Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807060461/fj2073sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807060461/fj2073Isup2.hkl |
CCDC reference: 672762
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.029
- wR factor = 0.085
- Data-to-parameter ratio = 16.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.83 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C12 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C15 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C7 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.11 Ratio
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT793_ALERT_1_G Check the Absolute Configuration of N1 ..... S PLAT793_ALERT_1_G Check the Absolute Configuration of N2 ..... S
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For related literature, see: Dealwis et al. (1995); Burley et al. (1990); Roderick & Mathews (1993); Dutta et al. (2005); Mandal & Nag (1986); Bazzicalupi et al. (1997).
The ligand C22H32N4O2 (H2L) was prepared by the reported procedure (Mandal & Nag, 1986). A mixture of H2L (0.05 g, 0.13 mmol), Zn(OH)2 (0.026 g, 0.26 mmol) and maleic acid (0.03 g,0.26 mmol) in methanol (20 ml) was stirred for 10 min. The resulting solution was filtered. Colorless single crystals were obtained by slow evaporation of the filtrate at room temperature (yield 60%).
All H-atoms bound to carbon were refined using a riding model with d(C—H) = 0.93–0.97 Å, Uiso = 1.2Ueq (C) for aromatic and CH2 atoms, Uiso = 1.5Ueq (C) for CH3 atoms. The imino and hydroxy H atoms were located in a difference Fourier map and refined isotropically with Uiso(H) = 1.5 Ueq(N, O).
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Fig. 1. A view of the molecule of (I). Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. |
[Zn2(C22H22N4O2)(C4H7O4)2] | F(000) = 768 |
Mr = 743.37 | Dx = 1.593 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3166 reflections |
a = 9.4233 (7) Å | θ = 2.3–28.3° |
b = 11.2691 (8) Å | µ = 1.61 mm−1 |
c = 14.6870 (11) Å | T = 293 K |
β = 96.3816 (8)° | Block, colourless |
V = 1550.0 (2) Å3 | 0.35 × 0.30 × 0.25 mm |
Z = 2 |
Bruker APEX CCD area-detector diffractometer | 3614 independent reflections |
Radiation source: fine-focus sealed tube | 3166 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.015 |
ω scans | θmax = 28.3°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→10 |
Tmin = 0.548, Tmax = 0.667 | k = −11→14 |
9199 measured reflections | l = −19→19 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.085 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0484P)2 + 0.5671P] where P = (Fo2 + 2Fc2)/3 |
3614 reflections | (Δ/σ)max = 0.002 |
217 parameters | Δρmax = 0.86 e Å−3 |
0 restraints | Δρmin = −0.30 e Å−3 |
[Zn2(C22H22N4O2)(C4H7O4)2] | V = 1550.0 (2) Å3 |
Mr = 743.37 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 9.4233 (7) Å | µ = 1.61 mm−1 |
b = 11.2691 (8) Å | T = 293 K |
c = 14.6870 (11) Å | 0.35 × 0.30 × 0.25 mm |
β = 96.3816 (8)° |
Bruker APEX CCD area-detector diffractometer | 3614 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3166 reflections with I > 2σ(I) |
Tmin = 0.548, Tmax = 0.667 | Rint = 0.015 |
9199 measured reflections |
R[F2 > 2σ(F2)] = 0.029 | 0 restraints |
wR(F2) = 0.085 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | Δρmax = 0.86 e Å−3 |
3614 reflections | Δρmin = −0.30 e Å−3 |
217 parameters |
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 | 0.07989 (2) | 1.036471 (19) | 0.413650 (13) | 0.03090 (9) | |
C1 | 0.0822 (2) | 0.78759 (17) | 0.48550 (13) | 0.0347 (4) | |
C2 | 0.1329 (2) | 0.72414 (18) | 0.56441 (14) | 0.0367 (4) | |
C3 | 0.1730 (2) | 0.6061 (2) | 0.55428 (16) | 0.0441 (5) | |
H3 | 0.2051 | 0.5625 | 0.6063 | 0.053* | |
C4 | 0.1665 (2) | 0.55165 (19) | 0.46898 (18) | 0.0440 (5) | |
C5 | 0.1158 (2) | 0.61675 (19) | 0.39189 (16) | 0.0409 (4) | |
H5 | 0.1100 | 0.5810 | 0.3345 | 0.049* | |
C6 | 0.07315 (19) | 0.73491 (18) | 0.39866 (14) | 0.0356 (4) | |
C7 | 0.2131 (3) | 0.4238 (2) | 0.4611 (2) | 0.0575 (6) | |
H7A | 0.2015 | 0.4003 | 0.3979 | 0.086* | |
H7B | 0.1557 | 0.3738 | 0.4952 | 0.086* | |
H7C | 0.3116 | 0.4162 | 0.4852 | 0.086* | |
C8 | 0.0124 (2) | 0.80583 (19) | 0.31613 (14) | 0.0398 (4) | |
H8A | 0.0126 | 0.7571 | 0.2617 | 0.048* | |
H8B | −0.0859 | 0.8263 | 0.3227 | 0.048* | |
C9 | 0.0453 (3) | 0.9876 (2) | 0.22116 (15) | 0.0509 (6) | |
H9A | 0.0122 | 0.9343 | 0.1714 | 0.061* | |
H9B | 0.1250 | 1.0327 | 0.2027 | 0.061* | |
C10 | 0.0730 (3) | 0.9287 (2) | 0.76219 (15) | 0.0495 (5) | |
H10A | 0.1564 | 0.9737 | 0.7496 | 0.059* | |
H10B | 0.0988 | 0.8813 | 0.8166 | 0.059* | |
C11 | 0.1554 (2) | 0.7870 (2) | 0.65532 (15) | 0.0432 (5) | |
H11A | 0.1874 | 0.7293 | 0.7022 | 0.052* | |
H11B | 0.2314 | 0.8446 | 0.6531 | 0.052* | |
C12 | 0.3516 (2) | 1.14644 (19) | 0.42009 (14) | 0.0392 (4) | |
C13 | 0.4910 (2) | 1.1892 (2) | 0.46576 (17) | 0.0485 (5) | |
H13 | 0.5474 | 1.2276 | 0.4268 | 0.058* | |
C14 | 0.5497 (2) | 1.1825 (2) | 0.55234 (17) | 0.0505 (6) | |
H14 | 0.6399 | 1.2167 | 0.5623 | 0.061* | |
C15 | 0.4994 (2) | 1.1313 (2) | 0.63603 (16) | 0.0484 (5) | |
N1 | 0.09452 (19) | 0.91689 (17) | 0.30383 (11) | 0.0379 (4) | |
N2 | 0.0277 (2) | 0.84905 (16) | 0.68315 (11) | 0.0378 (4) | |
O1 | 0.04349 (18) | 0.90058 (12) | 0.49375 (10) | 0.0441 (4) | |
O2 | 0.27011 (17) | 1.09045 (18) | 0.46986 (11) | 0.0550 (4) | |
O3 | 0.3184 (2) | 1.1678 (2) | 0.33987 (12) | 0.0682 (6) | |
O4 | 0.3731 (2) | 1.0827 (2) | 0.63265 (13) | 0.0737 (6) | |
O5 | 0.5765 (2) | 1.1369 (2) | 0.70789 (12) | 0.0677 (5) | |
H2O | 0.318 (4) | 1.079 (4) | 0.578 (3) | 0.102* | |
HN1 | 0.181 (4) | 0.898 (4) | 0.296 (3) | 0.102* | |
HN2 | −0.035 (4) | 0.803 (3) | 0.698 (3) | 0.102* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.03147 (13) | 0.03791 (14) | 0.02267 (12) | −0.00489 (8) | 0.00010 (8) | 0.00140 (8) |
C1 | 0.0344 (9) | 0.0329 (9) | 0.0379 (10) | −0.0010 (7) | 0.0089 (8) | 0.0004 (8) |
C2 | 0.0323 (9) | 0.0385 (10) | 0.0392 (10) | −0.0019 (8) | 0.0038 (8) | 0.0028 (8) |
C3 | 0.0371 (10) | 0.0409 (11) | 0.0539 (12) | 0.0038 (9) | 0.0038 (9) | 0.0081 (10) |
C4 | 0.0349 (11) | 0.0368 (11) | 0.0613 (14) | 0.0011 (8) | 0.0100 (10) | −0.0013 (9) |
C5 | 0.0344 (10) | 0.0402 (11) | 0.0494 (11) | −0.0014 (8) | 0.0104 (9) | −0.0088 (9) |
C6 | 0.0294 (9) | 0.0375 (10) | 0.0408 (10) | −0.0009 (7) | 0.0076 (7) | −0.0019 (8) |
C7 | 0.0555 (14) | 0.0392 (12) | 0.0793 (18) | 0.0096 (11) | 0.0141 (13) | 0.0002 (12) |
C8 | 0.0355 (10) | 0.0463 (11) | 0.0367 (10) | 0.0021 (8) | −0.0003 (8) | −0.0082 (8) |
C9 | 0.0672 (16) | 0.0579 (14) | 0.0270 (10) | 0.0052 (12) | 0.0027 (10) | −0.0011 (9) |
C10 | 0.0617 (14) | 0.0528 (12) | 0.0307 (10) | 0.0034 (11) | −0.0089 (9) | −0.0002 (9) |
C11 | 0.0390 (10) | 0.0478 (12) | 0.0406 (11) | 0.0009 (9) | −0.0055 (8) | 0.0026 (9) |
C12 | 0.0336 (10) | 0.0443 (11) | 0.0394 (11) | 0.0002 (8) | 0.0031 (8) | −0.0005 (8) |
C13 | 0.0304 (10) | 0.0602 (14) | 0.0553 (13) | −0.0073 (9) | 0.0073 (9) | 0.0080 (11) |
C14 | 0.0290 (10) | 0.0620 (14) | 0.0587 (14) | −0.0079 (10) | −0.0033 (9) | −0.0027 (11) |
C15 | 0.0411 (11) | 0.0588 (14) | 0.0438 (12) | 0.0037 (10) | −0.0021 (9) | −0.0147 (10) |
N1 | 0.0401 (9) | 0.0457 (9) | 0.0277 (8) | 0.0045 (8) | 0.0030 (7) | 0.0015 (7) |
N2 | 0.0471 (10) | 0.0396 (9) | 0.0257 (8) | −0.0017 (7) | −0.0010 (7) | −0.0001 (6) |
O1 | 0.0686 (10) | 0.0315 (7) | 0.0355 (7) | 0.0069 (6) | 0.0215 (7) | 0.0050 (6) |
O2 | 0.0401 (8) | 0.0801 (12) | 0.0419 (8) | −0.0243 (8) | −0.0085 (7) | 0.0132 (8) |
O3 | 0.0540 (10) | 0.1097 (16) | 0.0403 (9) | −0.0140 (10) | 0.0023 (8) | 0.0091 (10) |
O4 | 0.0521 (11) | 0.1292 (19) | 0.0382 (9) | −0.0245 (12) | −0.0023 (8) | 0.0104 (11) |
O5 | 0.0567 (11) | 0.0953 (15) | 0.0468 (10) | 0.0056 (10) | −0.0138 (8) | −0.0173 (10) |
Zn1—O2 | 1.9838 (15) | C9—C10i | 1.501 (4) |
Zn1—O1 | 1.9840 (14) | C9—H9A | 0.9700 |
Zn1—O1i | 2.0140 (14) | C9—H9B | 0.9700 |
Zn1—N2i | 2.0960 (17) | C10—N2 | 1.492 (3) |
Zn1—N1 | 2.1181 (18) | C10—C9i | 1.501 (4) |
C1—O1 | 1.334 (2) | C10—H10A | 0.9700 |
C1—C2 | 1.400 (3) | C10—H10B | 0.9700 |
C1—C6 | 1.401 (3) | C11—N2 | 1.488 (3) |
C2—C3 | 1.395 (3) | C11—H11A | 0.9700 |
C2—C11 | 1.505 (3) | C11—H11B | 0.9700 |
C3—C4 | 1.390 (3) | C12—O3 | 1.209 (3) |
C3—H3 | 0.9300 | C12—O2 | 1.283 (3) |
C4—C5 | 1.389 (3) | C12—C13 | 1.488 (3) |
C4—C7 | 1.514 (3) | C13—C14 | 1.331 (3) |
C5—C6 | 1.397 (3) | C13—H13 | 0.9300 |
C5—H5 | 0.9300 | C14—C15 | 1.482 (4) |
C6—C8 | 1.510 (3) | C14—H14 | 0.9300 |
C7—H7A | 0.9600 | C15—O5 | 1.214 (3) |
C7—H7B | 0.9600 | C15—O4 | 1.306 (3) |
C7—H7C | 0.9600 | N1—HN1 | 0.86 (4) |
C8—N1 | 1.493 (3) | N2—Zn1i | 2.0960 (17) |
C8—H8A | 0.9700 | N2—HN2 | 0.83 (4) |
C8—H8B | 0.9700 | O1—Zn1i | 2.0140 (14) |
C9—N1 | 1.483 (3) | O4—H2O | 0.91 (4) |
O2—Zn1—O1 | 101.40 (7) | C10i—C9—H9B | 109.2 |
O2—Zn1—O1i | 100.00 (7) | H9A—C9—H9B | 107.9 |
O1—Zn1—O1i | 73.78 (6) | N2—C10—C9i | 110.56 (19) |
O2—Zn1—N2i | 116.11 (7) | N2—C10—H10A | 109.5 |
O1—Zn1—N2i | 140.78 (7) | C9i—C10—H10A | 109.5 |
O1i—Zn1—N2i | 88.23 (6) | N2—C10—H10B | 109.5 |
O2—Zn1—N1 | 112.32 (8) | C9i—C10—H10B | 109.5 |
O1—Zn1—N1 | 89.46 (6) | H10A—C10—H10B | 108.1 |
O1i—Zn1—N1 | 146.07 (7) | N2—C11—C2 | 115.23 (16) |
N2i—Zn1—N1 | 86.71 (7) | N2—C11—H11A | 108.5 |
O1—C1—C2 | 118.95 (18) | C2—C11—H11A | 108.5 |
O1—C1—C6 | 119.84 (18) | N2—C11—H11B | 108.5 |
C2—C1—C6 | 121.20 (18) | C2—C11—H11B | 108.5 |
C3—C2—C1 | 118.04 (19) | H11A—C11—H11B | 107.5 |
C3—C2—C11 | 121.99 (19) | O3—C12—O2 | 123.2 (2) |
C1—C2—C11 | 119.71 (18) | O3—C12—C13 | 119.6 (2) |
C4—C3—C2 | 122.1 (2) | O2—C12—C13 | 117.19 (18) |
C4—C3—H3 | 118.9 | C14—C13—C12 | 131.6 (2) |
C2—C3—H3 | 118.9 | C14—C13—H13 | 114.2 |
C5—C4—C3 | 118.56 (19) | C12—C13—H13 | 114.2 |
C5—C4—C7 | 121.1 (2) | C13—C14—C15 | 132.6 (2) |
C3—C4—C7 | 120.3 (2) | C13—C14—H14 | 113.7 |
C4—C5—C6 | 121.4 (2) | C15—C14—H14 | 113.7 |
C4—C5—H5 | 119.3 | O5—C15—O4 | 120.6 (2) |
C6—C5—H5 | 119.3 | O5—C15—C14 | 119.0 (2) |
C5—C6—C1 | 118.66 (19) | O4—C15—C14 | 120.4 (2) |
C5—C6—C8 | 122.23 (19) | C9—N1—C8 | 115.51 (18) |
C1—C6—C8 | 119.06 (18) | C9—N1—Zn1 | 103.92 (13) |
C4—C7—H7A | 109.5 | C8—N1—Zn1 | 111.27 (12) |
C4—C7—H7B | 109.5 | C9—N1—HN1 | 104 (3) |
H7A—C7—H7B | 109.5 | C8—N1—HN1 | 109 (3) |
C4—C7—H7C | 109.5 | Zn1—N1—HN1 | 114 (3) |
H7A—C7—H7C | 109.5 | C11—N2—C10 | 109.06 (17) |
H7B—C7—H7C | 109.5 | C11—N2—Zn1i | 116.63 (13) |
N1—C8—C6 | 112.68 (16) | C10—N2—Zn1i | 103.46 (13) |
N1—C8—H8A | 109.1 | C11—N2—HN2 | 114 (3) |
C6—C8—H8A | 109.1 | C10—N2—HN2 | 109 (3) |
N1—C8—H8B | 109.1 | Zn1i—N2—HN2 | 105 (3) |
C6—C8—H8B | 109.1 | C1—O1—Zn1 | 128.02 (12) |
H8A—C8—H8B | 107.8 | C1—O1—Zn1i | 125.58 (12) |
N1—C9—C10i | 112.01 (18) | Zn1—O1—Zn1i | 106.22 (6) |
N1—C9—H9A | 109.2 | C12—O2—Zn1 | 118.93 (13) |
C10i—C9—H9A | 109.2 | C15—O4—H2O | 119 (3) |
N1—C9—H9B | 109.2 | ||
O1—C1—C2—C3 | −179.92 (18) | O1—Zn1—N1—C9 | 150.36 (15) |
C6—C1—C2—C3 | −0.6 (3) | O1i—Zn1—N1—C9 | 91.32 (17) |
O1—C1—C2—C11 | −5.6 (3) | N2i—Zn1—N1—C9 | 9.41 (15) |
C6—C1—C2—C11 | 173.73 (18) | O2—Zn1—N1—C8 | 127.55 (13) |
C1—C2—C3—C4 | 1.2 (3) | O1—Zn1—N1—C8 | 25.43 (13) |
C11—C2—C3—C4 | −173.0 (2) | O1i—Zn1—N1—C8 | −33.61 (19) |
C2—C3—C4—C5 | −1.3 (3) | N2i—Zn1—N1—C8 | −115.52 (14) |
C2—C3—C4—C7 | 179.1 (2) | C2—C11—N2—C10 | −167.27 (18) |
C3—C4—C5—C6 | 0.7 (3) | C2—C11—N2—Zn1i | −50.6 (2) |
C7—C4—C5—C6 | −179.7 (2) | C9i—C10—N2—C11 | 167.38 (19) |
C4—C5—C6—C1 | −0.1 (3) | C9i—C10—N2—Zn1i | 42.6 (2) |
C4—C5—C6—C8 | −177.62 (19) | C2—C1—O1—Zn1 | 139.17 (16) |
O1—C1—C6—C5 | 179.37 (18) | C6—C1—O1—Zn1 | −40.2 (3) |
C2—C1—C6—C5 | 0.1 (3) | C2—C1—O1—Zn1i | −46.3 (2) |
O1—C1—C6—C8 | −3.0 (3) | C6—C1—O1—Zn1i | 134.36 (16) |
C2—C1—C6—C8 | 177.67 (18) | O2—Zn1—O1—C1 | −87.41 (18) |
C5—C6—C8—N1 | −123.2 (2) | O1i—Zn1—O1—C1 | 175.4 (2) |
C1—C6—C8—N1 | 59.3 (2) | N2i—Zn1—O1—C1 | 109.40 (18) |
C3—C2—C11—N2 | −129.6 (2) | N1—Zn1—O1—C1 | 25.27 (18) |
C1—C2—C11—N2 | 56.3 (3) | O2—Zn1—O1—Zn1i | 97.23 (9) |
O3—C12—C13—C14 | 176.7 (3) | O1i—Zn1—O1—Zn1i | 0.0 |
O2—C12—C13—C14 | −1.5 (4) | N2i—Zn1—O1—Zn1i | −65.96 (12) |
C12—C13—C14—C15 | −0.5 (5) | N1—Zn1—O1—Zn1i | −150.10 (8) |
C13—C14—C15—O5 | 179.6 (3) | O3—C12—O2—Zn1 | −0.3 (3) |
C13—C14—C15—O4 | −1.5 (5) | C13—C12—O2—Zn1 | 177.79 (16) |
C10i—C9—N1—C8 | 86.0 (2) | O1—Zn1—O2—C12 | 154.68 (18) |
C10i—C9—N1—Zn1 | −36.2 (2) | O1i—Zn1—O2—C12 | −130.03 (18) |
C6—C8—N1—C9 | 176.86 (17) | N2i—Zn1—O2—C12 | −37.1 (2) |
C6—C8—N1—Zn1 | −65.00 (18) | N1—Zn1—O2—C12 | 60.5 (2) |
O2—Zn1—N1—C9 | −107.52 (15) |
Symmetry code: (i) −x, −y+2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H2O···O2 | 0.91 (4) | 1.60 (4) | 2.480 (2) | 161 (4) |
Experimental details
Crystal data | |
Chemical formula | [Zn2(C22H22N4O2)(C4H7O4)2] |
Mr | 743.37 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 9.4233 (7), 11.2691 (8), 14.6870 (11) |
β (°) | 96.3816 (8) |
V (Å3) | 1550.0 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.61 |
Crystal size (mm) | 0.35 × 0.30 × 0.25 |
Data collection | |
Diffractometer | Bruker APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.548, 0.667 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9199, 3614, 3166 |
Rint | 0.015 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.085, 1.06 |
No. of reflections | 3614 |
No. of parameters | 217 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.86, −0.30 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990).
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H2O···O2 | 0.91 (4) | 1.60 (4) | 2.480 (2) | 161 (4) |
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Dinuclear zinc(II) cores have attracted much interest as a result of their siganificance in biological systems (Dealwis et al., 1995; Burley et al., 1990; Roderick & Mathews, 1993). In addition, some synthetic dinuclear zinc(II) compounds are found to have functions in dephosphorylation (Bazzicalupi et al., 1997). To further widen the scope of application of zinc compounds, there is a need to prepare new series of dinuclear zinc compounds. In this work, a new dinuclear zinc(II) compound has been synthesized and its structure (I) is reported here.
As shown in Fig. 1, [Zn2L(C4H7O4)2] is a centrosymmetric dinuclear zinc compound. The coordination environment around zinc is a square-pyramid with two N atoms and two O atoms from L ligand occupying the basal positions and one O atom from maleic acid anion occupying the apical position. In the crystal structure the two O atoms from L ligand act as bridging atoms, coordinating two zinc atoms to generate a four-numbered Zn2O2 ring. The Zn—O and Zn—N distances and angles are nomal (Dutta et al., 2005).
The molecule exhibits a strong intramolecular O4—H20···O2 hydrogen bond with an O4··· O2 distance of 2.480 (2) Å.