Literature DB >> 22346842

catena-Poly[[(5-phenyl-2,2'-bipyridine-κN,N')copper(I)]-μ-thio-cyanido-κN:S].

Shuxin Cui, Minghui Zuo, Jingping Zhang, Yulong Zhao, Hui Wang.   

Abstract

The title compound, [Cu(NCS)(C(16)H(12)N(2))](n), was synthesised under hydro-thermal conditions. The Cu(I) ion shows distorted tetra-hedral geometry being coordinated by two N atoms from a 5-phenyl-2,2'-bipyridine ligand and by the N and S atoms from two different thio-cyanate anions. The Cu(I) ions are bridged by thio-cyanide groups, forming a one-dimensional coordination polymer along the b axis. The crystal packing is through van der Waals contacts and C-H⋯π inter-actions.

Entities:  

Year:  2012        PMID： 22346842      PMCID： PMC3274895          DOI： 10.1107/S1600536812000682

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For applications of coordination metal complexes, see: Kong et al. (2008 ▶); Ohba et al. (2008 ▶). For related compounds, see Chen et al. (2009 ▶); Cui et al. (2011 ▶); Zhang et al. (2008 ▶).

Experimental

Crystal data

[Cu(NCS)(C16H12N2)] M = 353.90 Orthorhombic, a = 7.7978 (9) Å b = 10.7744 (12) Å c = 35.325 (4) Å V = 2967.8 (6) Å3 Z = 8 Mo Kα radiation μ = 1.61 mm−1 T = 153 K 0.42 × 0.09 × 0.06 mm

Data collection

Siemens SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ▶) T min = 0.840, T max = 0.914 15488 measured reflections 2932 independent reflections 2212 reflections with I > 2σ(I) R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.035 wR(F 2) = 0.091 S = 1.03 2932 reflections 199 parameters H-atom parameters constrained Δρmax = 0.32 e Å−3 Δρmin = −0.20 e Å−3 Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812000682/kp2379sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812000682/kp2379Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu(NCS)(C16H12N2)]F(000) = 1440
Mr = 353.90Dx = 1.584 Mg m−3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 15488 reflections
a = 7.7978 (9) Åθ = 2.3–26.0°
b = 10.7744 (12) ŵ = 1.61 mm−1
c = 35.325 (4) ÅT = 153 K
V = 2967.8 (6) Å3Block, red
Z = 80.42 × 0.09 × 0.06 mm
Siemens SMART CCD area-detector diffractometer2932 independent reflections
Radiation source: fine-focus sealed tube2212 reflections with I > 2σ(I)
graphiteRint = 0.033
Detector resolution: 9 pixels mm-1θmax = 26.0°, θmin = 2.3°
ω scansh = −9→9
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)k = −13→10
Tmin = 0.840, Tmax = 0.914l = −43→35
15488 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H-atom parameters constrained
S = 1.03w = 1/[σ2(Fo2) + (0.0444P)2 + 0.9913P] where P = (Fo2 + 2Fc2)/3
2932 reflections(Δ/σ)max = 0.001
199 parametersΔρmax = 0.32 e Å−3
0 restraintsΔρmin = −0.20 e Å−3
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.
xyzUiso*/Ueq
Cu11.11691 (4)0.67597 (3)0.345104 (9)0.04739 (14)
S11.40271 (9)0.61263 (7)0.34368 (3)0.0578 (2)
N11.1156 (3)0.8538 (2)0.34377 (6)0.0470 (6)
C11.3879 (3)0.4601 (3)0.34412 (7)0.0402 (6)
N30.9620 (3)0.59247 (18)0.38739 (6)0.0373 (5)
C120.8393 (3)0.6026 (2)0.49059 (6)0.0325 (5)
C70.8656 (3)0.4982 (2)0.37430 (7)0.0351 (5)
C100.8445 (3)0.5642 (2)0.45016 (6)0.0327 (5)
N20.9760 (3)0.5504 (2)0.31300 (6)0.0460 (5)
C60.8833 (3)0.4689 (2)0.33359 (7)0.0378 (6)
C80.7568 (3)0.4343 (3)0.39843 (7)0.0457 (6)
H80.69070.36910.38930.055*
C150.8303 (4)0.6706 (3)0.56739 (7)0.0461 (7)
H150.82720.69380.59270.055*
C110.9497 (3)0.6232 (2)0.42376 (7)0.0381 (6)
H111.01630.68910.43230.046*
C170.9373 (3)0.7005 (2)0.50432 (7)0.0423 (6)
H171.00770.74440.48780.051*
C160.9318 (3)0.7338 (3)0.54203 (8)0.0471 (7)
H160.99790.80020.55040.057*
C140.7336 (3)0.5726 (3)0.55461 (7)0.0465 (6)
H140.66490.52870.57140.056*
C90.7469 (3)0.4675 (2)0.43580 (7)0.0451 (6)
H90.67330.42440.45180.054*
C50.8093 (4)0.3650 (3)0.31698 (8)0.0490 (7)
H50.74760.30880.33160.059*
C130.7381 (3)0.5388 (2)0.51663 (7)0.0426 (6)
H130.67200.47220.50840.051*
C30.9202 (4)0.4297 (3)0.25767 (9)0.0643 (9)
H30.93320.41940.23170.077*
C40.8281 (4)0.3458 (3)0.27870 (9)0.0621 (9)
H40.77890.27680.26720.074*
C20.9924 (4)0.5287 (3)0.27587 (8)0.0607 (8)
H21.05680.58440.26160.073*
U11U22U33U12U13U23
Cu10.0601 (2)0.0344 (2)0.0477 (2)−0.00445 (15)0.00674 (16)0.00251 (14)
S10.0532 (4)0.0325 (4)0.0878 (6)−0.0041 (3)0.0084 (4)−0.0025 (4)
N10.0582 (15)0.0369 (13)0.0459 (14)0.0008 (11)−0.0004 (11)0.0028 (10)
C10.0414 (14)0.0413 (16)0.0378 (14)−0.0003 (11)0.0025 (11)−0.0002 (11)
N30.0432 (11)0.0341 (11)0.0346 (11)−0.0032 (9)0.0032 (9)0.0012 (9)
C120.0312 (12)0.0312 (12)0.0349 (13)0.0072 (10)0.0011 (10)0.0035 (10)
C70.0361 (12)0.0336 (13)0.0357 (13)0.0044 (11)−0.0020 (10)0.0018 (10)
C100.0323 (12)0.0324 (12)0.0334 (13)0.0048 (10)−0.0004 (10)0.0035 (10)
N20.0554 (13)0.0483 (13)0.0344 (12)−0.0005 (11)−0.0003 (10)0.0018 (10)
C60.0387 (13)0.0382 (14)0.0365 (13)0.0040 (11)−0.0043 (11)−0.0002 (11)
C80.0485 (15)0.0470 (15)0.0415 (14)−0.0155 (13)−0.0023 (12)−0.0002 (12)
C150.0520 (15)0.0526 (17)0.0337 (14)0.0146 (14)0.0011 (12)−0.0028 (12)
C110.0446 (14)0.0335 (13)0.0364 (14)−0.0058 (11)0.0010 (11)−0.0011 (11)
C170.0482 (14)0.0396 (15)0.0392 (14)−0.0019 (12)0.0032 (11)0.0023 (12)
C160.0535 (16)0.0406 (15)0.0473 (16)0.0018 (13)−0.0021 (12)−0.0062 (12)
C140.0467 (15)0.0547 (17)0.0381 (14)0.0032 (14)0.0070 (12)0.0049 (13)
C90.0443 (14)0.0525 (16)0.0386 (14)−0.0143 (13)0.0010 (12)0.0051 (12)
C50.0486 (15)0.0484 (16)0.0501 (17)−0.0032 (13)−0.0006 (13)−0.0068 (13)
C130.0436 (14)0.0425 (15)0.0416 (14)−0.0008 (12)0.0026 (12)0.0012 (11)
C30.076 (2)0.080 (2)0.0370 (16)0.0006 (19)−0.0013 (15)−0.0126 (16)
C40.0609 (18)0.066 (2)0.059 (2)0.0003 (16)−0.0046 (16)−0.0277 (16)
C20.074 (2)0.071 (2)0.0367 (16)−0.0054 (17)0.0034 (14)0.0021 (14)
Cu1—N11.917 (2)C8—H80.9300
Cu1—N22.079 (2)C15—C141.374 (4)
Cu1—N32.121 (2)C15—C161.376 (4)
Cu1—S12.3313 (9)C15—H150.9300
S1—C11.648 (3)C11—H110.9300
N1—C1i1.145 (4)C17—C161.380 (4)
C1—N1ii1.145 (4)C17—H170.9300
N3—C111.330 (3)C16—H160.9300
N3—C71.346 (3)C14—C131.390 (3)
C12—C171.390 (3)C14—H140.9300
C12—C131.393 (3)C9—H90.9300
C12—C101.487 (3)C5—C41.376 (4)
C7—C81.385 (3)C5—H50.9300
C7—C61.479 (3)C13—H130.9300
C10—C91.386 (3)C3—C21.367 (4)
C10—C111.395 (3)C3—C41.373 (5)
N2—C21.339 (3)C3—H30.9300
N2—C61.350 (3)C4—H40.9300
C6—C51.390 (4)C2—H20.9300
C8—C91.370 (4)
N1—Cu1—N2129.35 (9)C16—C15—H15120.6
N1—Cu1—N3115.99 (9)N3—C11—C10125.1 (2)
N2—Cu1—N378.88 (8)N3—C11—H11117.5
N1—Cu1—S1107.29 (7)C10—C11—H11117.5
N2—Cu1—S1107.64 (7)C16—C17—C12121.1 (2)
N3—Cu1—S1115.82 (6)C16—C17—H17119.4
C1—S1—Cu1102.99 (9)C12—C17—H17119.4
C1i—N1—Cu1177.7 (2)C15—C16—C17121.2 (3)
N1ii—C1—S1177.1 (2)C15—C16—H16119.4
C11—N3—C7118.7 (2)C17—C16—H16119.4
C11—N3—Cu1127.99 (17)C15—C14—C13120.3 (2)
C7—N3—Cu1113.34 (15)C15—C14—H14119.8
C17—C12—C13117.1 (2)C13—C14—H14119.8
C17—C12—C10122.1 (2)C8—C9—C10121.2 (2)
C13—C12—C10120.8 (2)C8—C9—H9119.4
N3—C7—C8120.3 (2)C10—C9—H9119.4
N3—C7—C6116.3 (2)C4—C5—C6119.4 (3)
C8—C7—C6123.3 (2)C4—C5—H5120.3
C9—C10—C11114.9 (2)C6—C5—H5120.3
C9—C10—C12123.0 (2)C14—C13—C12121.5 (2)
C11—C10—C12122.1 (2)C14—C13—H13119.3
C2—N2—C6117.8 (2)C12—C13—H13119.3
C2—N2—Cu1126.7 (2)C2—C3—C4118.3 (3)
C6—N2—Cu1114.36 (17)C2—C3—H3120.8
N2—C6—C5121.3 (2)C4—C3—H3120.8
N2—C6—C7115.8 (2)C3—C4—C5119.3 (3)
C5—C6—C7122.9 (2)C3—C4—H4120.4
C9—C8—C7119.9 (2)C5—C4—H4120.4
C9—C8—H8120.1N2—C2—C3123.9 (3)
C7—C8—H8120.1N2—C2—H2118.1
C14—C15—C16118.8 (2)C3—C2—H2118.1
C14—C15—H15120.6
N1—Cu1—S1—C1−178.99 (11)C8—C7—C6—N2171.1 (2)
N2—Cu1—S1—C1−36.25 (11)N3—C7—C6—C5171.7 (2)
N3—Cu1—S1—C149.68 (11)C8—C7—C6—C5−8.5 (4)
N1—Cu1—N3—C11−45.7 (2)N3—C7—C8—C90.2 (4)
N2—Cu1—N3—C11−174.2 (2)C6—C7—C8—C9−179.6 (2)
S1—Cu1—N3—C1181.5 (2)C7—N3—C11—C100.6 (4)
N1—Cu1—N3—C7133.67 (16)Cu1—N3—C11—C10179.92 (18)
N2—Cu1—N3—C75.13 (16)C9—C10—C11—N3−0.7 (4)
S1—Cu1—N3—C7−99.22 (16)C12—C10—C11—N3179.1 (2)
C11—N3—C7—C8−0.3 (3)C13—C12—C17—C16−1.0 (4)
Cu1—N3—C7—C8−179.74 (18)C10—C12—C17—C16−179.3 (2)
C11—N3—C7—C6179.4 (2)C14—C15—C16—C170.2 (4)
Cu1—N3—C7—C60.0 (3)C12—C17—C16—C150.5 (4)
C17—C12—C10—C9−179.4 (2)C16—C15—C14—C13−0.4 (4)
C13—C12—C10—C92.2 (3)C7—C8—C9—C10−0.2 (4)
C17—C12—C10—C110.9 (3)C11—C10—C9—C80.4 (4)
C13—C12—C10—C11−177.5 (2)C12—C10—C9—C8−179.3 (2)
N1—Cu1—N2—C268.4 (3)N2—C6—C5—C4−1.2 (4)
N3—Cu1—N2—C2−176.9 (3)C7—C6—C5—C4178.4 (3)
S1—Cu1—N2—C2−63.2 (2)C15—C14—C13—C12−0.1 (4)
N1—Cu1—N2—C6−124.53 (18)C17—C12—C13—C140.7 (4)
N3—Cu1—N2—C6−9.93 (18)C10—C12—C13—C14179.2 (2)
S1—Cu1—N2—C6103.86 (17)C2—C3—C4—C51.0 (5)
C2—N2—C6—C50.9 (4)C6—C5—C4—C30.2 (5)
Cu1—N2—C6—C5−167.4 (2)C6—N2—C2—C30.4 (5)
C2—N2—C6—C7−178.8 (2)Cu1—N2—C2—C3167.1 (2)
Cu1—N2—C6—C713.0 (3)C4—C3—C2—N2−1.4 (5)
N3—C7—C6—N2−8.7 (3)
Cg is the centroid of the C12–C17 ring.
D—H···AD—HH···AD···AD—H···A
C17—H17···Cgiii0.932.923.757 (3)150
Table 1

Selected bond lengths (Å)

Cu1—N11.917 (2)
Cu1—N22.079 (2)
Cu1—N32.121 (2)
Cu1—S12.3313 (9)
Table 2

Hydrogen-bond geometry (Å, °)

Cg is the centroid of the C12–C17 ring.

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C17—H17⋯Cgi0.932.923.757 (3)150

Symmetry code: (i) .

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4.  A short history of SHELX.

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5.  Poly[penta-kis-(μ-cyanido-κN:C)tris-(5-phenyl-2,2'-bipyridine-κN,N')penta-copper(I)].

Authors:  Shuxin Cui; Minghui Zuo; Jingping Zhang; Yulong Zhao; Rongxin Tan; Shujuan Liu; Shuangyue Su
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