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The title compound, [Cu(NCS)2(C6H16N2)]n, is a thio­cyanate-bridged polynuclear copper(II) complex. The CuII atom is five-coordinate in a square-pyramidal geometry, with two N atoms of the N,N-diethyl­ethane-1,2-diamine ligand and two N atoms from two thio­cyanate ligands defining the basal plane, and one S atom of another thio­cyanate ligand occupying the apical position. The [Cu(NCS)2(C6H16N2)] units are linked by bridging thio­cyanate ligands, forming chains running along the a axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807013608/rz2124sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807013608/rz2124Isup2.hkl
Contains datablock I

CCDC reference: 647311

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.025
  • wR factor = 0.057
  • Data-to-parameter ratio = 22.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.73 Ratio
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 3064 Count of symmetry unique reflns 1772 Completeness (_total/calc) 172.91% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1292 Fraction of Friedel pairs measured 0.729 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

catena-Poly[[(N,N-diethylethane-1,2-diamine)thiocyanatocopper(II)]- µ-thiocyanato] top
Crystal data top
[Cu(NCS)2(C6H16N2)]F(000) = 612
Mr = 295.91Dx = 1.468 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 4038 reflections
a = 9.5219 (9) Åθ = 2.5–27.2°
b = 9.9083 (9) ŵ = 1.92 mm1
c = 14.1931 (13) ÅT = 298 K
V = 1339.1 (2) Å3Block, blue
Z = 40.33 × 0.31 × 0.27 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
3064 independent reflections
Radiation source: fine-focus sealed tube2786 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
ω scansθmax = 27.5°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1212
Tmin = 0.542, Tmax = 0.594k = 129
8106 measured reflectionsl = 1816
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.025H-atom parameters constrained
wR(F2) = 0.057 w = 1/[σ2(Fo2) + (0.0236P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max < 0.001
3064 reflectionsΔρmax = 0.26 e Å3
138 parametersΔρmin = 0.34 e Å3
0 restraintsAbsolute structure: Flack (1983), 1295 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.022 (11)
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
Cu10.29860 (2)0.90739 (3)0.048221 (19)0.03798 (8)
S10.48247 (9)0.81909 (8)0.25222 (5)0.0669 (2)
S20.15882 (6)0.86953 (6)0.08568 (4)0.04357 (15)
N10.21786 (19)0.9143 (2)0.17626 (13)0.0459 (4)
H1A0.15230.97960.17920.055*
H1B0.17650.83500.18990.055*
N20.46580 (18)1.01435 (17)0.10763 (14)0.0393 (4)
N30.3911 (2)0.8893 (2)0.07294 (14)0.0481 (5)
N40.1070 (2)0.9063 (2)0.00789 (15)0.0505 (5)
C10.3299 (3)0.9420 (3)0.24473 (18)0.0546 (6)
H1C0.38690.86210.25450.066*
H1D0.29010.96920.30470.066*
C20.4176 (3)1.0546 (3)0.20384 (18)0.0538 (7)
H2A0.36231.13670.20010.065*
H2B0.49811.07170.24400.065*
C30.5889 (2)0.9215 (3)0.11330 (18)0.0462 (5)
H3A0.61010.89000.05020.055*
H3B0.56180.84340.15020.055*
C40.7221 (3)0.9792 (3)0.1553 (2)0.0700 (8)
H4A0.75251.05490.11840.105*
H4B0.79400.91130.15540.105*
H4C0.70421.00790.21880.105*
C50.5022 (3)1.1339 (3)0.0494 (3)0.0659 (7)
H5A0.55141.10400.00660.079*
H5B0.56541.19150.08490.079*
C60.3748 (4)1.2153 (3)0.0203 (3)0.1009 (13)
H6A0.31441.16050.01800.151*
H6B0.40451.29290.01500.151*
H6C0.32471.24410.07550.151*
C70.4297 (2)0.8604 (2)0.14650 (18)0.0422 (5)
C80.0040 (2)0.8909 (2)0.03927 (16)0.0370 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.02944 (12)0.05024 (15)0.03425 (14)0.00351 (11)0.00175 (11)0.00516 (13)
S10.0715 (4)0.0901 (5)0.0393 (4)0.0331 (4)0.0119 (3)0.0132 (4)
S20.0299 (3)0.0571 (3)0.0438 (3)0.0010 (2)0.0044 (2)0.0012 (3)
N10.0395 (10)0.0514 (11)0.0467 (11)0.0027 (10)0.0093 (8)0.0090 (10)
N20.0333 (9)0.0415 (10)0.0431 (11)0.0017 (8)0.0016 (8)0.0111 (8)
N30.0448 (11)0.0654 (14)0.0343 (11)0.0013 (10)0.0017 (8)0.0010 (10)
N40.0351 (10)0.0585 (12)0.0578 (13)0.0038 (10)0.0101 (9)0.0021 (11)
C10.0494 (14)0.0797 (18)0.0348 (13)0.0111 (12)0.0047 (11)0.0084 (12)
C20.0414 (12)0.0689 (18)0.0511 (15)0.0026 (11)0.0059 (12)0.0279 (13)
C30.0319 (11)0.0592 (14)0.0475 (13)0.0025 (11)0.0001 (10)0.0145 (12)
C40.0377 (14)0.099 (2)0.073 (2)0.0037 (14)0.0123 (14)0.0302 (17)
C50.0689 (17)0.0546 (14)0.074 (2)0.0191 (13)0.0061 (17)0.0021 (15)
C60.119 (3)0.059 (2)0.125 (3)0.006 (2)0.022 (3)0.0202 (19)
C70.0349 (11)0.0493 (13)0.0426 (14)0.0035 (9)0.0035 (10)0.0142 (11)
C80.0370 (10)0.0394 (11)0.0346 (11)0.0003 (9)0.0037 (10)0.0010 (10)
Geometric parameters (Å, º) top
Cu1—N31.940 (2)C1—H1C0.9700
Cu1—N11.974 (2)C1—H1D0.9700
Cu1—N41.991 (2)C2—H2A0.9700
Cu1—N22.090 (2)C2—H2B0.9700
Cu1—S2i2.8240 (7)C3—C41.513 (3)
S1—C71.634 (3)C3—H3A0.9700
S2—C81.628 (2)C3—H3B0.9700
N1—C11.469 (3)C4—H4A0.9600
N1—H1A0.9000C4—H4B0.9600
N1—H1B0.9000C4—H4C0.9600
N2—C51.485 (3)C5—C61.514 (5)
N2—C31.492 (3)C5—H5A0.9700
N2—C21.495 (3)C5—H5B0.9700
N3—C71.143 (3)C6—H6A0.9600
N4—C81.157 (3)C6—H6B0.9600
C1—C21.509 (4)C6—H6C0.9600
N3—Cu1—N1174.68 (8)N2—C2—H2A109.9
N3—Cu1—N493.49 (8)C1—C2—H2A109.9
N1—Cu1—N490.66 (8)N2—C2—H2B109.9
N3—Cu1—N293.36 (8)C1—C2—H2B109.9
N1—Cu1—N284.70 (7)H2A—C2—H2B108.3
N4—Cu1—N2149.56 (8)N2—C3—C4116.5 (2)
N1—Cu1—S2i85.21 (8)N2—C3—H3A108.2
N2—Cu1—S2i107.90 (8)C4—C3—H3A108.2
N3—Cu1—S2i90.70 (8)N2—C3—H3B108.2
N4—Cu1—S2i101.64 (8)C4—C3—H3B108.2
C1—N1—Cu1109.42 (14)H3A—C3—H3B107.3
C1—N1—H1A109.8C3—C4—H4A109.5
Cu1—N1—H1A109.8C3—C4—H4B109.5
C1—N1—H1B109.8H4A—C4—H4B109.5
Cu1—N1—H1B109.8C3—C4—H4C109.5
H1A—N1—H1B108.2H4A—C4—H4C109.5
C5—N2—C3109.78 (19)H4B—C4—H4C109.5
C5—N2—C2111.5 (2)N2—C5—C6112.9 (2)
C3—N2—C2110.89 (19)N2—C5—H5A109.0
C5—N2—Cu1110.97 (16)C6—C5—H5A109.0
C3—N2—Cu1107.91 (13)N2—C5—H5B109.0
C2—N2—Cu1105.65 (13)C6—C5—H5B109.0
C7—N3—Cu1168.0 (2)H5A—C5—H5B107.8
C8—N4—Cu1172.7 (2)C5—C6—H6A109.5
N1—C1—C2106.6 (2)C5—C6—H6B109.5
N1—C1—H1C110.4H6A—C6—H6B109.5
C2—C1—H1C110.4C5—C6—H6C109.5
N1—C1—H1D110.4H6A—C6—H6C109.5
C2—C1—H1D110.4H6B—C6—H6C109.5
H1C—C1—H1D108.6N3—C7—S1179.2 (2)
N2—C2—C1108.91 (19)N4—C8—S2178.8 (2)
Symmetry code: (i) x+1/2, y+3/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1B···S1ii0.902.553.396 (2)156
N1—H1A···S1iii0.902.563.413 (2)158
Symmetry codes: (ii) x1/2, y+3/2, z; (iii) x+1/2, y+2, z+1/2.
 

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