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In the title complex, [Zn(tp)(dbo)(H
2O)]
n, where tp is terephthalate (C
8H
4O
4) and dbo is 1,4-diazabicyclo[2.2.2]octane (C
6H
12N
2), each Zn
II atom is coordinated by three O atoms from two bis-monodentate tp ligands and one aqua ligand, and by two N atoms from two bridging dbo ligands, in a distorted trigonal–bipyramidal geometry, with the two N atoms located at the axial sites. The bridging tp ligands link the Zn
II atoms to form one-dimensional zigzag chains, running along [221]. These chains are assembled into layers parallel to the
ac plane by dbo ligands, which are extended into a three-dimensional network by O—H
O hydrogen bonds and π–π stacking interactions.
Supporting information
CCDC reference: 621421
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.003 Å
- R factor = 0.024
- wR factor = 0.065
- Data-to-parameter ratio = 14.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 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
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and OLEX (Dolomanov et al., 2003); software used to prepare material for publication: SHELXTL and OLEX.
poly[aqua-µ
2-1,4-diazabicyclo[2.2.2]octane-µ
2-terephthalato-zinc(II)]
top
Crystal data top
[Zn(C8H4O4)(C6H12N2)(H2O)] | F(000) = 744 |
Mr = 359.67 | Dx = 1.808 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1307 reflections |
a = 10.854 (3) Å | θ = 2–28° |
b = 18.955 (6) Å | µ = 1.89 mm−1 |
c = 7.1592 (19) Å | T = 273 K |
β = 116.23 (2)° | Block, colourless |
V = 1321.2 (7) Å3 | 0.26 × 0.13 × 0.06 mm |
Z = 4 | |
Data collection top
Bruker SMART APEX area-detector diffractometer | 1433 independent reflections |
Radiation source: fine-focus sealed tube | 1361 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
φ and ω scans | θmax = 27.0°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→11 |
Tmin = 0.640, Tmax = 0.895 | k = −23→24 |
3966 measured reflections | l = −9→8 |
Refinement top
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)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0367P)2 + 1.1622P] where P = (Fo2 + 2Fc2)/3 |
1433 reflections | (Δ/σ)max < 0.001 |
101 parameters | Δρmax = 0.39 e Å−3 |
0 restraints | Δρmin = −0.23 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Zn1 | 1.0000 | 0.355797 (14) | 0.2500 | 0.01664 (11) | |
N1 | 0.99898 (15) | 0.35015 (7) | −0.0672 (2) | 0.0172 (3) | |
O1 | 0.69103 (14) | 0.33501 (7) | 0.0353 (2) | 0.0294 (3) | |
O2 | 0.84035 (12) | 0.42311 (7) | 0.1480 (2) | 0.0213 (3) | |
O1W | 1.0000 | 0.24848 (9) | 0.2500 | 0.0282 (4) | |
H1WA | 0.9368 | 0.2229 | 0.1617 | 0.042* | |
C1 | 0.71820 (18) | 0.39851 (9) | 0.0718 (3) | 0.0187 (3) | |
C2 | 0.60519 (18) | 0.45119 (9) | 0.0318 (3) | 0.0188 (3) | |
C3 | 0.47443 (19) | 0.42819 (10) | −0.0041 (3) | 0.0236 (4) | |
H3A | 0.4564 | 0.3801 | −0.0072 | 0.028* | |
C4 | 0.62858 (18) | 0.52352 (10) | 0.0350 (3) | 0.0231 (4) | |
H4A | 0.7151 | 0.5397 | 0.0583 | 0.028* | |
C5 | 0.8756 (2) | 0.31444 (10) | −0.2266 (3) | 0.0250 (4) | |
H5A | 0.7938 | 0.3392 | −0.2405 | 0.030* | |
H5B | 0.8711 | 0.2666 | −0.1818 | 0.030* | |
C6 | 1.1209 (2) | 0.31248 (11) | −0.0605 (3) | 0.0259 (4) | |
H6A | 1.1190 | 0.2638 | −0.0201 | 0.031* | |
H6B | 1.2038 | 0.3342 | 0.0438 | 0.031* | |
C7 | 1.00125 (19) | 0.42303 (9) | −0.1416 (3) | 0.0205 (4) | |
H7A | 1.0834 | 0.4470 | −0.0434 | 0.025* | |
H7B | 0.9223 | 0.4488 | −0.1479 | 0.025* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.01413 (16) | 0.01615 (17) | 0.01873 (17) | 0.000 | 0.00643 (12) | 0.000 |
N1 | 0.0182 (8) | 0.0156 (7) | 0.0178 (7) | 0.0004 (5) | 0.0080 (6) | 0.0006 (5) |
O1 | 0.0254 (7) | 0.0205 (7) | 0.0377 (8) | 0.0008 (6) | 0.0099 (6) | −0.0023 (6) |
O2 | 0.0137 (6) | 0.0236 (6) | 0.0243 (7) | 0.0027 (5) | 0.0061 (5) | 0.0001 (5) |
O1W | 0.0315 (11) | 0.0170 (9) | 0.0252 (10) | 0.000 | 0.0026 (8) | 0.000 |
C1 | 0.0177 (8) | 0.0231 (9) | 0.0155 (8) | 0.0027 (7) | 0.0075 (7) | 0.0018 (7) |
C2 | 0.0154 (8) | 0.0245 (9) | 0.0158 (8) | 0.0017 (7) | 0.0063 (7) | −0.0001 (7) |
C3 | 0.0199 (9) | 0.0192 (8) | 0.0307 (10) | −0.0007 (7) | 0.0102 (8) | −0.0007 (7) |
C4 | 0.0144 (8) | 0.0259 (9) | 0.0286 (10) | −0.0011 (7) | 0.0091 (7) | −0.0004 (8) |
C5 | 0.0255 (10) | 0.0290 (10) | 0.0217 (10) | −0.0097 (8) | 0.0115 (8) | −0.0028 (8) |
C6 | 0.0255 (10) | 0.0308 (10) | 0.0211 (9) | 0.0107 (8) | 0.0101 (8) | 0.0037 (8) |
C7 | 0.0257 (10) | 0.0156 (8) | 0.0218 (9) | 0.0005 (7) | 0.0120 (7) | −0.0002 (7) |
Geometric parameters (Å, º) top
Zn1—O2i | 2.011 (1) | C3—C4ii | 1.385 (3) |
Zn1—O2 | 2.011 (1) | C3—H3A | 0.9300 |
Zn1—O1W | 2.034 (2) | C4—C3ii | 1.385 (3) |
Zn1—N1 | 2.269 (2) | C4—H4A | 0.9300 |
Zn1—N1i | 2.2686 (16) | C5—C6iii | 1.542 (3) |
N1—C5 | 1.484 (2) | C5—H5A | 0.9700 |
N1—C7 | 1.485 (2) | C5—H5B | 0.9700 |
N1—C6 | 1.486 (2) | C6—C5iii | 1.542 (3) |
O1—C1 | 1.239 (2) | C6—H6A | 0.9700 |
O2—C1 | 1.278 (2) | C6—H6B | 0.9700 |
O1W—H1WA | 0.8501 | C7—C7iii | 1.541 (3) |
C1—C2 | 1.508 (2) | C7—H7A | 0.9700 |
C2—C4 | 1.393 (3) | C7—H7B | 0.9700 |
C2—C3 | 1.396 (3) | | |
| | | |
O2i—Zn1—O2 | 101.26 (8) | C4ii—C3—C2 | 120.43 (17) |
O2i—Zn1—O1W | 129.37 (4) | C4ii—C3—H3A | 119.8 |
O2—Zn1—O1W | 129.37 (4) | C2—C3—H3A | 119.8 |
O2i—Zn1—N1 | 90.90 (5) | C3ii—C4—C2 | 121.30 (17) |
O2—Zn1—N1 | 92.54 (5) | C3ii—C4—H4A | 119.3 |
O1W—Zn1—N1 | 87.29 (4) | C2—C4—H4A | 119.3 |
O2i—Zn1—N1i | 92.54 (5) | N1—C5—C6iii | 111.28 (15) |
O2—Zn1—N1i | 90.90 (5) | N1—C5—H5A | 109.4 |
O1W—Zn1—N1i | 87.29 (4) | C6iii—C5—H5A | 109.4 |
N1—Zn1—N1i | 174.59 (7) | N1—C5—H5B | 109.4 |
C5—N1—C7 | 107.51 (14) | C6iii—C5—H5B | 109.4 |
C5—N1—C6 | 107.10 (15) | H5A—C5—H5B | 108.0 |
C7—N1—C6 | 107.64 (14) | N1—C6—C5iii | 111.54 (15) |
C5—N1—Zn1 | 113.24 (11) | N1—C6—H6A | 109.3 |
C7—N1—Zn1 | 108.76 (10) | C5iii—C6—H6A | 109.3 |
C6—N1—Zn1 | 112.34 (11) | N1—C6—H6B | 109.3 |
C1—O2—Zn1 | 119.23 (12) | C5iii—C6—H6B | 109.3 |
Zn1—O1W—H1WA | 124.8 | H6A—C6—H6B | 108.0 |
O1—C1—O2 | 123.34 (16) | N1—C7—C7iii | 111.45 (9) |
O1—C1—C2 | 120.36 (16) | N1—C7—H7A | 109.3 |
O2—C1—C2 | 116.28 (15) | C7iii—C7—H7A | 109.3 |
C4—C2—C3 | 118.27 (16) | N1—C7—H7B | 109.3 |
C4—C2—C1 | 121.45 (16) | C7iii—C7—H7B | 109.3 |
C3—C2—C1 | 120.25 (16) | H7A—C7—H7B | 108.0 |
Symmetry codes: (i) −x+2, y, −z+1/2; (ii) −x+1, −y+1, −z; (iii) −x+2, y, −z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O1iv | 0.85 | 1.84 | 2.6891 (19) | 176 |
C5—H5B···O1iv | 0.97 | 2.43 | 3.362 (2) | 162 |
Symmetry code: (iv) −x+3/2, −y+1/2, −z. |
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