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The asymmetric unit of the title compound, (C5H4Br2N)2[SnBr6], contains one cation and one half-anion. The anion exhibits a distorted octa­hedral arrangement about the Sn atom, which lies on a crystallographic twofold rotation axis. In the crystal structure, inter­molecular hydrogen bonds and short Br...Br inter­actions cause the formation of a supra­molecular architecture, in which they may be effective in the stabilization of the structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807008069/hk2204sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807008069/hk2204Isup2.hkl
Contains datablock I

CCDC reference: 640367

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](C-C) = 0.010 Å
  • R factor = 0.039
  • wR factor = 0.048
  • Data-to-parameter ratio = 20.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Sn1 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10 PLAT431_ALERT_2_C Short Inter HL..A Contact Br1 .. Br5 .. 3.44 Ang.
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.23 From the CIF: _reflns_number_total 2126 Count of symmetry unique reflns 1203 Completeness (_total/calc) 176.72% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 923 Fraction of Friedel pairs measured 0.767 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXP97 (Sheldrick, 1997); software used to prepare material for publication: SHELXCIF97 (Sheldrick, 1997).

2,5-Dibromopyridinium hexabromidostannate(IV) top
Crystal data top
(C5H4Br2N)2[SnBr6]Dx = 3.047 Mg m3
Mr = 1073.89Mo Kα radiation, λ = 0.71070 Å
Tetragonal, I42dCell parameters from 9875 reflections
Hall symbol: I -4 2bwθ = 1.2–27.9°
a = 24.566 (4) ŵ = 18.16 mm1
c = 7.7555 (12) ÅT = 294 K
V = 4680.4 (13) Å3Block, yellow
Z = 80.20 × 0.20 × 0.10 mm
F(000) = 3856
Data collection top
Rigaku Mercury
diffractometer
2126 independent reflections
Radiation source: fine-focus sealed tube2120 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.063
Detector resolution: 14.6306 pixels mm-1θmax = 25.2°, θmin = 2.3°
data integrate scansh = 2929
Absorption correction: numerical
Shape Tracing Software [Please provide reference]
k = 2923
Tmin = 0.044, Tmax = 0.163l = 99
26765 measured reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.039 w = 1/[σ2(Fo2)]
wR(F2) = 0.048(Δ/σ)max = 0.001
S = 1.21Δρmax = 0.39 e Å3
2126 reflectionsΔρmin = 0.40 e Å3
106 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.000518 (16)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983), 1442 Friedel pairs
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.008 (13)
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
Sn10.59942 (2)0.25000.12500.02781 (16)
Br20.67475 (3)0.25444 (3)0.10868 (10)0.04030 (19)
Br30.52636 (3)0.24040 (3)0.36258 (10)0.0435 (2)
Br10.59987 (3)0.14399 (3)0.09574 (10)0.0467 (2)
Br40.74778 (3)0.12955 (3)0.62230 (12)0.0543 (2)
Br50.49036 (3)0.08634 (4)0.52186 (12)0.0678 (3)
C20.6750 (3)0.1125 (3)0.5845 (9)0.0393 (19)
C50.5661 (3)0.0954 (3)0.5487 (9)0.0423 (18)
C30.6572 (3)0.0692 (3)0.4917 (10)0.044 (2)
H3A0.68200.04550.44090.053*
C40.6027 (3)0.0607 (3)0.4733 (9)0.047 (2)
H4A0.59030.03120.40940.056*
C60.5840 (3)0.1382 (3)0.6383 (10)0.0408 (18)
H6A0.55950.16260.68670.049*
N10.6377 (3)0.1455 (2)0.6579 (7)0.0442 (17)
H1A0.64880.17230.71990.053*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.0293 (4)0.0242 (3)0.0299 (3)0.0000.0000.0011 (3)
Br20.0362 (4)0.0423 (4)0.0424 (4)0.0059 (3)0.0106 (3)0.0037 (4)
Br30.0377 (4)0.0517 (5)0.0412 (4)0.0034 (3)0.0096 (4)0.0096 (4)
Br10.0669 (5)0.0244 (4)0.0486 (5)0.0031 (4)0.0000 (5)0.0006 (4)
Br40.0452 (4)0.0589 (5)0.0589 (5)0.0089 (4)0.0075 (6)0.0031 (4)
Br50.0414 (5)0.0844 (7)0.0776 (7)0.0051 (5)0.0037 (4)0.0010 (6)
C20.034 (4)0.046 (5)0.038 (5)0.004 (4)0.004 (4)0.006 (4)
C50.040 (4)0.049 (5)0.038 (4)0.001 (4)0.004 (4)0.006 (4)
C30.043 (5)0.037 (5)0.052 (5)0.006 (4)0.007 (4)0.015 (4)
C40.058 (6)0.040 (5)0.042 (5)0.000 (4)0.015 (4)0.007 (4)
C60.038 (5)0.045 (5)0.039 (4)0.006 (4)0.003 (4)0.001 (4)
N10.061 (5)0.038 (4)0.034 (4)0.003 (3)0.002 (3)0.012 (3)
Geometric parameters (Å, º) top
Sn1—Br3i2.5830 (9)C2—C31.356 (9)
Sn1—Br32.5830 (9)C5—C61.334 (9)
Sn1—Br2i2.5925 (9)C5—C41.370 (10)
Sn1—Br22.5925 (9)C3—C41.363 (9)
Sn1—Br12.6141 (9)C3—H3A0.9300
Sn1—Br1i2.6141 (9)C4—H4A0.9300
Br4—C21.860 (7)C6—N11.339 (8)
Br5—C51.886 (7)C6—H6A0.9300
C2—N11.349 (8)N1—H1A0.8600
Br3i—Sn1—Br391.96 (13)C3—C2—Br4124.7 (6)
Br3i—Sn1—Br2i176.87 (3)C6—C5—C4119.8 (7)
Br3—Sn1—Br2i89.63 (12)C6—C5—Br5118.4 (6)
Br3i—Sn1—Br289.63 (12)C4—C5—Br5121.7 (6)
Br3—Sn1—Br2176.87 (3)C2—C3—C4119.4 (7)
Br2i—Sn1—Br288.91 (13)C2—C3—H3A120.3
Br3i—Sn1—Br191.83 (3)C4—C3—H3A120.3
Br3—Sn1—Br188.50 (3)C3—C4—C5120.3 (7)
Br2i—Sn1—Br190.90 (3)C3—C4—H4A119.9
Br2—Sn1—Br188.75 (3)C5—C4—H4A119.9
Br3i—Sn1—Br1i88.50 (3)C5—C6—N1119.3 (7)
Br3—Sn1—Br1i91.83 (3)C5—C6—H6A120.4
Br2i—Sn1—Br1i88.75 (3)N1—C6—H6A120.4
Br2—Sn1—Br1i90.90 (3)C6—N1—C2122.7 (6)
Br1—Sn1—Br1i179.52 (4)C6—N1—H1A118.7
N1—C2—C3118.5 (6)C2—N1—H1A118.7
N1—C2—Br4116.8 (5)
N1—C2—C3—C40.9 (11)C4—C5—C6—N12.2 (11)
Br4—C2—C3—C4179.7 (5)Br5—C5—C6—N1179.6 (5)
C2—C3—C4—C50.3 (11)C5—C6—N1—C22.8 (11)
C6—C5—C4—C31.0 (11)C3—C2—N1—C62.2 (10)
Br5—C5—C4—C3178.3 (5)Br4—C2—N1—C6178.9 (5)
Symmetry code: (i) x, y+1/2, z+1/4.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3—H3A···Br3ii0.932.923.566 (9)128
N1—H1A···Br2iii0.862.503.357 (7)175
Symmetry codes: (ii) y+1, x+1/2, z+1/4; (iii) x, y, z+1.
 

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