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A novel centrosymmetric chair-like dimer, bis(2,2′-bi­pyridine)-1κ2N,N′;3κ2N,N′-tetra-μ-chloro-1:2κ2Cl;­2:3κ2Cl;­3:4κ2Cl;1:4κ2Cl-tetra­copper(I), [Cu4Cl4­(C10­H8­N2)2], has been solvothermally synthesized and structurally characterized. The complex self-assembles into a three-dimensional network via C—H...Cl hydrogen bonds, π–π stacking and weak Cu...Cl electrostatic interactions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100019855/bm1430sup1.cif
Contains datablocks III, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100019855/bm1430IIIsup2.hkl
Contains datablock cy2

CCDC reference: 163877

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: SAINT and SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(III) top
Crystal data top
[Cu4Cl4(C10H8N2)2]Z = 1
Mr = 708.33F(000) = 348
Triclinic, P1Dx = 2.055 Mg m3
a = 7.4252 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.4231 (7) ÅCell parameters from 1649 reflections
c = 9.4957 (9) Åθ = 2.4–25.0°
α = 64.253 (2)°µ = 4.15 mm1
β = 74.117 (2)°T = 293 K
γ = 88.504 (2)°Plate, purple
V = 572.28 (9) Å30.15 × 0.15 × 0.10 mm
Data collection top
Siemens SMART CCD area detector
diffractometer
2006 independent reflections
Radiation source: fine-focus sealed tube1596 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 88
Tmin = 0.526, Tmax = 0.661k = 118
2994 measured reflectionsl = 119
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)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.162H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.104P)2 + 0.663P]
where P = (Fo2 + 2Fc2)/3
2006 reflections(Δ/σ)max = 0.001
146 parametersΔρmax = 0.90 e Å3
0 restraintsΔρmin = 0.84 e Å3
Special details top

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
Cu10.36488 (12)0.37281 (9)0.76046 (9)0.0564 (4)
Cu20.27638 (12)0.55493 (9)0.46479 (10)0.0557 (3)
Cl10.1289 (2)0.33153 (19)0.6406 (2)0.0523 (4)
Cl20.4053 (2)0.78493 (18)0.2887 (2)0.0518 (4)
N10.2068 (7)0.2786 (6)1.0056 (6)0.0446 (12)
N20.3850 (6)0.5683 (6)0.7967 (6)0.0397 (11)
C10.1200 (10)0.1323 (8)1.1047 (8)0.0550 (16)
H1A0.13540.05621.06600.066*
C20.0090 (10)0.0902 (8)1.2617 (8)0.0586 (18)
H2A0.05200.01191.32660.070*
C30.0109 (10)0.1998 (8)1.3214 (8)0.0544 (16)
H3A0.08250.17261.42830.065*
C40.0765 (9)0.3504 (8)1.2213 (7)0.0491 (15)
H4A0.06140.42721.25920.059*
C50.1868 (8)0.3884 (7)1.0642 (7)0.0384 (12)
C60.2898 (8)0.5478 (6)0.9489 (6)0.0368 (12)
C70.2915 (9)0.6699 (7)0.9929 (8)0.0455 (14)
H7A0.22510.65431.09780.055*
C80.3911 (10)0.8139 (8)0.8816 (8)0.0522 (16)
H8A0.39370.89630.91030.063*
C90.4873 (9)0.8342 (8)0.7267 (8)0.0483 (14)
H9A0.55570.93070.64900.058*
C100.4807 (9)0.7103 (7)0.6889 (8)0.0455 (14)
H10B0.54530.72500.58400.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0737 (6)0.0552 (6)0.0444 (5)0.0022 (4)0.0044 (4)0.0331 (4)
Cu20.0681 (6)0.0521 (5)0.0497 (5)0.0014 (4)0.0079 (4)0.0303 (4)
Cl10.0543 (9)0.0551 (9)0.0513 (9)0.0020 (7)0.0133 (7)0.0276 (8)
Cl20.0597 (10)0.0452 (9)0.0524 (9)0.0068 (7)0.0105 (7)0.0270 (7)
N10.052 (3)0.045 (3)0.044 (3)0.009 (2)0.017 (2)0.025 (2)
N20.036 (3)0.049 (3)0.043 (3)0.009 (2)0.012 (2)0.029 (2)
C10.066 (4)0.052 (4)0.054 (4)0.005 (3)0.017 (3)0.030 (3)
C20.064 (4)0.053 (4)0.048 (4)0.004 (3)0.019 (3)0.012 (3)
C30.062 (4)0.060 (4)0.035 (3)0.006 (3)0.008 (3)0.019 (3)
C40.061 (4)0.055 (4)0.042 (3)0.016 (3)0.017 (3)0.031 (3)
C50.039 (3)0.047 (3)0.040 (3)0.011 (2)0.015 (2)0.027 (3)
C60.043 (3)0.044 (3)0.035 (3)0.011 (2)0.018 (2)0.024 (3)
C70.056 (4)0.048 (4)0.046 (3)0.008 (3)0.015 (3)0.033 (3)
C80.064 (4)0.051 (4)0.060 (4)0.008 (3)0.027 (3)0.036 (3)
C90.048 (3)0.049 (4)0.054 (4)0.003 (3)0.016 (3)0.028 (3)
C100.048 (3)0.048 (4)0.045 (3)0.003 (3)0.010 (3)0.026 (3)
Geometric parameters (Å, º) top
Cu1—N12.085 (5)N2—C61.353 (7)
Cu1—N22.032 (5)C1—C21.375 (10)
Cu1—Cl12.4556 (18)C2—C31.365 (10)
Cu1—Cl2i2.3184 (17)C3—C41.370 (10)
Cu2—Cl12.1176 (18)C4—C51.382 (8)
Cu2—Cl22.1196 (18)C5—C61.487 (8)
Cu1—Cu22.8327 (12)C6—C71.386 (8)
Cu1—Cu2i2.8008 (12)C7—C81.372 (9)
N1—C11.337 (8)C8—C91.378 (9)
N1—C51.360 (7)C9—C101.368 (9)
N2—C101.343 (8)
N1—Cu1—N281.2 (2)Cu2—Cl2—Cu1i78.12 (6)
N2—Cu1—Cl2i129.91 (14)C1—N1—C5118.4 (5)
N1—Cu1—Cl2i112.52 (14)C1—N1—Cu1129.1 (4)
N2—Cu1—Cl1121.91 (14)C5—N1—Cu1112.4 (4)
N1—Cu1—Cl1100.12 (15)C10—N2—C6118.4 (5)
Cl2i—Cu1—Cl1103.44 (6)C10—N2—Cu1127.6 (4)
N2—Cu1—Cu2i94.02 (14)C6—N2—Cu1114.0 (4)
N1—Cu1—Cu2i146.96 (15)N1—C1—C2122.5 (6)
Cl2i—Cu1—Cu2i47.78 (5)C3—C2—C1119.3 (7)
Cl1—Cu1—Cu2i109.85 (5)C2—C3—C4119.0 (6)
N2—Cu1—Cu290.95 (14)C3—C4—C5120.1 (6)
N1—Cu1—Cu2132.93 (14)N1—C5—C4120.7 (6)
Cl2i—Cu1—Cu2107.93 (5)N1—C5—C6115.8 (5)
Cl1—Cu1—Cu246.54 (4)C4—C5—C6123.5 (5)
Cu2i—Cu1—Cu279.51 (3)N2—C6—C7120.9 (5)
Cl1—Cu2—Cl2175.93 (8)N2—C6—C5116.4 (5)
Cl1—Cu2—Cu1i129.58 (6)C7—C6—C5122.7 (5)
Cl2—Cu2—Cu1i54.10 (5)C8—C7—C6120.0 (6)
Cl1—Cu2—Cu157.32 (5)C7—C8—C9118.9 (6)
Cl2—Cu2—Cu1125.25 (6)C10—C9—C8119.0 (6)
Cu1i—Cu2—Cu1100.49 (3)N2—C10—C9122.9 (6)
Cu2—Cl1—Cu176.15 (6)
Symmetry code: (i) x+1, y+1, z+1.
 

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