Download citation
Download citation
link to html
In the title compound, (C7H9Br2N2)2[SnBr6], the cations and centrosymmetric anions are stacked in alternating layers that show no significant inter­molecular inter­actions within each stack. Extensive cation...[SnBr6]2− inter­actions are found, represented by short Br...Br inter­actions, along with different Br...HN (pyridine and amine) and weaker Br...HCH2 hydrogen-bonding motifs.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107006452/ga3039sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270107006452/ga3039Isup2.hkl
Contains datablock I

CCDC reference: 645506

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus; program(s) used to solve structure: XS in SHELXTL (Sheldrick, 2004); program(s) used to refine structure: XL in SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: XCIF in SHELXTL.

Bis(2-amino-3,5-dibromo-4,6-dimethylpyridinium) hexabromidostannate(IV) top
Crystal data top
(C7H9Br2N2)2[SnBr6]Z = 2
Mr = 1160.11F(000) = 1060
Triclinic, P1Dx = 2.794 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.8574 (11) ÅCell parameters from 6288 reflections
b = 11.4847 (13) Åθ = 2.3–29.2°
c = 12.5957 (14) ŵ = 15.43 mm1
α = 94.245 (2)°T = 297 K
β = 103.258 (2)°Needle, yellow
γ = 93.898 (2)°0.20 × 0.11 × 0.06 mm
V = 1378.8 (3) Å3
Data collection top
Bruker SMART APEX
diffractometer
4979 independent reflections
Radiation source: normal-focus sealed tube4034 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Detector resolution: 8.3 pixels mm-1θmax = 25.3°, θmin = 1.7°
ω scansh = 1111
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
k = 1313
Tmin = 0.129, Tmax = 0.398l = 1515
20574 measured reflections
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.031P)2 + 0.9567P]
where P = (Fo2 + 2Fc2)/3
4979 reflections(Δ/σ)max = 0.001
269 parametersΔρmax = 0.96 e Å3
0 restraintsΔρmin = 0.58 e Å3
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
Br10.35361 (7)0.83736 (5)0.35026 (5)0.05546 (18)
Br20.72521 (7)0.93039 (6)0.45831 (5)0.05812 (19)
Br30.49589 (6)1.14973 (5)0.35498 (4)0.04422 (15)
Br40.75832 (6)0.46796 (6)0.01171 (5)0.05345 (17)
Br50.57305 (7)0.63247 (5)0.18713 (5)0.05168 (17)
Br60.47102 (6)0.31392 (5)0.10135 (5)0.04632 (16)
Br70.69803 (7)0.58116 (6)0.71103 (5)0.05476 (17)
Br81.01399 (7)0.26032 (6)0.52141 (7)0.0693 (2)
Br90.67940 (7)1.03716 (6)1.16141 (5)0.05773 (18)
Br101.00727 (7)0.74291 (5)0.95373 (6)0.06019 (19)
C20.6865 (6)0.5380 (5)0.4871 (4)0.0370 (12)
C30.7548 (6)0.5072 (4)0.5922 (4)0.0384 (13)
C40.8527 (6)0.4272 (5)0.6052 (5)0.0433 (14)
C50.8804 (6)0.3727 (5)0.5096 (5)0.0430 (14)
C60.8132 (6)0.3965 (5)0.4077 (4)0.0395 (13)
C80.7147 (5)1.0448 (5)0.9476 (5)0.0395 (13)
C90.7521 (6)0.9855 (5)1.0420 (4)0.0409 (13)
C100.8367 (6)0.8949 (5)1.0467 (5)0.0425 (14)
C110.8858 (5)0.8639 (5)0.9519 (5)0.0414 (13)
C120.8509 (5)0.9183 (5)0.8591 (5)0.0408 (13)
C4'0.9244 (7)0.3980 (6)0.7173 (5)0.0629 (18)
H4'10.92780.46410.76940.094*
H4'21.01780.37930.71740.094*
H4'30.87340.33190.73680.094*
C6'0.8327 (7)0.3402 (6)0.3020 (5)0.0614 (18)
H6'10.93060.34440.30310.092*
H6'20.78430.38040.24250.092*
H6'30.79580.25960.29270.092*
C10'0.8745 (7)0.8289 (6)1.1458 (5)0.0618 (18)
H10A0.83910.86521.20380.093*
H10B0.97450.83001.16880.093*
H10C0.83430.74941.12840.093*
C12'0.8970 (7)0.8946 (6)0.7562 (5)0.0547 (16)
H12A0.99670.91030.77030.082*
H12B0.85270.94410.70280.082*
H12C0.87130.81390.72880.082*
N10.7188 (4)0.4782 (4)0.4003 (3)0.0393 (11)
H10.67620.49320.33580.047*
N70.7652 (5)1.0069 (4)0.8608 (4)0.0413 (11)
H70.74121.04140.80190.050*
N2'0.5960 (5)0.6181 (4)0.4692 (4)0.0456 (12)
H2'10.55830.63190.40320.055*
H2'20.57480.65650.52350.055*
N8'0.6352 (5)1.1338 (4)0.9370 (4)0.0529 (13)
H8'10.61701.16590.87630.064*
H8'20.60191.15960.99080.064*
Sn10.50001.00000.50000.03184 (13)
Sn20.50000.50000.00000.03429 (14)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0763 (5)0.0401 (3)0.0423 (3)0.0043 (3)0.0012 (3)0.0024 (3)
Br20.0562 (4)0.0732 (5)0.0583 (4)0.0351 (3)0.0275 (3)0.0214 (3)
Br30.0601 (4)0.0409 (3)0.0375 (3)0.0165 (3)0.0161 (3)0.0155 (3)
Br40.0467 (4)0.0609 (4)0.0593 (4)0.0225 (3)0.0169 (3)0.0177 (3)
Br50.0769 (4)0.0472 (4)0.0308 (3)0.0112 (3)0.0111 (3)0.0018 (3)
Br60.0637 (4)0.0405 (3)0.0423 (3)0.0177 (3)0.0208 (3)0.0150 (3)
Br70.0765 (4)0.0539 (4)0.0344 (3)0.0097 (3)0.0141 (3)0.0011 (3)
Br80.0588 (4)0.0585 (4)0.0943 (6)0.0297 (3)0.0153 (4)0.0183 (4)
Br90.0644 (4)0.0611 (4)0.0502 (4)0.0033 (3)0.0213 (3)0.0015 (3)
Br100.0518 (4)0.0421 (4)0.0818 (5)0.0182 (3)0.0032 (3)0.0011 (3)
C20.041 (3)0.034 (3)0.037 (3)0.006 (2)0.009 (2)0.009 (2)
C30.048 (3)0.033 (3)0.034 (3)0.003 (2)0.008 (3)0.005 (2)
C40.042 (3)0.037 (3)0.046 (3)0.000 (3)0.002 (3)0.010 (3)
C50.037 (3)0.038 (3)0.055 (4)0.010 (2)0.008 (3)0.009 (3)
C60.039 (3)0.035 (3)0.042 (3)0.003 (2)0.008 (3)0.000 (3)
C80.031 (3)0.041 (3)0.043 (3)0.009 (2)0.001 (2)0.001 (3)
C90.040 (3)0.039 (3)0.042 (3)0.003 (3)0.007 (3)0.002 (3)
C100.039 (3)0.035 (3)0.049 (4)0.002 (2)0.000 (3)0.006 (3)
C110.036 (3)0.031 (3)0.053 (4)0.007 (2)0.001 (3)0.002 (3)
C120.035 (3)0.040 (3)0.043 (3)0.006 (2)0.003 (3)0.004 (3)
C4'0.072 (5)0.055 (4)0.051 (4)0.005 (3)0.011 (3)0.014 (3)
C6'0.071 (5)0.055 (4)0.057 (4)0.010 (3)0.017 (4)0.010 (3)
C10'0.068 (4)0.056 (4)0.062 (4)0.009 (3)0.012 (4)0.020 (3)
C12'0.055 (4)0.057 (4)0.050 (4)0.005 (3)0.010 (3)0.006 (3)
N10.043 (3)0.045 (3)0.030 (2)0.014 (2)0.006 (2)0.004 (2)
N70.044 (3)0.042 (3)0.035 (3)0.012 (2)0.001 (2)0.004 (2)
N2'0.062 (3)0.045 (3)0.034 (3)0.025 (2)0.011 (2)0.008 (2)
N8'0.058 (3)0.049 (3)0.051 (3)0.021 (3)0.007 (3)0.005 (3)
Sn10.0408 (3)0.0308 (3)0.0269 (3)0.0133 (2)0.0100 (2)0.0065 (2)
Sn20.0434 (3)0.0353 (3)0.0271 (3)0.0148 (2)0.0094 (2)0.0080 (2)
Geometric parameters (Å, º) top
Br1—Sn12.6443 (6)C12—N71.368 (7)
Br2—Sn12.5606 (6)C12—C12'1.482 (8)
Br3—Sn12.5954 (6)C4'—H4'10.9600
Br4—Sn22.5699 (6)C4'—H4'20.9600
Br5—Sn22.6326 (6)C4'—H4'30.9600
Br6—Sn22.6013 (6)C6'—H6'10.9600
Br7—C31.880 (5)C6'—H6'20.9600
Br8—C51.895 (5)C6'—H6'30.9600
Br9—C91.883 (6)C10'—H10A0.9600
Br10—C111.893 (5)C10'—H10B0.9600
C2—N2'1.320 (6)C10'—H10C0.9600
C2—N11.358 (6)C12'—H12A0.9600
C2—C31.423 (7)C12'—H12B0.9600
C3—C41.368 (7)C12'—H12C0.9600
C4—C51.407 (8)N1—H10.8600
C4—C4'1.500 (8)N7—H70.8600
C5—C61.360 (8)N2'—H2'10.8600
C6—N11.360 (6)N2'—H2'20.8600
C6—C6'1.494 (8)N8'—H8'10.8600
C8—N8'1.326 (6)N8'—H8'20.8600
C8—N71.357 (7)Sn1—Br2i2.5606 (6)
C8—C91.402 (7)Sn1—Br3i2.5954 (6)
C9—C101.374 (7)Sn1—Br1i2.6443 (6)
C10—C111.417 (8)Sn2—Br4ii2.5699 (6)
C10—C10'1.496 (8)Sn2—Br6ii2.6013 (6)
C11—C121.352 (8)Sn2—Br5ii2.6326 (6)
N2'—C2—N1119.2 (5)C12—C12'—H12A109.5
N2'—C2—C3125.0 (5)C12—C12'—H12B109.5
N1—C2—C3115.8 (5)H12A—C12'—H12B109.5
C4—C3—C2122.0 (5)C12—C12'—H12C109.5
C4—C3—Br7122.6 (4)H12A—C12'—H12C109.5
C2—C3—Br7115.4 (4)H12B—C12'—H12C109.5
C3—C4—C5117.3 (5)C2—N1—C6125.0 (5)
C3—C4—C4'120.7 (6)C2—N1—H1117.5
C5—C4—C4'122.0 (5)C6—N1—H1117.5
C6—C5—C4122.3 (5)C8—N7—C12125.4 (5)
C6—C5—Br8118.1 (4)C8—N7—H7117.3
C4—C5—Br8119.6 (4)C12—N7—H7117.3
N1—C6—C5117.5 (5)C2—N2'—H2'1120.0
N1—C6—C6'116.6 (5)C2—N2'—H2'2120.0
C5—C6—C6'125.9 (5)H2'1—N2'—H2'2120.0
N8'—C8—N7118.1 (5)C8—N8'—H8'1120.0
N8'—C8—C9125.4 (5)C8—N8'—H8'2120.0
N7—C8—C9116.4 (5)H8'1—N8'—H8'2120.0
C10—C9—C8121.7 (5)Br2i—Sn1—Br2180.0
C10—C9—Br9122.1 (4)Br2i—Sn1—Br391.007 (19)
C8—C9—Br9116.2 (4)Br2—Sn1—Br388.993 (19)
C9—C10—C11117.2 (5)Br2i—Sn1—Br3i88.993 (19)
C9—C10—C10'122.3 (6)Br2—Sn1—Br3i91.007 (19)
C11—C10—C10'120.5 (5)Br3—Sn1—Br3i180.0
C12—C11—C10122.8 (5)Br2i—Sn1—Br190.73 (2)
C12—C11—Br10117.6 (4)Br2—Sn1—Br189.27 (2)
C10—C11—Br10119.6 (4)Br3—Sn1—Br191.50 (2)
C11—C12—N7116.4 (5)Br3i—Sn1—Br188.50 (2)
C11—C12—C12'127.5 (5)Br2i—Sn1—Br1i89.27 (2)
N7—C12—C12'116.1 (5)Br2—Sn1—Br1i90.73 (2)
C4—C4'—H4'1109.5Br3—Sn1—Br1i88.50 (2)
C4—C4'—H4'2109.5Br3i—Sn1—Br1i91.50 (2)
H4'1—C4'—H4'2109.5Br1—Sn1—Br1i180.00 (2)
C4—C4'—H4'3109.5Br4ii—Sn2—Br4180.0
H4'1—C4'—H4'3109.5Br4ii—Sn2—Br689.419 (19)
H4'2—C4'—H4'3109.5Br4—Sn2—Br690.581 (19)
C6—C6'—H6'1109.5Br4ii—Sn2—Br6ii90.581 (19)
C6—C6'—H6'2109.5Br4—Sn2—Br6ii89.419 (19)
H6'1—C6'—H6'2109.5Br6—Sn2—Br6ii180.00 (2)
C6—C6'—H6'3109.5Br4ii—Sn2—Br5ii89.81 (2)
H6'1—C6'—H6'3109.5Br4—Sn2—Br5ii90.19 (2)
H6'2—C6'—H6'3109.5Br6—Sn2—Br5ii88.82 (2)
C10—C10'—H10A109.5Br6ii—Sn2—Br5ii91.18 (2)
C10—C10'—H10B109.5Br4ii—Sn2—Br590.19 (2)
H10A—C10'—H10B109.5Br4—Sn2—Br589.81 (2)
C10—C10'—H10C109.5Br6—Sn2—Br591.18 (2)
H10A—C10'—H10C109.5Br6ii—Sn2—Br588.82 (2)
H10B—C10'—H10C109.5Br5ii—Sn2—Br5180.000 (15)
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···Br50.862.623.419 (4)154
N7—H7···Br1i0.862.503.346 (4)170
N2—H21···Br50.862.763.525 (4)149
N2—H22···Br3i0.862.823.635 (4)158
N8—H81···Br1i0.862.933.683 (5)147
N8—H82···Br6iii0.862.743.542 (5)155
C4—H43···Br1iv0.962.823.622 (7)142
Symmetry codes: (i) x+1, y+2, z+1; (iii) x, y+1, z+1; (iv) x+1, y+1, z+1.
 

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds