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In the title complex, [Pd(C6H4O2)(C10H9N3)]·0.5H2O, the Pd atom has a distorted cis-square-planar geometry defined by an N,N-bidentate di-2-pyridylamine (bpa) and an O,O-bidentate benzenediolate (bd) ligand. There are two molecules in the asymmetric unit. The crystal structure is stabilized by intermolecular hydrogen bonds.
Supporting information
CCDC reference: 628419
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.004 Å
- R factor = 0.021
- wR factor = 0.070
- Data-to-parameter ratio = 16.0
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2005) and
CRYSTALS (Watkin et al., 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: CrystalStructure.
(Benzene-1,2-diolato-
κ2N,
N')(di-2-pyridylamine-
κ2N,
N')palladium(II) hemihydrate
top
Crystal data top
[Pd(C6H4O2)(C10H9N3)]·0.5H2O | Z = 4 |
Mr = 394.72 | F(000) = 788.00 |
Triclinic, P1 | Dx = 1.792 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.7107 Å |
a = 9.08 (1) Å | Cell parameters from 12902 reflections |
b = 12.70 (1) Å | θ = 3.0–27.5° |
c = 13.22 (1) Å | µ = 1.28 mm−1 |
α = 82.34 (3)° | T = 296 K |
β = 77.43 (4)° | Platelet, orange |
γ = 81.19 (4)° | 0.50 × 0.30 × 0.05 mm |
V = 1463 (2) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 5601 reflections with F2 > 2σ(F2) |
Detector resolution: 10.00 pixels mm-1 | Rint = 0.016 |
ω scans | θmax = 27.5° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −11→11 |
Tmin = 0.551, Tmax = 0.938 | k = −16→16 |
14387 measured reflections | l = −17→14 |
6621 independent reflections | |
Refinement top
Refinement on F2 | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.021 | w = 1/[σ2(Fo2) + (0.0401P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.070 | (Δ/σ)max = 0.002 |
S = 1.17 | Δρmax = 0.41 e Å−3 |
6621 reflections | Δρmin = −0.35 e Å−3 |
413 parameters | |
Special details top
Refinement. Refinement using all reflections. The weighted R-factor (wR) and
goodness of fit (S) are based on F2. R-factor (gt) are
based on F. The threshold expression of F2 > 2.0
σ(F2) is used only for calculating R-factor (gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pd1 | 0.17615 (2) | −0.00724 (1) | 0.91859 (1) | 0.03023 (6) | |
Pd2 | 0.59853 (2) | 0.36137 (1) | 0.51977 (1) | 0.03226 (6) | |
O1 | 0.1615 (2) | 0.1257 (1) | 0.8218 (1) | 0.0408 (3) | |
O2 | 0.0796 (2) | −0.0680 (1) | 0.8189 (1) | 0.0402 (4) | |
O3 | 0.4236 (2) | 0.3491 (1) | 0.6387 (1) | 0.0404 (4) | |
O4 | 0.6497 (2) | 0.4709 (1) | 0.5973 (1) | 0.0419 (4) | |
O5 | 0.4627 (2) | 0.1502 (1) | 0.7425 (1) | 0.0451 (4) | |
N1 | 0.1921 (2) | −0.1463 (1) | 1.0118 (1) | 0.0320 (4) | |
N2 | 0.3539 (2) | −0.0929 (1) | 1.1083 (1) | 0.0355 (4) | |
N3 | 0.2700 (2) | 0.0673 (1) | 1.0098 (1) | 0.0325 (4) | |
N4 | 0.7858 (2) | 0.3723 (1) | 0.4065 (1) | 0.0359 (4) | |
N5 | 0.7646 (2) | 0.2157 (1) | 0.3331 (1) | 0.0405 (4) | |
N6 | 0.5308 (2) | 0.2484 (1) | 0.4524 (1) | 0.0354 (4) | |
C1 | 0.1140 (3) | −0.2244 (2) | 0.9975 (2) | 0.0398 (5) | |
C2 | 0.1229 (3) | −0.3241 (2) | 1.0509 (2) | 0.0490 (6) | |
C3 | 0.2210 (3) | −0.3488 (2) | 1.1192 (2) | 0.0493 (6) | |
C4 | 0.2998 (3) | −0.2720 (2) | 1.1364 (2) | 0.0438 (5) | |
C5 | 0.2794 (2) | −0.1688 (2) | 1.0836 (2) | 0.0325 (4) | |
C6 | 0.3399 (2) | 0.0170 (2) | 1.0853 (1) | 0.0322 (4) | |
C7 | 0.4072 (3) | 0.0734 (2) | 1.1431 (2) | 0.0408 (5) | |
C8 | 0.4012 (3) | 0.1821 (2) | 1.1242 (2) | 0.0477 (6) | |
C9 | 0.3289 (3) | 0.2348 (2) | 1.0462 (2) | 0.0452 (6) | |
C10 | 0.2660 (3) | 0.1759 (2) | 0.9920 (2) | 0.0387 (5) | |
C11 | 0.0762 (2) | 0.1152 (2) | 0.7523 (2) | 0.0380 (5) | |
C12 | 0.0326 (3) | 0.2016 (2) | 0.6842 (2) | 0.0490 (6) | |
C13 | −0.0550 (3) | 0.1884 (3) | 0.6150 (2) | 0.0617 (7) | |
C14 | −0.0974 (3) | 0.0886 (3) | 0.6130 (2) | 0.0634 (8) | |
C15 | −0.0543 (3) | 0.0015 (2) | 0.6799 (2) | 0.0526 (6) | |
C16 | 0.0324 (3) | 0.0148 (2) | 0.7510 (2) | 0.0395 (5) | |
C17 | 0.8688 (3) | 0.4533 (2) | 0.4060 (2) | 0.0463 (6) | |
C18 | 1.0041 (3) | 0.4644 (2) | 0.3390 (2) | 0.0563 (7) | |
C19 | 1.0571 (3) | 0.3910 (2) | 0.2660 (2) | 0.0563 (7) | |
C20 | 0.9756 (3) | 0.3107 (2) | 0.2643 (2) | 0.0483 (6) | |
C21 | 0.8385 (3) | 0.3013 (2) | 0.3366 (2) | 0.0365 (5) | |
C22 | 0.6233 (3) | 0.1892 (2) | 0.3811 (2) | 0.0347 (4) | |
C23 | 0.5790 (3) | 0.0984 (2) | 0.3537 (2) | 0.0439 (6) | |
C24 | 0.4367 (3) | 0.0707 (2) | 0.3966 (2) | 0.0483 (6) | |
C25 | 0.3370 (3) | 0.1363 (2) | 0.4631 (2) | 0.0525 (6) | |
C26 | 0.3884 (3) | 0.2226 (2) | 0.4896 (2) | 0.0470 (6) | |
C27 | 0.4243 (3) | 0.4193 (2) | 0.7067 (2) | 0.0374 (5) | |
C28 | 0.3134 (3) | 0.4277 (2) | 0.7966 (2) | 0.0493 (6) | |
C29 | 0.3168 (4) | 0.5019 (2) | 0.8642 (2) | 0.0594 (7) | |
C30 | 0.4288 (4) | 0.5684 (2) | 0.8405 (2) | 0.0586 (7) | |
C31 | 0.5401 (3) | 0.5609 (2) | 0.7503 (2) | 0.0482 (6) | |
C32 | 0.5418 (3) | 0.4849 (2) | 0.6835 (2) | 0.0374 (5) | |
H1 | 0.0514 | −0.2092 | 0.9489 | 0.048* | |
H2 | 0.0639 | −0.3743 | 1.0414 | 0.059* | |
H3 | 0.2335 | −0.4175 | 1.1533 | 0.059* | |
H4 | 0.3662 | −0.2877 | 1.1824 | 0.053* | |
H5 | 0.4217 | −0.1182 | 1.1447 | 0.043* | |
H6 | 0.4562 | 0.0367 | 1.1947 | 0.049* | |
H7 | 0.4448 | 0.2201 | 1.1630 | 0.057* | |
H8 | 0.3235 | 0.3087 | 1.0312 | 0.054* | |
H9 | 0.2175 | 0.2118 | 0.9398 | 0.046* | |
H10 | 0.0625 | 0.2682 | 0.6853 | 0.059* | |
H11 | −0.0855 | 0.2461 | 0.5698 | 0.074* | |
H12 | −0.1560 | 0.0800 | 0.5658 | 0.076* | |
H13 | −0.0829 | −0.0652 | 0.6774 | 0.063* | |
H14 | 0.8313 | 0.5034 | 0.4536 | 0.056* | |
H15 | 1.0593 | 0.5194 | 0.3420 | 0.068* | |
H16 | 1.1483 | 0.3970 | 0.2185 | 0.068* | |
H17 | 1.0103 | 0.2618 | 0.2152 | 0.058* | |
H18 | 0.8173 | 0.1697 | 0.2930 | 0.049* | |
H19 | 0.6457 | 0.0566 | 0.3064 | 0.053* | |
H20 | 0.4078 | 0.0086 | 0.3810 | 0.058* | |
H21 | 0.2374 | 0.1223 | 0.4892 | 0.063* | |
H22 | 0.3219 | 0.2658 | 0.5357 | 0.056* | |
H23 | 0.2366 | 0.3839 | 0.8117 | 0.059* | |
H24 | 0.2437 | 0.5065 | 0.9254 | 0.071* | |
H25 | 0.4297 | 0.6188 | 0.8853 | 0.070* | |
H26 | 0.6140 | 0.6071 | 0.7346 | 0.058* | |
H27 | 0.3615 | 0.1429 | 0.7687 | 0.068* | |
H28 | 0.4604 | 0.2129 | 0.7001 | 0.068* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pd1 | 0.02937 (9) | 0.03161 (9) | 0.02990 (9) | −0.00416 (6) | −0.00536 (6) | −0.00462 (7) |
Pd2 | 0.0336 (1) | 0.03122 (9) | 0.03253 (9) | −0.00483 (7) | −0.00799 (7) | −0.00229 (7) |
O1 | 0.0465 (9) | 0.0398 (8) | 0.0384 (8) | −0.0081 (7) | −0.0149 (7) | 0.0013 (7) |
O2 | 0.0417 (9) | 0.0449 (9) | 0.0376 (8) | −0.0084 (7) | −0.0109 (7) | −0.0086 (7) |
O3 | 0.0462 (9) | 0.0382 (8) | 0.0372 (8) | −0.0116 (7) | −0.0039 (7) | −0.0056 (7) |
O4 | 0.0437 (9) | 0.0395 (8) | 0.0445 (9) | −0.0089 (7) | −0.0077 (7) | −0.0091 (7) |
O5 | 0.047 (1) | 0.0416 (9) | 0.048 (1) | −0.0083 (8) | −0.0142 (8) | 0.0034 (8) |
N1 | 0.0309 (9) | 0.0310 (8) | 0.0331 (9) | −0.0051 (7) | −0.0027 (7) | −0.0042 (7) |
N2 | 0.039 (1) | 0.0358 (9) | 0.0336 (9) | −0.0054 (8) | −0.0130 (8) | −0.0003 (8) |
N3 | 0.0329 (9) | 0.0320 (9) | 0.0326 (9) | −0.0042 (7) | −0.0042 (7) | −0.0069 (8) |
N4 | 0.034 (1) | 0.0358 (9) | 0.038 (1) | −0.0059 (7) | −0.0074 (8) | −0.0002 (8) |
N5 | 0.036 (1) | 0.043 (1) | 0.042 (1) | −0.0093 (8) | −0.0005 (8) | −0.0123 (9) |
N6 | 0.034 (1) | 0.041 (1) | 0.0317 (9) | −0.0081 (8) | −0.0069 (7) | −0.0029 (8) |
C1 | 0.038 (1) | 0.038 (1) | 0.045 (1) | −0.0075 (9) | −0.008 (1) | −0.009 (1) |
C2 | 0.048 (1) | 0.036 (1) | 0.063 (2) | −0.013 (1) | −0.003 (1) | −0.009 (1) |
C3 | 0.052 (2) | 0.031 (1) | 0.060 (2) | −0.007 (1) | −0.006 (1) | 0.003 (1) |
C4 | 0.044 (1) | 0.038 (1) | 0.048 (1) | −0.005 (1) | −0.013 (1) | 0.004 (1) |
C5 | 0.031 (1) | 0.033 (1) | 0.031 (1) | −0.0038 (8) | −0.0003 (8) | −0.0032 (9) |
C6 | 0.031 (1) | 0.034 (1) | 0.031 (1) | −0.0051 (8) | −0.0018 (8) | −0.0059 (9) |
C7 | 0.051 (1) | 0.042 (1) | 0.033 (1) | −0.008 (1) | −0.014 (1) | −0.004 (1) |
C8 | 0.057 (2) | 0.044 (1) | 0.048 (1) | −0.012 (1) | −0.013 (1) | −0.016 (1) |
C9 | 0.053 (1) | 0.032 (1) | 0.051 (1) | −0.006 (1) | −0.009 (1) | −0.010 (1) |
C10 | 0.043 (1) | 0.032 (1) | 0.040 (1) | −0.0020 (9) | −0.009 (1) | −0.004 (1) |
C11 | 0.031 (1) | 0.048 (1) | 0.033 (1) | −0.0001 (9) | −0.0044 (9) | −0.007 (1) |
C12 | 0.046 (1) | 0.050 (1) | 0.046 (1) | 0.003 (1) | −0.009 (1) | 0.001 (1) |
C13 | 0.052 (2) | 0.078 (2) | 0.051 (2) | 0.006 (1) | −0.019 (1) | 0.006 (1) |
C14 | 0.047 (2) | 0.097 (2) | 0.051 (2) | −0.008 (2) | −0.024 (1) | −0.003 (2) |
C15 | 0.044 (1) | 0.071 (2) | 0.047 (1) | −0.012 (1) | −0.016 (1) | −0.007 (1) |
C16 | 0.031 (1) | 0.051 (1) | 0.035 (1) | −0.002 (1) | −0.0030 (9) | −0.008 (1) |
C17 | 0.045 (1) | 0.044 (1) | 0.051 (1) | −0.013 (1) | −0.007 (1) | −0.007 (1) |
C18 | 0.051 (2) | 0.055 (1) | 0.067 (2) | −0.024 (1) | −0.006 (1) | −0.007 (1) |
C19 | 0.041 (1) | 0.065 (2) | 0.061 (2) | −0.019 (1) | 0.002 (1) | −0.008 (1) |
C20 | 0.038 (1) | 0.056 (1) | 0.050 (1) | −0.011 (1) | −0.001 (1) | −0.013 (1) |
C21 | 0.034 (1) | 0.040 (1) | 0.036 (1) | −0.0052 (9) | −0.0095 (9) | −0.003 (1) |
C22 | 0.035 (1) | 0.040 (1) | 0.031 (1) | −0.0074 (9) | −0.0080 (9) | −0.0035 (9) |
C23 | 0.046 (1) | 0.052 (1) | 0.036 (1) | −0.014 (1) | −0.003 (1) | −0.014 (1) |
C24 | 0.056 (2) | 0.057 (1) | 0.039 (1) | −0.026 (1) | −0.005 (1) | −0.013 (1) |
C25 | 0.041 (1) | 0.075 (2) | 0.047 (1) | −0.026 (1) | −0.002 (1) | −0.016 (1) |
C26 | 0.035 (1) | 0.063 (2) | 0.044 (1) | −0.012 (1) | −0.003 (1) | −0.016 (1) |
C27 | 0.046 (1) | 0.030 (1) | 0.037 (1) | 0.0007 (9) | −0.012 (1) | −0.0037 (9) |
C28 | 0.057 (2) | 0.039 (1) | 0.048 (1) | −0.009 (1) | 0.001 (1) | −0.007 (1) |
C29 | 0.075 (2) | 0.051 (1) | 0.047 (1) | −0.007 (1) | 0.004 (1) | −0.014 (1) |
C30 | 0.072 (2) | 0.050 (1) | 0.057 (2) | −0.003 (1) | −0.011 (1) | −0.026 (1) |
C31 | 0.051 (1) | 0.040 (1) | 0.059 (2) | −0.006 (1) | −0.017 (1) | −0.013 (1) |
C32 | 0.042 (1) | 0.033 (1) | 0.037 (1) | 0.0010 (9) | −0.014 (1) | −0.002 (1) |
Geometric parameters (Å, º) top
Pd1—O1 | 1.984 (3) | C8—H7 | 0.9300 |
Pd1—O2 | 2.020 (2) | C9—C10 | 1.360 (4) |
Pd1—N1 | 2.020 (2) | C9—H8 | 0.9300 |
Pd1—N3 | 2.018 (2) | C10—H9 | 0.9300 |
Pd2—O3 | 1.986 (3) | C11—C12 | 1.390 (3) |
Pd2—O4 | 1.996 (2) | C11—C16 | 1.396 (4) |
Pd2—N4 | 2.015 (2) | C12—C13 | 1.378 (4) |
Pd2—N6 | 2.020 (2) | C12—H10 | 0.9299 |
O1—C11 | 1.356 (3) | C13—C14 | 1.385 (5) |
O2—C16 | 1.369 (3) | C13—H11 | 0.9300 |
O3—C27 | 1.350 (3) | C14—C15 | 1.385 (4) |
O4—C32 | 1.343 (3) | C14—H12 | 0.9299 |
O5—H27 | 0.9224 | C15—C16 | 1.392 (4) |
O5—H28 | 0.9107 | C15—H13 | 0.9300 |
N1—C1 | 1.359 (3) | C17—C18 | 1.363 (4) |
N1—C5 | 1.340 (3) | C17—H14 | 0.9301 |
N2—C5 | 1.369 (3) | C18—C19 | 1.390 (4) |
N2—C6 | 1.380 (3) | C18—H15 | 0.9300 |
N2—H5 | 0.8600 | C19—C20 | 1.354 (4) |
N3—C6 | 1.338 (3) | C19—H16 | 0.9300 |
N3—C10 | 1.365 (3) | C20—C21 | 1.405 (3) |
N4—C17 | 1.364 (3) | C20—H17 | 0.9300 |
N4—C21 | 1.339 (3) | C22—C23 | 1.393 (4) |
N5—C21 | 1.372 (3) | C23—C24 | 1.371 (4) |
N5—C22 | 1.373 (3) | C23—H19 | 0.9301 |
N5—H18 | 0.8600 | C24—C25 | 1.381 (3) |
N6—C22 | 1.346 (3) | C24—H20 | 0.9299 |
N6—C26 | 1.353 (3) | C25—C26 | 1.368 (4) |
C1—C2 | 1.365 (3) | C25—H21 | 0.9299 |
C1—H1 | 0.9299 | C26—H22 | 0.9301 |
C2—C3 | 1.377 (4) | C27—C28 | 1.385 (3) |
C2—H2 | 0.9300 | C27—C32 | 1.411 (3) |
C3—C4 | 1.364 (4) | C28—C29 | 1.390 (4) |
C3—H3 | 0.9300 | C28—H23 | 0.9301 |
C4—C5 | 1.407 (3) | C29—C30 | 1.379 (5) |
C4—H4 | 0.9300 | C29—H24 | 0.9299 |
C6—C7 | 1.398 (4) | C30—C31 | 1.389 (4) |
C7—C8 | 1.364 (3) | C30—H25 | 0.9301 |
C7—H6 | 0.9300 | C31—C32 | 1.389 (4) |
C8—C9 | 1.386 (4) | C31—H26 | 0.9300 |
| | | |
Pd1···N2 | 3.252 (2) | C13···C16 | 2.784 (4) |
Pd1···C1 | 2.910 (2) | C13···H10 | 2.0121 |
Pd1···C5 | 2.992 (2) | C13···H12 | 2.0109 |
Pd1···C6 | 2.985 (2) | C13···H13 | 3.2513 |
Pd1···C10 | 2.924 (3) | C13···H21 | 2.8783 |
Pd1···C11 | 2.757 (2) | C14···C16 | 2.396 (4) |
Pd1···C16 | 2.770 (2) | C14···H10 | 3.2295 |
Pd1···H1 | 2.9057 | C14···H11 | 2.0187 |
Pd1···H9 | 2.9212 | C14···H12 | 3.5967 |
Pd1···H19 | 3.1541 | C14···H13 | 2.0216 |
Pd1···H27 | 2.9865 | C14···H20 | 3.2275 |
Pd2···O4 | 3.344 (2) | C14···H21 | 3.1854 |
Pd2···N5 | 3.244 (2) | C15···N5 | 3.502 (3) |
Pd2···C17 | 2.907 (3) | C15···H11 | 3.2499 |
Pd2···C21 | 2.980 (2) | C15···H12 | 2.0117 |
Pd2···C22 | 2.989 (2) | C15···H12 | 3.5853 |
Pd2···C26 | 2.908 (3) | C15···H17 | 3.4437 |
Pd2···C27 | 2.753 (2) | C15···H18 | 2.8597 |
Pd2···C32 | 2.754 (2) | C15···H20 | 3.4995 |
Pd2···C32 | 3.462 (2) | C16···N5 | 3.396 (3) |
Pd2···H11 | 3.1762 | C16···H10 | 3.2576 |
Pd2···H14 | 2.9039 | C16···H12 | 3.2335 |
Pd2···H22 | 2.9092 | C16···H13 | 2.0275 |
Pd2···H28 | 3.0061 | C16···H17 | 3.5520 |
O1···O2 | 2.684 (2) | C16···H18 | 2.5938 |
O1···O5 | 2.757 (2) | C16···H19 | 2.8884 |
O1···N3 | 2.836 (2) | C17···O3 | 3.456 (3) |
O1···C10 | 2.805 (3) | C17···C19 | 2.361 (3) |
O1···C12 | 2.393 (3) | C17···C20 | 2.703 (4) |
O1···C16 | 2.360 (3) | C17···C21 | 2.322 (4) |
O1···H9 | 2.2039 | C17···C27 | 3.418 (4) |
O1···H10 | 2.5843 | C17···C28 | 3.504 (4) |
O1···H19 | 3.1319 | C17···H11 | 3.2132 |
O1···H23 | 3.4304 | C17···H15 | 2.0074 |
O1···H27 | 1.8344 | C17···H16 | 3.2048 |
O1···H28 | 3.1189 | C17···H23 | 3.5330 |
O2···N1 | 2.946 (2) | C18···C20 | 2.374 (4) |
O2···N5 | 2.919 (2) | C18···C21 | 2.747 (4) |
O2···C1 | 2.915 (3) | C18···H3 | 3.2190 |
O2···C11 | 2.373 (3) | C18···H10 | 3.3417 |
O2···C15 | 2.418 (3) | C18···H14 | 1.9826 |
O2···C20 | 3.548 (3) | C18···H14 | 3.4903 |
O2···C23 | 3.428 (3) | C18···H16 | 2.0239 |
O2···H1 | 2.3160 | C18···H17 | 3.2163 |
O2···H13 | 2.6175 | C18···H23 | 3.4700 |
O2···H17 | 2.8290 | C18···H26 | 3.4049 |
O2···H18 | 2.0660 | C19···C21 | 2.390 (4) |
O2···H19 | 2.6892 | C19···H3 | 3.1448 |
O3···O4 | 2.677 (2) | C19···H14 | 3.1986 |
O3···O5 | 2.721 (2) | C19···H15 | 2.0323 |
O3···N6 | 2.840 (2) | C19···H17 | 1.9892 |
O3···C17 | 3.456 (3) | C19···H26 | 2.9879 |
O3···C26 | 2.801 (3) | C20···O2 | 3.548 (3) |
O3···C28 | 2.387 (3) | C20···H1 | 3.3218 |
O3···C32 | 2.366 (3) | C20···H13 | 3.1664 |
O3···H10 | 3.4878 | C20···H15 | 3.2171 |
O3···H14 | 3.1062 | C20···H16 | 1.9907 |
O3···H22 | 2.2489 | C20···H18 | 2.4061 |
O3···H23 | 2.5804 | C21···C22 | 2.515 (3) |
O3···H27 | 2.9938 | C21···H11 | 3.2670 |
O3···H28 | 1.8247 | C21···H13 | 3.4474 |
O4···Pd2 | 3.344 (2) | C21···H14 | 3.1553 |
O4···N4 | 2.909 (2) | C21···H16 | 3.2331 |
O4···C17 | 2.868 (3) | C21···H17 | 2.0354 |
O4···C27 | 2.362 (3) | C21···H18 | 1.8895 |
O4···C31 | 2.405 (3) | C22···C24 | 2.392 (4) |
O4···H11 | 3.4430 | C22···C25 | 2.738 (3) |
O4···H14 | 2.2655 | C22···C26 | 2.311 (3) |
O4···H15 | 2.9478 | C22···H7 | 3.5541 |
O4···H22 | 3.5835 | C22···H12 | 3.5033 |
O4···H26 | 2.6084 | C22···H18 | 1.8897 |
O5···C10 | 3.423 (3) | C22···H19 | 2.0256 |
O5···C11 | 3.577 (3) | C22···H20 | 3.2352 |
O5···C24 | 3.457 (3) | C22···H22 | 3.1453 |
O5···C26 | 3.529 (3) | C22···H26 | 3.5141 |
O5···C27 | 3.362 (3) | C23···O2 | 3.428 (3) |
O5···H9 | 3.1389 | C23···C7 | 3.544 (4) |
O5···H19 | 3.1321 | C23···C25 | 2.373 (3) |
O5···H20 | 2.7263 | C23···C26 | 2.697 (3) |
O5···H22 | 3.3380 | C23···H6 | 2.8281 |
O5···H23 | 3.4492 | C23···H7 | 3.1543 |
N1···N2 | 2.366 (3) | C23···H18 | 2.4079 |
N1···N3 | 2.902 (2) | C23···H20 | 2.0086 |
N1···C2 | 2.397 (3) | C23···H21 | 3.2177 |
N1···C3 | 2.772 (3) | C23···H27 | 3.5682 |
N1···C4 | 2.395 (3) | C24···O5 | 3.457 (3) |
N1···C6 | 3.001 (3) | C24···C7 | 3.414 (3) |
N1···H1 | 1.9786 | C24···C24 | 3.384 (3) |
N1···H2 | 3.2293 | C24···C26 | 2.359 (4) |
N1···H4 | 3.2266 | C24···H6 | 2.7231 |
N1···H5 | 3.0892 | C24···H7 | 3.3938 |
N2···N3 | 2.380 (2) | C24···H12 | 3.3316 |
N2···C1 | 3.584 (3) | C24···H13 | 3.5682 |
N2···C4 | 2.366 (3) | C24···H19 | 2.0052 |
N2···C7 | 2.361 (3) | C24···H20 | 3.4976 |
N2···C10 | 3.600 (3) | C24···H21 | 2.0222 |
N2···H4 | 2.5324 | C24···H22 | 3.1937 |
N2···H6 | 2.5119 | C25···H12 | 3.5118 |
N3···C5 | 3.021 (3) | C25···H13 | 3.5403 |
N3···C7 | 2.384 (3) | C25···H19 | 3.2151 |
N3···C8 | 2.782 (4) | C25···H20 | 2.0178 |
N3···C9 | 2.404 (3) | C25···H20 | 3.5728 |
N3···H5 | 3.0948 | C25···H22 | 1.9847 |
N3···H6 | 3.2142 | C26···H10 | 3.5107 |
N3···H8 | 3.2359 | C26···H20 | 3.2039 |
N3···H9 | 1.9812 | C26···H21 | 2.0104 |
N3···H27 | 3.1696 | C26···H26 | 3.4301 |
N4···N5 | 2.376 (3) | C26···H28 | 2.9771 |
N4···N6 | 2.908 (3) | C27···N4 | 3.395 (3) |
N4···C18 | 2.399 (3) | C27···C17 | 3.418 (4) |
N4···C19 | 2.765 (3) | C27···C29 | 2.403 (4) |
N4···C20 | 2.384 (3) | C27···C30 | 2.769 (4) |
N4···C22 | 3.030 (3) | C27···C31 | 2.408 (4) |
N4···C27 | 3.395 (3) | C27···H14 | 3.4253 |
N4···C32 | 3.587 (3) | C27···H22 | 3.5247 |
N4···H11 | 2.8624 | C27···H23 | 2.0177 |
N4···H14 | 1.9835 | C27···H24 | 3.2415 |
N4···H15 | 3.2345 | C27···H26 | 3.2506 |
N4···H17 | 3.2163 | C27···H28 | 2.6026 |
N4···H18 | 3.0949 | C28···C17 | 3.504 (4) |
N5···O2 | 2.919 (2) | C28···C30 | 2.396 (4) |
N5···N6 | 2.369 (2) | C28···C31 | 2.778 (4) |
N5···C15 | 3.502 (3) | C28···C32 | 2.426 (3) |
N5···C16 | 3.396 (3) | C28···H8 | 3.2769 |
N5···C20 | 2.368 (3) | C28···H9 | 3.2396 |
N5···C23 | 2.367 (3) | C28···H24 | 2.0228 |
N5···C26 | 3.583 (3) | C28···H25 | 3.2349 |
N5···H12 | 3.4815 | C28···H28 | 3.1511 |
N5···H13 | 3.1985 | C29···C2 | 3.528 (4) |
N5···H17 | 2.5275 | C29···C31 | 2.404 (4) |
N5···H19 | 2.5304 | C29···C32 | 2.794 (3) |
N6···C21 | 3.007 (3) | C29···H2 | 3.2812 |
N6···C23 | 2.384 (3) | C29···H8 | 3.0755 |
N6···C24 | 2.771 (4) | C29···H23 | 2.0227 |
N6···C25 | 2.398 (4) | C29···H25 | 2.0090 |
N6···C31 | 3.464 (3) | C29···H26 | 3.2388 |
N6···H18 | 3.0963 | C30···C32 | 2.411 (4) |
N6···H19 | 3.2168 | C30···H23 | 3.2351 |
N6···H21 | 3.2300 | C30···H24 | 2.0122 |
N6···H22 | 1.9713 | C30···H26 | 2.0193 |
N6···H26 | 3.2664 | C31···N6 | 3.464 (3) |
N6···H28 | 3.1809 | C31···H16 | 3.0806 |
C1···C3 | 2.358 (3) | C31···H24 | 3.2419 |
C1···C4 | 2.706 (4) | C31···H25 | 2.0187 |
C1···C5 | 2.310 (4) | C32···Pd2 | 3.462 (2) |
C1···H2 | 2.0060 | C32···N4 | 3.587 (3) |
C1···H3 | 3.2013 | C32···H14 | 3.5664 |
C1···H17 | 3.3628 | C32···H15 | 3.5559 |
C1···H25 | 3.4017 | C32···H23 | 3.2658 |
C2···C4 | 2.368 (4) | C32···H25 | 3.2471 |
C2···C5 | 2.730 (4) | C32···H26 | 2.0196 |
C2···C29 | 3.528 (4) | H1···C20 | 3.3218 |
C2···H1 | 1.9839 | H2···C29 | 3.2812 |
C2···H3 | 2.0120 | H3···C18 | 3.2190 |
C2···H4 | 3.2119 | H3···C19 | 3.1448 |
C2···H24 | 2.8321 | H6···C23 | 2.8281 |
C2···H25 | 3.1980 | H6···C24 | 2.7231 |
C3···C5 | 2.390 (3) | H7···C22 | 3.5541 |
C3···H1 | 3.1923 | H7···C23 | 3.1543 |
C3···H2 | 2.0165 | H7···C24 | 3.3938 |
C3···H4 | 2.0019 | H10···C18 | 3.3417 |
C3···H15 | 3.3453 | H11···Pd2 | 3.1762 |
C3···H16 | 3.4250 | H11···O4 | 3.4430 |
C3···H24 | 3.2998 | H11···N4 | 2.8624 |
C3···H25 | 3.2960 | H11···C17 | 3.2132 |
C4···H2 | 3.2111 | H11···C21 | 3.2670 |
C4···H3 | 2.0003 | H12···N5 | 3.4815 |
C4···H5 | 2.4137 | H12···C14 | 3.5967 |
C5···C6 | 2.507 (3) | H12···C15 | 3.5853 |
C5···H1 | 3.1453 | H12···C22 | 3.5033 |
C5···H3 | 3.2356 | H12···C24 | 3.3316 |
C5···H4 | 2.0414 | H12···C25 | 3.5118 |
C5···H5 | 1.8917 | H13···N5 | 3.1985 |
C6···C8 | 2.396 (4) | H13···C20 | 3.1664 |
C6···C9 | 2.737 (3) | H13···C21 | 3.4474 |
C6···C10 | 2.309 (3) | H13···C24 | 3.5682 |
C6···H5 | 1.9018 | H13···C25 | 3.5403 |
C6···H6 | 2.0279 | H14···O3 | 3.1062 |
C6···H7 | 3.2406 | H14···C18 | 3.4903 |
C6···H9 | 3.1434 | H14···C27 | 3.4253 |
C7···C9 | 2.366 (3) | H15···O4 | 2.9478 |
C7···C10 | 2.691 (3) | H15···C3 | 3.3453 |
C7···C23 | 3.544 (4) | H15···C12 | 3.5016 |
C7···C24 | 3.414 (3) | H15···C32 | 3.5559 |
C7···H5 | 2.4150 | H16···C3 | 3.4250 |
C7···H7 | 2.0047 | H16···C8 | 3.4667 |
C7···H8 | 3.2118 | H16···C9 | 3.2732 |
C7···H19 | 3.3420 | H16···C31 | 3.0806 |
C7···H20 | 3.1440 | H17···O2 | 2.8290 |
C8···C10 | 2.360 (4) | H17···C1 | 3.3628 |
C8···H6 | 1.9969 | H17···C8 | 3.5259 |
C8···H8 | 2.0256 | H17···C9 | 3.2503 |
C8···H9 | 3.1941 | H17···C10 | 3.5196 |
C8···H16 | 3.4667 | H17···C15 | 3.4437 |
C8···H17 | 3.5259 | H17···C16 | 3.5520 |
C9···H6 | 3.2097 | H18···O2 | 2.0660 |
C9···H7 | 2.0246 | H18···C15 | 2.8597 |
C9···H9 | 1.9761 | H18···C16 | 2.5938 |
C9···H16 | 3.2732 | H19···Pd1 | 3.1541 |
C9···H17 | 3.2503 | H19···O1 | 3.1319 |
C10···H7 | 3.2055 | H19···O2 | 2.6892 |
C10···H8 | 2.0016 | H19···O5 | 3.1321 |
C10···H17 | 3.5196 | H19···C7 | 3.3420 |
C10···H23 | 3.3329 | H19···C11 | 3.1057 |
C10···H27 | 2.9577 | H19···C16 | 2.8884 |
C11···C13 | 2.394 (4) | H20···O5 | 2.7263 |
C11···C14 | 2.753 (4) | H20···C7 | 3.1440 |
C11···C15 | 2.406 (4) | H20···C14 | 3.2275 |
C11···H9 | 3.4605 | H20···C15 | 3.4995 |
C11···H10 | 2.0232 | H20···C24 | 3.4976 |
C11···H11 | 3.2352 | H20···C25 | 3.5728 |
C11···H13 | 3.2496 | H22···O4 | 3.5835 |
C11···H19 | 3.1057 | H23···C17 | 3.5330 |
C11···H21 | 3.4618 | H23···C18 | 3.4700 |
C11···H27 | 2.7252 | H24···C2 | 2.8321 |
C12···C14 | 2.388 (5) | H24···C3 | 3.2998 |
C12···C15 | 2.786 (4) | H25···C1 | 3.4017 |
C12···C16 | 2.420 (3) | H25···C2 | 3.1980 |
C12···H11 | 2.0124 | H25···C3 | 3.2960 |
C12···H12 | 3.2239 | H26···N6 | 3.2664 |
C12···H15 | 3.5016 | H26···C18 | 3.4049 |
C12···H21 | 3.0246 | H26···C19 | 2.9879 |
C12···H22 | 3.0658 | H26···C22 | 3.5141 |
C12···H27 | 3.3570 | H26···C26 | 3.4301 |
C13···C15 | 2.414 (4) | H27···C23 | 3.5682 |
| | | |
O1—Pd1—O2 | 84.19 (7) | H9—C10—N3 | 118.1111 |
O1—Pd1—N1 | 177.51 (7) | H9—C10—C9 | 118.0968 |
O1—Pd1—N3 | 90.27 (7) | C12—C11—C16 | 120.6 (2) |
O2—Pd1—N1 | 93.67 (7) | C12—C11—O1 | 121.3 (2) |
O2—Pd1—N3 | 174.44 (6) | C16—C11—O1 | 118.1 (2) |
N1—Pd1—N3 | 91.88 (7) | C13—C12—C11 | 119.8 (3) |
O3—Pd2—O4 | 84.48 (7) | C13—C12—H10 | 120.1158 |
O3—Pd2—N4 | 175.91 (8) | H10—C12—C11 | 120.1225 |
O3—Pd2—N6 | 90.29 (7) | C14—C13—C12 | 119.7 (3) |
O4—Pd2—N4 | 92.99 (7) | C14—C13—H11 | 120.1544 |
O4—Pd2—N6 | 174.77 (7) | H11—C13—C12 | 120.1535 |
N4—Pd2—N6 | 92.22 (8) | C15—C14—C13 | 121.3 (3) |
C11—O1—Pd1 | 109.9 (1) | C15—C14—H12 | 119.3636 |
C16—O2—Pd1 | 108.1 (2) | H12—C14—C13 | 119.3501 |
C27—O3—Pd2 | 109.8 (1) | C16—C15—H13 | 120.3791 |
C32—O4—Pd2 | 109.6 (2) | C16—C15—C14 | 119.2 (3) |
H27—O5—H28 | 104.2843 | H13—C15—C14 | 120.3743 |
C1—N1—Pd1 | 117.6 (1) | C18—C17—N4 | 123.2 (2) |
C1—N1—C5 | 117.7 (2) | C18—C17—H14 | 118.4089 |
C5—N1—Pd1 | 124.7 (1) | H14—C17—N4 | 118.4161 |
C5—N2—C6 | 131.6 (2) | C19—C18—C17 | 118.0 (3) |
C5—N2—H5 | 114.2001 | C19—C18—H15 | 120.9930 |
C6—N2—H5 | 114.2217 | H15—C18—C17 | 120.9854 |
C6—N3—Pd1 | 124.4 (1) | C20—C19—C18 | 119.7 (2) |
C6—N3—C10 | 117.3 (2) | C20—C19—H16 | 120.1360 |
C10—N3—Pd1 | 118.3 (2) | H16—C19—C18 | 120.1201 |
C17—N4—Pd2 | 117.4 (1) | C21—C20—C19 | 120.0 (2) |
C17—N4—C21 | 118.4 (2) | C21—C20—H17 | 119.9757 |
C21—N4—Pd2 | 124.1 (2) | H17—C20—C19 | 119.9751 |
C21—N5—C22 | 132.7 (2) | C23—C22—N5 | 117.7 (2) |
C21—N5—H18 | 113.6510 | C23—C22—N6 | 121.0 (2) |
C22—N5—H18 | 113.6481 | C24—C23—C22 | 119.9 (2) |
C22—N6—Pd2 | 124.0 (2) | C24—C23—H19 | 120.0537 |
C22—N6—C26 | 117.8 (2) | H19—C23—C22 | 120.0513 |
C26—N6—Pd2 | 117.8 (2) | C25—C24—C23 | 119.2 (3) |
C2—C1—N1 | 123.2 (2) | C25—C24—H20 | 120.4222 |
C2—C1—H1 | 118.3886 | H20—C24—C23 | 120.4245 |
H1—C1—N1 | 118.3884 | C26—C25—C24 | 118.2 (2) |
C3—C2—C1 | 118.7 (3) | C26—C25—H21 | 120.8851 |
C3—C2—H2 | 120.6765 | H21—C25—C24 | 120.8829 |
H2—C2—C1 | 120.6671 | H22—C26—N6 | 118.2164 |
C4—C3—C2 | 119.6 (2) | H22—C26—C25 | 118.2173 |
C4—C3—H3 | 120.2158 | C28—C27—C32 | 120.5 (2) |
H3—C3—C2 | 120.2076 | C28—C27—O3 | 121.6 (2) |
C5—C4—C3 | 119.2 (2) | C32—C27—O3 | 117.9 (2) |
C5—C4—H4 | 120.3887 | C29—C28—C27 | 120.0 (3) |
H4—C4—C3 | 120.3835 | C29—C28—H23 | 120.0246 |
C7—C6—N2 | 116.5 (2) | H23—C28—C27 | 120.0103 |
C7—C6—N3 | 121.3 (2) | C30—C29—C28 | 119.9 (3) |
C8—C7—C6 | 120.4 (2) | C30—C29—H24 | 120.0483 |
C8—C7—H6 | 119.8227 | H24—C29—C28 | 120.0519 |
H6—C7—C6 | 119.8178 | C31—C30—C29 | 120.6 (3) |
C9—C8—C7 | 118.7 (3) | C31—C30—H25 | 119.7123 |
C9—C8—H7 | 120.6414 | H25—C30—C29 | 119.7051 |
H7—C8—C7 | 120.6406 | C32—C31—H26 | 119.7921 |
C10—C9—C8 | 118.5 (2) | C32—C31—C30 | 120.4 (3) |
C10—C9—H8 | 120.7379 | H26—C31—C30 | 119.7816 |
H8—C9—C8 | 120.7434 | | |
| | | |
O2—Pd1—O1—C11 | 9.9 (1) | C3—C4—C5—N1 | −4.4 (3) |
O1—Pd1—O2—C16 | −10.1 (1) | C3—C4—C5—N2 | 176.1 (2) |
O1—Pd1—N3—C6 | −166.3 (1) | N2—C6—C7—C8 | 178.8 (2) |
O4—Pd2—O3—C27 | 1.8 (1) | C6—C7—C8—C9 | −0.7 (3) |
O3—Pd2—O4—C32 | −3.1 (1) | C7—C8—C9—C10 | 0.4 (3) |
O3—Pd2—N6—C22 | −158.0 (2) | C8—C9—C10—N3 | −0.1 (3) |
Pd1—O1—C11—C12 | 171.9 (2) | O1—C11—C12—C13 | −179.5 (2) |
Pd1—O2—C16—C11 | 8.9 (2) | O1—C11—C16—O2 | −0.9 (3) |
Pd1—O2—C16—C15 | −172.5 (2) | O1—C11—C16—C15 | −179.5 (2) |
Pd2—O3—C27—C28 | 179.5 (2) | C11—C12—C13—C14 | −0.8 (4) |
Pd2—O4—C32—C27 | 3.9 (2) | C12—C13—C14—C15 | 0.4 (4) |
Pd2—O4—C32—C31 | −175.8 (2) | C13—C14—C15—C16 | 0.5 (4) |
Pd1—N1—C1—C2 | 175.8 (2) | C14—C15—C16—O2 | −179.6 (2) |
Pd1—N1—C5—N2 | 7.6 (3) | C14—C15—C16—C11 | −1.0 (3) |
Pd1—N1—C5—C4 | −171.8 (2) | N4—C17—C18—C19 | 1.9 (4) |
C6—N2—C5—N1 | 12.8 (3) | C17—C18—C19—C20 | −1.0 (4) |
C6—N2—C5—C4 | −167.8 (2) | C18—C19—C20—C21 | −0.5 (4) |
C5—N2—C6—N3 | −16.9 (3) | C19—C20—C21—N4 | 1.1 (4) |
Pd1—N3—C6—N2 | −0.2 (3) | C19—C20—C21—N5 | −177.5 (2) |
Pd1—N3—C10—C9 | −178.2 (2) | N5—C22—C23—C24 | −177.6 (2) |
Pd2—N4—C17—C18 | 174.5 (2) | C22—C23—C24—C25 | 2.8 (4) |
Pd2—N4—C21—N5 | 2.8 (3) | C23—C24—C25—C26 | −4.7 (4) |
Pd2—N4—C21—C20 | −175.7 (2) | C24—C25—C26—N6 | 1.5 (4) |
C22—N5—C21—N4 | 10.8 (4) | O3—C27—C28—C29 | −179.3 (2) |
C22—N5—C21—C20 | −170.5 (2) | O3—C27—C32—O4 | −2.6 (3) |
C21—N5—C22—N6 | −5.0 (4) | O3—C27—C32—C31 | 177.1 (2) |
Pd2—N6—C22—N5 | −13.3 (3) | C27—C28—C29—C30 | 1.4 (4) |
Pd2—N6—C26—C25 | −169.0 (2) | C28—C29—C30—C31 | −1.1 (4) |
N1—C1—C2—C3 | −3.2 (4) | C29—C30—C31—C32 | −1.1 (4) |
C1—C2—C3—C4 | 3.8 (4) | C30—C31—C32—O4 | −177.3 (2) |
C2—C3—C4—C5 | −0.2 (4) | C30—C31—C32—C27 | 2.9 (4) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H5···O5i | 0.86 | 1.97 | 2.805 (3) | 163 |
N5—H18···O2ii | 0.86 | 2.07 | 2.919 (2) | 170 |
O5—H27···O1 | 0.92 | 1.83 | 2.757 (2) | 179 |
O5—H28···O3 | 0.91 | 1.82 | 2.721 (2) | 167 |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+1, −y, −z+1. |
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