The title complex, [Cu(S
2O
3)(C
2H
8N
2)
2], exhibits a slightly distorted square-pyramidal geometry. The copper(II) atom is five-coordinated by four N atoms from two ethylenediamine molecules, and one S-atom from the thiosulfate anion. The crystal structure is stabilized by weak intermolecular Cu
S interactions and N—H
O hydrogen bonds.
Supporting information
CCDC reference: 216841
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.038
- wR factor = 0.099
- Data-to-parameter ratio = 14.9
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cu1 - S2 .. 48.24 su
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for S1
Alert level C
PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1A ... ?
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
Di(ethylendiamine-K2N,
N')(thiosulfato-KS) copper(II)
top
Crystal data top
[Cu(S2O3)(C2H8N2)2] | F(000) = 612 |
Mr = 295.87 | Dx = 1.803 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 1942 reflections |
a = 6.613 (2) Å | θ = 2.9–26.4° |
b = 11.858 (4) Å | µ = 2.38 mm−1 |
c = 13.936 (5) Å | T = 293 K |
β = 94.216 (4)° | Block, blue |
V = 1089.8 (6) Å3 | 0.29 × 0.17 × 0.15 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1893 independent reflections |
Radiation source: fine-focus sealed tube | 1356 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
φ and ο scans | θmax = 25.0°, θmin = 3.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −6→7 |
Tmin = 0.535, Tmax = 0.703 | k = −11→14 |
5507 measured reflections | l = −16→16 |
Refinement top
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.099 | H-atom parameters constrained |
S = 0.93 | w = 1/[σ2(Fo2) + (0.0621P)2] where P = (Fo2 + 2Fc2)/3 |
1893 reflections | (Δ/σ)max < 0.001 |
127 parameters | Δρmax = 0.56 e Å−3 |
0 restraints | Δρmin = −0.76 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 0.23342 (6) | 0.37955 (4) | 0.25294 (3) | 0.03270 (19) | |
N1 | 0.4436 (4) | 0.3795 (2) | 0.3655 (2) | 0.0316 (7) | |
H1A | 0.5159 | 0.3152 | 0.3664 | 0.038* | |
H1B | 0.5292 | 0.4380 | 0.3609 | 0.038* | |
N2 | 0.0405 (4) | 0.3327 (2) | 0.35177 (19) | 0.0301 (6) | |
H2A | −0.0506 | 0.3878 | 0.3590 | 0.036* | |
H2B | −0.0270 | 0.2701 | 0.3316 | 0.036* | |
N3 | 0.4317 (4) | 0.4086 (2) | 0.15242 (19) | 0.0288 (6) | |
H3A | 0.5062 | 0.4703 | 0.1682 | 0.035* | |
H3B | 0.5163 | 0.3495 | 0.1491 | 0.035* | |
N4 | 0.0265 (4) | 0.3659 (2) | 0.1398 (2) | 0.0321 (7) | |
H4A | −0.0556 | 0.3067 | 0.1481 | 0.039* | |
H4B | −0.0498 | 0.4287 | 0.1343 | 0.039* | |
O1 | −0.2113 (4) | 0.7270 (2) | 0.2982 (2) | 0.0639 (9) | |
O2 | −0.2132 (4) | 0.5309 (2) | 0.3329 (2) | 0.0553 (8) | |
O3 | −0.2276 (5) | 0.5910 (3) | 0.1707 (2) | 0.0784 (11) | |
S1 | −0.14657 (12) | 0.61659 (7) | 0.26698 (6) | 0.0256 (2) | |
S2 | 0.15847 (13) | 0.61592 (7) | 0.27158 (8) | 0.0377 (3) | |
C1 | 0.3348 (5) | 0.3892 (3) | 0.4536 (2) | 0.0339 (8) | |
H1C | 0.2895 | 0.4662 | 0.4616 | 0.041* | |
H1D | 0.4237 | 0.3688 | 0.5093 | 0.041* | |
C2 | 0.1548 (5) | 0.3105 (3) | 0.4441 (2) | 0.0374 (9) | |
H2C | 0.2006 | 0.2328 | 0.4466 | 0.045* | |
H2D | 0.0688 | 0.3230 | 0.4966 | 0.045* | |
C3 | 0.3184 (5) | 0.4255 (3) | 0.0591 (2) | 0.0371 (8) | |
H3C | 0.4040 | 0.4080 | 0.0075 | 0.044* | |
H3D | 0.2760 | 0.5036 | 0.0525 | 0.044* | |
C4 | 0.1363 (6) | 0.3499 (3) | 0.0531 (3) | 0.0397 (9) | |
H4C | 0.0487 | 0.3682 | −0.0037 | 0.048* | |
H4D | 0.1784 | 0.2718 | 0.0483 | 0.048* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0209 (3) | 0.0508 (3) | 0.0264 (3) | −0.00972 (19) | 0.00164 (17) | 0.00214 (19) |
N1 | 0.0252 (15) | 0.0331 (16) | 0.0364 (16) | −0.0048 (12) | 0.0012 (12) | 0.0001 (12) |
N2 | 0.0269 (15) | 0.0287 (15) | 0.0352 (16) | −0.0039 (13) | 0.0048 (12) | 0.0014 (13) |
N3 | 0.0238 (15) | 0.0284 (16) | 0.0344 (16) | −0.0024 (12) | 0.0031 (12) | 0.0024 (12) |
N4 | 0.0217 (15) | 0.0388 (18) | 0.0362 (16) | −0.0062 (12) | 0.0043 (12) | 0.0020 (12) |
O1 | 0.0254 (13) | 0.0318 (15) | 0.135 (3) | 0.0070 (12) | 0.0084 (15) | −0.0178 (17) |
O2 | 0.0358 (15) | 0.0499 (17) | 0.082 (2) | 0.0017 (13) | 0.0193 (14) | 0.0256 (15) |
O3 | 0.0515 (19) | 0.143 (3) | 0.0387 (17) | −0.002 (2) | −0.0122 (14) | −0.0069 (19) |
S1 | 0.0210 (4) | 0.0241 (5) | 0.0318 (5) | 0.0000 (3) | 0.0025 (3) | −0.0004 (3) |
S2 | 0.0215 (5) | 0.0248 (5) | 0.0678 (7) | 0.0009 (4) | 0.0090 (4) | 0.0000 (4) |
C1 | 0.035 (2) | 0.038 (2) | 0.0284 (18) | 0.0002 (16) | −0.0002 (15) | −0.0002 (16) |
C2 | 0.038 (2) | 0.040 (2) | 0.0336 (19) | −0.0044 (17) | 0.0039 (15) | 0.0096 (16) |
C3 | 0.033 (2) | 0.045 (2) | 0.034 (2) | −0.0084 (17) | 0.0056 (15) | 0.0063 (17) |
C4 | 0.036 (2) | 0.050 (2) | 0.033 (2) | −0.0082 (18) | −0.0006 (16) | −0.0027 (17) |
Geometric parameters (Å, º) top
Cu1—N4 | 2.016 (3) | N4—H4A | 0.9000 |
Cu1—N1 | 2.017 (3) | N4—H4B | 0.9000 |
Cu1—N3 | 2.018 (3) | O1—S1 | 1.454 (3) |
Cu1—N2 | 2.023 (3) | O2—S1 | 1.459 (3) |
Cu1—S2 | 2.8614 (13) | O3—S1 | 1.441 (3) |
Cu1—S2i | 3.2304 (14) | S1—S2 | 2.0134 (13) |
N1—C1 | 1.473 (4) | C1—C2 | 1.510 (5) |
N1—H1A | 0.9000 | C1—H1C | 0.9700 |
N1—H1B | 0.9000 | C1—H1D | 0.9700 |
N2—C2 | 1.467 (4) | C2—H2C | 0.9700 |
N2—H2A | 0.9000 | C2—H2D | 0.9700 |
N2—H2B | 0.9000 | C3—C4 | 1.498 (5) |
N3—C3 | 1.466 (4) | C3—H3C | 0.9700 |
N3—H3A | 0.9000 | C3—H3D | 0.9700 |
N3—H3B | 0.9000 | C4—H4C | 0.9700 |
N4—C4 | 1.468 (4) | C4—H4D | 0.9700 |
| | | |
N4—Cu1—N1 | 175.32 (11) | Cu1—N4—H4A | 110.1 |
N4—Cu1—N3 | 84.79 (11) | C4—N4—H4B | 110.1 |
N1—Cu1—N3 | 95.39 (11) | Cu1—N4—H4B | 110.1 |
N4—Cu1—N2 | 94.85 (11) | H4A—N4—H4B | 108.5 |
N1—Cu1—N2 | 84.47 (11) | O3—S1—O1 | 111.8 (2) |
N3—Cu1—N2 | 173.87 (11) | O3—S1—O2 | 109.3 (2) |
N4—Cu1—S2 | 92.16 (8) | O1—S1—O2 | 109.21 (19) |
N1—Cu1—S2 | 92.51 (8) | O3—S1—S2 | 109.39 (14) |
N3—Cu1—S2 | 91.24 (8) | O1—S1—S2 | 108.09 (11) |
N2—Cu1—S2 | 94.89 (9) | O2—S1—S2 | 109.00 (11) |
N4—Cu1—S2i | 88.98 (8) | S1—S2—Cu1 | 100.42 (4) |
N1—Cu1—S2i | 86.37 (8) | N1—C1—C2 | 108.0 (3) |
N3—Cu1—S2i | 86.07 (8) | N1—C1—H1C | 110.1 |
N2—Cu1—S2i | 87.80 (9) | C2—C1—H1C | 110.1 |
S2—Cu1—S2i | 176.975 (16) | N1—C1—H1D | 110.1 |
C1—N1—Cu1 | 107.3 (2) | C2—C1—H1D | 110.1 |
C1—N1—H1A | 110.3 | H1C—C1—H1D | 108.4 |
Cu1—N1—H1A | 110.3 | N2—C2—C1 | 108.6 (3) |
C1—N1—H1B | 110.3 | N2—C2—H2C | 110.0 |
Cu1—N1—H1B | 110.3 | C1—C2—H2C | 110.0 |
H1A—N1—H1B | 108.5 | N2—C2—H2D | 110.0 |
C2—N2—Cu1 | 109.7 (2) | C1—C2—H2D | 110.0 |
C2—N2—H2A | 109.7 | H2C—C2—H2D | 108.4 |
Cu1—N2—H2A | 109.7 | N3—C3—C4 | 108.9 (3) |
C2—N2—H2B | 109.7 | N3—C3—H3C | 109.9 |
Cu1—N2—H2B | 109.7 | C4—C3—H3C | 109.9 |
H2A—N2—H2B | 108.2 | N3—C3—H3D | 109.9 |
C3—N3—Cu1 | 108.9 (2) | C4—C3—H3D | 109.9 |
C3—N3—H3A | 109.9 | H3C—C3—H3D | 108.3 |
Cu1—N3—H3A | 109.9 | N4—C4—C3 | 108.7 (3) |
C3—N3—H3B | 109.9 | N4—C4—H4C | 110.0 |
Cu1—N3—H3B | 109.9 | C3—C4—H4C | 110.0 |
H3A—N3—H3B | 108.3 | N4—C4—H4D | 110.0 |
C4—N4—Cu1 | 107.8 (2) | C3—C4—H4D | 110.0 |
C4—N4—H4A | 110.1 | H4C—C4—H4D | 108.3 |
| | | |
N1—C1—C2—N2 | −51.3 (4) | N3—C3—C4—N4 | 50.9 (4) |
Symmetry code: (i) −x+1/2, y−1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1B···O2ii | 0.90 | 2.09 | 2.955 (4) | 161 |
N2—H2A···O2 | 0.90 | 2.03 | 2.889 (4) | 160 |
N2—H2B···O1iii | 0.90 | 2.46 | 3.164 (4) | 135 |
N3—H3B···O1i | 0.90 | 2.04 | 2.888 (4) | 156 |
N4—H4A···O1iii | 0.90 | 2.00 | 2.840 (4) | 155 |
N4—H4B···O3 | 0.90 | 2.33 | 3.201 (5) | 163 |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) x+1, y, z; (iii) −x−1/2, y−1/2, −z+1/2. |