance going beyond a descriptive one, but the underlying W-type structures reveal themselves in the materials’ behavior.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49636937","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Michael Johnscher, Birgit Gerke, Jutta Kösters, T. Block, O. Niehaus, M. Reimann, Rainer Pöttgen
Abstract The intermetallic compounds (Ca0.95Cd0.10)Pd2Cd3, SrPd2Cd3 and (Eu0.95Cd0.10)Pd2Cd3 were synthesized from the elements in sealed niobium ampoules in an induction furnace. The polycrystalline samples were characterized through their Guinier powder patterns. The structures were refined from single crystal X-ray diffractometer data: YNi2Al3 type, P6/mmm, a = 984.61(5), c = 455.33(3) pm, wR2 = 0.0216, 376 F2 values, 21 variables for (Ca0.95Cd0.10)Pd2Cd3, a = 998.55(8), c = 453.65(3) pm, wR2 = 0.0296, 341 F2 values, 17 variables for SrPd2Cd3 and a = 992.57(4), c = 457.34(2) pm, wR2 = 0.0300, 384 F2 values, 21 variables for (Eu0.95Cd0.10)Pd2Cd3. The striking crystal chemical motif in the three structures is a planar [PdCd2] Kagome-type layer. The two crystallographically independent Ca (Sr, Eu) atoms have a coordination number of 18 by 6 Pd and 12 Cd atoms. The calcium and europium compound show a small degree of Ca (Eu) substitution by Cd2 dumb-bells with 281 pm Cd–Cd in (Eu0.95Cd0.10)Pd2Cd3. Temperature dependent magnetic susceptibility measurements show Curie–Weiss behaviour (7.63(1) µB/Eu atom) for the europium compound and the onset of ferromagnetic ordering at TC = 14.9(2) K. The divalent character of europium is corroborated by 151Eu Mössbauer spectroscpy.
{"title":"(Ca0.95Cd0.10)Pd2Cd3, SrPd2Cd3 and (Eu0.95Cd0.10)Pd2Cd3 with YNi2Al3 type structure – crystal chemistry and magnetic hyperfine interactions","authors":"Michael Johnscher, Birgit Gerke, Jutta Kösters, T. Block, O. Niehaus, M. Reimann, Rainer Pöttgen","doi":"10.1515/zkri-2023-0025","DOIUrl":"https://doi.org/10.1515/zkri-2023-0025","url":null,"abstract":"Abstract The intermetallic compounds (Ca0.95Cd0.10)Pd2Cd3, SrPd2Cd3 and (Eu0.95Cd0.10)Pd2Cd3 were synthesized from the elements in sealed niobium ampoules in an induction furnace. The polycrystalline samples were characterized through their Guinier powder patterns. The structures were refined from single crystal X-ray diffractometer data: YNi2Al3 type, P6/mmm, a = 984.61(5), c = 455.33(3) pm, wR2 = 0.0216, 376 F2 values, 21 variables for (Ca0.95Cd0.10)Pd2Cd3, a = 998.55(8), c = 453.65(3) pm, wR2 = 0.0296, 341 F2 values, 17 variables for SrPd2Cd3 and a = 992.57(4), c = 457.34(2) pm, wR2 = 0.0300, 384 F2 values, 21 variables for (Eu0.95Cd0.10)Pd2Cd3. The striking crystal chemical motif in the three structures is a planar [PdCd2] Kagome-type layer. The two crystallographically independent Ca (Sr, Eu) atoms have a coordination number of 18 by 6 Pd and 12 Cd atoms. The calcium and europium compound show a small degree of Ca (Eu) substitution by Cd2 dumb-bells with 281 pm Cd–Cd in (Eu0.95Cd0.10)Pd2Cd3. Temperature dependent magnetic susceptibility measurements show Curie–Weiss behaviour (7.63(1) µB/Eu atom) for the europium compound and the onset of ferromagnetic ordering at TC = 14.9(2) K. The divalent character of europium is corroborated by 151Eu Mössbauer spectroscpy.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-07-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46036444","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Vincent Mauritz, Katharina E. Dehm, Simon P. Hager, Ryan W. Crisp
Abstract To gain insight into the applicability as building blocks for optoelectronic device development, alkaline earth metal sulfides are investigated. MgS, CaS, SrS, and BaS have been systematically synthesized as colloidal particles in olelyamine. The particle sizes range from around 819 nm for MgS to 12.8 nm for CaS, 25.0 nm for SrS, and 21.6 nm for BaS. The heat-up synthesis uses commerically available precursors without complicated procedures. The structural and optical properties are investigated with X-ray diffraction, spectroscopic ellipsometry, UV–vis spectrophotometry, scanning electron microscopy, and energy dispersive X-ray spectroscopy.
{"title":"Colloidal nanocrystal synthesis of alkaline earth metal sulfides for solution-processed solar cell contact layers","authors":"Vincent Mauritz, Katharina E. Dehm, Simon P. Hager, Ryan W. Crisp","doi":"10.1515/zkri-2023-0006","DOIUrl":"https://doi.org/10.1515/zkri-2023-0006","url":null,"abstract":"Abstract To gain insight into the applicability as building blocks for optoelectronic device development, alkaline earth metal sulfides are investigated. MgS, CaS, SrS, and BaS have been systematically synthesized as colloidal particles in olelyamine. The particle sizes range from around 819 nm for MgS to 12.8 nm for CaS, 25.0 nm for SrS, and 21.6 nm for BaS. The heat-up synthesis uses commerically available precursors without complicated procedures. The structural and optical properties are investigated with X-ray diffraction, spectroscopic ellipsometry, UV–vis spectrophotometry, scanning electron microscopy, and energy dispersive X-ray spectroscopy.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46811104","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
W. Tanthanuch, S. Tancharakorn, C. Rojviriya, U. Bismayer
Abstract Pottery excavated from the archeological UNESCO world heritage site Ban Chiang in Thailand stem from distinct periods. Black vessels with cord-mark design from Pre-metal Age (ca. 3000–1000 BC), Bronze Age pottery (ca 1000–300 BC) with yellow-brown surface and Iron Age samples (ca. 300 BC–200 AD) with red pictorial surface patterns. In a previous work [Bismayer U., Srilomsak S., Treekamol Y., Tanthanuch W., Suriyatham K. Artefacts from Ban Chiang, Thailand: pottery with hematite-red geometric patterns. Z. Kristallogr. 2020, 235, 559–568] we studied the mineralogical composition and their surface colour materials of shards from Bronze and Iron Age. In this work we focus on bulk features of the dark Pre-metal Age cord-marked ceramic shard PSN2-S10E13 and compare its elemental and mineralogical composition with bulk composition of sample 5412-S6E15 from Bronze Age. Experimental techniques are electron microprobe, X-ray powder diffraction, FTIR spectroscopy, optical microscopy and X-ray tomographic microscopy (XTM). Sample PSN2-S10E13 contains more quartz than 5412-S6E15. In the bulk of the Pre-metal Age shard, diffraction signals of mullite occur, indicating higher firing temperatures compared to the younger sample. Phyllosilicate signals are seen in FTIR spectra of both shards. E-modes of quartz dominate FTIR spectra of both samples. Optical thin sections show voids around micro-particles in PSN2-S10E13 and XTM indicates that the pore volume percentage of sample PSN2-S10E13 is higher than in 5412-S6E15. Because of the large age gap to younger samples from Ban Chiang, the proper age of our oldest sample PSN2-S10E13 was determined using an accelerator mass spectrometer (AMS) by simultaneous 14C/12C and 13C/12C isotope ratio measurements which yielded a radiocarbon age of 3609 ± 29 BP (resp. 1659 ± 29 BC).
{"title":"Artefacts from Ban Chiang, Thailand: Pre-metal Age cord-marked pottery","authors":"W. Tanthanuch, S. Tancharakorn, C. Rojviriya, U. Bismayer","doi":"10.1515/zkri-2023-0015","DOIUrl":"https://doi.org/10.1515/zkri-2023-0015","url":null,"abstract":"Abstract Pottery excavated from the archeological UNESCO world heritage site Ban Chiang in Thailand stem from distinct periods. Black vessels with cord-mark design from Pre-metal Age (ca. 3000–1000 BC), Bronze Age pottery (ca 1000–300 BC) with yellow-brown surface and Iron Age samples (ca. 300 BC–200 AD) with red pictorial surface patterns. In a previous work [Bismayer U., Srilomsak S., Treekamol Y., Tanthanuch W., Suriyatham K. Artefacts from Ban Chiang, Thailand: pottery with hematite-red geometric patterns. Z. Kristallogr. 2020, 235, 559–568] we studied the mineralogical composition and their surface colour materials of shards from Bronze and Iron Age. In this work we focus on bulk features of the dark Pre-metal Age cord-marked ceramic shard PSN2-S10E13 and compare its elemental and mineralogical composition with bulk composition of sample 5412-S6E15 from Bronze Age. Experimental techniques are electron microprobe, X-ray powder diffraction, FTIR spectroscopy, optical microscopy and X-ray tomographic microscopy (XTM). Sample PSN2-S10E13 contains more quartz than 5412-S6E15. In the bulk of the Pre-metal Age shard, diffraction signals of mullite occur, indicating higher firing temperatures compared to the younger sample. Phyllosilicate signals are seen in FTIR spectra of both shards. E-modes of quartz dominate FTIR spectra of both samples. Optical thin sections show voids around micro-particles in PSN2-S10E13 and XTM indicates that the pore volume percentage of sample PSN2-S10E13 is higher than in 5412-S6E15. Because of the large age gap to younger samples from Ban Chiang, the proper age of our oldest sample PSN2-S10E13 was determined using an accelerator mass spectrometer (AMS) by simultaneous 14C/12C and 13C/12C isotope ratio measurements which yielded a radiocarbon age of 3609 ± 29 BP (resp. 1659 ± 29 BC).","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-07-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46705941","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M. Noor, Hamza Chah, David Tresp, I. Bernal, R. Lalancette
Abstract Herein we report the results of preparing metal compounds (where the metal ions are Co2+, Ni2+, Cu2+, Zn2+) with the cyclic ligand 1,4,8,11-tetraazacyclotetradecane [cyclam] under a variety of conditions of metal-ligand ratios and solvent media. In all cases, we used metal Cl2·nH2O salts (except for anhydrous CoCl2), as specified. Outcome: we isolated species with a four-coordinate metal in the N4 cavity of the ligand alone, and also with either one or two additional axial ligands. Those axial ligands can be (a) a single chloride, leading to penta-coordinated moncationic products; (b) two chlorides, leading to octahedral-neutral compounds; (c) two waters, giving rise to hexa-coordinated [(cyclam)metal(H2O)2]2+ species. Finally, in the case of HCl added to the reaction medium, the cyclam can be di-protonated and appears as [(cyclam)H2]2+ in the crystals. With such a variety of products, it is not surprising that since the metal coordination numbers vary, the cyclam ligand stereochemistries are thereby affected. Interestingly, the [(cyclam)metal] species are invariably hydrogen-bonded to one another in infinite strings of two kinds: (1) those for which the crystal’s Z′ = 1 have single strings; (2) when Z′ = 2, there is a pair of homogeneous strings attached to one another by a variety of hydrogen-bonding linkages. Finally, we observed an interesting pair of hydroxonium cations: the first is hydoxonium cations in a pleated 2-D sheet consisting of fused pentagons located between sheets of [(cyclam)metal] moieties; the second one is an infinite string of composition {(H3O+)-(H2O)-(H3O+)-(H2O)-(H3O+)-(H2O)-(H3O+)}∞.
{"title":"The versatility of 1,4,8,11-tetraazacyclotetradecane (cyclam) in the formation of compounds of Co2+, Ni2+, Cu2+, and Zn2+ with metal ions in and out of the cyclic ligand ring","authors":"M. Noor, Hamza Chah, David Tresp, I. Bernal, R. Lalancette","doi":"10.1515/zkri-2023-0026","DOIUrl":"https://doi.org/10.1515/zkri-2023-0026","url":null,"abstract":"Abstract Herein we report the results of preparing metal compounds (where the metal ions are Co2+, Ni2+, Cu2+, Zn2+) with the cyclic ligand 1,4,8,11-tetraazacyclotetradecane [cyclam] under a variety of conditions of metal-ligand ratios and solvent media. In all cases, we used metal Cl2·nH2O salts (except for anhydrous CoCl2), as specified. Outcome: we isolated species with a four-coordinate metal in the N4 cavity of the ligand alone, and also with either one or two additional axial ligands. Those axial ligands can be (a) a single chloride, leading to penta-coordinated moncationic products; (b) two chlorides, leading to octahedral-neutral compounds; (c) two waters, giving rise to hexa-coordinated [(cyclam)metal(H2O)2]2+ species. Finally, in the case of HCl added to the reaction medium, the cyclam can be di-protonated and appears as [(cyclam)H2]2+ in the crystals. With such a variety of products, it is not surprising that since the metal coordination numbers vary, the cyclam ligand stereochemistries are thereby affected. Interestingly, the [(cyclam)metal] species are invariably hydrogen-bonded to one another in infinite strings of two kinds: (1) those for which the crystal’s Z′ = 1 have single strings; (2) when Z′ = 2, there is a pair of homogeneous strings attached to one another by a variety of hydrogen-bonding linkages. Finally, we observed an interesting pair of hydroxonium cations: the first is hydoxonium cations in a pleated 2-D sheet consisting of fused pentagons located between sheets of [(cyclam)metal] moieties; the second one is an infinite string of composition {(H3O+)-(H2O)-(H3O+)-(H2O)-(H3O+)-(H2O)-(H3O+)}∞.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"243 - 251"},"PeriodicalIF":1.2,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43400983","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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