(2-Phenyl­ethyl)­ammonium tetra­bromo­thallate(III)

The structure of the title compound, (C₈H₁₂N)[TlBr₄], is characterized by tetracoordinate thallium, forming a regular tetrahedron TlBr₄ with Tl-Br distances ranging between 2.528 (2) and 2.562 (2) Å. Chains of TlBr₄ tetrahedra oriented along the c axis form pseudo-hexagonal rings, containing two columns formed by obliquely stacked amine cations.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.029 Å
• R factor = 0.051
• wR factor = 0.132
• Data-to-parameter ratio = 24.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ...         29

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C3
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         Tl
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.06
PLAT420_ALERT_2_C D-H Without Acceptor       N      -   HA     ...          ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          3

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           21.40
           From the CIF: _reflns_number_total               3190
           Count of symmetry unique reflns         1842
           Completeness (_total/calc)            173.18%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1348
           Fraction of Friedel pairs measured     0.732
           Are heavy atom types Z>Si present          yes

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   1 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
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: KappaCCD; cell refinement: DIRAX/LSQ (Duisenberg & Schreurs, 2000); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

(2-Phenylethyl)ammonium tetrabromothallate(III)

Crystal data

(C8H12N)[TlBr4]	Dx = 2.895 Mg m^−3
Mr = 646.18	Ag Kα radiation, λ = 0.56085 Å
Orthorhombic, Pna21	Cell parameters from 1924 reflections
Hall symbol: P 2c -2n	θ = 3.1–18.4°
a = 17.944 (1) Å	µ = 11.71 mm^−1
b = 11.9692 (6) Å	T = 298 K
c = 6.9072 (3) Å	Parallelipiped, yellow
V = 1483.50 (13) Å^3	0.52 × 0.13 × 0.12 mm
Z = 4

Data collection

Nonius KappaCCD diffractometer	2167 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.082
CCD scans	θmax = 21.4°, θmin = 3.0°
Absorption correction: integration Gaussian integration (Coppens, 1970)	h = −23→23
Tmin = 0.139, Tmax = 0.288	k = −12→15
6988 measured reflections	l = −8→8
3190 independent reflections

Refinement

Refinement on F^2	H-atom parameters constrained
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0638P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.051	(Δ/σ)max < 0.001
wR(F^2) = 0.132	Δρmax = 1.52 e Å^−3
S = 1.03	Δρmin = −1.67 e Å^−3
3190 reflections	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
128 parameters	Extinction coefficient: 0.0081 (6)
1 restraint	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.02 (4)
Secondary atom site location: difference Fourier map

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
C1	0.4144 (10)	0.2725 (15)	0.922 (3)	0.049 (5)
C8	0.3830 (10)	0.3765 (18)	0.482 (3)	0.057 (6)
C7	0.4119 (17)	0.4432 (18)	0.339 (3)	0.074 (8)
C6	0.4848 (17)	0.431 (2)	0.286 (3)	0.072 (7)
C5	0.5266 (12)	0.343 (2)	0.365 (3)	0.062 (6)
C4	0.4969 (10)	0.2838 (16)	0.512 (3)	0.051 (5)
N	0.3875 (10)	0.1965 (13)	1.082 (2)	0.059 (4)
C2	0.3938 (10)	0.2219 (16)	0.731 (2)	0.045 (4)
C3	0.4246 (7)	0.2951 (13)	0.570 (3)	0.032 (3)
Br2	0.16729 (10)	0.42333 (17)	0.4239 (3)	0.0547 (5)
Br3	0.26472 (13)	0.5524 (2)	−0.0808 (4)	0.0710 (6)
Br4	0.04493 (9)	0.47275 (18)	−0.0879 (3)	0.0505 (5)
Br1	0.19706 (13)	0.21593 (19)	−0.0509 (4)	0.0704 (6)
Tl	0.17097 (3)	0.41572 (5)	0.05576 (10)	0.0412 (2)
H1A	0.4673	0.2843	0.9286	0.059*
H1B	0.3892	0.3430	0.9311	0.059*
H8	0.3335	0.3872	0.5320	0.069*
H7	0.3787	0.4945	0.2755	0.088*
H6	0.5072	0.4825	0.1959	0.086*
H5	0.5761	0.3318	0.3160	0.074*
H4	0.5268	0.2283	0.5757	0.061*
HA	0.3989	0.2291	1.2059	0.071*
HB	0.4128	0.1262	1.0701	0.071*
HC	0.3346	0.1849	1.0726	0.071*
H2A	0.4159	0.1488	0.7260	0.054*
H2B	0.3407	0.2155	0.7196	0.054*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.077 (12)	0.033 (11)	0.036 (8)	−0.024 (9)	0.006 (9)	0.002 (9)
C8	0.045 (10)	0.065 (15)	0.062 (12)	0.030 (10)	−0.015 (8)	−0.032 (10)
C7	0.15 (2)	0.034 (13)	0.041 (10)	0.016 (14)	−0.022 (14)	0.009 (9)
C6	0.12 (2)	0.063 (17)	0.034 (11)	−0.040 (15)	0.010 (12)	−0.011 (10)
C5	0.061 (12)	0.070 (17)	0.054 (12)	−0.008 (12)	0.011 (9)	−0.022 (11)
C4	0.063 (11)	0.038 (12)	0.050 (13)	−0.012 (9)	0.000 (8)	−0.004 (8)
N	0.091 (10)	0.045 (9)	0.041 (9)	−0.009 (8)	−0.007 (9)	0.011 (8)
C2	0.052 (9)	0.050 (12)	0.032 (8)	−0.013 (8)	0.003 (8)	−0.007 (9)
C3	0.031 (6)	0.038 (9)	0.026 (7)	0.003 (6)	−0.004 (8)	0.003 (10)
Br2	0.0598 (11)	0.0650 (15)	0.0393 (9)	0.0037 (9)	−0.0021 (9)	0.0001 (10)
Br3	0.0702 (12)	0.0749 (16)	0.0679 (12)	−0.0246 (12)	0.0139 (12)	0.0049 (13)
Br4	0.0465 (8)	0.0582 (12)	0.0470 (8)	0.0039 (9)	−0.0062 (9)	−0.0034 (10)
Br1	0.0815 (13)	0.0450 (13)	0.0848 (15)	0.0085 (11)	0.0086 (13)	−0.0126 (12)
Tl	0.0410 (3)	0.0417 (4)	0.0409 (3)	0.0007 (3)	0.0023 (4)	−0.0011 (5)

Geometric parameters (Å, º)

C1—C2	1.50 (3)	C1—H1A	0.9601
C1—N	1.51 (2)	C1—H1B	0.9599
C8—C7	1.37 (3)	C8—H8	0.9600
C8—C3	1.37 (2)	C7—H7	0.9600
C7—C6	1.37 (4)	C6—H6	0.9600
C6—C5	1.41 (4)	C5—H5	0.9601
C5—C4	1.35 (3)	C4—H4	0.9599
C4—C3	1.36 (2)	N—HA	0.9600
C2—C3	1.52 (2)	N—HB	0.9599
Br2—Tl	2.545 (2)	N—HC	0.9603
Br3—Tl	2.528 (2)	C2—H2A	0.9601
Br4—Tl	2.562 (2)	C2—H2B	0.9599
Br1—Tl	2.545 (2)
C2—C1—N	108.9 (14)	C7—C8—H8	121.9
C7—C8—C3	121.8 (19)	C3—C8—H8	116.2
C8—C7—C6	120 (2)	C8—C7—H7	117.9
C7—C6—C5	119 (2)	C6—C7—H7	122.5
C4—C5—C6	118 (2)	C7—C6—H6	120.4
C3—C4—C5	123 (2)	C5—C6—H6	120.6
C1—C2—C3	108.7 (13)	C4—C5—H5	124.2
C4—C3—C8	117.3 (18)	C6—C5—H5	117.2
C4—C3—C2	120.3 (15)	C3—C4—H4	117.8
C8—C3—C2	122.4 (15)	C5—C4—H4	119.0
Br3—Tl—Br2	111.52 (8)	C1—N—HA	109.8
Br3—Tl—Br1	112.17 (8)	C1—N—HB	108.1
Br2—Tl—Br1	109.12 (8)	HA—N—HB	109.5
Br3—Tl—Br4	105.68 (8)	C1—N—HC	110.6
Br2—Tl—Br4	110.76 (7)	HA—N—HC	109.5
Br1—Tl—Br4	107.49 (8)	HB—N—HC	109.5
C2—C1—H1A	110.3	C1—C2—H2A	107.3
N—C1—H1A	111.6	C3—C2—H2A	110.5
C2—C1—H1B	107.3	C1—C2—H2B	110.5
N—C1—H1B	109.1	C3—C2—H2B	110.4
H1A—C1—H1B	109.5	H2A—C2—H2B	109.5