Literature DB >> 21582350

[μ-Bis(trimethyl-silyl)amido]bis-[μ-N,N-dimethyl-N',N''-bis-(trimethyl-silyl)guanidinato]-triangulo-tricopper(I).

Donglong Guo, Xiaoli Qiao, Hong-Bo Tong, Meisu Zhou.

Abstract

The title compound, [Cu(3)(C(6)H(18)NSi(2))(C(9)H(24)N(3)Si(2))(2)], is a trinuclear Cu(I) complex. A crystallographic twofold axis passes through one Cu(I) atom and the N atom of the bis-(trimethyl-silyl)amide ligand that bridges between the other two Cu(I) atoms. The Cu-Cu bonds bridged by the guanadinate ligands [2.7913 (9) Å] are slightly longer than the Cu-Cu bond bridged by the bis-(trimethyl-silyl)amide ligand [2.6405 (11) Å].

Entities: CellLine Chemical Disease Gene

Year: 2009 PMID： 21582350 PMCID： PMC2968876 DOI： 10.1107/S1600536809008745

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

Related literature

For background literature concerning the coordination chemistry of guanidinates, see: Chandra et al. (1970 ▶); Barker & Kilner (1994 ▶); Edelmann (1994 ▶); Bailey & Pace (2001 ▶); Zhou et al. (2007 ▶).

Experimental

Crystal data

[Cu3(C6H18NSi2)(C9H24N3Si2)2] M = 812.00 Monoclinic, a = 16.445 (3) Å b = 18.653 (4) Å c = 14.046 (3) Å β = 96.943 (3)° V = 4277.1 (15) Å3 Z = 4 Mo Kα radiation μ = 1.67 mm−1 T = 213 K 0.30 × 0.20 × 0.20 mm

Data collection

Siemens SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1997 ▶) T min = 0.622, T max = 0.717 8714 measured reflections 3773 independent reflections 3394 reflections with I > 2σ(I) R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.056 wR(F 2) = 0.118 S = 1.26 3773 reflections 193 parameters H-atom parameters constrained Δρmax = 0.57 e Å−3 Δρmin = −0.46 e Å−3 Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809008745/bi2357sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809008745/bi2357Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cu₃(C₆H₁₈NSi₂)(C₉H₂₄N₃Si₂)₂]	F(000) = 1720
M_r = 812.00	D_x = 1.261 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3322 reflections
a = 16.445 (3) Å	θ = 2.3–27.5°
b = 18.653 (4) Å	µ = 1.67 mm⁻¹
c = 14.046 (3) Å	T = 213 K
β = 96.943 (3)°	Block, colourless
V = 4277.1 (15) Å³	0.30 × 0.20 × 0.20 mm
Z = 4

Siemens SMART CCD diffractometer	3773 independent reflections
Radiation source: fine-focus sealed tube	3394 reflections with I > 2σ(I)
graphite	R_int = 0.033
ω scans	θ_max = 25.0°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1997)	h = −19→16
T_min = 0.622, T_max = 0.717	k = −21→22
8714 measured reflections	l = −16→15

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)] = 0.056	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.118	H-atom parameters constrained
S = 1.26	w = 1/[σ²(F_o²) + (0.0417P)² + 4.1466P] where P = (F_o² + 2F_c²)/3
3773 reflections	(Δ/σ)_max < 0.001
193 parameters	Δρ_max = 0.57 e Å⁻³
0 restraints	Δρ_min = −0.46 e Å⁻³

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.

	x	y	z	U_iso*/U_eq
Cu1	0.00565 (3)	0.28899 (3)	0.65704 (4)	0.03181 (17)
Cu2	0.0000	0.15714 (4)	0.7500	0.0297 (2)
N1	0.0253 (2)	0.22736 (18)	0.5568 (2)	0.0335 (8)
N2	0.1160 (3)	0.1407 (2)	0.5116 (3)	0.0489 (11)
N3	0.0812 (2)	0.14177 (18)	0.6683 (3)	0.0327 (8)
N4	0.0000	0.3629 (2)	0.7500	0.0331 (12)
Si1	−0.03059 (9)	0.24764 (8)	0.44721 (9)	0.0484 (4)
Si2	0.16644 (8)	0.10002 (7)	0.73019 (10)	0.0384 (3)
Si3	0.09487 (9)	0.40530 (7)	0.75808 (11)	0.0444 (4)
C1	0.0727 (3)	0.1708 (2)	0.5803 (3)	0.0326 (10)
C2	0.1565 (4)	0.1842 (3)	0.4465 (4)	0.0711 (18)
H2A	0.1295	0.1780	0.3817	0.107*
H2B	0.2134	0.1697	0.4493	0.107*
H2C	0.1538	0.2342	0.4648	0.107*
C3	0.1235 (4)	0.0641 (3)	0.5000 (4)	0.077 (2)
H3A	0.0899	0.0397	0.5419	0.116*
H3B	0.1803	0.0501	0.5163	0.116*
H3C	0.1055	0.0512	0.4339	0.116*
C4	−0.0495 (4)	0.1674 (4)	0.3693 (4)	0.085 (2)
H4A	0.0018	0.1512	0.3490	0.127*
H4B	−0.0875	0.1796	0.3133	0.127*
H4C	−0.0726	0.1294	0.4048	0.127*
C5	0.0166 (4)	0.3231 (4)	0.3864 (5)	0.087 (2)
H5A	0.0322	0.3609	0.4325	0.131*
H5B	−0.0226	0.3417	0.3352	0.131*
H5C	0.0648	0.3060	0.3598	0.131*
C6	−0.1333 (3)	0.2798 (4)	0.4694 (4)	0.0747 (19)
H6A	−0.1633	0.2407	0.4946	0.112*
H6B	−0.1629	0.2966	0.4097	0.112*
H6C	−0.1273	0.3187	0.5155	0.112*
C7	0.2640 (3)	0.1337 (3)	0.6908 (4)	0.0577 (15)
H7A	0.2668	0.1196	0.6248	0.087*
H7B	0.3102	0.1133	0.7315	0.087*
H7C	0.2658	0.1855	0.6957	0.087*
C8	0.1675 (3)	0.1227 (3)	0.8591 (4)	0.0543 (14)
H8A	0.1733	0.1742	0.8675	0.081*
H8B	0.2131	0.0987	0.8962	0.081*
H8C	0.1165	0.1072	0.8809	0.081*
C9	0.1591 (4)	0.0000 (2)	0.7255 (4)	0.0586 (15)
H9A	0.1034	−0.0146	0.7321	0.088*
H9B	0.1962	−0.0205	0.7774	0.088*
H9C	0.1738	−0.0169	0.6646	0.088*
C10	0.1033 (4)	0.4625 (3)	0.6504 (5)	0.085 (2)
H10A	0.0660	0.5027	0.6504	0.128*
H10B	0.0894	0.4343	0.5927	0.128*
H10C	0.1590	0.4801	0.6523	0.128*
C11	0.1138 (4)	0.4635 (3)	0.8661 (5)	0.080 (2)
H11A	0.0990	0.4379	0.9216	0.120*
H11B	0.0808	0.5067	0.8564	0.120*
H11C	0.1713	0.4765	0.8767	0.120*
C12	0.1783 (3)	0.3378 (3)	0.7637 (4)	0.0574 (15)
H12A	0.2309	0.3620	0.7708	0.086*
H12B	0.1725	0.3097	0.7052	0.086*
H12C	0.1751	0.3064	0.8182	0.086*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.0350 (3)	0.0301 (3)	0.0309 (3)	0.0019 (2)	0.0064 (2)	0.0008 (2)
Cu2	0.0272 (4)	0.0326 (4)	0.0308 (4)	0.000	0.0095 (3)	0.000
N1	0.037 (2)	0.040 (2)	0.0247 (19)	0.0004 (18)	0.0059 (15)	−0.0007 (16)
N2	0.058 (3)	0.053 (3)	0.040 (2)	0.002 (2)	0.025 (2)	−0.0066 (19)
N3	0.032 (2)	0.0316 (19)	0.037 (2)	0.0019 (16)	0.0125 (16)	−0.0031 (16)
N4	0.035 (3)	0.031 (3)	0.035 (3)	0.000	0.007 (2)	0.000
Si1	0.0512 (9)	0.0670 (10)	0.0269 (7)	−0.0083 (7)	0.0038 (6)	0.0050 (6)
Si2	0.0318 (7)	0.0326 (7)	0.0523 (8)	0.0043 (6)	0.0111 (6)	0.0007 (6)
Si3	0.0451 (8)	0.0317 (7)	0.0583 (9)	−0.0068 (6)	0.0139 (7)	−0.0011 (6)
C1	0.032 (3)	0.039 (3)	0.029 (2)	−0.008 (2)	0.0146 (19)	−0.0080 (19)
C2	0.065 (4)	0.104 (5)	0.051 (4)	0.006 (4)	0.033 (3)	0.002 (3)
C3	0.106 (5)	0.069 (4)	0.060 (4)	0.018 (4)	0.024 (4)	−0.023 (3)
C4	0.082 (5)	0.118 (6)	0.052 (4)	−0.026 (4)	−0.003 (3)	−0.024 (4)
C5	0.092 (5)	0.107 (5)	0.062 (4)	−0.017 (4)	0.005 (4)	0.042 (4)
C6	0.061 (4)	0.107 (5)	0.054 (4)	0.014 (4)	−0.004 (3)	0.017 (3)
C7	0.035 (3)	0.056 (3)	0.085 (4)	0.002 (3)	0.020 (3)	0.007 (3)
C8	0.048 (3)	0.053 (3)	0.059 (3)	0.007 (3)	−0.003 (3)	0.004 (3)
C9	0.063 (4)	0.038 (3)	0.077 (4)	0.007 (3)	0.019 (3)	0.005 (3)
C10	0.074 (5)	0.074 (4)	0.109 (6)	−0.022 (4)	0.017 (4)	0.041 (4)
C11	0.074 (4)	0.064 (4)	0.105 (5)	−0.029 (3)	0.021 (4)	−0.042 (4)
C12	0.041 (3)	0.046 (3)	0.086 (4)	−0.008 (2)	0.013 (3)	−0.010 (3)

Cu1—Cu1ⁱ	2.6405 (11)	C3—H3B	0.970
Cu1—Cu2	2.7913 (9)	C3—H3C	0.970
Cu2—Cu1ⁱ	2.7912 (9)	C4—H4A	0.970
Cu1—N1	1.875 (3)	C4—H4B	0.970
Cu1—N4	1.908 (3)	C4—H4C	0.970
Cu2—N3	1.885 (3)	C5—H5A	0.970
Cu2—N3ⁱ	1.885 (3)	C5—H5B	0.970
N1—C1	1.329 (5)	C5—H5C	0.970
N1—Si1	1.737 (4)	C6—H6A	0.970
N2—C1	1.386 (5)	C6—H6B	0.970
N2—C3	1.444 (6)	C6—H6C	0.970
N2—C2	1.445 (6)	C7—H7A	0.970
N3—C1	1.341 (5)	C7—H7B	0.970
N3—Si2	1.742 (4)	C7—H7C	0.970
N4—Si3	1.741 (3)	C8—H8A	0.970
N4—Si3ⁱ	1.741 (3)	C8—H8B	0.970
N4—Cu1ⁱ	1.909 (3)	C8—H8C	0.970
Si1—C6	1.853 (6)	C9—H9A	0.970
Si1—C4	1.859 (6)	C9—H9B	0.970
Si1—C5	1.865 (6)	C9—H9C	0.970
Si2—C8	1.858 (5)	C10—H10A	0.970
Si2—C7	1.868 (5)	C10—H10B	0.970
Si2—C9	1.871 (5)	C10—H10C	0.970
Si3—C12	1.856 (5)	C11—H11A	0.970
Si3—C11	1.862 (6)	C11—H11B	0.970
Si3—C10	1.870 (6)	C11—H11C	0.970
C2—H2A	0.970	C12—H12A	0.970
C2—H2B	0.970	C12—H12B	0.970
C2—H2C	0.970	C12—H12C	0.970
C3—H3A	0.970

N1—Cu1—N4	169.49 (13)	N2—C3—H3C	109.5
N1—Cu1—Cu1ⁱ	141.39 (11)	H3A—C3—H3C	109.5
N4—Cu1—Cu1ⁱ	46.23 (10)	H3B—C3—H3C	109.5
N1—Cu1—Cu2	80.18 (11)	Si1—C4—H4A	109.5
N4—Cu1—Cu2	108.00 (10)	Si1—C4—H4B	109.5
Cu1ⁱ—Cu1—Cu2	61.768 (14)	H4A—C4—H4B	109.5
N3—Cu2—N3ⁱ	162.5 (2)	Si1—C4—H4C	109.5
N3—Cu2—Cu1ⁱ	119.01 (11)	H4A—C4—H4C	109.5
N3ⁱ—Cu2—Cu1ⁱ	77.47 (10)	H4B—C4—H4C	109.5
N3—Cu2—Cu1	77.47 (10)	Si1—C5—H5A	109.5
N3ⁱ—Cu2—Cu1	119.02 (11)	Si1—C5—H5B	109.5
Cu1ⁱ—Cu2—Cu1	56.46 (3)	H5A—C5—H5B	109.5
C1—N1—Si1	128.6 (3)	Si1—C5—H5C	109.5
C1—N1—Cu1	116.7 (3)	H5A—C5—H5C	109.5
Si1—N1—Cu1	114.3 (2)	H5B—C5—H5C	109.5
C1—N2—C3	122.5 (4)	Si1—C6—H6A	109.5
C1—N2—C2	121.9 (4)	Si1—C6—H6B	109.5
C3—N2—C2	115.6 (4)	H6A—C6—H6B	109.5
C1—N3—Si2	129.0 (3)	Si1—C6—H6C	109.5
C1—N3—Cu2	119.8 (3)	H6A—C6—H6C	109.5
Si2—N3—Cu2	110.53 (19)	H6B—C6—H6C	109.5
Si3—N4—Si3ⁱ	125.9 (3)	Si2—C7—H7A	109.5
Si3—N4—Cu1	104.80 (7)	Si2—C7—H7B	109.5
Si3ⁱ—N4—Cu1	113.64 (8)	H7A—C7—H7B	109.5
Si3—N4—Cu1ⁱ	113.64 (8)	Si2—C7—H7C	109.5
Si3ⁱ—N4—Cu1ⁱ	104.80 (7)	H7A—C7—H7C	109.5
Cu1—N4—Cu1ⁱ	87.5 (2)	H7B—C7—H7C	109.5
N1—Si1—C6	108.5 (2)	Si2—C8—H8A	109.5
N1—Si1—C4	112.3 (3)	Si2—C8—H8B	109.5
C6—Si1—C4	105.6 (3)	H8A—C8—H8B	109.5
N1—Si1—C5	111.4 (3)	Si2—C8—H8C	109.5
C6—Si1—C5	105.7 (3)	H8A—C8—H8C	109.5
C4—Si1—C5	112.8 (3)	H8B—C8—H8C	109.5
N3—Si2—C8	107.3 (2)	Si2—C9—H9A	109.5
N3—Si2—C7	111.7 (2)	Si2—C9—H9B	109.5
C8—Si2—C7	107.8 (3)	H9A—C9—H9B	109.5
N3—Si2—C9	112.6 (2)	Si2—C9—H9C	109.5
C8—Si2—C9	104.8 (2)	H9A—C9—H9C	109.5
C7—Si2—C9	112.3 (2)	H9B—C9—H9C	109.5
N4—Si3—C12	110.3 (2)	Si3—C10—H10A	109.5
N4—Si3—C11	112.2 (2)	Si3—C10—H10B	109.5
C12—Si3—C11	108.1 (3)	H10A—C10—H10B	109.5
N4—Si3—C10	111.1 (2)	Si3—C10—H10C	109.5
C12—Si3—C10	107.1 (3)	H10A—C10—H10C	109.5
C11—Si3—C10	107.7 (3)	H10B—C10—H10C	109.5
N1—C1—N3	122.8 (3)	Si3—C11—H11A	109.5
N1—C1—N2	119.0 (4)	Si3—C11—H11B	109.5
N3—C1—N2	118.2 (4)	H11A—C11—H11B	109.5
N2—C2—H2A	109.5	Si3—C11—H11C	109.5
N2—C2—H2B	109.5	H11A—C11—H11C	109.5
H2A—C2—H2B	109.5	H11B—C11—H11C	109.5
N2—C2—H2C	109.5	Si3—C12—H12A	109.5
H2A—C2—H2C	109.5	Si3—C12—H12B	109.5
H2B—C2—H2C	109.5	H12A—C12—H12B	109.5
N2—C3—H3A	109.5	Si3—C12—H12C	109.5
N2—C3—H3B	109.5	H12A—C12—H12C	109.5
H3A—C3—H3B	109.5	H12B—C12—H12C	109.5

1 in total

1. A short history of SHELX.

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

1 in total

1. Bis{μ-N-[(dimethyl-amino)-dimethyl-sil-yl]-2,6-dimethyl-anilido}-κN:N';κN':N-dicopper(I).

Authors: Juan Chen
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2010-10-30

1 in total