The title polymeric complex, [PbPd(NCS)4(C20H36O6)(H2O)]n or {[Pb(DC18C6-A)(H2O)][Pd(SCN)4]}n (DC18C6-A = cis-syn-cis-dicyclohexyl-18-crown-6), has been synthesized by the reaction of dicyclohexyl-18-crown-6 with PdCl2 and Pb(SCN)2. The SCN groups bridge [Pb(DC18C6-A)(H2O)]2+ complex cations and [Pd(SCN)4]2− complex anions to form infinite polymeric chains.
Supporting information
CCDC reference: 227557
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.009 Å
- R factor = 0.033
- wR factor = 0.046
- Data-to-parameter ratio = 15.5
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for N1
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.241 0.259
Tmin and Tmax expected: 0.245 0.347
RR = 1.316
Please check that your absorption correction is appropriate.
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.29
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.34
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S1
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S3
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C10
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Pb1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Pd1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C21
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 1.340
Tmax scaled 0.347 Tmin scaled 0.323
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
13 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
10 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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
catena-Poly[[aqua(
cis-
syn-
cis-dicyclohexyl-18-crown-6)lead(II)]-µ-
thiocyanato-
κ2N:
S-[dithiocyanatopallalium(II)]-µ-thiocyanato-
κ2S:
N]
top
Crystal data top
[PbPd(NCS)4(C20H36O6)(H2O)] | F(000) = 1832 |
Mr = 936.41 | Dx = 1.866 Mg m−3 |
Monoclinic, P21/n | Melting point: 162 K |
Hall symbol: -P 2yn | Mo Kα radiation, λ = 0.71073 Å |
a = 14.177 (5) Å | Cell parameters from 4334 reflections |
b = 12.967 (4) Å | θ = 1.9–25.0° |
c = 18.885 (6) Å | µ = 5.88 mm−1 |
β = 106.237 (5)° | T = 298 K |
V = 3333.4 (19) Å3 | Block, red |
Z = 4 | 0.25 × 0.23 × 0.18 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 5836 independent reflections |
Radiation source: fine-focus sealed tube | 3801 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
φ and ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→16 |
Tmin = 0.241, Tmax = 0.259 | k = −15→15 |
17097 measured reflections | l = −20→22 |
Refinement top
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.046 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0003P)2] where P = (Fo2 + 2Fc2)/3 |
5836 reflections | (Δ/σ)max = 0.001 |
376 parameters | Δρmax = 1.37 e Å−3 |
39 restraints | Δρmin = −0.95 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pb1 | 0.486276 (15) | 0.886729 (16) | 0.238646 (13) | 0.04022 (7) | |
Pd1 | 0.47460 (3) | 0.38702 (3) | 0.21000 (2) | 0.03788 (12) | |
N1 | 0.5352 (4) | 0.6980 (4) | 0.2576 (3) | 0.0800 (18) | |
N2 | 0.2280 (4) | 0.5468 (5) | 0.1276 (4) | 0.100 (2) | |
N3 | 0.5102 (5) | 0.0778 (4) | 0.1630 (3) | 0.077 (2) | |
N4 | 0.5141 (4) | 0.3061 (4) | 0.4312 (3) | 0.0793 (19) | |
O1 | 0.3032 (2) | 0.8176 (3) | 0.1839 (2) | 0.0506 (11) | |
O2 | 0.3997 (3) | 0.8635 (2) | 0.0847 (2) | 0.0481 (11) | |
O3 | 0.6012 (3) | 0.8499 (3) | 0.1486 (2) | 0.0513 (11) | |
O4 | 0.6883 (3) | 0.9153 (3) | 0.2958 (2) | 0.0533 (11) | |
O5 | 0.5760 (3) | 0.8747 (3) | 0.3854 (2) | 0.0499 (10) | |
O6 | 0.3866 (3) | 0.8178 (3) | 0.3326 (2) | 0.0523 (11) | |
O7 | 0.4030 (3) | 1.0402 (3) | 0.2853 (3) | 0.0715 (15) | |
S1 | 0.50877 (13) | 0.50134 (11) | 0.30794 (10) | 0.0643 (5) | |
S2 | 0.41945 (11) | 0.51371 (11) | 0.12009 (10) | 0.0573 (5) | |
S3 | 0.43701 (13) | 0.27301 (12) | 0.11076 (10) | 0.0676 (5) | |
S4 | 0.53623 (11) | 0.25512 (10) | 0.29195 (10) | 0.0515 (5) | |
C1 | 0.2480 (4) | 0.8563 (4) | 0.1142 (4) | 0.0544 (18) | |
H1 | 0.1834 | 0.8230 | 0.1012 | 0.065* | |
C2 | 0.2328 (4) | 0.9712 (4) | 0.1160 (4) | 0.0632 (19) | |
H2A | 0.1964 | 0.9870 | 0.1512 | 0.076* | |
H2B | 0.2961 | 1.0052 | 0.1323 | 0.076* | |
C3 | 0.1778 (5) | 1.0120 (5) | 0.0417 (5) | 0.089 (2) | |
H3A | 0.1726 | 1.0864 | 0.0438 | 0.106* | |
H3B | 0.1119 | 0.9834 | 0.0272 | 0.106* | |
C4 | 0.2316 (5) | 0.9824 (5) | −0.0141 (4) | 0.083 (2) | |
H4A | 0.1945 | 1.0069 | −0.0624 | 0.099* | |
H4B | 0.2951 | 1.0164 | −0.0014 | 0.099* | |
C5 | 0.2465 (5) | 0.8680 (5) | −0.0177 (4) | 0.079 (2) | |
H5A | 0.2844 | 0.8534 | −0.0520 | 0.095* | |
H5B | 0.1832 | 0.8343 | −0.0356 | 0.095* | |
C6 | 0.2996 (4) | 0.8256 (4) | 0.0576 (4) | 0.0533 (17) | |
H6 | 0.3011 | 0.7502 | 0.0548 | 0.064* | |
C7 | 0.4643 (4) | 0.8139 (4) | 0.0488 (4) | 0.0623 (19) | |
H7A | 0.4376 | 0.8189 | −0.0043 | 0.075* | |
H7B | 0.4711 | 0.7415 | 0.0622 | 0.075* | |
C8 | 0.5604 (4) | 0.8647 (4) | 0.0721 (4) | 0.0577 (18) | |
H8A | 0.6036 | 0.8357 | 0.0455 | 0.069* | |
H8B | 0.5530 | 0.9378 | 0.0611 | 0.069* | |
C9 | 0.6970 (5) | 0.8936 (6) | 0.1734 (4) | 0.073 (2) | |
H9A | 0.6929 | 0.9681 | 0.1684 | 0.088* | |
H9B | 0.7374 | 0.8681 | 0.1433 | 0.088* | |
C10 | 0.7421 (4) | 0.8659 (5) | 0.2510 (4) | 0.081 (2) | |
H10A | 0.7407 | 0.7917 | 0.2570 | 0.098* | |
H10B | 0.8101 | 0.8883 | 0.2662 | 0.098* | |
C11 | 0.7351 (4) | 0.8997 (5) | 0.3736 (4) | 0.0589 (18) | |
H11 | 0.7485 | 0.8260 | 0.3827 | 0.071* | |
C12 | 0.8307 (4) | 0.9597 (5) | 0.4026 (4) | 0.074 (2) | |
H12A | 0.8596 | 0.9432 | 0.4542 | 0.089* | |
H12B | 0.8767 | 0.9390 | 0.3757 | 0.089* | |
C13 | 0.8140 (5) | 1.0737 (5) | 0.3945 (4) | 0.092 (3) | |
H13A | 0.7890 | 1.0913 | 0.3427 | 0.110* | |
H13B | 0.8756 | 1.1099 | 0.4144 | 0.110* | |
C14 | 0.7412 (5) | 1.1064 (5) | 0.4350 (4) | 0.077 (2) | |
H14A | 0.7286 | 1.1798 | 0.4279 | 0.092* | |
H14B | 0.7689 | 1.0940 | 0.4874 | 0.092* | |
C15 | 0.6454 (4) | 1.0479 (4) | 0.4078 (4) | 0.0567 (18) | |
H15A | 0.6016 | 1.0671 | 0.4370 | 0.068* | |
H15B | 0.6138 | 1.0662 | 0.3569 | 0.068* | |
C16 | 0.6634 (4) | 0.9337 (4) | 0.4136 (3) | 0.0474 (16) | |
H16 | 0.6907 | 0.9164 | 0.4658 | 0.057* | |
C17 | 0.5141 (4) | 0.8703 (5) | 0.4341 (3) | 0.0605 (18) | |
H17A | 0.4832 | 0.9366 | 0.4359 | 0.073* | |
H17B | 0.5525 | 0.8522 | 0.4836 | 0.073* | |
C18 | 0.4382 (5) | 0.7899 (5) | 0.4040 (4) | 0.0636 (19) | |
H18A | 0.4694 | 0.7234 | 0.4037 | 0.076* | |
H18B | 0.3937 | 0.7847 | 0.4346 | 0.076* | |
C19 | 0.3063 (5) | 0.7515 (5) | 0.3003 (4) | 0.0632 (19) | |
H19A | 0.2682 | 0.7393 | 0.3349 | 0.076* | |
H19B | 0.3304 | 0.6858 | 0.2881 | 0.076* | |
C20 | 0.2445 (4) | 0.7999 (5) | 0.2335 (4) | 0.0631 (18) | |
H20A | 0.1896 | 0.7552 | 0.2105 | 0.076* | |
H20B | 0.2187 | 0.8647 | 0.2457 | 0.076* | |
C21 | 0.5227 (4) | 0.6158 (4) | 0.2743 (3) | 0.0549 (16) | |
C22 | 0.3060 (5) | 0.5326 (4) | 0.1262 (4) | 0.0566 (19) | |
C23 | 0.4806 (5) | 0.1568 (5) | 0.1431 (4) | 0.0582 (19) | |
C24 | 0.5233 (4) | 0.2888 (4) | 0.3732 (4) | 0.0507 (18) | |
H21 | 0.370 (4) | 1.037 (3) | 0.319 (3) | 0.080* | |
H22 | 0.418 (4) | 1.1042 (19) | 0.279 (3) | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pb1 | 0.04467 (14) | 0.03358 (11) | 0.04657 (16) | −0.00189 (12) | 0.01961 (10) | 0.00093 (13) |
Pd1 | 0.0403 (3) | 0.0317 (2) | 0.0431 (3) | 0.0011 (2) | 0.0141 (2) | 0.0033 (2) |
N1 | 0.124 (5) | 0.039 (3) | 0.091 (5) | −0.004 (3) | 0.053 (4) | 0.009 (3) |
N2 | 0.086 (5) | 0.109 (5) | 0.122 (7) | 0.025 (4) | 0.056 (5) | 0.038 (4) |
N3 | 0.130 (5) | 0.039 (3) | 0.081 (5) | −0.004 (3) | 0.057 (4) | −0.003 (3) |
N4 | 0.094 (5) | 0.082 (4) | 0.060 (5) | 0.001 (3) | 0.018 (4) | 0.022 (4) |
O1 | 0.039 (2) | 0.064 (3) | 0.049 (3) | −0.004 (2) | 0.012 (2) | 0.012 (2) |
O2 | 0.045 (2) | 0.054 (3) | 0.049 (3) | −0.005 (2) | 0.019 (2) | −0.012 (2) |
O3 | 0.048 (3) | 0.068 (3) | 0.045 (3) | 0.005 (2) | 0.025 (2) | 0.002 (2) |
O4 | 0.045 (2) | 0.075 (3) | 0.042 (3) | 0.006 (2) | 0.016 (2) | −0.002 (2) |
O5 | 0.060 (3) | 0.047 (2) | 0.048 (3) | −0.007 (2) | 0.024 (2) | −0.003 (2) |
O6 | 0.059 (3) | 0.053 (3) | 0.046 (3) | −0.013 (2) | 0.018 (2) | 0.011 (2) |
O7 | 0.087 (3) | 0.041 (2) | 0.113 (5) | −0.012 (2) | 0.071 (3) | −0.013 (3) |
S1 | 0.1009 (14) | 0.0336 (9) | 0.0544 (13) | −0.0049 (9) | 0.0150 (10) | 0.0010 (8) |
S2 | 0.0579 (11) | 0.0561 (10) | 0.0576 (13) | 0.0055 (8) | 0.0156 (9) | 0.0214 (9) |
S3 | 0.0984 (15) | 0.0530 (11) | 0.0512 (14) | 0.0081 (10) | 0.0203 (11) | −0.0050 (9) |
S4 | 0.0611 (11) | 0.0343 (8) | 0.0600 (14) | 0.0055 (8) | 0.0183 (9) | 0.0105 (8) |
C1 | 0.048 (4) | 0.057 (4) | 0.057 (5) | −0.009 (3) | 0.014 (4) | 0.003 (3) |
C2 | 0.065 (5) | 0.061 (4) | 0.070 (6) | 0.012 (4) | 0.031 (4) | 0.005 (4) |
C3 | 0.070 (5) | 0.093 (6) | 0.095 (8) | 0.016 (4) | 0.010 (5) | 0.029 (5) |
C4 | 0.070 (5) | 0.102 (6) | 0.067 (7) | −0.002 (4) | 0.004 (4) | 0.025 (5) |
C5 | 0.066 (5) | 0.104 (6) | 0.062 (6) | −0.017 (4) | 0.008 (4) | −0.011 (5) |
C6 | 0.051 (4) | 0.055 (4) | 0.049 (5) | −0.002 (3) | 0.005 (4) | −0.001 (3) |
C7 | 0.075 (5) | 0.071 (4) | 0.048 (5) | 0.010 (4) | 0.029 (4) | −0.015 (4) |
C8 | 0.061 (4) | 0.070 (5) | 0.052 (5) | −0.001 (4) | 0.031 (4) | −0.007 (4) |
C9 | 0.060 (5) | 0.122 (6) | 0.045 (5) | 0.010 (5) | 0.029 (4) | 0.009 (5) |
C10 | 0.044 (4) | 0.134 (6) | 0.072 (6) | 0.012 (4) | 0.027 (4) | −0.012 (5) |
C11 | 0.053 (4) | 0.055 (4) | 0.069 (6) | 0.012 (4) | 0.019 (4) | 0.005 (4) |
C12 | 0.045 (4) | 0.095 (6) | 0.074 (6) | 0.000 (4) | 0.005 (4) | −0.012 (4) |
C13 | 0.065 (5) | 0.086 (6) | 0.119 (8) | −0.033 (4) | 0.018 (5) | 0.002 (5) |
C14 | 0.069 (5) | 0.047 (4) | 0.096 (7) | −0.004 (4) | −0.007 (4) | −0.008 (4) |
C15 | 0.055 (4) | 0.039 (4) | 0.071 (5) | −0.001 (3) | 0.009 (4) | −0.001 (3) |
C16 | 0.054 (4) | 0.044 (4) | 0.041 (5) | 0.001 (3) | 0.008 (3) | 0.002 (3) |
C17 | 0.068 (4) | 0.082 (5) | 0.039 (5) | −0.010 (4) | 0.027 (4) | −0.003 (4) |
C18 | 0.068 (5) | 0.077 (5) | 0.054 (6) | −0.008 (4) | 0.029 (4) | 0.009 (4) |
C19 | 0.071 (5) | 0.066 (4) | 0.063 (6) | −0.017 (4) | 0.036 (4) | 0.009 (4) |
C20 | 0.049 (4) | 0.078 (4) | 0.069 (5) | −0.007 (4) | 0.028 (4) | 0.017 (4) |
C21 | 0.069 (4) | 0.036 (3) | 0.070 (5) | 0.004 (4) | 0.036 (3) | −0.002 (4) |
C22 | 0.071 (5) | 0.049 (4) | 0.055 (5) | 0.016 (4) | 0.025 (4) | 0.024 (3) |
C23 | 0.084 (5) | 0.044 (4) | 0.055 (5) | −0.008 (4) | 0.033 (4) | −0.014 (4) |
C24 | 0.051 (4) | 0.048 (4) | 0.045 (5) | −0.001 (3) | 0.000 (4) | 0.019 (4) |
Geometric parameters (Å, º) top
Pb1—N1 | 2.542 (5) | C4—C5 | 1.503 (8) |
Pb1—N3i | 2.927 (5) | C4—H4A | 0.9700 |
Pb1—O1 | 2.666 (4) | C4—H4B | 0.9700 |
Pb1—O2 | 2.839 (4) | C5—C6 | 1.514 (8) |
Pb1—O3 | 2.706 (3) | C5—H5A | 0.9700 |
Pb1—O4 | 2.789 (4) | C5—H5B | 0.9700 |
Pb1—O5 | 2.711 (4) | C6—H6 | 0.9800 |
Pb1—O6 | 2.710 (4) | C7—C8 | 1.465 (7) |
Pb1—O7 | 2.591 (3) | C7—H7A | 0.9700 |
Pd1—S1 | 2.3136 (18) | C7—H7B | 0.9700 |
Pd1—S2 | 2.3347 (17) | C8—H8A | 0.9700 |
Pd1—S3 | 2.3288 (18) | C8—H8B | 0.9700 |
Pd1—S4 | 2.3082 (16) | C9—C10 | 1.471 (8) |
N1—C21 | 1.139 (6) | C9—H9A | 0.9700 |
N2—C22 | 1.128 (6) | C9—H9B | 0.9700 |
N3—C23 | 1.130 (6) | C10—H10A | 0.9700 |
N4—C24 | 1.160 (7) | C10—H10B | 0.9700 |
O1—C1 | 1.421 (7) | C11—C16 | 1.491 (7) |
O1—C20 | 1.434 (6) | C11—C12 | 1.526 (7) |
O2—C6 | 1.452 (6) | C11—H11 | 0.9800 |
O2—C7 | 1.434 (5) | C12—C13 | 1.498 (7) |
O3—C8 | 1.412 (7) | C12—H12A | 0.9700 |
O3—C9 | 1.425 (6) | C12—H12B | 0.9700 |
O4—C10 | 1.437 (6) | C13—C14 | 1.507 (8) |
O4—C11 | 1.447 (7) | C13—H13A | 0.9700 |
O5—C16 | 1.427 (6) | C13—H13B | 0.9700 |
O5—C17 | 1.440 (5) | C14—C15 | 1.515 (7) |
O6—C18 | 1.391 (7) | C14—H14A | 0.9700 |
O6—C19 | 1.421 (6) | C14—H14B | 0.9700 |
O7—H21 | 0.90 (3) | C15—C16 | 1.502 (6) |
O7—H22 | 0.874 (18) | C15—H15A | 0.9700 |
S1—C21 | 1.648 (6) | C15—H15B | 0.9700 |
S2—C22 | 1.663 (7) | C16—H16 | 0.9800 |
S3—C23 | 1.678 (7) | C17—C18 | 1.492 (7) |
S4—C24 | 1.654 (7) | C17—H17A | 0.9700 |
C1—C2 | 1.508 (7) | C17—H17B | 0.9700 |
C1—C6 | 1.508 (7) | C18—H18A | 0.9700 |
C1—H1 | 0.9800 | C18—H18B | 0.9700 |
C2—C3 | 1.497 (8) | C19—C20 | 1.460 (8) |
C2—H2A | 0.9700 | C19—H19A | 0.9700 |
C2—H2B | 0.9700 | C19—H19B | 0.9700 |
C3—C4 | 1.514 (8) | C20—H20A | 0.9700 |
C3—H3A | 0.9700 | C20—H20B | 0.9700 |
C3—H3B | 0.9700 | | |
| | | |
N1—Pb1—O7 | 145.49 (15) | O2—C7—H7A | 110.0 |
N1—Pb1—O1 | 85.92 (15) | C8—C7—H7A | 110.0 |
O7—Pb1—O1 | 84.44 (13) | O2—C7—H7B | 110.0 |
N1—Pb1—O3 | 74.35 (13) | C8—C7—H7B | 110.0 |
O7—Pb1—O3 | 139.53 (11) | H7A—C7—H7B | 108.3 |
O1—Pb1—O3 | 112.90 (13) | O3—C8—C7 | 109.0 (5) |
N1—Pb1—O6 | 76.23 (14) | O3—C8—H8A | 109.9 |
O7—Pb1—O6 | 70.13 (12) | C7—C8—H8A | 109.9 |
O1—Pb1—O6 | 60.89 (13) | O3—C8—H8B | 109.9 |
O3—Pb1—O6 | 150.34 (11) | C7—C8—H8B | 109.9 |
N1—Pb1—O5 | 76.65 (15) | H8A—C8—H8B | 108.3 |
O7—Pb1—O5 | 79.91 (14) | O3—C9—C10 | 109.8 (5) |
O1—Pb1—O5 | 120.31 (11) | O3—C9—H9A | 109.7 |
O3—Pb1—O5 | 116.05 (12) | C10—C9—H9A | 109.7 |
O6—Pb1—O5 | 59.57 (12) | O3—C9—H9B | 109.7 |
N1—Pb1—O2 | 93.72 (15) | C10—C9—H9B | 109.7 |
O7—Pb1—O2 | 108.80 (14) | H9A—C9—H9B | 108.2 |
O1—Pb1—O2 | 58.13 (11) | O4—C10—C9 | 108.9 (5) |
O3—Pb1—O2 | 60.09 (12) | O4—C10—H10A | 109.9 |
O6—Pb1—O2 | 118.71 (12) | C9—C10—H10A | 109.9 |
O5—Pb1—O2 | 170.37 (9) | O4—C10—H10B | 109.9 |
S4—Pd1—S1 | 89.05 (6) | C9—C10—H10B | 109.9 |
S4—Pd1—S3 | 91.59 (6) | H10A—C10—H10B | 108.3 |
S1—Pd1—S3 | 178.88 (6) | O4—C11—C16 | 106.8 (5) |
S4—Pd1—S2 | 174.90 (6) | O4—C11—C12 | 113.7 (5) |
S1—Pd1—S2 | 94.77 (7) | C16—C11—C12 | 109.3 (5) |
S3—Pd1—S2 | 84.65 (6) | O4—C11—H11 | 109.0 |
C21—N1—Pb1 | 151.9 (5) | C16—C11—H11 | 109.0 |
C1—O1—C20 | 113.1 (4) | C12—C11—H11 | 109.0 |
C1—O1—Pb1 | 117.7 (3) | C13—C12—C11 | 111.5 (5) |
C20—O1—Pb1 | 118.7 (4) | C13—C12—H12A | 109.3 |
C7—O2—C6 | 111.9 (4) | C11—C12—H12A | 109.3 |
C7—O2—Pb1 | 112.4 (3) | C13—C12—H12B | 109.3 |
C6—O2—Pb1 | 119.7 (3) | C11—C12—H12B | 109.3 |
C8—O3—C9 | 111.3 (4) | H12A—C12—H12B | 108.0 |
C8—O3—Pb1 | 118.2 (3) | C12—C13—C14 | 109.8 (5) |
C9—O3—Pb1 | 114.2 (3) | C12—C13—H13A | 109.7 |
C10—O4—C11 | 111.6 (4) | C14—C13—H13A | 109.7 |
C16—O5—C17 | 113.8 (4) | C12—C13—H13B | 109.7 |
C16—O5—Pb1 | 117.4 (3) | C14—C13—H13B | 109.7 |
C17—O5—Pb1 | 117.4 (3) | H13A—C13—H13B | 108.2 |
C18—O6—C19 | 113.6 (4) | C13—C14—C15 | 111.3 (5) |
C18—O6—Pb1 | 119.4 (3) | C13—C14—H14A | 109.4 |
C19—O6—Pb1 | 114.9 (3) | C15—C14—H14A | 109.4 |
Pb1—O7—H21 | 126 (3) | C13—C14—H14B | 109.4 |
Pb1—O7—H22 | 122 (3) | C15—C14—H14B | 109.4 |
H21—O7—H22 | 110 (3) | H14A—C14—H14B | 108.0 |
C21—S1—Pd1 | 106.9 (2) | C16—C15—C14 | 110.5 (5) |
C22—S2—Pd1 | 100.8 (2) | C16—C15—H15A | 109.5 |
C23—S3—Pd1 | 107.4 (2) | C14—C15—H15A | 109.5 |
C24—S4—Pd1 | 107.9 (2) | C16—C15—H15B | 109.5 |
O1—C1—C6 | 108.3 (5) | C14—C15—H15B | 109.5 |
O1—C1—C2 | 111.9 (5) | H15A—C15—H15B | 108.1 |
C6—C1—C2 | 112.2 (5) | O5—C16—C11 | 107.2 (5) |
O1—C1—H1 | 108.1 | O5—C16—C15 | 112.9 (5) |
C6—C1—H1 | 108.1 | C11—C16—C15 | 112.4 (5) |
C2—C1—H1 | 108.1 | O5—C16—H16 | 108.0 |
C3—C2—C1 | 111.6 (6) | C11—C16—H16 | 108.0 |
C3—C2—H2A | 109.3 | C15—C16—H16 | 108.0 |
C1—C2—H2A | 109.3 | O5—C17—C18 | 106.7 (5) |
C3—C2—H2B | 109.3 | O5—C17—H17A | 110.4 |
C1—C2—H2B | 109.3 | C18—C17—H17A | 110.4 |
H2A—C2—H2B | 108.0 | O5—C17—H17B | 110.4 |
C2—C3—C4 | 109.4 (6) | C18—C17—H17B | 110.4 |
C2—C3—H3A | 109.8 | H17A—C17—H17B | 108.6 |
C4—C3—H3A | 109.8 | O6—C18—C17 | 108.4 (5) |
C2—C3—H3B | 109.8 | O6—C18—H18A | 110.0 |
C4—C3—H3B | 109.8 | C17—C18—H18A | 110.0 |
H3A—C3—H3B | 108.2 | O6—C18—H18B | 110.0 |
C5—C4—C3 | 112.6 (6) | C17—C18—H18B | 110.0 |
C5—C4—H4A | 109.1 | H18A—C18—H18B | 108.4 |
C3—C4—H4A | 109.1 | O6—C19—C20 | 109.0 (5) |
C5—C4—H4B | 109.1 | O6—C19—H19A | 109.9 |
C3—C4—H4B | 109.1 | C20—C19—H19A | 109.9 |
H4A—C4—H4B | 107.8 | O6—C19—H19B | 109.9 |
C4—C5—C6 | 110.9 (6) | C20—C19—H19B | 109.9 |
C4—C5—H5A | 109.5 | H19A—C19—H19B | 108.3 |
C6—C5—H5A | 109.5 | O1—C20—C19 | 108.4 (5) |
C4—C5—H5B | 109.5 | O1—C20—H20A | 110.0 |
C6—C5—H5B | 109.5 | C19—C20—H20A | 110.0 |
H5A—C5—H5B | 108.1 | O1—C20—H20B | 110.0 |
O2—C6—C1 | 106.3 (5) | C19—C20—H20B | 110.0 |
O2—C6—C5 | 112.8 (5) | H20A—C20—H20B | 108.4 |
C1—C6—C5 | 110.9 (5) | N1—C21—S1 | 173.7 (6) |
O2—C6—H6 | 108.9 | N2—C22—S2 | 177.3 (7) |
C1—C6—H6 | 108.9 | N3—C23—S3 | 178.0 (6) |
C5—C6—H6 | 108.9 | N4—C24—S4 | 175.9 (6) |
O2—C7—C8 | 108.7 (5) | | |
| | | |
O7—Pb1—N1—C21 | 33.0 (14) | S2—Pd1—S1—C21 | −21.7 (2) |
O1—Pb1—N1—C21 | −41.0 (12) | S1—Pd1—S2—C22 | −79.7 (2) |
O3—Pb1—N1—C21 | −156.2 (12) | S3—Pd1—S2—C22 | 99.3 (2) |
O6—Pb1—N1—C21 | 20.0 (12) | S4—Pd1—S3—C23 | −5.3 (2) |
O5—Pb1—N1—C21 | 81.4 (12) | S2—Pd1—S3—C23 | 171.3 (2) |
O2—Pb1—N1—C21 | −98.7 (12) | S1—Pd1—S4—C24 | 26.3 (2) |
N1—Pb1—O1—C1 | −129.4 (4) | S3—Pd1—S4—C24 | −152.8 (2) |
O7—Pb1—O1—C1 | 83.8 (4) | C20—O1—C1—C6 | −153.6 (5) |
O3—Pb1—O1—C1 | −58.3 (4) | Pb1—O1—C1—C6 | 62.0 (5) |
O6—Pb1—O1—C1 | 154.1 (4) | C20—O1—C1—C2 | 82.3 (6) |
O5—Pb1—O1—C1 | 158.6 (3) | Pb1—O1—C1—C2 | −62.1 (5) |
O2—Pb1—O1—C1 | −32.5 (3) | O1—C1—C2—C3 | 177.9 (5) |
N1—Pb1—O1—C20 | 88.2 (4) | C6—C1—C2—C3 | 56.0 (7) |
O7—Pb1—O1—C20 | −58.6 (4) | C1—C2—C3—C4 | −56.0 (7) |
O3—Pb1—O1—C20 | 159.3 (3) | C2—C3—C4—C5 | 56.8 (8) |
O6—Pb1—O1—C20 | 11.7 (3) | C3—C4—C5—C6 | −55.9 (8) |
O5—Pb1—O1—C20 | 16.3 (4) | C7—O2—C6—C1 | 162.3 (5) |
O2—Pb1—O1—C20 | −174.8 (4) | Pb1—O2—C6—C1 | 27.8 (5) |
N1—Pb1—O2—C7 | −51.5 (3) | C7—O2—C6—C5 | −75.9 (6) |
O7—Pb1—O2—C7 | 155.1 (3) | Pb1—O2—C6—C5 | 149.5 (4) |
O1—Pb1—O2—C7 | −134.3 (3) | O1—C1—C6—O2 | −54.8 (6) |
O3—Pb1—O2—C7 | 18.1 (3) | C2—C1—C6—O2 | 69.1 (6) |
O6—Pb1—O2—C7 | −127.8 (3) | O1—C1—C6—C5 | −177.9 (5) |
N1—Pb1—O2—C6 | 82.9 (3) | C2—C1—C6—C5 | −53.9 (7) |
O7—Pb1—O2—C6 | −70.6 (3) | C4—C5—C6—O2 | −65.8 (7) |
O1—Pb1—O2—C6 | 0.0 (3) | C4—C5—C6—C1 | 53.4 (7) |
O3—Pb1—O2—C6 | 152.4 (4) | C6—O2—C7—C8 | 173.1 (5) |
O6—Pb1—O2—C6 | 6.6 (4) | Pb1—O2—C7—C8 | −48.9 (5) |
N1—Pb1—O3—C8 | 119.7 (4) | C9—O3—C8—C7 | 177.1 (5) |
O7—Pb1—O3—C8 | −68.3 (4) | Pb1—O3—C8—C7 | −47.8 (5) |
O1—Pb1—O3—C8 | 41.1 (4) | O2—C7—C8—O3 | 63.9 (6) |
O6—Pb1—O3—C8 | 112.2 (4) | C8—O3—C9—C10 | −173.0 (5) |
O5—Pb1—O3—C8 | −174.1 (3) | Pb1—O3—C9—C10 | 49.9 (6) |
O2—Pb1—O3—C8 | 15.9 (3) | C11—O4—C10—C9 | −174.1 (5) |
N1—Pb1—O3—C9 | −106.5 (4) | O3—C9—C10—O4 | −66.6 (7) |
O7—Pb1—O3—C9 | 65.5 (5) | C10—O4—C11—C16 | −168.2 (5) |
O1—Pb1—O3—C9 | 175.0 (4) | C10—O4—C11—C12 | 71.2 (6) |
O6—Pb1—O3—C9 | −114.0 (4) | O4—C11—C12—C13 | 61.8 (7) |
O5—Pb1—O3—C9 | −40.3 (4) | C16—C11—C12—C13 | −57.5 (7) |
O2—Pb1—O3—C9 | 149.7 (4) | C11—C12—C13—C14 | 58.0 (8) |
N1—Pb1—O5—C16 | 117.3 (3) | C12—C13—C14—C15 | −56.8 (8) |
O7—Pb1—O5—C16 | −88.2 (3) | C13—C14—C15—C16 | 55.4 (7) |
O1—Pb1—O5—C16 | −165.6 (3) | C17—O5—C16—C11 | 158.9 (5) |
O3—Pb1—O5—C16 | 52.4 (3) | Pb1—O5—C16—C11 | −58.3 (5) |
O6—Pb1—O5—C16 | −161.0 (3) | C17—O5—C16—C15 | −76.7 (6) |
N1—Pb1—O5—C17 | −101.3 (4) | Pb1—O5—C16—C15 | 66.1 (5) |
O7—Pb1—O5—C17 | 53.2 (3) | O4—C11—C16—O5 | 57.3 (6) |
O1—Pb1—O5—C17 | −24.2 (4) | C12—C11—C16—O5 | −179.2 (5) |
O3—Pb1—O5—C17 | −166.1 (3) | O4—C11—C16—C15 | −67.3 (6) |
O6—Pb1—O5—C17 | −19.6 (3) | C12—C11—C16—C15 | 56.1 (7) |
N1—Pb1—O6—C18 | 67.8 (4) | C14—C15—C16—O5 | −177.2 (5) |
O7—Pb1—O6—C18 | −104.4 (4) | C14—C15—C16—C11 | −55.7 (7) |
O1—Pb1—O6—C18 | 160.8 (4) | C16—O5—C17—C18 | −168.8 (4) |
O3—Pb1—O6—C18 | 75.3 (5) | Pb1—O5—C17—C18 | 48.4 (5) |
O5—Pb1—O6—C18 | −14.6 (4) | C19—O6—C18—C17 | −174.8 (5) |
O2—Pb1—O6—C18 | 154.5 (4) | Pb1—O6—C18—C17 | 44.6 (6) |
N1—Pb1—O6—C19 | −72.3 (4) | O5—C17—C18—O6 | −58.7 (6) |
O7—Pb1—O6—C19 | 115.5 (4) | C18—O6—C19—C20 | 167.1 (5) |
O1—Pb1—O6—C19 | 20.7 (3) | Pb1—O6—C19—C20 | −50.4 (6) |
O3—Pb1—O6—C19 | −64.9 (5) | C1—O1—C20—C19 | 174.8 (5) |
O5—Pb1—O6—C19 | −154.8 (4) | Pb1—O1—C20—C19 | −41.2 (6) |
O2—Pb1—O6—C19 | 14.3 (4) | O6—C19—C20—O1 | 59.1 (7) |
S4—Pd1—S1—C21 | 154.9 (2) | | |
Symmetry code: (i) x, y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H21···N2ii | 0.90 (3) | 1.93 (3) | 2.805 (7) | 165 (6) |
O7—H22···S4i | 0.87 (2) | 2.54 (3) | 3.349 (4) | 154 (5) |
Symmetry codes: (i) x, y+1, z; (ii) −x+1/2, y+1/2, −z+1/2. |