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The Fe3+ centre in the complex anion of the title compound, [(C4H9)4N][FeBrCl3], is surrounded by three chloride anions and one bromide anion. The Br atom in [FeBrCl3]- is disordered, replacing Cl atoms. The Fe and N atoms lie on a twofold rotation axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806012402/bt2051sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806012402/bt2051Isup2.hkl
Contains datablock I

CCDC reference: 608375

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.006 Å
  • Disorder in solvent or counterion
  • R factor = 0.063
  • wR factor = 0.164
  • Data-to-parameter ratio = 18.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.04 Ratio PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Fe1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 44.00 Perc.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrysAlis CCD (UNIL IC & Kuma, 2000); cell refinement: CrysAlis RED (UNIL IC & Kuma, 2000); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL/PC (Sheldrick, 1990) and ORTEP-3 (Version 1.062; Farrugia, 1997); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

Tetrabutylammonium bromotrichloroferrate(III) top
Crystal data top
(C16H36N)[FeBrCl3]F(000) = 1004
Mr = 484.57Dx = 1.305 Mg m3
Orthorhombic, PnnaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2a 2bcCell parameters from 4782 reflections
a = 18.5191 (11) Åθ = 5–20°
b = 11.5864 (7) ŵ = 2.55 mm1
c = 11.4957 (7) ÅT = 291 K
V = 2466.6 (3) Å3Prism, orange
Z = 40.35 × 0.27 × 0.14 mm
Data collection top
Kuma KM-4-CCD
diffractometer
2197 independent reflections
Radiation source: fine-focus sealed tube1840 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.089
Detector resolution: 1048576 pixels mm-1θmax = 25.1°, θmin = 3.3°
ω scansh = 2221
Absorption correction: numerical
(X-RED32; Stoe & Cie, 1999)
k = 1310
Tmin = 0.476, Tmax = 0.711l = 1313
24549 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)] = 0.063Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.164H-atom parameters constrained
S = 1.27 w = 1/[σ2(Fo2) + (0.0766P)2]
where P = (Fo2 + 2Fc2)/3
2197 reflections(Δ/σ)max = 0.001
121 parametersΔρmax = 0.30 e Å3
0 restraintsΔρmin = 0.20 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*/UeqOcc. (<1)
Fe10.09291 (4)0.25000.25000.0885 (4)
Cl10.1567 (5)0.3881 (8)0.1895 (7)0.129 (3)0.75
Cl20.0151 (3)0.3010 (5)0.3817 (5)0.158 (2)0.75
Br10.1658 (5)0.3997 (8)0.1763 (7)0.0915 (11)0.25
Br20.0379 (4)0.3429 (5)0.4072 (5)0.1269 (15)0.25
N20.4364 (2)0.25000.25000.0600 (8)
C10.48270 (18)0.3276 (3)0.1730 (3)0.0711 (9)
H1A0.50580.27950.11490.085*
H1B0.45090.38040.13230.085*
C20.5400 (2)0.3972 (3)0.2322 (3)0.0895 (11)
H2A0.57350.34630.27170.107*
H2B0.51810.44750.28980.107*
C30.5805 (3)0.4699 (5)0.1415 (4)0.1239 (17)
H3A0.59770.41940.08020.149*
H3B0.54710.52440.10690.149*
C40.6422 (3)0.5338 (6)0.1896 (5)0.168 (3)
H4A0.62630.60810.21630.252*
H4B0.67820.54370.13040.252*
H4C0.66240.49140.25360.252*
C50.39081 (18)0.3258 (3)0.3276 (3)0.0691 (8)
H5A0.42310.37380.37310.083*
H5B0.36290.37690.27810.083*
C60.33950 (19)0.2674 (3)0.4101 (3)0.0789 (9)
H6A0.30720.21780.36640.095*
H6B0.36670.21940.46350.095*
C70.2961 (3)0.3526 (4)0.4777 (4)0.1119 (14)
H7A0.32930.40330.51830.134*
H7B0.26930.39970.42290.134*
C80.2444 (3)0.3059 (5)0.5639 (4)0.1279 (16)
H8A0.21260.25200.52640.192*
H8B0.21650.36800.59640.192*
H8C0.27040.26750.62490.192*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0952 (6)0.0947 (7)0.0756 (5)0.0000.0000.0136 (4)
Cl10.159 (5)0.071 (2)0.158 (5)0.0188 (19)0.045 (2)0.0057 (19)
Cl20.167 (4)0.180 (4)0.128 (3)0.048 (3)0.068 (2)0.038 (3)
Br10.1035 (18)0.067 (3)0.1040 (18)0.0065 (19)0.0227 (19)0.0065 (17)
Br20.171 (4)0.116 (3)0.093 (2)0.029 (2)0.046 (2)0.0300 (18)
N20.080 (2)0.049 (2)0.0514 (17)0.0000.0000.0014 (15)
C10.084 (2)0.066 (2)0.0634 (17)0.0059 (17)0.0043 (15)0.0052 (15)
C20.095 (2)0.082 (3)0.092 (2)0.018 (2)0.004 (2)0.0117 (19)
C30.115 (3)0.132 (4)0.124 (3)0.045 (3)0.014 (3)0.023 (3)
C40.128 (4)0.188 (6)0.188 (6)0.072 (4)0.030 (4)0.055 (5)
C50.090 (2)0.056 (2)0.0618 (16)0.0050 (16)0.0020 (15)0.0047 (14)
C60.086 (2)0.075 (2)0.076 (2)0.0037 (17)0.0095 (17)0.0011 (17)
C70.128 (3)0.118 (3)0.090 (3)0.032 (3)0.028 (3)0.011 (2)
C80.126 (3)0.154 (4)0.104 (3)0.019 (3)0.035 (3)0.020 (3)
Geometric parameters (Å, º) top
Fe1—Cl12.107 (10)C4—H4A0.9600
Fe1—Cl22.172 (6)C4—H4B0.9600
Fe1—Br22.337 (6)C4—H4C0.9600
Fe1—Br12.356 (12)C5—C61.504 (4)
N2—C51.509 (4)C5—H5A0.9700
N2—C11.525 (4)C5—H5B0.9700
C1—C21.497 (5)C6—C71.492 (5)
C1—H1A0.9700C6—H6A0.9700
C1—H1B0.9700C6—H6B0.9700
C2—C31.536 (6)C7—C81.480 (6)
C2—H2A0.9700C7—H7A0.9700
C2—H2B0.9700C7—H7B0.9700
C3—C41.469 (6)C8—H8A0.9600
C3—H3A0.9700C8—H8B0.9600
C3—H3B0.9700C8—H8C0.9600
Cl1—Fe1—Cl1i111.8 (4)C2—C3—H3A108.8
Cl1—Fe1—Cl2i110.4 (3)C4—C3—H3B108.8
Cl1—Fe1—Cl2113.3 (2)C2—C3—H3B108.8
Cl2i—Fe1—Cl296.9 (3)H3A—C3—H3B107.7
Cl1—Fe1—Br2i109.8 (3)C3—C4—H4A109.5
Cl1—Fe1—Br298.6 (2)C3—C4—H4B109.5
Cl2i—Fe1—Br2112.06 (16)H4A—C4—H4B109.5
Cl2—Fe1—Br217.6 (2)C3—C4—H4C109.5
Br2i—Fe1—Br2128.4 (3)H4A—C4—H4C109.5
Cl1—Fe1—Br12.3 (4)H4B—C4—H4C109.5
Cl1i—Fe1—Br1110.86 (8)C6—C5—N2117.7 (3)
Cl2i—Fe1—Br1109.3 (2)C6—C5—H5A107.9
Cl2—Fe1—Br1115.5 (2)N2—C5—H5A107.9
Br2i—Fe1—Br1108.1 (2)C6—C5—H5B107.9
Br2—Fe1—Br1100.9 (2)N2—C5—H5B107.9
Br1—Fe1—Br1i110.0 (3)H5A—C5—H5B107.2
C5i—N2—C5112.0 (3)C7—C6—C5111.9 (3)
C5i—N2—C1108.34 (16)C7—C6—H6A109.2
C5—N2—C1108.31 (17)C5—C6—H6A109.2
C1i—N2—C1111.6 (3)C7—C6—H6B109.2
C2—C1—N2116.9 (3)C5—C6—H6B109.2
C2—C1—H1A108.1H6A—C6—H6B107.9
N2—C1—H1A108.1C8—C7—C6117.1 (4)
C2—C1—H1B108.1C8—C7—H7A108.0
N2—C1—H1B108.1C6—C7—H7A108.0
H1A—C1—H1B107.3C8—C7—H7B108.0
C1—C2—C3109.5 (3)C6—C7—H7B108.0
C1—C2—H2A109.8H7A—C7—H7B107.3
C3—C2—H2A109.8C7—C8—H8A109.5
C1—C2—H2B109.8C7—C8—H8B109.5
C3—C2—H2B109.8H8A—C8—H8B109.5
H2A—C2—H2B108.2C7—C8—H8C109.5
C4—C3—C2113.6 (4)H8A—C8—H8C109.5
C4—C3—H3A108.8H8B—C8—H8C109.5
Symmetry code: (i) x, y+1/2, z+1/2.
 

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