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The title complex, [Cu2(N3)3(C10H8N4)]n, shows a three-dimensional poylmeric structure. Each Cu atom is surrounded by five N atoms from three bridging azide ligands and one di-2-pyridyldiazene ligand [Cu—N = 2.002 (5), 2.317 (6), 2.020 (4), 1.995 (5) and 1.985 (3) Å], forming a CuN5 trigonal bipyramid. One μ1,1-azide bridges two Cu atoms and the other two μ1,1-azides bridge pairs of Cu atoms, forming a —Cu—N—Cu—N2— chain. The di-2-pyridyldiazene bridges two Cu atoms of different —Cu—N—Cu—N2— chains, forming a three-dimensional polymeric structure. On the basis of charge equilibrium, the presence of one CuII and one CuI ion are deduced and the two ions are disordered because of the occurrence of only one unique Cu atom in the structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806028613/hg2048sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806028613/hg2048Isup2.hkl
Contains datablock I

CCDC reference: 621340

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](C-C) = 0.011 Å
  • R factor = 0.073
  • wR factor = 0.189
  • Data-to-parameter ratio = 16.3

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT430_ALERT_2_A Short Inter D...A Contact N4 .. N4 .. 1.32 Ang. PLAT430_ALERT_2_A Short Inter D...A Contact N4 .. N5 .. 2.53 Ang. PLAT432_ALERT_2_A Short Inter X...Y Contact N4 .. C1 .. 2.25 Ang.
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact N1 .. N1 .. 2.75 Ang.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.04 PLAT213_ALERT_2_C Atom N8 has ADP max/min Ratio ............. 3.10 prola PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.35 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 - N1_m .. 6.73 su PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11 PLAT432_ALERT_2_C Short Inter X...Y Contact N8 .. C5 .. 2.96 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact N8 .. C5 .. 2.96 Ang. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 80.00 A   3 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.18 Ratio
Alert level G PLAT804_ALERT_5_G ARU-Pack Problem in PLATON Analysis ............ 34 Times
3 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: CrystalStructure (Rigaku/MSC, 2004); cell refinement: CrystalStructure; data reduction: CrystalStructure; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXTL.

poly[tri-µ-azido-µ-di-2-pyridyldiazene-dicopper(I,II)] top
Crystal data top
[Cu2(N3)3(C10H8N4)]F(000) = 3472
Mr = 437.37Dx = 1.789 Mg m3
Orthorhombic, FdddMo Kα radiation, λ = 0.71073 Å
Hall symbol: -F 2uv 2vwCell parameters from 787 reflections
a = 13.520 (3) Åθ = 3.6–25.8°
b = 18.127 (4) ŵ = 2.64 mm1
c = 26.501 (5) ÅT = 292 K
V = 6495 (2) Å3Block, black
Z = 160.12 × 0.08 × 0.06 mm
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
1876 independent reflections
Radiation source: fine-focus sealed tube1808 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.077
Oscillation scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1717
Tmin = 0.774, Tmax = 0.852k = 2323
18086 measured reflectionsl = 3433
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)] = 0.074Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.189H-atom parameters constrained
S = 1.24 w = 1/[σ2(Fo2) + (0.0802P)2 + 91.4266P]
where P = (Fo2 + 2Fc2)/3
1876 reflections(Δ/σ)max = 0.003
115 parametersΔρmax = 1.35 e Å3
0 restraintsΔρmin = 0.45 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
Cu10.54121 (5)0.55171 (4)0.54779 (2)0.0358 (3)
N10.4302 (4)0.5552 (3)0.4979 (2)0.0528 (14)
N20.4080 (6)0.6099 (4)0.4741 (3)0.076 (2)
N30.3874 (9)0.6623 (5)0.4491 (4)0.113 (4)
N40.6087 (3)0.5258 (3)0.64846 (16)0.0366 (10)
N50.4552 (3)0.5362 (3)0.60805 (18)0.0388 (10)
N60.62500.62500.5121 (2)0.0430 (16)
N70.62500.62500.4664 (3)0.069 (3)
N80.62500.62500.4231 (3)0.123 (6)
C10.5064 (4)0.5232 (3)0.6512 (2)0.0371 (11)
C20.4597 (5)0.5043 (5)0.6962 (3)0.0556 (17)
H2A0.49560.49680.72570.067*
C30.3578 (6)0.4971 (6)0.6954 (3)0.076 (3)
H3A0.32460.48260.72450.091*
C40.3057 (5)0.5108 (6)0.6526 (4)0.080 (3)
H4A0.23710.50680.65260.096*
C50.3551 (4)0.5309 (5)0.6092 (3)0.0583 (18)
H5A0.31910.54110.58010.070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0372 (4)0.0401 (4)0.0300 (4)0.0048 (3)0.0064 (2)0.0007 (2)
N10.052 (3)0.053 (3)0.053 (3)0.002 (2)0.025 (3)0.003 (2)
N20.087 (5)0.071 (4)0.069 (4)0.016 (4)0.047 (4)0.011 (3)
N30.156 (9)0.072 (5)0.111 (7)0.029 (6)0.077 (7)0.003 (5)
N40.033 (2)0.051 (3)0.026 (2)0.001 (2)0.0020 (17)0.0009 (19)
N50.031 (2)0.044 (2)0.041 (2)0.0068 (19)0.0029 (18)0.000 (2)
N60.056 (4)0.046 (4)0.027 (3)0.016 (3)0.0000.000
N70.110 (8)0.051 (5)0.045 (4)0.032 (5)0.0000.000
N80.253 (18)0.088 (8)0.029 (4)0.081 (10)0.0000.000
C10.036 (3)0.042 (3)0.033 (3)0.004 (2)0.001 (2)0.001 (2)
C20.041 (3)0.082 (5)0.044 (3)0.004 (3)0.007 (3)0.001 (3)
C30.041 (4)0.123 (8)0.064 (5)0.005 (4)0.014 (3)0.012 (5)
C40.034 (3)0.121 (8)0.084 (6)0.022 (4)0.012 (4)0.004 (5)
C50.032 (3)0.076 (5)0.067 (4)0.007 (3)0.008 (3)0.001 (4)
Geometric parameters (Å, º) top
Cu1—N12.001 (5)N5—C51.357 (7)
Cu1—N1i2.318 (6)N6—N71.210 (10)
Cu1—N4ii2.020 (4)N6—Cu1iii1.986 (3)
Cu1—N51.995 (5)N7—N81.149 (12)
Cu1—N61.986 (3)C1—C21.394 (8)
N1—N21.213 (9)C2—C31.383 (10)
N1—Cu1i2.318 (6)C2—H2A0.9300
N2—N31.192 (10)C3—C41.358 (13)
N4—N4ii1.319 (8)C3—H3A0.9300
N4—C11.387 (7)C4—C51.379 (11)
N4—Cu1ii2.020 (4)C4—H4A0.9300
N5—C11.356 (7)C5—H5A0.9300
N1—Cu1—N4ii167.3 (2)N7—N6—Cu1118.44 (16)
N1—Cu1—N1i78.8 (2)N7—N6—Cu1iii118.44 (16)
N2—N1—Cu1123.7 (5)N8—N7—N6180.000 (3)
N2—N1—Cu1i116.9 (5)Cu1—N6—Cu1iii123.1 (3)
N3—N2—N1177.4 (10)Cu1—N1—Cu1i101.2 (2)
N4ii—N4—C1112.5 (5)C1—N4—Cu1ii129.8 (4)
N4ii—N4—Cu1ii116.2 (4)C1—N5—C5118.5 (5)
N4ii—Cu1—N1i93.60 (19)C1—N5—Cu1113.7 (3)
N4—C1—C2120.3 (5)C1—C2—H2A121.3
N5—Cu1—N195.5 (2)C2—C3—H3A119.6
N5—Cu1—N1i113.5 (2)C3—C2—C1117.4 (7)
N5—Cu1—N4ii78.07 (19)C3—C2—H2A121.3
N5—C1—N4117.3 (5)C3—C4—C5119.5 (7)
N5—C1—C2122.3 (5)C3—C4—H4A120.2
N5—C5—C4121.4 (7)C4—C3—C2120.9 (7)
N5—C5—H5A119.3C4—C3—H3A119.6
N6—Cu1—N5143.88 (19)C4—C5—H5A119.3
N6—Cu1—N195.3 (2)C5—N5—Cu1127.5 (5)
N6—Cu1—N1i102.4 (2)C5—C4—H4A120.2
N6—Cu1—N4ii96.26 (18)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+5/4, y, z+5/4; (iii) x+5/4, y+5/4, z.
 

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