Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801006511/cf6059sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801006511/cf6059Isup2.hkl |
CCDC reference: 165633
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.017 Å Some non-H atoms missing
- R factor = 0.040
- wR factor = 0.100
- Data-to-parameter ratio = 10.9
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_320 Alert C Check Hybridisation of C(8) in main residue ? PLAT_320 Alert C Check Hybridisation of C(9A) in main residue ? PLAT_320 Alert C Check Hybridisation of C(9B) in main residue ? PLAT_320 Alert C Check Hybridisation of C(10) in main residue ? PLAT_320 Alert C Check Hybridisation of H(8A) in main residue ? PLAT_320 Alert C Check Hybridisation of H(10A) in main residue ? PLAT_320 Alert C Check Hybridisation of H(10B) in main residue ? PLAT_320 Alert C Check Hybridisation of H(91A) in main residue ? PLAT_320 Alert C Check Hybridisation of H(91B) in main residue ? General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C34 H32 Cu2 I2 N4 O4 Pb1 Atom count from the _atom_site data: C35 H34 Cu2 I2 N4 O4 Pb1 CELLZ_01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C34 H32 Cu2 I2 N4 O4 Pb TEST: Compare cell contents of formula and atom_site data Note that site occupancies missing: assumed 1.0 atom Z*formula cif sites diff C 68.00 70.00 -2.00 H 64.00 68.00 -4.00 Cu 4.00 4.00 0.00 I 4.00 4.00 0.00 N 8.00 8.00 0.00 O 8.00 8.00 0.00 Pb 2.00 2.00 0.00 Difference between formula and atom_site contents detected. ALERT: Large difference may be due to a symmetry error - see SYMMG tests CHEMW_03 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 1148.71 TEST: Calculate formula weight from _atom_site_* Note that site occupancies missing: assumed 1.0 atom mass num sum Pb 207.20 1.00 207.20 I 126.90 2.00 253.81 Cu 63.55 2.00 127.09 O 16.00 4.00 64.00 N 14.01 4.00 56.03 C 12.01 35.00 420.38 H 1.01 34.00 34.27 Calculated formula weight 1162.78 The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
9 Alert Level C = Please check
A solution of N,N'-bis(salicylidene)-1,3-propanediamine (0.585 g, 0.002 mol) was dissolved in 50 ml hot ethanol. Then a solution of CuCl2.2H2O (0.340 g, 0.002 mol) in 30 ml hot water and 10 ml concentrated ammonia was added to it. The green complex [Cu(C17H16N2O2)], which precipitated out after a few hours, was filtered off and dried in an oven at 353 K. 0.344 g (0.001 mol) of this complex was then dissolved in 150 ml dimethylformamide (DMF) at 373 K. In another beaker, PbI2 (0.454 g, 0.001 mol) and 1 g finely ground KI were heated in a mixture of 50 ml acetone and 50 ml DMF until all the PbI2 was dissolved (KPbI3 formation) (Hofmann et al., 1966). The excess KI was filtered off and the two hot solutions were mixed and stirred and allowed to cool for 48 h. The brown crystals formed were filtered off and dried in air.
H atoms were placed geometrically (C—H = 0.93 and 0.97 Å) from their parent C atoms and a riding model was used for all H atoms, with Uiso(H) = 1.3Ueq(C). The disorder of atoms C9A and C9B was refined, with occupancies of 0.564 (16) and 0.436 (16), respectively. The largest peak and deepest hole in the final difference Fourier map were located 0.90 and 0.99 Å from Pb, respectively.
Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1993); cell refinement: CAD-4 EXPRESS; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
[Cu2PbI2(C17H16N2O2)2] | Z = 2 |
Mr = 1148.71 | F(000) = 1084 |
Triclinic, P1 | Dx = 2.228 Mg m−3 |
a = 10.516 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.381 (2) Å | Cell parameters from 25 reflections |
c = 14.558 (3) Å | θ = 4.1–14.3° |
α = 87.23 (2)° | µ = 7.98 mm−1 |
β = 79.73 (1)° | T = 293 K |
γ = 88.54 (1)° | Needle, brown |
V = 1712.2 (5) Å3 | 0.22 × 0.05 × 0.03 mm |
Enraf-Nonius CAD-4 diffractometer | Rint = 0.026 |
ω/2θ scans | θmax = 26.0°, θmin = 1.4° |
Absorption correction: ψ scan (Fair, 1990) | h = −12→1 |
Tmin = 0.626, Tmax = 0.787 | k = −14→14 |
7106 measured reflections | l = −17→17 |
6685 independent reflections | 3 standard reflections every 120 min |
4611 reflections with I > 2σ(I) | intensity decay: 3% |
Refinement on F2 | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.040 | w = 1/[σ2(Fo2) + (0.0651P)2 + 3.3407P], where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.100 | (Δ/σ)max = 0.0001 |
S = 1.01 | Δρmax = 2.48 e Å−3 |
4611 reflections | Δρmin = −2.14 e Å−3 |
423 parameters |
[Cu2PbI2(C17H16N2O2)2] | γ = 88.54 (1)° |
Mr = 1148.71 | V = 1712.2 (5) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.516 (1) Å | Mo Kα radiation |
b = 11.381 (2) Å | µ = 7.98 mm−1 |
c = 14.558 (3) Å | T = 293 K |
α = 87.23 (2)° | 0.22 × 0.05 × 0.03 mm |
β = 79.73 (1)° |
Enraf-Nonius CAD-4 diffractometer | 4611 reflections with I > 2σ(I) |
Absorption correction: ψ scan (Fair, 1990) | Rint = 0.026 |
Tmin = 0.626, Tmax = 0.787 | 3 standard reflections every 120 min |
7106 measured reflections | intensity decay: 3% |
6685 independent reflections |
R[F2 > 2σ(F2)] = 0.040 | 423 parameters |
wR(F2) = 0.100 | H-atom parameters constrained |
S = 1.01 | Δρmax = 2.48 e Å−3 |
4611 reflections | Δρmin = −2.14 e Å−3 |
x | y | z | Uiso*/Ueq | ||
Pb | 0.13254 (3) | 0.25142 (3) | 0.23015 (2) | 0.03534 (11) | |
I1 | 0.35365 (7) | 0.07696 (7) | 0.28096 (6) | 0.0645 (2) | |
I2 | 0.24631 (8) | 0.49910 (6) | 0.17962 (5) | 0.0591 (2) | |
Cu1 | −0.05057 (11) | 0.13745 (10) | 0.06562 (8) | 0.0409 (3) | |
Cu2 | −0.12747 (10) | 0.28835 (10) | 0.42099 (7) | 0.0374 (3) | |
O1 | 0.1188 (6) | 0.2042 (6) | 0.0588 (4) | 0.0471 (16) | |
O2 | −0.0169 (6) | 0.0896 (6) | 0.1877 (4) | 0.0440 (15) | |
O3 | −0.0922 (6) | 0.3224 (6) | 0.2883 (4) | 0.0428 (15) | |
O4 | 0.0579 (5) | 0.2969 (6) | 0.4053 (4) | 0.0423 (15) | |
N1 | −0.0469 (10) | 0.1750 (8) | −0.0684 (6) | 0.057 (2) | |
N2 | −0.2291 (8) | 0.0767 (7) | 0.0960 (6) | 0.048 (2) | |
N3 | −0.3055 (7) | 0.2432 (7) | 0.4187 (5) | 0.0403 (18) | |
N4 | −0.1460 (8) | 0.2944 (7) | 0.5574 (5) | 0.0431 (19) | |
C1 | 0.2064 (10) | 0.2356 (8) | −0.0141 (6) | 0.041 (2) | |
C2 | 0.3324 (10) | 0.2587 (9) | −0.0044 (7) | 0.049 (2) | |
C3 | 0.4218 (12) | 0.2956 (10) | −0.0792 (8) | 0.061 (3) | |
C4 | 0.3919 (13) | 0.3099 (11) | −0.1685 (7) | 0.065 (3) | |
C5 | 0.2716 (13) | 0.2840 (10) | −0.1792 (7) | 0.062 (3) | |
C6 | 0.1729 (11) | 0.2459 (9) | −0.1042 (6) | 0.048 (2) | |
C7 | 0.0515 (12) | 0.2184 (9) | −0.1241 (7) | 0.056 (3) | |
C8 | −0.1641 (14) | 0.1589 (15) | −0.1121 (9) | 0.090 (5) | |
C9A | −0.2607 (18) | 0.0766 (17) | −0.0637 (12) | 0.047 (3) | |
C9B | −0.274 (2) | 0.165 (2) | −0.0610 (16) | 0.047 (3) | |
C10 | −0.3171 (12) | 0.0888 (12) | 0.0267 (9) | 0.070 (3) | |
C11 | −0.2777 (9) | 0.0274 (9) | 0.1744 (7) | 0.049 (2) | |
C12 | −0.2174 (9) | 0.0029 (8) | 0.2553 (7) | 0.043 (2) | |
C13 | −0.2916 (10) | −0.0564 (10) | 0.3332 (8) | 0.056 (3) | |
C14 | −0.2422 (12) | −0.0847 (10) | 0.4112 (8) | 0.061 (3) | |
C15 | −0.1145 (11) | −0.0582 (10) | 0.4129 (8) | 0.058 (3) | |
C16 | −0.0415 (10) | 0.0018 (9) | 0.3392 (7) | 0.049 (2) | |
C17 | −0.0917 (9) | 0.0336 (8) | 0.2585 (7) | 0.041 (2) | |
C18 | −0.1774 (10) | 0.3459 (7) | 0.2326 (6) | 0.040 (2) | |
C19 | −0.1341 (10) | 0.3974 (9) | 0.1442 (7) | 0.049 (2) | |
C20 | −0.2221 (12) | 0.4251 (10) | 0.0844 (8) | 0.057 (3) | |
C21 | −0.3484 (12) | 0.3989 (10) | 0.1108 (9) | 0.063 (3) | |
C22 | −0.3921 (10) | 0.3469 (9) | 0.1959 (8) | 0.051 (3) | |
C23 | −0.3069 (9) | 0.3195 (8) | 0.2583 (7) | 0.044 (2) | |
C24 | −0.3624 (9) | 0.2642 (9) | 0.3485 (8) | 0.050 (3) | |
C25 | −0.3824 (10) | 0.1870 (11) | 0.5021 (7) | 0.058 (3) | |
C26 | −0.3838 (11) | 0.2609 (11) | 0.5846 (8) | 0.061 (3) | |
C27 | −0.2622 (11) | 0.2529 (12) | 0.6229 (7) | 0.063 (3) | |
C28 | −0.0590 (10) | 0.3406 (9) | 0.5952 (7) | 0.046 (2) | |
C29 | 0.0692 (9) | 0.3727 (8) | 0.5541 (6) | 0.041 (2) | |
C30 | 0.1451 (11) | 0.4231 (8) | 0.6102 (7) | 0.048 (2) | |
C31 | 0.2740 (10) | 0.4446 (9) | 0.5791 (7) | 0.049 (2) | |
C32 | 0.3283 (10) | 0.4151 (8) | 0.4902 (7) | 0.048 (2) | |
C33 | 0.2563 (9) | 0.3670 (8) | 0.4327 (7) | 0.043 (2) | |
C34 | 0.1259 (9) | 0.3440 (8) | 0.4619 (6) | 0.037 (2) | |
H2 | 0.3561 | 0.2489 | 0.0541 | 0.059* | |
H3 | 0.5050 | 0.3116 | −0.0704 | 0.073* | |
H4 | 0.4530 | 0.3365 | −0.2189 | 0.078* | |
H5 | 0.2516 | 0.2914 | −0.2390 | 0.074* | |
H7 | 0.0407 | 0.2336 | −0.1856 | 0.067* | |
H8A | −0.2061 | 0.2352 | −0.1176 | 0.108* | |
H8B | −0.1351 | 0.1327 | −0.1749 | 0.108* | |
H9A1 | −0.3298 | 0.0767 | −0.0998 | 0.056* | |
H9A2 | −0.2208 | −0.0012 | −0.0675 | 0.056* | |
H9B1 | −0.3361 | 0.1524 | −0.1014 | 0.056* | |
H9B2 | −0.2859 | 0.2454 | −0.0425 | 0.056* | |
H10A | −0.3840 | 0.0304 | 0.0430 | 0.083* | |
H10B | −0.3992 | 0.1202 | 0.0580 | 0.083* | |
H11 | −0.3631 | 0.0042 | 0.1804 | 0.059* | |
H13 | −0.3761 | −0.0764 | 0.3309 | 0.068* | |
H14 | −0.2930 | −0.1215 | 0.4629 | 0.073* | |
H15 | −0.0782 | −0.0815 | 0.4648 | 0.070* | |
H16 | 0.0427 | 0.0218 | 0.3427 | 0.058* | |
H19 | −0.0468 | 0.4133 | 0.1249 | 0.059* | |
H20 | −0.1935 | 0.4619 | 0.0262 | 0.068* | |
H21 | −0.4057 | 0.4166 | 0.0701 | 0.076* | |
H22 | −0.4792 | 0.3292 | 0.2132 | 0.061* | |
H24 | −0.4482 | 0.2418 | 0.3560 | 0.060* | |
H25A | −0.3459 | 0.1098 | 0.5141 | 0.070* | |
H25B | −0.4701 | 0.1770 | 0.4920 | 0.070* | |
H26A | −0.3995 | 0.3423 | 0.5664 | 0.073* | |
H26B | −0.4548 | 0.2368 | 0.6334 | 0.073* | |
H27A | −0.2730 | 0.2987 | 0.6784 | 0.075* | |
H27B | −0.2475 | 0.1716 | 0.6420 | 0.075* | |
H28 | −0.0832 | 0.3551 | 0.6583 | 0.055* | |
H30 | 0.1077 | 0.4428 | 0.6704 | 0.057* | |
H31 | 0.3234 | 0.4784 | 0.6175 | 0.059* | |
H32 | 0.4157 | 0.4281 | 0.4687 | 0.057* | |
H33 | 0.2956 | 0.3491 | 0.3725 | 0.051* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb | 0.03396 (2) | 0.0422 (2) | 0.0312 (2) | −0.0020 (1) | −0.0089 (1) | −0.0038 (1) |
I1 | 0.0458 (4) | 0.0576 (4) | 0.0926 (6) | 0.0047 (4) | −0.0209 (4) | −0.0024 (3) |
I2 | 0.0759 (5) | 0.0518 (4) | 0.0487 (4) | 0.0049 (3) | −0.0090 (4) | −0.0137 (4) |
Cu1 | 0.0432 (6) | 0.0428 (6) | 0.0409 (6) | −0.0018 (5) | −0.0186 (5) | −0.0043 (5) |
Cu2 | 0.0337 (6) | 0.0473 (6) | 0.0322 (5) | −0.0022 (5) | −0.0072 (4) | −0.0053 (5) |
O1 | 0.044 (4) | 0.065 (4) | 0.034 (3) | 0.002 (3) | −0.010 (3) | −0.013 (3) |
O2 | 0.035 (3) | 0.052 (4) | 0.046 (4) | 0.008 (3) | −0.010 (3) | −0.014 (3) |
O3 | 0.032 (3) | 0.056 (4) | 0.044 (4) | 0.004 (3) | −0.015 (3) | −0.003 (3) |
O4 | 0.021 (3) | 0.072 (4) | 0.034 (3) | −0.009 (3) | −0.001 (2) | −0.010 (3) |
N1 | 0.069 (6) | 0.064 (6) | 0.045 (5) | 0.001 (4) | −0.028 (5) | −0.007 (5) |
N2 | 0.040 (5) | 0.051 (5) | 0.059 (5) | −0.007 (4) | −0.021 (4) | 0.000 (4) |
N3 | 0.026 (4) | 0.050 (5) | 0.046 (4) | −0.012 (4) | −0.003 (3) | −0.016 (3) |
N4 | 0.050 (5) | 0.044 (5) | 0.033 (4) | 0.000 (3) | −0.002 (4) | −0.001 (4) |
C1 | 0.052 (6) | 0.039 (5) | 0.034 (5) | −0.006 (4) | −0.007 (4) | −0.003 (4) |
C2 | 0.051 (6) | 0.060 (7) | 0.036 (5) | 0.002 (5) | −0.007 (4) | −0.004 (5) |
C3 | 0.062 (7) | 0.062 (7) | 0.053 (6) | −0.009 (5) | 0.008 (5) | −0.010 (6) |
C4 | 0.078 (9) | 0.070 (8) | 0.039 (6) | −0.004 (5) | 0.015 (6) | −0.013 (7) |
C5 | 0.090 (9) | 0.060 (7) | 0.031 (5) | −0.001 (5) | −0.001 (6) | −0.005 (6) |
C6 | 0.068 (7) | 0.044 (5) | 0.033 (5) | −0.002 (4) | −0.015 (5) | −0.005 (5) |
C7 | 0.082 (8) | 0.051 (6) | 0.041 (6) | 0.001 (5) | −0.027 (6) | 0.010 (6) |
C8 | 0.096 (11) | 0.122 (12) | 0.067 (8) | 0.028 (8) | −0.058 (8) | −0.032 (9) |
C9A | 0.057 (11) | 0.030 (10) | 0.070 (9) | −0.015 (7) | −0.039 (8) | 0.010 (8) |
C9B | 0.057 (14) | 0.030 (11) | 0.070 (10) | −0.015 (9) | −0.039 (7) | 0.010 (8) |
C10 | 0.054 (7) | 0.080 (8) | 0.085 (9) | 0.005 (7) | −0.045 (7) | −0.003 (6) |
C11 | 0.032 (5) | 0.053 (6) | 0.062 (7) | −0.004 (5) | −0.005 (5) | −0.011 (4) |
C12 | 0.037 (5) | 0.033 (5) | 0.061 (6) | −0.005 (4) | −0.014 (5) | −0.007 (4) |
C13 | 0.039 (6) | 0.063 (7) | 0.064 (7) | 0.004 (6) | −0.002 (5) | −0.016 (5) |
C14 | 0.064 (8) | 0.055 (7) | 0.058 (7) | 0.006 (5) | 0.008 (6) | −0.019 (6) |
C15 | 0.051 (7) | 0.058 (7) | 0.066 (7) | 0.012 (6) | −0.015 (6) | −0.011 (5) |
C16 | 0.049 (6) | 0.052 (6) | 0.046 (6) | 0.002 (5) | −0.013 (5) | −0.013 (5) |
C17 | 0.039 (5) | 0.034 (5) | 0.050 (5) | 0.003 (4) | −0.013 (4) | −0.005 (4) |
C18 | 0.054 (6) | 0.031 (5) | 0.042 (5) | −0.008 (4) | −0.025 (4) | 0.007 (4) |
C19 | 0.049 (6) | 0.055 (6) | 0.046 (6) | −0.002 (5) | −0.016 (5) | 0.006 (5) |
C20 | 0.067 (8) | 0.059 (7) | 0.049 (6) | −0.003 (5) | −0.023 (6) | 0.008 (6) |
C21 | 0.074 (9) | 0.060 (7) | 0.066 (8) | −0.010 (6) | −0.042 (7) | 0.021 (6) |
C22 | 0.037 (5) | 0.061 (7) | 0.063 (7) | −0.023 (5) | −0.025 (5) | 0.012 (5) |
C23 | 0.041 (6) | 0.046 (5) | 0.052 (6) | −0.016 (4) | −0.025 (5) | 0.003 (4) |
C24 | 0.027 (5) | 0.057 (6) | 0.071 (7) | −0.014 (5) | −0.019 (5) | −0.003 (4) |
C25 | 0.040 (6) | 0.073 (8) | 0.058 (7) | −0.002 (6) | 0.002 (5) | −0.022 (5) |
C26 | 0.050 (7) | 0.072 (8) | 0.056 (7) | −0.007 (6) | 0.006 (5) | −0.025 (6) |
C27 | 0.059 (7) | 0.083 (8) | 0.042 (6) | −0.001 (6) | 0.002 (5) | −0.015 (6) |
C28 | 0.052 (6) | 0.051 (6) | 0.032 (5) | −0.004 (4) | −0.000 (4) | −0.001 (5) |
C29 | 0.048 (6) | 0.037 (5) | 0.039 (5) | 0.001 (4) | −0.013 (4) | −0.001 (4) |
C30 | 0.069 (7) | 0.041 (5) | 0.039 (5) | −0.005 (4) | −0.023 (5) | 0.001 (5) |
C31 | 0.055 (6) | 0.049 (6) | 0.050 (6) | −0.008 (5) | −0.024 (5) | −0.007 (5) |
C32 | 0.052 (6) | 0.043 (6) | 0.053 (6) | −0.006 (5) | −0.018 (5) | −0.010 (5) |
C33 | 0.040 (5) | 0.046 (5) | 0.044 (5) | −0.002 (4) | −0.011 (4) | −0.006 (4) |
C34 | 0.035 (5) | 0.038 (5) | 0.041 (5) | 0.000 (4) | −0.018 (4) | 0.001 (4) |
Pb—O1 | 2.607 (6) | C9B—H9B1 | 0.970 |
Pb—O2 | 2.616 (6) | C9B—H9B2 | 0.970 |
Pb—O3 | 2.492 (6) | C10—H10A | 0.970 |
Pb—O4 | 2.603 (6) | C10—H10B | 0.970 |
Pb—I1 | 3.1831 (9) | C11—C12 | 1.446 (14) |
Pb—I2 | 3.0945 (9) | C11—H11 | 0.930 |
Pb—Cu1 | 3.6331 (12) | C12—C17 | 1.385 (13) |
Pb—Cu2 | 3.5662 (12) | C12—C13 | 1.410 (14) |
Cu1—O1 | 1.938 (6) | C13—C14 | 1.353 (16) |
Cu1—O2 | 1.924 (6) | C13—H13 | 0.930 |
Cu2—O3 | 1.924 (6) | C14—C15 | 1.389 (15) |
Cu2—O4 | 1.926 (5) | C14—H14 | 0.930 |
Cu1—N1 | 1.970 (9) | C15—C16 | 1.367 (14) |
Cu1—N2 | 1.985 (8) | C15—H15 | 0.930 |
Cu2—N3 | 1.961 (7) | C16—C17 | 1.401 (13) |
Cu2—N4 | 1.966 (7) | C16—H16 | 0.930 |
O1—C1 | 1.317 (11) | C18—C23 | 1.382 (14) |
O2—C17 | 1.327 (11) | C18—C19 | 1.393 (14) |
O3—C18 | 1.326 (10) | C19—C20 | 1.400 (14) |
O4—C34 | 1.324 (10) | C19—H19 | 0.930 |
N1—C7 | 1.289 (14) | C20—C21 | 1.352 (17) |
N1—C8 | 1.503 (14) | C20—H20 | 0.930 |
N2—C11 | 1.275 (13) | C21—C22 | 1.356 (16) |
N2—C10 | 1.485 (13) | C21—H21 | 0.930 |
N3—C24 | 1.283 (12) | C22—C23 | 1.405 (13) |
N3—C25 | 1.462 (12) | C22—H22 | 0.930 |
N4—C28 | 1.283 (13) | C23—C24 | 1.459 (15) |
N4—C27 | 1.482 (13) | C24—H24 | 0.930 |
C1—C2 | 1.390 (14) | C25—C26 | 1.497 (15) |
C1—C6 | 1.417 (13) | C25—H25A | 0.970 |
C2—C3 | 1.362 (14) | C25—H25B | 0.970 |
C2—H2 | 0.930 | C26—C27 | 1.483 (16) |
C3—C4 | 1.392 (16) | C26—H26A | 0.970 |
C3—H3 | 0.930 | C26—H26B | 0.970 |
C4—C5 | 1.344 (17) | C27—H27A | 0.970 |
C4—H4 | 0.930 | C27—H27B | 0.970 |
C5—C6 | 1.425 (15) | C28—C29 | 1.423 (14) |
C5—H5 | 0.930 | C28—H28 | 0.930 |
C6—C7 | 1.404 (15) | C29—C30 | 1.391 (13) |
C7—H7 | 0.930 | C29—C34 | 1.417 (13) |
C8—C9B | 1.26 (3) | C30—C31 | 1.374 (15) |
C8—C9A | 1.46 (2) | C30—H30 | 0.930 |
C8—H8A | 0.970 | C31—C32 | 1.372 (14) |
C8—H8B | 0.970 | C31—H31 | 0.930 |
C9A—C10 | 1.36 (2) | C32—C33 | 1.366 (13) |
C9A—C9B | 1.01 (3) | C32—H32 | 0.930 |
C9A—H9A1 | 0.970 | C33—C34 | 1.389 (13) |
C9A—H9A2 | 0.970 | C33—H33 | 0.930 |
C9B—C10 | 1.51 (3) | ||
O1—Pb—O2 | 56.7 (2) | C10—C9A—C8 | 122.9 (16) |
O3—Pb—O4 | 59.31 (18) | C10—C9A—H9A1 | 106.6 |
O3—Pb—O1 | 101.2 (2) | C8—C9A—H9A1 | 106.6 |
O4—Pb—O1 | 159.6 (2) | C10—C9A—H9A2 | 106.6 |
O3—Pb—O2 | 74.8 (2) | C8—C9A—H9A2 | 106.6 |
O4—Pb—O2 | 108.39 (19) | H9A1—C9A—H9A2 | 106.6 |
O3—Pb—I2 | 95.52 (15) | C8—C9B—C10 | 124.7 (19) |
O4—Pb—I2 | 93.01 (15) | C8—C9B—H9B1 | 105.7 |
O1—Pb—I2 | 95.08 (15) | C10—C9B—H9B1 | 105.7 |
O2—Pb—I2 | 146.22 (14) | C8—C9B—H9B2 | 105.7 |
O3—Pb—I1 | 142.81 (14) | C10—C9B—H9B2 | 105.7 |
O4—Pb—I1 | 91.15 (14) | H9B1—C9B—H9B2 | 106.1 |
O1—Pb—I1 | 103.75 (16) | C9A—C10—N2 | 115.8 (12) |
O2—Pb—I1 | 96.58 (15) | C9A—C10—C9B | 40.9 (12) |
I2—Pb—I1 | 109.13 (3) | N2—C10—C9B | 117.7 (13) |
O3—Pb—Cu2 | 31.05 (14) | C9A—C10—H10A | 108.3 |
O4—Pb—Cu2 | 31.78 (12) | N2—C10—H10A | 108.3 |
O1—Pb—Cu2 | 127.85 (15) | C9B—C10—H10A | 131.9 |
O2—Pb—Cu2 | 82.73 (13) | C9A—C10—H10B | 134.89 |
I2—Pb—Cu2 | 105.77 (3) | N2—C10—H10B | 108.3 |
I1—Pb—Cu2 | 112.99 (3) | C9B—C10—H10B | 107.75 |
O3—Pb—Cu1 | 76.67 (14) | H10A—C10—H10B | 66.06 |
O4—Pb—Cu1 | 129.57 (13) | N2—C11—C12 | 128.4 (9) |
O1—Pb—Cu1 | 30.99 (14) | N2—C11—H11 | 115.8 |
O2—Pb—Cu1 | 30.72 (13) | C12—C11—H11 | 115.8 |
I2—Pb—Cu1 | 115.92 (3) | C17—C12—C13 | 119.6 (9) |
I1—Pb—Cu1 | 114.07 (3) | C17—C12—C11 | 123.1 (9) |
Cu2—Pb—Cu1 | 98.32 (3) | C13—C12—C11 | 117.3 (9) |
O2—Cu1—O1 | 80.0 (3) | C14—C13—C12 | 121.2 (10) |
O2—Cu1—N1 | 167.8 (4) | C14—C13—H13 | 119.4 |
O1—Cu1—N1 | 91.2 (3) | C12—C13—H13 | 119.4 |
O2—Cu1—N2 | 91.8 (3) | C13—C14—C15 | 119.3 (10) |
O1—Cu1—N2 | 169.9 (3) | C13—C14—H14 | 120.4 |
N1—Cu1—N2 | 97.7 (4) | C15—C14—H14 | 120.4 |
O2—Cu1—Pb | 44.0 (2) | C16—C15—C14 | 120.7 (10) |
O1—Cu1—Pb | 43.83 (18) | C16—C15—H15 | 119.7 |
N1—Cu1—Pb | 131.5 (3) | C14—C15—H15 | 119.7 |
N2—Cu1—Pb | 126.1 (3) | C15—C16—C17 | 120.8 (10) |
O3—Cu2—O4 | 81.9 (3) | C15—C16—H16 | 119.6 |
O3—Cu2—N3 | 92.5 (3) | C17—C16—H16 | 119.6 |
O4—Cu2—N3 | 165.2 (3) | O2—C17—C12 | 122.6 (9) |
O3—Cu2—N4 | 165.2 (3) | O2—C17—C16 | 119.1 (9) |
O4—Cu2—N4 | 91.8 (3) | C12—C17—C16 | 118.3 (9) |
N3—Cu2—N4 | 96.7 (3) | O3—C18—C23 | 122.6 (9) |
O3—Cu2—Pb | 41.92 (18) | O3—C18—C19 | 118.5 (9) |
O4—Cu2—Pb | 45.37 (18) | C23—C18—C19 | 118.9 (9) |
N3—Cu2—Pb | 123.4 (2) | C18—C19—C20 | 119.8 (10) |
N4—Cu2—Pb | 136.2 (2) | C18—C19—H19 | 120.07 |
C1—O1—Cu1 | 130.5 (6) | C20—C19—H19 | 120.07 |
C1—O1—Pb | 123.8 (6) | C21—C20—C19 | 120.5 (11) |
Cu1—O1—Pb | 105.2 (3) | C21—C20—H20 | 119.7 |
C17—O2—Cu1 | 130.0 (6) | C19—C20—H20 | 119.7 |
C17—O2—Pb | 116.7 (5) | C20—C21—C22 | 120.5 (10) |
Cu1—O2—Pb | 105.3 (3) | C20—C21—H21 | 119.7 |
C18—O3—Cu2 | 127.3 (6) | C22—C21—H21 | 119.7 |
C18—O3—Pb | 123.0 (6) | C21—C22—C23 | 120.5 (10) |
Cu2—O3—Pb | 107.0 (2) | C21—C22—H22 | 119.8 |
C34—O4—Cu2 | 127.2 (6) | C23—C22—H22 | 119.8 |
C34—O4—Pb | 127.9 (5) | C18—C23—C22 | 119.7 (10) |
Cu2—O4—Pb | 102.9 (2) | C18—C23—C24 | 123.5 (8) |
C7—N1—C8 | 114.5 (10) | C22—C23—C24 | 116.8 (9) |
C7—N1—Cu1 | 124.0 (7) | N3—C24—C23 | 127.0 (9) |
C8—N1—Cu1 | 121.4 (8) | N3—C24—H24 | 116.5 |
C11—N2—C10 | 115.0 (9) | C23—C24—H24 | 116.5 |
C11—N2—Cu1 | 124.0 (7) | N3—C25—C26 | 110.1 (9) |
C10—N2—Cu1 | 121.0 (8) | N3—C25—H25A | 109.6 |
C24—N3—C25 | 116.7 (8) | C26—C25—H25A | 109.6 |
C24—N3—Cu2 | 123.7 (7) | N3—C25—H25B | 109.6 |
C25—N3—Cu2 | 119.5 (6) | C26—C25—H25B | 109.6 |
C28—N4—C27 | 115.5 (8) | H25A—C25—H25B | 108.2 |
C28—N4—Cu2 | 121.2 (7) | C27—C26—C25 | 113.9 (10) |
C27—N4—Cu2 | 123.2 (7) | C27—C26—H26A | 108.8 |
O1—C1—C2 | 121.1 (8) | C25—C26—H26A | 108.8 |
O1—C1—C6 | 120.0 (9) | C27—C26—H26B | 108.8 |
C2—C1—C6 | 118.9 (9) | C25—C26—H26B | 108.8 |
C3—C2—C1 | 121.2 (10) | H26A—C26—H26B | 107.7 |
C3—C2—H2 | 119.4 | C26—C27—N4 | 114.6 (9) |
C1—C2—H2 | 119.4 | C26—C27—H27A | 108.58 |
C2—C3—C4 | 121.6 (12) | N4—C27—H27A | 108.54 |
C2—C3—H3 | 119.2 | C26—C27—H27B | 108.58 |
C4—C3—H3 | 119.2 | N4—C27—H27B | 108.54 |
C5—C4—C3 | 117.8 (10) | H27A—C27—H27B | 107.49 |
C5—C4—H4 | 121.1 | N4—C28—C29 | 129.0 (9) |
C3—C4—H4 | 121.1 | N4—C28—H28 | 115.5 |
C4—C5—C6 | 123.6 (10) | C29—C28—H28 | 115.5 |
C4—C5—H5 | 118.2 | C30—C29—C34 | 119.1 (9) |
C6—C5—H5 | 118.2 | C30—C29—C28 | 118.1 (9) |
C7—C6—C1 | 124.4 (10) | C34—C29—C28 | 122.5 (9) |
C7—C6—C5 | 118.7 (9) | C31—C30—C29 | 122.0 (9) |
C1—C6—C5 | 116.9 (10) | C31—C30—H30 | 119.0 |
N1—C7—C6 | 128.5 (9) | C29—C30—H30 | 119.0 |
N1—C7—H7 | 115.7 | C30—C31—C32 | 118.5 (9) |
C6—C7—H7 | 115.7 | C30—C31—H31 | 120.7 |
C9B—C8—C9A | 43.0 (14) | C32—C31—H31 | 120.7 |
C9B—C8—N1 | 118.2 (15) | C33—C32—C31 | 121.1 (10) |
C9A—C8—N1 | 117.0 (11) | C33—C32—H32 | 119.5 |
C9B—C8—H8A | 67.21 | C31—C32—H32 | 119.5 |
C9A—C8—H8A | 108.0 | C32—C33—C34 | 121.7 (9) |
N1—C8—H8A | 108.0 | C32—C33—H33 | 119.1 |
C9B—C8—H8B | 132.3 | C34—C33—H33 | 119.1 |
C9A—C8—H8B | 108.0 | O4—C34—C33 | 120.7 (8) |
N1—C8—H8B | 108.0 | O4—C34—C29 | 121.7 (8) |
H8A—C8—H8B | 107.3 | C33—C34—C29 | 117.6 (8) |
O3—Pb—Cu1—O2 | −82.7 (3) | Cu1—Pb—O4—Cu2 | −12.1 (4) |
O4—Pb—Cu1—O2 | −53.9 (3) | O2—Cu1—N1—C7 | −39 (2) |
O1—Pb—Cu1—O2 | 135.8 (4) | O1—Cu1—N1—C7 | 5.1 (9) |
I2—Pb—Cu1—O2 | −172.4 (3) | N2—Cu1—N1—C7 | −179.6 (9) |
I1—Pb—Cu1—O2 | 59.6 (3) | Pb—Cu1—N1—C7 | 24.3 (11) |
Cu2—Pb—Cu1—O2 | −60.3 (3) | O2—Cu1—N1—C8 | 143.1 (15) |
O3—Pb—Cu1—O1 | 141.5 (3) | O1—Cu1—N1—C8 | −173.1 (10) |
O4—Pb—Cu1—O1 | 170.3 (4) | N2—Cu1—N1—C8 | 2.2 (11) |
O2—Pb—Cu1—O1 | −135.8 (4) | Pb—Cu1—N1—C8 | −153.8 (9) |
I2—Pb—Cu1—O1 | 51.8 (3) | O2—Cu1—N2—C11 | −0.1 (9) |
I1—Pb—Cu1—O1 | −76.2 (3) | O1—Cu1—N2—C11 | −36 (2) |
Cu2—Pb—Cu1—O1 | 163.9 (3) | N1—Cu1—N2—C11 | 172.2 (9) |
O3—Pb—Cu1—N1 | 113.1 (4) | Pb—Cu1—N2—C11 | −29.9 (10) |
O4—Pb—Cu1—N1 | 141.9 (4) | O2—Cu1—N2—C10 | 178.8 (9) |
O1—Pb—Cu1—N1 | −28.4 (5) | O1—Cu1—N2—C10 | 143.3 (17) |
O2—Pb—Cu1—N1 | −164.2 (5) | N1—Cu1—N2—C10 | −8.9 (9) |
I2—Pb—Cu1—N1 | 23.4 (4) | Pb—Cu1—N2—C10 | 149.0 (7) |
I1—Pb—Cu1—N1 | −104.6 (4) | O3—Cu2—N3—C24 | −13.1 (8) |
Cu2—Pb—Cu1—N1 | 135.5 (4) | O4—Cu2—N3—C24 | −80.1 (15) |
O3—Pb—Cu1—N2 | −37.0 (3) | N4—Cu2—N3—C24 | 155.3 (8) |
O4—Pb—Cu1—N2 | −8.2 (4) | Pb—Cu2—N3—C24 | −43.4 (9) |
O1—Pb—Cu1—N2 | −178.6 (4) | O3—Cu2—N3—C25 | 169.9 (7) |
O2—Pb—Cu1—N2 | 45.6 (4) | O4—Cu2—N3—C25 | 102.9 (13) |
I2—Pb—Cu1—N2 | −126.7 (3) | N4—Cu2—N3—C25 | −21.7 (8) |
I1—Pb—Cu1—N2 | 105.2 (3) | Pb—Cu2—N3—C25 | 139.6 (7) |
Cu2—Pb—Cu1—N2 | −14.6 (3) | O3—Cu2—N4—C28 | −39.9 (17) |
O4—Pb—Cu2—O3 | 143.4 (4) | O4—Cu2—N4—C28 | 24.3 (8) |
O1—Pb—Cu2—O3 | −35.6 (4) | N3—Cu2—N4—C28 | −167.9 (8) |
O2—Pb—Cu2—O3 | −72.6 (3) | Pb—Cu2—N4—C28 | 34.9 (9) |
I2—Pb—Cu2—O3 | 74.0 (3) | O3—Cu2—N4—C27 | 136.7 (12) |
I1—Pb—Cu2—O3 | −166.7 (3) | O4—Cu2—N4—C27 | −159.1 (8) |
Cu1—Pb—Cu2—O3 | −46.0 (3) | N3—Cu2—N4—C27 | 8.8 (9) |
O3—Pb—Cu2—O4 | −143.4 (4) | Pb—Cu2—N4—C27 | −148.5 (7) |
O1—Pb—Cu2—O4 | −179.0 (3) | Cu1—O1—C1—C2 | −166.3 (7) |
O2—Pb—Cu2—O4 | 144.4 (3) | Pb—O1—C1—C2 | 23.0 (12) |
I2—Pb—Cu2—O4 | −69.4 (3) | Cu1—O1—C1—C6 | 13.4 (13) |
I1—Pb—Cu2—O4 | 50.0 (3) | Pb—O1—C1—C6 | −157.2 (7) |
Cu1—Pb—Cu2—O4 | 170.6 (3) | O1—C1—C2—C3 | −177.4 (10) |
O3—Pb—Cu2—N3 | 49.0 (4) | C6—C1—C2—C3 | 2.8 (16) |
O4—Pb—Cu2—N3 | −167.6 (4) | C1—C2—C3—C4 | −1.0 (18) |
O1—Pb—Cu2—N3 | 13.4 (4) | C2—C3—C4—C5 | −1.3 (18) |
O2—Pb—Cu2—N3 | −23.6 (3) | C3—C4—C5—C6 | 1.7 (19) |
I2—Pb—Cu2—N3 | 123.0 (3) | O1—C1—C6—C7 | −3.5 (15) |
I1—Pb—Cu2—N3 | −117.7 (3) | C2—C1—C6—C7 | 176.2 (10) |
Cu1—Pb—Cu2—N3 | 3.0 (3) | O1—C1—C6—C5 | 177.9 (9) |
O3—Pb—Cu2—N4 | −158.4 (5) | C2—C1—C6—C5 | −2.3 (14) |
O4—Pb—Cu2—N4 | −15.0 (4) | C4—C5—C6—C7 | −178.5 (11) |
O1—Pb—Cu2—N4 | 166.0 (4) | C4—C5—C6—C1 | 0.1 (17) |
O2—Pb—Cu2—N4 | 129.1 (4) | C8—N1—C7—C6 | 179.4 (12) |
I2—Pb—Cu2—N4 | −84.3 (3) | Cu1—N1—C7—C6 | 1.1 (17) |
I1—Pb—Cu2—N4 | 35.0 (3) | C1—C6—C7—N1 | −3.8 (18) |
Cu1—Pb—Cu2—N4 | 155.6 (3) | C5—C6—C7—N1 | 174.7 (11) |
O2—Cu1—O1—C1 | 158.6 (9) | C7—N1—C8—C9B | −152.6 (18) |
N1—Cu1—O1—C1 | −12.8 (9) | Cu1—N1—C8—C9B | 26 (2) |
N2—Cu1—O1—C1 | −165.3 (16) | C7—N1—C8—C9A | 160.2 (13) |
Pb—Cu1—O1—C1 | −171.9 (10) | Cu1—N1—C8—C9A | −21.1 (17) |
O2—Cu1—O1—Pb | −29.4 (3) | C9B—C8—C9A—C10 | −49 (2) |
N1—Cu1—O1—Pb | 159.1 (4) | N1—C8—C9A—C10 | 54 (2) |
N2—Cu1—O1—Pb | 7 (2) | C9A—C8—C9B—C10 | 43.0 (18) |
O3—Pb—O1—C1 | 134.5 (7) | N1—C8—C9B—C10 | −55 (3) |
O4—Pb—O1—C1 | 150.8 (7) | C8—C9A—C10—N2 | −62 (2) |
O2—Pb—O1—C1 | −162.2 (8) | C8—C9A—C10—C9B | 40.8 (19) |
I2—Pb—O1—C1 | 37.8 (7) | C11—N2—C10—C9A | −145.1 (14) |
I1—Pb—O1—C1 | −73.3 (7) | Cu1—N2—C10—C9A | 35.8 (17) |
Cu2—Pb—O1—C1 | 152.3 (6) | C11—N2—C10—C9B | 169.5 (13) |
Cu1—Pb—O1—C1 | 172.6 (9) | Cu1—N2—C10—C9B | −7.9 (18) |
O3—Pb—O1—Cu1 | −38.1 (3) | C8—C9B—C10—C9A | −52 (2) |
O4—Pb—O1—Cu1 | −21.8 (8) | C8—C9B—C10—N2 | 45 (3) |
O2—Pb—O1—Cu1 | 25.2 (2) | C10—N2—C11—C12 | 179.8 (11) |
I2—Pb—O1—Cu1 | −134.8 (3) | Cu1—N2—C11—C12 | −1.2 (16) |
I1—Pb—O1—Cu1 | 114.1 (3) | N2—C11—C12—C17 | 1.0 (17) |
Cu2—Pb—O1—Cu1 | −20.3 (4) | N2—C11—C12—C13 | −178.1 (11) |
O1—Cu1—O2—C17 | 176.2 (8) | C17—C12—C13—C14 | −0.4 (16) |
N1—Cu1—O2—C17 | −138.9 (15) | C11—C12—C13—C14 | 178.8 (10) |
N2—Cu1—O2—C17 | 2.1 (8) | C12—C13—C14—C15 | −2.2 (18) |
Pb—Cu1—O2—C17 | 146.8 (9) | C13—C14—C15—C16 | 3.8 (18) |
O1—Cu1—O2—Pb | 29.3 (3) | C14—C15—C16—C17 | −2.8 (17) |
N1—Cu1—O2—Pb | 74.0 (16) | Cu1—O2—C17—C12 | −2.8 (14) |
N2—Cu1—O2—Pb | −144.7 (3) | Pb—O2—C17—C12 | 141.8 (7) |
O3—Pb—O2—C17 | −62.6 (6) | Cu1—O2—C17—C16 | 176.0 (7) |
O4—Pb—O2—C17 | −13.0 (6) | Pb—O2—C17—C16 | −40.2 (11) |
O1—Pb—O2—C17 | −177.4 (7) | C13—C12—C17—O2 | −179.9 (9) |
I2—Pb—O2—C17 | −139.6 (5) | C11—C12—C17—O2 | 1.0 (15) |
I1—Pb—O2—C17 | 80.5 (6) | C13—C12—C17—C16 | 1.4 (14) |
Cu2—Pb—O2—C17 | −32.0 (6) | C11—C12—C17—C16 | −177.7 (9) |
Cu1—Pb—O2—C17 | −152.0 (8) | C15—C16—C17—O2 | −178.6 (10) |
O3—Pb—O2—Cu1 | 89.4 (3) | C15—C16—C17—C12 | 0.2 (15) |
O4—Pb—O2—Cu1 | 139.0 (2) | Cu2—O3—C18—C23 | −17.3 (12) |
O1—Pb—O2—Cu1 | −25.4 (2) | Pb—O3—C18—C23 | 141.7 (7) |
I2—Pb—O2—Cu1 | 12.4 (4) | Cu2—O3—C18—C19 | 163.7 (7) |
I1—Pb—O2—Cu1 | −127.6 (2) | Pb—O3—C18—C19 | −37.3 (11) |
Cu2—Pb—O2—Cu1 | 120.0 (3) | O3—C18—C19—C20 | −178.8 (9) |
O4—Cu2—O3—C18 | −172.9 (7) | C23—C18—C19—C20 | 2.2 (15) |
N3—Cu2—O3—C18 | 20.8 (7) | C18—C19—C20—C21 | −2.1 (17) |
N4—Cu2—O3—C18 | −107.6 (13) | C19—C20—C21—C22 | 0.9 (17) |
Pb—Cu2—O3—C18 | 161.7 (9) | C20—C21—C22—C23 | 0.1 (17) |
O4—Cu2—O3—Pb | 25.4 (3) | O3—C18—C23—C22 | 179.9 (9) |
N3—Cu2—O3—Pb | −140.9 (3) | C19—C18—C23—C22 | −1.2 (14) |
N4—Cu2—O3—Pb | 90.7 (12) | O3—C18—C23—C24 | 0.3 (14) |
O4—Pb—O3—C18 | 175.9 (7) | C19—C18—C23—C24 | 179.3 (9) |
O1—Pb—O3—C18 | −10.6 (7) | C21—C22—C23—C18 | 0.0 (15) |
O2—Pb—O3—C18 | −61.4 (6) | C21—C22—C23—C24 | 179.6 (10) |
I2—Pb—O3—C18 | 85.7 (6) | C25—N3—C24—C23 | 179.8 (10) |
I1—Pb—O3—C18 | −142.1 (6) | Cu2—N3—C24—C23 | 2.7 (15) |
Cu2—Pb—O3—C18 | −162.7 (8) | C18—C23—C24—N3 | 7.3 (16) |
Cu1—Pb—O3—C18 | −29.7 (6) | C22—C23—C24—N3 | −172.3 (10) |
O4—Pb—O3—Cu2 | −21.4 (2) | C24—N3—C25—C26 | −123.5 (10) |
O1—Pb—O3—Cu2 | 152.0 (3) | Cu2—N3—C25—C26 | 53.7 (12) |
O2—Pb—O3—Cu2 | 101.3 (3) | N3—C25—C26—C27 | −76.3 (13) |
I2—Pb—O3—Cu2 | −111.6 (2) | C25—C26—C27—N4 | 62.2 (14) |
I1—Pb—O3—Cu2 | 20.6 (4) | C28—N4—C27—C26 | 148.5 (10) |
Cu1—Pb—O3—Cu2 | 133.0 (3) | Cu2—N4—C27—C26 | −28.3 (14) |
O3—Cu2—O4—C34 | 140.6 (7) | C27—N4—C28—C29 | 169.9 (10) |
N3—Cu2—O4—C34 | −151.1 (11) | Cu2—N4—C28—C29 | −13.2 (15) |
N4—Cu2—O4—C34 | −26.0 (7) | N4—C28—C29—C30 | 179.2 (10) |
Pb—Cu2—O4—C34 | 164.3 (9) | N4—C28—C29—C34 | −7.4 (16) |
O3—Cu2—O4—Pb | −23.7 (3) | C34—C29—C30—C31 | −0.9 (14) |
N3—Cu2—O4—Pb | 44.6 (13) | C28—C29—C30—C31 | 172.7 (9) |
N4—Cu2—O4—Pb | 169.7 (3) | C29—C30—C31—C32 | 0.1 (15) |
O3—Pb—O4—C34 | −143.2 (8) | C30—C31—C32—C33 | 0.8 (15) |
O1—Pb—O4—C34 | −161.9 (7) | C31—C32—C33—C34 | −0.9 (15) |
O2—Pb—O4—C34 | 158.0 (7) | Cu2—O4—C34—C33 | −166.0 (7) |
I2—Pb—O4—C34 | −48.6 (7) | Pb—O4—C34—C33 | −5.5 (12) |
I1—Pb—O4—C34 | 60.6 (7) | Cu2—O4—C34—C29 | 14.2 (12) |
Cu2—Pb—O4—C34 | −164.2 (9) | Pb—O4—C34—C29 | 174.7 (6) |
Cu1—Pb—O4—C34 | −176.3 (6) | C32—C33—C34—O4 | −179.8 (9) |
O3—Pb—O4—Cu2 | 21.0 (2) | C32—C33—C34—C29 | 0.0 (14) |
O1—Pb—O4—Cu2 | 2.3 (8) | C30—C29—C34—O4 | −179.3 (8) |
O2—Pb—O4—Cu2 | −37.8 (3) | C28—C29—C34—O4 | 7.4 (14) |
I2—Pb—O4—Cu2 | 115.6 (2) | C30—C29—C34—C33 | 0.8 (13) |
I1—Pb—O4—Cu2 | −135.2 (2) | C28—C29—C34—C33 | −172.4 (9) |
Experimental details
Crystal data | |
Chemical formula | [Cu2PbI2(C17H16N2O2)2] |
Mr | 1148.71 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 10.516 (1), 11.381 (2), 14.558 (3) |
α, β, γ (°) | 87.23 (2), 79.73 (1), 88.54 (1) |
V (Å3) | 1712.2 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 7.98 |
Crystal size (mm) | 0.22 × 0.05 × 0.03 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (Fair, 1990) |
Tmin, Tmax | 0.626, 0.787 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7106, 6685, 4611 |
Rint | 0.026 |
(sin θ/λ)max (Å−1) | 0.616 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.100, 1.01 |
No. of reflections | 4611 |
No. of parameters | 423 |
No. of restraints | ? |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.48, −2.14 |
Computer programs: CAD-4 EXPRESS (Enraf-Nonius, 1993), CAD-4 EXPRESS, X-RED (Stoe & Cie, 1996), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), SHELXL97.
Pb—O1 | 2.607 (6) | Cu1—O1 | 1.938 (6) |
Pb—O2 | 2.616 (6) | Cu1—O2 | 1.924 (6) |
Pb—O3 | 2.492 (6) | Cu2—O3 | 1.924 (6) |
Pb—O4 | 2.603 (6) | Cu2—O4 | 1.926 (5) |
Pb—I1 | 3.1831 (9) | Cu1—N1 | 1.970 (9) |
Pb—I2 | 3.0945 (9) | Cu1—N2 | 1.985 (8) |
Pb—Cu1 | 3.6331 (12) | Cu2—N3 | 1.961 (7) |
Pb—Cu2 | 3.5662 (12) | Cu2—N4 | 1.966 (7) |
O1—Pb—O2 | 56.7 (2) | O3—Pb—I1 | 142.81 (14) |
O3—Pb—O4 | 59.31 (18) | O4—Pb—I1 | 91.15 (14) |
O3—Pb—O1 | 101.2 (2) | O1—Pb—I1 | 103.75 (16) |
O4—Pb—O1 | 159.6 (2) | O2—Pb—I1 | 96.58 (15) |
O3—Pb—O2 | 74.8 (2) | I2—Pb—I1 | 109.13 (3) |
O4—Pb—O2 | 108.39 (19) | O2—Cu1—O1 | 80.0 (3) |
O4—Pb—I2 | 93.01 (15) | O1—Cu1—N1 | 91.2 (3) |
O1—Pb—I2 | 95.08 (15) | O2—Cu1—N2 | 91.8 (3) |
O2—Pb—I2 | 146.22 (14) | N1—Cu1—N2 | 97.7 (4) |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
Lead is environmentally significant and its solid solutions with other oxides are of great importance in a number of ferroelectric and electronic devices (Lashgari et al., 1998). The coordination sphere of Pb is mainly dominated by oxygen, generally six, seven, eight or ten in number (Virovets et al., 1993; Tahir et al., 1996; Schürman & Huber, 1998; Lashgari et al., 1998). Sometimes Pb is coordinated by weakly bonding N (Inoue et al., 1993; García-Granda et al., 1993). In addition to the above, some Cu–Pb heterodinuclear complexes with macrocyclic ligands have been reported recently (Guerrino et al., 1995; Yonemura et al., 1998).
We report here the crystal structure of a heterotrinuclear complex, [{Cu(C17H16N2O2)}2PbI2], (I), in which the phenolic O atoms of the organic ligands coordinate both Cu and Pb atoms, forming µ2 bridges.
The coordination of lead(II) in (I) is in the form of a distorted octahedron comprising four O and two I atoms (Fig. 1), with Pb—O distances of 2.492 (6), 2.603 (6), 2.607 (6) and 2.616 (6) Å, and Pb—I distances of 3.0945 (9) and 3.1831 (9) Å. The O—Pb—O bond angles range from 56.7 (2) to 159.6 (2)°. Copper(II) is four-coordinate in a highly deformed square-planar arangement, consisting of two phenolic O and two N atoms. The four-membered rings Pb—O1—Cu1—O2 and Pb—O4—Cu2—O3 are not entirely planar with, for example, Pb is -0.158 (2) Å out of the plane defined by O1, Cu1 and O2, but the angle between their least-squares planes is 50.80 (2)°. The six-membered Cu1—N1—C8—C9—C10—N2 chelate ring has a boat conformation in which C9 is disordered; the atom with suffix A has occupancy 0.564 (16) and that with suffix B has an occupancy of 0.436 (16). The Pb···Cu distances [3.6331 (12) and 3.5662 (12) Å] are rather long for a direct interaction.