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The coordinated water mol­ecule in the 1:1 adduct of tri­phenyl­tin tri­fluoro­acetate with 2,2′:6′,2′′-ter­pyridine, [Sn(C2F3O2)(C6H5)3(H2O)]·C15H11N3, interacts with the N atoms of the two outer pyridyl rings of the ter­pyridine heterocycle [O...N = 2.771 (3) and 2.797 (3) Å]; these outer rings are twisted by 25.6 (1) and 32.7 (1)° with respect to the central ring. The Sn atom is five-coordinate in a trans–C3SnO2 trigonal-bipyramidal environment [Sn—O = 2.221 (2) Å and Sn\leftarrow O = 2.274 (2) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680300583X/lh6044sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680300583X/lh6044Isup2.hkl
Contains datablock I

CCDC reference: 209890

Key indicators

  • Single-crystal X-ray study
  • T = 158 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.027
  • wR factor = 0.062
  • Data-to-parameter ratio = 15.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Comment top

In our previously reported structure of the 1:1 complex of aquatrifluoroacetatotriphenyltin and 2,4,6-tris(2-pyridyl)-1,3,5-triazine (Chee et al., 2002), the water molecule [Sn O = 2.311 (3) Å] forms hydrogen bonds to two of the N atoms of the 1-pyridyl and 3-pyridyl rings of the N-heterocycle [O···N = 2.841 (4) and 2.826 (4) Å]; the N atom in the 2-position of the triazine ring is not involved in the interaction. The heterocyclic ligand is relatively flat, the 1-pyridyl and 3-pyridyl rings being twisted by only 7.7 (2) and 13.4 (2)° with respect to the triazine ring. Without the 5-pyridyl group, the resulting N-heterocycle, viz. terpyridine, also furnishes a similar outer-sphere coordination complex. However, the terpyridine ligand in the title complex, (I) (Fig. 1), is severely twisted, the dihedral angle of the two outer rings with respect to the central pyridyl ring being 25.6 (1) and 32.7 (1)°. The twist contrasts with the virtually flat conformation of terpyridine itself, the corresponding dihedral angles being only only 5.1 and 7.2°. As the ligand exists in the trans,trans-conformation in the solid state (and also in solution) (Bessel et al., 1992), it would have to reorganize itself in order to function as a terdentate chelate. Interestingly, the two terpyridine ligands in 2-methyl-3-trimethylsilyl-2,3-dicarba-1-stanna-closo-heptaborane(6) bis(terpyridine), both exist in the cis,cis-conformation, although only one of them chelates coordinated to the SnII atom (Siriwardane & Hosmane, 1988).

The ligand also forms outer-sphere coordination complexes with triphenyltin chloride [Sn—Owater = 2.317 (2) Å; Prasad et al., 1982] and triphenyltin isothiocyanate [Sn—Owater = 2.252 (2) Å; Prasad & Smith, 1982]; the ligand is also severely twisted [14.3 (3) and 32.0 (2)° in the chloride, and 19.6 (3) and 29.5 (3)° in the isothiocyanate]. The Sn—Owater bond in the trifluoroacetate is similar to the distances found in the two complexes, but is much shorter than that [Sn—Owater = 2.335 (4) Å] in the 1,10-phenanthroline adduct, which has a different hydrogen-bonding feature (Ng et al., 1996).

Experimental top

The title compound was prepared by heating triphenyltin trifluoroacetate (0.73 g, 2 mmol), which was synthesized from triphenyltin hydroxide and trifluoroacetic acid, with an equimolar quantity of terpyridine (0.47 g, 2 mmol) in ethanol. The product was obtained as crystals upon evaporation of the solvent (m.p. 409–410 K).

Refinement top

The carbon-bound H atoms were positioned geometrically and were allowed to ride on their parent C atoms, with Uiso(H) = 1.2Ueq(C). The water H atoms were located and refined, subject to O—H = 0.85±0.01 Å.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. ORTEPII (Johnson, 1976) plot of (I), with ellipsoids at the 50% probability level. H atoms are drawn as spheres of arbitrary radii.
Aquatripheny(trifluoroacetato)ltin–2,2':6',2"-terpyridine (1/1) top
Crystal data top
[Sn(C2F3O2)(C6H5)3(H2O)]·C15H11N3F(000) = 1440
Mr = 714.29Dx = 1.512 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 6202 reflections
a = 10.4257 (7) Åθ = 2.0–26.4°
b = 10.0510 (7) ŵ = 0.87 mm1
c = 30.025 (2) ÅT = 158 K
β = 94.265 (1)°Plate, colorless
V = 3137.6 (4) Å30.50 × 0.24 × 0.15 mm
Z = 4
Data collection top
Bruker SMART area-detector
diffractometer
6320 independent reflections
Radiation source: fine-focus sealed tube5021 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
ω scansθmax = 26.4°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 126
Tmin = 0.744, Tmax = 0.877k = 1212
39984 measured reflectionsl = 3737
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.062H atoms treated by a mixture of independent and constrained refinement
S = 0.95 w = 1/[σ2(Fo2) + (0.0356P)2]
where P = (Fo2 + 2Fc2)/3
6320 reflections(Δ/σ)max = 0.001
414 parametersΔρmax = 0.50 e Å3
2 restraintsΔρmin = 0.43 e Å3
Crystal data top
[Sn(C2F3O2)(C6H5)3(H2O)]·C15H11N3V = 3137.6 (4) Å3
Mr = 714.29Z = 4
Monoclinic, P21/nMo Kα radiation
a = 10.4257 (7) ŵ = 0.87 mm1
b = 10.0510 (7) ÅT = 158 K
c = 30.025 (2) Å0.50 × 0.24 × 0.15 mm
β = 94.265 (1)°
Data collection top
Bruker SMART area-detector
diffractometer
6320 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5021 reflections with I > 2σ(I)
Tmin = 0.744, Tmax = 0.877Rint = 0.051
39984 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0272 restraints
wR(F2) = 0.062H atoms treated by a mixture of independent and constrained refinement
S = 0.95Δρmax = 0.50 e Å3
6320 reflectionsΔρmin = 0.43 e Å3
414 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sn10.34215 (1)0.65441 (2)0.37274 (1)0.0243 (1)
F10.0065 (2)0.8301 (2)0.4617 (1)0.0683 (5)
F20.1695 (2)0.9420 (2)0.4864 (1)0.0645 (5)
F30.0339 (2)1.0293 (2)0.4384 (1)0.0830 (6)
O10.2095 (2)0.7439 (2)0.4190 (1)0.034 (1)
O20.1917 (2)0.9364 (2)0.3810 (1)0.040 (1)
O1w0.4810 (2)0.5434 (2)0.3311 (1)0.029 (1)
N10.5289 (2)0.6492 (2)0.2488 (1)0.030 (1)
N20.7394 (2)0.6247 (2)0.3091 (1)0.029 (1)
N30.7033 (2)0.4772 (2)0.3845 (1)0.033 (1)
C10.4784 (2)0.8095 (2)0.3868 (1)0.029 (1)
C20.4993 (3)0.8628 (3)0.4295 (1)0.045 (1)
C30.5872 (3)0.9663 (3)0.4376 (1)0.055 (1)
C40.6536 (3)1.0159 (3)0.4033 (1)0.053 (1)
C50.6309 (2)0.9667 (3)0.3607 (1)0.046 (1)
C60.5434 (2)0.8630 (2)0.3527 (1)0.035 (1)
C70.2202 (2)0.6654 (2)0.3129 (1)0.027 (1)
C80.1465 (2)0.5549 (2)0.2983 (1)0.035 (1)
C90.0739 (2)0.5575 (3)0.2577 (1)0.043 (1)
C100.0740 (2)0.6695 (3)0.2307 (1)0.043 (1)
C110.1446 (2)0.7797 (3)0.2448 (1)0.037 (1)
C120.2170 (2)0.7780 (2)0.2855 (1)0.029 (1)
C130.3357 (2)0.4767 (2)0.4109 (1)0.031 (1)
C140.3269 (3)0.4804 (3)0.4569 (1)0.061 (1)
C150.3232 (4)0.3644 (4)0.4815 (1)0.085 (1)
C160.3275 (4)0.2427 (3)0.4608 (1)0.071 (1)
C170.3372 (3)0.2355 (3)0.4155 (1)0.053 (1)
C180.3414 (2)0.3516 (2)0.3907 (1)0.039 (1)
C190.1727 (2)0.8637 (2)0.4120 (1)0.031 (1)
C200.0938 (3)0.9171 (3)0.4497 (1)0.042 (1)
C210.4353 (2)0.6382 (2)0.2160 (1)0.036 (1)
C220.4498 (3)0.6776 (2)0.1722 (1)0.046 (1)
C230.5664 (3)0.7291 (3)0.1621 (1)0.050 (1)
C240.6622 (3)0.7427 (3)0.1954 (1)0.042 (1)
C250.6417 (2)0.7019 (2)0.2387 (1)0.030 (1)
C260.7404 (2)0.7167 (2)0.2763 (1)0.031 (1)
C270.8264 (2)0.8232 (2)0.2781 (1)0.039 (1)
C280.9110 (2)0.8355 (3)0.3151 (1)0.045 (1)
C290.9094 (2)0.7435 (3)0.3488 (1)0.042 (1)
C300.8221 (2)0.6387 (2)0.3450 (1)0.032 (1)
C310.8168 (2)0.5392 (2)0.3813 (1)0.033 (1)
C320.9223 (3)0.5118 (3)0.4110 (1)0.044 (1)
C330.9114 (3)0.4189 (3)0.4445 (1)0.051 (1)
C340.7965 (3)0.3565 (3)0.4479 (1)0.050 (1)
C350.6949 (3)0.3884 (3)0.4175 (1)0.043 (1)
H1w10.500 (3)0.582 (3)0.3075 (6)0.06 (1)*
H1w20.552 (2)0.527 (3)0.3456 (8)0.06 (1)*
H20.45350.82860.45320.054*
H30.60131.00250.46680.066*
H40.71531.08440.40910.063*
H50.67461.00320.33690.055*
H60.52840.82880.32320.041*
H80.14640.47750.31640.042*
H90.02390.48220.24830.052*
H100.02570.67030.20270.052*
H110.14360.85700.22660.044*
H120.26520.85460.29490.035*
H140.32350.56390.47160.073*
H150.31770.36880.51290.102*
H160.32380.16340.47780.086*
H170.34090.15140.40130.063*
H180.34840.34610.35940.047*
H210.35510.60180.22300.043*
H220.38090.66910.14990.055*
H230.58000.75500.13240.060*
H240.74260.77980.18900.051*
H270.82630.88560.25430.047*
H280.97050.90720.31730.054*
H290.96740.75140.37460.050*
H321.00150.55670.40830.052*
H330.98290.39890.46490.061*
H340.78630.29250.47060.059*
H350.61480.34500.42010.052*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.02413 (9)0.02435 (8)0.02434 (9)0.00214 (7)0.00159 (6)0.00168 (7)
F10.056 (1)0.082 (1)0.072 (1)0.015 (1)0.035 (1)0.025 (1)
F20.075 (1)0.080 (1)0.038 (1)0.005 (1)0.002 (1)0.023 (1)
F30.102 (2)0.078 (1)0.072 (1)0.054 (1)0.025 (1)0.004 (1)
O10.034 (1)0.032 (1)0.036 (1)0.002 (1)0.008 (1)0.001 (1)
O20.045 (1)0.036 (1)0.040 (1)0.002 (1)0.003 (1)0.003 (1)
O1w0.024 (1)0.033 (1)0.029 (1)0.000 (1)0.003 (1)0.003 (1)
N10.031 (1)0.030 (1)0.028 (1)0.002 (1)0.004 (1)0.004 (1)
N20.024 (1)0.029 (1)0.034 (1)0.001 (1)0.004 (1)0.001 (1)
N30.033 (1)0.034 (1)0.032 (1)0.002 (1)0.001 (1)0.001 (1)
C10.025 (1)0.025 (1)0.035 (1)0.002 (1)0.001 (1)0.001 (1)
C20.048 (2)0.049 (2)0.037 (2)0.010 (1)0.008 (1)0.004 (1)
C30.063 (2)0.048 (2)0.051 (2)0.012 (2)0.017 (2)0.010 (2)
C40.040 (2)0.035 (2)0.081 (2)0.013 (1)0.010 (2)0.004 (2)
C50.035 (2)0.032 (1)0.072 (2)0.005 (1)0.014 (1)0.002 (1)
C60.034 (1)0.030 (1)0.041 (2)0.002 (1)0.007 (1)0.003 (1)
C70.024 (1)0.028 (1)0.030 (1)0.001 (1)0.003 (1)0.002 (1)
C80.032 (1)0.031 (1)0.042 (2)0.001 (1)0.001 (1)0.001 (1)
C90.037 (2)0.045 (2)0.047 (2)0.003 (1)0.009 (1)0.014 (1)
C100.036 (2)0.059 (2)0.034 (1)0.008 (1)0.008 (1)0.009 (1)
C110.034 (1)0.045 (2)0.030 (1)0.008 (1)0.001 (1)0.005 (1)
C120.026 (1)0.032 (1)0.031 (1)0.001 (1)0.004 (1)0.000 (1)
C130.027 (1)0.031 (1)0.034 (1)0.002 (1)0.002 (1)0.007 (1)
C140.099 (3)0.043 (2)0.042 (2)0.009 (2)0.018 (2)0.011 (1)
C150.147 (4)0.065 (3)0.044 (2)0.005 (2)0.016 (2)0.026 (2)
C160.101 (3)0.048 (2)0.063 (2)0.013 (2)0.006 (2)0.032 (2)
C170.060 (2)0.030 (2)0.064 (2)0.009 (1)0.018 (2)0.009 (1)
C180.042 (2)0.034 (1)0.039 (1)0.008 (1)0.007 (1)0.006 (1)
C190.025 (1)0.037 (2)0.032 (1)0.003 (1)0.003 (1)0.005 (1)
C200.044 (2)0.043 (2)0.039 (2)0.007 (1)0.003 (1)0.008 (1)
C210.038 (1)0.032 (1)0.037 (1)0.006 (1)0.003 (1)0.008 (1)
C220.066 (2)0.032 (2)0.036 (2)0.013 (1)0.015 (1)0.005 (1)
C230.077 (2)0.038 (2)0.034 (2)0.003 (2)0.008 (2)0.009 (1)
C240.050 (2)0.038 (2)0.040 (2)0.001 (1)0.012 (1)0.010 (1)
C250.036 (1)0.022 (1)0.033 (1)0.002 (1)0.009 (1)0.000 (1)
C260.026 (1)0.030 (1)0.036 (1)0.001 (1)0.010 (1)0.001 (1)
C270.034 (1)0.031 (1)0.054 (2)0.004 (1)0.016 (1)0.002 (1)
C280.030 (1)0.038 (2)0.068 (2)0.012 (1)0.010 (1)0.009 (2)
C290.026 (1)0.041 (2)0.057 (2)0.006 (1)0.003 (1)0.010 (1)
C300.023 (1)0.033 (1)0.040 (1)0.001 (1)0.001 (1)0.005 (1)
C310.034 (1)0.032 (1)0.031 (1)0.003 (1)0.002 (1)0.009 (1)
C320.042 (2)0.045 (2)0.042 (2)0.002 (1)0.011 (1)0.010 (1)
C330.056 (2)0.055 (2)0.039 (2)0.010 (2)0.018 (1)0.010 (1)
C340.071 (2)0.047 (2)0.030 (1)0.011 (2)0.003 (1)0.002 (1)
C350.050 (2)0.044 (2)0.036 (2)0.001 (1)0.004 (1)0.004 (1)
Geometric parameters (Å, º) top
Sn1—C12.130 (2)C25—C261.478 (3)
Sn1—C72.126 (2)C26—C271.395 (3)
Sn1—C132.126 (2)C27—C281.372 (4)
Sn1—O12.221 (2)C28—C291.373 (4)
Sn1—O1w2.274 (2)C29—C301.391 (3)
F1—C201.330 (3)C30—C311.486 (3)
F2—C201.331 (3)C31—C321.391 (3)
F3—C201.321 (3)C32—C331.384 (4)
O1—C191.276 (3)C33—C341.363 (4)
O2—C191.211 (3)C34—C351.384 (4)
N1—C211.337 (3)O1w—H1w10.84 (1)
N1—C251.345 (3)O1w—H1w20.84 (1)
N2—C301.336 (3)C2—H20.95
N2—C261.352 (3)C3—H30.95
N3—C351.341 (3)C4—H40.95
N3—C311.347 (3)C5—H50.95
C1—C61.379 (3)C6—H60.95
C1—C21.393 (4)C8—H80.95
C2—C31.397 (4)C9—H90.95
C3—C41.376 (4)C10—H100.95
C4—C51.374 (4)C11—H110.95
C5—C61.394 (3)C12—H120.95
C7—C121.398 (3)C14—H140.95
C7—C81.402 (3)C15—H150.95
C8—C91.387 (3)C16—H160.95
C9—C101.386 (4)C17—H170.95
C10—C111.378 (4)C18—H180.95
C11—C121.387 (3)C21—H210.95
C13—C141.391 (4)C22—H220.95
C13—C181.399 (3)C23—H230.95
C14—C151.383 (4)C24—H240.95
C15—C161.374 (5)C27—H270.95
C16—C171.372 (4)C28—H280.95
C17—C181.387 (4)C29—H290.95
C19—C201.546 (3)C32—H320.95
C21—C221.392 (4)C33—H330.95
C22—C231.376 (4)C34—H340.95
C23—C241.366 (4)C35—H350.95
C24—C251.394 (3)
C1—Sn1—C7118.5 (1)N3—C31—C32121.4 (2)
C1—Sn1—C13123.8 (1)N3—C31—C30116.4 (2)
C1—Sn1—O191.0 (1)C32—C31—C30122.2 (2)
C1—Sn1—O1w91.4 (1)C33—C32—C31119.7 (3)
C7—Sn1—C13117.3 (1)C34—C33—C32119.0 (3)
C7—Sn1—O198.4 (1)C33—C34—C35118.6 (3)
C7—Sn1—O1w85.8 (1)N3—C35—C34123.5 (3)
C13—Sn1—O187.5 (1)Sn1—O1w—H1w1116 (2)
C13—Sn1—O1w86.0 (1)Sn1—O1w—H1w2112 (2)
O1—Sn1—O1w173.4 (1)H1w1—O1w—H1w2106 (3)
C19—O1—Sn1118.2 (2)C1—C2—H2119.9
C21—N1—C25118.0 (2)C3—C2—H2119.9
C30—N2—C26118.4 (2)C4—C3—H3120.0
C35—N3—C31117.8 (2)C2—C3—H3120.0
C6—C1—C2118.9 (2)C5—C4—H4119.8
C6—C1—Sn1119.7 (2)C3—C4—H4119.8
C2—C1—Sn1121.3 (2)C4—C5—H5120.1
C1—C2—C3120.2 (3)C6—C5—H5120.1
C4—C3—C2119.9 (3)C1—C6—H6119.6
C5—C4—C3120.3 (2)C5—C6—H6119.6
C4—C5—C6119.7 (3)C9—C8—H8119.7
C1—C6—C5120.9 (2)C7—C8—H8119.7
C12—C7—C8118.0 (2)C10—C9—H9119.9
C12—C7—Sn1121.8 (2)C8—C9—H9119.9
C8—C7—Sn1120.1 (2)C11—C10—H10120.1
C9—C8—C7120.7 (2)C9—C10—H10120.1
C10—C9—C8120.3 (2)C10—C11—H11119.9
C11—C10—C9119.8 (2)C12—C11—H11119.9
C10—C11—C12120.2 (2)C11—C12—H12119.5
C11—C12—C7121.0 (2)C7—C12—H12119.5
C14—C13—C18117.5 (2)C15—C14—H14119.5
C14—C13—Sn1121.3 (2)C13—C14—H14119.5
C18—C13—Sn1121.1 (2)C16—C15—H15119.9
C15—C14—C13121.0 (3)C14—C15—H15119.9
C16—C15—C14120.3 (3)C17—C16—H16119.9
C17—C16—C15120.2 (3)C15—C16—H16119.9
C16—C17—C18119.7 (3)C16—C17—H17120.2
C17—C18—C13121.3 (3)C18—C17—H17120.2
O2—C19—O1129.2 (2)C17—C18—H18119.4
O2—C19—C20118.6 (2)C13—C18—H18119.4
O1—C19—C20112.2 (2)N1—C21—H21118.5
F3—C20—F1108.1 (2)C22—C21—H21118.5
F3—C20—F2107.0 (2)C23—C22—H22120.8
F1—C20—F2106.0 (2)C21—C22—H22120.8
F3—C20—C19112.0 (2)C24—C23—H23120.4
F1—C20—C19112.4 (2)C22—C23—H23120.4
F2—C20—C19110.9 (2)C23—C24—H24120.1
N1—C21—C22123.1 (3)C25—C24—H24120.1
C23—C22—C21118.4 (3)C28—C27—H27120.9
C24—C23—C22119.1 (3)C26—C27—H27120.9
C23—C24—C25119.8 (3)C27—C28—H28120.2
N1—C25—C24121.6 (2)C29—C28—H28120.2
N1—C25—C26116.0 (2)C28—C29—H29120.3
C24—C25—C26122.4 (2)C30—C29—H29120.3
N2—C26—C27122.5 (2)C33—C32—H32120.1
N2—C26—C25116.5 (2)C31—C32—H32120.1
C27—C26—C25121.0 (2)C34—C33—H33120.5
C28—C27—C26118.2 (2)C32—C33—H33120.5
C27—C28—C29119.7 (2)C33—C34—H34120.7
C28—C29—C30119.5 (3)C35—C34—H34120.7
N2—C30—C29121.8 (2)N3—C35—H35118.2
N2—C30—C31117.7 (2)C34—C35—H35118.2
C29—C30—C31120.6 (2)
C7—Sn1—O1—C1961.9 (2)C15—C16—C17—C180.6 (5)
C13—Sn1—O1—C19179.1 (2)C16—C17—C18—C130.2 (4)
C1—Sn1—O1—C1957.1 (2)C14—C13—C18—C170.7 (4)
C7—Sn1—C1—C639.5 (2)Sn1—C13—C18—C17180.0 (2)
C13—Sn1—C1—C6132.7 (2)Sn1—O1—C19—O26.4 (3)
O1—Sn1—C1—C6139.6 (2)Sn1—O1—C19—C20173.5 (1)
O1w—Sn1—C1—C646.5 (2)O2—C19—C20—F313.2 (3)
C7—Sn1—C1—C2137.5 (2)O1—C19—C20—F3167.0 (2)
C13—Sn1—C1—C250.3 (2)O2—C19—C20—F1135.1 (2)
O1—Sn1—C1—C237.4 (2)O1—C19—C20—F145.0 (3)
O1w—Sn1—C1—C2136.5 (2)O2—C19—C20—F2106.4 (3)
C6—C1—C2—C31.7 (4)O1—C19—C20—F273.5 (3)
Sn1—C1—C2—C3178.7 (2)C25—N1—C21—C220.6 (3)
C1—C2—C3—C40.0 (4)N1—C21—C22—C230.6 (4)
C2—C3—C4—C52.0 (4)C21—C22—C23—C241.5 (4)
C3—C4—C5—C62.2 (4)C22—C23—C24—C251.3 (4)
C2—C1—C6—C51.5 (4)C21—N1—C25—C240.8 (3)
Sn1—C1—C6—C5178.5 (2)C21—N1—C25—C26177.8 (2)
C4—C5—C6—C10.5 (4)C23—C24—C25—N10.1 (4)
C13—Sn1—C7—C12179.8 (2)C23—C24—C25—C26178.6 (2)
C1—Sn1—C7—C127.5 (2)C30—N2—C26—C271.6 (3)
O1—Sn1—C7—C1288.2 (2)C30—N2—C26—C25176.1 (2)
O1w—Sn1—C7—C1296.9 (2)N1—C25—C26—N231.8 (3)
C13—Sn1—C7—C84.5 (2)C24—C25—C26—N2149.6 (2)
C1—Sn1—C7—C8168.2 (2)N1—C25—C26—C27145.9 (2)
O1—Sn1—C7—C896.1 (2)C24—C25—C26—C2732.7 (3)
O1w—Sn1—C7—C878.8 (2)N2—C26—C27—C281.2 (4)
C12—C7—C8—C90.6 (3)C25—C26—C27—C28176.4 (2)
Sn1—C7—C8—C9175.2 (2)C26—C27—C28—C290.3 (4)
C7—C8—C9—C100.5 (4)C27—C28—C29—C300.2 (4)
C8—C9—C10—C111.3 (4)C26—N2—C30—C291.0 (3)
C9—C10—C11—C121.1 (4)C26—N2—C30—C31178.1 (2)
C10—C11—C12—C70.0 (4)C28—C29—C30—N20.1 (4)
C8—C7—C12—C110.9 (3)C28—C29—C30—C31178.9 (2)
Sn1—C7—C12—C11174.9 (2)C35—N3—C31—C320.4 (4)
C7—Sn1—C13—C14133.3 (2)C35—N3—C31—C30178.9 (2)
C1—Sn1—C13—C1454.5 (3)N2—C30—C31—N325.5 (3)
O1—Sn1—C13—C1435.1 (2)C29—C30—C31—N3153.6 (2)
O1w—Sn1—C13—C14143.5 (2)N2—C30—C31—C32155.2 (2)
C7—Sn1—C13—C1847.4 (2)C29—C30—C31—C3225.7 (4)
C1—Sn1—C13—C18124.8 (2)N3—C31—C32—C330.2 (4)
O1—Sn1—C13—C18145.6 (2)C30—C31—C32—C33179.4 (2)
O1w—Sn1—C13—C1835.7 (2)C31—C32—C33—C340.4 (4)
C18—C13—C14—C150.4 (5)C32—C33—C34—C350.2 (4)
Sn1—C13—C14—C15179.8 (3)C31—N3—C35—C340.7 (4)
C13—C14—C15—C160.3 (6)C33—C34—C35—N30.4 (4)
C14—C15—C16—C170.8 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···N10.84 (1)1.93 (1)2.771 (3)171 (3)
O1w—H1w2···N30.84 (1)1.96 (1)2.797 (3)173 (3)

Experimental details

Crystal data
Chemical formula[Sn(C2F3O2)(C6H5)3(H2O)]·C15H11N3
Mr714.29
Crystal system, space groupMonoclinic, P21/n
Temperature (K)158
a, b, c (Å)10.4257 (7), 10.0510 (7), 30.025 (2)
β (°) 94.265 (1)
V3)3137.6 (4)
Z4
Radiation typeMo Kα
µ (mm1)0.87
Crystal size (mm)0.50 × 0.24 × 0.15
Data collection
DiffractometerBruker SMART area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.744, 0.877
No. of measured, independent and
observed [I > 2σ(I)] reflections
39984, 6320, 5021
Rint0.051
(sin θ/λ)max1)0.626
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.062, 0.95
No. of reflections6320
No. of parameters414
No. of restraints2
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.50, 0.43

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected geometric parameters (Å, º) top
Sn1—C12.130 (2)Sn1—O12.221 (2)
Sn1—C72.126 (2)Sn1—O1w2.274 (2)
Sn1—C132.126 (2)
C1—Sn1—C7118.5 (1)C7—Sn1—O198.4 (1)
C1—Sn1—C13123.8 (1)C7—Sn1—O1w85.8 (1)
C1—Sn1—O191.0 (1)C13—Sn1—O187.5 (1)
C1—Sn1—O1w91.4 (1)C13—Sn1—O1w86.0 (1)
C7—Sn1—C13117.3 (1)O1—Sn1—O1w173.4 (1)
 

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