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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
CCDC reference: 621340
Key indicators
- Single-crystal X-ray study
- T = 292 K
- Mean (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
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 = 437.37 | Dx = 1.789 Mg m−3 |
Orthorhombic, Fddd | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -F 2uv 2vw | Cell parameters from 787 reflections |
a = 13.520 (3) Å | θ = 3.6–25.8° |
b = 18.127 (4) Å | µ = 2.64 mm−1 |
c = 26.501 (5) Å | T = 292 K |
V = 6495 (2) Å3 | Block, black |
Z = 16 | 0.12 × 0.08 × 0.06 mm |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 1876 independent reflections |
Radiation source: fine-focus sealed tube | 1808 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.077 |
Oscillation scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −17→17 |
Tmin = 0.774, Tmax = 0.852 | k = −23→23 |
18086 measured reflections | l = −34→33 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.074 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.189 | H-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 parameters | Δρmax = 1.35 e Å−3 |
0 restraints | Δρmin = −0.45 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Cu1 | 0.54121 (5) | 0.55171 (4) | 0.54779 (2) | 0.0358 (3) | |
N1 | 0.4302 (4) | 0.5552 (3) | 0.4979 (2) | 0.0528 (14) | |
N2 | 0.4080 (6) | 0.6099 (4) | 0.4741 (3) | 0.076 (2) | |
N3 | 0.3874 (9) | 0.6623 (5) | 0.4491 (4) | 0.113 (4) | |
N4 | 0.6087 (3) | 0.5258 (3) | 0.64846 (16) | 0.0366 (10) | |
N5 | 0.4552 (3) | 0.5362 (3) | 0.60805 (18) | 0.0388 (10) | |
N6 | 0.6250 | 0.6250 | 0.5121 (2) | 0.0430 (16) | |
N7 | 0.6250 | 0.6250 | 0.4664 (3) | 0.069 (3) | |
N8 | 0.6250 | 0.6250 | 0.4231 (3) | 0.123 (6) | |
C1 | 0.5064 (4) | 0.5232 (3) | 0.6512 (2) | 0.0371 (11) | |
C2 | 0.4597 (5) | 0.5043 (5) | 0.6962 (3) | 0.0556 (17) | |
H2A | 0.4956 | 0.4968 | 0.7257 | 0.067* | |
C3 | 0.3578 (6) | 0.4971 (6) | 0.6954 (3) | 0.076 (3) | |
H3A | 0.3246 | 0.4826 | 0.7245 | 0.091* | |
C4 | 0.3057 (5) | 0.5108 (6) | 0.6526 (4) | 0.080 (3) | |
H4A | 0.2371 | 0.5068 | 0.6526 | 0.096* | |
C5 | 0.3551 (4) | 0.5309 (5) | 0.6092 (3) | 0.0583 (18) | |
H5A | 0.3191 | 0.5411 | 0.5801 | 0.070* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0372 (4) | 0.0401 (4) | 0.0300 (4) | −0.0048 (3) | −0.0064 (2) | 0.0007 (2) |
N1 | 0.052 (3) | 0.053 (3) | 0.053 (3) | −0.002 (2) | −0.025 (3) | 0.003 (2) |
N2 | 0.087 (5) | 0.071 (4) | 0.069 (4) | 0.016 (4) | −0.047 (4) | −0.011 (3) |
N3 | 0.156 (9) | 0.072 (5) | 0.111 (7) | 0.029 (6) | −0.077 (7) | 0.003 (5) |
N4 | 0.033 (2) | 0.051 (3) | 0.026 (2) | −0.001 (2) | −0.0020 (17) | 0.0009 (19) |
N5 | 0.031 (2) | 0.044 (2) | 0.041 (2) | −0.0068 (19) | −0.0029 (18) | 0.000 (2) |
N6 | 0.056 (4) | 0.046 (4) | 0.027 (3) | −0.016 (3) | 0.000 | 0.000 |
N7 | 0.110 (8) | 0.051 (5) | 0.045 (4) | −0.032 (5) | 0.000 | 0.000 |
N8 | 0.253 (18) | 0.088 (8) | 0.029 (4) | −0.081 (10) | 0.000 | 0.000 |
C1 | 0.036 (3) | 0.042 (3) | 0.033 (3) | −0.004 (2) | 0.001 (2) | −0.001 (2) |
C2 | 0.041 (3) | 0.082 (5) | 0.044 (3) | −0.004 (3) | 0.007 (3) | 0.001 (3) |
C3 | 0.041 (4) | 0.123 (8) | 0.064 (5) | −0.005 (4) | 0.014 (3) | 0.012 (5) |
C4 | 0.034 (3) | 0.121 (8) | 0.084 (6) | −0.022 (4) | 0.012 (4) | 0.004 (5) |
C5 | 0.032 (3) | 0.076 (5) | 0.067 (4) | −0.007 (3) | −0.008 (3) | −0.001 (4) |
Geometric parameters (Å, º) top
Cu1—N1 | 2.001 (5) | N5—C5 | 1.357 (7) |
Cu1—N1i | 2.318 (6) | N6—N7 | 1.210 (10) |
Cu1—N4ii | 2.020 (4) | N6—Cu1iii | 1.986 (3) |
Cu1—N5 | 1.995 (5) | N7—N8 | 1.149 (12) |
Cu1—N6 | 1.986 (3) | C1—C2 | 1.394 (8) |
N1—N2 | 1.213 (9) | C2—C3 | 1.383 (10) |
N1—Cu1i | 2.318 (6) | C2—H2A | 0.9300 |
N2—N3 | 1.192 (10) | C3—C4 | 1.358 (13) |
N4—N4ii | 1.319 (8) | C3—H3A | 0.9300 |
N4—C1 | 1.387 (7) | C4—C5 | 1.379 (11) |
N4—Cu1ii | 2.020 (4) | C4—H4A | 0.9300 |
N5—C1 | 1.356 (7) | C5—H5A | 0.9300 |
| | | |
N1—Cu1—N4ii | 167.3 (2) | N7—N6—Cu1 | 118.44 (16) |
N1—Cu1—N1i | 78.8 (2) | N7—N6—Cu1iii | 118.44 (16) |
N2—N1—Cu1 | 123.7 (5) | N8—N7—N6 | 180.000 (3) |
N2—N1—Cu1i | 116.9 (5) | Cu1—N6—Cu1iii | 123.1 (3) |
N3—N2—N1 | 177.4 (10) | Cu1—N1—Cu1i | 101.2 (2) |
N4ii—N4—C1 | 112.5 (5) | C1—N4—Cu1ii | 129.8 (4) |
N4ii—N4—Cu1ii | 116.2 (4) | C1—N5—C5 | 118.5 (5) |
N4ii—Cu1—N1i | 93.60 (19) | C1—N5—Cu1 | 113.7 (3) |
N4—C1—C2 | 120.3 (5) | C1—C2—H2A | 121.3 |
N5—Cu1—N1 | 95.5 (2) | C2—C3—H3A | 119.6 |
N5—Cu1—N1i | 113.5 (2) | C3—C2—C1 | 117.4 (7) |
N5—Cu1—N4ii | 78.07 (19) | C3—C2—H2A | 121.3 |
N5—C1—N4 | 117.3 (5) | C3—C4—C5 | 119.5 (7) |
N5—C1—C2 | 122.3 (5) | C3—C4—H4A | 120.2 |
N5—C5—C4 | 121.4 (7) | C4—C3—C2 | 120.9 (7) |
N5—C5—H5A | 119.3 | C4—C3—H3A | 119.6 |
N6—Cu1—N5 | 143.88 (19) | C4—C5—H5A | 119.3 |
N6—Cu1—N1 | 95.3 (2) | C5—N5—Cu1 | 127.5 (5) |
N6—Cu1—N1i | 102.4 (2) | C5—C4—H4A | 120.2 |
N6—Cu1—N4ii | 96.26 (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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