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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 65| Part 6| June 2009| Pages m643-m644
doi:10.1107/S1600536809017152

Bis[tris­(3-tert-butyl-5-methyl­pyrazol-1-yl)hydridoborato]ytterbium(II) toluene solvate

Kuburat O. Saliu,a Josef Takatsa and Michael J. Fergusonb*

aDepartment of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G 2G2, and bX-ray Crystallography Laboratory, Department of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G 2G2
*Correspondence e-mail: michael.ferguson@ualberta.ca

(Received 23 April 2009; accepted 6 May 2009; online 14 May 2009)

In the title compound, [Yb(C24H40BN6)2]·C7H8, the Yb atom is coordinated by two tris(3-tert-butyl-5-methyl­pyrazol-1-yl)hydridoborate [TptBu,Me] ligands. One ligand binds in the κ3 mode, throuh three N atoms of the pyrazolyl rings, the other ligand coordinates through two N atoms of the pyrazolyl rings and the H atom attached to the central B via an agostic-type inter­action through the B—H group of the second TptBu,Me ligand, giving an overall distorted octa­hedral geometry. One of the tert-butyl groups is disordered over two sites, with occupancies of 0.65 and 0.35.

Related literature

For full details of the synthesis and spectroscopic characterization of the title compound, see: Zhang et al. (1995[Zhang, X. W., McDonald, R. & Takats, J. (1995). New J. Chem. 19, 573-585.]). For the samarium analogue, see: Zhang et al. (1995[Zhang, X. W., McDonald, R. & Takats, J. (1995). New J. Chem. 19, 573-585.]). For the thulium analogue, see: Cheng et al. (2008[Cheng, J., Takats, J., Ferguson, M. J. & McDonald, R. (2008). J. Am. Chem. Soc. 130, 1544-1545.]). For B—H agostic inter­actions involving pyrazolylborate ligands, see: Calabrese et al. (1990[Calabrese, J. C., Donaille, P. J., Thompson, J. S. & Trofimenko, S. (1990). Inorg. Chem. 29, 4429-4447.]); Kosky et al. (1971[Kosky, C. A., Ganis, P. & Avitabile, G. (1971). Acta Cryst. B27, 1859-1864.]); Cotton et al. (1972[Cotton, F. A., Jeremic, M. & Shaver, A. (1972). Inorg. Chim. Acta, 6, 543-551.]).

[Scheme 1]

Experimental

Crystal data

  • [Yb(C24H40BN6)2]·C7H8

  • Mr = 1112.03

  • Triclinic, [P \overline 1]

  • a = 11.8621 (17) Å

  • b = 12.1587 (17) Å

  • c = 20.650 (3) Å

  • α = 96.1072 (19)°

  • β = 96.1001 (18)°

  • γ = 98.9737 (19)°

  • V = 2902.1 (7) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 1.66 mm−1

  • T = 193 K

  • 0.39 × 0.36 × 0.14 mm
Data collection

  • Bruker SMART 1000 diffractometer

  • Absorption correction: integration (SHELXTL; Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) Tmin = 0.564, Tmax = 0.801

  • 24467 measured reflections

  • 13091 independent reflections

  • 11816 reflections with I > 2σ(I)

  • Rint = 0.026
Refinement

  • R[F2 > 2σ(F2)] = 0.035

  • wR(F2) = 0.096

  • S = 1.10

  • 13091 reflections

  • 669 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 1.91 e Å−3

  • Δρmin = −1.74 e Å−3

Table 1
Selected geometric parameters (Å, °)

Yb—N32 2.477 (3)
Yb—N12 2.524 (3)
Yb—N22 2.547 (2)
Yb—N42 2.555 (2)
Yb—N52 2.632 (3)
Yb—N41 2.990 (2)
Yb—H2B 2.29 (4)
N11—B1 1.554 (4)
N21—B1 1.558 (4)
N31—B1 1.560 (4)
N41—B2 1.546 (4)
N51—B2 1.553 (4)
N61—B2 1.527 (4)
B2—H2B 1.16 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
B2—H2B⋯Yb 1.16 (3) 2.29 (4) 3.002 (3) 118 (2)

Data collection: SMART (Bruker, 1997[Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 1997[Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809017152/lh2812sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809017152/lh2812Isup2.hkl

checkCIF report


Comment top

The synthesis, solution structure and spectroscopic characterization of the title compound was reported by Zhang et al. (1995) along with the samarium analogue whose structure was reported then. The structure of the ytterbium analogue is similar to that reported for the samarium compound featuring a distorted six coordinate octahedral geometry formed by five N atoms of two TptBu,Me ligands and additional agostic B—H interaction from the B—H group of one TptBu,Me ligand. The axial sites are occupied by N32 and H2B. The distortion from ideal geometry is obvious from the deviation of the interatomic angles and distances from the idealized values. The intraligand equatorial bonds to the axial N32 are approximately 90° (87.15 (8)° and 93.28 (8)° to N12 and N22, respectively) whereas the corresponding angles to the inter-ligand equatorial N atoms are greater than 90° (97.77 (8)° and 108.92 (8)°, respectively). The distortion from the ideal geometry is also reflected in the non-lineal axial angle of 153.8 (9)°, which is comparable to the value of 152° observed in the samarium analogue. The presence of the B—H agostic interaction is evident in the short Yb—B2 interatomic distance of 3.002 (3) Å, compared to the much longer Yb—B1 separation of 3.310 (3) Å in the unperturbed ligand. Further, the average Yb—N bond distance in the κ3 ligand is shorter than that in the formally κ2 ligand, 2.52 (2) Å and 2.59 (4) Å, respectively.

Related literature top

For full details of the synthesis and spectroscopic characterization of the title compound, see: Zhang et al. (1995). For the samarium analogue, see: Zhang et al. (1995). For the thulium analogue, see: Cheng et al. (2008). For B—H agostic interactions involving pyrazolylborate ligands, see: Calabrese et al. (1990); Kosky et al. (1971); Cotton et al. (1972).

Experimental top

X-ray quality crystals of the titled compound were obtained via ligand redistribution while attempting to grow crystals of (TptBu,Me)Yb(BH4) from a dilute toluene solution cooled to 233 K over several days.

Refinement top

H atom H2B (attached to B atom B2) was allowed to freely refine; the remaining H atoms were generated in idealized positions (according to the sp2 or sp3 geometries of their parent C or B atoms), and then refined using a riding model with fixed C—H and B—H distances (C—H = 0.95–1.00 Å, B1—H1B = 1.00 Å) and with Uiso(H) = 1.2Ueq(C,B). One of the t-butyl groups is disordered over two sites with initially refined occupancies which were finally fixed at 0.65 and 0.35.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); 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).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound, showing the atom labelling scheme. Non-hydrogen atoms are represented by ellipsoids at the 30% probability level. H atoms attached to B atoms are shown with arbitrarily small radii; the remaining H atoms are not shown for clarity. The disorder and the solvent molecule are not shown.
Bis[tris(3-tert-butyl-5-methylpyrazol-1-yl)hydridoborato]ytterbium(II) toluene solvate top
Crystal data top
[Yb(C24H40BN6)2]·C7H8Z = 2
Mr = 1112.03F(000) = 1164
Triclinic, P1Dx = 1.273 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.8621 (17) ÅCell parameters from 6598 reflections
b = 12.1587 (17) Åθ = 2.2–27.5°
c = 20.650 (3) ŵ = 1.66 mm−1
α = 96.1072 (19)°T = 193 K
β = 96.1001 (18)°Block, yellow
γ = 98.9737 (19)°0.39 × 0.36 × 0.14 mm
V = 2902.1 (7) Å3
Data collection top
Bruker PLATFORM
diffractometer with SMART 1000 CCD area-detector		13091 independent reflections
Radiation source: fine-focus sealed tube11816 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.026
Detector resolution: 8.192 pixels mm-1θmax = 27.6°, θmin = 1.7°
ω scansh = −15→15
Absorption correction: integration
(SHELXTL; Sheldrick, 2008)		k = −15→15
Tmin = 0.564, Tmax = 0.801l = −26→26
24467 measured reflections
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)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H atoms treated by a mixture of independent and constrained refinement
S = 1.10 w = 1/[σ2(Fo2) + (0.0559P)2 + 1.1666P]
where P = (Fo2 + 2Fc2)/3
13091 reflections(Δ/σ)max = 0.001
669 parametersΔρmax = 1.91 e Å−3
0 restraintsΔρmin = −1.74 e Å−3
Crystal data top
[Yb(C24H40BN6)2]·C7H8γ = 98.9737 (19)°
Mr = 1112.03V = 2902.1 (7) Å3
Triclinic, P1Z = 2
a = 11.8621 (17) ÅMo Kα radiation
b = 12.1587 (17) ŵ = 1.66 mm−1
c = 20.650 (3) ÅT = 193 K
α = 96.1072 (19)°0.39 × 0.36 × 0.14 mm
β = 96.1001 (18)°
Data collection top
Bruker PLATFORM
diffractometer with SMART 1000 CCD area-detector		13091 independent reflections
Absorption correction: integration
(SHELXTL; Sheldrick, 2008)		11816 reflections with I > 2σ(I)
Tmin = 0.564, Tmax = 0.801Rint = 0.026
24467 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0350 restraints
wR(F2) = 0.096H atoms treated by a mixture of independent and constrained refinement
S = 1.10Δρmax = 1.91 e Å−3
13091 reflectionsΔρmin = −1.74 e Å−3
669 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*/UeqOcc. (<1)
Yb0.234066 (10)0.515202 (10)0.265241 (5)0.02764 (5)
N110.3907 (2)0.6798 (2)0.38158 (12)0.0297 (5)
N120.2745 (2)0.6378 (2)0.37444 (13)0.0336 (5)
N210.4464 (2)0.4848 (2)0.37392 (12)0.0298 (5)
N220.3382 (2)0.4220 (2)0.35293 (12)0.0284 (5)
N310.5013 (2)0.6172 (2)0.28709 (12)0.0292 (5)
N320.4151 (2)0.6195 (2)0.23690 (12)0.0298 (5)
N410.1149 (2)0.3613 (2)0.14689 (12)0.0285 (5)
N420.2164 (2)0.3423 (2)0.18056 (12)0.0295 (5)
N51−0.0193 (2)0.4987 (2)0.17664 (12)0.0300 (5)
N520.0614 (2)0.5913 (2)0.20427 (12)0.0301 (5)
N61−0.0833 (2)0.2865 (2)0.17723 (12)0.0309 (5)
N62−0.0989 (2)0.2068 (2)0.12360 (12)0.0319 (5)
C130.2270 (3)0.7081 (3)0.41270 (15)0.0358 (7)
C140.3108 (3)0.7970 (3)0.44379 (16)0.0401 (7)
H140.29930.85860.47320.048*
C150.4133 (3)0.7774 (3)0.42319 (14)0.0333 (6)
C160.5295 (3)0.8479 (3)0.43985 (18)0.0443 (8)
H16A0.55230.88120.40100.053*
H16B0.58530.80120.45420.053*
H16C0.52730.90780.47520.053*
C170.1020 (3)0.6831 (3)0.42488 (16)0.0439 (8)
C180.0510 (4)0.7912 (5)0.4291 (2)0.0684 (13)
H18A−0.02980.77430.43650.082*
H18B0.05610.82410.38800.082*
H18C0.09400.84460.46560.082*
C190.0306 (3)0.5959 (5)0.3714 (2)0.0634 (13)
H19A−0.04940.58220.38070.076*
H19B0.06170.52580.37060.076*
H19C0.03360.62390.32870.076*
C200.0994 (3)0.6359 (4)0.49101 (19)0.0540 (10)
H20A0.01970.61980.50050.065*
H20B0.14470.69120.52590.065*
H20C0.13220.56660.48880.065*
C230.3343 (3)0.3281 (3)0.38186 (15)0.0342 (6)
C240.4389 (3)0.3287 (3)0.42021 (17)0.0406 (7)
H240.45870.27170.44520.049*
C250.5073 (3)0.4286 (3)0.41436 (16)0.0365 (7)
C260.6280 (3)0.4703 (3)0.44679 (19)0.0484 (9)
H26A0.64710.42300.48050.058*
H26B0.63430.54790.46710.058*
H26C0.68150.46720.41390.058*
C270.2263 (3)0.2412 (3)0.37726 (17)0.0412 (7)
C28A0.1367 (6)0.2548 (6)0.3271 (3)0.0577 (17)0.65
H28A0.16840.26000.28540.069*0.65
H28B0.10660.32340.33980.069*0.65
H28C0.07450.19000.32210.069*0.65
C29A0.2611 (6)0.1207 (5)0.3635 (4)0.0610 (17)0.65
H29A0.31700.10970.39970.073*0.65
H29B0.29530.11520.32240.073*0.65
H29C0.19240.06300.36000.073*0.65
C30A0.1861 (6)0.2466 (7)0.4457 (3)0.0609 (17)0.65
H30A0.25260.25250.47910.073*0.65
H30B0.13150.17840.44830.073*0.65
H30C0.14860.31230.45320.073*0.65
C28B0.1896 (12)0.1808 (11)0.3063 (6)0.060 (3)0.35
H28D0.19210.23650.27530.072*0.35
H28E0.11110.13890.30290.072*0.35
H28F0.24230.12880.29590.072*0.35
C29B0.2290 (12)0.1627 (12)0.4256 (7)0.067 (4)0.35
H29D0.15620.10980.41920.080*0.35
H29E0.24000.20400.46980.080*0.35
H29F0.29270.12120.42030.080*0.35
C30B0.1189 (10)0.3114 (11)0.3882 (7)0.057 (3)0.35
H30D0.12090.37040.35940.069*0.35
H30E0.12710.34530.43410.069*0.35
H30F0.04550.25970.37780.069*0.35
C330.4685 (3)0.6383 (3)0.18325 (15)0.0335 (6)
C340.5866 (3)0.6460 (3)0.19885 (16)0.0397 (7)
H340.64340.65810.17000.048*
C350.6052 (3)0.6327 (3)0.26406 (16)0.0354 (7)
C360.7174 (3)0.6337 (4)0.3053 (2)0.0513 (9)
H36A0.71640.56160.32260.062*
H36B0.72870.69430.34190.062*
H36C0.78040.64580.27840.062*
C370.4057 (3)0.6577 (3)0.11836 (16)0.0392 (7)
C380.2797 (3)0.6037 (3)0.10966 (16)0.0425 (8)
H38A0.24250.61720.06720.051*
H38B0.24160.63630.14510.051*
H38C0.27380.52270.11110.051*
C390.4161 (4)0.7848 (4)0.1163 (2)0.0567 (10)
H39A0.37710.79880.07450.068*
H39B0.49750.81870.12060.068*
H39C0.38030.81810.15260.068*
C400.4633 (4)0.6068 (5)0.06140 (19)0.0675 (13)
H40A0.42340.61920.01950.081*
H40B0.45920.52600.06310.081*
H40C0.54410.64280.06550.081*
C430.2782 (3)0.3039 (3)0.13496 (15)0.0323 (6)
C440.2174 (3)0.2991 (3)0.07203 (15)0.0361 (7)
H440.24170.27490.03130.043*
C450.1162 (3)0.3364 (3)0.08108 (14)0.0330 (6)
C460.0227 (3)0.3551 (3)0.03069 (16)0.0435 (8)
H46A−0.04430.29590.02890.052*
H46B0.05040.3532−0.01240.052*
H46C0.00080.42830.04260.052*
C470.3911 (3)0.2634 (3)0.15263 (16)0.0367 (7)
C480.3633 (4)0.1369 (3)0.1577 (2)0.0541 (9)
H48A0.43480.10850.16920.065*
H48B0.32460.09730.11550.065*
H48C0.31280.12430.19180.065*
C490.4683 (4)0.2803 (4)0.0987 (2)0.0608 (11)
H49A0.54060.25360.11050.073*
H49B0.48460.36030.09360.073*
H49C0.42920.23790.05720.073*
C500.4547 (3)0.3237 (4)0.2175 (2)0.0537 (10)
H50A0.52670.29520.22710.064*
H50B0.40660.31030.25260.064*
H50C0.47170.40440.21470.064*
C530.0184 (3)0.6813 (3)0.18775 (14)0.0317 (6)
C54−0.0897 (3)0.6475 (3)0.15046 (16)0.0367 (7)
H54−0.13860.69490.13300.044*
C55−0.1110 (3)0.5320 (3)0.14419 (15)0.0342 (6)
C56−0.2151 (3)0.4535 (3)0.1098 (2)0.0494 (9)
H56A−0.26520.42850.14210.059*
H56B−0.19130.38830.08630.059*
H56C−0.25710.49230.07840.059*
C570.0799 (3)0.8017 (3)0.20749 (16)0.0386 (7)
C580.1913 (3)0.8086 (3)0.25287 (19)0.0451 (8)
H58A0.22570.88750.26620.054*
H58B0.24500.77030.22980.054*
H58C0.17490.77240.29180.054*
C590.1047 (4)0.8533 (3)0.1446 (2)0.0529 (9)
H59A0.14280.93150.15620.063*
H59B0.03220.85060.11640.063*
H59C0.15490.81070.12120.063*
C60−0.0021 (4)0.8676 (3)0.2430 (2)0.0559 (10)
H60A0.03670.94490.25760.067*
H60B−0.02360.83140.28120.067*
H60C−0.07150.86830.21280.067*
C63−0.1930 (3)0.1361 (3)0.12911 (15)0.0326 (6)
C64−0.2405 (3)0.1687 (3)0.18675 (16)0.0383 (7)
H64−0.30750.13190.20190.046*
C65−0.1688 (3)0.2649 (3)0.21601 (15)0.0361 (7)
C66−0.1746 (3)0.3395 (3)0.27764 (19)0.0511 (9)
H66A−0.16730.41760.26850.061*
H66B−0.11180.33240.31100.061*
H66C−0.24860.31750.29380.061*
C67−0.2372 (3)0.0362 (3)0.07715 (16)0.0371 (7)
C68−0.2400 (5)−0.0718 (4)0.1088 (3)0.0722 (14)
H68A−0.2658−0.13650.07510.087*
H68B−0.2933−0.07280.14200.087*
H68C−0.1627−0.07540.12970.087*
C69−0.3593 (5)0.0404 (5)0.0492 (3)0.0818 (17)
H69A−0.3879−0.02520.01640.098*
H69B−0.36100.10900.02840.098*
H69C−0.40820.04010.08450.098*
C70−0.1604 (5)0.0318 (5)0.0236 (3)0.095 (2)
H70A−0.1889−0.0355−0.00790.114*
H70B−0.08190.02920.04280.114*
H70C−0.16060.09870.00100.114*
B10.4809 (3)0.6082 (3)0.35989 (16)0.0293 (6)
H1B0.55550.63970.38780.035*
B20.0173 (3)0.3843 (3)0.18781 (16)0.0279 (6)
H2B0.062 (3)0.396 (3)0.2413 (17)0.032 (9)*
C1S0.7433 (4)0.0308 (4)0.3474 (2)0.0631 (11)
C2S0.6933 (5)−0.0606 (4)0.3026 (2)0.0618 (11)
H2S0.7379−0.11560.28950.074*
C3S0.5813 (5)−0.0732 (4)0.2769 (2)0.0708 (13)
H3S0.5484−0.13820.24720.085*
C4S0.5155 (5)0.0042 (5)0.2924 (3)0.0787 (15)
H4S0.4373−0.00590.27370.094*
C5S0.5635 (6)0.0986 (5)0.3358 (3)0.0779 (15)
H5S0.51900.15500.34620.093*
C6S0.6761 (5)0.1104 (4)0.3640 (2)0.0647 (12)
H6S0.70800.17390.39510.078*
C7S0.8648 (6)0.0440 (7)0.3760 (4)0.127 (3)
H7SA0.91020.01640.34270.152*
H7SB0.87060.00080.41340.152*
H7SC0.89450.12340.39100.152*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Yb0.02238 (7)0.03397 (8)0.02434 (7)0.00150 (5)0.00309 (4)−0.00177 (5)
N110.0299 (13)0.0335 (13)0.0243 (11)0.0036 (10)0.0042 (9)−0.0006 (9)
N120.0279 (13)0.0408 (14)0.0299 (12)0.0057 (11)0.0026 (10)−0.0037 (10)
N210.0264 (12)0.0340 (13)0.0278 (11)0.0037 (10)0.0033 (9)0.0014 (9)
N220.0244 (12)0.0296 (12)0.0301 (12)0.0008 (10)0.0056 (9)0.0018 (9)
N310.0242 (12)0.0309 (12)0.0322 (12)0.0033 (10)0.0074 (9)0.0006 (10)
N320.0285 (13)0.0329 (12)0.0267 (11)0.0003 (10)0.0068 (9)0.0017 (9)
N410.0249 (12)0.0331 (13)0.0263 (11)0.0007 (10)0.0052 (9)0.0020 (9)
N420.0250 (12)0.0337 (13)0.0279 (12)0.0019 (10)0.0049 (9)−0.0020 (9)
N510.0245 (12)0.0345 (13)0.0289 (12)0.0012 (10)0.0028 (9)0.0006 (10)
N520.0253 (12)0.0344 (13)0.0283 (12)0.0006 (10)0.0035 (9)0.0001 (10)
N610.0268 (12)0.0333 (13)0.0305 (12)−0.0014 (10)0.0082 (10)−0.0002 (10)
N620.0287 (13)0.0346 (13)0.0301 (12)0.0002 (10)0.0052 (10)−0.0004 (10)
C130.0384 (17)0.0443 (17)0.0261 (14)0.0124 (14)0.0073 (12)−0.0013 (12)
C140.049 (2)0.0404 (17)0.0315 (15)0.0105 (15)0.0098 (14)−0.0035 (13)
C150.0418 (17)0.0312 (15)0.0255 (13)0.0026 (13)0.0060 (12)0.0008 (11)
C160.050 (2)0.0354 (17)0.0430 (18)−0.0054 (15)0.0078 (15)0.0014 (14)
C170.0340 (17)0.065 (2)0.0340 (16)0.0173 (16)0.0083 (13)−0.0032 (15)
C180.066 (3)0.091 (4)0.061 (3)0.044 (3)0.021 (2)0.007 (2)
C190.0305 (19)0.103 (4)0.049 (2)0.006 (2)0.0065 (16)−0.018 (2)
C200.039 (2)0.079 (3)0.0436 (19)0.0042 (19)0.0140 (15)0.0048 (18)
C230.0369 (17)0.0362 (16)0.0296 (14)0.0042 (13)0.0078 (12)0.0040 (12)
C240.0408 (18)0.0419 (18)0.0413 (17)0.0073 (15)0.0069 (14)0.0127 (14)
C250.0342 (16)0.0413 (17)0.0353 (15)0.0083 (13)0.0048 (12)0.0078 (13)
C260.0354 (18)0.060 (2)0.050 (2)0.0091 (16)−0.0050 (15)0.0159 (17)
C270.0426 (19)0.0380 (17)0.0414 (17)−0.0034 (14)0.0114 (14)0.0062 (14)
C28A0.043 (3)0.067 (4)0.060 (4)−0.008 (3)−0.003 (3)0.029 (3)
C29A0.059 (4)0.041 (3)0.080 (5)−0.002 (3)0.011 (3)0.006 (3)
C30A0.047 (4)0.081 (5)0.052 (4)−0.004 (3)0.017 (3)0.010 (3)
C28B0.064 (8)0.052 (7)0.053 (7)−0.017 (6)0.015 (6)−0.011 (5)
C29B0.058 (8)0.069 (8)0.076 (9)−0.005 (7)0.005 (6)0.044 (7)
C30B0.036 (6)0.061 (7)0.077 (8)0.000 (5)0.026 (5)0.013 (6)
C330.0346 (16)0.0337 (15)0.0324 (15)0.0019 (13)0.0130 (12)0.0025 (12)
C340.0338 (17)0.0471 (19)0.0416 (17)0.0067 (14)0.0182 (13)0.0070 (14)
C350.0268 (15)0.0380 (16)0.0433 (17)0.0059 (13)0.0123 (12)0.0051 (13)
C360.0289 (17)0.074 (3)0.056 (2)0.0133 (17)0.0111 (15)0.0164 (19)
C370.0399 (18)0.0473 (19)0.0309 (15)0.0016 (15)0.0126 (13)0.0071 (13)
C380.0418 (19)0.0481 (19)0.0341 (16)−0.0036 (15)0.0053 (13)0.0051 (14)
C390.056 (2)0.056 (2)0.055 (2)−0.0096 (19)0.0012 (18)0.0247 (19)
C400.068 (3)0.102 (4)0.0349 (19)0.015 (3)0.0226 (19)0.003 (2)
C430.0302 (15)0.0312 (15)0.0342 (15)0.0013 (12)0.0105 (12)−0.0025 (12)
C440.0397 (18)0.0398 (17)0.0275 (14)0.0008 (14)0.0129 (12)−0.0020 (12)
C450.0352 (16)0.0345 (15)0.0263 (14)−0.0024 (13)0.0061 (11)0.0003 (11)
C460.0418 (19)0.058 (2)0.0295 (15)0.0031 (16)0.0039 (13)0.0105 (14)
C470.0334 (16)0.0365 (16)0.0417 (17)0.0095 (13)0.0125 (13)−0.0011 (13)
C480.053 (2)0.044 (2)0.065 (2)0.0124 (18)0.0056 (19)0.0027 (18)
C490.052 (2)0.077 (3)0.066 (3)0.028 (2)0.031 (2)0.018 (2)
C500.039 (2)0.057 (2)0.062 (2)0.0197 (17)−0.0040 (17)−0.0149 (18)
C530.0311 (15)0.0350 (15)0.0299 (14)0.0064 (12)0.0079 (11)0.0033 (11)
C540.0319 (16)0.0436 (17)0.0360 (16)0.0089 (14)0.0037 (12)0.0079 (13)
C550.0281 (15)0.0418 (17)0.0318 (14)0.0040 (13)0.0030 (11)0.0043 (12)
C560.0313 (18)0.052 (2)0.059 (2)0.0008 (15)−0.0073 (15)0.0017 (17)
C570.0404 (18)0.0342 (16)0.0398 (17)0.0049 (14)0.0038 (13)0.0025 (13)
C580.043 (2)0.0371 (17)0.050 (2)−0.0020 (15)0.0014 (15)0.0002 (15)
C590.056 (2)0.045 (2)0.057 (2)−0.0010 (18)0.0055 (18)0.0184 (17)
C600.060 (3)0.045 (2)0.062 (2)0.0214 (19)0.0019 (19)−0.0054 (18)
C630.0286 (15)0.0330 (15)0.0343 (15)0.0008 (12)0.0048 (11)0.0017 (12)
C640.0319 (16)0.0410 (17)0.0400 (17)−0.0028 (13)0.0120 (13)0.0015 (13)
C650.0297 (15)0.0424 (17)0.0350 (15)0.0005 (13)0.0107 (12)0.0009 (13)
C660.046 (2)0.055 (2)0.047 (2)−0.0077 (17)0.0220 (16)−0.0111 (16)
C670.0352 (17)0.0351 (16)0.0370 (16)0.0002 (13)0.0022 (13)−0.0022 (13)
C680.102 (4)0.042 (2)0.068 (3)0.007 (2)0.004 (3)0.001 (2)
C690.073 (3)0.072 (3)0.085 (4)0.023 (3)−0.037 (3)−0.028 (3)
C700.097 (4)0.087 (4)0.079 (3)−0.042 (3)0.050 (3)−0.043 (3)
B10.0228 (15)0.0347 (17)0.0286 (15)0.0042 (13)0.0009 (12)−0.0007 (12)
B20.0230 (15)0.0314 (16)0.0275 (15)−0.0013 (12)0.0051 (12)0.0018 (12)
C1S0.065 (3)0.060 (3)0.061 (3)−0.002 (2)0.021 (2)0.002 (2)
C2S0.078 (3)0.052 (2)0.056 (2)0.007 (2)0.023 (2)0.0016 (19)
C3S0.093 (4)0.062 (3)0.053 (3)0.006 (3)0.004 (2)0.003 (2)
C4S0.082 (4)0.079 (4)0.073 (3)0.015 (3)−0.006 (3)0.018 (3)
C5S0.096 (4)0.062 (3)0.085 (4)0.024 (3)0.030 (3)0.016 (3)
C6S0.083 (3)0.052 (2)0.054 (2)−0.008 (2)0.023 (2)−0.0041 (19)
C7S0.070 (4)0.127 (6)0.163 (8)−0.017 (4)0.024 (4)−0.034 (5)
Geometric parameters (Å, º) top
Yb—N322.477 (3)C36—H36C0.9800
Yb—N122.524 (3)C37—C381.519 (5)
Yb—N222.547 (2)C37—C391.537 (5)
Yb—N422.555 (2)C37—C401.544 (5)
Yb—N522.632 (3)C38—H38A0.9800
Yb—N412.990 (2)C38—H38B0.9800
Yb—H2B2.29 (4)C38—H38C0.9800
N11—C151.362 (4)C39—H39A0.9800
N11—N121.380 (4)C39—H39B0.9800
N11—B11.554 (4)C39—H39C0.9800
N12—C131.332 (4)C40—H40A0.9800
N21—C251.354 (4)C40—H40B0.9800
N21—N221.387 (3)C40—H40C0.9800
N21—B11.558 (4)C43—C441.408 (4)
N22—C231.341 (4)C43—C471.520 (5)
N31—C351.361 (4)C44—C451.372 (5)
N31—N321.382 (4)C44—H440.9500
N31—B11.560 (4)C45—C461.500 (5)
N32—C331.356 (4)C46—H46A0.9800
N41—C451.363 (4)C46—H46B0.9800
N41—N421.390 (3)C46—H46C0.9800
N41—B21.546 (4)C47—C501.518 (5)
N42—C431.342 (4)C47—C491.526 (5)
N51—C551.355 (4)C47—C481.540 (5)
N51—N521.385 (3)C48—H48A0.9800
N51—B21.553 (4)C48—H48B0.9800
N52—C531.338 (4)C48—H48C0.9800
N61—C651.368 (4)C49—H49A0.9800
N61—N621.369 (3)C49—H49B0.9800
N61—B21.527 (4)C49—H49C0.9800
N62—C631.321 (4)C50—H50A0.9800
C13—C141.396 (5)C50—H50B0.9800
C13—C171.519 (5)C50—H50C0.9800
C14—C151.377 (5)C53—C541.401 (4)
C14—H140.9500C53—C571.523 (4)
C15—C161.490 (5)C54—C551.378 (5)
C16—H16A0.9800C54—H540.9500
C16—H16B0.9800C55—C561.498 (5)
C16—H16C0.9800C56—H56A0.9800
C17—C191.527 (5)C56—H56B0.9800
C17—C181.528 (6)C56—H56C0.9800
C17—C201.538 (5)C57—C581.522 (5)
C18—H18A0.9800C57—C591.537 (5)
C18—H18B0.9800C57—C601.548 (5)
C18—H18C0.9800C58—H58A0.9800
C19—H19A0.9800C58—H58B0.9800
C19—H19B0.9800C58—H58C0.9800
C19—H19C0.9800C59—H59A0.9800
C20—H20A0.9800C59—H59B0.9800
C20—H20B0.9800C59—H59C0.9800
C20—H20C0.9800C60—H60A0.9800
C23—C241.397 (5)C60—H60B0.9800
C23—C271.516 (5)C60—H60C0.9800
C24—C251.377 (5)C63—C641.415 (4)
C24—H240.9500C63—C671.519 (4)
C25—C261.501 (5)C64—C651.374 (5)
C26—H26A0.9800C64—H640.9500
C26—H26B0.9800C65—C661.497 (5)
C26—H26C0.9800C66—H66A0.9800
C27—C28A1.444 (7)C66—H66B0.9800
C27—C29B1.454 (11)C66—H66C0.9800
C27—C30A1.536 (7)C67—C701.508 (6)
C27—C28B1.554 (12)C67—C691.512 (6)
C27—C29A1.588 (7)C67—C681.525 (6)
C27—C30B1.661 (13)C68—H68A0.9800
C28A—H28A0.9800C68—H68B0.9800
C28A—H28B0.9800C68—H68C0.9800
C28A—H28C0.9800C69—H69A0.9800
C29A—H29A0.9800C69—H69B0.9800
C29A—H29B0.9800C69—H69C0.9800
C29A—H29C0.9800C70—H70A0.9800
C30A—H30A0.9800C70—H70B0.9800
C30A—H30B0.9800C70—H70C0.9800
C30A—H30C0.9800B1—H1B1.0000
C28B—H28D0.9800B2—H2B1.16 (3)
C28B—H28E0.9800C1S—C2S1.380 (6)
C28B—H28F0.9800C1S—C6S1.386 (7)
C29B—H29D0.9800C1S—C7S1.476 (9)
C29B—H29E0.9800C2S—C3S1.356 (7)
C29B—H29F0.9800C2S—H2S0.9500
C30B—H30D0.9800C3S—C4S1.347 (8)
C30B—H30E0.9800C3S—H3S0.9500
C30B—H30F0.9800C4S—C5S1.384 (8)
C33—C341.391 (5)C4S—H4S0.9500
C33—C371.522 (5)C5S—C6S1.378 (8)
C34—C351.372 (5)C5S—H5S0.9500
C34—H340.9500C6S—H6S0.9500
C35—C361.500 (5)C7S—H7SA0.9800
C36—H36A0.9800C7S—H7SB0.9800
C36—H36B0.9800C7S—H7SC0.9800
N32—Yb—N1287.15 (8)C35—C36—H36C109.5
N32—Yb—N2293.28 (8)H36A—C36—H36C109.5
N12—Yb—N2268.27 (8)H36B—C36—H36C109.5
N32—Yb—N4297.77 (8)C38—C37—C33111.9 (3)
N12—Yb—N42159.83 (9)C38—C37—C39110.0 (3)
N22—Yb—N4291.85 (8)C33—C37—C39108.5 (3)
N32—Yb—N52107.92 (8)C38—C37—C40108.6 (3)
N12—Yb—N52103.07 (8)C33—C37—C40109.1 (3)
N22—Yb—N52156.96 (8)C39—C37—C40108.8 (3)
N42—Yb—N5294.05 (8)C37—C38—H38A109.5
N32—Yb—N41108.81 (7)C37—C38—H38B109.5
N12—Yb—N41162.84 (8)H38A—C38—H38B109.5
N22—Yb—N41115.54 (7)C37—C38—H38C109.5
N42—Yb—N4127.63 (7)H38A—C38—H38C109.5
N52—Yb—N4166.66 (7)H38B—C38—H38C109.5
N32—Yb—H2B153.8 (9)C37—C39—H39A109.5
N12—Yb—H2B118.2 (9)C37—C39—H39B109.5
N22—Yb—H2B101.8 (9)H39A—C39—H39B109.5
N42—Yb—H2B60.9 (9)C37—C39—H39C109.5
N52—Yb—H2B62.5 (9)H39A—C39—H39C109.5
N41—Yb—H2B45.3 (9)H39B—C39—H39C109.5
C15—N11—N12109.6 (2)C37—C40—H40A109.5
C15—N11—B1125.9 (3)C37—C40—H40B109.5
N12—N11—B1122.6 (2)H40A—C40—H40B109.5
C13—N12—N11106.7 (3)C37—C40—H40C109.5
C13—N12—Yb141.1 (2)H40A—C40—H40C109.5
N11—N12—Yb105.18 (17)H40B—C40—H40C109.5
C25—N21—N22109.8 (3)N42—C43—C44109.6 (3)
C25—N21—B1126.8 (3)N42—C43—C47122.5 (3)
N22—N21—B1122.8 (2)C44—C43—C47127.7 (3)
C23—N22—N21106.0 (2)C45—C44—C43106.5 (3)
C23—N22—Yb143.8 (2)C45—C44—H44126.7
N21—N22—Yb109.61 (17)C43—C44—H44126.7
C35—N31—N32109.6 (2)N41—C45—C44107.8 (3)
C35—N31—B1126.1 (3)N41—C45—C46123.1 (3)
N32—N31—B1124.2 (2)C44—C45—C46129.1 (3)
C33—N32—N31106.1 (2)C45—C46—H46A109.5
C33—N32—Yb139.4 (2)C45—C46—H46B109.5
N31—N32—Yb107.80 (17)H46A—C46—H46B109.5
C45—N41—N42109.6 (2)C45—C46—H46C109.5
C45—N41—B2131.9 (3)H46A—C46—H46C109.5
N42—N41—B2117.4 (2)H46B—C46—H46C109.5
C45—N41—Yb143.00 (19)C50—C47—C43112.0 (3)
N42—N41—Yb58.48 (13)C50—C47—C49109.3 (3)
B2—N41—Yb75.48 (15)C43—C47—C49110.3 (3)
C43—N42—N41106.5 (2)C50—C47—C48109.2 (3)
C43—N42—Yb137.2 (2)C43—C47—C48107.7 (3)
N41—N42—Yb93.89 (16)C49—C47—C48108.3 (3)
C55—N51—N52110.2 (3)C47—C48—H48A109.5
C55—N51—B2135.6 (3)C47—C48—H48B109.5
N52—N51—B2114.2 (2)H48A—C48—H48B109.5
C53—N52—N51106.1 (2)C47—C48—H48C109.5
C53—N52—Yb146.8 (2)H48A—C48—H48C109.5
N51—N52—Yb107.03 (17)H48B—C48—H48C109.5
C65—N61—N62110.6 (2)C47—C49—H49A109.5
C65—N61—B2127.9 (3)C47—C49—H49B109.5
N62—N61—B2121.5 (2)H49A—C49—H49B109.5
C63—N62—N61106.1 (2)C47—C49—H49C109.5
N12—C13—C14110.1 (3)H49A—C49—H49C109.5
N12—C13—C17122.5 (3)H49B—C49—H49C109.5
C14—C13—C17127.0 (3)C47—C50—H50A109.5
C15—C14—C13106.2 (3)C47—C50—H50B109.5
C15—C14—H14126.9H50A—C50—H50B109.5
C13—C14—H14126.9C47—C50—H50C109.5
N11—C15—C14107.4 (3)H50A—C50—H50C109.5
N11—C15—C16124.0 (3)H50B—C50—H50C109.5
C14—C15—C16128.6 (3)N52—C53—C54110.0 (3)
C15—C16—H16A109.5N52—C53—C57123.9 (3)
C15—C16—H16B109.5C54—C53—C57126.1 (3)
H16A—C16—H16B109.5C55—C54—C53106.4 (3)
C15—C16—H16C109.5C55—C54—H54126.8
H16A—C16—H16C109.5C53—C54—H54126.8
H16B—C16—H16C109.5N51—C55—C54107.3 (3)
C13—C17—C19111.7 (3)N51—C55—C56124.3 (3)
C13—C17—C18109.9 (4)C54—C55—C56128.4 (3)
C19—C17—C18110.1 (4)C55—C56—H56A109.5
C13—C17—C20107.6 (3)C55—C56—H56B109.5
C19—C17—C20108.6 (4)H56A—C56—H56B109.5
C18—C17—C20108.9 (3)C55—C56—H56C109.5
C17—C18—H18A109.5H56A—C56—H56C109.5
C17—C18—H18B109.5H56B—C56—H56C109.5
H18A—C18—H18B109.5C58—C57—C53112.2 (3)
C17—C18—H18C109.5C58—C57—C59110.2 (3)
H18A—C18—H18C109.5C53—C57—C59108.1 (3)
H18B—C18—H18C109.5C58—C57—C60109.2 (3)
C17—C19—H19A109.5C53—C57—C60108.0 (3)
C17—C19—H19B109.5C59—C57—C60109.0 (3)
H19A—C19—H19B109.5C57—C58—H58A109.5
C17—C19—H19C109.5C57—C58—H58B109.5
H19A—C19—H19C109.5H58A—C58—H58B109.5
H19B—C19—H19C109.5C57—C58—H58C109.5
C17—C20—H20A109.5H58A—C58—H58C109.5
C17—C20—H20B109.5H58B—C58—H58C109.5
H20A—C20—H20B109.5C57—C59—H59A109.5
C17—C20—H20C109.5C57—C59—H59B109.5
H20A—C20—H20C109.5H59A—C59—H59B109.5
H20B—C20—H20C109.5C57—C59—H59C109.5
N22—C23—C24110.3 (3)H59A—C59—H59C109.5
N22—C23—C27123.0 (3)H59B—C59—H59C109.5
C24—C23—C27126.4 (3)C57—C60—H60A109.5
C25—C24—C23106.0 (3)C57—C60—H60B109.5
C25—C24—H24127.0H60A—C60—H60B109.5
C23—C24—H24127.0C57—C60—H60C109.5
N21—C25—C24107.9 (3)H60A—C60—H60C109.5
N21—C25—C26125.1 (3)H60B—C60—H60C109.5
C24—C25—C26127.0 (3)N62—C63—C64111.0 (3)
C25—C26—H26A109.5N62—C63—C67120.6 (3)
C25—C26—H26B109.5C64—C63—C67128.4 (3)
H26A—C26—H26B109.5C65—C64—C63105.1 (3)
C25—C26—H26C109.5C65—C64—H64127.4
H26A—C26—H26C109.5C63—C64—H64127.4
H26B—C26—H26C109.5N61—C65—C64107.2 (3)
C28A—C27—C29B131.5 (7)N61—C65—C66122.2 (3)
C28A—C27—C23113.6 (4)C64—C65—C66130.5 (3)
C29B—C27—C23114.8 (6)C65—C66—H66A109.5
C28A—C27—C30A112.1 (5)C65—C66—H66B109.5
C29B—C27—C30A49.8 (7)H66A—C66—H66B109.5
C23—C27—C30A107.2 (4)C65—C66—H66C109.5
C28A—C27—C28B48.7 (6)H66A—C66—H66C109.5
C29B—C27—C28B112.3 (9)H66B—C66—H66C109.5
C23—C27—C28B111.9 (5)C70—C67—C69110.9 (4)
C30A—C27—C28B140.8 (6)C70—C67—C63111.4 (3)
C28A—C27—C29A110.0 (5)C69—C67—C63109.9 (3)
C29B—C27—C29A56.3 (7)C70—C67—C68108.1 (4)
C23—C27—C29A107.9 (4)C69—C67—C68107.1 (4)
C30A—C27—C29A105.7 (5)C63—C67—C68109.3 (3)
C28B—C27—C29A64.5 (6)C67—C68—H68A109.5
C28A—C27—C30B54.1 (6)C67—C68—H68B109.5
C29B—C27—C30B108.3 (8)H68A—C68—H68B109.5
C23—C27—C30B106.7 (5)C67—C68—H68C109.5
C30A—C27—C30B63.7 (6)H68A—C68—H68C109.5
C28B—C27—C30B101.9 (8)H68B—C68—H68C109.5
C29A—C27—C30B145.4 (6)C67—C69—H69A109.5
C27—C28A—H28A109.5C67—C69—H69B109.5
C27—C28A—H28B109.5H69A—C69—H69B109.5
H28A—C28A—H28B109.5C67—C69—H69C109.5
C27—C28A—H28C109.5H69A—C69—H69C109.5
H28A—C28A—H28C109.5H69B—C69—H69C109.5
H28B—C28A—H28C109.5C67—C70—H70A109.5
C27—C29A—H29A109.5C67—C70—H70B109.5
C27—C29A—H29B109.5H70A—C70—H70B109.5
H29A—C29A—H29B109.5C67—C70—H70C109.5
C27—C29A—H29C109.5H70A—C70—H70C109.5
H29A—C29A—H29C109.5H70B—C70—H70C109.5
H29B—C29A—H29C109.5N11—B1—N21110.2 (2)
C27—C30A—H30A109.5N11—B1—N31111.8 (2)
C27—C30A—H30B109.5N21—B1—N31113.0 (2)
H30A—C30A—H30B109.5N11—B1—H1B107.2
C27—C30A—H30C109.5N21—B1—H1B107.2
H30A—C30A—H30C109.5N31—B1—H1B107.2
H30B—C30A—H30C109.5N61—B2—N41112.3 (2)
C27—C28B—H28D109.5N61—B2—N51113.5 (2)
C27—C28B—H28E109.5N41—B2—N51110.9 (2)
H28D—C28B—H28E109.5N61—B2—H2B110.7 (18)
C27—C28B—H28F109.5N41—B2—H2B103.3 (18)
H28D—C28B—H28F109.5N51—B2—H2B105.5 (17)
H28E—C28B—H28F109.5C2S—C1S—C6S117.7 (5)
C27—C29B—H29D109.5C2S—C1S—C7S121.1 (5)
C27—C29B—H29E109.5C6S—C1S—C7S121.2 (5)
H29D—C29B—H29E109.5C3S—C2S—C1S121.0 (5)
C27—C29B—H29F109.5C3S—C2S—H2S119.5
H29D—C29B—H29F109.5C1S—C2S—H2S119.5
H29E—C29B—H29F109.5C4S—C3S—C2S121.7 (5)
C27—C30B—H30D109.5C4S—C3S—H3S119.2
C27—C30B—H30E109.5C2S—C3S—H3S119.2
H30D—C30B—H30E109.5C3S—C4S—C5S119.0 (5)
C27—C30B—H30F109.5C3S—C4S—H4S120.5
H30D—C30B—H30F109.5C5S—C4S—H4S120.5
H30E—C30B—H30F109.5C6S—C5S—C4S119.8 (5)
N32—C33—C34109.8 (3)C6S—C5S—H5S120.1
N32—C33—C37123.3 (3)C4S—C5S—H5S120.1
C34—C33—C37126.7 (3)C5S—C6S—C1S120.7 (5)
C35—C34—C33106.5 (3)C5S—C6S—H6S119.7
C35—C34—H34126.7C1S—C6S—H6S119.7
C33—C34—H34126.7C1S—C7S—H7SA109.5
N31—C35—C34108.0 (3)C1S—C7S—H7SB109.5
N31—C35—C36123.8 (3)H7SA—C7S—H7SB109.5
C34—C35—C36128.3 (3)C1S—C7S—H7SC109.5
C35—C36—H36A109.5H7SA—C7S—H7SC109.5
C35—C36—H36B109.5H7SB—C7S—H7SC109.5
H36A—C36—H36B109.5
C15—N11—N12—C13−1.4 (3)C24—C23—C27—C28A−172.3 (5)
B1—N11—N12—C13163.8 (3)N22—C23—C27—C29B−163.5 (8)
C15—N11—N12—Yb155.98 (19)C24—C23—C27—C29B10.3 (9)
B1—N11—N12—Yb−38.8 (3)N22—C23—C27—C30A−110.5 (5)
N32—Yb—N12—C13124.1 (4)C24—C23—C27—C30A63.3 (5)
N22—Yb—N12—C13−141.2 (4)N22—C23—C27—C28B67.0 (7)
N42—Yb—N12—C13−131.0 (4)C24—C23—C27—C28B−119.2 (7)
N52—Yb—N12—C1316.4 (4)N22—C23—C27—C29A136.1 (4)
N41—Yb—N12—C13−34.8 (6)C24—C23—C27—C29A−50.1 (5)
N32—Yb—N12—N11−19.97 (19)N22—C23—C27—C30B−43.6 (6)
N22—Yb—N12—N1174.70 (18)C24—C23—C27—C30B130.2 (6)
N42—Yb—N12—N1184.9 (3)N31—N32—C33—C340.9 (3)
N52—Yb—N12—N11−127.71 (18)Yb—N32—C33—C34−144.7 (3)
N41—Yb—N12—N11−178.9 (2)N31—N32—C33—C37−174.2 (3)
C25—N21—N22—C230.7 (3)Yb—N32—C33—C3740.2 (5)
B1—N21—N22—C23−171.0 (3)N32—C33—C34—C35−0.7 (4)
C25—N21—N22—Yb−172.4 (2)C37—C33—C34—C35174.2 (3)
B1—N21—N22—Yb15.9 (3)N32—N31—C35—C340.5 (4)
N32—Yb—N22—C23−146.8 (3)B1—N31—C35—C34−174.7 (3)
N12—Yb—N22—C23127.6 (4)N32—N31—C35—C36−179.3 (3)
N42—Yb—N22—C23−48.9 (3)B1—N31—C35—C365.5 (5)
N52—Yb—N22—C2355.9 (4)C33—C34—C35—N310.1 (4)
N41—Yb—N22—C23−34.2 (4)C33—C34—C35—C36179.8 (4)
N32—Yb—N22—N2121.95 (18)N32—C33—C37—C38−25.9 (4)
N12—Yb—N22—N21−63.67 (17)C34—C33—C37—C38159.9 (3)
N42—Yb—N22—N21119.84 (17)N32—C33—C37—C3995.5 (4)
N52—Yb—N22—N21−135.3 (2)C34—C33—C37—C39−78.7 (4)
N41—Yb—N22—N21134.62 (16)N32—C33—C37—C40−146.1 (3)
C35—N31—N32—C33−0.9 (3)C34—C33—C37—C4039.7 (5)
B1—N31—N32—C33174.5 (3)N41—N42—C43—C440.5 (3)
C35—N31—N32—Yb156.5 (2)Yb—N42—C43—C44−114.5 (3)
B1—N31—N32—Yb−28.2 (3)N41—N42—C43—C47−174.5 (3)
N12—Yb—N32—C33−162.7 (3)Yb—N42—C43—C4770.4 (4)
N22—Yb—N32—C33129.3 (3)N42—C43—C44—C450.2 (4)
N42—Yb—N32—C3336.9 (3)C47—C43—C44—C45174.9 (3)
N52—Yb—N32—C33−59.9 (3)N42—N41—C45—C441.2 (3)
N41—Yb—N32—C3310.9 (3)B2—N41—C45—C44−166.4 (3)
N12—Yb—N32—N3152.01 (18)Yb—N41—C45—C4464.5 (4)
N22—Yb—N32—N31−16.02 (18)N42—N41—C45—C46−175.9 (3)
N42—Yb—N32—N31−108.34 (17)B2—N41—C45—C4616.6 (5)
N52—Yb—N32—N31154.82 (16)Yb—N41—C45—C46−112.5 (4)
N41—Yb—N32—N31−134.43 (16)C43—C44—C45—N41−0.8 (4)
N32—Yb—N41—C45−10.9 (4)C43—C44—C45—C46176.0 (3)
N12—Yb—N41—C45146.8 (3)N42—C43—C47—C50−30.1 (5)
N22—Yb—N41—C45−114.2 (3)C44—C43—C47—C50155.9 (3)
N42—Yb—N41—C45−80.8 (4)N42—C43—C47—C49−152.0 (3)
N52—Yb—N41—C4591.1 (3)C44—C43—C47—C4934.0 (5)
N32—Yb—N41—N4269.95 (17)N42—C43—C47—C4890.0 (4)
N12—Yb—N41—N42−132.3 (3)C44—C43—C47—C48−84.1 (4)
N22—Yb—N41—N42−33.33 (17)N51—N52—C53—C540.7 (3)
N52—Yb—N41—N42171.90 (17)Yb—N52—C53—C54179.5 (3)
N32—Yb—N41—B2−154.31 (16)N51—N52—C53—C57−179.4 (3)
N12—Yb—N41—B23.4 (3)Yb—N52—C53—C57−0.7 (5)
N22—Yb—N41—B2102.41 (17)N52—C53—C54—C55−0.5 (4)
N42—Yb—N41—B2135.7 (2)C57—C53—C54—C55179.6 (3)
N52—Yb—N41—B2−52.36 (16)N52—N51—C55—C540.3 (3)
C45—N41—N42—C43−1.0 (3)B2—N51—C55—C54−177.3 (3)
B2—N41—N42—C43168.5 (3)N52—N51—C55—C56−178.7 (3)
Yb—N41—N42—C43−141.9 (2)B2—N51—C55—C563.7 (6)
C45—N41—N42—Yb140.9 (2)C53—C54—C55—N510.1 (3)
B2—N41—N42—Yb−49.5 (2)C53—C54—C55—C56179.1 (3)
N32—Yb—N42—C433.3 (3)N52—C53—C57—C58−4.8 (4)
N12—Yb—N42—C43−99.8 (4)C54—C53—C57—C58175.1 (3)
N22—Yb—N42—C43−90.3 (3)N52—C53—C57—C59117.0 (3)
N52—Yb—N42—C43112.0 (3)C54—C53—C57—C59−63.2 (4)
N41—Yb—N42—C43119.4 (4)N52—C53—C57—C60−125.2 (3)
N32—Yb—N42—N41−116.17 (16)C54—C53—C57—C6054.6 (4)
N12—Yb—N42—N41140.8 (2)N61—N62—C63—C64−0.1 (4)
N22—Yb—N42—N41150.26 (16)N61—N62—C63—C67179.5 (3)
N52—Yb—N42—N41−7.45 (16)N62—C63—C64—C650.3 (4)
C55—N51—N52—C53−0.6 (3)C67—C63—C64—C65−179.3 (3)
B2—N51—N52—C53177.5 (2)N62—N61—C65—C640.3 (4)
C55—N51—N52—Yb−179.92 (19)B2—N61—C65—C64179.5 (3)
B2—N51—N52—Yb−1.8 (3)N62—N61—C65—C66−179.0 (3)
N32—Yb—N52—C53−44.1 (4)B2—N61—C65—C660.2 (5)
N12—Yb—N52—C5347.1 (4)C63—C64—C65—N61−0.4 (4)
N22—Yb—N52—C53112.0 (4)C63—C64—C65—C66178.9 (4)
N42—Yb—N52—C53−143.6 (4)N62—C63—C67—C700.8 (5)
N41—Yb—N52—C53−147.4 (4)C64—C63—C67—C70−179.8 (5)
N32—Yb—N52—N51134.66 (17)N62—C63—C67—C69−122.6 (4)
N12—Yb—N52—N51−134.12 (17)C64—C63—C67—C6956.9 (5)
N22—Yb—N52—N51−69.3 (3)N62—C63—C67—C68120.1 (4)
N42—Yb—N52—N5135.14 (17)C64—C63—C67—C68−60.4 (5)
N41—Yb—N52—N5131.38 (16)C15—N11—B1—N21125.8 (3)
C65—N61—N62—C63−0.1 (3)N12—N11—B1—N21−36.9 (4)
B2—N61—N62—C63−179.4 (3)C15—N11—B1—N31−107.6 (3)
N11—N12—C13—C141.2 (4)N12—N11—B1—N3189.7 (3)
Yb—N12—C13—C14−142.6 (3)C25—N21—B1—N11−118.6 (3)
N11—N12—C13—C17−172.2 (3)N22—N21—B1—N1151.7 (3)
Yb—N12—C13—C1744.0 (5)C25—N21—B1—N31115.6 (3)
N12—C13—C14—C15−0.6 (4)N22—N21—B1—N31−74.2 (3)
C17—C13—C14—C15172.5 (3)C35—N31—B1—N11134.9 (3)
N12—N11—C15—C141.1 (3)N32—N31—B1—N11−39.6 (4)
B1—N11—C15—C14−163.5 (3)C35—N31—B1—N21−100.1 (3)
N12—N11—C15—C16−177.4 (3)N32—N31—B1—N2185.3 (3)
B1—N11—C15—C1618.0 (5)C65—N61—B2—N41162.1 (3)
C13—C14—C15—N11−0.3 (4)N62—N61—B2—N41−18.8 (4)
C13—C14—C15—C16178.0 (3)C65—N61—B2—N51−71.2 (4)
N12—C13—C17—C19−20.8 (5)N62—N61—B2—N51108.0 (3)
C14—C13—C17—C19167.0 (4)C45—N41—B2—N6157.9 (4)
N12—C13—C17—C18−143.3 (3)N42—N41—B2—N61−108.9 (3)
C14—C13—C17—C1844.4 (5)Yb—N41—B2—N61−151.0 (2)
N12—C13—C17—C2098.2 (4)C45—N41—B2—N51−70.3 (4)
C14—C13—C17—C20−74.0 (5)N42—N41—B2—N51123.0 (3)
N21—N22—C23—C24−0.9 (3)Yb—N41—B2—N5180.9 (2)
Yb—N22—C23—C24168.1 (2)C55—N51—B2—N61−20.9 (5)
N21—N22—C23—C27173.8 (3)N52—N51—B2—N61161.6 (2)
Yb—N22—C23—C27−17.2 (5)C55—N51—B2—N41106.6 (4)
N22—C23—C24—C250.8 (4)N52—N51—B2—N41−70.9 (3)
C27—C23—C24—C25−173.7 (3)C6S—C1S—C2S—C3S−1.6 (7)
N22—N21—C25—C24−0.2 (4)C7S—C1S—C2S—C3S179.3 (6)
B1—N21—C25—C24171.1 (3)C1S—C2S—C3S—C4S2.1 (8)
N22—N21—C25—C26−179.9 (3)C2S—C3S—C4S—C5S−0.3 (8)
B1—N21—C25—C26−8.5 (5)C3S—C4S—C5S—C6S−1.9 (8)
C23—C24—C25—N21−0.3 (4)C4S—C5S—C6S—C1S2.4 (8)
C23—C24—C25—C26179.3 (3)C2S—C1S—C6S—C5S−0.6 (7)
N22—C23—C27—C28A13.9 (6)C7S—C1S—C6S—C5S178.5 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
B2—H2B···Yb1.16 (3)2.29 (4)3.002 (3)118 (2)

Experimental details

Crystal data
Chemical formula[Yb(C24H40BN6)2]·C7H8
Mr1112.03
Crystal system, space groupTriclinic, P1
Temperature (K)193
a, b, c (Å)11.8621 (17), 12.1587 (17), 20.650 (3)
α, β, γ (°)96.1072 (19), 96.1001 (18), 98.9737 (19)
V (Å3)2902.1 (7)
Z2
Radiation typeMo Kα
µ (mm−1)1.66
Crystal size (mm)0.39 × 0.36 × 0.14
Data collection
DiffractometerBruker PLATFORM
diffractometer with SMART 1000 CCD area-detector
Absorption correctionIntegration
(SHELXTL; Sheldrick, 2008)
Tmin, Tmax0.564, 0.801
No. of measured, independent and
observed [I > 2σ(I)] reflections		24467, 13091, 11816
Rint0.026
(sin θ/λ)max (Å−1)0.651
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.035, 0.096, 1.10
No. of reflections13091
No. of parameters669
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)1.91, −1.74

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Yb—N322.477 (3)N11—B11.554 (4)
Yb—N122.524 (3)N21—B11.558 (4)
Yb—N222.547 (2)N31—B11.560 (4)
Yb—N422.555 (2)N41—B21.546 (4)
Yb—N522.632 (3)N51—B21.553 (4)
Yb—N412.990 (2)N61—B21.527 (4)
Yb—H2B2.29 (4)B2—H2B1.16 (3)
N32—Yb—N1287.15 (8)N12—Yb—N41162.84 (8)
N32—Yb—N2293.28 (8)N22—Yb—N41115.54 (7)
N12—Yb—N2268.27 (8)N42—Yb—N4127.63 (7)
N32—Yb—N4297.77 (8)N52—Yb—N4166.66 (7)
N12—Yb—N42159.83 (9)N32—Yb—H2B153.8 (9)
N22—Yb—N4291.85 (8)N12—Yb—H2B118.2 (9)
N32—Yb—N52107.92 (8)N22—Yb—H2B101.8 (9)
N12—Yb—N52103.07 (8)N42—Yb—H2B60.9 (9)
N22—Yb—N52156.96 (8)N52—Yb—H2B62.5 (9)
N42—Yb—N5294.05 (8)N41—Yb—H2B45.3 (9)
N32—Yb—N41108.81 (7)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
B2—H2B···Yb1.16 (3)2.29 (4)3.002 (3)118 (2)
 

Acknowledgements

This work was supported by the Natural Science and Engineering Research Council of Canada and the University of Alberta.

References

First citationBruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationCalabrese, J. C., Donaille, P. J., Thompson, J. S. & Trofimenko, S. (1990). Inorg. Chem. 29, 4429–4447.  CSD CrossRef CAS Web of Science Google Scholar
 First citationCheng, J., Takats, J., Ferguson, M. J. & McDonald, R. (2008). J. Am. Chem. Soc. 130, 1544–1545.  Web of Science CSD CrossRef PubMed CAS Google Scholar
 First citationCotton, F. A., Jeremic, M. & Shaver, A. (1972). Inorg. Chim. Acta, 6, 543–551.  CSD CrossRef CAS Google Scholar
 First citationKosky, C. A., Ganis, P. & Avitabile, G. (1971). Acta Cryst. B27, 1859–1864.  CSD CrossRef CAS IUCr Journals Web of Science Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationZhang, X. W., McDonald, R. & Takats, J. (1995). New J. Chem. 19, 573–585.  CAS Google Scholar

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ISSN: 2056-9890
Volume 65| Part 6| June 2009| Pages m643-m644
doi:10.1107/S1600536809017152
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