metal-organic compounds
The PbII atom in the title compound, [Pb(C9H6NO)2], is N,O-chelated by two organic ligands, and two molecules are linked across a centre of inversion to form a dinuclear entity. These dinuclear entities are linked by somewhat weaker PbO bonds into a chain. There are two independent molecules in the asymmetric unit with similar geometry around the Pb atoms, which have a pseudo-pentagonal–bipyramidal coordination with one of the axial positions occupied by the Pb lone pair. Some distances involving the Pb atoms are significantly different between the two molecules.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805011852/dn6216sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805011852/dn6216Isup2.hkl |
CCDC reference: 274388
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.009 Å
- R factor = 0.030
- wR factor = 0.075
- Data-to-parameter ratio = 16.8
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT061_ALERT_3_A Tmax/Tmin Range Test RR' too Large ............. 0.48
Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.116 0.290 Tmin' and Tmax expected: 0.123 0.193 RR' = 0.627 Please check that your absorption correction is appropriate.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.67 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C36 H24 N4 O4 Pb2 Atom count from _chemical_formula_moiety:C9 H6 N1 O1 Pb24 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 0.665 Tmax scaled 0.193 Tmin scaled 0.077
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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
Computing details top
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEPIII for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
Crystal data top
[Pb(C9H6NO)2] | F(000) = 3712 |
Mr = 495.59 | Dx = 2.138 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 4994 reflections |
a = 35.937 (2) Å | θ = 2.5–27.4° |
b = 8.3365 (4) Å | µ = 10.97 mm−1 |
c = 25.432 (1) Å | T = 295 K |
β = 126.076 (1)° | Column, yellow |
V = 6158.1 (5) Å3 | 0.18 × 0.17 × 0.15 mm |
Z = 16 |
Data collection top
Bruker APEX CCD area-detector diffractometer | 6956 independent reflections |
Radiation source: fine-focus sealed tube | 4910 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
φ and ω scans | θmax = 27.5°, θmin = 1.4° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −41→46 |
Tmin = 0.077, Tmax = 0.193 | k = −10→10 |
20725 measured reflections | l = −32→31 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.075 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0333P)2] where P = (Fo2 + 2Fc2)/3 |
6956 reflections | (Δ/σ)max = 0.001 |
415 parameters | Δρmax = 1.07 e Å−3 |
0 restraints | Δρmin = −1.12 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Pb1 | 0.231838 (7) | 0.50370 (2) | 0.489411 (8) | 0.03595 (7) | |
Pb2 | 0.002870 (5) | 0.25041 (2) | 0.502647 (7) | 0.03364 (7) | |
O1 | 0.2049 (1) | 0.7784 (3) | 0.4769 (2) | 0.045 (1) | |
O2 | 0.2101 (1) | 0.2648 (3) | 0.4259 (2) | 0.046 (1) | |
O3 | 0.0093 (1) | 0.0165 (3) | 0.5623 (2) | 0.041 (1) | |
O4 | 0.0440 (1) | 0.4799 (3) | 0.5029 (2) | 0.045 (1) | |
N1 | 0.1452 (2) | 0.5296 (4) | 0.4204 (2) | 0.037 (1) | |
N2 | 0.2202 (1) | 0.5482 (5) | 0.3842 (2) | 0.039 (1) | |
N3 | 0.0457 (1) | 0.3040 (4) | 0.6206 (2) | 0.033 (1) | |
N4 | 0.0850 (1) | 0.1902 (4) | 0.5504 (2) | 0.037 (1) | |
C1 | 0.1165 (2) | 0.4073 (6) | 0.3925 (3) | 0.051 (2) | |
C2 | 0.0687 (2) | 0.4261 (8) | 0.3615 (3) | 0.067 (2) | |
C3 | 0.0515 (2) | 0.5730 (8) | 0.3599 (3) | 0.067 (2) | |
C4 | 0.0816 (2) | 0.7037 (6) | 0.3901 (3) | 0.049 (1) | |
C5 | 0.0663 (2) | 0.8559 (7) | 0.3928 (3) | 0.069 (2) | |
C6 | 0.0976 (3) | 0.9764 (6) | 0.4249 (3) | 0.061 (2) | |
C7 | 0.1445 (2) | 0.9525 (6) | 0.4535 (3) | 0.049 (2) | |
C8 | 0.1612 (2) | 0.8055 (5) | 0.4510 (2) | 0.039 (1) | |
C9 | 0.1286 (2) | 0.6775 (6) | 0.4195 (2) | 0.037 (1) | |
C10 | 0.2257 (2) | 0.6878 (6) | 0.3645 (3) | 0.054 (2) | |
C11 | 0.2173 (2) | 0.7050 (7) | 0.3029 (3) | 0.065 (2) | |
C12 | 0.2027 (2) | 0.5777 (8) | 0.2625 (3) | 0.064 (2) | |
C13 | 0.1960 (2) | 0.4308 (7) | 0.2820 (3) | 0.054 (2) | |
C14 | 0.1795 (2) | 0.2975 (8) | 0.2408 (3) | 0.074 (2) | |
C15 | 0.1731 (2) | 0.1567 (8) | 0.2630 (3) | 0.080 (2) | |
C16 | 0.1829 (2) | 0.1433 (6) | 0.3252 (3) | 0.061 (2) | |
C17 | 0.1998 (2) | 0.2731 (6) | 0.3675 (2) | 0.041 (1) | |
C18 | 0.2050 (2) | 0.4186 (6) | 0.3434 (2) | 0.038 (1) | |
C19 | 0.0629 (2) | 0.4435 (6) | 0.6490 (2) | 0.042 (1) | |
C20 | 0.0866 (2) | 0.4699 (6) | 0.7152 (3) | 0.052 (2) | |
C21 | 0.0928 (2) | 0.3424 (7) | 0.7533 (2) | 0.057 (2) | |
C22 | 0.0744 (2) | 0.1887 (6) | 0.7259 (2) | 0.044 (1) | |
C23 | 0.0777 (2) | 0.0557 (7) | 0.7621 (3) | 0.065 (2) | |
C24 | 0.0590 (2) | −0.0830 (8) | 0.7309 (3) | 0.068 (2) | |
C25 | 0.0362 (2) | −0.1030 (6) | 0.6639 (3) | 0.053 (2) | |
C26 | 0.0317 (2) | 0.0262 (5) | 0.6255 (3) | 0.037 (1) | |
C27 | 0.0513 (2) | 0.1743 (5) | 0.6583 (2) | 0.034 (1) | |
C28 | 0.1054 (2) | 0.0505 (6) | 0.5748 (3) | 0.048 (1) | |
C29 | 0.1524 (2) | 0.0263 (6) | 0.6074 (3) | 0.057 (2) | |
C30 | 0.1792 (2) | 0.1538 (7) | 0.6147 (3) | 0.056 (2) | |
C31 | 0.1595 (2) | 0.3048 (6) | 0.5895 (2) | 0.040 (1) | |
C32 | 0.1844 (2) | 0.4418 (7) | 0.5952 (3) | 0.055 (2) | |
C33 | 0.1623 (2) | 0.5842 (7) | 0.5710 (3) | 0.053 (2) | |
C34 | 0.1153 (2) | 0.5998 (6) | 0.5401 (2) | 0.046 (1) | |
C35 | 0.0881 (2) | 0.4711 (5) | 0.5315 (2) | 0.038 (1) | |
C36 | 0.1112 (2) | 0.3197 (5) | 0.5573 (2) | 0.033 (1) | |
H1 | 0.1280 | 0.3066 | 0.3934 | 0.061* | |
H2 | 0.0491 | 0.3384 | 0.3423 | 0.080* | |
H3 | 0.0201 | 0.5866 | 0.3388 | 0.081* | |
H5 | 0.0352 | 0.8745 | 0.3729 | 0.083* | |
H6 | 0.0876 | 1.0766 | 0.4279 | 0.074* | |
H7 | 0.1649 | 1.0376 | 0.4745 | 0.059* | |
H10 | 0.2353 | 0.7765 | 0.3918 | 0.065* | |
H11 | 0.2218 | 0.8036 | 0.2903 | 0.077* | |
H12 | 0.1971 | 0.5879 | 0.2220 | 0.077* | |
H14 | 0.1730 | 0.3037 | 0.1996 | 0.088* | |
H15 | 0.1619 | 0.0674 | 0.2359 | 0.096* | |
H16 | 0.1780 | 0.0460 | 0.3382 | 0.073* | |
H19 | 0.0589 | 0.5299 | 0.6229 | 0.051* | |
H20 | 0.0979 | 0.5710 | 0.7331 | 0.062* | |
H21 | 0.1093 | 0.3564 | 0.7980 | 0.068* | |
H23 | 0.0927 | 0.0636 | 0.8068 | 0.078* | |
H24 | 0.0612 | −0.1710 | 0.7551 | 0.082* | |
H25 | 0.0241 | −0.2026 | 0.6448 | 0.064* | |
H28 | 0.0873 | −0.0364 | 0.5698 | 0.058* | |
H29 | 0.1654 | −0.0741 | 0.6240 | 0.068* | |
H30 | 0.2107 | 0.1399 | 0.6367 | 0.067* | |
H32 | 0.2160 | 0.4351 | 0.6155 | 0.066* | |
H33 | 0.1791 | 0.6742 | 0.5754 | 0.064* | |
H34 | 0.1017 | 0.7000 | 0.5246 | 0.055* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.0361 (1) | 0.0271 (1) | 0.0307 (1) | 0.0056 (1) | 0.0119 (1) | 0.0010 (1) |
Pb2 | 0.0329 (1) | 0.0259 (1) | 0.0327 (1) | 0.0028 (1) | 0.0141 (1) | −0.0022 (1) |
O1 | 0.034 (2) | 0.032 (2) | 0.054 (2) | 0.006 (1) | 0.018 (2) | −0.003 (2) |
O2 | 0.050 (2) | 0.030 (2) | 0.044 (2) | 0.004 (2) | 0.020 (2) | −0.003 (2) |
O3 | 0.054 (2) | 0.029 (2) | 0.041 (2) | −0.002 (1) | 0.028 (2) | −0.004 (1) |
O4 | 0.041 (2) | 0.032 (2) | 0.060 (2) | 0.007 (1) | 0.029 (2) | 0.002 (2) |
N1 | 0.037 (3) | 0.037 (2) | 0.034 (2) | −0.002 (2) | 0.020 (2) | −0.003 (2) |
N2 | 0.033 (2) | 0.039 (2) | 0.036 (2) | −0.003 (2) | 0.015 (2) | −0.003 (2) |
N3 | 0.031 (2) | 0.027 (2) | 0.037 (2) | −0.001 (2) | 0.018 (2) | −0.005 (2) |
N4 | 0.037 (2) | 0.031 (2) | 0.046 (2) | 0.0083 (17) | 0.027 (2) | 0.003 (2) |
C1 | 0.047 (3) | 0.043 (3) | 0.061 (4) | −0.008 (3) | 0.031 (3) | −0.002 (3) |
C2 | 0.051 (4) | 0.064 (4) | 0.080 (5) | −0.017 (3) | 0.036 (4) | 0.000 (4) |
C3 | 0.035 (3) | 0.077 (4) | 0.089 (5) | −0.003 (3) | 0.036 (4) | −0.003 (4) |
C4 | 0.044 (3) | 0.050 (3) | 0.065 (4) | 0.007 (3) | 0.039 (3) | 0.008 (3) |
C5 | 0.048 (4) | 0.071 (4) | 0.098 (5) | 0.017 (3) | 0.049 (4) | 0.011 (4) |
C6 | 0.072 (5) | 0.053 (4) | 0.080 (5) | 0.025 (3) | 0.056 (4) | 0.011 (3) |
C7 | 0.059 (4) | 0.038 (3) | 0.054 (3) | 0.010 (3) | 0.035 (3) | −0.002 (3) |
C8 | 0.043 (3) | 0.034 (3) | 0.034 (3) | 0.008 (2) | 0.019 (2) | 0.004 (2) |
C9 | 0.035 (3) | 0.041 (3) | 0.037 (3) | 0.007 (2) | 0.022 (2) | 0.007 (2) |
C10 | 0.057 (4) | 0.043 (3) | 0.058 (4) | −0.007 (3) | 0.032 (3) | −0.004 (3) |
C11 | 0.071 (4) | 0.067 (4) | 0.053 (4) | −0.004 (3) | 0.035 (3) | 0.014 (3) |
C12 | 0.078 (5) | 0.074 (4) | 0.053 (4) | 0.006 (4) | 0.046 (4) | 0.002 (4) |
C13 | 0.048 (3) | 0.060 (4) | 0.046 (3) | 0.007 (3) | 0.024 (3) | −0.008 (3) |
C14 | 0.091 (5) | 0.073 (4) | 0.045 (4) | 0.017 (4) | 0.034 (4) | −0.015 (3) |
C15 | 0.083 (5) | 0.073 (5) | 0.057 (4) | 0.009 (4) | 0.027 (4) | −0.032 (4) |
C16 | 0.058 (4) | 0.044 (3) | 0.054 (4) | 0.001 (3) | 0.019 (3) | −0.011 (3) |
C17 | 0.034 (3) | 0.039 (3) | 0.037 (3) | 0.013 (2) | 0.012 (2) | −0.005 (2) |
C18 | 0.032 (3) | 0.039 (3) | 0.035 (3) | 0.003 (2) | 0.017 (2) | −0.006 (2) |
C19 | 0.042 (3) | 0.034 (3) | 0.043 (3) | 0.001 (2) | 0.020 (3) | −0.006 (2) |
C20 | 0.047 (4) | 0.047 (4) | 0.045 (3) | −0.004 (2) | 0.018 (3) | −0.015 (3) |
C21 | 0.042 (3) | 0.077 (4) | 0.031 (3) | 0.003 (3) | 0.010 (3) | −0.014 (3) |
C22 | 0.041 (3) | 0.050 (3) | 0.038 (3) | 0.010 (2) | 0.022 (3) | 0.001 (2) |
C23 | 0.086 (5) | 0.062 (4) | 0.042 (3) | 0.012 (4) | 0.035 (4) | 0.008 (3) |
C24 | 0.099 (5) | 0.059 (4) | 0.057 (4) | 0.024 (4) | 0.052 (4) | 0.025 (3) |
C25 | 0.078 (4) | 0.038 (3) | 0.064 (4) | 0.012 (3) | 0.053 (4) | 0.004 (3) |
C26 | 0.041 (3) | 0.037 (3) | 0.043 (3) | 0.007 (2) | 0.030 (3) | 0.001 (2) |
C27 | 0.026 (2) | 0.037 (3) | 0.032 (2) | 0.008 (2) | 0.014 (2) | 0.001 (2) |
C28 | 0.050 (3) | 0.036 (3) | 0.060 (4) | 0.005 (3) | 0.034 (3) | 0.001 (3) |
C29 | 0.045 (4) | 0.042 (3) | 0.073 (4) | 0.017 (3) | 0.030 (3) | 0.006 (3) |
C30 | 0.036 (3) | 0.071 (4) | 0.056 (4) | 0.014 (3) | 0.024 (3) | 0.010 (3) |
C31 | 0.035 (3) | 0.053 (3) | 0.035 (3) | 0.004 (2) | 0.023 (2) | 0.003 (2) |
C32 | 0.048 (4) | 0.065 (4) | 0.061 (4) | −0.008 (3) | 0.038 (3) | 0.003 (3) |
C33 | 0.060 (4) | 0.045 (3) | 0.060 (4) | −0.019 (3) | 0.038 (3) | −0.006 (3) |
C34 | 0.062 (4) | 0.033 (3) | 0.056 (3) | −0.006 (3) | 0.042 (3) | 0.002 (2) |
C35 | 0.044 (3) | 0.035 (3) | 0.041 (3) | −0.001 (2) | 0.029 (3) | 0.001 (2) |
C36 | 0.038 (3) | 0.035 (3) | 0.030 (2) | 0.002 (2) | 0.023 (2) | −0.002 (2) |
Geometric parameters (Å, º) top
Pb1—O1 | 2.433 (3) | C19—C20 | 1.387 (7) |
Pb1—O1i | 2.627 (3) | C20—C21 | 1.365 (7) |
Pb1—O2 | 2.387 (3) | C21—C22 | 1.422 (7) |
Pb1—O2ii | 2.952 (3) | C22—C23 | 1.400 (7) |
Pb1—N1 | 2.528 (4) | C22—C27 | 1.407 (6) |
Pb1—N2 | 2.482 (4) | C23—C24 | 1.339 (8) |
Pb2—O3 | 2.396 (3) | C24—C25 | 1.401 (7) |
Pb2—O3iii | 2.649 (3) | C25—C26 | 1.396 (7) |
Pb2—O4 | 2.416 (3) | C26—C27 | 1.423 (6) |
Pb2—O4iv | 2.763 (3) | C28—C29 | 1.389 (8) |
Pb2—N3 | 2.475 (4) | C29—C30 | 1.371 (7) |
Pb2—N4 | 2.493 (4) | C30—C31 | 1.400 (7) |
O1—C8 | 1.318 (5) | C31—C32 | 1.404 (7) |
O2—C17 | 1.303 (6) | C31—C36 | 1.423 (6) |
O3—C26 | 1.311 (6) | C32—C33 | 1.359 (7) |
O4—C35 | 1.299 (7) | C33—C34 | 1.385 (7) |
N1—C1 | 1.320 (6) | C34—C35 | 1.378 (6) |
N1—C9 | 1.364 (5) | C35—C36 | 1.440 (6) |
N2—C10 | 1.326 (6) | C1—H1 | 0.93 |
N2—C18 | 1.368 (6) | C2—H2 | 0.93 |
N3—C19 | 1.315 (5) | C3—H3 | 0.93 |
N3—C27 | 1.378 (5) | C5—H5 | 0.93 |
N4—C28 | 1.320 (5) | C6—H6 | 0.93 |
N4—C36 | 1.375 (5) | C7—H7 | 0.93 |
C1—C2 | 1.414 (7) | C10—H10 | 0.93 |
C2—C3 | 1.361 (8) | C11—H11 | 0.93 |
C3—C4 | 1.402 (7) | C12—H12 | 0.93 |
C4—C5 | 1.399 (7) | C14—H14 | 0.93 |
C4—C9 | 1.406 (7) | C15—H15 | 0.93 |
C5—C6 | 1.363 (8) | C16—H16 | 0.93 |
C6—C7 | 1.405 (9) | C19—H19 | 0.93 |
C7—C8 | 1.381 (6) | C20—H20 | 0.93 |
C8—C9 | 1.430 (6) | C21—H21 | 0.93 |
C10—C11 | 1.417 (7) | C23—H23 | 0.93 |
C11—C12 | 1.349 (7) | C24—H24 | 0.93 |
C12—C13 | 1.394 (8) | C25—H25 | 0.93 |
C13—C14 | 1.398 (7) | C28—H28 | 0.93 |
C13—C18 | 1.401 (7) | C29—H29 | 0.93 |
C14—C15 | 1.380 (8) | C30—H30 | 0.93 |
C15—C16 | 1.410 (8) | C32—H32 | 0.93 |
C16—C17 | 1.388 (6) | C33—H33 | 0.93 |
C17—C18 | 1.419 (7) | C34—H34 | 0.93 |
O1—Pb1—O1i | 66.0 (1) | C13—C18—C17 | 122.7 (5) |
O1—Pb1—O2 | 138.6 (1) | N3—C19—C20 | 124.1 (5) |
O1—Pb1—O2ii | 149.9 (1) | C21—C20—C19 | 117.7 (5) |
O1—Pb1—N1 | 66.2 (1) | C20—C21—C22 | 121.3 (5) |
O1—Pb1—N2 | 85.2 (1) | C23—C22—C27 | 119.8 (5) |
O1i—Pb1—O2 | 132.3 (1) | C23—C22—C21 | 123.8 (5) |
O1i—Pb1—O2ii | 100.5 (1) | C27—C22—C21 | 116.4 (5) |
O1i—Pb1—N1 | 130.0 (1) | C24—C23—C22 | 118.4 (5) |
O1i—Pb1—N2 | 79.2 (1) | C23—C24—C25 | 123.6 (6) |
O2—Pb1—O2ii | 70.8 (1) | C24—C25—C26 | 120.2 (5) |
O2—Pb1—N1 | 79.8 (1) | O3—C26—C25 | 123.0 (5) |
O2—Pb1—N2 | 67.3 (1) | O3—C26—C27 | 120.4 (4) |
O2ii—Pb1—N1 | 128.6 (1) | C25—C26—C27 | 116.5 (5) |
O2ii—Pb1—N2 | 119.9 (1) | N3—C27—C22 | 121.6 (4) |
N1—Pb1—N2 | 83.3 (1) | N3—C27—C26 | 117.0 (4) |
O3—Pb2—O3iii | 68.3 (1) | C22—C27—C26 | 121.4 (5) |
O3—Pb2—O4 | 144.3 (1) | N4—C28—C29 | 123.5 (5) |
O3—Pb2—O4iv | 121.5 (1) | C30—C29—C28 | 118.5 (5) |
O3—Pb2—N3 | 67.7 (1) | C29—C30—C31 | 120.7 (5) |
O3—Pb2—N4 | 83.3 (1) | C30—C31—C32 | 124.4 (5) |
O3iii—Pb2—O4 | 122.9 (1) | C30—C31—C36 | 117.2 (5) |
O3iii—Pb2—O4iv | 141.3 (1) | C32—C31—C36 | 118.4 (5) |
O3iii—Pb2—N3 | 131.6 (1) | C33—C32—C31 | 119.7 (5) |
O3iii—Pb2—N4 | 81.2 (1) | C32—C33—C34 | 122.2 (5) |
O4—Pb2—O4iv | 73.1 (1) | C33—C34—C35 | 121.9 (5) |
O4—Pb2—N3 | 84.9 (1) | O4—C35—C34 | 124.1 (4) |
O4—Pb2—N4 | 67.1 (1) | O4—C35—C36 | 119.4 (4) |
O4iv—Pb2—N3 | 80.8 (1) | C34—C35—C36 | 116.5 (5) |
O4iv—Pb2—N4 | 134.4 (1) | N4—C36—C31 | 121.2 (4) |
N3—Pb2—N4 | 74.5 (1) | N4—C36—C35 | 117.5 (4) |
C8—O1—Pb1 | 119.4 (3) | C31—C36—C35 | 121.3 (5) |
C8—O1—Pb1i | 126.4 (3) | N1—C1—H1 | 119.3 |
Pb1—O1—Pb1i | 114.1 (1) | C2—C1—H1 | 119.3 |
C17—O2—Pb1 | 119.2 (3) | C3—C2—H2 | 120.1 |
C26—O3—Pb2 | 119.2 (3) | C1—C2—H2 | 120.1 |
C26—O3—Pb2iii | 125.0 (3) | C2—C3—H3 | 120.2 |
Pb2—O3—Pb2iii | 111.7 (1) | C4—C3—H3 | 120.2 |
C35—O4—Pb2 | 120.0 (3) | C6—C5—H5 | 120.3 |
C1—N1—C9 | 119.6 (5) | C4—C5—H5 | 120.3 |
C1—N1—Pb1 | 124.1 (3) | C5—C6—H6 | 119.3 |
C9—N1—Pb1 | 115.8 (3) | C7—C6—H6 | 119.3 |
C10—N2—C18 | 119.4 (5) | C8—C7—H7 | 119.2 |
C10—N2—Pb1 | 124.7 (3) | C6—C7—H7 | 119.2 |
C18—N2—Pb1 | 115.8 (3) | N2—C10—H10 | 119.2 |
C19—N3—C27 | 118.8 (4) | C11—C10—H10 | 119.2 |
C19—N3—Pb2 | 125.5 (3) | C12—C11—H11 | 120.1 |
C27—N3—Pb2 | 115.7 (3) | C10—C11—H11 | 120.1 |
C28—N4—C36 | 118.9 (4) | C11—C12—H12 | 120.3 |
C28—N4—Pb2 | 125.3 (3) | C13—C12—H12 | 120.3 |
C36—N4—Pb2 | 115.5 (3) | C15—C14—H14 | 121.0 |
N1—C1—C2 | 121.4 (5) | C13—C14—H14 | 121.0 |
C3—C2—C1 | 119.8 (6) | C14—C15—H15 | 118.8 |
C2—C3—C4 | 119.6 (5) | C16—C15—H15 | 118.8 |
C3—C4—C5 | 122.3 (5) | C17—C16—H16 | 119.5 |
C3—C4—C9 | 117.9 (5) | C15—C16—H16 | 119.5 |
C5—C4—C9 | 119.8 (5) | N3—C19—H19 | 117.9 |
C6—C5—C4 | 119.4 (5) | C20—C19—H19 | 117.9 |
C5—C6—C7 | 121.3 (5) | C21—C20—H20 | 121.1 |
C8—C7—C6 | 121.6 (5) | C19—C20—H20 | 121.1 |
O1—C8—C7 | 123.4 (5) | C20—C21—H21 | 119.3 |
O1—C8—C9 | 119.6 (4) | C22—C21—H21 | 119.3 |
C7—C8—C9 | 117.0 (5) | C24—C23—H23 | 120.8 |
N1—C9—C4 | 121.7 (5) | C22—C23—H23 | 120.8 |
N1—C9—C8 | 117.4 (4) | C23—C24—H24 | 118.2 |
C4—C9—C8 | 120.9 (5) | C25—C24—H24 | 118.2 |
N2—C10—C11 | 121.5 (5) | C24—C25—H25 | 119.9 |
C12—C11—C10 | 119.7 (6) | C26—C25—H25 | 119.9 |
C11—C12—C13 | 119.4 (6) | N4—C28—H28 | 118.2 |
C12—C13—C14 | 121.2 (6) | C29—C28—H28 | 118.2 |
C12—C13—C18 | 119.1 (5) | C30—C29—H29 | 120.7 |
C14—C13—C18 | 119.7 (6) | C28—C29—H29 | 120.7 |
C15—C14—C13 | 118.0 (6) | C29—C30—H30 | 119.6 |
C14—C15—C16 | 122.4 (5) | C31—C30—H30 | 119.6 |
C17—C16—C15 | 120.9 (6) | C33—C32—H32 | 120.1 |
O2—C17—C16 | 122.8 (5) | C31—C32—H32 | 120.1 |
O2—C17—C18 | 121.0 (4) | C32—C33—H33 | 118.9 |
C16—C17—C18 | 116.2 (5) | C34—C33—H33 | 118.9 |
N2—C18—C13 | 120.8 (5) | C33—C34—H34 | 119.0 |
N2—C18—C17 | 116.4 (5) | C35—C34—H34 | 119.0 |
O2—Pb1—O1—C8 | 48.4 (4) | Pb1—N1—C9—C8 | 7.1 (5) |
N2—Pb1—O1—C8 | 95.6 (3) | C3—C4—C9—N1 | −1.5 (8) |
N1—Pb1—O1—C8 | 10.8 (3) | C5—C4—C9—N1 | 177.2 (5) |
O1i—Pb1—O1—C8 | 175.9 (4) | C3—C4—C9—C8 | 179.7 (5) |
O2ii—Pb1—O1—C8 | −116.0 (3) | C5—C4—C9—C8 | −1.6 (8) |
O2—Pb1—O1—Pb1i | −127.5 (2) | O1—C8—C9—N1 | 2.8 (7) |
N2—Pb1—O1—Pb1i | −80.3 (2) | C7—C8—C9—N1 | −176.1 (4) |
N1—Pb1—O1—Pb1i | −165.0 (2) | O1—C8—C9—C4 | −178.4 (5) |
O1i—Pb1—O1—Pb1i | 0.0 | C7—C8—C9—C4 | 2.8 (7) |
O2ii—Pb1—O1—Pb1i | 68.1 (3) | C18—N2—C10—C11 | −1.8 (8) |
O1—Pb1—O2—C17 | 47.7 (4) | Pb1—N2—C10—C11 | −178.3 (4) |
N2—Pb1—O2—C17 | −4.7 (3) | N2—C10—C11—C12 | 1.0 (9) |
N1—Pb1—O2—C17 | 82.2 (3) | C10—C11—C12—C13 | 0.1 (9) |
O1i—Pb1—O2—C17 | −53.8 (4) | C11—C12—C13—C14 | 177.8 (6) |
O2ii—Pb1—O2—C17 | −140.6 (4) | C11—C12—C13—C18 | −0.4 (8) |
O4—Pb2—O3—C26 | 41.7 (5) | C12—C13—C14—C15 | −179.0 (6) |
N3—Pb2—O3—C26 | −0.9 (4) | C18—C13—C14—C15 | −0.9 (9) |
N4—Pb2—O3—C26 | 75.0 (4) | C13—C14—C15—C16 | 0 (1) |
O3iii—Pb2—O3—C26 | 158.3 (5) | C14—C15—C16—C17 | 0 (1) |
O4iv—Pb2—O3—C26 | −64.0 (4) | Pb1—O2—C17—C16 | −174.1 (4) |
O4—Pb2—O3—Pb2iii | −116.6 (2) | Pb1—O2—C17—C18 | 5.3 (6) |
N3—Pb2—O3—Pb2iii | −159.2 (2) | C15—C16—C17—O2 | −178.7 (5) |
N4—Pb2—O3—Pb2iii | −83.2 (2) | C15—C16—C17—C18 | 1.9 (8) |
O3iii—Pb2—O3—Pb2iii | 0.0 | C10—N2—C18—C13 | 1.4 (7) |
O4iv—Pb2—O3—Pb2iii | 137.8 (1) | Pb1—N2—C18—C13 | 178.3 (4) |
O3—Pb2—O4—C35 | 30.2 (5) | C10—N2—C18—C17 | −179.8 (4) |
N3—Pb2—O4—C35 | 69.2 (4) | Pb1—N2—C18—C17 | −2.9 (5) |
N4—Pb2—O4—C35 | −6.1 (4) | C12—C13—C18—N2 | −0.4 (8) |
O3iii—Pb2—O4—C35 | −68.1 (4) | C14—C13—C18—N2 | −178.6 (5) |
O4iv—Pb2—O4—C35 | 151.1 (5) | C12—C13—C18—C17 | −179.0 (5) |
O2—Pb1—N1—C1 | 23.3 (4) | C14—C13—C18—C17 | 2.8 (8) |
O1—Pb1—N1—C1 | 179.2 (4) | O2—C17—C18—N2 | −1.4 (7) |
N2—Pb1—N1—C1 | 91.4 (4) | C16—C17—C18—N2 | 178.1 (4) |
O1i—Pb1—N1—C1 | 161.2 (4) | O2—C17—C18—C13 | 177.3 (5) |
O2ii—Pb1—N1—C1 | −31.7 (5) | C16—C17—C18—C13 | −3.2 (7) |
O2—Pb1—N1—C9 | −164.8 (3) | C27—N3—C19—C20 | −0.1 (8) |
O1—Pb1—N1—C9 | −9.0 (3) | Pb2—N3—C19—C20 | 179.7 (4) |
N2—Pb1—N1—C9 | −96.7 (3) | N3—C19—C20—C21 | 0.6 (9) |
O1i—Pb1—N1—C9 | −26.9 (4) | C19—C20—C21—C22 | −1.9 (9) |
O2ii—Pb1—N1—C9 | 140.1 (3) | C20—C21—C22—C23 | −176.9 (6) |
O2—Pb1—N2—C10 | −179.4 (4) | C20—C21—C22—C27 | 2.5 (8) |
O1—Pb1—N2—C10 | 32.3 (4) | C27—C22—C23—C24 | 0.5 (9) |
N1—Pb1—N2—C10 | 98.8 (4) | C21—C22—C23—C24 | 179.9 (6) |
O1i—Pb1—N2—C10 | −34.1 (4) | C22—C23—C24—C25 | 0 (1) |
O2ii—Pb1—N2—C10 | −130.1 (4) | C23—C24—C25—C26 | −1 (1) |
O2—Pb1—N2—C18 | 3.9 (3) | Pb2—O3—C26—C25 | 178.6 (4) |
O1—Pb1—N2—C18 | −144.4 (3) | Pb2iii—O3—C26—C25 | −26.3 (7) |
N1—Pb1—N2—C18 | −77.8 (3) | Pb2—O3—C26—C27 | 1.0 (6) |
O1i—Pb1—N2—C18 | 149.2 (3) | Pb2iii—O3—C26—C27 | 156.1 (3) |
O2ii—Pb1—N2—C18 | 53.2 (3) | C24—C25—C26—O3 | −177.3 (5) |
O3—Pb2—N3—C19 | −179.0 (4) | C24—C25—C26—C27 | 0.4 (8) |
O4—Pb2—N3—C19 | 24.3 (4) | C19—N3—C27—C22 | 0.9 (7) |
N4—Pb2—N3—C19 | 92.0 (4) | Pb2—N3—C27—C22 | −179.0 (3) |
O3iii—Pb2—N3—C19 | 154.8 (4) | C19—N3—C27—C26 | 179.2 (4) |
O4iv—Pb2—N3—C19 | −49.4 (4) | Pb2—N3—C27—C26 | −0.7 (5) |
O3—Pb2—N3—C27 | 0.8 (3) | C23—C22—C27—N3 | 177.4 (5) |
O4—Pb2—N3—C27 | −155.8 (3) | C21—C22—C27—N3 | −2.0 (7) |
N4—Pb2—N3—C27 | −88.2 (3) | C23—C22—C27—C26 | −0.8 (8) |
O3iii—Pb2—N3—C27 | −25.3 (4) | C21—C22—C27—C26 | 179.8 (5) |
O4iv—Pb2—N3—C27 | 130.5 (3) | O3—C26—C27—N3 | −0.2 (7) |
O3—Pb2—N4—C28 | 19.0 (4) | C25—C26—C27—N3 | −177.9 (4) |
O4—Pb2—N4—C28 | 178.6 (4) | O3—C26—C27—C22 | 178.1 (5) |
N3—Pb2—N4—C28 | 87.6 (4) | C25—C26—C27—C22 | 0.4 (7) |
O3iii—Pb2—N4—C28 | −50.0 (4) | C36—N4—C28—C29 | 0.2 (8) |
O4iv—Pb2—N4—C28 | 147.4 (4) | Pb2—N4—C28—C29 | −172.6 (5) |
O3—Pb2—N4—C36 | −154.0 (3) | N4—C28—C29—C30 | −0 (1) |
O4—Pb2—N4—C36 | 5.6 (3) | C28—C29—C30—C31 | 0.3 (9) |
N3—Pb2—N4—C36 | −85.3 (3) | C29—C30—C31—C32 | 179.4 (6) |
O3iii—Pb2—N4—C36 | 137.0 (3) | C29—C30—C31—C36 | 1.0 (8) |
O4iv—Pb2—N4—C36 | −25.6 (4) | C30—C31—C32—C33 | −177.6 (5) |
C9—N1—C1—C2 | 0.2 (8) | C36—C31—C32—C33 | 0.9 (8) |
Pb1—N1—C1—C2 | 171.8 (4) | C31—C32—C33—C34 | −0.4 (9) |
N1—C1—C2—C3 | 0.1 (9) | C32—C33—C34—C35 | −0.5 (9) |
C1—C2—C3—C4 | −1.2 (9) | Pb2—O4—C35—C34 | −173.0 (4) |
C2—C3—C4—C5 | −176.9 (6) | Pb2—O4—C35—C36 | 6.0 (6) |
C2—C3—C4—C9 | 1.8 (9) | C33—C34—C35—O4 | 179.8 (5) |
C3—C4—C5—C6 | 177.7 (6) | C33—C34—C35—C36 | 0.9 (8) |
C9—C4—C5—C6 | −0.9 (9) | C28—N4—C36—C31 | 0.5 (7) |
C4—C5—C6—C7 | 2.1 (10) | Pb2—N4—C36—C31 | 173.9 (3) |
C5—C6—C7—C8 | −0.8 (10) | C28—N4—C36—C35 | −178.6 (5) |
Pb1—O1—C8—C7 | 166.9 (4) | Pb2—N4—C36—C35 | −5.2 (5) |
Pb1i—O1—C8—C7 | −17.8 (7) | C30—C31—C36—N4 | −1.0 (7) |
Pb1—O1—C8—C9 | −11.9 (6) | C32—C31—C36—N4 | −179.6 (4) |
Pb1i—O1—C8—C9 | 163.4 (3) | C30—C31—C36—C35 | 178.1 (5) |
C6—C7—C8—O1 | 179.6 (5) | C32—C31—C36—C35 | −0.5 (7) |
C6—C7—C8—C9 | −1.6 (8) | O4—C35—C36—N4 | −0.2 (7) |
C1—N1—C9—C4 | 0.5 (8) | C34—C35—C36—N4 | 178.7 (4) |
Pb1—N1—C9—C4 | −171.8 (4) | O4—C35—C36—C31 | −179.4 (5) |
C1—N1—C9—C8 | 179.3 (5) | C34—C35—C36—C31 | −0.4 (7) |
Symmetry codes: (i) −x+1/2, −y+3/2, −z+1; (ii) −x+1/2, −y+1/2, −z+1; (iii) −x, −y, −z+1; (iv) −x, −y+1, −z+1. |