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A novel three-dimensional Cd
II complex, poly[aqua{
2-1,4-bis[2-(pyridin-4-yl)ethenyl]benzene-
2N:
N'}[
4-2,2'-(1,4-phenylene)diacetato-
4O,
O':
O'',
O''']cadmium(II)], [Cd(C
10H
8O
4)(C
20H
16N
2)(H
2O)]
n, has been prepared by hydrothermal assembly of Cd(NO
3)
2·4H
2O, 1,4-bis[2-(pyridin-4-yl)ethenyl]benzene (1,4-bpeb) and 2,2'-(1,4-phenylene)diacetic acid (1,4-H
2pda). Each Cd
II centre is located on a twofold axis in a distorted pentagonal bipyramidal coordination environment formed by one O atom from a water molecule, which lies on the same twofold axis, four O atoms from two different 1,4-pda ligands and two N atoms from two different 1,4-bpeb ligands. The Cd
II centres are bridged by the 1,4-bpeb and 1,4-pda ligands, which lie across centres of inversion. The three-dimensional net can be regarded as a diamondoid network by treating the Cd
II atoms as nodes and the 1,4-bpeb and 1,4-pda ligands as linkers. The single net leaves voids that are filled by mutual interpenetration of four independent equivalent frameworks in a fivefold interpenetrating architecture.
Supporting information
CCDC reference: 964523
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).
Poly[aqua{µ
2-1,4-bis[2-(pyridin-4-yl)ethenyl]benzene-
κ2N:
N'}[µ
4-2,2'-(1,4-phenylene)diacetato-
κ4O,
O':
O'',
O''']cadmium(II)]
top
Crystal data top
[Cd(C10H8O4)(C20H16N2)(H2O)] | F(000) = 1232 |
Mr = 606.94 | Dx = 1.572 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 6132 reflections |
a = 18.537 (4) Å | θ = 3.0–27.5° |
b = 16.886 (3) Å | µ = 0.90 mm−1 |
c = 8.3534 (17) Å | T = 223 K |
β = 101.26 (3)° | Block, yellow |
V = 2564.4 (9) Å3 | 0.20 × 0.17 × 0.15 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2937 independent reflections |
Radiation source: fine-focus sealed tube | 2641 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
φ and ω scans | θmax = 27.5°, θmin = 3.2° |
Absorption correction: multi-scan (SADABS; Bruker, 1997) | h = −24→17 |
Tmin = 0.841, Tmax = 0.877 | k = −20→21 |
11458 measured reflections | l = −10→9 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.032 | H-atom parameters constrained |
wR(F2) = 0.077 | w = 1/[σ2(Fo2) + (0.0429P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.14 | (Δ/σ)max < 0.001 |
2937 reflections | Δρmax = 1.19 e Å−3 |
174 parameters | Δρmin = −0.64 e Å−3 |
0 restraints | Extinction correction: SHELXTL (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0073 (4) |
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 | |
Cd1 | 0.0000 | 0.371789 (12) | −0.2500 | 0.02882 (11) | |
N1 | 0.12006 (11) | 0.38606 (11) | −0.0941 (2) | 0.0344 (4) | |
O1 | −0.04623 (11) | 0.26880 (10) | −0.1026 (2) | 0.0438 (4) | |
O2 | −0.04436 (11) | 0.38739 (10) | 0.0024 (2) | 0.0413 (4) | |
O3 | 0.0000 | 0.51095 (14) | −0.2500 | 0.0431 (6) | |
H1W | −0.0151 | 0.5424 | −0.3289 | 0.065* | |
C1 | 0.17741 (14) | 0.34306 (15) | −0.1179 (3) | 0.0383 (5) | |
H1 | 0.1698 | 0.3046 | −0.2010 | 0.046* | |
C2 | 0.24752 (14) | 0.35233 (15) | −0.0264 (3) | 0.0388 (5) | |
H2 | 0.2861 | 0.3205 | −0.0482 | 0.047* | |
C3 | 0.26146 (13) | 0.40866 (14) | 0.0984 (3) | 0.0348 (5) | |
C4 | 0.20107 (14) | 0.45446 (14) | 0.1198 (3) | 0.0395 (6) | |
H4 | 0.2071 | 0.4942 | 0.2002 | 0.047* | |
C5 | 0.13303 (14) | 0.44152 (14) | 0.0238 (3) | 0.0378 (5) | |
H5 | 0.0935 | 0.4730 | 0.0413 | 0.045* | |
C6 | 0.33442 (14) | 0.41656 (15) | 0.2006 (3) | 0.0384 (5) | |
H6 | 0.3665 | 0.3731 | 0.2057 | 0.046* | |
C7 | 0.35898 (14) | 0.48043 (15) | 0.2871 (3) | 0.0380 (5) | |
H7 | 0.3269 | 0.5240 | 0.2788 | 0.046* | |
C8 | 0.43147 (13) | 0.48958 (14) | 0.3944 (3) | 0.0342 (5) | |
C9 | 0.45649 (14) | 0.56443 (14) | 0.4483 (3) | 0.0371 (5) | |
H9 | 0.4267 | 0.6087 | 0.4141 | 0.045* | |
C10 | 0.47621 (14) | 0.42438 (14) | 0.4496 (3) | 0.0374 (5) | |
H10 | 0.4604 | 0.3729 | 0.4170 | 0.045* | |
C11 | −0.20096 (14) | 0.18840 (15) | 0.0389 (3) | 0.0409 (6) | |
H11 | −0.1679 | 0.1459 | 0.0644 | 0.049* | |
C12 | −0.17611 (13) | 0.26537 (15) | 0.0695 (3) | 0.0359 (5) | |
C13 | −0.22592 (15) | 0.32652 (15) | 0.0292 (3) | 0.0426 (6) | |
H13 | −0.2099 | 0.3791 | 0.0483 | 0.051* | |
C14 | −0.09549 (14) | 0.28267 (17) | 0.1395 (3) | 0.0430 (6) | |
H14A | −0.0707 | 0.2340 | 0.1845 | 0.052* | |
H14B | −0.0917 | 0.3215 | 0.2279 | 0.052* | |
C15 | −0.05847 (12) | 0.31506 (14) | 0.0051 (3) | 0.0325 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.02084 (15) | 0.02927 (16) | 0.03468 (16) | 0.000 | 0.00127 (9) | 0.000 |
N1 | 0.0245 (11) | 0.0354 (10) | 0.0402 (10) | 0.0001 (8) | −0.0010 (8) | 0.0020 (8) |
O1 | 0.0516 (12) | 0.0328 (9) | 0.0510 (10) | −0.0015 (8) | 0.0198 (8) | 0.0004 (7) |
O2 | 0.0469 (11) | 0.0355 (9) | 0.0410 (9) | −0.0082 (8) | 0.0069 (8) | −0.0027 (7) |
O3 | 0.0539 (17) | 0.0311 (12) | 0.0397 (12) | 0.000 | −0.0025 (11) | 0.000 |
C1 | 0.0313 (14) | 0.0361 (12) | 0.0438 (13) | 0.0012 (10) | −0.0020 (10) | −0.0029 (10) |
C2 | 0.0260 (13) | 0.0395 (13) | 0.0486 (14) | 0.0043 (10) | 0.0014 (10) | −0.0018 (10) |
C3 | 0.0251 (12) | 0.0355 (12) | 0.0408 (12) | −0.0042 (10) | −0.0013 (9) | 0.0030 (9) |
C4 | 0.0320 (14) | 0.0390 (13) | 0.0443 (13) | 0.0005 (10) | 0.0000 (10) | −0.0059 (10) |
C5 | 0.0279 (13) | 0.0381 (13) | 0.0449 (13) | 0.0040 (10) | 0.0012 (10) | −0.0012 (10) |
C6 | 0.0240 (13) | 0.0440 (14) | 0.0447 (13) | −0.0002 (10) | 0.0011 (10) | −0.0016 (10) |
C7 | 0.0288 (13) | 0.0390 (13) | 0.0444 (13) | −0.0013 (10) | 0.0028 (10) | 0.0013 (10) |
C8 | 0.0259 (13) | 0.0377 (13) | 0.0374 (11) | −0.0027 (10) | 0.0024 (9) | −0.0012 (9) |
C9 | 0.0300 (13) | 0.0329 (12) | 0.0456 (13) | 0.0015 (10) | 0.0006 (10) | 0.0006 (9) |
C10 | 0.0307 (14) | 0.0330 (12) | 0.0460 (13) | −0.0049 (10) | 0.0012 (10) | −0.0033 (9) |
C11 | 0.0355 (14) | 0.0407 (13) | 0.0465 (13) | 0.0005 (11) | 0.0082 (11) | 0.0047 (10) |
C12 | 0.0298 (13) | 0.0481 (14) | 0.0303 (11) | −0.0074 (10) | 0.0075 (9) | 0.0014 (9) |
C13 | 0.0410 (15) | 0.0361 (13) | 0.0507 (14) | −0.0090 (11) | 0.0091 (11) | −0.0013 (10) |
C14 | 0.0332 (14) | 0.0570 (16) | 0.0380 (13) | −0.0088 (12) | 0.0046 (10) | 0.0055 (11) |
C15 | 0.0193 (11) | 0.0391 (13) | 0.0364 (12) | −0.0022 (9) | −0.0013 (9) | 0.0029 (9) |
Geometric parameters (Å, º) top
Cd1—O3 | 2.350 (2) | C5—H5 | 0.9400 |
Cd1—N1i | 2.361 (2) | C6—C7 | 1.328 (3) |
Cd1—N1 | 2.361 (2) | C6—H6 | 0.9400 |
Cd1—O1 | 2.3845 (17) | C7—C8 | 1.471 (3) |
Cd1—O1i | 2.3845 (17) | C7—H7 | 0.9400 |
Cd1—O2i | 2.4221 (18) | C8—C9 | 1.390 (3) |
Cd1—O2 | 2.4221 (18) | C8—C10 | 1.401 (3) |
Cd1—C15 | 2.745 (2) | C9—C10ii | 1.380 (3) |
Cd1—C15i | 2.745 (2) | C9—H9 | 0.9400 |
N1—C1 | 1.334 (3) | C10—C9ii | 1.380 (3) |
N1—C5 | 1.346 (3) | C10—H10 | 0.9400 |
O1—C15 | 1.246 (3) | C11—C12 | 1.386 (3) |
O2—C15 | 1.250 (3) | C11—C13iii | 1.387 (4) |
O3—H1W | 0.8499 | C11—H11 | 0.9400 |
C1—C2 | 1.382 (3) | C12—C13 | 1.382 (4) |
C1—H1 | 0.9400 | C12—C14 | 1.523 (3) |
C2—C3 | 1.397 (3) | C13—C11iii | 1.387 (4) |
C2—H2 | 0.9400 | C13—H13 | 0.9400 |
C3—C4 | 1.401 (3) | C14—C15 | 1.526 (3) |
C3—C6 | 1.458 (3) | C14—H14A | 0.9800 |
C4—C5 | 1.374 (3) | C14—H14B | 0.9800 |
C4—H4 | 0.9400 | | |
| | | |
O3—Cd1—N1i | 84.15 (5) | C3—C2—H2 | 119.8 |
O3—Cd1—N1 | 84.14 (5) | C2—C3—C4 | 115.8 (2) |
N1i—Cd1—N1 | 168.29 (9) | C2—C3—C6 | 121.0 (2) |
O3—Cd1—O1 | 136.83 (4) | C4—C3—C6 | 123.2 (2) |
N1i—Cd1—O1 | 87.94 (7) | C5—C4—C3 | 120.2 (2) |
N1—Cd1—O1 | 100.65 (7) | C5—C4—H4 | 119.9 |
O3—Cd1—O1i | 136.83 (4) | C3—C4—H4 | 119.9 |
N1i—Cd1—O1i | 100.64 (7) | N1—C5—C4 | 123.4 (2) |
N1—Cd1—O1i | 87.94 (7) | N1—C5—H5 | 118.3 |
O1—Cd1—O1i | 86.35 (8) | C4—C5—H5 | 118.3 |
O3—Cd1—O2i | 83.75 (4) | C7—C6—C3 | 125.0 (2) |
N1i—Cd1—O2i | 87.28 (7) | C7—C6—H6 | 117.5 |
N1—Cd1—O2i | 91.45 (7) | C3—C6—H6 | 117.5 |
O1—Cd1—O2i | 138.24 (6) | C6—C7—C8 | 126.3 (2) |
O1i—Cd1—O2i | 54.03 (6) | C6—C7—H7 | 116.8 |
O3—Cd1—O2 | 83.76 (4) | C8—C7—H7 | 116.8 |
N1i—Cd1—O2 | 91.45 (7) | C9—C8—C10 | 118.0 (2) |
N1—Cd1—O2 | 87.28 (7) | C9—C8—C7 | 120.0 (2) |
O1—Cd1—O2 | 54.03 (6) | C10—C8—C7 | 122.0 (2) |
O1i—Cd1—O2 | 138.24 (6) | C10ii—C9—C8 | 121.9 (2) |
O2i—Cd1—O2 | 167.51 (8) | C10ii—C9—H9 | 119.0 |
O3—Cd1—C15 | 110.42 (5) | C8—C9—H9 | 119.0 |
N1i—Cd1—C15 | 89.50 (7) | C9ii—C10—C8 | 120.1 (2) |
N1—Cd1—C15 | 94.59 (7) | C9ii—C10—H10 | 120.0 |
O1—Cd1—C15 | 26.95 (6) | C8—C10—H10 | 120.0 |
O1i—Cd1—C15 | 112.49 (7) | C12—C11—C13iii | 120.6 (2) |
O2i—Cd1—C15 | 165.07 (7) | C12—C11—H11 | 119.7 |
O2—Cd1—C15 | 27.09 (6) | C13iii—C11—H11 | 119.7 |
O3—Cd1—C15i | 110.42 (5) | C13—C12—C11 | 118.3 (2) |
N1i—Cd1—C15i | 94.59 (7) | C13—C12—C14 | 120.6 (2) |
N1—Cd1—C15i | 89.50 (7) | C11—C12—C14 | 121.1 (2) |
O1—Cd1—C15i | 112.49 (7) | C12—C13—C11iii | 121.1 (2) |
O1i—Cd1—C15i | 26.95 (6) | C12—C13—H13 | 119.4 |
O2i—Cd1—C15i | 27.09 (6) | C11iii—C13—H13 | 119.4 |
O2—Cd1—C15i | 165.07 (7) | C12—C14—C15 | 109.57 (19) |
C15—Cd1—C15i | 139.16 (10) | C12—C14—H14A | 109.8 |
C1—N1—C5 | 117.0 (2) | C15—C14—H14A | 109.8 |
C1—N1—Cd1 | 123.71 (16) | C12—C14—H14B | 109.8 |
C5—N1—Cd1 | 119.27 (16) | C15—C14—H14B | 109.8 |
C15—O1—Cd1 | 92.89 (14) | H14A—C14—H14B | 108.2 |
C15—O2—Cd1 | 91.02 (13) | O1—C15—O2 | 122.1 (2) |
Cd1—O3—H1W | 128.6 | O1—C15—C14 | 118.6 (2) |
N1—C1—C2 | 123.1 (2) | O2—C15—C14 | 119.3 (2) |
N1—C1—H1 | 118.4 | O1—C15—Cd1 | 60.16 (12) |
C2—C1—H1 | 118.4 | O2—C15—Cd1 | 61.90 (12) |
C1—C2—C3 | 120.4 (2) | C14—C15—Cd1 | 176.42 (16) |
C1—C2—H2 | 119.8 | | |
Symmetry codes: (i) −x, y, −z−1/2; (ii) −x+1, −y+1, −z+1; (iii) −x−1/2, −y+1/2, −z. |
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