Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106030198/bg3015sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270106030198/bg3015Isup2.hkl |
CCDC reference: 621266
A mixture of lead(II) nitrate (0.165 g, 0.49 mmol), 4-carboxybenzeneboronic acid (0.079 g, 0.48 mmol), 1,10-phenanthroline monohydrate (0.090 g, 0.45 mmol) and water (15 ml) was sealed in a 30 ml Teflon-lined stainless steel autoclave and heated at 423 K for 4 d. After cooling of the autoclave, a solution with some powder residue was obtained, and this solid was filtered off. The filtrate was allowed to evaporate, and after one week, pale-yellow crystals in the form of blocks were obtained by filtration.
All H atoms were placed in calculated positions and treated as riding, with C—H distances of 0.93 Å and Uiso(H) values of 1.2Ueq(carrier). The highest peak in the final difference Fourier map lies 0.99 Å from atom Pb2.
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: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Pb2(C7H5O2)3(NO3)(C12H8N2)2] | F(000) = 2288 |
Mr = 1200.13 | Dx = 1.975 Mg m−3 |
MonoclinicP21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 4675 reflections |
a = 17.2481 (10) Å | θ = 2.2–25.0° |
b = 20.6393 (12) Å | µ = 8.40 mm−1 |
c = 11.5549 (6) Å | T = 295 K |
β = 101.167 (1)° | Block, pale yellow |
V = 4035.5 (4) Å3 | 0.13 × 0.09 × 0.08 mm |
Z = 4 |
Bruker APEX area-detector diffractometer | 7182 independent reflections |
Radiation source: fine-focus sealed tube | 5090 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 25.1°, θmin = 1.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −20→20 |
Tmin = 0.417, Tmax = 0.521 | k = −13→24 |
20990 measured reflections | l = −13→13 |
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.093 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0391P)2 + 4.7224P] where P = (Fo2 + 2Fc2)/3 |
7182 reflections | (Δ/σ)max = 0.002 |
550 parameters | Δρmax = 2.23 e Å−3 |
0 restraints | Δρmin = −0.75 e Å−3 |
[Pb2(C7H5O2)3(NO3)(C12H8N2)2] | V = 4035.5 (4) Å3 |
Mr = 1200.13 | Z = 4 |
MonoclinicP21/c | Mo Kα radiation |
a = 17.2481 (10) Å | µ = 8.40 mm−1 |
b = 20.6393 (12) Å | T = 295 K |
c = 11.5549 (6) Å | 0.13 × 0.09 × 0.08 mm |
β = 101.167 (1)° |
Bruker APEX area-detector diffractometer | 7182 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | 5090 reflections with I > 2σ(I) |
Tmin = 0.417, Tmax = 0.521 | Rint = 0.031 |
20990 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.093 | H-atom parameters constrained |
S = 1.02 | Δρmax = 2.23 e Å−3 |
7182 reflections | Δρmin = −0.75 e Å−3 |
550 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Pb1 | 0.108557 (13) | 0.518681 (14) | 0.94389 (2) | 0.04490 (10) | |
Pb2 | 0.386656 (14) | 0.515049 (14) | 1.07443 (2) | 0.05231 (10) | |
O1 | 0.2554 (3) | 0.5743 (3) | 0.9349 (5) | 0.0776 (16) | |
O2 | 0.1425 (3) | 0.6019 (2) | 0.8222 (4) | 0.0636 (14) | |
O3 | −0.0010 (3) | 0.5868 (3) | 0.9983 (4) | 0.0616 (14) | |
O4 | 0.1150 (3) | 0.6176 (3) | 1.0952 (5) | 0.0859 (18) | |
O5 | 0.5111 (3) | 0.5739 (3) | 0.9839 (5) | 0.0720 (15) | |
O6 | 0.4470 (3) | 0.6238 (3) | 1.1046 (4) | 0.0696 (14) | |
O7 | 0.3359 (4) | 0.4184 (3) | 1.2130 (5) | 0.0849 (18) | |
O8 | 0.2446 (3) | 0.4462 (4) | 1.0717 (6) | 0.104 (2) | |
O9 | 0.2237 (4) | 0.3695 (4) | 1.1844 (7) | 0.124 (3) | |
N1 | 0.1413 (3) | 0.4462 (3) | 0.7685 (5) | 0.0531 (15) | |
N2 | −0.0022 (3) | 0.5059 (3) | 0.7596 (5) | 0.0470 (14) | |
N3 | 0.3517 (3) | 0.5647 (3) | 1.2504 (5) | 0.0573 (16) | |
N4 | 0.4975 (4) | 0.5128 (3) | 1.2490 (5) | 0.0571 (16) | |
N5 | 0.2666 (4) | 0.4115 (4) | 1.1589 (7) | 0.0703 (19) | |
C1 | 0.2097 (5) | 0.4177 (4) | 0.7717 (7) | 0.065 (2) | |
H1 | 0.2512 | 0.4287 | 0.8328 | 0.078* | |
C2 | 0.2243 (5) | 0.3719 (4) | 0.6895 (8) | 0.079 (3) | |
H2 | 0.2735 | 0.3524 | 0.6955 | 0.095* | |
C3 | 0.1633 (6) | 0.3572 (4) | 0.6004 (7) | 0.080 (3) | |
H3 | 0.1708 | 0.3269 | 0.5441 | 0.096* | |
C4 | 0.0896 (5) | 0.3864 (4) | 0.5911 (6) | 0.064 (2) | |
C5 | 0.0237 (6) | 0.3747 (5) | 0.4966 (7) | 0.084 (3) | |
H5 | 0.0289 | 0.3444 | 0.4390 | 0.100* | |
C6 | −0.0438 (6) | 0.4055 (4) | 0.4892 (7) | 0.076 (3) | |
H6 | −0.0844 | 0.3978 | 0.4250 | 0.092* | |
C7 | −0.0561 (5) | 0.4503 (4) | 0.5769 (6) | 0.061 (2) | |
C8 | −0.1261 (5) | 0.4841 (5) | 0.5729 (7) | 0.073 (3) | |
H8 | −0.1679 | 0.4773 | 0.5100 | 0.087* | |
C9 | −0.1349 (4) | 0.5271 (4) | 0.6595 (7) | 0.069 (2) | |
H9 | −0.1819 | 0.5495 | 0.6571 | 0.083* | |
C10 | −0.0701 (4) | 0.5360 (4) | 0.7520 (6) | 0.057 (2) | |
H10 | −0.0754 | 0.5649 | 0.8116 | 0.068* | |
C11 | 0.0062 (4) | 0.4634 (3) | 0.6732 (5) | 0.0495 (18) | |
C12 | 0.0808 (4) | 0.4316 (4) | 0.6787 (6) | 0.0542 (19) | |
C13 | 0.2158 (4) | 0.6083 (4) | 0.8565 (7) | 0.0554 (19) | |
C14 | 0.2565 (4) | 0.6596 (3) | 0.7982 (6) | 0.0491 (17) | |
C15 | 0.3361 (4) | 0.6723 (4) | 0.8363 (7) | 0.068 (2) | |
H15 | 0.3646 | 0.6487 | 0.8990 | 0.081* | |
C16 | 0.3736 (5) | 0.7188 (4) | 0.7839 (8) | 0.080 (3) | |
H16 | 0.4274 | 0.7261 | 0.8105 | 0.096* | |
C17 | 0.3329 (5) | 0.7551 (4) | 0.6919 (8) | 0.078 (3) | |
H17 | 0.3589 | 0.7867 | 0.6565 | 0.093* | |
C18 | 0.2539 (5) | 0.7444 (4) | 0.6531 (7) | 0.074 (2) | |
H18 | 0.2259 | 0.7686 | 0.5909 | 0.088* | |
C19 | 0.2156 (4) | 0.6970 (4) | 0.7070 (6) | 0.0600 (19) | |
H19 | 0.1617 | 0.6904 | 0.6814 | 0.072* | |
C20 | 0.0419 (4) | 0.6230 (4) | 1.0718 (6) | 0.0565 (19) | |
C21 | 0.0024 (4) | 0.6737 (3) | 1.1342 (6) | 0.0522 (18) | |
C22 | −0.0783 (4) | 0.6849 (4) | 1.1028 (7) | 0.064 (2) | |
H22 | −0.1091 | 0.6622 | 1.0409 | 0.077* | |
C23 | −0.1119 (5) | 0.7305 (4) | 1.1653 (9) | 0.080 (3) | |
H23 | −0.1662 | 0.7372 | 1.1460 | 0.097* | |
C24 | −0.0684 (7) | 0.7662 (5) | 1.2544 (9) | 0.091 (3) | |
H24 | −0.0923 | 0.7972 | 1.2943 | 0.109* | |
C25 | 0.0107 (6) | 0.7552 (4) | 1.2834 (8) | 0.087 (3) | |
H25 | 0.0413 | 0.7790 | 1.3439 | 0.105* | |
C26 | 0.0460 (5) | 0.7096 (4) | 1.2250 (7) | 0.070 (2) | |
H26 | 0.1002 | 0.7027 | 1.2466 | 0.084* | |
C27 | 0.2815 (5) | 0.5882 (4) | 1.2526 (7) | 0.063 (2) | |
H27 | 0.2415 | 0.5818 | 1.1871 | 0.076* | |
C28 | 0.2641 (5) | 0.6219 (4) | 1.3476 (8) | 0.076 (2) | |
H28 | 0.2126 | 0.6352 | 1.3475 | 0.092* | |
C29 | 0.3223 (6) | 0.6355 (4) | 1.4407 (8) | 0.084 (3) | |
H29 | 0.3117 | 0.6596 | 1.5038 | 0.101* | |
C30 | 0.3997 (5) | 0.6128 (4) | 1.4408 (7) | 0.072 (2) | |
C31 | 0.4672 (6) | 0.6237 (5) | 1.5371 (7) | 0.086 (3) | |
H31 | 0.4605 | 0.6482 | 1.6020 | 0.103* | |
C32 | 0.5374 (6) | 0.5995 (5) | 1.5336 (8) | 0.093 (3) | |
H32 | 0.5793 | 0.6080 | 1.5954 | 0.111* | |
C33 | 0.5505 (5) | 0.5610 (4) | 1.4388 (7) | 0.067 (2) | |
C34 | 0.6236 (5) | 0.5348 (5) | 1.4333 (8) | 0.084 (3) | |
H34 | 0.6665 | 0.5427 | 1.4940 | 0.100* | |
C35 | 0.6329 (5) | 0.4984 (5) | 1.3415 (9) | 0.084 (3) | |
H35 | 0.6818 | 0.4803 | 1.3384 | 0.101* | |
C36 | 0.5682 (5) | 0.4877 (4) | 1.2502 (8) | 0.071 (2) | |
H36 | 0.5752 | 0.4617 | 1.1872 | 0.086* | |
C37 | 0.4884 (4) | 0.5490 (4) | 1.3432 (6) | 0.0584 (19) | |
C38 | 0.4113 (4) | 0.5762 (4) | 1.3449 (6) | 0.0580 (19) | |
C39 | 0.5036 (4) | 0.6207 (4) | 1.0506 (7) | 0.0562 (18) | |
C40 | 0.5629 (4) | 0.6734 (4) | 1.0700 (6) | 0.0545 (18) | |
C41 | 0.6135 (5) | 0.6814 (4) | 0.9951 (7) | 0.077 (2) | |
H41 | 0.6113 | 0.6533 | 0.9317 | 0.092* | |
C42 | 0.6687 (5) | 0.7313 (5) | 1.0118 (9) | 0.094 (3) | |
H42 | 0.7027 | 0.7370 | 0.9592 | 0.113* | |
C43 | 0.6725 (5) | 0.7716 (4) | 1.1052 (9) | 0.084 (3) | |
H43 | 0.7094 | 0.8050 | 1.1166 | 0.101* | |
C44 | 0.6235 (5) | 0.7638 (4) | 1.1817 (8) | 0.078 (2) | |
H44 | 0.6271 | 0.7914 | 1.2462 | 0.093* | |
C45 | 0.5680 (4) | 0.7151 (4) | 1.1645 (7) | 0.067 (2) | |
H45 | 0.5338 | 0.7103 | 1.2170 | 0.081* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.03574 (15) | 0.05208 (19) | 0.04518 (15) | −0.00450 (13) | 0.00361 (11) | 0.00366 (12) |
Pb2 | 0.04347 (17) | 0.0543 (2) | 0.05633 (18) | −0.00122 (14) | 0.00252 (13) | −0.00941 (14) |
O1 | 0.053 (3) | 0.079 (4) | 0.096 (4) | −0.005 (3) | 0.002 (3) | 0.035 (4) |
O2 | 0.047 (3) | 0.060 (4) | 0.083 (3) | −0.008 (3) | 0.010 (3) | 0.020 (3) |
O3 | 0.055 (3) | 0.066 (4) | 0.061 (3) | 0.000 (3) | 0.003 (3) | −0.015 (3) |
O4 | 0.041 (3) | 0.093 (5) | 0.122 (5) | −0.002 (3) | 0.012 (3) | −0.036 (4) |
O5 | 0.061 (3) | 0.058 (4) | 0.097 (4) | −0.002 (3) | 0.016 (3) | −0.021 (3) |
O6 | 0.054 (3) | 0.068 (4) | 0.089 (4) | −0.001 (3) | 0.020 (3) | −0.010 (3) |
O7 | 0.085 (4) | 0.074 (4) | 0.081 (4) | 0.004 (4) | −0.020 (3) | 0.010 (3) |
O8 | 0.066 (4) | 0.120 (6) | 0.116 (5) | 0.000 (4) | −0.005 (3) | 0.061 (5) |
O9 | 0.095 (5) | 0.117 (6) | 0.167 (7) | 0.000 (5) | 0.045 (5) | 0.052 (6) |
N1 | 0.058 (4) | 0.048 (4) | 0.055 (3) | −0.007 (3) | 0.015 (3) | −0.002 (3) |
N2 | 0.044 (3) | 0.052 (4) | 0.044 (3) | −0.002 (3) | 0.006 (3) | 0.008 (3) |
N3 | 0.047 (4) | 0.058 (4) | 0.065 (4) | −0.007 (3) | 0.006 (3) | −0.005 (3) |
N4 | 0.052 (4) | 0.063 (4) | 0.054 (3) | 0.002 (3) | 0.004 (3) | −0.007 (3) |
N5 | 0.072 (5) | 0.053 (5) | 0.093 (5) | 0.016 (4) | 0.033 (4) | 0.021 (4) |
C1 | 0.055 (5) | 0.069 (6) | 0.073 (5) | −0.001 (5) | 0.019 (4) | 0.006 (5) |
C2 | 0.082 (6) | 0.068 (6) | 0.096 (7) | 0.014 (5) | 0.042 (5) | 0.004 (5) |
C3 | 0.111 (8) | 0.067 (6) | 0.071 (5) | 0.010 (6) | 0.038 (5) | 0.000 (5) |
C4 | 0.081 (6) | 0.054 (5) | 0.058 (5) | −0.004 (5) | 0.019 (4) | 0.003 (4) |
C5 | 0.114 (8) | 0.075 (7) | 0.061 (5) | −0.008 (6) | 0.015 (5) | −0.014 (5) |
C6 | 0.098 (7) | 0.079 (7) | 0.046 (4) | −0.021 (6) | −0.003 (5) | −0.005 (4) |
C7 | 0.066 (5) | 0.064 (5) | 0.049 (4) | −0.017 (4) | 0.000 (4) | 0.007 (4) |
C8 | 0.056 (5) | 0.098 (8) | 0.055 (5) | −0.020 (5) | −0.013 (4) | 0.018 (5) |
C9 | 0.049 (4) | 0.101 (7) | 0.055 (5) | 0.008 (5) | 0.003 (4) | 0.011 (5) |
C10 | 0.049 (4) | 0.071 (6) | 0.050 (4) | 0.004 (4) | 0.009 (3) | 0.010 (4) |
C11 | 0.059 (4) | 0.048 (4) | 0.041 (4) | −0.010 (4) | 0.008 (3) | 0.014 (3) |
C12 | 0.068 (5) | 0.049 (5) | 0.047 (4) | −0.013 (4) | 0.013 (4) | 0.016 (3) |
C13 | 0.053 (5) | 0.048 (5) | 0.070 (5) | 0.000 (4) | 0.024 (4) | 0.011 (4) |
C14 | 0.047 (4) | 0.043 (4) | 0.060 (4) | 0.001 (4) | 0.016 (3) | −0.005 (3) |
C15 | 0.054 (5) | 0.053 (5) | 0.095 (6) | −0.004 (4) | 0.014 (4) | 0.008 (4) |
C16 | 0.057 (5) | 0.069 (6) | 0.121 (8) | −0.015 (5) | 0.036 (5) | −0.001 (6) |
C17 | 0.081 (6) | 0.059 (6) | 0.108 (7) | −0.011 (5) | 0.054 (5) | −0.004 (5) |
C18 | 0.097 (7) | 0.050 (5) | 0.079 (5) | −0.003 (5) | 0.028 (5) | 0.011 (4) |
C19 | 0.061 (5) | 0.046 (5) | 0.074 (5) | 0.002 (4) | 0.016 (4) | −0.003 (4) |
C20 | 0.048 (4) | 0.057 (5) | 0.064 (5) | −0.010 (4) | 0.011 (4) | −0.002 (4) |
C21 | 0.055 (4) | 0.047 (4) | 0.058 (4) | −0.004 (4) | 0.018 (4) | 0.004 (4) |
C22 | 0.056 (5) | 0.065 (6) | 0.073 (5) | 0.010 (4) | 0.018 (4) | 0.022 (4) |
C23 | 0.070 (6) | 0.064 (6) | 0.116 (7) | 0.021 (5) | 0.042 (6) | 0.028 (6) |
C24 | 0.114 (8) | 0.061 (6) | 0.112 (8) | 0.018 (6) | 0.059 (7) | 0.015 (6) |
C25 | 0.118 (8) | 0.062 (6) | 0.084 (6) | 0.003 (6) | 0.026 (6) | −0.017 (5) |
C26 | 0.064 (5) | 0.068 (6) | 0.076 (5) | −0.003 (5) | 0.011 (4) | −0.011 (5) |
C27 | 0.063 (5) | 0.057 (5) | 0.073 (5) | −0.008 (4) | 0.021 (4) | −0.001 (4) |
C28 | 0.066 (5) | 0.078 (7) | 0.090 (6) | 0.006 (5) | 0.027 (5) | 0.011 (5) |
C29 | 0.118 (8) | 0.065 (6) | 0.081 (6) | 0.013 (6) | 0.048 (6) | −0.004 (5) |
C30 | 0.091 (6) | 0.068 (6) | 0.061 (5) | −0.014 (5) | 0.020 (5) | −0.012 (4) |
C31 | 0.122 (8) | 0.072 (7) | 0.063 (5) | −0.020 (7) | 0.015 (6) | −0.008 (5) |
C32 | 0.104 (8) | 0.095 (8) | 0.068 (6) | −0.021 (7) | −0.013 (6) | −0.009 (5) |
C33 | 0.065 (5) | 0.069 (6) | 0.062 (5) | −0.021 (5) | −0.005 (4) | −0.001 (4) |
C34 | 0.065 (6) | 0.098 (8) | 0.077 (6) | −0.024 (6) | −0.014 (5) | 0.009 (5) |
C35 | 0.052 (5) | 0.104 (8) | 0.092 (7) | −0.001 (5) | 0.001 (5) | 0.016 (6) |
C36 | 0.049 (5) | 0.083 (7) | 0.081 (6) | 0.006 (5) | 0.009 (4) | 0.006 (5) |
C37 | 0.061 (5) | 0.055 (5) | 0.058 (4) | −0.011 (4) | 0.005 (4) | −0.002 (4) |
C38 | 0.064 (5) | 0.055 (5) | 0.058 (4) | −0.006 (4) | 0.018 (4) | 0.003 (4) |
C39 | 0.052 (4) | 0.044 (5) | 0.071 (5) | 0.008 (4) | 0.008 (4) | −0.003 (4) |
C40 | 0.048 (4) | 0.052 (5) | 0.062 (4) | 0.002 (4) | 0.007 (4) | −0.005 (4) |
C41 | 0.081 (6) | 0.071 (6) | 0.084 (6) | −0.009 (5) | 0.029 (5) | −0.023 (5) |
C42 | 0.095 (7) | 0.084 (7) | 0.115 (8) | −0.032 (6) | 0.046 (6) | −0.015 (6) |
C43 | 0.064 (6) | 0.062 (6) | 0.122 (8) | −0.009 (5) | 0.008 (5) | −0.027 (6) |
C44 | 0.071 (6) | 0.061 (6) | 0.095 (6) | −0.003 (5) | −0.002 (5) | −0.026 (5) |
C45 | 0.063 (5) | 0.066 (6) | 0.071 (5) | 0.006 (5) | 0.012 (4) | −0.017 (4) |
Pb1—O2 | 2.363 (5) | C14—C19 | 1.384 (9) |
Pb1—O3 | 2.531 (5) | C15—C16 | 1.364 (10) |
Pb1—N2 | 2.585 (5) | C15—H15 | 0.9300 |
Pb1—N1 | 2.666 (6) | C16—C17 | 1.376 (11) |
Pb1—O4 | 2.677 (5) | C16—H16 | 0.9300 |
Pb1—O1 | 2.802 (5) | C17—C18 | 1.367 (11) |
Pb1—O8 | 2.929 (6) | C17—H17 | 0.9300 |
Pb1—O3i | 3.019 (5) | C18—C19 | 1.393 (10) |
Pb2—N3 | 2.454 (6) | C18—H18 | 0.9300 |
Pb2—O6 | 2.470 (5) | C19—H19 | 0.9300 |
Pb2—N4 | 2.497 (6) | C20—C21 | 1.506 (10) |
Pb2—O5ii | 2.720 (5) | C21—C26 | 1.382 (9) |
Pb2—O1 | 2.793 (5) | C21—C22 | 1.389 (9) |
Pb2—O7 | 2.802 (6) | C22—C23 | 1.381 (11) |
Pb2—O8 | 2.827 (6) | C22—H22 | 0.9300 |
Pb2—O5 | 2.837 (5) | C23—C24 | 1.365 (12) |
O1—C13 | 1.241 (8) | C23—H23 | 0.9300 |
O2—C13 | 1.256 (8) | C24—C25 | 1.360 (12) |
O3—C20 | 1.258 (8) | C24—H24 | 0.9300 |
O4—C20 | 1.243 (8) | C25—C26 | 1.368 (11) |
O5—C39 | 1.257 (8) | C25—H25 | 0.9300 |
O6—C39 | 1.258 (8) | C26—H26 | 0.9300 |
O7—N5 | 1.246 (8) | C27—C28 | 1.381 (10) |
O8—N5 | 1.234 (8) | C27—H27 | 0.9300 |
O9—N5 | 1.213 (8) | C28—C29 | 1.351 (11) |
N1—C1 | 1.313 (9) | C28—H28 | 0.9300 |
N1—C12 | 1.355 (8) | C29—C30 | 1.415 (11) |
N2—C10 | 1.312 (8) | C29—H29 | 0.9300 |
N2—C11 | 1.358 (9) | C30—C38 | 1.387 (10) |
N3—C27 | 1.309 (8) | C30—C31 | 1.464 (11) |
N3—C38 | 1.367 (8) | C31—C32 | 1.317 (13) |
N4—C36 | 1.322 (9) | C31—H31 | 0.9300 |
N4—C37 | 1.355 (9) | C32—C33 | 1.407 (12) |
C1—C2 | 1.397 (11) | C32—H32 | 0.9300 |
C1—H1 | 0.9300 | C33—C34 | 1.384 (11) |
C2—C3 | 1.356 (11) | C33—C37 | 1.403 (9) |
C2—H2 | 0.9300 | C34—C35 | 1.334 (13) |
C3—C4 | 1.391 (10) | C34—H34 | 0.9300 |
C3—H3 | 0.9300 | C35—C36 | 1.397 (11) |
C4—C12 | 1.405 (10) | C35—H35 | 0.9300 |
C4—C5 | 1.436 (10) | C36—H36 | 0.9300 |
C5—C6 | 1.315 (12) | C37—C38 | 1.447 (10) |
C5—H5 | 0.9300 | C39—C40 | 1.479 (10) |
C6—C7 | 1.418 (11) | C40—C41 | 1.354 (10) |
C6—H6 | 0.9300 | C40—C45 | 1.381 (9) |
C7—C8 | 1.387 (11) | C41—C42 | 1.390 (11) |
C7—C11 | 1.414 (9) | C41—H41 | 0.9300 |
C8—C9 | 1.368 (12) | C42—C43 | 1.353 (11) |
C8—H8 | 0.9300 | C42—H42 | 0.9300 |
C9—C10 | 1.401 (10) | C43—C44 | 1.346 (11) |
C9—H9 | 0.9300 | C43—H43 | 0.9300 |
C10—H10 | 0.9300 | C44—C45 | 1.375 (11) |
C11—C12 | 1.436 (9) | C44—H44 | 0.9300 |
C13—C14 | 1.501 (9) | C45—H45 | 0.9300 |
C14—C15 | 1.383 (9) | ||
O2—Pb1—O3 | 91.55 (17) | C8—C9—H9 | 121.4 |
O2—Pb1—N2 | 79.20 (17) | C10—C9—H9 | 121.4 |
O3—Pb1—N2 | 78.06 (16) | N2—C10—C9 | 124.0 (7) |
O2—Pb1—N1 | 80.90 (18) | N2—C10—H10 | 118.0 |
O3—Pb1—N1 | 141.18 (16) | C9—C10—H10 | 118.0 |
N2—Pb1—N1 | 63.13 (18) | N2—C11—C7 | 121.9 (7) |
O2—Pb1—O4 | 81.41 (19) | N2—C11—C12 | 119.1 (6) |
O3—Pb1—O4 | 49.62 (15) | C7—C11—C12 | 119.0 (7) |
N2—Pb1—O4 | 123.13 (17) | N1—C12—C4 | 121.6 (7) |
N1—Pb1—O4 | 159.47 (17) | N1—C12—C11 | 118.8 (7) |
O2—Pb1—O1 | 49.48 (15) | C4—C12—C11 | 119.5 (7) |
O3—Pb1—O1 | 120.37 (18) | O1—C13—O2 | 123.3 (7) |
N2—Pb1—O1 | 122.73 (16) | O1—C13—C14 | 119.1 (7) |
N1—Pb1—O1 | 82.84 (18) | O2—C13—C14 | 117.6 (7) |
O4—Pb1—O1 | 77.77 (17) | C15—C14—C19 | 117.7 (7) |
O2—Pb1—O8 | 113.83 (17) | C15—C14—C13 | 120.9 (7) |
O3—Pb1—O8 | 136.23 (18) | C19—C14—C13 | 121.4 (6) |
N2—Pb1—O8 | 139.1 (2) | C16—C15—C14 | 121.3 (8) |
N1—Pb1—O8 | 80.2 (2) | C16—C15—H15 | 119.4 |
O4—Pb1—O8 | 97.59 (19) | C14—C15—H15 | 119.4 |
O1—Pb1—O8 | 65.54 (16) | C15—C16—C17 | 120.7 (8) |
O2—Pb1—O3i | 152.80 (14) | C15—C16—H16 | 119.6 |
O3—Pb1—O3i | 79.96 (18) | C17—C16—H16 | 119.6 |
N2—Pb1—O3i | 73.78 (14) | C18—C17—C16 | 119.5 (8) |
N1—Pb1—O3i | 89.61 (15) | C18—C17—H17 | 120.2 |
O4—Pb1—O3i | 110.84 (15) | C16—C17—H17 | 120.2 |
O1—Pb1—O3i | 154.53 (14) | C17—C18—C19 | 119.7 (8) |
O8—Pb1—O3i | 89.25 (15) | C17—C18—H18 | 120.1 |
N3—Pb2—O6 | 70.60 (18) | C19—C18—H18 | 120.1 |
N3—Pb2—N4 | 67.09 (19) | C14—C19—C18 | 121.1 (7) |
O6—Pb2—N4 | 70.57 (19) | C14—C19—H19 | 119.5 |
N3—Pb2—O5ii | 139.66 (18) | C18—C19—H19 | 119.5 |
O6—Pb2—O5ii | 111.90 (16) | O4—C20—O3 | 122.2 (7) |
N4—Pb2—O5ii | 75.85 (18) | O4—C20—C21 | 119.5 (7) |
N3—Pb2—O1 | 89.67 (19) | O3—C20—C21 | 118.3 (6) |
O6—Pb2—O1 | 87.46 (16) | C26—C21—C22 | 118.7 (7) |
N4—Pb2—O1 | 151.97 (19) | C26—C21—C20 | 120.4 (7) |
O5ii—Pb2—O1 | 130.11 (17) | C22—C21—C20 | 120.9 (7) |
N3—Pb2—O7 | 70.71 (19) | C23—C22—C21 | 118.5 (8) |
O6—Pb2—O7 | 137.37 (17) | C23—C22—H22 | 120.7 |
N4—Pb2—O7 | 78.46 (18) | C21—C22—H22 | 120.7 |
O5ii—Pb2—O7 | 87.16 (18) | C24—C23—C22 | 122.5 (9) |
O1—Pb2—O7 | 109.49 (16) | C24—C23—H23 | 118.7 |
N3—Pb2—O8 | 82.4 (2) | C22—C23—H23 | 118.7 |
O6—Pb2—O8 | 142.99 (19) | C25—C24—C23 | 118.3 (9) |
N4—Pb2—O8 | 121.74 (19) | C25—C24—H24 | 120.9 |
O5ii—Pb2—O8 | 105.08 (19) | C23—C24—H24 | 120.9 |
O1—Pb2—O8 | 67.04 (16) | C24—C25—C26 | 121.0 (9) |
O7—Pb2—O8 | 44.17 (16) | C24—C25—H25 | 119.5 |
N3—Pb2—O5 | 116.82 (17) | C26—C25—H25 | 119.5 |
O6—Pb2—O5 | 48.29 (15) | C25—C26—C21 | 121.0 (8) |
N4—Pb2—O5 | 77.89 (18) | C25—C26—H26 | 119.5 |
O5ii—Pb2—O5 | 67.96 (19) | C21—C26—H26 | 119.5 |
O1—Pb2—O5 | 100.71 (15) | N3—C27—C28 | 123.1 (8) |
O7—Pb2—O5 | 149.10 (17) | N3—C27—H27 | 118.4 |
O8—Pb2—O5 | 158.00 (18) | C28—C27—H27 | 118.4 |
C13—O1—Pb2 | 159.9 (5) | C29—C28—C27 | 119.7 (8) |
C13—O1—Pb1 | 83.4 (4) | C29—C28—H28 | 120.2 |
Pb2—O1—Pb1 | 115.89 (19) | C27—C28—H28 | 120.2 |
C13—O2—Pb1 | 103.8 (4) | C28—C29—C30 | 119.2 (8) |
C20—O3—Pb1 | 97.4 (4) | C28—C29—H29 | 120.4 |
C20—O4—Pb1 | 90.8 (5) | C30—C29—H29 | 120.4 |
C39—O5—Pb2ii | 145.0 (5) | C38—C30—C29 | 117.5 (8) |
C39—O5—Pb2 | 85.8 (5) | C38—C30—C31 | 118.4 (8) |
Pb2ii—O5—Pb2 | 112.04 (19) | C29—C30—C31 | 124.1 (8) |
C39—O6—Pb2 | 103.3 (5) | C32—C31—C30 | 121.2 (9) |
N5—O7—Pb2 | 99.8 (5) | C32—C31—H31 | 119.4 |
N5—O8—Pb2 | 98.9 (5) | C30—C31—H31 | 119.4 |
N5—O8—Pb1 | 142.8 (5) | C31—C32—C33 | 121.7 (9) |
Pb2—O8—Pb1 | 110.9 (2) | C31—C32—H32 | 119.1 |
C1—N1—C12 | 118.5 (7) | C33—C32—H32 | 119.1 |
C1—N1—Pb1 | 123.4 (5) | C34—C33—C37 | 117.3 (8) |
C12—N1—Pb1 | 117.5 (5) | C34—C33—C32 | 122.7 (8) |
C10—N2—C11 | 118.5 (6) | C37—C33—C32 | 119.9 (8) |
C10—N2—Pb1 | 121.0 (5) | C35—C34—C33 | 120.4 (8) |
C11—N2—Pb1 | 120.3 (4) | C35—C34—H34 | 119.8 |
C27—N3—C38 | 118.4 (7) | C33—C34—H34 | 119.8 |
C27—N3—Pb2 | 123.2 (5) | C34—C35—C36 | 119.3 (9) |
C38—N3—Pb2 | 117.9 (5) | C34—C35—H35 | 120.4 |
C36—N4—C37 | 117.3 (7) | C36—C35—H35 | 120.4 |
C36—N4—Pb2 | 125.2 (5) | N4—C36—C35 | 123.0 (9) |
C37—N4—Pb2 | 116.7 (5) | N4—C36—H36 | 118.5 |
O9—N5—O8 | 120.6 (8) | C35—C36—H36 | 118.5 |
O9—N5—O7 | 122.0 (8) | N4—C37—C33 | 122.6 (7) |
O8—N5—O7 | 117.1 (7) | N4—C37—C38 | 118.4 (6) |
N1—C1—C2 | 124.2 (8) | C33—C37—C38 | 119.0 (7) |
N1—C1—H1 | 117.9 | N3—C38—C30 | 122.0 (7) |
C2—C1—H1 | 117.9 | N3—C38—C37 | 118.2 (6) |
C3—C2—C1 | 116.9 (8) | C30—C38—C37 | 119.8 (7) |
C3—C2—H2 | 121.6 | O5—C39—O6 | 121.7 (7) |
C1—C2—H2 | 121.6 | O5—C39—C40 | 120.5 (7) |
C2—C3—C4 | 121.6 (8) | O6—C39—C40 | 117.8 (7) |
C2—C3—H3 | 119.2 | C41—C40—C45 | 118.6 (8) |
C4—C3—H3 | 119.2 | C41—C40—C39 | 120.4 (7) |
C3—C4—C12 | 117.2 (8) | C45—C40—C39 | 121.1 (7) |
C3—C4—C5 | 124.2 (8) | C40—C41—C42 | 120.7 (8) |
C12—C4—C5 | 118.7 (8) | C40—C41—H41 | 119.6 |
C6—C5—C4 | 121.9 (8) | C42—C41—H41 | 119.6 |
C6—C5—H5 | 119.1 | C43—C42—C41 | 119.5 (9) |
C4—C5—H5 | 119.1 | C43—C42—H42 | 120.3 |
C5—C6—C7 | 121.5 (8) | C41—C42—H42 | 120.3 |
C5—C6—H6 | 119.3 | C44—C43—C42 | 120.8 (9) |
C7—C6—H6 | 119.3 | C44—C43—H43 | 119.6 |
C8—C7—C11 | 117.0 (7) | C42—C43—H43 | 119.6 |
C8—C7—C6 | 123.6 (8) | C43—C44—C45 | 120.0 (8) |
C11—C7—C6 | 119.4 (8) | C43—C44—H44 | 120.0 |
C9—C8—C7 | 121.4 (7) | C45—C44—H44 | 120.0 |
C9—C8—H8 | 119.3 | C44—C45—C40 | 120.5 (8) |
C7—C8—H8 | 119.3 | C44—C45—H45 | 119.8 |
C8—C9—C10 | 117.3 (7) | C40—C45—H45 | 119.8 |
N3—Pb2—O1—C13 | 122.5 (16) | N3—Pb2—N4—C36 | 179.7 (7) |
O6—Pb2—O1—C13 | 51.9 (16) | O6—Pb2—N4—C36 | −103.8 (7) |
N4—Pb2—O1—C13 | 89.6 (17) | O5ii—Pb2—N4—C36 | 16.0 (6) |
O5ii—Pb2—O1—C13 | −64.9 (16) | O1—Pb2—N4—C36 | −144.1 (6) |
O7—Pb2—O1—C13 | −168.1 (16) | O7—Pb2—N4—C36 | 105.9 (7) |
O8—Pb2—O1—C13 | −155.6 (17) | O8—Pb2—N4—C36 | 115.2 (6) |
O5—Pb2—O1—C13 | 5.3 (16) | O5—Pb2—N4—C36 | −54.0 (6) |
N3—Pb2—O1—Pb1 | −75.5 (3) | N3—Pb2—N4—C37 | −11.4 (5) |
O6—Pb2—O1—Pb1 | −146.0 (2) | O6—Pb2—N4—C37 | 65.1 (5) |
N4—Pb2—O1—Pb1 | −108.4 (4) | O5ii—Pb2—N4—C37 | −175.1 (6) |
O5ii—Pb2—O1—Pb1 | 97.2 (3) | O1—Pb2—N4—C37 | 24.8 (8) |
O7—Pb2—O1—Pb1 | −6.1 (3) | O7—Pb2—N4—C37 | −85.1 (5) |
O8—Pb2—O1—Pb1 | 6.4 (2) | O8—Pb2—N4—C37 | −75.9 (6) |
O5—Pb2—O1—Pb1 | 167.3 (2) | O5—Pb2—N4—C37 | 114.9 (5) |
O2—Pb1—O1—C13 | 1.0 (4) | Pb2—O8—N5—O9 | −174.1 (7) |
O3—Pb1—O1—C13 | −61.7 (5) | Pb1—O8—N5—O9 | 42.4 (15) |
N2—Pb1—O1—C13 | 33.6 (5) | Pb2—O8—N5—O7 | 0.7 (8) |
N1—Pb1—O1—C13 | 85.1 (5) | Pb1—O8—N5—O7 | −142.9 (7) |
O4—Pb1—O1—C13 | −88.1 (5) | Pb2—O7—N5—O9 | 174.0 (7) |
O8—Pb1—O1—C13 | 167.6 (5) | Pb2—O7—N5—O8 | −0.7 (8) |
O3i—Pb1—O1—C13 | 158.9 (4) | C12—N1—C1—C2 | −1.2 (11) |
O2—Pb1—O1—Pb2 | −172.9 (4) | Pb1—N1—C1—C2 | 169.9 (6) |
O3—Pb1—O1—Pb2 | 124.5 (2) | N1—C1—C2—C3 | 0.8 (13) |
N2—Pb1—O1—Pb2 | −140.3 (2) | C1—C2—C3—C4 | 0.1 (13) |
N1—Pb1—O1—Pb2 | −88.8 (2) | C2—C3—C4—C12 | −0.5 (12) |
O4—Pb1—O1—Pb2 | 98.0 (2) | C2—C3—C4—C5 | 177.6 (8) |
O8—Pb1—O1—Pb2 | −6.3 (2) | C3—C4—C5—C6 | −177.1 (9) |
O3i—Pb1—O1—Pb2 | −15.0 (5) | C12—C4—C5—C6 | 0.9 (13) |
O3—Pb1—O2—C13 | 129.0 (5) | C4—C5—C6—C7 | −2.4 (14) |
N2—Pb1—O2—C13 | −153.5 (5) | C5—C6—C7—C8 | 179.9 (9) |
N1—Pb1—O2—C13 | −89.3 (5) | C5—C6—C7—C11 | 1.5 (13) |
O4—Pb1—O2—C13 | 80.2 (5) | C11—C7—C8—C9 | −1.3 (12) |
O1—Pb1—O2—C13 | −1.0 (4) | C6—C7—C8—C9 | −179.7 (8) |
O8—Pb1—O2—C13 | −14.3 (5) | C7—C8—C9—C10 | 0.4 (13) |
O3i—Pb1—O2—C13 | −160.2 (4) | C11—N2—C10—C9 | −0.2 (11) |
O2—Pb1—O3—C20 | −77.5 (4) | Pb1—N2—C10—C9 | −174.4 (6) |
N2—Pb1—O3—C20 | −156.1 (4) | C8—C9—C10—N2 | 0.3 (12) |
N1—Pb1—O3—C20 | −154.8 (4) | C10—N2—C11—C7 | −0.7 (10) |
O4—Pb1—O3—C20 | −0.1 (4) | Pb1—N2—C11—C7 | 173.6 (5) |
O1—Pb1—O3—C20 | −35.0 (5) | C10—N2—C11—C12 | 178.3 (6) |
O8—Pb1—O3—C20 | 50.3 (5) | Pb1—N2—C11—C12 | −7.4 (8) |
O3i—Pb1—O3—C20 | 128.5 (5) | C8—C7—C11—N2 | 1.4 (10) |
O2—Pb1—O4—C20 | 99.6 (5) | C6—C7—C11—N2 | 179.9 (7) |
O3—Pb1—O4—C20 | 0.1 (4) | C8—C7—C11—C12 | −177.6 (6) |
N2—Pb1—O4—C20 | 28.6 (5) | C6—C7—C11—C12 | 0.9 (10) |
N1—Pb1—O4—C20 | 130.3 (5) | C1—N1—C12—C4 | 0.8 (10) |
O1—Pb1—O4—C20 | 149.8 (5) | Pb1—N1—C12—C4 | −170.8 (5) |
O8—Pb1—O4—C20 | −147.3 (5) | C1—N1—C12—C11 | −178.9 (6) |
O3i—Pb1—O4—C20 | −55.2 (5) | Pb1—N1—C12—C11 | 9.5 (8) |
N3—Pb2—O5—C39 | −13.1 (5) | C3—C4—C12—N1 | 0.0 (10) |
O6—Pb2—O5—C39 | 5.2 (4) | C5—C4—C12—N1 | −178.2 (7) |
N4—Pb2—O5—C39 | −69.4 (5) | C3—C4—C12—C11 | 179.7 (6) |
O5ii—Pb2—O5—C39 | −148.9 (5) | C5—C4—C12—C11 | 1.5 (10) |
O1—Pb2—O5—C39 | 82.0 (4) | N2—C11—C12—N1 | −1.7 (9) |
O7—Pb2—O5—C39 | −110.3 (5) | C7—C11—C12—N1 | 177.3 (6) |
O8—Pb2—O5—C39 | 135.7 (6) | N2—C11—C12—C4 | 178.6 (6) |
N3—Pb2—O5—Pb2ii | 135.8 (2) | C7—C11—C12—C4 | −2.4 (10) |
O6—Pb2—O5—Pb2ii | 154.1 (3) | Pb2—O1—C13—O2 | 162.1 (11) |
N4—Pb2—O5—Pb2ii | 79.5 (2) | Pb1—O1—C13—O2 | −1.7 (7) |
O5ii—Pb2—O5—Pb2ii | 0.0 | Pb2—O1—C13—C14 | −17 (2) |
O1—Pb2—O5—Pb2ii | −129.1 (2) | Pb1—O1—C13—C14 | 178.8 (6) |
O7—Pb2—O5—Pb2ii | 38.7 (4) | Pb1—O2—C13—O1 | 2.0 (9) |
O8—Pb2—O5—Pb2ii | −75.4 (5) | Pb1—O2—C13—C14 | −178.4 (5) |
N3—Pb2—O6—C39 | 157.3 (5) | O1—C13—C14—C15 | −4.7 (11) |
N4—Pb2—O6—C39 | 85.6 (5) | O2—C13—C14—C15 | 175.8 (7) |
O5ii—Pb2—O6—C39 | 20.5 (5) | O1—C13—C14—C19 | 177.3 (7) |
O1—Pb2—O6—C39 | −112.1 (5) | O2—C13—C14—C19 | −2.2 (10) |
O7—Pb2—O6—C39 | 131.5 (5) | C19—C14—C15—C16 | −1.9 (11) |
O8—Pb2—O6—C39 | −157.1 (4) | C13—C14—C15—C16 | 180.0 (7) |
O5—Pb2—O6—C39 | −5.4 (4) | C14—C15—C16—C17 | 0.9 (13) |
N3—Pb2—O7—N5 | 99.6 (5) | C15—C16—C17—C18 | 0.1 (13) |
O6—Pb2—O7—N5 | 125.4 (4) | C16—C17—C18—C19 | 0.1 (13) |
N4—Pb2—O7—N5 | 169.1 (5) | C15—C14—C19—C18 | 2.1 (11) |
O5ii—Pb2—O7—N5 | −114.8 (5) | C13—C14—C19—C18 | −179.8 (7) |
O1—Pb2—O7—N5 | 17.0 (5) | C17—C18—C19—C14 | −1.3 (12) |
O8—Pb2—O7—N5 | 0.4 (5) | Pb1—O4—C20—O3 | −0.3 (8) |
O5—Pb2—O7—N5 | −150.2 (4) | Pb1—O4—C20—C21 | 178.6 (6) |
N3—Pb2—O8—N5 | −70.5 (5) | Pb1—O3—C20—O4 | 0.3 (8) |
O6—Pb2—O8—N5 | −113.3 (5) | Pb1—O3—C20—C21 | −178.6 (5) |
N4—Pb2—O8—N5 | −13.4 (6) | O4—C20—C21—C26 | −6.3 (11) |
O5ii—Pb2—O8—N5 | 69.0 (5) | O3—C20—C21—C26 | 172.7 (7) |
O1—Pb2—O8—N5 | −163.3 (6) | O4—C20—C21—C22 | 174.2 (7) |
O7—Pb2—O8—N5 | −0.4 (5) | O3—C20—C21—C22 | −6.8 (10) |
O5—Pb2—O8—N5 | 137.3 (5) | C26—C21—C22—C23 | −1.4 (11) |
N3—Pb2—O8—Pb1 | 86.9 (3) | C20—C21—C22—C23 | 178.1 (7) |
O6—Pb2—O8—Pb1 | 44.1 (4) | C21—C22—C23—C24 | 1.9 (12) |
N4—Pb2—O8—Pb1 | 144.0 (2) | C22—C23—C24—C25 | −1.2 (14) |
O5ii—Pb2—O8—Pb1 | −133.5 (2) | C23—C24—C25—C26 | 0.0 (14) |
O1—Pb2—O8—Pb1 | −5.9 (2) | C24—C25—C26—C21 | 0.4 (14) |
O7—Pb2—O8—Pb1 | 157.0 (4) | C22—C21—C26—C25 | 0.3 (12) |
O5—Pb2—O8—Pb1 | −65.3 (6) | C20—C21—C26—C25 | −179.2 (7) |
O2—Pb1—O8—N5 | 158.2 (10) | C38—N3—C27—C28 | −2.4 (11) |
O3—Pb1—O8—N5 | 37.9 (11) | Pb2—N3—C27—C28 | −173.2 (6) |
N2—Pb1—O8—N5 | −100.5 (10) | N3—C27—C28—C29 | 4.4 (13) |
N1—Pb1—O8—N5 | −126.4 (10) | C27—C28—C29—C30 | −2.3 (13) |
O4—Pb1—O8—N5 | 74.2 (10) | C28—C29—C30—C38 | −1.3 (13) |
O1—Pb1—O8—N5 | 147.1 (11) | C28—C29—C30—C31 | −179.1 (8) |
O3i—Pb1—O8—N5 | −36.7 (10) | C38—C30—C31—C32 | 0.0 (14) |
O2—Pb1—O8—Pb2 | 17.1 (3) | C29—C30—C31—C32 | 177.8 (10) |
O3—Pb1—O8—Pb2 | −103.2 (3) | C30—C31—C32—C33 | −1.3 (15) |
N2—Pb1—O8—Pb2 | 118.4 (3) | C31—C32—C33—C34 | −179.8 (10) |
N1—Pb1—O8—Pb2 | 92.5 (3) | C31—C32—C33—C37 | 1.8 (14) |
O4—Pb1—O8—Pb2 | −66.8 (3) | C37—C33—C34—C35 | −1.7 (14) |
O1—Pb1—O8—Pb2 | 6.0 (2) | C32—C33—C34—C35 | 179.8 (9) |
O3i—Pb1—O8—Pb2 | −177.8 (2) | C33—C34—C35—C36 | 0.9 (15) |
O2—Pb1—N1—C1 | 97.3 (6) | C37—N4—C36—C35 | −1.7 (12) |
O3—Pb1—N1—C1 | 178.4 (5) | Pb2—N4—C36—C35 | 167.1 (6) |
N2—Pb1—N1—C1 | 179.8 (6) | C34—C35—C36—N4 | 0.9 (14) |
O4—Pb1—N1—C1 | 66.6 (8) | C36—N4—C37—C33 | 0.8 (11) |
O1—Pb1—N1—C1 | 47.4 (6) | Pb2—N4—C37—C33 | −169.1 (6) |
O8—Pb1—N1—C1 | −18.9 (6) | C36—N4—C37—C38 | −179.0 (7) |
O3i—Pb1—N1—C1 | −108.3 (6) | Pb2—N4—C37—C38 | 11.1 (9) |
O2—Pb1—N1—C12 | −91.5 (5) | C34—C33—C37—N4 | 0.9 (12) |
O3—Pb1—N1—C12 | −10.4 (6) | C32—C33—C37—N4 | 179.4 (8) |
N2—Pb1—N1—C12 | −9.0 (4) | C34—C33—C37—C38 | −179.3 (8) |
O4—Pb1—N1—C12 | −122.2 (6) | C32—C33—C37—C38 | −0.7 (12) |
O1—Pb1—N1—C12 | −141.4 (5) | C27—N3—C38—C30 | −1.5 (11) |
O8—Pb1—N1—C12 | 152.2 (5) | Pb2—N3—C38—C30 | 169.8 (6) |
O3i—Pb1—N1—C12 | 62.9 (5) | C27—N3—C38—C37 | 178.8 (7) |
O2—Pb1—N2—C10 | −92.3 (5) | Pb2—N3—C38—C37 | −9.9 (9) |
O3—Pb1—N2—C10 | 1.6 (5) | C29—C30—C38—N3 | 3.3 (12) |
N1—Pb1—N2—C10 | −177.5 (6) | C31—C30—C38—N3 | −178.8 (7) |
O4—Pb1—N2—C10 | −20.1 (6) | C29—C30—C38—C37 | −177.0 (7) |
O1—Pb1—N2—C10 | −116.9 (5) | C31—C30—C38—C37 | 1.0 (11) |
O8—Pb1—N2—C10 | 153.6 (5) | N4—C37—C38—N3 | −1.0 (10) |
O3i—Pb1—N2—C10 | 84.5 (5) | C33—C37—C38—N3 | 179.2 (7) |
O2—Pb1—N2—C11 | 93.5 (5) | N4—C37—C38—C30 | 179.2 (7) |
O3—Pb1—N2—C11 | −172.5 (5) | C33—C37—C38—C30 | −0.6 (11) |
N1—Pb1—N2—C11 | 8.3 (4) | Pb2ii—O5—C39—O6 | −132.5 (7) |
O4—Pb1—N2—C11 | 165.7 (4) | Pb2—O5—C39—O6 | −9.0 (7) |
O1—Pb1—N2—C11 | 68.9 (5) | Pb2ii—O5—C39—C40 | 46.1 (13) |
O8—Pb1—N2—C11 | −20.5 (6) | Pb2—O5—C39—C40 | 169.6 (6) |
O3i—Pb1—N2—C11 | −89.7 (5) | Pb2—O6—C39—O5 | 10.6 (9) |
O6—Pb2—N3—C27 | 105.3 (6) | Pb2—O6—C39—C40 | −168.0 (5) |
N4—Pb2—N3—C27 | −178.2 (6) | O5—C39—C40—C41 | 17.3 (11) |
O5ii—Pb2—N3—C27 | −153.4 (5) | O6—C39—C40—C41 | −164.0 (7) |
O1—Pb2—N3—C27 | 17.9 (6) | O5—C39—C40—C45 | −162.5 (7) |
O7—Pb2—N3—C27 | −92.9 (6) | O6—C39—C40—C45 | 16.2 (11) |
O8—Pb2—N3—C27 | −49.0 (6) | C45—C40—C41—C42 | −1.0 (13) |
O5—Pb2—N3—C27 | 119.7 (6) | C39—C40—C41—C42 | 179.1 (8) |
O6—Pb2—N3—C38 | −65.5 (5) | C40—C41—C42—C43 | 1.1 (14) |
N4—Pb2—N3—C38 | 10.9 (5) | C41—C42—C43—C44 | −0.1 (15) |
O5ii—Pb2—N3—C38 | 35.8 (6) | C42—C43—C44—C45 | −0.9 (14) |
O1—Pb2—N3—C38 | −153.0 (5) | C43—C44—C45—C40 | 0.9 (13) |
O7—Pb2—N3—C38 | 96.2 (5) | C41—C40—C45—C44 | 0.0 (12) |
O8—Pb2—N3—C38 | 140.2 (5) | C39—C40—C45—C44 | 179.9 (7) |
O5—Pb2—N3—C38 | −51.1 (6) |
Symmetry codes: (i) −x, −y+1, −z+2; (ii) −x+1, −y+1, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Pb2(C7H5O2)3(NO3)(C12H8N2)2] |
Mr | 1200.13 |
Crystal system, space group | MonoclinicP21/c |
Temperature (K) | 295 |
a, b, c (Å) | 17.2481 (10), 20.6393 (12), 11.5549 (6) |
β (°) | 101.167 (1) |
V (Å3) | 4035.5 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 8.40 |
Crystal size (mm) | 0.13 × 0.09 × 0.08 |
Data collection | |
Diffractometer | Bruker APEX area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2002) |
Tmin, Tmax | 0.417, 0.521 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 20990, 7182, 5090 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.597 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.093, 1.02 |
No. of reflections | 7182 |
No. of parameters | 550 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.23, −0.75 |
Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
Pb1—O2 | 2.363 (5) | Pb2—N3 | 2.454 (6) |
Pb1—O3 | 2.531 (5) | Pb2—O6 | 2.470 (5) |
Pb1—N2 | 2.585 (5) | Pb2—N4 | 2.497 (6) |
Pb1—N1 | 2.666 (6) | Pb2—O5ii | 2.720 (5) |
Pb1—O4 | 2.677 (5) | Pb2—O1 | 2.793 (5) |
Pb1—O1 | 2.802 (5) | Pb2—O7 | 2.802 (6) |
Pb1—O8 | 2.929 (6) | Pb2—O8 | 2.827 (6) |
Pb1—O3i | 3.019 (5) | Pb2—O5 | 2.837 (5) |
Symmetry codes: (i) −x, −y+1, −z+2; (ii) −x+1, −y+1, −z+2. |
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4-Carboxybenzeneboronic acid (Hcbba) has not been so far reported to take part of metal coordination compounds, and only a few organic complexes have been documented in the Cambridge Structural Database (CSD; May 2006 update; Allen, 2002). Zhu & Hu (2006) describe how this ligand can be converted into a benzoate ligand under hydrothermal conditions. In order to understand the coordination chemistry of Hcbba with heavy metal ions, the Pb2+ ion was selected for exploring the assembly of novel structures. The Pb2+ ion can exhibit a variety of coordination modes and possesses a stereochemically active lone pair of electrons, which is important for structural assembly, electron-charge transfer, and physical or chemical properties (Hancock et al., 2004; Nordell et al., 2004; Esteban-Gomez et al., 2005; Panda et al., 2004). Moreover, removing this toxic metal ion through the formation of insoluble complexes is a field of increasing importance (Kurtarun et al., 2005; Magyar et al., 2005). Therefore, the Pb2+/Hcbba/1,10-phenanthroline system was investigated by hydrothermal synthesis and the mixed-anion coordination polymer [Pb2(NO3)(C7H5O2)3(C12H8N2)2]n, (I), which is reported here, was obtained.
The structure consists of a one-dimensional chain in which dimeric units formulated as [Pb2(NO3)(ba)3(phen)2] (ba is benzoate and phen is 1,10-phenanthroline) are linked by benzoate bridges. In the dimeric unit, each one of the two independent Pb atoms is eight-coordinated by one nitrate, three benzoate and one 1,10-phenanthroline ligands in a PbN2O6 chromophore (Fig. 1 and Table 1). However, these two Pb atoms in fact adopt somewhat different coordination environments, i.e. atom Pb1 is coordinated by two N donors from one 1,10-phenanthroline ligand, five O atoms from three benzoate ligands and one O atom from one nitrate ligand, while atom Pb2 is coordinated by two N donors from one 1,10-phenanthroline ligand, four O atoms from three benzoate ligands and two O atoms from one nitrate ligand. Three four-membered Pb2O2 rings (where usually weak Pb···Pb interactions build up) are formed within (and between) dimeric units. There are a variety of Pb···Pb separation distances: Pb1···Pb2, bridged by both nitrate and benzoate ligands, is 4.7420 (4) Å, which is longer than that in catena[bis(µ6-pyrazole-3,5-dicarboxylato)bis(µ2-nitrato)tetraaquatrilead(II)] [4.425 (1) Å; Bentiss et al., 2004]. On the other hand, the Pb1···Pb1 and Pb2···Pb2 separations, bridged by benzoate ligands between dimeric units, are 4.2639 (5) and 4.6083 (6) Å, respectively. The Pb···Pb separation in the three Pb2O2 units is longer than the commonly accepted limit for a weak interaction (4.10 Å; Magyar et al., 2005; Morsali & Mahjoub, 2004a), suggesting that the number and type of ligands present in (I) may not favour the Pb···Pb interaction in the Pb2O2 loops.
The Pb1—N bond lengths are slightly longer than those of Pb2—N, but all are in the normal range. The chelating Pb1—O (except Pb1—O8) distances are significantly shorter than those of Pb2—O. Such coordination geometries around Pb atoms indicate that the lone pair of electrons on atom Pb1 is inactive, while that on Pb2 is active, a very similar case to {[Pb3{N(CH2COO)2}3]2(H2O)5}n (Chow & Mak, 1993). Oddly, only two PbII–benzoate complexes can be found in the CSD, and the carboxylates in these two complexes act in a chelating mode (Yonemura et al., 1997; Hamilton et al., 2004) and with rather similar Pb—O(COO) bond lengths, in contrast to the benzoate ligands in (I), which are converted from 4-carboxybenzeneboronic acid and adopt a bridging–chelating mode with a broad span of Pb—O coordination distances (Table 1).
The nitrate anion is a versatile ligand, which may coordinate to metal atoms using one, two or three O atoms. In the present case it acts as a two-atom chelate to Pb2, while also bridging the dimer (Fig. 1), a situation that is rare in lead(II) complexes and only two examples, (µ2-nitrato-O,O,O')(µ2-nitrato-O,O')tetrakis(1,2-ethylenediamine)dilead(II) dinitrate and bis(µ2-nitrato)-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)(nitrato)lead(II), have been reported (Harrowfield, Miyamae, Skelton et al., 1996; Harrowfield, Miyamae, Shand et al., 1996). The coexistence of both nitrate and carboxylate bridges is also interesting, the former acting as a dimeric linker, while the latter extend these dimeric units into one-dimensional chains (Fig. 2). Only one more example containing both types of bridges has been previously reported (Bentiss et al., 2004).
In general, lone-pair activity of lead(II) and π–π stacking interactions can play a significant role in the structural assembly of the solid state (Morsali & Mahjoub, 2004b). Both factors can be found in the title complex. The former has already been discussed above; regarding the latter, abundant ba–ba, ba–phen and phen–phen stacking interactions occur in neighbouring chains, with a centroid-to-centroid distance range of 3.544 (5)–3.885 (5) Å. These π–π interactions are not perfect face-to-face contacts but rather correspond to the offset type.