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Acta Cryst. (2007). E63, m1968    [ doi:10.1107/S1600536807029923 ]

Tetrakis(2,2':6',2''-terpyridinium) hexabromidorhenate(IV) bis[aquatetrabromidooxidorhenate(V)] tetrabromide dihydrate

A. Kochel

Abstract top

The title compound, (C15H13N3)4[ReBr6][ReBr4O(H2O)]2Br4·2H2O, is a mixed-valence molecular salt containing rhenium(IV) (as centrosymmetric [ReBr6]2- anions) and rhenium(V) (as trans-[ReO(H2O)Br4]- oxidoanions). The Re-O and Re-Br distances are consistent with the different oxidation states of Re in the anions. A complex hydrogen-bonding network helps to establish the crystal packing.

Comment top

This paper reports the crystal structure of the title mixed valence rhenium compound, (I). One of rhenium atoms lies on a centre of symmetry and other one in general position.

Compound (I) (Fig. 1) and some of its derivatives show interesting magnetic properties (Rose et al., 1996). Several papers describing the crystal structures of bromorhenates are available in the literature (Preetz & Struess, 1988, Chiozzone et al., 2006) but surprisingly the crystal structure of (I) has not been determined yet.

The [ReO(H2O)Br4]− units in (I) shows a distorted octahedral geometry about the Re(V) site defined by the terminal oxo ligand, the trans aqua ligand, and four bromide ions (Table 1). The Re—Br bond lengths in (I) agree with those in related crystal structures (Kochel, 2007; Abram et al., 1996).

In the crystal packing of (I), layers of rhenate anions and terpyridinium cations could be distinguished. However, the anion layer is additionally filled with the water molecules and bromide anions. The crystal structure is consolidated by a complex hydrogen bond system including various C—H···O links (Table 2).

Related literature top

For related literature, see: Abram et al. (1996); Chiozzone et al. (2006); Kochel (2007); Rose et al. (1996); Preetz & Struess (1988); Watt & Thompson (1963).

Experimental top

(NH4)2ReBr6 was obtained by the method of Watt & Thompson (1963). A mixture of (NH4)2ReBr6 (0.46 g) and the terpy lignad (0.50 g) was dissolved in 50-ml of 1:1 v/v water-ethanol solution. Then it was sealed under nitrogen and heated for 15 h to 423 K. After the reaction the mixture colour was yellow orange. The solution was diluted with ethanol and left standing for evaporation. After five days orange plates of (I) appeared. Anal. Calc. C23.69 H 1.98 N 5.52 /% found C 21.40 H 1.20 N 5.14 /%.

Refinement top

The water H atoms were located in a difference map and refined as riding in their as-found relative positions with Uiso(H) = 1.2Ueq(O). The other H atoms were placed in idealized positions (N—H = 0.86 Å, C—H = 0.93 Å) and refined as riding with Uiso(H) = 1.2Ueq(carrier).

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, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003) and XP (Bruker, 1999); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I) showing 50% displacement ellipsoids (arbitrary spheres for the H atoms). Symmetry code: (i) −x, 1 − y, 1 − z.
[Figure 2] Fig. 2. The crystal packing in (I).
Tetrakis(2,2':6',2''-terpyridinium) hexabromidorhenate(IV) bis[aquatetrabromidooxidorhenate(V)] tetrabromide dihydrate top
Crystal data top
(C15H13N3)4[ReBr6][ReBr4O(H2O)]2Br4·2H2OZ = 1
Mr = 3042.03F000 = 1407
Triclinic, P1Dx = 2.578 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 10.3458 (6) ÅCell parameters from 5311 reflections
b = 10.3563 (6) Åθ = 2.7–28.6º
c = 19.0582 (14) ŵ = 13.85 mm−1
α = 81.361 (6)ºT = 100 (2) K
β = 79.041 (6)ºPrism, orange
γ = 79.987 (5)º0.10 × 0.10 × 0.05 mm
V = 1959.7 (2) Å3
Data collection top
Oxford Diffraction KM-4-CCD
diffractometer		9275 independent reflections
Radiation source: fine-focus sealed tube5991 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.056
T = 100(2) Kθmax = 28.6º
ω scansθmin = 2.7º
Absorption correction: numerical
(CrysAlis RED; Oxford Diffraction, 2003)		h = −13→13
Tmin = 0.456, Tmax = 0.794k = −13→13
24231 measured reflectionsl = −25→25
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.062  w = 1/[σ2(Fo2) + (0.0215P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.94(Δ/σ)max < 0.001
9275 reflectionsΔρmax = 1.24 e Å−3
448 parametersΔρmin = −0.94 e Å−3
4 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
(C15H13N3)4[ReBr6][ReBr4O(H2O)]2Br4·2H2Oγ = 79.987 (5)º
Mr = 3042.03V = 1959.7 (2) Å3
Triclinic, P1Z = 1
a = 10.3458 (6) ÅMo Kα
b = 10.3563 (6) ŵ = 13.85 mm−1
c = 19.0582 (14) ÅT = 100 (2) K
α = 81.361 (6)º0.10 × 0.10 × 0.05 mm
β = 79.041 (6)º
Data collection top
Oxford Diffraction KM-4-CCD
diffractometer		9275 independent reflections
Absorption correction: numerical
(CrysAlis RED; Oxford Diffraction, 2003)		5991 reflections with I > 2σ(I)
Tmin = 0.456, Tmax = 0.794Rint = 0.056
24231 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0364 restraints
wR(F2) = 0.062H-atom parameters constrained
S = 0.94Δρmax = 1.24 e Å−3
9275 reflectionsΔρmin = −0.94 e Å−3
448 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 > 2sigma(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
N10.1742 (5)0.0591 (5)0.6381 (3)0.0177 (12)
H1N0.19770.10540.66610.021*
N20.3703 (5)0.2058 (5)0.6009 (3)0.0173 (12)
N30.3926 (5)0.3432 (5)0.7045 (3)0.0186 (12)
H3N0.33930.28630.70890.022*
C10.0747 (7)−0.0095 (6)0.6643 (4)0.0261 (16)
H10.0315−0.00470.71160.031*
C20.0346 (6)−0.0877 (6)0.6222 (3)0.0210 (15)
H2−0.0351−0.13560.64030.025*
C30.1013 (6)−0.0925 (6)0.5524 (4)0.0255 (16)
H30.0786−0.14730.52370.031*
C40.2019 (6)−0.0166 (6)0.5246 (3)0.0193 (14)
H40.2430−0.01650.47680.023*
C50.2408 (6)0.0599 (5)0.5696 (3)0.0155 (14)
C60.3483 (6)0.1416 (5)0.5493 (3)0.0145 (13)
C70.4232 (6)0.1521 (6)0.4791 (3)0.0211 (15)
H70.40620.10740.44390.025*
C80.5220 (7)0.2300 (6)0.4644 (3)0.0215 (15)
H80.57280.23860.41860.026*
C90.5459 (6)0.2957 (6)0.5175 (3)0.0190 (14)
H90.61390.34720.50840.023*
C100.4666 (6)0.2831 (6)0.5845 (3)0.0160 (14)
C110.4774 (6)0.3597 (6)0.6420 (3)0.0168 (14)
C120.5655 (6)0.4496 (6)0.6356 (3)0.0206 (15)
H120.62710.46170.59370.025*
C130.5607 (6)0.5214 (6)0.6924 (3)0.0201 (15)
H130.61870.58240.68830.024*
C140.4699 (6)0.5021 (6)0.7550 (3)0.0214 (15)
H140.46540.55060.79290.026*
C150.3863 (6)0.4102 (6)0.7604 (3)0.0206 (15)
H150.32590.39450.80240.025*
N40.2439 (5)0.5363 (5)0.1040 (3)0.0184 (12)
H4N0.23350.47980.07750.022*
N50.0414 (5)0.3972 (5)0.1317 (2)0.0158 (11)
N60.0141 (5)0.2830 (5)0.0195 (3)0.0218 (13)
H6N0.07130.33480.01820.026*
C210.3407 (6)0.6082 (6)0.0809 (4)0.0235 (15)
H210.39430.59780.03640.028*
C220.3632 (7)0.6978 (6)0.1214 (4)0.0251 (16)
H220.43210.74760.10550.030*
C230.2800 (7)0.7120 (6)0.1872 (4)0.0245 (16)
H230.29210.77320.21550.029*
C240.1791 (6)0.6352 (6)0.2107 (3)0.0222 (15)
H240.12490.64320.25520.027*
C250.1599 (6)0.5473 (6)0.1676 (3)0.0182 (14)
C260.0557 (6)0.4606 (6)0.1854 (3)0.0173 (14)
C27−0.0240 (6)0.4503 (6)0.2539 (3)0.0203 (15)
H27−0.01350.49730.28980.024*
C28−0.1191 (6)0.3664 (6)0.2652 (3)0.0244 (16)
H28−0.17210.35430.31030.029*
C29−0.1359 (6)0.3010 (6)0.2104 (3)0.0203 (15)
H29−0.20080.24620.21750.024*
C30−0.0533 (6)0.3188 (6)0.1443 (3)0.0186 (14)
C31−0.0661 (6)0.2550 (6)0.0832 (3)0.0182 (14)
C32−0.1550 (6)0.1664 (6)0.0841 (4)0.0265 (16)
H32−0.21010.14110.12670.032*
C33−0.1602 (6)0.1163 (6)0.0211 (4)0.0243 (16)
H33−0.21980.05840.02160.029*
C34−0.0770 (6)0.1524 (6)−0.0426 (4)0.0256 (16)
H34−0.08070.1205−0.08510.031*
C350.0101 (6)0.2361 (6)−0.0406 (3)0.0220 (15)
H350.06820.2601−0.08220.026*
Re20.38002 (2)0.12190 (2)0.218448 (13)0.01424 (7)
Br40.56622 (6)0.13304 (6)0.28386 (3)0.01760 (14)
Br50.23701 (6)0.05495 (6)0.14103 (3)0.02149 (15)
Br60.49427 (7)0.24963 (6)0.10751 (3)0.02226 (15)
Br70.30660 (6)−0.05229 (6)0.31752 (3)0.01964 (15)
O10.5235 (4)−0.0491 (4)0.1763 (2)0.0189 (10)
H1W0.6001−0.06120.19320.023*
H2W0.5545−0.05550.13000.023*
O20.2755 (4)0.2512 (4)0.2478 (2)0.0202 (10)
Re10.00000.50000.50000.01419 (9)
Br10.07213 (6)0.68849 (6)0.40966 (3)0.01884 (15)
Br20.14274 (6)0.34007 (6)0.42001 (3)0.01800 (14)
Br30.19123 (6)0.50460 (6)0.56235 (3)0.02026 (15)
O3A0.6108 (4)0.8904 (4)0.0401 (2)0.0269 (11)
H3W0.62560.9008−0.00730.032*
H4W0.64220.80450.04810.032*
Br80.82755 (6)0.83705 (6)0.21020 (3)0.01960 (15)
Br90.73144 (6)0.56873 (6)0.05088 (3)0.01989 (15)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.022 (3)0.015 (3)0.020 (3)−0.003 (2)−0.005 (2)−0.012 (2)
N20.019 (3)0.012 (3)0.019 (3)0.001 (2)−0.004 (2)0.004 (2)
N30.023 (3)0.016 (3)0.018 (3)−0.004 (2)−0.003 (2)−0.004 (2)
C10.028 (4)0.029 (4)0.020 (4)0.003 (3)−0.010 (3)−0.001 (3)
C20.022 (4)0.016 (3)0.025 (4)−0.002 (3)−0.006 (3)0.000 (3)
C30.021 (4)0.024 (4)0.033 (4)0.004 (3)−0.006 (3)−0.011 (3)
C40.020 (4)0.025 (4)0.015 (3)0.001 (3)−0.005 (3)−0.010 (3)
C50.022 (4)0.009 (3)0.016 (3)0.003 (3)−0.007 (3)−0.003 (3)
C60.016 (3)0.009 (3)0.017 (3)0.004 (2)−0.002 (3)−0.003 (3)
C70.025 (4)0.021 (4)0.016 (3)0.007 (3)−0.009 (3)−0.004 (3)
C80.030 (4)0.021 (4)0.013 (3)−0.004 (3)−0.002 (3)−0.005 (3)
C90.020 (4)0.020 (3)0.016 (3)−0.002 (3)0.000 (3)−0.002 (3)
C100.021 (4)0.013 (3)0.014 (3)−0.001 (3)−0.008 (3)0.000 (3)
C110.016 (3)0.017 (3)0.018 (3)0.001 (3)−0.002 (3)−0.005 (3)
C120.009 (3)0.026 (4)0.025 (4)−0.002 (3)−0.001 (3)−0.001 (3)
C130.024 (4)0.017 (3)0.022 (4)−0.008 (3)−0.004 (3)−0.005 (3)
C140.026 (4)0.015 (3)0.025 (4)−0.005 (3)−0.002 (3)−0.010 (3)
C150.021 (4)0.021 (4)0.020 (4)0.000 (3)−0.007 (3)−0.002 (3)
N40.020 (3)0.017 (3)0.018 (3)−0.002 (2)−0.001 (2)−0.003 (2)
N50.018 (3)0.015 (3)0.012 (3)0.002 (2)−0.002 (2)0.002 (2)
N60.021 (3)0.023 (3)0.023 (3)−0.008 (2)−0.004 (3)0.000 (3)
C210.021 (4)0.024 (4)0.026 (4)−0.006 (3)0.001 (3)−0.007 (3)
C220.022 (4)0.020 (4)0.035 (4)−0.010 (3)−0.006 (3)0.003 (3)
C230.032 (4)0.011 (3)0.033 (4)−0.001 (3)−0.015 (3)−0.002 (3)
C240.023 (4)0.024 (4)0.017 (3)−0.001 (3)−0.003 (3)−0.001 (3)
C250.022 (4)0.017 (3)0.016 (3)−0.004 (3)−0.008 (3)0.003 (3)
C260.019 (4)0.015 (3)0.018 (3)0.002 (3)−0.008 (3)0.000 (3)
C270.024 (4)0.020 (4)0.017 (3)−0.001 (3)−0.005 (3)−0.007 (3)
C280.027 (4)0.022 (4)0.016 (3)0.003 (3)0.007 (3)0.002 (3)
C290.026 (4)0.016 (3)0.018 (3)−0.006 (3)−0.006 (3)0.008 (3)
C300.019 (4)0.013 (3)0.023 (4)−0.003 (3)−0.004 (3)0.002 (3)
C310.019 (4)0.021 (3)0.016 (3)−0.005 (3)−0.004 (3)0.000 (3)
C320.022 (4)0.031 (4)0.024 (4)−0.004 (3)−0.005 (3)0.003 (3)
C330.026 (4)0.022 (4)0.029 (4)−0.003 (3)−0.012 (3)−0.007 (3)
C340.027 (4)0.022 (4)0.031 (4)−0.004 (3)−0.012 (3)−0.003 (3)
C350.023 (4)0.025 (4)0.017 (3)0.002 (3)−0.001 (3)−0.010 (3)
Re20.01566 (15)0.01453 (14)0.01316 (14)−0.00219 (11)−0.00329 (11)−0.00269 (11)
Br40.0190 (4)0.0191 (3)0.0172 (3)−0.0046 (3)−0.0060 (3)−0.0042 (3)
Br50.0228 (4)0.0224 (4)0.0227 (4)−0.0037 (3)−0.0104 (3)−0.0050 (3)
Br60.0269 (4)0.0208 (4)0.0179 (3)−0.0054 (3)−0.0030 (3)0.0028 (3)
Br70.0213 (4)0.0215 (4)0.0153 (3)−0.0064 (3)0.0005 (3)−0.0007 (3)
O10.021 (2)0.017 (2)0.019 (2)−0.0025 (18)−0.0044 (19)−0.0049 (19)
O20.023 (2)0.018 (2)0.021 (2)0.0033 (18)−0.009 (2)−0.0073 (19)
Re10.0168 (2)0.01280 (19)0.01210 (19)−0.00249 (15)−0.00024 (16)−0.00106 (15)
Br10.0234 (4)0.0151 (3)0.0161 (3)−0.0048 (3)0.0003 (3)0.0017 (3)
Br20.0175 (3)0.0175 (3)0.0183 (3)−0.0012 (3)−0.0004 (3)−0.0051 (3)
Br30.0178 (3)0.0245 (4)0.0190 (3)−0.0031 (3)−0.0045 (3)−0.0027 (3)
O3A0.038 (3)0.023 (3)0.019 (2)−0.004 (2)0.003 (2)−0.010 (2)
Br80.0198 (3)0.0238 (4)0.0159 (3)−0.0051 (3)−0.0010 (3)−0.0052 (3)
Br90.0225 (4)0.0212 (4)0.0155 (3)−0.0050 (3)0.0005 (3)−0.0033 (3)
Geometric parameters (Å, °) top
N1—C11.329 (8)C21—C221.368 (8)
N1—C51.354 (7)C21—H210.9300
N1—H1N0.8600C22—C231.391 (9)
N2—C61.340 (7)C22—H220.9300
N2—C101.348 (7)C23—C241.388 (8)
N3—C151.341 (7)C23—H230.9299
N3—C111.345 (7)C24—C251.376 (8)
N3—H3N0.8600C24—H240.9301
C1—C21.382 (8)C25—C261.479 (8)
C1—H10.9298C26—C271.405 (8)
C2—C31.380 (9)C27—C281.389 (8)
C2—H20.9300C27—H270.9300
C3—C41.390 (8)C28—C291.380 (8)
C3—H30.9301C28—H280.9300
C4—C51.405 (8)C29—C301.388 (8)
C4—H40.9300C29—H290.9299
C5—C61.472 (8)C30—C311.460 (8)
C6—C71.412 (8)C31—C321.404 (8)
C7—C81.372 (8)C32—C331.391 (8)
C7—H70.9299C32—H320.9300
C8—C91.383 (8)C33—C341.390 (9)
C8—H80.9301C33—H330.9299
C9—C101.382 (8)C34—C351.365 (8)
C9—H90.9300C34—H340.9299
C10—C111.476 (8)C35—H350.9300
C11—C121.390 (8)Re1—Br3i2.5043 (6)
C12—C131.390 (8)Re1—Br32.5044 (6)
C12—H120.9301Re1—Br22.5099 (6)
C13—C141.384 (8)Re1—Br2i2.5100 (6)
C13—H130.9300Re1—Br12.5179 (6)
C14—C151.374 (8)Re1—Br1i2.5180 (6)
C14—H140.9299Re2—O21.663 (4)
C15—H150.9299Re2—O12.246 (4)
N4—C211.321 (7)Re2—Br72.5108 (7)
N4—C251.359 (7)Re2—Br42.5123 (7)
N4—H4N0.8600Re2—Br52.5182 (7)
N5—C261.340 (7)Re2—Br62.5239 (7)
N5—C301.343 (7)O1—H1W0.8929
N6—C351.318 (7)O1—H2W0.8879
N6—C311.357 (7)O3A—H3W0.8787
N6—H6N0.8600O3A—H4W0.8932
C1—N1—C5123.5 (5)C25—C24—H24120.3
C1—N1—H1N118.2C23—C24—H24120.2
C5—N1—H1N118.2N4—C25—C24118.2 (6)
C6—N2—C10118.4 (5)N4—C25—C26116.5 (5)
C15—N3—C11124.0 (5)C24—C25—C26125.3 (6)
C15—N3—H3N118.0N5—C26—C27123.4 (6)
C11—N3—H3N118.0N5—C26—C25115.5 (5)
N1—C1—C2120.7 (6)C27—C26—C25121.1 (6)
N1—C1—H1119.6C28—C27—C26116.7 (6)
C2—C1—H1119.6C28—C27—H27121.7
C3—C2—C1118.0 (6)C26—C27—H27121.6
C3—C2—H2121.0C29—C28—C27120.7 (6)
C1—C2—H2121.0C29—C28—H28119.7
C2—C3—C4120.8 (6)C27—C28—H28119.6
C2—C3—H3119.6C28—C29—C30118.2 (6)
C4—C3—H3119.6C28—C29—H29120.9
C3—C4—C5119.2 (6)C30—C29—H29120.8
C3—C4—H4120.4N5—C30—C29122.8 (6)
C5—C4—H4120.4N5—C30—C31115.5 (5)
N1—C5—C4117.6 (6)C29—C30—C31121.7 (6)
N1—C5—C6116.5 (5)N6—C31—C32116.3 (6)
C4—C5—C6125.9 (6)N6—C31—C30117.9 (5)
N2—C6—C7122.0 (6)C32—C31—C30125.7 (6)
N2—C6—C5116.3 (5)C33—C32—C31119.8 (6)
C7—C6—C5121.7 (6)C33—C32—H32120.1
C8—C7—C6118.2 (6)C31—C32—H32120.1
C8—C7—H7120.9C34—C33—C32120.4 (6)
C6—C7—H7120.9C34—C33—H33119.8
C7—C8—C9120.1 (6)C32—C33—H33119.8
C7—C8—H8119.9C35—C34—C33117.8 (6)
C9—C8—H8120.0C35—C34—H34121.1
C10—C9—C8118.5 (6)C33—C34—H34121.1
C10—C9—H9120.7N6—C35—C34121.2 (6)
C8—C9—H9120.8N6—C35—H35119.4
N2—C10—C9122.7 (6)C34—C35—H35119.4
N2—C10—C11115.4 (5)O2—Re2—O1178.43 (18)
C9—C10—C11121.8 (5)O2—Re2—Br798.52 (14)
N3—C11—C12117.9 (6)O1—Re2—Br783.05 (10)
N3—C11—C10117.1 (5)O2—Re2—Br498.19 (13)
C12—C11—C10125.0 (6)O1—Re2—Br481.84 (10)
C11—C12—C13119.5 (6)Br7—Re2—Br487.55 (2)
C11—C12—H12120.2O2—Re2—Br597.92 (13)
C13—C12—H12120.3O1—Re2—Br582.07 (10)
C14—C13—C12120.1 (6)Br7—Re2—Br589.73 (2)
C14—C13—H13119.9Br4—Re2—Br5163.89 (2)
C12—C13—H13119.9O2—Re2—Br695.66 (14)
C15—C14—C13119.0 (6)O1—Re2—Br682.77 (10)
C15—C14—H14120.5Br7—Re2—Br6165.81 (2)
C13—C14—H14120.5Br4—Re2—Br690.20 (2)
N3—C15—C14119.5 (6)Br5—Re2—Br688.55 (2)
N3—C15—H15120.3Re2—O1—H1W112.3
C14—C15—H15120.3Re2—O1—H2W124.6
C21—N4—C25123.1 (5)H1W—O1—H2W99.9
C21—N4—H4N118.4Br3i—Re1—Br3180.0
C25—N4—H4N118.4Br3i—Re1—Br289.34 (2)
C26—N5—C30118.1 (5)Br3—Re1—Br290.66 (2)
C35—N6—C31124.4 (5)Br3i—Re1—Br2i90.66 (2)
C35—N6—H6N117.8Br3—Re1—Br2i89.34 (2)
C31—N6—H6N117.8Br2—Re1—Br2i180.0
N4—C21—C22120.9 (6)Br3i—Re1—Br190.53 (2)
N4—C21—H21119.5Br3—Re1—Br189.47 (2)
C22—C21—H21119.6Br2—Re1—Br189.44 (2)
C21—C22—C23118.0 (6)Br2i—Re1—Br190.56 (2)
C21—C22—H22121.0Br3i—Re1—Br1i89.47 (2)
C23—C22—H22121.0Br3—Re1—Br1i90.53 (2)
C24—C23—C22120.3 (6)Br2—Re1—Br1i90.56 (2)
C24—C23—H23119.9Br2i—Re1—Br1i89.44 (2)
C22—C23—H23119.9Br1—Re1—Br1i180.0
C25—C24—C23119.5 (6)H3W—O3A—H4W99.5
C5—N1—C1—C21.3 (9)C25—N4—C21—C221.2 (9)
N1—C1—C2—C30.2 (9)N4—C21—C22—C23−0.8 (9)
C1—C2—C3—C4−2.6 (9)C21—C22—C23—C241.0 (9)
C2—C3—C4—C53.6 (9)C22—C23—C24—C25−1.6 (9)
C1—N1—C5—C4−0.3 (8)C21—N4—C25—C24−1.7 (9)
C1—N1—C5—C6179.8 (5)C21—N4—C25—C26179.4 (6)
C3—C4—C5—N1−2.1 (8)C23—C24—C25—N41.9 (9)
C3—C4—C5—C6177.7 (6)C23—C24—C25—C26−179.3 (6)
C10—N2—C6—C70.4 (8)C30—N5—C26—C27−0.6 (9)
C10—N2—C6—C5−179.2 (5)C30—N5—C26—C25−178.9 (5)
N1—C5—C6—N20.6 (7)N4—C25—C26—N5−10.8 (8)
C4—C5—C6—N2−179.2 (5)C24—C25—C26—N5170.4 (5)
N1—C5—C6—C7−178.9 (5)N4—C25—C26—C27170.9 (5)
C4—C5—C6—C71.2 (9)C24—C25—C26—C27−7.9 (9)
N2—C6—C7—C80.6 (9)N5—C26—C27—C281.8 (9)
C5—C6—C7—C8−179.9 (5)C25—C26—C27—C28180.0 (5)
C6—C7—C8—C9−0.1 (9)C26—C27—C28—C29−2.2 (9)
C7—C8—C9—C10−1.4 (9)C27—C28—C29—C301.5 (9)
C6—N2—C10—C9−1.9 (8)C26—N5—C30—C29−0.2 (9)
C6—N2—C10—C11174.9 (5)C26—N5—C30—C31178.5 (5)
C8—C9—C10—N22.4 (9)C28—C29—C30—N5−0.3 (9)
C8—C9—C10—C11−174.2 (5)C28—C29—C30—C31−178.9 (5)
C15—N3—C11—C121.4 (9)C35—N6—C31—C322.2 (9)
C15—N3—C11—C10−176.9 (5)C35—N6—C31—C30−177.6 (6)
N2—C10—C11—N31.1 (8)N5—C30—C31—N6−2.1 (8)
C9—C10—C11—N3177.9 (5)C29—C30—C31—N6176.7 (5)
N2—C10—C11—C12−177.1 (6)N5—C30—C31—C32178.1 (6)
C9—C10—C11—C12−0.2 (9)C29—C30—C31—C32−3.1 (10)
N3—C11—C12—C13−1.8 (9)N6—C31—C32—C33−2.2 (9)
C10—C11—C12—C13176.3 (5)C30—C31—C32—C33177.7 (6)
C11—C12—C13—C140.8 (9)C31—C32—C33—C340.7 (10)
C12—C13—C14—C150.8 (9)C32—C33—C34—C351.0 (9)
C11—N3—C15—C140.2 (9)C31—N6—C35—C34−0.7 (10)
C13—C14—C15—N3−1.3 (9)C33—C34—C35—N6−1.0 (9)
Symmetry codes: (i) −x, −y+1, −z+1.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···Br8ii0.862.473.228 (6)146
O1—H1W···Br8iii0.892.463.310 (4)157
O1—H2W···O3Aiii0.881.832.710 (5)166
N3—H3N···Br8ii0.852.483.236 (5)147
O3A—H3W···Br5iv0.882.683.517 (4)157
N4—H4N···Br9iv0.862.513.247 (6)143
O3A—H4W···Br90.892.453.338 (4)171
N6—H6N···Br9iv0.852.483.245 (5)147
C9—H9···Br3ii0.932.763.664 (6)162
C15—H15···Br9ii0.922.813.598 (6)142
C22—H22···O3A0.922.583.504 (8)170
C23—H23···Br7v0.922.883.810 (7)172
C29—H29···Br4vi0.932.853.738 (6)158
C35—H35···Br8iv0.922.733.474 (6)137
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x, y−1, z; (iv) −x+1, −y+1, −z; (v) x, y+1, z; (vi) x−1, y, z.
Selected geometric parameters (Å) top
Re1—Br32.5044 (6)Re2—Br72.5108 (7)
Re1—Br22.5099 (6)Re2—Br42.5123 (7)
Re1—Br12.5179 (6)Re2—Br52.5182 (7)
Re2—O21.663 (4)Re2—Br62.5239 (7)
Re2—O12.246 (4)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···Br8i0.862.473.228 (6)146
O1—H1W···Br8ii0.892.463.310 (4)157
O1—H2W···O3Aii0.881.832.710 (5)166
N3—H3N···Br8i0.852.483.236 (5)147
O3A—H3W···Br5iii0.882.683.517 (4)157
N4—H4N···Br9iii0.862.513.247 (6)143
O3A—H4W···Br90.892.453.338 (4)171
N6—H6N···Br9iii0.852.483.245 (5)147
C9—H9···Br3i0.932.763.664 (6)162
C15—H15···Br9i0.922.813.598 (6)142
C22—H22···O3A0.922.583.504 (8)170
C23—H23···Br7iv0.922.883.810 (7)172
C29—H29···Br4v0.932.853.738 (6)158
C35—H35···Br8iii0.922.733.474 (6)137
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y−1, z; (iii) −x+1, −y+1, −z; (iv) x, y+1, z; (v) x−1, y, z.
references
References top

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