research communications
μ2-acetato-bis[tribromidorhenate(III)] 1,1,2-trichloroethane hemisolvate
of bis(ethylenedithio)tetrathiafulvaleniumaDepartment of Inorganic Chemistry, Ukrainian State University of Chemical Technology, Gagarin Ave. 8, Dnipropetrovsk 49005, Ukraine, bApplied Chemistry Department, V. N. Karazin Kharkiv National University, 4 Svoboda Square, Kharkiv, 61022, Ukraine, cSSI "Institute for Single Crystals" NAS of Ukraine, 60 Nauky Ave., Kharkiv, 61072, Ukraine, dInstitute of Chemistry, Jan Kochanowski University, 25-406 Kielce, Poland, and eInstitute of Molecular Physics, Polish Academy of Sciences, 60-179 Poznan, Poland
*Correspondence e-mail: golichenko_alex@i.ua
The 10H8S8)[Re2Br6(CH3COO)]·0.5C2H3Cl3, contains one bis(ethylenedithio)tetrathiafulvalene (ET) one μ2-acetato-bis[tribromidorhenate(III)] anion and a 1,1,2-trichloroethane molecule with half-occupancy disordered about a twofold rotation axis. The tetrathiafulvalene fragment adopts an almost planar configuration typical of the ET The C atoms of both ethylenedithio fragments in the cation are disordered over two orientations with occupancy factors 0.65:0.35 and 0.77:0.23. In the anion, six Br atoms and a μ2-acetate ligand form a strongly distorted cubic O2Br6 around the Re2 dinuclear centre. In the crystal, centrosymmetrically related ET cations and Re2O2Br6 anions are linked into dimers by π–π stacking interactions [centroid-to-centroid distance = 3.826 (8) Å] and by pairs of additional Re⋯Br contacts [3.131 (3) Å], respectively. The dimers are further packed into a three-dimensional network by non-directional interionic electrostatic forces and by C—H⋯Br and C—H⋯S hydrogen bonds. The disordered 1,1,2-trichloroethane molecules occupy solvent-accessible channels along the b axis.
of the title salt, (CKeywords: crystal structure; radical cation salt; bis(ethylenedithio)tetrathiafulvalene; rhenium; quadruple metal–metal bond.
CCDC reference: 1473493
1. Chemical context
In the past few decades, molecular low-dimensional conducting materials have attracted much interest owing to their physical properties, in particular their electrical, magnetic and spectroscopic properties. The packing of radical cations in the crystal and the properties of et al., 1999; Mori, 1999). Labile equatorial chloride or bromide groups around the Re26+ cluster unit are the reactive centres in interactions with other chemical compounds and biological macromolecules (Shtemenko et al., 2013, 2015). Only one salt containing a rhenium–rhenium quadruple bond has been described so far {(ET)2[Re2Cl8] [ET = bis(ethylenedithio)tetrathiafulvalene]; Reinheimer et al., 2008}. In this context, we present the synthesis and of a new salt of ET with the dirhenium(III) anion [Re2Br6(CH3COO)]−. Neither acetic acid nor acetate was used in the synthesis of this salt. Evidently, the acetate ligand arose by hydrolysis of CH3CN (Cotton et al., 1991). Complex compounds of dirhenium(III) with one equatorial carboxylato ligand are not well studied, the structure of only three such rhenium compounds having been reported to date (Lau et al., 2000; Vega et al., 2002; Beck & Zink, 2011).
salts depend substantially on the type of anions involved (Mori2. Structural commentary
The title compound (Fig. 1) consists of bis(ethylenedithio)tetrathiafulvalene (ET) radical cations, μ2-acetato-bis[tribromidorhenate(III)] anions and 1,1,2-trichloroethane molecules in the stoichiometric molar ratio of 1:1:0.5. The solvent molecule is disordered over two orientations of equal occupancy about a twofold rotation axis intersecting the mid-point of the C—C ethane bond. The tetrathiafulvalene fragment adopts an almost planar configuration (r.m.s. deviation = 0.033 Å) that is typical for ET radical cations. The dihedral angle between the five-membered rings is 0.3 (6)°. The carbon atoms of both ethylenedithio fragments (C4/C5 and C9/C10) are disordered over two sets of sites with occupancy ratios of 0.65:0.35 and 0.77:0.23, respectively.
In the anion, each ReIII atom is coordinated by three Br atoms forming ReBr3 units which are linked by a Re—Re multiple bond [2.2174 (10) Å] and a bridging μ2-acetate ligand, forming a strongly distorted cubic O2Br6 around the Re2 core. The length of the Re—Re bond is very close to the mean value of 2.222 Å for quadruple bonds (Groom et al., 2016), and the six bromine ligands are arranged into an eclipsed conformation. It is also known that the presence of O,O-bridging ligands in such structures has a negligible effect on the Re—Re bond length [it varies in the range 2.2067 (7)–2.2731 (9) Å for compounds with no bridging ligands and in the range 2.2168 (8)–2.2532 (2) Å for compounds with O,O-bridging ligands (Poineau et al., 2015)]. Thus, the structure of the Re2Br6CH3COO− anion corresponds to the typical structure of compounds with quadruple Re—Re bonds in an Re26+ core (Cotton et al., 2005). The Re—Br and Re—O bonds vary in the ranges 2.435 (3)–2.451 (3) Å and 2.009 (15)–2.040 (16) Å, respectively. The distortion from an ideal cubic geometry is mainly due to the short distance between the O atoms of the acetate group [2.24 (2) Å], while the Br⋯Br separations between adjacent Br atoms vary in the range 3.411 (3)–3.553 (4) Å.
3. Supramolecular features
In the crystal (Fig. 2), pairs of centrosymmetrically related ET cations are linked in a `head-to-tail' manner into dimers by π–π stacking interactions, with centroid-to-centroid separations of 3.836 (8) Å, perpendicular interplanar distances of 3.518 (6) Å and offsets of 1.52 (2) Å. Pairs of Re2O2Br6 anions are also linked into dimers by additional pairwise Re⋯Br contacts [Br6⋯Re2 = 3.131 (3) Å]. Cationic and anionic dimers are packed into a three-dimensional network by non-directional intermolecular electrostatic forces and by C—H⋯Br and C—H⋯S hydrogen bonds (Table 1). Solvent-accessible channels along the b axis are occupied by the disordered 1,1,2-trichloroethane molecules.
4. Database survey
A search of the Cambridge Structural Database (Version 5.36; last update February 2015; Groom et al., 2016) for related compounds of bis(ethylenedithio)tetrathiafulvalene with simple Re-containing anions resulted in eight hits, amongst which one closely related structure containing the ET cation and Re2Cl8 anion (Reinheimer et al., 2008). A search for Re2HalxLy anionic moieties, where Hal is a halogen atom and L is the μ2-carboxylic group, resulted in nine hits. Some closely related patterns were found, e.g. one containing the (μ2-acetato)-hexachloridodirhenate anion exhibiting the same structure of the title compound (Vega et al., 2002), and one containing the di-μ2-acetato-bis(dibromidorhenate) anion (Koz'min et al., 1981).
5. Synthesis and crystallization
The synthesis of the −1) in a two-electrode U-shaped glass cell with platinum electrodes. The initial current intensity of 0.1 µA was increased by 0.05 µA per day to a final value of 0.45 µA. A mixture of 1,1,2-trichloroethane/acetonitrile (12:1 v/v) was used as solvent. [(C4H9)4N]2[Re2Br8] (0.008 mol l−1) was used as electrolyte. After a period of 6–7 weeks, black shiny plate-shaped crystals of the title salt suitable for X-ray analysis were formed.
title salt was performed by galvanostatic anodic oxidation of ET (0.002 mol l6. Refinement
Crystal data, data collection and structure . All hydrogen atoms were placed in idealized positions and refined using a riding-model approximation, with C—H = 0.96–0.97 Å, and with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(C) for methyl H atoms. The 1,1,2-trichloroethane molecule is disordered over two sets of sites about a twofold rotation axis with equal occupancy. The C4–C5 and C9–C10 groups of the ET cations are disordered over two orientations with occupancy factors of 0.65/0.35 and 0.77/0.23, respectively. These occupancies were initially obtained as free variables by the full-matrix and were then fixed in the final cycles. The C—C and C—Cl bond lengths in the solvent molecule were constrained to be 1.52 (1) and 1.80 (1) Å, respectively, and the C—Cl bonds of the solvent molecule were restrained to have the same lengths to within 0.01 Å. The C—S and C—C bonds of the disordered fragments of the ET cation were also restrained to have the same lengths to within 0.005 Å. The atoms of each disordered fragment, including the solvent molecule, were restrained to have approximately the same displacement parameters to within 0.02–0.04 Å2. DELU restraints to within 0.01 Å2 were applied to atoms C4B, C5B, C9B, C10B, C1S and Cl2S. In addition, all non-hydrogen atoms of the solvent molecule were restrained to be approximately isotropic to within 0.03–0.06 Å2. Several outlier reflections (67) that were believed to be affected by the contribution of several unresolved minor twin domains were omitted from the final cycles of reducing the R factor from 0.061 to 0.052. Attempts to refine the structure using a two-component twin model were unsuccessful. Moreover, the crystals of the title compound are stable but show a strong tendency to splicing. The poor quality of the available crystal may account for the rather low bond precision of the C—C bonds and the presence of several large residual density peaks.
details are summarized in Table 2
|
Supporting information
CCDC reference: 1473493
10.1107/S2056989016006058/rz5188sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S2056989016006058/rz5188Isup2.hkl
In the past few decades, molecular low-dimensional conducting materials have attracted much interest owing to their physical properties, in particular their electrical, magnetic and spectroscopic properties. The packing of radical cations in the crystal and the properties of
salts depend substantially on the type of anions involved (Mori et al., 1999; Mori, 1999). Labile equatorial chloride or bromide groups around the Re26+ cluster unit are the reactive centres in interactions with other chemical compounds and biological macromolecules (Shtemenko et al., 2013, 2015). Only one salt containing a rhenium–rhenium quadruple bond has been described so far {(ET)2[Re2Cl8] [ET = bis(ethylenedithio)tetrathiafulvalene]; Reinheimer et al., 2008}. In this context, we present the synthesis and of a new salt of ET with the dirhenium(III) anion [Re2Br6(CH3COO)]–. Neither acetic acid nor acetate was used in the synthesis of this salt. Evidently, the acetate ligand arose by hydrolysis of CH3CN (Cotton et al., 1991). Complex compounds of dirhenium(III) with one equatorial carboxylato ligand are not well studied, the structure of only three such rhenium compounds having been reported to date (Lau et al., 2000; Vega et al., 2002; Beck et al., 2011).The title compound (Fig. 1) consists of bis(ethylenedithio)tetrathiafulvalene (ET) radical cations, µ2-acetato-bis[tribromidorhenate(III)] anions and 1,1,2-trichloroethane molecules in the stoichiometric molar ratio of 1:1:0.5. The solvent molecule is disordered over two orientations of equal occupancy about a twofold rotation axis intersecting the mid-point of the C—C ethane bond. The tetrathiafulvalene fragment of the ET cation adopts an almost planar configuration (r.m.s. deviation = 0.033 Å) that is typical for ET radical cations. The dihedral angle formed by the five-membered rings is 0.3 (6)°. The carbon atoms of both ethylenedithio fragments (C4/C5 and C9/C10) are disordered over two sets of sites with occupancy ratios of 0.65:0.35 and 0.77:0.23, respectively.
In the anion, each Re atom is coordinated by three Br atoms forming ReBr3 units which are linked by a Re—Re multiple bond [2.2174 (10) Å] and a µ2-acetate ligand, forming a strongly distorted cubic O2Br6
around the Re2 core. The length of the Re—-Re bond is very close to the mean value of 2.222 Å for quadruple bonds (Groom et al., 2016), and the six bromine ligands are arranged into an eclipsed conformation. It is also known that the presence of O,O-bridging ligands in such structures has a negligible effect on the Re—-Re bond length [it varies in the range 2.2067 (7)–2.2731 (9) Å for compounds with no bridging ligands and in the range 2.2168 (8)–2.2532 (2) Å for compounds with O,O-bridging ligands (Poineau et al. , 2015)]. Thus, the structure of the Re2Br6CH3COO– anion corresponds to the typical structure of compounds with quadruple Re—Re bonds in an Re26+ core (Cotton et al., 2005). The Re—Br and Re—O bonds vary in the ranges 2.435 (3)–2.451 (3) Å and 2.009 (15)–2.040 (16) Å, respectively. The distortion from an ideal cubic geometry is mainly due to the short distance between the O atoms of the acetate group [2.24 (2) Å], while the Br···Br separations between adjacent Br atoms vary in the range 3.411 (3)–3.553 (4) Å.In the crystal (Fig. 2), pairs of centrosymmetrically related ET cations are linked in a `head-to-tail' manner into dimers by π–π stacking interactions, with centroid-to-centroid separations of 3.836 (8) Å, perpendicular interplanar distances of 3.518 (6) Å and offsets of 1.52 (2) Å. Pairs of Re2O2Br6 anions are also linked into dimers by additional pairwise Re···Br contacts [Br6···Re2 = 3.131 (3) Å]. Cationic and anionic dimers are packed into a three-dimensional network by non-directional intermolecular electrostatic forces and by C—H···Br and C—H···S hydrogen bonds (Table 1). Solvent-accessible channels along the b axis are occupied by the disordered 1,1,2-trichloroethane molecules.
A search of the Cambridge Structural Database (Version 5.36; last update February 2015; Groom et al., 2016) for related compounds of bis(ethylenedithio)tetrathiafulvalene with simple Re-containing anions resulted in eight hits, amongst which one closely related structure containing the ET cation and Re2Cl8 anion (Reinheimer et al., 2008). A search for Re2HalxLy anionic moieties, where Hal is a halogen atom and L is the µ2-carboxylic group, resulted in nine hits. Some closely related patterns were found, e.g. one containing the (µ2-acetato)-hexachlorodirhenate anion exhibiting the same structure of the title compound (Vega et al., 2002), and one containing the di-µ2-acetato-bis(dibromidorhenate) anion (Koz'min et al., 1981).
The synthesis of that
title salt was performed by galvanostatic anodic oxidation of ET (0.002 mol l-1) in a two-electrode U-shaped glass cell with platinum electrodes. The initial current intensity of 0.1 µA was increased by 0.05 µA per day to a final value of 0.45 µA. A mixture of 1,1,2-trichloroethane/acetonitrile (12:1 v/v) was used as solvent. [(C4H9)4N]2[Re2Br8] (0.008 mol l-1) was used as electrolyte. After a period of 6–7 weeks, black shiny plate-shaped crystals of the title salt suitable for X-ray analysis were formed.Crystal data, data collection and structure
details are summarized in Table 2. All hydrogen atoms were placed in idealized positions and refined using a riding-model approximation, with C—H = 0.96–0.97 Å, and with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(C) for methyl H atoms. The 1,1,2-trichloroethane molecule is disordered on two sets of sites about a twofold axis with equal occupancy. The C4–C5 and C9–C10 groups of the ET cations are disordered over two orientations with occupancy factors of 0.65/0.35 and 0.77/0.23, respectively. These occupancies were initially obtained as a free variables by the full-matrix and were then fixed in the final cycles. The C—C and C—Cl bond lengths in the solvent molecule were constrained to be 1.52 (1) and 1.80 (1) Å, respectively, and the C—Cl bonds of the solvent molecule were restrained to have the same lengths to within 0.01 Å. The C—S and C—C bonds of the disordered fragments of the ET cation were also restrained to have the same lengths to within 0.005 Å. The atoms of each disordered fragment, including the solvent molecule, were restrained to have approximately the same displacement parameters to within 0.02–0.04 Å2. DELU restraints to within 0.01 Å2 were applied to atoms C4B, C5B, C9B, C10B, C1S and Cl2S. In addition, all non-hydrogen atoms of the solvent molecule were restrained to be approximately isotropic to within 0.03–0.06 Å2. Several outlier reflections (67) that were believed to be affected by the contribution of several unresolved minor twin domains were omitted from the final cycles of reducing the factor from 0.061 to 0.052. Attempts to refine the structure using a two-component twin model were unsuccessful. Moreover, the crystals of title compound are stable but show a strong tendency to splicing. The poor quality of the available crystal may account for the rather low bond precision of the C—C bonds and the presence of several large residual peaks/holes.In the past few decades, molecular low-dimensional conducting materials have attracted much interest owing to their physical properties, in particular their electrical, magnetic and spectroscopic properties. The packing of radical cations in the crystal and the properties of
salts depend substantially on the type of anions involved (Mori et al., 1999; Mori, 1999). Labile equatorial chloride or bromide groups around the Re26+ cluster unit are the reactive centres in interactions with other chemical compounds and biological macromolecules (Shtemenko et al., 2013, 2015). Only one salt containing a rhenium–rhenium quadruple bond has been described so far {(ET)2[Re2Cl8] [ET = bis(ethylenedithio)tetrathiafulvalene]; Reinheimer et al., 2008}. In this context, we present the synthesis and of a new salt of ET with the dirhenium(III) anion [Re2Br6(CH3COO)]–. Neither acetic acid nor acetate was used in the synthesis of this salt. Evidently, the acetate ligand arose by hydrolysis of CH3CN (Cotton et al., 1991). Complex compounds of dirhenium(III) with one equatorial carboxylato ligand are not well studied, the structure of only three such rhenium compounds having been reported to date (Lau et al., 2000; Vega et al., 2002; Beck et al., 2011).The title compound (Fig. 1) consists of bis(ethylenedithio)tetrathiafulvalene (ET) radical cations, µ2-acetato-bis[tribromidorhenate(III)] anions and 1,1,2-trichloroethane molecules in the stoichiometric molar ratio of 1:1:0.5. The solvent molecule is disordered over two orientations of equal occupancy about a twofold rotation axis intersecting the mid-point of the C—C ethane bond. The tetrathiafulvalene fragment of the ET cation adopts an almost planar configuration (r.m.s. deviation = 0.033 Å) that is typical for ET radical cations. The dihedral angle formed by the five-membered rings is 0.3 (6)°. The carbon atoms of both ethylenedithio fragments (C4/C5 and C9/C10) are disordered over two sets of sites with occupancy ratios of 0.65:0.35 and 0.77:0.23, respectively.
In the anion, each Re atom is coordinated by three Br atoms forming ReBr3 units which are linked by a Re—Re multiple bond [2.2174 (10) Å] and a µ2-acetate ligand, forming a strongly distorted cubic O2Br6
around the Re2 core. The length of the Re—-Re bond is very close to the mean value of 2.222 Å for quadruple bonds (Groom et al., 2016), and the six bromine ligands are arranged into an eclipsed conformation. It is also known that the presence of O,O-bridging ligands in such structures has a negligible effect on the Re—-Re bond length [it varies in the range 2.2067 (7)–2.2731 (9) Å for compounds with no bridging ligands and in the range 2.2168 (8)–2.2532 (2) Å for compounds with O,O-bridging ligands (Poineau et al. , 2015)]. Thus, the structure of the Re2Br6CH3COO– anion corresponds to the typical structure of compounds with quadruple Re—Re bonds in an Re26+ core (Cotton et al., 2005). The Re—Br and Re—O bonds vary in the ranges 2.435 (3)–2.451 (3) Å and 2.009 (15)–2.040 (16) Å, respectively. The distortion from an ideal cubic geometry is mainly due to the short distance between the O atoms of the acetate group [2.24 (2) Å], while the Br···Br separations between adjacent Br atoms vary in the range 3.411 (3)–3.553 (4) Å.In the crystal (Fig. 2), pairs of centrosymmetrically related ET cations are linked in a `head-to-tail' manner into dimers by π–π stacking interactions, with centroid-to-centroid separations of 3.836 (8) Å, perpendicular interplanar distances of 3.518 (6) Å and offsets of 1.52 (2) Å. Pairs of Re2O2Br6 anions are also linked into dimers by additional pairwise Re···Br contacts [Br6···Re2 = 3.131 (3) Å]. Cationic and anionic dimers are packed into a three-dimensional network by non-directional intermolecular electrostatic forces and by C—H···Br and C—H···S hydrogen bonds (Table 1). Solvent-accessible channels along the b axis are occupied by the disordered 1,1,2-trichloroethane molecules.
A search of the Cambridge Structural Database (Version 5.36; last update February 2015; Groom et al., 2016) for related compounds of bis(ethylenedithio)tetrathiafulvalene with simple Re-containing anions resulted in eight hits, amongst which one closely related structure containing the ET cation and Re2Cl8 anion (Reinheimer et al., 2008). A search for Re2HalxLy anionic moieties, where Hal is a halogen atom and L is the µ2-carboxylic group, resulted in nine hits. Some closely related patterns were found, e.g. one containing the (µ2-acetato)-hexachlorodirhenate anion exhibiting the same structure of the title compound (Vega et al., 2002), and one containing the di-µ2-acetato-bis(dibromidorhenate) anion (Koz'min et al., 1981).
The synthesis of that
title salt was performed by galvanostatic anodic oxidation of ET (0.002 mol l-1) in a two-electrode U-shaped glass cell with platinum electrodes. The initial current intensity of 0.1 µA was increased by 0.05 µA per day to a final value of 0.45 µA. A mixture of 1,1,2-trichloroethane/acetonitrile (12:1 v/v) was used as solvent. [(C4H9)4N]2[Re2Br8] (0.008 mol l-1) was used as electrolyte. After a period of 6–7 weeks, black shiny plate-shaped crystals of the title salt suitable for X-ray analysis were formed. detailsCrystal data, data collection and structure
details are summarized in Table 2. All hydrogen atoms were placed in idealized positions and refined using a riding-model approximation, with C—H = 0.96–0.97 Å, and with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(C) for methyl H atoms. The 1,1,2-trichloroethane molecule is disordered on two sets of sites about a twofold axis with equal occupancy. The C4–C5 and C9–C10 groups of the ET cations are disordered over two orientations with occupancy factors of 0.65/0.35 and 0.77/0.23, respectively. These occupancies were initially obtained as a free variables by the full-matrix and were then fixed in the final cycles. The C—C and C—Cl bond lengths in the solvent molecule were constrained to be 1.52 (1) and 1.80 (1) Å, respectively, and the C—Cl bonds of the solvent molecule were restrained to have the same lengths to within 0.01 Å. The C—S and C—C bonds of the disordered fragments of the ET cation were also restrained to have the same lengths to within 0.005 Å. The atoms of each disordered fragment, including the solvent molecule, were restrained to have approximately the same displacement parameters to within 0.02–0.04 Å2. DELU restraints to within 0.01 Å2 were applied to atoms C4B, C5B, C9B, C10B, C1S and Cl2S. In addition, all non-hydrogen atoms of the solvent molecule were restrained to be approximately isotropic to within 0.03–0.06 Å2. Several outlier reflections (67) that were believed to be affected by the contribution of several unresolved minor twin domains were omitted from the final cycles of reducing the factor from 0.061 to 0.052. Attempts to refine the structure using a two-component twin model were unsuccessful. Moreover, the crystals of title compound are stable but show a strong tendency to splicing. The poor quality of the available crystal may account for the rather low bond precision of the C—C bonds and the presence of several large residual peaks/holes.Data collection: CrysAlis PRO (Agilent, 2014); cell
CrysAlis PRO (Agilent, 2014); data reduction: CrysAlis PRO (Agilent, 2014); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).Fig. 1. The asymmetric unit of the title compound, with displacement ellipsoids drawn at the 50% probability level. [Symmetry code: (i) -1/2 - x, y, -z.] Only one component of the disordered 1,1,2-trichloroethane molecule and the major component of the ET cation are shown. Colour codes: C, grey; H, white; O, red; S, yellow; Cl, green; Br, brown, Re, violet. | |
Fig. 2. Partial crystal packing of the title compound, with displacement ellipsoids shown at the 50% probability level. Only one component of the disordered 1,1,2-trichloroethane molecules and the major component of the ET molecule are shown. Colour codes: C, grey, H, white, O, red, S, yellow, Cl, green, Br, brown, Re, violet. |
(C10H8S8)[Re2Br6(C2H3O2)]·0.5C2H3Cl3 | F(000) = 4960 |
Mr = 1362.24 | Dx = 3.046 Mg m−3 |
Monoclinic, I2/a | Mo Kα radiation, λ = 0.71073 Å |
a = 27.1825 (5) Å | Cell parameters from 18811 reflections |
b = 8.53737 (13) Å | θ = 2.9–30.7° |
c = 26.0667 (5) Å | µ = 16.93 mm−1 |
β = 100.8440 (17)° | T = 298 K |
V = 5941.21 (18) Å3 | Block, metallic dark violet |
Z = 8 | 0.4 × 0.4 × 0.1 mm |
Agilent Xcalibur Sapphire3 diffractometer | 6755 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 6304 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: 16.1827 pixels mm-1 | θmax = 27.5°, θmin = 2.9° |
ω scans | h = −35→35 |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2014) | k = −11→9 |
Tmin = 0.067, Tmax = 1.000 | l = −33→33 |
36051 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.052 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0534P)2 + 229.8497P] where P = (Fo2 + 2Fc2)/3 |
6755 reflections | (Δ/σ)max = 0.001 |
334 parameters | Δρmax = 1.77 e Å−3 |
99 restraints | Δρmin = −1.90 e Å−3 |
(C10H8S8)[Re2Br6(C2H3O2)]·0.5C2H3Cl3 | V = 5941.21 (18) Å3 |
Mr = 1362.24 | Z = 8 |
Monoclinic, I2/a | Mo Kα radiation |
a = 27.1825 (5) Å | µ = 16.93 mm−1 |
b = 8.53737 (13) Å | T = 298 K |
c = 26.0667 (5) Å | 0.4 × 0.4 × 0.1 mm |
β = 100.8440 (17)° |
Agilent Xcalibur Sapphire3 diffractometer | 6755 independent reflections |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2014) | 6304 reflections with I > 2σ(I) |
Tmin = 0.067, Tmax = 1.000 | Rint = 0.039 |
36051 measured reflections |
R[F2 > 2σ(F2)] = 0.052 | 99 restraints |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0534P)2 + 229.8497P] where P = (Fo2 + 2Fc2)/3 |
6755 reflections | Δρmax = 1.77 e Å−3 |
334 parameters | Δρmin = −1.90 e Å−3 |
Experimental. Absorption correction: CrysAlisPro (Agilent, 2014) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
S1 | 0.0279 (2) | −0.3844 (7) | 0.1248 (2) | 0.0486 (13) | |
S2 | −0.0188 (2) | −0.1562 (6) | 0.0484 (2) | 0.0411 (11) | |
S3 | −0.0801 (3) | −0.0100 (7) | 0.1157 (3) | 0.0532 (14) | |
S4 | −0.0284 (3) | −0.2886 (8) | 0.2057 (2) | 0.0602 (17) | |
S5 | 0.0889 (2) | −0.5248 (8) | 0.0393 (2) | 0.0484 (13) | |
S6 | 0.0408 (2) | −0.2918 (6) | −0.0354 (2) | 0.0436 (12) | |
S7 | 0.0915 (3) | −0.3875 (7) | −0.1204 (2) | 0.0586 (17) | |
S8 | 0.1502 (3) | −0.6653 (9) | −0.0297 (2) | 0.0590 (16) | |
C1 | 0.0209 (7) | −0.313 (2) | 0.0627 (7) | 0.034 (4) | |
C2 | −0.0374 (7) | −0.152 (2) | 0.1079 (8) | 0.037 (4) | |
C3 | −0.0160 (8) | −0.262 (3) | 0.1431 (8) | 0.043 (5) | |
C4 | −0.065 (3) | −0.122 (6) | 0.220 (3) | 0.064 (11) | 0.35 |
H4A | −0.1001 | −0.1537 | 0.2165 | 0.077* | 0.35 |
H4B | −0.0538 | −0.0909 | 0.2563 | 0.077* | 0.35 |
C4A | −0.0391 (15) | −0.084 (3) | 0.2196 (15) | 0.056 (8) | 0.65 |
H4AA | −0.0440 | −0.0750 | 0.2554 | 0.067* | 0.65 |
H4AB | −0.0094 | −0.0242 | 0.2166 | 0.067* | 0.65 |
C5A | −0.0822 (16) | −0.015 (5) | 0.1850 (9) | 0.060 (9) | 0.65 |
H5AA | −0.0864 | 0.0909 | 0.1965 | 0.072* | 0.65 |
H5AB | −0.1118 | −0.0737 | 0.1893 | 0.072* | 0.65 |
C5B | −0.062 (3) | 0.011 (9) | 0.1862 (9) | 0.061 (12) | 0.35 |
H5BA | −0.0272 | 0.0463 | 0.1933 | 0.073* | 0.35 |
H5BB | −0.0817 | 0.0950 | 0.1967 | 0.073* | 0.35 |
C6 | 0.0472 (7) | −0.372 (2) | 0.0258 (7) | 0.035 (4) | |
C7 | 0.1061 (8) | −0.523 (2) | −0.0214 (8) | 0.039 (4) | |
C8 | 0.0834 (9) | −0.415 (2) | −0.0558 (8) | 0.044 (5) | |
C9A | 0.1534 (9) | −0.479 (4) | −0.1154 (13) | 0.057 (8) | 0.77 |
H9AA | 0.1634 | −0.4736 | −0.1492 | 0.068* | 0.77 |
H9AB | 0.1777 | −0.4205 | −0.0908 | 0.068* | 0.77 |
C9B | 0.134 (4) | −0.548 (10) | −0.130 (4) | 0.05 (2) | 0.23 |
H9BA | 0.1153 | −0.6449 | −0.1362 | 0.060* | 0.23 |
H9BB | 0.1493 | −0.5262 | −0.1596 | 0.060* | 0.23 |
C10A | 0.1547 (13) | −0.643 (4) | −0.0988 (9) | 0.051 (7) | 0.77 |
H10A | 0.1857 | −0.6902 | −0.1045 | 0.061* | 0.77 |
H10B | 0.1272 | −0.6987 | −0.1202 | 0.061* | 0.77 |
C10B | 0.173 (4) | −0.566 (13) | −0.083 (3) | 0.05 (2) | 0.23 |
H10C | 0.1860 | −0.4639 | −0.0715 | 0.059* | 0.23 |
H10D | 0.2006 | −0.6266 | −0.0923 | 0.059* | 0.23 |
Re1 | 0.12639 (3) | 0.02771 (9) | 0.15999 (3) | 0.0325 (2) | |
Re2 | 0.18894 (3) | 0.19389 (8) | 0.18533 (3) | 0.0285 (2) | |
Br1 | 0.05027 (9) | 0.1855 (3) | 0.15459 (12) | 0.0621 (7) | |
Br2 | 0.10600 (9) | −0.1027 (3) | 0.23712 (10) | 0.0541 (6) | |
Br3 | 0.11180 (11) | 0.0172 (4) | 0.06499 (10) | 0.0623 (7) | |
Br4 | 0.20677 (9) | 0.2898 (3) | 0.10198 (9) | 0.0529 (6) | |
Br5 | 0.15056 (10) | 0.4496 (3) | 0.19753 (11) | 0.0560 (6) | |
Br6 | 0.20369 (9) | 0.1635 (3) | 0.28134 (8) | 0.0476 (5) | |
O1 | 0.2381 (6) | 0.0139 (18) | 0.1841 (6) | 0.047 (3) | |
O2 | 0.1742 (6) | −0.1510 (17) | 0.1587 (6) | 0.046 (3) | |
C11 | 0.2221 (8) | −0.129 (2) | 0.1733 (7) | 0.039 (4) | |
C12 | 0.2582 (11) | −0.260 (3) | 0.1768 (12) | 0.066 (7) | |
H12A | 0.2756 | −0.2551 | 0.1480 | 0.100* | |
H12B | 0.2404 | −0.3578 | 0.1756 | 0.100* | |
H12C | 0.2819 | −0.2533 | 0.2090 | 0.100* | |
Cl1S | −0.1993 (6) | 0.0569 (19) | 0.0673 (6) | 0.150 (6) | |
Cl2S | −0.2811 (11) | 0.288 (3) | 0.0317 (11) | 0.140 (10) | 0.50 |
C1S | −0.2592 (9) | 0.090 (4) | 0.0257 (5) | 0.15 (2) | |
H1S | −0.2848 | 0.0099 | 0.0239 | 0.180* | |
H1SA | −0.2718 | 0.1918 | 0.0336 | 0.180* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
S1 | 0.052 (3) | 0.062 (3) | 0.035 (2) | 0.022 (3) | 0.013 (2) | 0.012 (2) |
S2 | 0.053 (3) | 0.036 (2) | 0.037 (2) | 0.010 (2) | 0.016 (2) | 0.008 (2) |
S3 | 0.064 (4) | 0.044 (3) | 0.055 (3) | 0.018 (3) | 0.022 (3) | 0.001 (2) |
S4 | 0.080 (4) | 0.065 (4) | 0.043 (3) | 0.015 (3) | 0.032 (3) | 0.013 (3) |
S5 | 0.049 (3) | 0.065 (4) | 0.034 (2) | 0.018 (3) | 0.014 (2) | 0.010 (2) |
S6 | 0.062 (3) | 0.036 (2) | 0.036 (2) | 0.009 (2) | 0.017 (2) | 0.0036 (19) |
S7 | 0.102 (5) | 0.041 (3) | 0.040 (3) | 0.018 (3) | 0.032 (3) | 0.006 (2) |
S8 | 0.064 (4) | 0.075 (4) | 0.042 (3) | 0.028 (3) | 0.020 (3) | 0.008 (3) |
C1 | 0.033 (9) | 0.043 (10) | 0.028 (8) | 0.000 (8) | 0.008 (7) | 0.002 (7) |
C2 | 0.040 (10) | 0.038 (10) | 0.036 (9) | −0.002 (8) | 0.015 (8) | 0.000 (8) |
C3 | 0.049 (11) | 0.050 (12) | 0.033 (9) | 0.010 (9) | 0.015 (8) | 0.007 (9) |
C4 | 0.071 (17) | 0.065 (16) | 0.061 (15) | 0.002 (14) | 0.025 (14) | −0.003 (12) |
C4A | 0.070 (18) | 0.053 (15) | 0.057 (15) | 0.000 (14) | 0.040 (14) | −0.015 (13) |
C5A | 0.074 (19) | 0.059 (17) | 0.058 (15) | 0.008 (16) | 0.043 (14) | −0.007 (14) |
C5B | 0.066 (18) | 0.061 (16) | 0.060 (16) | 0.000 (14) | 0.023 (13) | −0.004 (12) |
C6 | 0.039 (10) | 0.039 (10) | 0.030 (8) | −0.002 (8) | 0.011 (7) | 0.002 (7) |
C7 | 0.042 (10) | 0.045 (11) | 0.031 (9) | 0.004 (8) | 0.012 (8) | −0.004 (8) |
C8 | 0.067 (14) | 0.036 (10) | 0.030 (9) | −0.010 (10) | 0.014 (9) | −0.007 (8) |
C9A | 0.07 (2) | 0.061 (19) | 0.050 (17) | −0.023 (17) | 0.030 (16) | −0.004 (15) |
C9B | 0.05 (2) | 0.05 (3) | 0.05 (2) | 0.000 (17) | 0.013 (15) | 0.001 (17) |
C10A | 0.058 (18) | 0.050 (17) | 0.050 (16) | 0.014 (15) | 0.025 (14) | 0.003 (14) |
C10B | 0.05 (2) | 0.05 (3) | 0.05 (2) | 0.000 (17) | 0.013 (15) | −0.001 (17) |
Re1 | 0.0300 (4) | 0.0326 (4) | 0.0333 (4) | −0.0033 (3) | 0.0025 (3) | 0.0011 (3) |
Re2 | 0.0294 (4) | 0.0276 (3) | 0.0275 (3) | −0.0007 (2) | 0.0027 (3) | 0.0040 (2) |
Br1 | 0.0443 (12) | 0.0641 (15) | 0.0752 (17) | 0.0068 (11) | 0.0042 (11) | 0.0085 (13) |
Br2 | 0.0564 (13) | 0.0555 (13) | 0.0517 (12) | −0.0093 (10) | 0.0140 (10) | 0.0070 (10) |
Br3 | 0.0602 (15) | 0.0809 (18) | 0.0408 (11) | −0.0144 (13) | −0.0036 (10) | −0.0037 (11) |
Br4 | 0.0481 (12) | 0.0703 (15) | 0.0389 (11) | −0.0074 (11) | 0.0047 (9) | 0.0135 (10) |
Br5 | 0.0561 (13) | 0.0389 (11) | 0.0737 (16) | 0.0048 (10) | 0.0142 (12) | 0.0065 (11) |
Br6 | 0.0513 (12) | 0.0517 (12) | 0.0388 (10) | −0.0108 (10) | 0.0056 (9) | 0.0051 (9) |
O1 | 0.050 (9) | 0.041 (8) | 0.048 (8) | 0.002 (7) | 0.005 (7) | 0.004 (7) |
O2 | 0.056 (9) | 0.034 (7) | 0.048 (8) | −0.001 (6) | 0.009 (7) | −0.004 (6) |
C11 | 0.056 (12) | 0.033 (9) | 0.031 (9) | 0.005 (9) | 0.014 (8) | −0.001 (8) |
C12 | 0.074 (18) | 0.048 (14) | 0.085 (19) | 0.023 (13) | 0.034 (15) | 0.014 (13) |
Cl1S | 0.133 (11) | 0.148 (12) | 0.153 (12) | 0.021 (9) | −0.014 (9) | −0.014 (10) |
Cl2S | 0.15 (2) | 0.115 (17) | 0.14 (2) | 0.048 (16) | −0.024 (17) | 0.005 (15) |
C1S | 0.15 (4) | 0.12 (2) | 0.19 (4) | 0.02 (3) | 0.05 (3) | −0.01 (3) |
S1—C1 | 1.708 (19) | C7—C8 | 1.35 (3) |
S1—C3 | 1.72 (2) | C9A—H9AA | 0.9700 |
S2—C1 | 1.71 (2) | C9A—H9AB | 0.9700 |
S2—C2 | 1.72 (2) | C9A—C10A | 1.46 (5) |
S3—C2 | 1.72 (2) | C9B—H9BA | 0.9700 |
S3—C5A | 1.82 (2) | C9B—H9BB | 0.9700 |
S3—C5B | 1.82 (2) | C9B—C10B | 1.46 (14) |
S4—C3 | 1.74 (2) | C10A—H10A | 0.9700 |
S4—C4 | 1.82 (2) | C10A—H10B | 0.9700 |
S4—C4A | 1.82 (2) | C10B—H10C | 0.9700 |
S5—C6 | 1.72 (2) | C10B—H10D | 0.9700 |
S5—C7 | 1.73 (2) | Re1—Re2 | 2.2174 (10) |
S6—C6 | 1.716 (19) | Re1—Br1 | 2.451 (3) |
S6—C8 | 1.72 (2) | Re1—Br2 | 2.451 (2) |
S7—C8 | 1.75 (2) | Re1—Br3 | 2.435 (3) |
S7—C9A | 1.84 (2) | Re1—O2 | 2.009 (15) |
S7—C9B | 1.84 (2) | Re2—Br4 | 2.454 (2) |
S8—C7 | 1.75 (2) | Re2—Br5 | 2.465 (2) |
S8—C10A | 1.84 (2) | Re2—Br6 | 2.473 (2) |
S8—C10B | 1.84 (2) | Re2—O1 | 2.040 (16) |
C1—C6 | 1.40 (3) | O1—C11 | 1.30 (3) |
C2—C3 | 1.36 (3) | O2—C11 | 1.30 (3) |
C4—H4A | 0.9700 | C11—C12 | 1.48 (3) |
C4—H4B | 0.9700 | C12—H12A | 0.9600 |
C4—C5B | 1.46 (4) | C12—H12B | 0.9600 |
C4A—H4AA | 0.9700 | C12—H12C | 0.9600 |
C4A—H4AB | 0.9700 | Cl1S—C1S | 1.800 (16) |
C4A—C5A | 1.46 (4) | Cl2S—C1S | 1.81 (2) |
C5A—H5AA | 0.9700 | Cl2S—H1SA | 0.8557 |
C5A—H5AB | 0.9700 | C1S—C1Si | 1.515 (18) |
C5B—H5BA | 0.9700 | C1S—H1S | 0.9700 |
C5B—H5BB | 0.9700 | C1S—H1SA | 0.9703 |
C1—S1—C3 | 94.9 (10) | C10A—C9A—H9AA | 108.9 |
C1—S2—C2 | 95.6 (9) | C10A—C9A—H9AB | 108.9 |
C2—S3—C5A | 104.3 (14) | S7—C9B—H9BA | 109.6 |
C2—S3—C5B | 97 (3) | S7—C9B—H9BB | 109.6 |
C5A—S3—C5B | 19 (3) | H9BA—C9B—H9BB | 108.1 |
C3—S4—C4 | 108 (2) | C10B—C9B—S7 | 110 (7) |
C3—S4—C4A | 97.4 (15) | C10B—C9B—H9BA | 109.6 |
C4A—S4—C4 | 25 (3) | C10B—C9B—H9BB | 109.6 |
C6—S5—C7 | 94.9 (9) | S8—C10A—H10A | 109.0 |
C6—S6—C8 | 94.9 (10) | S8—C10A—H10B | 109.0 |
C8—S7—C9A | 98.9 (13) | C9A—C10A—S8 | 113 (2) |
C8—S7—C9B | 103 (3) | C9A—C10A—H10A | 109.0 |
C9A—S7—C9B | 26 (4) | C9A—C10A—H10B | 109.0 |
C7—S8—C10A | 102.8 (12) | H10A—C10A—H10B | 107.8 |
C7—S8—C10B | 96 (4) | S8—C10B—H10C | 109.1 |
C10B—S8—C10A | 28 (4) | S8—C10B—H10D | 109.1 |
S1—C1—S2 | 116.1 (11) | C9B—C10B—S8 | 112 (7) |
C6—C1—S1 | 122.7 (15) | C9B—C10B—H10C | 109.1 |
C6—C1—S2 | 121.1 (15) | C9B—C10B—H10D | 109.1 |
S3—C2—S2 | 116.0 (12) | H10C—C10B—H10D | 107.9 |
C3—C2—S2 | 115.7 (15) | Re2—Re1—Br1 | 104.91 (8) |
C3—C2—S3 | 128.3 (16) | Re2—Re1—Br2 | 108.99 (7) |
S1—C3—S4 | 116.6 (12) | Re2—Re1—Br3 | 107.19 (7) |
C2—C3—S1 | 117.5 (15) | Br1—Re1—Br2 | 88.73 (10) |
C2—C3—S4 | 125.9 (17) | Br3—Re1—Br1 | 89.29 (11) |
S4—C4—H4A | 109.2 | Br3—Re1—Br2 | 143.01 (9) |
S4—C4—H4B | 109.2 | O2—Re1—Re2 | 91.6 (4) |
H4A—C4—H4B | 107.9 | O2—Re1—Br1 | 163.4 (4) |
C5B—C4—S4 | 112 (5) | O2—Re1—Br2 | 85.2 (5) |
C5B—C4—H4A | 109.2 | O2—Re1—Br3 | 86.4 (4) |
C5B—C4—H4B | 109.2 | Re1—Re2—Br4 | 102.59 (6) |
S4—C4A—H4AA | 108.8 | Re1—Re2—Br5 | 106.59 (7) |
S4—C4A—H4AB | 108.8 | Re1—Re2—Br6 | 101.74 (6) |
H4AA—C4A—H4AB | 107.7 | Br4—Re2—Br5 | 88.72 (9) |
C5A—C4A—S4 | 114 (3) | Br4—Re2—Br6 | 155.47 (8) |
C5A—C4A—H4AA | 108.8 | Br5—Re2—Br6 | 87.39 (9) |
C5A—C4A—H4AB | 108.8 | O1—Re2—Re1 | 88.9 (4) |
S3—C5A—H5AA | 108.1 | O1—Re2—Br4 | 89.9 (5) |
S3—C5A—H5AB | 108.1 | O1—Re2—Br5 | 164.3 (4) |
C4A—C5A—S3 | 117 (2) | O1—Re2—Br6 | 87.4 (5) |
C4A—C5A—H5AA | 108.1 | C11—O1—Re2 | 120.9 (14) |
C4A—C5A—H5AB | 108.1 | C11—O2—Re1 | 119.9 (13) |
H5AA—C5A—H5AB | 107.3 | O1—C11—C12 | 120 (2) |
S3—C5B—H5BA | 107.3 | O2—C11—O1 | 118.4 (18) |
S3—C5B—H5BB | 107.3 | O2—C11—C12 | 121 (2) |
C4—C5B—S3 | 120 (5) | C11—C12—H12A | 109.5 |
C4—C5B—H5BA | 107.3 | C11—C12—H12B | 109.5 |
C4—C5B—H5BB | 107.3 | C11—C12—H12C | 109.5 |
H5BA—C5B—H5BB | 106.9 | H12A—C12—H12B | 109.5 |
S6—C6—S5 | 116.3 (11) | H12A—C12—H12C | 109.5 |
C1—C6—S5 | 122.5 (15) | H12B—C12—H12C | 109.5 |
C1—C6—S6 | 121.2 (15) | C1S—Cl2S—H1SA | 8.9 |
S5—C7—S8 | 114.5 (12) | Cl1S—C1S—Cl2S | 112 (2) |
C8—C7—S5 | 116.4 (16) | Cl1S—C1S—H1S | 118.6 |
C8—C7—S8 | 129.0 (16) | Cl1S—C1S—H1SA | 109.2 |
S6—C8—S7 | 115.3 (13) | Cl2S—C1S—H1S | 114.7 |
C7—C8—S6 | 117.5 (16) | Cl2S—C1S—H1SA | 7.8 |
C7—C8—S7 | 127.2 (18) | C1Si—C1S—Cl1S | 97 (2) |
S7—C9A—H9AA | 108.9 | C1Si—C1S—Cl2S | 104.2 (12) |
S7—C9A—H9AB | 108.9 | C1Si—C1S—H1S | 108.0 |
H9AA—C9A—H9AB | 107.7 | C1Si—C1S—H1SA | 112.0 |
C10A—C9A—S7 | 114 (2) | H1S—C1S—H1SA | 111.3 |
S1—C1—C6—S5 | 0 (3) | C7—S8—C10A—C9A | 40 (3) |
S1—C1—C6—S6 | −177.4 (11) | C7—S8—C10B—C9B | −63 (7) |
S2—C1—C6—S5 | 177.7 (11) | C8—S6—C6—S5 | 0.2 (14) |
S2—C1—C6—S6 | 0 (2) | C8—S6—C6—C1 | 178.1 (17) |
S2—C2—C3—S1 | 2 (3) | C8—S7—C9A—C10A | 58 (3) |
S2—C2—C3—S4 | −178.8 (14) | C8—S7—C9B—C10B | −42 (7) |
S3—C2—C3—S1 | −177.1 (13) | C9A—S7—C8—S6 | 158.8 (15) |
S3—C2—C3—S4 | 2 (3) | C9A—S7—C8—C7 | −22 (2) |
S4—C4—C5B—S3 | 58 (9) | C9A—S7—C9B—C10B | 42 (6) |
S4—C4A—C5A—S3 | −61 (4) | C9B—S7—C8—S6 | −175 (4) |
S5—C7—C8—S6 | 1 (2) | C9B—S7—C8—C7 | 4 (4) |
S5—C7—C8—S7 | −178.2 (13) | C9B—S7—C9A—C10A | −43 (8) |
S7—C9A—C10A—S8 | −71 (3) | C10A—S8—C7—S5 | 174.5 (16) |
S7—C9B—C10B—S8 | 77 (9) | C10A—S8—C7—C8 | −4 (3) |
S8—C7—C8—S6 | 179.3 (13) | C10A—S8—C10B—C9B | 43 (6) |
S8—C7—C8—S7 | 0 (3) | C10B—S8—C7—S5 | −158 (4) |
C1—S1—C3—S4 | 176.8 (14) | C10B—S8—C7—C8 | 23 (4) |
C1—S1—C3—C2 | −4 (2) | C10B—S8—C10A—C9A | −40 (8) |
C1—S2—C2—S3 | −179.7 (12) | Re1—Re2—O1—C11 | −3.2 (15) |
C1—S2—C2—C3 | 0.9 (19) | Re1—O2—C11—O1 | −6 (2) |
C2—S2—C1—S1 | −3.7 (13) | Re1—O2—C11—C12 | 175.2 (17) |
C2—S2—C1—C6 | 178.7 (17) | Re2—Re1—O2—C11 | 3.0 (15) |
C2—S3—C5A—C4A | 22 (4) | Re2—O1—C11—O2 | 6 (3) |
C2—S3—C5B—C4 | −61 (7) | Re2—O1—C11—C12 | −175.0 (17) |
C3—S1—C1—S2 | 4.6 (14) | Br1—Re1—Re2—Br4 | −90.90 (10) |
C3—S1—C1—C6 | −177.8 (18) | Br1—Re1—Re2—Br5 | 1.54 (11) |
C3—S4—C4—C5B | −19 (7) | Br1—Re1—Re2—Br6 | 92.30 (10) |
C3—S4—C4A—C5A | 63 (3) | Br1—Re1—Re2—O1 | 179.4 (5) |
C4—S4—C3—S1 | 168 (3) | Br1—Re1—O2—C11 | −174.7 (11) |
C4—S4—C3—C2 | −11 (4) | Br2—Re1—Re2—Br4 | 175.23 (10) |
C4—S4—C4A—C5A | −54 (6) | Br2—Re1—Re2—Br5 | −92.32 (10) |
C4A—S4—C3—S1 | 144.9 (18) | Br2—Re1—Re2—Br6 | −1.56 (10) |
C4A—S4—C3—C2 | −34 (3) | Br2—Re1—Re2—O1 | 85.6 (5) |
C4A—S4—C4—C5B | 50 (4) | Br2—Re1—O2—C11 | −105.9 (15) |
C5A—S3—C2—S2 | −169.7 (19) | Br3—Re1—Re2—Br4 | 3.05 (11) |
C5A—S3—C2—C3 | 10 (3) | Br3—Re1—Re2—Br5 | 95.49 (11) |
C5A—S3—C5B—C4 | 53 (6) | Br3—Re1—Re2—Br6 | −173.75 (10) |
C5B—S3—C2—S2 | −152 (3) | Br3—Re1—Re2—O1 | −86.6 (5) |
C5B—S3—C2—C3 | 28 (3) | Br3—Re1—O2—C11 | 110.1 (15) |
C5B—S3—C5A—C4A | −48 (8) | Br4—Re2—O1—C11 | −105.8 (15) |
C6—S5—C7—S8 | −179.3 (12) | Br5—Re2—O1—C11 | 169.2 (11) |
C6—S5—C7—C8 | −0.5 (19) | Br6—Re2—O1—C11 | 98.6 (15) |
C6—S6—C8—S7 | 178.5 (13) | O2—Re1—Re2—Br4 | 89.8 (5) |
C6—S6—C8—C7 | −0.6 (19) | O2—Re1—Re2—Br5 | −177.8 (5) |
C7—S5—C6—S6 | 0.1 (14) | O2—Re1—Re2—Br6 | −87.0 (5) |
C7—S5—C6—C1 | −177.7 (18) | O2—Re1—Re2—O1 | 0.1 (6) |
Symmetry code: (i) −x−1/2, y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C5B—H5BA···Br1 | 0.98 | 2.77 | 3.63 (8) | 147 |
C9A—H9AA···Br6ii | 0.97 | 2.80 | 3.60 (3) | 140 |
C9B—H9BA···S4iii | 0.97 | 2.75 | 3.46 (10) | 130 |
C9B—H9BB···Br6ii | 0.96 | 2.61 | 3.40 (11) | 140 |
C10A—H10A···Br4iv | 0.97 | 2.92 | 3.83 (4) | 156 |
C10A—H10B···S3iii | 0.97 | 2.81 | 3.57 (3) | 136 |
C10B—H10D···Br4iv | 0.98 | 2.67 | 3.61 (11) | 161 |
Symmetry codes: (ii) x, −y−1/2, z−1/2; (iii) −x, −y−1, −z; (iv) −x+1/2, y−1, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C5B—H5BA···Br1 | 0.98 | 2.77 | 3.63 (8) | 147 |
C9A—H9AA···Br6i | 0.97 | 2.80 | 3.60 (3) | 140 |
C9B—H9BA···S4ii | 0.97 | 2.75 | 3.46 (10) | 130 |
C9B—H9BB···Br6i | 0.96 | 2.61 | 3.40 (11) | 140 |
C10A—H10A···Br4iii | 0.97 | 2.92 | 3.83 (4) | 156 |
C10A—H10B···S3ii | 0.97 | 2.81 | 3.57 (3) | 136 |
C10B—H10D···Br4iii | 0.98 | 2.67 | 3.61 (11) | 161 |
Symmetry codes: (i) x, −y−1/2, z−1/2; (ii) −x, −y−1, −z; (iii) −x+1/2, y−1, −z. |
Experimental details
Crystal data | |
Chemical formula | (C10H8S8)[Re2Br6(C2H3O2)]·0.5C2H3Cl3 |
Mr | 1362.24 |
Crystal system, space group | Monoclinic, I2/a |
Temperature (K) | 298 |
a, b, c (Å) | 27.1825 (5), 8.53737 (13), 26.0667 (5) |
β (°) | 100.8440 (17) |
V (Å3) | 5941.21 (18) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 16.93 |
Crystal size (mm) | 0.4 × 0.4 × 0.1 |
Data collection | |
Diffractometer | Agilent Xcalibur Sapphire3 |
Absorption correction | Multi-scan (CrysAlis PRO; Agilent, 2014) |
Tmin, Tmax | 0.067, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 36051, 6755, 6304 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.052, 0.137, 1.14 |
No. of reflections | 6755 |
No. of parameters | 334 |
No. of restraints | 99 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0534P)2 + 229.8497P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.77, −1.90 |
Computer programs: CrysAlis PRO (Agilent, 2014), SHELXS97 (Sheldrick, 2008), SHELXL2014 (Sheldrick, 2015), OLEX2 (Dolomanov et al., 2009).
Acknowledgements
This work was supported by a grant for Science Research (No. 0111U000111) from the Ministry of Education and Science of Ukraine. We also thank COST Action CM1105 for supporting this study.
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