Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807054852/bt2574sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807054852/bt2574Isup2.hkl |
CCDC reference: 672612
A solution of salicylic acid (1.0 mmol, 0.138 g) and sodium hydroxde (1.0 mmol, 0.040 g) in methanol (8 ml) was added to a solution of zinc acetate (1.0 mmol, 0.183 g) in methanol (8 ml). 1,10-Phenanthroline (1.0 mmol, 0.180 g), dissolved in methanol (5 ml), was then added. The mixture was placed in a 25-ml Teflon-lined stainless-steel Parr bomb. The bomb was heated at 363 K for five days. Colorless prismatic crystals were collected manually from the cool solution.
The hydroxy group of one of the two salicylate groups is disordered over two positions. The phenylene ring was refined as a rigid hexagon of 1.39 Å sides, and the hydroxy group was placed on both ortho-positions, subject to the two C–O distances being within 0.01 Å of each other. These were restrained to be nearly coplanar with the ring.
Carbon-hydrogen atoms were placed in calculated positions (C—H 0.93 Å), and were included in the refinement in the riding model approximation, with their temperature factors set to 1.2 times the Ueq of the parent atoms.
Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
Fig. 1. Thermal displacement ellipsoid plot (50% probability) showing the numbering scheme. Hydrogen atoms are drawn as spheres of arbitrary radii; the minor disorder component is not shown. |
[Zn3(C2H3O2)2(C7H5O3)4(C12H8N2)2] | F(000) = 1248 |
Mr = 1223.05 | Dx = 1.608 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 873 reflections |
a = 10.534 (3) Å | θ = 2.6–27.3° |
b = 11.682 (3) Å | µ = 1.49 mm−1 |
c = 20.533 (5) Å | T = 293 K |
β = 91.847 (3)° | Prism, colorless |
V = 2526 (1) Å3 | 0.20 × 0.16 × 0.15 mm |
Z = 2 |
Bruker SMART diffractometer | 5515 independent reflections |
Radiation source: fine-focus sealed tube | 4428 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
ϕ and ω scans | θmax = 27.1°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→13 |
Tmin = 0.524, Tmax = 0.807 | k = −13→15 |
14442 measured reflections | l = −22→26 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 0.87 | w = 1/[σ2(Fo2) + (0.0711P)2 + 2.1051P] where P = (Fo2 + 2Fc2)/3 |
5515 reflections | (Δ/σ)max = 0.001 |
369 parameters | Δρmax = 0.65 e Å−3 |
6 restraints | Δρmin = −0.66 e Å−3 |
[Zn3(C2H3O2)2(C7H5O3)4(C12H8N2)2] | V = 2526 (1) Å3 |
Mr = 1223.05 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.534 (3) Å | µ = 1.49 mm−1 |
b = 11.682 (3) Å | T = 293 K |
c = 20.533 (5) Å | 0.20 × 0.16 × 0.15 mm |
β = 91.847 (3)° |
Bruker SMART diffractometer | 5515 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4428 reflections with I > 2σ(I) |
Tmin = 0.524, Tmax = 0.807 | Rint = 0.027 |
14442 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 6 restraints |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 0.87 | Δρmax = 0.65 e Å−3 |
5515 reflections | Δρmin = −0.66 e Å−3 |
369 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Zn1 | 0.5000 | 0.5000 | 0.5000 | 0.03664 (12) | |
Zn2 | 0.66125 (3) | 0.24138 (2) | 0.481223 (14) | 0.03545 (10) | |
O1 | 0.4523 (2) | 0.42396 (19) | 0.41149 (10) | 0.0558 (5) | |
O2 | 0.52731 (19) | 0.24531 (17) | 0.40656 (10) | 0.0469 (5) | |
O3 | 0.4709 (3) | 0.1262 (3) | 0.30547 (17) | 0.0597 (11) | 0.678 (6) |
H3O | 0.5132 | 0.1318 | 0.3395 | 0.072* | 0.678 (6) |
O3' | 0.3022 (7) | 0.4892 (6) | 0.3252 (4) | 0.129 (6) | 0.322 (6) |
H3' | 0.3424 | 0.4992 | 0.3596 | 0.155* | 0.322 (6) |
O4 | 0.4271 (2) | 0.36795 (18) | 0.55363 (12) | 0.0564 (6) | |
O5 | 0.54382 (19) | 0.20916 (17) | 0.55701 (10) | 0.0449 (5) | |
O6 | 0.2546 (3) | 0.4024 (2) | 0.63370 (17) | 0.0939 (11) | |
H6O | 0.1961 | 0.4394 | 0.6486 | 0.113* | |
O7 | 0.68027 (17) | 0.41700 (17) | 0.49590 (10) | 0.0436 (4) | |
O8 | 0.8313 (2) | 0.3264 (2) | 0.54866 (12) | 0.0654 (6) | |
N1 | 0.8123 (2) | 0.23767 (18) | 0.41080 (11) | 0.0383 (5) | |
N2 | 0.7265 (2) | 0.06882 (19) | 0.48697 (11) | 0.0387 (5) | |
C1 | 0.4616 (2) | 0.3288 (2) | 0.38461 (13) | 0.0402 (6) | |
C2 | 0.3911 (2) | 0.3120 (3) | 0.32077 (13) | 0.0410 (6) | |
C3 | 0.3126 (3) | 0.3986 (3) | 0.29541 (15) | 0.0538 (8) | |
H3 | 0.3066 | 0.4674 | 0.3179 | 0.065* | 0.322 (6) |
C4 | 0.2437 (3) | 0.3843 (4) | 0.23748 (17) | 0.0643 (9) | |
H4 | 0.1895 | 0.4418 | 0.2222 | 0.077* | |
C5 | 0.2556 (3) | 0.2851 (4) | 0.20281 (17) | 0.0654 (10) | |
H5 | 0.2105 | 0.2759 | 0.1635 | 0.078* | |
C6 | 0.3336 (4) | 0.1993 (4) | 0.22567 (17) | 0.0666 (10) | |
H6 | 0.3430 | 0.1331 | 0.2011 | 0.080* | |
C7 | 0.3996 (3) | 0.2101 (3) | 0.28591 (16) | 0.0519 (7) | |
H7 | 0.4486 | 0.1499 | 0.3024 | 0.062* | 0.678 (6) |
C8 | 0.4555 (3) | 0.2705 (2) | 0.57659 (13) | 0.0382 (6) | |
C9 | 0.3734 (3) | 0.2265 (2) | 0.62912 (13) | 0.0415 (6) | |
C10 | 0.2767 (3) | 0.2940 (3) | 0.65424 (17) | 0.0570 (8) | |
C11 | 0.1974 (4) | 0.2487 (4) | 0.7010 (2) | 0.0700 (10) | |
H11 | 0.1336 | 0.2936 | 0.7180 | 0.084* | |
C12 | 0.2137 (4) | 0.1386 (4) | 0.72163 (18) | 0.0705 (11) | |
H12 | 0.1600 | 0.1090 | 0.7525 | 0.085* | |
C13 | 0.3079 (4) | 0.0706 (3) | 0.69766 (17) | 0.0648 (9) | |
H13 | 0.3177 | −0.0046 | 0.7118 | 0.078* | |
C14 | 0.3882 (3) | 0.1158 (3) | 0.65202 (15) | 0.0504 (7) | |
H14 | 0.4534 | 0.0708 | 0.6365 | 0.060* | |
C15 | 0.7842 (3) | 0.4174 (3) | 0.53085 (14) | 0.0437 (6) | |
C16 | 0.8460 (3) | 0.5300 (3) | 0.5450 (2) | 0.0737 (11) | |
H16A | 0.9148 | 0.5196 | 0.5762 | 0.110* | |
H16B | 0.7849 | 0.5818 | 0.5623 | 0.110* | |
H16C | 0.8782 | 0.5612 | 0.5055 | 0.110* | |
C17 | 0.8725 (2) | 0.1351 (2) | 0.40841 (13) | 0.0381 (6) | |
C18 | 0.8542 (3) | 0.3217 (3) | 0.37389 (15) | 0.0494 (7) | |
H18 | 0.8133 | 0.3921 | 0.3750 | 0.059* | |
C19 | 0.9572 (3) | 0.3090 (3) | 0.33339 (16) | 0.0584 (8) | |
H19 | 0.9847 | 0.3705 | 0.3088 | 0.070* | |
C20 | 1.0167 (3) | 0.2069 (3) | 0.33018 (17) | 0.0587 (8) | |
H20 | 1.0847 | 0.1974 | 0.3029 | 0.070* | |
C21 | 0.9755 (3) | 0.1147 (3) | 0.36844 (15) | 0.0468 (7) | |
C22 | 1.0342 (3) | 0.0040 (3) | 0.36999 (18) | 0.0603 (9) | |
H22 | 1.1030 | −0.0097 | 0.3438 | 0.072* | |
C23 | 0.9925 (3) | −0.0803 (3) | 0.40818 (18) | 0.0567 (8) | |
H23 | 1.0324 | −0.1513 | 0.4078 | 0.068* | |
C24 | 0.8880 (3) | −0.0626 (2) | 0.44929 (15) | 0.0466 (7) | |
C25 | 0.8397 (3) | −0.1471 (3) | 0.49062 (18) | 0.0560 (8) | |
H25 | 0.8769 | −0.2192 | 0.4925 | 0.067* | |
C26 | 0.7391 (3) | −0.1231 (3) | 0.52754 (19) | 0.0581 (8) | |
H26 | 0.7064 | −0.1790 | 0.5546 | 0.070* | |
C27 | 0.6841 (3) | −0.0141 (3) | 0.52503 (16) | 0.0492 (7) | |
H27 | 0.6153 | 0.0010 | 0.5510 | 0.059* | |
C28 | 0.8269 (2) | 0.0453 (2) | 0.44954 (13) | 0.0380 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.0366 (2) | 0.0344 (2) | 0.0390 (2) | 0.00356 (17) | 0.00383 (17) | −0.00187 (16) |
Zn2 | 0.03094 (17) | 0.03523 (17) | 0.04044 (18) | 0.00558 (11) | 0.00519 (12) | −0.00037 (12) |
O1 | 0.0630 (14) | 0.0581 (13) | 0.0454 (11) | 0.0113 (11) | −0.0103 (10) | −0.0113 (10) |
O2 | 0.0380 (10) | 0.0533 (12) | 0.0489 (11) | 0.0051 (9) | −0.0029 (9) | −0.0045 (9) |
O3 | 0.070 (2) | 0.0418 (18) | 0.066 (2) | 0.0129 (15) | −0.0090 (17) | −0.0103 (15) |
O3' | 0.197 (14) | 0.058 (6) | 0.126 (10) | 0.027 (7) | −0.093 (9) | −0.004 (5) |
O4 | 0.0528 (13) | 0.0425 (11) | 0.0755 (15) | 0.0102 (9) | 0.0252 (11) | 0.0150 (10) |
O5 | 0.0420 (11) | 0.0445 (10) | 0.0490 (11) | 0.0098 (9) | 0.0151 (9) | 0.0066 (9) |
O6 | 0.091 (2) | 0.0586 (16) | 0.136 (3) | 0.0258 (15) | 0.064 (2) | 0.0017 (16) |
O7 | 0.0328 (9) | 0.0445 (10) | 0.0535 (11) | 0.0034 (8) | 0.0017 (8) | −0.0069 (9) |
O8 | 0.0687 (16) | 0.0620 (15) | 0.0647 (15) | 0.0163 (12) | −0.0107 (12) | 0.0029 (12) |
N1 | 0.0340 (11) | 0.0385 (11) | 0.0425 (12) | 0.0029 (9) | 0.0054 (9) | −0.0004 (9) |
N2 | 0.0295 (11) | 0.0382 (11) | 0.0485 (13) | 0.0000 (9) | 0.0031 (9) | −0.0008 (10) |
C1 | 0.0317 (13) | 0.0522 (16) | 0.0368 (13) | −0.0007 (11) | 0.0050 (10) | 0.0010 (12) |
C2 | 0.0333 (13) | 0.0541 (16) | 0.0360 (13) | −0.0066 (12) | 0.0057 (11) | −0.0014 (12) |
C3 | 0.0505 (18) | 0.066 (2) | 0.0440 (16) | −0.0023 (15) | −0.0028 (14) | 0.0100 (15) |
C4 | 0.0525 (19) | 0.091 (3) | 0.0493 (18) | −0.0137 (18) | −0.0038 (15) | 0.0202 (18) |
C5 | 0.052 (2) | 0.099 (3) | 0.0448 (17) | −0.023 (2) | 0.0001 (15) | 0.0067 (18) |
C6 | 0.064 (2) | 0.080 (2) | 0.056 (2) | −0.021 (2) | 0.0080 (17) | −0.0212 (18) |
C7 | 0.0437 (16) | 0.0589 (18) | 0.0535 (18) | −0.0064 (14) | 0.0071 (14) | −0.0056 (14) |
C8 | 0.0337 (13) | 0.0402 (14) | 0.0409 (14) | 0.0000 (11) | 0.0046 (11) | −0.0002 (11) |
C9 | 0.0377 (14) | 0.0491 (15) | 0.0379 (14) | −0.0026 (12) | 0.0056 (11) | −0.0011 (11) |
C10 | 0.0523 (19) | 0.0594 (19) | 0.0605 (19) | 0.0004 (15) | 0.0206 (15) | −0.0074 (16) |
C11 | 0.057 (2) | 0.088 (3) | 0.067 (2) | −0.0026 (18) | 0.0285 (18) | −0.0063 (19) |
C12 | 0.059 (2) | 0.102 (3) | 0.051 (2) | −0.019 (2) | 0.0160 (16) | 0.0064 (19) |
C13 | 0.064 (2) | 0.073 (2) | 0.058 (2) | −0.0118 (18) | 0.0048 (17) | 0.0216 (17) |
C14 | 0.0454 (16) | 0.0560 (18) | 0.0499 (17) | 0.0018 (14) | 0.0045 (13) | 0.0088 (14) |
C15 | 0.0356 (14) | 0.0475 (16) | 0.0483 (16) | 0.0001 (12) | 0.0071 (12) | −0.0066 (12) |
C16 | 0.051 (2) | 0.066 (2) | 0.105 (3) | −0.0151 (17) | 0.009 (2) | −0.028 (2) |
C17 | 0.0296 (12) | 0.0433 (14) | 0.0415 (14) | 0.0036 (10) | 0.0022 (10) | −0.0070 (11) |
C18 | 0.0488 (17) | 0.0483 (16) | 0.0514 (17) | 0.0019 (13) | 0.0065 (13) | 0.0045 (13) |
C19 | 0.0503 (18) | 0.069 (2) | 0.0561 (19) | −0.0085 (16) | 0.0112 (15) | 0.0123 (16) |
C20 | 0.0429 (17) | 0.078 (2) | 0.0565 (19) | 0.0025 (16) | 0.0166 (14) | −0.0009 (17) |
C21 | 0.0332 (14) | 0.0600 (18) | 0.0475 (16) | 0.0049 (12) | 0.0073 (12) | −0.0122 (13) |
C22 | 0.0428 (17) | 0.070 (2) | 0.069 (2) | 0.0168 (15) | 0.0123 (15) | −0.0173 (17) |
C23 | 0.0453 (17) | 0.0496 (17) | 0.075 (2) | 0.0146 (14) | 0.0012 (15) | −0.0216 (16) |
C24 | 0.0371 (14) | 0.0393 (14) | 0.0628 (18) | 0.0056 (11) | −0.0061 (13) | −0.0117 (13) |
C25 | 0.0543 (19) | 0.0330 (14) | 0.080 (2) | 0.0044 (13) | −0.0091 (16) | −0.0025 (14) |
C26 | 0.0549 (19) | 0.0410 (16) | 0.078 (2) | −0.0074 (14) | 0.0013 (17) | 0.0116 (15) |
C27 | 0.0370 (15) | 0.0475 (16) | 0.0635 (19) | −0.0033 (12) | 0.0082 (13) | 0.0048 (14) |
C28 | 0.0293 (12) | 0.0387 (13) | 0.0457 (14) | 0.0031 (10) | −0.0012 (11) | −0.0063 (11) |
Zn1—O4 | 2.058 (2) | C6—H6 | 0.9300 |
Zn1—O4i | 2.058 (2) | C7—H7 | 0.9300 |
Zn1—O1i | 2.070 (2) | C8—C9 | 1.496 (4) |
Zn1—O1 | 2.070 (2) | C9—C14 | 1.382 (4) |
Zn1—O7i | 2.1362 (19) | C9—C10 | 1.400 (4) |
Zn1—O7 | 2.1362 (19) | C10—C11 | 1.396 (5) |
Zn2—O2 | 2.050 (2) | C11—C12 | 1.363 (6) |
Zn2—O5 | 2.0537 (19) | C11—H11 | 0.9300 |
Zn2—O7 | 2.082 (2) | C12—C13 | 1.375 (6) |
Zn2—N2 | 2.132 (2) | C12—H12 | 0.9300 |
Zn2—N1 | 2.185 (2) | C13—C14 | 1.387 (4) |
Zn2—O8 | 2.440 (3) | C13—H13 | 0.9300 |
O1—C1 | 1.246 (3) | C14—H14 | 0.9300 |
O2—C1 | 1.270 (3) | C15—C16 | 1.492 (4) |
O3—C7 | 1.291 (4) | C16—H16A | 0.9600 |
O3—H3O | 0.8200 | C16—H16B | 0.9600 |
O3'—C3 | 1.228 (8) | C16—H16C | 0.9600 |
O3'—H3' | 0.8200 | C17—C21 | 1.401 (4) |
O4—C8 | 1.265 (3) | C17—C28 | 1.439 (4) |
O5—C8 | 1.250 (3) | C18—C19 | 1.396 (4) |
O6—C10 | 1.353 (4) | C18—H18 | 0.9300 |
O6—H6O | 0.8200 | C19—C20 | 1.350 (5) |
O7—C15 | 1.290 (3) | C19—H19 | 0.9300 |
O8—C15 | 1.224 (4) | C20—C21 | 1.410 (5) |
N1—C18 | 1.324 (4) | C20—H20 | 0.9300 |
N1—C17 | 1.357 (3) | C21—C22 | 1.433 (4) |
N2—C27 | 1.331 (4) | C22—C23 | 1.342 (5) |
N2—C28 | 1.356 (3) | C22—H22 | 0.9300 |
C1—C2 | 1.499 (4) | C23—C24 | 1.424 (4) |
C2—C7 | 1.393 (4) | C23—H23 | 0.9300 |
C2—C3 | 1.397 (4) | C24—C25 | 1.407 (5) |
C3—C4 | 1.384 (5) | C24—C28 | 1.415 (4) |
C3—H3 | 0.9300 | C25—C26 | 1.352 (5) |
C4—C5 | 1.368 (6) | C25—H25 | 0.9300 |
C4—H4 | 0.9300 | C26—C27 | 1.399 (4) |
C5—C6 | 1.370 (6) | C26—H26 | 0.9300 |
C5—H5 | 0.9300 | C27—H27 | 0.9300 |
C6—C7 | 1.405 (5) | ||
O4—Zn1—O4i | 180.00 (8) | C2—C7—C6 | 119.4 (3) |
O4—Zn1—O1i | 86.34 (10) | C2—C7—H7 | 120.3 |
O4i—Zn1—O1i | 93.66 (10) | C6—C7—H7 | 120.3 |
O4—Zn1—O1 | 93.66 (10) | O5—C8—O4 | 124.4 (3) |
O4i—Zn1—O1 | 86.34 (10) | O5—C8—C9 | 119.2 (2) |
O1i—Zn1—O1 | 180.0 | O4—C8—C9 | 116.3 (2) |
O4—Zn1—O7i | 88.39 (8) | C14—C9—C10 | 118.5 (3) |
O4i—Zn1—O7i | 91.61 (8) | C14—C9—C8 | 120.4 (3) |
O1i—Zn1—O7i | 87.79 (8) | C10—C9—C8 | 121.1 (3) |
O1—Zn1—O7i | 92.21 (8) | O6—C10—C11 | 118.0 (3) |
O4—Zn1—O7 | 91.61 (8) | O6—C10—C9 | 122.2 (3) |
O4i—Zn1—O7 | 88.39 (8) | C11—C10—C9 | 119.9 (3) |
O1i—Zn1—O7 | 92.21 (8) | C12—C11—C10 | 120.0 (4) |
O1—Zn1—O7 | 87.79 (8) | C12—C11—H11 | 120.0 |
O7i—Zn1—O7 | 180.0 | C10—C11—H11 | 120.0 |
O2—Zn2—O5 | 98.85 (9) | C11—C12—C13 | 121.2 (3) |
O2—Zn2—O7 | 98.44 (8) | C11—C12—H12 | 119.4 |
O5—Zn2—O7 | 97.38 (8) | C13—C12—H12 | 119.4 |
O2—Zn2—N2 | 105.98 (8) | C12—C13—C14 | 119.0 (4) |
O5—Zn2—N2 | 89.18 (8) | C12—C13—H13 | 120.5 |
O7—Zn2—N2 | 153.43 (8) | C14—C13—H13 | 120.5 |
O2—Zn2—N1 | 90.23 (9) | C9—C14—C13 | 121.4 (3) |
O5—Zn2—N1 | 165.29 (8) | C9—C14—H14 | 119.3 |
O7—Zn2—N1 | 92.67 (8) | C13—C14—H14 | 119.3 |
N2—Zn2—N1 | 77.15 (8) | O8—C15—O7 | 119.4 (3) |
O2—Zn2—O8 | 152.90 (8) | O8—C15—C16 | 122.5 (3) |
O5—Zn2—O8 | 95.38 (9) | O7—C15—C16 | 118.0 (3) |
O7—Zn2—O8 | 56.72 (8) | C15—C16—H16A | 109.5 |
N2—Zn2—O8 | 97.13 (8) | C15—C16—H16B | 109.5 |
N1—Zn2—O8 | 81.17 (9) | H16A—C16—H16B | 109.5 |
C1—O1—Zn1 | 138.7 (2) | C15—C16—H16C | 109.5 |
C1—O2—Zn2 | 129.52 (18) | H16A—C16—H16C | 109.5 |
C7—O3—H3O | 120.0 | H16B—C16—H16C | 109.5 |
C3—O3'—H3' | 120.0 | N1—C17—C21 | 122.9 (3) |
C8—O4—Zn1 | 141.86 (19) | N1—C17—C28 | 117.2 (2) |
C8—O5—Zn2 | 127.65 (18) | C21—C17—C28 | 119.9 (3) |
C10—O6—H6O | 120.0 | N1—C18—C19 | 122.8 (3) |
C15—O7—Zn2 | 99.21 (17) | N1—C18—H18 | 118.6 |
C15—O7—Zn1 | 135.74 (18) | C19—C18—H18 | 118.6 |
Zn2—O7—Zn1 | 111.80 (9) | C20—C19—C18 | 119.6 (3) |
C15—O8—Zn2 | 84.32 (18) | C20—C19—H19 | 120.2 |
C18—N1—C17 | 118.0 (2) | C18—C19—H19 | 120.2 |
C18—N1—Zn2 | 128.86 (19) | C19—C20—C21 | 119.7 (3) |
C17—N1—Zn2 | 113.11 (17) | C19—C20—H20 | 120.1 |
C27—N2—C28 | 117.9 (2) | C21—C20—H20 | 120.1 |
C27—N2—Zn2 | 127.40 (19) | C17—C21—C20 | 117.0 (3) |
C28—N2—Zn2 | 114.59 (17) | C17—C21—C22 | 118.8 (3) |
O1—C1—O2 | 125.3 (3) | C20—C21—C22 | 124.1 (3) |
O1—C1—C2 | 117.4 (3) | C23—C22—C21 | 121.7 (3) |
O2—C1—C2 | 117.3 (2) | C23—C22—H22 | 119.1 |
C7—C2—C3 | 118.3 (3) | C21—C22—H22 | 119.1 |
C7—C2—C1 | 121.6 (3) | C22—C23—C24 | 120.9 (3) |
C3—C2—C1 | 120.1 (3) | C22—C23—H23 | 119.6 |
O3'—C3—C4 | 118.6 (6) | C24—C23—H23 | 119.6 |
O3'—C3—C2 | 120.0 (5) | C25—C24—C28 | 116.7 (3) |
C4—C3—C2 | 121.4 (3) | C25—C24—C23 | 123.8 (3) |
C4—C3—H3 | 119.3 | C28—C24—C23 | 119.5 (3) |
C2—C3—H3 | 119.3 | C26—C25—C24 | 119.9 (3) |
C5—C4—C3 | 119.7 (4) | C26—C25—H25 | 120.1 |
C5—C4—H4 | 120.2 | C24—C25—H25 | 120.1 |
C3—C4—H4 | 120.2 | C25—C26—C27 | 119.9 (3) |
C4—C5—C6 | 120.4 (3) | C25—C26—H26 | 120.0 |
C4—C5—H5 | 119.8 | C27—C26—H26 | 120.0 |
C6—C5—H5 | 119.8 | N2—C27—C26 | 122.5 (3) |
C5—C6—C7 | 120.7 (4) | N2—C27—H27 | 118.7 |
C5—C6—H6 | 119.7 | C26—C27—H27 | 118.7 |
C7—C6—H6 | 119.7 | N2—C28—C24 | 123.1 (3) |
O3—C7—C2 | 122.4 (3) | N2—C28—C17 | 117.8 (2) |
O3—C7—C6 | 118.1 (3) | C24—C28—C17 | 119.1 (2) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Zn3(C2H3O2)2(C7H5O3)4(C12H8N2)2] |
Mr | 1223.05 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 10.534 (3), 11.682 (3), 20.533 (5) |
β (°) | 91.847 (3) |
V (Å3) | 2526 (1) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.49 |
Crystal size (mm) | 0.20 × 0.16 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.524, 0.807 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14442, 5515, 4428 |
Rint | 0.027 |
(sin θ/λ)max (Å−1) | 0.642 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.109, 0.87 |
No. of reflections | 5515 |
No. of parameters | 369 |
No. of restraints | 6 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.65, −0.66 |
Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
The 2,2'-bipyridine adduct of zinc disalicylate exists in two form, a monomeric form (Lemoine et al., 2004) and a cyclotetrameric form (Wang et al., 2004). The attempt to synthesize the 1,10-phenanthroline analog gave the trinuclear compound in which part of the acetate entity that was present as the counterion is incorporated. The centrosymmetric trinuclear compound has six carboxylate groups each bridging two metal centers. The zinc atom on a center-of-inversion is coordinated to six oxygen atoms in an octahedral environment. The other zinc atoms are each chelated by the N-heterocycle, but their coordination number is six as the acetate group that is engaged in bridging also functions as a chelating group (Fig. 1).