Literature DB >> 21200490

catena-Poly[[bis-(1H-benzimidazole-κN)palladium(II)]-μ-benzene-1,4-dicarboxyl-ato-κO:O].

Qingguo Meng1, Lintong Wang, Yanzhen Liu, Yan Pang.   

Abstract

In the title compound, [Pd(C(8)H(4)O(4))(C(7)H(6)N(2))(2)](n), the Pd atom is tetra-coordinated by two carboxyl-ate O atoms from two benzene-1,4-dicarboxyl-ate (bdc) dianions and two N atoms from two benzimidazole ligands, resulting in a slightly distorted tetra-hedral PdO(2)N(2) geometry. The bdc ligand acts as a bridge, linking the Pd atoms into a chain. Inter-chain N-H⋯O hydrogen bonds help to stabilize the crystal structure.

Entities:  

Year:  2007        PMID： 21200490      PMCID： PMC2915081          DOI： 10.1107/S1600536807065051

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For background, see: Okabe & Oya (2000 ▶).

Experimental

Crystal data

[Pd(C8H4O4)(C7H6N2)2] M = 506.79 Monoclinic, a = 17.0627 (5) Å b = 7.3612 (10) Å c = 18.0210 (5) Å β = 114.362 (3)° V = 2061.9 (3) Å3 Z = 4 Mo Kα radiation μ = 0.94 mm−1 T = 273 (2) K 0.43 × 0.28 × 0.22 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.689, T max = 0.820 10244 measured reflections 3763 independent reflections 3136 reflections with I > 2σ(I) R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.021 wR(F 2) = 0.044 S = 1.00 3763 reflections 280 parameters H-atom parameters constrained Δρmax = 0.25 e Å−3 Δρmin = −0.30 e Å−3 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. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807065051/hb2670sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807065051/hb2670Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pd(C8H4O4)(C7H6N2)2]F000 = 1016
Mr = 506.79Dx = 1.633 Mg m−3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 3823 reflections
a = 17.0627 (5) Åθ = 2.5–25.5º
b = 7.3612 (10) ŵ = 0.94 mm−1
c = 18.0210 (5) ÅT = 273 (2) K
β = 114.362 (3)ºBlock, colourless
V = 2061.9 (3) Å30.43 × 0.28 × 0.22 mm
Z = 4
Bruker APEXII CCD diffractometer3763 independent reflections
Radiation source: fine-focus sealed tube3136 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.021
T = 273(2) Kθmax = 25.5º
φ and ω scansθmin = 2.5º
Absorption correction: multi-scan(SADABS; Bruker, 2001)h = −20→18
Tmin = 0.689, Tmax = 0.820k = −8→8
10244 measured reflectionsl = −16→21
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021H-atom parameters constrained
wR(F2) = 0.044  w = 1/[σ2(Fo2) + (0.0204P)2 + 0.1114P] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.007
3763 reflectionsΔρmax = 0.25 e Å−3
280 parametersΔρmin = −0.30 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
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.
xyzUiso*/Ueq
Pd10.386453 (9)0.87505 (2)0.131047 (8)0.03602 (6)
C10.38692 (14)0.4922 (3)0.05522 (12)0.0501 (5)
H10.32730.50280.03200.060*
C20.51274 (14)0.3771 (3)0.08708 (12)0.0465 (5)
C30.51865 (12)0.5488 (3)0.12239 (11)0.0414 (5)
C40.58302 (16)0.2724 (3)0.09742 (14)0.0600 (6)
H40.57810.15950.07270.072*
C50.59695 (13)0.6213 (3)0.17173 (13)0.0514 (5)
H50.60210.73480.19590.062*
C60.66649 (15)0.5167 (4)0.18295 (14)0.0642 (6)
H60.72080.56010.21640.077*
C70.65997 (17)0.3453 (4)0.14617 (15)0.0677 (7)
H70.71000.28030.15560.081*
C80.23606 (14)0.7875 (3)0.18459 (14)0.0558 (6)
H80.19700.78110.13030.067*
C90.35186 (13)0.8107 (3)0.29148 (12)0.0442 (5)
C100.28633 (14)0.7875 (3)0.31634 (13)0.0498 (5)
C110.30073 (17)0.7824 (4)0.39652 (15)0.0698 (7)
H110.25590.76680.41260.084*
C120.43443 (14)0.8292 (3)0.34715 (13)0.0549 (6)
H120.47930.84570.33120.066*
C130.44869 (17)0.8227 (4)0.42700 (15)0.0749 (8)
H130.50470.83340.46650.090*
C140.3826 (2)0.8007 (4)0.45121 (16)0.0843 (8)
H140.39480.79850.50650.101*
C150.49046 (12)1.1428 (3)0.23451 (11)0.0402 (5)
C160.56002 (11)1.2527 (3)0.29649 (11)0.0381 (4)
C170.64130 (13)1.1842 (3)0.32852 (12)0.0508 (5)
H170.65281.07300.31070.061*
C180.54456 (13)1.4201 (3)0.32342 (12)0.0500 (5)
H180.48931.46830.30100.060*
C190.60938 (13)1.5157 (3)0.38254 (12)0.0517 (6)
H190.59801.62740.40010.062*
C200.70605 (13)1.2803 (3)0.38725 (12)0.0512 (5)
H200.76171.23380.40880.061*
C210.68998 (12)1.4463 (3)0.41515 (11)0.0392 (4)
C220.75824 (12)1.5416 (3)0.48470 (11)0.0423 (5)
N10.21398 (12)0.7742 (3)0.24689 (12)0.0596 (5)
H1A0.16270.75960.24360.072*
N20.31782 (11)0.8103 (2)0.20759 (10)0.0477 (4)
N30.42774 (12)0.3463 (2)0.04448 (10)0.0527 (5)
H3A0.40450.25140.01600.063*
N40.43772 (11)0.6190 (2)0.10114 (10)0.0456 (4)
O10.74180 (9)1.6814 (2)0.51415 (9)0.0616 (4)
O20.41604 (8)1.1972 (2)0.20972 (8)0.0517 (4)
O30.83114 (8)1.46812 (19)0.51434 (8)0.0510 (4)
O40.51057 (8)0.99635 (19)0.20976 (8)0.0516 (4)
U11U22U33U12U13U23
Pd10.02818 (8)0.04723 (9)0.02930 (9)−0.00258 (7)0.00849 (6)0.00106 (6)
C10.0435 (12)0.0563 (13)0.0459 (12)−0.0098 (10)0.0138 (10)−0.0010 (10)
C20.0561 (13)0.0490 (12)0.0371 (11)−0.0015 (11)0.0221 (10)0.0066 (10)
C30.0410 (12)0.0494 (12)0.0360 (11)−0.0018 (9)0.0180 (9)0.0026 (9)
C40.0762 (18)0.0561 (14)0.0552 (14)0.0118 (13)0.0348 (13)0.0061 (11)
C50.0415 (12)0.0627 (13)0.0506 (13)−0.0062 (11)0.0196 (10)−0.0052 (11)
C60.0425 (14)0.0929 (19)0.0581 (15)−0.0005 (13)0.0217 (11)0.0025 (14)
C70.0602 (17)0.090 (2)0.0626 (16)0.0250 (14)0.0351 (14)0.0149 (14)
C80.0415 (13)0.0714 (15)0.0541 (14)−0.0101 (11)0.0194 (11)0.0052 (12)
C90.0449 (12)0.0463 (11)0.0448 (12)0.0012 (9)0.0219 (10)0.0057 (9)
C100.0491 (13)0.0530 (12)0.0538 (14)−0.0008 (10)0.0277 (11)0.0044 (11)
C110.0730 (18)0.0872 (18)0.0654 (17)−0.0066 (15)0.0448 (15)0.0048 (14)
C120.0468 (13)0.0694 (15)0.0496 (13)0.0032 (11)0.0210 (11)0.0093 (11)
C130.0617 (16)0.108 (2)0.0487 (15)−0.0052 (14)0.0164 (13)0.0122 (14)
C140.094 (2)0.115 (2)0.0515 (16)−0.0136 (18)0.0375 (16)0.0058 (15)
C150.0316 (11)0.0570 (13)0.0334 (10)−0.0034 (9)0.0148 (8)0.0020 (9)
C160.0337 (10)0.0493 (12)0.0310 (10)−0.0023 (9)0.0128 (8)−0.0015 (8)
C170.0377 (12)0.0596 (13)0.0492 (13)0.0047 (10)0.0120 (10)−0.0170 (10)
C180.0344 (11)0.0571 (13)0.0470 (12)0.0087 (9)0.0053 (9)−0.0043 (10)
C190.0425 (12)0.0527 (13)0.0475 (13)0.0081 (10)0.0060 (10)−0.0107 (10)
C200.0320 (11)0.0648 (14)0.0487 (13)0.0076 (10)0.0084 (9)−0.0102 (11)
C210.0361 (11)0.0482 (11)0.0311 (10)0.0000 (9)0.0117 (8)−0.0008 (9)
C220.0386 (12)0.0510 (12)0.0335 (11)−0.0001 (10)0.0110 (9)0.0021 (9)
N10.0430 (11)0.0751 (13)0.0693 (13)−0.0076 (10)0.0317 (10)0.0075 (11)
N20.0404 (10)0.0595 (11)0.0452 (10)−0.0043 (8)0.0196 (8)0.0014 (8)
N30.0598 (12)0.0479 (11)0.0458 (10)−0.0114 (9)0.0171 (9)−0.0077 (8)
N40.0412 (10)0.0491 (10)0.0432 (10)−0.0059 (8)0.0141 (8)−0.0053 (8)
O10.0449 (9)0.0736 (10)0.0552 (10)0.0035 (7)0.0097 (7)−0.0251 (8)
O20.0290 (8)0.0759 (10)0.0461 (8)−0.0005 (7)0.0114 (6)−0.0057 (7)
O30.0378 (8)0.0546 (9)0.0441 (8)0.0077 (7)0.0002 (6)−0.0024 (7)
O40.0390 (8)0.0575 (9)0.0528 (9)−0.0046 (7)0.0134 (7)−0.0161 (7)
Pd1—O42.1945 (13)C11—C141.343 (3)
Pd1—N22.1987 (17)C11—H110.9300
Pd1—N42.2355 (17)C12—C131.358 (3)
Pd1—O3i2.2382 (13)C12—H120.9300
Pd1—O1i2.5324 (14)C13—C141.377 (4)
C1—N41.310 (2)C13—H130.9300
C1—N31.337 (3)C14—H140.9300
C1—H10.9300C15—O21.227 (2)
C2—N31.351 (3)C15—O41.267 (2)
C2—C41.372 (3)C15—C161.489 (3)
C2—C31.400 (3)C16—C171.360 (3)
C3—C51.371 (3)C16—C181.389 (3)
C3—N41.373 (2)C17—C201.370 (3)
C4—C71.354 (3)C17—H170.9300
C4—H40.9300C18—C191.372 (3)
C5—C61.358 (3)C18—H180.9300
C5—H50.9300C19—C211.353 (3)
C6—C71.408 (3)C19—H190.9300
C6—H60.9300C20—C211.391 (3)
C7—H70.9300C20—H200.9300
C8—N21.292 (2)C21—C221.488 (3)
C8—N11.327 (3)C22—O11.242 (2)
C8—H80.9300C22—O31.256 (2)
C9—C121.358 (3)N1—H1A0.8600
C9—C101.376 (3)N3—H3A0.8600
C9—N21.378 (2)O1—Pd1ii2.5324 (14)
C10—N11.351 (3)O3—Pd1ii2.2382 (13)
C10—C111.363 (3)
O4—Pd1—N2107.72 (6)C14—C13—H13119.1
O4—Pd1—N497.45 (6)C11—C14—C13121.3 (2)
N2—Pd1—N4109.34 (6)C11—C14—H14119.4
O4—Pd1—O3i108.54 (5)C13—C14—H14119.4
N2—Pd1—O3i125.04 (6)O2—C15—O4122.67 (18)
N4—Pd1—O3i105.28 (6)O2—C15—C16118.73 (19)
N4—C1—N3114.5 (2)O4—C15—C16118.60 (17)
N4—C1—H1122.7C17—C16—C18119.19 (18)
N3—C1—H1122.7C17—C16—C15118.35 (18)
N3—C2—C4131.0 (2)C18—C16—C15122.46 (17)
N3—C2—C3105.61 (18)C16—C17—C20119.53 (19)
C4—C2—C3123.4 (2)C16—C17—H17120.2
C5—C3—N4129.27 (19)C20—C17—H17120.2
C5—C3—C2121.0 (2)C19—C18—C16121.20 (18)
N4—C3—C2109.73 (17)C19—C18—H18119.4
C7—C4—C2115.1 (2)C16—C18—H18119.4
C7—C4—H4122.4C21—C19—C18119.55 (19)
C2—C4—H4122.4C21—C19—H19120.2
C6—C5—C3115.7 (2)C18—C19—H19120.2
C6—C5—H5122.2C17—C20—C21121.10 (18)
C3—C5—H5122.2C17—C20—H20119.4
C5—C6—C7122.9 (2)C21—C20—H20119.4
C5—C6—H6118.5C19—C21—C20119.41 (18)
C7—C6—H6118.5C19—C21—C22119.34 (18)
C4—C7—C6121.9 (2)C20—C21—C22121.06 (17)
C4—C7—H7119.1O1—C22—O3122.26 (18)
C6—C7—H7119.1O1—C22—C21120.94 (18)
N2—C8—N1112.6 (2)O3—C22—C21116.68 (18)
N2—C8—H8123.7C8—N1—C10107.97 (19)
N1—C8—H8123.7C8—N1—H1A126.0
C12—C9—C10120.5 (2)C10—N1—H1A126.0
C12—C9—N2130.5 (2)C8—N2—C9105.25 (18)
C10—C9—N2109.00 (18)C8—N2—Pd1127.66 (15)
N1—C10—C11132.6 (2)C9—N2—Pd1126.54 (13)
N1—C10—C9105.20 (19)C1—N3—C2106.50 (17)
C11—C10—C9122.2 (2)C1—N3—H3A126.7
C14—C11—C10117.0 (2)C2—N3—H3A126.7
C14—C11—H11121.5C1—N4—C3103.61 (17)
C10—C11—H11121.5C1—N4—Pd1122.03 (15)
C9—C12—C13117.2 (2)C3—N4—Pd1134.34 (13)
C9—C12—H12121.4C22—O1—Pd1ii84.55 (11)
C13—C12—H12121.4C22—O3—Pd1ii97.89 (12)
C12—C13—C14121.9 (2)C15—O4—Pd1104.15 (12)
C12—C13—H13119.1
D—H···AD—HH···AD···AD—H···A
N3—H3A···O3iii0.862.042.762 (2)142
N1—H1A···O2iv0.861.912.699 (2)152
Table 1

Selected bond lengths (Å)

Pd1—O42.1945 (13)
Pd1—N22.1987 (17)
Pd1—N42.2355 (17)
Pd1—O3i2.2382 (13)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
N3—H3A⋯O3ii0.862.042.762 (2)142
N1—H1A⋯O2iii0.861.912.699 (2)152

Symmetry codes: (ii) ; (iii) .

  1 in total

1.  Bis(mu-pyridine-2,6-carboxylato-O,N, O':O)bis[triaquamanganese(II)]-pyridine-2,6-dicarboxylic acid (1/2).

Authors:  N Okabe; N Oya
Journal:  Acta Crystallogr C       Date:  2000-12       Impact factor: 1.172
  1 in total
  1 in total

1.  Retraction of articles.

Authors: 
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-06-13
  1 in total

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