Di-μ-hydro­xo-bis[(N,N,N′,N′-tetra­methyl­ethyl­enedi­amine)copper(II)] dichloride from X-ray powder data

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 Cu...Cu 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 [O...Cl = 2.993 (14) Å].

Key indicators

• Powder X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.018 Å
• R factor = 0.000
• wR factor = 0.000
• Data-to-parameter ratio = 0.0

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT023_ALERT_3_A Resolution (too) Low [sin(th)/Lambda < 0.6].....       0.00 Deg.
PLAT037_ALERT_1_A _diffrn_reflns_theta_full .......... Not Given .          ?
PLAT038_ALERT_1_A _diffrn_measured_fraction_theta_max  Not Given .          ?
PLAT039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given .          ?

Alert level B
PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) .......          6
PLAT210_ALERT_3_B No Anisotropic ADP's Found in CIF ..............          ?
PLAT341_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ...         18
PLAT411_ALERT_2_B Short Inter H...H Contact  H1A    ..  H1A     ..       2.06 Ang.

Alert level C
RADNW01_ALERT_1_C  The radiation wavelength lies outside the expected range
            for the supplied radiation type. Expected range 1.54175-1.54180
            Wavelength given =    1.54060

Author Response: The focussing monochromator strips only K\a~1~

PLAT030_ALERT_1_C _diffrn_reflns_number .LE. _reflns_number_total .         ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT087_ALERT_2_C Unsatisfactory S value (Too High) ..............       3.70
PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          1
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors  for        Cu1
PLAT360_ALERT_2_C Short  C(sp3)-C(sp3) Bond  C1     -   C1_a   ...       1.40 Ang.

Author Response: See _publ_section_comment

Alert level G
RADNT01_ALERT_1_G  Extra text has been found in the _diffrn_radiation_type field.
            Radiation given as Cu K\a~1~
            Radiation identified as Cu K\a

   4 ALERT level A = In general: serious problem
   4 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

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

Crystal data

[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) Å^3	flat_sheet, 15 × 15 mm
Z = 8

Data collection

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

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 (Ų)

	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)

Cu1—N1	2.088 (11)	C3—H3A	0.95
Cu1—O1	1.956 (8)	C3—H3B	0.96
C1—C1^i	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—C1^i	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.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···Cl1	0.93	2.06	2.993 (14)	180