Tetra­chlorido­(1,10-phenanthroline-κ2N,N′)tin(IV) 1,2-dichloro­ethane hemisolvate

Momeni, B.Z.; Rominger, F.; Hosseini, S.S.

doi:10.1107/S1600536809017346

metal-organic compounds

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Volume 65| Part 6| June 2009| Page m690

doi:10.1107/S1600536809017346

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Tetrachlorido(1,10-phenanthroline-κ²N,N′)tin(IV) 1,2-dichloroethane hemisolvate

Badri Z. Momeni,^a ^* Frank Rominger ^b and Simin S. Hosseini ^a

^aDepartment of Chemistry, K. N. Toosi University of Technology, PO Box 16315-1618, Tehran 15418, Iran, and ^bOrganisch-Chemisches Institut, Universität Heidelberg, Im Neuenheimer Feld 270, 69120 Heidelberg, Germany
^*Correspondence e-mail: momeni@kntu.ac.ir

(Received 30 April 2009; accepted 8 May 2009; online 29 May 2009)

The asymmetric unit of the title compound, [SnCl₄(C₁₂H₈N₂)]·0.5C₂H₄Cl₂, contains a tin complex and one disordered half-molecule of the solvent dichloroethane [occupancies 0.71 (2):0.29 (2)]. The six coordinate Sn(IV) atom adopts a distorted octahedral geometry. π–π interactions between adjacent aromatic rings [interplanar distance 3.483 (5) Å] seem to be effective in the stabilization of the crystal packing.

Related literature

For tin(IV) halide complexes with a variety of Lewis bases, see: Harrison et al. (1972 ). For 1:1 complexes of the type [SnX₄(NN)] (X = halide; NN = 1,10-phenanthroline or 2,2′-bipyridyl ligand), see: Matsubayashi & Iyoda (1977 ). For the structure of the title complex without the co-crystallized solvent, see: Su et al. (2007 ) and with co-crystallized benzene, see: Hall & Tiekink (1996 ). For the preparation of trans-[PtClMe₂(CH₂Cl)(phen)] used in the synthesis, see: Monaghan & Puddephatt (1985 ).

Experimental

Crystal data

[SnCl₄(C₁₂H₈N₂)]·0.5C₂H₄Cl₂
M_r = 490.17
Orthorhombic, P b c a
a = 14.4478 (2) Å
b = 12.3681 (1) Å
c = 18.3551 (2) Å
V = 3279.91 (6) Å³
Z = 8
Mo Kα radiation
μ = 2.37 mm⁻¹
T = 200 K
0.20 × 0.18 × 0.12 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a ) T_min = 0.649, T_max = 0.765
31457 measured reflections
3747 independent reflections
2954 reflections with I > 2σ(I)
R_int = 0.058

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.085
S = 1.05
3747 reflections
195 parameters
H-atom parameters constrained
Δρ_max = 0.43 e Å⁻³
Δρ_min = −1.16 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Sn1—N21	2.224 (3)
Sn1—N11	2.238 (3)
Sn1—Cl2	2.3333 (12)
Sn1—Cl1	2.3708 (10)
Sn1—Cl4	2.4095 (10)
Sn1—Cl3	2.4480 (10)

Data collection: SMART (Bruker, 1995 ); cell refinement: SAINT (Bruker, 1995); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008b ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809017346/hg2511sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809017346/hg2511Isup2.hkl

checkCIF report

Comment top

It has long been known that tin(IV) halides form complexes with a variety of Lewis bases (Harrison et al., 1972). Bidentate diimine ligandes are one of the strongest bases towards tin(IV) halides and more often form 1:1 complexes of the type [SnX₄(NN)] (X = halide; NN = diimine ligand). Among them, the 1,10-phenanthroline and 2,2'-bipyridyl ligands are of particular interest (Matsubayashi & Iyoda, 1977). The title compound reported here, an adventitious result of our work on organoplatinum complexes, has a distorted octahedral geometry including different Sn—Cl and Sn—N bond lengths (see Fig. 1). The Cl3—Sn—Cl4 geometry shows remarkable deviation from linearity with a bond angle of 170.32 (4)°. The contraction of N11—Sn1—N21 to 74.7 (1) from the ideal 90° is typical for a chelating phenanthroline ligand. Figure 2 depicts the π-π interaction between adjacent aromatic rings, which seems, among Cl···Cl van der Waals contacts, to be significant in the stabilization of the crystal packing, as both preliminary structure determinations of the same complex, either without cocrystallized solvent (Su et al., 2007) or with co-crystallized benzene (Hall & Tiekink, 1996) show the same intermolecular contact features.

Related literature top

For tin(IV) halide complexes with a variety of Lewis bases, see: Harrison et al. (1972). For 1:1 complexes of the type [SnX₄(NN)] (X = halide; NN = 1,10-phenanthroline or 2,2'-bipyridyl ligand, see: Matsubayashi & Iyoda (1977). For the structure of the title complex without cocrystallized solvent, Su et al. (2007) and with co-crystallized benzene, see: Hall & Tiekink (1996). For the preparation of trans-[PtClMe₂{CH₂Cl}(phen)] used in the synthesis, see: Monaghan & Puddephatt (1985).

Experimental top

A solution of SnCl₂*2H₂O (40 mg, 0.18 mmol) in THF (1 ml) and a solution of PPh₃ (26 mg, 0.10 mmol) in dichloromethane (1 ml) were added to a dichloromethane solution (10 ml) of cis- and trans-[PtClMe₂{CH₂Cl}(phen)] (50 mg, 0.10 mmol) (Monaghan & Puddephatt, 1985) under Argon atmosphere. The reaction mixture was stirred for 3 h whereupon the yellow solution turned colourless. The solvent was removed under vacuum and the resulting white oily residue was solidified from CH₂Cl₂-diethylether solution to afford trans-[PtMe₂(CH₂Cl)(phen)(PPh₃)][SnCl₃]* C₂Cl₂H₄. Yield: 85%; m.p. 429 K. Anal. Calc. for C₃₅H₃₅Cl₆N₂PPtSn: C, 40.4; H, 3.4; N, 2.7. Found: C, 39.7; H, 3.0; N, 2.5. NMR data in 1,2-dichloroethane/CDCl₃: δ (³¹P) 1.50 [¹J(¹⁹⁵Pt-³¹P) = 1036 Hz]. The title complex crystallized during the slow decomposition of the organoplatinum(IV) species from a 1,2-dichloroethane solution yielding yellow polyhedral crystals.

Computing details top

Data collection: SMART (Bruker, 1995); cell refinement: SAINT (Bruker, 1995); data reduction: SAINT (Bruker, 1995); program(s) used to solve structure: SHELXTL (Sheldrick, 2008b); program(s) used to refine structure: SHELXTL (Sheldrick, 2008b); molecular graphics: SHELXTL (Sheldrick, 2008b); software used to prepare material for publication: SHELXTL (Sheldrick, 2008b).

Figures top

	Fig. 1. The disordered solvent molecule is omitted for clarity. Displacement ellipsoids are drawn at 50% probability level.
	Fig. 2. A pair of two molecules in the crystal packing showing π-π interactions. The (symmetry imposed) parallel and overlapping phenanthroline planes have a distance of 3.483 (5) Å.

Tetrachlorido(1,10-phenanthroline-κ²N,N')tin(IV) 1,2-dichloroethane hemisolvate top

Crystal data top

[SnCl₄(C₁₂H₈N₂)]·0.5C₂H₄Cl₂	D_x = 1.985 Mg m⁻³
M_r = 490.17	Melting point: 429 K
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 7233 reflections
a = 14.4478 (2) Å	θ = 3.3–24.3°
b = 12.3681 (1) Å	µ = 2.37 mm⁻¹
c = 18.3551 (2) Å	T = 200 K
V = 3279.91 (6) Å³	Polyhedron, yellow
Z = 8	0.20 × 0.18 × 0.12 mm
F(000) = 1896

Data collection top

Bruker SMART CCD diffractometer	3747 independent reflections
Radiation source: fine-focus sealed tube	2954 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.058
ω scans	θ_max = 27.5°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a)	h = −18→18
T_min = 0.649, T_max = 0.765	k = −16→16
31457 measured reflections	l = −23→23

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.085	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0328P)² + 8.0328P] where P = (F_o² + 2F_c²)/3
3747 reflections	(Δ/σ)_max = 0.001
195 parameters	Δρ_max = 0.43 e Å⁻³
0 restraints	Δρ_min = −1.16 e Å⁻³

Crystal data top

[SnCl₄(C₁₂H₈N₂)]·0.5C₂H₄Cl₂	V = 3279.91 (6) Å³
M_r = 490.17	Z = 8
Orthorhombic, Pbca	Mo Kα radiation
a = 14.4478 (2) Å	µ = 2.37 mm⁻¹
b = 12.3681 (1) Å	T = 200 K
c = 18.3551 (2) Å	0.20 × 0.18 × 0.12 mm

Data collection top

Bruker SMART CCD diffractometer	3747 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a)	2954 reflections with I > 2σ(I)
T_min = 0.649, T_max = 0.765	R_int = 0.058
31457 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	0 restraints
wR(F²) = 0.085	H-atom parameters constrained
S = 1.05	Δρ_max = 0.43 e Å⁻³
3747 reflections	Δρ_min = −1.16 e Å⁻³
195 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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Sn1	0.373296 (17)	0.288908 (19)	0.309792 (13)	0.02635 (9)
Cl1	0.36021 (8)	0.11063 (8)	0.26347 (6)	0.0421 (3)
Cl2	0.22059 (8)	0.34733 (10)	0.29708 (7)	0.0511 (3)
Cl3	0.34492 (8)	0.22870 (8)	0.43486 (5)	0.0390 (2)
Cl4	0.42343 (8)	0.36387 (9)	0.19523 (6)	0.0435 (3)
N11	0.4206 (2)	0.4450 (2)	0.35899 (17)	0.0283 (7)
C12	0.5099 (3)	0.4445 (3)	0.38213 (19)	0.0269 (8)
C13	0.5508 (3)	0.5344 (3)	0.4160 (2)	0.0306 (8)
C14	0.4951 (3)	0.6273 (3)	0.4237 (2)	0.0374 (9)
H14	0.5197	0.6900	0.4463	0.045*
C15	0.4064 (3)	0.6278 (3)	0.3989 (2)	0.0408 (10)
H15	0.3695	0.6911	0.4029	0.049*
C16	0.3698 (3)	0.5334 (3)	0.3672 (2)	0.0366 (9)
H16	0.3073	0.5330	0.3512	0.044*
C17	0.6451 (3)	0.5263 (3)	0.4401 (2)	0.0387 (10)
H17	0.6726	0.5861	0.4643	0.046*
N21	0.5220 (2)	0.2640 (2)	0.33599 (17)	0.0283 (7)
C22	0.5637 (3)	0.3483 (3)	0.37021 (19)	0.0274 (8)
C23	0.6563 (3)	0.3443 (3)	0.3932 (2)	0.0327 (9)
C24	0.7061 (3)	0.2487 (4)	0.3787 (2)	0.0407 (10)
H24	0.7690	0.2426	0.3931	0.049*
C25	0.6635 (3)	0.1650 (4)	0.3438 (2)	0.0404 (10)
H25	0.6967	0.1004	0.3337	0.049*
C26	0.5708 (3)	0.1745 (3)	0.3230 (2)	0.0342 (9)
H26	0.5418	0.1156	0.2990	0.041*
C27	0.6951 (3)	0.4365 (4)	0.4294 (2)	0.0404 (10)
H27	0.7574	0.4339	0.4460	0.048*
Cl11	0.61683 (10)	0.09903 (12)	0.52665 (8)	0.0666 (4)
C31	0.5152 (6)	0.0229 (6)	0.5363 (4)	0.049 (3)	0.71 (2)
H31A	0.5260	−0.0370	0.5711	0.058*	0.71 (2)
H31B	0.4654	0.0693	0.5563	0.058*	0.71 (2)
C31B	0.5342 (18)	0.024 (2)	0.4789 (13)	0.066 (8)*	0.29 (2)
H31C	0.5043	0.0714	0.4427	0.079*	0.29 (2)
H31D	0.5666	−0.0343	0.4517	0.079*	0.29 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sn1	0.03044 (14)	0.02244 (13)	0.02617 (14)	−0.00135 (10)	0.00109 (10)	−0.00118 (10)
Cl1	0.0475 (6)	0.0298 (5)	0.0491 (6)	−0.0029 (4)	−0.0022 (5)	−0.0091 (4)
Cl2	0.0451 (6)	0.0513 (7)	0.0567 (7)	0.0050 (5)	−0.0043 (5)	−0.0082 (6)
Cl3	0.0451 (5)	0.0396 (6)	0.0323 (5)	−0.0064 (4)	0.0046 (4)	0.0031 (4)
Cl4	0.0548 (7)	0.0421 (6)	0.0335 (5)	−0.0053 (5)	0.0050 (5)	0.0067 (5)
N11	0.0316 (17)	0.0237 (15)	0.0296 (16)	−0.0005 (13)	−0.0005 (13)	0.0005 (13)
C12	0.0291 (19)	0.0265 (18)	0.0251 (18)	−0.0028 (15)	0.0044 (15)	0.0024 (15)
C13	0.040 (2)	0.0279 (19)	0.0237 (18)	−0.0065 (16)	0.0035 (16)	0.0045 (15)
C14	0.050 (3)	0.026 (2)	0.037 (2)	−0.0082 (18)	0.0038 (19)	−0.0034 (17)
C15	0.053 (3)	0.027 (2)	0.043 (2)	0.0033 (19)	0.000 (2)	−0.0039 (18)
C16	0.038 (2)	0.030 (2)	0.042 (2)	0.0034 (17)	−0.0026 (18)	−0.0033 (17)
C17	0.042 (2)	0.038 (2)	0.036 (2)	−0.0172 (18)	−0.0013 (18)	0.0018 (18)
N21	0.0305 (17)	0.0263 (16)	0.0282 (16)	0.0008 (13)	0.0025 (13)	0.0005 (13)
C22	0.0311 (19)	0.0263 (19)	0.0246 (18)	−0.0041 (15)	0.0046 (15)	0.0046 (15)
C23	0.0290 (19)	0.038 (2)	0.032 (2)	−0.0010 (17)	0.0037 (16)	0.0092 (17)
C24	0.031 (2)	0.044 (2)	0.048 (3)	0.0015 (19)	0.0030 (19)	0.013 (2)
C25	0.039 (2)	0.035 (2)	0.047 (3)	0.0108 (19)	0.009 (2)	0.0086 (19)
C26	0.038 (2)	0.0292 (19)	0.035 (2)	0.0025 (17)	0.0072 (17)	0.0012 (16)
C27	0.032 (2)	0.047 (3)	0.041 (2)	−0.0098 (19)	−0.0041 (18)	0.009 (2)
Cl11	0.0691 (9)	0.0617 (8)	0.0691 (9)	−0.0178 (7)	0.0144 (7)	−0.0220 (7)
C31	0.061 (5)	0.048 (4)	0.037 (4)	−0.005 (3)	0.021 (3)	−0.008 (3)

Geometric parameters (Å, º) top

Sn1—N21	2.224 (3)	N21—C26	1.334 (5)
Sn1—N11	2.238 (3)	N21—C22	1.357 (5)
Sn1—Cl2	2.3333 (12)	C22—C23	1.404 (5)
Sn1—Cl1	2.3708 (10)	C23—C24	1.410 (6)
Sn1—Cl4	2.4095 (10)	C23—C27	1.434 (6)
Sn1—Cl3	2.4480 (10)	C24—C25	1.363 (6)
Cl1—Cl2ⁱ	3.5140 (16)	C24—H24	0.9500
N11—C16	1.325 (5)	C25—C26	1.397 (6)
N11—C12	1.358 (5)	C25—H25	0.9500
C12—C13	1.404 (5)	C26—H26	0.9500
C12—C22	1.438 (5)	C27—H27	0.9500
C13—C14	1.409 (6)	Cl11—C31B	1.75 (3)
C13—C17	1.436 (6)	Cl11—C31	1.754 (8)
C14—C15	1.360 (6)	C31—C31ⁱⁱ	1.513 (17)
C14—H14	0.9500	C31—H31A	0.9900
C15—C16	1.407 (6)	C31—H31B	0.9900
C15—H15	0.9500	C31B—C31Bⁱⁱ	1.38 (5)
C16—H16	0.9500	C31B—H31C	0.9900
C17—C27	1.339 (6)	C31B—H31D	0.9900
C17—H17	0.9500

N21—Sn1—N11	74.74 (11)	C15—C16—H16	119.2
N21—Sn1—Cl2	168.06 (9)	C27—C17—C13	121.7 (4)
N11—Sn1—Cl2	93.56 (9)	C27—C17—H17	119.2
N21—Sn1—Cl1	91.48 (8)	C13—C17—H17	119.2
N11—Sn1—Cl1	166.22 (8)	C26—N21—C22	119.1 (3)
Cl2—Sn1—Cl1	100.18 (4)	C26—N21—Sn1	126.0 (3)
N21—Sn1—Cl4	87.22 (9)	C22—N21—Sn1	115.0 (2)
N11—Sn1—Cl4	85.89 (8)	N21—C22—C23	122.3 (4)
Cl2—Sn1—Cl4	94.46 (4)	N21—C22—C12	117.8 (3)
Cl1—Sn1—Cl4	93.95 (4)	C23—C22—C12	119.8 (4)
N21—Sn1—Cl3	85.24 (8)	C22—C23—C24	117.3 (4)
N11—Sn1—Cl3	86.29 (8)	C22—C23—C27	119.0 (4)
Cl2—Sn1—Cl3	91.70 (4)	C24—C23—C27	123.8 (4)
Cl1—Sn1—Cl3	92.29 (4)	C25—C24—C23	119.7 (4)
Cl4—Sn1—Cl3	170.32 (4)	C25—C24—H24	120.1
C16—N11—C12	119.6 (3)	C23—C24—H24	120.1
C16—N11—Sn1	126.0 (3)	C24—C25—C26	119.8 (4)
C12—N11—Sn1	114.4 (2)	C24—C25—H25	120.1
N11—C12—C13	122.3 (3)	C26—C25—H25	120.1
N11—C12—C22	118.0 (3)	N21—C26—C25	121.9 (4)
C13—C12—C22	119.7 (3)	N21—C26—H26	119.1
C12—C13—C14	116.7 (4)	C25—C26—H26	119.1
C12—C13—C17	118.7 (4)	C17—C27—C23	121.1 (4)
C14—C13—C17	124.6 (4)	C17—C27—H27	119.5
C15—C14—C13	120.6 (4)	C23—C27—H27	119.5
C15—C14—H14	119.7	C31B—Cl11—C31	36.2 (7)
C13—C14—H14	119.7	Cl11—C31—H31A	109.5
C14—C15—C16	119.2 (4)	Cl11—C31—H31B	109.5
C14—C15—H15	120.4	H31A—C31—H31B	108.1
C16—C15—H15	120.4	Cl11—C31B—H31C	108.4
N11—C16—C15	121.6 (4)	Cl11—C31B—H31D	108.4
N11—C16—H16	119.2	H31C—C31B—H31D	107.4

N21—Sn1—N11—C16	177.5 (3)	Cl4—Sn1—N21—C26	−92.4 (3)
Cl2—Sn1—N11—C16	−4.9 (3)	Cl3—Sn1—N21—C26	93.7 (3)
Cl1—Sn1—N11—C16	179.1 (3)	N11—Sn1—N21—C22	3.2 (2)
Cl4—Sn1—N11—C16	89.3 (3)	Cl2—Sn1—N21—C22	−8.7 (6)
Cl3—Sn1—N11—C16	−96.4 (3)	Cl1—Sn1—N21—C22	−176.4 (2)
N21—Sn1—N11—C12	−2.9 (2)	Cl4—Sn1—N21—C22	89.7 (2)
Cl2—Sn1—N11—C12	174.6 (2)	Cl3—Sn1—N21—C22	−84.2 (2)
Cl1—Sn1—N11—C12	−1.3 (5)	C26—N21—C22—C23	−0.7 (5)
Cl4—Sn1—N11—C12	−91.2 (2)	Sn1—N21—C22—C23	177.4 (3)
Cl3—Sn1—N11—C12	83.1 (2)	C26—N21—C22—C12	178.7 (3)
C16—N11—C12—C13	1.2 (5)	Sn1—N21—C22—C12	−3.2 (4)
Sn1—N11—C12—C13	−178.4 (3)	N11—C12—C22—N21	0.5 (5)
C16—N11—C12—C22	−178.1 (3)	C13—C12—C22—N21	−178.7 (3)
Sn1—N11—C12—C22	2.4 (4)	N11—C12—C22—C23	180.0 (3)
N11—C12—C13—C14	−1.4 (5)	C13—C12—C22—C23	0.7 (5)
C22—C12—C13—C14	177.9 (3)	N21—C22—C23—C24	0.7 (5)
N11—C12—C13—C17	178.8 (3)	C12—C22—C23—C24	−178.7 (3)
C22—C12—C13—C17	−2.0 (5)	N21—C22—C23—C27	−179.7 (3)
C12—C13—C14—C15	−0.1 (6)	C12—C22—C23—C27	1.0 (5)
C17—C13—C14—C15	179.7 (4)	C22—C23—C24—C25	−0.3 (6)
C13—C14—C15—C16	1.7 (6)	C27—C23—C24—C25	−179.9 (4)
C12—N11—C16—C15	0.5 (6)	C23—C24—C25—C26	−0.2 (6)
Sn1—N11—C16—C15	−180.0 (3)	C22—N21—C26—C25	0.1 (6)
C14—C15—C16—N11	−2.0 (7)	Sn1—N21—C26—C25	−177.7 (3)
C12—C13—C17—C27	1.7 (6)	C24—C25—C26—N21	0.3 (6)
C14—C13—C17—C27	−178.1 (4)	C13—C17—C27—C23	−0.1 (6)
N11—Sn1—N21—C26	−178.8 (3)	C22—C23—C27—C17	−1.3 (6)
Cl2—Sn1—N21—C26	169.2 (3)	C24—C23—C27—C17	178.3 (4)
Cl1—Sn1—N21—C26	1.5 (3)

Symmetry codes: (i) −x+1/2, y−1/2, z; (ii) −x+1, −y, −z+1.

Experimental details

Crystal data
Chemical formula	[SnCl₄(C₁₂H₈N₂)]·0.5C₂H₄Cl₂
M_r	490.17
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	200
a, b, c (Å)	14.4478 (2), 12.3681 (1), 18.3551 (2)
V (Å³)	3279.91 (6)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	2.37
Crystal size (mm)	0.20 × 0.18 × 0.12

Data collection
Diffractometer	Bruker SMART CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2008a)
T_min, T_max	0.649, 0.765
No. of measured, independent and observed [I > 2σ(I)] reflections	31457, 3747, 2954
R_int	0.058
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.085, 1.05
No. of reflections	3747
No. of parameters	195
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.43, −1.16

Computer programs: SMART (Bruker, 1995), SAINT (Bruker, 1995), SHELXTL (Sheldrick, 2008b).

Selected geometric parameters (Å, º) top

Sn1—N21	2.224 (3)	Sn1—Cl4	2.4095 (10)
Sn1—N11	2.238 (3)	Sn1—Cl3	2.4480 (10)
Sn1—Cl2	2.3333 (12)	Cl1—Cl2ⁱ	3.5140 (16)
Sn1—Cl1	2.3708 (10)

N21—Sn1—N11	74.74 (11)	Cl4—Sn1—Cl3	170.32 (4)
Cl2—Sn1—Cl1	100.18 (4)

Symmetry code: (i) −x+1/2, y−1/2, z.

Acknowledgements

We thank the Science Research Council of K. N. Toosi University of Technology for financial support. We also thank Johnson Matthey for the generous loan of platinum salt.

References

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