Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807039050/rk2033sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807039050/rk2033Isup2.hkl |
CCDC reference: 1101493
A mixture of palladium acetate (0.1 mmol), 3,3',4,4'-benzophenone tetracarboxylic acid (0.1 mmol), and 1,10-phenanthroline (0.2 mmol) in 16 ml 1:1 solution of methanol and acetonitrile was sealed in an 25 ml teflon-lined stainless autoclave, and kept at 393 K for 2 days. Colorless, block-shaped crystals were obtained after slowly cooling to room temperature with a yield of 8%. Anal. Calc. for C65H42N8O11Pd2: C 58.92, H 3.17, N 8.46%; Found: C 58.91, H 3.12, N 8.38%.
All H atoms on C atoms were generated geometrically and refined as riding atoms with C–H = 0.93Å and Uiso(H) = 1.2Ueq(C). The H atoms of the water molecule were located from difference density maps and were refined with distance restraints of d(H–H) = 1.38 (2) Å, d(O–H) = 0.82 (2) Å, and with a fixed Uiso of 0.80 Å2.
The structure contains solvent accessible voids along y axis with the nearest distance of 2.915 Å between O3 and its symmetric site. The position (1/2, 0.766, 3/4) of Δρmax peack (1.46 e A-3) is 0.819 Å to Pd1 atom.
As shown on Fig. 1, the palladium 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 ligand, exhibiting a distorted octahedral geometry. Each two Pd atoms form one circle via four carboxylate group belonging two of 3,3',4,4'-benzophenone tetracarboxylate, which are further linked to form one dimensional chain (Fig.2). Interestinfly, the benzophenone carbonyl group (C33?O5) lies on a twofold rotation axis. Moreover, the hydrogen bonds link the chains into a three-dimensional structure (Fig. 3).
For the isostructural Cd2+ analogue, see: Gao et al. (2007).
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.
[Pd2(C17H6O9)(C12H8N2)4]·2H2O | F(000) = 2672 |
Mr = 1323.91 | Dx = 1.620 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 4924 reflections |
a = 24.483 (2) Å | θ = 1.8–25.5° |
b = 10.0027 (10) Å | µ = 0.74 mm−1 |
c = 23.7133 (15) Å | T = 273 K |
β = 110.786 (2)° | Block, colourless |
V = 5429.4 (8) Å3 | 0.12 × 0.10 × 0.08 mm |
Z = 4 |
Bruker APEXII CCD area-detector diffractometer | 4924 independent reflections |
Radiation source: fine-focus sealed tube | 3659 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
φ and ω scans | θmax = 25.5°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −29→29 |
Tmin = 0.917, Tmax = 0.943 | k = −12→12 |
21160 measured 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) = 0.114 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.053P)2 + 2.9034P] where P = (Fo2 + 2Fc2)/3 |
4924 reflections | (Δ/σ)max < 0.001 |
395 parameters | Δρmax = 1.46 e Å−3 |
4 restraints | Δρmin = −1.86 e Å−3 |
[Pd2(C17H6O9)(C12H8N2)4]·2H2O | V = 5429.4 (8) Å3 |
Mr = 1323.91 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 24.483 (2) Å | µ = 0.74 mm−1 |
b = 10.0027 (10) Å | T = 273 K |
c = 23.7133 (15) Å | 0.12 × 0.10 × 0.08 mm |
β = 110.786 (2)° |
Bruker APEXII CCD area-detector diffractometer | 4924 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 3659 reflections with I > 2σ(I) |
Tmin = 0.917, Tmax = 0.943 | Rint = 0.042 |
21160 measured reflections |
R[F2 > 2σ(F2)] = 0.047 | 4 restraints |
wR(F2) = 0.114 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Δρmax = 1.46 e Å−3 |
4924 reflections | Δρmin = −1.86 e Å−3 |
395 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 > 2σ(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 | ||
C1 | 0.66566 (15) | 0.4950 (4) | −0.05461 (18) | 0.0373 (10) | |
C2 | 0.62534 (14) | 0.4085 (4) | −0.10507 (17) | 0.0343 (9) | |
C3 | 0.56800 (16) | 0.4503 (5) | −0.1303 (2) | 0.0555 (13) | |
H3 | 0.5561 | 0.5266 | −0.1154 | 0.067* | |
C4 | 0.52765 (16) | 0.3801 (5) | −0.1776 (2) | 0.0590 (14) | |
H4 | 0.4894 | 0.4110 | −0.1942 | 0.071* | |
C5 | 0.54343 (16) | 0.2665 (5) | −0.1999 (2) | 0.0430 (11) | |
C6 | 0.60110 (15) | 0.2225 (4) | −0.17500 (19) | 0.0370 (10) | |
H6 | 0.6122 | 0.1447 | −0.1895 | 0.044* | |
C7 | 0.64201 (14) | 0.2932 (4) | −0.12896 (17) | 0.0319 (9) | |
C8 | 0.70470 (15) | 0.2476 (4) | −0.10605 (19) | 0.0357 (9) | |
C9 | 0.64853 (17) | 0.5203 (5) | 0.1397 (2) | 0.0490 (11) | |
H9 | 0.6487 | 0.5760 | 0.1083 | 0.059* | |
C10 | 0.63881 (19) | 0.5773 (5) | 0.1897 (2) | 0.0594 (13) | |
H10 | 0.6315 | 0.6684 | 0.1903 | 0.071* | |
C11 | 0.64011 (19) | 0.4991 (5) | 0.2371 (2) | 0.0594 (13) | |
H11 | 0.6336 | 0.5366 | 0.2701 | 0.071* | |
C12 | 0.65129 (16) | 0.3610 (5) | 0.2361 (2) | 0.0454 (11) | |
C13 | 0.6573 (2) | 0.2742 (5) | 0.2862 (2) | 0.0566 (13) | |
H13 | 0.6514 | 0.3077 | 0.3202 | 0.068* | |
C14 | 0.67135 (19) | 0.1438 (5) | 0.2842 (2) | 0.0544 (12) | |
H14 | 0.6751 | 0.0888 | 0.3170 | 0.065* | |
C15 | 0.68055 (15) | 0.0892 (5) | 0.23266 (18) | 0.0420 (10) | |
C16 | 0.69707 (16) | −0.0448 (5) | 0.2297 (2) | 0.0486 (11) | |
H16 | 0.7015 | −0.1029 | 0.2617 | 0.058* | |
C17 | 0.70654 (16) | −0.0889 (5) | 0.1790 (2) | 0.0474 (11) | |
H17 | 0.7178 | −0.1768 | 0.1765 | 0.057* | |
C18 | 0.69913 (15) | −0.0010 (4) | 0.1317 (2) | 0.0423 (10) | |
H18 | 0.7058 | −0.0327 | 0.0978 | 0.051* | |
C19 | 0.67424 (14) | 0.1712 (4) | 0.18226 (18) | 0.0355 (9) | |
C20 | 0.65990 (14) | 0.3125 (4) | 0.18437 (18) | 0.0364 (9) | |
C21 | 0.52649 (17) | 0.3400 (5) | 0.0298 (2) | 0.0550 (13) | |
H21 | 0.5424 | 0.4064 | 0.0585 | 0.066* | |
C22 | 0.46590 (18) | 0.3256 (5) | 0.0063 (2) | 0.0597 (14) | |
H22 | 0.4419 | 0.3809 | 0.0189 | 0.072* | |
C23 | 0.44262 (17) | 0.2268 (5) | −0.0361 (2) | 0.0554 (14) | |
H23 | 0.4024 | 0.2149 | −0.0524 | 0.066* | |
C24 | 0.47889 (15) | 0.1454 (5) | −0.0545 (2) | 0.0463 (11) | |
C25 | 0.45739 (17) | 0.0411 (5) | −0.0985 (2) | 0.0611 (14) | |
H25 | 0.4173 | 0.0278 | −0.1160 | 0.073* | |
C26 | 0.49285 (18) | −0.0363 (5) | −0.1150 (2) | 0.0596 (14) | |
H26 | 0.4772 | −0.1010 | −0.1445 | 0.072* | |
C27 | 0.55525 (16) | −0.0220 (5) | −0.08808 (19) | 0.0433 (10) | |
C28 | 0.59378 (18) | −0.1059 (5) | −0.1020 (2) | 0.0538 (13) | |
H28 | 0.5797 | −0.1740 | −0.1301 | 0.065* | |
C29 | 0.65242 (17) | −0.0878 (5) | −0.07395 (19) | 0.0456 (11) | |
H29 | 0.6790 | −0.1445 | −0.0817 | 0.055* | |
C30 | 0.67154 (15) | 0.0188 (4) | −0.03310 (18) | 0.0392 (10) | |
H30 | 0.7116 | 0.0321 | −0.0150 | 0.047* | |
C31 | 0.57785 (14) | 0.0811 (4) | −0.04579 (17) | 0.0338 (9) | |
C32 | 0.53967 (14) | 0.1670 (4) | −0.02838 (18) | 0.0366 (9) | |
C33 | 0.5000 | 0.1896 (8) | −0.2500 | 0.0489 (17) | |
N1 | 0.68306 (12) | 0.1255 (3) | 0.13182 (15) | 0.0355 (8) | |
N2 | 0.65744 (12) | 0.3913 (3) | 0.13563 (16) | 0.0384 (8) | |
N3 | 0.63681 (11) | 0.1008 (3) | −0.01866 (14) | 0.0348 (8) | |
N4 | 0.56281 (13) | 0.2633 (4) | 0.01335 (18) | 0.0434 (9) | |
O1 | 0.66798 (11) | 0.4721 (3) | −0.00036 (12) | 0.0419 (7) | |
O2 | 0.68966 (13) | 0.5899 (3) | −0.06934 (14) | 0.0556 (8) | |
O3 | 0.73884 (10) | 0.3048 (3) | −0.06008 (12) | 0.0411 (7) | |
O4 | 0.71905 (11) | 0.1556 (3) | −0.13319 (15) | 0.0578 (9) | |
O5 | 0.5000 | 0.0672 (6) | −0.2500 | 0.0717 (16) | |
O6 | 0.71087 (16) | 0.7293 (4) | 0.0615 (2) | 0.0735 (11) | |
Pd1 | 0.672614 (10) | 0.28061 (3) | 0.051225 (12) | 0.02952 (12) | |
H2W | 0.705 (2) | 0.661 (3) | 0.042 (2) | 0.080* | |
H1W | 0.689 (2) | 0.746 (5) | 0.080 (2) | 0.080* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0348 (18) | 0.039 (2) | 0.035 (2) | 0.0049 (17) | 0.0085 (15) | 0.000 (2) |
C2 | 0.0313 (17) | 0.041 (2) | 0.027 (2) | 0.0024 (16) | 0.0061 (14) | 0.0044 (19) |
C3 | 0.041 (2) | 0.065 (3) | 0.051 (3) | 0.015 (2) | 0.0039 (18) | −0.009 (3) |
C4 | 0.0332 (19) | 0.076 (4) | 0.054 (3) | 0.016 (2) | −0.0017 (18) | −0.009 (3) |
C5 | 0.0329 (18) | 0.052 (3) | 0.036 (3) | 0.0034 (18) | 0.0027 (16) | −0.001 (2) |
C6 | 0.0360 (18) | 0.040 (3) | 0.028 (2) | 0.0013 (17) | 0.0027 (15) | 0.0019 (19) |
C7 | 0.0287 (16) | 0.038 (2) | 0.026 (2) | −0.0003 (15) | 0.0066 (14) | 0.0017 (18) |
C8 | 0.0313 (18) | 0.044 (3) | 0.030 (2) | 0.0019 (16) | 0.0093 (15) | 0.004 (2) |
C9 | 0.051 (2) | 0.037 (3) | 0.060 (3) | 0.006 (2) | 0.020 (2) | 0.006 (2) |
C10 | 0.065 (3) | 0.041 (3) | 0.074 (4) | 0.005 (2) | 0.028 (3) | −0.010 (3) |
C11 | 0.062 (3) | 0.059 (3) | 0.064 (3) | 0.000 (2) | 0.031 (2) | −0.023 (3) |
C12 | 0.044 (2) | 0.053 (3) | 0.043 (3) | −0.005 (2) | 0.0210 (17) | −0.012 (2) |
C13 | 0.071 (3) | 0.070 (4) | 0.038 (3) | −0.012 (3) | 0.030 (2) | −0.010 (3) |
C14 | 0.071 (3) | 0.056 (3) | 0.040 (3) | −0.004 (2) | 0.025 (2) | 0.009 (3) |
C15 | 0.0382 (19) | 0.052 (3) | 0.034 (2) | −0.0040 (19) | 0.0118 (16) | 0.003 (2) |
C16 | 0.045 (2) | 0.051 (3) | 0.049 (3) | 0.003 (2) | 0.0149 (19) | 0.014 (2) |
C17 | 0.045 (2) | 0.041 (3) | 0.056 (3) | 0.0047 (19) | 0.0173 (19) | 0.004 (2) |
C18 | 0.0406 (19) | 0.038 (3) | 0.051 (3) | 0.0024 (18) | 0.0193 (17) | 0.001 (2) |
C19 | 0.0276 (16) | 0.046 (3) | 0.032 (2) | −0.0023 (16) | 0.0108 (14) | 0.001 (2) |
C20 | 0.0310 (17) | 0.046 (3) | 0.034 (2) | −0.0003 (16) | 0.0139 (15) | −0.004 (2) |
C21 | 0.046 (2) | 0.056 (3) | 0.061 (3) | 0.006 (2) | 0.017 (2) | −0.010 (3) |
C22 | 0.043 (2) | 0.063 (3) | 0.076 (4) | 0.017 (2) | 0.025 (2) | 0.004 (3) |
C23 | 0.0311 (19) | 0.065 (3) | 0.068 (4) | 0.004 (2) | 0.015 (2) | 0.004 (3) |
C24 | 0.0306 (18) | 0.055 (3) | 0.051 (3) | 0.0002 (19) | 0.0113 (17) | 0.006 (2) |
C25 | 0.0303 (19) | 0.074 (4) | 0.071 (3) | −0.012 (2) | 0.008 (2) | −0.009 (3) |
C26 | 0.043 (2) | 0.068 (4) | 0.061 (3) | −0.018 (2) | 0.011 (2) | −0.023 (3) |
C27 | 0.042 (2) | 0.050 (3) | 0.039 (2) | −0.0088 (19) | 0.0148 (17) | −0.004 (2) |
C28 | 0.051 (2) | 0.063 (3) | 0.046 (3) | −0.006 (2) | 0.0155 (19) | −0.017 (3) |
C29 | 0.047 (2) | 0.050 (3) | 0.042 (3) | 0.003 (2) | 0.0180 (18) | −0.007 (2) |
C30 | 0.0332 (17) | 0.048 (3) | 0.036 (2) | 0.0047 (17) | 0.0121 (15) | 0.000 (2) |
C31 | 0.0310 (17) | 0.039 (2) | 0.029 (2) | −0.0028 (16) | 0.0084 (14) | 0.0035 (19) |
C32 | 0.0293 (17) | 0.042 (2) | 0.037 (2) | −0.0041 (17) | 0.0104 (15) | 0.005 (2) |
C33 | 0.033 (3) | 0.058 (5) | 0.045 (4) | 0.000 | 0.002 (2) | 0.000 |
N1 | 0.0354 (15) | 0.039 (2) | 0.0353 (19) | 0.0023 (14) | 0.0164 (13) | 0.0034 (16) |
N2 | 0.0363 (15) | 0.037 (2) | 0.043 (2) | 0.0006 (14) | 0.0147 (13) | 0.0009 (18) |
N3 | 0.0266 (13) | 0.042 (2) | 0.0331 (18) | −0.0027 (13) | 0.0077 (12) | −0.0015 (16) |
N4 | 0.0342 (16) | 0.048 (2) | 0.049 (2) | 0.0040 (15) | 0.0161 (15) | −0.0023 (19) |
O1 | 0.0530 (15) | 0.0407 (18) | 0.0297 (16) | 0.0017 (13) | 0.0119 (11) | −0.0015 (14) |
O2 | 0.0666 (18) | 0.0462 (19) | 0.053 (2) | −0.0146 (16) | 0.0201 (15) | 0.0032 (17) |
O3 | 0.0272 (12) | 0.059 (2) | 0.0339 (16) | −0.0001 (12) | 0.0073 (10) | −0.0051 (14) |
O4 | 0.0384 (14) | 0.064 (2) | 0.068 (2) | 0.0075 (15) | 0.0145 (14) | −0.021 (2) |
O5 | 0.058 (3) | 0.066 (4) | 0.067 (4) | 0.000 | −0.006 (2) | 0.000 |
O6 | 0.076 (2) | 0.074 (3) | 0.079 (3) | −0.004 (2) | 0.039 (2) | −0.033 (2) |
Pd1 | 0.02651 (15) | 0.0337 (2) | 0.02745 (19) | 0.00278 (11) | 0.00847 (10) | 0.00078 (13) |
C1—O2 | 1.230 (5) | C19—C20 | 1.461 (6) |
C1—O1 | 1.288 (5) | C20—N2 | 1.383 (5) |
C1—C2 | 1.522 (5) | C21—N4 | 1.334 (6) |
C2—C3 | 1.381 (5) | C21—C22 | 1.395 (6) |
C2—C7 | 1.407 (5) | C21—H21 | 0.9300 |
C3—C4 | 1.393 (6) | C22—C23 | 1.381 (7) |
C3—H3 | 0.9300 | C22—H22 | 0.9300 |
C4—C5 | 1.366 (6) | C23—C24 | 1.384 (6) |
C4—H4 | 0.9300 | C23—H23 | 0.9300 |
C5—C6 | 1.394 (5) | C24—C32 | 1.411 (5) |
C5—C33 | 1.496 (5) | C24—C25 | 1.437 (7) |
C6—C7 | 1.386 (5) | C25—C26 | 1.322 (7) |
C6—H6 | 0.9300 | C25—H25 | 0.9300 |
C7—C8 | 1.506 (5) | C26—C27 | 1.439 (5) |
C8—O4 | 1.243 (5) | C26—H26 | 0.9300 |
C8—O3 | 1.252 (5) | C27—C28 | 1.387 (6) |
C9—N2 | 1.318 (5) | C27—C31 | 1.408 (6) |
C9—C10 | 1.410 (7) | C28—C29 | 1.363 (6) |
C9—H9 | 0.9300 | C28—H28 | 0.9300 |
C10—C11 | 1.361 (7) | C29—C30 | 1.404 (6) |
C10—H10 | 0.9300 | C29—H29 | 0.9300 |
C11—C12 | 1.410 (7) | C30—N3 | 1.312 (5) |
C11—H11 | 0.9300 | C30—H30 | 0.9300 |
C12—C20 | 1.404 (6) | C31—N3 | 1.370 (4) |
C12—C13 | 1.436 (7) | C31—C32 | 1.434 (6) |
C13—C14 | 1.354 (7) | C32—N4 | 1.353 (6) |
C13—H13 | 0.9300 | C33—O5 | 1.224 (8) |
C14—C15 | 1.428 (6) | C33—C5i | 1.496 (5) |
C14—H14 | 0.9300 | N1—Pd1 | 2.404 (3) |
C15—C16 | 1.409 (6) | N2—Pd1 | 2.428 (4) |
C15—C19 | 1.412 (6) | N3—Pd1 | 2.391 (3) |
C16—C17 | 1.375 (6) | N4—Pd1 | 2.520 (3) |
C16—H16 | 0.9300 | O1—Pd1 | 2.253 (3) |
C17—C18 | 1.386 (6) | O3—Pd1ii | 2.270 (2) |
C17—H17 | 0.9300 | O6—H2W | 0.81 (3) |
C18—N1 | 1.326 (5) | O6—H1W | 0.82 (5) |
C18—H18 | 0.9300 | Pd1—O3ii | 2.270 (2) |
C19—N1 | 1.367 (5) | ||
O2—C1—O1 | 124.4 (4) | C21—C22—H22 | 121.0 |
O2—C1—C2 | 117.2 (4) | C22—C23—C24 | 120.3 (4) |
O1—C1—C2 | 118.0 (4) | C22—C23—H23 | 119.8 |
C3—C2—C7 | 118.0 (4) | C24—C23—H23 | 119.8 |
C3—C2—C1 | 116.4 (4) | C23—C24—C32 | 117.8 (4) |
C7—C2—C1 | 125.6 (3) | C23—C24—C25 | 123.0 (4) |
C2—C3—C4 | 121.2 (4) | C32—C24—C25 | 119.2 (4) |
C2—C3—H3 | 119.4 | C26—C25—C24 | 122.0 (4) |
C4—C3—H3 | 119.4 | C26—C25—H25 | 119.0 |
C5—C4—C3 | 120.9 (4) | C24—C25—H25 | 119.0 |
C5—C4—H4 | 119.5 | C25—C26—C27 | 121.1 (4) |
C3—C4—H4 | 119.5 | C25—C26—H26 | 119.5 |
C4—C5—C6 | 118.8 (4) | C27—C26—H26 | 119.5 |
C4—C5—C33 | 121.1 (4) | C28—C27—C31 | 118.9 (3) |
C6—C5—C33 | 120.1 (4) | C28—C27—C26 | 122.6 (4) |
C7—C6—C5 | 120.9 (4) | C31—C27—C26 | 118.4 (4) |
C7—C6—H6 | 119.6 | C29—C28—C27 | 119.5 (4) |
C5—C6—H6 | 119.6 | C29—C28—H28 | 120.3 |
C6—C7—C2 | 120.2 (3) | C27—C28—H28 | 120.3 |
C6—C7—C8 | 119.2 (4) | C28—C29—C30 | 118.2 (4) |
C2—C7—C8 | 120.5 (3) | C28—C29—H29 | 120.9 |
O4—C8—O3 | 124.4 (3) | C30—C29—H29 | 120.9 |
O4—C8—C7 | 118.5 (3) | N3—C30—C29 | 124.5 (3) |
O3—C8—C7 | 117.1 (4) | N3—C30—H30 | 117.7 |
N2—C9—C10 | 122.6 (5) | C29—C30—H30 | 117.7 |
N2—C9—H9 | 118.7 | N3—C31—C27 | 121.5 (4) |
C10—C9—H9 | 118.7 | N3—C31—C32 | 117.7 (3) |
C11—C10—C9 | 120.1 (5) | C27—C31—C32 | 120.8 (3) |
C11—C10—H10 | 120.0 | N4—C32—C24 | 122.2 (4) |
C9—C10—H10 | 120.0 | N4—C32—C31 | 119.4 (3) |
C10—C11—C12 | 119.8 (5) | C24—C32—C31 | 118.4 (4) |
C10—C11—H11 | 120.1 | O5—C33—C5 | 121.0 (3) |
C12—C11—H11 | 120.1 | O5—C33—C5i | 121.0 (3) |
C20—C12—C11 | 116.3 (4) | C5—C33—C5i | 118.1 (6) |
C20—C12—C13 | 120.7 (4) | C18—N1—C19 | 117.4 (4) |
C11—C12—C13 | 122.8 (5) | C18—N1—Pd1 | 124.2 (3) |
C14—C13—C12 | 120.4 (4) | C19—N1—Pd1 | 118.3 (3) |
C14—C13—H13 | 119.8 | C9—N2—C20 | 117.2 (4) |
C12—C13—H13 | 119.8 | C9—N2—Pd1 | 125.8 (3) |
C13—C14—C15 | 121.2 (4) | C20—N2—Pd1 | 117.1 (3) |
C13—C14—H14 | 119.4 | C30—N3—C31 | 117.4 (3) |
C15—C14—H14 | 119.4 | C30—N3—Pd1 | 122.6 (2) |
C16—C15—C19 | 117.3 (4) | C31—N3—Pd1 | 120.0 (3) |
C16—C15—C14 | 122.8 (4) | C21—N4—C32 | 118.3 (3) |
C19—C15—C14 | 119.9 (4) | C21—N4—Pd1 | 126.4 (3) |
C17—C16—C15 | 119.2 (4) | C32—N4—Pd1 | 115.2 (3) |
C17—C16—H16 | 120.4 | C1—O1—Pd1 | 132.1 (3) |
C15—C16—H16 | 120.4 | C8—O3—Pd1ii | 103.2 (2) |
C16—C17—C18 | 119.4 (4) | H2W—O6—H1W | 117 (3) |
C16—C17—H17 | 120.3 | O1—Pd1—O3ii | 103.45 (10) |
C18—C17—H17 | 120.3 | O1—Pd1—N3 | 109.11 (11) |
N1—C18—C17 | 123.8 (4) | O3ii—Pd1—N3 | 83.34 (10) |
N1—C18—H18 | 118.1 | O1—Pd1—N1 | 161.94 (11) |
C17—C18—H18 | 118.1 | O3ii—Pd1—N1 | 81.65 (10) |
N1—C19—C15 | 122.8 (4) | N3—Pd1—N1 | 88.57 (12) |
N1—C19—C20 | 117.9 (4) | O1—Pd1—N2 | 93.84 (11) |
C15—C19—C20 | 119.2 (4) | O3ii—Pd1—N2 | 121.06 (10) |
N2—C20—C12 | 123.9 (4) | N3—Pd1—N2 | 142.04 (11) |
N2—C20—C19 | 117.5 (4) | N1—Pd1—N2 | 69.10 (12) |
C12—C20—C19 | 118.5 (4) | O1—Pd1—N4 | 91.32 (11) |
N4—C21—C22 | 123.3 (5) | O3ii—Pd1—N4 | 150.49 (11) |
N4—C21—H21 | 118.4 | N3—Pd1—N4 | 67.60 (11) |
C22—C21—H21 | 118.4 | N1—Pd1—N4 | 92.18 (11) |
C23—C22—C21 | 118.1 (5) | N2—Pd1—N4 | 82.48 (11) |
C23—C22—H22 | 121.0 |
Symmetry codes: (i) −x+1, y, −z−1/2; (ii) −x+3/2, −y+1/2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H2W···O1 | 0.81 (3) | 2.18 (4) | 2.964 (5) | 163 (4) |
Experimental details
Crystal data | |
Chemical formula | [Pd2(C17H6O9)(C12H8N2)4]·2H2O |
Mr | 1323.91 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 273 |
a, b, c (Å) | 24.483 (2), 10.0027 (10), 23.7133 (15) |
β (°) | 110.786 (2) |
V (Å3) | 5429.4 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.74 |
Crystal size (mm) | 0.12 × 0.10 × 0.08 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.917, 0.943 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 21160, 4924, 3659 |
Rint | 0.042 |
(sin θ/λ)max (Å−1) | 0.606 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.114, 1.00 |
No. of reflections | 4924 |
No. of parameters | 395 |
No. of restraints | 4 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.46, −1.86 |
Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SAINT-Plus, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H2W···O1 | 0.81 (3) | 2.18 (4) | 2.964 (5) | 163 (4) |
As shown on Fig. 1, the palladium 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 ligand, exhibiting a distorted octahedral geometry. Each two Pd atoms form one circle via four carboxylate group belonging two of 3,3',4,4'-benzophenone tetracarboxylate, which are further linked to form one dimensional chain (Fig.2). Interestinfly, the benzophenone carbonyl group (C33?O5) lies on a twofold rotation axis. Moreover, the hydrogen bonds link the chains into a three-dimensional structure (Fig. 3).