Coordination of bis­(pyrazol-1-yl)amine to palladium(II): influence of the co-ligands and counter-ions on the mol­ecular and crystal structures

The crystal structures for five Pd^II complexes containing the tridentate ligand bis­[2-(3,5-di­methyl­pyrazol-1-yl)eth­yl]amine (pza) are reported. The co-ligand completing the square-planar coordination of the Pd^II centre influences the conformation of the pza ligand.

Key indicators

Structure: 1

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.013 Å
• R factor = 0.060
• wR factor = 0.158
• Data-to-parameter ratio = 14.7

Structure: 2

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.009 Å
• R factor = 0.051
• wR factor = 0.148
• Data-to-parameter ratio = 21.5

Structure: 3

• Single-crystal X-ray study
• T = 299 K
• Mean [sigma](C-C) = 0.013 Å
• R factor = 0.040
• wR factor = 0.101
• Data-to-parameter ratio = 16.5

Structure: 4

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.036
• wR factor = 0.097
• Data-to-parameter ratio = 16.3

Structure: 5

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.007 Å
• Disorder in main residue
• R factor = 0.039
• wR factor = 0.107
• Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Datablock: 1


Alert level B
PLAT019_ALERT_1_B  _diffrn_measured_fraction_theta_full/_max < 1.0      0.978 Report

Alert level C
PLAT241_ALERT_2_C High      Ueq as Compared to Neighbors for .....         C9 Check
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of         N20 Check
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0128 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H4A    ..  N20     ..       2.66 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H16A   ..  O1      ..       2.64 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H18B   ..  O1      ..       2.61 Ang.
PLAT906_ALERT_3_C Large K value in the Analysis of Variance ......      3.922 Check
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.596          6 Report

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          1 Report
PLAT909_ALERT_3_G Percentage of Observed Data at Theta(Max) still          31 %

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
   8 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   2 ALERT level G = General information/check it is not something unexpected

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check




Datablock: 2


Alert level C
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of         N20 Check
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0094 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H4A    ..  N20     ..       2.66 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H7C    ..  BR1     ..       3.06 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H16A   ..  O1      ..       2.65 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H17C   ..  BR1     ..       2.98 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H18B   ..  O1      ..       2.65 Ang.
PLAT906_ALERT_3_C Large K value in the Analysis of Variance ......      2.199 Check
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          6 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1 Note
PLAT976_ALERT_2_C Check Calcd Residual Density  0.86A From      O3      -0.46 eA-3

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          1 Report

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
  11 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   1 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   6 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check




Datablock: 3


Alert level B
PLAT019_ALERT_1_B  _diffrn_measured_fraction_theta_full/_max < 1.0      0.974 Report

Alert level C
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0129 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H30A   ..  I4      ..       3.30 Ang.
PLAT906_ALERT_3_C Large K value in the Analysis of Variance ......      2.505 Check
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.595         78 Report

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          4 Report
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT045_ALERT_1_G Calculated and Reported Z Differ by ............       0.50 Ratio
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large.       6.40 Why ?
PLAT152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ...          2 Units
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  I1     --  Pd1     ..        8.0 su
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  I2     --  Pd2     ..        7.8 su
PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety .....        C36 Check
PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety .....        C37 Check
PLAT909_ALERT_3_G Percentage of Observed Data at Theta(Max) still          36 %
PLAT910_ALERT_3_G Missing # of FCF Reflections Below Th(Min) .....          1 Report

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
   4 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  11 ALERT level G = General information/check it is not something unexpected

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   5 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check




Datablock: 4


Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor       O1     -   H11    ...     Please Check

Alert level C
PLAT241_ALERT_2_C High      Ueq as Compared to Neighbors for .....         C9 Check
PLAT241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        C19 Check
PLAT242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        N21 Check
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of         N31 Check
PLAT480_ALERT_4_C Long H...A H-Bond Reported H10    ..  N31     ..       2.66 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H11    ..  N32     ..       2.67 Ang.
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          3 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          2 Note
PLAT975_ALERT_2_C Check Calcd Residual Density  0.91A From     N30       0.45 eA-3

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          3 Report
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          2 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
   9 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   2 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check




Datablock: 5


Alert level C
PLAT241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        S22 Check
PLAT242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        Pd2 Check
PLAT242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        C23 Check
PLAT242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....        C26 Check
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          6 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1 Note

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          2 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Pd2    --  S25     ..        5.7 su
PLAT301_ALERT_3_G Main Residue  Disorder ............ Percentage =          3 Note
PLAT380_ALERT_4_G Incorrectly? Oriented X(sp2)-Methyl Moiety .....        C16 Check
PLAT910_ALERT_3_G Missing # of FCF Reflections Below Th(Min) .....          1 Report
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          8 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   6 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   6 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

---

Computing details

For all compounds, data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS (Siemens, 1996); data reduction: XSCANS (Siemens, 1996); program(s) used to solve structure: SHELXS2014 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2008). Molecular graphics: SHELXTL (Sheldrick, 2008) for (1), (3), (4), (5); SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al., 2008) for (2). For all compounds, software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

(1) {Bis[2-(3,5-dimethylpyrazol-1-yl-κN²)ethyl]amine-κN}chloridopalladium nitrate

Crystal data

[PdCl(C14H23N5)]NO3	F(000) = 944
Mr = 465.23	Dx = 1.620 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 11.046 (2) Å	Cell parameters from 51 reflections
b = 12.2941 (15) Å	θ = 4.2–11.4°
c = 14.0978 (16) Å	µ = 1.14 mm^−1
β = 94.740 (16)°	T = 298 K
V = 1907.9 (5) Å^3	Irregular, yellow
Z = 4	0.40 × 0.12 × 0.10 mm

Data collection

Siemens P4 diffractometer	2110 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube, FN4	Rint = 0.044
Graphite monochromator	θmax = 25.1°, θmin = 2.2°
ω scans	h = −13→2
Absorption correction: ψ scan (XSCANS; Siemens, 1996)	k = −14→1
Tmin = 0.469, Tmax = 0.517	l = −16→16
4513 measured reflections	2 standard reflections every 98 reflections
3372 independent reflections	intensity decay: 2.5%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.060	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.158	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0649P)^2 + 4.1623P] where P = (Fo^2 + 2Fc^2)/3
3372 reflections	(Δ/σ)max = 0.001
230 parameters	Δρmax = 1.45 e Å^−3
0 restraints	Δρmin = −1.11 e Å^−3
0 constraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0.72319 (6)	0.71729 (4)	0.48704 (4)	0.0531 (2)
Cl1	0.8178 (2)	0.79157 (19)	0.36252 (16)	0.0787 (7)
N1	0.6837 (6)	0.8628 (5)	0.5434 (4)	0.0526 (15)
N2	0.5729 (6)	0.8737 (5)	0.5775 (4)	0.0590 (17)
C3	0.5644 (8)	0.9712 (7)	0.6217 (6)	0.063 (2)
C4	0.6727 (8)	1.0222 (7)	0.6145 (6)	0.062 (2)
H4A	0.6935	1.0913	0.6372	0.074*
C5	0.7454 (8)	0.9534 (6)	0.5679 (6)	0.057 (2)
C6	0.4531 (9)	1.0055 (9)	0.6675 (8)	0.094 (3)
H6A	0.3833	0.9982	0.6227	0.141*
H6B	0.4614	1.0800	0.6874	0.141*
H6C	0.4433	0.9603	0.7219	0.141*
C7	0.8714 (9)	0.9703 (8)	0.5461 (8)	0.087 (3)
H7A	0.9208	0.9113	0.5717	0.131*
H7B	0.9010	1.0375	0.5740	0.131*
H7C	0.8752	0.9734	0.4784	0.131*
C8	0.4865 (8)	0.7861 (7)	0.5628 (6)	0.071 (2)
H8A	0.4758	0.7689	0.4955	0.086*
H8B	0.4086	0.8094	0.5827	0.086*
C9	0.5280 (9)	0.6844 (8)	0.6183 (7)	0.085 (3)
H9A	0.5163	0.6950	0.6851	0.102*
H9B	0.4782	0.6232	0.5956	0.102*
N10	0.6567 (6)	0.6590 (5)	0.6082 (4)	0.0592 (17)
H10	0.6972	0.6969	0.6553	0.071*
N11	0.7516 (6)	0.5655 (5)	0.4398 (4)	0.0592 (17)
N12	0.8073 (7)	0.4924 (5)	0.5011 (4)	0.0668 (19)
C13	0.8283 (8)	0.3993 (7)	0.4553 (6)	0.066 (2)
C14	0.7855 (8)	0.4148 (6)	0.3638 (6)	0.065 (2)
H14A	0.7896	0.3645	0.3148	0.078*
C15	0.7349 (7)	0.5173 (6)	0.3546 (5)	0.0550 (19)
C16	0.8887 (11)	0.3031 (8)	0.5040 (7)	0.096 (3)
H16A	0.8463	0.2837	0.5583	0.145*
H16B	0.9714	0.3210	0.5244	0.145*
H16C	0.8872	0.2429	0.4605	0.145*
C17	0.6704 (9)	0.5709 (8)	0.2707 (6)	0.081 (3)
H17A	0.5987	0.6063	0.2896	0.121*
H17B	0.6478	0.5173	0.2230	0.121*
H17C	0.7229	0.6238	0.2453	0.121*
C18	0.8104 (10)	0.5127 (7)	0.6030 (5)	0.078 (3)
H18A	0.8676	0.5707	0.6201	0.094*
H18B	0.8380	0.4477	0.6373	0.094*
C19	0.6873 (11)	0.5438 (7)	0.6310 (6)	0.080 (3)
H19A	0.6268	0.4969	0.5982	0.096*
H19B	0.6845	0.5323	0.6989	0.096*
N20	0.8548 (9)	0.7786 (5)	0.7798 (5)	0.069 (2)
O1	0.7422 (7)	0.7795 (6)	0.7736 (5)	0.0859 (19)
O2	0.9057 (8)	0.7441 (7)	0.7123 (6)	0.105 (2)
O3	0.9127 (7)	0.8085 (5)	0.8529 (5)	0.097 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd1	0.0779 (5)	0.0434 (3)	0.0381 (3)	0.0043 (3)	0.0053 (3)	0.0013 (3)
Cl1	0.0987 (17)	0.0776 (15)	0.0621 (13)	0.0096 (13)	0.0200 (12)	0.0223 (11)
N1	0.056 (4)	0.045 (4)	0.057 (4)	0.001 (3)	0.009 (3)	−0.004 (3)
N2	0.065 (5)	0.060 (4)	0.052 (4)	−0.002 (4)	0.004 (3)	−0.003 (3)
C3	0.072 (6)	0.063 (5)	0.053 (5)	0.019 (5)	−0.003 (4)	−0.006 (4)
C4	0.068 (6)	0.047 (4)	0.070 (5)	0.006 (4)	0.005 (4)	−0.012 (4)
C5	0.065 (6)	0.046 (4)	0.061 (5)	−0.002 (4)	0.006 (4)	0.010 (4)
C6	0.082 (7)	0.102 (8)	0.100 (8)	0.024 (6)	0.010 (6)	−0.029 (6)
C7	0.095 (8)	0.063 (6)	0.105 (8)	−0.015 (5)	0.021 (6)	−0.005 (5)
C8	0.070 (6)	0.083 (6)	0.060 (5)	−0.007 (5)	−0.004 (4)	−0.010 (5)
C9	0.095 (8)	0.088 (7)	0.071 (6)	−0.030 (6)	0.011 (5)	−0.007 (5)
N10	0.083 (5)	0.053 (4)	0.042 (3)	−0.014 (4)	0.006 (3)	−0.003 (3)
N11	0.097 (5)	0.044 (3)	0.036 (3)	0.015 (4)	0.004 (3)	0.000 (3)
N12	0.098 (6)	0.050 (4)	0.050 (4)	0.013 (4)	−0.010 (4)	0.003 (3)
C13	0.081 (6)	0.050 (5)	0.069 (6)	0.010 (4)	0.015 (5)	0.003 (4)
C14	0.080 (6)	0.052 (5)	0.064 (5)	0.009 (5)	0.014 (5)	−0.007 (4)
C15	0.063 (5)	0.061 (5)	0.041 (4)	0.006 (4)	0.002 (4)	−0.008 (4)
C16	0.131 (9)	0.073 (7)	0.089 (7)	0.039 (6)	0.028 (7)	0.012 (5)
C17	0.100 (7)	0.096 (7)	0.045 (5)	0.023 (6)	−0.003 (5)	−0.010 (5)
C18	0.137 (9)	0.047 (5)	0.046 (5)	0.008 (6)	−0.017 (5)	0.004 (4)
C19	0.147 (9)	0.057 (5)	0.037 (4)	−0.013 (6)	0.007 (5)	0.005 (4)
N20	0.102 (7)	0.045 (4)	0.058 (5)	−0.003 (5)	−0.004 (5)	0.003 (4)
O1	0.086 (5)	0.094 (5)	0.077 (4)	−0.004 (4)	0.003 (4)	−0.018 (4)
O2	0.115 (6)	0.110 (6)	0.091 (5)	−0.002 (4)	0.005 (5)	−0.024 (4)
O3	0.136 (6)	0.073 (4)	0.075 (4)	−0.005 (4)	−0.039 (4)	−0.004 (3)

Geometric parameters (Å, º)

Pd1—N11	2.015 (6)	N10—C19	1.485 (10)
Pd1—N1	2.019 (6)	N10—H10	0.9000
Pd1—N10	2.045 (6)	N11—C15	1.339 (9)
Pd1—Cl1	2.305 (2)	N11—N12	1.357 (8)
N1—C5	1.337 (9)	N12—C13	1.344 (10)
N1—N2	1.358 (9)	N12—C18	1.455 (10)
N2—C3	1.358 (10)	C13—C14	1.351 (11)
N2—C8	1.442 (10)	C13—C16	1.496 (12)
C3—C4	1.362 (11)	C14—C15	1.380 (11)
C3—C6	1.495 (12)	C14—H14A	0.9300
C4—C5	1.372 (11)	C15—C17	1.484 (11)
C4—H4A	0.9300	C16—H16A	0.9600
C5—C7	1.465 (12)	C16—H16B	0.9600
C6—H6A	0.9600	C16—H16C	0.9600
C6—H6B	0.9600	C17—H17A	0.9600
C6—H6C	0.9600	C17—H17B	0.9600
C7—H7A	0.9600	C17—H17C	0.9600
C7—H7B	0.9600	C18—C19	1.497 (13)
C7—H7C	0.9600	C18—H18A	0.9700
C8—C9	1.525 (13)	C18—H18B	0.9700
C8—H8A	0.9700	C19—H19A	0.9700
C8—H8B	0.9700	C19—H19B	0.9700
C9—N10	1.473 (11)	N20—O2	1.219 (10)
C9—H9A	0.9700	N20—O3	1.223 (9)
C9—H9B	0.9700	N20—O1	1.239 (9)
N11—Pd1—N1	174.3 (3)	C19—N10—Pd1	115.1 (5)
N11—Pd1—N10	91.6 (3)	C9—N10—H10	104.1
N1—Pd1—N10	83.0 (3)	C19—N10—H10	104.1
N11—Pd1—Cl1	91.30 (19)	Pd1—N10—H10	104.1
N1—Pd1—Cl1	94.30 (19)	C15—N11—N12	107.5 (6)
N10—Pd1—Cl1	172.9 (2)	C15—N11—Pd1	133.8 (5)
C5—N1—N2	106.4 (6)	N12—N11—Pd1	118.5 (4)
C5—N1—Pd1	135.9 (6)	C13—N12—N11	110.2 (6)
N2—N1—Pd1	117.2 (5)	C13—N12—C18	128.9 (7)
C3—N2—N1	110.4 (7)	N11—N12—C18	119.2 (6)
C3—N2—C8	130.9 (8)	N12—C13—C14	106.1 (7)
N1—N2—C8	118.7 (7)	N12—C13—C16	122.8 (8)
N2—C3—C4	106.1 (7)	C14—C13—C16	131.1 (8)
N2—C3—C6	122.5 (9)	C13—C14—C15	109.0 (7)
C4—C3—C6	131.3 (8)	C13—C14—H14A	125.5
C3—C4—C5	107.7 (7)	C15—C14—H14A	125.5
C3—C4—H4A	126.1	N11—C15—C14	107.2 (7)
C5—C4—H4A	126.1	N11—C15—C17	122.7 (7)
N1—C5—C4	109.3 (7)	C14—C15—C17	130.1 (7)
N1—C5—C7	122.6 (8)	C13—C16—H16A	109.5
C4—C5—C7	128.1 (8)	C13—C16—H16B	109.5
C3—C6—H6A	109.5	H16A—C16—H16B	109.5
C3—C6—H6B	109.5	C13—C16—H16C	109.5
H6A—C6—H6B	109.5	H16A—C16—H16C	109.5
C3—C6—H6C	109.5	H16B—C16—H16C	109.5
H6A—C6—H6C	109.5	C15—C17—H17A	109.5
H6B—C6—H6C	109.5	C15—C17—H17B	109.5
C5—C7—H7A	109.5	H17A—C17—H17B	109.5
C5—C7—H7B	109.5	C15—C17—H17C	109.5
H7A—C7—H7B	109.5	H17A—C17—H17C	109.5
C5—C7—H7C	109.5	H17B—C17—H17C	109.5
H7A—C7—H7C	109.5	N12—C18—C19	110.9 (7)
H7B—C7—H7C	109.5	N12—C18—H18A	109.5
N2—C8—C9	111.8 (7)	C19—C18—H18A	109.5
N2—C8—H8A	109.3	N12—C18—H18B	109.5
C9—C8—H8A	109.3	C19—C18—H18B	109.5
N2—C8—H8B	109.3	H18A—C18—H18B	108.1
C9—C8—H8B	109.3	N10—C19—C18	112.5 (7)
H8A—C8—H8B	107.9	N10—C19—H19A	109.1
N10—C9—C8	112.1 (7)	C18—C19—H19A	109.1
N10—C9—H9A	109.2	N10—C19—H19B	109.1
C8—C9—H9A	109.2	C18—C19—H19B	109.1
N10—C9—H9B	109.2	H19A—C19—H19B	107.8
C8—C9—H9B	109.2	O2—N20—O3	121.2 (10)
H9A—C9—H9B	107.9	O2—N20—O1	118.2 (8)
C9—N10—C19	112.7 (7)	O3—N20—O1	120.5 (9)
C9—N10—Pd1	115.0 (5)
C5—N1—N2—C3	1.1 (8)	C15—N11—N12—C13	1.2 (10)
Pd1—N1—N2—C3	173.7 (5)	Pd1—N11—N12—C13	−174.5 (6)
C5—N1—N2—C8	−179.0 (7)	C15—N11—N12—C18	−165.2 (8)
Pd1—N1—N2—C8	−6.4 (8)	Pd1—N11—N12—C18	19.0 (10)
N1—N2—C3—C4	0.1 (9)	N11—N12—C13—C14	0.4 (10)
C8—N2—C3—C4	−179.8 (8)	C18—N12—C13—C14	165.2 (9)
N1—N2—C3—C6	−179.2 (8)	N11—N12—C13—C16	180.0 (9)
C8—N2—C3—C6	0.9 (13)	C18—N12—C13—C16	−15.3 (15)
N2—C3—C4—C5	−1.2 (9)	N12—C13—C14—C15	−1.8 (10)
C6—C3—C4—C5	178.0 (9)	C16—C13—C14—C15	178.6 (10)
N2—N1—C5—C4	−1.8 (8)	N12—N11—C15—C14	−2.3 (9)
Pd1—N1—C5—C4	−172.4 (6)	Pd1—N11—C15—C14	172.5 (6)
N2—N1—C5—C7	177.9 (7)	N12—N11—C15—C17	176.7 (8)
Pd1—N1—C5—C7	7.3 (12)	Pd1—N11—C15—C17	−8.5 (13)
C3—C4—C5—N1	2.0 (9)	C13—C14—C15—N11	2.6 (10)
C3—C4—C5—C7	−177.8 (8)	C13—C14—C15—C17	−176.4 (9)
C3—N2—C8—C9	−113.1 (9)	C13—N12—C18—C19	−115.9 (10)
N1—N2—C8—C9	67.0 (9)	N11—N12—C18—C19	47.7 (10)
N2—C8—C9—N10	−45.8 (10)	C9—N10—C19—C18	168.9 (7)
C8—C9—N10—C19	−159.6 (7)	Pd1—N10—C19—C18	34.4 (8)
C8—C9—N10—Pd1	−25.0 (9)	N12—C18—C19—N10	−78.4 (9)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···N20^i	0.93	2.66	3.510 (10)	153
C7—H7C···Cl1	0.96	2.81	3.410 (10)	121
C8—H8A···O3^ii	0.97	2.28	3.222 (10)	163
N10—H10···N20	0.90	2.57	3.453 (10)	167
N10—H10···O1	0.90	1.98	2.857 (9)	164
N10—H10···O2	0.90	2.45	3.186 (10)	140
C14—H14A···Cl1^iii	0.93	2.82	3.629 (9)	146
C16—H16A···O1^iv	0.96	2.64	3.572 (12)	164
C17—H17A···O3^ii	0.96	2.53	3.491 (12)	175
C17—H17C···Cl1	0.96	2.79	3.367 (10)	119
C18—H18A···O2	0.97	2.51	3.364 (11)	146
C18—H18B···O1^iv	0.97	2.61	3.428 (11)	142
C19—H19A···O3^iv	0.97	2.47	3.112 (11)	124

Symmetry codes: (i) −x+3/2, y+1/2, −z+3/2; (ii) x−1/2, −y+3/2, z−1/2; (iii) −x+3/2, y−1/2, −z+1/2; (iv) −x+3/2, y−1/2, −z+3/2.

(2) {Bis[2-(3,5-dimethylpyrazol-1-yl-κN²)ethyl]amine-κN}bromidopalladium nitrate

Crystal data

[PdBr(C14H23N5)]NO3	F(000) = 1016
Mr = 509.69	Dx = 1.769 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 10.934 (6) Å	Cell parameters from 70 reflections
b = 12.443 (4) Å	θ = 5.0–12.5°
c = 14.112 (6) Å	µ = 3.08 mm^−1
β = 94.76 (4)°	T = 298 K
V = 1913.4 (14) Å^3	Prism, yellow
Z = 4	0.60 × 0.40 × 0.18 mm

Data collection

Siemens P4 diffractometer	3329 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.080
Graphite monochromator	θmax = 28.8°, θmin = 2.2°
ω scans	h = −14→14
Absorption correction: ψ scan (XSCANS; Siemens, 1996)	k = −16→16
Tmin = 0.206, Tmax = 0.352	l = −19→19
12224 measured reflections	3 standard reflections every 97 reflections
4962 independent reflections	intensity decay: 2.5%

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.051	H-atom parameters constrained
wR(F^2) = 0.148	w = 1/[σ^2(Fo^2) + (0.0488P)^2 + 3.056P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max = 0.001
4962 reflections	Δρmax = 1.10 e Å^−3
231 parameters	Δρmin = −1.01 e Å^−3
0 restraints	Extinction correction: SHELXL2014, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 constraints	Extinction coefficient: 0.0042 (5)
Primary atom site location: structure-invariant direct methods

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0.72527 (4)	0.72194 (3)	0.49024 (3)	0.04869 (16)
Br1	0.82828 (6)	0.79805 (6)	0.36061 (5)	0.0713 (2)
N1	0.6855 (4)	0.8654 (4)	0.5458 (3)	0.0527 (10)
N2	0.5720 (4)	0.8754 (4)	0.5774 (3)	0.0559 (11)
C3	0.5614 (6)	0.9701 (5)	0.6223 (4)	0.0653 (15)
C4	0.6697 (6)	1.0215 (5)	0.6178 (5)	0.0683 (16)
H4A	0.6890	1.0898	0.6412	0.082*
C5	0.7463 (6)	0.9545 (4)	0.5723 (4)	0.0590 (14)
C6	0.4475 (7)	1.0010 (7)	0.6655 (6)	0.095 (3)
H6A	0.3795	0.9988	0.6179	0.143*
H6B	0.4561	1.0724	0.6908	0.143*
H6C	0.4330	0.9517	0.7157	0.143*
C7	0.8768 (6)	0.9714 (6)	0.5555 (6)	0.089 (2)
H7A	0.9217	0.9060	0.5686	0.134*
H7B	0.9105	1.0273	0.5966	0.134*
H7C	0.8827	0.9917	0.4904	0.134*
C8	0.4863 (6)	0.7883 (5)	0.5612 (5)	0.0694 (17)
H8A	0.4791	0.7704	0.4940	0.083*
H8B	0.4062	0.8114	0.5781	0.083*
C9	0.5245 (6)	0.6902 (6)	0.6176 (5)	0.0741 (18)
H9A	0.5108	0.7022	0.6838	0.089*
H9B	0.4740	0.6299	0.5949	0.089*
N10	0.6556 (4)	0.6634 (4)	0.6103 (3)	0.0566 (11)
H10	0.6956	0.7007	0.6579	0.068*
N11	0.7515 (5)	0.5725 (4)	0.4438 (3)	0.0590 (12)
N12	0.8088 (5)	0.5000 (4)	0.5054 (3)	0.0607 (12)
C13	0.8290 (6)	0.4082 (4)	0.4598 (4)	0.0596 (14)
C14	0.7837 (6)	0.4222 (5)	0.3675 (4)	0.0617 (14)
H14A	0.7853	0.3720	0.3188	0.074*
C15	0.7353 (5)	0.5240 (5)	0.3597 (4)	0.0577 (13)
C16	0.8890 (8)	0.3118 (6)	0.5076 (6)	0.091 (2)
H16A	0.8366	0.2833	0.5529	0.137*
H16B	0.9662	0.3325	0.5398	0.137*
H16C	0.9024	0.2581	0.4608	0.137*
C17	0.6657 (7)	0.5744 (6)	0.2765 (4)	0.081 (2)
H17A	0.6015	0.6186	0.2979	0.121*
H17B	0.6305	0.5194	0.2351	0.121*
H17C	0.7201	0.6179	0.2427	0.121*
C18	0.8102 (7)	0.5208 (5)	0.6062 (4)	0.0715 (18)
H18A	0.8671	0.5787	0.6233	0.086*
H18B	0.8384	0.4571	0.6412	0.086*
C19	0.6851 (7)	0.5506 (5)	0.6330 (4)	0.0704 (18)
H19A	0.6811	0.5390	0.7006	0.084*
H19B	0.6246	0.5045	0.5994	0.084*
N20	0.8449 (4)	0.7830 (3)	0.7852 (3)	0.0351 (8)
O1	0.7422 (7)	0.7835 (4)	0.7749 (4)	0.1053 (19)
O2	0.9013 (7)	0.7448 (6)	0.7245 (6)	0.125 (2)
O3	0.9009 (7)	0.8139 (5)	0.8568 (5)	0.113 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd1	0.0552 (3)	0.0486 (2)	0.0429 (2)	0.00212 (18)	0.00814 (16)	0.00166 (16)
Br1	0.0761 (4)	0.0797 (4)	0.0608 (4)	0.0144 (3)	0.0225 (3)	0.0231 (3)
N1	0.048 (2)	0.057 (3)	0.054 (2)	0.002 (2)	0.012 (2)	−0.002 (2)
N2	0.048 (2)	0.069 (3)	0.051 (2)	0.006 (2)	0.008 (2)	−0.004 (2)
C3	0.070 (4)	0.067 (4)	0.058 (3)	0.018 (3)	0.002 (3)	−0.011 (3)
C4	0.082 (4)	0.057 (3)	0.065 (4)	0.005 (3)	0.005 (3)	−0.012 (3)
C5	0.068 (3)	0.048 (3)	0.061 (3)	−0.004 (3)	0.004 (3)	0.003 (3)
C6	0.078 (5)	0.120 (6)	0.089 (5)	0.034 (5)	0.013 (4)	−0.034 (5)
C7	0.071 (4)	0.079 (4)	0.120 (6)	−0.021 (4)	0.022 (4)	−0.013 (5)
C8	0.050 (3)	0.088 (5)	0.072 (4)	−0.002 (3)	0.014 (3)	−0.007 (3)
C9	0.069 (4)	0.081 (4)	0.075 (4)	−0.024 (4)	0.024 (3)	−0.009 (4)
N10	0.066 (3)	0.061 (3)	0.044 (2)	−0.011 (2)	0.010 (2)	−0.003 (2)
N11	0.077 (3)	0.055 (2)	0.045 (2)	0.011 (2)	0.005 (2)	0.002 (2)
N12	0.080 (3)	0.049 (2)	0.052 (3)	0.008 (2)	−0.003 (2)	0.001 (2)
C13	0.064 (3)	0.049 (3)	0.066 (3)	0.009 (3)	0.010 (3)	0.002 (3)
C14	0.069 (3)	0.058 (3)	0.059 (3)	0.010 (3)	0.008 (3)	−0.010 (3)
C15	0.057 (3)	0.062 (3)	0.054 (3)	0.009 (3)	0.004 (3)	−0.008 (3)
C16	0.110 (6)	0.067 (4)	0.096 (5)	0.032 (4)	0.010 (5)	0.008 (4)
C17	0.095 (5)	0.093 (5)	0.052 (3)	0.032 (4)	−0.009 (3)	−0.009 (3)
C18	0.107 (5)	0.050 (3)	0.055 (3)	0.006 (4)	−0.011 (3)	0.007 (3)
C19	0.109 (5)	0.057 (3)	0.046 (3)	−0.011 (4)	0.017 (3)	0.007 (3)
N20	0.051 (2)	0.0202 (15)	0.0322 (17)	−0.0047 (17)	−0.0085 (16)	−0.0046 (13)
O1	0.145 (6)	0.093 (4)	0.079 (4)	−0.003 (4)	0.014 (4)	−0.016 (3)
O2	0.115 (5)	0.117 (5)	0.139 (6)	−0.022 (4)	−0.021 (5)	−0.010 (5)
O3	0.140 (5)	0.090 (4)	0.103 (4)	−0.014 (4)	−0.027 (4)	0.006 (3)

Geometric parameters (Å, º)

Pd1—N11	2.000 (5)	N10—C19	1.470 (8)
Pd1—N1	2.012 (4)	N10—H10	0.9000
Pd1—N10	2.048 (4)	N11—C15	1.330 (7)
Pd1—Br1	2.4194 (11)	N11—N12	1.368 (6)
N1—C5	1.330 (7)	N12—C13	1.339 (7)
N1—N2	1.359 (6)	N12—C18	1.444 (7)
N2—C3	1.347 (7)	C13—C14	1.366 (8)
N2—C8	1.438 (7)	C13—C16	1.500 (8)
C3—C4	1.352 (9)	C14—C15	1.373 (8)
C3—C6	1.482 (9)	C14—H14A	0.9300
C4—C5	1.378 (8)	C15—C17	1.484 (8)
C4—H4A	0.9300	C16—H16A	0.9600
C5—C7	1.480 (9)	C16—H16B	0.9600
C6—H6A	0.9600	C16—H16C	0.9600
C6—H6B	0.9600	C17—H17A	0.9600
C6—H6C	0.9600	C17—H17B	0.9600
C7—H7A	0.9600	C17—H17C	0.9600
C7—H7B	0.9600	C18—C19	1.496 (10)
C7—H7C	0.9600	C18—H18A	0.9700
C8—C9	1.498 (9)	C18—H18B	0.9700
C8—H8A	0.9700	C19—H19A	0.9700
C8—H8B	0.9700	C19—H19B	0.9700
C9—N10	1.484 (8)	N20—O2	1.195 (8)
C9—H9A	0.9700	N20—O3	1.200 (7)
C9—H9B	0.9700	N20—O1	1.121 (8)
N11—Pd1—N1	173.81 (19)	C19—N10—Pd1	115.5 (4)
N11—Pd1—N10	90.80 (19)	C9—N10—H10	104.1
N1—Pd1—N10	83.45 (19)	C19—N10—H10	104.1
N11—Pd1—Br1	91.58 (14)	Pd1—N10—H10	104.1
N1—Pd1—Br1	94.40 (13)	C15—N11—N12	106.7 (4)
N10—Pd1—Br1	173.21 (14)	C15—N11—Pd1	134.7 (4)
C5—N1—N2	106.3 (5)	N12—N11—Pd1	118.4 (3)
C5—N1—Pd1	136.9 (4)	C13—N12—N11	110.0 (4)
N2—N1—Pd1	116.2 (4)	C13—N12—C18	129.6 (5)
N1—N2—C3	110.5 (5)	N11—N12—C18	118.4 (5)
N1—N2—C8	118.7 (5)	C14—C13—N12	106.8 (5)
C3—N2—C8	130.8 (5)	C14—C13—C16	129.9 (6)
C4—C3—N2	106.4 (5)	N12—C13—C16	123.3 (6)
C4—C3—C6	131.8 (6)	C13—C14—C15	107.5 (5)
N2—C3—C6	121.9 (6)	C13—C14—H14A	126.2
C3—C4—C5	107.7 (5)	C15—C14—H14A	126.2
C3—C4—H4A	126.1	N11—C15—C14	109.0 (5)
C5—C4—H4A	126.1	N11—C15—C17	122.3 (5)
N1—C5—C4	109.0 (6)	C14—C15—C17	128.5 (5)
N1—C5—C7	122.6 (6)	C13—C16—H16A	109.5
C4—C5—C7	128.3 (6)	C13—C16—H16B	109.5
C3—C6—H6A	109.5	H16A—C16—H16B	109.5
C3—C6—H6B	109.5	C13—C16—H16C	109.5
H6A—C6—H6B	109.5	H16A—C16—H16C	109.5
C3—C6—H6C	109.5	H16B—C16—H16C	109.5
H6A—C6—H6C	109.5	C15—C17—H17A	109.5
H6B—C6—H6C	109.5	C15—C17—H17B	109.5
C5—C7—H7A	109.5	H17A—C17—H17B	109.5
C5—C7—H7B	109.5	C15—C17—H17C	109.5
H7A—C7—H7B	109.5	H17A—C17—H17C	109.5
C5—C7—H7C	109.5	H17B—C17—H17C	109.5
H7A—C7—H7C	109.5	N12—C18—C19	111.0 (5)
H7B—C7—H7C	109.5	N12—C18—H18A	109.4
N2—C8—C9	112.3 (5)	C19—C18—H18A	109.4
N2—C8—H8A	109.1	N12—C18—H18B	109.4
C9—C8—H8A	109.1	C19—C18—H18B	109.4
N2—C8—H8B	109.1	H18A—C18—H18B	108.0
C9—C8—H8B	109.1	C18—C19—N10	111.8 (5)
H8A—C8—H8B	107.9	C18—C19—H19A	109.3
N10—C9—C8	112.0 (5)	N10—C19—H19A	109.3
N10—C9—H9A	109.2	C18—C19—H19B	109.3
C8—C9—H9A	109.2	N10—C19—H19B	109.3
N10—C9—H9B	109.2	H19A—C19—H19B	107.9
C8—C9—H9B	109.2	O2—N20—O3	118.3 (6)
H9A—C9—H9B	107.9	O2—N20—O1	118.7 (5)
C9—N10—C19	113.3 (5)	O3—N20—O1	122.9 (6)
C9—N10—Pd1	113.9 (4)
C5—N1—N2—C3	0.7 (6)	C15—N11—N12—C13	0.7 (7)
Pd1—N1—N2—C3	173.2 (4)	Pd1—N11—N12—C13	−174.0 (4)
C5—N1—N2—C8	−178.2 (5)	C15—N11—N12—C18	−164.6 (6)
Pd1—N1—N2—C8	−5.6 (6)	Pd1—N11—N12—C18	20.7 (7)
N1—N2—C3—C4	0.8 (7)	N11—N12—C13—C14	−0.1 (7)
C8—N2—C3—C4	179.5 (6)	C18—N12—C13—C14	163.1 (7)
N1—N2—C3—C6	−178.8 (6)	N11—N12—C13—C16	−179.2 (6)
C8—N2—C3—C6	−0.2 (10)	C18—N12—C13—C16	−16.0 (11)
N2—C3—C4—C5	−1.9 (7)	N12—C13—C14—C15	−0.5 (7)
C6—C3—C4—C5	177.6 (7)	C16—C13—C14—C15	178.5 (7)
N2—N1—C5—C4	−1.9 (6)	N12—N11—C15—C14	−1.0 (7)
Pd1—N1—C5—C4	−172.0 (4)	Pd1—N11—C15—C14	172.4 (5)
N2—N1—C5—C7	176.5 (6)	N12—N11—C15—C17	174.4 (6)
Pd1—N1—C5—C7	6.3 (10)	Pd1—N11—C15—C17	−12.1 (10)
C3—C4—C5—N1	2.4 (7)	C13—C14—C15—N11	0.9 (7)
C3—C4—C5—C7	−175.8 (7)	C13—C14—C15—C17	−174.1 (7)
N1—N2—C8—C9	68.0 (7)	C13—N12—C18—C19	−114.3 (7)
C3—N2—C8—C9	−110.6 (7)	N11—N12—C18—C19	47.7 (7)
N2—C8—C9—N10	−47.3 (7)	N12—C18—C19—N10	−79.3 (6)
C8—C9—N10—C19	−158.6 (5)	C9—N10—C19—C18	168.4 (5)
C8—C9—N10—Pd1	−23.9 (7)	Pd1—N10—C19—C18	34.5 (6)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···N20^i	0.93	2.66	3.540 (7)	159
C7—H7C···Br1	0.96	3.06	3.500 (8)	110
C8—H8A···O3^ii	0.97	2.30	3.219 (9)	157
N10—H10···N20	0.90	2.54	3.427 (6)	169
N10—H10···O1	0.90	1.98	2.857 (7)	166
N10—H10···O2	0.90	2.43	3.181 (8)	142
C14—H14A···Br1^iii	0.93	2.88	3.687 (6)	146
C16—H16A···O1^iv	0.96	2.65	3.511 (10)	150
C17—H17A···O3^ii	0.96	2.55	3.485 (10)	164
C17—H17C···Br1	0.96	2.98	3.459 (8)	112
C18—H18A···O2	0.97	2.52	3.358 (9)	144
C18—H18B···O1^iv	0.97	2.65	3.468 (8)	142
C19—H19B···O3^iv	0.97	2.47	3.099 (9)	122

Symmetry codes: (i) −x+3/2, y+1/2, −z+3/2; (ii) x−1/2, −y+3/2, z−1/2; (iii) −x+3/2, y−1/2, −z+1/2; (iv) −x+3/2, y−1/2, −z+3/2.

(3) {Bis[2-(3,5-dimethylpyrazol-1-yl-κN²)ethyl]amine-κN}iodidopalladium iodide hemihydrate

Crystal data

[PdI(C14H2N5)]I·0.5H2O	Z = 4
Mr = 630.58	F(000) = 1196
Triclinic, P1	Dx = 2.124 Mg m^−3
a = 12.013 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 12.089 (4) Å	Cell parameters from 68 reflections
c = 15.162 (5) Å	θ = 4.2–12.0°
α = 106.17 (2)°	µ = 4.08 mm^−1
β = 97.34 (3)°	T = 299 K
γ = 106.79 (3)°	Plate, orange
V = 1972.0 (11) Å^3	0.20 × 0.15 × 0.04 mm

Data collection

Siemens P4 diffractometer	4559 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.043
Graphite monochromator	θmax = 25.0°, θmin = 1.8°
ω scans	h = −14→3
Absorption correction: ψ scan (XSCANS; Siemens, 1996)	k = −13→13
Tmin = 0.446, Tmax = 0.523	l = −18→18
8975 measured reflections	3 standard reflections every 97 reflections
6835 independent reflections	intensity decay: 1.5%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.040	Hydrogen site location: mixed
wR(F^2) = 0.101	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0324P)^2 + 6.3989P] where P = (Fo^2 + 2Fc^2)/3
6835 reflections	(Δ/σ)max = 0.001
414 parameters	Δρmax = 0.85 e Å^−3
0 restraints	Δρmin = −1.04 e Å^−3
0 constraints

Special details

Refinement. Geometry of the water molecule first regularized with soft restraints: DFIX 0.85 0.02 O1 H1 O1 H2 DANG 1.34 0.04 H1 H2 then fixed in last l.s. cycles.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0.64608 (5)	0.84173 (5)	0.70510 (4)	0.03566 (15)
I1	0.75703 (5)	0.76282 (6)	0.57898 (4)	0.05531 (17)
N1	0.6227 (5)	0.7009 (6)	0.7556 (4)	0.0393 (15)
N2	0.6504 (5)	0.7285 (6)	0.8519 (4)	0.0405 (15)
C3	0.6317 (7)	0.6248 (8)	0.8731 (6)	0.045 (2)
C4	0.5940 (7)	0.5293 (8)	0.7912 (6)	0.047 (2)
H4A	0.5768	0.4468	0.7844	0.057*
C5	0.5864 (7)	0.5794 (7)	0.7195 (6)	0.045 (2)
C6	0.6539 (9)	0.6222 (10)	0.9712 (6)	0.067 (3)
H6A	0.7355	0.6698	1.0025	0.101*
H6B	0.6382	0.5391	0.9697	0.101*
H6C	0.6022	0.6560	1.0047	0.101*
C7	0.5422 (8)	0.5142 (8)	0.6166 (6)	0.062 (3)
H7A	0.5253	0.5693	0.5863	0.093*
H7B	0.4707	0.4460	0.6052	0.093*
H7C	0.6019	0.4852	0.5917	0.093*
C8	0.6637 (7)	0.8494 (7)	0.9118 (5)	0.046 (2)
H8A	0.7347	0.9082	0.9063	0.055*
H8B	0.6738	0.8519	0.9769	0.055*
C9	0.5567 (7)	0.8842 (8)	0.8854 (6)	0.049 (2)
H9A	0.4845	0.8156	0.8749	0.058*
H9B	0.5558	0.9523	0.9371	0.058*
N10	0.5581 (5)	0.9190 (6)	0.7995 (4)	0.0389 (15)
H10A	0.6005	0.9996	0.8206	0.047*
N11	0.6523 (5)	0.9860 (5)	0.6634 (4)	0.0355 (14)
N12	0.5449 (5)	1.0022 (6)	0.6428 (4)	0.0417 (15)
C13	0.5610 (7)	1.1056 (7)	0.6222 (5)	0.0433 (19)
C14	0.6808 (7)	1.1565 (8)	0.6286 (6)	0.051 (2)
H14A	0.7183	1.2276	0.6161	0.061*
C15	0.7350 (7)	1.0819 (7)	0.6569 (5)	0.0405 (18)
C16	0.4620 (8)	1.1495 (8)	0.5978 (7)	0.059 (2)
H16A	0.3928	1.0808	0.5603	0.089*
H16B	0.4854	1.2038	0.5626	0.089*
H16C	0.4438	1.1922	0.6545	0.089*
C17	0.8642 (7)	1.0992 (9)	0.6824 (6)	0.057 (2)
H17A	0.8845	1.0992	0.7457	0.085*
H17B	0.9107	1.1760	0.6780	0.085*
H17C	0.8806	1.0337	0.6398	0.085*
C18	0.4389 (6)	0.9129 (7)	0.6494 (6)	0.047 (2)
H18A	0.4311	0.8324	0.6081	0.056*
H18B	0.3694	0.9319	0.6276	0.056*
C19	0.4409 (7)	0.9094 (7)	0.7490 (6)	0.047 (2)
H19A	0.4181	0.9763	0.7843	0.057*
H19B	0.3821	0.8334	0.7461	0.057*
Pd2	0.89057 (5)	0.31577 (5)	0.31013 (4)	0.03801 (16)
I2	0.78206 (5)	0.41030 (5)	0.43265 (4)	0.06044 (19)
N21	0.8807 (5)	0.1716 (6)	0.3554 (4)	0.0408 (15)
N22	0.8361 (5)	0.0562 (6)	0.2895 (4)	0.0413 (15)
C23	0.8361 (7)	−0.0288 (8)	0.3313 (6)	0.0441 (19)
C24	0.8777 (7)	0.0336 (8)	0.4249 (6)	0.053 (2)
H24A	0.8851	−0.0005	0.4723	0.064*
C25	0.9072 (6)	0.1582 (8)	0.4373 (5)	0.0428 (19)
C26	0.7980 (8)	−0.1613 (8)	0.2781 (7)	0.061 (2)
H26A	0.7264	−0.1845	0.2309	0.091*
H26B	0.7830	−0.2070	0.3205	0.091*
H26C	0.8598	−0.1783	0.2482	0.091*
C27	0.9661 (8)	0.2630 (8)	0.5245 (6)	0.059 (2)
H27A	1.0039	0.3345	0.5090	0.089*
H27B	1.0251	0.2453	0.5618	0.089*
H27C	0.9078	0.2777	0.5597	0.089*
C28	0.8342 (7)	0.0419 (7)	0.1900 (5)	0.045 (2)
H28A	0.7730	0.0697	0.1648	0.055*
H28B	0.8152	−0.0439	0.1541	0.055*
C29	0.9540 (7)	0.1153 (7)	0.1807 (5)	0.0435 (19)
H29A	1.0163	0.1051	0.2217	0.052*
H29B	0.9618	0.0845	0.1163	0.052*
N30	0.9695 (5)	0.2441 (5)	0.2048 (4)	0.0380 (15)
H30A	0.9298	0.2498	0.1527	0.046*
N31	0.9132 (5)	0.4530 (6)	0.2548 (5)	0.0436 (16)
N32	1.0221 (5)	0.4929 (6)	0.2337 (5)	0.0437 (16)
C33	1.0186 (7)	0.5512 (8)	0.1718 (6)	0.051 (2)
C34	0.9048 (8)	0.5537 (8)	0.1536 (7)	0.061 (2)
H34A	0.8753	0.5902	0.1139	0.073*
C35	0.8427 (7)	0.4922 (8)	0.2053 (7)	0.054 (2)
C36	1.1245 (8)	0.5984 (9)	0.1333 (7)	0.070 (3)
H36A	1.1892	0.6565	0.1841	0.104*
H36B	1.1040	0.6375	0.0897	0.104*
H36C	1.1482	0.5314	0.1014	0.104*
C37	0.7122 (8)	0.4641 (10)	0.2050 (8)	0.079 (3)
H37A	0.6921	0.4198	0.2476	0.118*
H37B	0.6656	0.4153	0.1425	0.118*
H37C	0.6957	0.5392	0.2245	0.118*
C38	1.1151 (6)	0.4525 (7)	0.2691 (5)	0.044 (2)
H38A	1.1185	0.4627	0.3352	0.053*
H38B	1.1914	0.5033	0.2641	0.053*
C39	1.0946 (6)	0.3211 (7)	0.2160 (6)	0.0430 (19)
H39A	1.1120	0.3141	0.1544	0.052*
H39B	1.1481	0.2923	0.2497	0.052*
I3	0.44634 (6)	0.76946 (6)	0.10827 (4)	0.06206 (19)
I4	−0.00003 (8)	0.83190 (7)	0.05319 (5)	0.0843 (2)
O1	0.2414 (8)	0.8235 (8)	−0.0455 (6)	0.112 (3)
H1	0.3020	0.8127	−0.0184	0.168*
H2	0.1967	0.8227	−0.0063	0.168*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd1	0.0346 (3)	0.0398 (3)	0.0366 (3)	0.0169 (3)	0.0098 (3)	0.0139 (3)
I1	0.0580 (4)	0.0757 (4)	0.0464 (3)	0.0390 (3)	0.0199 (3)	0.0212 (3)
N1	0.046 (4)	0.040 (4)	0.036 (4)	0.021 (3)	0.004 (3)	0.015 (3)
N2	0.041 (4)	0.041 (4)	0.039 (4)	0.014 (3)	0.008 (3)	0.013 (3)
C3	0.039 (4)	0.056 (5)	0.060 (5)	0.024 (4)	0.026 (4)	0.035 (5)
C4	0.051 (5)	0.041 (5)	0.059 (6)	0.023 (4)	0.018 (4)	0.022 (4)
C5	0.041 (4)	0.041 (5)	0.058 (5)	0.017 (4)	0.014 (4)	0.020 (4)
C6	0.078 (7)	0.090 (8)	0.058 (6)	0.040 (6)	0.027 (5)	0.045 (6)
C7	0.065 (6)	0.044 (5)	0.057 (6)	0.017 (5)	−0.004 (5)	−0.002 (4)
C8	0.054 (5)	0.050 (5)	0.030 (4)	0.015 (4)	0.009 (4)	0.013 (4)
C9	0.062 (6)	0.050 (5)	0.045 (5)	0.028 (4)	0.028 (4)	0.017 (4)
N10	0.035 (3)	0.033 (3)	0.048 (4)	0.011 (3)	0.013 (3)	0.012 (3)
N11	0.031 (3)	0.039 (4)	0.040 (4)	0.015 (3)	0.009 (3)	0.015 (3)
N12	0.035 (4)	0.044 (4)	0.051 (4)	0.018 (3)	0.009 (3)	0.017 (3)
C13	0.047 (5)	0.043 (5)	0.042 (5)	0.019 (4)	0.012 (4)	0.013 (4)
C14	0.048 (5)	0.049 (5)	0.053 (5)	0.007 (4)	0.009 (4)	0.025 (4)
C15	0.040 (4)	0.042 (5)	0.038 (4)	0.006 (4)	0.008 (3)	0.017 (4)
C16	0.065 (6)	0.059 (6)	0.071 (6)	0.038 (5)	0.013 (5)	0.030 (5)
C17	0.032 (4)	0.071 (6)	0.061 (6)	0.006 (4)	0.010 (4)	0.027 (5)
C18	0.029 (4)	0.042 (5)	0.065 (6)	0.011 (4)	0.003 (4)	0.018 (4)
C19	0.038 (4)	0.037 (5)	0.066 (6)	0.011 (4)	0.020 (4)	0.015 (4)
Pd2	0.0361 (3)	0.0380 (3)	0.0417 (3)	0.0144 (3)	0.0132 (3)	0.0122 (3)
I2	0.0549 (4)	0.0480 (3)	0.0688 (4)	0.0130 (3)	0.0295 (3)	0.0026 (3)
N21	0.042 (4)	0.040 (4)	0.038 (4)	0.014 (3)	0.009 (3)	0.009 (3)
N22	0.039 (4)	0.046 (4)	0.039 (4)	0.014 (3)	0.010 (3)	0.015 (3)
C23	0.034 (4)	0.054 (5)	0.051 (5)	0.018 (4)	0.013 (4)	0.023 (4)
C24	0.043 (5)	0.060 (6)	0.055 (6)	0.011 (4)	0.007 (4)	0.027 (5)
C25	0.030 (4)	0.060 (6)	0.036 (4)	0.006 (4)	0.009 (3)	0.022 (4)
C26	0.062 (6)	0.042 (5)	0.084 (7)	0.016 (4)	0.018 (5)	0.029 (5)
C27	0.063 (6)	0.063 (6)	0.043 (5)	0.006 (5)	0.013 (4)	0.019 (5)
C28	0.048 (5)	0.045 (5)	0.040 (5)	0.018 (4)	0.006 (4)	0.008 (4)
C29	0.052 (5)	0.050 (5)	0.038 (4)	0.028 (4)	0.012 (4)	0.017 (4)
N30	0.040 (4)	0.041 (4)	0.037 (3)	0.020 (3)	0.009 (3)	0.014 (3)
N31	0.036 (4)	0.038 (4)	0.062 (4)	0.015 (3)	0.018 (3)	0.019 (3)
N32	0.034 (4)	0.045 (4)	0.056 (4)	0.014 (3)	0.012 (3)	0.020 (3)
C33	0.052 (5)	0.047 (5)	0.067 (6)	0.020 (4)	0.019 (4)	0.032 (5)
C34	0.063 (6)	0.058 (6)	0.088 (7)	0.036 (5)	0.023 (5)	0.044 (5)
C35	0.041 (5)	0.042 (5)	0.085 (7)	0.018 (4)	0.010 (5)	0.026 (5)
C36	0.062 (6)	0.080 (7)	0.091 (7)	0.028 (5)	0.034 (6)	0.053 (6)
C37	0.048 (6)	0.082 (8)	0.124 (9)	0.031 (5)	0.019 (6)	0.052 (7)
C38	0.027 (4)	0.060 (6)	0.046 (5)	0.013 (4)	0.009 (3)	0.020 (4)
C39	0.034 (4)	0.054 (5)	0.052 (5)	0.023 (4)	0.013 (4)	0.025 (4)
I3	0.0659 (4)	0.0564 (4)	0.0662 (4)	0.0252 (3)	0.0144 (3)	0.0195 (3)
I4	0.1379 (7)	0.0760 (5)	0.0587 (4)	0.0551 (5)	0.0243 (4)	0.0319 (4)
O1	0.123 (7)	0.129 (7)	0.089 (6)	0.055 (6)	−0.014 (5)	0.047 (5)

Geometric parameters (Å, º)

Pd1—N11	1.999 (6)	Pd2—N31	2.026 (6)
Pd1—N1	2.018 (6)	Pd2—N30	2.071 (6)
Pd1—N10	2.061 (6)	Pd2—I2	2.5987 (11)
Pd1—I1	2.5910 (11)	N21—C25	1.307 (9)
N1—C5	1.330 (10)	N21—N22	1.374 (8)
N1—N2	1.376 (8)	N22—C23	1.349 (10)
N2—C3	1.343 (10)	N22—C28	1.467 (9)
N2—C8	1.440 (10)	C23—C24	1.355 (11)
C3—C4	1.356 (11)	C23—C26	1.480 (12)
C3—C6	1.487 (11)	C24—C25	1.395 (12)
C4—C5	1.389 (11)	C24—H24A	0.9300
C4—H4A	0.9300	C25—C27	1.472 (11)
C5—C7	1.483 (11)	C26—H26A	0.9600
C6—H6A	0.9600	C26—H26B	0.9600
C6—H6B	0.9600	C26—H26C	0.9600
C6—H6C	0.9600	C27—H27A	0.9600
C7—H7A	0.9600	C27—H27B	0.9600
C7—H7B	0.9600	C27—H27C	0.9600
C7—H7C	0.9600	C28—C29	1.504 (11)
C8—C9	1.505 (11)	C28—H28A	0.9700
C8—H8A	0.9700	C28—H28B	0.9700
C8—H8B	0.9700	C29—N30	1.446 (9)
C9—N10	1.477 (10)	C29—H29A	0.9700
C9—H9A	0.9700	C29—H29B	0.9700
C9—H9B	0.9700	N30—C39	1.481 (9)
N10—C19	1.471 (10)	N30—H30A	0.9000
N10—H10A	0.9000	N31—C35	1.331 (10)
N11—C15	1.329 (9)	N31—N32	1.370 (8)
N11—N12	1.371 (8)	N32—C33	1.326 (10)
N12—C13	1.337 (10)	N32—C38	1.442 (9)
N12—C18	1.448 (10)	C33—C34	1.371 (12)
C13—C14	1.371 (11)	C33—C36	1.496 (12)
C13—C16	1.481 (11)	C34—C35	1.370 (12)
C14—C15	1.381 (11)	C34—H34A	0.9300
C14—H14A	0.9300	C35—C37	1.503 (12)
C15—C17	1.488 (11)	C36—H36A	0.9600
C16—H16A	0.9600	C36—H36B	0.9600
C16—H16B	0.9600	C36—H36C	0.9600
C16—H16C	0.9600	C37—H37A	0.9600
C17—H17A	0.9600	C37—H37B	0.9600
C17—H17B	0.9600	C37—H37C	0.9600
C17—H17C	0.9600	C38—C39	1.497 (11)
C18—C19	1.519 (11)	C38—H38A	0.9700
C18—H18A	0.9700	C38—H38B	0.9700
C18—H18B	0.9700	C39—H39A	0.9700
C19—H19A	0.9700	C39—H39B	0.9700
C19—H19B	0.9700	O1—H1	0.8507
Pd2—N21	2.023 (6)	O1—H2	0.8502
N11—Pd1—N1	172.4 (2)	N21—Pd2—N30	89.6 (2)
N11—Pd1—N10	82.6 (2)	N31—Pd2—N30	83.6 (2)
N1—Pd1—N10	90.1 (2)	N21—Pd2—I2	93.85 (17)
N11—Pd1—I1	91.33 (17)	N31—Pd2—I2	93.00 (18)
N1—Pd1—I1	95.91 (17)	N30—Pd2—I2	175.52 (17)
N10—Pd1—I1	173.96 (17)	C25—N21—N22	106.8 (6)
C5—N1—N2	105.8 (6)	C25—N21—Pd2	135.2 (6)
C5—N1—Pd1	136.5 (5)	N22—N21—Pd2	118.0 (5)
N2—N1—Pd1	117.6 (5)	C23—N22—N21	110.3 (6)
C3—N2—N1	109.8 (6)	C23—N22—C28	126.8 (7)
C3—N2—C8	129.0 (7)	N21—N22—C28	119.3 (6)
N1—N2—C8	119.1 (6)	N22—C23—C24	106.1 (7)
N2—C3—C4	108.0 (7)	N22—C23—C26	123.0 (7)
N2—C3—C6	123.6 (8)	C24—C23—C26	131.0 (8)
C4—C3—C6	128.3 (8)	C23—C24—C25	107.6 (8)
C3—C4—C5	106.1 (7)	C23—C24—H24A	126.2
C3—C4—H4A	126.9	C25—C24—H24A	126.2
C5—C4—H4A	126.9	N21—C25—C24	109.1 (7)
N1—C5—C4	110.1 (7)	N21—C25—C27	122.5 (8)
N1—C5—C7	121.7 (7)	C24—C25—C27	128.3 (8)
C4—C5—C7	128.2 (8)	C23—C26—H26A	109.5
C3—C6—H6A	109.5	C23—C26—H26B	109.5
C3—C6—H6B	109.5	H26A—C26—H26B	109.5
H6A—C6—H6B	109.5	C23—C26—H26C	109.5
C3—C6—H6C	109.5	H26A—C26—H26C	109.5
H6A—C6—H6C	109.5	H26B—C26—H26C	109.5
H6B—C6—H6C	109.5	C25—C27—H27A	109.5
C5—C7—H7A	109.5	C25—C27—H27B	109.5
C5—C7—H7B	109.5	H27A—C27—H27B	109.5
H7A—C7—H7B	109.5	C25—C27—H27C	109.5
C5—C7—H7C	109.5	H27A—C27—H27C	109.5
H7A—C7—H7C	109.5	H27B—C27—H27C	109.5
H7B—C7—H7C	109.5	N22—C28—C29	109.8 (6)
N2—C8—C9	111.2 (6)	N22—C28—H28A	109.7
N2—C8—H8A	109.4	C29—C28—H28A	109.7
C9—C8—H8A	109.4	N22—C28—H28B	109.7
N2—C8—H8B	109.4	C29—C28—H28B	109.7
C9—C8—H8B	109.4	H28A—C28—H28B	108.2
H8A—C8—H8B	108.0	N30—C29—C28	111.9 (6)
N10—C9—C8	111.5 (6)	N30—C29—H29A	109.2
N10—C9—H9A	109.3	C28—C29—H29A	109.2
C8—C9—H9A	109.3	N30—C29—H29B	109.2
N10—C9—H9B	109.3	C28—C29—H29B	109.2
C8—C9—H9B	109.3	H29A—C29—H29B	107.9
H9A—C9—H9B	108.0	C29—N30—C39	112.6 (6)
C19—N10—C9	114.8 (6)	C29—N30—Pd2	117.1 (5)
C19—N10—Pd1	109.8 (5)	C39—N30—Pd2	113.2 (5)
C9—N10—Pd1	116.8 (4)	C29—N30—H30A	104.0
C19—N10—H10A	104.6	C39—N30—H30A	104.0
C9—N10—H10A	104.6	Pd2—N30—H30A	104.0
Pd1—N10—H10A	104.6	C35—N31—N32	104.9 (6)
C15—N11—N12	106.5 (6)	C35—N31—Pd2	136.2 (6)
C15—N11—Pd1	137.8 (5)	N32—N31—Pd2	114.9 (5)
N12—N11—Pd1	115.4 (4)	C33—N32—N31	111.6 (6)
C13—N12—N11	110.1 (6)	C33—N32—C38	129.8 (7)
C13—N12—C18	131.7 (6)	N31—N32—C38	117.9 (6)
N11—N12—C18	118.1 (6)	N32—C33—C34	106.4 (7)
N12—C13—C14	107.1 (7)	N32—C33—C36	122.2 (8)
N12—C13—C16	123.2 (7)	C34—C33—C36	131.4 (8)
C14—C13—C16	129.7 (8)	C35—C34—C33	106.8 (8)
C13—C14—C15	106.8 (7)	C35—C34—H34A	126.6
C13—C14—H14A	126.6	C33—C34—H34A	126.6
C15—C14—H14A	126.6	N31—C35—C34	110.4 (7)
N11—C15—C14	109.4 (7)	N31—C35—C37	122.7 (8)
N11—C15—C17	121.0 (7)	C34—C35—C37	126.9 (8)
C14—C15—C17	129.5 (7)	C33—C36—H36A	109.5
C13—C16—H16A	109.5	C33—C36—H36B	109.5
C13—C16—H16B	109.5	H36A—C36—H36B	109.5
H16A—C16—H16B	109.5	C33—C36—H36C	109.5
C13—C16—H16C	109.5	H36A—C36—H36C	109.5
H16A—C16—H16C	109.5	H36B—C36—H36C	109.5
H16B—C16—H16C	109.5	C35—C37—H37A	109.5
C15—C17—H17A	109.5	C35—C37—H37B	109.5
C15—C17—H17B	109.5	H37A—C37—H37B	109.5
H17A—C17—H17B	109.5	C35—C37—H37C	109.5
C15—C17—H17C	109.5	H37A—C37—H37C	109.5
H17A—C17—H17C	109.5	H37B—C37—H37C	109.5
H17B—C17—H17C	109.5	N32—C38—C39	111.9 (6)
N12—C18—C19	112.9 (6)	N32—C38—H38A	109.2
N12—C18—H18A	109.0	C39—C38—H38A	109.2
C19—C18—H18A	109.0	N32—C38—H38B	109.2
N12—C18—H18B	109.0	C39—C38—H38B	109.2
C19—C18—H18B	109.0	H38A—C38—H38B	107.9
H18A—C18—H18B	107.8	N30—C39—C38	110.8 (6)
N10—C19—C18	113.5 (6)	N30—C39—H39A	109.5
N10—C19—H19A	108.9	C38—C39—H39A	109.5
C18—C19—H19A	108.9	N30—C39—H39B	109.5
N10—C19—H19B	108.9	C38—C39—H39B	109.5
C18—C19—H19B	108.9	H39A—C39—H39B	108.1
H19A—C19—H19B	107.7	H1—O1—H2	103.6
N21—Pd2—N31	173.1 (2)
C5—N1—N2—C3	0.4 (8)	C25—N21—N22—C23	−0.5 (8)
Pd1—N1—N2—C3	−178.9 (5)	Pd2—N21—N22—C23	179.8 (5)
C5—N1—N2—C8	−164.4 (6)	C25—N21—N22—C28	−160.6 (6)
Pd1—N1—N2—C8	16.2 (8)	Pd2—N21—N22—C28	19.8 (8)
N1—N2—C3—C4	1.1 (8)	N21—N22—C23—C24	1.9 (8)
C8—N2—C3—C4	164.1 (7)	C28—N22—C23—C24	160.1 (7)
N1—N2—C3—C6	179.5 (7)	N21—N22—C23—C26	−177.3 (7)
C8—N2—C3—C6	−17.5 (12)	C28—N22—C23—C26	−19.1 (12)
N2—C3—C4—C5	−2.2 (9)	N22—C23—C24—C25	−2.5 (9)
C6—C3—C4—C5	179.5 (8)	C26—C23—C24—C25	176.6 (8)
N2—N1—C5—C4	−1.8 (8)	N22—N21—C25—C24	−1.1 (8)
Pd1—N1—C5—C4	177.4 (6)	Pd2—N21—C25—C24	178.5 (6)
N2—N1—C5—C7	176.5 (7)	N22—N21—C25—C27	175.3 (7)
Pd1—N1—C5—C7	−4.2 (12)	Pd2—N21—C25—C27	−5.1 (12)
C3—C4—C5—N1	2.6 (9)	C23—C24—C25—N21	2.3 (9)
C3—C4—C5—C7	−175.7 (8)	C23—C24—C25—C27	−173.8 (8)
C3—N2—C8—C9	−109.2 (8)	C23—N22—C28—C29	−108.1 (8)
N1—N2—C8—C9	52.5 (9)	N21—N22—C28—C29	48.3 (9)
N2—C8—C9—N10	−76.7 (8)	N22—C28—C29—N30	−78.6 (8)
C8—C9—N10—C19	158.1 (7)	C28—C29—N30—C39	167.7 (6)
C8—C9—N10—Pd1	27.4 (8)	C28—C29—N30—Pd2	33.9 (8)
C15—N11—N12—C13	1.1 (8)	C35—N31—N32—C33	−1.7 (9)
Pd1—N11—N12—C13	175.7 (5)	Pd2—N31—N32—C33	159.5 (6)
C15—N11—N12—C18	−177.0 (6)	C35—N31—N32—C38	−173.3 (7)
Pd1—N11—N12—C18	−2.3 (8)	Pd2—N31—N32—C38	−12.0 (8)
N11—N12—C13—C14	0.7 (9)	N31—N32—C33—C34	2.0 (10)
C18—N12—C13—C14	178.4 (8)	C38—N32—C33—C34	172.3 (8)
N11—N12—C13—C16	−179.4 (7)	N31—N32—C33—C36	−176.9 (8)
C18—N12—C13—C16	−1.7 (13)	C38—N32—C33—C36	−6.6 (14)
N12—C13—C14—C15	−2.1 (9)	N32—C33—C34—C35	−1.5 (11)
C16—C13—C14—C15	177.9 (8)	C36—C33—C34—C35	177.3 (10)
N12—N11—C15—C14	−2.4 (8)	N32—N31—C35—C34	0.7 (10)
Pd1—N11—C15—C14	−175.2 (6)	Pd2—N31—C35—C34	−154.4 (7)
N12—N11—C15—C17	175.1 (7)	N32—N31—C35—C37	177.6 (9)
Pd1—N11—C15—C17	2.3 (12)	Pd2—N31—C35—C37	22.5 (14)
C13—C14—C15—N11	2.9 (9)	C33—C34—C35—N31	0.5 (11)
C13—C14—C15—C17	−174.4 (8)	C33—C34—C35—C37	−176.3 (10)
C13—N12—C18—C19	−113.8 (9)	C33—N32—C38—C39	−95.7 (10)
N11—N12—C18—C19	63.7 (9)	N31—N32—C38—C39	74.1 (8)
C9—N10—C19—C18	−164.8 (6)	C29—N30—C39—C38	−162.3 (6)
Pd1—N10—C19—C18	−30.8 (7)	Pd2—N30—C39—C38	−26.7 (7)
N12—C18—C19—N10	−41.1 (9)	N32—C38—C39—N30	−46.9 (9)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···I3	0.85	2.68	3.497 (7)	161
O1—H2···I4	0.85	2.66	3.443 (10)	155
N10—H10A···I3^i	0.90	2.94	3.653 (6)	137
N30—H30A···O1^ii	0.90	2.22	3.011 (9)	146
N30—H30A···I4^ii	0.90	3.30	3.853 (6)	122

Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1, −y+1, −z.

(4) Azido{bis[2-(3,5-dimethylpyrazol-1-yl-κN²)ethyl]amine-κN}palladium azide monohydrate

Crystal data

[Pd(N3)(C14H23N5)]N3·H2O	F(000) = 960
Mr = 469.85	Dx = 1.562 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 8.132 (3) Å	Cell parameters from 65 reflections
b = 22.851 (5) Å	θ = 4.7–12.6°
c = 11.372 (3) Å	µ = 0.96 mm^−1
β = 109.03 (2)°	T = 296 K
V = 1997.8 (10) Å^3	Prism, yellow
Z = 4	0.5 × 0.4 × 0.4 mm

Data collection

Siemens P4 diffractometer	3528 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube, FN4	Rint = 0.056
Graphite monochromator	θmax = 26.3°, θmin = 1.8°
2θ/ω scans	h = −10→10
Absorption correction: ψ scan (XSCANS; Siemens, 1996)	k = −28→1
Tmin = 0.266, Tmax = 0.366	l = −13→14
8431 measured reflections	3 standard reflections every 97 reflections
4032 independent reflections	intensity decay: 1%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.036	Hydrogen site location: mixed
wR(F^2) = 0.097	H-atom parameters constrained
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0346P)^2 + 1.7119P] where P = (Fo^2 + 2Fc^2)/3
4032 reflections	(Δ/σ)max = 0.001
248 parameters	Δρmax = 0.55 e Å^−3
0 restraints	Δρmin = −1.04 e Å^−3
0 constraints

Special details

Refinement. Geometry of the water molecule first regularized with soft restraints: DFIX 0.85 0.02 O1 H1 O1 H2 DANG 1.34 0.04 H1 H2 then fixed in last l.s. cycles.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Pd1	0.35885 (3)	0.66267 (2)	0.24025 (2)	0.04508 (11)
N1	0.1428 (3)	0.62778 (11)	0.1211 (2)	0.0464 (6)
N2	−0.0024 (3)	0.62721 (12)	0.1552 (3)	0.0517 (6)
C3	−0.1283 (4)	0.59569 (14)	0.0740 (3)	0.0537 (8)
C4	−0.0629 (4)	0.57587 (15)	−0.0140 (3)	0.0565 (8)
H4A	−0.1212	0.5534	−0.0832	0.068*
C5	0.1059 (4)	0.59528 (13)	0.0184 (3)	0.0464 (7)
C6	−0.3035 (5)	0.5885 (2)	0.0869 (5)	0.0792 (12)
H6A	−0.2931	0.5670	0.1616	0.119*
H6B	−0.3777	0.5675	0.0164	0.119*
H6C	−0.3526	0.6263	0.0913	0.119*
C7	0.2369 (5)	0.58174 (18)	−0.0428 (4)	0.0643 (9)
H7A	0.1815	0.5620	−0.1201	0.096*
H7B	0.3256	0.5570	0.0105	0.096*
H7C	0.2885	0.6174	−0.0584	0.096*
C8	0.0001 (6)	0.65831 (19)	0.2670 (4)	0.0703 (11)
H8A	−0.1165	0.6594	0.2723	0.084*
H8B	0.0375	0.6983	0.2626	0.084*
C9	0.1213 (7)	0.6293 (3)	0.3823 (4)	0.0890 (15)
H9A	0.1389	0.6553	0.4528	0.107*
H9B	0.0675	0.5938	0.3988	0.107*
N10	0.2933 (5)	0.61468 (16)	0.3697 (3)	0.0689 (9)
H10	0.2793	0.5781	0.3385	0.083*
N11	0.5755 (4)	0.69476 (13)	0.3678 (2)	0.0563 (7)
N12	0.6733 (4)	0.65951 (14)	0.4606 (3)	0.0622 (8)
C13	0.8151 (5)	0.6887 (2)	0.5324 (3)	0.0683 (10)
C14	0.8074 (5)	0.7426 (2)	0.4839 (4)	0.0738 (12)
H14A	0.8889	0.7722	0.5131	0.089*
C15	0.6568 (5)	0.74619 (17)	0.3827 (3)	0.0597 (9)
C16	0.9454 (7)	0.6607 (3)	0.6430 (4)	0.0970 (17)
H16A	1.0466	0.6852	0.6721	0.146*
H16B	0.9778	0.6231	0.6199	0.146*
H16C	0.8952	0.6560	0.7080	0.146*
C17	0.5864 (7)	0.79739 (18)	0.3015 (5)	0.0816 (13)
H17A	0.6404	0.8325	0.3426	0.122*
H17B	0.4630	0.7997	0.2847	0.122*
H17C	0.6103	0.7931	0.2247	0.122*
C18	0.6068 (7)	0.6028 (2)	0.4785 (4)	0.0870 (15)
H18A	0.6858	0.5846	0.5524	0.104*
H18B	0.5994	0.5779	0.4078	0.104*
C19	0.4296 (7)	0.6086 (3)	0.4921 (4)	0.0988 (18)
H19A	0.4058	0.5744	0.5343	0.119*
H19B	0.4278	0.6427	0.5427	0.119*
N20	0.4246 (4)	0.70475 (14)	0.1065 (3)	0.0600 (7)
N21	0.3172 (4)	0.71867 (13)	0.0122 (3)	0.0589 (7)
N22	0.2246 (6)	0.7317 (2)	−0.0830 (4)	0.1040 (15)
N30	0.542 (2)	0.4721 (5)	0.2466 (9)	0.203 (6)
N31	0.416 (2)	0.4860 (4)	0.2612 (6)	0.157 (6)
N32	0.2861 (19)	0.4965 (4)	0.2913 (8)	0.183 (6)
O1	0.9351 (15)	0.4889 (3)	0.3750 (6)	0.244 (5)
H11	0.9691	0.4949	0.3136	0.366*
H12	0.8315	0.5015	0.3571	0.366*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd1	0.04258 (15)	0.05370 (16)	0.03330 (14)	−0.01038 (9)	0.00459 (10)	0.00120 (9)
N1	0.0367 (12)	0.0553 (15)	0.0446 (13)	−0.0056 (11)	0.0099 (11)	−0.0003 (11)
N2	0.0407 (14)	0.0581 (16)	0.0564 (16)	−0.0047 (11)	0.0159 (12)	−0.0024 (12)
C3	0.0363 (15)	0.0486 (17)	0.071 (2)	−0.0015 (13)	0.0100 (15)	0.0008 (15)
C4	0.0394 (16)	0.0531 (18)	0.065 (2)	−0.0003 (13)	0.0004 (15)	−0.0092 (15)
C5	0.0367 (14)	0.0488 (16)	0.0464 (16)	0.0012 (12)	0.0033 (12)	−0.0028 (13)
C6	0.0398 (19)	0.083 (3)	0.116 (4)	−0.0074 (18)	0.027 (2)	−0.006 (3)
C7	0.0514 (19)	0.073 (2)	0.065 (2)	−0.0005 (17)	0.0144 (17)	−0.0200 (18)
C8	0.063 (2)	0.088 (3)	0.071 (3)	−0.0140 (19)	0.036 (2)	−0.013 (2)
C9	0.084 (3)	0.127 (4)	0.062 (2)	−0.029 (3)	0.031 (2)	0.009 (3)
N10	0.072 (2)	0.082 (2)	0.0445 (15)	−0.0231 (17)	0.0080 (15)	0.0131 (15)
N11	0.0532 (16)	0.0667 (17)	0.0399 (14)	−0.0133 (13)	0.0028 (12)	−0.0016 (12)
N12	0.0562 (18)	0.078 (2)	0.0396 (15)	−0.0063 (14)	−0.0024 (13)	−0.0018 (13)
C13	0.050 (2)	0.100 (3)	0.0449 (18)	−0.001 (2)	0.0018 (15)	−0.022 (2)
C14	0.056 (2)	0.091 (3)	0.064 (2)	−0.021 (2)	0.0061 (18)	−0.028 (2)
C15	0.0526 (19)	0.068 (2)	0.0548 (19)	−0.0141 (16)	0.0129 (16)	−0.0172 (16)
C16	0.068 (3)	0.147 (5)	0.053 (2)	0.012 (3)	−0.012 (2)	−0.014 (3)
C17	0.090 (3)	0.060 (2)	0.084 (3)	−0.021 (2)	0.014 (3)	−0.003 (2)
C18	0.091 (3)	0.085 (3)	0.057 (2)	−0.012 (2)	−0.014 (2)	0.023 (2)
C19	0.098 (4)	0.135 (4)	0.047 (2)	−0.042 (3)	0.001 (2)	0.033 (2)
N20	0.0526 (16)	0.078 (2)	0.0443 (15)	−0.0160 (14)	0.0094 (14)	0.0058 (14)
N21	0.0582 (17)	0.0623 (17)	0.0562 (18)	0.0005 (14)	0.0188 (15)	0.0111 (14)
N22	0.093 (3)	0.124 (4)	0.077 (3)	0.006 (3)	0.004 (2)	0.048 (3)
N30	0.361 (17)	0.170 (8)	0.121 (6)	−0.016 (10)	0.140 (9)	0.001 (5)
N31	0.296 (17)	0.101 (5)	0.044 (3)	−0.072 (9)	0.014 (6)	−0.004 (3)
N32	0.293 (15)	0.094 (5)	0.087 (6)	−0.068 (7)	−0.041 (6)	0.019 (4)
O1	0.406 (14)	0.215 (7)	0.160 (6)	−0.041 (8)	0.159 (8)	−0.020 (5)

Geometric parameters (Å, º)

Pd1—N1	2.002 (3)	N11—C15	1.332 (5)
Pd1—N20	2.014 (3)	N11—N12	1.360 (4)
Pd1—N11	2.020 (3)	N12—C13	1.351 (5)
Pd1—N10	2.041 (3)	N12—C18	1.443 (5)
N1—C5	1.334 (4)	C13—C14	1.342 (6)
N1—N2	1.358 (4)	C13—C16	1.498 (6)
N2—C3	1.343 (4)	C14—C15	1.383 (5)
N2—C8	1.451 (5)	C14—H14A	0.9300
C3—C4	1.355 (5)	C15—C17	1.485 (6)
C3—C6	1.488 (5)	C16—H16A	0.9600
C4—C5	1.373 (5)	C16—H16B	0.9600
C4—H4A	0.9300	C16—H16C	0.9600
C5—C7	1.483 (5)	C17—H17A	0.9600
C6—H6A	0.9600	C17—H17B	0.9600
C6—H6B	0.9600	C17—H17C	0.9600
C6—H6C	0.9600	C18—C19	1.504 (8)
C7—H7A	0.9600	C18—H18A	0.9700
C7—H7B	0.9600	C18—H18B	0.9700
C7—H7C	0.9600	C19—H19A	0.9700
C8—C9	1.512 (7)	C19—H19B	0.9700
C8—H8A	0.9700	N20—N21	1.184 (4)
C8—H8B	0.9700	N21—N22	1.139 (5)
C9—N10	1.490 (6)	N30—N31	1.129 (16)
C9—H9A	0.9700	N31—N32	1.239 (17)
C9—H9B	0.9700	O1—H11	0.8421
N10—C19	1.477 (5)	O1—H12	0.8503
N10—H10	0.9000
N1—Pd1—N20	93.98 (11)	C9—N10—Pd1	115.0 (3)
N1—Pd1—N11	176.78 (11)	C19—N10—H10	104.1
N20—Pd1—N11	89.15 (12)	C9—N10—H10	104.1
N1—Pd1—N10	84.03 (12)	Pd1—N10—H10	104.1
N20—Pd1—N10	175.99 (14)	C15—N11—N12	106.5 (3)
N11—Pd1—N10	92.80 (12)	C15—N11—Pd1	133.8 (3)
C5—N1—N2	106.1 (2)	N12—N11—Pd1	119.7 (2)
C5—N1—Pd1	135.4 (2)	C13—N12—N11	110.2 (3)
N2—N1—Pd1	117.6 (2)	C13—N12—C18	130.0 (4)
C3—N2—N1	110.3 (3)	N11—N12—C18	119.3 (3)
C3—N2—C8	131.0 (3)	C14—C13—N12	106.7 (4)
N1—N2—C8	118.7 (3)	C14—C13—C16	131.4 (4)
N2—C3—C4	107.0 (3)	N12—C13—C16	121.8 (5)
N2—C3—C6	122.1 (4)	C13—C14—C15	107.9 (4)
C4—C3—C6	130.9 (3)	C13—C14—H14A	126.1
C3—C4—C5	107.1 (3)	C15—C14—H14A	126.1
C3—C4—H4A	126.5	N11—C15—C14	108.7 (4)
C5—C4—H4A	126.5	N11—C15—C17	122.8 (3)
N1—C5—C4	109.5 (3)	C14—C15—C17	128.5 (4)
N1—C5—C7	122.4 (3)	C13—C16—H16A	109.5
C4—C5—C7	128.0 (3)	C13—C16—H16B	109.5
C3—C6—H6A	109.5	H16A—C16—H16B	109.5
C3—C6—H6B	109.5	C13—C16—H16C	109.5
H6A—C6—H6B	109.5	H16A—C16—H16C	109.5
C3—C6—H6C	109.5	H16B—C16—H16C	109.5
H6A—C6—H6C	109.5	C15—C17—H17A	109.5
H6B—C6—H6C	109.5	C15—C17—H17B	109.5
C5—C7—H7A	109.5	H17A—C17—H17B	109.5
C5—C7—H7B	109.5	C15—C17—H17C	109.5
H7A—C7—H7B	109.5	H17A—C17—H17C	109.5
C5—C7—H7C	109.5	H17B—C17—H17C	109.5
H7A—C7—H7C	109.5	N12—C18—C19	110.5 (4)
H7B—C7—H7C	109.5	N12—C18—H18A	109.5
N2—C8—C9	111.4 (4)	C19—C18—H18A	109.5
N2—C8—H8A	109.4	N12—C18—H18B	109.5
C9—C8—H8A	109.4	C19—C18—H18B	109.5
N2—C8—H8B	109.4	H18A—C18—H18B	108.1
C9—C8—H8B	109.4	N10—C19—C18	111.1 (4)
H8A—C8—H8B	108.0	N10—C19—H19A	109.4
N10—C9—C8	112.5 (3)	C18—C19—H19A	109.4
N10—C9—H9A	109.1	N10—C19—H19B	109.4
C8—C9—H9A	109.1	C18—C19—H19B	109.4
N10—C9—H9B	109.1	H19A—C19—H19B	108.0
C8—C9—H9B	109.1	N21—N20—Pd1	120.9 (2)
H9A—C9—H9B	107.8	N22—N21—N20	174.2 (4)
C19—N10—C9	111.7 (4)	N30—N31—N32	171.4 (11)
C19—N10—Pd1	116.0 (3)	H11—O1—H12	108.2
C5—N1—N2—C3	−1.0 (4)	C15—N11—N12—C13	−0.4 (4)
Pd1—N1—N2—C3	−171.8 (2)	Pd1—N11—N12—C13	177.6 (3)
C5—N1—N2—C8	178.7 (3)	C15—N11—N12—C18	172.2 (4)
Pd1—N1—N2—C8	7.9 (4)	Pd1—N11—N12—C18	−9.9 (5)
N1—N2—C3—C4	−0.2 (4)	N11—N12—C13—C14	−0.5 (5)
C8—N2—C3—C4	−179.8 (4)	C18—N12—C13—C14	−172.0 (5)
N1—N2—C3—C6	−178.9 (3)	N11—N12—C13—C16	179.2 (4)
C8—N2—C3—C6	1.5 (6)	C18—N12—C13—C16	7.7 (7)
N2—C3—C4—C5	1.3 (4)	N12—C13—C14—C15	1.2 (5)
C6—C3—C4—C5	179.8 (4)	C16—C13—C14—C15	−178.5 (5)
N2—N1—C5—C4	1.8 (4)	N12—N11—C15—C14	1.1 (4)
Pd1—N1—C5—C4	170.1 (2)	Pd1—N11—C15—C14	−176.5 (3)
N2—N1—C5—C7	−175.5 (3)	N12—N11—C15—C17	−177.7 (4)
Pd1—N1—C5—C7	−7.2 (5)	Pd1—N11—C15—C17	4.7 (6)
C3—C4—C5—N1	−1.9 (4)	C13—C14—C15—N11	−1.4 (5)
C3—C4—C5—C7	175.2 (3)	C13—C14—C15—C17	177.3 (4)
C3—N2—C8—C9	111.5 (5)	C13—N12—C18—C19	117.0 (5)
N1—N2—C8—C9	−68.1 (4)	N11—N12—C18—C19	−53.8 (5)
N2—C8—C9—N10	46.9 (5)	C9—N10—C19—C18	−171.5 (4)
C8—C9—N10—C19	157.6 (4)	Pd1—N10—C19—C18	−37.1 (6)
C8—C9—N10—Pd1	22.7 (5)	N12—C18—C19—N10	80.6 (5)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N10—H10···N32	0.90	1.95	2.838 (11)	171
N10—H10···N31	0.90	2.66	3.460 (13)	148
O1—H11···N32^i	0.84	2.67	3.295 (19)	132
O1—H12···N30	0.85	2.38	3.08 (2)	140

Symmetry code: (i) x+1, y, z.

(5) Bis[{bis[2-(3,5-dimethylpyrazol-1-yl-κN²)ethyl]amine-κN}(thiocyanato-κN)palladium] tetrakis(thiocyanato-κS)palladate

Crystal data

[Pd(NCS)(C14H23N5)]2[Pd(NCS)4]	Z = 1
Mr = 1190.43	F(000) = 596
Triclinic, P1	Dx = 1.686 Mg m^−3
a = 9.0286 (17) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.532 (2) Å	Cell parameters from 75 reflections
c = 13.066 (3) Å	θ = 4.7–12.4°
α = 94.838 (14)°	µ = 1.45 mm^−1
β = 100.947 (12)°	T = 298 K
γ = 103.989 (13)°	Irregular_Plate, pink
V = 1172.5 (4) Å^3	0.40 × 0.40 × 0.12 mm

Data collection

Siemens P4 diffractometer	4874 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube, FN4	Rint = 0.038
Graphite monochromator	θmax = 27.5°, θmin = 2.0°
2θ/ω scans	h = −11→6
Absorption correction: ψ scan (XSCANS; Siemens, 1996)	k = −13→13
Tmin = 0.256, Tmax = 0.378	l = −16→16
8889 measured reflections	3 standard reflections every 97 reflections
5367 independent reflections	intensity decay: 1%

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.107	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.0569P)^2 + 1.1014P] where P = (Fo^2 + 2Fc^2)/3
5367 reflections	(Δ/σ)max < 0.001
282 parameters	Δρmax = 0.83 e Å^−3
0 restraints	Δρmin = −1.06 e Å^−3
0 constraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Pd1	0.36057 (3)	0.61306 (2)	0.33358 (2)	0.03862 (9)
S1	0.88007 (13)	0.60961 (16)	0.47191 (8)	0.0735 (4)
N1	0.3690 (3)	0.4656 (3)	0.2291 (2)	0.0420 (6)
N2	0.2424 (3)	0.3584 (3)	0.2003 (2)	0.0453 (6)
C3	0.2603 (4)	0.2765 (4)	0.1225 (3)	0.0526 (8)
C4	0.4009 (5)	0.3330 (4)	0.0994 (3)	0.0545 (9)
H4A	0.4443	0.2987	0.0479	0.065*
C5	0.4667 (4)	0.4500 (4)	0.1663 (2)	0.0448 (7)
C6	0.1425 (6)	0.1487 (5)	0.0757 (4)	0.0814 (15)
H6A	0.0469	0.1661	0.0415	0.122*
H6B	0.1228	0.0957	0.1304	0.122*
H6C	0.1822	0.1024	0.0253	0.122*
C7	0.6181 (5)	0.5472 (5)	0.1716 (3)	0.0610 (9)
H7A	0.6078	0.6349	0.1879	0.091*
H7B	0.6475	0.5390	0.1050	0.091*
H7C	0.6969	0.5308	0.2254	0.091*
C8	0.1152 (4)	0.3501 (4)	0.2545 (3)	0.0531 (8)
H8A	0.1555	0.3552	0.3295	0.064*
H8B	0.0391	0.2653	0.2308	0.064*
C9	0.0363 (4)	0.4580 (4)	0.2354 (3)	0.0564 (9)
H9A	−0.0338	0.4356	0.1666	0.068*	0.770 (18)
H9B	−0.0264	0.4637	0.2874	0.068*	0.770 (18)
H9C	0.0179	0.4648	0.1608	0.068*	0.230 (18)
H9D	−0.0650	0.4328	0.2538	0.068*	0.230 (18)
N10A	0.1465 (5)	0.5881 (4)	0.2405 (5)	0.0423 (14)	0.770 (18)
H10A	0.1658	0.5870	0.1754	0.051*	0.770 (18)
N10B	0.1157 (15)	0.5806 (14)	0.2894 (18)	0.041 (4)	0.230 (18)
H10B	0.0858	0.5793	0.3513	0.049*	0.230 (18)
N11	0.3365 (3)	0.7611 (3)	0.4311 (2)	0.0450 (6)
N12	0.2638 (3)	0.8493 (3)	0.3896 (2)	0.0490 (6)
C13	0.2571 (5)	0.9392 (4)	0.4656 (4)	0.0641 (11)
C14	0.3268 (6)	0.9078 (5)	0.5585 (4)	0.0698 (12)
H14A	0.3399	0.9534	0.6251	0.084*
C15	0.3743 (5)	0.7964 (4)	0.5356 (3)	0.0571 (9)
C16	0.1801 (7)	1.0477 (6)	0.4450 (6)	0.0965 (19)
H16A	0.2306	1.1016	0.3993	0.145*
H16B	0.1883	1.1009	0.5102	0.145*
H16C	0.0717	1.0105	0.4120	0.145*
C17	0.4503 (7)	0.7208 (6)	0.6096 (3)	0.0769 (13)
H17A	0.5170	0.6803	0.5766	0.115*
H17B	0.3717	0.6535	0.6288	0.115*
H17C	0.5115	0.7793	0.6716	0.115*
C18	0.1923 (5)	0.8273 (4)	0.2784 (3)	0.0552 (9)
H18A	0.2722	0.8288	0.2380	0.066*
H18B	0.1442	0.8981	0.2613	0.066*
C19	0.0713 (4)	0.6981 (4)	0.2488 (3)	0.0517 (8)
H19A	0.0083	0.6857	0.3014	0.062*	0.770 (18)
H19B	0.0028	0.6979	0.1818	0.062*	0.770 (18)
H19C	0.0421	0.6799	0.1726	0.062*	0.230 (18)
H19D	−0.0209	0.7072	0.2734	0.062*	0.230 (18)
N20	0.5799 (4)	0.6337 (3)	0.4077 (3)	0.0558 (8)
C21	0.7053 (4)	0.6233 (4)	0.4336 (3)	0.0517 (8)
Pd2	0.5000	1.0000	1.0000	0.03984 (10)
S22	0.27722 (13)	0.83780 (12)	0.91759 (10)	0.0736 (3)
C23	0.2457 (4)	0.7188 (5)	0.9922 (3)	0.0567 (9)
N24	0.2159 (6)	0.6323 (5)	1.0375 (3)	0.0849 (13)
S25	0.45759 (12)	1.11365 (12)	0.85705 (8)	0.0604 (3)
C26	0.2664 (5)	1.0806 (5)	0.8121 (3)	0.0617 (10)
N27	0.1366 (6)	1.0626 (6)	0.7789 (4)	0.1036 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Pd1	0.03258 (13)	0.04589 (15)	0.03637 (13)	0.01607 (10)	0.00092 (9)	−0.00186 (9)
S1	0.0489 (5)	0.1354 (11)	0.0481 (5)	0.0505 (6)	0.0069 (4)	0.0103 (6)
N1	0.0391 (13)	0.0488 (15)	0.0379 (12)	0.0161 (11)	0.0053 (10)	−0.0014 (11)
N2	0.0382 (13)	0.0543 (16)	0.0404 (13)	0.0122 (12)	0.0071 (11)	−0.0062 (11)
C3	0.0485 (18)	0.060 (2)	0.0478 (17)	0.0214 (16)	0.0059 (14)	−0.0103 (15)
C4	0.051 (2)	0.069 (2)	0.0476 (18)	0.0254 (18)	0.0139 (15)	−0.0029 (16)
C5	0.0432 (16)	0.0583 (19)	0.0394 (15)	0.0249 (15)	0.0095 (12)	0.0067 (13)
C6	0.069 (3)	0.077 (3)	0.085 (3)	0.005 (2)	0.021 (2)	−0.031 (3)
C7	0.053 (2)	0.071 (3)	0.066 (2)	0.0196 (19)	0.0231 (18)	0.0106 (19)
C8	0.0507 (19)	0.058 (2)	0.0485 (18)	0.0084 (16)	0.0190 (15)	−0.0036 (15)
C9	0.0334 (16)	0.070 (2)	0.062 (2)	0.0129 (15)	0.0098 (15)	−0.0085 (18)
N10A	0.0321 (19)	0.059 (2)	0.038 (3)	0.0197 (16)	0.0053 (18)	0.0015 (17)
N10B	0.025 (5)	0.064 (8)	0.037 (9)	0.017 (5)	0.010 (5)	0.000 (6)
N11	0.0449 (14)	0.0451 (15)	0.0455 (14)	0.0178 (12)	0.0061 (11)	−0.0001 (11)
N12	0.0422 (14)	0.0464 (15)	0.0599 (17)	0.0171 (12)	0.0089 (12)	0.0043 (13)
C13	0.051 (2)	0.046 (2)	0.091 (3)	0.0135 (16)	0.012 (2)	−0.0113 (19)
C14	0.071 (3)	0.066 (3)	0.065 (2)	0.017 (2)	0.012 (2)	−0.021 (2)
C15	0.062 (2)	0.055 (2)	0.0474 (18)	0.0104 (17)	0.0080 (16)	−0.0063 (15)
C16	0.085 (4)	0.062 (3)	0.142 (5)	0.037 (3)	0.014 (4)	−0.015 (3)
C17	0.093 (4)	0.085 (3)	0.045 (2)	0.022 (3)	0.001 (2)	0.005 (2)
C18	0.0502 (19)	0.065 (2)	0.062 (2)	0.0296 (17)	0.0175 (16)	0.0199 (18)
C19	0.0364 (16)	0.075 (2)	0.0500 (18)	0.0282 (16)	0.0056 (13)	0.0091 (16)
N20	0.0388 (15)	0.0595 (19)	0.0648 (19)	0.0215 (13)	−0.0024 (13)	−0.0102 (15)
C21	0.0473 (19)	0.065 (2)	0.0425 (16)	0.0237 (16)	0.0014 (14)	−0.0029 (15)
Pd2	0.02961 (16)	0.0489 (2)	0.04031 (18)	0.01548 (13)	0.00172 (12)	0.00076 (14)
S22	0.0517 (6)	0.0667 (7)	0.0806 (7)	0.0003 (5)	−0.0215 (5)	0.0161 (5)
C23	0.0440 (18)	0.070 (2)	0.0495 (19)	0.0088 (17)	0.0082 (15)	−0.0040 (17)
N24	0.085 (3)	0.096 (3)	0.057 (2)	−0.007 (2)	0.015 (2)	0.016 (2)
S25	0.0460 (5)	0.0790 (7)	0.0549 (5)	0.0166 (4)	0.0031 (4)	0.0192 (5)
C26	0.056 (2)	0.081 (3)	0.051 (2)	0.032 (2)	0.0013 (17)	0.0122 (19)
N27	0.062 (3)	0.153 (5)	0.103 (4)	0.046 (3)	−0.001 (2)	0.044 (4)

Geometric parameters (Å, º)

Pd1—N20	1.984 (3)	N10B—H10B	0.9000
Pd1—N1	2.005 (3)	N11—C15	1.340 (5)
Pd1—N11	2.009 (3)	N11—N12	1.353 (4)
Pd1—N10A	2.022 (4)	N12—C13	1.335 (5)
Pd1—N10B	2.111 (12)	N12—C18	1.447 (5)
S1—C21	1.607 (4)	C13—C14	1.362 (7)
N1—C5	1.342 (4)	C13—C16	1.493 (7)
N1—N2	1.365 (4)	C14—C15	1.372 (6)
N2—C3	1.336 (4)	C14—H14A	0.9300
N2—C8	1.449 (4)	C15—C17	1.478 (6)
C3—C4	1.366 (6)	C16—H16A	0.9600
C3—C6	1.496 (6)	C16—H16B	0.9600
C4—C5	1.379 (5)	C16—H16C	0.9600
C4—H4A	0.9300	C17—H17A	0.9600
C5—C7	1.482 (5)	C17—H17B	0.9600
C6—H6A	0.9600	C17—H17C	0.9600
C6—H6B	0.9600	C18—C19	1.493 (6)
C6—H6C	0.9600	C18—H18A	0.9700
C7—H7A	0.9600	C18—H18B	0.9700
C7—H7B	0.9600	C19—H19A	0.9700
C7—H7C	0.9600	C19—H19B	0.9700
C8—C9	1.494 (6)	C19—H19C	0.9700
C8—H8A	0.9700	C19—H19D	0.9700
C8—H8B	0.9700	N20—C21	1.153 (5)
C9—N10B	1.373 (14)	Pd2—S22	2.3085 (12)
C9—N10A	1.474 (6)	Pd2—S22^i	2.3085 (12)
C9—H9A	0.9700	Pd2—S25	2.3227 (11)
C9—H9B	0.9700	Pd2—S25^i	2.3227 (11)
C9—H9C	0.9700	S22—C23	1.656 (5)
C9—H9D	0.9700	C23—N24	1.133 (6)
N10A—C19	1.483 (5)	S25—C26	1.654 (4)
N10A—H10A	0.9000	C26—N27	1.133 (6)
N10B—C19	1.498 (15)
N20—Pd1—N1	91.68 (12)	C19—N10B—Pd1	111.8 (9)
N20—Pd1—N11	92.64 (12)	C9—N10B—H10B	103.3
N1—Pd1—N11	175.60 (11)	C19—N10B—H10B	103.3
N20—Pd1—N10A	172.5 (2)	Pd1—N10B—H10B	103.3
N1—Pd1—N10A	82.54 (18)	C15—N11—N12	106.7 (3)
N11—Pd1—N10A	93.08 (18)	C15—N11—Pd1	134.6 (3)
N20—Pd1—N10B	166.4 (7)	N12—N11—Pd1	118.6 (2)
N1—Pd1—N10B	94.8 (5)	C13—N12—N11	110.3 (3)
N11—Pd1—N10B	81.2 (5)	C13—N12—C18	129.9 (3)
C5—N1—N2	106.4 (3)	N11—N12—C18	119.4 (3)
C5—N1—Pd1	134.7 (3)	N12—C13—C14	107.0 (4)
N2—N1—Pd1	118.4 (2)	N12—C13—C16	123.0 (5)
C3—N2—N1	110.7 (3)	C14—C13—C16	129.9 (5)
C3—N2—C8	130.8 (3)	C13—C14—C15	107.3 (4)
N1—N2—C8	118.5 (3)	C13—C14—H14A	126.4
N2—C3—C4	106.7 (3)	C15—C14—H14A	126.4
N2—C3—C6	123.2 (4)	N11—C15—C14	108.7 (4)
C4—C3—C6	130.1 (3)	N11—C15—C17	123.2 (4)
C3—C4—C5	107.6 (3)	C14—C15—C17	128.1 (4)
C3—C4—H4A	126.2	C13—C16—H16A	109.5
C5—C4—H4A	126.2	C13—C16—H16B	109.5
N1—C5—C4	108.6 (3)	H16A—C16—H16B	109.5
N1—C5—C7	123.2 (3)	C13—C16—H16C	109.5
C4—C5—C7	128.2 (3)	H16A—C16—H16C	109.5
C3—C6—H6A	109.5	H16B—C16—H16C	109.5
C3—C6—H6B	109.5	C15—C17—H17A	109.5
H6A—C6—H6B	109.5	C15—C17—H17B	109.5
C3—C6—H6C	109.5	H17A—C17—H17B	109.5
H6A—C6—H6C	109.5	C15—C17—H17C	109.5
H6B—C6—H6C	109.5	H17A—C17—H17C	109.5
C5—C7—H7A	109.5	H17B—C17—H17C	109.5
C5—C7—H7B	109.5	N12—C18—C19	111.4 (3)
H7A—C7—H7B	109.5	N12—C18—H18A	109.4
C5—C7—H7C	109.5	C19—C18—H18A	109.4
H7A—C7—H7C	109.5	N12—C18—H18B	109.4
H7B—C7—H7C	109.5	C19—C18—H18B	109.4
N2—C8—C9	112.1 (3)	H18A—C18—H18B	108.0
N2—C8—H8A	109.2	N10A—C19—C18	110.4 (3)
C9—C8—H8A	109.2	C18—C19—N10B	116.8 (5)
N2—C8—H8B	109.2	N10A—C19—H19A	109.6
C9—C8—H8B	109.2	C18—C19—H19A	109.6
H8A—C8—H8B	107.9	N10A—C19—H19B	109.6
N10B—C9—C8	115.9 (6)	C18—C19—H19B	109.6
N10A—C9—C8	113.3 (3)	H19A—C19—H19B	108.1
N10A—C9—H9A	108.9	C18—C19—H19C	108.1
C8—C9—H9A	108.9	N10B—C19—H19C	108.1
N10A—C9—H9B	108.9	C18—C19—H19D	108.1
C8—C9—H9B	108.9	N10B—C19—H19D	108.1
H9A—C9—H9B	107.7	H19C—C19—H19D	107.3
N10B—C9—H9C	108.3	C21—N20—Pd1	164.8 (3)
C8—C9—H9C	108.3	N20—C21—S1	179.0 (4)
N10B—C9—H9D	108.3	S22—Pd2—S22^i	180.0
C8—C9—H9D	108.3	S22—Pd2—S25	87.77 (4)
H9C—C9—H9D	107.4	S22^i—Pd2—S25	92.23 (4)
C9—N10A—C19	112.4 (4)	S22—Pd2—S25^i	92.23 (4)
C9—N10A—Pd1	115.1 (3)	S22^i—Pd2—S25^i	87.77 (4)
C19—N10A—Pd1	117.4 (3)	S25—Pd2—S25^i	180.0
C9—N10A—H10A	103.2	C23—S22—Pd2	109.52 (14)
C19—N10A—H10A	103.2	N24—C23—S22	175.1 (4)
Pd1—N10A—H10A	103.2	C26—S25—Pd2	107.53 (16)
C9—N10B—C19	117.7 (11)	N27—C26—S25	176.9 (5)
C9—N10B—Pd1	115.0 (8)
C5—N1—N2—C3	0.8 (4)	C15—N11—N12—C13	0.6 (4)
Pd1—N1—N2—C3	173.4 (2)	Pd1—N11—N12—C13	179.3 (3)
C5—N1—N2—C8	−178.9 (3)	C15—N11—N12—C18	−172.6 (3)
Pd1—N1—N2—C8	−6.4 (4)	Pd1—N11—N12—C18	6.1 (4)
N1—N2—C3—C4	−0.9 (4)	N11—N12—C13—C14	−0.1 (5)
C8—N2—C3—C4	178.8 (4)	C18—N12—C13—C14	172.2 (4)
N1—N2—C3—C6	178.5 (4)	N11—N12—C13—C16	−178.4 (4)
C8—N2—C3—C6	−1.7 (7)	C18—N12—C13—C16	−6.1 (7)
N2—C3—C4—C5	0.6 (4)	N12—C13—C14—C15	−0.4 (5)
C6—C3—C4—C5	−178.8 (5)	C16—C13—C14—C15	177.7 (5)
N2—N1—C5—C4	−0.4 (4)	N12—N11—C15—C14	−0.8 (5)
Pd1—N1—C5—C4	−171.2 (3)	Pd1—N11—C15—C14	−179.3 (3)
N2—N1—C5—C7	179.1 (3)	N12—N11—C15—C17	177.5 (4)
Pd1—N1—C5—C7	8.3 (5)	Pd1—N11—C15—C17	−1.0 (7)
C3—C4—C5—N1	−0.1 (4)	C13—C14—C15—N11	0.8 (5)
C3—C4—C5—C7	−179.6 (4)	C13—C14—C15—C17	−177.4 (5)
C3—N2—C8—C9	−115.1 (4)	C13—N12—C18—C19	−113.4 (4)
N1—N2—C8—C9	64.6 (4)	N11—N12—C18—C19	58.3 (4)
N2—C8—C9—N10B	−75.9 (12)	C9—N10A—C19—C18	166.9 (4)
N2—C8—C9—N10A	−42.8 (5)	Pd1—N10A—C19—C18	30.0 (6)
N10B—C9—N10A—C19	−63.7 (12)	C9—N10A—C19—N10B	58.3 (11)
C8—C9—N10A—C19	−165.4 (4)	Pd1—N10A—C19—N10B	−78.6 (10)
N10B—C9—N10A—Pd1	74.3 (11)	N12—C18—C19—N10A	−77.7 (5)
C8—C9—N10A—Pd1	−27.4 (6)	N12—C18—C19—N10B	−46.7 (11)
N10A—C9—N10B—C19	68.0 (18)	C9—N10B—C19—N10A	−72.5 (18)
C8—C9—N10B—C19	160.4 (10)	Pd1—N10B—C19—N10A	64.0 (11)
N10A—C9—N10B—Pd1	−67.2 (12)	C9—N10B—C19—C18	−156.5 (11)
C8—C9—N10B—Pd1	25.2 (17)	Pd1—N10B—C19—C18	−20.0 (15)

Symmetry code: (i) −x+1, −y+2, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N10A—H10A···N24^ii	0.90	2.01	2.889 (9)	166
N10B—H10B···S1^iii	0.90	2.71	3.52 (2)	151

Symmetry codes: (ii) x, y, z−1; (iii) x−1, y, z.