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Chloro­tris(2,4,6-tri­methyl­phenyl)­tin(IV), crystallizes from ethanol as solvent-free needles, [Sn(C9H11)3Cl], (I), and as the hemisolvate, [Sn(C9H11)3Cl]·0.5C2H6O, (II). The asymmetric unit in (I) has three independent mol­ecules, whereas in (II), there are two [Sn(C9H11)3Cl] mol­ecules together with one ethanol molecule. In the unit cell of (II), the ethanol mol­ecules lie in channels between stacks of (Mes)3SnCl mol­ecules (Mes is 2,4,6-tri­methyl­phenyl) and each ethanol mol­ecule is disordered (0.50:0.50) over two positions. A comparison of the structures of the title compounds and other (Mes)3SnX (X = F, Br or I) systems with those of the tri­phenyl­tin analogues shows that the steric requirements of the o-CH3 groups are met by a flattening of the SnC3 skeleton and increases in the average Sn-X and Sn-C values. Comparing Sn-X data for (Mes)3SnX (X = F, Cl, Br or I) systems with values for the tris(o-methoxy­phenyl)­tin analogues suggests that the Sn-F distance of 1.961 Å in (Mes)3SnF may well be characteristic of sterically unhindered four-coordinate Ar3SnF systems.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102012362/fg1654sup1.cif
Contains datablocks I, II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102012362/fg1654Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102012362/fg1654IIsup3.hkl
Contains datablock II

CCDC references: 195602; 195603

Comment top

Replacement of the phenyl groups in Ph3SnX by mesityl (mesityl is 2,4,6-trimethylphenyl) produces structural changes that are attributed to the steric effects of the two ortho-methyl groups. Thus, while Ph3SnX with X = OH (Glidewell et al., 2002), F (Tudela et al., 1992) or OAc (Molloy et al., 1984) are polymeric, with five-coordinate Sn and planar C3Sn units, the mesityl analogues with X = OH or F (Reuter & Puff, 1989) or OAc (Wharf & Simard, 1992) are monomeric, with pyramidal C3SnX structures. Even when both (Mes)3SnX (Mes is mesityl) and Ph3SnX are four-coordinate monomers, e.g. with X = I (Simard & Wharf, 1994) or Br (Preut & Huber, 1979; Dakternieks et al., 2000), replacement of ortho-H atoms by CH3 groups still gives small but significant changes in the geometry around Sn, as well as an increase in the mean Sn—X distance of 0.05 Å when phenyl is replaced by mesityl in Ar3SnX (X = Br or I). We now report the structures of (Mes)3SnCl, (I), and of its ethanol hemisolvate, (II), first for comparison with those of Ph3SnCl (Tse et al., 1986; Ng, 1995), and then to enable the trends in geometry around Sn for the complete (Mes)3SnX series to be assessed. \sch

Two quite different sets of crystals, (I) and (II), were produced by slow evaporation of an ethanol solution of (Mes)3SnCl. Needles, (I), were found to be solvent-free and to have the same space group as (Mes)3SnF, but with three molecules in the asymmetric unit rather than two as in the fluoride case. The three molecules differ in detail (Table 1 and Fig. 1), but the averaged environment around Sn is almost the same in each case. The molecules in the solvent-free crystals, (I), are closely packed. However, it would appear that, as X in (Mes)3SnX increases in size from F to I, solvent-free packing of (Mes)3SnX units becomes more difficult and has yet to be established with X = Br or I.

In contrast, (II), the solvate [(Mes)3SnCl]2·EtOH (Table 2), has two molecules in the asymmetric unit, with solvent molecules occupying the channels between stacks of (Mes)3SnX molecules, as in the isomorphous compounds [(Mes)3SnBr]2.acetone (Dakternieks et al., 2000) and [(Mes)3SnI]2·CDCl3 (Simard & Wharf, 1994). However, unlike the trimesityltin iodide solvate, where the CDCl3 molecules are not disordered, the packing of (II) (Fig. 2) requires the ethanol molecules partially to occupy voids in the crystal lattice; they are completely disordered (0.50/0.50) over two positions. There are, in fact, several models possible for the disorder. That used here was chosen as the most chemically feasible.

The geometries around Sn in various (Mes)3SnX molecules can be summarized by the averaged values of C—Sn—X and C—Sn—C, and the difference [C—Sn—C - C—Sn—X] (Table 3), as used earlier when comparing Ph3SnX and (o-Anis)3SnX structures (Anis is ?; Wharf et al., 1999).

For the (Mes)3SnX (X = Cl, Br or I) systems, the SnC3 pyramid is significantly flatter and Sn—C is longer by ~0.04 Å, when compared with the Ph3SnX analogues. Moreover, the Sn environment is essentially the same in all three (Mes)3SnX (X = Cl, Br or I) molecules, and it would appear that repulsions between the proximal o-CH3 groups and distal o-CH3···X interactions give a limiting geometry around Sn. Only when comparing (Mes)3SnF with (Mes)3SnCl is a further flattening of the SnC3 pyramid seen, but the effect is less than was noted earlier for the comparison of (o-Anis)3SnF with (o-Anis)3SnCl (Wharf et al., 1999).

The effect of increasing repulsion between X and distal o-CH3 groups, as Cl is replaced by Br and then I, is shown by increases in Sn—X of 0.03 Å (X = Cl) and 0.05 Å (X = Br or I) when comparing Ph3SnX with (Mes)3SnX (Table 4). The effect of distal o-CH3 groups on Sn—F is less obvious, since monomeric Ph3SnF does not exist. However, comparison with Sn—X values for (o-Anis)3SnX provides some insight. For (o-Anis)3SnX (X = Cl or I), Sn—X distances are longer (0.015–0.01 Å) than in the corresponding Ph3SnX, perhaps due to the weak Sn···OCH3 interaction trans to Sn—X in (o-Anis)3SnX, but are still shorter than Sn—X in the corresponding (Mes)3SnX molecules (Table 4). In contrast, Sn—F in (o-Anis)3SnX is longer by 0.01 Å than in (Mes)3SnF, which would suggest there is no significant repulsion between F and distal o-CH3 groups in the latter molecule. Thus, the value for Sn—F of 1.96 Å in (Mes)3SnF may well be characteristic for sterically unhindered four-coordinate Ar3SnF systems.

Experimental top

Slow evaporation of an ethanol solution of previously prepared trimesityltin chloride (Wharf & Simard, 1997) produced crystals which could be readily identified visually as two different products, (I) and (II). A suitable crystal of each type was chosen for X-ray study.

Refinement top

For both (I) and (II), H atoms were constrained to the parent site and refined using a riding model, with C—H distances in the range 0.93–0.97 Å and O—H = 0.82 Å. For (I), the H atoms of the methyl groups were found from a difference Fourier map and allowed to refine by their torsion angles. In (II), the ethanol molecule was disordered over two positions (0.50/0.50); these atoms were refined isotropically using restraints (DFIX) to model an ethanol molecule in a crystalline environment (Jonsson, 1976). For (I), a total of 20 peaks of 0.91–0.30 e Å-3 were found located at < 1.10 Å from the heavy atoms. The general background was found to be < 0.30 e Å-3. A final verification of possible voids was performed using the VOID routine of PLATON (Spek, 1995). A small hole remained in this structure, accounting for one electron and 84.3 Å3 of the volume of the cell. For (II), a final verification of possible voids was performed using the VOID routine of PLATON.

Computing details top

For both compounds, data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL96 (Sheldrick, 1996b); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL96.

Figures top
[Figure 1] Fig. 1. A view of the molecule of [SnCl(C9H11)3] in the asymmetric unit of the solvent-free compound, (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii.
[Figure 2] Fig. 2. A packing diagram for the hemisolvate, (II). For clarity, only one of the two ethanol conformations is shown.
(I) Chlorotris(2,4,6-trimethylphenyl)tin(IV) top
Crystal data top
[SnCl(C9H11)3]F(000) = 3144.0
Mr = 511.67Dx = 1.331 Mg m3
Monoclinic, P21/nCu Kα radiation, λ = 1.54178 Å
Hall symbol: -P 2ynCell parameters from 39847 reflections
a = 8.2337 (1) Åθ = 2.9–72.9°
b = 30.7435 (3) ŵ = 8.97 mm1
c = 30.3142 (2) ÅT = 293 K
β = 93.270 (1)°Needle, colourless
V = 7661.02 (13) Å30.64 × 0.05 × 0.02 mm
Z = 12
Data collection top
Bruker Platform with SMART 2K CCD area-detector
diffractometer
14917 independent reflections
Radiation source: normal-focus xray tube10064 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.072
Detector resolution: 5.5 pixels mm-1θmax = 73.0°, θmin = 2.1°
ω scansh = 97
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996a)
k = 3838
Tmin = 0.560, Tmax = 0.860l = 3737
92036 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.101H-atom parameters constrained
S = 0.94 w = 1/[σ2(Fo2) + (0.0558P)2]
where P = (Fo2 + 2Fc2)/3
14917 reflections(Δ/σ)max = 0.006
811 parametersΔρmax = 0.91 e Å3
0 restraintsΔρmin = 0.51 e Å3
Crystal data top
[SnCl(C9H11)3]V = 7661.02 (13) Å3
Mr = 511.67Z = 12
Monoclinic, P21/nCu Kα radiation
a = 8.2337 (1) ŵ = 8.97 mm1
b = 30.7435 (3) ÅT = 293 K
c = 30.3142 (2) Å0.64 × 0.05 × 0.02 mm
β = 93.270 (1)°
Data collection top
Bruker Platform with SMART 2K CCD area-detector
diffractometer
14917 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996a)
10064 reflections with I > 2σ(I)
Tmin = 0.560, Tmax = 0.860Rint = 0.072
92036 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0490 restraints
wR(F2) = 0.101H-atom parameters constrained
S = 0.94Δρmax = 0.91 e Å3
14917 reflectionsΔρmin = 0.51 e Å3
811 parameters
Special details top

Experimental. X-ray crystallographic data for (I) were collected from a single-crystal sample, which was mounted on a glass fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8 Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sn10.21562 (4)0.161877 (10)0.902503 (10)0.04779 (9)
Cl10.02552 (17)0.19358 (5)0.84934 (5)0.0789 (4)
C1110.3501 (5)0.11604 (15)0.86503 (16)0.0522 (12)
C1120.4105 (6)0.12904 (16)0.82496 (17)0.0589 (13)
C1130.4924 (6)0.09872 (18)0.80027 (17)0.0687 (15)
H1130.53060.10730.77330.082*
C1140.5189 (6)0.05686 (19)0.81420 (18)0.0669 (14)
C1150.4638 (6)0.04524 (16)0.85494 (18)0.0613 (13)
H1150.48330.01720.86550.074*
C1160.3807 (5)0.07406 (15)0.88028 (16)0.0510 (12)
C1170.3951 (7)0.17486 (17)0.80751 (19)0.0893 (19)
H11A0.30410.17660.78630.134*
H11B0.49280.18270.79360.134*
H11C0.37860.19450.83150.134*
C1180.6090 (8)0.0244 (2)0.7870 (2)0.104 (2)
H11D0.62960.03700.75890.156*
H11E0.54410.00140.78260.156*
H11F0.71050.01690.80240.156*
C1190.3316 (7)0.05825 (17)0.92478 (17)0.0769 (16)
H11G0.21750.05150.92310.115*
H11H0.35330.08050.94650.115*
H11I0.39260.03260.93300.115*
C1210.0551 (5)0.13071 (14)0.94722 (16)0.0467 (11)
C1220.0707 (6)0.10491 (15)0.92887 (17)0.0543 (12)
C1230.1821 (6)0.08796 (16)0.9576 (2)0.0702 (16)
H1230.26650.07070.94580.084*
C1240.1726 (7)0.09565 (19)1.0020 (2)0.0761 (17)
C1250.0417 (7)0.11998 (17)1.01912 (19)0.0712 (15)
H1250.03020.12471.04940.085*
C1260.0724 (6)0.13741 (15)0.99229 (17)0.0545 (12)
C1270.0925 (7)0.09281 (18)0.88108 (18)0.0804 (17)
H12A0.16150.11380.86590.121*
H12B0.14160.06450.87840.121*
H12C0.01150.09230.86830.121*
C1280.3009 (8)0.0782 (2)1.0311 (2)0.124 (3)
H12D0.40390.09131.02280.186*
H12E0.27110.08491.06150.186*
H12F0.30900.04721.02760.186*
C1290.2148 (6)0.16081 (16)1.01505 (17)0.0712 (15)
H12G0.31450.14921.00500.107*
H12H0.21240.15691.04640.107*
H12I0.20830.19131.00820.107*
C1310.3473 (5)0.21801 (13)0.92714 (14)0.0451 (10)
C1320.5177 (6)0.22008 (16)0.92788 (15)0.0543 (12)
C1330.5957 (6)0.25820 (15)0.94047 (16)0.0597 (13)
H1330.70840.25950.94000.072*
C1340.5131 (6)0.29435 (15)0.95368 (15)0.0538 (12)
C1350.3454 (6)0.29157 (15)0.95445 (15)0.0552 (12)
H1350.28760.31540.96400.066*
C1360.2609 (5)0.25402 (15)0.94127 (15)0.0496 (11)
C1370.6220 (6)0.18206 (17)0.9169 (2)0.0872 (19)
H13A0.63700.18170.88580.131*
H13B0.56990.15560.92520.131*
H13C0.72580.18450.93280.131*
C1380.6020 (6)0.33518 (15)0.96694 (18)0.0741 (16)
H13D0.70520.32790.98140.111*
H13E0.53880.35150.98680.111*
H13F0.61890.35230.94110.111*
C1390.0774 (5)0.25415 (16)0.94432 (18)0.0689 (15)
H13G0.02590.25760.91530.103*
H13H0.04670.27780.96280.103*
H13I0.04360.22710.95680.103*
Sn21.01692 (4)0.390945 (10)0.090275 (10)0.04566 (9)
Cl21.18339 (17)0.39000 (5)0.02832 (4)0.0721 (4)
C2111.1981 (5)0.39518 (15)0.14497 (14)0.0479 (11)
C2121.3095 (6)0.42925 (16)0.14492 (16)0.0538 (12)
C2131.4208 (6)0.43356 (17)0.18103 (17)0.0623 (14)
H2131.49690.45590.18090.075*
C2141.4227 (7)0.4064 (2)0.21669 (18)0.0686 (15)
C2151.3090 (7)0.37355 (17)0.21632 (17)0.0654 (15)
H2151.30780.35500.24060.078*
C2161.1954 (6)0.36692 (16)0.18106 (16)0.0547 (12)
C2171.3165 (6)0.46254 (17)0.10848 (17)0.0706 (15)
H21A1.37440.48780.11940.106*
H21B1.20790.47070.09850.106*
H21C1.37150.45030.08430.106*
C2181.5442 (8)0.4123 (2)0.25633 (19)0.115 (3)
H21D1.56190.44280.26160.173*
H21E1.64540.39860.25030.173*
H21F1.50160.39920.28200.173*
C2191.0732 (7)0.33099 (17)0.18462 (17)0.0744 (16)
H21G0.96800.34330.18880.112*
H21H1.10480.31270.20930.112*
H21I1.06860.31400.15800.112*
C2210.8863 (5)0.33032 (14)0.08085 (14)0.0469 (11)
C2220.9680 (6)0.29253 (16)0.07035 (14)0.0527 (12)
C2230.8797 (6)0.25498 (16)0.06012 (15)0.0567 (13)
H2230.93540.23020.05200.068*
C2240.7136 (7)0.25304 (17)0.06160 (17)0.0625 (14)
C2250.6346 (6)0.28972 (17)0.07372 (17)0.0672 (15)
H2250.52240.28860.07570.081*
C2260.7153 (6)0.32885 (16)0.08326 (16)0.0586 (13)
C2271.1511 (6)0.28906 (16)0.07147 (17)0.0666 (14)
H22A1.18360.26030.08070.100*
H22B1.19820.31000.09190.100*
H22C1.18780.29460.04250.100*
C2280.6193 (7)0.21201 (17)0.0517 (2)0.0919 (19)
H22D0.61970.19430.07780.138*
H22E0.66880.19630.02860.138*
H22F0.50930.21920.04230.138*
C2290.6157 (6)0.36709 (19)0.0974 (2)0.091 (2)
H22G0.66230.37850.12470.136*
H22H0.50620.35780.10130.136*
H22I0.61550.38930.07510.136*
C2310.8733 (5)0.44974 (15)0.08546 (17)0.0532 (12)
C2320.8383 (5)0.47154 (16)0.12432 (18)0.0579 (13)
C2330.7478 (6)0.50963 (17)0.1214 (2)0.0680 (15)
H2330.72680.52430.14730.082*
C2340.6881 (6)0.52646 (17)0.0820 (2)0.0750 (17)
C2350.7193 (7)0.50466 (19)0.0442 (2)0.0804 (18)
H2350.67810.51560.01720.097*
C2360.8122 (6)0.46608 (18)0.04476 (19)0.0670 (14)
C2370.8876 (6)0.45485 (19)0.17007 (17)0.0798 (17)
H23A0.85600.42490.17240.120*
H23B0.83460.47180.19170.120*
H23C1.00330.45730.17520.120*
C2380.5849 (8)0.56740 (18)0.0803 (3)0.121 (3)
H23D0.47320.55980.08370.181*
H23E0.59450.58160.05230.181*
H23F0.62180.58670.10370.181*
C2390.8363 (8)0.4435 (2)0.00130 (19)0.102 (2)
H23G0.94390.44930.00780.153*
H23H0.75760.45400.02070.153*
H23I0.82270.41270.00490.153*
Sn30.99350 (4)0.883231 (11)0.756542 (11)0.06317 (11)
Cl31.1704 (3)0.93787 (6)0.73092 (6)0.1273 (7)
C3111.1546 (6)0.82899 (17)0.76827 (17)0.0642 (14)
C3121.1527 (8)0.8053 (2)0.8072 (2)0.0901 (19)
C3131.2613 (10)0.7716 (2)0.8140 (2)0.114 (3)
H3131.26120.75610.84040.137*
C3141.3689 (10)0.7601 (3)0.7835 (3)0.119 (3)
C3151.3678 (8)0.7825 (3)0.7452 (3)0.110 (2)
H3151.43990.77460.72400.132*
C3161.2599 (8)0.8174 (2)0.7365 (2)0.0868 (19)
C3171.0328 (10)0.8129 (2)0.8420 (2)0.155 (4)
H31A1.03920.78940.86290.233*
H31B0.92480.81420.82830.233*
H31C1.05770.83980.85690.233*
C3181.4878 (12)0.7224 (3)0.7919 (3)0.205 (5)
H31D1.43000.69530.78900.307*
H31E1.53790.72480.82110.307*
H31F1.57000.72340.77070.307*
C3191.2614 (9)0.8387 (2)0.6909 (2)0.132 (3)
H31G1.32710.86450.69290.198*
H31H1.15230.84620.68090.198*
H31I1.30590.81880.67050.198*
C3210.8183 (6)0.87686 (16)0.70163 (16)0.0605 (13)
C3220.7823 (6)0.83734 (17)0.68065 (17)0.0635 (14)
C3230.6768 (7)0.83684 (18)0.64348 (18)0.0735 (16)
H3230.65360.81040.62960.088*
C3240.6045 (6)0.87416 (19)0.62620 (17)0.0656 (14)
C3250.6380 (7)0.91228 (19)0.64814 (18)0.0734 (16)
H3250.58750.93770.63780.088*
C3260.7439 (7)0.91452 (17)0.68507 (17)0.0696 (15)
C3270.8487 (8)0.79392 (17)0.6975 (2)0.101 (2)
H32A0.95730.79010.68830.152*
H32B0.78070.77080.68580.152*
H32C0.85000.79340.72920.152*
C3280.4889 (7)0.8726 (2)0.58571 (18)0.097 (2)
H32D0.39300.85670.59240.146*
H32E0.54100.85840.56210.146*
H32F0.45930.90160.57690.146*
C3290.7662 (10)0.95860 (19)0.7074 (2)0.122 (3)
H32G0.72750.95720.73670.183*
H32H0.70570.98020.69050.183*
H32I0.87940.96620.70910.183*
C3310.8996 (6)0.91061 (16)0.81569 (15)0.0578 (13)
C3320.9996 (7)0.9350 (2)0.84499 (18)0.0745 (16)
C3330.9380 (7)0.95170 (19)0.88306 (18)0.0789 (17)
H3331.00470.96890.90170.095*
C3340.7809 (8)0.94354 (18)0.89414 (19)0.0712 (15)
C3350.6851 (7)0.91958 (19)0.8654 (2)0.0745 (16)
H3350.57810.91420.87210.089*
C3360.7397 (7)0.90289 (17)0.82656 (18)0.0666 (14)
C3371.1798 (8)0.9427 (3)0.8385 (2)0.145 (3)
H33A1.19170.96700.81910.217*
H33B1.22590.91720.82590.217*
H33C1.23530.94880.86660.217*
C3380.7212 (8)0.9613 (2)0.93708 (19)0.098 (2)
H33D0.62000.97630.93120.147*
H33E0.80040.98110.95000.147*
H33F0.70570.93770.95720.147*
C3390.6232 (8)0.8759 (2)0.7974 (2)0.115 (3)
H33G0.67890.85080.78700.173*
H33H0.58290.89310.77270.173*
H33I0.53380.86670.81420.173*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.04165 (18)0.04644 (18)0.0556 (2)0.00072 (13)0.00605 (13)0.00066 (15)
Cl10.0727 (9)0.0892 (10)0.0730 (9)0.0107 (7)0.0113 (7)0.0135 (8)
C1110.048 (3)0.049 (3)0.059 (3)0.004 (2)0.004 (2)0.003 (2)
C1120.055 (3)0.055 (3)0.067 (3)0.000 (2)0.009 (3)0.005 (3)
C1130.073 (4)0.077 (4)0.057 (3)0.001 (3)0.013 (3)0.007 (3)
C1140.063 (4)0.072 (4)0.066 (4)0.006 (3)0.001 (3)0.020 (3)
C1150.051 (3)0.051 (3)0.081 (4)0.005 (2)0.001 (3)0.006 (3)
C1160.038 (3)0.054 (3)0.062 (3)0.002 (2)0.007 (2)0.004 (2)
C1170.111 (5)0.068 (4)0.093 (5)0.012 (3)0.045 (4)0.021 (3)
C1180.121 (6)0.099 (5)0.094 (5)0.039 (4)0.015 (4)0.030 (4)
C1190.078 (4)0.062 (4)0.093 (4)0.019 (3)0.024 (3)0.016 (3)
C1210.035 (3)0.045 (3)0.061 (3)0.0042 (19)0.008 (2)0.002 (2)
C1220.046 (3)0.049 (3)0.067 (3)0.007 (2)0.002 (2)0.008 (3)
C1230.048 (3)0.054 (3)0.109 (5)0.009 (2)0.007 (3)0.014 (3)
C1240.058 (4)0.076 (4)0.096 (5)0.005 (3)0.022 (3)0.032 (4)
C1250.068 (4)0.071 (4)0.075 (4)0.007 (3)0.011 (3)0.015 (3)
C1260.049 (3)0.046 (3)0.069 (4)0.005 (2)0.007 (2)0.002 (3)
C1270.069 (4)0.085 (4)0.086 (4)0.021 (3)0.008 (3)0.026 (3)
C1280.089 (5)0.142 (7)0.145 (7)0.019 (5)0.042 (5)0.052 (5)
C1290.078 (4)0.072 (4)0.062 (3)0.004 (3)0.004 (3)0.002 (3)
C1310.038 (3)0.042 (3)0.056 (3)0.0015 (19)0.006 (2)0.002 (2)
C1320.046 (3)0.055 (3)0.062 (3)0.012 (2)0.009 (2)0.001 (2)
C1330.034 (3)0.054 (3)0.091 (4)0.003 (2)0.006 (2)0.003 (3)
C1340.054 (3)0.048 (3)0.059 (3)0.005 (2)0.002 (2)0.004 (2)
C1350.051 (3)0.047 (3)0.068 (3)0.008 (2)0.005 (2)0.006 (2)
C1360.037 (3)0.057 (3)0.055 (3)0.004 (2)0.006 (2)0.006 (2)
C1370.052 (4)0.069 (4)0.141 (6)0.015 (3)0.008 (3)0.030 (4)
C1380.070 (4)0.056 (3)0.095 (4)0.014 (3)0.004 (3)0.004 (3)
C1390.043 (3)0.062 (3)0.103 (4)0.009 (2)0.016 (3)0.009 (3)
Sn20.04028 (18)0.04885 (18)0.04758 (18)0.00109 (13)0.00010 (12)0.00485 (14)
Cl20.0714 (9)0.0885 (10)0.0579 (8)0.0015 (7)0.0178 (6)0.0036 (7)
C2110.037 (3)0.061 (3)0.045 (3)0.003 (2)0.0004 (19)0.009 (2)
C2120.043 (3)0.062 (3)0.056 (3)0.009 (2)0.002 (2)0.002 (3)
C2130.049 (3)0.068 (4)0.068 (4)0.001 (2)0.009 (2)0.010 (3)
C2140.057 (4)0.088 (4)0.059 (4)0.017 (3)0.010 (3)0.007 (3)
C2150.072 (4)0.070 (4)0.053 (3)0.024 (3)0.002 (3)0.007 (3)
C2160.046 (3)0.060 (3)0.059 (3)0.011 (2)0.010 (2)0.002 (3)
C2170.061 (4)0.075 (4)0.074 (4)0.014 (3)0.008 (3)0.004 (3)
C2180.100 (5)0.164 (7)0.076 (5)0.012 (5)0.042 (4)0.007 (4)
C2190.086 (4)0.076 (4)0.062 (4)0.005 (3)0.013 (3)0.016 (3)
C2210.040 (3)0.050 (3)0.050 (3)0.002 (2)0.0015 (19)0.008 (2)
C2220.047 (3)0.065 (3)0.047 (3)0.004 (2)0.002 (2)0.001 (2)
C2230.058 (3)0.053 (3)0.060 (3)0.000 (2)0.005 (2)0.011 (2)
C2240.068 (4)0.053 (3)0.065 (4)0.014 (3)0.006 (3)0.002 (3)
C2250.043 (3)0.070 (4)0.087 (4)0.009 (3)0.009 (3)0.000 (3)
C2260.041 (3)0.061 (3)0.074 (4)0.007 (2)0.001 (2)0.004 (3)
C2270.053 (3)0.065 (3)0.082 (4)0.007 (3)0.011 (3)0.005 (3)
C2280.086 (4)0.066 (4)0.123 (5)0.023 (3)0.004 (4)0.006 (4)
C2290.043 (4)0.075 (4)0.155 (6)0.008 (3)0.013 (3)0.018 (4)
C2310.041 (3)0.051 (3)0.066 (3)0.002 (2)0.003 (2)0.000 (3)
C2320.038 (3)0.058 (3)0.077 (4)0.003 (2)0.002 (2)0.009 (3)
C2330.052 (3)0.059 (4)0.093 (4)0.001 (3)0.005 (3)0.015 (3)
C2340.049 (3)0.047 (3)0.129 (6)0.001 (2)0.010 (3)0.004 (4)
C2350.065 (4)0.073 (4)0.100 (5)0.007 (3)0.013 (3)0.027 (4)
C2360.055 (3)0.074 (4)0.071 (4)0.004 (3)0.009 (3)0.003 (3)
C2370.068 (4)0.101 (5)0.069 (4)0.018 (3)0.005 (3)0.021 (3)
C2380.091 (5)0.064 (4)0.208 (8)0.028 (4)0.019 (5)0.025 (5)
C2390.108 (5)0.127 (6)0.068 (4)0.018 (4)0.019 (4)0.004 (4)
Sn30.0735 (3)0.0646 (2)0.0512 (2)0.00186 (18)0.00168 (17)0.00781 (17)
Cl30.1759 (19)0.1199 (15)0.0874 (12)0.0653 (14)0.0199 (12)0.0184 (11)
C3110.065 (4)0.069 (4)0.058 (3)0.011 (3)0.003 (3)0.001 (3)
C3120.107 (5)0.089 (5)0.074 (4)0.035 (4)0.006 (4)0.006 (4)
C3130.153 (7)0.101 (6)0.087 (5)0.051 (5)0.006 (5)0.001 (4)
C3140.117 (7)0.107 (6)0.129 (7)0.052 (5)0.024 (6)0.016 (5)
C3150.084 (5)0.127 (7)0.118 (6)0.034 (5)0.006 (4)0.032 (5)
C3160.072 (4)0.112 (5)0.076 (5)0.010 (4)0.002 (3)0.010 (4)
C3170.211 (9)0.147 (7)0.114 (6)0.100 (7)0.073 (6)0.072 (5)
C3180.230 (11)0.179 (10)0.201 (10)0.148 (9)0.020 (8)0.024 (8)
C3190.131 (7)0.187 (8)0.081 (5)0.019 (6)0.047 (5)0.007 (5)
C3210.074 (4)0.055 (3)0.051 (3)0.012 (3)0.005 (3)0.003 (2)
C3220.069 (4)0.059 (3)0.062 (3)0.013 (3)0.001 (3)0.003 (3)
C3230.074 (4)0.070 (4)0.075 (4)0.007 (3)0.006 (3)0.008 (3)
C3240.063 (4)0.081 (4)0.052 (3)0.011 (3)0.002 (3)0.002 (3)
C3250.082 (4)0.074 (4)0.064 (4)0.027 (3)0.003 (3)0.014 (3)
C3260.103 (4)0.058 (3)0.049 (3)0.020 (3)0.005 (3)0.006 (3)
C3270.116 (5)0.053 (4)0.130 (6)0.021 (3)0.034 (4)0.001 (4)
C3280.095 (5)0.120 (5)0.073 (4)0.011 (4)0.025 (4)0.002 (4)
C3290.202 (8)0.064 (4)0.096 (5)0.040 (5)0.039 (5)0.020 (4)
C3310.060 (3)0.065 (3)0.048 (3)0.002 (3)0.001 (2)0.003 (2)
C3320.057 (4)0.103 (5)0.064 (4)0.012 (3)0.004 (3)0.002 (3)
C3330.081 (4)0.091 (5)0.064 (4)0.019 (3)0.001 (3)0.004 (3)
C3340.077 (4)0.065 (4)0.072 (4)0.016 (3)0.013 (3)0.003 (3)
C3350.050 (4)0.092 (5)0.082 (4)0.002 (3)0.009 (3)0.006 (3)
C3360.062 (4)0.070 (4)0.068 (4)0.007 (3)0.000 (3)0.006 (3)
C3370.083 (5)0.259 (10)0.094 (5)0.064 (6)0.014 (4)0.055 (6)
C3380.108 (5)0.093 (5)0.095 (5)0.019 (4)0.033 (4)0.007 (4)
C3390.089 (5)0.152 (7)0.104 (5)0.051 (5)0.002 (4)0.023 (5)
Geometric parameters (Å, º) top
Sn1—C1312.149 (4)C225—C2261.397 (6)
Sn1—C1112.155 (5)C225—H2250.9300
Sn1—C1212.169 (4)C226—C2291.509 (6)
Sn1—Cl12.3896 (13)C227—H22A0.9600
C111—C1161.389 (6)C227—H22B0.9600
C111—C1121.397 (6)C227—H22C0.9600
C112—C1131.393 (6)C228—H22D0.9600
C112—C1171.508 (7)C228—H22E0.9600
C113—C1141.368 (7)C228—H22F0.9600
C113—H1130.9300C229—H22G0.9600
C114—C1151.387 (7)C229—H22H0.9600
C114—C1181.516 (7)C229—H22I0.9600
C115—C1161.379 (6)C231—C2361.399 (6)
C115—H1150.9300C231—C2321.400 (6)
C116—C1191.511 (6)C232—C2331.388 (6)
C117—H11A0.9600C232—C2371.512 (7)
C117—H11B0.9600C233—C2341.368 (7)
C117—H11C0.9600C233—H2330.9300
C118—H11D0.9600C234—C2351.365 (8)
C118—H11E0.9600C234—C2381.518 (7)
C118—H11F0.9600C235—C2361.411 (7)
C119—H11G0.9600C235—H2350.9300
C119—H11H0.9600C236—C2391.513 (7)
C119—H11I0.9600C237—H23A0.9600
C121—C1261.381 (6)C237—H23B0.9600
C121—C1221.395 (6)C237—H23C0.9600
C122—C1231.401 (6)C238—H23D0.9600
C122—C1271.497 (7)C238—H23E0.9600
C123—C1241.366 (8)C238—H23F0.9600
C123—H1230.9300C239—H23G0.9600
C124—C1251.388 (8)C239—H23H0.9600
C124—C1281.513 (7)C239—H23I0.9600
C125—C1261.385 (6)Sn3—C3112.148 (5)
C125—H1250.9300Sn3—C3212.149 (5)
C126—C1291.509 (6)Sn3—C3312.163 (5)
C127—H12A0.9600Sn3—Cl32.3824 (16)
C127—H12B0.9600C311—C3161.378 (7)
C127—H12C0.9600C311—C3121.388 (7)
C128—H12D0.9600C312—C3131.377 (8)
C128—H12E0.9600C312—C3171.503 (8)
C128—H12F0.9600C313—C3141.364 (9)
C129—H12G0.9600C313—H3130.9300
C129—H12H0.9600C314—C3151.349 (9)
C129—H12I0.9600C314—C3181.530 (9)
C131—C1361.397 (6)C315—C3161.408 (8)
C131—C1321.403 (6)C315—H3150.9300
C132—C1331.379 (6)C316—C3191.531 (8)
C132—C1371.499 (6)C317—H31A0.9600
C133—C1341.374 (6)C317—H31B0.9600
C133—H1330.9300C317—H31C0.9600
C134—C1351.385 (6)C318—H31D0.9600
C134—C1381.496 (6)C318—H31E0.9600
C135—C1361.395 (6)C318—H31F0.9600
C135—H1350.9300C319—H31G0.9600
C136—C1391.519 (6)C319—H31H0.9600
C137—H13A0.9600C319—H31I0.9600
C137—H13B0.9600C321—C3261.390 (6)
C137—H13C0.9600C321—C3221.395 (6)
C138—H13D0.9600C322—C3231.383 (7)
C138—H13E0.9600C322—C3271.520 (6)
C138—H13F0.9600C323—C3241.382 (7)
C139—H13G0.9600C323—H3230.9300
C139—H13H0.9600C324—C3251.368 (7)
C139—H13I0.9600C324—C3281.511 (7)
Sn2—C2312.160 (5)C325—C3261.381 (7)
Sn2—C2212.163 (4)C325—H3250.9300
Sn2—C2112.170 (4)C326—C3291.521 (7)
Sn2—Cl22.3875 (13)C327—H32A0.9600
C211—C2121.392 (6)C327—H32B0.9600
C211—C2161.398 (6)C327—H32C0.9600
C212—C2131.393 (6)C328—H32D0.9600
C212—C2171.509 (6)C328—H32E0.9600
C213—C2141.366 (7)C328—H32F0.9600
C213—H2130.9300C329—H32G0.9600
C214—C2151.376 (7)C329—H32H0.9600
C214—C2181.530 (7)C329—H32I0.9600
C215—C2161.395 (6)C331—C3361.395 (7)
C215—H2150.9300C331—C3321.395 (7)
C216—C2191.502 (6)C332—C3331.385 (7)
C217—H21A0.9600C332—C3371.526 (7)
C217—H21B0.9600C333—C3341.378 (7)
C217—H21C0.9600C333—H3330.9300
C218—H21D0.9600C334—C3351.359 (7)
C218—H21E0.9600C334—C3381.519 (7)
C218—H21F0.9600C335—C3361.382 (7)
C219—H21G0.9600C335—H3350.9300
C219—H21H0.9600C336—C3391.514 (7)
C219—H21I0.9600C337—H33A0.9600
C221—C2221.389 (6)C337—H33B0.9600
C221—C2261.415 (6)C337—H33C0.9600
C222—C2231.390 (6)C338—H33D0.9600
C222—C2271.509 (6)C338—H33E0.9600
C223—C2241.372 (6)C338—H33F0.9600
C223—H2230.9300C339—H33G0.9600
C224—C2251.363 (7)C339—H33H0.9600
C224—C2281.503 (6)C339—H33I0.9600
C131—Sn1—C111116.35 (16)C225—C226—C221118.7 (4)
C131—Sn1—C121116.80 (17)C225—C226—C229118.1 (4)
C111—Sn1—C121112.96 (17)C221—C226—C229123.2 (5)
C131—Sn1—Cl1101.83 (12)C222—C227—H22A109.5
C111—Sn1—Cl1104.34 (13)C222—C227—H22B109.5
C121—Sn1—Cl1101.70 (12)H22A—C227—H22B109.5
C116—C111—C112119.2 (4)C222—C227—H22C109.5
C116—C111—Sn1121.4 (3)H22A—C227—H22C109.5
C112—C111—Sn1119.4 (3)H22B—C227—H22C109.5
C113—C112—C111118.9 (5)C224—C228—H22D109.5
C113—C112—C117118.1 (5)C224—C228—H22E109.5
C111—C112—C117123.0 (4)H22D—C228—H22E109.5
C114—C113—C112122.5 (5)C224—C228—H22F109.5
C114—C113—H113118.8H22D—C228—H22F109.5
C112—C113—H113118.8H22E—C228—H22F109.5
C113—C114—C115117.6 (5)C226—C229—H22G109.5
C113—C114—C118121.8 (5)C226—C229—H22H109.5
C115—C114—C118120.7 (5)H22G—C229—H22H109.5
C116—C115—C114121.9 (5)C226—C229—H22I109.5
C116—C115—H115119.0H22G—C229—H22I109.5
C114—C115—H115119.0H22H—C229—H22I109.5
C115—C116—C111119.9 (5)C236—C231—C232119.3 (5)
C115—C116—C119117.2 (5)C236—C231—Sn2121.9 (4)
C111—C116—C119122.9 (4)C232—C231—Sn2118.8 (4)
C112—C117—H11A109.5C233—C232—C231119.1 (5)
C112—C117—H11B109.5C233—C232—C237117.3 (5)
H11A—C117—H11B109.5C231—C232—C237123.5 (5)
C112—C117—H11C109.5C234—C233—C232122.7 (5)
H11A—C117—H11C109.5C234—C233—H233118.7
H11B—C117—H11C109.5C232—C233—H233118.7
C114—C118—H11D109.5C235—C234—C233118.2 (5)
C114—C118—H11E109.5C235—C234—C238120.7 (6)
H11D—C118—H11E109.5C233—C234—C238121.1 (6)
C114—C118—H11F109.5C234—C235—C236122.0 (6)
H11D—C118—H11F109.5C234—C235—H235119.0
H11E—C118—H11F109.5C236—C235—H235119.0
C116—C119—H11G109.5C231—C236—C235118.7 (5)
C116—C119—H11H109.5C231—C236—C239123.0 (5)
H11G—C119—H11H109.5C235—C236—C239118.3 (5)
C116—C119—H11I109.5C232—C237—H23A109.5
H11G—C119—H11I109.5C232—C237—H23B109.5
H11H—C119—H11I109.5H23A—C237—H23B109.5
C126—C121—C122120.8 (4)C232—C237—H23C109.5
C126—C121—Sn1121.3 (3)H23A—C237—H23C109.5
C122—C121—Sn1117.8 (4)H23B—C237—H23C109.5
C121—C122—C123117.5 (5)C234—C238—H23D109.5
C121—C122—C127125.0 (5)C234—C238—H23E109.5
C123—C122—C127117.5 (5)H23D—C238—H23E109.5
C124—C123—C122123.1 (5)C234—C238—H23F109.5
C124—C123—H123118.5H23D—C238—H23F109.5
C122—C123—H123118.5H23E—C238—H23F109.5
C123—C124—C125117.5 (5)C236—C239—H23G109.5
C123—C124—C128120.8 (6)C236—C239—H23H109.5
C125—C124—C128121.8 (6)H23G—C239—H23H109.5
C126—C125—C124121.8 (6)C236—C239—H23I109.5
C126—C125—H125119.1H23G—C239—H23I109.5
C124—C125—H125119.1H23H—C239—H23I109.5
C121—C126—C125119.2 (5)C311—Sn3—C321116.00 (19)
C121—C126—C129123.9 (4)C311—Sn3—C331114.30 (19)
C125—C126—C129116.8 (5)C321—Sn3—C331114.95 (19)
C122—C127—H12A109.5C311—Sn3—Cl3102.59 (16)
C122—C127—H12B109.5C321—Sn3—Cl3101.99 (15)
H12A—C127—H12B109.5C331—Sn3—Cl3104.47 (15)
C122—C127—H12C109.5C316—C311—C312119.7 (5)
H12A—C127—H12C109.5C316—C311—Sn3119.5 (4)
H12B—C127—H12C109.5C312—C311—Sn3120.8 (4)
C124—C128—H12D109.5C313—C312—C311119.0 (6)
C124—C128—H12E109.5C313—C312—C317117.3 (6)
H12D—C128—H12E109.5C311—C312—C317123.7 (5)
C124—C128—H12F109.5C314—C313—C312122.2 (7)
H12D—C128—H12F109.5C314—C313—H313118.9
H12E—C128—H12F109.5C312—C313—H313118.9
C126—C129—H12G109.5C315—C314—C313118.8 (7)
C126—C129—H12H109.5C315—C314—C318120.1 (8)
H12G—C129—H12H109.5C313—C314—C318121.1 (8)
C126—C129—H12I109.5C314—C315—C316121.4 (7)
H12G—C129—H12I109.5C314—C315—H315119.3
H12H—C129—H12I109.5C316—C315—H315119.3
C136—C131—C132119.1 (4)C311—C316—C315118.9 (6)
C136—C131—Sn1119.1 (3)C311—C316—C319123.8 (6)
C132—C131—Sn1121.8 (3)C315—C316—C319117.2 (6)
C133—C132—C131119.5 (4)C312—C317—H31A109.5
C133—C132—C137117.4 (4)C312—C317—H31B109.5
C131—C132—C137123.1 (4)H31A—C317—H31B109.5
C134—C133—C132122.5 (4)C312—C317—H31C109.5
C134—C133—H133118.7H31A—C317—H31C109.5
C132—C133—H133118.7H31B—C317—H31C109.5
C133—C134—C135117.7 (4)C314—C318—H31D109.5
C133—C134—C138121.0 (5)C314—C318—H31E109.5
C135—C134—C138121.3 (4)H31D—C318—H31E109.5
C134—C135—C136121.9 (4)C314—C318—H31F109.5
C134—C135—H135119.1H31D—C318—H31F109.5
C136—C135—H135119.1H31E—C318—H31F109.5
C135—C136—C131119.3 (4)C316—C319—H31G109.5
C135—C136—C139117.5 (4)C316—C319—H31H109.5
C131—C136—C139123.2 (4)H31G—C319—H31H109.5
C132—C137—H13A109.5C316—C319—H31I109.5
C132—C137—H13B109.5H31G—C319—H31I109.5
H13A—C137—H13B109.5H31H—C319—H31I109.5
C132—C137—H13C109.5C326—C321—C322118.9 (5)
H13A—C137—H13C109.5C326—C321—Sn3117.8 (4)
H13B—C137—H13C109.5C322—C321—Sn3123.3 (4)
C134—C138—H13D109.5C323—C322—C321119.2 (5)
C134—C138—H13E109.5C323—C322—C327117.5 (5)
H13D—C138—H13E109.5C321—C322—C327123.2 (5)
C134—C138—H13F109.5C324—C323—C322122.4 (5)
H13D—C138—H13F109.5C324—C323—H323118.8
H13E—C138—H13F109.5C322—C323—H323118.8
C136—C139—H13G109.5C325—C324—C323117.2 (5)
C136—C139—H13H109.5C325—C324—C328121.5 (5)
H13G—C139—H13H109.5C323—C324—C328121.2 (5)
C136—C139—H13I109.5C324—C325—C326122.5 (5)
H13G—C139—H13I109.5C324—C325—H325118.7
H13H—C139—H13I109.5C326—C325—H325118.7
C231—Sn2—C221116.48 (16)C325—C326—C321119.7 (5)
C231—Sn2—C211110.56 (17)C325—C326—C329117.4 (5)
C221—Sn2—C211117.89 (17)C321—C326—C329122.8 (5)
C231—Sn2—Cl2107.07 (13)C322—C327—H32A109.5
C221—Sn2—Cl2100.91 (12)C322—C327—H32B109.5
C211—Sn2—Cl2101.61 (12)H32A—C327—H32B109.5
C212—C211—C216120.5 (4)C322—C327—H32C109.5
C212—C211—Sn2117.9 (3)H32A—C327—H32C109.5
C216—C211—Sn2121.3 (3)H32B—C327—H32C109.5
C211—C212—C213118.3 (5)C324—C328—H32D109.5
C211—C212—C217124.3 (4)C324—C328—H32E109.5
C213—C212—C217117.4 (5)H32D—C328—H32E109.5
C214—C213—C212122.8 (5)C324—C328—H32F109.5
C214—C213—H213118.6H32D—C328—H32F109.5
C212—C213—H213118.6H32E—C328—H32F109.5
C213—C214—C215117.7 (5)C326—C329—H32G109.5
C213—C214—C218121.7 (6)C326—C329—H32H109.5
C215—C214—C218120.5 (5)H32G—C329—H32H109.5
C214—C215—C216122.7 (5)C326—C329—H32I109.5
C214—C215—H215118.7H32G—C329—H32I109.5
C216—C215—H215118.7H32H—C329—H32I109.5
C215—C216—C211118.0 (5)C336—C331—C332118.1 (5)
C215—C216—C219118.4 (5)C336—C331—Sn3121.1 (4)
C211—C216—C219123.6 (4)C332—C331—Sn3120.7 (4)
C212—C217—H21A109.5C333—C332—C331119.9 (5)
C212—C217—H21B109.5C333—C332—C337117.0 (5)
H21A—C217—H21B109.5C331—C332—C337123.0 (5)
C212—C217—H21C109.5C334—C333—C332122.0 (5)
H21A—C217—H21C109.5C334—C333—H333119.0
H21B—C217—H21C109.5C332—C333—H333119.0
C214—C218—H21D109.5C335—C334—C333117.4 (5)
C214—C218—H21E109.5C335—C334—C338122.7 (6)
H21D—C218—H21E109.5C333—C334—C338119.8 (6)
C214—C218—H21F109.5C334—C335—C336122.8 (5)
H21D—C218—H21F109.5C334—C335—H335118.6
H21E—C218—H21F109.5C336—C335—H335118.6
C216—C219—H21G109.5C335—C336—C331119.7 (5)
C216—C219—H21H109.5C335—C336—C339118.2 (5)
H21G—C219—H21H109.5C331—C336—C339122.1 (5)
C216—C219—H21I109.5C332—C337—H33A109.5
H21G—C219—H21I109.5C332—C337—H33B109.5
H21H—C219—H21I109.5H33A—C337—H33B109.5
C222—C221—C226118.8 (4)C332—C337—H33C109.5
C222—C221—Sn2120.5 (3)H33A—C337—H33C109.5
C226—C221—Sn2120.7 (3)H33B—C337—H33C109.5
C221—C222—C223119.5 (4)C334—C338—H33D109.5
C221—C222—C227123.4 (4)C334—C338—H33E109.5
C223—C222—C227117.1 (4)H33D—C338—H33E109.5
C224—C223—C222122.6 (5)C334—C338—H33F109.5
C224—C223—H223118.7H33D—C338—H33F109.5
C222—C223—H223118.7H33E—C338—H33F109.5
C225—C224—C223117.7 (5)C336—C339—H33G109.5
C225—C224—C228119.9 (5)C336—C339—H33H109.5
C223—C224—C228122.3 (5)H33G—C339—H33H109.5
C224—C225—C226122.7 (5)C336—C339—H33I109.5
C224—C225—H225118.7H33G—C339—H33I109.5
C226—C225—H225118.7H33H—C339—H33I109.5
C131—Sn1—C111—C116114.8 (4)C227—C222—C223—C224174.5 (5)
C121—Sn1—C111—C11624.4 (4)C222—C223—C224—C2250.1 (8)
Cl1—Sn1—C111—C116134.0 (4)C222—C223—C224—C228178.3 (5)
C131—Sn1—C111—C11264.0 (4)C223—C224—C225—C2261.9 (8)
C121—Sn1—C111—C112156.9 (4)C228—C224—C225—C226179.9 (5)
Cl1—Sn1—C111—C11247.3 (4)C224—C225—C226—C2210.9 (8)
C116—C111—C112—C1133.4 (7)C224—C225—C226—C229178.6 (5)
Sn1—C111—C112—C113177.8 (4)C222—C221—C226—C2251.8 (7)
C116—C111—C112—C117175.0 (5)Sn2—C221—C226—C225175.3 (4)
Sn1—C111—C112—C1173.8 (7)C222—C221—C226—C229175.7 (5)
C111—C112—C113—C1141.4 (8)Sn2—C221—C226—C2297.2 (7)
C117—C112—C113—C114177.1 (5)C221—Sn2—C231—C23675.3 (4)
C112—C113—C114—C1151.3 (8)C211—Sn2—C231—C236146.6 (4)
C112—C113—C114—C118179.7 (5)Cl2—Sn2—C231—C23636.7 (4)
C113—C114—C115—C1161.9 (8)C221—Sn2—C231—C232103.6 (4)
C118—C114—C115—C116179.7 (5)C211—Sn2—C231—C23234.6 (4)
C114—C115—C116—C1110.1 (7)Cl2—Sn2—C231—C232144.4 (3)
C114—C115—C116—C119178.0 (5)C236—C231—C232—C2331.9 (7)
C112—C111—C116—C1152.8 (7)Sn2—C231—C232—C233179.2 (3)
Sn1—C111—C116—C115178.4 (3)C236—C231—C232—C237175.3 (5)
C112—C111—C116—C119175.2 (5)Sn2—C231—C232—C2373.6 (6)
Sn1—C111—C116—C1193.6 (6)C231—C232—C233—C2341.3 (8)
C131—Sn1—C121—C12619.3 (4)C237—C232—C233—C234176.0 (5)
C111—Sn1—C121—C126119.6 (4)C232—C233—C234—C2350.1 (8)
Cl1—Sn1—C121—C126129.1 (3)C232—C233—C234—C238178.0 (5)
C131—Sn1—C121—C122158.2 (3)C233—C234—C235—C2360.9 (8)
C111—Sn1—C121—C12262.8 (4)C238—C234—C235—C236178.8 (5)
Cl1—Sn1—C121—C12248.4 (3)C232—C231—C236—C2351.1 (7)
C126—C121—C122—C1232.9 (7)Sn2—C231—C236—C235180.0 (4)
Sn1—C121—C122—C123174.6 (3)C232—C231—C236—C239176.7 (5)
C126—C121—C122—C127175.0 (5)Sn2—C231—C236—C2392.1 (7)
Sn1—C121—C122—C1277.4 (6)C234—C235—C236—C2310.3 (8)
C121—C122—C123—C1240.1 (7)C234—C235—C236—C239178.2 (5)
C127—C122—C123—C124178.2 (5)C321—Sn3—C311—C31662.6 (5)
C122—C123—C124—C1252.7 (8)C331—Sn3—C311—C316160.1 (4)
C122—C123—C124—C128177.2 (5)Cl3—Sn3—C311—C31647.6 (5)
C123—C124—C125—C1262.4 (8)C321—Sn3—C311—C312116.7 (5)
C128—C124—C125—C126177.5 (5)C331—Sn3—C311—C31220.6 (6)
C122—C121—C126—C1253.2 (7)Cl3—Sn3—C311—C312133.1 (5)
Sn1—C121—C126—C125174.2 (3)C316—C311—C312—C3132.6 (10)
C122—C121—C126—C129173.2 (4)Sn3—C311—C312—C313178.0 (5)
Sn1—C121—C126—C1299.3 (6)C316—C311—C312—C317174.4 (7)
C124—C125—C126—C1210.5 (7)Sn3—C311—C312—C3174.9 (10)
C124—C125—C126—C129176.2 (5)C311—C312—C313—C3141.2 (12)
C111—Sn1—C131—C136163.4 (3)C317—C312—C313—C314176.0 (8)
C121—Sn1—C131—C13659.1 (4)C312—C313—C314—C3150.5 (13)
Cl1—Sn1—C131—C13650.6 (4)C312—C313—C314—C318179.7 (8)
C111—Sn1—C131—C13214.2 (4)C313—C314—C315—C3160.8 (13)
C121—Sn1—C131—C132123.3 (4)C318—C314—C315—C316180.0 (7)
Cl1—Sn1—C131—C132126.9 (4)C312—C311—C316—C3152.4 (9)
C136—C131—C132—C1333.1 (7)Sn3—C311—C316—C315178.3 (5)
Sn1—C131—C132—C133174.5 (4)C312—C311—C316—C319174.4 (6)
C136—C131—C132—C137174.9 (5)Sn3—C311—C316—C3194.9 (9)
Sn1—C131—C132—C1377.5 (7)C314—C315—C316—C3110.7 (11)
C131—C132—C133—C1341.9 (8)C314—C315—C316—C319176.4 (7)
C137—C132—C133—C134176.2 (5)C311—Sn3—C321—C326162.2 (4)
C132—C133—C134—C1350.5 (8)C331—Sn3—C321—C32660.7 (5)
C132—C133—C134—C138179.8 (5)Cl3—Sn3—C321—C32651.7 (4)
C133—C134—C135—C1361.7 (7)C311—Sn3—C321—C32214.4 (5)
C138—C134—C135—C136178.6 (5)C331—Sn3—C321—C322122.6 (4)
C134—C135—C136—C1310.4 (7)Cl3—Sn3—C321—C322125.0 (4)
C134—C135—C136—C139178.8 (4)C326—C321—C322—C3231.5 (8)
C132—C131—C136—C1352.0 (7)Sn3—C321—C322—C323175.2 (4)
Sn1—C131—C136—C135175.7 (3)C326—C321—C322—C327176.3 (5)
C132—C131—C136—C139176.3 (4)Sn3—C321—C322—C3277.1 (8)
Sn1—C131—C136—C1396.1 (6)C321—C322—C323—C3240.2 (9)
C231—Sn2—C211—C21258.2 (4)C327—C322—C323—C324177.6 (5)
C221—Sn2—C211—C212164.3 (3)C322—C323—C324—C3251.7 (9)
Cl2—Sn2—C211—C21255.2 (3)C322—C323—C324—C328179.6 (5)
C231—Sn2—C211—C216116.5 (4)C323—C324—C325—C3262.5 (9)
C221—Sn2—C211—C21621.0 (4)C328—C324—C325—C326179.6 (5)
Cl2—Sn2—C211—C216130.1 (3)C324—C325—C326—C3211.3 (9)
C216—C211—C212—C2131.9 (7)C324—C325—C326—C329177.9 (6)
Sn2—C211—C212—C213176.7 (3)C322—C321—C326—C3250.7 (8)
C216—C211—C212—C217177.0 (4)Sn3—C321—C326—C325176.1 (4)
Sn2—C211—C212—C2172.3 (6)C322—C321—C326—C329175.7 (6)
C211—C212—C213—C2141.3 (7)Sn3—C321—C326—C3297.5 (8)
C217—C212—C213—C214177.7 (5)C311—Sn3—C331—C336104.7 (4)
C212—C213—C214—C2150.1 (8)C321—Sn3—C331—C33633.1 (5)
C212—C213—C214—C218178.9 (5)Cl3—Sn3—C331—C336144.0 (4)
C213—C214—C215—C2160.9 (8)C311—Sn3—C331—C33272.6 (5)
C218—C214—C215—C216179.7 (5)C321—Sn3—C331—C332149.6 (4)
C214—C215—C216—C2110.3 (7)Cl3—Sn3—C331—C33238.7 (4)
C214—C215—C216—C219178.1 (5)C336—C331—C332—C3331.6 (8)
C212—C211—C216—C2151.1 (7)Sn3—C331—C332—C333178.9 (4)
Sn2—C211—C216—C215175.7 (3)C336—C331—C332—C337175.2 (6)
C212—C211—C216—C219176.6 (4)Sn3—C331—C332—C3372.2 (8)
Sn2—C211—C216—C2192.0 (6)C331—C332—C333—C3342.6 (9)
C231—Sn2—C221—C222160.9 (3)C337—C332—C333—C334174.3 (6)
C211—Sn2—C221—C22264.1 (4)C332—C333—C334—C3352.3 (9)
Cl2—Sn2—C221—C22245.4 (4)C332—C333—C334—C338177.8 (5)
C231—Sn2—C221—C22616.2 (4)C333—C334—C335—C3361.1 (9)
C211—Sn2—C221—C226118.8 (4)C338—C334—C335—C336179.1 (5)
Cl2—Sn2—C221—C226131.7 (4)C334—C335—C336—C3310.1 (9)
C226—C221—C222—C2233.5 (7)C334—C335—C336—C339178.8 (6)
Sn2—C221—C222—C223173.6 (3)C332—C331—C336—C3350.4 (8)
C226—C221—C222—C227173.4 (4)Sn3—C331—C336—C335177.7 (4)
Sn2—C221—C222—C2279.5 (6)C332—C331—C336—C339178.5 (6)
C221—C222—C223—C2242.6 (7)Sn3—C331—C336—C3391.2 (7)
(II) Chlorotris(2,4,6-trimethylphenyl)tin(IV) ethanol hemisolvate top
Crystal data top
[SnCl(C9H11)3]·0.5C2H6OZ = 4
Mr = 534.71F(000) = 1100
Triclinic, P1Dx = 1.319 Mg m3
Hall symbol: -P 1Cu Kα radiation, λ = 1.54178 Å
a = 8.2564 (1) ÅCell parameters from 18284 reflections
b = 16.8363 (1) Åθ = 2.3–72.9°
c = 19.5759 (1) ŵ = 8.55 mm1
α = 94.996 (1)°T = 293 K
β = 96.568 (1)°Block, colourless
γ = 90.539 (1)°0.20 × 0.18 × 0.15 mm
V = 2692.54 (4) Å3
Data collection top
Bruker Platform with SMART 2K CCD area-detector
diffractometer
10291 independent reflections
Radiation source: normal-focus sealed tube7198 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
Detector resolution: 5.5 pixels mm-1θmax = 72.9°, θmin = 2.3°
ω scansh = 1010
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996a)
k = 1720
Tmin = 0.160, Tmax = 0.277l = 2424
32709 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 0.94 w = 1/[σ2(Fo2) + (0.0621P)2]
where P = (Fo2 + 2Fc2)/3
10291 reflections(Δ/σ)max = 0.002
565 parametersΔρmax = 0.96 e Å3
6 restraintsΔρmin = 0.40 e Å3
Crystal data top
[SnCl(C9H11)3]·0.5C2H6Oγ = 90.539 (1)°
Mr = 534.71V = 2692.54 (4) Å3
Triclinic, P1Z = 4
a = 8.2564 (1) ÅCu Kα radiation
b = 16.8363 (1) ŵ = 8.55 mm1
c = 19.5759 (1) ÅT = 293 K
α = 94.996 (1)°0.20 × 0.18 × 0.15 mm
β = 96.568 (1)°
Data collection top
Bruker Platform with SMART 2K CCD area-detector
diffractometer
10291 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996a)
7198 reflections with I > 2σ(I)
Tmin = 0.160, Tmax = 0.277Rint = 0.037
32709 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0466 restraints
wR(F2) = 0.115H-atom parameters constrained
S = 0.94Δρmax = 0.96 e Å3
10291 reflectionsΔρmin = 0.40 e Å3
565 parameters
Special details top

Experimental. X-ray crystallographic data for (II) were collected from a single-crystal sample, which was mounted on a glass fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8 Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn10.12279 (4)0.579048 (18)0.243899 (15)0.04721 (10)
Cl10.15971 (17)0.59857 (10)0.25488 (8)0.0847 (5)
C1110.1851 (5)0.6793 (3)0.1888 (2)0.0490 (11)
C1120.1372 (6)0.7558 (3)0.2102 (3)0.0551 (12)
C1130.1692 (7)0.8175 (3)0.1706 (3)0.0699 (16)
H1130.13660.86860.18450.084*
C1140.2465 (7)0.8071 (3)0.1121 (3)0.0666 (15)
C1150.2959 (6)0.7317 (3)0.0934 (3)0.0647 (14)
H1150.34870.72300.05400.078*
C1160.2698 (6)0.6677 (3)0.1315 (3)0.0526 (12)
C1170.0560 (7)0.7744 (3)0.2752 (3)0.0797 (18)
H11A0.05930.76450.26520.120*
H11B0.07590.82940.29170.120*
H11C0.10000.74120.30990.120*
C1180.2836 (8)0.8757 (3)0.0704 (3)0.095 (2)
H11D0.39910.87960.06850.142*
H11E0.24640.92450.09180.142*
H11F0.22890.86610.02440.142*
C1190.3439 (7)0.5891 (3)0.1100 (3)0.0715 (16)
H11G0.25920.54910.09870.107*
H11H0.41940.57350.14730.107*
H11I0.40030.59460.07040.107*
C1210.1088 (5)0.4637 (2)0.1847 (2)0.0446 (10)
C1220.0018 (6)0.4535 (3)0.1236 (2)0.0495 (11)
C1230.0211 (6)0.3778 (3)0.0902 (3)0.0569 (12)
H1230.09020.37090.04900.068*
C1240.0553 (6)0.3119 (3)0.1157 (3)0.0595 (13)
C1250.1659 (7)0.3245 (3)0.1732 (3)0.0603 (13)
H1250.22260.28130.18950.072*
C1260.1965 (6)0.3988 (3)0.2078 (2)0.0520 (11)
C1270.0897 (6)0.5211 (3)0.0913 (3)0.0681 (14)
H12A0.11210.50810.04240.102*
H12B0.02450.56920.10020.102*
H12C0.19050.52870.11080.102*
C1280.0156 (8)0.2290 (3)0.0794 (3)0.0825 (18)
H12D0.09960.21850.07660.124*
H12E0.07330.18990.10510.124*
H12F0.04800.22640.03370.124*
C1290.3274 (7)0.4051 (3)0.2687 (3)0.0798 (17)
H12G0.37010.45880.27630.120*
H12H0.41370.36940.25940.120*
H12I0.28170.39120.30910.120*
C1310.2303 (6)0.5821 (3)0.3498 (2)0.0520 (11)
C1320.3695 (6)0.6295 (3)0.3740 (3)0.0635 (14)
C1330.4272 (7)0.6339 (4)0.4434 (3)0.0754 (16)
H1330.51770.66640.45940.090*
C1340.3555 (8)0.5919 (4)0.4897 (3)0.0819 (18)
C1350.2238 (8)0.5439 (4)0.4645 (3)0.0821 (18)
H1350.17540.51430.49500.098*
C1360.1588 (7)0.5373 (3)0.3951 (3)0.0646 (14)
C1370.4623 (7)0.6746 (4)0.3269 (3)0.0825 (18)
H13A0.47040.64190.28480.124*
H13B0.56970.68820.34930.124*
H13C0.40570.72250.31660.124*
C1380.4222 (9)0.5993 (5)0.5655 (3)0.121 (3)
H13D0.43550.54710.58130.181*
H13E0.34750.62860.59180.181*
H13F0.52580.62690.57150.181*
C1390.0164 (8)0.4807 (4)0.3743 (3)0.091 (2)
H13G0.01970.43960.40540.137*
H13H0.02180.45710.32820.137*
H13I0.08340.50930.37600.137*
Sn20.74145 (4)0.078734 (19)0.242534 (16)0.05293 (11)
Cl21.03059 (17)0.09686 (11)0.25147 (9)0.0985 (5)
C2110.7157 (6)0.0368 (3)0.1860 (2)0.0485 (11)
C2120.6386 (6)0.1000 (3)0.2110 (2)0.0582 (13)
C2130.6516 (6)0.1773 (3)0.1792 (3)0.0629 (14)
H2130.60240.21970.19680.075*
C2140.7361 (6)0.1922 (3)0.1221 (3)0.0583 (13)
C2150.8006 (6)0.1279 (3)0.0952 (3)0.0566 (12)
H2150.85050.13640.05500.068*
C2160.7940 (6)0.0505 (3)0.1259 (2)0.0532 (12)
C2170.5371 (7)0.0903 (3)0.2706 (3)0.0843 (19)
H21A0.60750.08630.31340.126*
H21B0.46490.13560.26890.126*
H21C0.47430.04280.26750.126*
C2180.7576 (8)0.2764 (3)0.0918 (3)0.0817 (18)
H21D0.86900.29130.10230.123*
H21E0.73020.27940.04260.123*
H21F0.68740.31190.11110.123*
C2190.8718 (7)0.0146 (3)0.0922 (3)0.0775 (17)
H21G0.81690.06370.10130.116*
H21H0.86360.00090.04330.116*
H21I0.98460.02080.11050.116*
C2210.6560 (6)0.1796 (3)0.1889 (2)0.0518 (11)
C2220.5419 (6)0.1715 (3)0.1298 (3)0.0570 (13)
C2230.4971 (7)0.2379 (3)0.0961 (3)0.0655 (14)
H2230.42310.23180.05640.079*
C2240.5588 (7)0.3131 (3)0.1196 (3)0.0666 (15)
C2250.6675 (7)0.3208 (3)0.1779 (3)0.0691 (16)
H2250.70920.37130.19430.083*
C2260.7183 (6)0.2558 (3)0.2138 (3)0.0618 (14)
C2270.4558 (7)0.0933 (3)0.1031 (3)0.0809 (18)
H22A0.37690.10170.06460.121*
H22B0.40170.07310.13910.121*
H22C0.53410.05550.08880.121*
C2280.5031 (8)0.3849 (3)0.0831 (3)0.093 (2)
H22D0.53080.37900.03660.140*
H22E0.55580.43210.10700.140*
H22F0.38710.38940.08230.140*
C2290.8352 (8)0.2713 (3)0.2797 (3)0.088 (2)
H22G0.94490.26240.26950.133*
H22H0.80860.23590.31280.133*
H22I0.82580.32550.29830.133*
C2310.6915 (6)0.0826 (3)0.3487 (2)0.0592 (13)
C2320.7876 (7)0.0379 (4)0.3950 (3)0.0724 (16)
C2330.7576 (9)0.0432 (4)0.4637 (3)0.0885 (19)
H2330.81810.01210.49390.106*
C2340.6433 (9)0.0920 (4)0.4886 (3)0.0853 (19)
C2350.5464 (8)0.1329 (4)0.4422 (3)0.0820 (18)
H2350.46330.16400.45790.098*
C2360.5686 (7)0.1293 (3)0.3729 (3)0.0664 (14)
C2370.9161 (9)0.0193 (4)0.3737 (3)0.102 (2)
H23A0.88410.04270.32750.153*
H23B0.92780.06060.40470.153*
H23C1.01830.00890.37530.153*
C2380.6189 (10)0.0977 (5)0.5646 (3)0.126 (3)
H23D0.58640.04650.57680.188*
H23E0.53570.13560.57310.188*
H23F0.71920.11480.59190.188*
C2390.4485 (7)0.1741 (4)0.3250 (3)0.093 (2)
H23G0.50480.21730.30830.139*
H23H0.36250.19480.35010.139*
H23I0.40310.13820.28670.139*
C10.886 (4)0.742 (2)0.5695 (10)0.304 (18)*0.50
H1A0.90490.69600.59530.456*0.50
H1B0.77360.74270.55120.456*0.50
H1C0.91450.78940.59920.456*0.50
C20.991 (3)0.737 (2)0.5109 (12)0.26 (3)*0.50
H2A1.07630.77770.52010.309*0.50
H2B1.04240.68540.50790.309*0.50
O30.896 (3)0.7476 (19)0.4469 (10)0.323 (13)*0.50
H30.94530.77780.42540.485*0.50
C40.881 (4)0.6774 (15)0.4571 (17)0.282 (17)*0.50
H4A0.87470.67600.40770.423*0.50
H4B0.77380.68620.47100.423*0.50
H4C0.92050.62760.47190.423*0.50
C50.995 (3)0.744 (2)0.490 (2)0.29 (3)*0.50
H5A1.08550.72250.51740.353*0.50
H5B1.03800.77130.45360.353*0.50
O60.914 (3)0.8006 (13)0.5318 (15)0.332 (13)*0.50
H60.86920.77720.55980.498*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.05002 (19)0.0475 (2)0.04422 (18)0.00201 (13)0.00962 (14)0.00112 (13)
Cl10.0566 (8)0.1072 (12)0.0924 (11)0.0131 (8)0.0230 (8)0.0000 (9)
C1110.049 (3)0.042 (3)0.053 (3)0.003 (2)0.005 (2)0.005 (2)
C1120.051 (3)0.054 (3)0.055 (3)0.005 (2)0.010 (2)0.007 (2)
C1130.065 (4)0.044 (3)0.092 (5)0.005 (2)0.025 (3)0.002 (3)
C1140.064 (3)0.046 (3)0.084 (4)0.008 (2)0.018 (3)0.016 (3)
C1150.061 (3)0.060 (4)0.073 (4)0.010 (3)0.007 (3)0.010 (3)
C1160.057 (3)0.040 (3)0.061 (3)0.002 (2)0.005 (2)0.007 (2)
C1170.095 (5)0.065 (4)0.073 (4)0.025 (3)0.004 (3)0.015 (3)
C1180.102 (5)0.067 (4)0.114 (5)0.017 (3)0.018 (4)0.043 (4)
C1190.088 (4)0.056 (3)0.079 (4)0.007 (3)0.042 (3)0.009 (3)
C1210.052 (3)0.038 (3)0.045 (3)0.0009 (19)0.016 (2)0.0012 (18)
C1220.054 (3)0.043 (3)0.052 (3)0.001 (2)0.010 (2)0.005 (2)
C1230.061 (3)0.054 (3)0.056 (3)0.008 (2)0.013 (2)0.000 (2)
C1240.067 (3)0.048 (3)0.066 (3)0.009 (2)0.029 (3)0.008 (2)
C1250.077 (4)0.051 (3)0.058 (3)0.010 (2)0.026 (3)0.010 (2)
C1260.063 (3)0.052 (3)0.044 (3)0.006 (2)0.015 (2)0.007 (2)
C1270.074 (4)0.060 (4)0.067 (4)0.003 (3)0.006 (3)0.003 (3)
C1280.099 (5)0.050 (4)0.099 (5)0.015 (3)0.034 (4)0.015 (3)
C1290.097 (5)0.082 (4)0.057 (3)0.033 (3)0.006 (3)0.004 (3)
C1310.059 (3)0.055 (3)0.042 (3)0.004 (2)0.008 (2)0.002 (2)
C1320.058 (3)0.065 (4)0.066 (4)0.012 (3)0.003 (3)0.001 (3)
C1330.071 (4)0.082 (4)0.067 (4)0.004 (3)0.007 (3)0.008 (3)
C1340.092 (5)0.105 (5)0.046 (3)0.018 (4)0.001 (3)0.004 (3)
C1350.101 (5)0.098 (5)0.049 (3)0.008 (4)0.019 (3)0.004 (3)
C1360.074 (4)0.066 (4)0.053 (3)0.005 (3)0.012 (3)0.005 (2)
C1370.058 (4)0.101 (5)0.088 (5)0.014 (3)0.004 (3)0.018 (4)
C1380.126 (7)0.180 (8)0.048 (4)0.016 (6)0.014 (4)0.007 (4)
C1390.112 (5)0.104 (5)0.059 (4)0.036 (4)0.021 (4)0.007 (3)
Sn20.0507 (2)0.0543 (2)0.0520 (2)0.00476 (14)0.00234 (15)0.00032 (15)
Cl20.0496 (8)0.1244 (15)0.1185 (14)0.0138 (8)0.0015 (8)0.0054 (11)
C2110.054 (3)0.047 (3)0.044 (3)0.004 (2)0.001 (2)0.005 (2)
C2120.058 (3)0.070 (4)0.044 (3)0.011 (2)0.002 (2)0.008 (2)
C2130.071 (4)0.057 (3)0.058 (3)0.016 (3)0.012 (3)0.015 (2)
C2140.061 (3)0.044 (3)0.064 (3)0.005 (2)0.016 (3)0.001 (2)
C2150.061 (3)0.056 (3)0.052 (3)0.012 (2)0.000 (2)0.007 (2)
C2160.056 (3)0.049 (3)0.056 (3)0.010 (2)0.006 (2)0.015 (2)
C2170.097 (5)0.092 (5)0.066 (4)0.038 (4)0.026 (3)0.004 (3)
C2180.091 (4)0.050 (4)0.097 (5)0.009 (3)0.014 (4)0.005 (3)
C2190.105 (5)0.060 (4)0.076 (4)0.005 (3)0.040 (3)0.014 (3)
C2210.058 (3)0.043 (3)0.056 (3)0.000 (2)0.016 (2)0.002 (2)
C2220.052 (3)0.042 (3)0.077 (4)0.003 (2)0.013 (3)0.001 (2)
C2230.065 (3)0.061 (4)0.071 (4)0.011 (3)0.012 (3)0.011 (3)
C2240.080 (4)0.048 (3)0.080 (4)0.012 (3)0.039 (3)0.010 (3)
C2250.084 (4)0.046 (3)0.082 (4)0.007 (3)0.042 (3)0.005 (3)
C2260.062 (3)0.058 (3)0.067 (3)0.012 (2)0.028 (3)0.011 (3)
C2270.079 (4)0.051 (4)0.103 (5)0.001 (3)0.029 (3)0.003 (3)
C2280.114 (5)0.062 (4)0.116 (5)0.015 (4)0.054 (4)0.024 (4)
C2290.107 (5)0.077 (4)0.077 (4)0.034 (4)0.012 (4)0.021 (3)
C2310.063 (3)0.064 (3)0.047 (3)0.010 (3)0.004 (2)0.007 (2)
C2320.076 (4)0.081 (4)0.055 (3)0.003 (3)0.006 (3)0.006 (3)
C2330.100 (5)0.104 (5)0.057 (4)0.003 (4)0.007 (4)0.002 (3)
C2340.095 (5)0.109 (6)0.050 (4)0.023 (4)0.010 (3)0.006 (3)
C2350.079 (4)0.094 (5)0.073 (4)0.016 (3)0.026 (3)0.014 (3)
C2360.065 (3)0.067 (4)0.067 (4)0.013 (3)0.013 (3)0.003 (3)
C2370.113 (6)0.113 (6)0.076 (5)0.042 (4)0.005 (4)0.009 (4)
C2380.148 (7)0.173 (8)0.057 (4)0.036 (6)0.034 (4)0.012 (4)
C2390.072 (4)0.123 (6)0.089 (5)0.018 (4)0.024 (4)0.018 (4)
Geometric parameters (Å, º) top
Sn1—C1312.156 (5)C213—C2141.390 (7)
Sn1—C1212.168 (4)C213—H2130.9300
Sn1—C1112.169 (4)C214—C2151.372 (7)
Sn1—Cl12.3898 (14)C214—C2181.508 (7)
C111—C1161.388 (6)C215—C2161.391 (6)
C111—C1121.395 (6)C215—H2150.9300
C112—C1131.390 (7)C216—C2191.503 (6)
C112—C1171.516 (7)C217—H21A0.9600
C113—C1141.371 (8)C217—H21B0.9600
C113—H1130.9300C217—H21C0.9600
C114—C1151.370 (7)C218—H21D0.9600
C114—C1181.520 (7)C218—H21E0.9600
C115—C1161.391 (6)C218—H21F0.9600
C115—H1150.9300C219—H21G0.9600
C116—C1191.511 (6)C219—H21H0.9600
C117—H11A0.9600C219—H21I0.9600
C117—H11B0.9600C221—C2221.402 (7)
C117—H11C0.9600C221—C2261.403 (6)
C118—H11D0.9600C222—C2231.379 (7)
C118—H11E0.9600C222—C2271.514 (6)
C118—H11F0.9600C223—C2241.381 (7)
C119—H11G0.9600C223—H2230.9300
C119—H11H0.9600C224—C2251.365 (8)
C119—H11I0.9600C224—C2281.507 (7)
C121—C1261.396 (6)C225—C2261.395 (7)
C121—C1221.399 (6)C225—H2250.9300
C122—C1231.383 (6)C226—C2291.521 (7)
C122—C1271.516 (6)C227—H22A0.9600
C123—C1241.384 (7)C227—H22B0.9600
C123—H1230.9300C227—H22C0.9600
C124—C1251.365 (7)C228—H22D0.9600
C124—C1281.526 (6)C228—H22E0.9600
C125—C1261.376 (7)C228—H22F0.9600
C125—H1250.9300C229—H22G0.9600
C126—C1291.511 (7)C229—H22H0.9600
C127—H12A0.9600C229—H22I0.9600
C127—H12B0.9600C231—C2361.390 (7)
C127—H12C0.9600C231—C2321.408 (7)
C128—H12D0.9600C232—C2331.391 (8)
C128—H12E0.9600C232—C2371.509 (8)
C128—H12F0.9600C233—C2341.361 (9)
C129—H12G0.9600C233—H2330.9300
C129—H12H0.9600C234—C2351.375 (9)
C129—H12I0.9600C234—C2381.520 (8)
C131—C1361.389 (7)C235—C2361.387 (7)
C131—C1321.405 (7)C235—H2350.9300
C132—C1331.383 (7)C236—C2391.534 (8)
C132—C1371.513 (7)C237—H23A0.9600
C133—C1341.377 (8)C237—H23B0.9600
C133—H1330.9300C237—H23C0.9600
C134—C1351.368 (8)C238—H23D0.9600
C134—C1381.517 (7)C238—H23E0.9600
C135—C1361.399 (7)C238—H23F0.9600
C135—H1350.9300C239—H23G0.9600
C136—C1391.503 (7)C239—H23H0.9600
C137—H13A0.9600C239—H23I0.9600
C137—H13B0.9600C1—C21.508 (5)
C137—H13C0.9600C1—H1A0.9600
C138—H13D0.9600C1—H1B0.9600
C138—H13E0.9600C1—H1C0.9600
C138—H13F0.9600C2—O31.425 (5)
C139—H13G0.9600C2—H2A0.9700
C139—H13H0.9600C2—H2B0.9700
C139—H13I0.9600O3—H30.8200
Sn2—C2112.149 (4)C4—C51.511 (5)
Sn2—C2212.155 (5)C4—H4A0.9600
Sn2—C2312.160 (5)C4—H4B0.9600
Sn2—Cl22.3884 (14)C4—H4C0.9600
C211—C2121.388 (6)C5—O61.421 (5)
C211—C2161.408 (6)C5—H5A0.9700
C212—C2131.402 (7)C5—H5B0.9700
C212—C2171.512 (7)O6—H60.8200
C131—Sn1—C121116.54 (17)C214—C213—H213119.1
C131—Sn1—C111115.60 (18)C212—C213—H213119.1
C121—Sn1—C111115.62 (17)C215—C214—C213117.7 (5)
C131—Sn1—Cl1102.75 (13)C215—C214—C218121.6 (5)
C121—Sn1—Cl199.96 (12)C213—C214—C218120.7 (5)
C111—Sn1—Cl1102.74 (13)C214—C215—C216122.4 (5)
C116—C111—C112119.7 (4)C214—C215—H215118.8
C116—C111—Sn1120.5 (3)C216—C215—H215118.8
C112—C111—Sn1119.8 (4)C215—C216—C211119.2 (4)
C113—C112—C111118.0 (5)C215—C216—C219117.3 (5)
C113—C112—C117119.1 (5)C211—C216—C219123.5 (4)
C111—C112—C117122.9 (5)C212—C217—H21A109.5
C114—C113—C112123.4 (5)C212—C217—H21B109.5
C114—C113—H113118.3H21A—C217—H21B109.5
C112—C113—H113118.3C212—C217—H21C109.5
C115—C114—C113117.2 (5)H21A—C217—H21C109.5
C115—C114—C118120.1 (6)H21B—C217—H21C109.5
C113—C114—C118122.7 (6)C214—C218—H21D109.5
C114—C115—C116122.1 (5)C214—C218—H21E109.5
C114—C115—H115118.9H21D—C218—H21E109.5
C116—C115—H115118.9C214—C218—H21F109.5
C111—C116—C115119.4 (5)H21D—C218—H21F109.5
C111—C116—C119123.0 (4)H21E—C218—H21F109.5
C115—C116—C119117.4 (5)C216—C219—H21G109.5
C112—C117—H11A109.5C216—C219—H21H109.5
C112—C117—H11B109.5H21G—C219—H21H109.5
H11A—C117—H11B109.5C216—C219—H21I109.5
C112—C117—H11C109.5H21G—C219—H21I109.5
H11A—C117—H11C109.5H21H—C219—H21I109.5
H11B—C117—H11C109.5C222—C221—C226119.0 (5)
C114—C118—H11D109.5C222—C221—Sn2122.3 (3)
C114—C118—H11E109.5C226—C221—Sn2118.7 (4)
H11D—C118—H11E109.5C223—C222—C221119.6 (5)
C114—C118—H11F109.5C223—C222—C227117.4 (5)
H11D—C118—H11F109.5C221—C222—C227122.8 (5)
H11E—C118—H11F109.5C222—C223—C224122.0 (6)
C116—C119—H11G109.5C222—C223—H223119.0
C116—C119—H11H109.5C224—C223—H223119.0
H11G—C119—H11H109.5C225—C224—C223118.2 (5)
C116—C119—H11I109.5C225—C224—C228121.0 (6)
H11G—C119—H11I109.5C223—C224—C228120.7 (6)
H11H—C119—H11I109.5C224—C225—C226122.4 (5)
C126—C121—C122119.5 (4)C224—C225—H225118.8
C126—C121—Sn1121.8 (3)C226—C225—H225118.8
C122—C121—Sn1118.6 (3)C225—C226—C221118.8 (5)
C123—C122—C121118.5 (4)C225—C226—C229118.1 (5)
C123—C122—C127117.7 (4)C221—C226—C229123.0 (5)
C121—C122—C127123.8 (4)C222—C227—H22A109.5
C122—C123—C124122.3 (5)C222—C227—H22B109.5
C122—C123—H123118.8H22A—C227—H22B109.5
C124—C123—H123118.8C222—C227—H22C109.5
C125—C124—C123117.7 (5)H22A—C227—H22C109.5
C125—C124—C128122.4 (5)H22B—C227—H22C109.5
C123—C124—C128120.0 (5)C224—C228—H22D109.5
C124—C125—C126122.4 (5)C224—C228—H22E109.5
C124—C125—H125118.8H22D—C228—H22E109.5
C126—C125—H125118.8C224—C228—H22F109.5
C125—C126—C121119.2 (5)H22D—C228—H22F109.5
C125—C126—C129117.1 (5)H22E—C228—H22F109.5
C121—C126—C129123.7 (4)C226—C229—H22G109.5
C122—C127—H12A109.5C226—C229—H22H109.5
C122—C127—H12B109.5H22G—C229—H22H109.5
H12A—C127—H12B109.5C226—C229—H22I109.5
C122—C127—H12C109.5H22G—C229—H22I109.5
H12A—C127—H12C109.5H22H—C229—H22I109.5
H12B—C127—H12C109.5C236—C231—C232119.1 (5)
C124—C128—H12D109.5C236—C231—Sn2121.7 (4)
C124—C128—H12E109.5C232—C231—Sn2119.3 (4)
H12D—C128—H12E109.5C233—C232—C231118.6 (6)
C124—C128—H12F109.5C233—C232—C237117.6 (6)
H12D—C128—H12F109.5C231—C232—C237123.8 (5)
H12E—C128—H12F109.5C234—C233—C232122.8 (6)
C126—C129—H12G109.5C234—C233—H233118.6
C126—C129—H12H109.5C232—C233—H233118.6
H12G—C129—H12H109.5C233—C234—C235117.8 (6)
C126—C129—H12I109.5C233—C234—C238120.8 (7)
H12G—C129—H12I109.5C235—C234—C238121.4 (7)
H12H—C129—H12I109.5C234—C235—C236122.1 (6)
C136—C131—C132119.6 (5)C234—C235—H235118.9
C136—C131—Sn1119.2 (4)C236—C235—H235118.9
C132—C131—Sn1121.2 (4)C235—C236—C231119.5 (6)
C133—C132—C131119.0 (5)C235—C236—C239117.8 (6)
C133—C132—C137118.2 (5)C231—C236—C239122.6 (5)
C131—C132—C137122.7 (5)C232—C237—H23A109.5
C134—C133—C132122.4 (6)C232—C237—H23B109.5
C134—C133—H133118.8H23A—C237—H23B109.5
C132—C133—H133118.8C232—C237—H23C109.5
C135—C134—C133117.5 (6)H23A—C237—H23C109.5
C135—C134—C138122.0 (7)H23B—C237—H23C109.5
C133—C134—C138120.5 (7)C234—C238—H23D109.5
C134—C135—C136122.8 (6)C234—C238—H23E109.5
C134—C135—H135118.6H23D—C238—H23E109.5
C136—C135—H135118.6C234—C238—H23F109.5
C131—C136—C135118.5 (5)H23D—C238—H23F109.5
C131—C136—C139124.3 (5)H23E—C238—H23F109.5
C135—C136—C139117.1 (5)C236—C239—H23G109.5
C132—C137—H13A109.5C236—C239—H23H109.5
C132—C137—H13B109.5H23G—C239—H23H109.5
H13A—C137—H13B109.5C236—C239—H23I109.5
C132—C137—H13C109.5H23G—C239—H23I109.5
H13A—C137—H13C109.5H23H—C239—H23I109.5
H13B—C137—H13C109.5C2—C1—H1A109.5
C134—C138—H13D109.5C2—C1—H1B109.5
C134—C138—H13E109.5H1A—C1—H1B109.5
H13D—C138—H13E109.5C2—C1—H1C109.5
C134—C138—H13F109.5H1A—C1—H1C109.5
H13D—C138—H13F109.5H1B—C1—H1C109.5
H13E—C138—H13F109.5O3—C2—C1111.2 (8)
C136—C139—H13G109.5O3—C2—H2A109.4
C136—C139—H13H109.5C1—C2—H2A109.4
H13G—C139—H13H109.5O3—C2—H2B109.4
C136—C139—H13I109.5C1—C2—H2B109.4
H13G—C139—H13I109.5H2A—C2—H2B108.0
H13H—C139—H13I109.5C2—O3—H3109.5
C211—Sn2—C221117.38 (17)C5—C4—H4A109.5
C211—Sn2—C231115.39 (18)C5—C4—H4B109.5
C221—Sn2—C231114.82 (19)H4A—C4—H4B109.5
C211—Sn2—Cl299.92 (13)C5—C4—H4C109.5
C221—Sn2—Cl2102.14 (13)H4A—C4—H4C109.5
C231—Sn2—Cl2103.65 (14)H4B—C4—H4C109.5
C212—C211—C216119.3 (4)O6—C5—C4111.5 (8)
C212—C211—Sn2121.6 (4)O6—C5—H5A109.3
C216—C211—Sn2118.7 (3)C4—C5—H5A109.3
C211—C212—C213119.2 (5)O6—C5—H5B109.3
C211—C212—C217123.4 (5)C4—C5—H5B109.3
C213—C212—C217117.3 (5)H5A—C5—H5B108.0
C214—C213—C212121.9 (5)C5—O6—H6109.5
C131—Sn1—C111—C116117.3 (4)C221—Sn2—C211—C212126.7 (4)
C121—Sn1—C111—C11623.9 (4)C231—Sn2—C211—C21213.5 (4)
Cl1—Sn1—C111—C116131.6 (4)Cl2—Sn2—C211—C212123.9 (4)
C131—Sn1—C111—C11263.9 (4)C221—Sn2—C211—C21660.0 (4)
C121—Sn1—C111—C112155.0 (3)C231—Sn2—C211—C216159.7 (3)
Cl1—Sn1—C111—C11247.2 (4)Cl2—Sn2—C211—C21649.3 (4)
C116—C111—C112—C1133.3 (7)C216—C211—C212—C2135.2 (7)
Sn1—C111—C112—C113175.5 (3)Sn2—C211—C212—C213168.1 (3)
C116—C111—C112—C117175.2 (5)C216—C211—C212—C217173.7 (5)
Sn1—C111—C112—C1176.0 (6)Sn2—C211—C212—C21713.1 (7)
C111—C112—C113—C1140.5 (7)C211—C212—C213—C2141.8 (7)
C117—C112—C113—C114178.0 (5)C217—C212—C213—C214177.1 (5)
C112—C113—C114—C1151.1 (8)C212—C213—C214—C2153.1 (7)
C112—C113—C114—C118178.7 (5)C212—C213—C214—C218175.9 (5)
C113—C114—C115—C1160.1 (8)C213—C214—C215—C2164.6 (7)
C118—C114—C115—C116177.7 (5)C218—C214—C215—C216174.4 (5)
C112—C111—C116—C1154.4 (7)C214—C215—C216—C2111.3 (7)
Sn1—C111—C116—C115174.4 (3)C214—C215—C216—C219178.9 (5)
C112—C111—C116—C119172.3 (5)C212—C211—C216—C2153.7 (7)
Sn1—C111—C116—C1198.9 (7)Sn2—C211—C216—C215169.7 (3)
C114—C115—C116—C1112.7 (8)C212—C211—C216—C219176.0 (5)
C114—C115—C116—C119174.2 (5)Sn2—C211—C216—C21910.5 (6)
C131—Sn1—C121—C12614.3 (4)C211—Sn2—C221—C22221.0 (5)
C111—Sn1—C121—C126126.5 (4)C231—Sn2—C221—C222119.5 (4)
Cl1—Sn1—C121—C126124.1 (3)Cl2—Sn2—C221—C222129.1 (4)
C131—Sn1—C121—C122162.2 (3)C211—Sn2—C221—C226158.3 (3)
C111—Sn1—C121—C12256.9 (4)C231—Sn2—C221—C22661.1 (4)
Cl1—Sn1—C121—C12252.5 (3)Cl2—Sn2—C221—C22650.3 (4)
C126—C121—C122—C1234.0 (7)C226—C221—C222—C2232.1 (7)
Sn1—C121—C122—C123172.7 (3)Sn2—C221—C222—C223177.3 (4)
C126—C121—C122—C127175.4 (4)C226—C221—C222—C227173.9 (5)
Sn1—C121—C122—C1278.0 (6)Sn2—C221—C222—C2276.7 (7)
C121—C122—C123—C1241.3 (7)C221—C222—C223—C2241.4 (8)
C127—C122—C123—C124179.3 (4)C227—C222—C223—C224174.8 (5)
C122—C123—C124—C1255.0 (7)C222—C223—C224—C2250.2 (8)
C122—C123—C124—C128175.4 (4)C222—C223—C224—C228177.8 (5)
C123—C124—C125—C1263.4 (7)C223—C224—C225—C2260.4 (8)
C128—C124—C125—C126177.0 (5)C228—C224—C225—C226178.4 (5)
C124—C125—C126—C1211.7 (7)C224—C225—C226—C2210.3 (8)
C124—C125—C126—C129177.2 (5)C224—C225—C226—C229177.8 (5)
C122—C121—C126—C1255.5 (7)C222—C221—C226—C2251.5 (7)
Sn1—C121—C126—C125171.0 (3)Sn2—C221—C226—C225177.8 (4)
C122—C121—C126—C129173.4 (5)C222—C221—C226—C229176.5 (5)
Sn1—C121—C126—C12910.1 (6)Sn2—C221—C226—C2294.1 (6)
C121—Sn1—C131—C13660.4 (4)C211—Sn2—C231—C236119.9 (4)
C111—Sn1—C131—C136158.8 (4)C221—Sn2—C231—C23621.4 (5)
Cl1—Sn1—C131—C13647.7 (4)Cl2—Sn2—C231—C236132.0 (4)
C121—Sn1—C131—C132120.5 (4)C211—Sn2—C231—C23261.3 (5)
C111—Sn1—C131—C13220.3 (5)C221—Sn2—C231—C232157.4 (4)
Cl1—Sn1—C131—C132131.4 (4)Cl2—Sn2—C231—C23246.8 (4)
C136—C131—C132—C1333.6 (8)C236—C231—C232—C2331.1 (8)
Sn1—C131—C132—C133175.5 (4)Sn2—C231—C232—C233177.8 (4)
C136—C131—C132—C137174.9 (5)C236—C231—C232—C237175.5 (6)
Sn1—C131—C132—C1376.1 (7)Sn2—C231—C232—C2375.7 (8)
C131—C132—C133—C1341.6 (9)C231—C232—C233—C2342.5 (10)
C137—C132—C133—C134176.9 (6)C237—C232—C233—C234179.2 (6)
C132—C133—C134—C1350.8 (9)C232—C233—C234—C2354.8 (10)
C132—C133—C134—C138179.4 (6)C232—C233—C234—C238178.0 (6)
C133—C134—C135—C1361.4 (10)C233—C234—C235—C2363.8 (10)
C138—C134—C135—C136178.9 (6)C238—C234—C235—C236179.0 (6)
C132—C131—C136—C1353.1 (8)C234—C235—C236—C2310.5 (9)
Sn1—C131—C136—C135176.0 (4)C234—C235—C236—C239177.1 (6)
C132—C131—C136—C139176.0 (5)C232—C231—C236—C2352.0 (8)
Sn1—C131—C136—C1394.9 (7)Sn2—C231—C236—C235176.8 (4)
C134—C135—C136—C1310.6 (9)C232—C231—C236—C239174.5 (5)
C134—C135—C136—C139178.6 (6)Sn2—C231—C236—C2396.7 (7)

Experimental details

(I)(II)
Crystal data
Chemical formula[SnCl(C9H11)3][SnCl(C9H11)3]·0.5C2H6O
Mr511.67534.71
Crystal system, space groupMonoclinic, P21/nTriclinic, P1
Temperature (K)293293
a, b, c (Å)8.2337 (1), 30.7435 (3), 30.3142 (2)8.2564 (1), 16.8363 (1), 19.5759 (1)
α, β, γ (°)90, 93.270 (1), 9094.996 (1), 96.568 (1), 90.539 (1)
V3)7661.02 (13)2692.54 (4)
Z124
Radiation typeCu KαCu Kα
µ (mm1)8.978.55
Crystal size (mm)0.64 × 0.05 × 0.020.20 × 0.18 × 0.15
Data collection
DiffractometerBruker Platform with SMART 2K CCD area-detector
diffractometer
Bruker Platform with SMART 2K CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996a)
Multi-scan
(SADABS; Sheldrick, 1996a)
Tmin, Tmax0.560, 0.8600.160, 0.277
No. of measured, independent and
observed [I > 2σ(I)] reflections
92036, 14917, 10064 32709, 10291, 7198
Rint0.0720.037
(sin θ/λ)max1)0.6200.620
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.101, 0.94 0.046, 0.115, 0.94
No. of reflections1491710291
No. of parameters811565
No. of restraints06
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.91, 0.510.96, 0.40

Computer programs: SMART (Bruker, 1999), SAINT (Bruker, 1999), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL96 (Sheldrick, 1996b), SHELXTL (Bruker, 1997), SHELXL96.

Selected geometric parameters (Å, º) for (I) top
Sn1—C1312.149 (4)Sn2—C2112.170 (4)
Sn1—C1112.155 (5)Sn2—Cl22.3875 (13)
Sn1—C1212.169 (4)Sn3—C3112.148 (5)
Sn1—Cl12.3896 (13)Sn3—C3212.149 (5)
Sn2—C2312.160 (5)Sn3—C3312.163 (5)
Sn2—C2212.163 (4)Sn3—Cl32.3824 (16)
C131—Sn1—C111116.35 (16)C231—Sn2—Cl2107.07 (13)
C131—Sn1—C121116.80 (17)C221—Sn2—Cl2100.91 (12)
C111—Sn1—C121112.96 (17)C211—Sn2—Cl2101.61 (12)
C131—Sn1—Cl1101.83 (12)C311—Sn3—C321116.00 (19)
C111—Sn1—Cl1104.34 (13)C311—Sn3—C331114.30 (19)
C121—Sn1—Cl1101.70 (12)C321—Sn3—C331114.95 (19)
C231—Sn2—C221116.48 (16)C311—Sn3—Cl3102.59 (16)
C231—Sn2—C211110.56 (17)C321—Sn3—Cl3101.99 (15)
C221—Sn2—C211117.89 (17)C331—Sn3—Cl3104.47 (15)
Selected geometric parameters (Å, º) for (II) top
Sn1—C1312.156 (5)Sn2—C2112.149 (4)
Sn1—C1212.168 (4)Sn2—C2212.155 (5)
Sn1—C1112.169 (4)Sn2—C2312.160 (5)
Sn1—Cl12.3898 (14)Sn2—Cl22.3884 (14)
C131—Sn1—C121116.54 (17)C211—Sn2—C221117.38 (17)
C131—Sn1—C111115.60 (18)C211—Sn2—C231115.39 (18)
C121—Sn1—C111115.62 (17)C221—Sn2—C231114.82 (19)
C131—Sn1—Cl1102.75 (13)C211—Sn2—Cl299.92 (13)
C121—Sn1—Cl199.96 (12)C221—Sn2—Cl2102.14 (13)
C111—Sn1—Cl1102.74 (13)C231—Sn2—Cl2103.65 (14)
Averaged angles (°) around Sn in (Mes)3SnX systems top
compoundC-Sn-XC-Sn-CC-Sn-C - C-Sn-X
(Mes)3SnFa303 (1)349 (1)46 (2)
(Mes)3SnClb309 (1)345 (1)36 (2)
(Mes)3SnCl.1/2C2H5OHb306 (1)348 (1)42 (2)
(Mes)3SnBr.1/2(CH3)2COc306 (1)348 (1)42 (2)
(Mes)3SnI.1/2CDCl3d308 (1)346 (1)38 (2)
(Mes)3SnI.1/2C6H5CH3d307 (1)348 (1)41 (2)
(a) Reuter & Puff (1989); (b) This work; (c) Dakternieks et al. (2000); (d) Simard & Wharf (1994)
Averaged Sn-X distances (Å) for various Ar3SnX complexes top
ArX = FX = ClX = BrX = I
Ph2.359 (8)a2.495 (15)b2.70 (1)c
Mes1.96 (1)d2.388 (2)e2.546 (3)f2.751 (3)c
o-Anis1.972 (5)g2.371 (5)g2.713 (1)h
(a) Tse et al. (1986) and Ng (1995); (b) Preut & Huber (1979); (c) Simard & Wharf (1994); (d) Reuter & Puff (1989); (e) This work; (f) Dakternieks et al. (2000); (g) Wharf et al. (1999); (h) Howie et al. (1994)
 

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