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The title complex, [Zn(C2H8N2)3][Zn(C4N2S2)2], exists as discrete ions, both of which lie on twofold rotation axes. The [Zn(C2H8N2)3]2+ cation exhibits a slightly distorted octahedral geometry. In the [Zn(C4N2S2)2]2− anion, the ZnII atom is surrounded by two chelating ligands in a distorted tetrahedral geometry. The crystal structure 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/S160053680402714X/cf6385sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680402714X/cf6385Isup2.hkl
Contains datablock I

CCDC reference: 179808

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.011 Å
  • R factor = 0.054
  • wR factor = 0.138
  • Data-to-parameter ratio = 16.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for Zn2
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn2 - N3 .. 5.10 su PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for N3 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for N5 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C5 - C6 ... 1.42 Ang. PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C7 - C7_b ... 1.39 Ang. PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C3 - C4 ... 1.43 Ang. PLAT420_ALERT_2_C D-H Without Acceptor N4 - H4B ... ?
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 10 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 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 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, 1997a); 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[2,3-dimercaptobutenedinitrile(2-)-κ2S,S']zincate(II) top
Crystal data top
[Zn(C2H8N2)3][Zn(C4N2S2)2]Dx = 1.573 Mg m3
Mr = 591.41Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcnCell parameters from 1781 reflections
a = 12.0231 (12) Åθ = 2.6–20.7°
b = 14.269 (3) ŵ = 2.28 mm1
c = 14.559 (3) ÅT = 296 K
V = 2497.8 (8) Å3Block, colourless
Z = 40.25 × 0.20 × 0.10 mm
F(000) = 1208
Data collection top
Bruker SMART CCD area-detector
diffractometer
2158 independent reflections
Radiation source: fine-focus sealed tube1150 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.060
φ and ω scansθmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1413
Tmin = 0.600, Tmax = 0.804k = 1616
12094 measured reflectionsl = 1617
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)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.138H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0649P)2]
where P = (Fo2 + 2Fc2)/3
2158 reflections(Δ/σ)max < 0.001
130 parametersΔρmax = 0.75 e Å3
0 restraintsΔρmin = 0.75 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
Zn10.00000.46180 (7)0.25000.0509 (3)
Zn20.00000.89594 (7)0.25000.0523 (3)
N10.3136 (5)0.5639 (5)0.0127 (4)0.0827 (19)
N20.1415 (6)0.3519 (6)0.5997 (5)0.101 (2)
N30.1767 (5)0.8768 (5)0.2716 (4)0.093 (2)
H3A0.21320.93050.25990.112*
H3B0.18990.86020.33020.112*
N40.0378 (5)0.7939 (4)0.1416 (4)0.080
H4A0.01930.73580.16020.096*
H4B0.00130.80730.09050.096*
N50.0037 (6)1.0133 (5)0.1537 (5)0.0978 (19)
H5A0.07211.01980.12940.117*
H5B0.04521.00400.10780.117*
S10.14412 (14)0.55308 (11)0.19266 (12)0.0557 (5)
S20.01484 (14)0.37256 (12)0.38355 (12)0.0592 (5)
C10.2399 (6)0.5362 (5)0.0298 (5)0.0624 (17)
C20.1553 (5)0.5005 (4)0.0858 (4)0.0507 (16)
C30.1182 (6)0.3874 (5)0.5308 (6)0.0695 (19)
C40.0894 (5)0.4265 (4)0.4437 (4)0.0532 (16)
C50.2151 (7)0.8014 (5)0.2078 (8)0.096 (3)
H5C0.29360.81030.19530.115*
H5D0.20660.74120.23810.115*
C60.1564 (8)0.7991 (6)0.1228 (6)0.097 (3)
H6A0.17950.74500.08720.117*
H6B0.17280.85510.08750.117*
C70.0269 (7)1.0982 (7)0.2078 (6)0.101 (3)
H7A0.00651.15400.17370.121*
H7B0.10681.09930.21740.121*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0512 (6)0.0469 (6)0.0547 (6)0.0000.0026 (5)0.000
Zn20.0513 (6)0.0516 (6)0.0539 (6)0.0000.0026 (5)0.000
N10.074 (4)0.101 (5)0.074 (4)0.003 (4)0.008 (4)0.010 (4)
N20.124 (6)0.112 (6)0.067 (5)0.004 (5)0.005 (4)0.026 (4)
N30.079 (5)0.109 (5)0.092 (5)0.016 (4)0.005 (4)0.010 (4)
N40.0800.0800.0800.017 (3)0.007 (4)0.017 (3)
N50.133 (6)0.0800.0800.003 (4)0.000 (4)0.016 (4)
S10.0602 (10)0.0463 (9)0.0605 (10)0.0064 (8)0.0051 (9)0.0052 (9)
S20.0642 (11)0.0506 (10)0.0627 (10)0.0050 (8)0.0061 (9)0.0051 (8)
C10.061 (4)0.076 (5)0.050 (4)0.006 (4)0.003 (4)0.005 (4)
C20.049 (4)0.050 (4)0.054 (4)0.008 (3)0.001 (3)0.013 (3)
C30.070 (5)0.064 (5)0.074 (5)0.002 (4)0.008 (4)0.000 (4)
C40.068 (4)0.049 (4)0.043 (4)0.006 (3)0.009 (3)0.000 (3)
C50.083 (6)0.055 (5)0.149 (9)0.003 (4)0.051 (6)0.006 (5)
C60.138 (8)0.065 (5)0.089 (6)0.022 (5)0.068 (6)0.019 (5)
C70.0800.142 (8)0.0800.009 (5)0.001 (5)0.029 (6)
Geometric parameters (Å, º) top
Zn1—S1i2.3229 (17)N5—C71.491 (11)
Zn1—S12.3229 (17)N5—H5A0.9000
Zn1—S2i2.3311 (18)N5—H5B0.9000
Zn1—S22.3311 (18)S1—C21.733 (6)
Zn2—N3i2.164 (6)S2—C41.712 (7)
Zn2—N32.164 (6)C1—C21.399 (9)
Zn2—N5i2.185 (6)C2—C4i1.388 (8)
Zn2—N52.185 (6)C3—C41.428 (11)
Zn2—N42.195 (6)C4—C2i1.388 (8)
Zn2—N4i2.195 (6)C5—C61.425 (11)
N1—C11.151 (8)C5—H5C0.9700
N2—C31.159 (9)C5—H5D0.9700
N3—C51.495 (10)C6—H6A0.9700
N3—H3A0.9000C6—H6B0.9700
N3—H3B0.9000C7—C7i1.389 (16)
N4—C61.455 (9)C7—H7A0.9700
N4—H4A0.9000C7—H7B0.9700
N4—H4B0.9000
S1i—Zn1—S1111.79 (9)C7—N5—H5A110.5
S1i—Zn1—S2i123.30 (6)Zn2—N5—H5A110.5
S1—Zn1—S2i93.65 (6)C7—N5—H5B110.5
S1i—Zn1—S293.65 (6)Zn2—N5—H5B110.5
S1—Zn1—S2123.30 (6)H5A—N5—H5B108.7
S2i—Zn1—S2113.78 (10)C2—S1—Zn197.9 (2)
N3i—Zn2—N3165.5 (4)C4—S2—Zn197.2 (2)
N3i—Zn2—N5i99.8 (3)N1—C1—C2176.2 (7)
N3—Zn2—N5i91.4 (3)C4i—C2—C1120.8 (6)
N3i—Zn2—N591.4 (3)C4i—C2—S1124.2 (5)
N3—Zn2—N599.8 (3)C1—C2—S1115.0 (5)
N5i—Zn2—N579.9 (4)N2—C3—C4177.0 (8)
N3i—Zn2—N490.9 (2)C2i—C4—C3115.7 (6)
N3—Zn2—N479.5 (2)C2i—C4—S2127.0 (5)
N5i—Zn2—N4167.0 (2)C3—C4—S2117.1 (5)
N5—Zn2—N492.5 (3)C6—C5—N3113.8 (7)
N3i—Zn2—N4i79.5 (2)C6—C5—H5C108.8
N3—Zn2—N4i90.9 (2)N3—C5—H5C108.8
N5i—Zn2—N4i92.5 (3)C6—C5—H5D108.8
N5—Zn2—N4i167.0 (2)N3—C5—H5D108.8
N4—Zn2—N4i96.9 (3)H5C—C5—H5D107.7
C5—N3—Zn2107.7 (5)C5—C6—N4108.8 (6)
C5—N3—H3A110.2C5—C6—H6A109.9
Zn2—N3—H3A110.2N4—C6—H6A109.9
C5—N3—H3B110.2C5—C6—H6B109.9
Zn2—N3—H3B110.2N4—C6—H6B109.9
H3A—N3—H3B108.5H6A—C6—H6B108.3
C6—N4—Zn2107.7 (4)C7i—C7—N5110.6 (6)
C6—N4—H4A110.2C7i—C7—H7A109.5
Zn2—N4—H4A110.2N5—C7—H7A109.5
C6—N4—H4B110.2C7i—C7—H7B109.5
Zn2—N4—H4B110.2N5—C7—H7B109.5
H4A—N4—H4B108.5H7A—C7—H7B108.1
C7—N5—Zn2106.2 (5)
N5—C7—C7i—N5i59.6 (14)N3—C5—C6—N453.6 (9)
Symmetry code: (i) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N5—H5B···N1ii0.902.403.265 (10)162
N5—H5A···N1iii0.902.563.348 (9)146
N4—H4A···N2iv0.902.463.056 (9)124
N3—H3B···N1v0.902.533.255 (9)138
N3—H3A···S1iii0.902.643.505 (8)162
Symmetry codes: (ii) x1/2, y+3/2, z; (iii) x+1/2, y+1/2, z; (iv) x, y+1, z1/2; (v) x+1/2, y+3/2, z+1/2.
 

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