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In the title complex [Yb(SAr*)2(thf)4] (Ar* is 2,6-Trip2C6H3, C36H49S, where Trip is 2,4,6-iPr3C6H2; thf is tetrahydro­furan, C4H8O), the Yb atom occupies a special position on the inversion center. It shows a slightly distorted trans-octahedral environment formed by the O atoms of four tetra­hydro­furan ligands (average Yb-O 2.400 Å) and the S atoms of two thiol­ate ligands [Yb-S 2.8023 (13) Å]. The overcrowding caused by the sterically encumbered Ar* ligands is reflected in the large Yb-S-C angle of 151.16 (16)°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680101306X/ya6051sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680101306X/ya6051Isup2.hkl
Contains datablock I

CCDC reference: 172191

Key indicators

  • Single-crystal X-ray study
  • T = 188 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.052
  • wR factor = 0.128
  • Data-to-parameter ratio = 17.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Comment top

In a continuation of our work on low-coordinate σ-bonded rare earth compounds, we have recently reported (Niemeyer, 2001) the synthesis and structural characterization of the σ-donor-free m-terphenyl-based metal thiolates M(SAr*)2 (M = Eu, Yb; Ar* = 2,6-Trip2C6H3; Trip = 2,4,6-iPr3C6H2). The preparation of these compounds by a one-pot direct-synthesis/protolysis route involves the synthesis of the solvated complexes M(SAr*)2(thf)n. Remarkably, the coordinated tetrahydrofuran can be removed completely either by crystallization from weakly coordinating solvents (M = Eu) or by evacuation at ambient temperature (M = Yb). However, in the case of the ytterbium derivative, prolonged storage at low temperature leads to crystallization of the intact solvate.

The title complex, (I), comprises a six-coordinate Yb atom, occupying a special position in the inversion center. It is bonded to the S atoms of two thiolate ligands in trans positions, as well as to the O atoms of four tetrahydrofuran ligands. The symmetry-independent half of the molecule of the complex is shown in Fig. 1. The full molecule (without the isopropyl groups, which were omitted for clarity) is depicted in Fig. 2. The Yb—S distance of 2.8023 (13) Å is considerably longer than the distance of 2.691 Å which was observed in donor-free Yb(SAr*)2 (Niemeyer, 2001). It may be compared with the Yb—S bond lengths in other six-coordinate σ-donor stabilized YbII thiolates which were reported as 2.739 Å in Yb(SAr*)2(dme)2 (Niemeyer, 2001), 2.756 Å in Yb(SMes*)2(dme)2 (Mes* = 2,4,6-tri-tert-butylphenyl; Cetinkaya et al., 1992) and 2.827 Å in Yb(SPh)2(py)4 (Brewer et al., 1994). The Yb—S—C1 angle in (I) is widened to 151.16 (16)°, obviously due to overcrowding caused by the sterically encumbered Ar* ligands.

Experimental top

The title compound was synthesized and characterized as described previously (Niemeyer, 2001). Yellow crystals were obtained after storing a heptane/tetrahydrofuran (4:1) solution at 258 K for several months.

Refinement top

The H atoms were placed in the idealized positions and refined in a riding model approximation, including free rotation for methyl groups. For most H atoms, the assigned Uiso was allowed to refine freely. Isotropic displacement parameters larger than 0.15 Å2 were constrained to 1.2Ueq (CH, CH2) or 1.5 Ueq (CH3) of the parent atom.

Computing details top

Data collection: P3 (Siemens, 1989); cell refinement: P3; data reduction: XDISK (Siemens, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot (at the 40% probability level) for the asymmetric unit of (I). H atoms have been omitted for clarity. Bonds from the Yb atom to symmetry-related atoms are indicated by broken lines.
[Figure 2] Fig. 2. The molecular structure of (I). H atoms and isopropyl C atoms have been omitted for clarity.
trans-bis(2,4,6,2'',4'',6''-hexaisopropyl-1,1':3',1''-terphenyl-2'-thiolato-S)- tetrakis(tetrahydrofuran-O)ytterbium(II) top
Crystal data top
[Yb(C36H49S)2(C4H8O)4]F(000) = 1584
Mr = 1489.08Dx = 1.212 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 13.666 (3) ÅCell parameters from 50 reflections
b = 16.277 (3) Åθ = 16.7–25.1°
c = 18.575 (4) ŵ = 1.24 mm1
β = 98.99 (3)°T = 188 K
V = 4081.0 (14) Å3Plate, yellow
Z = 20.45 × 0.40 × 0.10 mm
Data collection top
Rebuild Syntex P21/Siemens P3 four-circle
diffractometer
6008 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.053
Graphite monochromatorθmax = 27.0°, θmin = 1.7°
Wyckoff scansh = 017
Absorption correction: ψ scan
(North et al., 1968)
k = 200
Tmin = 0.604, Tmax = 0.886l = 2323
9278 measured reflections2 standard reflections every 198 reflections
8906 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.052Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.128Only H-atom displacement parameters refined
S = 1.08 w = 1/[σ2(Fo2) + (0.0646P)2]
where P = (Fo2 + 2Fc2)/3
8906 reflections(Δ/σ)max = 0.001
499 parametersΔρmax = 0.76 e Å3
0 restraintsΔρmin = 1.04 e Å3
Crystal data top
[Yb(C36H49S)2(C4H8O)4]V = 4081.0 (14) Å3
Mr = 1489.08Z = 2
Monoclinic, P21/nMo Kα radiation
a = 13.666 (3) ŵ = 1.24 mm1
b = 16.277 (3) ÅT = 188 K
c = 18.575 (4) Å0.45 × 0.40 × 0.10 mm
β = 98.99 (3)°
Data collection top
Rebuild Syntex P21/Siemens P3 four-circle
diffractometer
6008 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.053
Tmin = 0.604, Tmax = 0.8862 standard reflections every 198 reflections
9278 measured reflections intensity decay: none
8906 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0520 restraints
wR(F2) = 0.128Only H-atom displacement parameters refined
S = 1.08Δρmax = 0.76 e Å3
8906 reflectionsΔρmin = 1.04 e Å3
499 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Yb0.50000.00000.00000.02386 (9)
S0.45036 (9)0.07155 (8)0.12668 (7)0.0312 (3)
O410.4317 (3)0.1229 (2)0.0444 (2)0.0439 (10)
O510.6568 (2)0.0450 (3)0.06324 (19)0.0383 (9)
C10.4527 (3)0.1551 (3)0.1877 (2)0.0225 (9)
C20.5310 (3)0.1647 (3)0.2465 (2)0.0242 (10)
C30.5306 (4)0.2310 (3)0.2948 (3)0.0298 (11)
H3A0.58460.23770.33320.056 (19)*
C40.4535 (4)0.2864 (3)0.2876 (3)0.0352 (12)
H4A0.45530.33210.31960.026 (13)*
C50.3732 (4)0.2745 (3)0.2328 (3)0.0304 (11)
H5A0.31860.31120.22890.042 (16)*
C60.3709 (3)0.2102 (3)0.1834 (2)0.0221 (9)
C70.6142 (3)0.1035 (3)0.2661 (2)0.0249 (10)
C80.5966 (4)0.0313 (3)0.3044 (3)0.0294 (10)
C90.6761 (4)0.0195 (3)0.3298 (3)0.0338 (13)
H9A0.66420.06800.35560.040 (16)*
C100.7727 (3)0.0023 (4)0.3191 (3)0.0352 (10)
C110.7883 (4)0.0686 (3)0.2822 (3)0.0341 (12)
H11A0.85380.08150.27480.056 (19)*
C120.7106 (3)0.1232 (3)0.2549 (3)0.0304 (11)
C130.4944 (4)0.0111 (4)0.3207 (3)0.0366 (13)
H13A0.44620.04780.29000.024 (13)*
C140.4882 (6)0.0300 (6)0.4008 (4)0.071 (2)
H14A0.50240.08830.41050.12 (4)*
H14B0.42140.01730.41070.08 (2)*
H14C0.53670.00350.43240.11 (4)*
C150.4637 (5)0.0773 (4)0.3022 (4)0.0583 (18)
H15A0.46780.08800.25090.10 (3)*
H15B0.50810.11480.33310.036 (15)*
H15C0.39550.08580.31080.07 (2)*
C160.8558 (4)0.0627 (4)0.3484 (3)0.0477 (15)
H16A0.83330.11860.33080.030 (14)*
C170.8728 (6)0.0653 (5)0.4317 (4)0.069 (2)
H17A0.92440.10570.44870.07 (2)*
H17B0.89380.01100.45090.107*
H17C0.81110.08100.44880.09 (3)*
C180.9517 (5)0.0454 (6)0.3199 (5)0.072 (2)
H18A0.99820.09070.33340.10 (3)*
H18B0.93840.04020.26670.10 (3)*
H18C0.98060.00590.34120.11 (4)*
C190.7315 (4)0.1983 (4)0.2123 (3)0.0388 (13)
H19A0.68320.24150.22190.038 (15)*
C200.8356 (4)0.2344 (4)0.2342 (4)0.0555 (18)
H20A0.84860.24250.28710.15 (4)*
H20B0.88480.19650.21980.07 (2)*
H20C0.83980.28730.20970.10 (3)*
C210.7116 (5)0.1801 (5)0.1315 (3)0.062 (2)
H21A0.64280.16180.11780.093*
H21B0.72230.22990.10420.07 (2)*
H21C0.75650.13680.12010.05 (2)*
C220.2756 (3)0.2017 (3)0.1307 (3)0.0247 (10)
C230.2519 (3)0.2590 (3)0.0734 (3)0.0298 (11)
C240.1571 (4)0.2571 (4)0.0318 (3)0.0373 (12)
H24A0.14120.29580.00660.037 (15)*
C250.0862 (4)0.2012 (4)0.0444 (3)0.0371 (12)
C260.1114 (4)0.1444 (3)0.1004 (3)0.0369 (13)
H26A0.06340.10510.10950.041 (16)*
C270.2049 (3)0.1432 (3)0.1439 (3)0.0298 (11)
C280.3228 (3)0.3251 (3)0.0557 (3)0.0321 (11)
H28A0.39050.31140.08170.035 (15)*
C290.2944 (4)0.4090 (3)0.0819 (3)0.0418 (13)
H29A0.30200.40910.13520.051 (18)*
H29B0.33750.45110.06580.028 (13)*
H29C0.22530.42090.06150.08 (2)*
C300.3275 (4)0.3288 (4)0.0261 (3)0.0467 (15)
H30A0.32850.27290.04550.034 (15)*
H30B0.26930.35810.05110.057 (19)*
H30C0.38780.35790.03390.055 (19)*
C310.0162 (4)0.2056 (4)0.0027 (4)0.0472 (15)
H31A0.00560.22180.05280.09 (3)*
C320.0776 (4)0.2712 (5)0.0240 (4)0.0600 (19)
H32A0.13850.27880.01100.047 (17)*
H32B0.09460.25530.07140.049 (19)*
H32C0.04020.32280.02900.08 (3)*
C330.0674 (5)0.1229 (5)0.0092 (4)0.064 (2)
H33A0.13020.12740.04270.08 (2)*
H33B0.02480.08240.02800.13 (4)*
H33C0.08050.10540.03890.06 (2)*
C340.2280 (4)0.0814 (3)0.2061 (3)0.0371 (12)
H34A0.30140.07300.21540.07 (2)*
C350.1977 (8)0.1148 (5)0.2752 (4)0.082 (3)
H35A0.21850.07660.31540.08 (3)*
H35B0.22920.16830.28660.08 (2)*
H35C0.12550.12120.26840.08 (3)*
C360.1801 (5)0.0017 (4)0.1886 (4)0.0514 (14)
H36A0.20250.04010.22850.07 (2)*
H36B0.10790.00390.18280.07 (2)*
H36C0.19900.02280.14330.10 (3)*
C420.3515 (5)0.1281 (5)0.0848 (5)0.068 (2)
H42A0.35510.08250.12050.07 (2)*
H42B0.28750.12450.05170.112*
C430.3600 (8)0.2079 (6)0.1230 (6)0.093 (3)
H43A0.29370.23090.12610.140*
H43B0.39750.20220.17280.140*
C440.4136 (10)0.2602 (6)0.0779 (6)0.115 (4)
H44A0.45820.29850.10890.172*
H44B0.36650.29280.04330.172*
C450.4717 (6)0.2044 (4)0.0380 (5)0.064 (2)
H45A0.46520.22080.01390.06 (2)*
H45B0.54260.20600.05950.085*
C520.7480 (4)0.0547 (5)0.0345 (3)0.0482 (16)
H52A0.74240.09960.00190.07 (2)*
H52B0.76570.00330.01110.11 (3)*
C530.8250 (4)0.0755 (5)0.1005 (3)0.059 (2)
H53A0.85610.02510.12360.07 (3)*
H53B0.87730.11170.08680.06 (2)*
C540.7650 (4)0.1189 (5)0.1502 (4)0.0521 (17)
H54A0.75210.17680.13530.13 (4)*
H54B0.79810.11720.20150.038 (15)*
C550.6708 (4)0.0688 (4)0.1391 (3)0.0403 (13)
H55A0.67770.01970.17110.053 (19)*
H55B0.61410.10190.14990.07 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Yb0.02124 (12)0.02869 (15)0.02139 (13)0.00341 (16)0.00249 (8)0.00141 (18)
S0.0341 (6)0.0327 (7)0.0267 (6)0.0039 (5)0.0046 (5)0.0095 (5)
O410.042 (2)0.033 (2)0.058 (3)0.0002 (17)0.0124 (18)0.002 (2)
O510.0292 (17)0.056 (3)0.0274 (19)0.0153 (17)0.0020 (14)0.0029 (18)
C10.030 (2)0.022 (2)0.016 (2)0.0001 (18)0.0058 (17)0.0016 (18)
C20.029 (2)0.022 (2)0.021 (2)0.0008 (18)0.0030 (17)0.0030 (19)
C30.032 (2)0.026 (3)0.029 (3)0.001 (2)0.0011 (19)0.002 (2)
C40.043 (3)0.031 (3)0.028 (3)0.006 (2)0.005 (2)0.010 (2)
C50.034 (2)0.023 (3)0.034 (3)0.007 (2)0.003 (2)0.001 (2)
C60.024 (2)0.021 (2)0.021 (2)0.0012 (17)0.0009 (17)0.0004 (19)
C70.028 (2)0.027 (3)0.018 (2)0.0048 (19)0.0040 (17)0.0032 (19)
C80.036 (2)0.029 (2)0.022 (2)0.001 (2)0.0023 (19)0.001 (2)
C90.045 (3)0.029 (4)0.026 (2)0.006 (2)0.001 (2)0.001 (2)
C100.040 (2)0.031 (3)0.030 (2)0.003 (3)0.0084 (18)0.007 (3)
C110.030 (2)0.032 (3)0.039 (3)0.006 (2)0.001 (2)0.005 (2)
C120.031 (2)0.031 (3)0.027 (3)0.000 (2)0.0013 (19)0.001 (2)
C130.042 (2)0.035 (4)0.034 (3)0.006 (3)0.012 (2)0.012 (3)
C140.083 (5)0.088 (6)0.053 (4)0.022 (5)0.041 (4)0.011 (4)
C150.050 (4)0.054 (5)0.072 (5)0.005 (3)0.011 (3)0.008 (4)
C160.052 (3)0.039 (3)0.044 (3)0.016 (3)0.017 (3)0.006 (3)
C170.085 (5)0.065 (5)0.049 (4)0.042 (4)0.017 (4)0.003 (4)
C180.048 (4)0.080 (6)0.081 (6)0.030 (4)0.013 (4)0.011 (5)
C190.028 (2)0.041 (3)0.047 (3)0.002 (2)0.003 (2)0.005 (3)
C200.043 (3)0.048 (4)0.072 (5)0.014 (3)0.002 (3)0.012 (4)
C210.071 (4)0.075 (5)0.038 (4)0.022 (4)0.004 (3)0.016 (4)
C220.024 (2)0.024 (2)0.026 (2)0.0017 (18)0.0038 (17)0.003 (2)
C230.026 (2)0.032 (3)0.030 (3)0.002 (2)0.0011 (19)0.005 (2)
C240.031 (2)0.038 (3)0.039 (3)0.006 (2)0.007 (2)0.002 (3)
C250.028 (2)0.043 (3)0.038 (3)0.005 (2)0.004 (2)0.007 (3)
C260.027 (2)0.036 (3)0.048 (3)0.011 (2)0.008 (2)0.005 (3)
C270.030 (2)0.028 (3)0.032 (3)0.002 (2)0.0079 (19)0.008 (2)
C280.028 (2)0.032 (3)0.034 (3)0.003 (2)0.000 (2)0.008 (2)
C290.053 (3)0.028 (3)0.044 (3)0.004 (3)0.008 (3)0.005 (3)
C300.050 (3)0.046 (4)0.044 (4)0.002 (3)0.008 (3)0.002 (3)
C310.028 (3)0.070 (4)0.042 (3)0.006 (3)0.000 (3)0.009 (3)
C320.028 (3)0.073 (5)0.077 (5)0.003 (3)0.004 (3)0.007 (4)
C330.040 (3)0.066 (5)0.079 (6)0.018 (3)0.010 (3)0.011 (4)
C340.045 (3)0.033 (3)0.035 (3)0.009 (2)0.011 (2)0.003 (2)
C350.156 (10)0.048 (5)0.051 (5)0.017 (5)0.043 (5)0.007 (4)
C360.061 (3)0.031 (3)0.064 (4)0.006 (4)0.014 (3)0.008 (4)
C420.056 (4)0.046 (4)0.109 (7)0.008 (3)0.037 (4)0.011 (5)
C430.123 (8)0.066 (6)0.102 (8)0.016 (6)0.048 (6)0.015 (5)
C440.201 (12)0.049 (5)0.110 (8)0.008 (7)0.078 (9)0.012 (6)
C450.069 (4)0.043 (4)0.080 (6)0.017 (4)0.008 (4)0.009 (4)
C520.031 (3)0.078 (5)0.035 (3)0.005 (3)0.002 (2)0.006 (3)
C530.026 (3)0.099 (6)0.048 (4)0.014 (3)0.002 (2)0.006 (4)
C540.050 (3)0.063 (5)0.041 (4)0.015 (3)0.003 (3)0.001 (3)
C550.039 (3)0.053 (4)0.027 (3)0.009 (3)0.002 (2)0.006 (3)
Geometric parameters (Å, º) top
Yb—S2.8023 (13)C22—C271.405 (7)
Yb—Si2.8023 (13)C22—C231.414 (7)
Yb—O412.408 (4)C23—C241.403 (6)
Yb—O41i2.408 (4)C23—C281.518 (7)
Yb—O512.392 (3)C24—C251.375 (8)
Yb—O51i2.392 (3)C24—H24A0.9500
S—C11.767 (5)C25—C261.395 (8)
O41—C421.424 (7)C25—C311.530 (7)
O41—C451.446 (7)C26—C271.401 (7)
O51—C521.440 (6)C26—H26A0.9500
O51—C551.445 (6)C27—C341.528 (7)
C1—C21.413 (6)C28—C291.520 (7)
C1—C61.426 (6)C28—C301.531 (8)
C2—C31.403 (7)C28—H28A1.0000
C2—C71.513 (6)C29—H29A0.9800
C3—C41.378 (7)C29—H29B0.9800
C3—H3A0.9500C29—H29C0.9800
C4—C51.389 (7)C30—H30A0.9800
C4—H4A0.9500C30—H30B0.9800
C5—C61.388 (7)C30—H30C0.9800
C5—H5A0.9500C31—C321.490 (9)
C6—C221.508 (6)C31—C331.514 (9)
C7—C121.403 (7)C31—H31A1.0000
C7—C81.413 (7)C32—H32A0.9800
C8—C91.389 (7)C32—H32B0.9800
C8—C131.511 (7)C32—H32C0.9800
C9—C101.394 (7)C33—H33A0.9800
C9—H9A0.9500C33—H33B0.9800
C10—C111.376 (8)C33—H33C0.9800
C10—C161.534 (7)C34—C351.509 (8)
C11—C121.416 (7)C34—C361.516 (8)
C11—H11A0.9500C34—H34A1.0000
C12—C191.507 (8)C35—H35A0.9800
C13—C151.522 (8)C35—H35B0.9800
C13—C141.534 (8)C35—H35C0.9800
C13—H13A1.0000C36—H36A0.9800
C14—H14A0.9800C36—H36B0.9800
C14—H14B0.9800C36—H36C0.9800
C14—H14C0.9800C42—C431.476 (11)
C15—H15A0.9800C42—H42A0.9900
C15—H15B0.9800C42—H42B0.9900
C15—H15C0.9800C43—C441.468 (13)
C16—C181.515 (10)C43—H43A0.9900
C16—C171.529 (9)C43—H43B0.9900
C16—H16A1.0000C44—C451.479 (12)
C17—H17A0.9800C44—H44A0.9900
C17—H17B0.9800C44—H44B0.9900
C17—H17C0.9800C45—H45A0.9900
C18—H18A0.9800C45—H45B0.9900
C18—H18B0.9800C52—C531.524 (8)
C18—H18C0.9800C52—H52A0.9900
C19—C211.513 (8)C52—H52B0.9900
C19—C201.534 (7)C53—C541.504 (9)
C19—H19A1.0000C53—H53A0.9900
C20—H20A0.9800C53—H53B0.9900
C20—H20B0.9800C54—C551.512 (8)
C20—H20C0.9800C54—H54A0.9900
C21—H21A0.9800C54—H54B0.9900
C21—H21B0.9800C55—H55A0.9900
C21—H21C0.9800C55—H55B0.9900
O51—Yb—O51i180.0 (3)C24—C23—C28117.5 (5)
O51—Yb—O4186.70 (14)C22—C23—C28123.5 (4)
O51i—Yb—O4193.30 (14)C25—C24—C23122.4 (5)
O51—Yb—O41i93.30 (14)C25—C24—H24A118.8
O51i—Yb—O41i86.70 (14)C23—C24—H24A118.8
O41—Yb—O41i180.0 (2)C24—C25—C26117.8 (5)
O51—Yb—S91.77 (9)C24—C25—C31118.5 (5)
O51i—Yb—S88.23 (9)C26—C25—C31123.7 (5)
O41—Yb—S84.26 (10)C25—C26—C27122.4 (5)
O41i—Yb—S95.74 (10)C25—C26—H26A118.8
O51—Yb—Si88.23 (9)C27—C26—H26A118.8
O51i—Yb—Si91.77 (9)C26—C27—C22118.7 (5)
O41—Yb—Si95.74 (10)C26—C27—C34120.5 (5)
O41i—Yb—Si84.26 (10)C22—C27—C34120.8 (4)
S—Yb—Si180.00 (7)C23—C28—C29111.3 (4)
C1—S—Yb151.16 (16)C23—C28—C30111.7 (4)
C42—O41—C45108.7 (5)C29—C28—C30109.6 (5)
C42—O41—Yb126.9 (4)C23—C28—H28A108.0
C45—O41—Yb124.2 (4)C29—C28—H28A108.0
C52—O51—C55110.0 (4)C30—C28—H28A108.0
C52—O51—Yb127.8 (3)C28—C29—H29A109.5
C55—O51—Yb122.2 (3)C28—C29—H29B109.5
C2—C1—C6117.8 (4)H29A—C29—H29B109.5
C2—C1—S121.1 (3)C28—C29—H29C109.5
C6—C1—S120.8 (3)H29A—C29—H29C109.5
C3—C2—C1120.0 (4)H29B—C29—H29C109.5
C3—C2—C7115.5 (4)C28—C30—H30A109.5
C1—C2—C7124.3 (4)C28—C30—H30B109.5
C4—C3—C2121.4 (5)H30A—C30—H30B109.5
C4—C3—H3A119.3C28—C30—H30C109.5
C2—C3—H3A119.3H30A—C30—H30C109.5
C3—C4—C5118.9 (5)H30B—C30—H30C109.5
C3—C4—H4A120.5C32—C31—C33112.7 (5)
C5—C4—H4A120.5C32—C31—C25110.9 (5)
C6—C5—C4121.6 (4)C33—C31—C25112.0 (6)
C6—C5—H5A119.2C32—C31—H31A107.0
C4—C5—H5A119.2C33—C31—H31A107.0
C5—C6—C1120.0 (4)C25—C31—H31A107.0
C5—C6—C22115.2 (4)C31—C32—H32A109.5
C1—C6—C22124.7 (4)C31—C32—H32B109.5
C12—C7—C8120.2 (4)H32A—C32—H32B109.5
C12—C7—C2120.2 (4)C31—C32—H32C109.5
C8—C7—C2119.2 (4)H32A—C32—H32C109.5
C9—C8—C7118.7 (5)H32B—C32—H32C109.5
C9—C8—C13120.0 (5)C31—C33—H33A109.5
C7—C8—C13121.2 (5)C31—C33—H33B109.5
C8—C9—C10122.7 (5)H33A—C33—H33B109.5
C8—C9—H9A118.7C31—C33—H33C109.5
C10—C9—H9A118.7H33A—C33—H33C109.5
C11—C10—C9117.6 (5)H33B—C33—H33C109.5
C11—C10—C16123.4 (5)C35—C34—C36109.7 (5)
C9—C10—C16119.1 (6)C35—C34—C27110.7 (5)
C10—C11—C12122.7 (5)C36—C34—C27113.2 (5)
C10—C11—H11A118.7C35—C34—H34A107.7
C12—C11—H11A118.7C36—C34—H34A107.7
C7—C12—C11118.2 (5)C27—C34—H34A107.7
C7—C12—C19121.5 (4)C34—C35—H35A109.5
C11—C12—C19120.3 (5)C34—C35—H35B109.5
C8—C13—C15113.0 (5)H35A—C35—H35B109.5
C8—C13—C14110.1 (5)C34—C35—H35C109.5
C15—C13—C14110.7 (6)H35A—C35—H35C109.5
C8—C13—H13A107.6H35B—C35—H35C109.5
C15—C13—H13A107.6C34—C36—H36A109.5
C14—C13—H13A107.6C34—C36—H36B109.5
C13—C14—H14A109.5H36A—C36—H36B109.5
C13—C14—H14B109.5C34—C36—H36C109.5
H14A—C14—H14B109.5H36A—C36—H36C109.5
C13—C14—H14C109.5H36B—C36—H36C109.5
H14A—C14—H14C109.5O41—C42—C43107.2 (6)
H14B—C14—H14C109.5O41—C42—H42A110.3
C13—C15—H15A109.5C43—C42—H42A110.3
C13—C15—H15B109.5O41—C42—H42B110.3
H15A—C15—H15B109.5C43—C42—H42B110.3
C13—C15—H15C109.5H42A—C42—H42B108.5
H15A—C15—H15C109.5C44—C43—C42104.2 (7)
H15B—C15—H15C109.5C44—C43—H43A110.9
C18—C16—C17110.8 (6)C42—C43—H43A110.9
C18—C16—C10113.0 (5)C44—C43—H43B110.9
C17—C16—C10111.3 (5)C42—C43—H43B110.9
C18—C16—H16A107.1H43A—C43—H43B108.9
C17—C16—H16A107.1C43—C44—C45106.5 (7)
C10—C16—H16A107.1C43—C44—H44A110.4
C16—C17—H17A109.5C45—C44—H44A110.4
C16—C17—H17B109.5C43—C44—H44B110.4
H17A—C17—H17B109.5C45—C44—H44B110.4
C16—C17—H17C109.5H44A—C44—H44B108.6
H17A—C17—H17C109.5O41—C45—C44106.4 (6)
H17B—C17—H17C109.5O41—C45—H45A110.4
C16—C18—H18A109.5C44—C45—H45A110.4
C16—C18—H18B109.5O41—C45—H45B110.4
H18A—C18—H18B109.5C44—C45—H45B110.4
C16—C18—H18C109.5H45A—C45—H45B108.6
H18A—C18—H18C109.5O51—C52—C53104.8 (5)
H18B—C18—H18C109.5O51—C52—H52A110.8
C12—C19—C21110.0 (5)C53—C52—H52A110.8
C12—C19—C20114.5 (5)O51—C52—H52B110.8
C21—C19—C20110.8 (5)C53—C52—H52B110.8
C12—C19—H19A107.0H52A—C52—H52B108.9
C21—C19—H19A107.0C54—C53—C52102.9 (5)
C20—C19—H19A107.0C54—C53—H53A111.2
C19—C20—H20A109.5C52—C53—H53A111.2
C19—C20—H20B109.5C54—C53—H53B111.2
H20A—C20—H20B109.5C52—C53—H53B111.2
C19—C20—H20C109.5H53A—C53—H53B109.1
H20A—C20—H20C109.5C53—C54—C55101.4 (5)
H20B—C20—H20C109.5C53—C54—H54A111.5
C19—C21—H21A109.5C55—C54—H54A111.5
C19—C21—H21B109.5C53—C54—H54B111.5
H21A—C21—H21B109.5C55—C54—H54B111.5
C19—C21—H21C109.5H54A—C54—H54B109.3
H21A—C21—H21C109.5O51—C55—C54104.9 (4)
H21B—C21—H21C109.5O51—C55—H55A110.8
C27—C22—C23119.7 (4)C54—C55—H55A110.8
C27—C22—C6119.7 (4)O51—C55—H55B110.8
C23—C22—C6120.1 (4)C54—C55—H55B110.8
C24—C23—C22118.9 (5)H55A—C55—H55B108.8
O51—Yb—S—C186.3 (3)C7—C8—C13—C15132.5 (5)
O51i—Yb—S—C193.7 (3)C9—C8—C13—C1474.1 (7)
O41—Yb—S—C1172.8 (3)C7—C8—C13—C14103.1 (6)
O41i—Yb—S—C17.2 (3)C11—C10—C16—C1811.4 (8)
O51—Yb—O41—C42125.4 (5)C9—C10—C16—C18168.4 (6)
O51i—Yb—O41—C4254.6 (5)C11—C10—C16—C17114.1 (7)
S—Yb—O41—C4233.2 (5)C9—C10—C16—C1766.2 (7)
Si—Yb—O41—C42146.8 (5)C7—C12—C19—C2182.6 (6)
O51—Yb—O41—C4550.2 (5)C11—C12—C19—C2194.9 (6)
O51i—Yb—O41—C45129.8 (5)C7—C12—C19—C20151.9 (5)
S—Yb—O41—C45142.3 (5)C11—C12—C19—C2030.6 (8)
Si—Yb—O41—C4537.7 (5)C5—C6—C22—C2799.6 (5)
O41—Yb—O51—C52127.1 (5)C1—C6—C22—C2776.7 (6)
O41i—Yb—O51—C5252.9 (5)C5—C6—C22—C2372.6 (6)
S—Yb—O51—C52148.8 (5)C1—C6—C22—C23111.1 (5)
Si—Yb—O51—C5231.2 (5)C27—C22—C23—C241.3 (7)
O41—Yb—O51—C5551.5 (4)C6—C22—C23—C24170.8 (4)
O41i—Yb—O51—C55128.5 (4)C27—C22—C23—C28179.2 (5)
S—Yb—O51—C5532.7 (4)C6—C22—C23—C287.0 (7)
Si—Yb—O51—C55147.3 (4)C22—C23—C24—C250.3 (8)
Yb—S—C1—C288.5 (5)C28—C23—C24—C25178.3 (5)
Yb—S—C1—C697.8 (4)C23—C24—C25—C260.6 (9)
C6—C1—C2—C35.3 (7)C23—C24—C25—C31178.3 (5)
S—C1—C2—C3179.3 (4)C24—C25—C26—C270.6 (8)
C6—C1—C2—C7169.4 (4)C31—C25—C26—C27178.2 (5)
S—C1—C2—C74.5 (6)C25—C26—C27—C220.4 (8)
C1—C2—C3—C41.9 (8)C25—C26—C27—C34178.2 (5)
C7—C2—C3—C4173.3 (5)C23—C22—C27—C261.4 (7)
C2—C3—C4—C52.2 (8)C6—C22—C27—C26170.9 (4)
C3—C4—C5—C62.8 (8)C23—C22—C27—C34179.2 (5)
C4—C5—C6—C10.8 (8)C6—C22—C27—C347.0 (7)
C4—C5—C6—C22175.7 (5)C24—C23—C28—C2973.7 (6)
C2—C1—C6—C54.8 (7)C22—C23—C28—C29104.1 (6)
S—C1—C6—C5178.7 (4)C24—C23—C28—C3049.1 (7)
C2—C1—C6—C22171.3 (4)C22—C23—C28—C30133.0 (5)
S—C1—C6—C222.6 (6)C24—C25—C31—C3280.3 (7)
C3—C2—C7—C1275.2 (6)C26—C25—C31—C3298.6 (7)
C1—C2—C7—C12109.8 (5)C24—C25—C31—C33152.9 (6)
C3—C2—C7—C896.6 (5)C26—C25—C31—C3328.3 (9)
C1—C2—C7—C878.3 (6)C26—C27—C34—C3587.1 (7)
C12—C7—C8—C90.5 (7)C22—C27—C34—C3590.7 (7)
C2—C7—C8—C9172.3 (4)C26—C27—C34—C3636.6 (7)
C12—C7—C8—C13176.7 (5)C22—C27—C34—C36145.6 (5)
C2—C7—C8—C134.8 (7)C45—O41—C42—C4317.0 (9)
C7—C8—C9—C100.1 (8)Yb—O41—C42—C43159.0 (5)
C13—C8—C9—C10177.3 (5)O41—C42—C43—C4425.9 (11)
C8—C9—C10—C110.5 (8)C42—C43—C44—C4524.9 (12)
C8—C9—C10—C16179.2 (5)C42—O41—C45—C441.2 (9)
C9—C10—C11—C120.5 (8)Yb—O41—C45—C44175.0 (6)
C16—C10—C11—C12179.3 (5)C43—C44—C45—O4115.1 (12)
C8—C7—C12—C110.5 (7)C55—O51—C52—C537.4 (7)
C2—C7—C12—C11172.3 (4)Yb—O51—C52—C53173.9 (4)
C8—C7—C12—C19178.1 (5)O51—C52—C53—C5429.5 (8)
C2—C7—C12—C1910.2 (7)C52—C53—C54—C5539.3 (7)
C10—C11—C12—C70.0 (8)C52—O51—C55—C5417.6 (7)
C10—C11—C12—C19177.6 (5)Yb—O51—C55—C54161.2 (4)
C9—C8—C13—C1550.4 (7)C53—C54—C55—O5135.3 (7)
Symmetry code: (i) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Yb(C36H49S)2(C4H8O)4]
Mr1489.08
Crystal system, space groupMonoclinic, P21/n
Temperature (K)188
a, b, c (Å)13.666 (3), 16.277 (3), 18.575 (4)
β (°) 98.99 (3)
V3)4081.0 (14)
Z2
Radiation typeMo Kα
µ (mm1)1.24
Crystal size (mm)0.45 × 0.40 × 0.10
Data collection
DiffractometerRebuild Syntex P21/Siemens P3 four-circle
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.604, 0.886
No. of measured, independent and
observed [I > 2σ(I)] reflections
9278, 8906, 6008
Rint0.053
(sin θ/λ)max1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.052, 0.128, 1.08
No. of reflections8906
No. of parameters499
H-atom treatmentOnly H-atom displacement parameters refined
Δρmax, Δρmin (e Å3)0.76, 1.04

Computer programs: P3 (Siemens, 1989), P3, XDISK (Siemens, 1989), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 1998), SHELXTL.

Selected geometric parameters (Å, º) top
Yb—S2.8023 (13)S—C11.767 (5)
Yb—O412.408 (4)C1—C21.413 (6)
Yb—O512.392 (3)C1—C61.426 (6)
O51—Yb—O4186.70 (14)C2—C1—C6117.8 (4)
O51—Yb—S91.77 (9)C2—C1—S121.1 (3)
O41—Yb—S84.26 (10)C6—C1—S120.8 (3)
C1—S—Yb151.16 (16)
 

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