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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 ]
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)
= 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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2007 guan re-o4

  • 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. 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. = 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