Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804010451/na6322sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804010451/na6322Isup2.hkl |
CCDC reference: 242035
Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL96 (Sheldrick, 1996b); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL96 (Sheldrick, 1996b).
[PdCl2(C19H20N2)2]·CH2Cl2 | F(000) = 1672.0 |
Mr = 814.97 | Dx = 1.405 Mg m−3 |
Orthorhombic, P212121 | Cu Kα radiation, λ = 1.54178 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 6850 reflections |
a = 11.6567 (1) Å | θ = 3.7–72.9° |
b = 13.6627 (1) Å | µ = 6.68 mm−1 |
c = 24.1997 (2) Å | T = 220 K |
V = 3854.09 (5) Å3 | Plate, colourless |
Z = 4 | 0.41 × 0.30 × 0.05 mm |
Bruker AXS SMART 2K/Platform diffractometer | 7556 independent reflections |
Radiation source: normal-focus xray tube | 6917 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.055 |
Detector resolution: 5.5 pixels mm-1 | θmax = 72.9°, θmin = 3.7° |
ω scans | h = −13→11 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996a) | k = −16→16 |
Tmin = 0.135, Tmax = 0.715 | l = −29→30 |
46333 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
wR(F2) = 0.083 | w = 1/[σ2(Fo2) + (0.0517P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.003 |
7556 reflections | Δρmax = 0.71 e Å−3 |
437 parameters | Δρmin = −0.37 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 3255 Friedel Pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.023 (7) |
Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a glass fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8 Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis. |
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. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factor_obs 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. Data reduction processing was carried out by the use of the program SAINT (SAINT, 1999), which applied Lorentz and polarization corrections to three-dimensionally integrated diffraction spots. The program SADABS (Sheldrick, 1996 A) was utilized for the scaling of diffraction data, the application of a decay correction, and an empirical absorption correction based on redundant reflections. The space group was confirmed by XPREP routine in SHELXTL program (Sheldrick, 1997). The structure was solved by direct method using SHELXS97 (Sheldrick, 1997) and difmap synthesis using SHELXL96 (Sheldrick, 1996B). All non-hydrogen atoms anisotropic, hydrogen atoms isotropic. |
x | y | z | Uiso*/Ueq | ||
Pd | 0.19627 (2) | 0.454290 (18) | 0.890623 (9) | 0.02722 (7) | |
Cl1 | 0.31940 (9) | 0.36987 (7) | 0.94793 (4) | 0.0475 (2) | |
Cl2 | 0.07669 (8) | 0.53321 (7) | 0.82879 (4) | 0.0433 (2) | |
N11 | 0.3609 (3) | 0.6161 (2) | 0.85314 (11) | 0.0328 (7) | |
C12 | 0.2988 (3) | 0.5749 (2) | 0.89434 (13) | 0.0298 (6) | |
N13 | 0.3156 (3) | 0.6340 (2) | 0.93800 (10) | 0.0339 (6) | |
C14 | 0.3853 (4) | 0.7120 (3) | 0.92442 (16) | 0.0463 (10) | |
H14 | 0.4080 | 0.7632 | 0.9479 | 0.056* | |
C15 | 0.4143 (4) | 0.7006 (3) | 0.87148 (16) | 0.0454 (10) | |
H15 | 0.4619 | 0.7421 | 0.8506 | 0.054* | |
C111 | 0.3819 (3) | 0.5688 (3) | 0.79845 (14) | 0.0378 (9) | |
H111 | 0.3182 | 0.5223 | 0.7919 | 0.045* | |
C112 | 0.4909 (5) | 0.5097 (4) | 0.8013 (2) | 0.0658 (14) | |
H11A | 0.5556 | 0.5531 | 0.8071 | 0.099* | |
H11B | 0.5012 | 0.4741 | 0.7670 | 0.099* | |
H11C | 0.4860 | 0.4636 | 0.8318 | 0.099* | |
C113 | 0.3764 (3) | 0.6457 (3) | 0.75310 (14) | 0.0343 (8) | |
C114 | 0.4721 (4) | 0.6725 (3) | 0.72286 (16) | 0.0481 (10) | |
H114 | 0.5439 | 0.6451 | 0.7315 | 0.058* | |
C115 | 0.4632 (5) | 0.7394 (4) | 0.67985 (19) | 0.0605 (13) | |
H115 | 0.5288 | 0.7578 | 0.6598 | 0.073* | |
C116 | 0.3587 (5) | 0.7786 (3) | 0.66687 (16) | 0.0599 (14) | |
H116 | 0.3524 | 0.8226 | 0.6372 | 0.072* | |
C117 | 0.2622 (4) | 0.7541 (3) | 0.69687 (16) | 0.0498 (11) | |
H117 | 0.1910 | 0.7825 | 0.6883 | 0.060* | |
C118 | 0.2713 (4) | 0.6873 (3) | 0.73959 (16) | 0.0427 (10) | |
H118 | 0.2054 | 0.6699 | 0.7598 | 0.051* | |
C131 | 0.2635 (3) | 0.6198 (3) | 0.99349 (14) | 0.0369 (8) | |
H131 | 0.2426 | 0.5498 | 0.9965 | 0.044* | |
C132 | 0.1535 (4) | 0.6781 (4) | 0.9983 (2) | 0.0670 (15) | |
H13A | 0.1706 | 0.7473 | 0.9953 | 0.101* | |
H13B | 0.1178 | 0.6649 | 1.0337 | 0.101* | |
H13C | 0.1015 | 0.6592 | 0.9688 | 0.101* | |
C133 | 0.3532 (3) | 0.6401 (3) | 1.03759 (14) | 0.0342 (8) | |
C134 | 0.3577 (4) | 0.7270 (3) | 1.06673 (15) | 0.0440 (10) | |
H134 | 0.3023 | 0.7756 | 1.0601 | 0.053* | |
C135 | 0.4430 (4) | 0.7434 (3) | 1.10566 (17) | 0.0531 (11) | |
H135 | 0.4461 | 0.8034 | 1.1247 | 0.064* | |
C136 | 0.5222 (4) | 0.6725 (4) | 1.11631 (17) | 0.0589 (12) | |
H136 | 0.5792 | 0.6836 | 1.1431 | 0.071* | |
C137 | 0.5195 (4) | 0.5850 (4) | 1.08832 (19) | 0.0577 (12) | |
H137 | 0.5747 | 0.5366 | 1.0956 | 0.069* | |
C138 | 0.4340 (3) | 0.5686 (3) | 1.04899 (16) | 0.0441 (10) | |
H138 | 0.4313 | 0.5085 | 1.0301 | 0.053* | |
N21 | 0.0842 (3) | 0.2584 (2) | 0.86001 (11) | 0.0314 (6) | |
C22 | 0.0879 (3) | 0.3372 (2) | 0.89231 (14) | 0.0285 (6) | |
N23 | 0.0046 (2) | 0.3235 (2) | 0.92985 (12) | 0.0310 (6) | |
C24 | −0.0511 (3) | 0.2358 (3) | 0.92120 (15) | 0.0344 (8) | |
H24 | −0.1117 | 0.2100 | 0.9423 | 0.041* | |
C25 | −0.0024 (3) | 0.1946 (3) | 0.87708 (15) | 0.0356 (8) | |
H25 | −0.0225 | 0.1346 | 0.8607 | 0.043* | |
C211 | 0.1510 (3) | 0.2441 (3) | 0.80903 (15) | 0.0396 (9) | |
H211 | 0.2181 | 0.2884 | 0.8107 | 0.048* | |
C212 | 0.0764 (4) | 0.2769 (4) | 0.76019 (17) | 0.0579 (12) | |
H21A | 0.0054 | 0.2399 | 0.7601 | 0.087* | |
H21B | 0.1173 | 0.2655 | 0.7259 | 0.087* | |
H21C | 0.0593 | 0.3461 | 0.7637 | 0.087* | |
C213 | 0.1959 (4) | 0.1407 (3) | 0.80621 (14) | 0.0402 (8) | |
C214 | 0.2647 (4) | 0.1059 (3) | 0.84889 (18) | 0.0501 (11) | |
H214 | 0.2838 | 0.1476 | 0.8784 | 0.060* | |
C215 | 0.3050 (4) | 0.0122 (4) | 0.8485 (2) | 0.0636 (12) | |
H215 | 0.3513 | −0.0103 | 0.8777 | 0.076* | |
C216 | 0.2781 (4) | −0.0501 (4) | 0.8053 (2) | 0.0695 (14) | |
H216 | 0.3062 | −0.1146 | 0.8050 | 0.083* | |
C217 | 0.2102 (5) | −0.0172 (4) | 0.7631 (3) | 0.0837 (19) | |
H217 | 0.1901 | −0.0592 | 0.7339 | 0.100* | |
C218 | 0.1715 (4) | 0.0783 (4) | 0.7638 (2) | 0.0641 (15) | |
H218 | 0.1269 | 0.1010 | 0.7342 | 0.077* | |
C231 | −0.0262 (3) | 0.3943 (3) | 0.97402 (15) | 0.0352 (8) | |
H231 | 0.0223 | 0.4529 | 0.9683 | 0.042* | |
C232 | 0.0038 (4) | 0.3539 (3) | 1.03051 (15) | 0.0467 (10) | |
H23A | −0.0101 | 0.4035 | 1.0584 | 0.070* | |
H23B | 0.0840 | 0.3352 | 1.0312 | 0.070* | |
H23C | −0.0434 | 0.2970 | 1.0382 | 0.070* | |
C233 | −0.1502 (3) | 0.4267 (2) | 0.96566 (15) | 0.0337 (8) | |
C234 | −0.1725 (4) | 0.4991 (3) | 0.92659 (17) | 0.0447 (10) | |
H234 | −0.1115 | 0.5281 | 0.9071 | 0.054* | |
C235 | −0.2836 (4) | 0.5283 (3) | 0.91643 (19) | 0.0538 (11) | |
H235 | −0.2977 | 0.5780 | 0.8904 | 0.065* | |
C236 | −0.3739 (4) | 0.4860 (3) | 0.94370 (17) | 0.0477 (10) | |
H236 | −0.4494 | 0.5068 | 0.9368 | 0.057* | |
C237 | −0.3529 (4) | 0.4133 (3) | 0.98106 (18) | 0.0493 (11) | |
H237 | −0.4146 | 0.3826 | 0.9991 | 0.059* | |
C238 | −0.2416 (4) | 0.3842 (3) | 0.99267 (16) | 0.0425 (9) | |
H238 | −0.2283 | 0.3353 | 1.0192 | 0.051* | |
C3 | 0.2469 (5) | 0.5564 (4) | 0.1705 (2) | 0.090 (2) | |
H3A | 0.3135 | 0.5882 | 0.1535 | 0.108* | |
H3B | 0.2745 | 0.5142 | 0.2004 | 0.108* | |
Cl3 | 0.1765 (2) | 0.48595 (16) | 0.12138 (7) | 0.1570 (11) | |
Cl4 | 0.15182 (16) | 0.64873 (18) | 0.19853 (9) | 0.1258 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pd | 0.02756 (12) | 0.02972 (11) | 0.02438 (10) | −0.00239 (10) | −0.00130 (9) | 0.00333 (10) |
Cl1 | 0.0451 (6) | 0.0410 (5) | 0.0565 (6) | −0.0016 (4) | −0.0197 (4) | 0.0138 (4) |
Cl2 | 0.0366 (5) | 0.0494 (6) | 0.0440 (5) | −0.0009 (4) | −0.0103 (4) | 0.0155 (4) |
N11 | 0.0373 (17) | 0.0399 (17) | 0.0213 (14) | −0.0069 (13) | −0.0004 (12) | 0.0031 (12) |
C12 | 0.0306 (17) | 0.0333 (16) | 0.0254 (15) | −0.0044 (14) | −0.0022 (15) | 0.0059 (13) |
N13 | 0.0426 (19) | 0.0364 (16) | 0.0228 (13) | −0.0043 (14) | 0.0009 (12) | 0.0013 (11) |
C14 | 0.065 (3) | 0.043 (2) | 0.031 (2) | −0.017 (2) | −0.0060 (18) | −0.0025 (17) |
C15 | 0.056 (3) | 0.047 (2) | 0.0330 (19) | −0.022 (2) | −0.0015 (17) | 0.0055 (16) |
C111 | 0.044 (2) | 0.044 (2) | 0.0252 (17) | −0.0046 (16) | −0.0002 (14) | 0.0006 (15) |
C112 | 0.077 (4) | 0.075 (3) | 0.046 (3) | 0.028 (3) | 0.003 (2) | 0.005 (2) |
C113 | 0.042 (2) | 0.038 (2) | 0.0229 (16) | −0.0062 (16) | 0.0013 (14) | −0.0026 (15) |
C114 | 0.042 (3) | 0.063 (3) | 0.039 (2) | −0.007 (2) | 0.0077 (18) | −0.0008 (19) |
C115 | 0.074 (4) | 0.066 (3) | 0.042 (2) | −0.017 (3) | 0.018 (2) | 0.010 (2) |
C116 | 0.113 (4) | 0.041 (2) | 0.026 (2) | −0.017 (3) | −0.004 (2) | 0.0106 (17) |
C117 | 0.068 (3) | 0.043 (2) | 0.039 (2) | 0.002 (2) | −0.016 (2) | 0.0015 (18) |
C118 | 0.045 (3) | 0.048 (2) | 0.036 (2) | −0.0043 (17) | −0.0012 (16) | −0.0006 (17) |
C131 | 0.039 (2) | 0.046 (2) | 0.0258 (17) | 0.0025 (16) | 0.0033 (14) | 0.0045 (16) |
C132 | 0.053 (3) | 0.099 (4) | 0.049 (3) | 0.028 (3) | −0.006 (2) | −0.008 (3) |
C133 | 0.043 (2) | 0.038 (2) | 0.0219 (17) | −0.0029 (16) | 0.0047 (14) | −0.0005 (14) |
C134 | 0.063 (3) | 0.037 (2) | 0.0326 (19) | 0.0033 (18) | 0.0025 (18) | 0.0042 (16) |
C135 | 0.082 (3) | 0.047 (2) | 0.030 (2) | −0.015 (2) | −0.002 (2) | −0.0046 (19) |
C136 | 0.065 (3) | 0.081 (3) | 0.032 (2) | −0.017 (2) | −0.012 (2) | 0.001 (2) |
C137 | 0.058 (3) | 0.067 (3) | 0.048 (2) | 0.006 (2) | −0.011 (2) | 0.003 (2) |
C138 | 0.051 (3) | 0.046 (2) | 0.0349 (19) | 0.0040 (17) | −0.0005 (17) | −0.0064 (17) |
N21 | 0.0300 (17) | 0.0361 (16) | 0.0283 (15) | −0.0041 (12) | 0.0030 (12) | 0.0001 (12) |
C22 | 0.0276 (17) | 0.0331 (17) | 0.0249 (15) | −0.0030 (13) | −0.0035 (14) | 0.0029 (15) |
N23 | 0.0279 (17) | 0.0352 (16) | 0.0300 (15) | −0.0010 (12) | 0.0021 (11) | −0.0035 (12) |
C24 | 0.030 (2) | 0.037 (2) | 0.0363 (19) | −0.0037 (15) | 0.0043 (15) | 0.0001 (16) |
C25 | 0.035 (2) | 0.035 (2) | 0.037 (2) | −0.0087 (15) | 0.0001 (15) | −0.0025 (15) |
C211 | 0.044 (2) | 0.043 (2) | 0.0322 (19) | −0.0086 (17) | 0.0081 (16) | −0.0046 (16) |
C212 | 0.074 (3) | 0.065 (3) | 0.035 (2) | 0.005 (3) | 0.004 (2) | 0.008 (2) |
C213 | 0.032 (2) | 0.053 (2) | 0.0355 (18) | −0.0088 (19) | 0.0082 (17) | −0.0116 (16) |
C214 | 0.053 (3) | 0.058 (3) | 0.039 (2) | −0.003 (2) | 0.0017 (18) | −0.006 (2) |
C215 | 0.057 (3) | 0.068 (3) | 0.067 (3) | 0.012 (3) | −0.003 (3) | 0.003 (2) |
C216 | 0.061 (3) | 0.055 (3) | 0.092 (4) | 0.008 (3) | 0.011 (3) | −0.015 (3) |
C217 | 0.079 (4) | 0.079 (4) | 0.093 (4) | 0.008 (3) | −0.008 (4) | −0.049 (3) |
C218 | 0.062 (4) | 0.076 (3) | 0.054 (3) | 0.009 (2) | −0.013 (2) | −0.028 (2) |
C231 | 0.038 (2) | 0.032 (2) | 0.0354 (19) | −0.0039 (15) | 0.0060 (15) | −0.0070 (15) |
C232 | 0.042 (2) | 0.064 (3) | 0.034 (2) | −0.001 (2) | −0.0040 (16) | −0.0046 (19) |
C233 | 0.033 (2) | 0.033 (2) | 0.0350 (18) | −0.0034 (14) | 0.0042 (14) | −0.0052 (14) |
C234 | 0.043 (3) | 0.040 (2) | 0.051 (2) | −0.0068 (17) | 0.0053 (18) | 0.0058 (18) |
C235 | 0.059 (3) | 0.045 (3) | 0.057 (2) | 0.000 (2) | −0.005 (2) | 0.005 (2) |
C236 | 0.043 (3) | 0.051 (3) | 0.050 (2) | 0.0091 (18) | 0.0017 (18) | −0.0084 (19) |
C237 | 0.038 (2) | 0.060 (3) | 0.050 (3) | 0.0021 (19) | 0.0161 (19) | −0.003 (2) |
C238 | 0.044 (2) | 0.046 (2) | 0.038 (2) | 0.0017 (17) | 0.0106 (17) | 0.0037 (17) |
C3 | 0.120 (5) | 0.102 (5) | 0.047 (3) | −0.051 (4) | 0.015 (3) | 0.001 (3) |
Cl3 | 0.230 (2) | 0.1677 (19) | 0.0730 (10) | −0.1436 (19) | −0.0261 (12) | 0.0245 (11) |
Cl4 | 0.0788 (13) | 0.169 (2) | 0.1293 (17) | 0.0260 (13) | −0.0100 (11) | 0.0090 (16) |
Pd—C12 | 2.038 (3) | N21—C22 | 1.331 (4) |
Pd—C22 | 2.039 (3) | N21—C25 | 1.396 (4) |
Pd—Cl1 | 2.3050 (9) | N21—C211 | 1.472 (4) |
Pd—Cl2 | 2.3119 (9) | C22—N23 | 1.342 (4) |
N11—C12 | 1.354 (4) | N23—C24 | 1.379 (4) |
N11—C15 | 1.385 (5) | N23—C231 | 1.486 (4) |
N11—C111 | 1.493 (4) | C24—C25 | 1.333 (5) |
C12—N13 | 1.344 (4) | C24—H24 | 0.9400 |
N13—C14 | 1.380 (5) | C25—H25 | 0.9400 |
N13—C131 | 1.486 (4) | C211—C213 | 1.508 (5) |
C14—C15 | 1.334 (6) | C211—C212 | 1.534 (5) |
C14—H14 | 0.9400 | C211—H211 | 0.9900 |
C15—H15 | 0.9400 | C212—H21A | 0.9700 |
C111—C112 | 1.507 (6) | C212—H21B | 0.9700 |
C111—C113 | 1.520 (5) | C212—H21C | 0.9700 |
C111—H111 | 0.9900 | C213—C218 | 1.363 (5) |
C112—H11A | 0.9700 | C213—C214 | 1.391 (6) |
C112—H11B | 0.9700 | C214—C215 | 1.365 (6) |
C112—H11C | 0.9700 | C214—H214 | 0.9400 |
C113—C114 | 1.384 (5) | C215—C216 | 1.384 (7) |
C113—C118 | 1.390 (5) | C215—H215 | 0.9400 |
C114—C115 | 1.389 (6) | C216—C217 | 1.368 (7) |
C114—H114 | 0.9400 | C216—H216 | 0.9400 |
C115—C116 | 1.367 (7) | C217—C218 | 1.381 (7) |
C115—H115 | 0.9400 | C217—H217 | 0.9400 |
C116—C117 | 1.379 (6) | C218—H218 | 0.9400 |
C116—H116 | 0.9400 | C231—C232 | 1.515 (5) |
C117—C118 | 1.382 (5) | C231—C233 | 1.525 (5) |
C117—H117 | 0.9400 | C231—H231 | 0.9900 |
C118—H118 | 0.9400 | C232—H23A | 0.9700 |
C131—C132 | 1.514 (5) | C232—H23B | 0.9700 |
C131—C133 | 1.520 (5) | C232—H23C | 0.9700 |
C131—H131 | 0.9900 | C233—C238 | 1.378 (5) |
C132—H13A | 0.9700 | C233—C234 | 1.393 (5) |
C132—H13B | 0.9700 | C234—C235 | 1.377 (6) |
C132—H13C | 0.9700 | C234—H234 | 0.9400 |
C133—C134 | 1.381 (5) | C235—C236 | 1.370 (6) |
C133—C138 | 1.385 (5) | C235—H235 | 0.9400 |
C134—C135 | 1.387 (6) | C236—C237 | 1.366 (6) |
C134—H134 | 0.9400 | C236—H236 | 0.9400 |
C135—C136 | 1.363 (6) | C237—C238 | 1.386 (6) |
C135—H135 | 0.9400 | C237—H237 | 0.9400 |
C136—C137 | 1.375 (6) | C238—H238 | 0.9400 |
C136—H136 | 0.9400 | C3—Cl3 | 1.736 (5) |
C137—C138 | 1.396 (6) | C3—Cl4 | 1.811 (6) |
C137—H137 | 0.9400 | C3—H3A | 0.9800 |
C138—H138 | 0.9400 | C3—H3B | 0.9800 |
C12—Pd—C22 | 175.64 (14) | C22—N21—C25 | 110.8 (3) |
C12—Pd—Cl1 | 90.74 (9) | C22—N21—C211 | 125.7 (3) |
C22—Pd—Cl1 | 88.91 (9) | C25—N21—C211 | 123.2 (3) |
C12—Pd—Cl2 | 90.29 (9) | N21—C22—N23 | 105.1 (3) |
C22—Pd—Cl2 | 90.32 (9) | N21—C22—Pd | 130.0 (3) |
Cl1—Pd—Cl2 | 176.55 (4) | N23—C22—Pd | 124.8 (2) |
C12—N11—C15 | 110.5 (3) | C22—N23—C24 | 111.0 (3) |
C12—N11—C111 | 124.1 (3) | C22—N23—C231 | 124.8 (3) |
C15—N11—C111 | 124.8 (3) | C24—N23—C231 | 124.1 (3) |
N13—C12—N11 | 104.6 (3) | C25—C24—N23 | 106.7 (3) |
N13—C12—Pd | 127.3 (2) | C25—C24—H24 | 126.7 (2) |
N11—C12—Pd | 128.1 (2) | N23—C24—H24 | 126.7 |
C12—N13—C14 | 111.2 (3) | C24—C25—N21 | 106.4 (3) |
C12—N13—C131 | 124.9 (3) | C24—C25—H25 | 126.8 |
C14—N13—C131 | 123.8 (3) | N21—C25—H25 | 126.8 |
C15—C14—N13 | 106.7 (4) | N21—C211—C213 | 110.3 (3) |
C15—C14—H14 | 126.6 | N21—C211—C212 | 107.8 (3) |
N13—C14—H14 | 126.6 | C213—C211—C212 | 115.9 (3) |
C14—C15—N11 | 106.9 (4) | N21—C211—H211 | 107.5 |
C14—C15—H15 | 126.5 | C213—C211—H211 | 107.5 |
N11—C15—H15 | 126.5 | C212—C211—H211 | 107.5 |
N11—C111—C112 | 109.2 (3) | C211—C212—H21A | 109.5 |
N11—C111—C113 | 109.5 (3) | C211—C212—H21B | 109.5 |
C112—C111—C113 | 116.1 (3) | H21A—C212—H21B | 109.5 |
N11—C111—H111 | 107.2 | C211—C212—H21C | 109.5 |
C112—C111—H111 | 107.2 | H21A—C212—H21C | 109.5 |
C113—C111—H111 | 107.2 | H21B—C212—H21C | 109.5 |
C111—C112—H11A | 109.5 | C218—C213—C214 | 117.7 (4) |
C111—C112—H11B | 109.5 | C218—C213—C211 | 123.2 (4) |
H11A—C112—H11B | 109.5 | C214—C213—C211 | 119.1 (3) |
C111—C112—H11C | 109.5 | C215—C214—C213 | 120.9 (4) |
H11A—C112—H11C | 109.5 | C215—C214—H214 | 119.6 |
H11B—C112—H11C | 109.5 | C213—C214—H214 | 119.6 |
C114—C113—C118 | 118.5 (4) | C214—C215—C216 | 120.3 (5) |
C114—C113—C111 | 122.0 (4) | C214—C215—H215 | 119.8 |
C118—C113—C111 | 119.4 (3) | C216—C215—H215 | 119.8 |
C113—C114—C115 | 120.7 (4) | C217—C216—C215 | 119.5 (5) |
C113—C114—H114 | 119.7 | C217—C216—H216 | 120.2 |
C115—C114—H114 | 119.7 | C215—C216—H216 | 120.2 |
C116—C115—C114 | 119.7 (4) | C216—C217—C218 | 119.3 (5) |
C116—C115—H115 | 120.1 | C216—C217—H217 | 120.3 |
C114—C115—H115 | 120.1 | C218—C217—H217 | 120.3 |
C115—C116—C117 | 120.7 (4) | C213—C218—C217 | 122.2 (5) |
C115—C116—H116 | 119.6 | C213—C218—H218 | 118.9 |
C117—C116—H116 | 119.6 | C217—C218—H218 | 118.9 |
C116—C117—C118 | 119.5 (4) | N23—C231—C232 | 110.8 (3) |
C116—C117—H117 | 120.3 | N23—C231—C233 | 108.8 (3) |
C118—C117—H117 | 120.3 | C232—C231—C233 | 116.4 (3) |
C117—C118—C113 | 120.9 (4) | N23—C231—H231 | 106.8 |
C117—C118—H118 | 119.6 | C232—C231—H231 | 106.8 |
C113—C118—H118 | 119.6 | C233—C231—H231 | 106.8 |
N13—C131—C132 | 110.3 (3) | C231—C232—H23A | 109.5 |
N13—C131—C133 | 109.2 (3) | C231—C232—H23B | 109.5 |
C132—C131—C133 | 115.7 (3) | H23A—C232—H23B | 109.5 |
N13—C131—H131 | 107.1 | C231—C232—H23C | 109.5 |
C132—C131—H131 | 107.1 | H23A—C232—H23C | 109.5 |
C133—C131—H131 | 107.1 | H23B—C232—H23C | 109.5 |
C131—C132—H13A | 109.5 | C238—C233—C234 | 118.5 (4) |
C131—C132—H13B | 109.5 | C238—C233—C231 | 123.2 (3) |
H13A—C132—H13B | 109.5 | C234—C233—C231 | 118.2 (3) |
C131—C132—H13C | 109.5 | C235—C234—C233 | 120.1 (4) |
H13A—C132—H13C | 109.5 | C235—C234—H234 | 119.9 |
H13B—C132—H13C | 109.5 | C233—C234—H234 | 119.9 |
C134—C133—C138 | 118.6 (4) | C236—C235—C234 | 121.0 (4) |
C134—C133—C131 | 122.8 (4) | C236—C235—H235 | 119.5 |
C138—C133—C131 | 118.6 (3) | C234—C235—H235 | 119.5 |
C133—C134—C135 | 120.9 (4) | C237—C236—C235 | 119.2 (4) |
C133—C134—H134 | 119.6 | C237—C236—H236 | 120.4 |
C135—C134—H134 | 119.6 | C235—C236—H236 | 120.4 |
C136—C135—C134 | 119.9 (4) | C236—C237—C238 | 120.7 (4) |
C136—C135—H135 | 120.1 | C236—C237—H237 | 119.7 |
C134—C135—H135 | 120.1 | C238—C237—H237 | 119.7 |
C135—C136—C137 | 120.6 (4) | C233—C238—C237 | 120.5 (4) |
C135—C136—H136 | 119.7 | C233—C238—H238 | 119.7 |
C137—C136—H136 | 119.7 | C237—C238—H238 | 119.7 |
C136—C137—C138 | 119.5 (4) | Cl3—C3—Cl4 | 110.7 (4) |
C136—C137—H137 | 120.2 | Cl3—C3—H3A | 109.5 |
C138—C137—H137 | 120.2 | Cl4—C3—H3A | 109.5 |
C133—C138—C137 | 120.5 (4) | Cl3—C3—H3B | 109.5 |
C133—C138—H138 | 119.8 | Cl4—C3—H3B | 109.5 |
C137—C138—H138 | 119.8 | H3A—C3—H3B | 108.1 |
C15—N11—C12—N13 | −0.6 (4) | C25—N21—C22—N23 | 0.3 (4) |
C111—N11—C12—N13 | 171.1 (3) | C211—N21—C22—N23 | 173.1 (3) |
C15—N11—C12—Pd | 176.6 (3) | C25—N21—C22—Pd | 178.2 (3) |
C111—N11—C12—Pd | −11.6 (5) | C211—N21—C22—Pd | −9.0 (5) |
Cl1—Pd—C12—N13 | −70.1 (3) | Cl1—Pd—C22—N21 | −88.6 (3) |
Cl2—Pd—C12—N13 | 113.2 (3) | Cl2—Pd—C22—N21 | 88.0 (3) |
Cl1—Pd—C12—N11 | 113.2 (3) | Cl1—Pd—C22—N23 | 88.9 (3) |
Cl2—Pd—C12—N11 | −63.5 (3) | Cl2—Pd—C22—N23 | −94.5 (3) |
N11—C12—N13—C14 | 1.0 (4) | N21—C22—N23—C24 | 0.2 (4) |
Pd—C12—N13—C14 | −176.3 (3) | Pd—C22—N23—C24 | −177.8 (2) |
N11—C12—N13—C131 | 179.3 (3) | N21—C22—N23—C231 | −178.1 (3) |
Pd—C12—N13—C131 | 2.0 (5) | Pd—C22—N23—C231 | 3.8 (5) |
C12—N13—C14—C15 | −1.0 (5) | C22—N23—C24—C25 | −0.7 (4) |
C131—N13—C14—C15 | −179.3 (4) | C231—N23—C24—C25 | 177.7 (3) |
N13—C14—C15—N11 | 0.6 (5) | N23—C24—C25—N21 | 0.8 (4) |
C12—N11—C15—C14 | 0.0 (5) | C22—N21—C25—C24 | −0.7 (4) |
C111—N11—C15—C14 | −171.7 (4) | C211—N21—C25—C24 | −173.8 (3) |
C12—N11—C111—C112 | −90.6 (4) | C22—N21—C211—C213 | 138.5 (3) |
C15—N11—C111—C112 | 80.0 (5) | C25—N21—C211—C213 | −49.5 (5) |
C12—N11—C111—C113 | 141.2 (3) | C22—N21—C211—C212 | −94.1 (4) |
C15—N11—C111—C113 | −48.2 (5) | C25—N21—C211—C212 | 77.9 (4) |
N11—C111—C113—C114 | 112.8 (4) | N21—C211—C213—C218 | 121.8 (4) |
C112—C111—C113—C114 | −11.5 (5) | C212—C211—C213—C218 | −1.0 (6) |
N11—C111—C113—C118 | −70.3 (4) | N21—C211—C213—C214 | −57.5 (5) |
C112—C111—C113—C118 | 165.5 (4) | C212—C211—C213—C214 | 179.6 (4) |
C118—C113—C114—C115 | −0.2 (6) | C218—C213—C214—C215 | −0.8 (7) |
C111—C113—C114—C115 | 176.8 (4) | C211—C213—C214—C215 | 178.5 (4) |
C113—C114—C115—C116 | −0.6 (7) | C213—C214—C215—C216 | 0.1 (7) |
C114—C115—C116—C117 | 1.6 (7) | C214—C215—C216—C217 | −0.4 (8) |
C115—C116—C117—C118 | −1.6 (7) | C215—C216—C217—C218 | 1.2 (9) |
C116—C117—C118—C113 | 0.8 (6) | C214—C213—C218—C217 | 1.7 (8) |
C114—C113—C118—C117 | 0.1 (6) | C211—C213—C218—C217 | −177.6 (5) |
C111—C113—C118—C117 | −177.0 (3) | C216—C217—C218—C213 | −2.0 (9) |
C12—N13—C131—C132 | −94.1 (4) | C22—N23—C231—C232 | −112.3 (4) |
C14—N13—C131—C132 | 84.0 (5) | C24—N23—C231—C232 | 69.5 (4) |
C12—N13—C131—C133 | 137.7 (4) | C22—N23—C231—C233 | 118.5 (4) |
C14—N13—C131—C133 | −44.2 (5) | C24—N23—C231—C233 | −59.7 (4) |
N13—C131—C133—C134 | 101.3 (4) | N23—C231—C233—C238 | 95.6 (4) |
C132—C131—C133—C134 | −23.8 (5) | C232—C231—C233—C238 | −30.4 (5) |
N13—C131—C133—C138 | −78.6 (4) | N23—C231—C233—C234 | −80.8 (4) |
C132—C131—C133—C138 | 156.3 (4) | C232—C231—C233—C234 | 153.1 (4) |
C138—C133—C134—C135 | 1.6 (6) | C238—C233—C234—C235 | 1.3 (6) |
C131—C133—C134—C135 | −178.3 (4) | C231—C233—C234—C235 | 177.9 (4) |
C133—C134—C135—C136 | −1.3 (6) | C233—C234—C235—C236 | −1.0 (7) |
C134—C135—C136—C137 | 0.8 (7) | C234—C235—C236—C237 | −0.6 (6) |
C135—C136—C137—C138 | −0.6 (7) | C235—C236—C237—C238 | 1.9 (7) |
C134—C133—C138—C137 | −1.3 (6) | C234—C233—C238—C237 | 0.0 (6) |
C131—C133—C138—C137 | 178.6 (4) | C231—C233—C238—C237 | −176.4 (4) |
C136—C137—C138—C133 | 0.8 (7) | C236—C237—C238—C233 | −1.6 (7) |