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The title compound, (C19H18P)2[ReCl6], has been prepared by a new method and its structure redetermined [Hołynska, Korabik & Lis (2006). Acta Cryst. E62, m3178–m3180]. The previously observed orientational disorder of the [ReCl6]2− anion (Re site symmetry \overline{1}) is reinter­preted as being due to a minor cocrystallized ReV-containing impurity. Revised magnetic, MS and spectroscopic data are also presented and discussed. The crystal structure involves C—H...Cl hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807052579/hb2601sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807052579/hb2601Isup2.hkl
Contains datablock I

CCDC reference: 667251

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.053
  • wR factor = 0.056
  • Data-to-parameter ratio = 35.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H121 .. CL3 .. 2.85 Ang.
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Re (4) 4.22
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 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 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

During our recent unpublished studies on the reaction of gaseous hydrogen chloride with rhenates(VII) (continuation of the work of Lis & Jeżowska-Trzebiatowska, 1977) formation of crystalline products with rhenium at different oxidation states was observed. It was confirmed with a number of physicochemical methods that these products usually contained minor quantity of cocrystallizing impurities, sometimes hardly detectable. This induced us to reinspect all our previous results for compounds obtained by this method.

In our previous paper on the title compound, (I), bis(methyltriphenylphosphonium) hexachlororhenate(IV) we reported the crystal structure of the product obtained from the suspension of methyltriphenylphosphonium rhenate(VII) in acetone exposed to gaseous HCl (Hołyńska et al., 2006). It was assumed that the crystal structure consists of methyltriphenylphoshonium cations and slightly disordered hexachlororhenate(IV) anions. The reinspection showed that one of the three independent Re–Cl bond lengths was slightly shorter than expected based on the literature data [2.323 (3) Å in comparison to 2.3545 (9) reported for potassium hexachlororhenate(IV) by Takazawa et al., 1990]. This work investigates whether this was a result either of minor impurity content or artifact connected with disorder. The other aim is to obtain a pure compound with reliable geometric parameters for the hexachlororhenate(IV) anion.

Therefore recently we used a different method to prepare (I), namely simple precipitation in reaction between methyltriphenylphoshonium chloride and potassium hexachlororhenate(IV). It was assumed that if the different method yields results not arguable from crystallographic point of view, the previous results were affected by impurity content rather than disorder artifacts. The X-ray studies performed on the crystal obtained in recrystallization from ethanol yield different results than in the previous work (Hołyńska et al., 2006). Therefore, the previously reported slightly distorted geometry of the hexachlororhenate(IV) anion, its apparent "disorder" as well as high peaks on the difference Fourier map, could be a result of a co-crystallized impurity, most probably by a ReV complex. For one thing, it was observed that methyltriphenylphosphonium trans-aquatetrachlorooxorhenate(V) monohydrate could be obtained in crystalline form as a second reaction product in the previously investigated system (Hołyńska et al., unpublished). In this salt each anion consists of the central ReV atom bonded to the oxo ligand and aqua ligand in trans position to the oxo ligand and four chlorine ligands lying in the distorted coordination octahedron equatorial plane. The trans-aquatetrachlorooxorhenate(V) anion could in small amount cocrystallize with the hexachlororhenate(IV) product. However, the attempt to take such impurity into account during the crystal structure re-refinement was unsuccessful. The reason for this situation could be the very small amounts of the impurity or that the ReV anion is disordered in many positions in the crystal structure. The position of peaks on the difference Fourier map (Hołyńska et al., 2006) as well as the mode of the hexachlororhenate(IV) anion distortion suggest that the Re atom of the ReV complex anion is in the same position as the hexachlororhenate(IV) anion Re atom. Moreover, none of the possible anion orientations allows the water molecule coordinated to the ReV atom to be involved in any strong hydrogen bonds. This is poorly confirmed by the IR spectra obtained in nujol mull in the 3100–3400 cm-1 region (hardly detectable bands at 3580 and 3600 cm-1). On the other hand, a weak band at approximately 937 cm-1 could be observed which could be assigned to the Re—O stretching mode. The mass spectra obtained for the pure and impure title compound differ to a small extent, especially with respect to the 200–350 m/Z range where for the latter high noise level is present and some minor peaks could be interpreted as a result of an oxocomplex anion defragmentation [assuming after Lukas (1978) that ReOCl3+ and ReOCl2+ ions could be formed]. The previously reported (Hołyńska et al., 2006) magnetic susceptibility data for the impure compound assuming the additivity of gram magnetic susceptibilities (König, 1966) at room temperature allow us to estimate the ReV impurity amount at about 7–8%.

The structure described here for (I) seems to be more reliable than the structure reported previously (Hołyńska et al., 2006). The title crystal structure consists of hexachlororhenate(IV) anions and methyltriphenylphosphophonium cations (Fig. 1). Each hexachlororhenate(IV) anion is generated by inversion and is of octahedral geometry (Table 1). The geometry of the methyltriphenylphosphonium cation does not differ from our previous results (Hołyńska et al., 2006). The overall crystal structure (Fig. 2) is also as previously reported (Hołyńska et al., 2006). The weak C—H···Cl hydrogen bonding scheme (Table 2) is essentially conserved in comparison to the previously reported structure (Hołyńska et al., 2006) taking into consideration the higher-occupancy component of the hexachlororhenate(IV) anion.

The magnetic susceptibility data collected for the newly obtained compound (Fig. 3) reveal in comparison to the previously published data (Hołyńska et al., 2006) a similar effective magnetic moment temperature dependence with lower values at 300 K (3.54µB) in comparison to the here reported 3.71µB. This is understandable assuming the diamagnetic properties of the ReV impurity. The impurity causes lowering of the χmT values in the temperature range 50 - 300 K (Fig. 3). In the 50 – 300 K temperature range the χmT values for the "impure" compound are nearly constant which is another effect introduced by the diamagnetic impurity. The new value of the parameter D is 17 (2) cm-1 which is higher than 14 (2) cm-1 obtained previously (Hołyńska et al., 2006). The remaining fitted parameters are g (perpendicular) and g (parallel). For the 'pure' compound their values are 1.68 and 2.28, respectively (the minimalized R = 4.0 × 10-4). For the 'impure' compound their values are 1.71 and 2.04, respectively (the minimalized value R = 2.73 × 10-5).

Related literature top

For the previous structure, see: Hołyńska et al. (2006). For background, see: König (1966); Lis & Jeżowska-Trzebiatowska (1977); Lukas (1978); Takazawa et al. (1990).

Experimental top

0.5 g of potassium hexachlororhenate(IV) was dissolved in hot concentrated hydrochloric acid. Stoichiometric quantity of methyltriphenylphosphonium chloride dissolved in concentrated hydrochloric acid was added. As a result, a fine greenish precipitate was formed. The product was recrystallized from hot ethanol to yield green needles of (I). The crystal taken for X-ray measurement was cut from a larger needle. ESI-MS spectrum was collected in acetonitrile for the 'pure' compound as well as for the 'impure' compound obtained with the aid of the method described previously (Hołyńska et al., 2006). The device used was micrOTOF-Q (data for the 'pure' compound (m/Z for negative ions): 363.8 (ReCl5-); 326.8 (ReCl4-); (m/Z for positive ions): 277.1 (PPh3CH3+); 1230.1 (evidently for the cluster ions formed during the ionization process). IR spectra were collected for suspensions in nujol mull on BRUKER spectrometer. The magnetic measurements were performed for 0.02831 g powdered sample of the title complex, at the magnetic field 0.5 T, using Quantum Design SQUID Magnetometer (type MPMS-XL5), at 1.8 to 300 K temperature range. The corrections introduced for diamagnetism of the constituent atoms were introduced based on the Pascal constants (König, 1966).

Refinement top

The non-hydrogen atom coordinates from the previously study (Hołyńska et al., 2006) were used as the starting model for the present refinement. The H atoms were generated geometrically (C—H = 0.95–0.98 Å) and refined as riding with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C). The highest difference peak is 0.6–0.9 Å from Re.

Structure description top

During our recent unpublished studies on the reaction of gaseous hydrogen chloride with rhenates(VII) (continuation of the work of Lis & Jeżowska-Trzebiatowska, 1977) formation of crystalline products with rhenium at different oxidation states was observed. It was confirmed with a number of physicochemical methods that these products usually contained minor quantity of cocrystallizing impurities, sometimes hardly detectable. This induced us to reinspect all our previous results for compounds obtained by this method.

In our previous paper on the title compound, (I), bis(methyltriphenylphosphonium) hexachlororhenate(IV) we reported the crystal structure of the product obtained from the suspension of methyltriphenylphosphonium rhenate(VII) in acetone exposed to gaseous HCl (Hołyńska et al., 2006). It was assumed that the crystal structure consists of methyltriphenylphoshonium cations and slightly disordered hexachlororhenate(IV) anions. The reinspection showed that one of the three independent Re–Cl bond lengths was slightly shorter than expected based on the literature data [2.323 (3) Å in comparison to 2.3545 (9) reported for potassium hexachlororhenate(IV) by Takazawa et al., 1990]. This work investigates whether this was a result either of minor impurity content or artifact connected with disorder. The other aim is to obtain a pure compound with reliable geometric parameters for the hexachlororhenate(IV) anion.

Therefore recently we used a different method to prepare (I), namely simple precipitation in reaction between methyltriphenylphoshonium chloride and potassium hexachlororhenate(IV). It was assumed that if the different method yields results not arguable from crystallographic point of view, the previous results were affected by impurity content rather than disorder artifacts. The X-ray studies performed on the crystal obtained in recrystallization from ethanol yield different results than in the previous work (Hołyńska et al., 2006). Therefore, the previously reported slightly distorted geometry of the hexachlororhenate(IV) anion, its apparent "disorder" as well as high peaks on the difference Fourier map, could be a result of a co-crystallized impurity, most probably by a ReV complex. For one thing, it was observed that methyltriphenylphosphonium trans-aquatetrachlorooxorhenate(V) monohydrate could be obtained in crystalline form as a second reaction product in the previously investigated system (Hołyńska et al., unpublished). In this salt each anion consists of the central ReV atom bonded to the oxo ligand and aqua ligand in trans position to the oxo ligand and four chlorine ligands lying in the distorted coordination octahedron equatorial plane. The trans-aquatetrachlorooxorhenate(V) anion could in small amount cocrystallize with the hexachlororhenate(IV) product. However, the attempt to take such impurity into account during the crystal structure re-refinement was unsuccessful. The reason for this situation could be the very small amounts of the impurity or that the ReV anion is disordered in many positions in the crystal structure. The position of peaks on the difference Fourier map (Hołyńska et al., 2006) as well as the mode of the hexachlororhenate(IV) anion distortion suggest that the Re atom of the ReV complex anion is in the same position as the hexachlororhenate(IV) anion Re atom. Moreover, none of the possible anion orientations allows the water molecule coordinated to the ReV atom to be involved in any strong hydrogen bonds. This is poorly confirmed by the IR spectra obtained in nujol mull in the 3100–3400 cm-1 region (hardly detectable bands at 3580 and 3600 cm-1). On the other hand, a weak band at approximately 937 cm-1 could be observed which could be assigned to the Re—O stretching mode. The mass spectra obtained for the pure and impure title compound differ to a small extent, especially with respect to the 200–350 m/Z range where for the latter high noise level is present and some minor peaks could be interpreted as a result of an oxocomplex anion defragmentation [assuming after Lukas (1978) that ReOCl3+ and ReOCl2+ ions could be formed]. The previously reported (Hołyńska et al., 2006) magnetic susceptibility data for the impure compound assuming the additivity of gram magnetic susceptibilities (König, 1966) at room temperature allow us to estimate the ReV impurity amount at about 7–8%.

The structure described here for (I) seems to be more reliable than the structure reported previously (Hołyńska et al., 2006). The title crystal structure consists of hexachlororhenate(IV) anions and methyltriphenylphosphophonium cations (Fig. 1). Each hexachlororhenate(IV) anion is generated by inversion and is of octahedral geometry (Table 1). The geometry of the methyltriphenylphosphonium cation does not differ from our previous results (Hołyńska et al., 2006). The overall crystal structure (Fig. 2) is also as previously reported (Hołyńska et al., 2006). The weak C—H···Cl hydrogen bonding scheme (Table 2) is essentially conserved in comparison to the previously reported structure (Hołyńska et al., 2006) taking into consideration the higher-occupancy component of the hexachlororhenate(IV) anion.

The magnetic susceptibility data collected for the newly obtained compound (Fig. 3) reveal in comparison to the previously published data (Hołyńska et al., 2006) a similar effective magnetic moment temperature dependence with lower values at 300 K (3.54µB) in comparison to the here reported 3.71µB. This is understandable assuming the diamagnetic properties of the ReV impurity. The impurity causes lowering of the χmT values in the temperature range 50 - 300 K (Fig. 3). In the 50 – 300 K temperature range the χmT values for the "impure" compound are nearly constant which is another effect introduced by the diamagnetic impurity. The new value of the parameter D is 17 (2) cm-1 which is higher than 14 (2) cm-1 obtained previously (Hołyńska et al., 2006). The remaining fitted parameters are g (perpendicular) and g (parallel). For the 'pure' compound their values are 1.68 and 2.28, respectively (the minimalized R = 4.0 × 10-4). For the 'impure' compound their values are 1.71 and 2.04, respectively (the minimalized value R = 2.73 × 10-5).

For the previous structure, see: Hołyńska et al. (2006). For background, see: König (1966); Lis & Jeżowska-Trzebiatowska (1977); Lukas (1978); Takazawa et al. (1990).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. View of the molecular structure of (I) with atom labelling scheme adopted from our previous work (Hołyńska et al., 2006). The non-labelled non-hydrogen atoms are related by the symmetry operation: (i) 1 - x, 1 - y, 1 - z.
[Figure 2] Fig. 2. The packing for (I) viewed along [001] showing cation layers perpendicular to [010]. H atoms were omitted for clarity.
[Figure 3] Fig. 3. The χmT temperature dependence (χm - the molar magnetic susceptibility) for the "impure" (blue open triangles) and "pure" (black open circles) compounds. The calculated curves are denoted with solid lines (see text). The red squares illustrate the simulated χmT temperature dependence of the "pure" compound with 7% diamagnetic impurity.
bis(methyltriphenylphosphonium) hexachloridorhenate(IV) top
Crystal data top
(C19H18P)2[ReCl6]F(000) = 942
Mr = 953.52Dx = 1.658 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 12158 reflections
a = 9.155 (4) Åθ = 3–35°
b = 16.429 (5) ŵ = 3.71 mm1
c = 12.964 (5) ÅT = 100 K
β = 101.61 (3)°Needle, green
V = 1910 (1) Å30.23 × 0.04 × 0.03 mm
Z = 2
Data collection top
Oxford Diffraction KM-4-CCD
diffractometer
7666 independent reflections
Radiation source: fine-focus sealed tube5027 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.083
ω scansθmax = 35.0°, θmin = 3.0°
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2006)
h = 1413
Tmin = 0.597, Tmax = 0.894k = 2625
27585 measured reflectionsl = 2015
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.053H-atom parameters constrained
wR(F2) = 0.056 w = 1/[σ2(Fo2) + (0.0084P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.002
7666 reflectionsΔρmax = 0.82 e Å3
214 parametersΔρmin = 0.98 e Å3
Crystal data top
(C19H18P)2[ReCl6]V = 1910 (1) Å3
Mr = 953.52Z = 2
Monoclinic, P21/nMo Kα radiation
a = 9.155 (4) ŵ = 3.71 mm1
b = 16.429 (5) ÅT = 100 K
c = 12.964 (5) Å0.23 × 0.04 × 0.03 mm
β = 101.61 (3)°
Data collection top
Oxford Diffraction KM-4-CCD
diffractometer
7666 independent reflections
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2006)
5027 reflections with I > 2σ(I)
Tmin = 0.597, Tmax = 0.894Rint = 0.083
27585 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0530 restraints
wR(F2) = 0.056H-atom parameters constrained
S = 1.00Δρmax = 0.82 e Å3
7666 reflectionsΔρmin = 0.98 e Å3
214 parameters
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
Re0.50000.50000.50000.01104 (4)
Cl20.56433 (10)0.48672 (5)0.33339 (6)0.0217 (2)
Cl10.60865 (9)0.63048 (5)0.51815 (6)0.01666 (17)
Cl30.27081 (9)0.55985 (5)0.41870 (7)0.02034 (19)
P0.00563 (10)0.71920 (5)0.63598 (7)0.01511 (18)
C10.0052 (4)0.6349 (2)0.5511 (3)0.0254 (8)
H1110.06690.59210.59060.038*
H1210.04980.65270.49220.038*
H1310.09520.61370.52400.038*
C110.1190 (4)0.79804 (19)0.5638 (2)0.0156 (7)
C210.2431 (4)0.8290 (2)0.5957 (3)0.0207 (8)
H210.27170.80810.65700.025*
C310.3261 (4)0.8906 (2)0.5381 (3)0.0277 (9)
H310.41280.91090.55920.033*
C410.2831 (4)0.9222 (2)0.4509 (3)0.0292 (9)
H410.33810.96550.41300.035*
C510.1599 (5)0.8910 (2)0.4182 (3)0.0328 (10)
H510.13190.91220.35680.039*
C610.0775 (4)0.8296 (2)0.4739 (3)0.0297 (9)
H610.00750.80860.45130.036*
C120.1785 (4)0.7612 (2)0.6796 (2)0.0158 (7)
C220.3037 (4)0.7143 (2)0.6761 (2)0.0183 (7)
H220.29280.66070.64810.022*
C320.4455 (4)0.7463 (2)0.7138 (3)0.0210 (8)
H320.53150.71450.71140.025*
C420.4610 (4)0.8241 (2)0.7546 (3)0.0227 (8)
H420.55780.84550.78070.027*
C520.3353 (4)0.8715 (2)0.7577 (3)0.0236 (8)
H520.34630.92530.78530.028*
C620.1945 (4)0.8397 (2)0.7203 (3)0.0211 (8)
H620.10870.87160.72240.025*
C130.0826 (4)0.68715 (19)0.7461 (2)0.0154 (7)
C230.1450 (4)0.6100 (2)0.7468 (3)0.0190 (8)
H230.14560.57400.68940.023*
C330.2064 (4)0.5858 (2)0.8313 (3)0.0254 (9)
H330.24970.53330.83170.031*
C430.2043 (4)0.6387 (3)0.9156 (3)0.0259 (9)
H430.24510.62190.97400.031*
C530.1429 (4)0.7155 (2)0.9143 (3)0.0266 (9)
H530.14290.75150.97170.032*
C630.0815 (4)0.7405 (2)0.8306 (3)0.0214 (8)
H630.03910.79320.83020.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re0.01165 (8)0.00856 (7)0.01278 (8)0.00030 (12)0.00211 (6)0.00037 (12)
Cl20.0359 (5)0.0136 (5)0.0191 (4)0.0011 (3)0.0137 (3)0.0003 (3)
Cl10.0174 (4)0.0103 (4)0.0209 (4)0.0019 (3)0.0006 (3)0.0001 (3)
Cl30.0143 (4)0.0141 (4)0.0295 (5)0.0028 (3)0.0030 (4)0.0003 (3)
P0.0136 (5)0.0179 (4)0.0137 (4)0.0000 (3)0.0023 (4)0.0046 (3)
C10.025 (2)0.027 (2)0.0229 (18)0.0021 (16)0.0025 (16)0.0129 (15)
C110.0140 (19)0.0165 (17)0.0149 (16)0.0003 (13)0.0005 (14)0.0020 (13)
C210.022 (2)0.0181 (19)0.0225 (19)0.0001 (15)0.0070 (17)0.0021 (15)
C310.019 (2)0.021 (2)0.042 (3)0.0035 (16)0.0030 (19)0.0053 (17)
C410.030 (2)0.023 (2)0.029 (2)0.0033 (17)0.0055 (18)0.0001 (16)
C510.044 (3)0.039 (2)0.0142 (18)0.002 (2)0.0048 (18)0.0064 (16)
C610.031 (2)0.040 (2)0.0193 (19)0.0048 (18)0.0084 (17)0.0040 (17)
C120.0136 (18)0.0188 (18)0.0144 (16)0.0010 (13)0.0013 (14)0.0004 (13)
C220.021 (2)0.0188 (18)0.0162 (17)0.0003 (14)0.0064 (15)0.0021 (13)
C320.015 (2)0.032 (2)0.0172 (17)0.0011 (15)0.0057 (15)0.0004 (15)
C420.018 (2)0.036 (2)0.0140 (17)0.0076 (16)0.0024 (15)0.0033 (15)
C520.020 (2)0.0233 (19)0.028 (2)0.0051 (15)0.0050 (16)0.0071 (15)
C620.015 (2)0.025 (2)0.0244 (19)0.0020 (15)0.0064 (16)0.0031 (15)
C130.0140 (19)0.0171 (17)0.0143 (16)0.0019 (13)0.0007 (14)0.0015 (13)
C230.0149 (19)0.0227 (19)0.0167 (17)0.0004 (14)0.0033 (14)0.0028 (14)
C330.023 (2)0.0218 (19)0.028 (2)0.0073 (15)0.0053 (16)0.0067 (16)
C430.015 (2)0.041 (3)0.022 (2)0.0022 (18)0.0038 (17)0.0077 (19)
C530.033 (2)0.029 (2)0.0191 (19)0.0078 (17)0.0077 (17)0.0040 (15)
C630.024 (2)0.0184 (18)0.0214 (18)0.0050 (15)0.0045 (16)0.0028 (14)
Geometric parameters (Å, º) top
Re—Cl12.3549 (10)C61—H610.95
Re—Cl22.3604 (11)C12—C621.389 (5)
Re—Cl32.3644 (12)C12—C221.390 (5)
Re—Cl1i2.3549 (10)C22—C321.395 (5)
Re—Cl2i2.3604 (11)C22—H220.95
Re—Cl3i2.3644 (12)C32—C421.380 (5)
P—C11.783 (3)C32—H320.95
P—C131.793 (3)C42—C521.397 (5)
P—C111.800 (3)C42—H420.95
P—C121.804 (3)C52—C621.385 (5)
C1—H1110.98C52—H520.95
C1—H1210.98C62—H620.95
C1—H1310.98C13—C231.391 (4)
C11—C211.381 (5)C13—C631.401 (4)
C11—C611.396 (5)C23—C331.386 (5)
C21—C311.390 (5)C23—H230.95
C21—H210.95C33—C431.393 (5)
C31—C411.371 (5)C33—H330.95
C31—H310.95C43—C531.383 (5)
C41—C511.380 (5)C43—H430.95
C41—H410.95C53—C631.382 (5)
C51—C611.376 (5)C53—H530.95
C51—H510.95C63—H630.95
Cl1—Re—Cl289.85 (3)C22—C12—P120.2 (3)
Cl1—Re—Cl389.14 (4)C12—C22—C32119.7 (3)
Cl2—Re—Cl389.60 (4)C12—C22—H22120.1
C1—P—C13110.0 (1)C32—C22—H22120.1
C1—P—C11109.6 (1)C42—C32—C22120.0 (3)
C13—P—C11110.3 (1)C42—C32—H32120.0
C1—P—C12109.0 (1)C22—C32—H32120.0
C13—P—C12110.7 (1)C32—C42—C52120.4 (3)
C11—P—C12107.0 (1)C32—C42—H42119.8
P—C1—H111109.5C52—C42—H42119.8
P—C1—H121109.5C62—C52—C42119.5 (3)
H111—C1—H121109.5C62—C52—H52120.3
P—C1—H131109.5C42—C52—H52120.3
H111—C1—H131109.5C52—C62—C12120.3 (3)
H121—C1—H131109.5C52—C62—H62119.9
C21—C11—C61119.4 (3)C12—C62—H62119.9
C21—C11—P122.2 (3)C23—C13—C63120.2 (3)
C61—C11—P118.4 (3)C23—C13—P120.0 (3)
C11—C21—C31120.1 (4)C63—C13—P119.8 (3)
C11—C21—H21119.9C33—C23—C13119.9 (3)
C31—C21—H21119.9C33—C23—H23120.0
C41—C31—C21120.1 (4)C13—C23—H23120.0
C41—C31—H31120.0C23—C33—C43119.8 (3)
C21—C31—H31120.0C23—C33—H33120.1
C31—C41—C51120.1 (4)C43—C33—H33120.1
C31—C41—H41120.0C53—C43—C33120.1 (4)
C51—C41—H41120.0C53—C43—H43120.0
C61—C51—C41120.4 (4)C33—C43—H43120.0
C61—C51—H51119.8C63—C53—C43120.7 (3)
C41—C51—H51119.8C63—C53—H53119.6
C51—C61—C11119.9 (4)C43—C53—H53119.6
C51—C61—H61120.1C53—C63—C13119.2 (3)
C11—C61—H61120.1C53—C63—H63120.4
C62—C12—C22120.1 (3)C13—C63—H63120.4
C62—C12—P119.7 (3)
C1—P—C11—C21123.7 (3)P—C12—C22—C32177.5 (2)
C13—P—C11—C212.4 (3)C12—C22—C32—C420.1 (5)
C12—P—C11—C21118.2 (3)C22—C32—C42—C520.5 (5)
C1—P—C11—C6157.6 (3)C32—C42—C52—C620.5 (5)
C13—P—C11—C61178.8 (3)C42—C52—C62—C120.2 (5)
C12—P—C11—C6160.6 (3)C22—C12—C62—C520.2 (5)
C61—C11—C21—C310.4 (5)P—C12—C62—C52177.6 (3)
P—C11—C21—C31179.1 (3)C1—P—C13—C2310.1 (3)
C11—C21—C31—C411.5 (6)C11—P—C13—C23111.0 (3)
C21—C31—C41—C512.1 (6)C12—P—C13—C23130.7 (3)
C31—C41—C51—C611.5 (6)C1—P—C13—C63170.8 (3)
C41—C51—C61—C110.4 (6)C11—P—C13—C6368.1 (3)
C21—C11—C61—C510.1 (5)C12—P—C13—C6350.2 (3)
P—C11—C61—C51178.6 (3)C63—C13—C23—C330.0 (5)
C1—P—C12—C62161.3 (3)P—C13—C23—C33179.1 (3)
C13—P—C12—C6277.5 (3)C13—C23—C33—C430.5 (5)
C11—P—C12—C6242.8 (3)C23—C33—C43—C530.8 (6)
C1—P—C12—C2220.9 (3)C33—C43—C53—C630.8 (6)
C13—P—C12—C22100.3 (3)C43—C53—C63—C130.3 (6)
C11—P—C12—C22139.4 (3)C23—C13—C63—C530.1 (5)
C62—C12—C22—C320.2 (5)P—C13—C63—C53179.2 (3)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C22—H22···Cl2i0.952.743.527 (4)141
C62—H62···Cl2ii0.952.813.523 (4)133
C1—H131···Cl1iii0.982.713.570 (4)147
C63—H63···Cl1ii0.952.833.426 (4)122
C1—H121···Cl30.982.853.473 (4)122
C42—H42···Cl3iv0.952.833.712 (4)155
C23—H23···Cl3v0.952.733.567 (4)147
Symmetry codes: (i) x+1, y+1, z+1; (ii) x1/2, y+3/2, z+1/2; (iii) x1, y, z; (iv) x+1/2, y+3/2, z+1/2; (v) x, y+1, z+1.

Experimental details

Crystal data
Chemical formula(C19H18P)2[ReCl6]
Mr953.52
Crystal system, space groupMonoclinic, P21/n
Temperature (K)100
a, b, c (Å)9.155 (4), 16.429 (5), 12.964 (5)
β (°) 101.61 (3)
V3)1910 (1)
Z2
Radiation typeMo Kα
µ (mm1)3.71
Crystal size (mm)0.23 × 0.04 × 0.03
Data collection
DiffractometerOxford Diffraction KM-4-CCD
Absorption correctionAnalytical
(CrysAlis RED; Oxford Diffraction, 2006)
Tmin, Tmax0.597, 0.894
No. of measured, independent and
observed [I > 2σ(I)] reflections
27585, 7666, 5027
Rint0.083
(sin θ/λ)max1)0.807
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.053, 0.056, 1.00
No. of reflections7666
No. of parameters214
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.82, 0.98

Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg & Putz, 2005).

Selected bond lengths (Å) top
Re—Cl12.3549 (10)Re—Cl32.3644 (12)
Re—Cl22.3604 (11)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C22—H22···Cl2i0.952.743.527 (4)141
C62—H62···Cl2ii0.952.813.523 (4)133
C1—H131···Cl1iii0.982.713.570 (4)147
C63—H63···Cl1ii0.952.833.426 (4)122
C1—H121···Cl30.982.853.473 (4)122
C42—H42···Cl3iv0.952.833.712 (4)155
C23—H23···Cl3v0.952.733.567 (4)147
Symmetry codes: (i) x+1, y+1, z+1; (ii) x1/2, y+3/2, z+1/2; (iii) x1, y, z; (iv) x+1/2, y+3/2, z+1/2; (v) x, y+1, z+1.
 

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