Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The cation in the title complex, [Pd2(OH)2(C10H8N2)2](CF3SO3)2, is essentially planar and features square-planar Pd centers that are linked via a pair of symmetric hydroxo bridges. In the crystal structure, extensive O—H...O hydrogen bonding and π–π inter­actions lead to the formation of cationic columns.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005782/hg2008sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005782/hg2008Isup2.hkl
Contains datablock I

CCDC reference: 601181

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.027
  • wR factor = 0.057
  • Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C22 PLAT432_ALERT_2_C Short Inter X...Y Contact O7 .. C15 .. 2.95 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O7 .. C16 .. 2.99 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2005); cell refinement: TwinSolve (Rigaku, 2002); data reduction: Twinsolve; program(s) used to solve structure: PATTY in DIRDIF92 (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Di-µ-hydroxo-bis[(2,2'-bipyridine)palladium(II)] trifluoromethanesulfonate top
Crystal data top
[Pd2(OH)2(C10H8N2)2](CF3O3S)2Z = 2
Mr = 857.32F(000) = 840
Triclinic, P1Dx = 2.083 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 7.6162 (1) ÅCell parameters from 24414 reflections
b = 12.7248 (2) Åθ = 2.1–25.6°
c = 14.6448 (2) ŵ = 1.57 mm1
α = 86.626 (1)°T = 153 K
β = 84.153 (1)°Block, yellow
γ = 75.610 (1)°0.30 × 0.20 × 0.15 mm
V = 1366.79 (3) Å3
Data collection top
Rigaku R-AXIS SPIDER
diffractometer
5114 independent reflections
Radiation source: fine-focus sealed tube4826 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
ω scansθmax = 25.6°, θmin = 2.1°
Absorption correction: numerical
(Katayama, 1986; Paturle & Coppens, 1988)
h = 99
Tmin = 0.754, Tmax = 0.918k = 1515
42226 measured reflectionsl = 1717
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.057H-atom parameters constrained
S = 1.18 w = 1/[σ2(Fo2) + (0.0188P)2 + 2.6048P]
where P = (Fo2 + 2Fc2)/3
5114 reflections(Δ/σ)max = 0.002
397 parametersΔρmax = 0.48 e Å3
0 restraintsΔρmin = 0.41 e Å3
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
xyzUiso*/Ueq
Pd10.21847 (3)0.493717 (16)0.469263 (14)0.01154 (6)
Pd20.43435 (3)0.383400 (17)0.630555 (14)0.01202 (6)
S10.71398 (10)0.15744 (6)0.35765 (5)0.01729 (15)
S20.21427 (10)0.26255 (6)0.97076 (5)0.02006 (16)
F10.7459 (3)0.22519 (16)0.18585 (13)0.0375 (5)
F20.5010 (3)0.17186 (18)0.22594 (14)0.0381 (5)
F30.7581 (3)0.05432 (15)0.20453 (13)0.0352 (5)
F40.1014 (4)0.1156 (2)1.07670 (17)0.0626 (8)
F50.3232 (3)0.04992 (19)0.9771 (2)0.0612 (8)
F60.0562 (3)0.11149 (17)0.93393 (17)0.0445 (6)
O10.3465 (3)0.34368 (15)0.51447 (13)0.0152 (4)
H1O0.43290.31730.47580.023*
O20.2825 (3)0.53066 (15)0.59194 (13)0.0146 (4)
H2O0.33470.58140.59120.023*
O30.6244 (3)0.27055 (16)0.37860 (15)0.0202 (4)
O40.9088 (3)0.13130 (19)0.35826 (17)0.0306 (5)
O50.6233 (3)0.08042 (18)0.40401 (15)0.0289 (5)
O60.0335 (3)0.33191 (19)0.98494 (16)0.0324 (6)
O70.2901 (3)0.2608 (2)0.87624 (16)0.0338 (6)
O80.3366 (3)0.2680 (2)1.03778 (17)0.0356 (6)
N10.0826 (3)0.63997 (19)0.42591 (16)0.0143 (5)
N20.1421 (3)0.45179 (19)0.35364 (16)0.0137 (5)
N30.5148 (3)0.41899 (19)0.74775 (16)0.0141 (5)
N40.5632 (3)0.23443 (19)0.67120 (16)0.0142 (5)
C10.0539 (4)0.7319 (2)0.4713 (2)0.0174 (6)
H10.10000.72910.52950.021*
C20.0405 (4)0.8305 (2)0.4364 (2)0.0208 (6)
H20.05950.89470.46990.025*
C30.1071 (4)0.8341 (2)0.3511 (2)0.0220 (7)
H30.17070.90130.32520.026*
C40.0807 (4)0.7395 (2)0.3038 (2)0.0182 (6)
H40.12680.74070.24570.022*
C50.0148 (4)0.6427 (2)0.34294 (19)0.0147 (6)
C60.0459 (4)0.5351 (2)0.30254 (19)0.0142 (6)
C70.0197 (4)0.5172 (2)0.2216 (2)0.0174 (6)
H70.08450.57630.18610.021*
C80.0105 (4)0.4117 (3)0.1932 (2)0.0206 (6)
H80.03340.39770.13780.025*
C90.1053 (4)0.3266 (3)0.2462 (2)0.0205 (6)
H90.12550.25370.22820.025*
C100.1700 (4)0.3495 (2)0.3259 (2)0.0174 (6)
H100.23580.29130.36210.021*
C110.4824 (4)0.5193 (2)0.7806 (2)0.0170 (6)
H110.41050.57870.74820.020*
C120.5511 (4)0.5383 (2)0.8607 (2)0.0182 (6)
H120.52740.60980.88260.022*
C130.6548 (4)0.4514 (3)0.9079 (2)0.0199 (6)
H130.70550.46270.96210.024*
C140.6843 (4)0.3473 (2)0.8756 (2)0.0185 (6)
H140.75280.28670.90820.022*
C150.6124 (4)0.3333 (2)0.7954 (2)0.0157 (6)
C160.6355 (4)0.2277 (2)0.75299 (19)0.0153 (6)
C170.7211 (4)0.1281 (2)0.7910 (2)0.0206 (6)
H170.76900.12380.84890.025*
C180.7358 (4)0.0346 (2)0.7431 (2)0.0236 (7)
H180.79580.03420.76760.028*
C190.6627 (4)0.0425 (2)0.6597 (2)0.0217 (7)
H190.67230.02060.62610.026*
C200.5752 (4)0.1438 (2)0.6259 (2)0.0182 (6)
H200.52230.14940.56920.022*
C210.6777 (4)0.1513 (2)0.2366 (2)0.0233 (7)
C220.1738 (5)0.1273 (3)0.9908 (2)0.0310 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.01055 (11)0.01229 (11)0.01163 (11)0.00245 (8)0.00079 (8)0.00104 (8)
Pd20.01139 (11)0.01279 (11)0.01170 (11)0.00252 (8)0.00107 (8)0.00072 (8)
S10.0186 (4)0.0153 (3)0.0175 (4)0.0022 (3)0.0022 (3)0.0049 (3)
S20.0211 (4)0.0237 (4)0.0165 (4)0.0057 (3)0.0061 (3)0.0010 (3)
F10.0573 (14)0.0274 (11)0.0242 (10)0.0091 (10)0.0078 (9)0.0028 (8)
F20.0327 (11)0.0474 (13)0.0327 (11)0.0009 (10)0.0158 (9)0.0066 (10)
F30.0544 (13)0.0219 (10)0.0234 (10)0.0039 (9)0.0040 (9)0.0101 (8)
F40.0778 (19)0.0730 (19)0.0449 (15)0.0386 (16)0.0106 (13)0.0304 (13)
F50.0493 (15)0.0287 (12)0.102 (2)0.0113 (11)0.0354 (15)0.0110 (13)
F60.0419 (13)0.0338 (12)0.0658 (16)0.0158 (10)0.0254 (11)0.0037 (11)
O10.0155 (10)0.0146 (10)0.0150 (10)0.0026 (8)0.0010 (8)0.0024 (8)
O20.0167 (10)0.0119 (10)0.0160 (10)0.0050 (8)0.0018 (8)0.0004 (8)
O30.0193 (10)0.0164 (10)0.0241 (11)0.0027 (8)0.0006 (9)0.0060 (9)
O40.0200 (11)0.0330 (13)0.0354 (14)0.0043 (10)0.0065 (10)0.0145 (11)
O50.0461 (15)0.0227 (12)0.0212 (12)0.0155 (11)0.0001 (10)0.0010 (9)
O60.0309 (13)0.0309 (13)0.0306 (13)0.0060 (10)0.0085 (10)0.0092 (10)
O70.0271 (12)0.0568 (17)0.0197 (12)0.0161 (12)0.0015 (10)0.0048 (11)
O80.0380 (14)0.0420 (15)0.0317 (14)0.0114 (12)0.0198 (11)0.0061 (11)
N10.0100 (11)0.0170 (12)0.0161 (12)0.0043 (9)0.0008 (9)0.0016 (10)
N20.0112 (11)0.0140 (12)0.0155 (12)0.0035 (9)0.0015 (9)0.0009 (9)
N30.0112 (11)0.0164 (12)0.0147 (12)0.0037 (9)0.0001 (9)0.0009 (9)
N40.0143 (12)0.0162 (12)0.0133 (12)0.0061 (10)0.0002 (9)0.0015 (9)
C10.0137 (13)0.0180 (15)0.0214 (15)0.0054 (11)0.0008 (11)0.0028 (12)
C20.0178 (15)0.0162 (15)0.0282 (17)0.0045 (12)0.0007 (12)0.0034 (12)
C30.0207 (15)0.0166 (15)0.0266 (17)0.0024 (12)0.0003 (13)0.0040 (13)
C40.0176 (14)0.0192 (15)0.0178 (15)0.0051 (12)0.0010 (12)0.0021 (12)
C50.0101 (13)0.0189 (14)0.0152 (14)0.0049 (11)0.0017 (11)0.0003 (11)
C60.0114 (13)0.0166 (14)0.0149 (14)0.0059 (11)0.0026 (11)0.0005 (11)
C70.0143 (14)0.0232 (16)0.0143 (14)0.0044 (12)0.0016 (11)0.0021 (12)
C80.0193 (15)0.0282 (17)0.0158 (15)0.0076 (13)0.0011 (12)0.0053 (12)
C90.0208 (15)0.0198 (15)0.0216 (16)0.0061 (12)0.0003 (12)0.0045 (12)
C100.0159 (14)0.0174 (15)0.0178 (15)0.0029 (12)0.0014 (11)0.0016 (12)
C110.0139 (13)0.0165 (14)0.0195 (15)0.0027 (11)0.0016 (11)0.0012 (12)
C120.0174 (14)0.0202 (15)0.0175 (15)0.0058 (12)0.0019 (12)0.0049 (12)
C130.0171 (14)0.0299 (17)0.0136 (14)0.0074 (13)0.0011 (11)0.0057 (12)
C140.0151 (14)0.0234 (16)0.0166 (15)0.0033 (12)0.0038 (11)0.0002 (12)
C150.0122 (13)0.0185 (15)0.0172 (14)0.0065 (11)0.0012 (11)0.0001 (11)
C160.0123 (13)0.0177 (14)0.0165 (14)0.0057 (11)0.0006 (11)0.0003 (11)
C170.0207 (15)0.0210 (16)0.0218 (16)0.0061 (12)0.0085 (12)0.0024 (12)
C180.0230 (16)0.0154 (15)0.0313 (18)0.0021 (12)0.0067 (13)0.0042 (13)
C190.0204 (15)0.0157 (15)0.0296 (17)0.0052 (12)0.0013 (13)0.0027 (13)
C200.0168 (14)0.0212 (15)0.0175 (15)0.0060 (12)0.0016 (12)0.0011 (12)
C210.0278 (17)0.0184 (15)0.0209 (16)0.0001 (13)0.0020 (13)0.0021 (12)
C220.0303 (18)0.0297 (18)0.035 (2)0.0086 (15)0.0115 (15)0.0024 (15)
Geometric parameters (Å, º) top
Pd1—O12.0228 (19)C1—H10.9500
Pd1—O22.0195 (19)C2—C31.390 (5)
Pd1—N11.994 (2)C2—H20.9500
Pd1—N21.988 (2)C3—C41.385 (4)
Pd2—O12.0233 (19)C3—H30.9500
Pd2—O22.0249 (19)C4—C51.389 (4)
Pd2—N31.992 (2)C4—H40.9500
Pd2—N41.993 (2)C5—C61.478 (4)
Pd1—Pd23.0834 (3)C6—C71.384 (4)
S1—O51.436 (2)C7—C81.386 (4)
S1—O41.439 (2)C7—H70.9500
S1—O31.467 (2)C8—C91.387 (4)
S1—C211.831 (3)C8—H80.9500
S2—O81.436 (2)C9—C101.385 (4)
S2—O61.441 (2)C9—H90.9500
S2—O71.444 (2)C10—H100.9500
S2—C221.825 (4)C11—C121.389 (4)
F1—C211.337 (4)C11—H110.9500
F2—C211.329 (4)C12—C131.383 (4)
F3—C211.324 (4)C12—H120.9500
F4—C221.336 (4)C13—C141.389 (4)
F5—C221.313 (4)C13—H130.9500
F6—C221.341 (4)C14—C151.384 (4)
O1—H1O0.8380C14—H140.9500
O2—H2O0.8375C15—C161.477 (4)
N1—C51.363 (4)C16—C171.386 (4)
N1—C11.339 (4)C17—C181.391 (4)
N2—C61.361 (4)C17—H170.9500
N2—C101.346 (4)C18—C191.382 (5)
N3—C151.357 (4)C18—H180.9500
N3—C111.346 (4)C19—C201.384 (4)
N4—C201.343 (4)C19—H190.9500
N4—C161.358 (4)C20—H200.9500
C1—C21.380 (4)
O1—Pd1—O280.45 (8)C3—C4—H4120.7
O1—Pd1—N1177.66 (8)N1—C5—C4121.2 (3)
O1—Pd1—N298.02 (9)N1—C5—C6114.2 (2)
O2—Pd1—N1100.12 (9)C4—C5—C6124.6 (3)
O2—Pd1—N2175.69 (8)N2—C6—C7121.4 (3)
N1—Pd1—N281.25 (9)N2—C6—C5114.1 (2)
O1—Pd2—O280.30 (8)C7—C6—C5124.4 (3)
O1—Pd2—N3177.71 (8)C6—C7—C8119.0 (3)
O1—Pd2—N497.94 (9)C6—C7—H7120.5
O2—Pd2—N3100.55 (9)C8—C7—H7120.5
O2—Pd2—N4174.91 (8)C9—C8—C7119.5 (3)
N3—Pd2—N481.03 (9)C9—C8—H8120.3
N1—Pd1—Pd2140.39 (7)C7—C8—H8120.3
N2—Pd1—Pd2138.35 (7)C8—C9—C10119.0 (3)
O2—Pd1—Pd240.39 (5)C8—C9—H9120.5
O1—Pd1—Pd240.36 (5)C10—C9—H9120.5
N4—Pd2—Pd1138.27 (7)N2—C10—C9121.8 (3)
N3—Pd2—Pd1140.69 (7)N2—C10—H10119.1
O2—Pd2—Pd140.26 (5)C9—C10—H10119.1
O1—Pd2—Pd140.35 (5)N3—C11—C12121.9 (3)
O5—S1—O4116.10 (15)N3—C11—H11119.1
O5—S1—O3113.55 (13)C12—C11—H11119.1
O4—S1—O3114.06 (13)C13—C12—C11118.7 (3)
O5—S1—C21104.35 (14)C13—C12—H12120.6
O4—S1—C21104.04 (14)C11—C12—H12120.6
O3—S1—C21102.69 (13)C14—C13—C12119.6 (3)
O8—S2—O6115.87 (15)C14—C13—H13120.2
O8—S2—O7115.66 (15)C12—C13—H13120.2
O6—S2—O7113.63 (15)C13—C14—C15119.1 (3)
O8—S2—C22103.77 (16)C13—C14—H14120.4
O6—S2—C22102.41 (16)C15—C14—H14120.4
O7—S2—C22102.96 (17)N3—C15—C14121.3 (3)
Pd1—O1—Pd299.29 (8)N3—C15—C16114.1 (2)
Pd1—O1—H1O109.0C14—C15—C16124.6 (3)
Pd2—O1—H1O112.2N4—C16—C17120.9 (3)
Pd1—O2—Pd299.35 (8)N4—C16—C15114.3 (2)
Pd1—O2—H2O116.1C17—C16—C15124.8 (3)
Pd2—O2—H2O114.8C16—C17—C18119.0 (3)
C5—N1—C1119.4 (2)C16—C17—H17120.5
C5—N1—Pd1115.03 (19)C18—C17—H17120.5
C1—N1—Pd1125.6 (2)C17—C18—C19119.6 (3)
C6—N2—C10119.2 (2)C17—C18—H18120.2
C6—N2—Pd1115.38 (19)C19—C18—H18120.2
C10—N2—Pd1125.3 (2)C20—C19—C18119.0 (3)
C15—N3—C11119.3 (2)C20—C19—H19120.5
C15—N3—Pd2115.37 (19)C18—C19—H19120.5
C11—N3—Pd2125.3 (2)N4—C20—C19121.6 (3)
C20—N4—C16119.9 (2)N4—C20—H20119.2
C20—N4—Pd2124.8 (2)C19—C20—H20119.2
C16—N4—Pd2115.20 (19)F3—C21—F2108.6 (3)
N1—C1—C2122.2 (3)F3—C21—F1108.2 (3)
N1—C1—H1118.9F2—C21—F1107.9 (3)
C2—C1—H1118.9F3—C21—S1110.9 (2)
C3—C2—C1118.6 (3)F2—C21—S1110.6 (2)
C3—C2—H2120.7F1—C21—S1110.5 (2)
C1—C2—H2120.7F5—C22—F4108.4 (3)
C2—C3—C4119.9 (3)F5—C22—F6107.1 (3)
C2—C3—H3120.0F4—C22—F6107.5 (3)
C4—C3—H3120.0F5—C22—S2112.5 (3)
C5—C4—C3118.6 (3)F4—C22—S2110.6 (3)
C5—C4—H4120.7F6—C22—S2110.5 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1o···O30.841.942.772 (3)174
O2—H2o···O3i0.842.062.858 (3)158
C1—H1···O4i0.952.473.201 (4)133
C3—H3···F3ii0.952.543.439 (3)157
C4—H4···O7iii0.952.283.218 (4)168
C7—H7···O7iii0.952.463.392 (4)168
C8—H8···O6iv0.952.403.245 (4)148
C11—H11···O3i0.952.573.438 (3)151
C12—H12···O8v0.952.473.280 (4)143
C20—H20···O50.952.603.356 (4)137
Symmetry codes: (i) x+1, y+1, z+1; (ii) x1, y+1, z; (iii) x, y+1, z+1; (iv) x, y, z1; (v) x+1, y+1, z+2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds