metal-organic compounds
The crystal structure of the title complex, [Cu2(OH)2(TMEDA)2]Cl2 (TMEDA is N,N,N′,N′-tetramethylethylenediamine, C6H16N2), has been characterized by X-ray powder diffraction. The cation is a binuclear complex with a CuCu distance of 3.031 (7) Å and occupies a special position of 222 symmetry, while the chloride anions are on a twofold axis. There is a hydrogen bond linking a bridging hydroxy group with the anion [OCl = 2.993 (14) Å].
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804018264/ya6211sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S1600536804018264/ya6211Isup2.rtv |
CCDC reference: 248760
Computing details top
Data collection: HUBER G670 (Huber, 1998); cell refinement: MRIA (Zlokazov & Chernyshev, 1992); program(s) used to solve structure: MRIA, SHELXS97 and SHELXL97 (Sheldrick, 1997); program(s) used to refine structure: MRIA; molecular graphics: PLUTON (Spek, 1996); software used to prepare material for publication: MRIA, SHELXL, PARST (Nardelli, 1995).
Di-µ-hydroxo-[(N,N,N',N'-tetramethylethylenediamine)copper(II)] dichloride top
Crystal data top
[Cu2(OH)2(C6H16N2)2]Cl2 | F(000) = 1936 |
Mr = 464.43 | Dx = 1.610 Mg m−3 |
Orthorhombic, Fddd | Cu Kα1 radiation, λ = 1.54060 Å |
Hall symbol: -F 2uv 2vw | µ = 5.40 mm−1 |
a = 16.612 (9) Å | T = 295 K |
b = 18.311 (9) Å | Particle morphology: lump-like |
c = 12.598 (7) Å | colourless |
V = 3832 (4) Å3 | flat_sheet, 15 × 15 mm |
Z = 8 |
Data collection top
Huber Guinier camera G670 diffractometer | Data collection mode: transmission |
Radiation source: Fine focus sealed X-ray tube, Crystalloflex | Scan method: step |
Ge focussing monochromator | 2θmin = 5.00°, 2θmax = 100.00°, 2θstep = 0.01° |
Specimen mounting: pressed as a thin layer in the specimen holder of the camera |
Refinement top
Refinement on Inet | 7 restraints |
Least-squares matrix: full with fixed elements per cycle | 0 constraints |
Rp = 0.023 | H-atom parameters not refined |
Rwp = 0.033 | Weighting scheme based on measured s.u.'s |
Rexp = 0.009 | (Δ/σ)max = 0.02 |
9501 data points | Background function: Chebyshev polynomial up to the 5th order |
Profile function: split-type pseudo-Voigt | Preferred orientation correction: none |
72 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cu1 | 0.1250 | 0.1250 | 0.5047 (4) | 0.078 (2)* | |
Cl1 | 0.3797 (5) | 0.1250 | 0.6250 | 0.0392 (7)* | |
C1 | 0.1641 (7) | 0.111 (1) | 0.2584 (9) | 0.0391 (7)* | |
C2 | 0.2545 (8) | 0.1892 (8) | 0.380 (3) | 0.0393 (4)* | |
C3 | 0.2473 (8) | 0.0604 (8) | 0.401 (2) | 0.0684 (7)* | |
N1 | 0.1990 (6) | 0.1245 (8) | 0.3707 (8) | 0.0592 (3)* | |
O1 | 0.1995 (7) | 0.1250 | 0.6250 | 0.0395 (5)* | |
H2A | 0.2249 | 0.2331 | 0.3612 | 0.0500* | |
H2B | 0.2987 | 0.1836 | 0.3320 | 0.0500* | |
H2C | 0.2735 | 0.1936 | 0.4511 | 0.0500* | |
H3A | 0.2155 | 0.0172 | 0.3963 | 0.0500* | |
H3B | 0.2675 | 0.0665 | 0.4716 | 0.0500* | |
H3C | 0.2927 | 0.0564 | 0.3525 | 0.0500* | |
H1 | 0.2556 | 0.1250 | 0.6250 | 0.0500* | |
H1A | 0.1971 | 0.1345 | 0.2055 | 0.0500* | |
H1B | 0.1631 | 0.0585 | 0.2433 | 0.0500* |
Geometric parameters (Å, º) top
Cu1—N1 | 2.088 (11) | C3—H3A | 0.95 |
Cu1—O1 | 1.956 (8) | C3—H3B | 0.96 |
C1—C1i | 1.397 (17) | C3—H3C | 0.97 |
C2—N1 | 1.505 (19) | N1—C1 | 1.549 (16) |
C2—H2A | 0.97 | O1—H1 | 0.93 |
C2—H2B | 0.95 | C1—H1A | 0.96 |
C2—H2C | 0.95 | C1—H1B | 0.98 |
C3—N1 | 1.47 (2) | ||
N1—Cu1—O1 | 104.7 (3) | H3A—C3—H3C | 109.3 |
N1—C1—C1i | 106.8 (12) | H3B—C3—H3C | 108.6 |
N1—C2—H2A | 108.8 | Cu1—N1—C2 | 107.1 (9) |
N1—C2—H2B | 109.7 | Cu1—N1—C3 | 96.7 (9) |
N1—C2—H2C | 110.0 | Cu1—N1—C1 | 121.2 (7) |
H2A—C2—H2B | 108.9 | C2—N1—C3 | 105.9 (12) |
H2A—C2—H2C | 109.0 | C2—N1—C1 | 115.4 (11) |
H2B—C2—H2C | 110.4 | C3—N1—C1 | 107.9 (11) |
N1—C3—H3A | 110.2 | Cu1—O1—H1 | 129.2 |
N1—C3—H3B | 109.7 | N1—C1—H1A | 110.0 |
N1—C3—H3C | 108.8 | N1—C1—H1B | 109.9 |
H3A—C3—H3B | 110.1 | H1A—C1—H1B | 108.9 |
Symmetry code: (i) −x+1/4, −y+1/4, z. |