61 Helices from Tetrahedral Ribbons [BP2O]: Isostructural Borophosphates MIMII(H2O)2[BP2O8] · H2O (MI = Na, K; MII = Mg, Mn, Fe, Co, Ni, Zn) and Their Dehydration to Microporous Phases MIMII(H2O)[BP2O8]
10.1002/anie.199710131
Crossref journal-article
Wiley
Angewandte Chemie International Edition in English (311)
Bibliography

Kniep, R., Will, H. G., Boy, I., & Röhr, C. (1997). 61 Helices from Tetrahedral Ribbons [BP2O]: Isostructural Borophosphates MIMII(H2O)2[BP2O8] · H2O (MI = Na, K; MII = Mg, Mn, Fe, Co, Ni, Zn) and Their Dehydration to Microporous Phases MIMII(H2O)[BP2O8]. Angewandte Chemie International Edition in English, 36(9), 1013–1014. Portico.

Authors 4
  1. Rüdiger Kniep (first)
  2. Horst Günter Will (additional)
  3. Insan Boy (additional)
  4. Caroline Röhr (additional)
References 21 Referenced 113
  1. 10.1002/ange.19941060715
  2. 10.1002/anie.199407491
  3. {'key': 'e_1_2_1_2_2', 'first-page': '1400', 'volume': '76', 'author': 'Gupta P. K. S.', 'year': '1991', 'journal-title': 'Amer. Mineral.'} / Amer. Mineral. by Gupta P. K. S. (1991)
  4. {'key': 'e_1_2_1_2_3', 'first-page': '1527', 'volume': '56', 'author': 'Moore P. B.', 'year': '1971', 'journal-title': 'Amer. Mineral.'} / Amer. Mineral. by Moore P. B. (1971)
  5. 10.1515/znb-1995-1107
  6. 10.1524/zkri.1995.210.6.446
  7. 10.1524/zkri.1996.211.10.707
  8. 10.1524/zkri.1996.211.10.705
  9. Li[B3PO6(OH)3]:Z. Kristallogr. in print.
  10. (a) Crystal structure data for NaMn(H2O)2[BP2O8.]·H2O atT= 275 K: hexagonal space groupP6122 (no. 178) a= 958.9(5) c= 1593.9(9) pm V= 1269(1) Å3 Z= 4 ρcalcd= 2.57 gcm−3; diffractometer: Philips PW 1100 (MoKαradiation graphite monochromator); μ(MoKα= 2.042 mm−1); 2θmax= 50°; 2463 measured reflections. 755 independent reflections; Lorentzian and polarization correction; structure solved by direct methods [4c] and refined with least‐squares methods (all atoms anisotropi) with SHELXL‐93 [4d]; 75 free parameters; GOF = 1.09 Rvalues (I> 2σ(I)):R1 = 0.080 wR2 = 0.141 Flack‐x parameter: −0.01(0.1); max./min. residual electron density: 0.53/‐0.64 e−× 10−6pm−3.
  11. (b) Crystal structure data for NaMg(H2O)2[BP2O8]·H2O atT= 275 K: hexagonal space groupP16 22 (no. 178) a= 942.8(5) c= 1582.0(8) pm V= 1218(1) Å33.Z= 4. ρcalcd= 2.42gcm−3; diffractometer: Philips PW 11OO (MoKαradiation graphite monochromator); μ(MoKα) = 0.72 mm−1; 2θmax= 47°; 744 measured reflections 604 independent reflections; Lorentzian and polarization correction; structure solved by direct methods [4c] and refined with least‐squares methods (Na Mg and P atoms anisotropic O atoms isotropic) with SHELXL‐93 [4d]; 44 free parameters; GOF = 0.96 Rvalues (I> 2σ(I)):R1 = 0.089 wR2 = 0.175 Flack‐x parameter: 0.17(1.18)‐thus in this case no statement about the absolute structure is possible; max./min. residual electron density: 0.541/‐0.55 e−× 1O−6ppm−3. The site parameters of the hydrogen atoms could not be determined due to the relatively highRfactors that could not be significantly reduced even with the use of empirical absorption corrections; the clearly anisotropic O(6) atom in NaMn and the fact that the O atomic positions in NaMg could only be refined isotropically compounded the problem. Further details of the crystal structure investigations may be obtained from the Fachinformationszentrum Karlsruhe Gesellschaft für wissenschaftlich‐technische Information mbH D‐76344 Eggenstein‐Leopoldshafen (Germany) on quoting the depository numbers CSD‐406 228 and CSD‐406 229.
  12. 10.1107/S0108767390000277
  13. (d)G.Sheldrick Program SHELXL‐93 J. Appl. Crystallogr.1993.
  14. 10.1107/S0021889883011292
  15. I.Boy Ph. D. dissertation TH Darmstadt in preparation.
  16. Selected bond lengths [pm] and angles [°] of NaMn(H2O)2[BP2O8]·H2O: B‐O 146–149 P‐O 148–157 MnOp 213–215 MnOH2O231 NaO 239–265; O‐B‐O 101–113 O‐P‐O 105–115 OH2O‐Mn‐OH2O88.
  17. Hydrothermal synthesis of the borophosphates MIMII(H2O)2[BP2O8]·H2O: sealed glass ampules (vol 10–12 mL degree of filling 25–30%) T= 150°C (Mg Mn Ni Co) or 120°C (Fe) 2 weeks. MII= Mg (colorless) Mn (slightly pink) Ni (yellow‐green): MIIHPO4(1 mmol) (MI)2B4O7(2 mmol) HCl (0.85 mL 18%) and H2O (1 mL). MII= Fe (light gray‐violet): FeCl2·4H2O (2 mmol) (M)B4O7(1 mmol) (MI)2HPO4(7 mmol) HCl(0.85 mL 18%) and H2O (0.7 mL). MII= Co (violet):.CoCl2(1 mmol) (MI)2B4O7(1.85 mmol) (MI)2HPO4(6 mmol) HCl (0.8 mL 18%) and H2O (1 mL). Solid reaction products were obtained after washing with hot water (≈50% with respecpt to the amount of solid starting material). NaZn (colorless): ZnCl2Na2B4O7·10 H2O and Na2HPO4in a molar ratio of 2:1:7 (total 7.3 g) as well as H2O (20 mL)and HCl (8 mL 18 %). The mixture was evaporated to 10 mL at 100 °C and the gel treated in a tenon autoclave (vol 20 mL degree of filling 50%) at 120 °C for twp weeks. The single‐phase reaction product was obtained after washing with hot water.
  18. 10.1002/ange.19961082218
  19. 10.1002/anie.199626301
  20. 10.1021/ic960808d
  21. Note added in proof (March 24 1997): The first borophosphate anion partial structure with a three‐dimensional framework has been obtained in [Cs{B2P2O8(OH)}] (C.Hauf R.Kniep unpublished results).
Dates
Type When
Created 21 years, 7 months ago (Jan. 16, 2004, 9:39 a.m.)
Deposited 1 year, 10 months ago (Oct. 10, 2023, 8:46 p.m.)
Indexed 2 months, 2 weeks ago (June 16, 2025, 9:29 a.m.)
Issued 28 years, 3 months ago (May 16, 1997)
Published 28 years, 3 months ago (May 16, 1997)
Published Online 21 years, 8 months ago (Dec. 22, 2003)
Published Print 28 years, 3 months ago (May 16, 1997)
Funders 0

None

@article{Kniep_1997, title={61 Helices from Tetrahedral Ribbons [BP2O]: Isostructural Borophosphates MIMII(H2O)2[BP2O8] · H2O (MI = Na, K; MII = Mg, Mn, Fe, Co, Ni, Zn) and Their Dehydration to Microporous Phases MIMII(H2O)[BP2O8]}, volume={36}, ISSN={0570-0833}, url={http://dx.doi.org/10.1002/anie.199710131}, DOI={10.1002/anie.199710131}, number={9}, journal={Angewandte Chemie International Edition in English}, publisher={Wiley}, author={Kniep, Rüdiger and Will, Horst Günter and Boy, Insan and Röhr, Caroline}, year={1997}, month=may, pages={1013–1014} }