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The crystal structure of the title compound, (C24H20As)[ReCl4O(H2O)], has been re-examined at 100 K. The complex contains distorted octa­hedral [ReOCl4(H2O)]- anions, with the Re atom and disordered aqua ligand located on a fourfold axis, and [Ph4As]+ cations with the As atom located on a fourfold inversion axis. In the anion, the terminal Re=O bond, 1.662 (2) Å, is trans to the aqua ligand and the Re-(OH2) and Re-Cl distances are 2.325 (3) and 2.3479 (5) Å, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806001747/tk6296sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806001747/tk6296Isup2.hkl
Contains datablock I

CCDC reference: 298554

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.018
  • wR factor = 0.039
  • Data-to-parameter ratio = 35.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O2 - *H1W ... ?
Alert level G ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.562 0.686 Tmin(prime) and Tmax expected: 0.349 0.363 RR(prime) = 0.853 Please check that your absorption correction is appropriate.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 0 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 1 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 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction 2003); cell refinement: CrysAlis RED (Oxford Diffraction 2003); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97.

Tetraphenyloarsonium aqua-tetrachlorooxorhenate(V) top
Crystal data top
(C24H20As)[ReCl4O(H2O)]Dx = 2.018 Mg m3
Mr = 745.34Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/nCell parameters from 20865 reflections
Hall symbol: -P 4aθ = 3.2–37.3°
a = 13.021 (2) ŵ = 6.75 mm1
c = 7.236 (2) ÅT = 100 K
V = 1226.8 (4) Å3Quadratic plates, yellow
Z = 20.15 × 0.15 × 0.15 mm
F(000) = 716
Data collection top
Kuma KM-4-CCD κ-geometry
diffractometer
2671 independent reflections
Radiation source: fine-focus sealed tube2535 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.043
ω scansθmax = 35.0°, θmin = 3.2°
Absorption correction: numerical
(CrysAlis RED; Oxford Diffraction, 2003)
h = 2021
Tmin = 0.562, Tmax = 0.686k = 2121
19131 measured reflectionsl = 911
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)] = 0.018Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.039H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0156P)2 + 0.8991P]
where P = (Fo2 + 2Fc2)/3
2671 reflections(Δ/σ)max = 0.002
76 parametersΔρmax = 1.52 e Å3
0 restraintsΔρmin = 0.98 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)
Re0.250.250.192727 (15)0.01176 (3)
Cl0.18918 (3)0.08326 (3)0.13541 (6)0.02091 (7)
As0.250.7500.01178 (5)
O10.250.250.4223 (3)0.0162 (4)
O20.250.250.1285 (4)0.0280 (5)
H1W0.26890.19220.16720.042*0.50
C10.14160 (11)0.70549 (11)0.1580 (2)0.0135 (2)
C20.10510 (12)0.77601 (12)0.2889 (2)0.0173 (3)
H20.13350.84310.29610.021*
C30.02683 (13)0.74642 (12)0.4078 (2)0.0192 (3)
H30.00110.79340.49690.023*
C40.01399 (12)0.64769 (13)0.3963 (2)0.0189 (3)
H40.06810.62800.47700.023*
C50.02361 (12)0.57777 (12)0.2680 (2)0.0180 (3)
H50.00450.51050.26200.022*
C60.10256 (11)0.60609 (11)0.1480 (2)0.0152 (2)
H60.12920.55840.06100.018*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re0.01260 (4)0.01260 (4)0.01008 (5)000
Cl0.02085 (16)0.01480 (14)0.02707 (18)0.00251 (13)0.00119 (14)0.00346 (13)
As0.01002 (7)0.01002 (7)0.01530 (13)000
O10.0221 (6)0.0221 (6)0.0044 (8)000
O20.0343 (9)0.0343 (9)0.0154 (11)000
C10.0107 (5)0.0121 (5)0.0176 (6)0.0006 (5)0.0001 (4)0.0003 (4)
C20.0179 (6)0.0142 (6)0.0198 (7)0.0001 (5)0.0012 (5)0.0019 (5)
C30.0193 (6)0.0187 (6)0.0195 (7)0.0023 (6)0.0032 (5)0.0019 (5)
C40.0159 (6)0.0203 (6)0.0206 (7)0.0001 (5)0.0032 (5)0.0031 (5)
C50.0162 (6)0.0154 (6)0.0222 (7)0.0027 (5)0.0015 (5)0.0026 (5)
C60.0141 (6)0.0129 (5)0.0187 (6)0.0007 (5)0.0002 (5)0.0006 (5)
Geometric parameters (Å, º) top
Re—O11.662 (2)C1—C61.392 (2)
Re—O22.325 (3)C1—C21.402 (2)
Re—Cl2.3479 (5)C2—C31.388 (2)
Re—Cli2.3479 (5)C2—H20.9500
Re—Clii2.3479 (5)C3—C41.394 (2)
Re—Cliii2.3479 (5)C3—H30.9500
As—C1iv1.9067 (15)C4—C51.389 (2)
As—C1v1.9067 (14)C4—H40.9500
As—C11.907 (2)C5—C61.395 (2)
As—C1vi1.9067 (15)C5—H50.9500
O2—H1W0.8400C6—H60.9500
O1—Re—O2180.0C1—As—C1vi111.08 (5)
O1—Re—Cl100.18 (1)Re—O2—H1W109.5
O2—Re—Cl79.83 (1)C6—C1—C2121.33 (14)
O1—Re—Cli100.175 (12)C6—C1—As121.45 (11)
O2—Re—Cli79.825 (12)C2—C1—As117.19 (11)
Cl—Re—Cli88.21 (1)C3—C2—C1119.06 (14)
O1—Re—Clii100.175 (12)C3—C2—H2120.5
O2—Re—Clii79.825 (12)C1—C2—H2120.5
Cl—Re—Clii159.65 (2)C2—C3—C4119.93 (15)
Cli—Re—Clii88.212 (4)C2—C3—H3120.0
O1—Re—Cliii100.175 (12)C4—C3—H3120.0
O2—Re—Cliii79.825 (12)C5—C4—C3120.66 (15)
Cl—Re—Cliii88.212 (4)C5—C4—H4119.7
Cli—Re—Cliii159.65 (2)C3—C4—H4119.7
Clii—Re—Cliii88.212 (4)C4—C5—C6120.14 (14)
C1iv—As—C1v111.08 (5)C4—C5—H5119.9
C1iv—As—C1106.31 (9)C6—C5—H5119.9
C1v—As—C1111.08 (5)C1—C6—C5118.85 (14)
C1iv—As—C1vi111.08 (5)C1—C6—H6120.6
C1v—As—C1vi106.31 (9)C5—C6—H6120.6
C1iv—As—C1—C6122.29 (14)As—C1—C2—C3179.44 (12)
C1v—As—C1—C6116.76 (15)C1—C2—C3—C40.2 (2)
C1vi—As—C1—C61.34 (12)C2—C3—C4—C50.7 (3)
C1iv—As—C1—C255.66 (11)C3—C4—C5—C60.4 (2)
C1v—As—C1—C265.29 (9)C2—C1—C6—C51.8 (2)
C1vi—As—C1—C2176.61 (12)As—C1—C6—C5179.63 (11)
C6—C1—C2—C31.5 (2)C4—C5—C6—C10.8 (2)
Symmetry codes: (i) y, x+1/2, z; (ii) x+1/2, y+1/2, z; (iii) y+1/2, x, z; (iv) x+1/2, y+3/2, z; (v) y1/2, x+1, z; (vi) y+1, x+1/2, z.
 

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