Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806025724/hb2103sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806025724/hb2103Isup2.hkl |
CCDC reference: 618209
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.002 Å
- R factor = 0.019
- wR factor = 0.059
- Data-to-parameter ratio = 13.7
checkCIF/PLATON results
No syntax errors found
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 27.00 From the CIF: _reflns_number_total 1232 Count of symmetry unique reflns 781 Completeness (_total/calc) 157.75% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 451 Fraction of Friedel pairs measured 0.577 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 0 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 0 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
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Zn(CHO2)2(C10H8N2)] | Dx = 1.839 Mg m−3 |
Mr = 311.59 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P41212 | Cell parameters from 4955 reflections |
Hall symbol: P 4abw 2nw | θ = 2.8–28.0° |
a = 7.9687 (3) Å | µ = 2.19 mm−1 |
c = 17.7213 (11) Å | T = 295 K |
V = 1125.31 (9) Å3 | Block, colorless |
Z = 4 | 0.39 × 0.30 × 0.22 mm |
F(000) = 632 |
Bruker APEX CCD diffractometer | 1232 independent reflections |
Radiation source: fine-focus sealed tube | 1206 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
φ and ω scans | θmax = 27.0°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −9→10 |
Tmin = 0.452, Tmax = 0.613 | k = −10→9 |
6797 measured reflections | l = −20→22 |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.019 | w = 1/[σ2(Fo2) + (0.0566P)2 + 0.0576P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.059 | (Δ/σ)max < 0.001 |
S = 0.87 | Δρmax = 0.28 e Å−3 |
1232 reflections | Δρmin = −0.34 e Å−3 |
90 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0145 (15) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 451 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.008 (13) |
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. |
x | y | z | Uiso*/Ueq | ||
Zn1 | 0.23747 (2) | 0.23747 (2) | 0.0000 | 0.01722 (12) | |
N1 | 0.05054 (15) | 0.05054 (15) | 0.0000 | 0.0184 (4) | |
N2 | −0.57438 (14) | −0.57438 (14) | 0.0000 | 0.0205 (4) | |
O1 | 0.39334 (15) | 0.09838 (14) | −0.07880 (6) | 0.0247 (3) | |
O2 | 0.59977 (16) | 0.12558 (15) | −0.16311 (7) | 0.0287 (3) | |
C1 | 0.06961 (19) | −0.09104 (19) | −0.03993 (9) | 0.0235 (3) | |
H1 | 0.1664 | −0.1044 | −0.0686 | 0.028* | |
C2 | −0.04862 (19) | −0.21809 (19) | −0.04023 (9) | 0.0245 (4) | |
H2 | −0.0291 | −0.3165 | −0.0670 | 0.029* | |
C3 | −0.19708 (19) | −0.19708 (19) | 0.0000 | 0.0208 (5) | |
C4 | −0.32845 (19) | −0.32845 (19) | 0.0000 | 0.0205 (4) | |
C5 | −0.4954 (2) | −0.28612 (18) | −0.01169 (9) | 0.0246 (3) | |
H5 | −0.5271 | −0.1750 | −0.0191 | 0.029* | |
C6 | −0.61370 (19) | −0.41319 (19) | −0.01204 (9) | 0.0244 (3) | |
H6 | −0.7253 | −0.3855 | −0.0210 | 0.029* | |
C7 | 0.47357 (19) | 0.1748 (2) | −0.12899 (7) | 0.0238 (4) | |
H7 | 0.4337 | 0.2806 | −0.1421 | 0.029* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.01527 (13) | 0.01527 (13) | 0.02111 (17) | −0.00381 (10) | −0.00004 (6) | 0.00004 (6) |
N1 | 0.0161 (5) | 0.0161 (5) | 0.0228 (8) | −0.0023 (7) | −0.0022 (5) | 0.0022 (5) |
N2 | 0.0167 (6) | 0.0167 (6) | 0.0279 (9) | −0.0022 (7) | −0.0011 (5) | 0.0011 (5) |
O1 | 0.0263 (6) | 0.0208 (6) | 0.0271 (6) | −0.0026 (5) | 0.0096 (5) | 0.0006 (5) |
O2 | 0.0276 (6) | 0.0261 (7) | 0.0325 (6) | 0.0041 (5) | 0.0127 (6) | 0.0041 (5) |
C1 | 0.0199 (8) | 0.0220 (8) | 0.0284 (8) | −0.0033 (6) | 0.0042 (6) | −0.0022 (6) |
C2 | 0.0232 (8) | 0.0184 (8) | 0.0318 (9) | −0.0041 (7) | 0.0048 (6) | −0.0061 (6) |
C3 | 0.0178 (7) | 0.0178 (7) | 0.0267 (11) | −0.0033 (8) | −0.0015 (6) | 0.0015 (6) |
C4 | 0.0200 (7) | 0.0200 (7) | 0.0216 (10) | −0.0037 (9) | 0.0010 (6) | −0.0010 (6) |
C5 | 0.0210 (8) | 0.0157 (7) | 0.0370 (8) | −0.0013 (6) | −0.0016 (7) | 0.0018 (6) |
C6 | 0.0151 (7) | 0.0201 (8) | 0.0381 (9) | 0.0000 (6) | −0.0036 (6) | 0.0018 (7) |
C7 | 0.0289 (8) | 0.0201 (8) | 0.0225 (8) | 0.0013 (7) | 0.0034 (7) | 0.0015 (5) |
Zn1—N1 | 2.1065 (17) | C1—C2 | 1.383 (2) |
Zn1—N2i | 2.1204 (16) | C1—H1 | 0.9300 |
Zn1—O1 | 2.1729 (11) | C2—C3 | 1.3913 (18) |
Zn1—O1ii | 2.1729 (11) | C2—H2 | 0.9300 |
Zn1—O2iii | 2.1831 (11) | C3—C4 | 1.480 (3) |
Zn1—O2iv | 2.1831 (11) | C4—C5 | 1.3884 (18) |
N1—C1 | 1.3404 (17) | C5—C6 | 1.383 (2) |
N2—C6 | 1.3392 (17) | C5—H5 | 0.9300 |
C7—O1 | 1.2535 (17) | C6—H6 | 0.9300 |
C7—O2 | 1.2373 (18) | C7—H7 | 0.9300 |
N1—Zn1—N2i | 180.0 | C7—O2—Zn1vi | 126.48 (12) |
N1—Zn1—O1 | 92.50 (3) | N1—C1—C2 | 122.75 (14) |
N2i—Zn1—O1 | 87.50 (3) | N1—C1—H1 | 118.6 |
N1—Zn1—O1ii | 92.50 (3) | C2—C1—H1 | 118.6 |
N2i—Zn1—O1ii | 87.50 (3) | C1—C2—C3 | 119.29 (15) |
O1—Zn1—O1ii | 175.01 (6) | C1—C2—H2 | 120.4 |
N1—Zn1—O2iii | 89.89 (3) | C3—C2—H2 | 120.4 |
N2i—Zn1—O2iii | 90.11 (3) | C2—C3—C2ii | 117.8 (2) |
O1—Zn1—O2iii | 84.90 (5) | C2—C3—C4 | 121.08 (10) |
O1ii—Zn1—O2iii | 95.11 (5) | C2ii—C3—C4 | 121.08 (10) |
N1—Zn1—O2iv | 89.89 (3) | C5—C4—C5ii | 119.2 (2) |
N2i—Zn1—O2iv | 90.11 (3) | C5—C4—C3 | 120.40 (10) |
O1—Zn1—O2iv | 95.11 (5) | C5ii—C4—C3 | 120.40 (10) |
O1ii—Zn1—O2iv | 84.90 (5) | C6—C5—C4 | 118.41 (15) |
O2iii—Zn1—O2iv | 179.78 (7) | C6—C5—H5 | 120.8 |
C1—N1—C1ii | 118.00 (18) | C4—C5—H5 | 120.8 |
C1—N1—Zn1 | 121.00 (9) | N2—C6—C5 | 122.82 (14) |
C1ii—N1—Zn1 | 121.00 (9) | N2—C6—H6 | 118.6 |
C6—N2—C6ii | 118.30 (18) | C5—C6—H6 | 118.6 |
C6—N2—Zn1v | 120.85 (9) | O2—C7—O1 | 127.38 (18) |
C6ii—N2—Zn1v | 120.85 (9) | O2—C7—H7 | 116.3 |
C7—O1—Zn1 | 119.98 (11) | O1—C7—H7 | 116.3 |
O1—Zn1—N1—C1 | 2.02 (8) | N1—C1—C2—C3 | 2.6 (2) |
O1ii—Zn1—N1—C1 | −177.98 (8) | C1—C2—C3—C2ii | −1.21 (10) |
O2iii—Zn1—N1—C1 | −82.87 (9) | C1—C2—C3—C4 | 178.79 (10) |
O2iv—Zn1—N1—C1 | 97.13 (9) | C2—C3—C4—C5 | −133.30 (11) |
O1—Zn1—N1—C1ii | −177.98 (8) | C2ii—C3—C4—C5 | 46.70 (11) |
O1ii—Zn1—N1—C1ii | 2.02 (8) | C2—C3—C4—C5ii | 46.70 (11) |
O2iii—Zn1—N1—C1ii | 97.13 (9) | C2ii—C3—C4—C5ii | −133.30 (11) |
O2iv—Zn1—N1—C1ii | −82.87 (9) | C5ii—C4—C5—C6 | −0.69 (11) |
N1—Zn1—O1—C7 | 142.07 (11) | C3—C4—C5—C6 | 179.31 (11) |
N2i—Zn1—O1—C7 | −37.93 (11) | C6ii—N2—C6—C5 | −0.75 (12) |
O2iii—Zn1—O1—C7 | −128.26 (12) | Zn1v—N2—C6—C5 | 179.25 (12) |
O2iv—Zn1—O1—C7 | 51.96 (11) | C4—C5—C6—N2 | 1.5 (2) |
C1ii—N1—C1—C2 | −1.31 (11) | Zn1vi—O2—C7—O1 | −179.69 (12) |
Zn1—N1—C1—C2 | 178.69 (11) | Zn1—O1—C7—O2 | 157.77 (15) |
Symmetry codes: (i) x+1, y+1, z; (ii) y, x, −z; (iii) −y+1/2, x−1/2, z+1/4; (iv) x−1/2, −y+1/2, −z−1/4; (v) x−1, y−1, z; (vi) x+1/2, −y+1/2, −z−1/4. |