Literature DB >> 21583047

Tetra-chlorido-(1,10-phenanthroline-κN,N')tin(IV) 1,2-dichloro-ethane hemisolvate.

Badri Z Momeni, Frank Rominger, Simin S Hosseini.   

Abstract

The asymmetric unit of the title compound, [SnCl(4)(C(12)n class="Species">H(8)N(2))]·0.5C(2)H(4)Cl(2), contains a tin complex and one disordered half-mol-ecule of the solvent dichloro-ethane [occupancies 0.71 (2):0.29 (2)]. The six coordinate Sn(IV) atom adopts a distorted octa-hedral geometry. π-π inter-actions between adjacent aromatic rings [interplanar distance 3.483 (5) Å] seem to be effective in the stabilization of the crystal packing.

Entities:  

Year:  2009        PMID： 21583047      PMCID： PMC2969692          DOI： 10.1107/S1600536809017346

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


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 [SnX 4(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 = 490.17 Orthorhombic, 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[F 2 > 2σ(F 2)] = 0.032 wR(F 2) = 0.085 S = 1.05 3747 reflections 195 parameters H-atom parameters constrained Δρmax = 0.43 e Å−3 Δρmin = −1.16 e Å−3 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. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809017346/hg2511sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809017346/hg2511Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[SnCl4(C12H8N2)]·0.5C2H4Cl2Dx = 1.985 Mg m−3
Mr = 490.17Melting point: 429 K
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 7233 reflections
a = 14.4478 (2) Åθ = 3.3–24.3°
b = 12.3681 (1) ŵ = 2.37 mm−1
c = 18.3551 (2) ÅT = 200 K
V = 3279.91 (6) Å3Polyhedron, yellow
Z = 80.20 × 0.18 × 0.12 mm
F(000) = 1896
Bruker SMART CCD diffractometer3747 independent reflections
Radiation source: fine-focus sealed tube2954 reflections with I > 2σ(I)
graphiteRint = 0.058
ω scansθmax = 27.5°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a)h = −18→18
Tmin = 0.649, Tmax = 0.765k = −16→16
31457 measured reflectionsl = −23→23
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H-atom parameters constrained
S = 1.05w = 1/[σ2(Fo2) + (0.0328P)2 + 8.0328P] where P = (Fo2 + 2Fc2)/3
3747 reflections(Δ/σ)max = 0.001
195 parametersΔρmax = 0.43 e Å−3
0 restraintsΔρmin = −1.16 e Å−3
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.
xyzUiso*/UeqOcc. (<1)
Sn10.373296 (17)0.288908 (19)0.309792 (13)0.02635 (9)
Cl10.36021 (8)0.11063 (8)0.26347 (6)0.0421 (3)
Cl20.22059 (8)0.34733 (10)0.29708 (7)0.0511 (3)
Cl30.34492 (8)0.22870 (8)0.43486 (5)0.0390 (2)
Cl40.42343 (8)0.36387 (9)0.19523 (6)0.0435 (3)
N110.4206 (2)0.4450 (2)0.35899 (17)0.0283 (7)
C120.5099 (3)0.4445 (3)0.38213 (19)0.0269 (8)
C130.5508 (3)0.5344 (3)0.4160 (2)0.0306 (8)
C140.4951 (3)0.6273 (3)0.4237 (2)0.0374 (9)
H140.51970.69000.44630.045*
C150.4064 (3)0.6278 (3)0.3989 (2)0.0408 (10)
H150.36950.69110.40290.049*
C160.3698 (3)0.5334 (3)0.3672 (2)0.0366 (9)
H160.30730.53300.35120.044*
C170.6451 (3)0.5263 (3)0.4401 (2)0.0387 (10)
H170.67260.58610.46430.046*
N210.5220 (2)0.2640 (2)0.33599 (17)0.0283 (7)
C220.5637 (3)0.3483 (3)0.37021 (19)0.0274 (8)
C230.6563 (3)0.3443 (3)0.3932 (2)0.0327 (9)
C240.7061 (3)0.2487 (4)0.3787 (2)0.0407 (10)
H240.76900.24260.39310.049*
C250.6635 (3)0.1650 (4)0.3438 (2)0.0404 (10)
H250.69670.10040.33370.049*
C260.5708 (3)0.1745 (3)0.3230 (2)0.0342 (9)
H260.54180.11560.29900.041*
C270.6951 (3)0.4365 (4)0.4294 (2)0.0404 (10)
H270.75740.43390.44600.048*
Cl110.61683 (10)0.09903 (12)0.52665 (8)0.0666 (4)
C310.5152 (6)0.0229 (6)0.5363 (4)0.049 (3)0.71 (2)
H31A0.5260−0.03700.57110.058*0.71 (2)
H31B0.46540.06930.55630.058*0.71 (2)
C31B0.5342 (18)0.024 (2)0.4789 (13)0.066 (8)*0.29 (2)
H31C0.50430.07140.44270.079*0.29 (2)
H31D0.5666−0.03430.45170.079*0.29 (2)
U11U22U33U12U13U23
Sn10.03044 (14)0.02244 (13)0.02617 (14)−0.00135 (10)0.00109 (10)−0.00118 (10)
Cl10.0475 (6)0.0298 (5)0.0491 (6)−0.0029 (4)−0.0022 (5)−0.0091 (4)
Cl20.0451 (6)0.0513 (7)0.0567 (7)0.0050 (5)−0.0043 (5)−0.0082 (6)
Cl30.0451 (5)0.0396 (6)0.0323 (5)−0.0064 (4)0.0046 (4)0.0031 (4)
Cl40.0548 (7)0.0421 (6)0.0335 (5)−0.0053 (5)0.0050 (5)0.0067 (5)
N110.0316 (17)0.0237 (15)0.0296 (16)−0.0005 (13)−0.0005 (13)0.0005 (13)
C120.0291 (19)0.0265 (18)0.0251 (18)−0.0028 (15)0.0044 (15)0.0024 (15)
C130.040 (2)0.0279 (19)0.0237 (18)−0.0065 (16)0.0035 (16)0.0045 (15)
C140.050 (3)0.026 (2)0.037 (2)−0.0082 (18)0.0038 (19)−0.0034 (17)
C150.053 (3)0.027 (2)0.043 (2)0.0033 (19)0.000 (2)−0.0039 (18)
C160.038 (2)0.030 (2)0.042 (2)0.0034 (17)−0.0026 (18)−0.0033 (17)
C170.042 (2)0.038 (2)0.036 (2)−0.0172 (18)−0.0013 (18)0.0018 (18)
N210.0305 (17)0.0263 (16)0.0282 (16)0.0008 (13)0.0025 (13)0.0005 (13)
C220.0311 (19)0.0263 (19)0.0246 (18)−0.0041 (15)0.0046 (15)0.0046 (15)
C230.0290 (19)0.038 (2)0.032 (2)−0.0010 (17)0.0037 (16)0.0092 (17)
C240.031 (2)0.044 (2)0.048 (3)0.0015 (19)0.0030 (19)0.013 (2)
C250.039 (2)0.035 (2)0.047 (3)0.0108 (19)0.009 (2)0.0086 (19)
C260.038 (2)0.0292 (19)0.035 (2)0.0025 (17)0.0072 (17)0.0012 (16)
C270.032 (2)0.047 (3)0.041 (2)−0.0098 (19)−0.0041 (18)0.009 (2)
Cl110.0691 (9)0.0617 (8)0.0691 (9)−0.0178 (7)0.0144 (7)−0.0220 (7)
C310.061 (5)0.048 (4)0.037 (4)−0.005 (3)0.021 (3)−0.008 (3)
Sn1—N212.224 (3)N21—C261.334 (5)
Sn1—N112.238 (3)N21—C221.357 (5)
Sn1—Cl22.3333 (12)C22—C231.404 (5)
Sn1—Cl12.3708 (10)C23—C241.410 (6)
Sn1—Cl42.4095 (10)C23—C271.434 (6)
Sn1—Cl32.4480 (10)C24—C251.363 (6)
Cl1—Cl2i3.5140 (16)C24—H240.9500
N11—C161.325 (5)C25—C261.397 (6)
N11—C121.358 (5)C25—H250.9500
C12—C131.404 (5)C26—H260.9500
C12—C221.438 (5)C27—H270.9500
C13—C141.409 (6)Cl11—C31B1.75 (3)
C13—C171.436 (6)Cl11—C311.754 (8)
C14—C151.360 (6)C31—C31ii1.513 (17)
C14—H140.9500C31—H31A0.9900
C15—C161.407 (6)C31—H31B0.9900
C15—H150.9500C31B—C31Bii1.38 (5)
C16—H160.9500C31B—H31C0.9900
C17—C271.339 (6)C31B—H31D0.9900
C17—H170.9500
N21—Sn1—N1174.74 (11)C15—C16—H16119.2
N21—Sn1—Cl2168.06 (9)C27—C17—C13121.7 (4)
N11—Sn1—Cl293.56 (9)C27—C17—H17119.2
N21—Sn1—Cl191.48 (8)C13—C17—H17119.2
N11—Sn1—Cl1166.22 (8)C26—N21—C22119.1 (3)
Cl2—Sn1—Cl1100.18 (4)C26—N21—Sn1126.0 (3)
N21—Sn1—Cl487.22 (9)C22—N21—Sn1115.0 (2)
N11—Sn1—Cl485.89 (8)N21—C22—C23122.3 (4)
Cl2—Sn1—Cl494.46 (4)N21—C22—C12117.8 (3)
Cl1—Sn1—Cl493.95 (4)C23—C22—C12119.8 (4)
N21—Sn1—Cl385.24 (8)C22—C23—C24117.3 (4)
N11—Sn1—Cl386.29 (8)C22—C23—C27119.0 (4)
Cl2—Sn1—Cl391.70 (4)C24—C23—C27123.8 (4)
Cl1—Sn1—Cl392.29 (4)C25—C24—C23119.7 (4)
Cl4—Sn1—Cl3170.32 (4)C25—C24—H24120.1
C16—N11—C12119.6 (3)C23—C24—H24120.1
C16—N11—Sn1126.0 (3)C24—C25—C26119.8 (4)
C12—N11—Sn1114.4 (2)C24—C25—H25120.1
N11—C12—C13122.3 (3)C26—C25—H25120.1
N11—C12—C22118.0 (3)N21—C26—C25121.9 (4)
C13—C12—C22119.7 (3)N21—C26—H26119.1
C12—C13—C14116.7 (4)C25—C26—H26119.1
C12—C13—C17118.7 (4)C17—C27—C23121.1 (4)
C14—C13—C17124.6 (4)C17—C27—H27119.5
C15—C14—C13120.6 (4)C23—C27—H27119.5
C15—C14—H14119.7C31B—Cl11—C3136.2 (7)
C13—C14—H14119.7Cl11—C31—H31A109.5
C14—C15—C16119.2 (4)Cl11—C31—H31B109.5
C14—C15—H15120.4H31A—C31—H31B108.1
C16—C15—H15120.4Cl11—C31B—H31C108.4
N11—C16—C15121.6 (4)Cl11—C31B—H31D108.4
N11—C16—H16119.2H31C—C31B—H31D107.4
N21—Sn1—N11—C16177.5 (3)Cl4—Sn1—N21—C26−92.4 (3)
Cl2—Sn1—N11—C16−4.9 (3)Cl3—Sn1—N21—C2693.7 (3)
Cl1—Sn1—N11—C16179.1 (3)N11—Sn1—N21—C223.2 (2)
Cl4—Sn1—N11—C1689.3 (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—C2289.7 (2)
Cl2—Sn1—N11—C12174.6 (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—C23177.4 (3)
Cl3—Sn1—N11—C1283.1 (2)C26—N21—C22—C12178.7 (3)
C16—N11—C12—C131.2 (5)Sn1—N21—C22—C12−3.2 (4)
Sn1—N11—C12—C13−178.4 (3)N11—C12—C22—N210.5 (5)
C16—N11—C12—C22−178.1 (3)C13—C12—C22—N21−178.7 (3)
Sn1—N11—C12—C222.4 (4)N11—C12—C22—C23180.0 (3)
N11—C12—C13—C14−1.4 (5)C13—C12—C22—C230.7 (5)
C22—C12—C13—C14177.9 (3)N21—C22—C23—C240.7 (5)
N11—C12—C13—C17178.8 (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—C271.0 (5)
C17—C13—C14—C15179.7 (4)C22—C23—C24—C25−0.3 (6)
C13—C14—C15—C161.7 (6)C27—C23—C24—C25−179.9 (4)
C12—N11—C16—C150.5 (6)C23—C24—C25—C26−0.2 (6)
Sn1—N11—C16—C15−180.0 (3)C22—N21—C26—C250.1 (6)
C14—C15—C16—N11−2.0 (7)Sn1—N21—C26—C25−177.7 (3)
C12—C13—C17—C271.7 (6)C24—C25—C26—N210.3 (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—C26169.2 (3)C24—C23—C27—C17178.3 (4)
Cl1—Sn1—N21—C261.5 (3)
Table 1

Selected geometric parameters (Å, °)

Sn1—N212.224 (3)
Sn1—N112.238 (3)
Sn1—Cl22.3333 (12)
Sn1—Cl12.3708 (10)
Sn1—Cl42.4095 (10)
Sn1—Cl32.4480 (10)
  1 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
  1 in total
  3 in total

1.  Tetra-aqua-(5,5'-dimethyl-2,2'-bipyridine-κN,N')zinc(II) sulfate.

Authors:  Qing-Lan Zhao; Hui-Feng Bai
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-07-04

2.  Aqua-bis(benzoato-κO)(5,5'-dimethyl-2,2'-bipyridine-κN,N')copper(II).

Authors:  Xi-Yan Dong; Xiaojie Xu; Lei Yang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-10-03

3.  (Carbonato-κ(2)O,O')bis-(5,5'-dimethyl-2,2'-bipyridyl-κ(2)N,N')cobalt(III) bromide trihydrate.

Authors:  Kannan Arun Kumar; Parthsarathi Meera; Madhavan Amutha Selvi; Arunachalam Dayalan
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-03-07
  3 in total

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