Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270108042236/fg3072sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270108042236/fg3072Isup2.hkl |
CCDC reference: 718111
The title salt was prepared by reaction of Pb(ClO4)2.3H2O (5 mg, 0.0215 mmol) and terpyridine (9.9 mg, 0.0215 mmol) in MeCN (5 ml). Crystals were grown by diffusion of diethyl ether into the reaction mixture. Analysis found (calculated for C15H11Cl2N3O8Pb): C 28.10 (28.18), H 1.80 (1.73), N 6.55 (6.57).
H atoms were placed geometrically and refined riding at a distance of 0.95 Å from their parent C atoms with Uiso(H) = 1.2Ueq(C). Rigid bond restraints were applied to all anisotropic displacement parameters.
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: enCIFer (Allen et al., 2004), PLATON (Spek, 2003), publCIF (Westrip, 2008).
[Pb(ClO4)2(C15H11N3)] | F(000) = 6040 |
Mr = 639.36 | Dx = 2.359 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2817 reflections |
a = 25.440 (4) Å | θ = 2.5–27.9° |
b = 16.333 (3) Å | µ = 9.72 mm−1 |
c = 21.916 (4) Å | T = 150 K |
β = 98.671 (2)° | Column, colourless |
V = 9002 (4) Å3 | 0.25 × 0.08 × 0.05 mm |
Z = 20 |
Bruker SMART APEX CCD area-detector diffractometer | 8832 independent reflections |
Radiation source: sealed tube | 4705 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
ω scans | θmax = 26.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −32→30 |
Tmin = 0.514, Tmax = 1.000 | k = −12→21 |
27358 measured reflections | l = −24→27 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.126 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ^2^(Fo^2^) + (0.027P)^2^ + 69.73P] where P = (Fo^2^ + 2Fc^2^)/3 |
8832 reflections | (Δ/σ)max = 0.003 |
655 parameters | Δρmax = 2.07 e Å−3 |
220 restraints | Δρmin = −2.43 e Å−3 |
[Pb(ClO4)2(C15H11N3)] | V = 9002 (4) Å3 |
Mr = 639.36 | Z = 20 |
Monoclinic, C2/c | Mo Kα radiation |
a = 25.440 (4) Å | µ = 9.72 mm−1 |
b = 16.333 (3) Å | T = 150 K |
c = 21.916 (4) Å | 0.25 × 0.08 × 0.05 mm |
β = 98.671 (2)° |
Bruker SMART APEX CCD area-detector diffractometer | 8832 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4705 reflections with I > 2σ(I) |
Tmin = 0.514, Tmax = 1.000 | Rint = 0.052 |
27358 measured reflections |
R[F2 > 2σ(F2)] = 0.045 | 220 restraints |
wR(F2) = 0.126 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ^2^(Fo^2^) + (0.027P)^2^ + 69.73P] where P = (Fo^2^ + 2Fc^2^)/3 |
8832 reflections | Δρmax = 2.07 e Å−3 |
655 parameters | Δρmin = −2.43 e Å−3 |
Geometry. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 23.5451 (0.0492) x + 1.7226 (0.0859) y + 4.8224 (0.1106) z = 9.1427 (0.0561) * 0.0033 (0.0088) N3 * 0.0025 (0.0089) C11 * -0.0014 (0.0090) C12 * -0.0049 (0.0092) C13 * 0.0107 (0.0096) C14 * -0.0101 (0.0092) C15 - 0.4850 (0.0196) Pb1 Rms deviation of fitted atoms = 0.0066 23.5313 (0.0506) x - 1.6446 (0.0850) y + 4.8831 (0.1126) z = 6.4665 (0.0630) Angle to previous plane (with approximate e.s.d.) = 11.83 (0.48) * -0.0214 (0.0082) N1 * 0.0286 (0.0090) C1 * -0.0173 (0.0099) C2 * -0.0006 (0.0103) C3 * 0.0068 (0.0096) C4 * 0.0040 (0.0089) C5 0.2393 (0.0198) Pb1 Rms deviation of fitted atoms = 0.0165 24.0082 (0.0420) x - 0.7988 (0.0824) y + 3.9689 (0.1077) z = 2.4376 (0.0345) Angle to previous plane (with approximate e.s.d.) = 3.88 (0.49) * -0.0160 (0.0081) N4 * 0.0038 (0.0087) C26 * 0.0021 (0.0095) C27 * 0.0029 (0.0095) C28 * -0.0141 (0.0089) C29 * 0.0212 (0.0087) C30 0.0065 (0.0192) Pb2 Rms deviation of fitted atoms = 0.0124 24.0055 (0.0418) x + 1.1685 (0.0899) y + 3.8852 (0.1065) z = 2.9174 (0.0326) Angle to previous plane (with approximate e.s.d.) = 6.91 (0.44) * 0.0014 (0.0085) N6 * -0.0042 (0.0090) C16 * 0.0097 (0.0089) C17 * -0.0118 (0.0091) C18 * 0.0083 (0.0090) C19 * -0.0034 (0.0089) C20 0.3427 (0.0191) Pb2 Rms deviation of fitted atoms = 0.0074 24.0996 (0.0400) x - 0.6892 (0.1045) y + 3.7494 (0.1053) z = 12.8401 (0.0432) Angle to previous plane (with approximate e.s.d.) = 6.53 (0.43) * 0.0110 (0.0067) N8 * -0.0050 (0.0037) C32 * -0.0050 (0.0037) C32 * 0.0093 (0.0099) C33 * 0.0014 (0.0086) C34 * -0.0116 (0.0086) C35 - 0.1401 (0.0209) Pb3 Rms deviation of fitted atoms = 0.0081 24.1132 (0.0401) x + 0.6461 (0.0816) y + 3.7202 (0.1065) z = 13.1264 (0.0266) Angle to previous plane (with approximate e.s.d.) = 4.69 (0.42) * -0.0156 (0.0080) N8_$1 * 0.0089 (0.0086) C31_$1 * 0.0029 (0.0087) C32_$1 * -0.0076 (0.0088) C33_$1 * 0.0008 (0.0089) C34_$1 * 0.0107 (0.0084) C35_$1 Rms deviation of fitted atoms = 0.0092 |
x | y | z | Uiso*/Ueq | ||
Pb1 | 0.29584 (2) | 0.58101 (3) | 0.14318 (2) | 0.0274 (1) | |
Pb2 | 0.10584 (2) | 0.41745 (3) | 0.05993 (2) | 0.0204 (1) | |
Pb3 | 0.50000 | 0.41658 (5) | 0.25000 | 0.0265 (2) | |
Cl1 | 0.36484 (14) | 0.4067 (2) | 0.26047 (12) | 0.0301 (10) | |
Cl2 | 0.23748 (13) | 0.4117 (3) | 0.03496 (12) | 0.0300 (9) | |
Cl3 | 0.16410 (13) | 0.5837 (3) | 0.16825 (11) | 0.0300 (10) | |
Cl4 | 0.43245 (12) | 0.5844 (2) | 0.13279 (11) | 0.0257 (9) | |
Cl5 | −0.03225 (12) | 0.4109 (2) | 0.06172 (11) | 0.0243 (9) | |
O1 | 0.4021 (4) | 0.3798 (7) | 0.2208 (4) | 0.052 (3) | |
O2 | 0.3876 (4) | 0.4700 (7) | 0.2983 (5) | 0.062 (4) | |
O3 | 0.3162 (4) | 0.4330 (7) | 0.2227 (4) | 0.041 (3) | |
O4 | 0.3533 (5) | 0.3375 (8) | 0.2960 (5) | 0.083 (5) | |
O5 | 0.2041 (4) | 0.3644 (6) | 0.0685 (4) | 0.044 (3) | |
O6 | 0.2881 (4) | 0.4250 (7) | 0.0713 (4) | 0.044 (3) | |
O7 | 0.2113 (4) | 0.4887 (8) | 0.0218 (5) | 0.069 (4) | |
O8 | 0.2434 (5) | 0.3708 (10) | −0.0191 (5) | 0.105 (5) | |
O9 | 0.1980 (4) | 0.6303 (7) | 0.1360 (4) | 0.047 (3) | |
O10 | 0.1597 (5) | 0.6207 (10) | 0.2234 (5) | 0.109 (6) | |
O11 | 0.1867 (4) | 0.5058 (8) | 0.1775 (6) | 0.077 (4) | |
O12 | 0.1125 (4) | 0.5753 (7) | 0.1328 (4) | 0.040 (3) | |
O13 | 0.3941 (4) | 0.6119 (7) | 0.1706 (4) | 0.051 (3) | |
O14 | 0.4106 (5) | 0.5172 (8) | 0.0973 (6) | 0.081 (5) | |
O15 | 0.4404 (5) | 0.6522 (8) | 0.0951 (5) | 0.085 (5) | |
O16 | 0.4804 (4) | 0.5653 (7) | 0.1720 (4) | 0.045 (3) | |
O17 | −0.0441 (4) | 0.3410 (6) | 0.0940 (4) | 0.043 (3) | |
O18 | −0.0116 (4) | 0.4752 (6) | 0.1035 (4) | 0.036 (3) | |
O19 | 0.0074 (3) | 0.3918 (6) | 0.0233 (3) | 0.034 (2) | |
O20 | −0.0793 (3) | 0.4383 (6) | 0.0218 (4) | 0.035 (3) | |
N1 | 0.3101 (4) | 0.6465 (7) | 0.0433 (4) | 0.026 (2) | |
N2 | 0.2996 (5) | 0.7336 (5) | 0.1448 (5) | 0.0292 (19) | |
N3 | 0.2904 (5) | 0.6446 (8) | 0.2461 (4) | 0.033 (2) | |
N4 | 0.0867 (4) | 0.3526 (7) | 0.1596 (4) | 0.027 (2) | |
N5 | 0.1002 (4) | 0.2645 (7) | 0.0590 (4) | 0.023 (2) | |
N6 | 0.1118 (4) | 0.3524 (7) | −0.0421 (4) | 0.026 (2) | |
N7 | 0.50000 | 0.2636 (9) | 0.25000 | 0.025 (3) | |
N8 | 0.4883 (4) | 0.3527 (7) | 0.3517 (4) | 0.025 (2) | |
C1 | 0.3186 (5) | 0.5980 (9) | −0.0050 (5) | 0.032 (4) | |
C2 | 0.3302 (5) | 0.6293 (9) | −0.0584 (5) | 0.032 (4) | |
C3 | 0.3375 (6) | 0.7111 (10) | −0.0635 (6) | 0.040 (4) | |
C4 | 0.3317 (6) | 0.7632 (9) | −0.0146 (6) | 0.033 (3) | |
C5 | 0.3173 (5) | 0.7264 (9) | 0.0384 (5) | 0.027 (3) | |
C6 | 0.3087 (5) | 0.7767 (8) | 0.0939 (5) | 0.026 (3) | |
C7 | 0.3099 (5) | 0.8620 (9) | 0.0928 (6) | 0.031 (4) | |
C8 | 0.3005 (7) | 0.9038 (7) | 0.1461 (6) | 0.034 (3) | |
C9 | 0.2912 (6) | 0.8619 (9) | 0.1969 (6) | 0.037 (4) | |
C10 | 0.2904 (5) | 0.7757 (9) | 0.1953 (5) | 0.028 (3) | |
C11 | 0.2838 (5) | 0.7267 (9) | 0.2503 (5) | 0.026 (3) | |
C12 | 0.2705 (5) | 0.7600 (9) | 0.3029 (5) | 0.030 (3) | |
C13 | 0.2632 (6) | 0.7119 (10) | 0.3538 (6) | 0.034 (4) | |
C14 | 0.2710 (6) | 0.6279 (9) | 0.3477 (5) | 0.037 (4) | |
C15 | 0.2837 (5) | 0.5989 (9) | 0.2937 (5) | 0.031 (4) | |
C16 | 0.1166 (5) | 0.4016 (9) | −0.0889 (4) | 0.032 (4) | |
C17 | 0.1273 (5) | 0.3707 (9) | −0.1456 (5) | 0.029 (3) | |
C18 | 0.1320 (5) | 0.2886 (9) | −0.1522 (5) | 0.031 (4) | |
C19 | 0.1270 (6) | 0.2348 (9) | −0.1020 (5) | 0.035 (4) | |
C20 | 0.1163 (5) | 0.2725 (8) | −0.0471 (5) | 0.025 (3) | |
C21 | 0.1087 (5) | 0.2215 (8) | 0.0074 (5) | 0.023 (3) | |
C22 | 0.1090 (5) | 0.1389 (9) | 0.0050 (5) | 0.029 (3) | |
C23 | 0.0998 (5) | 0.0969 (10) | 0.0579 (5) | 0.031 (4) | |
C24 | 0.0900 (6) | 0.1373 (9) | 0.1100 (5) | 0.030 (4) | |
C25 | 0.0909 (5) | 0.2230 (8) | 0.1091 (5) | 0.025 (3) | |
C26 | 0.0835 (5) | 0.2717 (8) | 0.1648 (5) | 0.021 (3) | |
C27 | 0.0731 (6) | 0.2342 (9) | 0.2189 (5) | 0.033 (4) | |
C28 | 0.0666 (6) | 0.2840 (9) | 0.2689 (5) | 0.032 (4) | |
C29 | 0.0697 (5) | 0.3687 (9) | 0.2634 (5) | 0.028 (3) | |
C30 | 0.0810 (5) | 0.3989 (8) | 0.2073 (4) | 0.025 (3) | |
C31 | 0.4813 (5) | 0.3994 (8) | 0.3996 (5) | 0.029 (3) | |
C32 | 0.4721 (5) | 0.3689 (9) | 0.4554 (5) | 0.031 (4) | |
C33 | 0.4697 (6) | 0.2843 (9) | 0.4623 (5) | 0.032 (4) | |
C34 | 0.4757 (5) | 0.2349 (9) | 0.4110 (5) | 0.028 (3) | |
C35 | 0.4848 (5) | 0.2696 (8) | 0.3568 (5) | 0.026 (3) | |
C36 | 0.4922 (5) | 0.2216 (8) | 0.3015 (5) | 0.027 (3) | |
C37 | 0.4911 (5) | 0.1354 (9) | 0.3029 (6) | 0.033 (4) | |
C38 | 0.50000 | 0.0928 (13) | 0.25000 | 0.033 (5) | |
H1 | 0.31640 | 0.54020 | −0.00090 | 0.0380* | |
H2 | 0.33320 | 0.59420 | −0.09230 | 0.0380* | |
H3 | 0.34660 | 0.73300 | −0.10060 | 0.0480* | |
H4 | 0.33730 | 0.82050 | −0.01700 | 0.0400* | |
H7 | 0.31680 | 0.89090 | 0.05720 | 0.0370* | |
H8 | 0.30060 | 0.96200 | 0.14670 | 0.0410* | |
H9 | 0.28530 | 0.89040 | 0.23310 | 0.0440* | |
H12 | 0.26600 | 0.81760 | 0.30510 | 0.0360* | |
H13 | 0.25360 | 0.73500 | 0.39030 | 0.0420* | |
H14 | 0.26750 | 0.59160 | 0.38080 | 0.0440* | |
H15 | 0.28800 | 0.54140 | 0.29000 | 0.0370* | |
H16 | 0.11270 | 0.45900 | −0.08410 | 0.0380* | |
H17 | 0.13120 | 0.40670 | −0.17870 | 0.0350* | |
H18 | 0.13860 | 0.26670 | −0.19050 | 0.0370* | |
H19 | 0.13060 | 0.17720 | −0.10530 | 0.0430* | |
H22 | 0.11510 | 0.11060 | −0.03110 | 0.0340* | |
H23 | 0.10040 | 0.03870 | 0.05790 | 0.0370* | |
H24 | 0.08290 | 0.10820 | 0.14540 | 0.0360* | |
H27 | 0.07050 | 0.17630 | 0.22150 | 0.0400* | |
H28 | 0.06000 | 0.26020 | 0.30660 | 0.0390* | |
H29 | 0.06440 | 0.40430 | 0.29620 | 0.0340* | |
H30 | 0.08480 | 0.45640 | 0.20330 | 0.0300* | |
H31 | 0.48290 | 0.45710 | 0.39490 | 0.0350* | |
H32 | 0.46750 | 0.40450 | 0.48840 | 0.0370* | |
H33 | 0.46410 | 0.26060 | 0.50040 | 0.0380* | |
H34 | 0.47330 | 0.17700 | 0.41420 | 0.0330* | |
H37 | 0.48450 | 0.10690 | 0.33880 | 0.0390* | |
H38 | 0.50000 | 0.03460 | 0.25000 | 0.0400* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.0347 (2) | 0.0180 (2) | 0.0335 (2) | 0.0002 (3) | 0.0177 (2) | −0.0009 (2) |
Pb2 | 0.0282 (2) | 0.0172 (3) | 0.0177 (2) | 0.0010 (2) | 0.0092 (2) | −0.0001 (2) |
Pb3 | 0.0382 (4) | 0.0152 (4) | 0.0297 (3) | 0.0000 | 0.0172 (3) | 0.0000 |
Cl1 | 0.0349 (17) | 0.029 (2) | 0.0261 (12) | 0.0061 (17) | 0.0039 (12) | 0.0002 (12) |
Cl2 | 0.0287 (16) | 0.036 (2) | 0.0258 (12) | −0.0015 (18) | 0.0060 (11) | −0.0054 (14) |
Cl3 | 0.0326 (17) | 0.035 (2) | 0.0239 (12) | −0.0066 (18) | 0.0092 (11) | −0.0030 (14) |
Cl4 | 0.0277 (15) | 0.025 (2) | 0.0250 (12) | −0.0010 (17) | 0.0060 (11) | 0.0018 (13) |
Cl5 | 0.0324 (16) | 0.0214 (19) | 0.0200 (11) | 0.0065 (16) | 0.0072 (10) | −0.0021 (12) |
O1 | 0.036 (4) | 0.071 (8) | 0.048 (4) | 0.019 (4) | 0.005 (3) | −0.026 (4) |
O2 | 0.055 (7) | 0.060 (6) | 0.065 (6) | 0.016 (5) | −0.008 (5) | −0.042 (5) |
O3 | 0.039 (5) | 0.040 (7) | 0.041 (5) | 0.012 (5) | −0.003 (4) | −0.003 (4) |
O4 | 0.083 (9) | 0.082 (8) | 0.081 (7) | −0.005 (7) | 0.004 (6) | 0.054 (6) |
O5 | 0.025 (3) | 0.044 (6) | 0.061 (5) | 0.000 (3) | 0.003 (3) | 0.022 (4) |
O6 | 0.033 (4) | 0.036 (7) | 0.058 (5) | −0.006 (4) | −0.007 (4) | −0.009 (5) |
O7 | 0.044 (6) | 0.066 (6) | 0.102 (8) | 0.016 (5) | 0.028 (6) | 0.059 (5) |
O8 | 0.063 (8) | 0.187 (13) | 0.069 (6) | −0.020 (8) | 0.026 (5) | −0.082 (7) |
O9 | 0.032 (3) | 0.056 (6) | 0.054 (4) | −0.007 (3) | 0.013 (3) | 0.020 (4) |
O10 | 0.064 (8) | 0.220 (14) | 0.046 (5) | −0.022 (8) | 0.022 (4) | −0.071 (7) |
O11 | 0.036 (6) | 0.056 (5) | 0.139 (10) | 0.001 (5) | 0.014 (6) | 0.050 (6) |
O12 | 0.027 (4) | 0.043 (7) | 0.049 (4) | −0.002 (4) | 0.006 (3) | −0.013 (4) |
O13 | 0.031 (3) | 0.086 (8) | 0.036 (4) | 0.015 (4) | 0.005 (3) | −0.018 (4) |
O14 | 0.055 (8) | 0.063 (7) | 0.119 (9) | 0.007 (6) | −0.008 (6) | −0.062 (6) |
O15 | 0.086 (9) | 0.094 (8) | 0.074 (7) | −0.016 (7) | 0.008 (6) | 0.059 (6) |
O16 | 0.032 (4) | 0.057 (8) | 0.044 (5) | 0.011 (5) | −0.001 (4) | 0.003 (4) |
O17 | 0.062 (6) | 0.035 (5) | 0.034 (4) | −0.004 (4) | 0.019 (4) | 0.009 (3) |
O18 | 0.039 (6) | 0.031 (5) | 0.037 (4) | 0.002 (4) | −0.001 (4) | −0.007 (3) |
O19 | 0.026 (3) | 0.048 (6) | 0.029 (3) | 0.004 (3) | 0.010 (2) | 0.001 (3) |
O20 | 0.028 (4) | 0.039 (6) | 0.036 (4) | 0.004 (4) | −0.001 (3) | −0.001 (3) |
N1 | 0.023 (5) | 0.022 (4) | 0.034 (3) | −0.005 (5) | 0.005 (3) | 0.000 (3) |
N2 | 0.029 (4) | 0.021 (3) | 0.038 (3) | −0.002 (4) | 0.006 (4) | 0.000 (3) |
N3 | 0.036 (5) | 0.028 (4) | 0.037 (3) | −0.002 (6) | 0.012 (3) | −0.003 (3) |
N4 | 0.038 (5) | 0.020 (4) | 0.023 (3) | −0.004 (5) | 0.006 (3) | 0.003 (3) |
N5 | 0.023 (5) | 0.022 (3) | 0.025 (3) | −0.002 (3) | 0.004 (4) | −0.002 (3) |
N6 | 0.033 (5) | 0.023 (4) | 0.023 (3) | −0.001 (5) | 0.008 (3) | −0.005 (3) |
N7 | 0.020 (7) | 0.019 (4) | 0.040 (5) | 0.0000 | 0.019 (6) | 0.0000 |
N8 | 0.022 (5) | 0.022 (4) | 0.035 (3) | −0.005 (5) | 0.014 (3) | 0.003 (3) |
C1 | 0.037 (8) | 0.028 (6) | 0.031 (4) | 0.005 (6) | 0.007 (5) | 0.000 (4) |
C2 | 0.030 (8) | 0.034 (6) | 0.031 (4) | 0.003 (6) | 0.004 (5) | 0.000 (4) |
C3 | 0.041 (9) | 0.037 (7) | 0.046 (6) | −0.001 (7) | 0.018 (6) | 0.005 (5) |
C4 | 0.029 (7) | 0.025 (6) | 0.047 (5) | −0.008 (6) | 0.013 (5) | 0.005 (4) |
C5 | 0.020 (7) | 0.022 (4) | 0.038 (4) | −0.001 (6) | 0.004 (5) | 0.003 (3) |
C6 | 0.022 (8) | 0.018 (3) | 0.037 (4) | −0.004 (6) | 0.000 (4) | 0.001 (3) |
C7 | 0.022 (8) | 0.019 (4) | 0.053 (6) | −0.002 (6) | 0.007 (5) | 0.003 (4) |
C8 | 0.033 (6) | 0.012 (4) | 0.057 (6) | 0.014 (8) | 0.004 (5) | 0.001 (4) |
C9 | 0.033 (9) | 0.022 (4) | 0.055 (6) | 0.008 (7) | 0.007 (6) | −0.003 (4) |
C10 | 0.020 (7) | 0.022 (4) | 0.043 (4) | −0.010 (6) | 0.009 (5) | −0.006 (3) |
C11 | 0.016 (7) | 0.027 (4) | 0.036 (4) | 0.000 (6) | 0.003 (4) | −0.004 (3) |
C12 | 0.024 (7) | 0.028 (6) | 0.038 (5) | −0.004 (6) | 0.005 (5) | −0.008 (4) |
C13 | 0.030 (8) | 0.038 (7) | 0.036 (5) | 0.005 (7) | 0.008 (5) | −0.004 (5) |
C14 | 0.044 (9) | 0.037 (6) | 0.028 (4) | −0.004 (7) | 0.000 (5) | −0.003 (5) |
C15 | 0.032 (8) | 0.027 (6) | 0.033 (4) | −0.006 (6) | 0.003 (5) | −0.004 (4) |
C16 | 0.044 (8) | 0.032 (6) | 0.022 (4) | 0.004 (7) | 0.014 (5) | −0.002 (3) |
C17 | 0.023 (7) | 0.038 (6) | 0.028 (4) | 0.011 (6) | 0.012 (5) | −0.003 (4) |
C18 | 0.028 (8) | 0.039 (7) | 0.026 (4) | 0.011 (6) | 0.009 (5) | −0.005 (4) |
C19 | 0.052 (10) | 0.032 (6) | 0.022 (4) | 0.002 (7) | 0.005 (5) | −0.009 (4) |
C20 | 0.027 (8) | 0.024 (4) | 0.025 (4) | −0.001 (6) | 0.006 (4) | −0.009 (3) |
C21 | 0.017 (7) | 0.022 (3) | 0.030 (4) | 0.005 (5) | 0.006 (4) | −0.005 (3) |
C22 | 0.024 (8) | 0.023 (4) | 0.039 (5) | 0.000 (6) | 0.004 (5) | −0.002 (4) |
C23 | 0.033 (9) | 0.021 (6) | 0.039 (5) | −0.007 (6) | 0.010 (5) | −0.006 (4) |
C24 | 0.032 (9) | 0.023 (4) | 0.035 (5) | 0.005 (6) | 0.006 (5) | 0.001 (4) |
C25 | 0.022 (7) | 0.020 (3) | 0.033 (4) | 0.008 (6) | 0.007 (4) | 0.005 (3) |
C26 | 0.015 (7) | 0.019 (4) | 0.029 (4) | 0.005 (5) | 0.005 (4) | 0.006 (3) |
C27 | 0.044 (9) | 0.027 (6) | 0.030 (4) | 0.011 (6) | 0.008 (5) | 0.013 (4) |
C28 | 0.037 (9) | 0.034 (6) | 0.026 (4) | −0.005 (7) | 0.009 (5) | 0.011 (4) |
C29 | 0.025 (7) | 0.033 (6) | 0.028 (4) | −0.003 (6) | 0.012 (4) | −0.002 (4) |
C30 | 0.028 (7) | 0.023 (5) | 0.024 (4) | 0.000 (6) | 0.006 (4) | 0.004 (3) |
C31 | 0.030 (7) | 0.023 (5) | 0.035 (4) | −0.002 (6) | 0.010 (5) | 0.003 (4) |
C32 | 0.034 (8) | 0.032 (6) | 0.023 (4) | 0.004 (6) | −0.006 (5) | 0.000 (4) |
C33 | 0.034 (8) | 0.035 (6) | 0.027 (4) | −0.002 (6) | 0.005 (5) | 0.013 (4) |
C34 | 0.018 (6) | 0.025 (6) | 0.043 (5) | −0.002 (5) | 0.011 (5) | 0.006 (4) |
C35 | 0.022 (7) | 0.022 (4) | 0.036 (4) | −0.002 (6) | 0.009 (5) | 0.003 (3) |
C36 | 0.024 (7) | 0.018 (4) | 0.041 (5) | 0.000 (6) | 0.011 (5) | 0.004 (3) |
C37 | 0.022 (8) | 0.018 (4) | 0.061 (7) | 0.000 (6) | 0.017 (6) | 0.002 (4) |
C38 | 0.024 (10) | 0.011 (7) | 0.069 (9) | 0.0000 | 0.022 (8) | 0.0000 |
Pb1—O3 | 2.980 (11) | C6—C7 | 1.39 (2) |
Pb1—O6 | 2.987 (11) | C7—C8 | 1.404 (19) |
Pb1—O9 | 2.598 (10) | C8—C9 | 1.358 (19) |
Pb1—O13 | 2.532 (10) | C9—C10 | 1.41 (2) |
Pb1—N1 | 2.511 (9) | C10—C11 | 1.477 (17) |
Pb1—N2 | 2.494 (8) | C11—C12 | 1.363 (17) |
Pb1—N3 | 2.506 (10) | C12—C13 | 1.400 (19) |
Pb2—O5 | 2.626 (10) | C13—C14 | 1.40 (2) |
Pb2—O12 | 3.024 (11) | C14—C15 | 1.358 (17) |
Pb2—O19 | 2.547 (8) | C16—C17 | 1.405 (15) |
Pb2—O20i | 2.975 (9) | C17—C18 | 1.36 (2) |
Pb2—N4 | 2.540 (9) | C18—C19 | 1.429 (18) |
Pb2—N5 | 2.502 (11) | C19—C20 | 1.414 (17) |
Pb2—N6 | 2.501 (9) | C20—C21 | 1.493 (17) |
Pb3—O1 | 2.548 (10) | C21—C22 | 1.35 (2) |
Pb3—O16 | 2.969 (11) | C22—C23 | 1.397 (17) |
Pb3—N7 | 2.499 (15) | C23—C24 | 1.374 (18) |
Pb3—N8 | 2.519 (9) | C24—C25 | 1.40 (2) |
Cl1—O1 | 1.448 (10) | C25—C26 | 1.493 (16) |
Cl1—O2 | 1.395 (12) | C26—C27 | 1.395 (17) |
Cl1—O3 | 1.446 (10) | C27—C28 | 1.394 (18) |
Cl1—O4 | 1.428 (13) | C28—C29 | 1.39 (2) |
Cl2—O5 | 1.431 (10) | C29—C30 | 1.394 (15) |
Cl2—O6 | 1.425 (10) | C31—C32 | 1.373 (16) |
Cl2—O7 | 1.432 (13) | C32—C33 | 1.39 (2) |
Cl2—O8 | 1.388 (13) | C33—C34 | 1.411 (18) |
Cl3—O9 | 1.417 (11) | C34—C35 | 1.367 (16) |
Cl3—O10 | 1.371 (13) | C35—C36 | 1.479 (16) |
Cl3—O11 | 1.398 (14) | C36—C37 | 1.41 (2) |
Cl3—O12 | 1.428 (10) | C37—C38 | 1.400 (17) |
Cl4—O13 | 1.444 (10) | C1—H1 | 0.9500 |
Cl4—O14 | 1.410 (13) | C2—H2 | 0.9500 |
Cl4—O15 | 1.414 (13) | C3—H3 | 0.9500 |
Cl4—O16 | 1.417 (10) | C4—H4 | 0.9500 |
Cl5—O17 | 1.400 (10) | C7—H7 | 0.9500 |
Cl5—O18 | 1.440 (10) | C8—H8 | 0.9500 |
Cl5—O19 | 1.442 (8) | C9—H9 | 0.9500 |
Cl5—O20 | 1.443 (9) | C12—H12 | 0.9500 |
N1—C1 | 1.365 (16) | C13—H13 | 0.9500 |
N1—C5 | 1.324 (19) | C14—H14 | 0.9500 |
N2—C6 | 1.368 (16) | C15—H15 | 0.9500 |
N2—C10 | 1.353 (16) | C16—H16 | 0.9500 |
N3—C11 | 1.36 (2) | C17—H17 | 0.9500 |
N3—C15 | 1.315 (16) | C18—H18 | 0.9500 |
N4—C26 | 1.330 (17) | C19—H19 | 0.9500 |
N4—C30 | 1.316 (14) | C22—H22 | 0.9500 |
N5—C21 | 1.376 (15) | C23—H23 | 0.9500 |
N5—C25 | 1.341 (15) | C24—H24 | 0.9500 |
N6—C16 | 1.323 (15) | C27—H27 | 0.9500 |
N6—C20 | 1.316 (17) | C28—H28 | 0.9500 |
N7—C36 | 1.361 (14) | C29—H29 | 0.9500 |
N7—C36ii | 1.361 (14) | C30—H30 | 0.9500 |
N8—C31 | 1.331 (15) | C31—H31 | 0.9500 |
N8—C35 | 1.366 (17) | C32—H32 | 0.9500 |
C1—C2 | 1.350 (17) | C33—H33 | 0.9500 |
C2—C3 | 1.36 (2) | C34—H34 | 0.9500 |
C3—C4 | 1.39 (2) | C37—H37 | 0.9500 |
C4—C5 | 1.405 (18) | C38—H38 | 0.9500 |
C5—C6 | 1.511 (17) | ||
O3—Pb1—O6 | 66.9 (3) | Pb3—N8—C35 | 120.1 (7) |
O3—Pb1—O9 | 111.6 (3) | C31—N8—C35 | 119.1 (10) |
O3—Pb1—O13 | 86.8 (3) | N1—C1—C2 | 122.2 (13) |
O3—Pb1—N1 | 145.1 (3) | C1—C2—C3 | 119.7 (12) |
O3—Pb1—N2 | 143.1 (3) | C2—C3—C4 | 120.4 (13) |
O3—Pb1—N3 | 80.7 (3) | C3—C4—C5 | 116.5 (13) |
O6—Pb1—O9 | 104.2 (3) | N1—C5—C4 | 123.0 (12) |
O6—Pb1—O13 | 106.2 (3) | N1—C5—C6 | 115.6 (10) |
O6—Pb1—N1 | 84.9 (3) | C4—C5—C6 | 121.4 (13) |
O6—Pb1—N2 | 149.3 (3) | N2—C6—C5 | 116.1 (11) |
O6—Pb1—N3 | 145.1 (3) | N2—C6—C7 | 122.4 (11) |
O9—Pb1—O13 | 148.8 (4) | C5—C6—C7 | 121.6 (11) |
O9—Pb1—N1 | 94.5 (3) | C6—C7—C8 | 117.7 (12) |
O9—Pb1—N2 | 74.1 (4) | C7—C8—C9 | 120.6 (12) |
O9—Pb1—N3 | 75.2 (3) | C8—C9—C10 | 119.2 (12) |
O13—Pb1—N1 | 81.7 (3) | N2—C10—C9 | 121.7 (11) |
O13—Pb1—N2 | 76.3 (4) | N2—C10—C11 | 116.6 (12) |
O13—Pb1—N3 | 83.7 (4) | C9—C10—C11 | 121.6 (11) |
N1—Pb1—N2 | 65.0 (4) | N3—C11—C10 | 116.7 (10) |
N1—Pb1—N3 | 130.0 (4) | N3—C11—C12 | 120.1 (12) |
N2—Pb1—N3 | 65.2 (4) | C10—C11—C12 | 123.2 (13) |
O5—Pb2—O12 | 105.5 (3) | C11—C12—C13 | 122.0 (14) |
O5—Pb2—O19 | 148.1 (3) | C12—C13—C14 | 116.0 (12) |
O5—Pb2—O20i | 115.6 (3) | C13—C14—C15 | 118.8 (12) |
O5—Pb2—N4 | 96.0 (3) | N3—C15—C14 | 124.7 (14) |
O5—Pb2—N5 | 74.0 (3) | N6—C16—C17 | 121.3 (13) |
O5—Pb2—N6 | 74.8 (3) | C16—C17—C18 | 118.8 (12) |
O12—Pb2—O19 | 106.3 (3) | C17—C18—C19 | 120.4 (11) |
O12—Pb2—O20i | 68.4 (3) | C18—C19—C20 | 116.0 (13) |
O12—Pb2—N4 | 84.5 (3) | N6—C20—C19 | 122.2 (11) |
O12—Pb2—N5 | 148.7 (3) | N6—C20—C21 | 117.6 (10) |
O12—Pb2—N6 | 145.9 (3) | C19—C20—C21 | 120.2 (12) |
O19—Pb2—O20i | 79.5 (3) | N5—C21—C20 | 115.4 (11) |
O19—Pb2—N4 | 84.0 (3) | N5—C21—C22 | 123.0 (11) |
O19—Pb2—N5 | 77.3 (3) | C20—C21—C22 | 121.6 (10) |
O19—Pb2—N6 | 80.7 (3) | C21—C22—C23 | 117.1 (12) |
O20i—Pb2—N4 | 142.4 (3) | C22—C23—C24 | 121.9 (14) |
O20i—Pb2—N5 | 141.1 (3) | C23—C24—C25 | 117.6 (12) |
O20i—Pb2—N6 | 80.6 (3) | N5—C25—C24 | 121.5 (11) |
N4—Pb2—N5 | 64.7 (3) | N5—C25—C26 | 117.4 (11) |
N4—Pb2—N6 | 129.6 (4) | C24—C25—C26 | 121.1 (10) |
N5—Pb2—N6 | 65.2 (3) | N4—C26—C25 | 116.3 (10) |
O1—Pb3—O16 | 88.6 (3) | N4—C26—C27 | 122.1 (11) |
O1—Pb3—N7 | 76.4 (3) | C25—C26—C27 | 121.7 (12) |
O1—Pb3—N8 | 83.3 (3) | C26—C27—C28 | 118.2 (13) |
O1—Pb3—O1ii | 152.7 (4) | C27—C28—C29 | 119.8 (11) |
O1—Pb3—O16ii | 114.2 (3) | C28—C29—C30 | 116.7 (11) |
O1—Pb3—N8ii | 85.5 (3) | N4—C30—C29 | 124.0 (12) |
O16—Pb3—N7 | 144.9 (2) | N8—C31—C32 | 123.8 (12) |
O16—Pb3—N8 | 144.7 (3) | C31—C32—C33 | 118.2 (11) |
O16—Pb3—O16ii | 70.2 (3) | C32—C33—C34 | 118.0 (11) |
O16—Pb3—N8ii | 82.0 (3) | C33—C34—C35 | 120.6 (13) |
N7—Pb3—N8 | 65.5 (3) | N8—C35—C34 | 120.3 (11) |
N8—Pb3—N8ii | 131.1 (4) | N8—C35—C36 | 116.2 (10) |
O1—Cl1—O2 | 109.3 (6) | C34—C35—C36 | 123.5 (12) |
O1—Cl1—O3 | 109.1 (5) | N7—C36—C35 | 117.7 (12) |
O1—Cl1—O4 | 107.1 (7) | N7—C36—C37 | 121.9 (11) |
O2—Cl1—O3 | 111.3 (7) | C35—C36—C37 | 120.4 (11) |
O2—Cl1—O4 | 111.3 (7) | C36—C37—C38 | 118.2 (13) |
O3—Cl1—O4 | 108.6 (7) | C37—C38—C37ii | 120.4 (17) |
O5—Cl2—O6 | 110.6 (6) | N1—C1—H1 | 119.00 |
O5—Cl2—O7 | 106.5 (6) | C2—C1—H1 | 119.00 |
O5—Cl2—O8 | 109.1 (8) | C1—C2—H2 | 120.00 |
O6—Cl2—O7 | 109.4 (7) | C3—C2—H2 | 120.00 |
O6—Cl2—O8 | 110.2 (7) | C2—C3—H3 | 120.00 |
O7—Cl2—O8 | 111.0 (8) | C4—C3—H3 | 120.00 |
O9—Cl3—O10 | 109.9 (8) | C3—C4—H4 | 122.00 |
O9—Cl3—O11 | 107.1 (7) | C5—C4—H4 | 122.00 |
O9—Cl3—O12 | 111.1 (6) | C6—C7—H7 | 121.00 |
O10—Cl3—O11 | 111.1 (8) | C8—C7—H7 | 121.00 |
O10—Cl3—O12 | 109.4 (7) | C7—C8—H8 | 120.00 |
O11—Cl3—O12 | 108.4 (7) | C9—C8—H8 | 120.00 |
O13—Cl4—O14 | 108.3 (7) | C8—C9—H9 | 120.00 |
O13—Cl4—O15 | 105.1 (7) | C10—C9—H9 | 120.00 |
O13—Cl4—O16 | 108.4 (5) | C11—C12—H12 | 119.00 |
O14—Cl4—O15 | 111.5 (7) | C13—C12—H12 | 119.00 |
O14—Cl4—O16 | 113.3 (7) | C12—C13—H13 | 122.00 |
O15—Cl4—O16 | 109.9 (7) | C14—C13—H13 | 122.00 |
O17—Cl5—O18 | 111.1 (5) | C13—C14—H14 | 121.00 |
O17—Cl5—O19 | 110.0 (6) | C15—C14—H14 | 121.00 |
O17—Cl5—O20 | 109.7 (6) | N3—C15—H15 | 118.00 |
O18—Cl5—O19 | 108.0 (6) | C14—C15—H15 | 118.00 |
O18—Cl5—O20 | 110.4 (6) | N6—C16—H16 | 119.00 |
O19—Cl5—O20 | 107.6 (5) | C17—C16—H16 | 119.00 |
Pb3—O1—Cl1 | 118.8 (5) | C16—C17—H17 | 121.00 |
Pb1—O3—Cl1 | 129.4 (6) | C18—C17—H17 | 121.00 |
Pb2—O5—Cl2 | 114.7 (5) | C17—C18—H18 | 120.00 |
Pb1—O6—Cl2 | 114.0 (6) | C19—C18—H18 | 120.00 |
Pb1—O9—Cl3 | 116.9 (6) | C18—C19—H19 | 122.00 |
Pb2—O12—Cl3 | 110.1 (6) | C20—C19—H19 | 122.00 |
Pb1—O13—Cl4 | 122.0 (5) | C21—C22—H22 | 121.00 |
Pb3—O16—Cl4 | 125.7 (6) | C23—C22—H22 | 121.00 |
Pb2—O19—Cl5 | 121.4 (4) | C22—C23—H23 | 119.00 |
Pb2—O20i—Cl5i | 134.7 (5) | C24—C23—H23 | 119.00 |
Pb1—N1—C1 | 119.3 (9) | C23—C24—H24 | 121.00 |
Pb1—N1—C5 | 122.0 (7) | C25—C24—H24 | 121.00 |
C1—N1—C5 | 118.0 (10) | C26—C27—H27 | 121.00 |
Pb1—N2—C6 | 120.9 (8) | C28—C27—H27 | 121.00 |
Pb1—N2—C10 | 120.6 (8) | C27—C28—H28 | 120.00 |
C6—N2—C10 | 118.5 (10) | C29—C28—H28 | 120.00 |
Pb1—N3—C11 | 119.7 (7) | C28—C29—H29 | 122.00 |
Pb1—N3—C15 | 120.7 (10) | C30—C29—H29 | 121.00 |
C11—N3—C15 | 118.4 (11) | N4—C30—H30 | 118.00 |
Pb2—N4—C26 | 120.7 (7) | C29—C30—H30 | 118.00 |
Pb2—N4—C30 | 120.1 (8) | N8—C31—H31 | 118.00 |
C26—N4—C30 | 119.2 (10) | C32—C31—H31 | 118.00 |
Pb2—N5—C21 | 120.0 (8) | C31—C32—H32 | 121.00 |
Pb2—N5—C25 | 121.0 (8) | C33—C32—H32 | 121.00 |
C21—N5—C25 | 118.9 (11) | C32—C33—H33 | 121.00 |
Pb2—N6—C16 | 117.4 (9) | C34—C33—H33 | 121.00 |
Pb2—N6—C20 | 120.9 (7) | C33—C34—H34 | 120.00 |
C16—N6—C20 | 121.2 (10) | C35—C34—H34 | 120.00 |
Pb3—N7—C36 | 120.3 (8) | C36—C37—H37 | 121.00 |
Pb3—N7—C36ii | 120.3 (8) | C38—C37—H37 | 121.00 |
C36—N7—C36ii | 119.5 (13) | C37—C38—H38 | 120.00 |
Pb3—N8—C31 | 120.5 (8) | C37ii—C38—H38 | 120.00 |
C5—N1—C1—C2 | −4.8 (18) | C9—C10—C11—C12 | 10 (2) |
C1—N1—C5—C4 | 1.9 (19) | N3—C11—C12—C13 | 0 (2) |
C1—N1—C5—C6 | −178.5 (11) | C10—C11—C12—C13 | 178.4 (13) |
C10—N2—C6—C5 | −178.5 (11) | C11—C12—C13—C14 | 1 (2) |
C10—N2—C6—C7 | 1.4 (19) | C12—C13—C14—C15 | −1 (2) |
C6—N2—C10—C9 | −1 (2) | C13—C14—C15—N3 | 1 (2) |
C6—N2—C10—C11 | −176.7 (12) | N6—C16—C17—C18 | 0.9 (19) |
C15—N3—C11—C10 | −178.6 (12) | C16—C17—C18—C19 | −1.0 (19) |
C15—N3—C11—C12 | −0.1 (19) | C17—C18—C19—C20 | 1 (2) |
C11—N3—C15—C14 | −1 (2) | C18—C19—C20—N6 | −1 (2) |
C30—N4—C26—C25 | −179.4 (11) | C18—C19—C20—C21 | 178.1 (12) |
C30—N4—C26—C27 | 1.5 (19) | N6—C20—C21—N5 | −3.1 (17) |
C26—N4—C30—C29 | −2.5 (19) | N6—C20—C21—C22 | 175.4 (12) |
C25—N5—C21—C20 | 177.4 (11) | C19—C20—C21—N5 | 178.0 (12) |
C25—N5—C21—C22 | −1.1 (18) | C19—C20—C21—C22 | −3.5 (19) |
C21—N5—C25—C24 | 0.4 (18) | N5—C21—C22—C23 | 0.4 (19) |
C21—N5—C25—C26 | 178.2 (11) | C20—C21—C22—C23 | −178.0 (12) |
C20—N6—C16—C17 | −0.7 (19) | C21—C22—C23—C24 | 1.0 (19) |
C16—N6—C20—C19 | 0.7 (19) | C22—C23—C24—C25 | −2 (2) |
C16—N6—C20—C21 | −178.2 (11) | C23—C24—C25—N5 | 1 (2) |
C36ii—N7—C36—C35 | 179.0 (10) | C23—C24—C25—C26 | −176.8 (12) |
C36ii—N7—C36—C37 | −1.0 (15) | N5—C25—C26—N4 | 0.2 (17) |
C35—N8—C31—C32 | 1.9 (19) | N5—C25—C26—C27 | 179.3 (12) |
C31—N8—C35—C34 | −1.8 (18) | C24—C25—C26—N4 | 178.0 (12) |
C31—N8—C35—C36 | 179.1 (11) | C24—C25—C26—C27 | −3 (2) |
N1—C1—C2—C3 | 5 (2) | N4—C26—C27—C28 | −1 (2) |
C1—C2—C3—C4 | −2 (2) | C25—C26—C27—C28 | −179.9 (13) |
C2—C3—C4—C5 | −1 (2) | C26—C27—C28—C29 | 1 (2) |
C3—C4—C5—N1 | 1 (2) | C27—C28—C29—C30 | −2 (2) |
C3—C4—C5—C6 | −178.7 (12) | C28—C29—C30—N4 | 2.7 (19) |
N1—C5—C6—N2 | 6.1 (17) | N8—C31—C32—C33 | 0 (2) |
N1—C5—C6—C7 | −173.7 (12) | C31—C32—C33—C34 | −1 (2) |
C4—C5—C6—N2 | −174.2 (13) | C32—C33—C34—C35 | 2 (2) |
C4—C5—C6—C7 | 6.0 (19) | C33—C34—C35—N8 | 0.1 (19) |
N2—C6—C7—C8 | −1 (2) | C33—C34—C35—C36 | 179.1 (12) |
C5—C6—C7—C8 | 178.8 (13) | N8—C35—C36—N7 | −2.2 (16) |
C6—C7—C8—C9 | 1 (2) | N8—C35—C36—C37 | 177.8 (11) |
C7—C8—C9—C10 | −1 (2) | C34—C35—C36—N7 | 178.8 (11) |
C8—C9—C10—N2 | 1 (2) | C34—C35—C36—C37 | −1.2 (19) |
C8—C9—C10—C11 | 176.2 (14) | N7—C36—C37—C38 | 2.0 (17) |
N2—C10—C11—N3 | 3.4 (18) | C35—C36—C37—C38 | −178.0 (10) |
N2—C10—C11—C12 | −175.0 (12) | C36—C37—C38—C37ii | −1.0 (15) |
C9—C10—C11—N3 | −171.8 (13) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, y, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3···O4iii | 0.95 | 2.57 | 3.263 (17) | 130 |
C3—H3···O9iv | 0.95 | 2.57 | 3.101 (19) | 116 |
C13—H13···O5v | 0.95 | 2.48 | 3.061 (18) | 120 |
C14—H14···O8vi | 0.95 | 2.44 | 3.104 (16) | 126 |
C15—H15···O3 | 0.95 | 2.48 | 3.292 (17) | 144 |
C16—H16···O20i | 0.95 | 2.40 | 3.213 (16) | 144 |
C17—H17···O10iii | 0.95 | 2.41 | 3.107 (16) | 130 |
C22—H22···O14vii | 0.95 | 2.57 | 3.382 (19) | 144 |
C31—H31···O16ii | 0.95 | 2.56 | 3.349 (17) | 141 |
C37—H37···O18viii | 0.95 | 2.54 | 3.317 (17) | 139 |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, y, −z+1/2; (iii) x, −y+1, z−1/2; (iv) −x+1/2, −y+3/2, −z; (v) −x+1/2, y+1/2, −z+1/2; (vi) x, −y+1, z+1/2; (vii) −x+1/2, −y+1/2, −z; (viii) −x+1/2, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Pb(ClO4)2(C15H11N3)] |
Mr | 639.36 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 150 |
a, b, c (Å) | 25.440 (4), 16.333 (3), 21.916 (4) |
β (°) | 98.671 (2) |
V (Å3) | 9002 (4) |
Z | 20 |
Radiation type | Mo Kα |
µ (mm−1) | 9.72 |
Crystal size (mm) | 0.25 × 0.08 × 0.05 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.514, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 27358, 8832, 4705 |
Rint | 0.052 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.126, 1.03 |
No. of reflections | 8832 |
No. of parameters | 655 |
No. of restraints | 220 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ^2^(Fo^2^) + (0.027P)^2^ + 69.73P] where P = (Fo^2^ + 2Fc^2^)/3 | |
Δρmax, Δρmin (e Å−3) | 2.07, −2.43 |
Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), enCIFer (Allen et al., 2004), PLATON (Spek, 2003), publCIF (Westrip, 2008).
Pb1—O3 | 2.980 (11) | Pb2—O19 | 2.547 (8) |
Pb1—O6 | 2.987 (11) | Pb2—O20i | 2.975 (9) |
Pb1—O9 | 2.598 (10) | Pb2—N4 | 2.540 (9) |
Pb1—O13 | 2.532 (10) | Pb2—N5 | 2.502 (11) |
Pb1—N1 | 2.511 (9) | Pb2—N6 | 2.501 (9) |
Pb1—N2 | 2.494 (8) | Pb3—O1 | 2.548 (10) |
Pb1—N3 | 2.506 (10) | Pb3—O16 | 2.969 (11) |
Pb2—O5 | 2.626 (10) | Pb3—N7 | 2.499 (15) |
Pb2—O12 | 3.024 (11) | Pb3—N8 | 2.519 (9) |
O9—Pb1—O13 | 148.8 (4) | Pb1—O9—Cl3 | 116.9 (6) |
O5—Pb2—O19 | 148.1 (3) | Pb2—O12—Cl3 | 110.1 (6) |
O1—Pb3—O1ii | 152.7 (4) | Pb1—O13—Cl4 | 122.0 (5) |
Pb3—O1—Cl1 | 118.8 (5) | Pb3—O16—Cl4 | 125.7 (6) |
Pb1—O3—Cl1 | 129.4 (6) | Pb2—O19—Cl5 | 121.4 (4) |
Pb2—O5—Cl2 | 114.7 (5) | Pb2—O20i—Cl5i | 134.7 (5) |
Pb1—O6—Cl2 | 114.0 (6) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, y, −z+1/2. |
Polydentate analogues of the pyridine molecule have played an important role in the development of coordination chemistry and continue to be of considerable interest, in particular the metal complexes of N,N'-bidentate aromatic ligands such as 2,2'-bipyridine (bipy), 1,10-phenanthroline (phen) and the tridentate analogue 2,2':6',2''-terpyridine (terpy). This interest stems not only from the similarity of these ligands to biologically important nitrogen-containing heterocyclic ligands such as porphyrins and purines, but also from their use as building blocks in the construction of supramolecular systems, macromolecules, metallo-oligomers and polymers exhibiting a wide variety of chromophoric, electrochemical, luminescent and magnetic properties (Sauvage et al., 1994; Kaes et al., 2000; Chelucci & Thummel, 2002; Hofmeier et al., 2004; Baronoff et al., 2004; Eryazici et al., 2008; Glasson et al., 2008; Constable, 2007, 2008). In particular, 2,2':6',2''-terpyridine (terpy) is a ligand with a very extensive coordination chemistry. In principle, it can exhibit a variety of coordination modes towards metals, i.e. monodentate, bidentate, terdentate and bridging, but, in practice, it almost invariably acts as a planar tridentate ligand forming 1:1 and 1:2 (metal to ligand) five- or six-coordinate complexes with divalent transition and post-transition metal ions (Brandt et al., 1954; Cargill Thompson, 1997). Particularly interesting from a structural point of view are the 1:1 complexes in which the coordination sphere of the metal ion is completed by solvent or adventitious oxygenated ligands which can also function as bridging ligands, resulting in extended polynuclear architectures of different dimensionalities. In this paper, we report the crystal structure of a new polymorph of [Pb(terpy)(ClO4)2] obtained by reacting a 1:1 molar ratio of Pb(ClO4)2 and terpy in acetonitrile.
In the title compound (I), the molecules containing Pb1 (Fig. 1) and Pb2 occupy general positions while Pb3 lies on a crystallographic twofold axis that also passes through the middle of the central pyridyl ring (atoms N7, C38 and H38). Each metal centre is coordinated by all three N pyridyl donors from its terpy ligand [Pb—N 2.494 (8)–2.540 (9) Å; Table 1] in the equatorial plane and by two axial perchlorate O donors at distances of 2.532 (10)–2.626 (10) Å. Considering only these linkages, the anions may be regarded as unidentate with respect to any one metal centre; an alternative description as strongly asymmetrically bidentate (see below) would involve the consideration of a wide range of much longer Pb—O distances of 3.151 (12)–3.404 (14) Å. The seven coordination at each of the three metal centres in (I) is completed by two equatorial O atoms [Pb—O 2.969 (11)–3.024 (11) Å; Table 1] from two anions bridging to two different adjacent metal centres (Fig. 2). The significant deviations of these O donors in opposing directions out of the equatorial plane represent the principal distortion from pentagonal bipyramidal geometry at each metal centre.
Other notable features of the coordination geometry are the markedly nonlinear O(axial)—Pb—O(axial) angles (Table 1) which have values of around 150°, and the dihedral angles between the outer rings of the terpy ligands which adopt a narrow range of values, namely 11.8 (5), 6.9 (4) and 4.7 (4) ° for Pb1, Pb2 and Pb3, respectively.
The pairs of asymmetrically bridging perchlorate anions described above lead to an extended structure wherein the PbII centres are linked into undulating chains which run parallel to the [201] direction (Fig. 3a) and which are significantly interdigitated. The spacing of the PbII centres is irregular [Pb1···Pb2 5.5835 (10), Pb2···Pb2 6.2364 (11), Pb1···Pb3 6.0004 (10) Å] and this can be traced to variations in the Pb—O—Cl angles associated with the perchlorate bridges: for the shortest Pb1···Pb2 distance, these range between 110.1 (6) and 116.9 (6) °, averaging 114 °; for the longest Pb2···Pb2 distance, the angles are much wider [121.4 (4) and 134.7 (5), average 128 °]; while for the intermediate Pb1···Pb3 distance, the angles [118.8 (5)–129.4 (6), average 124°] are correspondingly intermediate. In the literature, the main distribution of M—O—Cl angles in perchlorate bridges covers a wide range (115–140°, with a few examples extending this range to between 105 and 150 °; Allen, 2002). We believe that this flexibility in the coordination geometry of the perchlorate anion is the prime factor that allows different polymorphs to exist. We have every reason to suspect the existence of other polymorphs based on different proportions of perchlorate geometries. Fig. 3(b) shows alternating regions of hydrophilic perchlorate and hydrophobic terpy units along the b axis.
Crystals of the previously published polymorph were prepared by a different synthetic route (cf. Experimental): hot equimolar solutions of Pb(ClO4)2.3H2O in water and terpyridine in MeOH were combined and the mixture boiled before being allowed to cool overnight (Engelhardt et al., 1996). The resulting structure is considerably simpler, with a single unique PbII centre: this lies on a crystallographic twofold axis, with pairs of symmetry-related perchlorate anions linking successive PbII centres into a one-dimensional polymeric chain. The authors characterize each perchlorate as a highly asymmetric O,O'-bidentate ligand [Pb—O 2.554 (5) and 3.258 (9) Å] to one metal centre while another O atom forms one of the links to the adjacent metal. The same paper reports closely similar chain structures for complexes with other small oxoanions (nitrate and nitrite). The structure of the current polymorph may be formally converted into that of the original one by removal of the [bis(perchlorato)(terpy)lead(II)] units centred on Pb1 and Pb2 and linking Pb3-centred units directly via pairwise perchlorate bridges. The unique repeat distance along the chain in the original polymorph is 6.0670 (6) Å, while in the current structure the Pb3···Pb3 distance is 26.280 (4) Å. Because of the irregularity of the Pb···Pb distances (see above), this considerably longer distance must be regarded as the fundamental repeat distance along the chain. Interestingly, similar undulating chains of doubly-bridged [(terpy)lead(II)] units are observed in the extended structures of {[Pb(C15H11N3)(NO3)2]}∞ (Engelhardt et al., 1996) and {[Pb(C15H11N3)(SCN)2]}∞ (Engelhardt et al., 1989), with Pb···Pb repeat distances of 6.892 (3) and 6.018 (4) Å, respectively.