Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802002088/na6135sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802002088/na6135Isup2.hkl |
CCDC reference: 182588
Key indicators
- Single-crystal X-ray study
- T = 160 K
- Mean (C-C) = 0.003 Å
- R factor = 0.027
- wR factor = 0.072
- Data-to-parameter ratio = 13.5
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.70 From the CIF: _reflns_number_total 3940 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 4306 Completeness (_total/calc) 91.50% Alert C: < 95% complete General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.70 From the CIF: _reflns_number_total 3940 From the CIF: _diffrn_reflns_limit_ max hkl 20. 12. 24. From the CIF: _diffrn_reflns_limit_ min hkl -23. -12. -22. TEST1: Expected hkl limits for theta max Calculated maximum hkl 23. 13. 26. Calculated minimum hkl -23. -13. -26. ALERT: Expected hkl max differ from CIF values
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
The title complex was prepared by the reaction of zinc benzoate (10 mmol) and diethylnicotinamide (20 mmol) in 100 ml of water. The reaction mixture was filtered and set aside for crystallization at room temperature for several days, during which time colourless single crystals were deposited.
The data at the highest angles are incomplete because of a relatively large crystal-to-detector distance in an early experiment with one of the first commercial CCD diffractometers before operating parameters were optimized; nevertheless, data are essentially complete to θ = 24°. H atoms were placed geometrically and refined with a riding model (including free rotation about C—C bonds), and with Uiso constrained to be 1.2 (1.5 for methyl groups) times Ueq of the carrier atom.
Data collection: SMART (Siemens, 1995); cell refinement: local programs; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.
Fig. 1. The molecular structure of (I) with atom labels and 50% probability ellipsoids for non-H atoms. |
[Zn2(C7H5O2)4(C10H14N2O)2] | Dx = 1.426 Mg m−3 |
Mr = 971.64 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pbca | Cell parameters from 14194 reflections |
a = 19.5680 (19) Å | θ = 2.1–25.6° |
b = 10.6989 (10) Å | µ = 1.12 mm−1 |
c = 21.617 (2) Å | T = 160 K |
V = 4525.6 (8) Å3 | Block, colourless |
Z = 4 | 0.32 × 0.26 × 0.26 mm |
F(000) = 2016 |
Siemens SMART 1K CCD diffractometer | 3940 independent reflections |
Radiation source: sealed tube | 3659 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
Detector resolution: 8.192 pixels mm-1 | θmax = 25.7°, θmin = 1.9° |
ω rotation with narrow frames scans | h = −23→20 |
Absorption correction: multi-scan (SHELXTL; Sheldrick, 1977) | k = −12→12 |
Tmin = 0.683, Tmax = 0.782 | l = −22→24 |
18548 measured reflections |
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0328P)2 + 2.6031P] where P = (Fo2 + 2Fc2)/3 |
3940 reflections | (Δ/σ)max = 0.001 |
291 parameters | Δρmax = 0.20 e Å−3 |
0 restraints | Δρmin = −0.56 e Å−3 |
[Zn2(C7H5O2)4(C10H14N2O)2] | V = 4525.6 (8) Å3 |
Mr = 971.64 | Z = 4 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 19.5680 (19) Å | µ = 1.12 mm−1 |
b = 10.6989 (10) Å | T = 160 K |
c = 21.617 (2) Å | 0.32 × 0.26 × 0.26 mm |
Siemens SMART 1K CCD diffractometer | 3940 independent reflections |
Absorption correction: multi-scan (SHELXTL; Sheldrick, 1977) | 3659 reflections with I > 2σ(I) |
Tmin = 0.683, Tmax = 0.782 | Rint = 0.034 |
18548 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 0 restraints |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.07 | Δρmax = 0.20 e Å−3 |
3940 reflections | Δρmin = −0.56 e Å−3 |
291 parameters |
x | y | z | Uiso*/Ueq | ||
Zn | 0.560102 (10) | 0.566370 (19) | 0.481129 (9) | 0.02554 (8) | |
N1 | 0.63461 (7) | 0.67277 (13) | 0.44297 (7) | 0.0260 (3) | |
C1 | 0.63995 (9) | 0.79616 (17) | 0.45364 (9) | 0.0298 (4) | |
H1 | 0.6112 | 0.8336 | 0.4838 | 0.036* | |
C2 | 0.68588 (10) | 0.86979 (17) | 0.42214 (9) | 0.0336 (4) | |
H2 | 0.6887 | 0.9568 | 0.4306 | 0.040* | |
C3 | 0.72797 (9) | 0.81603 (17) | 0.37801 (9) | 0.0314 (4) | |
H3 | 0.7591 | 0.8659 | 0.3550 | 0.038* | |
C4 | 0.72399 (9) | 0.68788 (16) | 0.36791 (8) | 0.0267 (4) | |
C5 | 0.67585 (9) | 0.62079 (16) | 0.40094 (8) | 0.0263 (4) | |
H5 | 0.6719 | 0.5336 | 0.3934 | 0.032* | |
C6 | 0.76254 (10) | 0.62152 (17) | 0.31765 (8) | 0.0302 (4) | |
O1 | 0.73000 (7) | 0.54980 (12) | 0.28417 (6) | 0.0383 (3) | |
N2 | 0.82950 (8) | 0.64603 (16) | 0.30974 (7) | 0.0347 (4) | |
C7 | 0.87344 (10) | 0.70831 (19) | 0.35534 (10) | 0.0381 (5) | |
H7A | 0.8459 | 0.7282 | 0.3925 | 0.046* | |
H7B | 0.8899 | 0.7882 | 0.3377 | 0.046* | |
C8 | 0.93473 (10) | 0.6299 (2) | 0.37465 (11) | 0.0443 (5) | |
H8A | 0.9590 | 0.6719 | 0.4084 | 0.066* | |
H8B | 0.9656 | 0.6197 | 0.3393 | 0.066* | |
H8C | 0.9191 | 0.5476 | 0.3886 | 0.066* | |
C9 | 0.86106 (12) | 0.6020 (2) | 0.25174 (10) | 0.0505 (6) | |
H9A | 0.8500 | 0.5124 | 0.2458 | 0.061* | |
H9B | 0.9113 | 0.6097 | 0.2551 | 0.061* | |
C10 | 0.83693 (14) | 0.6743 (3) | 0.19640 (11) | 0.0663 (8) | |
H10A | 0.8614 | 0.6456 | 0.1595 | 0.099* | |
H10B | 0.8458 | 0.7635 | 0.2028 | 0.099* | |
H10C | 0.7878 | 0.6611 | 0.1908 | 0.099* | |
O2 | 0.48325 (7) | 0.69643 (13) | 0.47514 (6) | 0.0379 (3) | |
O3 | 0.38838 (7) | 0.59680 (13) | 0.50390 (7) | 0.0396 (3) | |
C11 | 0.41960 (10) | 0.68954 (18) | 0.48215 (8) | 0.0291 (4) | |
C12 | 0.37798 (9) | 0.80002 (17) | 0.46178 (8) | 0.0292 (4) | |
C13 | 0.41007 (11) | 0.90458 (19) | 0.43798 (9) | 0.0381 (5) | |
H13 | 0.4586 | 0.9087 | 0.4372 | 0.046* | |
C14 | 0.37191 (13) | 1.0030 (2) | 0.41535 (10) | 0.0496 (6) | |
H14 | 0.3942 | 1.0743 | 0.3987 | 0.059* | |
C15 | 0.30160 (14) | 0.9982 (2) | 0.41680 (11) | 0.0539 (6) | |
H15 | 0.2757 | 1.0661 | 0.4009 | 0.065* | |
C16 | 0.26849 (12) | 0.8952 (2) | 0.44127 (10) | 0.0498 (6) | |
H16 | 0.2200 | 0.8924 | 0.4426 | 0.060* | |
C17 | 0.30678 (10) | 0.7960 (2) | 0.46387 (9) | 0.0374 (5) | |
H17 | 0.2844 | 0.7250 | 0.4808 | 0.045* | |
O4 | 0.56982 (7) | 0.60802 (15) | 0.57151 (6) | 0.0406 (3) | |
O5 | 0.47506 (7) | 0.50770 (13) | 0.60018 (6) | 0.0380 (3) | |
C18 | 0.52625 (10) | 0.57482 (16) | 0.61110 (9) | 0.0297 (4) | |
C19 | 0.53511 (9) | 0.62254 (17) | 0.67583 (8) | 0.0290 (4) | |
C20 | 0.58731 (11) | 0.70568 (18) | 0.68966 (9) | 0.0370 (4) | |
H20 | 0.6198 | 0.7272 | 0.6588 | 0.044* | |
C21 | 0.59224 (13) | 0.7576 (2) | 0.74836 (11) | 0.0482 (6) | |
H21 | 0.6276 | 0.8156 | 0.7575 | 0.058* | |
C22 | 0.54567 (13) | 0.7246 (2) | 0.79333 (11) | 0.0520 (6) | |
H22 | 0.5486 | 0.7610 | 0.8333 | 0.062* | |
C23 | 0.49472 (12) | 0.6389 (2) | 0.78053 (9) | 0.0463 (5) | |
H23 | 0.4634 | 0.6150 | 0.8120 | 0.056* | |
C24 | 0.48923 (11) | 0.58776 (19) | 0.72190 (9) | 0.0355 (4) | |
H24 | 0.4542 | 0.5290 | 0.7131 | 0.043* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn | 0.02454 (13) | 0.02756 (14) | 0.02451 (13) | −0.00250 (8) | 0.00191 (8) | 0.00215 (8) |
N1 | 0.0250 (7) | 0.0262 (7) | 0.0266 (8) | −0.0004 (6) | 0.0011 (6) | 0.0002 (6) |
C1 | 0.0287 (9) | 0.0293 (9) | 0.0315 (10) | 0.0015 (8) | 0.0018 (8) | −0.0030 (8) |
C2 | 0.0337 (10) | 0.0227 (9) | 0.0445 (11) | −0.0014 (8) | 0.0005 (9) | −0.0021 (8) |
C3 | 0.0281 (9) | 0.0266 (9) | 0.0393 (11) | −0.0021 (7) | 0.0029 (8) | 0.0055 (8) |
C4 | 0.0255 (9) | 0.0269 (9) | 0.0277 (9) | 0.0016 (7) | 0.0003 (7) | 0.0029 (7) |
C5 | 0.0271 (9) | 0.0242 (9) | 0.0275 (9) | 0.0000 (7) | 0.0002 (7) | 0.0019 (7) |
C6 | 0.0356 (10) | 0.0270 (9) | 0.0282 (9) | 0.0021 (8) | 0.0047 (8) | 0.0054 (8) |
O1 | 0.0440 (8) | 0.0353 (7) | 0.0354 (7) | −0.0010 (6) | 0.0031 (6) | −0.0039 (6) |
N2 | 0.0327 (8) | 0.0421 (9) | 0.0292 (8) | 0.0046 (7) | 0.0090 (7) | 0.0026 (7) |
C7 | 0.0316 (10) | 0.0397 (11) | 0.0430 (11) | −0.0025 (8) | 0.0077 (9) | −0.0013 (9) |
C8 | 0.0321 (11) | 0.0456 (12) | 0.0551 (14) | −0.0013 (9) | 0.0003 (9) | 0.0006 (11) |
C9 | 0.0448 (12) | 0.0719 (15) | 0.0348 (12) | 0.0084 (12) | 0.0130 (10) | −0.0020 (11) |
C10 | 0.0592 (15) | 0.107 (2) | 0.0325 (12) | −0.0148 (15) | 0.0060 (11) | 0.0093 (13) |
O2 | 0.0306 (7) | 0.0371 (8) | 0.0460 (8) | 0.0062 (6) | 0.0031 (6) | 0.0034 (6) |
O3 | 0.0376 (8) | 0.0320 (7) | 0.0492 (9) | 0.0019 (6) | 0.0001 (7) | 0.0096 (7) |
C11 | 0.0331 (10) | 0.0308 (10) | 0.0234 (9) | 0.0042 (8) | −0.0003 (7) | −0.0032 (7) |
C12 | 0.0346 (10) | 0.0307 (10) | 0.0222 (8) | 0.0058 (8) | 0.0014 (7) | −0.0009 (7) |
C13 | 0.0446 (12) | 0.0355 (10) | 0.0342 (11) | 0.0039 (9) | 0.0055 (9) | 0.0007 (9) |
C14 | 0.0710 (16) | 0.0357 (11) | 0.0420 (12) | 0.0120 (11) | 0.0089 (11) | 0.0077 (10) |
C15 | 0.0718 (16) | 0.0502 (14) | 0.0395 (12) | 0.0329 (13) | 0.0016 (11) | 0.0055 (11) |
C16 | 0.0432 (13) | 0.0641 (15) | 0.0421 (12) | 0.0224 (11) | −0.0023 (10) | 0.0006 (11) |
C17 | 0.0355 (10) | 0.0439 (12) | 0.0329 (10) | 0.0057 (9) | 0.0006 (8) | 0.0012 (9) |
O4 | 0.0348 (7) | 0.0605 (9) | 0.0264 (7) | −0.0044 (7) | 0.0006 (6) | −0.0008 (7) |
O5 | 0.0456 (8) | 0.0382 (8) | 0.0303 (7) | −0.0103 (7) | −0.0046 (6) | −0.0020 (6) |
C18 | 0.0335 (10) | 0.0270 (9) | 0.0287 (10) | 0.0069 (8) | −0.0032 (8) | 0.0025 (7) |
C19 | 0.0347 (9) | 0.0279 (9) | 0.0244 (9) | 0.0061 (8) | −0.0059 (8) | 0.0010 (7) |
C20 | 0.0435 (11) | 0.0327 (10) | 0.0347 (10) | 0.0005 (9) | −0.0091 (9) | 0.0044 (9) |
C21 | 0.0608 (15) | 0.0386 (11) | 0.0453 (12) | 0.0003 (11) | −0.0242 (12) | −0.0047 (10) |
C22 | 0.0724 (16) | 0.0527 (14) | 0.0309 (11) | 0.0150 (12) | −0.0171 (11) | −0.0102 (10) |
C23 | 0.0560 (14) | 0.0571 (14) | 0.0256 (10) | 0.0176 (11) | −0.0004 (10) | 0.0038 (9) |
C24 | 0.0384 (11) | 0.0383 (10) | 0.0299 (10) | 0.0061 (9) | −0.0027 (8) | 0.0041 (8) |
Zn—Zni | 2.8662 (4) | C18—C19 | 1.500 (3) |
Zn—N1 | 2.0254 (14) | C19—C20 | 1.387 (3) |
Zn—O2 | 2.0530 (13) | C19—C24 | 1.391 (3) |
Zn—O3i | 2.0417 (14) | C20—C21 | 1.389 (3) |
Zn—O4 | 2.0130 (14) | C21—C22 | 1.378 (4) |
Zn—O5i | 2.0471 (13) | C22—C23 | 1.383 (4) |
N1—C1 | 1.344 (2) | C23—C24 | 1.385 (3) |
N1—C5 | 1.336 (2) | C1—H1 | 0.950 |
C1—C2 | 1.375 (3) | C2—H2 | 0.950 |
C2—C3 | 1.385 (3) | C3—H3 | 0.950 |
C3—C4 | 1.391 (2) | C5—H5 | 0.950 |
C4—C5 | 1.383 (2) | C7—H7A | 0.990 |
C4—C6 | 1.501 (2) | C7—H7B | 0.990 |
C6—O1 | 1.232 (2) | C8—H8A | 0.980 |
C6—N2 | 1.347 (2) | C8—H8B | 0.980 |
N2—C7 | 1.468 (3) | C8—H8C | 0.980 |
N2—C9 | 1.475 (3) | C9—H9A | 0.990 |
C7—C8 | 1.522 (3) | C9—H9B | 0.990 |
C9—C10 | 1.501 (3) | C10—H10A | 0.980 |
O2—C11 | 1.257 (2) | C10—H10B | 0.980 |
O3—Zni | 2.0417 (14) | C10—H10C | 0.980 |
O3—C11 | 1.256 (2) | C13—H13 | 0.950 |
C11—C12 | 1.501 (3) | C14—H14 | 0.950 |
C12—C13 | 1.382 (3) | C15—H15 | 0.950 |
C12—C17 | 1.395 (3) | C16—H16 | 0.950 |
C13—C14 | 1.380 (3) | C17—H17 | 0.950 |
C14—C15 | 1.377 (4) | C20—H20 | 0.950 |
C15—C16 | 1.384 (4) | C21—H21 | 0.950 |
C16—C17 | 1.388 (3) | C22—H22 | 0.950 |
O4—C18 | 1.259 (2) | C23—H23 | 0.950 |
O5—Zni | 2.0471 (13) | C24—H24 | 0.950 |
O5—C18 | 1.255 (2) | ||
Zni—Zn—N1 | 170.12 (4) | C20—C21—C22 | 119.8 (2) |
Zni—Zn—O2 | 75.68 (4) | C21—C22—C23 | 120.4 (2) |
Zni—Zn—O3i | 86.35 (4) | C22—C23—C24 | 120.1 (2) |
Zni—Zn—O4 | 84.89 (4) | C19—C24—C23 | 120.0 (2) |
Zni—Zn—O5i | 77.10 (4) | N1—C1—H1 | 119.1 |
N1—Zn—O2 | 96.93 (6) | C2—C1—H1 | 119.1 |
N1—Zn—O3i | 100.94 (6) | C1—C2—H2 | 120.3 |
N1—Zn—O4 | 101.71 (6) | C3—C2—H2 | 120.3 |
N1—Zn—O5i | 96.31 (6) | C2—C3—H3 | 120.5 |
O2—Zn—O3i | 162.03 (6) | C4—C3—H3 | 120.5 |
O2—Zn—O4 | 88.87 (6) | N1—C5—H5 | 118.4 |
O2—Zn—O5i | 87.82 (6) | C4—C5—H5 | 118.4 |
O3i—Zn—O4 | 89.35 (6) | N2—C7—H7A | 108.9 |
O3i—Zn—O5i | 88.34 (6) | C8—C7—H7A | 108.9 |
O4—Zn—O5i | 161.95 (6) | N2—C7—H7B | 108.9 |
Zn—N1—C1 | 122.55 (12) | C8—C7—H7B | 108.9 |
Zn—N1—C5 | 118.54 (12) | H7A—C7—H7B | 107.7 |
C1—N1—C5 | 118.58 (15) | C7—C8—H8A | 109.5 |
N1—C1—C2 | 121.89 (17) | C7—C8—H8B | 109.5 |
C1—C2—C3 | 119.44 (17) | H8A—C8—H8B | 109.5 |
C2—C3—C4 | 118.97 (17) | C7—C8—H8C | 109.5 |
C3—C4—C5 | 117.96 (17) | H8A—C8—H8C | 109.5 |
C3—C4—C6 | 123.50 (16) | H8B—C8—H8C | 109.5 |
C5—C4—C6 | 118.07 (16) | N2—C9—H9A | 109.1 |
N1—C5—C4 | 123.12 (16) | C10—C9—H9A | 109.1 |
C4—C6—O1 | 117.40 (16) | N2—C9—H9B | 109.1 |
C4—C6—N2 | 119.24 (17) | C10—C9—H9B | 109.1 |
O1—C6—N2 | 123.31 (17) | H9A—C9—H9B | 107.9 |
C6—N2—C7 | 124.95 (16) | C9—C10—H10A | 109.5 |
C6—N2—C9 | 116.93 (17) | C9—C10—H10B | 109.5 |
C7—N2—C9 | 118.07 (17) | H10A—C10—H10B | 109.5 |
N2—C7—C8 | 113.31 (17) | C9—C10—H10C | 109.5 |
N2—C9—C10 | 112.4 (2) | H10A—C10—H10C | 109.5 |
Zn—O2—C11 | 132.73 (13) | H10B—C10—H10C | 109.5 |
Zni—O3—C11 | 119.64 (13) | C14—C13—H13 | 119.9 |
O2—C11—O3 | 124.97 (18) | C12—C13—H13 | 119.9 |
O2—C11—C12 | 117.13 (17) | C15—C14—H14 | 119.9 |
O3—C11—C12 | 117.89 (17) | C13—C14—H14 | 119.9 |
C11—C12—C13 | 120.00 (17) | C14—C15—H15 | 119.8 |
C11—C12—C17 | 120.52 (18) | C16—C15—H15 | 119.8 |
C13—C12—C17 | 119.41 (18) | C15—C16—H16 | 120.3 |
C12—C13—C14 | 120.2 (2) | C17—C16—H16 | 120.3 |
C13—C14—C15 | 120.3 (2) | C16—C17—H17 | 119.9 |
C14—C15—C16 | 120.4 (2) | C12—C17—H17 | 119.9 |
C15—C16—C17 | 119.4 (2) | C19—C20—H20 | 119.8 |
C12—C17—C16 | 120.3 (2) | C21—C20—H20 | 119.8 |
Zn—O4—C18 | 122.23 (13) | C22—C21—H21 | 120.1 |
Zni—O5—C18 | 130.65 (13) | C20—C21—H21 | 120.1 |
O4—C18—O5 | 125.03 (18) | C21—C22—H22 | 119.8 |
O4—C18—C19 | 117.38 (17) | C23—C22—H22 | 119.8 |
O5—C18—C19 | 117.56 (17) | C22—C23—H23 | 120.0 |
C18—C19—C20 | 120.30 (17) | C24—C23—H23 | 120.0 |
C18—C19—C24 | 120.15 (17) | C23—C24—H24 | 120.0 |
C20—C19—C24 | 119.50 (18) | C19—C24—H24 | 120.0 |
C19—C20—C21 | 120.3 (2) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Zn2(C7H5O2)4(C10H14N2O)2] |
Mr | 971.64 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 160 |
a, b, c (Å) | 19.5680 (19), 10.6989 (10), 21.617 (2) |
V (Å3) | 4525.6 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.12 |
Crystal size (mm) | 0.32 × 0.26 × 0.26 |
Data collection | |
Diffractometer | Siemens SMART 1K CCD diffractometer |
Absorption correction | Multi-scan (SHELXTL; Sheldrick, 1977) |
Tmin, Tmax | 0.683, 0.782 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18548, 3940, 3659 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.610 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.073, 1.07 |
No. of reflections | 3940 |
No. of parameters | 291 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.20, −0.56 |
Computer programs: SMART (Siemens, 1995), SAINT (Siemens, 1995), SHELXTL (Sheldrick, 1997), SHELXTL and local programs.
Zn—N1 | 2.0254 (14) | O2—C11 | 1.257 (2) |
Zn—O2 | 2.0530 (13) | O3—C11 | 1.256 (2) |
Zn—O3i | 2.0417 (14) | O4—C18 | 1.259 (2) |
Zn—O4 | 2.0130 (14) | O5—C18 | 1.255 (2) |
Zn—O5i | 2.0471 (13) | ||
N1—Zn—O2 | 96.93 (6) | O2—Zn—O4 | 88.87 (6) |
N1—Zn—O3i | 100.94 (6) | O2—Zn—O5i | 87.82 (6) |
N1—Zn—O4 | 101.71 (6) | O3i—Zn—O4 | 89.35 (6) |
N1—Zn—O5i | 96.31 (6) | O3i—Zn—O5i | 88.34 (6) |
O2—Zn—O3i | 162.03 (6) | O4—Zn—O5i | 161.95 (6) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
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The title compound, (I), was prepared as part of a series of studies of the coordination chemistry of the ligand N,N-diethylnicotinamide (DENA), particularly in conjunction with carboxylate ligands.
Crystallographic investigation shows that the molecule is a centrosymmetric dimer (Fig. 1), in which the two zinc ions are bridged by four benzoate ligands. DENA acts as a terminal monodentate ligand through its pyridine N atom, with one DENA ligand attached to each end of the Zn···Zn axis. Such a dimeric arrangement with two metal ions bridged by four carboxylates is common for transition metals, whether the metals have a direct formal metal–metal bond or not, but it has been observed for only four previous zinc complex structures, two of them being polymorphs of the same complex (Clegg et al., 1986, 1995; Singh et al., 1997).
The two zinc ions are not considered to be directly bonded to each other in this structure. The Zn···Zn separation of 2.8660 (4) Å is the shortest observed for zinc complexes of this kind, previous values ranging from 2.893 to 2.976 Å. The benzoate bridges are essentially symmetrical, with no significant variation in the C—O bond lengths. The central Zn2(O2C)4N2 core of the molecule has approximate 4/mmm (D4 h) symmetry. Each Zn atom has square-pyramidal coordination, with DENA in the apical site.
There are no significant intermolecular interactions.