In the structure of the title compound, [CuNa2(C2H3O2)2(N3)2]n, the copper(II) cation is coordinated by two N atoms of two symmetry-related azide anions and two O atoms of two symmetry-related carboxylate anions within a distorted tetragonal plane. The sodium cation is surrounded by four O atoms of four symmetry-equivalent carboxylate anions and two N atoms of two azide anions within an irregular polyhedron. The copper(II) cations are located on a twofold axis, whereas all other atoms are located in general positions. The copper(II) and sodium cations are connected via the carboxylate anions into sheets parallel to (010). These sheets are linked by the azide anions via μ-N,N coordination into a three-dimensional coordination network.
Supporting information
CCDC reference: 263556
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.004 Å
- R factor = 0.039
- wR factor = 0.105
- Data-to-parameter ratio = 15.0
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.96
Alert level C
PLAT128_ALERT_4_C Non-standard setting of Space group P2/c .... P2/n
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.59 Ratio
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS (Stoe & Cie, 1998); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL7 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXL97.
Poly[di-µ
4-acetato-di-µ
2-azido-copper(II)disodium(II)]
top
Crystal data top
[CuNa2(C2H3O2)2(N3)2] | F(000) = 310 |
Mr = 311.67 | Dx = 2.027 Mg m−3 |
Monoclinic, P2/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yac | Cell parameters from 5742 reflections |
a = 6.6691 (4) Å | θ = 2.5–28° |
b = 7.8721 (7) Å | µ = 2.24 mm−1 |
c = 9.7547 (6) Å | T = 150 K |
β = 94.404 (7)° | Block, blue |
V = 510.61 (6) Å3 | 0.08 × 0.05 × 0.05 mm |
Z = 2 | |
Data collection top
Stoe Imaging Plate Diffraction System diffractometer | 1077 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.046 |
Graphite monochromator | θmax = 28.1°, θmin = 2.6° |
φ scans | h = −8→8 |
4743 measured reflections | k = −10→10 |
1200 independent reflections | l = −12→12 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.039 | H-atom parameters constrained |
wR(F2) = 0.105 | w = 1/[σ2(Fo2) + (0.0567P)2 + 1.0984P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max < 0.001 |
1200 reflections | Δρmax = 0.54 e Å−3 |
80 parameters | Δρmin = −0.71 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.066 (7) |
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 | 0.7500 | 0.61798 (6) | 0.7500 | 0.0136 (2) | |
O1 | 0.7209 (3) | 0.4447 (3) | 0.6016 (2) | 0.0151 (4) | |
O2 | 1.0480 (3) | 0.4057 (3) | 0.6565 (2) | 0.0168 (5) | |
C1 | 0.8890 (4) | 0.3661 (3) | 0.5886 (3) | 0.0137 (6) | |
C2 | 0.8828 (5) | 0.2222 (4) | 0.4878 (4) | 0.0212 (6) | |
H2A | 1.0202 | 0.1862 | 0.4735 | 0.032* | |
H2B | 0.8154 | 0.2596 | 0.4002 | 0.032* | |
H2C | 0.8085 | 0.1268 | 0.5239 | 0.032* | |
N1 | 0.6184 (4) | 0.7805 (3) | 0.6223 (3) | 0.0201 (6) | |
N2 | 0.5594 (4) | 0.9177 (3) | 0.6554 (3) | 0.0181 (5) | |
N3 | 0.4984 (5) | 1.0497 (4) | 0.6812 (3) | 0.0268 (6) | |
Na1 | 0.38410 (17) | 0.34543 (16) | 0.60652 (13) | 0.0175 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0154 (3) | 0.0130 (3) | 0.0119 (3) | 0.000 | −0.00153 (17) | 0.000 |
O1 | 0.0128 (9) | 0.0175 (10) | 0.0150 (10) | 0.0009 (7) | 0.0004 (7) | −0.0029 (8) |
O2 | 0.0132 (9) | 0.0226 (11) | 0.0146 (11) | −0.0005 (8) | 0.0000 (8) | 0.0016 (8) |
C1 | 0.0157 (13) | 0.0123 (12) | 0.0133 (15) | −0.0013 (9) | 0.0022 (10) | 0.0023 (9) |
C2 | 0.0188 (14) | 0.0195 (14) | 0.0261 (17) | 0.0005 (11) | 0.0058 (12) | −0.0070 (12) |
N1 | 0.0272 (13) | 0.0173 (12) | 0.0147 (14) | 0.0063 (10) | −0.0053 (10) | 0.0000 (9) |
N2 | 0.0211 (12) | 0.0184 (12) | 0.0146 (13) | 0.0024 (10) | −0.0001 (10) | 0.0022 (9) |
N3 | 0.0347 (15) | 0.0211 (13) | 0.0243 (16) | 0.0081 (12) | −0.0003 (12) | −0.0006 (11) |
Na1 | 0.0138 (6) | 0.0237 (6) | 0.0148 (7) | 0.0000 (4) | 0.0006 (4) | −0.0026 (5) |
Geometric parameters (Å, º) top
Cu1—N1i | 1.947 (3) | C2—H2A | 0.9800 |
Cu1—N1 | 1.947 (3) | C2—H2B | 0.9800 |
Cu1—O1 | 1.988 (2) | C2—H2C | 0.9800 |
Cu1—O1i | 1.988 (2) | N1—N2 | 1.203 (4) |
Cu1—Na1 | 3.4630 (13) | N1—Na1ii | 2.441 (3) |
Cu1—Na1i | 3.4630 (13) | N2—N3 | 1.151 (4) |
Cu1—Na1ii | 3.5355 (13) | N3—Na1v | 2.539 (3) |
Cu1—Na1iii | 3.5355 (13) | Na1—O2i | 2.369 (3) |
O1—C1 | 1.295 (3) | Na1—O2vi | 2.378 (2) |
O1—Na1 | 2.382 (2) | Na1—N1ii | 2.441 (3) |
O1—Na1ii | 2.669 (3) | Na1—N3vii | 2.539 (3) |
O2—C1 | 1.246 (4) | Na1—O1ii | 2.669 (3) |
O2—Na1i | 2.369 (3) | Na1—Na1viii | 3.436 (2) |
O2—Na1iv | 2.378 (2) | Na1—Cu1ii | 3.5355 (13) |
C1—C2 | 1.498 (4) | Na1—Na1ii | 3.623 (3) |
| | | |
N1i—Cu1—N1 | 97.86 (16) | Cu1—N1—Na1ii | 106.83 (12) |
N1i—Cu1—O1 | 158.59 (10) | N3—N2—N1 | 176.9 (3) |
N1—Cu1—O1 | 88.33 (10) | N2—N3—Na1v | 150.3 (3) |
N1i—Cu1—O1i | 88.33 (10) | O2i—Na1—O2vi | 82.67 (9) |
N1—Cu1—O1i | 158.59 (10) | O2i—Na1—O1 | 81.04 (8) |
O1—Cu1—O1i | 93.32 (13) | O2vi—Na1—O1 | 147.54 (9) |
N1i—Cu1—Na1 | 159.17 (9) | O2i—Na1—N1ii | 163.92 (10) |
N1—Cu1—Na1 | 83.08 (9) | O2vi—Na1—N1ii | 109.15 (10) |
O1—Cu1—Na1 | 41.76 (6) | O1—Na1—N1ii | 93.15 (10) |
O1i—Cu1—Na1 | 84.00 (7) | O2i—Na1—N3vii | 82.70 (10) |
N1i—Cu1—Na1i | 83.08 (8) | O2vi—Na1—N3vii | 113.03 (10) |
N1—Cu1—Na1i | 159.17 (9) | O1—Na1—N3vii | 92.50 (10) |
O1—Cu1—Na1i | 84.00 (7) | N1ii—Na1—N3vii | 82.58 (10) |
O1i—Cu1—Na1i | 41.76 (6) | O2i—Na1—O1ii | 129.60 (9) |
Na1—Cu1—Na1i | 103.43 (4) | O2vi—Na1—O1ii | 80.56 (8) |
N1i—Cu1—Na1ii | 130.05 (8) | O1—Na1—O1ii | 88.53 (8) |
N1—Cu1—Na1ii | 41.36 (8) | N1ii—Na1—O1ii | 64.72 (8) |
O1—Cu1—Na1ii | 48.42 (7) | N3vii—Na1—O1ii | 147.29 (10) |
O1i—Cu1—Na1ii | 140.85 (7) | O2i—Na1—Na1viii | 43.73 (6) |
Na1—Cu1—Na1ii | 62.34 (4) | O2vi—Na1—Na1viii | 43.54 (6) |
Na1i—Cu1—Na1ii | 124.42 (3) | O1—Na1—Na1viii | 124.55 (8) |
N1i—Cu1—Na1iii | 41.36 (8) | N1ii—Na1—Na1viii | 141.03 (9) |
N1—Cu1—Na1iii | 130.05 (8) | N3vii—Na1—Na1viii | 85.98 (8) |
O1—Cu1—Na1iii | 140.85 (7) | O1ii—Na1—Na1viii | 119.81 (6) |
O1i—Cu1—Na1iii | 48.42 (7) | O2i—Na1—Cu1 | 53.54 (6) |
Na1—Cu1—Na1iii | 124.42 (3) | O2vi—Na1—Cu1 | 116.07 (7) |
Na1i—Cu1—Na1iii | 62.34 (4) | O1—Na1—Cu1 | 33.77 (5) |
Na1ii—Cu1—Na1iii | 170.65 (4) | N1ii—Na1—Cu1 | 125.19 (8) |
C1—O1—Cu1 | 111.23 (18) | N3vii—Na1—Cu1 | 105.39 (8) |
C1—O1—Na1 | 132.08 (18) | O1ii—Na1—Cu1 | 93.40 (6) |
Cu1—O1—Na1 | 104.47 (9) | Na1viii—Na1—Cu1 | 93.75 (4) |
C1—O1—Na1ii | 113.56 (18) | O2i—Na1—Cu1ii | 163.41 (7) |
Cu1—O1—Na1ii | 97.71 (9) | O2vi—Na1—Cu1ii | 90.81 (6) |
Na1—O1—Na1ii | 91.47 (8) | O1—Na1—Cu1ii | 96.95 (7) |
C1—O2—Na1i | 124.02 (19) | N1ii—Na1—Cu1ii | 31.81 (6) |
C1—O2—Na1iv | 128.2 (2) | N3vii—Na1—Cu1ii | 113.87 (8) |
Na1i—O2—Na1iv | 92.73 (9) | O1ii—Na1—Cu1ii | 33.86 (5) |
O2—C1—O1 | 122.4 (3) | Na1viii—Na1—Cu1ii | 133.89 (5) |
O2—C1—C2 | 121.2 (3) | Cu1—Na1—Cu1ii | 117.66 (4) |
O1—C1—C2 | 116.4 (3) | O2i—Na1—Na1ii | 111.54 (8) |
C1—C2—H2A | 109.5 | O2vi—Na1—Na1ii | 115.72 (8) |
C1—C2—H2B | 109.5 | O1—Na1—Na1ii | 47.43 (6) |
H2A—C2—H2B | 109.5 | N1ii—Na1—Na1ii | 73.84 (8) |
C1—C2—H2C | 109.5 | N3vii—Na1—Na1ii | 130.43 (9) |
H2A—C2—H2C | 109.5 | O1ii—Na1—Na1ii | 41.09 (5) |
H2B—C2—H2C | 109.5 | Na1viii—Na1—Na1ii | 137.66 (4) |
N2—N1—Cu1 | 124.0 (2) | Cu1—Na1—Na1ii | 59.81 (3) |
N2—N1—Na1ii | 129.1 (2) | Cu1ii—Na1—Na1ii | 57.85 (3) |
Symmetry codes: (i) −x+3/2, y, −z+3/2; (ii) −x+1, −y+1, −z+1; (iii) x+1/2, −y+1, z+1/2; (iv) x+1, y, z; (v) x, y+1, z; (vi) x−1, y, z; (vii) x, y−1, z; (viii) −x+1/2, y, −z+3/2. |