In the title compound, [Cd2(C6H4NO2)4(C12H10N2)(H2O)2], the CdII atom, the water O atom and the bridging trans-1,2-bis(4-pyridyl)ethene ligand are located on a mirror plane. An inversion center is located at the mid-point of the ethene link. Each CdII atom is in an octahedral environment, coordinated by one water molecule, one trans-1,2-bis(4-pyridyl)ethene molecule and four isonicotinate anions. This forms an interpenetrated framework composed of bilayered cuboidal motifs.
Supporting information
CCDC reference: 234792
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å
- R factor = 0.023
- wR factor = 0.058
- Data-to-parameter ratio = 12.3
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT027_ALERT_3_A _diffrn_reflns_theta_full too Low .............. 24.99 Deg.
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C4
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.10
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 42.00 A 3
PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.19 Ratio
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 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
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Bruker, 1992); cell refinement: XSCANS; data reduction: SHELXTL XPREP (Bruker, 1994); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL XP; software used to prepare material for publication: SHELXTL XCIF.
Crystal data top
[Cd2(C6H4NO2)4(C12H10N2)(H2O)2] | F(000) = 928 |
Mr = 465.74 | Dx = 1.634 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2y | Cell parameters from 25 reflections |
a = 12.6311 (19) Å | θ = 12.3–12.5° |
b = 14.6070 (19) Å | µ = 1.19 mm−1 |
c = 11.1428 (15) Å | T = 298 K |
β = 112.94 (2)° | Parallelepiped, colorless |
V = 1893.3 (5) Å3 | 0.50 × 0.30 × 0.20 mm |
Z = 4 | |
Data collection top
Bruker P4 diffractometer | 1647 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.039 |
Graphite monochromator | θmax = 25.0°, θmin = 2.0° |
θ/2θ scans | h = −11→14 |
Absorption correction: ψ scan (North et al., 1968) | k = −16→11 |
Tmin = 0.588, Tmax = 0.797 | l = −13→13 |
3920 measured reflections | 3 standard reflections every 97 reflections |
1737 independent reflections | intensity decay: none |
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)] = 0.023 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.058 | w = 1/[σ2(Fo2) + (0.0288P)2 + 1.2195P] where P = (Fo2 + 2Fc2)/3 |
S = 1.21 | (Δ/σ)max < 0.001 |
1737 reflections | Δρmax = 0.65 e Å−3 |
141 parameters | Δρmin = −0.60 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0045 (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 | |
Cd | 0.221543 (17) | 0.5000 | 0.320511 (19) | 0.01853 (12) | |
N1 | 0.2859 (2) | 0.5000 | 0.5487 (3) | 0.0282 (6) | |
N2 | 0.58932 (17) | 0.11980 (15) | 0.29590 (19) | 0.0304 (5) | |
O1 | 0.1525 (2) | 0.5000 | 0.0914 (2) | 0.0281 (5) | |
O2 | 0.35581 (14) | 0.38724 (12) | 0.33713 (16) | 0.0300 (4) | |
O3 | 0.2870 (2) | 0.35810 (16) | 0.12321 (19) | 0.0597 (7) | |
C1 | 0.3997 (3) | 0.5000 | 0.6125 (3) | 0.0322 (8) | |
H1 | 0.4449 | 0.5000 | 0.5636 | 0.039* | |
C2 | 0.4542 (3) | 0.5000 | 0.7453 (3) | 0.0337 (8) | |
H2 | 0.5341 | 0.5000 | 0.7841 | 0.040* | |
C3 | 0.3907 (3) | 0.5000 | 0.8220 (3) | 0.0384 (9) | |
C4 | 0.2721 (4) | 0.5000 | 0.7561 (4) | 0.0684 (18) | |
H4 | 0.2250 | 0.5000 | 0.8028 | 0.082* | |
C5 | 0.2240 (3) | 0.5000 | 0.6223 (4) | 0.0527 (13) | |
H5 | 0.1443 | 0.5000 | 0.5808 | 0.063* | |
C6 | 0.4447 (3) | 0.5000 | 0.9643 (4) | 0.0512 (12) | |
H6 | 0.3957 | 0.5000 | 1.0085 | 0.061* | |
C7 | 0.3524 (2) | 0.34318 (18) | 0.2385 (2) | 0.0317 (5) | |
C8 | 0.4373 (2) | 0.26547 (18) | 0.2600 (2) | 0.0311 (5) | |
C9 | 0.5379 (2) | 0.25962 (18) | 0.3715 (2) | 0.0344 (6) | |
H9 | 0.5561 | 0.3044 | 0.4358 | 0.041* | |
C10 | 0.6099 (2) | 0.18612 (18) | 0.3848 (2) | 0.0334 (6) | |
H10 | 0.6766 | 0.1824 | 0.4600 | 0.040* | |
C11 | 0.4935 (2) | 0.1277 (2) | 0.1875 (3) | 0.0404 (7) | |
H11 | 0.4784 | 0.0830 | 0.1234 | 0.048* | |
C12 | 0.4169 (2) | 0.1982 (2) | 0.1663 (3) | 0.0428 (7) | |
H12 | 0.3516 | 0.2008 | 0.0894 | 0.051* | |
H1W | 0.194 (3) | 0.454 (2) | 0.092 (3) | 0.062 (11)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd | 0.01732 (16) | 0.01592 (15) | 0.02085 (15) | 0.000 | 0.00579 (10) | 0.000 |
N1 | 0.0240 (15) | 0.0354 (16) | 0.0238 (13) | 0.000 | 0.0080 (11) | 0.000 |
N2 | 0.0248 (10) | 0.0259 (11) | 0.0346 (10) | 0.0090 (9) | 0.0053 (8) | −0.0064 (9) |
O1 | 0.0267 (13) | 0.0243 (13) | 0.0303 (12) | 0.000 | 0.0080 (10) | 0.000 |
O2 | 0.0277 (9) | 0.0258 (9) | 0.0340 (9) | 0.0104 (7) | 0.0093 (7) | −0.0042 (7) |
O3 | 0.0627 (14) | 0.0586 (14) | 0.0362 (10) | 0.0390 (12) | −0.0042 (10) | −0.0108 (10) |
C1 | 0.0269 (19) | 0.047 (2) | 0.0264 (16) | 0.000 | 0.0140 (15) | 0.000 |
C2 | 0.0237 (18) | 0.052 (2) | 0.0233 (16) | 0.000 | 0.0070 (14) | 0.000 |
C3 | 0.0295 (19) | 0.062 (3) | 0.0238 (16) | 0.000 | 0.0100 (14) | 0.000 |
C4 | 0.030 (2) | 0.153 (6) | 0.0275 (19) | 0.000 | 0.0158 (17) | 0.000 |
C5 | 0.0201 (19) | 0.105 (4) | 0.0297 (19) | 0.000 | 0.0061 (16) | 0.000 |
C6 | 0.034 (2) | 0.098 (4) | 0.0244 (18) | 0.000 | 0.0145 (15) | 0.000 |
C7 | 0.0277 (12) | 0.0272 (12) | 0.0347 (13) | 0.0106 (11) | 0.0062 (10) | −0.0045 (11) |
C8 | 0.0318 (13) | 0.0274 (13) | 0.0298 (12) | 0.0082 (11) | 0.0073 (10) | −0.0036 (10) |
C9 | 0.0331 (13) | 0.0301 (13) | 0.0341 (12) | 0.0034 (11) | 0.0066 (11) | −0.0101 (11) |
C10 | 0.0256 (12) | 0.0297 (13) | 0.0352 (12) | 0.0076 (11) | 0.0014 (10) | −0.0059 (11) |
C11 | 0.0352 (15) | 0.0364 (15) | 0.0370 (13) | 0.0123 (12) | 0.0004 (11) | −0.0156 (12) |
C12 | 0.0353 (14) | 0.0412 (16) | 0.0373 (13) | 0.0150 (13) | −0.0016 (11) | −0.0129 (12) |
Geometric parameters (Å, º) top
Cd—O2i | 2.3191 (16) | C3—C4 | 1.388 (6) |
Cd—O2 | 2.3191 (16) | C3—C6 | 1.461 (5) |
Cd—N1 | 2.349 (3) | C4—C5 | 1.373 (6) |
Cd—O1 | 2.354 (2) | C4—H4 | 0.9300 |
Cd—N2ii | 2.360 (2) | C5—H5 | 0.9300 |
Cd—N2iii | 2.360 (2) | C6—C6v | 1.310 (8) |
N1—C1 | 1.332 (5) | C6—H6 | 0.9300 |
N1—C5 | 1.335 (5) | C7—O3 | 1.246 (3) |
N2—C10 | 1.337 (3) | C7—C8 | 1.515 (3) |
N2—C11 | 1.341 (3) | C8—C12 | 1.384 (4) |
N2—Cdiv | 2.360 (2) | C8—C9 | 1.391 (4) |
O1—H1W | 0.86 (3) | C9—C10 | 1.377 (4) |
O2—C7 | 1.260 (3) | C9—H9 | 0.9300 |
O3—C7 | 1.246 (3) | C10—H10 | 0.9300 |
C1—C2 | 1.368 (5) | C11—C12 | 1.369 (4) |
C1—H1 | 0.9300 | C11—H11 | 0.9300 |
C2—C3 | 1.382 (5) | C12—H12 | 0.9300 |
C2—H2 | 0.9300 | | |
| | | |
O2i—Cd—O2 | 90.50 (9) | C4—C3—C6 | 121.7 (3) |
O2i—Cd—N1 | 88.84 (7) | C5—C4—C3 | 120.2 (3) |
O2—Cd—N1 | 88.84 (7) | C5—C4—H4 | 119.9 |
O2i—Cd—O1 | 92.12 (6) | C3—C4—H4 | 119.9 |
O2—Cd—O1 | 92.12 (6) | N1—C5—C4 | 123.4 (3) |
N1—Cd—O1 | 178.63 (9) | N1—C5—H5 | 118.3 |
O2i—Cd—N2ii | 176.60 (7) | C4—C5—H5 | 118.3 |
O2—Cd—N2ii | 86.85 (7) | C6v—C6—C3 | 126.6 (5) |
N1—Cd—N2ii | 93.23 (7) | C6v—C6—H6 | 116.7 |
O1—Cd—N2ii | 85.85 (7) | C3—C6—H6 | 116.7 |
O2i—Cd—N2iii | 86.85 (7) | O3—C7—O2 | 126.4 (2) |
O2—Cd—N2iii | 176.60 (7) | O3—C7—O2 | 126.4 (2) |
N1—Cd—N2iii | 93.23 (7) | O3—C7—C8 | 116.0 (2) |
O1—Cd—N2iii | 85.85 (7) | O3—C7—C8 | 116.0 (2) |
N2ii—Cd—N2iii | 95.71 (11) | O2—C7—C8 | 117.6 (2) |
C1—N1—C5 | 116.1 (3) | C12—C8—C9 | 117.8 (2) |
C1—N1—Cd | 115.1 (2) | C12—C8—C7 | 120.1 (2) |
C5—N1—Cd | 128.8 (2) | C9—C8—C7 | 122.1 (2) |
C10—N2—C11 | 116.9 (2) | C10—C9—C8 | 118.6 (2) |
C10—N2—Cdiv | 121.80 (16) | C10—C9—H9 | 120.7 |
C11—N2—Cdiv | 121.17 (16) | C8—C9—H9 | 120.7 |
Cd—O1—H1W | 92 (2) | N2—C10—C9 | 123.8 (2) |
C7—O2—Cd | 121.18 (15) | N2—C10—H10 | 118.1 |
N1—C1—C2 | 124.1 (3) | C9—C10—H10 | 118.1 |
N1—C1—H1 | 118.0 | N2—C11—C12 | 123.3 (2) |
C2—C1—H1 | 118.0 | N2—C11—H11 | 118.4 |
C1—C2—C3 | 120.1 (3) | C12—C11—H11 | 118.4 |
C1—C2—H2 | 120.0 | C11—C12—C8 | 119.6 (2) |
C3—C2—H2 | 120.0 | C11—C12—H12 | 120.2 |
C2—C3—C4 | 116.1 (3) | C8—C12—H12 | 120.2 |
C2—C3—C6 | 122.2 (3) | | |
| | | |
O2i—Cd—N1—C1 | −45.26 (4) | O3—C7—C8—C12 | −20.8 (4) |
O2—Cd—N1—C1 | 45.26 (4) | O2—C7—C8—C12 | 160.4 (3) |
N2ii—Cd—N1—C1 | 132.04 (5) | O3—C7—C8—C9 | 158.1 (3) |
N2iii—Cd—N1—C1 | −132.04 (5) | O3—C7—C8—C9 | 158.1 (3) |
O2i—Cd—N1—C5 | 134.74 (4) | O2—C7—C8—C9 | −20.7 (4) |
O2—Cd—N1—C5 | −134.74 (4) | C12—C8—C9—C10 | −2.0 (4) |
N2ii—Cd—N1—C5 | −47.96 (5) | C7—C8—C9—C10 | 179.1 (3) |
N2iii—Cd—N1—C5 | 47.96 (5) | C11—N2—C10—C9 | 1.2 (4) |
O2i—Cd—O2—C7 | −103.75 (19) | Cdiv—N2—C10—C9 | 176.8 (2) |
N1—Cd—O2—C7 | 167.4 (2) | C8—C9—C10—N2 | 0.5 (4) |
O1—Cd—O2—C7 | −11.6 (2) | C10—N2—C11—C12 | −1.4 (4) |
N2ii—Cd—O2—C7 | 74.1 (2) | Cdiv—N2—C11—C12 | −177.0 (2) |
Cd—O2—C7—O3 | 6.4 (4) | N2—C11—C12—C8 | −0.1 (5) |
Cd—O2—C7—O3 | 6.4 (4) | C9—C8—C12—C11 | 1.8 (4) |
Cd—O2—C7—C8 | −175.00 (17) | C7—C8—C12—C11 | −179.2 (3) |
O3—C7—C8—C12 | −20.8 (4) | | |
Symmetry codes: (i) x, −y+1, z; (ii) x−1/2, −y+1/2, z; (iii) x−1/2, y+1/2, z; (iv) x+1/2, y−1/2, z; (v) −x+1, −y+1, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1W···O3 | 0.86 (3) | 1.77 (3) | 2.615 (2) | 170 (3) |