Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107047282/av3103sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107047282/av3103Isup2.hkl |
CCDC reference: 677206
For related literature, see: Branum et al. (2001); Chiari et al. (1982, 1983); Gao, Meng & Wei (2004); Gao, Meng & Zhu (2004); Hegg & Burstyn (1998); Kim & Wyckoff (1991); Krämer (1999); Lipscomb & Sträer (1996); Meng et al. (2004); Murch et al. (1987); Sakiyama et al. (1999).
All chemicals were of reagent grade and commercially available from the Beijing Chemical Reagents Company of China, and were used without further purification. The ligand CH3—HXTA was synthesized according to the published procedure (Branum et al., 2001). Zn(CH3COO)2·2H2O (0.4390 g, 2 mmol) and Na4(CH3—HXTA) (0.486 g, 1 mmol) were dissolved in water (5 ml) and mixed with stirring at 323 K for 3 h. The resulting colorless solution was filtered and the filtrate was left to stand at room temperature. Colorless crystals of (I) appeared after half a month as a result of slow evaporation of the aqueous solvent.
H atoms attached to C atoms were placed in geometrically idealized positions, with Csp3—H=0.980 (methyl) with Uiso(H)=1.5Ueq, Csp3—H=0.970 Å (methylene), Csp2=0.940 Å, and constrained to ride on their parentatoms, with Uiso(H)=1.2Ueq. H atoms attached to O atoms (in waters) were located in difference Fourier maps and constrained to ride on their parent atoms, with Uiso(H)=1.5Ueq.
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1999); software used to prepare material for publication: SHELXTL/PC (Sheldrick, 1999).
[Zn3(C2H3O2)(C17H17N2O9)(H2O)6]·8H2O | V = 1718.7 (5) Å3 |
Mr = 900.70 | Z = 2 |
Triclinic, P1 | F(000) = 932 |
Hall symbol: -P 1 | Dx = 1.740 Mg m−3 |
a = 10.0095 (18) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.293 (2) Å | µ = 2.17 mm−1 |
c = 14.052 (3) Å | T = 213 K |
α = 93.573 (3)° | Block, colorless |
β = 99.225 (3)° | 0.40 × 0.30 × 0.30 mm |
γ = 110.134 (2)° |
Bruker SMART 1K CCD area-detector diffractometer | 5932 independent reflections |
Radiation source: fine-focus sealed tube | 4769 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | h = −11→10 |
Tmin = 0.477, Tmax = 0.562 | k = −15→15 |
8459 measured reflections | l = −11→16 |
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)] = 0.069 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 1.18 | w = 1/[σ2(Fo2) + (0.0415P)2] where P = (Fo2 + 2Fc2)/3 |
5932 reflections | (Δ/σ)max < 0.001 |
446 parameters | Δρmax = 0.92 e Å−3 |
0 restraints | Δρmin = −0.88 e Å−3 |
[Zn3(C2H3O2)(C17H17N2O9)(H2O)6]·8H2O | γ = 110.134 (2)° |
Mr = 900.70 | V = 1718.7 (5) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.0095 (18) Å | Mo Kα radiation |
b = 13.293 (2) Å | µ = 2.17 mm−1 |
c = 14.052 (3) Å | T = 213 K |
α = 93.573 (3)° | 0.40 × 0.30 × 0.30 mm |
β = 99.225 (3)° |
Bruker SMART 1K CCD area-detector diffractometer | 5932 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | 4769 reflections with I > 2σ(I) |
Tmin = 0.477, Tmax = 0.562 | Rint = 0.035 |
8459 measured reflections |
R[F2 > 2σ(F2)] = 0.069 | 0 restraints |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 1.18 | Δρmax = 0.92 e Å−3 |
5932 reflections | Δρmin = −0.88 e Å−3 |
446 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 | 0.62423 (8) | 0.19713 (5) | 0.36362 (5) | 0.0189 (2) | |
Zn2 | 0.73994 (8) | 0.24244 (5) | 0.62603 (5) | 0.0190 (2) | |
Zn3 | 0.5000 | 0.0000 | 0.0000 | 0.0223 (3) | |
Zn4 | 1.0000 | 0.5000 | 1.0000 | 0.0221 (3) | |
N1 | 0.7606 (5) | 0.3152 (4) | 0.2906 (4) | 0.0188 (12) | |
N2 | 0.6389 (5) | 0.3399 (4) | 0.6913 (4) | 0.0185 (12) | |
C1 | 0.8216 (6) | 0.4544 (5) | 0.4318 (4) | 0.0192 (14) | |
C2 | 0.8481 (6) | 0.5632 (5) | 0.4319 (5) | 0.0223 (15) | |
H2A | 0.9065 | 0.6014 | 0.3903 | 0.027* | |
C3 | 0.7909 (7) | 0.6180 (5) | 0.4915 (5) | 0.0232 (16) | |
C4 | 0.7048 (6) | 0.5593 (5) | 0.5511 (5) | 0.0225 (15) | |
H4A | 0.6656 | 0.5954 | 0.5921 | 0.027* | |
C5 | 0.6735 (6) | 0.4498 (5) | 0.5533 (5) | 0.0199 (14) | |
C6 | 0.7353 (6) | 0.3969 (4) | 0.4945 (4) | 0.0171 (14) | |
C7 | 0.8255 (7) | 0.7379 (5) | 0.4927 (6) | 0.0364 (19) | |
H7B | 0.7757 | 0.7621 | 0.5378 | 0.055* | |
H7C | 0.7938 | 0.7531 | 0.4280 | 0.055* | |
H7D | 0.9293 | 0.7757 | 0.5129 | 0.055* | |
C8 | 0.8809 (6) | 0.3942 (5) | 0.3642 (5) | 0.0241 (15) | |
H8A | 0.9481 | 0.4459 | 0.3313 | 0.029* | |
H8B | 0.9346 | 0.3560 | 0.4022 | 0.029* | |
C9 | 0.6725 (6) | 0.3681 (5) | 0.2353 (5) | 0.0216 (15) | |
H9A | 0.6573 | 0.3431 | 0.1659 | 0.026* | |
H9B | 0.7263 | 0.4462 | 0.2451 | 0.026* | |
C10 | 0.5239 (7) | 0.3464 (5) | 0.2638 (5) | 0.0221 (15) | |
C11 | 0.8099 (6) | 0.2517 (5) | 0.2242 (5) | 0.0214 (15) | |
H11A | 0.8877 | 0.2321 | 0.2602 | 0.026* | |
H11B | 0.8480 | 0.2946 | 0.1737 | 0.026* | |
C12 | 0.6824 (7) | 0.1499 (5) | 0.1775 (5) | 0.0238 (16) | |
C13 | 0.5701 (6) | 0.3857 (5) | 0.6123 (5) | 0.0209 (15) | |
H13A | 0.5255 | 0.4322 | 0.6409 | 0.025* | |
H13B | 0.4926 | 0.3264 | 0.5690 | 0.025* | |
C14 | 0.5279 (6) | 0.2644 (4) | 0.7353 (5) | 0.0204 (15) | |
H14B | 0.4523 | 0.2941 | 0.7418 | 0.025* | |
H14A | 0.5720 | 0.2567 | 0.8006 | 0.025* | |
C15 | 0.4589 (7) | 0.1535 (5) | 0.6750 (5) | 0.0200 (15) | |
C16 | 0.7506 (6) | 0.4252 (4) | 0.7643 (5) | 0.0226 (15) | |
H16B | 0.7147 | 0.4264 | 0.8251 | 0.027* | |
H16A | 0.7655 | 0.4955 | 0.7410 | 0.027* | |
C17 | 0.8941 (7) | 0.4095 (5) | 0.7846 (5) | 0.0211 (15) | |
C18 | 0.8567 (7) | 0.0811 (5) | 0.6591 (5) | 0.0248 (16) | |
C19 | 0.9284 (8) | 0.0038 (6) | 0.6305 (6) | 0.045 (2) | |
H19A | 0.9254 | −0.0460 | 0.6784 | 0.068* | |
H19B | 1.0286 | 0.0442 | 0.6274 | 0.068* | |
H19C | 0.8774 | −0.0363 | 0.5674 | 0.068* | |
O1 | 0.7090 (4) | 0.2895 (3) | 0.4952 (3) | 0.0186 (10) | |
O2 | 0.4772 (4) | 0.2722 (3) | 0.3127 (3) | 0.0244 (11) | |
O3 | 0.4547 (5) | 0.4039 (3) | 0.2296 (4) | 0.0377 (13) | |
O4 | 0.5844 (4) | 0.1098 (3) | 0.2248 (3) | 0.0227 (10) | |
O5 | 0.6818 (4) | 0.1117 (3) | 0.0934 (3) | 0.0270 (11) | |
O6 | 0.5335 (4) | 0.1268 (3) | 0.6202 (3) | 0.0230 (10) | |
O7 | 0.3362 (5) | 0.0945 (3) | 0.6848 (3) | 0.0289 (11) | |
O8 | 0.9127 (4) | 0.3372 (3) | 0.7291 (3) | 0.0248 (11) | |
O9 | 0.9909 (4) | 0.4693 (3) | 0.8511 (3) | 0.0265 (11) | |
O10 | 0.7732 (4) | 0.1169 (3) | 0.3978 (3) | 0.0258 (11) | |
H10A | 0.7497 | 0.0494 | 0.3826 | 0.039* | |
H10B | 0.8100 | 0.1330 | 0.4581 | 0.039* | |
O11 | 0.4597 (4) | 0.0807 (3) | 0.4124 (3) | 0.0254 (11) | |
H11C | 0.4526 | 0.0844 | 0.4719 | 0.038* | |
H11D | 0.4589 | 0.0183 | 0.3939 | 0.038* | |
O12 | 0.8322 (5) | 0.1379 (3) | 0.5932 (3) | 0.0264 (11) | |
O13 | 0.8246 (5) | 0.0865 (3) | 0.7394 (3) | 0.0330 (12) | |
O14 | 0.3864 (4) | 0.1102 (3) | 0.0164 (3) | 0.0278 (11) | |
H14C | 0.3411 | 0.1021 | 0.0633 | 0.042* | |
H14D | 0.3261 | 0.0996 | −0.0366 | 0.042* | |
O15 | 0.4248 (4) | −0.0777 (3) | 0.1138 (3) | 0.0273 (11) | |
H15A | 0.4577 | −0.0444 | 0.1711 | 0.041* | |
H15B | 0.3372 | −0.1190 | 0.1099 | 0.041* | |
O16 | 1.1492 (4) | 0.4212 (3) | 1.0153 (3) | 0.0325 (12) | |
H16C | 1.1534 | 0.3858 | 1.0634 | 0.049* | |
H16D | 1.1300 | 0.3788 | 0.9630 | 0.049* | |
O17 | 1.1671 (5) | 0.6451 (3) | 1.0067 (4) | 0.0352 (13) | |
H17A | 1.1640 | 0.7080 | 1.0161 | 0.053* | |
H17B | 1.2534 | 0.6502 | 1.0039 | 0.053* | |
O18 | 0.9875 (5) | 0.0957 (4) | 0.0994 (4) | 0.0593 (17) | |
H18A | 0.9292 | 0.0479 | 0.1256 | 0.089* | |
H18B | 1.0464 | 0.0702 | 0.0793 | 0.089* | |
O19 | 0.5820 (5) | 0.5477 (3) | 0.1154 (4) | 0.0398 (13) | |
H19D | 0.5506 | 0.5104 | 0.1595 | 0.060* | |
H19E | 0.5981 | 0.5079 | 0.0723 | 0.060* | |
O20 | 0.2607 (4) | 0.0981 (3) | 0.1778 (3) | 0.0306 (11) | |
H20A | 0.2335 | 0.0439 | 0.2086 | 0.046* | |
H20B | 0.3229 | 0.1513 | 0.2164 | 0.046* | |
O21 | 0.4477 (5) | 0.6693 (4) | 0.0101 (3) | 0.0372 (12) | |
H21A | 0.4876 | 0.7305 | −0.0082 | 0.056* | |
H21B | 0.5072 | 0.6589 | 0.0552 | 0.056* | |
O22 | 0.1555 (5) | 0.3179 (3) | 0.1718 (4) | 0.0417 (13) | |
H22A | 0.2456 | 0.3288 | 0.1849 | 0.063* | |
H22B | 0.1271 | 0.3278 | 0.2243 | 0.063* | |
O23 | 0.8712 (5) | 0.1678 (3) | 0.9368 (4) | 0.0385 (13) | |
H23A | 0.9155 | 0.1453 | 0.9825 | 0.058* | |
H23B | 0.8983 | 0.1562 | 0.8842 | 0.058* | |
O24 | 0.2052 (5) | 0.1005 (3) | 0.8460 (3) | 0.0346 (12) | |
H24A | 0.1787 | 0.1547 | 0.8431 | 0.052* | |
H24B | 0.2504 | 0.0975 | 0.8002 | 0.052* | |
O25 | 0.1444 (5) | 0.2896 (4) | 0.8356 (4) | 0.0464 (14) | |
H25A | 0.0700 | 0.2986 | 0.8047 | 0.070* | |
H25B | 0.2187 | 0.3456 | 0.8362 | 0.070* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.0191 (4) | 0.0171 (4) | 0.0187 (4) | 0.0049 (3) | 0.0038 (3) | −0.0009 (3) |
Zn2 | 0.0205 (4) | 0.0177 (4) | 0.0190 (4) | 0.0078 (3) | 0.0034 (3) | 0.0002 (3) |
Zn3 | 0.0230 (6) | 0.0235 (6) | 0.0191 (6) | 0.0084 (5) | 0.0024 (5) | −0.0026 (5) |
Zn4 | 0.0197 (6) | 0.0198 (6) | 0.0238 (7) | 0.0064 (5) | −0.0005 (5) | −0.0026 (5) |
N1 | 0.013 (3) | 0.023 (3) | 0.020 (3) | 0.007 (2) | 0.000 (2) | 0.000 (2) |
N2 | 0.023 (3) | 0.012 (3) | 0.020 (3) | 0.006 (2) | 0.007 (2) | −0.001 (2) |
C1 | 0.015 (3) | 0.023 (3) | 0.014 (4) | 0.004 (3) | −0.005 (3) | −0.002 (3) |
C2 | 0.009 (3) | 0.018 (3) | 0.029 (4) | −0.004 (3) | −0.004 (3) | −0.002 (3) |
C3 | 0.020 (4) | 0.012 (3) | 0.032 (4) | 0.005 (3) | −0.005 (3) | −0.002 (3) |
C4 | 0.020 (4) | 0.024 (4) | 0.021 (4) | 0.009 (3) | −0.004 (3) | −0.007 (3) |
C5 | 0.015 (3) | 0.019 (3) | 0.020 (4) | 0.002 (3) | −0.002 (3) | −0.001 (3) |
C6 | 0.015 (3) | 0.014 (3) | 0.017 (4) | 0.004 (3) | −0.007 (3) | −0.002 (3) |
C7 | 0.030 (4) | 0.023 (4) | 0.053 (5) | 0.008 (3) | 0.009 (4) | 0.002 (4) |
C8 | 0.015 (3) | 0.027 (4) | 0.025 (4) | 0.003 (3) | −0.002 (3) | 0.003 (3) |
C9 | 0.021 (4) | 0.017 (3) | 0.020 (4) | 0.003 (3) | −0.005 (3) | −0.001 (3) |
C10 | 0.026 (4) | 0.016 (3) | 0.023 (4) | 0.009 (3) | 0.001 (3) | −0.001 (3) |
C11 | 0.018 (4) | 0.024 (3) | 0.020 (4) | 0.004 (3) | 0.005 (3) | 0.001 (3) |
C12 | 0.029 (4) | 0.025 (4) | 0.021 (4) | 0.017 (3) | −0.001 (3) | 0.001 (3) |
C13 | 0.012 (3) | 0.023 (3) | 0.026 (4) | 0.006 (3) | 0.001 (3) | −0.002 (3) |
C14 | 0.019 (3) | 0.023 (3) | 0.021 (4) | 0.008 (3) | 0.007 (3) | 0.000 (3) |
C15 | 0.018 (4) | 0.020 (3) | 0.020 (4) | 0.007 (3) | −0.001 (3) | 0.002 (3) |
C16 | 0.029 (4) | 0.014 (3) | 0.020 (4) | 0.006 (3) | 0.001 (3) | −0.008 (3) |
C17 | 0.022 (4) | 0.018 (3) | 0.024 (4) | 0.006 (3) | 0.006 (3) | 0.009 (3) |
C18 | 0.021 (4) | 0.025 (4) | 0.026 (4) | 0.009 (3) | −0.001 (3) | −0.004 (3) |
C19 | 0.065 (6) | 0.042 (5) | 0.044 (5) | 0.034 (4) | 0.017 (4) | 0.013 (4) |
O1 | 0.026 (2) | 0.013 (2) | 0.016 (2) | 0.0043 (18) | 0.0065 (19) | 0.0034 (18) |
O2 | 0.019 (2) | 0.024 (2) | 0.032 (3) | 0.009 (2) | 0.006 (2) | 0.003 (2) |
O3 | 0.031 (3) | 0.037 (3) | 0.055 (4) | 0.020 (2) | 0.012 (3) | 0.017 (3) |
O4 | 0.017 (2) | 0.027 (2) | 0.020 (3) | 0.0025 (19) | 0.006 (2) | −0.003 (2) |
O5 | 0.022 (3) | 0.030 (3) | 0.023 (3) | 0.004 (2) | 0.005 (2) | −0.004 (2) |
O6 | 0.023 (2) | 0.020 (2) | 0.026 (3) | 0.0073 (19) | 0.007 (2) | −0.002 (2) |
O7 | 0.025 (3) | 0.024 (2) | 0.038 (3) | 0.006 (2) | 0.013 (2) | 0.001 (2) |
O8 | 0.022 (2) | 0.022 (2) | 0.031 (3) | 0.011 (2) | 0.002 (2) | −0.005 (2) |
O9 | 0.018 (2) | 0.027 (2) | 0.027 (3) | 0.003 (2) | 0.000 (2) | −0.009 (2) |
O10 | 0.030 (3) | 0.022 (2) | 0.022 (3) | 0.010 (2) | −0.003 (2) | −0.005 (2) |
O11 | 0.028 (3) | 0.021 (2) | 0.027 (3) | 0.006 (2) | 0.009 (2) | 0.001 (2) |
O12 | 0.032 (3) | 0.025 (2) | 0.026 (3) | 0.015 (2) | 0.005 (2) | 0.000 (2) |
O13 | 0.045 (3) | 0.031 (3) | 0.023 (3) | 0.013 (2) | 0.010 (2) | 0.001 (2) |
O14 | 0.029 (3) | 0.034 (3) | 0.024 (3) | 0.015 (2) | 0.008 (2) | 0.003 (2) |
O15 | 0.026 (3) | 0.031 (3) | 0.017 (3) | 0.003 (2) | 0.000 (2) | −0.002 (2) |
O16 | 0.031 (3) | 0.035 (3) | 0.033 (3) | 0.019 (2) | −0.003 (2) | −0.004 (2) |
O17 | 0.026 (3) | 0.019 (2) | 0.057 (4) | 0.006 (2) | 0.009 (2) | −0.004 (2) |
O18 | 0.029 (3) | 0.060 (3) | 0.094 (5) | 0.017 (3) | 0.017 (3) | 0.030 (4) |
O19 | 0.045 (3) | 0.034 (3) | 0.042 (3) | 0.015 (2) | 0.008 (3) | 0.009 (3) |
O20 | 0.024 (3) | 0.033 (3) | 0.031 (3) | 0.006 (2) | 0.003 (2) | 0.005 (2) |
O21 | 0.025 (3) | 0.044 (3) | 0.037 (3) | 0.008 (2) | −0.001 (2) | 0.010 (3) |
O22 | 0.031 (3) | 0.045 (3) | 0.049 (4) | 0.015 (2) | 0.004 (3) | 0.003 (3) |
O23 | 0.038 (3) | 0.038 (3) | 0.040 (3) | 0.012 (2) | 0.015 (2) | −0.003 (3) |
O24 | 0.038 (3) | 0.040 (3) | 0.035 (3) | 0.022 (2) | 0.015 (2) | 0.009 (2) |
O25 | 0.035 (3) | 0.045 (3) | 0.065 (4) | 0.021 (3) | 0.007 (3) | 0.012 (3) |
Zn1—O1 | 2.036 (4) | C11—C12 | 1.523 (8) |
Zn1—O11 | 2.078 (4) | C11—H11A | 0.9800 |
Zn1—O2 | 2.106 (4) | C11—H11B | 0.9800 |
Zn1—O4 | 2.113 (4) | C12—O5 | 1.256 (7) |
Zn1—O10 | 2.126 (4) | C12—O4 | 1.257 (8) |
Zn1—N1 | 2.134 (5) | C13—H13A | 0.9800 |
Zn2—O12 | 1.984 (4) | C13—H13B | 0.9800 |
Zn2—O1 | 1.990 (4) | C14—C15 | 1.525 (8) |
Zn2—O8 | 2.036 (4) | C14—H14B | 0.9800 |
Zn2—O6 | 2.094 (4) | C14—H14A | 0.9800 |
Zn2—N2 | 2.143 (5) | C15—O7 | 1.244 (7) |
Zn3—O15i | 2.061 (4) | C15—O6 | 1.269 (7) |
Zn3—O15 | 2.061 (4) | C16—C17 | 1.507 (8) |
Zn3—O5 | 2.091 (4) | C16—H16B | 0.9800 |
Zn3—O5i | 2.091 (4) | C16—H16A | 0.9800 |
Zn3—O14 | 2.164 (4) | C17—O9 | 1.237 (7) |
Zn3—O14i | 2.164 (4) | C17—O8 | 1.282 (7) |
Zn4—O17 | 2.057 (4) | C18—O13 | 1.227 (8) |
Zn4—O17ii | 2.057 (4) | C18—O12 | 1.276 (8) |
Zn4—O9ii | 2.088 (4) | C18—C19 | 1.510 (8) |
Zn4—O9 | 2.088 (4) | C19—H19A | 0.9700 |
Zn4—O16ii | 2.092 (4) | C19—H19B | 0.9700 |
Zn4—O16 | 2.092 (4) | C19—H19C | 0.9700 |
N1—C9 | 1.468 (7) | O10—H10A | 0.8500 |
N1—C11 | 1.471 (7) | O10—H10B | 0.8501 |
N1—C8 | 1.489 (7) | O11—H11C | 0.8500 |
N2—C14 | 1.468 (7) | O11—H11D | 0.8500 |
N2—C16 | 1.483 (7) | O14—H14C | 0.8500 |
N2—C13 | 1.486 (7) | O14—H14D | 0.8500 |
C1—C2 | 1.378 (8) | O15—H15A | 0.8500 |
C1—C6 | 1.407 (8) | O15—H15B | 0.8500 |
C1—C8 | 1.518 (8) | O16—H16C | 0.8500 |
C2—C3 | 1.387 (8) | O16—H16D | 0.8500 |
C2—H2A | 0.9400 | O17—H17A | 0.8500 |
C3—C4 | 1.380 (9) | O17—H17B | 0.8499 |
C3—C7 | 1.508 (8) | O18—H18A | 0.8500 |
C4—C5 | 1.383 (8) | O18—H18B | 0.8500 |
C4—H4A | 0.9400 | O19—H19D | 0.8500 |
C5—C6 | 1.398 (8) | O19—H19E | 0.8500 |
C5—C13 | 1.496 (8) | O20—H20A | 0.8500 |
C6—O1 | 1.360 (6) | O20—H20B | 0.8500 |
C7—H7B | 0.9700 | O21—H21A | 0.8500 |
C7—H7C | 0.9700 | O21—H21B | 0.8500 |
C7—H7D | 0.9700 | O22—H22A | 0.8500 |
C8—H8A | 0.9800 | O22—H22B | 0.8506 |
C8—H8B | 0.9800 | O23—H23A | 0.8498 |
C9—C10 | 1.538 (8) | O23—H23B | 0.8499 |
C9—H9A | 0.9800 | O24—H24A | 0.8500 |
C9—H9B | 0.9800 | O24—H24B | 0.8499 |
C10—O2 | 1.238 (7) | O25—H25A | 0.8500 |
C10—O3 | 1.264 (7) | O25—H25B | 0.8500 |
O1—Zn1—O11 | 94.90 (16) | N1—C8—H8A | 109.5 |
O1—Zn1—O2 | 97.25 (16) | C1—C8—H8A | 109.5 |
O11—Zn1—O2 | 89.60 (16) | N1—C8—H8B | 109.5 |
O1—Zn1—O4 | 167.44 (16) | C1—C8—H8B | 109.5 |
O11—Zn1—O4 | 94.77 (16) | H8A—C8—H8B | 108.1 |
O2—Zn1—O4 | 90.82 (17) | N1—C9—C10 | 113.7 (5) |
O1—Zn1—O10 | 88.64 (16) | N1—C9—H9A | 108.8 |
O11—Zn1—O10 | 92.99 (16) | C10—C9—H9A | 108.8 |
O2—Zn1—O10 | 173.35 (17) | N1—C9—H9B | 108.8 |
O4—Zn1—O10 | 82.86 (16) | C10—C9—H9B | 108.8 |
O1—Zn1—N1 | 92.85 (17) | H9A—C9—H9B | 107.7 |
O11—Zn1—N1 | 168.87 (18) | O2—C10—O3 | 124.8 (6) |
O2—Zn1—N1 | 81.49 (17) | O2—C10—C9 | 119.4 (5) |
O4—Zn1—N1 | 78.80 (17) | O3—C10—C9 | 115.6 (6) |
O10—Zn1—N1 | 95.18 (17) | N1—C11—C12 | 109.0 (5) |
O12—Zn2—O1 | 97.96 (17) | N1—C11—H11A | 109.9 |
O12—Zn2—O8 | 94.54 (17) | C12—C11—H11A | 109.9 |
O1—Zn2—O8 | 119.23 (17) | N1—C11—H11B | 109.9 |
O12—Zn2—O6 | 95.87 (16) | C12—C11—H11B | 109.9 |
O1—Zn2—O6 | 99.32 (17) | H11A—C11—H11B | 108.3 |
O8—Zn2—O6 | 138.07 (18) | O5—C12—O4 | 124.1 (6) |
O12—Zn2—N2 | 167.19 (19) | O5—C12—C11 | 117.4 (6) |
O1—Zn2—N2 | 94.66 (18) | O4—C12—C11 | 118.5 (6) |
O8—Zn2—N2 | 81.15 (17) | N2—C13—C5 | 113.7 (5) |
O6—Zn2—N2 | 79.83 (17) | N2—C13—H13A | 108.8 |
O15i—Zn3—O15 | 180.00 (12) | C5—C13—H13A | 108.8 |
O15i—Zn3—O5 | 88.07 (16) | N2—C13—H13B | 108.8 |
O15—Zn3—O5 | 91.93 (16) | C5—C13—H13B | 108.8 |
O15i—Zn3—O5i | 91.93 (16) | H13A—C13—H13B | 107.7 |
O15—Zn3—O5i | 88.07 (16) | N2—C14—C15 | 112.1 (5) |
O5—Zn3—O5i | 180.0 (3) | N2—C14—H14B | 109.2 |
O15i—Zn3—O14 | 88.38 (16) | C15—C14—H14B | 109.2 |
O15—Zn3—O14 | 91.63 (16) | N2—C14—H14A | 109.2 |
O5—Zn3—O14 | 88.70 (16) | C15—C14—H14A | 109.2 |
O5i—Zn3—O14 | 91.30 (16) | H14B—C14—H14A | 107.9 |
O15i—Zn3—O14i | 91.62 (16) | O7—C15—O6 | 124.6 (5) |
O15—Zn3—O14i | 88.37 (16) | O7—C15—C14 | 118.2 (5) |
O5—Zn3—O14i | 91.30 (16) | O6—C15—C14 | 117.1 (5) |
O5i—Zn3—O14i | 88.70 (16) | N2—C16—C17 | 113.4 (5) |
O14—Zn3—O14i | 180.0 (3) | N2—C16—H16B | 108.9 |
O17—Zn4—O17ii | 180.000 (1) | C17—C16—H16B | 108.9 |
O17—Zn4—O9ii | 89.67 (18) | N2—C16—H16A | 108.9 |
O17ii—Zn4—O9ii | 90.33 (17) | C17—C16—H16A | 108.9 |
O17—Zn4—O9 | 90.33 (17) | H16B—C16—H16A | 107.7 |
O17ii—Zn4—O9 | 89.67 (18) | O9—C17—O8 | 122.6 (6) |
O9ii—Zn4—O9 | 180.000 (1) | O9—C17—C16 | 119.2 (6) |
O17—Zn4—O16ii | 90.14 (17) | O8—C17—C16 | 118.2 (5) |
O17ii—Zn4—O16ii | 89.86 (17) | O13—C18—O12 | 123.9 (6) |
O9ii—Zn4—O16ii | 84.85 (17) | O13—C18—C19 | 121.4 (7) |
O9—Zn4—O16ii | 95.15 (17) | O12—C18—C19 | 114.6 (6) |
O17—Zn4—O16 | 89.86 (17) | C18—C19—H19A | 109.5 |
O17ii—Zn4—O16 | 90.14 (17) | C18—C19—H19B | 109.5 |
O9ii—Zn4—O16 | 95.15 (17) | H19A—C19—H19B | 109.5 |
O9—Zn4—O16 | 84.85 (17) | C18—C19—H19C | 109.5 |
O16ii—Zn4—O16 | 180.000 (2) | H19A—C19—H19C | 109.5 |
C9—N1—C11 | 110.3 (5) | H19B—C19—H19C | 109.5 |
C9—N1—C8 | 111.4 (4) | C6—O1—Zn2 | 115.5 (4) |
C11—N1—C8 | 113.5 (5) | C6—O1—Zn1 | 115.4 (4) |
C9—N1—Zn1 | 108.4 (4) | Zn2—O1—Zn1 | 128.74 (19) |
C11—N1—Zn1 | 104.0 (3) | C10—O2—Zn1 | 115.1 (4) |
C8—N1—Zn1 | 108.8 (4) | C12—O4—Zn1 | 112.9 (4) |
C14—N2—C16 | 112.5 (5) | C12—O5—Zn3 | 124.8 (4) |
C14—N2—C13 | 110.4 (5) | C15—O6—Zn2 | 114.7 (4) |
C16—N2—C13 | 112.2 (4) | C17—O8—Zn2 | 117.5 (4) |
C14—N2—Zn2 | 104.9 (3) | C17—O9—Zn4 | 132.3 (4) |
C16—N2—Zn2 | 108.9 (4) | Zn1—O10—H10A | 122.2 |
C13—N2—Zn2 | 107.6 (4) | Zn1—O10—H10B | 108.5 |
C2—C1—C6 | 119.3 (6) | H10A—O10—H10B | 108.8 |
C2—C1—C8 | 121.7 (6) | Zn1—O11—H11C | 121.0 |
C6—C1—C8 | 119.0 (5) | Zn1—O11—H11D | 109.4 |
C1—C2—C3 | 121.9 (6) | H11C—O11—H11D | 109.0 |
C1—C2—H2A | 119.0 | C18—O12—Zn2 | 116.9 (4) |
C3—C2—H2A | 119.0 | Zn3—O14—H14C | 114.9 |
C4—C3—C2 | 117.5 (5) | Zn3—O14—H14D | 106.2 |
C4—C3—C7 | 121.6 (6) | H14C—O14—H14D | 109.1 |
C2—C3—C7 | 120.9 (6) | Zn3—O15—H15A | 118.4 |
C3—C4—C5 | 123.1 (6) | Zn3—O15—H15B | 123.0 |
C3—C4—H4A | 118.5 | H15A—O15—H15B | 109.0 |
C5—C4—H4A | 118.5 | Zn4—O16—H16C | 118.3 |
C4—C5—C6 | 118.4 (6) | Zn4—O16—H16D | 106.6 |
C4—C5—C13 | 122.3 (6) | H16C—O16—H16D | 108.9 |
C6—C5—C13 | 119.2 (5) | Zn4—O17—H17A | 127.2 |
O1—C6—C5 | 120.5 (5) | Zn4—O17—H17B | 123.4 |
O1—C6—C1 | 119.8 (5) | H17A—O17—H17B | 109.3 |
C5—C6—C1 | 119.7 (5) | H18A—O18—H18B | 109.1 |
C3—C7—H7B | 109.5 | H19D—O19—H19E | 109.2 |
C3—C7—H7C | 109.5 | H20A—O20—H20B | 109.2 |
H7B—C7—H7C | 109.5 | H21A—O21—H21B | 109.1 |
C3—C7—H7D | 109.5 | H22A—O22—H22B | 108.9 |
H7B—C7—H7D | 109.5 | H23A—O23—H23B | 109.4 |
H7C—C7—H7D | 109.5 | H24A—O24—H24B | 108.8 |
N1—C8—C1 | 110.5 (5) | H25A—O25—H25B | 108.9 |
O1—Zn1—N1—C9 | −105.6 (4) | N2—C16—C17—O9 | −172.8 (6) |
O11—Zn1—N1—C9 | 28.4 (11) | N2—C16—C17—O8 | 10.2 (8) |
O2—Zn1—N1—C9 | −8.7 (3) | C5—C6—O1—Zn2 | −50.4 (6) |
O4—Zn1—N1—C9 | 83.8 (4) | C1—C6—O1—Zn2 | 131.7 (5) |
O10—Zn1—N1—C9 | 165.5 (4) | C5—C6—O1—Zn1 | 123.8 (5) |
O1—Zn1—N1—C11 | 137.0 (3) | C1—C6—O1—Zn1 | −54.1 (6) |
O11—Zn1—N1—C11 | −89.0 (9) | O12—Zn2—O1—C6 | −139.7 (4) |
O2—Zn1—N1—C11 | −126.1 (4) | O8—Zn2—O1—C6 | −39.9 (4) |
O4—Zn1—N1—C11 | −33.6 (3) | O6—Zn2—O1—C6 | 122.9 (4) |
O10—Zn1—N1—C11 | 48.1 (4) | N2—Zn2—O1—C6 | 42.5 (4) |
O1—Zn1—N1—C8 | 15.7 (4) | O12—Zn2—O1—Zn1 | 47.0 (3) |
O11—Zn1—N1—C8 | 149.8 (8) | O8—Zn2—O1—Zn1 | 146.8 (2) |
O2—Zn1—N1—C8 | 112.6 (4) | O6—Zn2—O1—Zn1 | −50.3 (3) |
O4—Zn1—N1—C8 | −154.8 (4) | N2—Zn2—O1—Zn1 | −130.7 (3) |
O10—Zn1—N1—C8 | −73.2 (4) | O11—Zn1—O1—C6 | −131.7 (4) |
O12—Zn2—N2—C14 | −43.8 (10) | O2—Zn1—O1—C6 | −41.5 (4) |
O1—Zn2—N2—C14 | 126.2 (4) | O4—Zn1—O1—C6 | 88.1 (8) |
O8—Zn2—N2—C14 | −114.9 (4) | O10—Zn1—O1—C6 | 135.4 (4) |
O6—Zn2—N2—C14 | 27.5 (4) | N1—Zn1—O1—C6 | 40.3 (4) |
O12—Zn2—N2—C16 | 76.9 (9) | O11—Zn1—O1—Zn2 | 41.6 (3) |
O1—Zn2—N2—C16 | −113.1 (4) | O2—Zn1—O1—Zn2 | 131.8 (3) |
O8—Zn2—N2—C16 | 5.8 (4) | O4—Zn1—O1—Zn2 | −98.6 (7) |
O6—Zn2—N2—C16 | 148.2 (4) | O10—Zn1—O1—Zn2 | −51.3 (3) |
O12—Zn2—N2—C13 | −161.3 (7) | N1—Zn1—O1—Zn2 | −146.4 (3) |
O1—Zn2—N2—C13 | 8.7 (3) | O3—C10—O2—Zn1 | −177.4 (5) |
O8—Zn2—N2—C13 | 127.6 (4) | C9—C10—O2—Zn1 | 6.8 (7) |
O6—Zn2—N2—C13 | −90.0 (3) | O1—Zn1—O2—C10 | 93.0 (4) |
C6—C1—C2—C3 | −0.6 (9) | O11—Zn1—O2—C10 | −172.1 (4) |
C8—C1—C2—C3 | 178.2 (6) | O4—Zn1—O2—C10 | −77.3 (4) |
C1—C2—C3—C4 | −0.4 (9) | O10—Zn1—O2—C10 | −59.1 (15) |
C1—C2—C3—C7 | 177.9 (6) | N1—Zn1—O2—C10 | 1.2 (4) |
C2—C3—C4—C5 | −0.3 (9) | O5—C12—O4—Zn1 | 180.0 (5) |
C7—C3—C4—C5 | −178.6 (6) | C11—C12—O4—Zn1 | −0.5 (7) |
C3—C4—C5—C6 | 1.9 (9) | O1—Zn1—O4—C12 | −29.1 (10) |
C3—C4—C5—C13 | −174.8 (6) | O11—Zn1—O4—C12 | −169.2 (4) |
C4—C5—C6—O1 | 179.2 (5) | O2—Zn1—O4—C12 | 101.1 (4) |
C13—C5—C6—O1 | −4.0 (8) | O10—Zn1—O4—C12 | −76.8 (4) |
C4—C5—C6—C1 | −2.9 (9) | N1—Zn1—O4—C12 | 19.9 (4) |
C13—C5—C6—C1 | 173.9 (5) | O4—C12—O5—Zn3 | 16.2 (9) |
C2—C1—C6—O1 | −179.8 (5) | C11—C12—O5—Zn3 | −163.3 (4) |
C8—C1—C6—O1 | 1.4 (8) | O15i—Zn3—O5—C12 | 143.7 (5) |
C2—C1—C6—C5 | 2.3 (9) | O15—Zn3—O5—C12 | −36.3 (5) |
C8—C1—C6—C5 | −176.6 (5) | O5i—Zn3—O5—C12 | −97 (68) |
C9—N1—C8—C1 | 56.3 (7) | O14—Zn3—O5—C12 | 55.3 (5) |
C11—N1—C8—C1 | −178.4 (5) | O14i—Zn3—O5—C12 | −124.7 (5) |
Zn1—N1—C8—C1 | −63.2 (5) | O7—C15—O6—Zn2 | −177.0 (5) |
C2—C1—C8—N1 | −112.6 (6) | C14—C15—O6—Zn2 | 0.7 (7) |
C6—C1—C8—N1 | 66.2 (7) | O12—Zn2—O6—C15 | 151.2 (4) |
C11—N1—C9—C10 | 127.4 (5) | O1—Zn2—O6—C15 | −109.7 (4) |
C8—N1—C9—C10 | −105.5 (6) | O8—Zn2—O6—C15 | 47.7 (5) |
Zn1—N1—C9—C10 | 14.2 (6) | N2—Zn2—O6—C15 | −16.6 (4) |
N1—C9—C10—O2 | −14.9 (8) | O9—C17—O8—Zn2 | 178.1 (5) |
N1—C9—C10—O3 | 169.0 (5) | C16—C17—O8—Zn2 | −5.0 (7) |
C9—N1—C11—C12 | −74.0 (6) | O12—Zn2—O8—C17 | −168.4 (4) |
C8—N1—C11—C12 | 160.1 (5) | O1—Zn2—O8—C17 | 89.8 (4) |
Zn1—N1—C11—C12 | 42.1 (5) | O6—Zn2—O8—C17 | −64.4 (5) |
N1—C11—C12—O5 | 149.6 (5) | N2—Zn2—O8—C17 | −0.6 (4) |
N1—C11—C12—O4 | −29.9 (8) | O8—C17—O9—Zn4 | −124.3 (6) |
C14—N2—C13—C5 | −170.9 (5) | C16—C17—O9—Zn4 | 58.8 (8) |
C16—N2—C13—C5 | 62.7 (6) | O17—Zn4—O9—C17 | −158.4 (6) |
Zn2—N2—C13—C5 | −57.0 (5) | O17ii—Zn4—O9—C17 | 21.6 (6) |
C4—C5—C13—N2 | −116.0 (6) | O9ii—Zn4—O9—C17 | 72 (100) |
C6—C5—C13—N2 | 67.3 (7) | O16ii—Zn4—O9—C17 | −68.2 (6) |
C16—N2—C14—C15 | −153.4 (5) | O16—Zn4—O9—C17 | 111.8 (6) |
C13—N2—C14—C15 | 80.5 (6) | O13—C18—O12—Zn2 | 1.3 (8) |
Zn2—N2—C14—C15 | −35.1 (5) | C19—C18—O12—Zn2 | −179.4 (4) |
N2—C14—C15—O7 | −157.2 (5) | O1—Zn2—O12—C18 | −173.4 (4) |
N2—C14—C15—O6 | 24.9 (8) | O8—Zn2—O12—C18 | 66.2 (4) |
C14—N2—C16—C17 | 106.2 (6) | O6—Zn2—O12—C18 | −73.1 (4) |
C13—N2—C16—C17 | −128.6 (5) | N2—Zn2—O12—C18 | −3.5 (10) |
Zn2—N2—C16—C17 | −9.6 (6) |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+2, −y+1, −z+2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O25—H25B···O19iii | 0.85 | 1.99 | 2.789 (6) | 157 |
O25—H25A···O8iv | 0.85 | 1.99 | 2.835 (6) | 173 |
O24—H24B···O7 | 0.85 | 1.96 | 2.803 (6) | 173 |
O24—H24A···O25 | 0.85 | 1.94 | 2.790 (6) | 172 |
O23—H23B···O13 | 0.85 | 2.09 | 2.818 (7) | 144 |
O23—H23A···O18v | 0.85 | 1.93 | 2.772 (7) | 169 |
O22—H22A···O3 | 0.85 | 1.96 | 2.772 (6) | 160 |
O21—H21B···O19 | 0.85 | 2.04 | 2.786 (6) | 146 |
O21—H21A···O14vi | 0.85 | 2.08 | 2.910 (6) | 165 |
O20—H20B···O2 | 0.85 | 2.04 | 2.887 (6) | 177 |
O20—H20A···O13vii | 0.85 | 1.87 | 2.710 (6) | 172 |
O19—H19E···O21vi | 0.85 | 2.42 | 3.182 (6) | 150 |
O19—H19D···O3 | 0.85 | 1.85 | 2.687 (7) | 166 |
O18—H18B···O20viii | 0.85 | 2.26 | 2.768 (6) | 119 |
O18—H18A···O24vii | 0.85 | 2.07 | 2.893 (7) | 162 |
O17—H17B···O21ix | 0.85 | 1.86 | 2.707 (6) | 174 |
O17—H17A···O23ii | 0.85 | 1.91 | 2.734 (6) | 165 |
O16—H16D···O25viii | 0.85 | 2.14 | 2.964 (6) | 164 |
O16—H16C···O22ix | 0.85 | 1.82 | 2.667 (7) | 175 |
O15—H15B···O23vii | 0.85 | 1.94 | 2.737 (6) | 155 |
O15—H15A···O4 | 0.85 | 2.02 | 2.678 (5) | 133 |
O14—H14D···O24x | 0.85 | 1.89 | 2.728 (6) | 171 |
O14—H14C···O20 | 0.85 | 1.91 | 2.752 (6) | 173 |
O11—H11D···O6vii | 0.85 | 1.95 | 2.793 (5) | 168 |
O11—H11C···O6 | 0.85 | 2.08 | 2.867 (6) | 154 |
O10—H10B···O12 | 0.85 | 1.87 | 2.691 (6) | 162 |
O10—H10A···O7vii | 0.85 | 1.92 | 2.741 (5) | 163 |
Symmetry codes: (ii) −x+2, −y+1, −z+2; (iii) −x+1, −y+1, −z+1; (iv) x−1, y, z; (v) x, y, z+1; (vi) −x+1, −y+1, −z; (vii) −x+1, −y, −z+1; (viii) x+1, y, z; (ix) x+1, y, z+1; (x) x, y, z−1. |
Experimental details
Crystal data | |
Chemical formula | [Zn3(C2H3O2)(C17H17N2O9)(H2O)6]·8H2O |
Mr | 900.70 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 213 |
a, b, c (Å) | 10.0095 (18), 13.293 (2), 14.052 (3) |
α, β, γ (°) | 93.573 (3), 99.225 (3), 110.134 (2) |
V (Å3) | 1718.7 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.17 |
Crystal size (mm) | 0.40 × 0.30 × 0.30 |
Data collection | |
Diffractometer | Bruker SMART 1K CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2000) |
Tmin, Tmax | 0.477, 0.562 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8459, 5932, 4769 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.069, 0.131, 1.18 |
No. of reflections | 5932 |
No. of parameters | 446 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.92, −0.88 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL/PC (Sheldrick, 1999).
Zn1—O1 | 2.036 (4) | Zn2—N2 | 2.143 (5) |
Zn1—O11 | 2.078 (4) | Zn3—O15i | 2.061 (4) |
Zn1—O2 | 2.106 (4) | Zn3—O15 | 2.061 (4) |
Zn1—O4 | 2.113 (4) | Zn3—O14 | 2.164 (4) |
Zn1—O10 | 2.126 (4) | Zn4—O17 | 2.057 (4) |
Zn1—N1 | 2.134 (5) | Zn4—O9 | 2.088 (4) |
Zn2—O12 | 1.984 (4) | Zn4—O16 | 2.092 (4) |
Zn2—O1 | 1.990 (4) | C1—C6 | 1.407 (8) |
Zn2—O8 | 2.036 (4) | C1—C8 | 1.518 (8) |
Zn2—O6 | 2.094 (4) | ||
O1—Zn1—O11 | 94.90 (16) | O12—Zn2—O8 | 94.54 (17) |
O1—Zn1—O2 | 97.25 (16) | O1—Zn2—O8 | 119.23 (17) |
O11—Zn1—O2 | 89.60 (16) | O12—Zn2—O6 | 95.87 (16) |
O1—Zn1—O4 | 167.44 (16) | O1—Zn2—O6 | 99.32 (17) |
O11—Zn1—O4 | 94.77 (16) | O8—Zn2—O6 | 138.07 (18) |
O2—Zn1—O4 | 90.82 (17) | O12—Zn2—N2 | 167.19 (19) |
O1—Zn1—O10 | 88.64 (16) | O1—Zn2—N2 | 94.66 (18) |
O11—Zn1—O10 | 92.99 (16) | O8—Zn2—N2 | 81.15 (17) |
O2—Zn1—O10 | 173.35 (17) | O6—Zn2—N2 | 79.83 (17) |
O4—Zn1—O10 | 82.86 (16) | O15—Zn3—O5 | 91.93 (16) |
O1—Zn1—N1 | 92.85 (17) | O15—Zn3—O14 | 91.63 (16) |
O11—Zn1—N1 | 168.87 (18) | O5—Zn3—O14 | 88.70 (16) |
O2—Zn1—N1 | 81.49 (17) | O17—Zn4—O9 | 90.33 (17) |
O4—Zn1—N1 | 78.80 (17) | O17—Zn4—O16 | 89.86 (17) |
O10—Zn1—N1 | 95.18 (17) | O9—Zn4—O16 | 84.85 (17) |
O12—Zn2—O1 | 97.96 (17) |
Symmetry code: (i) −x+1, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O25—H25B···O19ii | 0.85 | 1.99 | 2.789 (6) | 156.8 |
O25—H25A···O8iii | 0.85 | 1.99 | 2.835 (6) | 172.9 |
O24—H24B···O7 | 0.85 | 1.96 | 2.803 (6) | 173.3 |
O24—H24A···O25 | 0.85 | 1.94 | 2.790 (6) | 172.4 |
O23—H23B···O13 | 0.85 | 2.09 | 2.818 (7) | 143.9 |
O23—H23A···O18iv | 0.85 | 1.93 | 2.772 (7) | 169.0 |
O22—H22A···O3 | 0.85 | 1.96 | 2.772 (6) | 160.1 |
O21—H21B···O19 | 0.85 | 2.04 | 2.786 (6) | 145.7 |
O21—H21A···O14v | 0.85 | 2.08 | 2.910 (6) | 165.4 |
O20—H20B···O2 | 0.85 | 2.04 | 2.887 (6) | 176.5 |
O20—H20A···O13vi | 0.85 | 1.87 | 2.710 (6) | 171.8 |
O19—H19E···O21v | 0.85 | 2.42 | 3.182 (6) | 150.0 |
O19—H19D···O3 | 0.85 | 1.85 | 2.687 (7) | 165.8 |
O18—H18A···O24vi | 0.85 | 2.07 | 2.893 (7) | 161.6 |
O17—H17B···O21vii | 0.85 | 1.86 | 2.707 (6) | 174.3 |
O17—H17A···O23viii | 0.85 | 1.91 | 2.734 (6) | 164.5 |
O16—H16D···O25ix | 0.85 | 2.14 | 2.964 (6) | 164.4 |
O16—H16C···O22vii | 0.85 | 1.82 | 2.667 (7) | 174.9 |
O15—H15B···O23vi | 0.85 | 1.94 | 2.737 (6) | 154.9 |
O15—H15A···O4 | 0.85 | 2.02 | 2.678 (5) | 133.3 |
O14—H14D···O24x | 0.85 | 1.89 | 2.728 (6) | 170.7 |
O14—H14C···O20 | 0.85 | 1.91 | 2.752 (6) | 172.7 |
O11—H11D···O6vi | 0.85 | 1.95 | 2.793 (5) | 168.3 |
O11—H11C···O6 | 0.85 | 2.08 | 2.867 (6) | 154.3 |
O10—H10B···O12 | 0.85 | 1.87 | 2.691 (6) | 161.6 |
O10—H10A···O7vi | 0.85 | 1.92 | 2.741 (5) | 163.0 |
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) x, y, z+1; (v) −x+1, −y+1, −z; (vi) −x+1, −y, −z+1; (vii) x+1, y, z+1; (viii) −x+2, −y+1, −z+2; (ix) x+1, y, z; (x) x, y, z−1. |
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Zinc enzymes often use coordinated water molecules or internal alcoholic hydroxy residues as nucleophiles to react with electrophilic substrates (Kim & Wyckoff, 1991). The role of zinc centers in these enzymes is to orientate and activate the substrates (Hegg & Burstyn, 1998; Krämer, 1999; Lipscomb & Sträer, 1996). The preparation and development of new metallic model compounds to mimic the activity of nucleases in hydrolytic cleavage of DNA is is an important and prosperous field in bioinorganic chemistry. Previously, we reported a few binuclear metal complexes including Ni2(Meng et al., 2004) and Mg2(Gao, Meng & Wei, 2004) complexes of Cl-HXTA (5-chloro-2-hydroxy-1,3-xylene-α,α-diamine -N,N,N',N'-tetraacetic acid), which are able to scissior DNA hydrolytically. Cl-HXTA is an acyclic dinucleating ligand with a phenolate bridge (Murch et al., 1987). As a pentavalent anionic ligand, it has four methoxycarbonyl chelating arms with two sets of donor atoms, i.e. one N and three O atoms, as the coordination sites. One of the advantages of Cl-HXTA is that most of its dinuclear metal complexes are highly soluble in water.
As a continuation of aforementioned study, we report here a newly synthesized binuclear zinc complex with CH3—HXTA (5-methyl-2-hydroxy-1,3-xylene-α,α-diamine-N,N,N',N'- tetraacetic acid), (I). CH3—HXTA is very similar to Cl-HXTA in structure, with the Cl atom in the later replaced by a methyl group in the former.
Selected geometric parameters of the title compound are listed in Table 1, while the molecular configuration and crystal packing are illustrated in Figs.1 and 2, respectively. Fig.1 shows that the coordination environments of the two oxo-bridged Zn ions are different in geometry and donor atoms, and differ from those in a related Zn complex (Gao, Meng & Zhu, 2004), where the two Zn atoms have similar coordination environments with distorted octahedral geometry. More specifically, The ion Zn1 adopts a distorted octahedral coordination composed of two carboxylate groups, one tertiary N atom, two water molecules, and the bridging phenolate ligand (O1); atom Zn2 adopts a five-coordinate pyramidal geometry, composed of two carboxylate groups, one tertiary N atom from another coordination arm, one acetate anion as the counter-anion, and the bridging phenolate (O1). The Zn1···Zn2 separation of 3.630 (4) Å, which is shorter than the value of 3.745 (3) Å reported by Gao, Meng & Zhu (2004), suggests no obvious metal-metal bond formation. The Zn1—O1 distance is 2.036 (4) Å, while Zn2—O1 distance is 1.990 (4) Å, indicating that the oxo-bridging atom is similar but not equivalent for both Zn1 and Zn2. The Zn1—O1—Zn2 angle is 128.74 (19)° which is less than that found by Gao, Meng & Zhu (2004) [131.7 (3)°]. In spite of this slight difference, the only oxo-bridge is similar to those in the structures reported previously [Zn—O—Zn (Gao, Mneg & Zhu et al., 2004), Ni—O—Ni(Meng et al., 2004) and Mg—O—Mg (Gao, Meng & Wei,2004). The average Zn—O bond length in the phenolate-bridge is 2.014 (4) Å, in accordance with that of the metal-phenolate bonds in other reported dinulear cocomplexes, such as [Fe2(sal)3trien(OMe)]Cl2 (sal=salicylic aldehyde and trien=trethylene tetraamine) (Chiari et al., 1982) and [Fe2(sal)3trien(OH)]Cl2 (Chiari et al., 1983). The complex anion as a whole has a pseudo-C2 axis passing through atoms C7, C3, C6 and O1, as has been reported previously (Sakiyama et al., 1999). The least-square plane of the phenyl ring of CH3—HXTA and the Zn1/O1/Zn2 plane are twisted with a dihedral angle of 52.75 (4)°. Zn3 and Zn4 atoms lie on inversion centers and join binuclear complex units containing Zn1 and Zn2 through O atoms of the carboxylate groups of the CH3—HXTA ligand into an infinire chain (Fig. 2). Zn3 and Zn4 atoms have equal octahedral environment consisting of four O atoms from four water molecules and two acetate carbonyl O atoms from CH3—HXTA ligand. Thus, an infinite one-dimensional coordination poylmer is constructed (Fig. 2). In this chain, the Zn1···Zn3 separation is 5.345 (4) Å and the Zn2···Zn4 separation is 5.775 (4) Å. Along the chain, the neighboring aromatic rings are distributed alternately above and below the chain. This chain extends infinitely with a repeating unit [e.g: Zn3A···Zn3B] of 28.955 (4) Å (Fig. 2). Between the coordination chains, the shortest Zn···Zn separations are 5.750 (4) and 6.806 (4) Å. The whole structure is stabilized by a hydrogen- bond net, which is formed maily by solvent water molecules, as shown in Fig.2. Their geometric parameters are also listed in Table 2.
In summary, we have described a novel coordination polymer structure constructed by Zn—O—Zn bridges and Zn-4H2O units. Its bioactivity, for example as DNA cleavage agent, is under investigation in our laboratory.