2007 guan re-o4

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guanidinium, rhenium, perrhenate

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2007 guan re-o4

  1. 1. electronic reprint Acta Crystallographica Section E Structure Reports Online ISSN 1600-5368 Editors: W. Clegg and D. G. Watson Guanidinium tetraoxidorhenate(VII) Mikhail S. Grigoriev, Konstantin E. German and Alesia Ya. Maruk Copyright © International Union of Crystallography Author(s) of this paper may load this reprint on their own web site or institutional repository provided that this cover page is retained. Republication of this article or its storage in electronic databases other than as specified above is not permitted without prior permission in writing from the IUCr. For further information see http://journals.iucr.org/services/authorrights.html Acta Cryst. (2007). E63, m2061 Grigoriev et al. ¯ (CH6 N3 )[ReO4 ]
  2. 2. metal-organic compounds Acta Crystallographica Section E Refinement Structure Reports Online R[F 2 > 2(F 2)] = 0.018 wR(F 2) = 0.040 S = 1.11 2698 reflections ISSN 1600-5368 Guanidinium tetraoxidorhenate(VII) 82 parameters H-atom parameters constrained ˚ Ámax = 1.59 e AÀ3 ˚ Ámin = À2.90 e AÀ3 Table 1 ˚ Selected geometric parameters (A, ). Mikhail S. Grigoriev,* Konstantin E. German and Alesia Ya. Maruk Re1—O1 Re1—O2 A. N. Frumkin Institute of Physical Chemistry and Electrochemistry, Russian Academy of Sciences, 31 Leninsky Prospekt, 119991 Moscow, Russian Federation Correspondence e-mail: grigoriev@ipc.rssi.ru O1—Re1—O2 O1—Re1—O3 O1—Re1—O4 1.727 (2) 1.728 (2) Re1—O3 Re1—O4 109.53 (12) 109.35 (11) 111.43 (11) 1.720 (2) 1.733 (2) O2—Re1—O3 O2—Re1—O4 O3—Re1—O4 108.35 (11) 109.43 (11) 108.69 (11) Received 29 June 2007; accepted 29 June 2007 ˚ Key indicators: single-crystal X-ray study; T = 100 K; mean (e–O) = 0.002 A; R factor = 0.018; wR factor = 0.040; data-to-parameter ratio = 32.9. The coordination geometry of the Re atom in the title compound, (CH6N3)[ReO4], is tetrahedral. The structure consists of alternating cationic and anionic layers parallel to the (120) plane; the layers are held in a three-dimensional structure by N—HÁ Á ÁO hydrogen bonds. Related literature The structures of tetraoxidorhenates of several cyclic derivatives of guanidinium were described by Leibnitz et al. (2001) and Tamm et al. (2004). Guanidinium perchlorate was reported by Koziol (1984) and guaninidium tetrafluoridoborate by Kozak et al. (1987). Table 2 ˚ Hydrogen-bond geometry (A, ). D—HÁ Á ÁA D—H HÁ Á ÁA DÁ Á ÁA D—HÁ Á ÁA N1—H1AÁ Á ÁO3i N1—H1AÁ Á ÁO4ii N1—H1BÁ Á ÁO2iii N2—H2AÁ Á ÁO1iv N2—H2AÁ Á ÁO3 N2—H2BÁ Á ÁO2iii N3—H3AÁ Á ÁO4ii N3—H3BÁ Á ÁO1iv N3—H3BÁ Á ÁO4v 0.88 0.88 0.88 0.88 0.88 0.88 0.88 0.88 0.88 2.41 2.45 2.10 2.22 2.49 2.27 2.08 2.14 2.50 3.101 3.177 2.911 2.966 3.164 3.037 2.901 2.907 3.080 136 140 153 142 134 145 155 146 124 (3) (3) (3) (3) (3) (3) (3) (3) (3) Symmetry codes: (i) x; y; z À 1; (ii) x þ 1; y; z À 1; (iii) Àx; Ày; Àz þ 1; (iv) x þ 1; y; z; (v) Àx þ 1; Ày þ 1; Àz þ 1. Data collection: APEX2 (Bruker, 2006); cell refinement: SAINTPlus (Bruker, 1998); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL97 (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL97. Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG2292). References Experimental Crystal data (CH6N3)[ReO4] Mr = 310.29 Triclinic, P1 ˚ a = 4.9657 (4) A ˚ b = 7.7187 (7) A ˚ c = 8.4423 (7) A = 75.314 (4)
  3. 3. = 88.707 (5) = 80.985 (5) ˚ V = 309.09 (5) A3 Z=2 Mo K radiation = 19.61 mmÀ1 T = 100 (2) K 0.12 Â 0.10 Â 0.06 mm Data collection Bruker Kappa APEXII areadetector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996) Tmin = 0.192, Tmax = 0.346 (expected range = 0.171–0.308) Acta Cryst. (2007). E63, m2061 11709 measured reflections 2698 independent reflections 2506 reflections with I 2(I) Rint = 0.027 Bruker (2006). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1998). SAINT-Plus. Version 6.01. Bruker AXS Inc., Madison, Wisconsin, USA. Kozak, A., Grottel, M., Koziol, A. E. Pajak, Z. (1987). J. Phys. C Solid State Phys. 20, 5433–5447. Koziol, A. E. (1984). Z. Kristallogr. 168, 313–316. Leibnitz, P., Reck, G., Pietzsch, H.-J. Spies, H. (2001). Report FZR-311, pp. 36-40. Forschungszentrum Rossendorf, Berlin, Germany. Sheldrick, G. M. (1996). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997a). SHELXS97 and SHELXL97. University of ¨ Gottingen, Germany. Sheldrick, G. M. (1997b). SHELXTL. Version 5.10. Bruker AXS Inc., Madison, Wisconsin, USA. Tamm, M. S., Beer, S. Herdtweck, E. (2004). Z. Naturforsch. Teil B, 59, 1497–1504. doi:10.1107/S1600536807031881 electronic reprint # 2007 International Union of Crystallography m2061
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