Redetermination of tetra­phenyl­arsonium trans-aqua­tetra­chloro­oxorhenate(V) at 100 K

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.

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

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Computing details

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)

Crystal data

(C24H20As)[ReCl4O(H2O)]	Dx = 2.018 Mg m^−3
Mr = 745.34	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/n	Cell parameters from 20865 reflections
Hall symbol: -P 4a	θ = 3.2–37.3°
a = 13.021 (2) Å	µ = 6.75 mm^−1
c = 7.236 (2) Å	T = 100 K
V = 1226.8 (4) Å^3	Quadratic plates, yellow
Z = 2	0.15 × 0.15 × 0.15 mm
F(000) = 716

Data collection

Kuma KM-4-CCD κ-geometry diffractometer	2671 independent reflections
Radiation source: fine-focus sealed tube	2535 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.043
ω scans	θmax = 35.0°, θmin = 3.2°
Absorption correction: numerical (CrysAlis RED; Oxford Diffraction, 2003)	h = −20→21
Tmin = 0.562, Tmax = 0.686	k = −21→21
19131 measured reflections	l = −9→11

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.018	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.039	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.0156P)^2 + 0.8991P] where P = (Fo^2 + 2Fc^2)/3
2671 reflections	(Δ/σ)max = 0.002
76 parameters	Δρmax = 1.52 e Å^−3
0 restraints	Δρmin = −0.98 e Å^−3

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	Occ. (<1)
Re	0.25	0.25	0.192727 (15)	0.01176 (3)
Cl	0.18918 (3)	0.08326 (3)	0.13541 (6)	0.02091 (7)
As	0.25	0.75	0	0.01178 (5)
O1	0.25	0.25	0.4223 (3)	0.0162 (4)
O2	0.25	0.25	−0.1285 (4)	0.0280 (5)
H1W	0.2689	0.1922	−0.1672	0.042*	0.50
C1	0.14160 (11)	0.70549 (11)	0.1580 (2)	0.0135 (2)
C2	0.10510 (12)	0.77601 (12)	0.2889 (2)	0.0173 (3)
H2	0.1335	0.8431	0.2961	0.021*
C3	0.02683 (13)	0.74642 (12)	0.4078 (2)	0.0192 (3)
H3	0.0011	0.7934	0.4969	0.023*
C4	−0.01399 (12)	0.64769 (13)	0.3963 (2)	0.0189 (3)
H4	−0.0681	0.6280	0.4770	0.023*
C5	0.02361 (12)	0.57777 (12)	0.2680 (2)	0.0180 (3)
H5	−0.0045	0.5105	0.2620	0.022*
C6	0.10256 (11)	0.60609 (11)	0.1480 (2)	0.0152 (2)
H6	0.1292	0.5584	0.0610	0.018*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re	0.01260 (4)	0.01260 (4)	0.01008 (5)	0	0	0
Cl	0.02085 (16)	0.01480 (14)	0.02707 (18)	−0.00251 (13)	0.00119 (14)	−0.00346 (13)
As	0.01002 (7)	0.01002 (7)	0.01530 (13)	0	0	0
O1	0.0221 (6)	0.0221 (6)	0.0044 (8)	0	0	0
O2	0.0343 (9)	0.0343 (9)	0.0154 (11)	0	0	0
C1	0.0107 (5)	0.0121 (5)	0.0176 (6)	0.0006 (5)	−0.0001 (4)	0.0003 (4)
C2	0.0179 (6)	0.0142 (6)	0.0198 (7)	−0.0001 (5)	0.0012 (5)	−0.0019 (5)
C3	0.0193 (6)	0.0187 (6)	0.0195 (7)	0.0023 (6)	0.0032 (5)	−0.0019 (5)
C4	0.0159 (6)	0.0203 (6)	0.0206 (7)	0.0001 (5)	0.0032 (5)	0.0031 (5)
C5	0.0162 (6)	0.0154 (6)	0.0222 (7)	−0.0027 (5)	0.0015 (5)	0.0026 (5)
C6	0.0141 (6)	0.0129 (5)	0.0187 (6)	0.0007 (5)	−0.0002 (5)	0.0006 (5)

Geometric parameters (Å, º)

Re—O1	1.662 (2)	C1—C6	1.392 (2)
Re—O2	2.325 (3)	C1—C2	1.402 (2)
Re—Cl	2.3479 (5)	C2—C3	1.388 (2)
Re—Cl^i	2.3479 (5)	C2—H2	0.9500
Re—Cl^ii	2.3479 (5)	C3—C4	1.394 (2)
Re—Cl^iii	2.3479 (5)	C3—H3	0.9500
As—C1^iv	1.9067 (15)	C4—C5	1.389 (2)
As—C1^v	1.9067 (14)	C4—H4	0.9500
As—C1	1.907 (2)	C5—C6	1.395 (2)
As—C1^vi	1.9067 (15)	C5—H5	0.9500
O2—H1W	0.8400	C6—H6	0.9500
O1—Re—O2	180.0	C1—As—C1^vi	111.08 (5)
O1—Re—Cl	100.18 (1)	Re—O2—H1W	109.5
O2—Re—Cl	79.83 (1)	C6—C1—C2	121.33 (14)
O1—Re—Cl^i	100.175 (12)	C6—C1—As	121.45 (11)
O2—Re—Cl^i	79.825 (12)	C2—C1—As	117.19 (11)
Cl—Re—Cl^i	88.21 (1)	C3—C2—C1	119.06 (14)
O1—Re—Cl^ii	100.175 (12)	C3—C2—H2	120.5
O2—Re—Cl^ii	79.825 (12)	C1—C2—H2	120.5
Cl—Re—Cl^ii	159.65 (2)	C2—C3—C4	119.93 (15)
Cl^i—Re—Cl^ii	88.212 (4)	C2—C3—H3	120.0
O1—Re—Cl^iii	100.175 (12)	C4—C3—H3	120.0
O2—Re—Cl^iii	79.825 (12)	C5—C4—C3	120.66 (15)
Cl—Re—Cl^iii	88.212 (4)	C5—C4—H4	119.7
Cl^i—Re—Cl^iii	159.65 (2)	C3—C4—H4	119.7
Cl^ii—Re—Cl^iii	88.212 (4)	C4—C5—C6	120.14 (14)
C1^iv—As—C1^v	111.08 (5)	C4—C5—H5	119.9
C1^iv—As—C1	106.31 (9)	C6—C5—H5	119.9
C1^v—As—C1	111.08 (5)	C1—C6—C5	118.85 (14)
C1^iv—As—C1^vi	111.08 (5)	C1—C6—H6	120.6
C1^v—As—C1^vi	106.31 (9)	C5—C6—H6	120.6
C1^iv—As—C1—C6	−122.29 (14)	As—C1—C2—C3	−179.44 (12)
C1^v—As—C1—C6	116.76 (15)	C1—C2—C3—C4	0.2 (2)
C1^vi—As—C1—C6	−1.34 (12)	C2—C3—C4—C5	0.7 (3)
C1^iv—As—C1—C2	55.66 (11)	C3—C4—C5—C6	−0.4 (2)
C1^v—As—C1—C2	−65.29 (9)	C2—C1—C6—C5	1.8 (2)
C1^vi—As—C1—C2	176.61 (12)	As—C1—C6—C5	179.63 (11)
C6—C1—C2—C3	−1.5 (2)	C4—C5—C6—C1	−0.8 (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) y−1/2, −x+1, −z; (vi) −y+1, x+1/2, −z.