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The title complex, [Zn(C2H8N2)3][Cu(C4N2S2)2], exists as discrete ions. The cation lies on a twofold rotation axis and the anion lies on an inversion centre. The [Zn(C2H8N2)3]2+ cation exhibits a distorted octahedral geometry. In the [Cu(C4N2S2)2]2− anion, the CuII atom is in a slightly distorted square-planar environment. The crystal packing is stabilized by hydrogen bonds of the types N—H...N and N—H...S.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804029630/ci6485sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804029630/ci6485Isup2.hkl
Contains datablock I

CCDC reference: 179825

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.025
  • wR factor = 0.065
  • Data-to-parameter ratio = 15.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT230_ALERT_2_C Hirshfeld Test Diff for C4 - C5 .. 5.02 su PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C4 - C5 ... 1.44 Ang. PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C6 - C7 ... 1.43 Ang. PLAT420_ALERT_2_C D-H Without Acceptor N3 - H3B ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H2A .. S1 .. 3.01 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 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 4 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); 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.

Tris(ethylenediamine-κ2N,N')zinc(II) bis(1,2-dicyanoethylenedithiolato-κ2S,S')cuprate(II) top
Crystal data top
[Zn(C2H8N2)3][Cu(C4N2S2)2]F(000) = 1204
Mr = 589.58Dx = 1.607 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3197 reflections
a = 11.7722 (13) Åθ = 2.3–26.3°
b = 14.4010 (16) ŵ = 2.22 mm1
c = 14.9053 (17) ÅT = 296 K
β = 105.285 (2)°Block, blue
V = 2437.5 (5) Å30.35 × 0.27 × 0.18 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
2142 independent reflections
Radiation source: fine-focus sealed tube1769 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
φ and ω scansθmax = 25.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1414
Tmin = 0.495, Tmax = 0.670k = 1717
6257 measured reflectionsl = 1710
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.065H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0371P)2]
where P = (Fo2 + 2Fc2)/3
2142 reflections(Δ/σ)max < 0.001
138 parametersΔρmax = 0.18 e Å3
0 restraintsΔρmin = 0.35 e Å3
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
xyzUiso*/Ueq
Cu10.25000.75000.50000.04040 (13)
Zn10.50000.14557 (2)0.75000.03839 (13)
N10.31349 (16)0.16042 (14)0.67503 (14)0.0485 (5)
H1A0.30620.19480.62340.058*
H1B0.28120.10430.65820.058*
N20.55568 (16)0.24793 (14)0.66195 (15)0.0526 (5)
H2A0.56000.22130.60830.063*
H2B0.50300.29460.64830.063*
N30.53272 (18)0.02678 (14)0.66624 (16)0.0601 (6)
H3A0.47210.02010.61530.072*
H3B0.59860.03670.64780.072*
N40.6139 (2)0.50541 (17)0.6717 (2)0.0777 (8)
N50.3095 (2)0.36528 (16)0.56144 (18)0.0747 (7)
S10.43406 (5)0.70968 (4)0.58076 (5)0.05499 (19)
S20.18959 (5)0.59919 (4)0.49652 (5)0.04919 (18)
C10.25405 (19)0.20651 (19)0.73847 (19)0.0566 (7)
H1C0.24040.16200.78330.068*
H1D0.17840.23040.70330.068*
C20.6715 (2)0.28423 (18)0.71198 (19)0.0559 (7)
H2C0.66240.33100.75640.067*
H2D0.70920.31290.66840.067*
C30.5459 (2)0.05735 (18)0.7234 (2)0.0740 (9)
H3C0.62380.05900.76630.089*
H3D0.53680.11190.68400.089*
C40.5280 (2)0.54136 (17)0.63432 (19)0.0547 (7)
C50.4222 (2)0.59032 (16)0.58780 (17)0.0440 (5)
C60.3201 (2)0.54383 (15)0.55262 (16)0.0440 (6)
C70.3157 (2)0.44453 (18)0.55870 (17)0.0512 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0374 (2)0.0398 (2)0.0423 (2)0.00149 (17)0.00747 (18)0.00433 (17)
Zn10.0339 (2)0.0373 (2)0.0430 (2)0.0000.00837 (16)0.000
N10.0394 (10)0.0567 (13)0.0456 (12)0.0011 (10)0.0044 (9)0.0018 (10)
N20.0460 (12)0.0613 (14)0.0518 (13)0.0072 (10)0.0149 (10)0.0130 (10)
N30.0516 (13)0.0559 (14)0.0749 (16)0.0079 (11)0.0201 (12)0.0209 (12)
N40.0550 (15)0.0581 (15)0.108 (2)0.0128 (13)0.0004 (14)0.0113 (14)
N50.0912 (19)0.0462 (15)0.0751 (18)0.0044 (13)0.0013 (15)0.0064 (12)
S10.0395 (3)0.0425 (4)0.0733 (5)0.0024 (3)0.0022 (3)0.0067 (3)
S20.0424 (3)0.0432 (4)0.0551 (4)0.0063 (3)0.0006 (3)0.0050 (3)
C10.0367 (13)0.0667 (18)0.0646 (18)0.0121 (13)0.0104 (13)0.0009 (14)
C20.0629 (16)0.0476 (15)0.0614 (18)0.0115 (13)0.0235 (14)0.0018 (13)
C30.0645 (18)0.0458 (16)0.096 (2)0.0109 (13)0.0069 (16)0.0215 (16)
C40.0519 (16)0.0422 (14)0.0674 (18)0.0006 (12)0.0114 (14)0.0022 (13)
C50.0425 (13)0.0411 (13)0.0462 (14)0.0025 (10)0.0078 (11)0.0039 (11)
C60.0504 (14)0.0395 (13)0.0406 (13)0.0008 (11)0.0096 (12)0.0032 (10)
C70.0544 (15)0.0477 (16)0.0465 (15)0.0003 (12)0.0042 (12)0.0034 (12)
Geometric parameters (Å, º) top
Cu1—S1i2.2597 (6)N3—H3B0.90
Cu1—S12.2597 (6)N4—C41.141 (3)
Cu1—S2i2.2816 (6)N5—C71.145 (3)
Cu1—S22.2816 (6)S1—C51.730 (2)
Zn1—N2ii2.1860 (19)S2—C61.738 (2)
Zn1—N22.1860 (19)C1—C2ii1.492 (3)
Zn1—N1ii2.1958 (18)C1—H1C0.97
Zn1—N12.1958 (18)C1—H1D0.97
Zn1—N32.211 (2)C2—C1ii1.492 (3)
Zn1—N3ii2.211 (2)C2—H2C0.97
N1—C11.474 (3)C2—H2D0.97
N1—H1A0.90C3—C3ii1.498 (6)
N1—H1B0.90C3—H3C0.97
N2—C21.467 (3)C3—H3D0.97
N2—H2A0.90C4—C51.440 (3)
N2—H2B0.90C5—C61.355 (3)
N3—C31.466 (3)C6—C71.435 (3)
N3—H3A0.90
S1i—Cu1—S1180.0C3—N3—H3A110.0
S1i—Cu1—S2i90.97 (2)Zn1—N3—H3A110.0
S1—Cu1—S2i89.03 (2)C3—N3—H3B110.0
S1i—Cu1—S289.03 (2)Zn1—N3—H3B110.0
S1—Cu1—S290.97 (2)H3A—N3—H3B108.4
S2i—Cu1—S2180.0C5—S1—Cu1101.91 (8)
N2ii—Zn1—N295.19 (12)C6—S2—Cu1101.25 (8)
N2ii—Zn1—N1ii92.68 (8)N1—C1—C2ii109.83 (19)
N2—Zn1—N1ii79.75 (7)N1—C1—H1C109.7
N2ii—Zn1—N179.75 (7)C2ii—C1—H1C109.7
N2—Zn1—N192.68 (8)N1—C1—H1D109.7
N1ii—Zn1—N1168.83 (10)C2ii—C1—H1D109.7
N2ii—Zn1—N3170.18 (8)H1C—C1—H1D108.2
N2—Zn1—N393.34 (8)N2—C2—C1ii109.3 (2)
N1ii—Zn1—N393.61 (8)N2—C2—H2C109.8
N1—Zn1—N395.03 (8)C1ii—C2—H2C109.8
N2ii—Zn1—N3ii93.34 (8)N2—C2—H2D109.8
N2—Zn1—N3ii170.18 (8)C1ii—C2—H2D109.8
N1ii—Zn1—N3ii95.03 (8)H2C—C2—H2D108.3
N1—Zn1—N3ii93.61 (8)N3—C3—C3ii109.08 (18)
N3—Zn1—N3ii78.60 (12)N3—C3—H3C109.9
C1—N1—Zn1107.30 (14)C3ii—C3—H3C109.9
C1—N1—H1A110.3N3—C3—H3D109.9
Zn1—N1—H1A110.3C3ii—C3—H3D109.9
C1—N1—H1B110.3H3C—C3—H3D108.3
Zn1—N1—H1B110.3N4—C4—C5177.7 (3)
H1A—N1—H1B108.5C6—C5—C4120.7 (2)
C2—N2—Zn1108.71 (15)C6—C5—S1123.02 (18)
C2—N2—H2A109.9C4—C5—S1116.26 (17)
Zn1—N2—H2A109.9C5—C6—C7120.7 (2)
C2—N2—H2B109.9C5—C6—S2122.77 (18)
Zn1—N2—H2B109.9C7—C6—S2116.47 (18)
H2A—N2—H2B108.3N5—C7—C6178.1 (3)
C3—N3—Zn1108.58 (17)
N1—C1—C1ii—N1ii111.0 (3)N3—C3—C3ii—N3ii58.0 (4)
N2—C2—C2ii—N2ii124.0 (3)
Symmetry codes: (i) x+1/2, y+3/2, z+1; (ii) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···N50.902.633.396 (3)144
N1—H1B···N4iii0.902.483.232 (3)141
N2—H2A···S1iv0.903.013.702 (2)135
N2—H2B···N50.902.523.348 (3)153
N3—H3A···S2v0.902.773.561 (2)147
N3—H3B···S2vi0.902.883.655 (2)145
Symmetry codes: (iii) x1/2, y1/2, z; (iv) x+1, y+1, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y1/2, z.
 

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