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The title compound, {[Pd2(C17H6O9)(C12H8N2)4]·2H2O}n, was prepared by hydro­thermal synthesis and is isostructural with its Cd2+-containing analogue. A twofold rotation axis passes through the carbonyl group of the benzophenone unit. In the asymmetric unit, the Pd atom exhibts a distorted octa­hedral geometry, consisting of two carboxyl­ate O atoms from two 4,4′-carbonyl­bis(benzene-3,4-dicarboxyl­ate) anions and four N atoms from two 1,10-phenanthroline ligands. The Pd—N and Pd—O bond lengths are in the ranges 2.391 (3)–2.520 (3) and 2.270 (2)–2.523 (3) Å, respectively. Two neighboring Pd atoms are bridged by 4,4′-carbonyl­bis(benzene-3,4-dicarboxyl­ate) anions, forming a dinuclear complex, which is further bridged by 4,4′-carbonyl­bis(benzene-3,4-dicarboxyl­ate) anions to form an infinite chain. Hydrogen bonds link the chains into a three-dimensional structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807039050/rk2033sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807039050/rk2033Isup2.hkl
Contains datablock I

CCDC reference: 1101493

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.047
  • wR factor = 0.114
  • Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O6 - H1W ... ?
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT415_ALERT_2_C Short Inter D-H..H-X H1W .. H23 .. 2.13 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 Pd1 (2) 1.26 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 1 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 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

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).

Related literature top

For the isostructural Cd2+ analogue, see: Gao et al. (2007).

Experimental top

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%.

Refinement top

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.

Structure description top

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).

Computing details top

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.

Figures top
[Figure 1] Fig. 1. The coordination of the Pd atom in the title structure, drawn with 30% probability displacement ellipsoids. Atom O3_I has the symmetry positions: (-x + 1, y, -z - 1/2).
[Figure 2] Fig. 2. A view of the chain structure of the title compound.
[Figure 3] Fig. 3. A view of the packing structure of the title compound.
Poly[[[µ4-4,4'-carbonylbis(benzene-3,4-dicarboxylato)]tetrakis(1,10-πhenanthroline)dipalladium(II)] dihydrate] top
Crystal data top
[Pd2(C17H6O9)(C12H8N2)4]·2H2OF(000) = 2672
Mr = 1323.91Dx = 1.620 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 4924 reflections
a = 24.483 (2) Åθ = 1.8–25.5°
b = 10.0027 (10) ŵ = 0.74 mm1
c = 23.7133 (15) ÅT = 273 K
β = 110.786 (2)°Block, colourless
V = 5429.4 (8) Å30.12 × 0.10 × 0.08 mm
Z = 4
Data collection top
Bruker APEXII CCD area-detector
diffractometer
4924 independent reflections
Radiation source: fine-focus sealed tube3659 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
φ and ω scansθmax = 25.5°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 2929
Tmin = 0.917, Tmax = 0.943k = 1212
21160 measured reflectionsl = 2828
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.114H 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 parametersΔρmax = 1.46 e Å3
4 restraintsΔρmin = 1.86 e Å3
Crystal data top
[Pd2(C17H6O9)(C12H8N2)4]·2H2OV = 5429.4 (8) Å3
Mr = 1323.91Z = 4
Monoclinic, C2/cMo Kα radiation
a = 24.483 (2) ŵ = 0.74 mm1
b = 10.0027 (10) ÅT = 273 K
c = 23.7133 (15) Å0.12 × 0.10 × 0.08 mm
β = 110.786 (2)°
Data collection top
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 = 0.943Rint = 0.042
21160 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0474 restraints
wR(F2) = 0.114H atoms treated by a mixture of independent and constrained refinement
S = 1.00Δρmax = 1.46 e Å3
4924 reflectionsΔρmin = 1.86 e Å3
395 parameters
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 > 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.66566 (15)0.4950 (4)0.05461 (18)0.0373 (10)
C20.62534 (14)0.4085 (4)0.10507 (17)0.0343 (9)
C30.56800 (16)0.4503 (5)0.1303 (2)0.0555 (13)
H30.55610.52660.11540.067*
C40.52765 (16)0.3801 (5)0.1776 (2)0.0590 (14)
H40.48940.41100.19420.071*
C50.54343 (16)0.2665 (5)0.1999 (2)0.0430 (11)
C60.60110 (15)0.2225 (4)0.17500 (19)0.0370 (10)
H60.61220.14470.18950.044*
C70.64201 (14)0.2932 (4)0.12896 (17)0.0319 (9)
C80.70470 (15)0.2476 (4)0.10605 (19)0.0357 (9)
C90.64853 (17)0.5203 (5)0.1397 (2)0.0490 (11)
H90.64870.57600.10830.059*
C100.63881 (19)0.5773 (5)0.1897 (2)0.0594 (13)
H100.63150.66840.19030.071*
C110.64011 (19)0.4991 (5)0.2371 (2)0.0594 (13)
H110.63360.53660.27010.071*
C120.65129 (16)0.3610 (5)0.2361 (2)0.0454 (11)
C130.6573 (2)0.2742 (5)0.2862 (2)0.0566 (13)
H130.65140.30770.32020.068*
C140.67135 (19)0.1438 (5)0.2842 (2)0.0544 (12)
H140.67510.08880.31700.065*
C150.68055 (15)0.0892 (5)0.23266 (18)0.0420 (10)
C160.69707 (16)0.0448 (5)0.2297 (2)0.0486 (11)
H160.70150.10290.26170.058*
C170.70654 (16)0.0889 (5)0.1790 (2)0.0474 (11)
H170.71780.17680.17650.057*
C180.69913 (15)0.0010 (4)0.1317 (2)0.0423 (10)
H180.70580.03270.09780.051*
C190.67424 (14)0.1712 (4)0.18226 (18)0.0355 (9)
C200.65990 (14)0.3125 (4)0.18437 (18)0.0364 (9)
C210.52649 (17)0.3400 (5)0.0298 (2)0.0550 (13)
H210.54240.40640.05850.066*
C220.46590 (18)0.3256 (5)0.0063 (2)0.0597 (14)
H220.44190.38090.01890.072*
C230.44262 (17)0.2268 (5)0.0361 (2)0.0554 (14)
H230.40240.21490.05240.066*
C240.47889 (15)0.1454 (5)0.0545 (2)0.0463 (11)
C250.45739 (17)0.0411 (5)0.0985 (2)0.0611 (14)
H250.41730.02780.11600.073*
C260.49285 (18)0.0363 (5)0.1150 (2)0.0596 (14)
H260.47720.10100.14450.072*
C270.55525 (16)0.0220 (5)0.08808 (19)0.0433 (10)
C280.59378 (18)0.1059 (5)0.1020 (2)0.0538 (13)
H280.57970.17400.13010.065*
C290.65242 (17)0.0878 (5)0.07395 (19)0.0456 (11)
H290.67900.14450.08170.055*
C300.67154 (15)0.0188 (4)0.03310 (18)0.0392 (10)
H300.71160.03210.01500.047*
C310.57785 (14)0.0811 (4)0.04579 (17)0.0338 (9)
C320.53967 (14)0.1670 (4)0.02838 (18)0.0366 (9)
C330.50000.1896 (8)0.25000.0489 (17)
N10.68306 (12)0.1255 (3)0.13182 (15)0.0355 (8)
N20.65744 (12)0.3913 (3)0.13563 (16)0.0384 (8)
N30.63681 (11)0.1008 (3)0.01866 (14)0.0348 (8)
N40.56281 (13)0.2633 (4)0.01335 (18)0.0434 (9)
O10.66798 (11)0.4721 (3)0.00036 (12)0.0419 (7)
O20.68966 (13)0.5899 (3)0.06934 (14)0.0556 (8)
O30.73884 (10)0.3048 (3)0.06008 (12)0.0411 (7)
O40.71905 (11)0.1556 (3)0.13319 (15)0.0578 (9)
O50.50000.0672 (6)0.25000.0717 (16)
O60.71087 (16)0.7293 (4)0.0615 (2)0.0735 (11)
Pd10.672614 (10)0.28061 (3)0.051225 (12)0.02952 (12)
H2W0.705 (2)0.661 (3)0.042 (2)0.080*
H1W0.689 (2)0.746 (5)0.080 (2)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0348 (18)0.039 (2)0.035 (2)0.0049 (17)0.0085 (15)0.000 (2)
C20.0313 (17)0.041 (2)0.027 (2)0.0024 (16)0.0061 (14)0.0044 (19)
C30.041 (2)0.065 (3)0.051 (3)0.015 (2)0.0039 (18)0.009 (3)
C40.0332 (19)0.076 (4)0.054 (3)0.016 (2)0.0017 (18)0.009 (3)
C50.0329 (18)0.052 (3)0.036 (3)0.0034 (18)0.0027 (16)0.001 (2)
C60.0360 (18)0.040 (3)0.028 (2)0.0013 (17)0.0027 (15)0.0019 (19)
C70.0287 (16)0.038 (2)0.026 (2)0.0003 (15)0.0066 (14)0.0017 (18)
C80.0313 (18)0.044 (3)0.030 (2)0.0019 (16)0.0093 (15)0.004 (2)
C90.051 (2)0.037 (3)0.060 (3)0.006 (2)0.020 (2)0.006 (2)
C100.065 (3)0.041 (3)0.074 (4)0.005 (2)0.028 (3)0.010 (3)
C110.062 (3)0.059 (3)0.064 (3)0.000 (2)0.031 (2)0.023 (3)
C120.044 (2)0.053 (3)0.043 (3)0.005 (2)0.0210 (17)0.012 (2)
C130.071 (3)0.070 (4)0.038 (3)0.012 (3)0.030 (2)0.010 (3)
C140.071 (3)0.056 (3)0.040 (3)0.004 (2)0.025 (2)0.009 (3)
C150.0382 (19)0.052 (3)0.034 (2)0.0040 (19)0.0118 (16)0.003 (2)
C160.045 (2)0.051 (3)0.049 (3)0.003 (2)0.0149 (19)0.014 (2)
C170.045 (2)0.041 (3)0.056 (3)0.0047 (19)0.0173 (19)0.004 (2)
C180.0406 (19)0.038 (3)0.051 (3)0.0024 (18)0.0193 (17)0.001 (2)
C190.0276 (16)0.046 (3)0.032 (2)0.0023 (16)0.0108 (14)0.001 (2)
C200.0310 (17)0.046 (3)0.034 (2)0.0003 (16)0.0139 (15)0.004 (2)
C210.046 (2)0.056 (3)0.061 (3)0.006 (2)0.017 (2)0.010 (3)
C220.043 (2)0.063 (3)0.076 (4)0.017 (2)0.025 (2)0.004 (3)
C230.0311 (19)0.065 (3)0.068 (4)0.004 (2)0.015 (2)0.004 (3)
C240.0306 (18)0.055 (3)0.051 (3)0.0002 (19)0.0113 (17)0.006 (2)
C250.0303 (19)0.074 (4)0.071 (3)0.012 (2)0.008 (2)0.009 (3)
C260.043 (2)0.068 (4)0.061 (3)0.018 (2)0.011 (2)0.023 (3)
C270.042 (2)0.050 (3)0.039 (2)0.0088 (19)0.0148 (17)0.004 (2)
C280.051 (2)0.063 (3)0.046 (3)0.006 (2)0.0155 (19)0.017 (3)
C290.047 (2)0.050 (3)0.042 (3)0.003 (2)0.0180 (18)0.007 (2)
C300.0332 (17)0.048 (3)0.036 (2)0.0047 (17)0.0121 (15)0.000 (2)
C310.0310 (17)0.039 (2)0.029 (2)0.0028 (16)0.0084 (14)0.0035 (19)
C320.0293 (17)0.042 (2)0.037 (2)0.0041 (17)0.0104 (15)0.005 (2)
C330.033 (3)0.058 (5)0.045 (4)0.0000.002 (2)0.000
N10.0354 (15)0.039 (2)0.0353 (19)0.0023 (14)0.0164 (13)0.0034 (16)
N20.0363 (15)0.037 (2)0.043 (2)0.0006 (14)0.0147 (13)0.0009 (18)
N30.0266 (13)0.042 (2)0.0331 (18)0.0027 (13)0.0077 (12)0.0015 (16)
N40.0342 (16)0.048 (2)0.049 (2)0.0040 (15)0.0161 (15)0.0023 (19)
O10.0530 (15)0.0407 (18)0.0297 (16)0.0017 (13)0.0119 (11)0.0015 (14)
O20.0666 (18)0.0462 (19)0.053 (2)0.0146 (16)0.0201 (15)0.0032 (17)
O30.0272 (12)0.059 (2)0.0339 (16)0.0001 (12)0.0073 (10)0.0051 (14)
O40.0384 (14)0.064 (2)0.068 (2)0.0075 (15)0.0145 (14)0.021 (2)
O50.058 (3)0.066 (4)0.067 (4)0.0000.006 (2)0.000
O60.076 (2)0.074 (3)0.079 (3)0.004 (2)0.039 (2)0.033 (2)
Pd10.02651 (15)0.0337 (2)0.02745 (19)0.00278 (11)0.00847 (10)0.00078 (13)
Geometric parameters (Å, º) top
C1—O21.230 (5)C19—C201.461 (6)
C1—O11.288 (5)C20—N21.383 (5)
C1—C21.522 (5)C21—N41.334 (6)
C2—C31.381 (5)C21—C221.395 (6)
C2—C71.407 (5)C21—H210.9300
C3—C41.393 (6)C22—C231.381 (7)
C3—H30.9300C22—H220.9300
C4—C51.366 (6)C23—C241.384 (6)
C4—H40.9300C23—H230.9300
C5—C61.394 (5)C24—C321.411 (5)
C5—C331.496 (5)C24—C251.437 (7)
C6—C71.386 (5)C25—C261.322 (7)
C6—H60.9300C25—H250.9300
C7—C81.506 (5)C26—C271.439 (5)
C8—O41.243 (5)C26—H260.9300
C8—O31.252 (5)C27—C281.387 (6)
C9—N21.318 (5)C27—C311.408 (6)
C9—C101.410 (7)C28—C291.363 (6)
C9—H90.9300C28—H280.9300
C10—C111.361 (7)C29—C301.404 (6)
C10—H100.9300C29—H290.9300
C11—C121.410 (7)C30—N31.312 (5)
C11—H110.9300C30—H300.9300
C12—C201.404 (6)C31—N31.370 (4)
C12—C131.436 (7)C31—C321.434 (6)
C13—C141.354 (7)C32—N41.353 (6)
C13—H130.9300C33—O51.224 (8)
C14—C151.428 (6)C33—C5i1.496 (5)
C14—H140.9300N1—Pd12.404 (3)
C15—C161.409 (6)N2—Pd12.428 (4)
C15—C191.412 (6)N3—Pd12.391 (3)
C16—C171.375 (6)N4—Pd12.520 (3)
C16—H160.9300O1—Pd12.253 (3)
C17—C181.386 (6)O3—Pd1ii2.270 (2)
C17—H170.9300O6—H2W0.81 (3)
C18—N11.326 (5)O6—H1W0.82 (5)
C18—H180.9300Pd1—O3ii2.270 (2)
C19—N11.367 (5)
O2—C1—O1124.4 (4)C21—C22—H22121.0
O2—C1—C2117.2 (4)C22—C23—C24120.3 (4)
O1—C1—C2118.0 (4)C22—C23—H23119.8
C3—C2—C7118.0 (4)C24—C23—H23119.8
C3—C2—C1116.4 (4)C23—C24—C32117.8 (4)
C7—C2—C1125.6 (3)C23—C24—C25123.0 (4)
C2—C3—C4121.2 (4)C32—C24—C25119.2 (4)
C2—C3—H3119.4C26—C25—C24122.0 (4)
C4—C3—H3119.4C26—C25—H25119.0
C5—C4—C3120.9 (4)C24—C25—H25119.0
C5—C4—H4119.5C25—C26—C27121.1 (4)
C3—C4—H4119.5C25—C26—H26119.5
C4—C5—C6118.8 (4)C27—C26—H26119.5
C4—C5—C33121.1 (4)C28—C27—C31118.9 (3)
C6—C5—C33120.1 (4)C28—C27—C26122.6 (4)
C7—C6—C5120.9 (4)C31—C27—C26118.4 (4)
C7—C6—H6119.6C29—C28—C27119.5 (4)
C5—C6—H6119.6C29—C28—H28120.3
C6—C7—C2120.2 (3)C27—C28—H28120.3
C6—C7—C8119.2 (4)C28—C29—C30118.2 (4)
C2—C7—C8120.5 (3)C28—C29—H29120.9
O4—C8—O3124.4 (3)C30—C29—H29120.9
O4—C8—C7118.5 (3)N3—C30—C29124.5 (3)
O3—C8—C7117.1 (4)N3—C30—H30117.7
N2—C9—C10122.6 (5)C29—C30—H30117.7
N2—C9—H9118.7N3—C31—C27121.5 (4)
C10—C9—H9118.7N3—C31—C32117.7 (3)
C11—C10—C9120.1 (5)C27—C31—C32120.8 (3)
C11—C10—H10120.0N4—C32—C24122.2 (4)
C9—C10—H10120.0N4—C32—C31119.4 (3)
C10—C11—C12119.8 (5)C24—C32—C31118.4 (4)
C10—C11—H11120.1O5—C33—C5121.0 (3)
C12—C11—H11120.1O5—C33—C5i121.0 (3)
C20—C12—C11116.3 (4)C5—C33—C5i118.1 (6)
C20—C12—C13120.7 (4)C18—N1—C19117.4 (4)
C11—C12—C13122.8 (5)C18—N1—Pd1124.2 (3)
C14—C13—C12120.4 (4)C19—N1—Pd1118.3 (3)
C14—C13—H13119.8C9—N2—C20117.2 (4)
C12—C13—H13119.8C9—N2—Pd1125.8 (3)
C13—C14—C15121.2 (4)C20—N2—Pd1117.1 (3)
C13—C14—H14119.4C30—N3—C31117.4 (3)
C15—C14—H14119.4C30—N3—Pd1122.6 (2)
C16—C15—C19117.3 (4)C31—N3—Pd1120.0 (3)
C16—C15—C14122.8 (4)C21—N4—C32118.3 (3)
C19—C15—C14119.9 (4)C21—N4—Pd1126.4 (3)
C17—C16—C15119.2 (4)C32—N4—Pd1115.2 (3)
C17—C16—H16120.4C1—O1—Pd1132.1 (3)
C15—C16—H16120.4C8—O3—Pd1ii103.2 (2)
C16—C17—C18119.4 (4)H2W—O6—H1W117 (3)
C16—C17—H17120.3O1—Pd1—O3ii103.45 (10)
C18—C17—H17120.3O1—Pd1—N3109.11 (11)
N1—C18—C17123.8 (4)O3ii—Pd1—N383.34 (10)
N1—C18—H18118.1O1—Pd1—N1161.94 (11)
C17—C18—H18118.1O3ii—Pd1—N181.65 (10)
N1—C19—C15122.8 (4)N3—Pd1—N188.57 (12)
N1—C19—C20117.9 (4)O1—Pd1—N293.84 (11)
C15—C19—C20119.2 (4)O3ii—Pd1—N2121.06 (10)
N2—C20—C12123.9 (4)N3—Pd1—N2142.04 (11)
N2—C20—C19117.5 (4)N1—Pd1—N269.10 (12)
C12—C20—C19118.5 (4)O1—Pd1—N491.32 (11)
N4—C21—C22123.3 (5)O3ii—Pd1—N4150.49 (11)
N4—C21—H21118.4N3—Pd1—N467.60 (11)
C22—C21—H21118.4N1—Pd1—N492.18 (11)
C23—C22—C21118.1 (5)N2—Pd1—N482.48 (11)
C23—C22—H22121.0
Symmetry codes: (i) x+1, y, z1/2; (ii) x+3/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H2W···O10.81 (3)2.18 (4)2.964 (5)163 (4)

Experimental details

Crystal data
Chemical formula[Pd2(C17H6O9)(C12H8N2)4]·2H2O
Mr1323.91
Crystal system, space groupMonoclinic, C2/c
Temperature (K)273
a, b, c (Å)24.483 (2), 10.0027 (10), 23.7133 (15)
β (°) 110.786 (2)
V3)5429.4 (8)
Z4
Radiation typeMo Kα
µ (mm1)0.74
Crystal size (mm)0.12 × 0.10 × 0.08
Data collection
DiffractometerBruker APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.917, 0.943
No. of measured, independent and
observed [I > 2σ(I)] reflections
21160, 4924, 3659
Rint0.042
(sin θ/λ)max1)0.606
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.114, 1.00
No. of reflections4924
No. of parameters395
No. of restraints4
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)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.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H2W···O10.81 (3)2.18 (4)2.964 (5)163 (4)
 

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