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The crystal structure of the double salt tetrakis­(anilinium) hexa­chloro­tin(IV) dichloride, (C6H8N)4[SnCl6]Cl2, exhibits alternating inorganic and organic layers parallel to the ab plane. In the inorganic layer, ammonium groups interact with chloride anions and isolated tilted [SnCl6]2− octahedra through N—H...Cl hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804004258/rn6013sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804004258/rn6013Isup2.hkl
Contains datablock I

CCDC reference: 236054

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.043
  • wR factor = 0.104
  • Data-to-parameter ratio = 31.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C1 PLAT331_ALERT_2_C Small Average Phenyl C-C Dist. C1 -C6 1.37 Ang. PLAT331_ALERT_2_C Small Average Phenyl C-C Dist. C7 -C12 1.37 Ang. PLAT331_ALERT_2_C Small Average Phenyl C-C Dist. C13 -C18 1.37 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999) and PLATON (Spek, 2000).

Tetrakis(anilinium) hexachlorotin(IV) dichloride top
Crystal data top
(C6H8N)4[SnCl6]Cl2F(000) = 1560
Mr = 778.83Dx = 1.541 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 185 reflections
a = 15.615 (4) Åθ = 2–32°
b = 10.543 (4) ŵ = 1.42 mm1
c = 20.403 (5) ÅT = 293 K
β = 92.40 (2)°Block, light brown
V = 3355.9 (17) Å30.50 × 0.20 × 0.20 mm
Z = 4
Data collection top
Oxford Excalibur2
diffractometer
10736 independent reflections
Radiation source: fine-focus sealed tube5357 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
ω–2θ scansθmax = 31.9°, θmin = 4.0°
Absorption correction: multi-scan
(Blessing, 1995)
h = 2222
Tmin = 0.532, Tmax = 0.757k = 1215
30679 measured reflectionsl = 2929
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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.104H-atom parameters constrained
S = 0.92 w = 1/[σ2(Fo2) + (0.0411P)2]
where P = (Fo2 + 2Fc2)/3
10736 reflections(Δ/σ)max = 0.005
338 parametersΔρmax = 1.02 e Å3
60 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
N20.25134 (19)0.1246 (2)0.16768 (12)0.0504 (7)
H2A0.20650.09200.19010.076*
H2B0.24770.20880.16800.076*
H2C0.29940.10080.18620.076*
N30.25710 (19)0.1214 (2)0.68417 (12)0.0523 (7)
H3A0.26250.20540.68630.078*
H3B0.30160.08510.70540.078*
H3C0.20890.09820.70260.078*
N10.4587 (2)0.8032 (3)0.19859 (15)0.0636 (9)
H1C0.49410.86280.21450.095*
H1A0.46530.73280.22230.095*
H1B0.40480.83020.20040.095*
N40.00100 (19)0.2450 (3)0.30654 (14)0.0648 (9)
H4A0.00670.16510.29320.097*
H4B0.04490.29090.29330.097*
H4C0.04780.27690.28960.097*
C240.0383 (2)0.3470 (3)0.41180 (19)0.0546 (9)
H240.06460.41180.38920.066*
C190.0002 (2)0.2482 (3)0.37854 (17)0.0450 (8)
C230.0374 (2)0.3491 (4)0.4793 (2)0.0636 (11)
H230.06340.41540.50270.076*
C220.0020 (2)0.2531 (4)0.5117 (2)0.0675 (11)
H220.00300.25520.55730.081*
C200.0396 (2)0.1518 (3)0.41058 (19)0.0550 (9)
H200.06580.08570.38720.066*
C210.0397 (3)0.1547 (4)0.4785 (2)0.0638 (11)
H210.06550.08960.50120.077*
Cl70.10229 (5)0.00270 (8)0.75179 (4)0.0504 (2)
Cl80.58691 (6)0.02214 (9)0.23994 (5)0.0609 (3)
C10.4781 (2)0.7764 (3)0.13001 (18)0.0496 (9)
C20.5265 (3)0.6724 (4)0.1173 (2)0.0722 (12)
H20.54780.62110.15130.087*
C30.5429 (3)0.6452 (4)0.0538 (3)0.0849 (14)
H30.57500.57360.04450.102*
C40.5134 (3)0.7210 (5)0.0036 (2)0.0839 (14)
H40.52580.70200.03950.101*
C60.4469 (3)0.8535 (4)0.0819 (2)0.0666 (11)
H60.41390.92370.09200.080*
C50.4643 (3)0.8271 (4)0.0178 (2)0.0769 (12)
H50.44350.87970.01580.092*
Sn0.230329 (14)0.00050 (2)0.257819 (10)0.03698 (7)
Cl10.12090 (5)0.10126 (8)0.32113 (4)0.0527 (2)
Cl20.34470 (5)0.09625 (8)0.19576 (4)0.0500 (2)
Cl50.23704 (6)0.19009 (7)0.18993 (4)0.0516 (2)
Cl60.34200 (5)0.09639 (7)0.33004 (4)0.0457 (2)
Cl40.22586 (6)0.18760 (8)0.32433 (4)0.0554 (2)
C160.2473 (2)0.0041 (4)0.48740 (17)0.0557 (9)
H160.24550.02160.44380.067*
C130.2543 (2)0.0810 (3)0.61508 (15)0.0400 (7)
C150.2930 (3)0.0643 (4)0.53349 (19)0.0626 (11)
H150.32170.13730.52120.075*
C140.2970 (3)0.0261 (3)0.59813 (18)0.0557 (10)
H140.32820.07250.62960.067*
C180.2067 (2)0.1487 (3)0.56973 (17)0.0566 (10)
H180.17640.22000.58230.068*
C170.2041 (3)0.1105 (4)0.50532 (18)0.0615 (10)
H170.17280.15710.47390.074*
Cl30.12225 (6)0.08995 (9)0.18308 (4)0.0550 (2)
C100.2499 (3)0.0069 (4)0.02631 (18)0.0631 (10)
H100.24930.03640.06930.076*
C80.2916 (2)0.0344 (3)0.08414 (18)0.0535 (9)
H80.31890.08100.11580.064*
C70.2521 (2)0.0784 (3)0.09941 (15)0.0407 (7)
C90.2895 (3)0.0765 (4)0.0204 (2)0.0658 (11)
H90.31530.15330.00890.079*
C110.2118 (3)0.1045 (4)0.00994 (17)0.0608 (10)
H110.18540.15180.04190.073*
C120.2119 (2)0.1486 (3)0.05360 (17)0.0532 (9)
H120.18510.22470.06510.064*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N20.067 (2)0.0447 (16)0.0391 (16)0.0066 (14)0.0030 (14)0.0021 (12)
N30.070 (2)0.0429 (16)0.0449 (17)0.0045 (14)0.0095 (15)0.0036 (13)
N10.060 (2)0.064 (2)0.067 (2)0.0042 (16)0.0062 (17)0.0076 (17)
N40.064 (2)0.072 (2)0.058 (2)0.0167 (17)0.0000 (16)0.0010 (17)
C240.053 (2)0.042 (2)0.069 (3)0.0071 (16)0.0014 (19)0.0013 (18)
C190.0381 (19)0.0433 (19)0.053 (2)0.0006 (15)0.0002 (16)0.0013 (16)
C230.055 (2)0.060 (2)0.075 (3)0.005 (2)0.007 (2)0.023 (2)
C220.055 (2)0.089 (3)0.059 (3)0.014 (2)0.004 (2)0.003 (2)
C200.051 (2)0.048 (2)0.067 (3)0.0077 (17)0.0010 (19)0.0044 (18)
C210.061 (3)0.065 (3)0.066 (3)0.005 (2)0.015 (2)0.014 (2)
Cl70.0432 (4)0.0510 (5)0.0571 (5)0.0009 (4)0.0016 (4)0.0087 (4)
Cl80.0458 (5)0.0752 (7)0.0616 (6)0.0024 (4)0.0021 (4)0.0162 (5)
C10.042 (2)0.047 (2)0.060 (2)0.0044 (16)0.0068 (17)0.0091 (18)
C20.057 (3)0.065 (3)0.096 (4)0.018 (2)0.017 (2)0.011 (2)
C30.082 (3)0.070 (3)0.105 (4)0.021 (3)0.032 (3)0.007 (3)
C40.089 (4)0.098 (4)0.067 (3)0.022 (3)0.030 (3)0.020 (3)
C60.067 (3)0.052 (2)0.081 (3)0.016 (2)0.006 (2)0.003 (2)
C50.077 (3)0.085 (3)0.069 (3)0.001 (3)0.001 (2)0.008 (3)
Sn0.04106 (12)0.03370 (11)0.03631 (11)0.00154 (10)0.00331 (8)0.00081 (9)
Cl10.0470 (5)0.0606 (5)0.0512 (5)0.0022 (4)0.0096 (4)0.0107 (4)
Cl20.0494 (5)0.0439 (5)0.0577 (5)0.0007 (4)0.0157 (4)0.0037 (4)
Cl50.0682 (6)0.0422 (5)0.0440 (5)0.0023 (4)0.0002 (4)0.0100 (4)
Cl60.0464 (5)0.0418 (4)0.0480 (5)0.0002 (4)0.0072 (4)0.0001 (4)
Cl40.0747 (6)0.0406 (5)0.0509 (5)0.0081 (4)0.0050 (5)0.0101 (4)
C160.060 (2)0.065 (2)0.0424 (19)0.002 (2)0.0073 (17)0.008 (2)
C130.0468 (19)0.0350 (17)0.0384 (18)0.0048 (14)0.0060 (15)0.0004 (14)
C150.067 (3)0.055 (2)0.066 (3)0.015 (2)0.006 (2)0.015 (2)
C140.070 (3)0.044 (2)0.052 (2)0.0128 (17)0.0067 (19)0.0020 (16)
C180.071 (3)0.048 (2)0.051 (2)0.0212 (19)0.006 (2)0.0019 (17)
C170.074 (3)0.063 (3)0.047 (2)0.016 (2)0.0038 (19)0.0030 (19)
Cl30.0497 (5)0.0650 (6)0.0497 (5)0.0078 (4)0.0026 (4)0.0139 (4)
C100.065 (3)0.082 (3)0.042 (2)0.007 (2)0.0042 (18)0.015 (2)
C80.063 (2)0.043 (2)0.056 (2)0.0036 (17)0.0129 (19)0.0040 (16)
C70.0467 (19)0.0374 (18)0.0376 (18)0.0105 (15)0.0011 (15)0.0024 (14)
C90.064 (3)0.052 (2)0.081 (3)0.007 (2)0.001 (2)0.026 (2)
C110.070 (3)0.073 (3)0.040 (2)0.004 (2)0.0051 (19)0.0056 (19)
C120.064 (2)0.046 (2)0.049 (2)0.0087 (17)0.0012 (18)0.0025 (17)
Geometric parameters (Å, º) top
N2—C71.475 (4)C4—C51.393 (6)
N2—H2A0.8900C4—H40.9300
N2—H2B0.8900C6—C51.374 (5)
N2—H2C0.8900C6—H60.9300
N3—C131.472 (4)C5—H50.9300
N3—H3A0.8900Sn—Cl42.4057 (10)
N3—H3B0.8900Sn—Cl32.4223 (10)
N3—H3C0.8900Sn—Cl12.4292 (10)
N1—C11.472 (4)Sn—Cl52.4366 (10)
N1—H1C0.8900Sn—Cl62.4533 (10)
N1—H1A0.8900Sn—Cl22.4541 (10)
N1—H1B0.8900C16—C151.363 (5)
N4—C191.470 (4)C16—C171.367 (5)
N4—H4A0.8900C16—H160.9300
N4—H4B0.8900C13—C141.363 (4)
N4—H4C0.8900C13—C181.364 (4)
C24—C191.368 (4)C15—C141.378 (5)
C24—C231.378 (5)C15—H150.9300
C24—H240.9300C14—H140.9300
C19—C201.369 (4)C18—C171.373 (4)
C23—C221.370 (5)C18—H180.9300
C23—H230.9300C17—H170.9300
C22—C211.359 (5)C10—C111.353 (5)
C22—H220.9300C10—C91.370 (5)
C20—C211.386 (5)C10—H100.9300
C20—H200.9300C8—C71.369 (4)
C21—H210.9300C8—C91.376 (5)
C1—C61.350 (5)C8—H80.9300
C1—C21.362 (5)C7—C121.365 (4)
C2—C31.362 (5)C9—H90.9300
C2—H20.9300C11—C121.377 (4)
C3—C41.363 (6)C11—H110.9300
C3—H30.9300C12—H120.9300
C7—N2—H2A109.5C5—C6—H6120.3
C7—N2—H2B109.5C6—C5—C4119.5 (4)
H2A—N2—H2B109.5C6—C5—H5120.3
C7—N2—H2C109.5C4—C5—H5120.3
H2A—N2—H2C109.5Cl4—Sn—Cl389.70 (4)
H2B—N2—H2C109.5Cl4—Sn—Cl191.31 (4)
C13—N3—H3A109.5Cl3—Sn—Cl191.14 (4)
C13—N3—H3B109.5Cl4—Sn—Cl5179.12 (3)
H3A—N3—H3B109.5Cl3—Sn—Cl590.60 (4)
C13—N3—H3C109.5Cl1—Sn—Cl589.51 (4)
H3A—N3—H3C109.5Cl4—Sn—Cl692.15 (3)
H3B—N3—H3C109.5Cl3—Sn—Cl6177.85 (3)
C1—N1—H1C109.5Cl1—Sn—Cl689.92 (3)
C1—N1—H1A109.5Cl5—Sn—Cl687.53 (3)
H1C—N1—H1A109.5Cl4—Sn—Cl289.28 (4)
C1—N1—H1B109.5Cl3—Sn—Cl290.83 (4)
H1C—N1—H1B109.5Cl1—Sn—Cl2177.95 (3)
H1A—N1—H1B109.5Cl5—Sn—Cl289.89 (3)
C19—N4—H4A109.5Cl6—Sn—Cl288.10 (3)
C19—N4—H4B109.5C15—C16—C17120.0 (3)
H4A—N4—H4B109.5C15—C16—H16120.0
C19—N4—H4C109.5C17—C16—H16120.0
H4A—N4—H4C109.5C14—C13—C18121.3 (3)
H4B—N4—H4C109.5C14—C13—N3119.2 (3)
C19—C24—C23119.0 (3)C18—C13—N3119.5 (3)
C19—C24—H24120.5C16—C15—C14120.4 (3)
C23—C24—H24120.5C16—C15—H15119.8
C24—C19—C20121.7 (3)C14—C15—H15119.8
C24—C19—N4119.3 (3)C13—C14—C15118.8 (3)
C20—C19—N4119.0 (3)C13—C14—H14120.6
C22—C23—C24119.6 (4)C15—C14—H14120.6
C22—C23—H23120.2C13—C18—C17119.3 (3)
C24—C23—H23120.2C13—C18—H18120.3
C21—C22—C23121.1 (4)C17—C18—H18120.3
C21—C22—H22119.4C16—C17—C18120.1 (3)
C23—C22—H22119.4C16—C17—H17120.0
C19—C20—C21118.7 (3)C18—C17—H17120.0
C19—C20—H20120.7C11—C10—C9120.0 (3)
C21—C20—H20120.7C11—C10—H10120.0
C22—C21—C20119.8 (4)C9—C10—H10120.0
C22—C21—H21120.1C7—C8—C9117.8 (3)
C20—C21—H21120.1C7—C8—H8121.1
C6—C1—C2122.2 (4)C9—C8—H8121.1
C6—C1—N1119.6 (3)C12—C7—C8122.0 (3)
C2—C1—N1118.3 (4)C12—C7—N2118.8 (3)
C1—C2—C3118.6 (4)C8—C7—N2119.1 (3)
C1—C2—H2120.7C10—C9—C8120.9 (3)
C3—C2—H2120.7C10—C9—H9119.5
C2—C3—C4121.3 (4)C8—C9—H9119.5
C2—C3—H3119.4C10—C11—C12120.5 (4)
C4—C3—H3119.4C10—C11—H11119.7
C3—C4—C5119.1 (4)C12—C11—H11119.7
C3—C4—H4120.4C7—C12—C11118.7 (3)
C5—C4—H4120.4C7—C12—H12120.7
C1—C6—C5119.3 (4)C11—C12—H12120.7
C1—C6—H6120.3
C23—C24—C19—C200.2 (5)C17—C16—C15—C140.9 (6)
C23—C24—C19—N4179.6 (3)C18—C13—C14—C151.4 (6)
C19—C24—C23—C220.3 (6)N3—C13—C14—C15179.1 (3)
C24—C23—C22—C210.6 (6)C16—C15—C14—C130.2 (6)
C24—C19—C20—C210.5 (5)C14—C13—C18—C172.2 (6)
N4—C19—C20—C21179.3 (3)N3—C13—C18—C17179.8 (3)
C23—C22—C21—C200.9 (6)C15—C16—C17—C180.1 (6)
C19—C20—C21—C220.9 (6)C13—C18—C17—C161.4 (6)
C6—C1—C2—C30.6 (6)C9—C8—C7—C120.3 (5)
N1—C1—C2—C3178.4 (4)C9—C8—C7—N2178.5 (3)
C1—C2—C3—C41.2 (7)C11—C10—C9—C80.3 (6)
C2—C3—C4—C51.0 (7)C7—C8—C9—C100.7 (6)
C2—C1—C6—C50.2 (6)C9—C10—C11—C120.4 (6)
N1—C1—C6—C5179.2 (4)C8—C7—C12—C110.5 (5)
C1—C6—C5—C40.4 (7)N2—C7—C12—C11179.2 (3)
C3—C4—C5—C60.1 (7)C10—C11—C12—C70.8 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···Cl7i0.892.213.098 (3)175
N2—H2B···Cl6ii0.892.533.266 (3)141
N2—H2B···Cl1ii0.892.823.538 (3)139
N2—H2C···Cl8iii0.892.283.167 (3)173
N3—H3A···Cl2iv0.892.463.280 (3)154
N3—H3B···Cl8v0.892.323.210 (3)176
N3—H3C···Cl70.892.223.097 (3)168
N1—H1C···Cl8vi0.892.263.148 (3)172
N1—H1A···Cl8vii0.892.503.307 (3)151
N1—H1B···Cl5vi0.892.633.459 (3)156
N4—H4A···Cl7viii0.892.603.267 (3)133
N4—H4B···Cl7ix0.892.513.313 (3)150
N4—H4C···Cl1x0.892.803.553 (3)143
Symmetry codes: (i) x, y, z1; (ii) x, y1/2, z1/2; (iii) x+1, y, z; (iv) x, y+1/2, z+1/2; (v) x+1, y, z+1; (vi) x, y+1, z; (vii) x+1, y+1/2, z+1/2; (viii) x, y, z+1; (ix) x, y+1/2, z1/2; (x) x, y+1/2, z+1/2.
 

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