Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807028425/is2175sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807028425/is2175Isup2.hkl |
CCDC reference: 1148879
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.007 Å
- R factor = 0.047
- wR factor = 0.136
- Data-to-parameter ratio = 11.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT223_ALERT_4_C Large Solvent/Anion H Ueq(max)/Ueq(min) ... 3.75 Ratio PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C1 - C2 ... 1.53 Ang. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 51.00 A 3
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Cd1 (2) 1.97 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 1 ALERT type 5 Informative message, check
For related compounds, see: Ngo et al. (2004); Evans et al. (2001); Vioux et al. (2004); Sanchez et al. (2003); Evans & Lin (2001); Jannasch (2003); Javaid et al. (2001); Honma et al. (2001); Sudik et al. (2005); Rowsell et al. (2004); Kitaura et al. (2002).
A mixture of cadmium acetate (0.5 mmol), 3,3',4,4'-benzophenone tetracarboxylic acid (0.5 mmol) and 1,10-phenanthroline (0.5 mmol) in 20 ml solution of water and ethanol (1:1) was sealed in an 30 ml Teflon-lined stainless autoclave, and kept at 423 K for 2 days. Colorless block-shaped crystals were obtained in 16% yield after slowly cooling to room temperature. Anal. Calc. for C65H42Cd2N8O11: C 58.38, H 3.14, N 8.38, Cd 16.83%; Found: C 58.31, H 3.11, N 8.29, Cd 16.76%.
C-bound H atoms were generated geometrically (C—H = 0.93 Å) and refined as riding, with Uiso(H)= 1.2Ueq(C). H atoms of the water molecule were located in a difference map and were refined with distance restraints of H···H = 1.38 (2) and O–H = 0.82 (2) Å, and with a fixed Uiso(H) of 0.80 Å2. The highest peak and deepest hole in the difference Fourier map are located 0.92 and 0.65 Å, respectively, from atoms Cd1 and O6.
Hybrid organic-inorganic materials occupy a prominent position by virtue of their applications to catalysis, optical materials, membranes, and sorption (Ngo et al., 2004; Evans et al., 2001; Vioux et al., 2004; Sanchez et al., 2003; Evans & Lin, 2001; Jannasch, 2003; Javaid et al., 2001; Honma et al., 2001; Sudik et al., 2005; Rowsell et al., 2004; Kitaura et al., 2002). The design of organic-inorganic hybrid materials is conceived of the metal, metal cluster, or metal oxide substructure as a node from which rigid or flexible multitopic organic ligands radiate to act as tethers to adjacent nodes in the bottom-up construction of complex extended architectures. While a variety of organic molecules have been investigated as potential tethers, materials incorporating multitopic carboxylates and pyridine ligands have witnessed the most significant development. However, ligands offering alternative tether lengths, different charge-balance requirements, and orientations of donor groups may afford advantages in the design of materials. Herein, We report the structure of the new title complex, (I). The cadmium cation is hexa-coordinated by two carboxylate oxygen atoms from two 3,3',4,4'-benzophenone tetracarboxylate and four nitrogen atoms from two 1,10-phenanthroline, showing a slightly distorted octahedral geometry (Fig. 1). Each two Cd atoms form one circle via two half of 3,3',4,4'-benzophenone tetracarboxylate, which are further linked to form chains (Fig. 2). The Cd—N and Cd—O bond lengths are in the range of 2.392 (4)–2.524 (4) and 2.255 (3)–2.275 (4) Å, respectively.
For related compounds, see: Ngo et al. (2004); Evans et al. (2001); Vioux et al. (2004); Sanchez et al. (2003); Evans & Lin (2001); Jannasch (2003); Javaid et al. (2001); Honma et al. (2001); Sudik et al. (2005); Rowsell et al. (2004); Kitaura et al. (2002).
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1999); software used to prepare material for publication: SHELXTL.
[Cd2(C17H6O9)(C12H8N2)4]·2H2O | F(000) = 2688 |
Mr = 1335.87 | Dx = 1.631 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3610 reflections |
a = 24.5326 (10) Å | θ = 4.0–27.4° |
b = 9.9826 (15) Å | µ = 0.86 mm−1 |
c = 23.761 (3) Å | T = 273 K |
β = 110.797 (2)° | Block, colorless |
V = 5439.9 (11) Å3 | 0.10 × 0.10 × 0.10 mm |
Z = 4 |
Bruker APEXII CCD area-detector diffractometer | 3527 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 25.0°, θmin = 1.8° |
φ and ω scans | h = −29→28 |
20482 measured reflections | k = −11→11 |
4681 independent reflections | l = −28→28 |
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)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.136 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0734P)2 + 4.4546P] where P = (Fo2 + 2Fc2)/3 |
4681 reflections | (Δ/σ)max < 0.001 |
398 parameters | Δρmax = 1.48 e Å−3 |
3 restraints | Δρmin = −1.39 e Å−3 |
[Cd2(C17H6O9)(C12H8N2)4]·2H2O | V = 5439.9 (11) Å3 |
Mr = 1335.87 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 24.5326 (10) Å | µ = 0.86 mm−1 |
b = 9.9826 (15) Å | T = 273 K |
c = 23.761 (3) Å | 0.10 × 0.10 × 0.10 mm |
β = 110.797 (2)° |
Bruker APEXII CCD area-detector diffractometer | 3527 reflections with I > 2σ(I) |
20482 measured reflections | Rint = 0.022 |
4681 independent reflections |
R[F2 > 2σ(F2)] = 0.047 | 3 restraints |
wR(F2) = 0.136 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Δρmax = 1.48 e Å−3 |
4681 reflections | Δρmin = −1.39 e Å−3 |
398 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Cd1 | 0.672613 (12) | 0.28062 (3) | 0.051215 (14) | 0.03039 (16) | |
C1 | 0.66588 (18) | 0.4960 (5) | −0.0547 (2) | 0.0350 (11) | |
C2 | 0.62528 (17) | 0.4085 (5) | −0.10503 (19) | 0.0317 (10) | |
C3 | 0.56796 (19) | 0.4497 (6) | −0.1303 (2) | 0.0522 (15) | |
H28 | 0.5560 | 0.5258 | −0.1153 | 0.063* | |
C4 | 0.52773 (19) | 0.3802 (6) | −0.1777 (2) | 0.0536 (15) | |
H29 | 0.4896 | 0.4114 | −0.1942 | 0.064* | |
C5 | 0.54344 (18) | 0.2669 (5) | −0.2001 (2) | 0.0392 (12) | |
C6 | 0.60108 (18) | 0.2224 (5) | −0.1749 (2) | 0.0341 (11) | |
H31 | 0.6121 | 0.1441 | −0.1892 | 0.041* | |
C7 | 0.64206 (16) | 0.2930 (4) | −0.1289 (2) | 0.0283 (10) | |
C8 | 0.70458 (18) | 0.2475 (5) | −0.1058 (2) | 0.0335 (11) | |
C9 | 0.5000 | 0.1883 (8) | −0.2500 | 0.0427 (18) | |
C10 | 0.67162 (18) | 0.0193 (5) | −0.0332 (2) | 0.0346 (11) | |
H13 | 0.7116 | 0.0334 | −0.0153 | 0.042* | |
C11 | 0.6526 (2) | −0.0881 (6) | −0.0740 (2) | 0.0429 (12) | |
H14 | 0.6792 | −0.1455 | −0.0814 | 0.052* | |
C12 | 0.5939 (2) | −0.1053 (6) | −0.1023 (2) | 0.0499 (14) | |
H15 | 0.5798 | −0.1725 | −0.1309 | 0.060* | |
C13 | 0.55538 (19) | −0.0220 (5) | −0.0881 (2) | 0.0407 (12) | |
C14 | 0.57798 (16) | 0.0817 (5) | −0.04594 (19) | 0.0305 (10) | |
C15 | 0.53995 (16) | 0.1662 (5) | −0.0282 (2) | 0.0345 (11) | |
C16 | 0.47858 (17) | 0.1462 (5) | −0.0548 (2) | 0.0423 (12) | |
C17 | 0.4574 (2) | 0.0417 (6) | −0.0988 (3) | 0.0582 (16) | |
H18 | 0.4174 | 0.0282 | −0.1164 | 0.070* | |
C18 | 0.4931 (2) | −0.0363 (6) | −0.1152 (3) | 0.0539 (15) | |
H17 | 0.4775 | −0.1012 | −0.1446 | 0.065* | |
C19 | 0.4427 (2) | 0.2264 (6) | −0.0360 (3) | 0.0530 (16) | |
H20 | 0.4025 | 0.2140 | −0.0520 | 0.064* | |
C20 | 0.4658 (2) | 0.3252 (6) | 0.0065 (3) | 0.0557 (15) | |
H21 | 0.4419 | 0.3803 | 0.0192 | 0.067* | |
C21 | 0.5267 (2) | 0.3397 (6) | 0.0299 (3) | 0.0512 (14) | |
H22 | 0.5426 | 0.4061 | 0.0584 | 0.061* | |
C22 | 0.69912 (18) | −0.0002 (5) | 0.1315 (2) | 0.0393 (12) | |
H1 | 0.7059 | −0.0314 | 0.0977 | 0.047* | |
C23 | 0.70645 (19) | −0.0893 (6) | 0.1788 (2) | 0.0447 (13) | |
H2 | 0.7177 | −0.1774 | 0.1762 | 0.054* | |
C24 | 0.69687 (19) | −0.0450 (5) | 0.2296 (2) | 0.0446 (13) | |
H3 | 0.7013 | −0.1032 | 0.2615 | 0.054* | |
C25 | 0.68045 (18) | 0.0886 (5) | 0.2326 (2) | 0.0385 (11) | |
C26 | 0.67419 (16) | 0.1711 (5) | 0.1821 (2) | 0.0325 (10) | |
C27 | 0.6712 (2) | 0.1433 (6) | 0.2843 (2) | 0.0492 (13) | |
H5 | 0.6750 | 0.0881 | 0.3170 | 0.059* | |
C28 | 0.6571 (3) | 0.2734 (6) | 0.2864 (3) | 0.0540 (15) | |
H6 | 0.6512 | 0.3069 | 0.3203 | 0.065* | |
C29 | 0.65118 (19) | 0.3610 (5) | 0.2359 (2) | 0.0423 (12) | |
C30 | 0.65990 (17) | 0.3122 (5) | 0.1843 (2) | 0.0329 (10) | |
C31 | 0.6484 (2) | 0.5214 (5) | 0.1396 (3) | 0.0458 (13) | |
H10 | 0.6484 | 0.5775 | 0.1083 | 0.055* | |
C32 | 0.6388 (2) | 0.5774 (6) | 0.1898 (3) | 0.0563 (15) | |
H9 | 0.6316 | 0.6688 | 0.1905 | 0.068* | |
C33 | 0.6400 (2) | 0.4995 (6) | 0.2370 (3) | 0.0551 (15) | |
H8 | 0.6335 | 0.5371 | 0.2699 | 0.066* | |
H1W | 0.706 (10) | 0.649 (5) | 0.046 (9) | 0.30 (17)* | |
H2W | 0.730 (3) | 0.774 (6) | 0.047 (3) | 0.08 (3)* | |
N1 | 0.68314 (14) | 0.1253 (4) | 0.13188 (16) | 0.0310 (8) | |
N2 | 0.65750 (15) | 0.3910 (4) | 0.13560 (18) | 0.0356 (9) | |
N3 | 0.63683 (13) | 0.1007 (4) | −0.01870 (16) | 0.0319 (9) | |
N4 | 0.56285 (16) | 0.2636 (4) | 0.0134 (2) | 0.0412 (11) | |
O1 | 0.66782 (13) | 0.4723 (3) | −0.00050 (14) | 0.0382 (8) | |
O2 | 0.68981 (15) | 0.5896 (4) | −0.06927 (16) | 0.0516 (10) | |
O3 | 0.73871 (12) | 0.3046 (3) | −0.06003 (14) | 0.0375 (8) | |
O4 | 0.71910 (13) | 0.1553 (4) | −0.13297 (17) | 0.0534 (10) | |
O5 | 0.5000 | 0.0672 (6) | −0.2500 | 0.0660 (17) | |
O6 | 0.7101 (2) | 0.7270 (5) | 0.0619 (2) | 0.0664 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0267 (2) | 0.0350 (3) | 0.0285 (2) | 0.00281 (13) | 0.00860 (13) | 0.00070 (14) |
C1 | 0.031 (2) | 0.038 (3) | 0.032 (3) | 0.004 (2) | 0.0066 (18) | −0.003 (2) |
C2 | 0.0277 (19) | 0.040 (3) | 0.024 (2) | 0.0007 (19) | 0.0047 (16) | 0.004 (2) |
C3 | 0.035 (2) | 0.063 (4) | 0.050 (3) | 0.015 (2) | 0.004 (2) | −0.012 (3) |
C4 | 0.030 (2) | 0.071 (4) | 0.048 (3) | 0.015 (2) | −0.001 (2) | −0.007 (3) |
C5 | 0.028 (2) | 0.048 (3) | 0.034 (3) | 0.004 (2) | 0.0012 (19) | 0.005 (2) |
C6 | 0.032 (2) | 0.037 (3) | 0.026 (2) | 0.0014 (19) | 0.0010 (18) | 0.002 (2) |
C7 | 0.0239 (19) | 0.035 (3) | 0.024 (2) | −0.0014 (17) | 0.0058 (16) | 0.0004 (19) |
C8 | 0.028 (2) | 0.040 (3) | 0.030 (3) | 0.0028 (19) | 0.0090 (19) | 0.006 (2) |
C9 | 0.031 (3) | 0.052 (5) | 0.036 (4) | 0.000 | 0.001 (3) | 0.000 |
C10 | 0.032 (2) | 0.038 (3) | 0.033 (3) | 0.0013 (19) | 0.0110 (18) | −0.004 (2) |
C11 | 0.043 (2) | 0.049 (3) | 0.040 (3) | 0.005 (2) | 0.018 (2) | −0.003 (3) |
C12 | 0.048 (3) | 0.057 (4) | 0.042 (3) | −0.006 (2) | 0.013 (2) | −0.019 (3) |
C13 | 0.039 (2) | 0.047 (3) | 0.037 (3) | −0.009 (2) | 0.0142 (19) | −0.005 (2) |
C14 | 0.0276 (19) | 0.035 (3) | 0.027 (2) | −0.0025 (18) | 0.0070 (16) | 0.003 (2) |
C15 | 0.026 (2) | 0.040 (3) | 0.036 (3) | −0.0054 (19) | 0.0094 (17) | 0.004 (2) |
C16 | 0.025 (2) | 0.052 (3) | 0.048 (3) | 0.002 (2) | 0.0105 (19) | 0.006 (3) |
C17 | 0.029 (2) | 0.070 (4) | 0.068 (4) | −0.014 (2) | 0.007 (2) | −0.009 (3) |
C18 | 0.039 (3) | 0.060 (4) | 0.058 (4) | −0.017 (3) | 0.011 (2) | −0.024 (3) |
C19 | 0.027 (2) | 0.063 (4) | 0.067 (4) | 0.004 (2) | 0.013 (2) | 0.006 (3) |
C20 | 0.038 (2) | 0.063 (4) | 0.069 (4) | 0.016 (3) | 0.023 (2) | 0.001 (3) |
C21 | 0.041 (3) | 0.053 (4) | 0.056 (4) | 0.006 (2) | 0.014 (2) | −0.009 (3) |
C22 | 0.035 (2) | 0.037 (3) | 0.048 (3) | 0.003 (2) | 0.018 (2) | 0.004 (2) |
C23 | 0.042 (2) | 0.040 (3) | 0.052 (3) | 0.004 (2) | 0.016 (2) | 0.001 (3) |
C24 | 0.043 (2) | 0.045 (3) | 0.044 (3) | 0.002 (2) | 0.013 (2) | 0.013 (3) |
C25 | 0.034 (2) | 0.050 (3) | 0.032 (3) | −0.004 (2) | 0.0116 (18) | 0.002 (2) |
C26 | 0.0233 (18) | 0.043 (3) | 0.032 (2) | −0.0025 (18) | 0.0097 (16) | −0.001 (2) |
C27 | 0.069 (3) | 0.047 (3) | 0.035 (3) | −0.002 (3) | 0.021 (2) | 0.008 (3) |
C28 | 0.068 (3) | 0.070 (4) | 0.033 (3) | −0.015 (3) | 0.028 (3) | −0.011 (3) |
C29 | 0.041 (2) | 0.049 (3) | 0.041 (3) | −0.007 (2) | 0.019 (2) | −0.015 (3) |
C30 | 0.0273 (19) | 0.043 (3) | 0.031 (2) | −0.0015 (19) | 0.0126 (17) | −0.006 (2) |
C31 | 0.047 (3) | 0.035 (3) | 0.058 (3) | 0.006 (2) | 0.021 (2) | 0.003 (3) |
C32 | 0.061 (3) | 0.037 (3) | 0.073 (4) | 0.003 (3) | 0.026 (3) | −0.011 (3) |
C33 | 0.058 (3) | 0.053 (4) | 0.061 (4) | −0.003 (3) | 0.029 (3) | −0.026 (3) |
N1 | 0.0319 (17) | 0.032 (2) | 0.032 (2) | 0.0018 (16) | 0.0154 (15) | 0.0049 (18) |
N2 | 0.0333 (18) | 0.034 (2) | 0.040 (2) | 0.0009 (16) | 0.0137 (15) | 0.000 (2) |
N3 | 0.0233 (16) | 0.038 (2) | 0.032 (2) | −0.0034 (15) | 0.0071 (14) | −0.0029 (18) |
N4 | 0.0303 (19) | 0.048 (3) | 0.047 (3) | 0.0035 (17) | 0.0151 (18) | −0.003 (2) |
O1 | 0.0489 (17) | 0.0366 (19) | 0.0269 (18) | 0.0026 (15) | 0.0106 (13) | −0.0013 (15) |
O2 | 0.062 (2) | 0.043 (2) | 0.050 (2) | −0.0156 (19) | 0.0203 (17) | 0.0016 (19) |
O3 | 0.0236 (14) | 0.055 (2) | 0.0314 (18) | −0.0001 (13) | 0.0064 (12) | −0.0064 (16) |
O4 | 0.0338 (16) | 0.058 (2) | 0.065 (3) | 0.0066 (17) | 0.0131 (16) | −0.019 (2) |
O5 | 0.055 (3) | 0.054 (4) | 0.064 (4) | 0.000 | −0.009 (3) | 0.000 |
O6 | 0.068 (3) | 0.065 (3) | 0.074 (3) | −0.006 (2) | 0.034 (2) | −0.019 (2) |
Cd1—O1 | 2.255 (3) | C16—C17 | 1.438 (8) |
Cd1—O3i | 2.275 (3) | C17—C18 | 1.328 (8) |
Cd1—N3 | 2.392 (4) | C17—H18 | 0.9300 |
Cd1—N1 | 2.407 (4) | C18—H17 | 0.9300 |
Cd1—N2 | 2.429 (4) | C19—C20 | 1.380 (8) |
Cd1—N4 | 2.524 (4) | C19—H20 | 0.9300 |
C1—O2 | 1.217 (6) | C20—C21 | 1.405 (7) |
C1—O1 | 1.293 (6) | C20—H21 | 0.9300 |
C1—C2 | 1.529 (6) | C21—N4 | 1.327 (7) |
C2—C3 | 1.381 (6) | C21—H22 | 0.9300 |
C2—C7 | 1.410 (6) | C22—N1 | 1.314 (6) |
C3—C4 | 1.390 (7) | C22—C23 | 1.394 (7) |
C3—H28 | 0.9300 | C22—H1 | 0.9300 |
C4—C5 | 1.363 (7) | C23—C24 | 1.382 (7) |
C4—H29 | 0.9300 | C23—H2 | 0.9300 |
C5—C6 | 1.398 (6) | C24—C25 | 1.402 (7) |
C5—C9 | 1.503 (6) | C24—H3 | 0.9300 |
C6—C7 | 1.386 (6) | C25—C26 | 1.419 (7) |
C6—H31 | 0.9300 | C25—C27 | 1.434 (7) |
C7—C8 | 1.504 (6) | C26—N1 | 1.366 (6) |
C8—O4 | 1.246 (6) | C26—C30 | 1.458 (7) |
C8—O3 | 1.250 (6) | C27—C28 | 1.349 (8) |
C9—O5 | 1.209 (9) | C27—H5 | 0.9300 |
C9—C5ii | 1.503 (6) | C28—C29 | 1.449 (8) |
C10—N3 | 1.310 (6) | C28—H6 | 0.9300 |
C10—C11 | 1.409 (7) | C29—C30 | 1.405 (7) |
C10—H13 | 0.9300 | C29—C33 | 1.411 (8) |
C11—C12 | 1.368 (7) | C30—N2 | 1.383 (6) |
C11—H14 | 0.9300 | C31—N2 | 1.330 (6) |
C12—C13 | 1.386 (7) | C31—C32 | 1.411 (8) |
C12—H15 | 0.9300 | C31—H10 | 0.9300 |
C13—C14 | 1.410 (7) | C32—C33 | 1.357 (8) |
C13—C18 | 1.440 (6) | C32—H9 | 0.9300 |
C14—N3 | 1.370 (5) | C33—H8 | 0.9300 |
C14—C15 | 1.427 (6) | O3—Cd1i | 2.275 (3) |
C15—N4 | 1.357 (7) | O6—H1W | 0.85 (5) |
C15—C16 | 1.425 (5) | O6—H2W | 0.84 (7) |
C16—C19 | 1.376 (8) | ||
O1—Cd1—O3i | 103.33 (12) | C16—C17—H18 | 118.9 |
O1—Cd1—N3 | 108.88 (12) | C17—C18—C13 | 121.1 (5) |
O3i—Cd1—N3 | 83.48 (11) | C17—C18—H17 | 119.5 |
O1—Cd1—N1 | 161.97 (12) | C13—C18—H17 | 119.4 |
O3i—Cd1—N1 | 81.79 (12) | C16—C19—C20 | 120.6 (4) |
N3—Cd1—N1 | 88.77 (13) | C16—C19—H20 | 119.7 |
O1—Cd1—N2 | 94.07 (12) | C20—C19—H20 | 119.7 |
O3i—Cd1—N2 | 120.99 (11) | C19—C20—C21 | 117.8 (5) |
N3—Cd1—N2 | 142.01 (13) | C19—C20—H21 | 121.1 |
N1—Cd1—N2 | 68.88 (13) | C21—C20—H21 | 121.1 |
O1—Cd1—N4 | 91.18 (13) | N4—C21—C20 | 123.5 (5) |
O3i—Cd1—N4 | 150.69 (13) | N4—C21—H22 | 118.2 |
N3—Cd1—N4 | 67.65 (13) | C20—C21—H22 | 118.2 |
N1—Cd1—N4 | 92.26 (13) | N1—C22—C23 | 123.7 (5) |
N2—Cd1—N4 | 82.44 (13) | N1—C22—H1 | 118.1 |
O2—C1—O1 | 124.9 (4) | C23—C22—H1 | 118.1 |
O2—C1—C2 | 117.5 (4) | C24—C23—C22 | 119.2 (5) |
O1—C1—C2 | 117.3 (4) | C24—C23—H2 | 120.4 |
C3—C2—C7 | 117.7 (4) | C22—C23—H2 | 120.4 |
C3—C2—C1 | 116.8 (4) | C23—C24—C25 | 119.3 (5) |
C7—C2—C1 | 125.4 (4) | C23—C24—H3 | 120.3 |
C2—C3—C4 | 121.6 (5) | C25—C24—H3 | 120.3 |
C2—C3—H28 | 119.2 | C24—C25—C26 | 117.1 (5) |
C4—C3—H28 | 119.2 | C24—C25—C27 | 122.8 (5) |
C5—C4—C3 | 120.8 (4) | C26—C25—C27 | 120.1 (5) |
C5—C4—H29 | 119.6 | N1—C26—C25 | 122.8 (4) |
C3—C4—H29 | 119.6 | N1—C26—C30 | 118.1 (4) |
C4—C5—C6 | 118.6 (4) | C25—C26—C30 | 119.0 (4) |
C4—C5—C9 | 121.5 (4) | C28—C27—C25 | 121.2 (5) |
C6—C5—C9 | 119.9 (5) | C28—C27—H5 | 119.4 |
C7—C6—C5 | 121.1 (4) | C25—C27—H5 | 119.4 |
C7—C6—H31 | 119.4 | C27—C28—C29 | 120.2 (5) |
C5—C6—H31 | 119.5 | C27—C28—H6 | 119.9 |
C6—C7—C2 | 120.0 (4) | C29—C28—H6 | 119.9 |
C6—C7—C8 | 119.6 (4) | C30—C29—C33 | 116.5 (5) |
C2—C7—C8 | 120.4 (4) | C30—C29—C28 | 120.7 (5) |
O4—C8—O3 | 124.1 (4) | C33—C29—C28 | 122.7 (5) |
O4—C8—C7 | 118.4 (4) | N2—C30—C29 | 124.0 (4) |
O3—C8—C7 | 117.5 (4) | N2—C30—C26 | 117.3 (4) |
O5—C9—C5 | 121.5 (3) | C29—C30—C26 | 118.7 (4) |
O5—C9—C5ii | 121.5 (3) | N2—C31—C32 | 122.0 (5) |
C5—C9—C5ii | 117.1 (7) | N2—C31—H10 | 119.0 |
N3—C10—C11 | 124.4 (4) | C32—C31—H10 | 119.0 |
N3—C10—H13 | 117.8 | C33—C32—C31 | 120.7 (5) |
C11—C10—H13 | 117.8 | C33—C32—H9 | 119.6 |
C12—C11—C10 | 117.8 (5) | C31—C32—H9 | 119.6 |
C12—C11—H14 | 121.1 | C32—C33—C29 | 119.6 (5) |
C10—C11—H14 | 121.1 | C32—C33—H8 | 120.2 |
C11—C12—C13 | 119.7 (5) | C29—C33—H8 | 120.2 |
C11—C12—H15 | 120.1 | C22—N1—C26 | 117.8 (4) |
C13—C12—H15 | 120.2 | C22—N1—Cd1 | 123.8 (3) |
C12—C13—C14 | 118.9 (4) | C26—N1—Cd1 | 118.3 (3) |
C12—C13—C18 | 122.6 (5) | C31—N2—C30 | 117.1 (5) |
C14—C13—C18 | 118.5 (5) | C31—N2—Cd1 | 125.5 (4) |
N3—C14—C13 | 121.3 (4) | C30—N2—Cd1 | 117.3 (3) |
N3—C14—C15 | 117.9 (4) | C10—N3—C14 | 117.8 (4) |
C13—C14—C15 | 120.7 (4) | C10—N3—Cd1 | 122.4 (3) |
N4—C15—C16 | 121.4 (5) | C14—N3—Cd1 | 119.8 (3) |
N4—C15—C14 | 119.5 (3) | C21—N4—C15 | 118.5 (4) |
C16—C15—C14 | 119.0 (4) | C21—N4—Cd1 | 126.6 (3) |
C19—C16—C15 | 118.2 (5) | C15—N4—Cd1 | 114.9 (3) |
C19—C16—C17 | 123.4 (4) | C1—O1—Cd1 | 132.4 (3) |
C15—C16—C17 | 118.4 (5) | C8—O3—Cd1i | 103.5 (3) |
C18—C17—C16 | 122.2 (4) | H1W—O6—H2W | 109 (16) |
C18—C17—H18 | 118.9 |
Symmetry codes: (i) −x+3/2, −y+1/2, −z; (ii) −x+1, y, −z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Cd2(C17H6O9)(C12H8N2)4]·2H2O |
Mr | 1335.87 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 273 |
a, b, c (Å) | 24.5326 (10), 9.9826 (15), 23.761 (3) |
β (°) | 110.797 (2) |
V (Å3) | 5439.9 (11) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.86 |
Crystal size (mm) | 0.10 × 0.10 × 0.10 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 20482, 4681, 3527 |
Rint | 0.022 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.136, 1.00 |
No. of reflections | 4681 |
No. of parameters | 398 |
No. of restraints | 3 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.48, −1.39 |
Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1999), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1999), SHELXTL.
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Hybrid organic-inorganic materials occupy a prominent position by virtue of their applications to catalysis, optical materials, membranes, and sorption (Ngo et al., 2004; Evans et al., 2001; Vioux et al., 2004; Sanchez et al., 2003; Evans & Lin, 2001; Jannasch, 2003; Javaid et al., 2001; Honma et al., 2001; Sudik et al., 2005; Rowsell et al., 2004; Kitaura et al., 2002). The design of organic-inorganic hybrid materials is conceived of the metal, metal cluster, or metal oxide substructure as a node from which rigid or flexible multitopic organic ligands radiate to act as tethers to adjacent nodes in the bottom-up construction of complex extended architectures. While a variety of organic molecules have been investigated as potential tethers, materials incorporating multitopic carboxylates and pyridine ligands have witnessed the most significant development. However, ligands offering alternative tether lengths, different charge-balance requirements, and orientations of donor groups may afford advantages in the design of materials. Herein, We report the structure of the new title complex, (I). The cadmium cation is hexa-coordinated by two carboxylate oxygen atoms from two 3,3',4,4'-benzophenone tetracarboxylate and four nitrogen atoms from two 1,10-phenanthroline, showing a slightly distorted octahedral geometry (Fig. 1). Each two Cd atoms form one circle via two half of 3,3',4,4'-benzophenone tetracarboxylate, which are further linked to form chains (Fig. 2). The Cd—N and Cd—O bond lengths are in the range of 2.392 (4)–2.524 (4) and 2.255 (3)–2.275 (4) Å, respectively.