Literature DB >> 26396864

Crystal structure of octa-μ3-selenido-(p-toluene-sulfonato-κO)penta-kis-(tri-ethyl-phosphane-κP)-octa-hedro-hexa-rhenium(III) p-toluene-sulfonate di-chloro-methane disolvate.

Julia A Edwards1, Robert McDonald2, Lisa F Szczepura1.   

Abstract

The title compound, [Re6Se8{O3SC6H4(CH3)}{P(C2H5)3}5](CH3C6H4SO3)·2CH2Cl2, contains the face-capped hexa-nuclear [Re6(μ3-Se)8](2+) cluster core. The [Re6Se8](2+) cluster core displays a non-crystallographic center of symmetry and is bonded through the Re(III) atoms to five n class="Chemical">tri-ethyl-phosphane ligands and one p-toluene-sulfonate ligand. One p-toluene-sulfonate counter-ion and two di-chloro-methane solvent mol-ecules are also present in the asymmetric unit. One of the ethyl chains of one triethylphos-phane ligand and one of the CH2Cl2 solvent molecules are disordered over two sets of sites (occupancy ratios 0.65:0.35 and 0.5:0.5, respectively). The Re-O(sulfon-ate) bond length of 2.123 (5) Å is similar to other Re-O bond lengths of hexa-nuclear rhenium chalcogenide clusters containing other O-donor ligands such as dimethyl sulfoxide (DMSO), di-methyl-formamide (DMF) and hydroxide.

Entities:  

Keywords:  [Re6(μ3-Se)8]2+ cluster core; crystal structure; rhenium complex; tosyl­ate

Year:  2015        PMID: 26396864      PMCID: PMC4555408          DOI: 10.1107/S2056989015014334

Source DB:  PubMed          Journal:  Acta Crystallogr E Crystallogr Commun


Related literature

Lindner & Grimmer (1971 ▸) reported the insertion of sulfur trioxide into the Re-alkyl bond of (p-tol­yl)n class="Chemical">Re(CO)5 to generate the first example of a rhenium complex to contain a tosyl­ate moiety. Later, Eremenko et al. (1993 ▸) determined the structure of [Re(P(OiPr)3)2(CO)(NO)(OTs)2] (OTs− = p-toluene­sulfonate anion) which represented the first structural report of a rhenium complex containing tosyl­ate ligands. In the synthesis of octa­hedral rhenium chalcogenide cluster complexes, the substitution of either halide or nitrile ligands has proven an effective means for generating a variety of new cluster complexes (Zheng & Holm, 1997 ▸; Knott et al., 2013 ▸; Yoshimura et al., 2000 ▸). Nitrile ligands are often considered weakly coordinating and substitution of alkyl and aryl nitrile ligands has often been used in single metal chemistry (Endres, 1987 ▸) and in the preparation of [Re6 Q 8]2+ (Q = S or Se) cluster complexes (Zheng & Holm, 1997 ▸; Durham et al., 2012 ▸). However, there have been reports of the hexa­nuclear rhenium selenide cluster core, [Re6Se8]2+, activating nitriles to undergo reactions other than substitution (Orto et al., 2007 ▸; Szczepura et al., 2007 ▸). While structural reports of rhenium chalcogenide clusters containing other oxygen donor ligands have been previously reported (Dorson et al., 2009 ▸; Mironov et al., 2011 ▸; Zheng & Holm, 1997 ▸; Zheng et al., 1999 ▸), this report represents the first example of tosyl­ate coordination to a [Re6 Q 8]2+ cluster core. The average Re—P bond length of the five terminal PEt3 ligands in the title compound [2.479 Å] is similar to that in other rhenium selenide clusters containing PEt3 ligands (Durham et al., 2012 ▸, 2015 ▸; Knott et al., 2013 ▸; Zheng & Holm, 1997 ▸; Zheng et al., 1999 ▸).

Experimental

Crystal data

[Re6Se8(C7H7O3S)(C6H15P)5](C7H7O3S)·2CH2Cl2 M = 2851.85 Triclinic, a = 11.7432 (10) Å b = 16.6878 (14) Å c = 18.9786 (16) Å α = 93.4729 (11)° β = 95.9862 (12)° γ = 100.0851 (11)° V = 3629.9 (5) Å3 Z = 2 Mo Kα radiation μ = 14.33 mm−1 T = 193 K 0.48 × 0.28 × 0.10 mm

Data collection

Bruker PLATFORM/SMART 1000 CCD area-detector diffractometer Absorption correction: integration (SADABS; Sheldrick, 2008 ▸) T min = 0.032, T max = 0.255 31748 measured reflections 16405 independent reflections 11401 reflections with I > 2σ(I) R int = 0.031

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.097 S = 1.02 16405 reflections 693 parameters H-atom parameters constrained Δρmax = 2.67 e Å−3 Δρmin = −1.26 e Å−3

Data collection: SMART (Bruker, 2006 ▸); cell refinement: SAINT (Bruker, 2006 ▸); data reduction: SAIn class="Chemical">NT; program(s) used to solve structure: DIRDIF99 (Beurskens et al., 2008 ▸); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015 ▸); molecular graphics: SHELXTL (Sheldrick, 2008 ▸); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) I, isu0804. DOI: 10.1107/S2056989015014334/pj2021sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989015014334/pj2021Isup2.hkl Click here for additional data file. 6 8 3 5 3 6 4 + . DOI: 10.1107/S2056989015014334/pj2021fig1.tif Perspective view of the [Re6Se8(PEt3)5(n class="Chemical">O3SC6H4Me)]+ ion showing the atom labelling scheme. Non-hydrogen atoms are represented by Gaussian ellipsoids at the 30% probability level. Hydrogen atoms omitted for clarity. CCDC reference: 1010097 Additional supporting information: crystallographic information; 3D view; checkCIF report
[Re6Se8(C7H7O3S)(C6H15P)5](C7H7O3S)·2CH2Cl2Z = 2
Mr = 2851.85F(000) = 2628
Triclinic, P1Dx = 2.609 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.7432 (10) ÅCell parameters from 7041 reflections
b = 16.6878 (14) Åθ = 2.2–27.4°
c = 18.9786 (16) ŵ = 14.33 mm1
α = 93.4729 (11)°T = 193 K
β = 95.9862 (12)°Prism, orange
γ = 100.0851 (11)°0.48 × 0.28 × 0.10 mm
V = 3629.9 (5) Å3
Bruker PLATFORM/SMART 1000 CCD area-detector diffractometer11401 reflections with I > 2σ(I)
Detector resolution: 8.192 pixels mm-1Rint = 0.031
ω scansθmax = 27.5°, θmin = 1.7°
Absorption correction: integration (SADABS; Sheldrick, 2008)h = −15→15
Tmin = 0.032, Tmax = 0.255k = −21→21
31748 measured reflectionsl = −24→24
16405 independent reflections
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.097w = 1/[σ2(Fo2) + (0.038P)2 + 7.5887P] where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
16405 reflectionsΔρmax = 2.67 e Å3
693 parametersΔρmin = −1.26 e Å3
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.
xyzUiso*/UeqOcc. (<1)
Re10.12366 (2)0.35432 (2)0.22926 (2)0.02007 (6)
Re20.16617 (2)0.29786 (2)0.10389 (2)0.02159 (7)
Re30.13895 (2)0.19879 (2)0.20606 (2)0.02062 (7)
Re40.30352 (2)0.29772 (2)0.29017 (2)0.02004 (6)
Re50.33294 (2)0.39696 (2)0.18802 (2)0.02136 (7)
Re60.34623 (2)0.24274 (2)0.16411 (2)0.02221 (7)
Se1−0.02863 (6)0.25580 (4)0.14801 (3)0.02465 (15)
Se20.10186 (6)0.25694 (4)0.32525 (3)0.02334 (14)
Se30.28647 (6)0.44606 (4)0.30833 (3)0.02378 (14)
Se40.15816 (6)0.44579 (4)0.12967 (4)0.02754 (16)
Se50.18447 (6)0.15003 (4)0.08552 (3)0.02631 (15)
Se60.31453 (6)0.14981 (4)0.26240 (4)0.02578 (15)
Se70.49890 (6)0.33842 (4)0.24662 (4)0.02539 (15)
Se80.36656 (6)0.34011 (4)0.06760 (4)0.02695 (15)
S10.58942 (18)0.19272 (12)0.10790 (11)0.0404 (5)
P1−0.02451 (16)0.42936 (10)0.27116 (10)0.0267 (4)
P20.06449 (18)0.29468 (11)−0.01759 (9)0.0289 (4)
P30.01218 (17)0.06768 (10)0.22232 (10)0.0277 (4)
P40.39486 (17)0.29590 (11)0.41376 (9)0.0266 (4)
P50.47147 (19)0.52475 (11)0.17694 (10)0.0357 (5)
O10.4663 (4)0.1748 (3)0.1248 (3)0.0323 (11)
O20.6306 (5)0.2788 (3)0.1027 (3)0.0562 (17)
O30.6607 (5)0.1522 (4)0.1537 (3)0.0618 (18)
C10.5763 (8)0.1441 (5)0.0219 (5)0.046 (2)
C20.6345 (11)0.0810 (7)0.0078 (6)0.083 (4)
H20.68050.06250.04560.100*
C30.6272 (11)0.0436 (7)−0.0609 (6)0.077 (3)
H30.66940.0011−0.06970.092*
C40.5604 (10)0.0679 (6)−0.1147 (6)0.064 (3)
C50.4992 (13)0.1288 (8)−0.1005 (6)0.108 (5)
H50.45000.1456−0.13750.130*
C60.5091 (13)0.1662 (9)−0.0313 (6)0.122 (6)
H60.46670.2085−0.02240.146*
C70.5535 (11)0.0278 (7)−0.1896 (6)0.083 (4)
H7A0.62870.0130−0.19700.100*
H7B0.53440.0662−0.22420.100*
H7C0.4929−0.0214−0.19580.100*
C11−0.0042 (7)0.4563 (4)0.3667 (4)0.0351 (17)
H11A−0.00400.40560.39100.042*
H11B0.07370.49100.37910.042*
C12−0.0937 (8)0.5010 (5)0.3965 (4)0.046 (2)
H12A−0.07470.51150.44820.055*
H12B−0.17150.46720.38570.055*
H12C−0.09250.55300.37490.055*
C13−0.1760 (7)0.3747 (4)0.2540 (4)0.0373 (18)
H13A−0.22800.41150.26930.045*
H13B−0.19590.36100.20220.045*
C14−0.1991 (7)0.2963 (4)0.2920 (4)0.0391 (18)
H14A−0.28250.27320.28450.047*
H14B−0.17420.30860.34300.047*
H14C−0.15520.25680.27290.047*
C15−0.0325 (7)0.5260 (4)0.2323 (4)0.0377 (18)
H15A−0.04610.51530.18000.045*
H15B−0.10080.54650.24780.045*
C160.0724 (8)0.5918 (4)0.2507 (4)0.045 (2)
H16A0.05680.64250.23160.053*
H16B0.13880.57550.23010.053*
H16C0.09050.60040.30250.053*
C21−0.0445 (7)0.2022 (5)−0.0443 (4)0.0394 (19)
H21A−0.00430.1548−0.04310.047*
H21B−0.09990.1961−0.00820.047*
C22−0.1147 (8)0.1979 (5)−0.1174 (4)0.049 (2)
H22A−0.16850.1454−0.12610.059*
H22B−0.06160.2030−0.15400.059*
H22C−0.15900.2425−0.11880.059*
C230.1580 (7)0.3016 (5)−0.0883 (4)0.0392 (19)
H23A0.11030.3071−0.13330.047*
H23B0.21760.3520−0.07800.047*
C240.2195 (8)0.2302 (5)−0.0994 (4)0.046 (2)
H24A0.26750.2394−0.13840.055*
H24B0.16170.1800−0.11110.055*
H24C0.26930.2250−0.05570.055*
C25−0.0151 (7)0.3782 (5)−0.0342 (4)0.0410 (19)
H25A0.04080.4305−0.02520.049*
H25B−0.04660.3727−0.08500.049*
C26−0.1155 (8)0.3824 (5)0.0105 (5)0.053 (2)
H26A−0.15150.4293−0.00130.064*
H26B−0.08560.38840.06110.064*
H26C−0.17370.33210.00040.064*
C31−0.0210 (8)−0.0054 (4)0.1442 (4)0.042 (2)
H31A0.0532−0.01230.12630.051*
H31B−0.0572−0.05880.15920.051*
C32−0.0993 (9)0.0163 (5)0.0844 (4)0.058 (3)
H32A−0.1149−0.02810.04640.069*
H32B−0.06180.06660.06600.069*
H32C−0.17280.02440.10130.069*
C33−0.1291 (7)0.0800 (5)0.2480 (4)0.0395 (19)
H33A−0.11650.11330.29410.047*
H33B−0.16650.11100.21230.047*
C34−0.2127 (8)0.0017 (5)0.2552 (5)0.055 (2)
H34A−0.28610.01470.26870.066*
H34B−0.1784−0.02880.29180.066*
H34C−0.2277−0.03150.20970.066*
C350.0707 (7)0.0060 (4)0.2885 (4)0.0348 (17)
H35A0.0161−0.04670.28650.042*
H35B0.1452−0.00600.27450.042*
C360.0925 (8)0.0420 (5)0.3650 (4)0.046 (2)
H36A0.12280.00310.39530.055*
H36B0.01930.05310.38050.055*
H36C0.14940.09300.36870.055*
C410.5134 (7)0.3820 (5)0.4418 (4)0.0407 (19)
H41A0.57390.38080.40930.049*
H41B0.48270.43300.43570.049*
C420.5712 (8)0.3856 (5)0.5176 (4)0.050 (2)
H42A0.63050.43530.52750.060*
H42B0.60800.33770.52360.060*
H42C0.51240.38610.55060.060*
C430.4584 (7)0.2066 (4)0.4322 (4)0.0375 (19)
H43A0.48220.20900.48400.045*
H43B0.39720.15750.41970.045*
C440.5638 (8)0.1958 (5)0.3935 (5)0.049 (2)
H44A0.59450.14830.40980.059*
H44B0.62440.24480.40390.059*
H44C0.53990.18740.34220.059*
C450.2999 (7)0.2951 (5)0.4839 (4)0.0393 (19)
H45A0.23590.24730.47330.047*
H45B0.34510.28740.52920.047*
C460.2465 (8)0.3717 (5)0.4943 (4)0.045 (2)
H46A0.19570.36500.53220.054*
H46B0.20080.37990.45000.054*
H46C0.30870.41920.50750.054*
C510.6216 (9)0.5128 (6)0.1577 (5)0.064 (3)
H51A0.67370.56650.16910.076*
H51B0.64950.47470.19070.076*
C520.6356 (9)0.4832 (6)0.0850 (5)0.070 (3)
H52A0.71870.48720.08020.085*
H52B0.60110.51650.05090.085*
H52C0.59640.42610.07560.085*
C530.5125 (10)0.5942 (5)0.2573 (5)0.068 (3)
H53A0.55580.64660.24440.081*
H53B0.44060.60540.27580.081*
C540.5877 (9)0.5626 (6)0.3171 (5)0.067 (3)
H54A0.60220.60210.35880.080*
H54B0.66200.55560.30080.080*
H54C0.54660.51010.32970.080*
C550.4257 (12)0.5886 (6)0.1134 (6)0.089 (4)
H55A0.49620.61850.09580.107*0.65
H55B0.38030.55300.07270.107*0.65
H55C0.42700.55780.06730.107*0.35
H55D0.34220.58640.11870.107*0.35
C56A0.3580 (17)0.6468 (11)0.1335 (10)0.085 (5)*0.65
H56A0.33890.67720.09260.102*0.65
H56B0.40240.68480.17210.102*0.65
H56C0.28590.61870.14950.102*0.65
C56B0.466 (3)0.672 (2)0.1006 (19)0.094 (11)*0.35
H56D0.41930.68590.05910.112*0.35
H56E0.54810.67850.09150.112*0.35
H56F0.45980.70740.14230.112*0.35
S20.1203 (2)0.25430 (12)0.69762 (10)0.0397 (5)
O40.2051 (6)0.3129 (3)0.7426 (3)0.0593 (18)
O50.0437 (5)0.2020 (3)0.7371 (3)0.0578 (17)
O60.0570 (8)0.2922 (4)0.6441 (4)0.085 (3)
C610.1949 (7)0.1916 (4)0.6514 (4)0.0346 (17)
C620.1339 (8)0.1340 (5)0.5971 (4)0.0409 (19)
H620.05270.13100.58470.049*
C630.1924 (9)0.0821 (5)0.5618 (5)0.053 (2)
H630.14980.04320.52570.064*
C640.3105 (9)0.0847 (5)0.5772 (5)0.050 (2)
C650.3699 (8)0.1410 (5)0.6309 (5)0.055 (2)
H650.45110.14380.64320.066*
C660.3122 (8)0.1937 (5)0.6671 (5)0.046 (2)
H660.35510.23210.70350.055*
C670.3712 (11)0.0272 (5)0.5381 (6)0.081 (4)
H67A0.34210.02230.48740.097*
H67B0.3559−0.02660.55690.097*
H67C0.45520.04830.54430.097*
Cl1S0.1511 (3)0.67463 (18)0.49345 (15)0.0790 (8)
Cl2S0.1300 (3)0.8404 (2)0.53900 (19)0.0944 (10)
C1S0.0595 (10)0.7443 (7)0.5080 (6)0.079 (3)
H1SA0.01090.74780.46290.094*
H1SB0.00650.72310.54270.094*
Cl3S0.2826 (7)0.8779 (5)0.3829 (4)0.105 (3)*0.5
Cl4S0.3255 (6)0.7327 (4)0.3274 (3)0.0828 (17)*0.5
Cl5S0.3045 (6)0.9045 (4)0.3569 (4)0.0836 (19)*0.5
Cl6S0.3205 (7)0.7571 (5)0.2778 (4)0.109 (2)*0.5
C2S0.2295 (12)0.8018 (8)0.3232 (8)0.109 (5)
H2SA0.22210.82180.27520.131*0.5
H2SB0.15150.77490.33320.131*0.5
H2SC0.20690.76940.36320.131*0.5
H2SD0.15800.80480.29160.131*0.5
U11U22U33U12U13U23
Re10.02175 (14)0.01753 (12)0.02081 (13)0.00464 (10)0.00118 (11)−0.00026 (9)
Re20.02488 (15)0.01949 (13)0.01971 (13)0.00389 (11)0.00088 (11)−0.00048 (10)
Re30.02332 (15)0.01668 (12)0.02117 (13)0.00340 (10)0.00110 (11)−0.00064 (9)
Re40.02163 (14)0.01778 (13)0.02046 (13)0.00447 (10)0.00114 (11)−0.00061 (9)
Re50.02378 (15)0.01844 (13)0.02146 (14)0.00346 (11)0.00243 (11)−0.00009 (10)
Re60.02424 (15)0.01994 (13)0.02252 (14)0.00545 (11)0.00282 (11)−0.00207 (10)
Se10.0241 (4)0.0240 (3)0.0248 (3)0.0040 (3)−0.0001 (3)−0.0005 (3)
Se20.0249 (4)0.0217 (3)0.0231 (3)0.0036 (3)0.0033 (3)0.0007 (2)
Se30.0261 (4)0.0196 (3)0.0246 (3)0.0035 (3)0.0019 (3)−0.0027 (2)
Se40.0326 (4)0.0225 (3)0.0278 (4)0.0069 (3)0.0012 (3)0.0029 (3)
Se50.0310 (4)0.0220 (3)0.0246 (3)0.0045 (3)0.0014 (3)−0.0044 (3)
Se60.0291 (4)0.0202 (3)0.0285 (4)0.0072 (3)0.0008 (3)0.0011 (3)
Se70.0235 (4)0.0252 (3)0.0271 (4)0.0050 (3)0.0021 (3)−0.0010 (3)
Se80.0302 (4)0.0275 (3)0.0227 (3)0.0037 (3)0.0047 (3)0.0000 (3)
S10.0315 (11)0.0419 (11)0.0480 (12)0.0094 (9)0.0045 (9)−0.0030 (9)
P10.0279 (10)0.0244 (9)0.0291 (9)0.0091 (8)0.0029 (8)0.0005 (7)
P20.0353 (11)0.0283 (9)0.0227 (9)0.0068 (8)0.0001 (8)0.0017 (7)
P30.0296 (10)0.0206 (8)0.0299 (10)−0.0010 (8)−0.0001 (8)0.0008 (7)
P40.0301 (10)0.0268 (9)0.0226 (9)0.0065 (8)0.0000 (8)0.0013 (7)
P50.0435 (13)0.0264 (10)0.0342 (11)−0.0022 (9)0.0063 (9)0.0013 (8)
O10.030 (3)0.025 (2)0.041 (3)0.005 (2)0.004 (2)−0.002 (2)
O20.046 (4)0.040 (3)0.074 (4)−0.012 (3)0.015 (3)−0.012 (3)
O30.037 (4)0.090 (5)0.062 (4)0.030 (4)−0.006 (3)0.007 (4)
C10.040 (5)0.046 (5)0.050 (5)0.010 (4)0.007 (4)−0.004 (4)
C20.103 (10)0.093 (9)0.072 (8)0.061 (8)0.018 (7)0.009 (7)
C30.094 (9)0.070 (7)0.078 (8)0.043 (7)0.020 (7)−0.003 (6)
C40.078 (8)0.052 (6)0.064 (7)0.014 (6)0.027 (6)−0.008 (5)
C50.147 (13)0.145 (12)0.056 (7)0.106 (11)0.000 (8)−0.019 (7)
C60.184 (16)0.161 (13)0.048 (6)0.143 (13)−0.023 (8)−0.027 (7)
C70.102 (10)0.074 (7)0.078 (8)0.023 (7)0.036 (7)−0.022 (6)
C110.036 (5)0.034 (4)0.038 (4)0.014 (3)0.008 (4)−0.002 (3)
C120.062 (6)0.045 (5)0.034 (4)0.021 (4)0.006 (4)−0.001 (4)
C130.042 (5)0.037 (4)0.034 (4)0.017 (4)−0.008 (4)0.000 (3)
C140.030 (4)0.042 (4)0.044 (5)0.002 (4)0.008 (4)0.005 (4)
C150.045 (5)0.029 (4)0.044 (5)0.018 (4)0.008 (4)0.009 (3)
C160.056 (6)0.028 (4)0.051 (5)0.011 (4)0.013 (4)0.004 (4)
C210.040 (5)0.040 (4)0.036 (4)0.006 (4)0.000 (4)0.000 (3)
C220.044 (5)0.056 (5)0.043 (5)0.009 (4)−0.006 (4)−0.005 (4)
C230.051 (5)0.040 (4)0.024 (4)−0.001 (4)0.006 (4)0.002 (3)
C240.050 (6)0.053 (5)0.036 (5)0.009 (4)0.011 (4)−0.002 (4)
C250.051 (5)0.040 (4)0.032 (4)0.013 (4)−0.005 (4)0.007 (3)
C260.058 (6)0.051 (5)0.053 (5)0.030 (5)−0.010 (5)0.004 (4)
C310.054 (6)0.025 (4)0.043 (5)−0.002 (4)0.002 (4)−0.005 (3)
C320.067 (7)0.055 (6)0.040 (5)−0.007 (5)−0.013 (5)0.000 (4)
C330.035 (5)0.038 (4)0.043 (5)−0.001 (4)0.002 (4)0.007 (3)
C340.042 (5)0.046 (5)0.076 (7)−0.001 (4)0.004 (5)0.018 (5)
C350.035 (4)0.022 (3)0.046 (5)0.002 (3)0.004 (4)0.009 (3)
C360.058 (6)0.037 (4)0.040 (5)0.005 (4)−0.005 (4)0.012 (4)
C410.041 (5)0.041 (4)0.039 (4)0.008 (4)−0.001 (4)0.001 (4)
C420.050 (6)0.045 (5)0.047 (5)0.003 (4)−0.013 (4)−0.012 (4)
C430.050 (5)0.033 (4)0.034 (4)0.020 (4)0.000 (4)0.008 (3)
C440.048 (5)0.047 (5)0.057 (5)0.023 (4)0.002 (4)0.003 (4)
C450.039 (5)0.049 (5)0.031 (4)0.012 (4)0.004 (4)0.004 (3)
C460.047 (5)0.056 (5)0.034 (4)0.014 (4)0.008 (4)−0.008 (4)
C510.060 (7)0.059 (6)0.067 (7)−0.009 (5)0.010 (5)0.020 (5)
C520.071 (8)0.053 (6)0.082 (8)−0.010 (5)0.029 (6)−0.010 (5)
C530.090 (8)0.044 (5)0.051 (6)−0.022 (5)−0.012 (6)−0.005 (4)
C540.070 (7)0.066 (6)0.048 (6)−0.028 (5)0.004 (5)−0.005 (5)
C550.122 (11)0.049 (6)0.087 (8)0.004 (7)−0.023 (8)0.025 (6)
S20.0549 (14)0.0320 (10)0.0315 (10)0.0047 (9)0.0068 (10)0.0020 (8)
O40.069 (5)0.044 (3)0.058 (4)−0.013 (3)0.025 (3)−0.013 (3)
O50.053 (4)0.046 (3)0.074 (4)−0.002 (3)0.031 (4)−0.008 (3)
O60.134 (7)0.088 (5)0.056 (4)0.083 (5)0.015 (4)0.001 (4)
C610.040 (5)0.026 (4)0.036 (4)0.003 (3)0.001 (4)0.009 (3)
C620.049 (5)0.040 (4)0.033 (4)0.008 (4)0.004 (4)0.000 (3)
C630.080 (8)0.038 (5)0.042 (5)0.010 (5)0.013 (5)−0.004 (4)
C640.062 (7)0.031 (4)0.057 (6)0.006 (4)0.017 (5)0.004 (4)
C650.043 (5)0.039 (5)0.088 (7)0.012 (4)0.013 (5)0.021 (5)
C660.045 (5)0.034 (4)0.054 (5)−0.001 (4)0.001 (4)−0.003 (4)
C670.118 (10)0.045 (6)0.101 (9)0.042 (6)0.058 (8)0.019 (6)
Cl1S0.085 (2)0.0841 (19)0.0724 (18)0.0330 (17)0.0007 (16)0.0012 (15)
Cl2S0.084 (2)0.080 (2)0.114 (3)0.0180 (18)−0.008 (2)−0.0070 (19)
C1S0.067 (8)0.101 (9)0.068 (7)0.022 (7)0.000 (6)0.005 (7)
C2S0.077 (10)0.109 (11)0.135 (12)0.022 (8)−0.012 (9)−0.020 (9)
Re1—P12.4818 (18)P2—C251.833 (7)
Re1—Se22.5171 (7)P3—C331.819 (8)
Re1—Se32.5199 (7)P3—C311.825 (7)
Re1—Se42.5218 (7)P3—C351.825 (7)
Re1—Se12.5232 (7)P4—C431.816 (7)
Re1—Re22.6341 (4)P4—C451.822 (7)
Re1—Re32.6464 (4)P4—C411.826 (8)
Re1—Re42.6480 (4)P5—C551.760 (10)
Re1—Re52.6486 (4)P5—C531.827 (9)
Re2—P22.4765 (18)P5—C511.880 (10)
Re2—Se42.5074 (7)C1—C61.327 (13)
Re2—Se82.5150 (8)C1—C21.380 (12)
Re2—Se12.5168 (7)C2—C31.399 (14)
Re2—Se52.5201 (7)C3—C41.347 (14)
Re2—Re32.6320 (4)C4—C51.372 (13)
Re2—Re62.6321 (4)C4—C71.523 (13)
Re2—Re52.6482 (4)C5—C61.403 (14)
Re3—P32.4771 (17)C11—C121.526 (10)
Re3—Se62.5097 (7)C13—C141.529 (10)
Re3—Se12.5144 (7)C15—C161.495 (11)
Re3—Se22.5170 (7)C21—C221.528 (10)
Re3—Se52.5227 (7)C23—C241.512 (10)
Re3—Re42.6322 (4)C25—C261.532 (11)
Re3—Re62.6356 (4)C31—C321.487 (11)
Re4—P42.4796 (18)C33—C341.513 (10)
Re4—Se72.5152 (7)C35—C361.515 (10)
Re4—Se22.5167 (7)C41—C421.520 (10)
Re4—Se62.5209 (7)C43—C441.535 (11)
Re4—Se32.5242 (7)C45—C461.530 (10)
Re4—Re52.6360 (4)C51—C521.471 (13)
Re4—Re62.6387 (4)C53—C541.540 (13)
Re5—P52.4798 (19)C55—C56A1.418 (19)
Re5—Se42.5148 (8)C55—C56B1.43 (3)
Re5—Se72.5171 (7)S2—O41.435 (6)
Re5—Se82.5171 (7)S2—O61.438 (7)
Re5—Se32.5243 (7)S2—O51.441 (6)
Re5—Re62.6206 (4)S2—C611.733 (8)
Re6—O12.123 (5)C61—C661.373 (11)
Re6—Se62.5131 (7)C61—C621.409 (10)
Re6—Se72.5149 (7)C62—C631.380 (11)
Re6—Se52.5154 (7)C63—C641.380 (13)
Re6—Se82.5236 (7)C64—C651.384 (12)
S1—O31.426 (6)C64—C671.497 (11)
S1—O21.445 (6)C65—C661.391 (11)
S1—O11.497 (5)Cl1S—C1S1.746 (11)
S1—C11.759 (9)Cl2S—C1S1.709 (12)
P1—C111.821 (7)Cl3S—C2S1.639 (14)
P1—C151.826 (7)Cl4S—C2S1.747 (14)
P1—C131.838 (8)Cl5S—C2S1.829 (14)
P2—C231.818 (7)Cl6S—C2S1.684 (14)
P2—C211.832 (8)
P1—Re1—Se292.64 (4)Se7—Re5—Re458.377 (17)
P1—Re1—Se392.22 (5)Se8—Re5—Re4119.023 (19)
Se2—Re1—Se389.78 (2)Se3—Re5—Re458.524 (17)
P1—Re1—Se492.08 (4)Re6—Re5—Re460.260 (10)
Se2—Re1—Se4175.28 (2)P5—Re5—Re2136.47 (5)
Se3—Re1—Se489.95 (2)Se4—Re5—Re258.040 (18)
P1—Re1—Se191.99 (5)Se7—Re5—Re2118.484 (19)
Se2—Re1—Se189.41 (2)Se8—Re5—Re258.208 (19)
Se3—Re1—Se1175.74 (2)Se3—Re5—Re2117.88 (2)
Se4—Re1—Se190.52 (2)Re6—Re5—Re259.939 (10)
P1—Re1—Re2134.53 (4)Re4—Re5—Re289.800 (12)
Se2—Re1—Re2118.069 (18)P5—Re5—Re1137.68 (5)
Se3—Re1—Re2118.568 (19)Se4—Re5—Re158.401 (18)
Se4—Re1—Re258.149 (17)Se7—Re5—Re1118.507 (19)
Se1—Re1—Re258.373 (17)Se8—Re5—Re1117.85 (2)
P1—Re1—Re3135.44 (4)Se3—Re5—Re158.245 (17)
Se2—Re1—Re358.284 (16)Re6—Re5—Re190.185 (11)
Se3—Re1—Re3118.027 (19)Re4—Re5—Re160.143 (10)
Se4—Re1—Re3117.904 (19)Re2—Re5—Re159.644 (11)
Se1—Re1—Re358.147 (17)O1—Re6—Se691.02 (13)
Re2—Re1—Re359.793 (9)O1—Re6—Se794.31 (13)
P1—Re1—Re4135.62 (4)Se6—Re6—Se789.57 (2)
Se2—Re1—Re458.255 (17)O1—Re6—Se588.99 (13)
Se3—Re1—Re458.415 (17)Se6—Re6—Se589.52 (2)
Se4—Re1—Re4117.82 (2)Se7—Re6—Se5176.59 (2)
Se1—Re1—Re4117.766 (18)O1—Re6—Se892.75 (13)
Re2—Re1—Re489.846 (12)Se6—Re6—Se8176.16 (2)
Re3—Re1—Re459.625 (10)Se7—Re6—Se890.87 (2)
P1—Re1—Re5135.03 (4)Se5—Re6—Se889.82 (2)
Se2—Re1—Re5117.935 (19)O1—Re6—Re5137.09 (13)
Se3—Re1—Re558.408 (17)Se6—Re6—Re5118.684 (18)
Se4—Re1—Re558.147 (18)Se7—Re6—Re558.655 (17)
Se1—Re1—Re5118.510 (19)Se5—Re6—Re5119.115 (19)
Re2—Re1—Re560.172 (10)Se8—Re6—Re558.553 (17)
Re3—Re1—Re589.532 (11)O1—Re6—Re2133.56 (13)
Re4—Re1—Re559.693 (11)Se6—Re6—Re2118.24 (2)
P2—Re2—Se492.27 (4)Se7—Re6—Re2119.176 (19)
P2—Re2—Se894.73 (5)Se5—Re6—Re258.571 (17)
Se4—Re2—Se888.80 (2)Se8—Re6—Re258.348 (18)
P2—Re2—Se188.81 (5)Re5—Re6—Re260.551 (10)
Se4—Re2—Se191.00 (2)O1—Re6—Re3132.52 (13)
Se8—Re2—Se1176.46 (2)Se6—Re6—Re358.289 (18)
P2—Re2—Se591.59 (4)Se7—Re6—Re3118.238 (19)
Se4—Re2—Se5176.02 (3)Se5—Re6—Re358.592 (18)
Se8—Re2—Se589.92 (2)Se8—Re6—Re3118.29 (2)
Se1—Re2—Se590.05 (2)Re5—Re6—Re390.372 (12)
P2—Re2—Re3132.58 (5)Re2—Re6—Re359.953 (11)
Se4—Re2—Re3118.978 (19)O1—Re6—Re4136.22 (13)
Se8—Re2—Re3118.744 (19)Se6—Re6—Re458.533 (17)
Se1—Re2—Re358.412 (17)Se7—Re6—Re458.365 (17)
Se5—Re2—Re358.587 (17)Se5—Re6—Re4118.46 (2)
P2—Re2—Re6136.88 (5)Se8—Re6—Re4118.677 (19)
Se4—Re2—Re6117.82 (2)Re5—Re6—Re460.158 (9)
Se8—Re2—Re658.667 (18)Re2—Re6—Re490.092 (12)
Se1—Re2—Re6118.490 (19)Re3—Re6—Re459.875 (10)
Se5—Re2—Re658.400 (18)Re3—Se1—Re263.085 (19)
Re3—Re2—Re660.089 (10)Re3—Se1—Re163.381 (19)
P2—Re2—Re1132.79 (5)Re2—Se1—Re163.019 (19)
Se4—Re2—Re158.681 (17)Re4—Se2—Re363.055 (17)
Se8—Re2—Re1118.468 (19)Re4—Se2—Re163.477 (17)
Se1—Re2—Re158.608 (17)Re3—Se2—Re163.431 (18)
Se5—Re2—Re1118.907 (18)Re1—Se3—Re463.332 (17)
Re3—Re2—Re160.335 (11)Re1—Se3—Re563.346 (18)
Re6—Re2—Re190.250 (12)Re4—Se3—Re562.950 (16)
P2—Re2—Re5137.53 (5)Re2—Se4—Re563.646 (18)
Se4—Re2—Re558.314 (18)Re2—Se4—Re163.170 (17)
Se8—Re2—Re558.284 (18)Re5—Se4—Re163.452 (18)
Se1—Re2—Re5118.757 (19)Re6—Se5—Re263.029 (18)
Se5—Re2—Re5117.90 (2)Re6—Se5—Re363.085 (18)
Re3—Re2—Re589.848 (12)Re2—Se5—Re362.925 (17)
Re6—Re2—Re559.510 (11)Re3—Se6—Re663.300 (18)
Re1—Re2—Re560.184 (11)Re3—Se6—Re463.097 (17)
P3—Re3—Se691.08 (5)Re6—Se6—Re463.225 (17)
P3—Re3—Se192.48 (5)Re6—Se7—Re463.279 (19)
Se6—Re3—Se1176.42 (2)Re6—Se7—Re562.771 (19)
P3—Re3—Se290.40 (5)Re4—Se7—Re563.177 (19)
Se6—Re3—Se290.67 (2)Re2—Se8—Re563.508 (18)
Se1—Re3—Se289.61 (2)Re2—Se8—Re662.985 (18)
P3—Re3—Se593.57 (5)Re5—Se8—Re662.651 (18)
Se6—Re3—Se589.43 (2)O3—S1—O2116.5 (4)
Se1—Re3—Se590.05 (2)O3—S1—O1109.9 (3)
Se2—Re3—Se5176.03 (2)O2—S1—O1112.6 (3)
P3—Re3—Re2136.60 (4)O3—S1—C1107.8 (4)
Se6—Re3—Re2118.36 (2)O2—S1—C1107.2 (4)
Se1—Re3—Re258.503 (17)O1—S1—C1101.5 (4)
Se2—Re3—Re2118.150 (18)C11—P1—C15104.1 (3)
Se5—Re3—Re258.489 (17)C11—P1—C13103.7 (4)
P3—Re3—Re4133.15 (4)C15—P1—C13102.5 (4)
Se6—Re3—Re458.659 (17)C11—P1—Re1113.8 (2)
Se1—Re3—Re4118.683 (19)C15—P1—Re1115.6 (3)
Se2—Re3—Re458.467 (18)C13—P1—Re1115.5 (2)
Se5—Re3—Re4118.44 (2)C23—P2—C21104.3 (4)
Re2—Re3—Re490.236 (12)C23—P2—C25101.6 (4)
P3—Re3—Re6135.68 (5)C21—P2—C25104.0 (4)
Se6—Re3—Re658.412 (18)C23—P2—Re2115.3 (3)
Se1—Re3—Re6118.449 (19)C21—P2—Re2114.2 (3)
Se2—Re3—Re6118.558 (19)C25—P2—Re2115.9 (3)
Se5—Re3—Re658.323 (18)C33—P3—C31104.8 (4)
Re2—Re3—Re659.958 (10)C33—P3—C35105.1 (4)
Re4—Re3—Re660.120 (11)C31—P3—C35101.1 (3)
P3—Re3—Re1134.37 (5)C33—P3—Re3113.3 (2)
Se6—Re3—Re1118.850 (19)C31—P3—Re3115.3 (3)
Se1—Re3—Re158.472 (17)C35—P3—Re3115.8 (2)
Se2—Re3—Re158.286 (16)C43—P4—C45100.0 (3)
Se5—Re3—Re1118.346 (18)C43—P4—C41104.2 (4)
Re2—Re3—Re159.872 (10)C45—P4—C41104.4 (4)
Re4—Re3—Re160.217 (10)C43—P4—Re4115.6 (3)
Re6—Re3—Re189.907 (11)C45—P4—Re4117.0 (3)
P4—Re4—Se791.66 (5)C41—P4—Re4113.8 (3)
P4—Re4—Se292.20 (5)C55—P5—C53102.8 (5)
Se7—Re4—Se2176.14 (2)C55—P5—C51105.0 (6)
P4—Re4—Se691.66 (4)C53—P5—C5198.4 (5)
Se7—Re4—Se689.39 (2)C55—P5—Re5115.9 (4)
Se2—Re4—Se690.42 (2)C53—P5—Re5116.1 (3)
P4—Re4—Se392.64 (4)C51—P5—Re5116.3 (3)
Se7—Re4—Se390.21 (2)S1—O1—Re6136.5 (3)
Se2—Re4—Se389.69 (2)C6—C1—C2118.0 (9)
Se6—Re4—Se3175.69 (2)C6—C1—S1121.1 (7)
P4—Re4—Re3134.62 (4)C2—C1—S1120.9 (8)
Se7—Re4—Re3118.358 (19)C1—C2—C3121.2 (10)
Se2—Re4—Re358.478 (17)C4—C3—C2120.1 (10)
Se6—Re4—Re358.244 (18)C3—C4—C5118.9 (10)
Se3—Re4—Re3118.399 (19)C3—C4—C7120.0 (9)
P4—Re4—Re5135.26 (4)C5—C4—C7121.1 (11)
Se7—Re4—Re558.446 (17)C4—C5—C6120.1 (11)
Se2—Re4—Re5118.418 (18)C1—C6—C5121.7 (10)
Se6—Re4—Re5117.818 (19)C12—C11—P1116.8 (6)
Se3—Re4—Re558.526 (17)C14—C13—P1113.7 (5)
Re3—Re4—Re590.112 (12)C16—C15—P1115.6 (6)
P4—Re4—Re6134.67 (4)C22—C21—P2117.0 (6)
Se7—Re4—Re658.355 (17)C24—C23—P2115.5 (5)
Se2—Re4—Re6118.454 (18)C26—C25—P2115.4 (5)
Se6—Re4—Re658.243 (17)C32—C31—P3116.0 (6)
Se3—Re4—Re6118.087 (18)C34—C33—P3115.7 (6)
Re3—Re4—Re660.005 (11)C36—C35—P3117.2 (5)
Re5—Re4—Re659.582 (11)C42—C41—P4116.5 (6)
P4—Re4—Re1135.52 (4)C44—C43—P4116.2 (5)
Se7—Re4—Re1118.598 (19)C46—C45—P4115.5 (5)
Se2—Re4—Re158.268 (17)C52—C51—P5117.6 (8)
Se6—Re4—Re1118.376 (19)C54—C53—P5114.8 (7)
Se3—Re4—Re158.254 (17)C56A—C55—P5119.1 (12)
Re3—Re4—Re160.158 (11)C56B—C55—P5133.1 (18)
Re5—Re4—Re160.164 (10)O4—S2—O6112.0 (4)
Re6—Re4—Re189.807 (12)O4—S2—O5112.8 (4)
P5—Re5—Se494.95 (5)O6—S2—O5112.1 (5)
P5—Re5—Se789.06 (5)O4—S2—C61107.5 (4)
Se4—Re5—Se7175.97 (2)O6—S2—C61105.4 (4)
P5—Re5—Se890.90 (5)O5—S2—C61106.5 (3)
Se4—Re5—Se888.59 (2)C66—C61—C62117.8 (7)
Se7—Re5—Se890.97 (2)C66—C61—S2122.5 (6)
P5—Re5—Se393.06 (5)C62—C61—S2119.7 (6)
Se4—Re5—Se390.01 (2)C63—C62—C61119.9 (8)
Se7—Re5—Se390.17 (2)C62—C63—C64122.4 (9)
Se8—Re5—Se3175.91 (2)C63—C64—C65117.5 (8)
P5—Re5—Re6132.11 (5)C63—C64—C67121.0 (9)
Se4—Re5—Re6117.978 (19)C65—C64—C67121.5 (10)
Se7—Re5—Re658.574 (17)C64—C65—C66120.9 (9)
Se8—Re5—Re658.797 (17)C61—C66—C65121.6 (8)
Se3—Re5—Re6118.763 (18)Cl2S—C1S—Cl1S114.6 (7)
P5—Re5—Re4133.61 (5)Cl3S—C2S—Cl4S107.5 (8)
Se4—Re5—Re4118.52 (2)Cl6S—C2S—Cl5S108.3 (8)
  9 in total

1.  Synthesis and electrochemical study of the first tetrazolate hexanuclear rhenium cluster complex.

Authors:  Lisa F Szczepura; Meghan K Oh; Stanley A Knott
Journal:  Chem Commun (Camb)       Date:  2007-10-19       Impact factor: 6.222

2.  Alcohol addition to acetonitrile activated by the [Re6(mu3-Se)8]2+ cluster core.

Authors:  Peter Orto; Hugh D Selby; Daniel Ferris; Jenine R Maeyer; Zhiping Zheng
Journal:  Inorg Chem       Date:  2007-04-26       Impact factor: 5.165

3.  Organometallic rhenium(III) chalcogenide clusters: coordination of N-heterocyclic carbenes.

Authors:  Jessica L Durham; Wade B Wilson; Daniel N Huh; Robert McDonald; Lisa F Szczepura
Journal:  Chem Commun (Camb)       Date:  2015-07-04       Impact factor: 6.222

4.  Preparation of a family of hexanuclear rhenium cluster complexes containing 5-(phenyl)tetrazol-2-yl ligands and alkylation of 5-substituted tetrazolate ligands.

Authors:  Jessica L Durham; Joan N Tirado; Stanley A Knott; Meghan K Oh; Robert McDonald; Lisa F Szczepura
Journal:  Inorg Chem       Date:  2012-07-05       Impact factor: 5.165

5.  Synthesis and Structures of Solvated Monoclusters and Bridged Di- and Triclusters Based on the Cubic Building Block [Re(6)(&mgr;(3)-Se)(8)](2+).

Authors:  Zhiping Zheng; Thomas G. Gray; R. H. Holm
Journal:  Inorg Chem       Date:  1999-10-18       Impact factor: 5.165

6.  Azide alkyne cycloaddition facilitated by hexanuclear rhenium chalcogenide cluster complexes.

Authors:  Stanley A Knott; Jeffrey N Templeton; Jessica L Durham; Angela M Howard; Robert McDonald; Lisa F Szczepura
Journal:  Dalton Trans       Date:  2013-04-15       Impact factor: 4.390

7.  Emission and metal- and ligand-centered-redox characteristics of the hexarhenium(III) clusters trans- and cis-[Re6(mu 3-S)8Cl4(L)2]2-, where L is a pyridine derivative or pyrazine.

Authors:  T Yoshimura; K Umakoshi; Y Sasaki; S Ishizaka; H B Kim; N Kitamura
Journal:  Inorg Chem       Date:  2000-04-17       Impact factor: 5.165

8.  Selective functionalisation of Re6 cluster anionic units: from hexa-hydroxo [Re6Q8(OH)6]4- (Q = S, Se) to neutral trans-[Re6Q8L4L'2] hybrid building blocks.

Authors:  Frédérick Dorson; Yann Molard; Stéphane Cordier; Bruno Fabre; Olga Efremova; David Rondeau; Yuri Mironov; Viorel Cîrcu; Nikolay Naumov; Christiane Perrin
Journal:  Dalton Trans       Date:  2009-02-28       Impact factor: 4.390

9.  Crystal structure refinement with SHELXL.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr C Struct Chem       Date:  2015-01-01       Impact factor: 1.172

  9 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.