Literature DB >> 21522921

Chlorido{N-[(diethyl-amino)-dimethyl-sil-yl]anilido-κN}(N,N,N',N'-tetra-methyl-ethane-1,2-diamine-κN,N')cobalt(II).

Sheng-Di Bai1, Min Hu.   

Abstract

In the title cobalt(II) compound, [Co(C(12)H(21)N(2)Si)Cl(C(6)H(16)N(2))], the ethane-1,2-diamine donor mol-ecule coordin-ates the metal atom in an N,N'-chelating mode, with Co-N distances of 2.136 (2) and 2.140 (3) Å. An anilide ligand connects to the Co(II) atom with a σ-bond, the Co-N(anilide) distance being 1.931 (2) Å. The four-coordinate Co(II) atom demonstrates a slightly distorted tetra-hedral geometry.

Entities:  

Year:  2011        PMID： 21522921      PMCID： PMC3051766          DOI： 10.1107/S1600536811002959

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For reviews of related metal amides, see: Holm et al. (1996 ▶); Kempe (2000 ▶). For the catalytic applications of related N–silylated analido–group 4 metal compounds towards olefin polymerization, see: Gibson et al. (1998 ▶); Hill & Hitchcock (2002 ▶); Yuan et al. (2010 ▶). For related organometallic compounds with analogous analido ligands, see: Schumann et al. (2000 ▶); Chen (2008 ▶, 2009 ▶).

Experimental

Crystal data

[Co(C12H21N2Si)Cl(C6H16N2)] M = 431.99 Monoclinic, a = 20.711 (2) Å b = 7.7110 (8) Å c = 29.844 (3) Å β = 99.009 (2)° V = 4707.4 (8) Å3 Z = 8 Mo Kα radiation μ = 0.90 mm−1 T = 295 K 0.30 × 0.25 × 0.20 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.774, T max = 0.840 13181 measured reflections 4630 independent reflections 3530 reflections with I > 2σ(I) R int = 0.035

Refinement

R[F 2 > 2σ(F 2)] = 0.048 wR(F 2) = 0.134 S = 1.05 4630 reflections 226 parameters H-atom parameters constrained Δρmax = 0.58 e Å−3 Δρmin = −0.35 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; 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: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811002959/rk2258sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811002959/rk2258Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C12H21N2Si)Cl(C6H16N2)]F(000) = 1848
Mr = 431.99Dx = 1.219 Mg m−3
Monoclinic, C2/cMelting point = 390–391 K
Hall symbol: -C 2ycMo Kα radiation, λ = 0.71073 Å
a = 20.711 (2) ÅCell parameters from 2838 reflections
b = 7.7110 (8) Åθ = 2.6–27.3°
c = 29.844 (3) ŵ = 0.90 mm−1
β = 99.009 (2)°T = 295 K
V = 4707.4 (8) Å3Block, green
Z = 80.30 × 0.25 × 0.20 mm
Bruker SMART CCD diffractometer4630 independent reflections
Radiation source: fine-focus sealed tube3530 reflections with I > 2σ(I)
graphiteRint = 0.035
φ and ω scansθmax = 26.0°, θmin = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −25→19
Tmin = 0.774, Tmax = 0.840k = −9→9
13181 measured reflectionsl = −33→36
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.134H-atom parameters constrained
S = 1.05w = 1/[σ2(Fo2) + (0.0786P)2 + 0.8817P] where P = (Fo2 + 2Fc2)/3
4630 reflections(Δ/σ)max = 0.002
226 parametersΔρmax = 0.58 e Å−3
0 restraintsΔρmin = −0.35 e Å−3
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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.
xyzUiso*/Ueq
Co10.409198 (18)0.55218 (5)0.588284 (12)0.04797 (15)
Si10.37709 (4)0.69888 (11)0.68265 (3)0.0512 (2)
Cl10.44296 (5)0.76779 (12)0.54620 (3)0.0749 (3)
N10.35134 (11)0.6003 (3)0.63160 (8)0.0499 (6)
N20.32211 (13)0.8549 (4)0.69276 (8)0.0615 (7)
N30.48921 (13)0.3793 (4)0.60883 (10)0.0685 (7)
N40.37541 (12)0.3566 (3)0.53954 (8)0.0561 (6)
C10.28473 (13)0.5721 (4)0.61545 (10)0.0514 (7)
C20.25669 (16)0.6353 (5)0.57293 (11)0.0669 (9)
H2A0.28180.70030.55580.080*
C30.1910 (2)0.6013 (6)0.55597 (15)0.0862 (13)
H3A0.17330.64300.52750.103*
C40.15266 (19)0.5085 (6)0.5803 (2)0.0968 (16)
H4A0.10920.48590.56850.116*
C50.17918 (19)0.4492 (5)0.62229 (17)0.0860 (12)
H5A0.15320.38710.63940.103*
C60.24433 (16)0.4799 (5)0.63991 (13)0.0668 (9)
H6A0.26120.43800.66860.080*
C70.45913 (16)0.7966 (5)0.67824 (12)0.0706 (9)
H7A0.45510.87250.65250.106*
H7B0.48970.70580.67470.106*
H7C0.47450.86120.70530.106*
C80.3881 (2)0.5524 (5)0.73357 (12)0.0802 (11)
H8A0.34680.50240.73710.120*
H8B0.40480.61820.76020.120*
H8C0.41840.46170.72940.120*
C90.3114 (2)0.9125 (5)0.73794 (13)0.0838 (11)
H9A0.31720.81420.75850.101*
H9B0.26650.95150.73600.101*
C100.3563 (3)1.0566 (7)0.75764 (17)0.134 (2)
H10A0.34661.08730.78700.201*
H10B0.35011.15580.73800.201*
H10C0.40091.01830.76040.201*
C110.29799 (18)0.9767 (5)0.65620 (12)0.0687 (9)
H11A0.31440.94160.62890.082*
H11B0.31531.09120.66450.082*
C120.2238 (2)0.9869 (6)0.64612 (17)0.1019 (14)
H12A0.21101.06830.62200.153*
H12B0.20721.02420.67280.153*
H12C0.20630.87460.63720.153*
C130.4960 (2)0.3208 (6)0.65667 (14)0.1036 (15)
H13A0.53290.24430.66310.155*
H13B0.45710.26060.66140.155*
H13C0.50250.41960.67640.155*
C140.55074 (19)0.4609 (7)0.6014 (2)0.1199 (19)
H14A0.58640.38260.61060.180*
H14B0.55750.56560.61890.180*
H14C0.54860.48780.56980.180*
C150.4741 (2)0.2226 (5)0.57985 (15)0.0912 (13)
H15A0.51470.16580.57590.109*
H15B0.44880.14180.59500.109*
C160.43702 (18)0.2672 (5)0.53474 (13)0.0784 (11)
H16A0.46340.34170.51870.094*
H16B0.42730.16220.51710.094*
C170.3459 (2)0.4245 (5)0.49423 (11)0.0786 (10)
H17A0.33190.32920.47440.118*
H17B0.37790.49160.48170.118*
H17C0.30910.49640.49740.118*
C180.32867 (18)0.2356 (5)0.55483 (13)0.0760 (10)
H18A0.31530.15160.53150.114*
H18B0.29110.29860.56120.114*
H18C0.34900.17750.58180.114*
U11U22U33U12U13U23
Co10.0462 (2)0.0454 (2)0.0532 (2)0.00471 (16)0.01055 (16)0.00056 (16)
Si10.0552 (5)0.0527 (5)0.0444 (4)−0.0009 (4)0.0040 (3)0.0029 (3)
Cl10.0905 (6)0.0578 (5)0.0813 (6)−0.0065 (4)0.0282 (5)0.0086 (4)
N10.0457 (12)0.0546 (14)0.0501 (13)0.0050 (11)0.0091 (10)−0.0031 (11)
N20.0739 (17)0.0605 (17)0.0522 (14)0.0004 (13)0.0162 (13)−0.0043 (12)
N30.0522 (15)0.0673 (18)0.0827 (19)0.0155 (13)0.0004 (14)−0.0027 (15)
N40.0575 (15)0.0519 (15)0.0607 (14)0.0012 (12)0.0146 (12)−0.0068 (12)
C10.0471 (15)0.0502 (17)0.0565 (16)0.0123 (13)0.0072 (13)−0.0146 (13)
C20.066 (2)0.070 (2)0.0608 (18)0.0201 (17)0.0009 (16)−0.0090 (16)
C30.076 (2)0.082 (3)0.089 (3)0.035 (2)−0.024 (2)−0.032 (2)
C40.049 (2)0.091 (3)0.143 (4)0.015 (2)−0.006 (3)−0.061 (3)
C50.058 (2)0.083 (3)0.120 (3)−0.0094 (19)0.024 (2)−0.039 (3)
C60.0573 (18)0.065 (2)0.080 (2)0.0011 (16)0.0160 (17)−0.0139 (17)
C70.066 (2)0.073 (2)0.071 (2)−0.0095 (18)0.0050 (17)−0.0026 (18)
C80.100 (3)0.075 (3)0.061 (2)0.001 (2)−0.0007 (19)0.0179 (18)
C90.110 (3)0.079 (3)0.069 (2)0.004 (2)0.033 (2)−0.0084 (19)
C100.208 (7)0.112 (4)0.084 (3)−0.037 (4)0.032 (4)−0.038 (3)
C110.082 (2)0.057 (2)0.067 (2)0.0101 (17)0.0106 (18)−0.0003 (16)
C120.091 (3)0.093 (3)0.116 (3)0.031 (3)0.000 (3)−0.007 (3)
C130.114 (3)0.088 (3)0.097 (3)0.037 (3)−0.019 (3)0.013 (2)
C140.048 (2)0.122 (4)0.189 (6)0.014 (2)0.018 (3)0.004 (4)
C150.079 (3)0.069 (3)0.123 (4)0.032 (2)0.009 (2)−0.016 (2)
C160.073 (2)0.075 (3)0.091 (3)0.0126 (19)0.024 (2)−0.021 (2)
C170.096 (3)0.082 (3)0.0575 (19)0.002 (2)0.0097 (18)−0.0130 (18)
C180.085 (2)0.060 (2)0.086 (2)−0.0138 (18)0.022 (2)−0.0144 (18)
Co1—N11.931 (2)C8—H8B0.9600
Co1—N42.136 (2)C8—H8C0.9600
Co1—N32.140 (3)C9—C101.508 (6)
Co1—Cl12.2595 (9)C9—H9A0.9700
Si1—N11.711 (2)C9—H9B0.9700
Si1—N21.715 (3)C10—H10A0.9600
Si1—C81.878 (3)C10—H10B0.9600
Si1—C71.882 (3)C10—H10C0.9600
N1—C11.405 (4)C11—C121.521 (5)
N2—C111.467 (4)C11—H11A0.9700
N2—C91.469 (4)C11—H11B0.9700
N3—C141.469 (5)C12—H12A0.9600
N3—C131.483 (5)C12—H12B0.9600
N3—C151.491 (5)C12—H12C0.9600
N4—C181.468 (4)C13—H13A0.9600
N4—C161.477 (4)C13—H13B0.9600
N4—C171.489 (4)C13—H13C0.9600
C1—C61.389 (5)C14—H14A0.9600
C1—C21.398 (4)C14—H14B0.9600
C2—C31.399 (5)C14—H14C0.9600
C2—H2A0.9300C15—C161.482 (5)
C3—C41.360 (7)C15—H15A0.9700
C3—H3A0.9300C15—H15B0.9700
C4—C51.367 (7)C16—H16A0.9700
C4—H4A0.9300C16—H16B0.9700
C5—C61.390 (5)C17—H17A0.9600
C5—H5A0.9300C17—H17B0.9600
C6—H6A0.9300C17—H17C0.9600
C7—H7A0.9600C18—H18A0.9600
C7—H7B0.9600C18—H18B0.9600
C7—H7C0.9600C18—H18C0.9600
C8—H8A0.9600
N1—Co1—N4114.84 (10)N2—C9—C10114.1 (3)
N1—Co1—N3117.50 (11)N2—C9—H9A108.7
N4—Co1—N384.94 (10)C10—C9—H9A108.7
N1—Co1—Cl1120.61 (8)N2—C9—H9B108.7
N4—Co1—Cl1103.76 (7)C10—C9—H9B108.7
N3—Co1—Cl1108.92 (9)H9A—C9—H9B107.6
N1—Si1—N2110.18 (12)C9—C10—H10A109.5
N1—Si1—C8115.75 (16)C9—C10—H10B109.5
N2—Si1—C8106.22 (16)H10A—C10—H10B109.5
N1—Si1—C7105.93 (14)C9—C10—H10C109.5
N2—Si1—C7111.30 (16)H10A—C10—H10C109.5
C8—Si1—C7107.49 (18)H10B—C10—H10C109.5
C1—N1—Si1121.77 (18)N2—C11—C12113.3 (3)
C1—N1—Co1114.80 (18)N2—C11—H11A108.9
Si1—N1—Co1122.79 (13)C12—C11—H11A108.9
C11—N2—C9114.0 (3)N2—C11—H11B108.9
C11—N2—Si1118.4 (2)C12—C11—H11B108.9
C9—N2—Si1125.0 (3)H11A—C11—H11B107.7
C14—N3—C13108.7 (4)C11—C12—H12A109.5
C14—N3—C15111.6 (3)C11—C12—H12B109.5
C13—N3—C15107.0 (3)H12A—C12—H12B109.5
C14—N3—Co1110.0 (3)C11—C12—H12C109.5
C13—N3—Co1114.7 (2)H12A—C12—H12C109.5
C15—N3—Co1104.9 (2)H12B—C12—H12C109.5
C18—N4—C16110.8 (3)N3—C13—H13A109.5
C18—N4—C17108.0 (3)N3—C13—H13B109.5
C16—N4—C17108.3 (3)H13A—C13—H13B109.5
C18—N4—Co1113.51 (19)N3—C13—H13C109.5
C16—N4—Co1101.5 (2)H13A—C13—H13C109.5
C17—N4—Co1114.5 (2)H13B—C13—H13C109.5
C6—C1—C2117.2 (3)N3—C14—H14A109.5
C6—C1—N1122.6 (3)N3—C14—H14B109.5
C2—C1—N1120.2 (3)H14A—C14—H14B109.5
C1—C2—C3120.3 (4)N3—C14—H14C109.5
C1—C2—H2A119.8H14A—C14—H14C109.5
C3—C2—H2A119.8H14B—C14—H14C109.5
C4—C3—C2121.4 (4)C16—C15—N3111.7 (3)
C4—C3—H3A119.3C16—C15—H15A109.3
C2—C3—H3A119.3N3—C15—H15A109.3
C3—C4—C5118.7 (4)C16—C15—H15B109.3
C3—C4—H4A120.6N3—C15—H15B109.3
C5—C4—H4A120.6H15A—C15—H15B107.9
C4—C5—C6121.1 (4)N4—C16—C15110.7 (3)
C4—C5—H5A119.4N4—C16—H16A109.5
C6—C5—H5A119.4C15—C16—H16A109.5
C1—C6—C5121.2 (4)N4—C16—H16B109.5
C1—C6—H6A119.4C15—C16—H16B109.5
C5—C6—H6A119.4H16A—C16—H16B108.1
Si1—C7—H7A109.5N4—C17—H17A109.5
Si1—C7—H7B109.5N4—C17—H17B109.5
H7A—C7—H7B109.5H17A—C17—H17B109.5
Si1—C7—H7C109.5N4—C17—H17C109.5
H7A—C7—H7C109.5H17A—C17—H17C109.5
H7B—C7—H7C109.5H17B—C17—H17C109.5
Si1—C8—H8A109.5N4—C18—H18A109.5
Si1—C8—H8B109.5N4—C18—H18B109.5
H8A—C8—H8B109.5H18A—C18—H18B109.5
Si1—C8—H8C109.5N4—C18—H18C109.5
H8A—C8—H8C109.5H18A—C18—H18C109.5
H8B—C8—H8C109.5H18B—C18—H18C109.5
N2—Si1—N1—C1−34.7 (3)N1—Co1—N4—C16−142.6 (2)
C8—Si1—N1—C185.8 (3)N3—Co1—N4—C16−24.6 (2)
C7—Si1—N1—C1−155.2 (2)Cl1—Co1—N4—C1683.7 (2)
N2—Si1—N1—Co1135.65 (16)N1—Co1—N4—C17101.0 (2)
C8—Si1—N1—Co1−103.8 (2)N3—Co1—N4—C17−141.0 (2)
C7—Si1—N1—Co115.2 (2)Cl1—Co1—N4—C17−32.7 (2)
N4—Co1—N1—C1−29.3 (2)Si1—N1—C1—C6−56.6 (4)
N3—Co1—N1—C1−126.8 (2)Co1—N1—C1—C6132.4 (2)
Cl1—Co1—N1—C196.0 (2)Si1—N1—C1—C2124.4 (3)
N4—Co1—N1—Si1159.74 (14)Co1—N1—C1—C2−46.6 (3)
N3—Co1—N1—Si162.2 (2)C6—C1—C2—C3−1.7 (4)
Cl1—Co1—N1—Si1−74.92 (17)N1—C1—C2—C3177.3 (3)
N1—Si1—N2—C11−46.8 (3)C1—C2—C3—C40.8 (5)
C8—Si1—N2—C11−172.9 (3)C2—C3—C4—C50.5 (6)
C7—Si1—N2—C1170.4 (3)C3—C4—C5—C6−1.0 (6)
N1—Si1—N2—C9152.6 (3)C2—C1—C6—C51.3 (5)
C8—Si1—N2—C926.5 (3)N1—C1—C6—C5−177.7 (3)
C7—Si1—N2—C9−90.2 (3)C4—C5—C6—C10.1 (5)
N1—Co1—N3—C14−127.3 (3)C11—N2—C9—C10−74.0 (5)
N4—Co1—N3—C14117.3 (3)Si1—N2—C9—C1087.3 (5)
Cl1—Co1—N3—C1414.5 (3)C9—N2—C11—C12−69.9 (4)
N1—Co1—N3—C13−4.4 (3)Si1—N2—C11—C12127.4 (3)
N4—Co1—N3—C13−119.8 (3)C14—N3—C15—C16−87.8 (4)
Cl1—Co1—N3—C13137.4 (3)C13—N3—C15—C16153.4 (3)
N1—Co1—N3—C15112.6 (3)Co1—N3—C15—C1631.2 (4)
N4—Co1—N3—C15−2.8 (3)C18—N4—C16—C15−71.2 (4)
Cl1—Co1—N3—C15−105.6 (2)C17—N4—C16—C15170.5 (3)
N1—Co1—N4—C18−23.7 (3)Co1—N4—C16—C1549.7 (4)
N3—Co1—N4—C1894.3 (2)N3—C15—C16—N4−58.0 (5)
Cl1—Co1—N4—C18−157.4 (2)
  5 in total

1.  Highlights in the Renaissance of Amidometal Chemistry.

Authors: 
Journal:  Angew Chem Int Ed Engl       Date:  2000-02       Impact factor: 15.336

2.  Structural and Functional Aspects of Metal Sites in Biology.

Authors:  Richard H. Holm; Pierre Kennepohl; Edward I. Solomon
Journal:  Chem Rev       Date:  1996-11-07       Impact factor: 60.622

3.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

4.  Chloridobis{N-[(dimethyl-amino)dimethyl-silyl]-2,6-dimethyl-anilido-κN,N'}iron(III).

Authors:  Juan Chen
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2008-06-19

5.  Dichloridobis{N-[(dimethyl-amino)dimethyl-silyl]-2,6-dimethyl-anilido-κN,N'}zirconium(IV).

Authors:  Juan Chen
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-10-07
  5 in total

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