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The title complex, [Zn(N3)(C6H4NO2)]n, formed from Zn cations, nicotinate and azide groups, exhibits a three-dimensional non-centrosymmetric covalent network. The coordination sphere of the central metal ions is completed by an N3O2 five-coordinate coordination model showing distorted trigonal–bipyramidal geometry. Adjacent Zn atoms are bonded by μ2-carboxylate groups and a μ2-azide bridge into one-dimensional helical double-stranded chains with the six-membered ring running along the a axis, and these chains are further linked by μ3-nicotinate groups via covalent bonds, extending into two-dimensional sheets and further generating a non-centrosymmetric three-dimensional covalent network.
Supporting information
CCDC reference: 260892
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.024
- wR factor = 0.060
- Data-to-parameter ratio = 10.5
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.94
Alert level C
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.65
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.19 Ratio
Alert level G
REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may
be needed to determine absolute structure
From the CIF: _diffrn_reflns_theta_max 28.99
From the CIF: _reflns_number_total 1247
Count of symmetry unique reflns 1246
Completeness (_total/calc) 100.08%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 1
Fraction of Friedel pairs measured 0.001
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
2 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
1 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: P3/P4-PC (Siemens, 1991); cell refinement: P3/P4-PC; data reduction: XDISK (Siemens, 1991); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Siemens, 1990); software used to prepare material for publication: SHELXL97.
Poly[zinc(II)-µ
2-azido-
κ2N1:
N1-µ
3-nicotinato-
κ3N:
O:
O']
top
Crystal data top
[Zn(N3)(C6H4NO2)] | F(000) = 456 |
Mr = 229.50 | Dx = 1.917 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 25 reflections |
a = 5.995 (4) Å | θ = 6.5–15.0° |
b = 10.540 (4) Å | µ = 3.06 mm−1 |
c = 12.586 (6) Å | T = 293 K |
V = 795.3 (7) Å3 | Prismatic, colourless |
Z = 4 | 0.28 × 0.24 × 0.19 mm |
Data collection top
Siemens R3m diffractometer | 1157 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.017 |
Graphite monochromator | θmax = 29.0°, θmin = 3.8° |
ω scans | h = 0→8 |
Absorption correction: ψ scan (Kopfman & Huber, 1968) | k = 0→14 |
Tmin = 0.454, Tmax = 0.560 | l = −1→17 |
1268 measured reflections | 2 standard reflections every 200 reflections |
1247 independent reflections | intensity decay: <0.1% |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.024 | w = 1/[σ2(Fo2) + (0.0354P)2 + 0.2937P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.060 | (Δ/σ)max = 0.001 |
S = 1.02 | Δρmax = 0.50 e Å−3 |
1247 reflections | Δρmin = −0.29 e Å−3 |
119 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0066 (18) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983) |
Secondary atom site location: difference Fourier map | Absolute structure parameter: −0.01 (2) |
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 | |
Zn1 | 0.21552 (6) | 0.17485 (3) | 0.01063 (2) | 0.02230 (12) | |
C1 | 0.5351 (6) | −0.1497 (3) | 0.3124 (2) | 0.0226 (7) | |
C2 | 0.5423 (6) | −0.1116 (3) | 0.1960 (2) | 0.0232 (7) | |
C3 | 0.6859 (7) | −0.1711 (4) | 0.1242 (2) | 0.0366 (9) | |
H3A | 0.7828 | −0.2380 | 0.1475 | 0.080* | |
C4 | 0.6792 (7) | −0.1336 (4) | 0.0184 (3) | 0.0414 (9) | |
H4A | 0.7776 | −0.1715 | −0.0328 | 0.080* | |
C5 | 0.5352 (6) | −0.0386 (3) | −0.0119 (2) | 0.0320 (7) | |
H5A | 0.5307 | −0.0133 | −0.0852 | 0.080* | |
C6 | 0.4035 (6) | −0.0168 (3) | 0.1598 (2) | 0.0236 (7) | |
H6A | 0.3076 | 0.0255 | 0.2095 | 0.080* | |
N1 | 0.3999 (5) | 0.0197 (2) | 0.05654 (19) | 0.0237 (5) | |
N2 | 0.4037 (5) | 0.3039 (3) | −0.0715 (2) | 0.0279 (6) | |
N3 | 0.3759 (5) | 0.3216 (3) | −0.1663 (2) | 0.0301 (6) | |
N4 | 0.3472 (7) | 0.3397 (4) | −0.2545 (2) | 0.0507 (10) | |
O1 | 0.6701 (5) | −0.2341 (2) | 0.34131 (17) | 0.0337 (6) | |
O2 | 0.3915 (4) | −0.0954 (2) | 0.36937 (17) | 0.0307 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.02415 (18) | 0.02769 (17) | 0.01506 (16) | 0.00226 (14) | 0.00022 (12) | 0.00231 (13) |
C1 | 0.0272 (18) | 0.0262 (16) | 0.0145 (12) | −0.0023 (13) | 0.0006 (12) | 0.0041 (11) |
C2 | 0.0278 (18) | 0.0269 (15) | 0.0149 (13) | 0.0020 (14) | 0.0009 (12) | 0.0014 (12) |
C3 | 0.044 (2) | 0.0436 (18) | 0.0224 (14) | 0.020 (2) | 0.0039 (15) | 0.0053 (15) |
C4 | 0.053 (3) | 0.051 (2) | 0.0199 (15) | 0.0236 (19) | 0.0088 (17) | 0.0017 (14) |
C5 | 0.044 (2) | 0.0378 (16) | 0.0144 (12) | 0.0078 (15) | 0.0031 (15) | 0.0032 (14) |
C6 | 0.0267 (18) | 0.0275 (15) | 0.0166 (13) | 0.0016 (14) | 0.0017 (13) | 0.0036 (12) |
N1 | 0.0290 (14) | 0.0265 (12) | 0.0155 (11) | 0.0056 (12) | −0.0024 (11) | 0.0022 (10) |
N2 | 0.0278 (14) | 0.0400 (16) | 0.0160 (11) | −0.0012 (14) | −0.0010 (11) | 0.0026 (11) |
N3 | 0.0256 (15) | 0.0419 (15) | 0.0228 (12) | −0.0006 (17) | −0.0012 (11) | 0.0050 (14) |
N4 | 0.047 (2) | 0.083 (3) | 0.0221 (14) | 0.000 (2) | −0.0020 (13) | 0.0163 (17) |
O1 | 0.0453 (18) | 0.0379 (12) | 0.0179 (10) | 0.0151 (13) | −0.0004 (11) | 0.0071 (9) |
O2 | 0.0373 (15) | 0.0363 (12) | 0.0185 (10) | 0.0075 (11) | 0.0059 (11) | 0.0058 (10) |
Geometric parameters (Å, º) top
Zn1—N2i | 2.032 (3) | C4—C5 | 1.375 (5) |
Zn1—N2 | 2.048 (3) | C4—H4A | 0.9600 |
Zn1—N1 | 2.057 (3) | C5—N1 | 1.334 (4) |
Zn1—O2ii | 2.067 (2) | C5—H5A | 0.9600 |
Zn1—O1iii | 2.206 (2) | C6—N1 | 1.355 (4) |
C1—O1 | 1.256 (4) | C6—H6A | 0.9600 |
C1—O2 | 1.258 (4) | N2—N3 | 1.219 (4) |
C1—C2 | 1.521 (4) | N2—Zn1iv | 2.032 (3) |
C2—C6 | 1.378 (5) | N3—N4 | 1.140 (4) |
C2—C3 | 1.397 (5) | O1—Zn1v | 2.206 (2) |
C3—C4 | 1.390 (4) | O2—Zn1vi | 2.067 (2) |
C3—H3A | 0.9600 | | |
| | | |
N2i—Zn1—N2 | 128.61 (8) | C5—C4—C3 | 119.4 (3) |
N2i—Zn1—N1 | 118.42 (11) | C5—C4—H4A | 120.2 |
N2—Zn1—N1 | 111.95 (13) | C3—C4—H4A | 120.4 |
N2i—Zn1—O2ii | 94.79 (11) | N1—C5—C4 | 122.6 (3) |
N2—Zn1—O2ii | 90.34 (10) | N1—C5—H5A | 118.3 |
N1—Zn1—O2ii | 94.95 (9) | C4—C5—H5A | 119.1 |
N2i—Zn1—O1iii | 85.39 (11) | N1—C6—C2 | 122.2 (3) |
N2—Zn1—O1iii | 88.05 (10) | N1—C6—H6A | 119.0 |
N1—Zn1—O1iii | 86.64 (10) | C2—C6—H6A | 118.9 |
O2ii—Zn1—O1iii | 178.07 (9) | C5—N1—C6 | 118.6 (3) |
O1—C1—O2 | 126.7 (3) | C5—N1—Zn1 | 120.8 (2) |
O1—C1—C2 | 116.6 (3) | C6—N1—Zn1 | 120.3 (2) |
O2—C1—C2 | 116.6 (3) | N3—N2—Zn1iv | 118.5 (2) |
C6—C2—C3 | 118.9 (3) | N3—N2—Zn1 | 121.3 (3) |
C6—C2—C1 | 119.6 (3) | Zn1iv—N2—Zn1 | 112.93 (13) |
C3—C2—C1 | 121.5 (3) | N4—N3—N2 | 178.8 (4) |
C4—C3—C2 | 118.3 (3) | C1—O1—Zn1v | 138.9 (2) |
C4—C3—H3A | 121.3 | C1—O2—Zn1vi | 121.2 (2) |
C2—C3—H3A | 120.3 | | |
Symmetry codes: (i) x−1/2, −y+1/2, −z; (ii) −x+1/2, −y, z−1/2; (iii) −x+1, y+1/2, −z+1/2; (iv) x+1/2, −y+1/2, −z; (v) −x+1, y−1/2, −z+1/2; (vi) −x+1/2, −y, z+1/2. |
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