Bis(2-amino-6-methylpyridinium) di-μ-chlorido-μ-oxido-bis[dichloridoantimonate(III)]

Abstract

Key indicators: single-crystal X-ray study; T = 298 K; mean (C-C) = 0.011 Å; R factor = 0.047; wR factor = 0.095; data-to-parameter ratio = 16.5.The title compound, (C 6 H 9 N 2 ) 2 [Sb 2 Cl 6 O], consists of one triple-bridged [Sb 2 Cl 6 O] 2À anion and two 2-amino-6-methylpyridinium cations that undergo aminium-iminium tautomerism. The counter-ion pair are linked together by N-HÁ Á ÁO and N-HÁ Á ÁCl hydrogen bonds. ExperimentalCrystal data (C 6 H 9 N 2 ) 2 [Sb 2 Cl 6 O] M r = 690.52 Monoclinic, P2 1 =n a = 10.0746 (10) Å b = 15.1972 (16) Å c = 15.4631 (14) Å = 101.597 (6) V = 2319.2 (4) Å 3 Z = 4 Mo K radiation = 3.03 mm À1 T = 298 (2) K 0.30 Â 0.30 Â 0.30 mm Data collection Bruker APEX area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000) T min = 0.419, T max = 0.419 12055 measured reflections 4137 independent reflections 3876 reflections with I > 2(I) R int = 0.026 Refinement R[F 2 > 2(F 2 )] = 0.048 wR(F 2 ) = 0.095 S = 1.24 4137 reflections 250 parameters 8 restraints H atoms treated by a mixture of independent and constrained refinement Á max = 0.86 e Å À3 Á min = À0.50 e Å À3 metal-organic compounds m1786 # 2007 International Union of Crystallography

N-Methylpiperazinediium pentachloridoantimonate(III) monohydrate

“…For related literature, see: Baker & Williams (1978); Bujak & Zaleski (1999); Clemente & Marzotto (2003); Feng et al (2007); Knodler et al (1988); Linden et al (1999); Marsh (1995).…”

“…Halogenoantimonates constitute a group of salts in which a number of compounds have been reported (e.g. Feng et al, 2007;Bujak & Zaleski, 1999;Knodler et al, 1988;Baker & Williams, 1978 and see: Clemente & Marzotto (2003); Marsh et al (1995) for corrected space groups of some of these types of compounds). In our laboratory, a compound containing pentachloridoantimonate has been synthesized, its crystal structure is reported herein.…”

Bis(2-amino-6-methylpyridinium) tetrachloridocuprate(II)

“…For complexes in which A is a protonated alkylamine, see: Zhou & Drumheller (1990), a heterocycle such as pyridine, see: Place & Willett (1987), 2-aminopyrimidine, see: Zanchini & Willett (1990) and 2-amino-3-methylpridine, see: Coffey et al (2000). For bond lengths and angles in related structures, see: Antolini et al (1988); Zhang et al (2005); Jin, Shun et al (2005); Feng et al (2007); Nahringbauer & Kvick (1977). For other 2-aminopyridinium structures, see: Luque et al (1997); Jin et al (2000Jin et al ( , 2001; Jin, Tu et al (2005).…”

Bis(dimethyloxonium) pentachloridoantimonate(III)

“…For related literature, see: Astruc et al (1990); Bagno & Bukala (1990); Blake et al (1990); Bujak & Zaleski (1998); Cai et al (1995); Cheng & Niu (1995); Einstein & Jones (1973); Feng et al (2007); Hall & Sowerby (1979); Ponikiewski & Rothenberger (2005); Rietz et al (1978); Shikada et al (1983); Spek (2003); Vojinovic et al (2006); Wang et al (2006); Wegman (1994); Zhou (2005). Hydrogen-bond geometry (Å , ).…”

“…Furthermore, the coordinated Sb-Cl bond is worthy of note. A survey of some structures containing antimony and chlorine reveals that normal Sb-Cl bond lengths generally lie between 2.3 and 2.4 Å (Einstein & Jones, 1973) and those involved in bridging range from 2.8 and 3.0 Å (Hall & Sowerby, 1979;Feng et al, 2007). It is noted that the upper limit for a Sb-Cl bond distance has been extended beyond 2.4 Å out and away, to 2.8847 (12) Å in the case of Sb1-Cl4 in (I).…”