Startseite Naturwissenschaften Crystal structure of Ba6Cd12Mn4SiF48
Artikel Open Access

Crystal structure of Ba6Cd12Mn4SiF48

  • Sun Woo Kim ORCID logo EMAIL logo
Veröffentlicht/Copyright: 5. April 2024

Abstract

Ba6Cd12Mn4SiF48, cubic, I m 3 (no. 204), a = 12.57060(10) Å, V = 1986.41(5) Å3, Z = 2, Rgt (F) = 0.0286, wRref (F 2) = 0.0784, T = 296(2) K.

CCDC no.: 2195611

The molecular structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Pink block
Size: 0.21 × 0.20 × 0.19 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 13.6 mm−1
Diffractometer, scan mode: Bruker APEX-II, φ and ω
θ max, completeness: 28.2°, >99 %
N(hkl)measured, N(hkl)unique, R int: 18,964, 472, 0.093
Criterion for I obs, N(hkl)gt: I obs > 2σ(I obs), 472
N(param)refined: 38
Programs: Bruker [1], SHELX [2, 3], WinGX/ORTEP [4]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

Atom x y z U iso*/U eq
Ba1 0.500000 0.500000 0.20122 (6) 0.0066 (3)
Cd1 0.14763 (6) 0.500000 0.17432 (6) 0.0100 (3)
Mn1 0.250000 0.750000 0.250000 0.0036 (4)
Si1 0.500000 0.500000 0.500000 0.0008 (14)
F1 0.1083 (7) 0.500000 0.000000 0.0121 (16)
F2 0.3119 (4) 0.500000 0.1070 (4) 0.0089 (11)
F3 0.1896 (4) 0.6070 (3) 0.3111 (3) 0.0142 (9)
F4a 0.5765 (8) 0.5765 (8) 0.5765 (8) 0.109 (9)
  1. aOccupancy: 0.75.

1 Source of materials

BaF2 (Alfa Asear, 99 %), CdF2 (Alfa Asear, 99.9 %), MnF3 (Alfa Asear, 98 %), SiO2 (Alfa Asear, 99.0 %) and CF3COOH (Alfa Aesar, 99 %) were used without any further purification. Crystals of Ba6Cd12Mn4SiF48 were obtained by hydrothermal method using a diluted CF3COOH aqueous solution. 0.100 g of BaF2 (0.570 mmol), 0.0860 g of CdF2 (0.570 mmol), 0.1276 g of MnF3 (1.14 mmol), 0.0180 g of SiO2 (0.300 mmol), 3 ml of CF3COOH (39 mmol) and 5 ml of H2O were combined in a 23-ml Teflon-lined stainless autoclave. The autoclave was subsequently closed, gradually heated to 230 °C, held for 24 h, and cooled slowly to room temperature at a rate of 6 °C/h. The mother liquor was decanted from the products, and products were recovered by filtration and washed with distilled water and ethanol. Pink colored block shaped crystals of Ba6Cd12Mn4SiF48 were isolated by hand sorting. Energy-dispersive X-ray spectroscopy (EDX) analysis of the crystal indicated a chemical composition of Ba6.12Cd11.8Mn3.94Si1.01F47.78.

2 Experimental details

The structure was solved by Direct Methods with SHELXS and further refined with the SHELXL program [5]. The crystal structure of Ba6Cd12Mn4SiF48 was refined as merohedral twin.

3 Comment

Mixed metal fluoride materials have been investigated thoroughly attributable to their diverse crystal structures and significant magnetic, electric, multiferroic, optical, and luminescent properties [6, 7]. A search for barium cadmium manganese silicon fluorides in the Inorganic Structure Database (ICSD, web version 5.1.0) [8] yielded no relevant results. In fact, only six crystal structures could be found in barium manganese fluorides, cadmium manganese fluorides and barium silicon fluorides, for example, BaMnF4 [9], BaMnF5 [10], BaMnF5(H2O) [11], Ba5Mn3F19 [12], CdMnF5 [13], and BaSiF6 [14].

The crystal structure of Ba6Cd12Mn4SiF48 belongs to the cubic I m 3 (no. 204) space group with lattice parameter a = b = c = 12.5706(1) Å. This structure manifests a complex three-dimensional arrangement comprising distinct sites for Ba, Cd, Mn, and Si. In moiety formula, the structure can be expressed as [( Cd 12 2 + Mn 4 2 + F 42 )10−(Si4+F6)2−], with charge balance maintained by six Ba2+ cations. The Mn atom coordinates with six fluorine atoms in an octahedral geometry, with Mn–F bond distances of 2.098(4) Å. The Cd atom exhibits coordination with eight fluorine atoms in a distorted square antiprismatic geometry, and the cadmium-fluorine bond distances range from 2.231(6) to 2.582(5) Å. The Ba atom resides in 12-fold coordination environments, with Ba–F distances ranging from 2.645(6) to 3.108(3) Å. The Si atom demonstrates coordination with eight fluorine atoms, each partially occupied at 0.75, arranged in a cubic geometry. Bond valence sum (BVS) calculations [15] resulted in values of 2.15, 2.03, and 2.04 for Ba, Cd, and Mn, respectively.


Corresponding author: Sun Woo Kim, Department of Chemistry Education, Chosun University, 309 Pilmun-daero, Dong-gu, Gwangju 61452, South Korea, E-mail:

Acknowledgments

This study was supported by research fund from Chosun University.

  1. Conflict of interest statement: The author declares no conflicts of interest regarding this article.

  2. Author contributions: The author has accepted responsibility for the entire content of this submitted manuscript and approved submission.

  3. Research funding: Research fund from Chosun University.

References

1. Bruker. SAINT, APEX2 and SADABS; Bruker AXS Inc.: Madison, Wisconsin, USA, 2009.Suche in Google Scholar

2. Sheldrick, G. M. SHELXTL – integrated space-group and crystal-structure determination. Acta Crystallogr. 2015, A71, 3–8; https://doi.org/10.1107/s2053273314026370.Suche in Google Scholar

3. Sheldrick, G. M. Crystal structure refinement with SHELXL. Acta Crystallogr. 2015, C71, 3–8; https://doi.org/10.1107/s2053229614024218.Suche in Google Scholar

4. Farrugia, L. J. WinGX and ORTEP for Windows: an update. J. Appl. Crystallogr. 2012, 45, 849–854; https://doi.org/10.1107/s0021889812029111.Suche in Google Scholar

5. Hübschle, C. B., Sheldrick, G. M., Dittrich, B. ShelXle: a Qt graphical user interface for SHELXL. J. Appl. Crystallogr. 2011, 44, 1281–1284; https://doi.org/10.1107/s0021889811043202.Suche in Google Scholar

6. Hagenmuller, P. INORGANIC SOLID FLUORIDES: Chemistry and Physics; Academic Press, Inc.: New York, 1985.Suche in Google Scholar

7. Leblanc, M., Maisonneuve, V., Tressaud, A. Crystal chemistry and selected physical properties of inorganic fluorides and oxide-fluorides. Chem. Rev. 2015, 115, 1191–1254; https://doi.org/10.1021/cr500173c.Suche in Google Scholar

8. Zagorac, D., Müller, H., Ruehl, S., Zagorac, J., Rehme, S. Recent developments in the inorganic crystal structure database: theoretical crystal structure data and related features. J. Appl. Crystallogr. 2019, 52, 918–925; https://doi.org/10.1107/s160057671900997x.Suche in Google Scholar

9. Kim, S. W., Chang, H. Y., Halasyamani, P. S. Selective pure-phase synthesis of the multiferroic BaMF4 (M = Mg, Mn, Co, Ni, and Zn) family. J. Am. Chem. Soc. 2010, 132, 17684–17685; https://doi.org/10.1021/ja108965s.Suche in Google Scholar

10. Bukovec, P., Hoppe, R. Zur Kenntnis von BaMnF5: Eine Jahn–Teller–verzerrte Variante von BaGaF5. Z. Anorg. Allg. Chem. 1984, 509, 138–144; https://doi.org/10.1002/zaac.19845090214.Suche in Google Scholar

11. Massa, W., Burck, V. Erdalkali-fluoromanganate(III): BaMnF5·H2O und SrMnF5·H2O. Z. Anorg. Allg. Chem. 1984, 516, 119–126; https://doi.org/10.1002/zaac.19845160916.Suche in Google Scholar

12. Dahlke, P., Graulich, J., Welsch, M., Pebler, J., Babel, D. Struktur- und magnetochemische Untersuchungen an Ba5Mn5F19 und verwandten Verbindungen A5II M3III F19. Z. Anorg. Allg. Chem. 2000, 626, 1255–1263; https://doi.org/10.1002/(sici)1521-3749(200005)626:5<1255::aid-zaac1255>3.0.co;2-j.10.1002/(SICI)1521-3749(200005)626:5<1255::AID-ZAAC1255>3.3.CO;2-ASuche in Google Scholar

13. Mueller, U., Hoppe, R. Korrektur zu den Kristallstrukturen von CaMnF5 und CdMnF5. Z. Anorg. Allg. Chem. 1990, 583, 205–208; https://doi.org/10.1002/zaac.19905830125.Suche in Google Scholar

14. Hoskins, B. F., Linden, A., Mulvaney, P. C., O’Donnell, T. A. The structures of barium hexafluorosilicate and cesium hexafluororhenate(V). Inorg. Chim. Acta 1984, 88, 217–222; https://doi.org/10.1016/s0020-1693(00)83600-2.Suche in Google Scholar

15. Brown, I. D. The Chemical Bond in Inorganic Chemistry: The Bond Valence Model; Oxford University Press: New York, 2002.Suche in Google Scholar

Received: 2024-02-22
Accepted: 2024-03-27
Published Online: 2024-04-05
Published in Print: 2024-06-25

© 2024 the author(s), published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

Artikel in diesem Heft

  1. Frontmatter
  2. New Crystal Structures
  3. The crystal structure of tris((Z)-2-hydroxy-N-((E)-pyridin-2-ylmethylene)benzohydrazonato-k2O,N)europium(III), C39H30N9O6Eu
  4. Crystal structure of (E)-3-(benzylideneamino)-2-phenylthiazolidin-4-one, C16H14N2OS
  5. The crystal structure of (E)-4-fluoro-N′-(1-(o-tolyl)ethylidene)benzohydrazide, C16H15FN2O
  6. Crystal structure of (6-chloropyridin-3-yl)methyl 2-(6-methoxynaphthalen-2-yl)propanoate, C20H18ClNO3
  7. Crystal structure of methyl 3-methoxy-4-(2-methoxy-2-oxoethoxy)benzoate, C12H14O6
  8. The crystal structure of bis[(4-methoxyphenyl)(picolinoyl)amido-κ2 N:N′]copper(II), C26H22CuN4O4
  9. The crystal structure of poly[di(μ2-aqua)-diaqua-bis(3-aminopyridine-4-carboxylate-κ2 O: O′)-tetra(μ2-3-aminopyridine-4-carboxylate-κ2 O: O′)-dineodymium(III), [Nd2(C6H5N2O2)6(H2O)4] n
  10. The crystal structure of t-butyl 7-[3-(4-fluorophenyl)-1-(propan-2-yl)-1H-indol-2-yl]-3,5-dihydroxyhept-6-enoate, C28H34FNO4
  11. Crystal structure of catena-poly[(benzylamine-κ1 N)-(sorbato-κ1 O)-(μ2-sorbato-κ2 O,O′)-copper(II), C19H23CuNO4
  12. Crystal structure of (4-(2-chlorophenyl)-1H-pyrrol-3-yl)(ferrocenyl) methanone, C21H16ClFeNO
  13. The crystal structure of N-[4-(4-bromophenyl)-1,3-thiazol-2-yl]-3-(2-methylphenyl)-2-sulfanylprop-2-enamide hydrate, C19H17BrN2O2S2
  14. The crystal structure of N′-{5-[2-(2,6-dimethylphenoxy) acetamido]-4-hydroxy-1,6-diphenylhexan-2-yl}-3-methyl-2-(2-oxo-1,3-diazinan-1-yl)butanamide hydrate
  15. Crystal structure of 2-(naphthalen-1-yl)ethyl 2-(6-methoxynaphthalen-2-yl)propanoate, C26H24O3
  16. Crystal structure of naphthalen-1-ylmethyl 2-(6-methoxynaphthalen-2-yl)propanoate, C25H22O3
  17. Crystal structure of poly[diaqua- (μ4-5-(1H-1,2,4-triazol-1-yl)benzene-1,3-dicarboxylato-κ5N:O,O’:O’’:O’’’)calcium(II), C10H9CaN3O6
  18. Crystal structure of (E)-N′-(4-((E)-3-(dimethylamino)acryloyl)-3-hydroxyphenyl)-N, N-dimethylformimidamide, C14H19N3O2
  19. Crystal structure of (E)-3-(dimethylamino)-1-(2-hydroxy-4,6-dimethoxyphenyl)prop-2-en-1-one, C13H17NO4
  20. Crystal structure of (2-chloropyridin-3-yl)methyl-2-(6-methoxynaphthalen-2-yl)propanoate, C20H18ClNO3
  21. The crystal structure of diethyl 4-(3,4-dimethylphenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate, C21H27NO4
  22. Crystal structure of (8R,9S,10R,13S,14S,17S)-17-hydroxy-10,13-dimethyl-17-((4-(2-phenylpropyl)phenyl)ethynyl)-1,2,6,7,8,9,10,11,12,13,14,15,16,17-tetradecahydro-3H-cyclopenta[a]phenanthren-3-one, C36H42O2
  23. Synthesis and crystal structure of 4-(4-cyclopropylnaphthalen-1-yl)-2,4-dihydro-3H-1,2,4-triazole-3-thione, C15H13N3S
  24. Crystal structure of catena-poly[aqua-(2,6-di-(2-pyridyl)-pyridine-κ3 N,N′, N″)(μ2-1,4-naphthalene dicarboxylato-κ2 O,O′)nickel(II)], C27H19NiN3O5
  25. Crystal structure of 3-(diphenylphosphoryl)-3-hydroxy-1-phenylpropan-1-one, C21H19O3P
  26. The crystal structure of R,S-{N-[(2-oxidonaphthalen-1-yl)methylidene]phenylglycinato}divinylsilicon, C23H19NO3Si
  27. The crystal structure of 1,2,4-tris(bromomethyl)benzene, C9H9Br3
  28. Crystal structure of chlorido-[4-(pyridin-2-yl)benzaldehyde-κ2 N,C]-(diethylamine-κ1 N)platinum(II), C16H18ClN2OPt
  29. Crystal structure of 3-(methoxycarbonyl)-1-(4-methoxyphenyl)-2,3,4,9- tetrahydro-1H-pyrido[3,4-b]indol-2-ium chloride hydrate, C40H48Cl2N4O9
  30. The crystal structure of 1-(2-chlorobenzyl)-3-(3-chlorophenyl)urea, C14H12Cl2N2O
  31. Hydrothermal synthesis and crystal structure of aqua-tris(4-acetamidobenzoato-κ2 O,O′)-(1,10-phenanthroline-κ2 N,N′)terbium(III) hydrate C39H36N5O11Tb
  32. The crystal structure of zwitterionic 3-aminoisonicotinic acid, C6H6N2O2
  33. The crystal structure of bis{[monoaqua-μ2-4-[(pyridine-4-carbonyl)-amino]-phthalato-κ3 N:O,O′-(2,2′-bipyridine κ2 N,N′)copper(II)]}decahydrate, C48H56N8O22Cu2
  34. Crystal structure of poly[μ10-4,4′-methylene-bis(oxy)benzoatodipotassium], C15H10K2O6
  35. The crystal structure of catena-poly[[tetraaqua[(μ2-1,4-di(4-methyl-1-imidazolyl)benzene] cobalt(II)]bis(formate)], C16H24CoN4O8
  36. The crystal structure of (E)-2-chloro-5-((2-(nitromethylene)imidazolidin-1-yl)methyl)pyridine, C10H11ClN4O2
  37. The crystal structure of (E)-1-(((2-amino-4,5-dimethylphenyl)iminio)methyl)naphthalen-2-olate, C19H18N2O
  38. Crystal structure of N-(acridin-9-yl)-2-(4-methylpiperidin-1-yl) acetamide monohydrate, C21H25N3O2
  39. The crystal structure of dichlorido-bis(3-methyl-3-imidazolium-1-ylpropionato-κ2 O,O′)-zinc(II), C14H20Cl2N4O4Zn
  40. The crystal structure of 2,8-diethyl-1,3,7,9-tetramethyl-4λ4,5λ4-spiro[dipyrrolo[1,2-c:2′,1′-f][1,3,2]diazaborinine-5,2′-naphtho[1,8-de][1,3,2]dioxaborinine], C25H29BN2O2
  41. The crystal structure of 5-tert-butyl-2-(5-tert-butyl-3-iodo-benzofuran-2-yl)-3-iodobenzofuran, C24H24I2O2
  42. Synthesis and crystal structure of methyl 2-{[4-(4-cyclopropyl-1-naphthyl)-4H-1,2,4-triazole-3-yl]thio} acetate, C18H17N3O2S
  43. The crystal structure of n-propylammonium bis(2,3-dimethylbutane-2,3-diolato)borate-boric acid (1/1), [C3H10N][C12H24BO4]·B(OH)3
  44. Crystal structure of methyl 1-(2-bromophenyl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-3-carboxylate, C19H17BrN2O2
  45. Crystal structure of (4-bromobenzyl)triphenylphosphonium bromide ethanol solvate, C52H48Br4OP2
  46. The crystal structure of unsymmetrical BOPHY C26H27BN4
  47. The crystal structure of Tb3B5O11(OH)2
  48. The crystal structure of (Z)-4-ethyl-2-((4-ethyl-3,5-dimethyl-1H-pyrrol-2-yl)methylene)-3,5-dimethyl-2H-pyrrol-1-ium 2,2'-spirobi[naphtho[1,8-de][1,3,2]dioxaborinin]-2-uide, C37H37BN2O4
  49. Crystal structure of bis(methylammonium) hexadecaselenidopalladate(II), (CH3NH3)2PdSe16
  50. The crystal structure of (2-diphenylphosphanylphenyl) 2-[7-(dimethylamino)-2-oxochromen-4-yl]acetate, C31H26NO4P
  51. Crystal structure of (E)-6-(4-ethylpiperazin-1-yl)-2-(3-fluorobenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C23H25FN2O
  52. The structure of RUB-56, (C6H16N)8 [Si32O64(OH)8]·32 H2O, a hydrous layer silicate (2D-zeolite) that contains microporous levyne-type silicate layers
  53. Crystal structure of 4-amino-3,5-dibromobenzonitrile, C7H4Br2N2
  54. Crystal structure of 2-(naphthalen-1-yl)ethyl 2-acetoxybenzoate, C21H18O4
  55. Single-crystal structure determination of Tm3B12O19(OH)7
  56. Crystal structure determination of NdB3.6O7
  57. The crystal structure of NdB6O8(OH)5·H3BO3
  58. Crystal structure of 2-(5-ethylpyridin-2-yl)ethyl 2-(6-methoxynaphthalen-2-yl)propanoate, C23H25NO3
  59. Crystal structure of N-(1-(3,4-dimethoxyphenyl)-2-methylpropyl)aniline, C18H23NO2
  60. Crystal structure of Ba6Cd12Mn4SiF48
  61. Synthesis and crystal structure of 5-fluoro-1-methyl-2-oxo-3-(2-oxochroman-4-yl)indolin-3-yl acetate, C20H16FNO5
  62. The crystal structure of 6-methacryloylbenzo[d][1,3]dioxol-5-yl 4-nitrobenzenesulfonate, C17H13NO8S
  63. Crystal structure of ethyl 2-(3-benzyl-4-oxo-3,4-dihydrophthalazin-1-yl)- 2,2-difluoroacetate, C19H16F2N2O3
  64. The crystal structure of tetrakis(μ 2-(1H-benzimidazole-2-methoxo-κ2 N,O:O:O)-(n-butanol-κO)-chlorido)-tetranickel(II), C48H68Cl4N8O8Ni4
  65. Synthesis and crystal structure of trans-tetraaqua-bis((1-((7-hydroxy-3-(4-methoxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)piperidin-1-ium-4-carbonyl)oxy-κO)zinc(II)hexahydrate, C46H64N2O28S2Zn
  66. The crystal structure of 1-(4-carboxybutyl)-3-methyl-1H-imidazol-3-ium hexafluoridophosphate, C9H15F6N2O2P
  67. Crystal structure of 1-(4-chlorophenyl)-4-(2-furoyl)-3-phenyl-1H-pyrazol-5-ol, C20H13ClN2O3
  68. Crystal structure of dimethyl (R)-2-(3-(1-phenylethyl)thioureido)-[1,1′-biphenyl]-4,4′-dicarboxylate, C25H24N2O4S
  69. The crystal structure of 1-(3-carboxypropyl)-1H-imidazole-3-oxide, C7H10N2O3
  70. Synthesis and crystal structure of dimethyl 4,4′-(propane-1,3-diylbis(oxy))dibenzoate, C19H20O6
  71. Crystal structure of methyl-1-(p-tolyl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-3-carboxylate, C20H20N2O2
  72. The crystal structure of 1-(1-adamantan-1-yl)ethyl-3-(3-methoxyphenyl)thiourea, C20H28N2OS
  73. The crystal structure of N,N′-carbonylbis(2,6-difluorobenzamide), C15H8F4N2O3
Heruntergeladen am 30.12.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2024-0083/html
Button zum nach oben scrollen