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The crystal structure of the title complex, [Cu
2(OH)
2(TMEDA)
2]Cl
2 (TMEDA is
N,
N,
N′,
N′-tetramethylethylenediamine, C
6H
16N
2), 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].
Supporting information
CCDC reference: 248760
Key indicators
- Powder X-ray study
- T = 295 K
- Mean (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
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. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···Cl1 | 0.93 | 2.06 | 2.993 (14) | 180 |
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