μ-Hydroxido-bis­[(2,2′-bipyridine)tricarbonyl­rhenium(I)] perrhenate

Ruth, K.; Morawitz, T.; Lerner, H.-W.; Bolte, M.

doi:10.1107/S160053680800490X

μ-Hydroxido-bis[(2,2′-bipyridine)tricarbonylrhenium(I)] perrhenate

K. Ruth, T. Morawitz, H.-W. Lerner and M. Bolte

The title compound, [Re₂(OH)(C₁₀H₈N₂)₂(CO)₆][ReO₄], is a mixed-valence rhenium compound containing discrete anions and cations. The Re^I atoms are in a slightly distorted octahedral environment, whereas the Re^VII atoms show the typical tetrahedral coordination mode. The dihedral angle between the two bipyridine groups is 34.3 (7)°.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680800490X/at2546sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S160053680800490X/at2546Isup2.hkl Contains datablock I

CCDC reference: 673905

checkCIF report

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.044 Å
R factor = 0.093
wR factor = 0.262
Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT342_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ...         44

Alert level C
DIFMN02_ALERT_2_C  The minimum difference density is < -0.1*ZMAX*0.75
            _refine_diff_density_min given =     -5.650
            Test value =     -5.625
DIFMN03_ALERT_1_C  The minimum difference density is < -0.1*ZMAX*0.75
            The relevant atom site should be identified.
RFACR01_ALERT_3_C  The value of the weighted R factor is > 0.25
            Weighted R factor given   0.262
PLAT084_ALERT_2_C High R2 Value ..................................       0.26
PLAT213_ALERT_2_C Atom C25     has ADP max/min Ratio .............       3.20 prola
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C13
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C16
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C23
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C25
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C43
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        N11
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Re3
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          1
            C3  -RE1 -C1  -O1     17.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          2
            C2  -RE1 -C1  -O1     10.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          3
            O7  -RE1 -C1  -O1      8.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          4
            N41 -RE1 -C1  -O1      1.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          5
            N31 -RE1 -C1  -O1      0.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          6
            C3  -RE1 -C2  -O2    -19.00 27.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          7
            C1  -RE1 -C2  -O2     68.00 27.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          8
            O7  -RE1 -C2  -O2   -127.00 25.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          9
            N41 -RE1 -C2  -O2    164.00 27.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         10
            N31 -RE1 -C2  -O2   -121.00 27.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         11
            C2  -RE1 -C3  -O3     10.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         12
            C1  -RE1 -C3  -O3      1.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         13
            O7  -RE1 -C3  -O3      9.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         14
            N41 -RE1 -C3  -O3     11.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         15
            N31 -RE1 -C3  -O3     16.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         16
            C6  -RE2 -C4  -O4     35.00 28.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         17
            C5  -RE2 -C4  -O4    125.00 29.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         18
            N11 -RE2 -C4  -O4      3.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         19
            O7  -RE2 -C4  -O4   -145.00 28.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         20
            N21 -RE2 -C4  -O4    -62.00 29.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         21
            C4  -RE2 -C5  -O5     13.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         22
            C6  -RE2 -C5  -O5     14.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         23
            N11 -RE2 -C5  -O5      5.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         24
            O7  -RE2 -C5  -O5      3.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         25
            N21 -RE2 -C5  -O5      1.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         26
            C4  -RE2 -C6  -O6      9.00  0.00   1.555   1.555   1.555   1.555
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            C5  -RE2 -C6  -O6     17.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         28
            N11 -RE2 -C6  -O6      9.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         29
            O7  -RE2 -C6  -O6     10.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         30
            N21 -RE2 -C6  -O6      1.00  0.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         32
            C2  -RE1 -O7  -RE2  -143.00  7.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         37
            C6  -RE2 -O7  -RE1  -173.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         41
            C4  -RE2 -N11 -C12   -40.00  7.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         46
            C4  -RE2 -N11 -C16   136.00  6.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         72
            C5  -RE2 -N21 -C26   121.00  5.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         77
            C5  -RE2 -N21 -C11   -53.00  6.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         89
            C1  -RE1 -N31 -C32     1.00  6.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         94
            C1  -RE1 -N31 -C36   179.00  5.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        108
            C3  -RE1 -N41 -C46   123.00  8.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        113
            C3  -RE1 -N41 -C42   -48.00  9.00   1.555   1.555   1.555   1.555

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  52 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   9 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
  41 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

We report here the X-ray crystal structure analysis of the mixed-valence rhenium compound [(Re(CO)₃bipy)₂OH]⁺[ReO₄]^- (bipy = C₁₀H₆N₂). Thereby Re features in the cation an oxidation state +1 whereas in the perrhenate anion the Re center possesses the oxidation number +7. Surprisingly we have obtained the title compound as an oxidation and hydrolysis product of [Re(CO)₃(bipy)O₃SCF₃]. X-ray quality crystals of the title compound were grown by diffusion of hexane into a tetrahydrofuran solution of the mixed-valence rhenium compound [(Re(CO)₃bipy)₂OH]⁺[ReO₄]^- at ambient temperature.

The title compound, [C₂₆H₁₇N₄O₇Re₂]⁺[ReO₄]^-, is a mixed-valence rhenium compound containing discrete anions and cations. The Re^I atoms are in a slightly distorted octahedral environment, whereas the Re^VII atoms show the typical tetrahedral coordination mode. The dihedral angle between the two bipyridine moieties is 34.3 (7)°. A comparable compound with the bipyridine residues substituted by methyl groups in the para-position to the N atoms was determined by Gibson et al. (2003).

Related literature top

For related literature, see: Gibson et al. (2003).

Experimental top

The title compound was obtained as an oxidation and hydrolysis product of [Re(CO)₃(bipy)O₃SCF₃] from a mixture of [Re(CO)₃(bipy)O₃SCF₃] (54 mg, 0.09 mmol) and 17.5 ml tetrahydrofuran. X-ray quality crystals of the title compound were grown by diffusion of hexane into a solution of the mixed-valence rhenium compound [(Re(CO)₃bipy)₂OH]⁺[ReO₄]^- in tetrahydrofuran at ambient temperature.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. Perspective view of the title compound with the atom numbering scheme; displacement ellipsoids are at the 30% probability level. H atoms are drawn as small spheres of arbitrary radii.

µ-Hydroxido-bis[(2,2'-bipyridine)tricarbonylrhenium(I)] perrhenate top

Crystal data top

[Re₂(OH)(C₁₀H₈N₂)₂(CO)₆][ReO₄]	Z = 2
M_r = 1120.04	F(000) = 1028
Triclinic, P1	D_x = 2.509 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.0304 (7) Å	Cell parameters from 19460 reflections
b = 11.0506 (9) Å	θ = 3.8–25.6°
c = 15.5152 (13) Å	µ = 12.28 mm⁻¹
α = 96.488 (7)°	T = 173 K
β = 94.768 (7)°	Block, orange
γ = 104.038 (6)°	0.16 × 0.15 × 0.14 mm
V = 1482.6 (2) Å³

Data collection top

Stoe IPDSII two-circle diffractometer	5550 independent reflections
Radiation source: fine-focus sealed tube	4782 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.090
ω scans	θ_max = 25.7°, θ_min = 3.7°
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995)	h = −10→10
T_min = 0.143, T_max = 0.188	k = −13→13
21159 measured reflections	l = −18→18

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.092	H-atom parameters constrained
wR(F²) = 0.262	w = 1/[σ²(F_o²) + (0.1565P)² + 50.8834P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max < 0.001
5550 reflections	Δρ_max = 4.57 e Å⁻³
398 parameters	Δρ_min = −5.65 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0058 (8)

Crystal data top

[Re₂(OH)(C₁₀H₈N₂)₂(CO)₆][ReO₄]	γ = 104.038 (6)°
M_r = 1120.04	V = 1482.6 (2) Å³
Triclinic, P1	Z = 2
a = 9.0304 (7) Å	Mo Kα radiation
b = 11.0506 (9) Å	µ = 12.28 mm⁻¹
c = 15.5152 (13) Å	T = 173 K
α = 96.488 (7)°	0.16 × 0.15 × 0.14 mm
β = 94.768 (7)°

Data collection top

Stoe IPDSII two-circle diffractometer	5550 independent reflections
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995)	4782 reflections with I > 2σ(I)
T_min = 0.143, T_max = 0.188	R_int = 0.090
21159 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.092	0 restraints
wR(F²) = 0.262	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.1565P)² + 50.8834P] where P = (F_o² + 2F_c²)/3
5550 reflections	Δρ_max = 4.57 e Å⁻³
398 parameters	Δρ_min = −5.65 e Å⁻³

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

	x	y	z	U_iso*/U_eq
Re1	0.76687 (9)	0.89450 (8)	0.70601 (5)	0.0392 (3)
C1	0.770 (3)	1.024 (3)	0.806 (2)	0.057 (7)
O1	0.771 (3)	1.0983 (16)	0.8628 (12)	0.069 (5)
C2	0.910 (3)	1.022 (3)	0.657 (2)	0.062 (7)
O2	1.004 (2)	1.0976 (19)	0.6342 (15)	0.073 (6)
C3	0.933 (3)	0.858 (2)	0.7703 (14)	0.052 (6)
O3	1.037 (2)	0.839 (2)	0.8152 (13)	0.071 (5)
Re2	0.42562 (9)	0.72867 (7)	0.83203 (5)	0.0352 (3)
C4	0.419 (3)	0.901 (2)	0.8481 (17)	0.052 (6)
O4	0.413 (3)	1.0039 (17)	0.8637 (16)	0.077 (6)
C5	0.270 (3)	0.706 (2)	0.7326 (16)	0.052 (6)
O5	0.181 (2)	0.689 (3)	0.6702 (13)	0.081 (7)
C6	0.266 (3)	0.705 (2)	0.9084 (13)	0.044 (5)
O6	0.175 (2)	0.6920 (19)	0.9559 (11)	0.061 (5)
O7	0.6037 (16)	0.7393 (13)	0.7439 (9)	0.038 (3)
H7	0.6092	0.6704	0.7208	0.046*
N11	0.441 (2)	0.5359 (17)	0.8331 (12)	0.044 (4)
C11	0.664 (3)	0.626 (2)	0.9353 (15)	0.046 (5)
C12	0.554 (4)	0.515 (2)	0.8855 (18)	0.062 (8)
C13	0.574 (5)	0.394 (3)	0.891 (2)	0.093 (14)
H13	0.6594	0.3841	0.9270	0.111*
C14	0.475 (3)	0.290 (3)	0.845 (2)	0.093 (6)
H14	0.4887	0.2082	0.8462	0.112*
C15	0.349 (4)	0.313 (2)	0.796 (2)	0.093 (6)
H15	0.2705	0.2424	0.7682	0.112*
C16	0.333 (5)	0.4335 (19)	0.786 (2)	0.093 (6)
H16	0.2511	0.4449	0.7476	0.111*
N21	0.620 (2)	0.7420 (17)	0.9301 (11)	0.040 (4)
C23	0.801 (4)	0.630 (4)	0.9854 (18)	0.083 (11)
H23	0.8352	0.5555	0.9873	0.100*
C24	0.883 (4)	0.739 (4)	1.031 (2)	0.079 (10)
H24	0.9750	0.7386	1.0654	0.095*
C25	0.846 (3)	0.850 (5)	1.0319 (17)	0.094 (14)
H25	0.9072	0.9244	1.0663	0.113*
C26	0.701 (3)	0.849 (2)	0.9750 (16)	0.053 (6)
H26	0.6697	0.9247	0.9717	0.063*
N31	0.728 (2)	0.755 (2)	0.5863 (14)	0.051 (5)
C32	0.602 (3)	0.747 (2)	0.5346 (13)	0.050 (6)
C33	0.560 (4)	0.651 (3)	0.4601 (17)	0.064 (7)
H33	0.4649	0.6393	0.4249	0.077*
C34	0.656 (4)	0.577 (4)	0.4399 (18)	0.087 (12)
H34	0.6272	0.5122	0.3915	0.104*
C35	0.795 (5)	0.597 (3)	0.490 (2)	0.083 (9)
H35	0.8670	0.5513	0.4741	0.100*
C36	0.828 (4)	0.687 (3)	0.5675 (17)	0.059 (7)
H36	0.9202	0.6991	0.6050	0.071*
N41	0.565 (2)	0.9191 (17)	0.6320 (11)	0.040 (4)
C42	0.501 (2)	0.826 (2)	0.5597 (13)	0.043 (5)
C43	0.365 (4)	0.827 (3)	0.513 (2)	0.071 (8)
H43	0.3297	0.7712	0.4605	0.085*
C44	0.277 (3)	0.911 (3)	0.5419 (16)	0.057 (6)
H44	0.1766	0.9049	0.5152	0.068*
C45	0.349 (3)	1.003 (3)	0.6129 (17)	0.056 (6)
H45	0.2990	1.0663	0.6312	0.067*
C46	0.484 (3)	1.005 (2)	0.6555 (16)	0.047 (5)
H46	0.5257	1.0682	0.7039	0.056*
Re3	0.84808 (14)	0.42214 (11)	0.72586 (9)	0.0663 (4)
O31	0.757 (3)	0.5413 (19)	0.7321 (13)	0.070 (5)
O32	0.705 (3)	0.286 (2)	0.7035 (13)	0.092 (8)
O33	0.930 (4)	0.422 (3)	0.831 (2)	0.126 (12)
O34	0.922 (6)	0.429 (3)	0.639 (2)	0.157 (17)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Re1	0.0339 (5)	0.0455 (5)	0.0412 (5)	0.0145 (3)	0.0033 (3)	0.0087 (3)
C1	0.042 (12)	0.061 (15)	0.080 (19)	0.022 (11)	0.010 (11)	0.038 (14)
O1	0.117 (17)	0.035 (8)	0.046 (10)	0.010 (9)	0.009 (10)	−0.014 (7)
C2	0.037 (12)	0.060 (15)	0.09 (2)	0.005 (11)	0.005 (12)	0.017 (14)
O2	0.063 (12)	0.063 (11)	0.087 (14)	−0.007 (9)	0.009 (10)	0.035 (10)
C3	0.062 (14)	0.065 (15)	0.029 (10)	0.026 (12)	0.012 (10)	−0.014 (10)
O3	0.057 (11)	0.098 (15)	0.066 (12)	0.047 (11)	−0.013 (9)	0.005 (10)
Re2	0.0400 (5)	0.0361 (5)	0.0358 (5)	0.0188 (3)	0.0109 (3)	0.0060 (3)
C4	0.057 (14)	0.055 (14)	0.057 (14)	0.031 (11)	0.027 (11)	0.012 (11)
O4	0.091 (14)	0.045 (10)	0.116 (18)	0.041 (10)	0.056 (13)	0.023 (10)
C5	0.061 (14)	0.055 (13)	0.050 (13)	0.018 (11)	0.031 (12)	0.025 (11)
O5	0.052 (10)	0.14 (2)	0.051 (11)	0.011 (11)	−0.008 (9)	0.047 (12)
C6	0.059 (13)	0.054 (12)	0.034 (10)	0.039 (11)	0.007 (9)	0.017 (9)
O6	0.069 (11)	0.080 (12)	0.048 (10)	0.027 (9)	0.032 (9)	0.025 (9)
O7	0.042 (7)	0.032 (7)	0.044 (8)	0.014 (6)	0.012 (6)	0.005 (6)
N11	0.047 (10)	0.041 (9)	0.047 (10)	0.008 (8)	0.016 (8)	0.012 (8)
C11	0.043 (11)	0.061 (13)	0.045 (12)	0.027 (10)	0.009 (9)	0.015 (10)
C12	0.10 (2)	0.050 (13)	0.058 (15)	0.045 (14)	0.051 (15)	0.025 (12)
C13	0.18 (4)	0.09 (2)	0.066 (18)	0.10 (3)	0.08 (2)	0.053 (17)
C14	0.144 (16)	0.030 (7)	0.103 (14)	0.003 (9)	0.071 (12)	−0.001 (8)
C15	0.144 (16)	0.030 (7)	0.103 (14)	0.003 (9)	0.071 (12)	−0.001 (8)
C16	0.144 (16)	0.030 (7)	0.103 (14)	0.003 (9)	0.071 (12)	−0.001 (8)
N21	0.041 (9)	0.045 (9)	0.031 (8)	0.008 (7)	0.013 (7)	0.003 (7)
C23	0.08 (2)	0.15 (3)	0.041 (14)	0.07 (2)	0.011 (14)	0.004 (18)
C24	0.059 (17)	0.13 (3)	0.065 (19)	0.05 (2)	0.036 (15)	0.01 (2)
C25	0.041 (14)	0.18 (4)	0.034 (13)	−0.006 (19)	−0.008 (11)	−0.025 (18)
C26	0.051 (13)	0.045 (12)	0.052 (13)	−0.002 (10)	0.006 (10)	−0.008 (10)
N31	0.042 (10)	0.058 (12)	0.058 (12)	0.016 (9)	0.011 (9)	0.018 (9)
C32	0.060 (14)	0.062 (14)	0.019 (9)	0.000 (11)	0.000 (9)	0.007 (9)
C33	0.081 (18)	0.067 (16)	0.046 (14)	0.032 (14)	0.013 (12)	−0.017 (12)
C34	0.12 (3)	0.12 (3)	0.037 (14)	0.08 (3)	0.024 (17)	−0.007 (16)
C35	0.10 (3)	0.08 (2)	0.08 (2)	0.035 (19)	0.04 (2)	0.016 (17)
C36	0.086 (18)	0.062 (15)	0.051 (14)	0.051 (14)	0.025 (13)	0.014 (11)
N41	0.046 (9)	0.049 (10)	0.036 (9)	0.029 (8)	0.015 (7)	0.010 (7)
C42	0.042 (11)	0.054 (12)	0.026 (9)	0.000 (9)	0.001 (8)	0.002 (9)
C43	0.064 (17)	0.08 (2)	0.067 (18)	0.011 (15)	0.010 (14)	0.017 (15)
C44	0.033 (11)	0.10 (2)	0.043 (12)	0.029 (12)	0.005 (9)	0.012 (13)
C45	0.064 (15)	0.069 (16)	0.052 (14)	0.036 (13)	0.014 (11)	0.030 (12)
C46	0.048 (12)	0.050 (12)	0.049 (13)	0.022 (10)	0.014 (10)	0.008 (10)
Re3	0.0648 (7)	0.0588 (7)	0.0775 (9)	0.0190 (5)	0.0181 (6)	0.0039 (6)
O31	0.095 (14)	0.065 (11)	0.068 (12)	0.045 (11)	0.037 (11)	0.016 (9)
O32	0.109 (18)	0.091 (16)	0.048 (11)	−0.020 (13)	0.006 (11)	−0.008 (10)
O33	0.17 (3)	0.11 (2)	0.11 (2)	0.08 (2)	−0.03 (2)	−0.008 (17)
O34	0.27 (5)	0.087 (19)	0.15 (3)	0.06 (2)	0.13 (3)	0.027 (19)

Geometric parameters (Å, º) top

Re1—C3	1.88 (3)	C23—C24	1.34 (5)
Re1—C2	1.93 (3)	C23—H23	0.9500
Re1—C1	1.98 (3)	C24—C25	1.34 (6)
Re1—O7	2.146 (14)	C24—H24	0.9500
Re1—N41	2.165 (17)	C25—C26	1.51 (4)
Re1—N31	2.22 (2)	C25—H25	0.9500
C1—O1	1.13 (3)	C26—H26	0.9500
C2—O2	1.15 (3)	N31—C32	1.32 (3)
C3—O3	1.20 (3)	N31—C36	1.33 (3)
Re2—C4	1.91 (2)	C32—C33	1.43 (3)
Re2—C6	1.93 (2)	C32—C42	1.46 (4)
Re2—C5	1.95 (3)	C33—C34	1.36 (4)
Re2—N11	2.171 (18)	C33—H33	0.9500
Re2—O7	2.185 (14)	C34—C35	1.38 (5)
Re2—N21	2.190 (18)	C34—H34	0.9500
C4—O4	1.15 (3)	C35—C36	1.43 (4)
C5—O5	1.17 (3)	C35—H35	0.9500
C6—O6	1.15 (3)	C36—H36	0.9500
O7—H7	0.8199	N41—C46	1.37 (3)
N11—C12	1.33 (4)	N41—C42	1.41 (3)
N11—C16	1.39 (4)	C42—C43	1.37 (4)
C11—C23	1.39 (4)	C43—C44	1.41 (4)
C11—N21	1.44 (3)	C43—H43	0.9500
C11—C12	1.47 (4)	C44—C45	1.41 (4)
C12—C13	1.40 (3)	C44—H44	0.9500
C13—C14	1.35 (5)	C45—C46	1.33 (4)
C13—H13	0.9500	C45—H45	0.9500
C14—C15	1.41 (4)	C46—H46	0.9500
C14—H14	0.9500	Re3—O34	1.56 (3)
C15—C16	1.40 (3)	Re3—O32	1.71 (2)
C15—H15	0.9500	Re3—O31	1.710 (18)
C16—H16	0.9500	Re3—O33	1.73 (3)
N21—C26	1.32 (3)

C3—Re1—C2	89.7 (12)	C15—C16—H16	121.2
C3—Re1—C1	86.7 (9)	C26—N21—C11	122 (2)
C2—Re1—C1	88.0 (12)	C26—N21—Re2	123.2 (17)
C3—Re1—O7	92.6 (9)	C11—N21—Re2	114.8 (14)
C2—Re1—O7	172.7 (10)	C24—C23—C11	120 (3)
C1—Re1—O7	99.1 (8)	C24—C23—H23	120.2
C3—Re1—N41	174.9 (10)	C11—C23—H23	120.2
C2—Re1—N41	94.8 (9)	C23—C24—C25	125 (3)
C1—Re1—N41	95.9 (8)	C23—C24—H24	117.5
O7—Re1—N41	82.7 (6)	C25—C24—H24	117.5
C3—Re1—N31	102.1 (8)	C24—C25—C26	117 (3)
C2—Re1—N31	93.7 (11)	C24—C25—H25	121.7
C1—Re1—N31	171.1 (8)	C26—C25—H25	121.7
O7—Re1—N31	79.1 (6)	N21—C26—C25	119 (3)
N41—Re1—N31	75.2 (7)	N21—C26—H26	120.7
O1—C1—Re1	179 (2)	C25—C26—H26	120.7
O2—C2—Re1	174 (3)	C32—N31—C36	123 (2)
O3—C3—Re1	176.5 (18)	C32—N31—Re1	114.8 (17)
C4—Re2—C6	84.8 (9)	C36—N31—Re1	122.3 (18)
C4—Re2—C5	86.5 (11)	N31—C32—C33	119 (3)
C6—Re2—C5	89.6 (9)	N31—C32—C42	119 (2)
C4—Re2—N11	172.1 (9)	C33—C32—C42	122 (2)
C6—Re2—N11	91.2 (8)	C34—C33—C32	120 (3)
C5—Re2—N11	100.3 (9)	C34—C33—H33	120.0
C4—Re2—O7	99.7 (8)	C32—C33—H33	120.0
C6—Re2—O7	175.5 (7)	C33—C34—C35	120 (3)
C5—Re2—O7	90.3 (7)	C33—C34—H34	120.2
N11—Re2—O7	84.4 (6)	C35—C34—H34	120.2
C4—Re2—N21	98.5 (9)	C34—C35—C36	119 (3)
C6—Re2—N21	97.7 (7)	C34—C35—H35	120.6
C5—Re2—N21	171.5 (8)	C36—C35—H35	120.6
N11—Re2—N21	75.3 (7)	N31—C36—C35	120 (3)
O7—Re2—N21	82.2 (6)	N31—C36—H36	120.2
O4—C4—Re2	175 (2)	C35—C36—H36	120.2
O5—C5—Re2	176 (2)	C46—N41—C42	117.9 (19)
O6—C6—Re2	178 (2)	C46—N41—Re1	125.9 (15)
Re1—O7—Re2	132.8 (6)	C42—N41—Re1	115.6 (14)
Re1—O7—H7	113.6	C43—C42—N41	120 (2)
Re2—O7—H7	113.6	C43—C42—C32	126 (2)
C12—N11—C16	119 (2)	N41—C42—C32	113.5 (18)
C12—N11—Re2	118.4 (16)	C42—C43—C44	122 (3)
C16—N11—Re2	122.6 (18)	C42—C43—H43	119.2
C23—C11—N21	119 (3)	C44—C43—H43	119.2
C23—C11—C12	128 (3)	C45—C44—C43	115 (2)
N21—C11—C12	113.7 (19)	C45—C44—H44	122.4
N11—C12—C13	123 (3)	C43—C44—H44	122.4
N11—C12—C11	117 (2)	C46—C45—C44	123 (2)
C13—C12—C11	120 (3)	C46—C45—H45	118.7
C14—C13—C12	121 (4)	C44—C45—H45	118.7
C14—C13—H13	119.4	C45—C46—N41	122 (2)
C12—C13—H13	119.4	C45—C46—H46	118.8
C13—C14—C15	115 (3)	N41—C46—H46	118.8
C13—C14—H14	122.3	O34—Re3—O32	102.9 (18)
C15—C14—H14	122.3	O34—Re3—O31	104.5 (15)
C14—C15—C16	124 (3)	O32—Re3—O31	105.8 (13)
C14—C15—H15	118.1	O34—Re3—O33	130 (2)
C16—C15—H15	118.1	O32—Re3—O33	105.1 (15)
N11—C16—C15	118 (3)	O31—Re3—O33	106.2 (12)
N11—C16—H16	121.2

C3—Re1—C1—O1	−168 (100)	C12—C11—N21—C26	176 (2)
C2—Re1—C1—O1	102 (100)	C23—C11—N21—Re2	169.9 (19)
O7—Re1—C1—O1	−76 (100)	C12—C11—N21—Re2	−11 (2)
N41—Re1—C1—O1	7 (100)	C4—Re2—N21—C26	−4.7 (19)
N31—Re1—C1—O1	1 (100)	C6—Re2—N21—C26	−90.6 (18)
C3—Re1—C2—O2	−19 (27)	C5—Re2—N21—C26	121 (5)
C1—Re1—C2—O2	68 (27)	N11—Re2—N21—C26	−179.8 (18)
O7—Re1—C2—O2	−127 (25)	O7—Re2—N21—C26	94.0 (18)
N41—Re1—C2—O2	164 (27)	C4—Re2—N21—C11	−178.0 (15)
N31—Re1—C2—O2	−121 (27)	C6—Re2—N21—C11	96.1 (15)
C2—Re1—C3—O3	102 (42)	C5—Re2—N21—C11	−53 (6)
C1—Re1—C3—O3	14 (42)	N11—Re2—N21—C11	6.9 (13)
O7—Re1—C3—O3	−85 (42)	O7—Re2—N21—C11	−79.3 (14)
N41—Re1—C3—O3	−106 (40)	N21—C11—C23—C24	3 (4)
N31—Re1—C3—O3	−164 (41)	C12—C11—C23—C24	−176 (3)
C6—Re2—C4—O4	35 (28)	C11—C23—C24—C25	−1 (5)
C5—Re2—C4—O4	125 (29)	C23—C24—C25—C26	−1 (5)
N11—Re2—C4—O4	−25 (33)	C11—N21—C26—C25	1 (3)
O7—Re2—C4—O4	−145 (28)	Re2—N21—C26—C25	−171.7 (18)
N21—Re2—C4—O4	−62 (29)	C24—C25—C26—N21	1 (4)
C4—Re2—C5—O5	131 (33)	C3—Re1—N31—C32	170.4 (17)
C6—Re2—C5—O5	−144 (33)	C2—Re1—N31—C32	−99.1 (18)
N11—Re2—C5—O5	−53 (33)	C1—Re1—N31—C32	1 (6)
O7—Re2—C5—O5	32 (33)	O7—Re1—N31—C32	80.1 (16)
N21—Re2—C5—O5	5 (37)	N41—Re1—N31—C32	−5.1 (16)
C4—Re2—C6—O6	−85 (55)	C3—Re1—N31—C36	−11 (2)
C5—Re2—C6—O6	−171 (55)	C2—Re1—N31—C36	79 (2)
N11—Re2—C6—O6	88 (55)	C1—Re1—N31—C36	179 (5)
O7—Re2—C6—O6	101 (57)	O7—Re1—N31—C36	−102 (2)
N21—Re2—C6—O6	13 (56)	N41—Re1—N31—C36	173 (2)
C3—Re1—O7—Re2	108.3 (10)	C36—N31—C32—C33	8 (4)
C2—Re1—O7—Re2	−143 (7)	Re1—N31—C32—C33	−174.1 (19)
C1—Re1—O7—Re2	21.2 (12)	C36—N31—C32—C42	−179 (2)
N41—Re1—O7—Re2	−73.6 (10)	Re1—N31—C32—C42	−1 (3)
N31—Re1—O7—Re2	−149.9 (11)	N31—C32—C33—C34	−5 (4)
C4—Re2—O7—Re1	13.1 (12)	C42—C32—C33—C34	−178 (3)
C6—Re2—O7—Re1	−173 (9)	C32—C33—C34—C35	−1 (5)
C5—Re2—O7—Re1	99.5 (11)	C33—C34—C35—C36	6 (5)
N11—Re2—O7—Re1	−160.1 (10)	C32—N31—C36—C35	−3 (4)
N21—Re2—O7—Re1	−84.3 (10)	Re1—N31—C36—C35	179 (2)
C4—Re2—N11—C12	−40 (7)	C34—C35—C36—N31	−4 (5)
C6—Re2—N11—C12	−99.6 (17)	C3—Re1—N41—C46	123 (8)
C5—Re2—N11—C12	170.6 (17)	C2—Re1—N41—C46	−86 (2)
O7—Re2—N11—C12	81.4 (16)	C1—Re1—N41—C46	2.2 (19)
N21—Re2—N11—C12	−2.0 (16)	O7—Re1—N41—C46	100.6 (18)
C4—Re2—N11—C16	136 (6)	N31—Re1—N41—C46	−178.8 (19)
C6—Re2—N11—C16	76 (2)	C3—Re1—N41—C42	−48 (9)
C5—Re2—N11—C16	−14 (2)	C2—Re1—N41—C42	103.1 (17)
O7—Re2—N11—C16	−102.9 (19)	C1—Re1—N41—C42	−168.5 (15)
N21—Re2—N11—C16	174 (2)	O7—Re1—N41—C42	−70.1 (14)
C16—N11—C12—C13	4 (3)	N31—Re1—N41—C42	10.6 (14)
Re2—N11—C12—C13	−179.8 (18)	C46—N41—C42—C43	3 (3)
C16—N11—C12—C11	−179 (2)	Re1—N41—C42—C43	174.5 (19)
Re2—N11—C12—C11	−3 (3)	C46—N41—C42—C32	174.2 (19)
C23—C11—C12—N11	−171 (3)	Re1—N41—C42—C32	−14 (2)
N21—C11—C12—N11	9 (3)	N31—C32—C42—C43	−179 (2)
C23—C11—C12—C13	5 (4)	C33—C32—C42—C43	−7 (4)
N21—C11—C12—C13	−174 (2)	N31—C32—C42—N41	10 (3)
N11—C12—C13—C14	−3 (4)	C33—C32—C42—N41	−177 (2)
C11—C12—C13—C14	−180 (2)	N41—C42—C43—C44	−8 (4)
C12—C13—C14—C15	−2 (4)	C32—C42—C43—C44	−178 (2)
C13—C14—C15—C16	7 (5)	C42—C43—C44—C45	9 (4)
C12—N11—C16—C15	0 (4)	C43—C44—C45—C46	−6 (4)
Re2—N11—C16—C15	−176 (2)	C44—C45—C46—N41	2 (4)
C14—C15—C16—N11	−6 (5)	C42—N41—C46—C45	0 (3)
C23—C11—N21—C26	−4 (3)	Re1—N41—C46—C45	−170.4 (18)

Experimental details

Crystal data
Chemical formula	[Re₂(OH)(C₁₀H₈N₂)₂(CO)₆][ReO₄]
M_r	1120.04
Crystal system, space group	Triclinic, P1
Temperature (K)	173
a, b, c (Å)	9.0304 (7), 11.0506 (9), 15.5152 (13)
α, β, γ (°)	96.488 (7), 94.768 (7), 104.038 (6)
V (Å³)	1482.6 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	12.28
Crystal size (mm)	0.16 × 0.15 × 0.14

Data collection
Diffractometer	Stoe IPDSII two-circle diffractometer
Absorption correction	Multi-scan (MULABS; Spek, 2003; Blessing, 1995)
T_min, T_max	0.143, 0.188
No. of measured, independent and observed [I > 2σ(I)] reflections	21159, 5550, 4782
R_int	0.090
(sin θ/λ)_max (Å⁻¹)	0.609

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.092, 0.262, 1.05
No. of reflections	5550
No. of parameters	398
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.1565P)² + 50.8834P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	4.57, −5.65

Computer programs: X-AREA (Stoe & Cie, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL-Plus (Sheldrick, 2008).

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μ-Hydroxido-bis­[(2,2′-bipyridine)tricarbonyl­rhenium(I)] perrhenate

Supporting information

Key indicators

checkCIF/PLATON results

μ-Hydroxido-bis[(2,2′-bipyridine)tricarbonylrhenium(I)] perrhenate