Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229616005222/yo3020sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229616005222/yo3020Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229616005222/yo3020sup3.pdf |
CCDC references: 990548; 1470881
Vanadium chemistry has attracted much attention due its biological relevance and medical applications (Crans et al., 2004). In particular, the interactions of high-valent vanadium ions with the S-atom donors of biologically important molecules, such as cysteine and glutathione, might be related to the redox conversion of vanadium in ascidians (Michibata et al., 2003), the function of amavadin (a vanadium-containing anion) isolated from Amanita mushrooms (Garner et al., 2000) and the antidiabetic behaviour of vanadium compounds (Rehder, 2003). To provide a mechanistic understanding for these aspects, the fundamental study of high-valent vanadium sulfur chemistry has been emphasized (Chang et al., 2011; Crans et al., 2010). High-valent vanadium ions are oxophilic and thus reported VIV and VV complexes mostly contain VO3+ and VO2+ units. In comparison, non-oxide high-valent vanadium complexes are relatively scarce (Hsu et al., 2006). The chemistry of non-oxide high-valent vanadium complexes has been of interest and has been investigated in our laboratory. We have utilized a tris(2-sulfanidylphenyl)phosphane ligand system to obtain a class of non-oxide divanadium complexes containing chalcogenide bridges (Wu et al., 2015). In a continuation of this research, a non-oxide divanadium(IV) complex with methanolate bridges has been synthesized and characterized at this work, namely tetraphenylphosphonium tri-µ-methanolato-bis({tris[2-sulfanidyl-3-(trimethylsilyl)phenyl]phosphane}vanadium(IV)) methanol disolvate, (Ph4P)[V2(MeO)3(PS3'')2].2MeOH, (I). To the best of our knowledge, several examples of divanadium(IV) and divanadium(V) complexes with bis(alkoxide) bridges have been reported (Westrup et al., 2011; Scales et al., 2010; Romero-Fernandez et al., 2010; Nishina et al., 2010; Arbaoui et al., 2009; Zhang & Nomura, 2008; Lorber et al., 2008; Homden et al., 2008; Nunes et al., 2005; Preuss, Vogel et al., 2001; Preuss, Fischbeck et al., 2001; Lutz et al., 1999; Castellano et al., 1999; Kempe & Spannenberg, 1997; Devore et al., 1987), but a tris(alkoxide) divanadium core structure is unprecedented in the literature.
All operations were carried out under an N2 atmosphere using standard Schlenk and glove-box techniques. Solvents were dried and distilled under N2 prior to use. The basic synthetic procedure was carried out according to our previous work. The PS3'' ligand, i.e. [P(C6H3-3-Me3Si-2-S)3]3- (Block et al., 1989), and VO(i-PrO)3 (Cornman et al., 1998) were synthesized according to literature methods. Electronic spectra were recorded at the range 300–1100 nm on a Hewlett Packard 8453 spectrophotometer. Elemental analyses were performed at the National Cheng Kung University with an Elemetar vario EL III. The electrospray ionization (ESI) mass spectrum was recorded at the Instrument Development Center of the National Cheng Kung University with a LTQ Orbitrap XL Thermo Fisher spectrometer. The NMR spectrum was recorded on a Bruker AMX400. The magnetization data was recorded on a SQUID magnetometer (Quantum Design MPMS SQUID VSM System) with an external 1 Tesla magnetic field for complex (I) over the temperature range 1.8 to 300 K.
H3PS3'' (0.100 g, 0.174 mmol) and NaOCH3 (0.029 g, 0.537 mmol) were dissolved in methanol. The solution was added to an isopropanol solution of VO(i-PrO)3 (0.043 g, 0.174 mmol). The resulting green solution was layered with (PPh4)Br (0.073 g, 0.174 mmol) in methanol to give a green crystalline solid of (I) after one week [yield 0.044 g, 0.026 mmol, ca 30.0% based on VO(i-PrO)3]. Calculated for C81H101O3P3S6Si6V2: C 57.96, H 6.07, S 11.46%; found: C 57.44, H 5.97, S 11.31%. 1H NMR: δ 7.96, 7.74, 7.50 (PPh4+); 3.32 (µ-OCH3); -0.43, -0.58 [P(C6H3-3-Me3Si-2-S)3]; -18.16, 9.6 [P(C6H3-3-Me3Si-2-S]3. UV–Vis–NIR [CH2Cl2, λmax (ε, M-1 cm-1)]: 598 (5.2 × 103), 846 (3.2 × 103), 997(2.7 × 103). Molecular mass (m/z) calculated: 1337.15; found: 1337.13 [M]-1. (Fig. 1).
Crystal data, data collection and structure refinement details are summarized in Table 1. A green needle-shape crystal of (I) was mounted under liquid-nitrogen vapour on a fine glass fibre with glue. All H atoms are included using the riding model. All other H atoms were placed in ideal positions, with C—H = 0.95 Å for aromatic groups or 0.98 Å for methyl groups, and refined using a riding model, with Uiso(H) = 1.2 or 1.5Ueq(C), respectively. Atoms S3, C9 and C29 are highly distorted and partial occupancies were used for their refinement; the assigned occupancies for S3/S3', C9/C9' and C29/C29' were 0.574 (6):0.426 (6), 0.574 (6):0.426 (6) and 0.5:0.5, respectively.
The anion of (I) consists of dinuclear VIV centres bridging by three methanolate groups (Fig. 2). The crystallographic C2 axis sits on one of bridging the O atoms (O2). Each VIV centre adopts a distorted monocapped trigonal antiprismatic geometry, where three S-atom donors of the PS3'' ligand and three bridging methanolate ligands form two triangular faces. The P atom of the PS3'' ligand is located on top of the triangular face formed by three S atoms. The average twist angle (φ) of two triangular faces is 54.13° (Fig. 3) (trigonal prism = 0°; trigonal antiprism and octahedron = 60°) (Muetterties & Guggenberger, 1974; Karpishin et al., 1993). The S1—V1—O1, S2—V1—O2 and S3—V1—O1 angles (Table 2) are much smaller from those in an ideal octahedron (the axis angle is 180°), but closer to those in a trigonal antiprism (Notni et al., 2009). The bond lengths of compound (I) are very similar to those in previously reported non-oxide divanadium complexes, [V2(µ-E)(µ-η2:η2-E2)(PS3)2]n (E = S or Se, n = 0 or 2-, and PS3 indicates a PS3'' derivative) (Wu et al., 2015). The V···V separation in (I) is 2.899 (2) Å, which is similar to the values seen in [V2(µ-E)(µ-η2:η2-E2)(PS3)2]n complexes (2.90–3.08 Å). The average V—S bond length in (I) is 2.426 Å, which is also close to those of [V2(µ-E)(µ-η2:η2-E2)(PS3)2]n complexes. The three V—OCH3 bond lengths are in the range 1.999 (4)–2.027 (4) Å (Table 2).
Complex (I) is not stable under aerobic conditions. It decomposes immediately in solution under exposure to the air. When dissolved in dichloromethane, the complex produced a green solution. The UV–Vis–NIR spectrum (NIR is near infrared) displays three intense peaks at 598 (ε = 5.2 × 103 M-1 cm-1), 846 (ε = 3.2 × 103 M-1 cm-1) and 997 nm (ε = 2.7 × 103 M-1 cm-1) (see Fig. S1 in the Supporting information). The absorption bands with the high molar extinction coefficients are likely associated with strong ligand-to-metal charge transfer bands (LMCT) that mask d–d transitions. The 1H NMR spectrum of (I) in DMSO-d6 exhibits resonances between 9.5 and -18.16 p.p.m., indicating a paramagnetic character of the divanadium(IV) centres (see Fig. S2 in the Supporting information). The SQUID data for (I) shows the nature of paramagnetism (Fig. 4). The spin-only effective magnetic moment is 2.51 µB at 2 K and 2.80 µB per dimer at 300 K, which are consistent with the spin-only value (2.83 µB) for an S = 1 (triplet) system. The nature of the paramagnetism between two VIV centres is also seen in two non-oxide divanadium(IV) complexes, [(µ-O)2V2{N(SiMe3)2}4] (Duan et al., 1996) and [{(C6F5NCH2CH2)2N(CH2CH2NHC6F5)}V(O)]2 [these seem to contain oxide?] (Rosenberger et al., 1997), that both contain V2O2 cores. The V···V separations for these two V2O2 complexes are 2.612 and 3.100 Å, respectively. A theoretical method is needed to elucidate the magnetic properties resulting from the orbital interaction in (I).
In summary, a non-oxide divanadium(IV) complex supported by a tris[2-sulfanidyl-3-(trimethylsilyl)phenyl]phosphane ligand has been synthesized and structurally characterized. Two VIV centres are bridged by three methanolate groups, forming a [VIV2(µ-OMe)3] core motif that is unprecedented in the literature. Each VIV centre adopts a monocapped trigonal antiprismatic geometry. Interestingly, complex (I) shows a paramagnetic nature and the magnetic data are consistent with an S = 1 system. The details of this chemistry and theoretical work is currently under investigation at our laboratory.
Vanadium chemistry has attracted much attention due its biological relevance and medical applications (Crans et al., 2004). In particular, the interactions of high-valent vanadium ions with the S-atom donors of biologically important molecules, such as cysteine and glutathione, might be related to the redox conversion of vanadium in ascidians (Michibata et al., 2003), the function of amavadin (a vanadium-containing anion) isolated from Amanita mushrooms (Garner et al., 2000) and the antidiabetic behaviour of vanadium compounds (Rehder, 2003). To provide a mechanistic understanding for these aspects, the fundamental study of high-valent vanadium sulfur chemistry has been emphasized (Chang et al., 2011; Crans et al., 2010). High-valent vanadium ions are oxophilic and thus reported VIV and VV complexes mostly contain VO3+ and VO2+ units. In comparison, non-oxide high-valent vanadium complexes are relatively scarce (Hsu et al., 2006). The chemistry of non-oxide high-valent vanadium complexes has been of interest and has been investigated in our laboratory. We have utilized a tris(2-sulfanidylphenyl)phosphane ligand system to obtain a class of non-oxide divanadium complexes containing chalcogenide bridges (Wu et al., 2015). In a continuation of this research, a non-oxide divanadium(IV) complex with methanolate bridges has been synthesized and characterized at this work, namely tetraphenylphosphonium tri-µ-methanolato-bis({tris[2-sulfanidyl-3-(trimethylsilyl)phenyl]phosphane}vanadium(IV)) methanol disolvate, (Ph4P)[V2(MeO)3(PS3'')2].2MeOH, (I). To the best of our knowledge, several examples of divanadium(IV) and divanadium(V) complexes with bis(alkoxide) bridges have been reported (Westrup et al., 2011; Scales et al., 2010; Romero-Fernandez et al., 2010; Nishina et al., 2010; Arbaoui et al., 2009; Zhang & Nomura, 2008; Lorber et al., 2008; Homden et al., 2008; Nunes et al., 2005; Preuss, Vogel et al., 2001; Preuss, Fischbeck et al., 2001; Lutz et al., 1999; Castellano et al., 1999; Kempe & Spannenberg, 1997; Devore et al., 1987), but a tris(alkoxide) divanadium core structure is unprecedented in the literature.
All operations were carried out under an N2 atmosphere using standard Schlenk and glove-box techniques. Solvents were dried and distilled under N2 prior to use. The basic synthetic procedure was carried out according to our previous work. The PS3'' ligand, i.e. [P(C6H3-3-Me3Si-2-S)3]3- (Block et al., 1989), and VO(i-PrO)3 (Cornman et al., 1998) were synthesized according to literature methods. Electronic spectra were recorded at the range 300–1100 nm on a Hewlett Packard 8453 spectrophotometer. Elemental analyses were performed at the National Cheng Kung University with an Elemetar vario EL III. The electrospray ionization (ESI) mass spectrum was recorded at the Instrument Development Center of the National Cheng Kung University with a LTQ Orbitrap XL Thermo Fisher spectrometer. The NMR spectrum was recorded on a Bruker AMX400. The magnetization data was recorded on a SQUID magnetometer (Quantum Design MPMS SQUID VSM System) with an external 1 Tesla magnetic field for complex (I) over the temperature range 1.8 to 300 K.
The anion of (I) consists of dinuclear VIV centres bridging by three methanolate groups (Fig. 2). The crystallographic C2 axis sits on one of bridging the O atoms (O2). Each VIV centre adopts a distorted monocapped trigonal antiprismatic geometry, where three S-atom donors of the PS3'' ligand and three bridging methanolate ligands form two triangular faces. The P atom of the PS3'' ligand is located on top of the triangular face formed by three S atoms. The average twist angle (φ) of two triangular faces is 54.13° (Fig. 3) (trigonal prism = 0°; trigonal antiprism and octahedron = 60°) (Muetterties & Guggenberger, 1974; Karpishin et al., 1993). The S1—V1—O1, S2—V1—O2 and S3—V1—O1 angles (Table 2) are much smaller from those in an ideal octahedron (the axis angle is 180°), but closer to those in a trigonal antiprism (Notni et al., 2009). The bond lengths of compound (I) are very similar to those in previously reported non-oxide divanadium complexes, [V2(µ-E)(µ-η2:η2-E2)(PS3)2]n (E = S or Se, n = 0 or 2-, and PS3 indicates a PS3'' derivative) (Wu et al., 2015). The V···V separation in (I) is 2.899 (2) Å, which is similar to the values seen in [V2(µ-E)(µ-η2:η2-E2)(PS3)2]n complexes (2.90–3.08 Å). The average V—S bond length in (I) is 2.426 Å, which is also close to those of [V2(µ-E)(µ-η2:η2-E2)(PS3)2]n complexes. The three V—OCH3 bond lengths are in the range 1.999 (4)–2.027 (4) Å (Table 2).
Complex (I) is not stable under aerobic conditions. It decomposes immediately in solution under exposure to the air. When dissolved in dichloromethane, the complex produced a green solution. The UV–Vis–NIR spectrum (NIR is near infrared) displays three intense peaks at 598 (ε = 5.2 × 103 M-1 cm-1), 846 (ε = 3.2 × 103 M-1 cm-1) and 997 nm (ε = 2.7 × 103 M-1 cm-1) (see Fig. S1 in the Supporting information). The absorption bands with the high molar extinction coefficients are likely associated with strong ligand-to-metal charge transfer bands (LMCT) that mask d–d transitions. The 1H NMR spectrum of (I) in DMSO-d6 exhibits resonances between 9.5 and -18.16 p.p.m., indicating a paramagnetic character of the divanadium(IV) centres (see Fig. S2 in the Supporting information). The SQUID data for (I) shows the nature of paramagnetism (Fig. 4). The spin-only effective magnetic moment is 2.51 µB at 2 K and 2.80 µB per dimer at 300 K, which are consistent with the spin-only value (2.83 µB) for an S = 1 (triplet) system. The nature of the paramagnetism between two VIV centres is also seen in two non-oxide divanadium(IV) complexes, [(µ-O)2V2{N(SiMe3)2}4] (Duan et al., 1996) and [{(C6F5NCH2CH2)2N(CH2CH2NHC6F5)}V(O)]2 [these seem to contain oxide?] (Rosenberger et al., 1997), that both contain V2O2 cores. The V···V separations for these two V2O2 complexes are 2.612 and 3.100 Å, respectively. A theoretical method is needed to elucidate the magnetic properties resulting from the orbital interaction in (I).
In summary, a non-oxide divanadium(IV) complex supported by a tris[2-sulfanidyl-3-(trimethylsilyl)phenyl]phosphane ligand has been synthesized and structurally characterized. Two VIV centres are bridged by three methanolate groups, forming a [VIV2(µ-OMe)3] core motif that is unprecedented in the literature. Each VIV centre adopts a monocapped trigonal antiprismatic geometry. Interestingly, complex (I) shows a paramagnetic nature and the magnetic data are consistent with an S = 1 system. The details of this chemistry and theoretical work is currently under investigation at our laboratory.
H3PS3'' (0.100 g, 0.174 mmol) and NaOCH3 (0.029 g, 0.537 mmol) were dissolved in methanol. The solution was added to an isopropanol solution of VO(i-PrO)3 (0.043 g, 0.174 mmol). The resulting green solution was layered with (PPh4)Br (0.073 g, 0.174 mmol) in methanol to give a green crystalline solid of (I) after one week [yield 0.044 g, 0.026 mmol, ca 30.0% based on VO(i-PrO)3]. Calculated for C81H101O3P3S6Si6V2: C 57.96, H 6.07, S 11.46%; found: C 57.44, H 5.97, S 11.31%. 1H NMR: δ 7.96, 7.74, 7.50 (PPh4+); 3.32 (µ-OCH3); -0.43, -0.58 [P(C6H3-3-Me3Si-2-S)3]; -18.16, 9.6 [P(C6H3-3-Me3Si-2-S]3. UV–Vis–NIR [CH2Cl2, λmax (ε, M-1 cm-1)]: 598 (5.2 × 103), 846 (3.2 × 103), 997(2.7 × 103). Molecular mass (m/z) calculated: 1337.15; found: 1337.13 [M]-1. (Fig. 1).
Crystal data, data collection and structure refinement details are summarized in Table 1. A green needle-shape crystal of (I) was mounted under liquid-nitrogen vapour on a fine glass fibre with glue. All H atoms are included using the riding model. All other H atoms were placed in ideal positions, with C—H = 0.95 Å for aromatic groups or 0.98 Å for methyl groups, and refined using a riding model, with Uiso(H) = 1.2 or 1.5Ueq(C), respectively. Atoms S3, C9 and C29 are highly distorted and partial occupancies were used for their refinement; the assigned occupancies for S3/S3', C9/C9' and C29/C29' were 0.574 (6):0.426 (6), 0.574 (6):0.426 (6) and 0.5:0.5, respectively.
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
(C24H20P)[V2(CH3O)3(C27H36PS3)2]·2CH4O | F(000) = 3672 |
Mr = 1742.39 | Dx = 1.290 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1430 reflections |
a = 18.4740 (12) Å | θ = 2.2–18.6° |
b = 25.4633 (18) Å | µ = 0.53 mm−1 |
c = 19.3663 (13) Å | T = 150 K |
β = 100.036 (2)° | Needle, dark-green |
V = 8970.7 (11) Å3 | 0.55 × 0.07 × 0.05 mm |
Z = 4 |
BRUKER SMART APEXCCD area detector diffractometer | 7880 independent reflections |
Radiation source: fine-focus sealed tube | 5218 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.100 |
ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | h = −19→21 |
Tmin = 0.760, Tmax = 0.974 | k = −30→30 |
20475 measured reflections | l = −21→23 |
Refinement on F2 | 8 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.088 | H-atom parameters constrained |
wR(F2) = 0.191 | w = 1/[σ2(Fo2) + (0.0653P)2 + 20.3783P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max < 0.001 |
7880 reflections | Δρmax = 0.81 e Å−3 |
494 parameters | Δρmin = −0.47 e Å−3 |
(C24H20P)[V2(CH3O)3(C27H36PS3)2]·2CH4O | V = 8970.7 (11) Å3 |
Mr = 1742.39 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 18.4740 (12) Å | µ = 0.53 mm−1 |
b = 25.4633 (18) Å | T = 150 K |
c = 19.3663 (13) Å | 0.55 × 0.07 × 0.05 mm |
β = 100.036 (2)° |
BRUKER SMART APEXCCD area detector diffractometer | 7880 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | 5218 reflections with I > 2σ(I) |
Tmin = 0.760, Tmax = 0.974 | Rint = 0.100 |
20475 measured reflections |
R[F2 > 2σ(F2)] = 0.088 | 8 restraints |
wR(F2) = 0.191 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0653P)2 + 20.3783P] where P = (Fo2 + 2Fc2)/3 |
7880 reflections | Δρmax = 0.81 e Å−3 |
494 parameters | Δρmin = −0.47 e Å−3 |
Experimental. A green needle-shape crystal of (I) was mounted under liquid-nitrogen vapor on a fine glass fiber with glue. Data were collected at 150 (2) K by a Nonius Kappa diffractometer equipped with a CCD detector. Least-squares refinement of the positional and anisotropic thermal parameters for the contribution of all non-hydrogen atoms and fixed hydrogen atoms was based on F2. A SADABS absorption correction was made. The SHELXTL structural refinement program was employed. All the non-hydrogen atoms were refined with anisotropic displacement factors. |
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) | |
V1 | 0.51582 (6) | 0.28696 (4) | 0.17927 (5) | 0.0268 (3) | |
S1 | 0.41938 (10) | 0.33631 (6) | 0.10672 (9) | 0.0349 (4) | |
S2 | 0.51154 (10) | 0.19719 (6) | 0.13735 (10) | 0.0371 (5) | |
S3 | 0.6450 (3) | 0.3206 (2) | 0.1860 (3) | 0.0303 (9) | 0.547 (5) |
S3' | 0.6224 (4) | 0.3396 (2) | 0.1889 (3) | 0.0303 (9) | 0.453 (5) |
P1 | 0.54546 (8) | 0.28845 (6) | 0.06435 (8) | 0.0209 (4) | |
Si1 | 0.26051 (11) | 0.36565 (8) | −0.01132 (13) | 0.0480 (6) | |
Si2 | 0.58025 (10) | 0.07536 (7) | 0.11356 (11) | 0.0351 (5) | |
Si3 | 0.76105 (11) | 0.42678 (8) | 0.18738 (11) | 0.0422 (5) | |
O1 | 0.4351 (2) | 0.25952 (15) | 0.2283 (2) | 0.0301 (10) | |
O2 | 0.5000 | 0.3411 (2) | 0.2500 | 0.0320 (15) | |
C1 | 0.4076 (3) | 0.3172 (2) | 0.0179 (3) | 0.0262 (14) | |
C2 | 0.4648 (3) | 0.2896 (2) | −0.0030 (3) | 0.0218 (13) | |
C3 | 0.4583 (3) | 0.2679 (2) | −0.0697 (3) | 0.0263 (14) | |
H3 | 0.4977 | 0.2485 | −0.0827 | 0.032* | |
C4 | 0.3933 (3) | 0.2749 (2) | −0.1167 (3) | 0.0300 (15) | |
H4 | 0.3871 | 0.2593 | −0.1619 | 0.036* | |
C5 | 0.3371 (3) | 0.3050 (2) | −0.0971 (3) | 0.0314 (15) | |
H5 | 0.2936 | 0.3107 | −0.1305 | 0.038* | |
C6 | 0.3421 (3) | 0.3271 (2) | −0.0307 (4) | 0.0328 (16) | |
C7 | 0.2129 (5) | 0.3917 (3) | −0.0988 (5) | 0.068 (3) | |
H7A | 0.1763 | 0.4180 | −0.0914 | 0.102* | |
H7B | 0.1884 | 0.3627 | −0.1270 | 0.102* | |
H7C | 0.2492 | 0.4079 | −0.1235 | 0.102* | |
C8 | 0.2847 (4) | 0.4245 (3) | 0.0445 (4) | 0.055 (2) | |
H8A | 0.3037 | 0.4135 | 0.0928 | 0.082* | |
H8B | 0.2408 | 0.4463 | 0.0438 | 0.082* | |
H8C | 0.3224 | 0.4449 | 0.0265 | 0.082* | |
C9 | 0.1923 (17) | 0.3197 (13) | 0.0138 (12) | 0.069 (7) | 0.547 (5) |
H9A | 0.1829 | 0.2914 | −0.0208 | 0.104* | 0.547 (5) |
H9B | 0.1464 | 0.3386 | 0.0155 | 0.104* | 0.547 (5) |
H9C | 0.2113 | 0.3049 | 0.0601 | 0.104* | 0.547 (5) |
C9' | 0.210 (2) | 0.3246 (16) | 0.0476 (16) | 0.069 (7) | 0.453 (5) |
H9'A | 0.2405 | 0.3211 | 0.0940 | 0.104* | 0.453 (5) |
H9'B | 0.1994 | 0.2897 | 0.0268 | 0.104* | 0.453 (5) |
H9'C | 0.1636 | 0.3420 | 0.0521 | 0.104* | 0.453 (5) |
C10 | 0.5769 (3) | 0.1872 (2) | 0.0819 (3) | 0.0243 (14) | |
C11 | 0.5984 (3) | 0.2316 (2) | 0.0483 (3) | 0.0233 (14) | |
C12 | 0.6503 (3) | 0.2287 (2) | 0.0056 (3) | 0.0255 (14) | |
H12 | 0.6641 | 0.2592 | −0.0172 | 0.031* | |
C13 | 0.6821 (3) | 0.1805 (2) | −0.0038 (3) | 0.0283 (15) | |
H13 | 0.7188 | 0.1777 | −0.0325 | 0.034* | |
C14 | 0.6601 (3) | 0.1369 (2) | 0.0288 (3) | 0.0287 (15) | |
H14 | 0.6822 | 0.1042 | 0.0212 | 0.034* | |
C15 | 0.6074 (3) | 0.1377 (2) | 0.0723 (3) | 0.0234 (13) | |
C16 | 0.6377 (4) | 0.0210 (3) | 0.0881 (4) | 0.051 (2) | |
H16A | 0.6894 | 0.0273 | 0.1083 | 0.077* | |
H16B | 0.6321 | 0.0195 | 0.0369 | 0.077* | |
H16C | 0.6219 | −0.0124 | 0.1058 | 0.077* | |
C17 | 0.4823 (4) | 0.0607 (3) | 0.0785 (5) | 0.068 (3) | |
H17A | 0.4780 | 0.0460 | 0.0311 | 0.102* | |
H17B | 0.4534 | 0.0930 | 0.0767 | 0.102* | |
H17C | 0.4638 | 0.0351 | 0.1090 | 0.102* | |
C18 | 0.5958 (5) | 0.0790 (3) | 0.2109 (4) | 0.067 (3) | |
H18A | 0.5714 | 0.0492 | 0.2294 | 0.101* | |
H18B | 0.5754 | 0.1119 | 0.2254 | 0.101* | |
H18C | 0.6486 | 0.0777 | 0.2292 | 0.101* | |
C19 | 0.6456 (3) | 0.3606 (2) | 0.1092 (3) | 0.0289 (15) | |
C20 | 0.5995 (3) | 0.3443 (2) | 0.0483 (3) | 0.0227 (14) | |
C21 | 0.6019 (3) | 0.3680 (2) | −0.0157 (3) | 0.0300 (15) | |
H21 | 0.5708 | 0.3562 | −0.0571 | 0.036* | |
C22 | 0.6508 (3) | 0.4093 (2) | −0.0183 (4) | 0.0315 (16) | |
H22 | 0.6521 | 0.4268 | −0.0613 | 0.038* | |
C23 | 0.6973 (3) | 0.4245 (2) | 0.0420 (4) | 0.0313 (16) | |
H23 | 0.7314 | 0.4519 | 0.0388 | 0.038* | |
C24 | 0.6968 (3) | 0.4018 (2) | 0.1073 (3) | 0.0282 (15) | |
C25 | 0.8353 (5) | 0.4642 (3) | 0.1554 (5) | 0.071 (3) | |
H25A | 0.8765 | 0.4694 | 0.1941 | 0.106* | |
H25B | 0.8163 | 0.4985 | 0.1375 | 0.106* | |
H25C | 0.8522 | 0.4445 | 0.1177 | 0.106* | |
C26 | 0.8076 (5) | 0.3746 (3) | 0.2441 (5) | 0.081 (3) | |
H26A | 0.8287 | 0.3489 | 0.2154 | 0.121* | |
H26B | 0.7720 | 0.3570 | 0.2683 | 0.121* | |
H26C | 0.8469 | 0.3899 | 0.2787 | 0.121* | |
C27 | 0.7078 (5) | 0.4706 (3) | 0.2377 (4) | 0.063 (2) | |
H27A | 0.6694 | 0.4501 | 0.2545 | 0.094* | |
H27B | 0.6851 | 0.4989 | 0.2072 | 0.094* | |
H27C | 0.7409 | 0.4856 | 0.2779 | 0.094* | |
C28 | 0.3697 (4) | 0.2325 (3) | 0.2063 (4) | 0.057 (2) | |
H28A | 0.3765 | 0.1954 | 0.2192 | 0.085* | |
H28B | 0.3556 | 0.2355 | 0.1552 | 0.085* | |
H28C | 0.3309 | 0.2475 | 0.2288 | 0.085* | |
C29 | 0.5217 (9) | 0.3949 (4) | 0.2462 (13) | 0.043 (5) | 0.5 |
H29A | 0.4806 | 0.4178 | 0.2522 | 0.065* | 0.5 |
H29B | 0.5355 | 0.4017 | 0.2004 | 0.065* | 0.5 |
H29C | 0.5637 | 0.4021 | 0.2834 | 0.065* | 0.5 |
P2 | 0.5000 | 0.60856 (8) | 0.2500 | 0.0234 (5) | |
C30 | 0.5154 (3) | 0.5667 (2) | 0.1800 (3) | 0.0263 (14) | |
C31 | 0.4792 (4) | 0.5194 (2) | 0.1685 (3) | 0.0380 (17) | |
H31 | 0.4434 | 0.5102 | 0.1962 | 0.046* | |
C32 | 0.4942 (4) | 0.4850 (3) | 0.1171 (3) | 0.0449 (19) | |
H32 | 0.4698 | 0.4520 | 0.1104 | 0.054* | |
C33 | 0.5448 (4) | 0.4992 (3) | 0.0759 (4) | 0.0436 (18) | |
H33 | 0.5572 | 0.4752 | 0.0422 | 0.052* | |
C34 | 0.5773 (4) | 0.5477 (3) | 0.0833 (4) | 0.0415 (18) | |
H34 | 0.6099 | 0.5579 | 0.0529 | 0.050* | |
C35 | 0.5631 (4) | 0.5820 (2) | 0.1347 (3) | 0.0349 (16) | |
H35 | 0.5856 | 0.6156 | 0.1394 | 0.042* | |
C36 | 0.4190 (3) | 0.6479 (2) | 0.2217 (3) | 0.0236 (13) | |
C37 | 0.3502 (4) | 0.6261 (3) | 0.2203 (4) | 0.0444 (18) | |
H37 | 0.3461 | 0.5909 | 0.2355 | 0.053* | |
C38 | 0.2879 (4) | 0.6545 (3) | 0.1973 (4) | 0.056 (2) | |
H38 | 0.2410 | 0.6394 | 0.1980 | 0.067* | |
C39 | 0.2930 (4) | 0.7040 (3) | 0.1737 (4) | 0.0473 (19) | |
H39 | 0.2496 | 0.7236 | 0.1575 | 0.057* | |
C40 | 0.3610 (4) | 0.7265 (3) | 0.1727 (3) | 0.0407 (18) | |
H40 | 0.3641 | 0.7613 | 0.1558 | 0.049* | |
C41 | 0.4239 (4) | 0.6985 (2) | 0.1962 (3) | 0.0295 (15) | |
H41 | 0.4706 | 0.7137 | 0.1950 | 0.035* | |
O3 | 0.5023 (14) | 0.1534 (10) | 0.8367 (13) | 0.161 (6)* | 0.453 (5) |
C42 | 0.4962 (12) | 0.1871 (8) | 0.7827 (10) | 0.073 (4)* | 0.453 (5) |
O4 | 0.5417 (11) | 0.1588 (8) | 0.8615 (11) | 0.161 (6)* | 0.547 (5) |
C43 | 0.4884 (9) | 0.1293 (7) | 0.8889 (9) | 0.073 (4)* | 0.547 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
V1 | 0.0404 (7) | 0.0204 (5) | 0.0246 (6) | −0.0050 (5) | 0.0197 (5) | −0.0023 (5) |
S1 | 0.0386 (11) | 0.0346 (9) | 0.0354 (10) | 0.0123 (8) | 0.0171 (8) | −0.0029 (8) |
S2 | 0.0518 (12) | 0.0194 (8) | 0.0508 (11) | −0.0047 (7) | 0.0387 (9) | −0.0051 (7) |
S3 | 0.035 (3) | 0.036 (3) | 0.0225 (11) | −0.0083 (17) | 0.0140 (16) | −0.0017 (19) |
S3' | 0.035 (3) | 0.036 (3) | 0.0225 (11) | −0.0083 (17) | 0.0140 (16) | −0.0017 (19) |
P1 | 0.0226 (9) | 0.0207 (8) | 0.0221 (8) | 0.0015 (7) | 0.0112 (6) | 0.0010 (7) |
Si1 | 0.0299 (12) | 0.0359 (11) | 0.0826 (17) | 0.0071 (9) | 0.0225 (11) | 0.0086 (11) |
Si2 | 0.0371 (12) | 0.0203 (9) | 0.0517 (13) | 0.0006 (8) | 0.0181 (9) | −0.0009 (8) |
Si3 | 0.0423 (13) | 0.0401 (11) | 0.0465 (13) | −0.0153 (9) | 0.0145 (10) | −0.0083 (10) |
O1 | 0.034 (3) | 0.028 (2) | 0.034 (3) | −0.003 (2) | 0.021 (2) | −0.0008 (19) |
O2 | 0.054 (4) | 0.018 (3) | 0.027 (3) | 0.000 | 0.015 (3) | 0.000 |
C1 | 0.031 (4) | 0.019 (3) | 0.032 (4) | 0.003 (3) | 0.012 (3) | 0.007 (3) |
C2 | 0.020 (3) | 0.022 (3) | 0.025 (3) | 0.003 (3) | 0.009 (3) | 0.005 (3) |
C3 | 0.035 (4) | 0.024 (3) | 0.022 (3) | −0.002 (3) | 0.014 (3) | 0.001 (3) |
C4 | 0.030 (4) | 0.031 (4) | 0.031 (4) | −0.005 (3) | 0.011 (3) | 0.000 (3) |
C5 | 0.020 (4) | 0.033 (4) | 0.039 (4) | −0.005 (3) | −0.002 (3) | 0.015 (3) |
C6 | 0.028 (4) | 0.026 (3) | 0.047 (4) | −0.002 (3) | 0.014 (3) | 0.007 (3) |
C7 | 0.052 (6) | 0.045 (5) | 0.100 (7) | 0.007 (4) | −0.003 (5) | 0.007 (5) |
C8 | 0.060 (6) | 0.053 (5) | 0.058 (5) | 0.015 (4) | 0.028 (4) | 0.000 (4) |
C9 | 0.050 (13) | 0.064 (8) | 0.106 (18) | 0.006 (8) | 0.051 (14) | 0.020 (14) |
C9' | 0.050 (13) | 0.064 (8) | 0.106 (18) | 0.006 (8) | 0.051 (14) | 0.020 (14) |
C10 | 0.030 (4) | 0.023 (3) | 0.022 (3) | −0.006 (3) | 0.009 (3) | −0.004 (3) |
C11 | 0.023 (4) | 0.022 (3) | 0.026 (3) | 0.005 (2) | 0.006 (3) | 0.000 (3) |
C12 | 0.016 (3) | 0.035 (4) | 0.026 (3) | 0.002 (3) | 0.007 (3) | 0.001 (3) |
C13 | 0.022 (4) | 0.029 (3) | 0.038 (4) | 0.008 (3) | 0.015 (3) | 0.000 (3) |
C14 | 0.021 (4) | 0.029 (3) | 0.037 (4) | 0.000 (3) | 0.009 (3) | −0.009 (3) |
C15 | 0.018 (3) | 0.024 (3) | 0.028 (3) | 0.004 (3) | 0.005 (3) | 0.001 (3) |
C16 | 0.053 (5) | 0.028 (4) | 0.079 (6) | 0.014 (3) | 0.028 (4) | 0.007 (4) |
C17 | 0.042 (5) | 0.036 (4) | 0.130 (9) | −0.010 (4) | 0.026 (5) | −0.006 (5) |
C18 | 0.123 (8) | 0.038 (5) | 0.050 (5) | 0.005 (5) | 0.039 (5) | 0.015 (4) |
C19 | 0.031 (4) | 0.030 (3) | 0.029 (4) | −0.010 (3) | 0.014 (3) | −0.003 (3) |
C20 | 0.020 (3) | 0.022 (3) | 0.030 (4) | −0.001 (2) | 0.015 (3) | 0.000 (3) |
C21 | 0.034 (4) | 0.023 (3) | 0.036 (4) | 0.005 (3) | 0.013 (3) | 0.003 (3) |
C22 | 0.032 (4) | 0.028 (3) | 0.039 (4) | 0.007 (3) | 0.021 (3) | 0.013 (3) |
C23 | 0.033 (4) | 0.018 (3) | 0.050 (4) | 0.000 (3) | 0.026 (3) | 0.001 (3) |
C24 | 0.029 (4) | 0.027 (3) | 0.034 (4) | −0.001 (3) | 0.020 (3) | −0.006 (3) |
C25 | 0.071 (6) | 0.064 (6) | 0.080 (7) | −0.033 (5) | 0.023 (5) | −0.012 (5) |
C26 | 0.047 (6) | 0.078 (7) | 0.104 (8) | −0.010 (5) | −0.024 (5) | 0.002 (6) |
C27 | 0.072 (6) | 0.068 (6) | 0.048 (5) | −0.001 (5) | 0.008 (4) | −0.023 (4) |
C28 | 0.054 (5) | 0.054 (5) | 0.071 (6) | −0.021 (4) | 0.036 (5) | −0.019 (4) |
C29 | 0.066 (17) | 0.011 (5) | 0.058 (10) | −0.002 (6) | 0.023 (12) | −0.008 (7) |
P2 | 0.0311 (14) | 0.0195 (11) | 0.0208 (12) | 0.000 | 0.0074 (10) | 0.000 |
C30 | 0.026 (4) | 0.028 (3) | 0.025 (3) | 0.006 (3) | 0.003 (3) | 0.001 (3) |
C31 | 0.057 (5) | 0.034 (4) | 0.026 (4) | −0.010 (3) | 0.016 (3) | 0.004 (3) |
C32 | 0.072 (6) | 0.031 (4) | 0.029 (4) | −0.004 (4) | 0.003 (4) | −0.006 (3) |
C33 | 0.046 (5) | 0.048 (5) | 0.034 (4) | 0.015 (4) | −0.001 (3) | −0.010 (3) |
C34 | 0.032 (4) | 0.058 (5) | 0.037 (4) | −0.002 (4) | 0.016 (3) | −0.013 (4) |
C35 | 0.036 (4) | 0.029 (4) | 0.043 (4) | 0.002 (3) | 0.018 (3) | 0.001 (3) |
C36 | 0.024 (4) | 0.026 (3) | 0.021 (3) | 0.002 (3) | 0.006 (3) | −0.002 (3) |
C37 | 0.038 (5) | 0.037 (4) | 0.054 (5) | −0.003 (3) | −0.005 (4) | 0.004 (3) |
C38 | 0.025 (4) | 0.070 (6) | 0.068 (6) | −0.002 (4) | −0.004 (4) | 0.006 (5) |
C39 | 0.038 (5) | 0.066 (5) | 0.036 (4) | 0.017 (4) | 0.003 (3) | 0.006 (4) |
C40 | 0.062 (5) | 0.035 (4) | 0.024 (4) | 0.018 (4) | 0.006 (3) | 0.003 (3) |
C41 | 0.034 (4) | 0.034 (4) | 0.025 (3) | 0.007 (3) | 0.018 (3) | 0.003 (3) |
V1—O1i | 1.988 (4) | C2—C3 | 1.391 (8) |
V1—O2 | 2.000 (4) | C3—C4 | 1.386 (9) |
V1—O1 | 2.027 (4) | C4—C5 | 1.396 (8) |
V1—S3' | 2.363 (7) | C5—C6 | 1.392 (9) |
V1—P1 | 2.3831 (17) | C10—C11 | 1.396 (8) |
V1—S1 | 2.420 (2) | C10—C15 | 1.408 (8) |
V1—S2 | 2.4224 (18) | C11—C12 | 1.373 (8) |
V1—S3 | 2.517 (5) | C12—C13 | 1.386 (8) |
V1—V1i | 2.8990 (19) | C13—C14 | 1.374 (8) |
S1—C1 | 1.764 (6) | C14—C15 | 1.394 (8) |
S2—C10 | 1.768 (6) | C19—C20 | 1.392 (8) |
S3—C19 | 1.804 (8) | C19—C24 | 1.417 (8) |
S3'—C19 | 1.756 (8) | C20—C21 | 1.386 (8) |
P1—C20 | 1.795 (6) | C21—C22 | 1.393 (8) |
P1—C2 | 1.802 (6) | C22—C23 | 1.379 (9) |
P1—C11 | 1.804 (6) | C23—C24 | 1.393 (8) |
Si1—C9 | 1.85 (3) | P2—C30 | 1.786 (6) |
Si1—C8 | 1.857 (8) | P2—C30i | 1.786 (6) |
Si1—C7 | 1.888 (9) | P2—C36i | 1.804 (6) |
Si1—C6 | 1.890 (7) | P2—C36 | 1.804 (6) |
Si1—C9' | 1.91 (4) | C30—C31 | 1.377 (8) |
Si2—C17 | 1.857 (8) | C30—C35 | 1.402 (8) |
Si2—C18 | 1.859 (8) | C31—C32 | 1.390 (9) |
Si2—C16 | 1.862 (6) | C32—C33 | 1.379 (10) |
Si2—C15 | 1.883 (6) | C33—C34 | 1.370 (9) |
Si3—C26 | 1.840 (9) | C34—C35 | 1.383 (9) |
Si3—C25 | 1.863 (8) | C36—C37 | 1.383 (9) |
Si3—C27 | 1.870 (7) | C36—C41 | 1.389 (8) |
Si3—C24 | 1.891 (7) | C37—C38 | 1.366 (10) |
O1—C28 | 1.391 (8) | C38—C39 | 1.350 (10) |
O1—V1i | 1.988 (4) | C39—C40 | 1.383 (10) |
O2—C29 | 1.434 (12) | C40—C41 | 1.371 (9) |
O2—V1i | 2.000 (4) | O3—C42 | 1.343 (17) |
C1—C2 | 1.387 (8) | O4—C43 | 1.414 (16) |
C1—C6 | 1.420 (9) | ||
O1i—V1—O2 | 73.95 (14) | C28—O1—V1i | 133.3 (4) |
O1i—V1—O1 | 73.4 (2) | C28—O1—V1 | 134.3 (4) |
O2—V1—O1 | 73.13 (14) | V1i—O1—V1 | 92.45 (18) |
O1i—V1—S3' | 83.4 (2) | C29—O2—V1i | 140.3 (10) |
O2—V1—S3' | 76.96 (16) | C29—O2—V1 | 123.2 (7) |
O1—V1—S3' | 146.12 (19) | V1i—O2—V1 | 92.9 (2) |
O1i—V1—P1 | 134.74 (13) | C2—C1—C6 | 120.1 (6) |
O2—V1—P1 | 135.50 (13) | C2—C1—S1 | 116.9 (5) |
O1—V1—P1 | 138.62 (14) | C6—C1—S1 | 123.0 (5) |
S3'—V1—P1 | 74.96 (15) | C1—C2—C3 | 121.7 (6) |
O1i—V1—S1 | 151.63 (12) | C1—C2—P1 | 111.9 (4) |
O2—V1—S1 | 81.90 (8) | C3—C2—P1 | 126.3 (4) |
O1—V1—S1 | 85.59 (13) | C4—C3—C2 | 118.9 (6) |
S3'—V1—S1 | 105.70 (17) | C3—C4—C5 | 119.5 (6) |
P1—V1—S1 | 73.45 (6) | C6—C5—C4 | 122.7 (6) |
O1i—V1—S2 | 87.33 (13) | C5—C6—C1 | 116.9 (6) |
O2—V1—S2 | 151.60 (12) | C5—C6—Si1 | 117.8 (5) |
O1—V1—S2 | 81.25 (12) | C1—C6—Si1 | 125.2 (5) |
S3'—V1—S2 | 122.66 (15) | C11—C10—C15 | 120.8 (5) |
P1—V1—S2 | 72.63 (6) | C11—C10—S2 | 116.6 (4) |
S1—V1—S2 | 108.53 (8) | C15—C10—S2 | 122.7 (4) |
O1i—V1—S3 | 78.08 (17) | C12—C11—C10 | 121.5 (5) |
O2—V1—S3 | 88.88 (13) | C12—C11—P1 | 127.1 (5) |
O1—V1—S3 | 149.52 (17) | C10—C11—P1 | 111.2 (4) |
P1—V1—S3 | 70.89 (12) | C11—C12—C13 | 118.9 (6) |
S1—V1—S3 | 116.65 (13) | C14—C13—C12 | 119.3 (5) |
S2—V1—S3 | 108.29 (13) | C13—C14—C15 | 124.1 (6) |
O1i—V1—V1i | 44.30 (11) | C14—C15—C10 | 115.5 (5) |
O2—V1—V1i | 43.56 (11) | C14—C15—Si2 | 120.7 (4) |
O1—V1—V1i | 43.25 (12) | C10—C15—Si2 | 123.9 (4) |
S3'—V1—V1i | 103.19 (15) | C20—C19—C24 | 120.8 (6) |
P1—V1—V1i | 178.14 (7) | C20—C19—S3' | 116.6 (5) |
S1—V1—V1i | 107.42 (6) | C24—C19—S3' | 120.9 (5) |
S2—V1—V1i | 108.45 (4) | C20—C19—S3 | 116.1 (5) |
S3—V1—V1i | 107.26 (12) | C24—C19—S3 | 122.6 (5) |
C1—S1—V1 | 112.1 (2) | C21—C20—C19 | 121.2 (5) |
C10—S2—V1 | 110.68 (19) | C21—C20—P1 | 127.2 (5) |
C19—S3—V1 | 107.0 (3) | C19—C20—P1 | 111.5 (4) |
C19—S3'—V1 | 115.5 (4) | C20—C21—C22 | 118.9 (6) |
C20—P1—C2 | 106.1 (3) | C23—C22—C21 | 119.6 (6) |
C20—P1—C11 | 105.7 (3) | C22—C23—C24 | 123.4 (6) |
C2—P1—C11 | 107.1 (3) | C23—C24—C19 | 116.1 (6) |
C20—P1—V1 | 113.5 (2) | C23—C24—Si3 | 120.2 (5) |
C2—P1—V1 | 112.36 (18) | C19—C24—Si3 | 123.7 (5) |
C11—P1—V1 | 111.6 (2) | C30—P2—C30i | 106.7 (4) |
C9—Si1—C8 | 117.6 (9) | C30—P2—C36i | 109.2 (3) |
C9—Si1—C7 | 103.1 (8) | C30i—P2—C36i | 109.5 (3) |
C8—Si1—C7 | 105.5 (4) | C30—P2—C36 | 109.5 (3) |
C9—Si1—C6 | 109.2 (10) | C30i—P2—C36 | 109.2 (3) |
C8—Si1—C6 | 114.5 (3) | C36i—P2—C36 | 112.6 (4) |
C7—Si1—C6 | 105.5 (4) | C31—C30—C35 | 118.9 (6) |
C8—Si1—C9' | 100.8 (11) | C31—C30—P2 | 120.5 (5) |
C7—Si1—C9' | 121.9 (11) | C35—C30—P2 | 120.6 (5) |
C6—Si1—C9' | 109.0 (12) | C30—C31—C32 | 121.0 (6) |
C17—Si2—C18 | 110.5 (4) | C33—C32—C31 | 119.3 (7) |
C17—Si2—C16 | 108.5 (4) | C34—C33—C32 | 120.3 (6) |
C18—Si2—C16 | 108.1 (4) | C33—C34—C35 | 120.7 (6) |
C17—Si2—C15 | 109.2 (3) | C34—C35—C30 | 119.6 (6) |
C18—Si2—C15 | 112.5 (3) | C37—C36—C41 | 118.8 (6) |
C16—Si2—C15 | 107.9 (3) | C37—C36—P2 | 119.6 (5) |
C26—Si3—C25 | 105.9 (4) | C41—C36—P2 | 121.4 (5) |
C26—Si3—C27 | 110.7 (4) | C38—C37—C36 | 120.9 (7) |
C25—Si3—C27 | 110.7 (4) | C39—C38—C37 | 120.0 (7) |
C26—Si3—C24 | 114.0 (3) | C38—C39—C40 | 120.5 (7) |
C25—Si3—C24 | 107.0 (3) | C41—C40—C39 | 120.0 (7) |
C27—Si3—C24 | 108.4 (3) | C40—C41—C36 | 119.8 (6) |
Symmetry code: (i) −x+1, y, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | (C24H20P)[V2(CH3O)3(C27H36PS3)2]·2CH4O |
Mr | 1742.39 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 150 |
a, b, c (Å) | 18.4740 (12), 25.4633 (18), 19.3663 (13) |
β (°) | 100.036 (2) |
V (Å3) | 8970.7 (11) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.53 |
Crystal size (mm) | 0.55 × 0.07 × 0.05 |
Data collection | |
Diffractometer | BRUKER SMART APEXCCD area detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2004) |
Tmin, Tmax | 0.760, 0.974 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 20475, 7880, 5218 |
Rint | 0.100 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.088, 0.191, 1.10 |
No. of reflections | 7880 |
No. of parameters | 494 |
No. of restraints | 8 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0653P)2 + 20.3783P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.81, −0.47 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).