metal-organic compounds
Poly[tetrabutylammonium [chloridohexamethyl-μ3-sulfato-distannate(IV)]]
aLaboratoire de Chimie Minérale et Analytique, Département de Chimie, Faculté des Sciences et Techniques, Université Cheikh Anta Diop, Dakar, Senegal, and bInstitut Européen des Membranes, Université de Montpellier II, 34000 Montpellier, France
*Correspondence e-mail: tijchimia@yahoo.fr
In the structure of the title coordination polymer, {(C16H36N)[Sn2(CH3)6Cl(SO4)]}n, the two independent SnIV atoms are coordinated in a trigonal–bipyramidal manner by three methyl groups in the equatorial plane and in the axial positions by either two O atoms of bridging SO42− anions or by a Cl atom and one O atom of a bridging SO42− anion, respectively. The [Sn2(CH3)6Cl(SO4)]− anion forms an infinite zigzag chain parallel to the c axis. The cations are situated between these chains. Two of the four butyl groups of the cation are partially disordered over two sets of sites with site occupancies of 0.79 (2):0.21 (2) and 0.75 (2):0.25 (2), respectively. Weak C—H⋯O hydrogen-bonding interactions help to consolidate the crystal packing.
Related literature
For related structures, see: Molloy et al. (1989); Zhang et al. (2008); Sadiq-ur-Rehman et al. (2004); Aziz-ur-Rehman et al. (2006); Diallo et al. (2009); Diop et al. (2012). For details of the use of constraints and restraints during the structure see: Cooper et al. (2010, 2012). For background to the weighting schemes used in the see: Prince (1982); Watkin (1994).
Experimental
Crystal data
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Data collection: CrysAlis PRO (Agilent, 2010); cell CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: CRYSTALS.
Supporting information
https://doi.org/10.1107/S1600536813016723/wm2750sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536813016723/wm2750Isup2.hkl
Ethanolic solutions containing (Bu4N)HSO4 (1.26 g, 4 mmol) and SnMe3Cl (1.59 g, 8 mmol) were mixed and stirred at room temperature for more than 1 h. After removing the precipitate, the filtrate was allowed to evaporate to yield colourless crystals of the title compound. The overall reaction is: (Bu4N)HSO4 + 2SnMe3Cl → (Bu4N)[Sn2(CH3)6Cl(SO4)] + HCl
Most of the H atoms were located in a difference map, but they were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularize their geometry (C—H in the range 0.93–0.98, Å) and Uiso(H) (in the range 1.2–1.5 times Ueq of the parent atom), after which the positions were refined with riding constraints (Cooper et al., 2010). The severe disorder in two of the four butyl chains of the tetrabutylammonium cation was treated by introducing a new carbon site and refining the occupancies of the two sets of sites. Restraints on the interatomic distances and on the anisotropic atomic displacement parameters were necessary in order to obtain a reasonable geometry. Initially shift limiting restraints were applied but in the final stages of the
removed. It proved also be necessary to apply interatomic distance restraints between pairs of non-splitted carbon atoms. Asymmetric atomic displacement restraints were used for the atomic displacement parameters of the disordered carbon atoms (Cooper et al., 2012). The size and shape of other carbon atoms in the butyl chains suggest that they are most probably disordered as well, but the disorder does not appear to be well-resolved, and it could not be modelled satisfactorily. The tree reflections (0 2 0), (1 1 1) and (2 0 0) have been omitted from the because they were found to be partially masked by the beamstop. The highest positive difference electron density, 1.44 e- Å-3, is found at 0.42 Å from C20, whereas the largest negative electron density, -2.06 e- Å-3, is found at 0.83 Å from C14.Among organotin(IV) complexes, a number of trimethyltin derivatives form polymeric structures with trigonal bipyramidal geometry around the SnIV atom, e.g. as reported by Molloy et al. (1989); Sadiq-ur-Rehman et al. (2004); Aziz-ur-Rehman et al. (2006); Zhang et al. (2008).
The title compound, {(C16H36N)[Sn2(CH3)6Cl(SO4)]}n, crystallizes with one tetrabutylammonium cation, Bu4N+, and one organotin(IV) complex anion in the
(Fig. 1). The two independent SnIV atoms within the trans-OXSnC3 (X = O, Cl) moieties have a distorted trigonal-bipyramidal environment. The axial positions involve either two O atoms of different sulfate anions [Sn11], or one O atom of a sulfate anion and a Cl atom [Sn1]; both SnIV atoms are bonded to three methyl groups in equatorial positions. The axial angle O10—Sn11—O9 is 176.23 (15)° and is more distorted from the ideal angle of linearity compared to Cl2—Sn1—O6 (177.89 (12)°). The axial Sn—O distances (Sn1—O6 2.345 (4) Å; Sn11—O10 2.286 (5) Å; Sn11—O9 2.269 (5) Å; Table 1) are shorter than the Sn—O distance of 2.450 (5) Å in the structure of the related compound (Bu4N)[Sn(CH3)3Cl(HSO4)] (Diallo et al., 2009), but are in the excepted range [2.262 (2)–2.305 (2) Å] found in (Bu4N)[Sn3(CH3)9(SO4)2] (Diop et al., 2012).The [Sn2(CH3)6Cl(SO4)]- anionic units in the title compound assemble into an infinite zigzag chain parallet to the c-axis formed by (SnMe3) units bridged by SO42- units (Fig. 2). The SO42- µ3-bridging anion itself bonds to a third (SnMe3)Cl unit. The [Sn2(CH3)6Cl(SO4)]-∞ chains are separated by Bu4N+ cations as to form distinct layers parallel to the bc plane (Fig. 3). Weak C—H···O hydrogen bond interactions (Table 2) are present between the sulfate O8 atoms and butyl chains of the Bu4N+ cations.
For related structures, see: Molloy et al. (1989); Zhang et al. (2008); Sadiq-ur-Rehman et al. (2004); Aziz-ur-Rehman et al. (2006); Diallo et al. (2009); Diop et al. (2012). For details of the use of constraints and restraints during the structure
see: Cooper et al. (2010, 2012). For background to the weighting schemes used in the see: Prince (1982); Watkin (1994).Data collection: CrysAlis PRO (Agilent, 2010); cell
CrysAlis PRO (Agilent, 2010); data reduction: CrysAlis PRO (Agilent, 2010); program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: CRYSTALS (Betteridge et al., 2003).Fig. 1. A view of the asymmetric unit of the title compound, showing the numbering scheme and displacement ellipsoids drawn at the 50% probability level. For the disordered part of the cation, only the mojor component is displayed. H atoms are shown as spheres of arbitary radius. | |
Fig. 2. A view of the polymeric chain of the organotin(IV) complex anion, [Sn2(CH3)6Cl(SO4)]-; displacement ellipsoids are drawn at the 50% probability level. | |
Fig. 3. A view of the packing of the title compound. Hydrogen atoms have been omitted for clarity. |
(C16H36N)[Sn2(CH3)6Cl(SO4)] | F(000) = 2864 |
Mr = 701.60 | Dx = 1.466 Mg m−3 |
Orthorhombic, Aba2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: A 2 -2ac | Cell parameters from 17152 reflections |
a = 27.2051 (6) Å | θ = 2.0–27.7° |
b = 20.4336 (5) Å | µ = 1.75 mm−1 |
c = 11.4370 (2) Å | T = 175 K |
V = 6357.8 (3) Å3 | Prism, colourless |
Z = 8 | 0.25 × 0.20 × 0.15 mm |
Agilent Xcalibur (Sapphire3, Gemini) diffractometer | 8068 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 7179 reflections with I > 2.0σ(I) |
Graphite monochromator | Rint = 0.049 |
Detector resolution: 16.0143 pixels mm-1 | θmax = 29.4°, θmin = 1.5° |
ω scans | h = −37→34 |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2010) | k = −27→26 |
Tmin = 0.651, Tmax = 1.000 | l = −15→15 |
59083 measured reflections |
Refinement on F | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.053 | Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A0*T0(x) + A1*T1(x) ··· + An-1]*Tn-1(x)] where Ai are the Chebychev coefficients listed below and x = F /Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)2]2 Ai are: 13.1 -3.14 6.69 3.90 -2.02 |
wR(F2) = 0.053 | (Δ/σ)max = 0.001 |
S = 1.07 | Δρmax = 1.44 e Å−3 |
7179 reflections | Δρmin = −2.06 e Å−3 |
301 parameters | Absolute structure: Flack (1983), 3709 Friedel pairs |
33 restraints | Absolute structure parameter: 0.05 (4) |
Primary atom site location: iterative |
(C16H36N)[Sn2(CH3)6Cl(SO4)] | V = 6357.8 (3) Å3 |
Mr = 701.60 | Z = 8 |
Orthorhombic, Aba2 | Mo Kα radiation |
a = 27.2051 (6) Å | µ = 1.75 mm−1 |
b = 20.4336 (5) Å | T = 175 K |
c = 11.4370 (2) Å | 0.25 × 0.20 × 0.15 mm |
Agilent Xcalibur (Sapphire3, Gemini) diffractometer | 8068 independent reflections |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2010) | 7179 reflections with I > 2.0σ(I) |
Tmin = 0.651, Tmax = 1.000 | Rint = 0.049 |
59083 measured reflections |
R[F2 > 2σ(F2)] = 0.053 | H-atom parameters constrained |
wR(F2) = 0.053 | Δρmax = 1.44 e Å−3 |
S = 1.07 | Δρmin = −2.06 e Å−3 |
7179 reflections | Absolute structure: Flack (1983), 3709 Friedel pairs |
301 parameters | Absolute structure parameter: 0.05 (4) |
33 restraints |
Refinement. Friedif = 325.1 Estimated Friedel difference = 106.9462 f computed from scattering factors, including f-prime Current Do—Dc R-factor (%)= 79.99 No of Reflections processed = 7181 No of Friedel Pairs found = 3241 No of Friedel Pairs used = 3241 No of Unpaired Reflections = 375 No of Centric Reflections = 324 Flack parameter obtained from original refinement Hooft parameter obtained with Flack x set to zero Reflections only used if /Fo+ - Fo-/ < 99999.00 * /Fc+ - Fc-/ Friedif = 325.12 Acta A63, (2007), 257–265 Flack & Shmueli (2007) recommend a value >200 for general structures and >80 for enantiopure crystals Flack Parameter & su 0.0477 0.0352 Hooft Parameter & su 0.0130 0.0149 Ton G & su 0.9739 0.0299 No of reflections for which delta(Fo) has same sign as delta(Fc) Same sign Opposite sign 2050 1191 For an enantiopure material, there are 2 choices, P2 P2(correct) 1.0000 i.e. 0.100000E+01 If 50:50 twinning is possible, there are 3 choices, P3 P3(correct) 1.0000 i.e. 0.100000E+01 P3(rac-twin) 0.0000 i.e. 0.000000E+00 P3(inverse) 0.0000 i.e. 0.000000E+00 G 0.9739 G S.U. 0.0299 FLEQ 0.0130 FLEQ S.U. 0.0149 i.e. 0.149430E-01 |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sn1 | 0.095395 (14) | 0.642868 (19) | 0.30555 (17) | 0.0371 | |
Cl2 | 0.03842 (7) | 0.72492 (9) | 0.2051 (2) | 0.0553 | |
C3 | 0.0556 (3) | 0.5604 (4) | 0.2468 (8) | 0.0574 | |
C4 | 0.0795 (3) | 0.6783 (4) | 0.4760 (6) | 0.0567 | |
C5 | 0.1567 (3) | 0.6826 (4) | 0.2163 (8) | 0.0594 | |
O6 | 0.14856 (17) | 0.5707 (2) | 0.4025 (4) | 0.0407 | |
S7 | 0.18192 (5) | 0.51883 (7) | 0.3647 (2) | 0.0326 | |
O8 | 0.15838 (16) | 0.4724 (2) | 0.2867 (4) | 0.0428 | |
O9 | 0.22483 (15) | 0.5494 (2) | 0.3060 (4) | 0.0395 | |
O10 | 0.19910 (16) | 0.4841 (2) | 0.4713 (4) | 0.0398 | |
Sn11 | 0.239704 (13) | 0.516838 (18) | 0.63624 (17) | 0.0326 | |
C12 | 0.1884 (3) | 0.5899 (4) | 0.6739 (6) | 0.0512 | |
C13 | 0.3026 (2) | 0.5367 (5) | 0.5346 (6) | 0.0503 | |
C14 | 0.2271 (3) | 0.4218 (3) | 0.6961 (7) | 0.0549 | |
N15 | 0.1078 (2) | 0.8008 (4) | −0.1571 (6) | 0.0660 | |
C16 | 0.1614 (3) | 0.8095 (5) | −0.1593 (8) | 0.0694 | |
C17 | 0.1865 (4) | 0.7718 (5) | −0.0667 (8) | 0.0909 | |
C18 | 0.2411 (4) | 0.7755 (8) | −0.0881 (16) | 0.1209 | |
C19 | 0.2674 (8) | 0.7363 (10) | 0.0005 (16) | 0.1779 | |
C20 | 0.0925 (5) | 0.7338 (4) | −0.1953 (10) | 0.0847 | 0.75 (2) |
C21 | 0.0846 (4) | 0.6772 (5) | −0.1147 (8) | 0.0905 | |
C22 | 0.0556 (4) | 0.6258 (4) | −0.1772 (8) | 0.0845 | |
C23 | 0.0525 (8) | 0.5731 (10) | −0.0870 (15) | 0.2003 | |
C24 | 0.0770 (4) | 0.8207 (5) | −0.0658 (9) | 0.0760 | |
C25 | 0.0910 (4) | 0.8850 (5) | −0.0131 (9) | 0.0844 | 0.79 (2) |
C26 | 0.0555 (5) | 0.9121 (6) | 0.0743 (15) | 0.1389 | |
C27 | 0.0722 (5) | 0.9755 (5) | 0.1224 (15) | 0.1060 | |
C28 | 0.0855 (4) | 0.8509 (6) | −0.2424 (8) | 0.0762 | |
C29 | 0.1037 (4) | 0.8465 (5) | −0.3628 (8) | 0.0891 | |
C30 | 0.0773 (7) | 0.8833 (9) | −0.4543 (9) | 0.1188 | |
C31 | 0.0985 (6) | 0.8812 (9) | −0.5722 (12) | 0.1342 | |
C251 | 0.0409 (7) | 0.8720 (12) | −0.029 (2) | 0.0842 | 0.21 (2) |
C201 | 0.0734 (7) | 0.7488 (5) | −0.115 (3) | 0.0825 | 0.25 (2) |
H161 | 0.1685 | 0.8563 | −0.1489 | 0.0840* | |
H162 | 0.1733 | 0.7947 | −0.2355 | 0.0843* | |
H171 | 0.1783 | 0.7893 | 0.0092 | 0.1081* | |
H172 | 0.1768 | 0.7268 | −0.0721 | 0.1082* | |
H231 | 0.0361 | 0.5360 | −0.1206 | 0.2980* | |
H232 | 0.0343 | 0.5883 | −0.0207 | 0.2980* | |
H233 | 0.0851 | 0.5606 | −0.0634 | 0.2980* | |
H271 | 0.0515 | 1.0102 | 0.0937 | 0.1599* | |
H272 | 0.1053 | 0.9833 | 0.0977 | 0.1599* | |
H273 | 0.0712 | 0.9748 | 0.2063 | 0.1600* | |
H41 | 0.1065 | 0.6699 | 0.5270 | 0.0864* | |
H42 | 0.0731 | 0.7248 | 0.4738 | 0.0860* | |
H43 | 0.0511 | 0.6560 | 0.5060 | 0.0862* | |
H31 | 0.0631 | 0.5239 | 0.2949 | 0.0852* | |
H32 | 0.0211 | 0.5696 | 0.2514 | 0.0851* | |
H33 | 0.0645 | 0.5508 | 0.1666 | 0.0850* | |
H51 | 0.1509 | 0.7279 | 0.2013 | 0.0890* | |
H52 | 0.1607 | 0.6600 | 0.1437 | 0.0891* | |
H53 | 0.1855 | 0.6773 | 0.2625 | 0.0892* | |
H121 | 0.2056 | 0.6301 | 0.6864 | 0.0762* | |
H122 | 0.1705 | 0.5780 | 0.7432 | 0.0765* | |
H123 | 0.1664 | 0.5950 | 0.6084 | 0.0760* | |
H141 | 0.2542 | 0.4064 | 0.7409 | 0.0820* | |
H142 | 0.1979 | 0.4221 | 0.7426 | 0.0822* | |
H143 | 0.2219 | 0.3935 | 0.6305 | 0.0822* | |
H131 | 0.3044 | 0.5074 | 0.4683 | 0.0762* | |
H132 | 0.3316 | 0.5311 | 0.5806 | 0.0760* | |
H133 | 0.3011 | 0.5809 | 0.5077 | 0.0760* | |
H221 | 0.0235 | 0.6429 | −0.1972 | 0.1000* | |
H222 | 0.0715 | 0.6107 | −0.2481 | 0.0999* | |
H301 | 0.0769 | 0.9290 | −0.4317 | 0.1441* | |
H302 | 0.0438 | 0.8664 | −0.4578 | 0.1442* | |
H291 | 0.1371 | 0.8637 | −0.3623 | 0.1052* | |
H292 | 0.1037 | 0.8006 | −0.3855 | 0.1051* | |
H281 | 0.0908 | 0.8950 | −0.2139 | 0.0911* | |
H282 | 0.0503 | 0.8419 | −0.2460 | 0.0910* | |
H181 | 0.2519 | 0.8205 | −0.0842 | 0.1501* | |
H182 | 0.2482 | 0.7580 | −0.1652 | 0.1502* | |
H251 | 0.1081 | 0.9092 | −0.0717 | 0.1240* | 0.79 (2) |
H252 | 0.1136 | 0.8866 | 0.0508 | 0.1240* | 0.79 (2) |
H2511 | 0.0149 | 0.8854 | −0.0808 | 0.1240* | 0.21 (2) |
H2512 | 0.0143 | 0.8465 | 0.0015 | 0.1240* | 0.21 (2) |
H201 | 0.0696 | 0.7337 | −0.2582 | 0.1321* | 0.75 (2) |
H202 | 0.1261 | 0.7214 | −0.2043 | 0.1319* | 0.75 (2) |
H2011 | 0.0744 | 0.7279 | −0.0401 | 0.1290* | 0.25 (2) |
H2012 | 0.0381 | 0.7501 | −0.1125 | 0.1290* | 0.25 (2) |
H241 | 0.0414 | 0.8104 | −0.0162 | 0.1181* | 0.79 (2) |
H242 | 0.0819 | 0.8014 | 0.0099 | 0.1122* | 0.79 (2) |
H243 | 0.1035 | 0.8274 | 0.0073 | 0.1180* | 0.21 (2) |
H244 | 0.0764 | 0.7722 | −0.0157 | 0.1205* | 0.21 (2) |
H211 | 0.1157 | 0.6638 | −0.0821 | 0.1384* | 0.75 (2) |
H212 | 0.1170 | 0.6617 | −0.0949 | 0.1383* | 0.75 (2) |
H213 | 0.1181 | 0.6647 | −0.0991 | 0.1381* | 0.25 (2) |
H214 | 0.1169 | 0.6649 | −0.0885 | 0.1381* | 0.25 (2) |
H311 | 0.0927 | 0.9220 | −0.6108 | 0.2010* | |
H312 | 0.1332 | 0.8731 | −0.5670 | 0.2010* | |
H313 | 0.0831 | 0.8467 | −0.6159 | 0.2011* | |
H191 | 0.2959 | 0.7172 | −0.0350 | 0.2810* | |
H192 | 0.2772 | 0.7643 | 0.0636 | 0.2810* | |
H193 | 0.2461 | 0.7024 | 0.0289 | 0.2809* | |
H261 | 0.0247 | 0.9184 | 0.0368 | 0.1704* | 0.79 (2) |
H262 | 0.0518 | 0.8817 | 0.1366 | 0.1704* | 0.79 (2) |
H263 | 0.0269 | 0.9062 | 0.1207 | 0.1704* | 0.21 (2) |
H264 | 0.0812 | 0.8851 | 0.1033 | 0.1704* | 0.21 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.04077 (18) | 0.03904 (18) | 0.03139 (16) | −0.00380 (16) | −0.00108 (18) | 0.00268 (18) |
Cl2 | 0.0568 (10) | 0.0501 (9) | 0.0589 (10) | 0.0069 (8) | −0.0059 (8) | 0.0132 (8) |
C3 | 0.055 (4) | 0.051 (4) | 0.066 (5) | −0.010 (3) | −0.023 (4) | 0.000 (3) |
C4 | 0.077 (5) | 0.065 (5) | 0.028 (3) | 0.001 (4) | 0.000 (3) | −0.008 (3) |
C5 | 0.056 (4) | 0.062 (5) | 0.060 (4) | −0.008 (4) | 0.008 (4) | 0.026 (4) |
O6 | 0.046 (2) | 0.051 (2) | 0.0252 (19) | 0.005 (2) | −0.0002 (17) | 0.0042 (17) |
S7 | 0.0359 (7) | 0.0386 (7) | 0.0232 (6) | −0.0024 (6) | −0.0004 (5) | 0.0037 (5) |
O8 | 0.046 (2) | 0.050 (2) | 0.032 (2) | −0.0083 (18) | −0.0009 (17) | −0.0023 (18) |
O9 | 0.0439 (19) | 0.047 (2) | 0.0278 (17) | −0.0062 (17) | −0.0002 (19) | −0.002 (2) |
O10 | 0.042 (2) | 0.044 (2) | 0.0330 (19) | 0.0026 (18) | 0.0010 (17) | 0.0058 (19) |
Sn11 | 0.03353 (15) | 0.03812 (17) | 0.02608 (14) | 0.00369 (15) | 0.00169 (16) | 0.00763 (18) |
C12 | 0.047 (4) | 0.073 (5) | 0.034 (3) | 0.024 (3) | −0.006 (2) | −0.010 (3) |
C13 | 0.038 (3) | 0.087 (6) | 0.026 (3) | −0.018 (3) | 0.007 (2) | 0.004 (3) |
C14 | 0.075 (5) | 0.036 (3) | 0.053 (4) | −0.004 (3) | −0.023 (4) | 0.007 (3) |
N15 | 0.065 (4) | 0.088 (5) | 0.045 (3) | −0.027 (4) | 0.002 (3) | 0.023 (3) |
C16 | 0.073 (5) | 0.068 (5) | 0.067 (5) | 0.009 (4) | 0.009 (4) | 0.009 (4) |
C17 | 0.165 (13) | 0.059 (5) | 0.048 (5) | −0.004 (6) | 0.016 (6) | 0.007 (4) |
C18 | 0.089 (9) | 0.116 (11) | 0.158 (18) | 0.032 (9) | 0.018 (9) | 0.041 (11) |
C19 | 0.22 (2) | 0.145 (16) | 0.165 (19) | 0.102 (16) | 0.116 (18) | 0.086 (15) |
C20 | 0.077 (7) | 0.126 (12) | 0.051 (6) | 0.019 (8) | 0.022 (7) | 0.020 (9) |
C21 | 0.085 (8) | 0.108 (9) | 0.079 (7) | 0.001 (6) | −0.011 (5) | −0.029 (7) |
C22 | 0.109 (8) | 0.089 (7) | 0.055 (6) | 0.029 (6) | −0.024 (5) | −0.039 (5) |
C23 | 0.19 (2) | 0.33 (3) | 0.086 (11) | 0.14 (2) | 0.003 (12) | 0.036 (16) |
C24 | 0.082 (6) | 0.082 (7) | 0.063 (5) | 0.004 (5) | 0.021 (5) | −0.017 (5) |
C25 | 0.082 (8) | 0.128 (12) | 0.044 (6) | −0.059 (8) | 0.006 (5) | 0.023 (7) |
C26 | 0.088 (8) | 0.052 (6) | 0.28 (2) | −0.017 (5) | 0.038 (12) | −0.018 (9) |
C27 | 0.125 (10) | 0.067 (6) | 0.126 (11) | −0.009 (6) | 0.045 (9) | −0.050 (7) |
C28 | 0.073 (6) | 0.094 (7) | 0.061 (5) | −0.002 (5) | −0.006 (4) | 0.011 (5) |
C29 | 0.093 (7) | 0.063 (5) | 0.112 (9) | −0.022 (5) | −0.045 (7) | 0.030 (6) |
C30 | 0.160 (13) | 0.131 (13) | 0.066 (7) | 0.059 (11) | −0.028 (8) | 0.000 (7) |
C31 | 0.112 (11) | 0.129 (12) | 0.161 (17) | −0.027 (10) | −0.037 (11) | 0.076 (12) |
C251 | 0.081 (4) | 0.127 (5) | 0.044 (5) | −0.059 (5) | 0.009 (5) | 0.025 (5) |
C201 | 0.077 (5) | 0.124 (5) | 0.046 (4) | 0.018 (5) | 0.019 (4) | 0.022 (5) |
Sn1—C3 | 2.112 (7) | C21—C22 | 1.4946 (10) |
Sn1—C4 | 2.124 (7) | C21—C201 | 1.4949 (10) |
Sn1—C5 | 2.117 (7) | C21—H211 | 0.963 |
Sn1—Cl2 | 2.5561 (18) | C21—H212 | 0.963 |
Sn1—O6 | 2.345 (4) | C21—H213 | 0.961 |
Sn11—C12 | 2.090 (7) | C21—H214 | 0.960 |
Sn11—C13 | 2.108 (6) | C22—C23 | 1.4951 (10) |
Sn11—C14 | 2.088 (7) | C22—H221 | 0.967 |
Sn11—O9i | 2.269 (5) | C22—H222 | 0.969 |
Sn11—O10 | 2.286 (5) | C23—H231 | 0.960 |
C3—H31 | 0.949 | C23—H232 | 0.958 |
C3—H32 | 0.960 | C23—H233 | 0.962 |
C3—H33 | 0.969 | C24—C25 | 1.4949 (10) |
C4—H41 | 0.955 | C24—C251 | 1.4950 (10) |
C4—H42 | 0.966 | C24—C201 | 1.58 (2) |
C4—H43 | 0.960 | C24—H241 | 1.143 |
C5—H51 | 0.955 | C24—H242 | 0.962 |
C5—H52 | 0.956 | C24—H243 | 1.113 |
C5—H53 | 0.951 | C24—H244 | 1.147 |
O6—S7 | 1.460 (5) | C25—C26 | 1.4953 (10) |
S7—O8 | 1.451 (5) | C25—C251 | 1.40 (3) |
S7—O9 | 1.485 (4) | C25—H251 | 0.954 |
S7—O10 | 1.487 (4) | C25—H252 | 0.956 |
C12—H121 | 0.957 | C25—H243 | 1.247 |
C12—H122 | 0.961 | C26—C27 | 1.479 (15) |
C12—H123 | 0.964 | C26—C251 | 1.4949 (10) |
C13—H131 | 0.967 | C26—H261 | 0.950 |
C13—H132 | 0.955 | C26—H262 | 0.950 |
C13—H133 | 0.955 | C26—H263 | 0.950 |
C14—H141 | 0.953 | C26—H264 | 0.950 |
C14—H142 | 0.954 | C27—H271 | 0.962 |
C14—H143 | 0.957 | C27—H272 | 0.958 |
N15—C16 | 1.469 (8) | C27—H273 | 0.960 |
N15—C20 | 1.4958 (10) | C28—C29 | 1.466 (9) |
N15—C24 | 1.399 (11) | C28—H281 | 0.968 |
N15—C28 | 1.539 (8) | C28—H282 | 0.976 |
N15—C201 | 1.4949 (10) | C29—C30 | 1.475 (8) |
C16—C17 | 1.478 (8) | C29—H291 | 0.974 |
C16—H161 | 0.982 | C29—H292 | 0.974 |
C16—H162 | 0.979 | C30—C31 | 1.467 (9) |
C17—C18 | 1.506 (9) | C30—H301 | 0.970 |
C17—H171 | 0.965 | C30—H302 | 0.975 |
C17—H172 | 0.959 | C31—H311 | 0.958 |
C18—C19 | 1.477 (9) | C31—H312 | 0.962 |
C18—H181 | 0.965 | C31—H313 | 0.960 |
C18—H182 | 0.971 | C251—H2511 | 0.961 |
C19—H191 | 0.960 | C251—H2512 | 0.959 |
C19—H192 | 0.959 | C251—H241 | 1.267 |
C19—H193 | 0.959 | C251—H261 | 1.291 |
C20—C21 | 1.4948 (10) | C201—H2011 | 0.960 |
C20—C201 | 1.10 (3) | C201—H2012 | 0.960 |
C20—H201 | 0.952 | C201—H244 | 1.238 |
C20—H202 | 0.956 | H242—H244 | 0.681 |
Cl2—Sn1—C3 | 94.0 (2) | C25—C24—C251 | 55.8 (12) |
Cl2—Sn1—C4 | 93.7 (2) | N15—C24—C201 | 59.9 (6) |
C3—Sn1—C4 | 117.4 (4) | C25—C24—C201 | 168.3 (14) |
Cl2—Sn1—C5 | 90.5 (2) | C251—C24—C201 | 135.4 (14) |
C3—Sn1—C5 | 123.8 (4) | N15—C24—H241 | 145.6 |
C4—Sn1—C5 | 118.2 (4) | C25—C24—H241 | 100.2 |
Cl2—Sn1—O6 | 177.89 (12) | C251—C24—H241 | 55.5 |
C3—Sn1—O6 | 88.0 (2) | C201—C24—H241 | 87.3 |
C4—Sn1—O6 | 84.6 (3) | N15—C24—H242 | 118.1 |
C5—Sn1—O6 | 89.1 (3) | C25—C24—H242 | 87.9 |
Sn1—C3—H31 | 109.5 | C251—C24—H242 | 97.3 |
Sn1—C3—H32 | 109.2 | C201—C24—H242 | 87.0 |
H31—C3—H32 | 109.4 | H241—C24—H242 | 66.0 |
Sn1—C3—H33 | 109.6 | N15—C24—H243 | 102.1 |
H31—C3—H33 | 109.6 | C25—C24—H243 | 54.8 |
H32—C3—H33 | 109.5 | C251—C24—H243 | 97.4 |
Sn1—C4—H41 | 110.1 | C201—C24—H243 | 115.2 |
Sn1—C4—H42 | 110.4 | H241—C24—H243 | 101.5 |
H41—C4—H42 | 109.2 | N15—C24—H244 | 97.5 |
Sn1—C4—H43 | 109.4 | C25—C24—H244 | 124.3 |
H41—C4—H43 | 108.4 | C251—C24—H244 | 117.2 |
H42—C4—H43 | 109.4 | C201—C24—H244 | 51.1 |
Sn1—C5—H51 | 109.2 | H241—C24—H244 | 65.1 |
Sn1—C5—H52 | 108.9 | H242—C24—H243 | 44.3 |
H51—C5—H52 | 109.3 | H242—C24—H244 | 36.4 |
Sn1—C5—H53 | 109.7 | H243—C24—H244 | 74.9 |
H51—C5—H53 | 110.2 | C24—C25—C26 | 115.5 (8) |
H52—C5—H53 | 109.4 | C24—C25—C251 | 62.1 (6) |
Sn1—O6—S7 | 134.4 (2) | C26—C25—C251 | 62.1 (6) |
O6—S7—O8 | 112.4 (3) | C24—C25—H251 | 107.2 |
O6—S7—O9 | 108.5 (3) | C26—C25—H251 | 126.4 |
O8—S7—O9 | 110.2 (3) | C251—C25—H251 | 118.7 |
O6—S7—O10 | 107.4 (2) | C24—C25—H252 | 120.1 |
O8—S7—O10 | 109.3 (3) | C26—C25—H252 | 83.8 |
O9—S7—O10 | 108.9 (3) | C251—C25—H252 | 137.2 |
Sn11ii—O9—S7 | 126.7 (2) | H251—C25—H252 | 101.8 |
S7—O10—Sn11 | 133.5 (3) | C24—C25—H243 | 46.8 |
O10—Sn11—O9i | 176.23 (15) | C26—C25—H243 | 113.6 |
O10—Sn11—C12 | 93.2 (2) | C251—C25—H243 | 96.4 |
O9i—Sn11—C12 | 84.1 (2) | H251—C25—H243 | 119.1 |
O10—Sn11—C13 | 89.6 (2) | H252—C25—H243 | 73.3 |
O9i—Sn11—C13 | 94.0 (2) | C25—C26—C27 | 112.0 (9) |
C12—Sn11—C13 | 121.2 (4) | C25—C26—C251 | 55.8 (12) |
O10—Sn11—C14 | 85.3 (2) | C27—C26—C251 | 148.9 (19) |
O9i—Sn11—C14 | 93.6 (2) | C25—C26—H261 | 108.5 |
C12—Sn11—C14 | 119.2 (4) | C27—C26—H261 | 108.6 |
C13—Sn11—C14 | 119.6 (4) | C251—C26—H261 | 58.8 |
Sn11—C12—H121 | 108.5 | C25—C26—H262 | 109.2 |
Sn11—C12—H122 | 109.1 | C27—C26—H262 | 109.1 |
H121—C12—H122 | 110.0 | C251—C26—H262 | 102.0 |
Sn11—C12—H123 | 109.3 | H261—C26—H262 | 109.5 |
H121—C12—H123 | 109.1 | C25—C26—H263 | 148.8 |
H122—C12—H123 | 110.9 | C27—C26—H263 | 98.9 |
Sn11—C13—H131 | 110.7 | C251—C26—H263 | 99.0 |
Sn11—C13—H132 | 110.1 | H261—C26—H263 | 63.1 |
H131—C13—H132 | 108.5 | H262—C26—H263 | 53.9 |
Sn11—C13—H133 | 108.9 | C25—C26—H264 | 62.9 |
H131—C13—H133 | 109.5 | C27—C26—H264 | 98.8 |
H132—C13—H133 | 109.1 | C251—C26—H264 | 98.9 |
Sn11—C14—H141 | 110.8 | H261—C26—H264 | 152.3 |
Sn11—C14—H142 | 108.2 | H262—C26—H264 | 55.7 |
H141—C14—H142 | 110.3 | H263—C26—H264 | 109.5 |
Sn11—C14—H143 | 109.2 | C26—C27—H271 | 109.8 |
H141—C14—H143 | 109.6 | C26—C27—H272 | 108.9 |
H142—C14—H143 | 108.6 | H271—C27—H272 | 109.1 |
C16—N15—C20 | 112.5 (8) | C26—C27—H273 | 110.5 |
C16—N15—C24 | 124.8 (8) | H271—C27—H273 | 109.6 |
C20—N15—C24 | 108.5 (7) | H272—C27—H273 | 109.0 |
C16—N15—C28 | 107.4 (6) | N15—C28—C29 | 114.9 (8) |
C20—N15—C28 | 108.3 (7) | N15—C28—H281 | 110.3 |
C24—N15—C28 | 92.5 (8) | C29—C28—H281 | 108.8 |
C16—N15—C201 | 135.5 (12) | N15—C28—H282 | 106.8 |
C24—N15—C201 | 66.0 (11) | C29—C28—H282 | 106.2 |
C28—N15—C201 | 115.4 (14) | H281—C28—H282 | 109.6 |
N15—C16—C17 | 112.6 (8) | C28—C29—C30 | 118.1 (10) |
N15—C16—H161 | 108.1 | C28—C29—H291 | 106.7 |
C17—C16—H161 | 109.2 | C30—C29—H291 | 105.9 |
N15—C16—H162 | 107.9 | C28—C29—H292 | 108.0 |
C17—C16—H162 | 108.9 | C30—C29—H292 | 107.6 |
H161—C16—H162 | 110.1 | H291—C29—H292 | 110.4 |
C16—C17—C18 | 108.2 (8) | C29—C30—C31 | 116.5 (11) |
C16—C17—H171 | 110.1 | C29—C30—H301 | 107.9 |
C18—C17—H171 | 110.8 | C31—C30—H301 | 106.2 |
C16—C17—H172 | 109.0 | C29—C30—H302 | 107.7 |
C18—C17—H172 | 108.1 | C31—C30—H302 | 108.6 |
H171—C17—H172 | 110.5 | H301—C30—H302 | 110.0 |
C17—C18—C19 | 109.8 (13) | C30—C31—H311 | 109.4 |
C17—C18—H181 | 110.0 | C30—C31—H312 | 109.5 |
C19—C18—H181 | 109.7 | H311—C31—H312 | 109.8 |
C17—C18—H182 | 109.0 | C30—C31—H313 | 109.3 |
C19—C18—H182 | 109.0 | H311—C31—H313 | 109.2 |
H181—C18—H182 | 109.4 | H312—C31—H313 | 109.6 |
C18—C19—H191 | 108.8 | C24—C251—C26 | 115.5 (8) |
C18—C19—H192 | 109.1 | C24—C251—C25 | 62.1 (6) |
H191—C19—H192 | 109.6 | C26—C251—C25 | 62.1 (6) |
C18—C19—H193 | 109.5 | C24—C251—H2511 | 120.8 |
H191—C19—H193 | 109.7 | C26—C251—H2511 | 121.7 |
H192—C19—H193 | 110.1 | C25—C251—H2511 | 138.1 |
N15—C20—C21 | 124.6 (8) | C24—C251—H2512 | 102.6 |
N15—C20—C201 | 68.5 (7) | C26—C251—H2512 | 101.9 |
C21—C20—C201 | 68.5 (7) | C25—C251—H2512 | 142.1 |
N15—C20—H201 | 113.9 | H2511—C251—H2512 | 79.8 |
C21—C20—H201 | 111.8 | C24—C251—H241 | 48.0 |
C201—C20—H201 | 108.7 | C26—C251—H241 | 116.6 |
N15—C20—H202 | 90.5 | C25—C251—H241 | 99.4 |
C21—C20—H202 | 89.9 | H2511—C251—H241 | 111.3 |
C201—C20—H202 | 128.2 | H2512—C251—H241 | 54.8 |
H201—C20—H202 | 123.0 | C24—C251—H261 | 154.5 |
C20—C21—C22 | 108.9 (8) | C26—C251—H261 | 39.0 |
C22—C21—C201 | 125.2 (17) | C25—C251—H261 | 96.6 |
C20—C21—H211 | 109.5 | H2511—C251—H261 | 84.2 |
C22—C21—H211 | 116.8 | H2512—C251—H261 | 85.8 |
C201—C21—H211 | 117.3 | H241—C251—H261 | 131.5 |
C20—C21—H212 | 105.5 | C24—C201—C21 | 154 (3) |
C22—C21—H212 | 111.5 | C24—C201—N15 | 54.1 (6) |
C201—C21—H212 | 120.6 | C21—C201—N15 | 124.7 (8) |
H211—C21—H212 | 9.4 | C24—C201—C20 | 122.0 (7) |
C20—C21—H213 | 100.6 | C21—C201—C20 | 68.5 (7) |
C22—C21—H213 | 113.8 | N15—C201—C20 | 68.5 (7) |
C201—C21—H213 | 117.0 | C24—C201—H2011 | 95.2 |
H211—C21—H213 | 12.3 | C21—C201—H2011 | 63.6 |
H212—C21—H213 | 4.9 | N15—C201—H2011 | 125.8 |
C20—C21—H214 | 105.4 | C20—C201—H2011 | 127.6 |
C22—C21—H214 | 116.6 | C24—C201—H2012 | 91.4 |
C201—C21—H214 | 116.4 | C21—C201—H2012 | 103.5 |
H211—C21—H214 | 4.9 | N15—C201—H2012 | 128.0 |
H212—C21—H214 | 5.8 | C20—C201—H2012 | 120.6 |
H213—C21—H214 | 7.5 | H2011—C201—H2012 | 90.7 |
C21—C22—C23 | 101.9 (13) | C24—C201—H244 | 46.1 |
C21—C22—H221 | 109.7 | C21—C201—H244 | 111.1 |
C23—C22—H221 | 111.8 | N15—C201—H244 | 88.8 |
C21—C22—H222 | 112.9 | C20—C201—H244 | 147.6 |
C23—C22—H222 | 111.8 | H2011—C201—H244 | 49.1 |
H221—C22—H222 | 108.7 | H2012—C201—H244 | 91.4 |
C22—C23—H231 | 108.6 | C24—H241—C251 | 76.5 |
C22—C23—H232 | 110.0 | C24—H242—H244 | 86.7 |
H231—C23—H232 | 109.4 | C24—H243—C25 | 78.4 |
C22—C23—H233 | 109.4 | H242—H244—C24 | 56.9 |
H231—C23—H233 | 109.5 | H242—H244—C201 | 138.4 |
H232—C23—H233 | 109.9 | C24—H244—C201 | 82.8 |
N15—C24—C25 | 113.9 (8) | C26—H261—C251 | 82.2 |
N15—C24—C251 | 143.6 (15) |
Symmetry codes: (i) −x+1/2, y, z+1/2; (ii) −x+1/2, y, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C16—H161···O8iii | 0.98 | 2.50 | 3.386 (18) | 150 (1) |
C12—H123···O6 | 0.96 | 2.46 | 3.311 (18) | 148 (1) |
C28—H281···O8iii | 0.97 | 2.43 | 3.195 (18) | 136 (1) |
C25—H251···O8iii | 0.95 | 2.48 | 3.434 (18) | 175 (1) |
Symmetry code: (iii) x, y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | (C16H36N)[Sn2(CH3)6Cl(SO4)] |
Mr | 701.60 |
Crystal system, space group | Orthorhombic, Aba2 |
Temperature (K) | 175 |
a, b, c (Å) | 27.2051 (6), 20.4336 (5), 11.4370 (2) |
V (Å3) | 6357.8 (3) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 1.75 |
Crystal size (mm) | 0.25 × 0.20 × 0.15 |
Data collection | |
Diffractometer | Agilent Xcalibur (Sapphire3, Gemini) |
Absorption correction | Multi-scan (CrysAlis PRO; Agilent, 2010) |
Tmin, Tmax | 0.651, 1.000 |
No. of measured, independent and observed [I > 2.0σ(I)] reflections | 59083, 8068, 7179 |
Rint | 0.049 |
(sin θ/λ)max (Å−1) | 0.691 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.053, 0.053, 1.07 |
No. of reflections | 7179 |
No. of parameters | 301 |
No. of restraints | 33 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.44, −2.06 |
Absolute structure | Flack (1983), 3709 Friedel pairs |
Absolute structure parameter | 0.05 (4) |
Computer programs: CrysAlis PRO (Agilent, 2010), SUPERFLIP (Palatinus & Chapuis, 2007), CRYSTALS (Betteridge et al., 2003), OLEX2 (Dolomanov et al., 2009).
Sn1—C3 | 2.112 (7) | Sn11—C12 | 2.090 (7) |
Sn1—C4 | 2.124 (7) | Sn11—C13 | 2.108 (6) |
Sn1—C5 | 2.117 (7) | Sn11—C14 | 2.088 (7) |
Sn1—Cl2 | 2.5561 (18) | Sn11—O9i | 2.269 (5) |
Sn1—O6 | 2.345 (4) | Sn11—O10 | 2.286 (5) |
Symmetry code: (i) −x+1/2, y, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C16—H161···O8ii | 0.982 | 2.500 | 3.386 (18) | 150.0 (2) |
C28—H281···O8ii | 0.968 | 2.426 | 3.195 (18) | 136.1 (3) |
C25—H251···O8ii | 0.954 | 2.482 | 3.434 (18) | 175.4 (3) |
Symmetry code: (ii) x, y+1/2, z−1/2. |
References
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
Among organotin(IV) complexes, a number of trimethyltin derivatives form polymeric structures with trigonal bipyramidal geometry around the SnIV atom, e.g. as reported by Molloy et al. (1989); Sadiq-ur-Rehman et al. (2004); Aziz-ur-Rehman et al. (2006); Zhang et al. (2008).
The title compound, {(C16H36N)[Sn2(CH3)6Cl(SO4)]}n, crystallizes with one tetrabutylammonium cation, Bu4N+, and one organotin(IV) complex anion in the asymmetric unit (Fig. 1). The two independent SnIV atoms within the trans-OXSnC3 (X = O, Cl) moieties have a distorted trigonal-bipyramidal environment. The axial positions involve either two O atoms of different sulfate anions [Sn11], or one O atom of a sulfate anion and a Cl atom [Sn1]; both SnIV atoms are bonded to three methyl groups in equatorial positions. The axial angle O10—Sn11—O9 is 176.23 (15)° and is more distorted from the ideal angle of linearity compared to Cl2—Sn1—O6 (177.89 (12)°). The axial Sn—O distances (Sn1—O6 2.345 (4) Å; Sn11—O10 2.286 (5) Å; Sn11—O9 2.269 (5) Å; Table 1) are shorter than the Sn—O distance of 2.450 (5) Å in the structure of the related compound (Bu4N)[Sn(CH3)3Cl(HSO4)] (Diallo et al., 2009), but are in the excepted range [2.262 (2)–2.305 (2) Å] found in (Bu4N)[Sn3(CH3)9(SO4)2] (Diop et al., 2012).
The [Sn2(CH3)6Cl(SO4)]- anionic units in the title compound assemble into an infinite zigzag chain parallet to the c-axis formed by (SnMe3) units bridged by SO42- units (Fig. 2). The SO42- µ3-bridging anion itself bonds to a third (SnMe3)Cl unit. The [Sn2(CH3)6Cl(SO4)]-∞ chains are separated by Bu4N+ cations as to form distinct layers parallel to the bc plane (Fig. 3). Weak C—H···O hydrogen bond interactions (Table 2) are present between the sulfate O8 atoms and butyl chains of the Bu4N+ cations.