Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301609X/ac6053sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680301609X/ac6053Isup2.hkl |
CCDC reference: 221650
Data collection: SMART-NT (Bruker, 1999); cell refinement: SAINT-Plus-NT (Bruker, 1999); data reduction: SAINT-Plus-NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: ATOMS (Dowty, 2001); software used to prepare material for publication: SHELXTL (Sheldrick, 1997b).
[Pd(C14H12N4O2)]·H2O·0.5CHCl3 | Z = 4 |
Mr = 452.38 | F(000) = 900 |
Triclinic, P1 | Dx = 1.893 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.3145 (5) Å | Cell parameters from 6121 reflections |
b = 10.2252 (6) Å | θ = 2.4–26.4° |
c = 21.7212 (14) Å | µ = 1.44 mm−1 |
α = 80.233 (2)° | T = 150 K |
β = 89.126 (2)° | Irregular, yellow |
γ = 82.418 (2)° | 0.32 × 0.22 × 0.16 mm |
V = 1586.99 (18) Å3 |
Bruker SMART APEX CCD diffractometer | 6448 independent reflections |
Radiation source: sealed tube | 6116 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ω scans | θmax = 26.4°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 1999) | h = −9→9 |
Tmin = 0.649, Tmax = 0.794 | k = −12→12 |
14485 measured reflections | l = −27→27 |
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)] = 0.024 | Hydrogen site location: geom & difmap |
wR(F2) = 0.062 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0295P)2 + 1.3475P] where P = (Fo2 + 2Fc2)/3 |
6448 reflections | (Δ/σ)max = 0.001 |
449 parameters | Δρmax = 0.54 e Å−3 |
6 restraints | Δρmin = −0.59 e Å−3 |
Geometry. ## Least-squares planes Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) # 6.7321 (0.0008) x - 2.5582 (0.0021) y - 3.4504 (0.0048) z = 0.3637 (0.0015) * 0.1093 (0.0005) Pd1 * 0.0356 (0.0022) C1 * 0.0019 (0.0022) C2 * -0.0210 (0.0022) C3 * -0.0330 (0.0022) C4 * -0.0077 (0.0020) C5 * -0.0195 (0.0022) C6 * -0.0295 (0.0021) C7 * 0.0230 (0.0022) C8 * 0.0720 (0.0023) C9 * 0.0420 (0.0021) C10 * -0.0240 (0.0023) C11 * -0.1008 (0.0023) C12 * -0.1087 (0.0022) C13 * -0.0110 (0.0022) C14 * 0.0341 (0.0018) N1 * 0.0781 (0.0019) N2 * 0.1095 (0.0019) N3 * 0.0624 (0.0018) N4 * -0.1836 (0.0018) O1 * -0.0290 (0.0019) O2 Rms deviation of fitted atoms = 0.0703 # 6.6331 (0.0008) x + 5.2942 (0.0018) y + 4.5122 (0.0044) z = 9.1975 (0.0028) Angle to previous plane (with approximate e.s.d.) = 47.94 (0.01) * -0.0058 (0.0004) Pd2 * 0.0465 (0.0021) C15 * 0.0275 (0.0020) C16 * -0.0177 (0.0020) C17 * -0.0443 (0.0021) C18 * -0.0342 (0.0020) C19 * -0.0882 (0.0022) C20 * 0.0289 (0.0019) C21 * 0.0249 (0.0020) C22 * -0.1035 (0.0022) C23 * -0.0444 (0.0020) C24 * -0.0998 (0.0021) C25 * -0.0277 (0.0020) C26 * 0.0933 (0.0020) C27 * 0.1109 (0.0021) C28 * 0.0116 (0.0018) N5 * -0.0731 (0.0019) N6 * -0.0654 (0.0019) N7 * 0.0392 (0.0018) N8 * 0.1233 (0.0016) O3 * 0.0980 (0.0017) O4 Rms deviation of fitted atoms = 0.0677 ##### 6.6681 (0.0028) x - 2.7182 (0.0090) y - 3.9365 (0.0210) z = 0.3152 (0.0032) * 0.0042 (0.0015) N1 * 0.0007 (0.0016) C1 * -0.0056 (0.0017) C2 * 0.0056 (0.0017) C3 * -0.0008 (0.0017) C4 * -0.0041 (0.0015) C5 Rms deviation of fitted atoms = 0.0040 # 6.7765 (0.0028) x - 2.5375 (0.0101) y - 2.0415 (0.0209) z = 0.5851 (0.0086) Angle to previous plane (with approximate e.s.d.) = 5.06 (0.10) * 0.0042 (0.0015) N4 * -0.0099 (0.0016) C10 * 0.0054 (0.0018) C11 * 0.0044 (0.0018) C12 * -0.0100 (0.0018) C13 * 0.0059 (0.0017) C14 Rms deviation of fitted atoms = 0.0071 ##### 6.6606 (0.0028) x + 5.3077 (0.0079) y + 3.7922 (0.0204) z = 8.8967 (0.0138) * -0.0014 (0.0014) N5 * 0.0035 (0.0016) C15 * -0.0021 (0.0016) C16 * -0.0013 (0.0016) C17 * 0.0033 (0.0016) C18 * -0.0021 (0.0015) C19 Rms deviation of fitted atoms = 0.0024 # 6.8461 (0.0025) x + 4.5985 (0.0088) y + 4.1992 (0.0192) z = 8.5400 (0.0140) Angle to previous plane (with approximate e.s.d.) = 4.79 (0.09) * -0.0077 (0.0014) N8 * 0.0128 (0.0015) C24 * -0.0064 (0.0016) C25 * -0.0048 (0.0016) C26 * 0.0098 (0.0016) C27 * -0.0038 (0.0016) C28 Rms deviation of fitted atoms = 0.0081 ##### 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. |
x | y | z | Uiso*/Ueq | ||
Pd1 | 0.29493 (2) | 0.582220 (16) | 0.006690 (7) | 0.01718 (6) | |
C1 | 0.1961 (3) | 0.2943 (2) | 0.04870 (12) | 0.0245 (5) | |
H1 | 0.2245 | 0.3032 | 0.0902 | 0.029* | |
C2 | 0.1409 (4) | 0.1759 (3) | 0.03850 (13) | 0.0306 (6) | |
H2 | 0.1302 | 0.1052 | 0.0723 | 0.037* | |
C3 | 0.1014 (3) | 0.1622 (2) | −0.02181 (14) | 0.0309 (6) | |
H3 | 0.0651 | 0.0811 | −0.0302 | 0.037* | |
C4 | 0.1150 (3) | 0.2673 (3) | −0.06970 (13) | 0.0275 (5) | |
H4 | 0.0869 | 0.2595 | −0.1114 | 0.033* | |
C5 | 0.1700 (3) | 0.3849 (2) | −0.05679 (11) | 0.0208 (5) | |
C6 | 0.1859 (3) | 0.5011 (2) | −0.10862 (11) | 0.0236 (5) | |
H6C | 0.2716 | 0.4722 | −0.1409 | 0.028* | |
H6D | 0.0637 | 0.5338 | −0.1285 | 0.028* | |
C7 | 0.2673 (3) | 0.7275 (2) | −0.11457 (11) | 0.0234 (5) | |
C8 | 0.3323 (3) | 0.8223 (2) | −0.07333 (12) | 0.0247 (5) | |
C9 | 0.3989 (3) | 0.8311 (2) | 0.03579 (12) | 0.0262 (5) | |
H9A | 0.3105 | 0.9133 | 0.0359 | 0.031* | |
H9B | 0.5243 | 0.8573 | 0.0296 | 0.031* | |
C10 | 0.3905 (3) | 0.7381 (2) | 0.09720 (12) | 0.0241 (5) | |
C11 | 0.4248 (4) | 0.7784 (3) | 0.15324 (13) | 0.0327 (6) | |
H11 | 0.4588 | 0.8650 | 0.1532 | 0.039* | |
C12 | 0.4097 (4) | 0.6938 (3) | 0.20875 (13) | 0.0360 (6) | |
H12 | 0.4328 | 0.7209 | 0.2473 | 0.043* | |
C13 | 0.3603 (3) | 0.5685 (3) | 0.20750 (12) | 0.0318 (6) | |
H13 | 0.3462 | 0.5088 | 0.2453 | 0.038* | |
C14 | 0.3315 (3) | 0.5311 (3) | 0.15089 (11) | 0.0250 (5) | |
H14 | 0.3006 | 0.4439 | 0.1505 | 0.030* | |
N1 | 0.2115 (3) | 0.39790 (19) | 0.00236 (9) | 0.0201 (4) | |
N2 | 0.2538 (3) | 0.6069 (2) | −0.08289 (9) | 0.0224 (4) | |
N3 | 0.3534 (3) | 0.76409 (19) | −0.01415 (10) | 0.0232 (4) | |
N4 | 0.3455 (3) | 0.6133 (2) | 0.09597 (9) | 0.0206 (4) | |
O1 | 0.2308 (3) | 0.76720 (19) | −0.17076 (8) | 0.0358 (4) | |
O2 | 0.3570 (3) | 0.93793 (19) | −0.09586 (10) | 0.0387 (5) | |
Pd2 | 0.31091 (2) | 0.935265 (15) | 0.482672 (7) | 0.01551 (5) | |
C15 | 0.0897 (3) | 1.2047 (2) | 0.50333 (11) | 0.0205 (4) | |
H15 | 0.0940 | 1.1697 | 0.5468 | 0.025* | |
C16 | −0.0011 (3) | 1.3317 (2) | 0.48363 (11) | 0.0229 (5) | |
H16 | −0.0589 | 1.3824 | 0.5131 | 0.028* | |
C17 | −0.0072 (3) | 1.3845 (2) | 0.42056 (12) | 0.0233 (5) | |
H17 | −0.0688 | 1.4718 | 0.4060 | 0.028* | |
C18 | 0.0787 (3) | 1.3072 (2) | 0.37906 (11) | 0.0214 (5) | |
H18 | 0.0773 | 1.3414 | 0.3356 | 0.026* | |
C19 | 0.1670 (3) | 1.1794 (2) | 0.40149 (10) | 0.0185 (4) | |
C20 | 0.2582 (3) | 1.0927 (2) | 0.35713 (10) | 0.0196 (4) | |
H20A | 0.1662 | 1.0780 | 0.3269 | 0.024* | |
H20B | 0.3559 | 1.1376 | 0.3335 | 0.024* | |
C21 | 0.4439 (3) | 0.8722 (2) | 0.36892 (10) | 0.0180 (4) | |
C22 | 0.5091 (3) | 0.7473 (2) | 0.41868 (11) | 0.0193 (4) | |
C23 | 0.4807 (3) | 0.6628 (2) | 0.53109 (10) | 0.0201 (4) | |
H23A | 0.6151 | 0.6348 | 0.5366 | 0.024* | |
H23B | 0.4213 | 0.5828 | 0.5275 | 0.024* | |
C24 | 0.4042 (3) | 0.7225 (2) | 0.58660 (10) | 0.0183 (4) | |
C25 | 0.4154 (3) | 0.6471 (2) | 0.64637 (11) | 0.0223 (5) | |
H25 | 0.4704 | 0.5563 | 0.6527 | 0.027* | |
C26 | 0.3462 (3) | 0.7047 (2) | 0.69646 (11) | 0.0234 (5) | |
H26 | 0.3537 | 0.6542 | 0.7375 | 0.028* | |
C27 | 0.2655 (3) | 0.8376 (2) | 0.68608 (11) | 0.0221 (5) | |
H27 | 0.2190 | 0.8800 | 0.7198 | 0.026* | |
C28 | 0.2544 (3) | 0.9062 (2) | 0.62565 (11) | 0.0204 (5) | |
H28 | 0.1972 | 0.9965 | 0.6184 | 0.024* | |
N5 | 0.1725 (2) | 1.12833 (18) | 0.46343 (9) | 0.0179 (4) | |
N6 | 0.3377 (3) | 0.96565 (18) | 0.39279 (9) | 0.0192 (4) | |
N7 | 0.4455 (3) | 0.76198 (18) | 0.47499 (9) | 0.0199 (4) | |
N8 | 0.3210 (2) | 0.85142 (18) | 0.57619 (9) | 0.0175 (4) | |
O3 | 0.4915 (2) | 0.87758 (16) | 0.31343 (7) | 0.0236 (3) | |
O4 | 0.6081 (2) | 0.64925 (16) | 0.40431 (8) | 0.0273 (4) | |
O5 | 0.1156 (3) | 0.2850 (2) | 0.21671 (10) | 0.0396 (5) | |
H5A | 0.016 (3) | 0.263 (3) | 0.2054 (17) | 0.054 (11)* | |
H5B | 0.199 (4) | 0.221 (3) | 0.2139 (19) | 0.066 (13)* | |
O6 | 0.4016 (3) | 0.0808 (2) | 0.20769 (10) | 0.0411 (5) | |
H6A | 0.427 (4) | 0.025 (3) | 0.2395 (10) | 0.043 (9)* | |
H6B | 0.489 (4) | 0.095 (4) | 0.1834 (15) | 0.070 (13)* | |
C29 | −0.1266 (3) | 0.7463 (2) | 0.28434 (12) | 0.0264 (5) | |
H29 | −0.2459 | 0.7547 | 0.3074 | 0.032* | |
Cl1 | −0.13785 (12) | 0.87710 (7) | 0.21978 (3) | 0.04359 (18) | |
Cl2 | −0.09492 (9) | 0.58953 (6) | 0.25947 (3) | 0.03162 (14) | |
Cl3 | 0.05370 (10) | 0.75798 (9) | 0.33562 (3) | 0.04393 (18) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd1 | 0.01880 (9) | 0.01703 (9) | 0.01537 (9) | −0.00191 (6) | −0.00091 (6) | −0.00205 (6) |
C1 | 0.0232 (12) | 0.0234 (12) | 0.0255 (12) | −0.0006 (9) | 0.0026 (9) | −0.0024 (10) |
C2 | 0.0278 (13) | 0.0219 (12) | 0.0409 (15) | −0.0021 (10) | 0.0078 (11) | −0.0032 (11) |
C3 | 0.0263 (13) | 0.0207 (12) | 0.0484 (17) | −0.0042 (10) | 0.0027 (11) | −0.0130 (11) |
C4 | 0.0234 (12) | 0.0289 (13) | 0.0328 (14) | −0.0022 (10) | −0.0011 (10) | −0.0137 (11) |
C5 | 0.0157 (10) | 0.0241 (12) | 0.0226 (12) | 0.0014 (9) | 0.0007 (9) | −0.0070 (9) |
C6 | 0.0246 (12) | 0.0277 (12) | 0.0188 (11) | −0.0010 (9) | −0.0021 (9) | −0.0067 (9) |
C7 | 0.0218 (11) | 0.0251 (12) | 0.0206 (12) | 0.0008 (9) | 0.0042 (9) | 0.0006 (9) |
C8 | 0.0205 (11) | 0.0246 (12) | 0.0265 (13) | −0.0015 (9) | 0.0016 (9) | 0.0016 (10) |
C9 | 0.0245 (12) | 0.0200 (11) | 0.0346 (14) | −0.0020 (9) | −0.0071 (10) | −0.0063 (10) |
C10 | 0.0166 (11) | 0.0260 (12) | 0.0305 (13) | 0.0007 (9) | −0.0008 (9) | −0.0096 (10) |
C11 | 0.0294 (13) | 0.0372 (15) | 0.0353 (15) | −0.0012 (11) | −0.0039 (11) | −0.0192 (12) |
C12 | 0.0290 (13) | 0.0567 (18) | 0.0272 (14) | −0.0022 (12) | −0.0013 (11) | −0.0231 (13) |
C13 | 0.0252 (12) | 0.0493 (16) | 0.0197 (12) | −0.0005 (11) | 0.0006 (10) | −0.0056 (11) |
C14 | 0.0219 (11) | 0.0323 (13) | 0.0205 (12) | −0.0033 (10) | −0.0006 (9) | −0.0032 (10) |
N1 | 0.0182 (9) | 0.0199 (9) | 0.0220 (10) | −0.0007 (7) | 0.0004 (7) | −0.0044 (8) |
N2 | 0.0265 (10) | 0.0248 (10) | 0.0160 (9) | −0.0028 (8) | 0.0000 (8) | −0.0039 (8) |
N3 | 0.0252 (10) | 0.0180 (9) | 0.0264 (11) | −0.0038 (8) | −0.0014 (8) | −0.0032 (8) |
N4 | 0.0175 (9) | 0.0244 (10) | 0.0202 (10) | −0.0011 (7) | −0.0013 (7) | −0.0056 (8) |
O1 | 0.0494 (12) | 0.0366 (10) | 0.0181 (9) | −0.0031 (9) | 0.0006 (8) | 0.0026 (8) |
O2 | 0.0509 (12) | 0.0251 (10) | 0.0382 (11) | −0.0116 (8) | −0.0059 (9) | 0.0059 (8) |
Pd2 | 0.01805 (9) | 0.01539 (9) | 0.01291 (9) | −0.00153 (6) | 0.00101 (6) | −0.00250 (6) |
C15 | 0.0220 (11) | 0.0219 (11) | 0.0181 (11) | −0.0033 (9) | 0.0004 (9) | −0.0041 (9) |
C16 | 0.0226 (11) | 0.0212 (11) | 0.0263 (12) | −0.0018 (9) | 0.0003 (9) | −0.0085 (9) |
C17 | 0.0217 (11) | 0.0184 (11) | 0.0294 (13) | −0.0016 (9) | −0.0034 (9) | −0.0032 (9) |
C18 | 0.0224 (11) | 0.0212 (11) | 0.0196 (11) | −0.0026 (9) | −0.0021 (9) | −0.0012 (9) |
C19 | 0.0165 (10) | 0.0215 (11) | 0.0179 (11) | −0.0042 (8) | −0.0006 (8) | −0.0033 (9) |
C20 | 0.0223 (11) | 0.0211 (11) | 0.0146 (10) | −0.0021 (9) | −0.0011 (8) | −0.0012 (9) |
C21 | 0.0179 (10) | 0.0200 (11) | 0.0180 (11) | −0.0064 (8) | 0.0011 (8) | −0.0056 (9) |
C22 | 0.0204 (11) | 0.0184 (11) | 0.0204 (11) | −0.0055 (9) | 0.0004 (9) | −0.0048 (9) |
C23 | 0.0228 (11) | 0.0180 (11) | 0.0187 (11) | −0.0011 (9) | 0.0009 (9) | −0.0021 (9) |
C24 | 0.0177 (10) | 0.0184 (11) | 0.0200 (11) | −0.0050 (8) | −0.0006 (8) | −0.0044 (9) |
C25 | 0.0258 (12) | 0.0198 (11) | 0.0202 (11) | −0.0022 (9) | −0.0016 (9) | −0.0010 (9) |
C26 | 0.0276 (12) | 0.0272 (12) | 0.0149 (11) | −0.0061 (10) | −0.0011 (9) | 0.0001 (9) |
C27 | 0.0243 (12) | 0.0251 (12) | 0.0182 (11) | −0.0057 (9) | 0.0017 (9) | −0.0061 (9) |
C28 | 0.0212 (11) | 0.0202 (11) | 0.0207 (11) | −0.0038 (9) | 0.0004 (9) | −0.0056 (9) |
N5 | 0.0179 (9) | 0.0188 (9) | 0.0175 (9) | −0.0025 (7) | 0.0000 (7) | −0.0040 (7) |
N6 | 0.0241 (10) | 0.0179 (9) | 0.0146 (9) | −0.0007 (7) | 0.0011 (7) | −0.0018 (7) |
N7 | 0.0242 (10) | 0.0173 (9) | 0.0173 (9) | 0.0001 (7) | 0.0019 (7) | −0.0025 (7) |
N8 | 0.0184 (9) | 0.0181 (9) | 0.0156 (9) | −0.0027 (7) | −0.0001 (7) | −0.0017 (7) |
O3 | 0.0292 (9) | 0.0249 (8) | 0.0166 (8) | −0.0018 (7) | 0.0039 (7) | −0.0048 (7) |
O4 | 0.0358 (10) | 0.0211 (8) | 0.0236 (9) | 0.0018 (7) | 0.0076 (7) | −0.0048 (7) |
O5 | 0.0397 (12) | 0.0348 (11) | 0.0408 (12) | −0.0013 (9) | −0.0015 (10) | 0.0012 (9) |
O6 | 0.0451 (12) | 0.0426 (12) | 0.0280 (11) | 0.0061 (10) | 0.0087 (9) | 0.0059 (9) |
C29 | 0.0269 (12) | 0.0289 (13) | 0.0247 (12) | −0.0045 (10) | 0.0018 (10) | −0.0081 (10) |
Cl1 | 0.0623 (5) | 0.0313 (3) | 0.0354 (4) | −0.0028 (3) | 0.0091 (3) | −0.0039 (3) |
Cl2 | 0.0387 (3) | 0.0266 (3) | 0.0298 (3) | −0.0015 (2) | −0.0022 (3) | −0.0073 (2) |
Cl3 | 0.0362 (4) | 0.0681 (5) | 0.0347 (4) | −0.0169 (3) | −0.0010 (3) | −0.0214 (4) |
Pd1—N3 | 1.9402 (19) | C15—N5 | 1.348 (3) |
Pd1—N2 | 1.9420 (19) | C15—C16 | 1.379 (3) |
Pd1—N4 | 2.0640 (19) | C15—H15 | 0.9500 |
Pd1—N1 | 2.0734 (19) | C16—C17 | 1.384 (3) |
C1—N1 | 1.347 (3) | C16—H16 | 0.9500 |
C1—C2 | 1.378 (4) | C17—C18 | 1.388 (3) |
C1—H1 | 0.9500 | C17—H17 | 0.9500 |
C2—C3 | 1.380 (4) | C18—C19 | 1.390 (3) |
C2—H2 | 0.9500 | C18—H18 | 0.9500 |
C3—C4 | 1.376 (4) | C19—N5 | 1.357 (3) |
C3—H3 | 0.9500 | C19—C20 | 1.508 (3) |
C4—C5 | 1.390 (3) | C20—N6 | 1.449 (3) |
C4—H4 | 0.9500 | C20—H20A | 0.9900 |
C5—N1 | 1.357 (3) | C20—H20B | 0.9900 |
C5—C6 | 1.507 (3) | C21—O3 | 1.244 (3) |
C6—N2 | 1.444 (3) | C21—N6 | 1.322 (3) |
C6—H6C | 0.9900 | C21—C22 | 1.554 (3) |
C6—H6D | 0.9900 | C22—O4 | 1.239 (3) |
C7—O1 | 1.241 (3) | C22—N7 | 1.327 (3) |
C7—N2 | 1.321 (3) | C23—N7 | 1.450 (3) |
C7—C8 | 1.549 (4) | C23—C24 | 1.510 (3) |
C8—O2 | 1.236 (3) | C23—H23A | 0.9900 |
C8—N3 | 1.324 (3) | C23—H23B | 0.9900 |
C9—N3 | 1.442 (3) | C24—N8 | 1.360 (3) |
C9—C10 | 1.507 (4) | C24—C25 | 1.391 (3) |
C9—H9A | 0.9900 | C25—C26 | 1.382 (3) |
C9—H9B | 0.9900 | C25—H25 | 0.9500 |
C10—N4 | 1.364 (3) | C26—C27 | 1.390 (3) |
C10—C11 | 1.386 (4) | C26—H26 | 0.9500 |
C11—C12 | 1.372 (4) | C27—C28 | 1.378 (3) |
C11—H11 | 0.9500 | C27—H27 | 0.9500 |
C12—C13 | 1.381 (4) | C28—N8 | 1.350 (3) |
C12—H12 | 0.9500 | C28—H28 | 0.9500 |
C13—C14 | 1.375 (3) | O5—H5A | 0.841 (18) |
C13—H13 | 0.9500 | O5—H5B | 0.844 (18) |
C14—N4 | 1.348 (3) | O6—H6A | 0.824 (14) |
C14—H14 | 0.9500 | O6—H6B | 0.835 (14) |
Pd2—N6 | 1.9352 (18) | C29—Cl1 | 1.761 (3) |
Pd2—N7 | 1.9420 (18) | C29—Cl2 | 1.763 (2) |
Pd2—N8 | 2.0648 (18) | C29—Cl3 | 1.768 (3) |
Pd2—N5 | 2.0741 (18) | C29—H29 | 1.0000 |
N3—Pd1—N2 | 82.09 (8) | N7—Pd2—N5 | 163.67 (8) |
N3—Pd1—N4 | 81.72 (8) | N8—Pd2—N5 | 114.46 (7) |
N2—Pd1—N4 | 163.65 (8) | N5—C15—C16 | 122.6 (2) |
N3—Pd1—N1 | 163.68 (8) | N5—C15—H15 | 118.7 |
N2—Pd1—N1 | 81.70 (8) | C16—C15—H15 | 118.7 |
N4—Pd1—N1 | 114.40 (8) | C15—C16—C17 | 119.3 (2) |
N1—C1—C2 | 122.8 (2) | C15—C16—H16 | 120.3 |
N1—C1—H1 | 118.6 | C17—C16—H16 | 120.3 |
C2—C1—H1 | 118.6 | C16—C17—C18 | 118.6 (2) |
C1—C2—C3 | 118.7 (2) | C16—C17—H17 | 120.7 |
C1—C2—H2 | 120.6 | C18—C17—H17 | 120.7 |
C3—C2—H2 | 120.6 | C17—C18—C19 | 119.6 (2) |
C4—C3—C2 | 119.3 (2) | C17—C18—H18 | 120.2 |
C4—C3—H3 | 120.3 | C19—C18—H18 | 120.2 |
C2—C3—H3 | 120.3 | N5—C19—C18 | 121.5 (2) |
C3—C4—C5 | 119.6 (2) | N5—C19—C20 | 118.01 (19) |
C3—C4—H4 | 120.2 | C18—C19—C20 | 120.5 (2) |
C5—C4—H4 | 120.2 | N6—C20—C19 | 108.85 (18) |
N1—C5—C4 | 121.2 (2) | N6—C20—H20A | 109.9 |
N1—C5—C6 | 118.4 (2) | C19—C20—H20A | 109.9 |
C4—C5—C6 | 120.5 (2) | N6—C20—H20B | 109.9 |
N2—C6—C5 | 108.97 (19) | C19—C20—H20B | 109.9 |
N2—C6—H6C | 109.9 | H20A—C20—H20B | 108.3 |
C5—C6—H6C | 109.9 | O3—C21—N6 | 126.5 (2) |
N2—C6—H6D | 109.9 | O3—C21—C22 | 120.98 (19) |
C5—C6—H6D | 109.9 | N6—C21—C22 | 112.51 (19) |
H6C—C6—H6D | 108.3 | O4—C22—N7 | 127.2 (2) |
O1—C7—N2 | 126.5 (2) | O4—C22—C21 | 121.2 (2) |
O1—C7—C8 | 120.9 (2) | N7—C22—C21 | 111.61 (18) |
N2—C7—C8 | 112.6 (2) | N7—C23—C24 | 109.03 (18) |
O2—C8—N3 | 127.1 (2) | N7—C23—H23A | 109.9 |
O2—C8—C7 | 121.1 (2) | C24—C23—H23A | 109.9 |
N3—C8—C7 | 111.8 (2) | N7—C23—H23B | 109.9 |
N3—C9—C10 | 109.15 (19) | C24—C23—H23B | 109.9 |
N3—C9—H9A | 109.9 | H23A—C23—H23B | 108.3 |
C10—C9—H9A | 109.9 | N8—C24—C25 | 121.1 (2) |
N3—C9—H9B | 109.9 | N8—C24—C23 | 117.99 (19) |
C10—C9—H9B | 109.9 | C25—C24—C23 | 120.9 (2) |
H9A—C9—H9B | 108.3 | C26—C25—C24 | 119.7 (2) |
N4—C10—C11 | 121.0 (2) | C26—C25—H25 | 120.1 |
N4—C10—C9 | 117.8 (2) | C24—C25—H25 | 120.1 |
C11—C10—C9 | 121.2 (2) | C25—C26—C27 | 119.2 (2) |
C12—C11—C10 | 120.2 (3) | C25—C26—H26 | 120.4 |
C12—C11—H11 | 119.9 | C27—C26—H26 | 120.4 |
C10—C11—H11 | 119.9 | C28—C27—C26 | 118.4 (2) |
C11—C12—C13 | 118.7 (2) | C28—C27—H27 | 120.8 |
C11—C12—H12 | 120.6 | C26—C27—H27 | 120.8 |
C13—C12—H12 | 120.6 | N8—C28—C27 | 123.2 (2) |
C14—C13—C12 | 119.3 (3) | N8—C28—H28 | 118.4 |
C14—C13—H13 | 120.4 | C27—C28—H28 | 118.4 |
C12—C13—H13 | 120.4 | C15—N5—C19 | 118.35 (19) |
N4—C14—C13 | 122.6 (2) | C15—N5—Pd2 | 128.92 (16) |
N4—C14—H14 | 118.7 | C19—N5—Pd2 | 112.73 (14) |
C13—C14—H14 | 118.7 | C21—N6—C20 | 124.29 (19) |
C1—N1—C5 | 118.3 (2) | C21—N6—Pd2 | 116.45 (15) |
C1—N1—Pd1 | 129.33 (16) | C20—N6—Pd2 | 118.92 (14) |
C5—N1—Pd1 | 112.33 (15) | C22—N7—C23 | 124.93 (19) |
C7—N2—C6 | 124.5 (2) | C22—N7—Pd2 | 116.57 (15) |
C7—N2—Pd1 | 116.36 (16) | C23—N7—Pd2 | 118.33 (14) |
C6—N2—Pd1 | 118.55 (15) | C28—N8—C24 | 118.39 (19) |
C8—N3—C9 | 124.2 (2) | C28—N8—Pd2 | 128.88 (15) |
C8—N3—Pd1 | 116.86 (16) | C24—N8—Pd2 | 112.72 (14) |
C9—N3—Pd1 | 118.62 (16) | H5A—O5—H5B | 108 (3) |
C14—N4—C10 | 118.1 (2) | H6A—O6—H6B | 116 (3) |
C14—N4—Pd1 | 129.10 (17) | Cl1—C29—Cl2 | 110.62 (14) |
C10—N4—Pd1 | 112.69 (16) | Cl1—C29—Cl3 | 110.38 (14) |
N6—Pd2—N7 | 82.19 (8) | Cl2—C29—Cl3 | 110.34 (14) |
N6—Pd2—N8 | 164.04 (8) | Cl1—C29—H29 | 108.5 |
N7—Pd2—N8 | 81.85 (7) | Cl2—C29—H29 | 108.5 |
N6—Pd2—N5 | 81.49 (7) | Cl3—C29—H29 | 108.5 |
N1—C1—C2—C3 | 0.7 (4) | N5—C15—C16—C17 | −0.6 (4) |
C1—C2—C3—C4 | −1.1 (4) | C15—C16—C17—C18 | 0.1 (3) |
C2—C3—C4—C5 | 0.7 (4) | C16—C17—C18—C19 | 0.4 (3) |
C3—C4—C5—N1 | 0.3 (3) | C17—C18—C19—N5 | −0.5 (3) |
C3—C4—C5—C6 | 180.0 (2) | C17—C18—C19—C20 | 178.9 (2) |
N1—C5—C6—N2 | 2.5 (3) | N5—C19—C20—N6 | −0.2 (3) |
C4—C5—C6—N2 | −177.2 (2) | C18—C19—C20—N6 | −179.6 (2) |
O1—C7—C8—O2 | −3.2 (4) | O3—C21—C22—O4 | −0.9 (3) |
N2—C7—C8—O2 | 178.1 (2) | N6—C21—C22—O4 | 179.2 (2) |
O1—C7—C8—N3 | 176.1 (2) | O3—C21—C22—N7 | 179.1 (2) |
N2—C7—C8—N3 | −2.6 (3) | N6—C21—C22—N7 | −0.7 (3) |
N3—C9—C10—N4 | 0.4 (3) | N7—C23—C24—N8 | −0.4 (3) |
N3—C9—C10—C11 | −178.7 (2) | N7—C23—C24—C25 | 178.4 (2) |
N4—C10—C11—C12 | −1.5 (4) | N8—C24—C25—C26 | −2.0 (3) |
C9—C10—C11—C12 | 177.6 (2) | C23—C24—C25—C26 | 179.2 (2) |
C10—C11—C12—C13 | 0.1 (4) | C24—C25—C26—C27 | 0.3 (4) |
C11—C12—C13—C14 | 1.4 (4) | C25—C26—C27—C28 | 1.2 (3) |
C12—C13—C14—N4 | −1.6 (4) | C26—C27—C28—N8 | −1.2 (3) |
C2—C1—N1—C5 | 0.3 (3) | C16—C15—N5—C19 | 0.5 (3) |
C2—C1—N1—Pd1 | −178.97 (17) | C16—C15—N5—Pd2 | −178.70 (17) |
C4—C5—N1—C1 | −0.7 (3) | C18—C19—N5—C15 | 0.1 (3) |
C6—C5—N1—C1 | 179.6 (2) | C20—C19—N5—C15 | −179.3 (2) |
C4—C5—N1—Pd1 | 178.63 (17) | C18—C19—N5—Pd2 | 179.37 (17) |
C6—C5—N1—Pd1 | −1.1 (2) | C20—C19—N5—Pd2 | 0.0 (2) |
N3—Pd1—N1—C1 | −174.7 (2) | N6—Pd2—N5—C15 | 179.4 (2) |
N2—Pd1—N1—C1 | 178.8 (2) | N7—Pd2—N5—C15 | 176.9 (2) |
N4—Pd1—N1—C1 | −4.2 (2) | N8—Pd2—N5—C15 | −0.1 (2) |
N3—Pd1—N1—C5 | 6.0 (4) | N6—Pd2—N5—C19 | 0.21 (15) |
N2—Pd1—N1—C5 | −0.43 (15) | N7—Pd2—N5—C19 | −2.3 (4) |
N4—Pd1—N1—C5 | 176.57 (14) | N8—Pd2—N5—C19 | −179.29 (14) |
O1—C7—N2—C6 | −2.5 (4) | O3—C21—N6—C20 | −0.2 (4) |
C8—C7—N2—C6 | 176.1 (2) | C22—C21—N6—C20 | 179.70 (19) |
O1—C7—N2—Pd1 | −173.3 (2) | O3—C21—N6—Pd2 | −173.41 (18) |
C8—C7—N2—Pd1 | 5.4 (3) | C22—C21—N6—Pd2 | 6.4 (2) |
C5—C6—N2—C7 | −173.4 (2) | C19—C20—N6—C21 | −172.7 (2) |
C5—C6—N2—Pd1 | −2.9 (2) | C19—C20—N6—Pd2 | 0.4 (2) |
N3—Pd1—N2—C7 | −4.89 (17) | N7—Pd2—N6—C21 | −7.44 (16) |
N4—Pd1—N2—C7 | 3.0 (4) | N8—Pd2—N6—C21 | −8.4 (4) |
N1—Pd1—N2—C7 | 173.27 (18) | N5—Pd2—N6—C21 | 173.28 (17) |
N3—Pd1—N2—C6 | −176.23 (18) | N7—Pd2—N6—C20 | 178.91 (17) |
N4—Pd1—N2—C6 | −168.3 (2) | N8—Pd2—N6—C20 | 178.0 (2) |
N1—Pd1—N2—C6 | 1.94 (16) | N5—Pd2—N6—C20 | −0.37 (16) |
O2—C8—N3—C9 | 4.2 (4) | O4—C22—N7—C23 | −0.4 (4) |
C7—C8—N3—C9 | −175.0 (2) | C21—C22—N7—C23 | 179.50 (19) |
O2—C8—N3—Pd1 | 177.9 (2) | O4—C22—N7—Pd2 | 174.78 (19) |
C7—C8—N3—Pd1 | −1.3 (3) | C21—C22—N7—Pd2 | −5.3 (2) |
C10—C9—N3—C8 | 173.8 (2) | C24—C23—N7—C22 | 173.4 (2) |
C10—C9—N3—Pd1 | 0.1 (3) | C24—C23—N7—Pd2 | −1.7 (2) |
N2—Pd1—N3—C8 | 3.27 (17) | N6—Pd2—N7—C22 | 7.02 (17) |
N4—Pd1—N3—C8 | −174.48 (18) | N8—Pd2—N7—C22 | −173.24 (18) |
N1—Pd1—N3—C8 | −3.2 (4) | N5—Pd2—N7—C22 | 9.5 (4) |
N2—Pd1—N3—C9 | 177.37 (18) | N6—Pd2—N7—C23 | −177.47 (18) |
N4—Pd1—N3—C9 | −0.38 (17) | N8—Pd2—N7—C23 | 2.28 (16) |
N1—Pd1—N3—C9 | 170.9 (2) | N5—Pd2—N7—C23 | −174.9 (2) |
C13—C14—N4—C10 | 0.2 (3) | C27—C28—N8—C24 | −0.5 (3) |
C13—C14—N4—Pd1 | −176.30 (18) | C27—C28—N8—Pd2 | 177.98 (17) |
C11—C10—N4—C14 | 1.3 (3) | C25—C24—N8—C28 | 2.1 (3) |
C9—C10—N4—C14 | −177.7 (2) | C23—C24—N8—C28 | −179.1 (2) |
C11—C10—N4—Pd1 | 178.38 (18) | C25—C24—N8—Pd2 | −176.63 (17) |
C9—C10—N4—Pd1 | −0.7 (3) | C23—C24—N8—Pd2 | 2.2 (2) |
N3—Pd1—N4—C14 | 177.2 (2) | N6—Pd2—N8—C28 | 180.0 (2) |
N2—Pd1—N4—C14 | 169.3 (2) | N7—Pd2—N8—C28 | 179.0 (2) |
N1—Pd1—N4—C14 | −0.1 (2) | N5—Pd2—N8—C28 | −1.8 (2) |
N3—Pd1—N4—C10 | 0.58 (15) | N6—Pd2—N8—C24 | −1.5 (4) |
N2—Pd1—N4—C10 | −7.4 (4) | N7—Pd2—N8—C24 | −2.39 (15) |
N1—Pd1—N4—C10 | −176.74 (14) | N5—Pd2—N8—C24 | 176.75 (14) |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O1i | 0.84 (2) | 2.05 (2) | 2.883 (3) | 173 (4) |
O5—H5B···O6 | 0.84 (2) | 1.94 (2) | 2.784 (3) | 177 (4) |
O6—H6A···O3ii | 0.82 (1) | 2.02 (2) | 2.845 (3) | 176 (3) |
O6—H6B···O2iii | 0.84 (1) | 2.25 (2) | 2.999 (3) | 150 (4) |
Symmetry codes: (i) −x, −y+1, −z; (ii) x, y−1, z; (iii) −x+1, −y+1, −z. |