[η5-2,3-Bis(trimethylsilyl)-2,3-dicarba-nido-hexaborane(2−)]chlorido(N,N,N′,N′-tetramethylethylenediamine)dysprosium(III)

Zheng, C.; Canseco-Melchor, G.; Maguire, J.A.; Hosmane, N.S.

doi:10.1107/S1600536808013615

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 6| June 2008| Page m799

doi:10.1107/S1600536808013615

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[η⁵-2,3-Bis(trimethylsilyl)-2,3-dicarba-nido-hexaborane(2−)]chlorido(N,N,N′,N′-tetramethylethylenediamine)dysprosium(III)

Chong Zheng,^a ^* Graciela Canseco-Melchor,^a John A. Maguire ^b and Narayan S. Hosmane ^a

^aDepartment of Chemistry and Biochemistry, Northern Illinois University, DeKalb, IL 60115, USA, and ^bDepartment of Chemistry, Southern Methodist University, Dallas, TX 75275, USA
^*Correspondence e-mail: zheng@cz.chem.niu.edu

(Received 26 March 2008; accepted 7 May 2008; online 10 May 2008)

The structure of the title compound, [Dy(C₈H₂₂B₄Si₂)Cl(C₆H₁₆N₂)], reveals that a center of symmetry exists within the dimeric half-sandwich units. Within each half-sandwich, the Dy^III ion is coordinated by the five-membered ring of the carborane, tetramethylethylenediamine and the chloride ion.

Related literature

For related literature, see: Bazan et al. (1993 ); Tomlinson et al. (2005 ); Wang et al. (2006 ).

Experimental

Crystal data

[Dy(C₈H₂₂B₄Si₂)Cl(C₆H₁₆N₂)]
M_r = 531.84
Monoclinic, P 2₁ /n
a = 11.4467 (8) Å
b = 14.862 (1) Å
c = 13.8615 (9) Å
β = 92.770 (1)°
V = 2355.4 (3) Å³
Z = 4
Mo Kα radiation
μ = 3.39 mm⁻¹
T = 293 (2) K
0.80 × 0.30 × 0.30 mm

Data collection

Bruker SMART CCD PLATFORM diffractometer
Absorption correction: multi-scan SADABS (Sheldrick, 2006 ) T_min = 0.257, T_max = 0.362
17271 measured reflections
4151 independent reflections
4142 reflections with I > 2σ(I)
R_int = 0.019

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.050
S = 1.44
4151 reflections
231 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.64 e Å⁻³
Δρ_min = −0.61 e Å⁻³

Data collection: SMART (Bruker, 2003 ); cell refinement: SMART and SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXTL (Sheldrick, 2008 ); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808013615/si2081sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808013615/si2081Isup2.hkl

checkCIF report

Comment top

The lanthanacarboranes (LnC₂B₄) cage systems are of interest in that their structural chemistry depends on the number and nature of the metal ligands other than the particular carborane. For example, the reaction of the tetrahydrofuran (THF) solvated dilithium compounds of B₄C₈H₂₂Si₂^2- with LnCl₃ in 2:1 molar ratios produced exclusively a trinuclear clusters (Tomlinson et al. 2005, Wang et al. 2006, and literature cited therein). The methoxide and oxide ions were thought to be the result of a degradation of the THF molecules. This is consistent with the observation that the reaction of the TMEDA lithiacarboranes with LnCl₃ in 2:1 molar ratios gave the expected full sandwich lanthanacarboranes. This tendency for TMEDA to disrupt complex aggregation and alter the course of a metalation reactions was also found in the d-block metals. The reaction of the THF solvated dilithium salts of B₄C₈H₂₂Si₂^2- with either CoCl₂ or NiCl₂ induced a metal disproportion reaction yielding commo-complexes and the respective metals. On the other hand, similar reactions with the TMEDA-solvated carborane dianions produced the corresponding closo-compound (Tomlinson et al. 2005). The reaction of a nido-compound with a number of lanthanide halides in 2:1 carborane-to-lanthanide molar ratios produced only the corresponding dimers (Wang et al. 2006). The presence of the reactive chlorides made these compounds potentially useful precursors in the syntheses of other lanthanacarboranes. Since dimer formation is thought to inhibit the reactions of the metallacatboranes (Bazan et al. 1993), the synthesis of a monomeric dysprosacarborane was attempted by the reaction of DyCl₃ and the nido-compound, giving the title compound. The structure of the title compound, shown in Figure 1, is somewhat surprising in that it still remains a dimer. The structure consists of two half-sandwich units bridged at the B4, B5 positions by two pairs of B—H—Dy bonds. The average coordination bond distances (Å) are: Dy—Cl 2.5851 (9), Dy—N1 2.598 (3), Dy—N2 2.698 (3), Dy—B4,B5 2.728 (4), 2.692 (4), Dy-av(C1, C2, B3, B4, B5) 2.720 and the corresponding bond angles (°) are Cl—Dy—N1 95.98 (7), Cl—Dy—B5 143.74 (8), N(1)—Dy—N(2) 68.3 (1), B(5)—Dy—B(4) 35.7 (1). The Dy-av(C₂B₃) distance of 2.712Å and the Dy—Cl distance of 2.5851 (9) Å in the structure are similar to the values of 2.717 Å and 2.5757 (14) Å, respectively, found in anther Dy compound (Wang et al. 2006). This is one of the few instances where the substitution of THF by TMEDA molecules does not change either the cluster or intermolecular geometries.

Related literature top

For related literature, see: Bazan et al. (1993); Tomlinson et al. (2005); Wang et al. (2006).

Experimental top

The reaction of DyCl₃ with the TMEDA solvated monosodium nido- compound, nido-1-Na(TMEDA)2–2,3-(SiMe₃)₂-2,3-C₂B₄H₄, in a 1:2 molar ratio in dry benzene at 60° C produced the corresponding half sandwich carborane in 88% yield.

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SMART and SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. Thermal ellipsoid drawing of the title compound shown at the 30% probability level. Atoms of the symmetry related moiety of the dimer complex are indicated "A" (symmetry code 1 - x, 2 - y, 1 - z).
	Fig. 2. Reaction scheme

[η⁵-2,3-Bis(trimethylsilyl)-2,3-dicarba-nido- hexaborane(2-)]chlorido(N,N,N',N'-tetramethylethylenediamine)dysprosium(III) top

Crystal data top

[Dy(C₈H₂₂B₄Si₂)Cl(C₆H₁₆N₂)]	F(000) = 1068
M_r = 531.84	D_x = 1.500 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 562 reflections
a = 11.4467 (8) Å	θ = −14–14°
b = 14.8624 (10) Å	µ = 3.39 mm⁻¹
c = 13.8615 (9) Å	T = 293 K
β = 92.770 (1)°	Column, colorless
V = 2355.4 (3) Å³	0.80 × 0.30 × 0.30 mm
Z = 4

Data collection top

Bruker SMART CCD PLATFORM diffractometer	4151 independent reflections
Radiation source: fine-focus sealed tube	4142 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.019
Detector resolution: 0 pixels mm^-1	θ_max = 25.0°, θ_min = 2.0°
ω scans	h = −13→13
Absorption correction: multi-scan SADABS (Sheldrick, 2006)	k = −17→17
T_min = 0.257, T_max = 0.362	l = −16→16
17271 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.050	H atoms treated by a mixture of independent and constrained refinement
S = 1.44	w = 1/[σ²(F_o²) + 3.9928P] where P = (F_o² + 2F_c²)/3
4151 reflections	(Δ/σ)_max = 0.013
231 parameters	Δρ_max = 0.64 e Å⁻³
0 restraints	Δρ_min = −0.61 e Å⁻³

Crystal data top

[Dy(C₈H₂₂B₄Si₂)Cl(C₆H₁₆N₂)]	V = 2355.4 (3) Å³
M_r = 531.84	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 11.4467 (8) Å	µ = 3.39 mm⁻¹
b = 14.8624 (10) Å	T = 293 K
c = 13.8615 (9) Å	0.80 × 0.30 × 0.30 mm
β = 92.770 (1)°

Data collection top

Bruker SMART CCD PLATFORM diffractometer	4151 independent reflections
Absorption correction: multi-scan SADABS (Sheldrick, 2006)	4142 reflections with I > 2σ(I)
T_min = 0.257, T_max = 0.362	R_int = 0.019
17271 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	0 restraints
wR(F²) = 0.050	H atoms treated by a mixture of independent and constrained refinement
S = 1.44	Δρ_max = 0.64 e Å⁻³
4151 reflections	Δρ_min = −0.61 e Å⁻³
231 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

	x	y	z	U_iso*/U_eq
Dy	0.584689 (12)	0.954047 (10)	0.626856 (11)	0.02053 (6)
Cl	0.65147 (8)	0.79787 (6)	0.69040 (8)	0.0406 (2)
Si1	0.37951 (8)	0.73248 (6)	0.55959 (7)	0.0268 (2)
Si2	0.31576 (8)	0.84186 (6)	0.80092 (7)	0.0269 (2)
C1	0.3894 (3)	0.8543 (2)	0.5966 (2)	0.0205 (6)
C2	0.3757 (3)	0.8993 (2)	0.6921 (2)	0.0221 (7)
B3	0.3682 (3)	1.0040 (3)	0.6794 (3)	0.0249 (8)
H3	0.3640	1.0465	0.7285	0.030*
B4	0.3693 (3)	1.0245 (2)	0.5630 (3)	0.0233 (8)
H4	0.3622	1.0799	0.5320	0.028*
B5	0.3862 (3)	0.9239 (2)	0.5134 (3)	0.0217 (7)
H5	0.3926	0.9117	0.4481	0.026*
B6	0.2804 (3)	0.9338 (3)	0.6029 (3)	0.0239 (8)
C7	0.4863 (4)	0.7136 (3)	0.4645 (3)	0.0501 (11)
H7A	0.4791	0.6531	0.4410	0.075*
H7B	0.5642	0.7232	0.4914	0.075*
H7C	0.4707	0.7550	0.4123	0.075*
C8	0.2302 (4)	0.7083 (3)	0.5048 (3)	0.0472 (11)
H8A	0.1723	0.7344	0.5441	0.071*
H8B	0.2185	0.6444	0.5012	0.071*
H8C	0.2230	0.7336	0.4411	0.071*
C9	0.4155 (3)	0.6475 (2)	0.6554 (3)	0.0380 (9)
H9A	0.3536	0.6453	0.6996	0.057*
H9B	0.4873	0.6639	0.6896	0.057*
H9C	0.4242	0.5894	0.6262	0.057*
C10	0.1876 (3)	0.7697 (3)	0.7643 (3)	0.0372 (9)
H10A	0.1693	0.7311	0.8170	0.056*
H10B	0.2062	0.7338	0.7095	0.056*
H10C	0.1214	0.8072	0.7474	0.056*
C11	0.4250 (4)	0.7748 (3)	0.8752 (3)	0.0450 (10)
H11A	0.4679	0.8139	0.9191	0.068*
H11B	0.4780	0.7458	0.8335	0.068*
H11C	0.3850	0.7300	0.9112	0.068*
C12	0.2567 (4)	0.9287 (3)	0.8824 (3)	0.0436 (10)
H12A	0.3179	0.9698	0.9023	0.065*
H12B	0.2270	0.9000	0.9382	0.065*
H12C	0.1947	0.9611	0.8487	0.065*
N1	0.6388 (3)	1.0410 (2)	0.7853 (2)	0.0323 (7)
C13	0.7672 (3)	1.0466 (3)	0.8066 (3)	0.0430 (10)
H13A	0.7826	1.0429	0.8760	0.052*
H13B	0.7950	1.1046	0.7854	0.052*
C14	0.8344 (3)	0.9737 (3)	0.7587 (3)	0.0367 (9)
H14A	0.9169	0.9798	0.7768	0.044*
H14B	0.8086	0.9155	0.7812	0.044*
N2	0.8178 (3)	0.9778 (2)	0.6525 (2)	0.0345 (7)
C15	0.5868 (4)	0.9852 (3)	0.8603 (3)	0.0442 (10)
H15A	0.6170	0.9250	0.8572	0.066*
H15B	0.5034	0.9840	0.8496	0.066*
H15C	0.6064	1.0102	0.9229	0.066*
C16	0.5897 (4)	1.1327 (3)	0.7910 (3)	0.0464 (10)
H16A	0.6069	1.1570	0.8543	0.070*
H16B	0.5064	1.1303	0.7788	0.070*
H16C	0.6237	1.1704	0.7436	0.070*
C17	0.8846 (3)	0.9040 (3)	0.6097 (4)	0.0554 (12)
H17A	0.9663	0.9113	0.6268	0.083*
H17B	0.8727	0.9054	0.5407	0.083*
H17C	0.8581	0.8474	0.6338	0.083*
C18	0.8693 (4)	1.0633 (3)	0.6189 (3)	0.0517 (12)
H18A	0.9477	1.0692	0.6460	0.078*
H18B	0.8230	1.1130	0.6392	0.078*
H18C	0.8706	1.0628	0.5497	0.078*
H6	0.191 (3)	0.916 (2)	0.600 (3)	0.029 (9)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy	0.01951 (8)	0.01862 (9)	0.02317 (9)	−0.00146 (6)	−0.00200 (6)	0.00244 (6)
Cl	0.0311 (5)	0.0249 (4)	0.0647 (6)	0.0002 (4)	−0.0081 (4)	0.0114 (4)
Si1	0.0314 (5)	0.0189 (5)	0.0301 (5)	−0.0025 (4)	0.0010 (4)	−0.0016 (4)
Si2	0.0303 (5)	0.0268 (5)	0.0238 (5)	−0.0015 (4)	0.0049 (4)	0.0036 (4)
C1	0.0178 (15)	0.0198 (16)	0.0238 (16)	−0.0006 (12)	0.0005 (12)	0.0010 (13)
C2	0.0196 (16)	0.0224 (16)	0.0242 (17)	−0.0003 (13)	0.0008 (13)	0.0005 (13)
B3	0.0251 (19)	0.0226 (19)	0.027 (2)	0.0016 (15)	0.0014 (15)	−0.0026 (15)
B4	0.0221 (18)	0.0163 (18)	0.031 (2)	0.0009 (14)	0.0003 (15)	0.0034 (15)
B5	0.0184 (17)	0.0230 (19)	0.0237 (18)	−0.0028 (14)	−0.0002 (14)	−0.0003 (15)
B6	0.0207 (18)	0.0231 (19)	0.028 (2)	0.0002 (15)	0.0010 (15)	0.0021 (15)
C7	0.067 (3)	0.036 (2)	0.049 (3)	0.008 (2)	0.022 (2)	−0.0054 (19)
C8	0.050 (3)	0.036 (2)	0.054 (3)	−0.0117 (19)	−0.019 (2)	−0.0039 (19)
C9	0.039 (2)	0.0247 (19)	0.049 (2)	−0.0006 (16)	−0.0026 (18)	0.0039 (17)
C10	0.033 (2)	0.040 (2)	0.040 (2)	−0.0074 (17)	0.0114 (17)	0.0021 (17)
C11	0.048 (2)	0.045 (2)	0.041 (2)	0.0010 (19)	−0.0038 (19)	0.0168 (19)
C12	0.053 (3)	0.042 (2)	0.036 (2)	−0.0025 (19)	0.0161 (19)	−0.0034 (18)
N1	0.0360 (17)	0.0301 (16)	0.0303 (16)	−0.0061 (13)	−0.0058 (13)	−0.0029 (13)
C13	0.037 (2)	0.047 (2)	0.044 (2)	−0.0102 (18)	−0.0129 (18)	−0.0051 (19)
C14	0.0300 (19)	0.039 (2)	0.039 (2)	−0.0056 (16)	−0.0141 (16)	0.0089 (17)
N2	0.0266 (15)	0.0383 (18)	0.0377 (17)	−0.0059 (13)	−0.0058 (13)	0.0031 (14)
C15	0.052 (2)	0.053 (3)	0.027 (2)	−0.011 (2)	−0.0055 (18)	0.0033 (18)
C16	0.053 (3)	0.034 (2)	0.052 (3)	−0.0002 (19)	−0.005 (2)	−0.0141 (19)
C17	0.025 (2)	0.068 (3)	0.073 (3)	−0.001 (2)	0.002 (2)	−0.016 (3)
C18	0.037 (2)	0.068 (3)	0.049 (3)	−0.023 (2)	−0.0137 (19)	0.020 (2)

Geometric parameters (Å, º) top

Dy—Cl	2.5851 (9)	C9—H9B	0.9600
Dy—N1	2.598 (3)	C9—H9C	0.9600
Dy—B5ⁱ	2.692 (4)	C10—H10A	0.9600
Dy—N2	2.698 (3)	C10—H10B	0.9600
Dy—C1	2.698 (3)	C10—H10C	0.9600
Dy—C2	2.723 (3)	C11—H11A	0.9600
Dy—B4ⁱ	2.728 (4)	C11—H11B	0.9600
Si1—C7	1.861 (4)	C11—H11C	0.9600
Si1—C9	1.865 (4)	C12—H12A	0.9600
Si1—C8	1.872 (4)	C12—H12B	0.9600
Si1—C1	1.884 (3)	C12—H12C	0.9600
Si2—C12	1.864 (4)	N1—C15	1.477 (5)
Si2—C10	1.867 (4)	N1—C16	1.477 (5)
Si2—C11	1.869 (4)	N1—C13	1.487 (5)
Si2—C2	1.890 (3)	C13—C14	1.502 (6)
C1—C2	1.498 (4)	C13—H13A	0.9700
C1—B5	1.548 (5)	C13—H13B	0.9700
C1—B6	1.724 (5)	C14—N2	1.477 (5)
C2—B3	1.568 (5)	C14—H14A	0.9700
C2—B6	1.689 (5)	C14—H14B	0.9700
B3—B4	1.642 (5)	N2—C17	1.478 (5)
B3—H3	0.9300	N2—C18	1.485 (5)
B4—B5	1.661 (5)	C15—H15A	0.9600
B4—Dyⁱ	2.728 (4)	C15—H15B	0.9600
B4—H4	0.9300	C15—H15C	0.9600
B5—Dyⁱ	2.692 (4)	C16—H16A	0.9600
B5—H5	0.9300	C16—H16B	0.9600
B6—H6	1.06 (4)	C16—H16C	0.9600
C7—H7A	0.9600	C17—H17A	0.9600
C7—H7B	0.9600	C17—H17B	0.9600
C7—H7C	0.9600	C17—H17C	0.9600
C8—H8A	0.9600	C18—H18A	0.9600
C8—H8B	0.9600	C18—H18B	0.9600
C8—H8C	0.9600	C18—H18C	0.9600
C9—H9A	0.9600

Cl—Dy—N1	95.98 (7)	Si1—C8—H8B	109.5
Cl—Dy—B5ⁱ	143.74 (8)	H8A—C8—H8B	109.5
N1—Dy—B5ⁱ	104.06 (10)	Si1—C8—H8C	109.5
Cl—Dy—N2	78.36 (7)	H8A—C8—H8C	109.5
N1—Dy—N2	68.26 (10)	H8B—C8—H8C	109.5
B5ⁱ—Dy—N2	81.43 (10)	Si1—C9—H9A	109.5
Cl—Dy—C1	77.81 (7)	Si1—C9—H9B	109.5
N1—Dy—C1	124.51 (10)	H9A—C9—H9B	109.5
B5ⁱ—Dy—C1	112.86 (10)	Si1—C9—H9C	109.5
N2—Dy—C1	154.04 (9)	H9A—C9—H9C	109.5
Cl—Dy—C2	82.45 (7)	H9B—C9—H9C	109.5
N1—Dy—C2	92.59 (10)	Si2—C10—H10A	109.5
B5ⁱ—Dy—C2	125.64 (10)	Si2—C10—H10B	109.5
N2—Dy—C2	151.01 (9)	H10A—C10—H10B	109.5
C1—Dy—C2	32.08 (9)	Si2—C10—H10C	109.5
Cl—Dy—B4ⁱ	111.47 (8)	H10A—C10—H10C	109.5
N1—Dy—B4ⁱ	135.13 (10)	H10B—C10—H10C	109.5
B5ⁱ—Dy—B4ⁱ	35.69 (11)	Si2—C11—H11A	109.5
N2—Dy—B4ⁱ	82.89 (10)	Si2—C11—H11B	109.5
C1—Dy—B4ⁱ	96.39 (10)	H11A—C11—H11B	109.5
C2—Dy—B4ⁱ	124.68 (10)	Si2—C11—H11C	109.5
C7—Si1—C9	105.8 (2)	H11A—C11—H11C	109.5
C7—Si1—C8	107.6 (2)	H11B—C11—H11C	109.5
C9—Si1—C8	108.95 (19)	Si2—C12—H12A	109.5
C7—Si1—C1	107.74 (17)	Si2—C12—H12B	109.5
C9—Si1—C1	116.69 (16)	H12A—C12—H12B	109.5
C8—Si1—C1	109.69 (17)	Si2—C12—H12C	109.5
C12—Si2—C10	105.03 (19)	H12A—C12—H12C	109.5
C12—Si2—C11	106.8 (2)	H12B—C12—H12C	109.5
C10—Si2—C11	109.84 (19)	C15—N1—C16	108.3 (3)
C12—Si2—C2	109.07 (17)	C15—N1—C13	108.6 (3)
C10—Si2—C2	110.65 (16)	C16—N1—C13	108.3 (3)
C11—Si2—C2	114.95 (17)	C15—N1—Dy	103.2 (2)
C2—C1—B5	111.1 (3)	C16—N1—Dy	115.3 (2)
C2—C1—B6	62.8 (2)	C13—N1—Dy	112.9 (2)
B5—C1—B6	65.7 (2)	N1—C13—C14	113.2 (3)
C2—C1—Si1	131.5 (2)	N1—C13—H13A	108.9
B5—C1—Si1	116.1 (2)	C14—C13—H13A	108.9
B6—C1—Si1	129.7 (2)	N1—C13—H13B	108.9
C2—C1—Dy	74.86 (17)	C14—C13—H13B	108.9
B5—C1—Dy	74.80 (17)	H13A—C13—H13B	107.7
B6—C1—Dy	102.23 (18)	N2—C14—C13	111.5 (3)
Si1—C1—Dy	127.49 (14)	N2—C14—H14A	109.3
C1—C2—B3	110.6 (3)	C13—C14—H14A	109.3
C1—C2—B6	65.2 (2)	N2—C14—H14B	109.3
B3—C2—B6	65.6 (2)	C13—C14—H14B	109.3
C1—C2—Si2	124.1 (2)	H14A—C14—H14B	108.0
B3—C2—Si2	121.2 (2)	C14—N2—C17	109.0 (3)
B6—C2—Si2	118.4 (2)	C14—N2—C18	108.3 (3)
C1—C2—Dy	73.05 (17)	C17—N2—C18	106.7 (3)
B3—C2—Dy	73.14 (18)	C14—N2—Dy	101.8 (2)
B6—C2—Dy	102.27 (19)	C17—N2—Dy	112.2 (2)
Si2—C2—Dy	139.32 (15)	C18—N2—Dy	118.4 (2)
C2—B3—B4	106.9 (3)	N1—C15—H15A	109.5
C2—B3—H3	126.5	N1—C15—H15B	109.5
B4—B3—H3	126.5	H15A—C15—H15B	109.5
B3—B4—B5	104.3 (3)	N1—C15—H15C	109.5
B3—B4—Dyⁱ	168.7 (2)	H15A—C15—H15C	109.5
B5—B4—Dyⁱ	70.97 (18)	H15B—C15—H15C	109.5
B3—B4—H4	127.9	N1—C16—H16A	109.5
B5—B4—H4	127.9	N1—C16—H16B	109.5
Dyⁱ—B4—H4	57.8	H16A—C16—H16B	109.5
C1—B5—B4	107.0 (3)	N1—C16—H16C	109.5
C1—B5—Dyⁱ	171.5 (2)	H16A—C16—H16C	109.5
B4—B5—Dyⁱ	73.34 (18)	H16B—C16—H16C	109.5
C1—B5—H5	126.5	N2—C17—H17A	109.5
B4—B5—H5	126.5	N2—C17—H17B	109.5
Dyⁱ—B5—H5	53.8	H17A—C17—H17B	109.5
C2—B6—C1	52.07 (18)	N2—C17—H17C	109.5
C2—B6—H6	122.4 (19)	H17A—C17—H17C	109.5
C1—B6—H6	122 (2)	H17B—C17—H17C	109.5
Si1—C7—H7A	109.5	N2—C18—H18A	109.5
Si1—C7—H7B	109.5	N2—C18—H18B	109.5
H7A—C7—H7B	109.5	H18A—C18—H18B	109.5
Si1—C7—H7C	109.5	N2—C18—H18C	109.5
H7A—C7—H7C	109.5	H18A—C18—H18C	109.5
H7B—C7—H7C	109.5	H18B—C18—H18C	109.5
Si1—C8—H8A	109.5

Symmetry code: (i) −x+1, −y+2, −z+1.

Experimental details

Crystal data
Chemical formula	[Dy(C₈H₂₂B₄Si₂)Cl(C₆H₁₆N₂)]
M_r	531.84
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	11.4467 (8), 14.8624 (10), 13.8615 (9)
β (°)	92.770 (1)
V (Å³)	2355.4 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.39
Crystal size (mm)	0.80 × 0.30 × 0.30

Data collection
Diffractometer	Bruker SMART CCD PLATFORM diffractometer
Absorption correction	Multi-scan SADABS (Sheldrick, 2006)
T_min, T_max	0.257, 0.362
No. of measured, independent and observed [I > 2σ(I)] reflections	17271, 4151, 4142
R_int	0.019
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.050, 1.44
No. of reflections	4151
No. of parameters	231
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.64, −0.61

Computer programs: SMART (Bruker, 2003), SMART and SAINT (Bruker, 2003), SAINT (Bruker, 2003), SIR97 (Altomare et al., 1999), SHELXTL (Sheldrick, 2008).

Acknowledgements

This work was supported by Northern Illinois University and by grants from the donors of the Petroleum Research Fund, administered by the American Chemical Society, and the National Science Foundation. JAM thanks the Robert A. Welch Foundation (grant N-1322).

References

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