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In the title compound, [Sn2Cl6(OH)2(H2O)2]·0.5C6H6·H2O, the benzene mol­ecule is located on a centre of inversion. The Sn atoms are in an octa­hedral environment, each coordinated by three Cl, one water and two briding hydr­oxide ligands. Two Cl atoms and the hydr­oxide groups are in the equatorial plane, whereas the third Cl atom and the water mol­ecules are located in the axial positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807049185/at2421sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807049185/at2421Isup2.hkl
Contains datablock I

CCDC reference: 667187

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.016 Å
  • H-atom completeness 46%
  • R factor = 0.040
  • wR factor = 0.107
  • Data-to-parameter ratio = 19.9

checkCIF/PLATON results

No syntax errors found



Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 577.20 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 3.00 36.03 H 1.01 5.00 5.04 Cl 35.45 6.00 212.72 O 16.00 5.00 79.99 Sn 118.71 2.00 237.42 Calculated formula weight 571.21 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 577.20 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.89 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 900 Deg. PLAT331_ALERT_2_C Small Average Phenyl C-C Dist. C1 -C3_a 1.36 Ang. PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 16 PLAT431_ALERT_2_C Short Inter HL..A Contact Cl3 .. O1 .. 3.19 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl5 .. O2 .. 3.23 Ang.
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C3 H11 Cl6 O5 Sn2 Atom count from _chemical_formula_moiety:C3 H5 Cl6 O5 Sn2 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C3 H11 Cl6 O5 Sn2 Atom count from the _atom_site data: C3 H5 Cl6 O5 Sn2 ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.892 Tmax scaled 0.443 Tmin scaled 0.404 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C3 H11 Cl6 O5 Sn2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 6.00 6.00 0.00 H 22.00 10.00 12.00 Cl 12.00 12.00 0.00 O 10.00 10.00 0.00 Sn 4.00 4.00 0.00 PLAT794_ALERT_5_G Check Predicted Bond Valency for Sn1 (4) 4.09 PLAT794_ALERT_5_G Check Predicted Bond Valency for Sn2 (4) 4.07
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 7 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check

Comment top

Recently we have reported the synthesis and structure of the SnCl4 complex with dimethylsulfide (Ruth et al., 2005) and of the adduct of Me3SnCl with Me3SnOH and H2O (Lerner et al., 2005) (Me = CH3). The structure of Me3SnCl.Me3SnOH.H2O features an array of Me3Sn units connected alternately by bridging Cl and OH ligands (Lerner et al., 2005) whereas the structure of the dimethylsulfide complex with tin tetrachloride consists of discrete [(SnCl4).(SMe2)2] molecules (Ruth et al., 2005). It is interesting to note that Me3SnCl.Me3SnOH.H2O represents an intermediate in Me3SnCl hydrolysis. Herein we report the X-ray crystal structure analysis of the HOSnCl3 complex with water which features a dimer in solid state. The synthesis of [HOSnCl3.H2O]2 was achieved by treatment of PhSnCl3 with an aqueous HCl solution as indicated in the equation below.

The asymmetric unit of the title compound contains one bis(µ-Hydroxo)-bis(aqua-trichloro-tin(iv)) molecule, a water molecule and half a benzene molecule. The latter is located on a centre of inversion. The Sn atoms are in an octahedral environment each coordinated by three Cl and one water and two briding hydroxyl ligands. Two Cl atom and the hydroxyl groups are in the equatorial plane, whereas the third Cl atom and the water molecules are located in the axial positions.

Related literature top

For related literature, see: Lerner et al. (2005); Ruth et al. (2005).

Experimental top

A solution of aqueous HCl (38%) was added at ambient temperature to a solution PhSnCl3 (50 mg) in 0.5 ml C6D6. Colourless crystals of the title compound were grown by storing this solution at ambient temperature for several days.

Refinement top

H atoms bonded to C and those of the solvent water molecule were refined with fixed individual displacement parameters [Uiso(H) = 1.2 Ueq(C,O)] using a riding model with C—H = 0.93Å and O—H = 0.88 Å. The H atoms of the hydroxyl O atoms and water O atoms bonded to Sn could not be located and were omitted from refinement.

Structure description top

Recently we have reported the synthesis and structure of the SnCl4 complex with dimethylsulfide (Ruth et al., 2005) and of the adduct of Me3SnCl with Me3SnOH and H2O (Lerner et al., 2005) (Me = CH3). The structure of Me3SnCl.Me3SnOH.H2O features an array of Me3Sn units connected alternately by bridging Cl and OH ligands (Lerner et al., 2005) whereas the structure of the dimethylsulfide complex with tin tetrachloride consists of discrete [(SnCl4).(SMe2)2] molecules (Ruth et al., 2005). It is interesting to note that Me3SnCl.Me3SnOH.H2O represents an intermediate in Me3SnCl hydrolysis. Herein we report the X-ray crystal structure analysis of the HOSnCl3 complex with water which features a dimer in solid state. The synthesis of [HOSnCl3.H2O]2 was achieved by treatment of PhSnCl3 with an aqueous HCl solution as indicated in the equation below.

The asymmetric unit of the title compound contains one bis(µ-Hydroxo)-bis(aqua-trichloro-tin(iv)) molecule, a water molecule and half a benzene molecule. The latter is located on a centre of inversion. The Sn atoms are in an octahedral environment each coordinated by three Cl and one water and two briding hydroxyl ligands. Two Cl atom and the hydroxyl groups are in the equatorial plane, whereas the third Cl atom and the water molecules are located in the axial positions.

For related literature, see: Lerner et al. (2005); Ruth et al. (2005).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. Perspective view of the title compound with the atom numbering scheme. Displacement ellipsoids are at the 50% probability level. H atoms are drawn as small spheres of arbitrary radii. The atoms with suffix A have been generated by the symmetry operator -x, -y + 1, -z + 2.
[Figure 2] Fig. 2. The formation of the title compound.
Di-µ-hydroxido-bis[aquatrichloridotin(IV)] benzene hemisolvate monohydrate top
Crystal data top
[Sn2Cl6(OH)2(H2O)2]·0.5C6H6·H2OZ = 2
Mr = 577.20F(000) = 542
Triclinic, P1Dx = 2.491 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.3682 (7) ÅCell parameters from 10632 reflections
b = 10.8299 (12) Åθ = 3.1–25.7°
c = 11.8619 (13) ŵ = 4.29 mm1
α = 74.180 (9)°T = 173 K
β = 78.048 (9)°Block, colourless
γ = 88.588 (9)°0.22 × 0.21 × 0.19 mm
V = 769.59 (15) Å3
Data collection top
Stoe IPDSII two-circle
diffractometer
2887 independent reflections
Radiation source: fine-focus sealed tube2382 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.079
ω scansθmax = 25.6°, θmin = 3.0°
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
h = 77
Tmin = 0.452, Tmax = 0.497k = 1313
11598 measured reflectionsl = 1414
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)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0647P)2 + 0.5227P]
where P = (Fo2 + 2Fc2)/3
2887 reflections(Δ/σ)max < 0.001
145 parametersΔρmax = 1.07 e Å3
0 restraintsΔρmin = 1.56 e Å3
Crystal data top
[Sn2Cl6(OH)2(H2O)2]·0.5C6H6·H2Oγ = 88.588 (9)°
Mr = 577.20V = 769.59 (15) Å3
Triclinic, P1Z = 2
a = 6.3682 (7) ÅMo Kα radiation
b = 10.8299 (12) ŵ = 4.29 mm1
c = 11.8619 (13) ÅT = 173 K
α = 74.180 (9)°0.22 × 0.21 × 0.19 mm
β = 78.048 (9)°
Data collection top
Stoe IPDSII two-circle
diffractometer
2887 independent reflections
Absorption correction: multi-scan
(MULABS; Spek, 2003; Blessing, 1995)
2382 reflections with I > 2σ(I)
Tmin = 0.452, Tmax = 0.497Rint = 0.079
11598 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0400 restraints
wR(F2) = 0.107H-atom parameters constrained
S = 1.04Δρmax = 1.07 e Å3
2887 reflectionsΔρmin = 1.56 e Å3
145 parameters
Special details top

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*/Ueq
Sn10.18222 (6)0.78127 (4)0.63209 (3)0.01735 (15)
Sn20.01184 (6)0.47034 (4)0.75109 (3)0.01833 (15)
Cl10.0470 (3)0.96136 (15)0.69735 (14)0.0272 (4)
Cl20.3898 (3)0.87397 (17)0.44209 (14)0.0298 (4)
Cl30.4706 (2)0.75927 (16)0.73589 (14)0.0248 (3)
Cl40.1403 (3)0.28184 (17)0.70417 (16)0.0337 (4)
Cl50.2737 (3)0.48558 (17)0.64389 (14)0.0270 (4)
Cl60.2008 (3)0.38714 (17)0.94412 (14)0.0302 (4)
O10.0872 (7)0.7947 (5)0.5432 (4)0.0260 (10)
O20.2802 (7)0.4640 (5)0.8379 (4)0.0257 (10)
O30.2191 (7)0.5961 (4)0.6082 (4)0.0208 (9)
O40.0274 (7)0.6559 (4)0.7707 (4)0.0190 (9)
O50.2830 (8)0.2681 (5)1.0377 (4)0.0278 (11)
H5A0.28250.32840.97580.033*
H5B0.20680.29051.09500.033*
C10.6070 (17)0.0702 (8)0.8914 (8)0.053 (3)
H10.68240.12110.81590.063*
C20.4107 (18)0.0216 (8)0.9002 (9)0.050 (2)
H20.34960.03480.83150.061*
C30.2988 (14)0.0484 (9)1.0120 (11)0.054 (3)
H30.15730.08091.02100.065*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.0166 (2)0.0156 (2)0.0180 (2)0.00007 (16)0.00268 (16)0.00222 (17)
Sn20.0197 (2)0.0152 (2)0.0189 (2)0.00060 (16)0.00191 (17)0.00422 (17)
Cl10.0309 (8)0.0194 (8)0.0307 (8)0.0043 (6)0.0049 (7)0.0075 (6)
Cl20.0268 (8)0.0334 (9)0.0215 (7)0.0035 (7)0.0020 (6)0.0001 (7)
Cl30.0207 (8)0.0288 (8)0.0256 (7)0.0002 (6)0.0085 (6)0.0061 (6)
Cl40.0428 (10)0.0222 (9)0.0397 (9)0.0073 (7)0.0092 (8)0.0145 (7)
Cl50.0219 (8)0.0339 (9)0.0287 (8)0.0006 (6)0.0057 (6)0.0139 (7)
Cl60.0320 (9)0.0292 (9)0.0229 (7)0.0082 (7)0.0043 (6)0.0033 (7)
O10.024 (2)0.031 (3)0.024 (2)0.0016 (19)0.0092 (19)0.005 (2)
O20.024 (2)0.028 (3)0.025 (2)0.0018 (19)0.0066 (19)0.006 (2)
O30.022 (2)0.019 (2)0.021 (2)0.0006 (17)0.0006 (17)0.0085 (17)
O40.019 (2)0.016 (2)0.021 (2)0.0000 (17)0.0017 (17)0.0039 (17)
O50.034 (3)0.029 (3)0.017 (2)0.007 (2)0.0055 (19)0.0013 (19)
C10.074 (7)0.029 (4)0.041 (5)0.000 (4)0.021 (5)0.011 (4)
C20.080 (7)0.031 (5)0.056 (5)0.018 (4)0.045 (5)0.016 (4)
C30.030 (4)0.039 (5)0.100 (8)0.004 (4)0.021 (5)0.025 (5)
Geometric parameters (Å, º) top
Sn1—O42.072 (4)Sn2—Cl52.4038 (17)
Sn1—O32.102 (4)O5—H5A0.8398
Sn1—O12.175 (5)O5—H5B0.8391
Sn1—Cl22.3307 (16)C1—C21.341 (14)
Sn1—Cl12.3685 (16)C1—C3i1.364 (15)
Sn1—Cl32.3876 (16)C1—H10.9500
Sn2—O42.088 (4)C2—C31.388 (15)
Sn2—O32.091 (4)C2—H20.9500
Sn2—O22.161 (5)C3—C1i1.364 (15)
Sn2—Cl42.3441 (17)C3—H30.9500
Sn2—Cl62.3537 (16)
O4—Sn1—O371.71 (16)O4—Sn2—Cl689.85 (12)
O4—Sn1—O182.67 (17)O3—Sn2—Cl6159.25 (13)
O3—Sn1—O186.18 (18)O2—Sn2—Cl686.68 (13)
O4—Sn1—Cl2160.56 (13)Cl4—Sn2—Cl6101.36 (7)
O3—Sn1—Cl291.84 (12)O4—Sn2—Cl593.53 (13)
O1—Sn1—Cl286.04 (13)O3—Sn2—Cl593.81 (13)
O4—Sn1—Cl192.10 (12)O2—Sn2—Cl5176.57 (13)
O3—Sn1—Cl1163.20 (12)Cl4—Sn2—Cl593.52 (6)
O1—Sn1—Cl187.29 (14)Cl6—Sn2—Cl596.63 (6)
Cl2—Sn1—Cl1103.15 (6)Sn2—O3—Sn1107.71 (18)
O4—Sn1—Cl395.04 (13)Sn1—O4—Sn2108.94 (18)
O3—Sn1—Cl392.68 (13)H5A—O5—H5B106.6
O1—Sn1—Cl3177.66 (13)C2—C1—C3i121.6 (9)
Cl2—Sn1—Cl396.05 (6)C2—C1—H1119.2
Cl1—Sn1—Cl393.25 (6)C3i—C1—H1119.2
O4—Sn2—O371.60 (16)C1—C2—C3118.6 (8)
O4—Sn2—O285.57 (18)C1—C2—H2120.7
O3—Sn2—O282.77 (18)C3—C2—H2120.7
O4—Sn2—Cl4165.97 (13)C1i—C3—C2119.7 (8)
O3—Sn2—Cl495.83 (13)C1i—C3—H3120.2
O2—Sn2—Cl486.68 (14)C2—C3—H3120.2
O4—Sn2—O3—Sn11.34 (18)O1—Sn1—O4—Sn289.7 (2)
O2—Sn2—O3—Sn186.4 (2)Cl2—Sn1—O4—Sn234.8 (5)
Cl4—Sn2—O3—Sn1172.27 (16)Cl1—Sn1—O4—Sn2176.74 (17)
Cl6—Sn2—O3—Sn126.3 (5)Cl3—Sn1—O4—Sn289.80 (17)
Cl5—Sn2—O3—Sn193.79 (17)O3—Sn2—O4—Sn11.36 (18)
O4—Sn1—O3—Sn21.35 (18)O2—Sn2—O4—Sn182.5 (2)
O1—Sn1—O3—Sn284.9 (2)Cl4—Sn2—O4—Sn125.8 (7)
Cl2—Sn1—O3—Sn2170.78 (17)Cl6—Sn2—O4—Sn1169.16 (17)
Cl1—Sn1—O3—Sn217.5 (6)Cl5—Sn2—O4—Sn194.21 (17)
Cl3—Sn1—O3—Sn293.08 (18)C3i—C1—C2—C32.5 (15)
O3—Sn1—O4—Sn21.36 (18)C1—C2—C3—C1i2.5 (15)
Symmetry code: (i) x+1, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5A···O20.841.882.719 (6)180
O5—H5B···O4ii0.841.972.813 (6)180
Symmetry code: (ii) x, y+1, z+2.

Experimental details

Crystal data
Chemical formula[Sn2Cl6(OH)2(H2O)2]·0.5C6H6·H2O
Mr577.20
Crystal system, space groupTriclinic, P1
Temperature (K)173
a, b, c (Å)6.3682 (7), 10.8299 (12), 11.8619 (13)
α, β, γ (°)74.180 (9), 78.048 (9), 88.588 (9)
V3)769.59 (15)
Z2
Radiation typeMo Kα
µ (mm1)4.29
Crystal size (mm)0.22 × 0.21 × 0.19
Data collection
DiffractometerStoe IPDSII two-circle
Absorption correctionMulti-scan
(MULABS; Spek, 2003; Blessing, 1995)
Tmin, Tmax0.452, 0.497
No. of measured, independent and
observed [I > 2σ(I)] reflections
11598, 2887, 2382
Rint0.079
(sin θ/λ)max1)0.608
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.040, 0.107, 1.04
No. of reflections2887
No. of parameters145
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.07, 1.56

Computer programs: X-AREA (Stoe & Cie, 2001), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP in SHELXTL-Plus (Sheldrick, 1991).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5A···O20.841.882.719 (6)179.6
O5—H5B···O4i0.841.972.813 (6)179.7
Symmetry code: (i) x, y+1, z+2.
 

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