Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806047994/cf2073sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806047994/cf2073Isup2.hkl |
CCDC reference: 629470
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.028 Å
- R factor = 0.074
- wR factor = 0.213
- Data-to-parameter ratio = 22.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 28
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.51 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.67 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C18 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C23 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C29 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C30 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for I4 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Pb1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Pb2 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C25 - C26 ... 1.54 Ang.
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.515 Tmax scaled 0.515 Tmin scaled 0.171 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
[Ni(C10H8N2)3][Pb2I6] | F(000) = 3024 |
Mr = 1703.04 | Dx = 2.773 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P2ybc | Cell parameters from 6737 reflections |
a = 17.2337 (14) Å | θ = 3.0–27.5° |
b = 14.7012 (8) Å | µ = 13.26 mm−1 |
c = 16.4273 (12) Å | T = 293 K |
β = 101.409 (5)° | Prism, orange |
V = 4079.7 (5) Å3 | 0.15 × 0.1 × 0.05 mm |
Z = 4 |
Rigaku Mercury CCD diffractometer | 9307 independent reflections |
Radiation source: Sealed Tube | 6421 reflections with I > 2σ(I) |
Graphite Monochromator monochromator | Rint = 0.058 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2000) | h = −22→20 |
Tmin = 0.332, Tmax = 1.000 | k = −19→19 |
31216 measured reflections | l = −18→21 |
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)] = 0.074 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.213 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0949P)2 + 47.3372P] where P = (Fo2 + 2Fc2)/3 |
9307 reflections | (Δ/σ)max = 0.005 |
406 parameters | Δρmax = 2.23 e Å−3 |
0 restraints | Δρmin = −2.30 e Å−3 |
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 | 0.75986 (4) | 0.26490 (4) | 0.09253 (4) | 0.04841 (18) | |
Pb2 | 0.76238 (4) | 0.24652 (4) | −0.15644 (4) | 0.05274 (19) | |
I1 | 0.84621 (7) | 0.12378 (8) | 0.22481 (7) | 0.0623 (3) | |
I2 | 0.82275 (7) | 0.41419 (8) | 0.23693 (9) | 0.0703 (4) | |
I3 | 0.61299 (6) | 0.25685 (7) | 0.18682 (7) | 0.0551 (3) | |
I4 | 0.69398 (9) | 0.41064 (9) | −0.05657 (9) | 0.0801 (4) | |
I5 | 0.67484 (7) | 0.11678 (8) | −0.04249 (7) | 0.0610 (3) | |
I6 | 0.90944 (7) | 0.24560 (9) | −0.00229 (8) | 0.0648 (3) | |
Ni1 | 0.24847 (11) | 0.25607 (12) | 0.19411 (13) | 0.0424 (4) | |
N1 | 0.3251 (7) | 0.3426 (8) | 0.2711 (7) | 0.042 (3) | |
N2 | 0.3437 (6) | 0.1687 (7) | 0.2386 (7) | 0.039 (3) | |
N3 | 0.3046 (8) | 0.2842 (8) | 0.0928 (8) | 0.049 (3) | |
N4 | 0.1934 (7) | 0.1623 (9) | 0.1076 (8) | 0.050 (3) | |
N5 | 0.1573 (8) | 0.3478 (10) | 0.1686 (9) | 0.060 (4) | |
N6 | 0.1837 (7) | 0.2188 (10) | 0.2836 (10) | 0.059 (4) | |
C1 | 0.3115 (10) | 0.4302 (10) | 0.2870 (11) | 0.054 (4) | |
H1A | 0.2600 | 0.4517 | 0.2712 | 0.065* | |
C2 | 0.3667 (14) | 0.4880 (13) | 0.3238 (12) | 0.076 (6) | |
H2A | 0.3545 | 0.5484 | 0.3323 | 0.092* | |
C3 | 0.4446 (13) | 0.4543 (13) | 0.3495 (13) | 0.076 (5) | |
H3A | 0.4850 | 0.4922 | 0.3759 | 0.091* | |
C4 | 0.4598 (10) | 0.3635 (12) | 0.3346 (11) | 0.062 (4) | |
H4A | 0.5105 | 0.3396 | 0.3501 | 0.074* | |
C5 | 0.3973 (8) | 0.3097 (9) | 0.2962 (9) | 0.040 (3) | |
C6 | 0.4070 (8) | 0.2122 (10) | 0.2853 (9) | 0.044 (3) | |
C7 | 0.4743 (8) | 0.1624 (11) | 0.3169 (10) | 0.050 (4) | |
H7A | 0.5190 | 0.1917 | 0.3463 | 0.060* | |
C8 | 0.4755 (10) | 0.0701 (11) | 0.3054 (11) | 0.061 (4) | |
H8A | 0.5199 | 0.0360 | 0.3282 | 0.073* | |
C9 | 0.4092 (9) | 0.0291 (11) | 0.2590 (12) | 0.064 (5) | |
H9A | 0.4084 | −0.0334 | 0.2506 | 0.077* | |
C10 | 0.3457 (8) | 0.0794 (10) | 0.2260 (10) | 0.047 (4) | |
H10A | 0.3021 | 0.0511 | 0.1935 | 0.056* | |
C11 | 0.3618 (10) | 0.3415 (14) | 0.0965 (11) | 0.066 (5) | |
H11A | 0.3644 | 0.3914 | 0.1317 | 0.079* | |
C12 | 0.4223 (12) | 0.3302 (16) | 0.0472 (12) | 0.077 (6) | |
H12A | 0.4607 | 0.3742 | 0.0457 | 0.093* | |
C13 | 0.4194 (15) | 0.2548 (16) | 0.0050 (13) | 0.086 (7) | |
H13A | 0.4612 | 0.2414 | −0.0213 | 0.103* | |
C14 | 0.3556 (12) | 0.1916 (16) | −0.0027 (12) | 0.078 (6) | |
H14A | 0.3528 | 0.1404 | −0.0364 | 0.094* | |
C15 | 0.2976 (10) | 0.2107 (13) | 0.0428 (11) | 0.062 (5) | |
C16 | 0.2260 (10) | 0.1499 (11) | 0.0411 (10) | 0.054 (4) | |
C17 | 0.1997 (10) | 0.0910 (14) | −0.0231 (11) | 0.065 (5) | |
H17A | 0.2245 | 0.0852 | −0.0682 | 0.078* | |
C18 | 0.1347 (14) | 0.0416 (14) | −0.0160 (13) | 0.088 (7) | |
H18A | 0.1152 | −0.0001 | −0.0575 | 0.106* | |
C19 | 0.0956 (12) | 0.0501 (13) | 0.0503 (14) | 0.079 (6) | |
H19A | 0.0504 | 0.0171 | 0.0540 | 0.095* | |
C20 | 0.1315 (10) | 0.1145 (11) | 0.1126 (12) | 0.062 (4) | |
H20A | 0.1089 | 0.1221 | 0.1591 | 0.075* | |
C21 | 0.1435 (13) | 0.4088 (12) | 0.1128 (12) | 0.075 (6) | |
H21A | 0.1820 | 0.4148 | 0.0806 | 0.090* | |
C22 | 0.0800 (12) | 0.4677 (16) | 0.0929 (14) | 0.089 (7) | |
H22A | 0.0770 | 0.5130 | 0.0529 | 0.106* | |
C23 | 0.0219 (14) | 0.4529 (19) | 0.1378 (16) | 0.105 (9) | |
H23A | −0.0243 | 0.4872 | 0.1281 | 0.126* | |
C24 | 0.0341 (12) | 0.3847 (15) | 0.1986 (15) | 0.083 (6) | |
H24A | −0.0045 | 0.3755 | 0.2301 | 0.100* | |
C25 | 0.0981 (9) | 0.3327 (15) | 0.2131 (13) | 0.074 (6) | |
C26 | 0.1163 (10) | 0.2634 (12) | 0.2843 (12) | 0.059 (4) | |
C27 | 0.0673 (15) | 0.2429 (14) | 0.3354 (14) | 0.082 (7) | |
H27A | 0.0187 | 0.2722 | 0.3298 | 0.098* | |
C28 | 0.0885 (14) | 0.1800 (16) | 0.3946 (16) | 0.093 (7) | |
H28A | 0.0549 | 0.1662 | 0.4308 | 0.112* | |
C29 | 0.1587 (14) | 0.137 (2) | 0.4017 (15) | 0.107 (9) | |
H29A | 0.1749 | 0.0951 | 0.4444 | 0.128* | |
C30 | 0.2061 (11) | 0.1548 (12) | 0.3451 (11) | 0.065 (5) | |
H30A | 0.2535 | 0.1235 | 0.3484 | 0.078* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.0501 (3) | 0.0550 (3) | 0.0416 (3) | 0.0019 (3) | 0.0126 (3) | 0.0055 (3) |
Pb2 | 0.0518 (4) | 0.0649 (4) | 0.0432 (4) | 0.0012 (3) | 0.0135 (3) | 0.0036 (3) |
I1 | 0.0713 (7) | 0.0620 (6) | 0.0552 (7) | 0.0176 (5) | 0.0164 (5) | 0.0121 (5) |
I2 | 0.0643 (7) | 0.0592 (7) | 0.0927 (9) | −0.0111 (5) | 0.0283 (6) | −0.0146 (6) |
I3 | 0.0437 (5) | 0.0618 (6) | 0.0622 (7) | 0.0007 (4) | 0.0164 (5) | −0.0037 (5) |
I4 | 0.0884 (9) | 0.0671 (8) | 0.0831 (9) | 0.0221 (7) | 0.0130 (7) | 0.0197 (7) |
I5 | 0.0577 (6) | 0.0674 (7) | 0.0554 (7) | −0.0088 (5) | 0.0054 (5) | 0.0006 (5) |
I6 | 0.0447 (6) | 0.0919 (9) | 0.0597 (7) | −0.0019 (5) | 0.0152 (5) | 0.0024 (6) |
Ni1 | 0.0349 (9) | 0.0433 (9) | 0.0504 (11) | 0.0024 (7) | 0.0117 (8) | −0.0038 (8) |
N1 | 0.045 (7) | 0.046 (6) | 0.038 (6) | 0.002 (5) | 0.014 (5) | 0.009 (5) |
N2 | 0.032 (6) | 0.042 (6) | 0.046 (7) | 0.003 (5) | 0.016 (5) | −0.003 (5) |
N3 | 0.060 (8) | 0.046 (7) | 0.045 (7) | 0.008 (6) | 0.020 (6) | −0.001 (6) |
N4 | 0.037 (6) | 0.058 (8) | 0.053 (8) | −0.008 (6) | 0.004 (6) | −0.017 (6) |
N5 | 0.052 (8) | 0.059 (8) | 0.068 (10) | 0.004 (7) | 0.009 (7) | −0.018 (8) |
N6 | 0.036 (7) | 0.065 (8) | 0.079 (10) | −0.003 (6) | 0.021 (7) | 0.012 (8) |
C1 | 0.051 (9) | 0.043 (8) | 0.071 (11) | 0.001 (7) | 0.018 (8) | −0.010 (8) |
C2 | 0.116 (17) | 0.055 (10) | 0.069 (13) | −0.005 (11) | 0.044 (12) | 0.003 (9) |
C3 | 0.084 (14) | 0.064 (11) | 0.079 (14) | −0.024 (10) | 0.017 (11) | −0.007 (10) |
C4 | 0.059 (10) | 0.064 (10) | 0.062 (11) | −0.009 (8) | 0.012 (8) | −0.009 (9) |
C5 | 0.035 (7) | 0.041 (7) | 0.052 (8) | 0.005 (6) | 0.025 (6) | −0.003 (6) |
C6 | 0.042 (8) | 0.052 (8) | 0.043 (8) | −0.003 (6) | 0.023 (6) | 0.010 (7) |
C7 | 0.035 (7) | 0.065 (10) | 0.052 (9) | 0.006 (7) | 0.013 (6) | −0.012 (8) |
C8 | 0.056 (10) | 0.053 (9) | 0.069 (12) | 0.008 (8) | 0.004 (8) | −0.011 (9) |
C9 | 0.052 (9) | 0.041 (8) | 0.102 (14) | 0.016 (7) | 0.020 (9) | −0.019 (9) |
C10 | 0.032 (7) | 0.046 (8) | 0.060 (10) | 0.000 (6) | 0.001 (6) | 0.002 (7) |
C11 | 0.054 (10) | 0.089 (13) | 0.060 (11) | 0.012 (9) | 0.024 (8) | 0.029 (10) |
C12 | 0.071 (12) | 0.097 (15) | 0.070 (13) | −0.027 (11) | 0.029 (10) | 0.003 (12) |
C13 | 0.097 (16) | 0.115 (18) | 0.057 (12) | −0.035 (13) | 0.040 (11) | −0.019 (12) |
C14 | 0.082 (14) | 0.095 (15) | 0.066 (12) | −0.005 (12) | 0.033 (11) | −0.008 (12) |
C15 | 0.059 (11) | 0.079 (12) | 0.045 (9) | 0.010 (9) | 0.005 (8) | 0.018 (9) |
C16 | 0.063 (10) | 0.049 (8) | 0.049 (9) | 0.011 (8) | 0.007 (8) | −0.005 (7) |
C17 | 0.042 (9) | 0.092 (13) | 0.059 (11) | 0.001 (9) | 0.004 (8) | −0.014 (10) |
C18 | 0.099 (16) | 0.082 (14) | 0.072 (14) | 0.010 (12) | −0.011 (12) | −0.047 (12) |
C19 | 0.069 (12) | 0.067 (12) | 0.095 (16) | −0.017 (10) | 0.000 (11) | −0.004 (11) |
C20 | 0.058 (10) | 0.058 (10) | 0.070 (12) | −0.007 (8) | 0.012 (9) | −0.015 (9) |
C21 | 0.098 (15) | 0.061 (11) | 0.051 (11) | 0.010 (10) | −0.021 (10) | −0.010 (9) |
C22 | 0.061 (13) | 0.099 (16) | 0.087 (16) | 0.027 (12) | −0.030 (12) | −0.027 (13) |
C23 | 0.070 (15) | 0.12 (2) | 0.10 (2) | 0.019 (14) | −0.031 (14) | −0.011 (16) |
C24 | 0.066 (13) | 0.082 (14) | 0.100 (17) | −0.001 (11) | 0.013 (12) | −0.001 (13) |
C25 | 0.031 (8) | 0.097 (14) | 0.095 (15) | −0.016 (9) | 0.017 (9) | −0.054 (13) |
C26 | 0.048 (9) | 0.062 (10) | 0.067 (12) | −0.018 (8) | 0.008 (8) | −0.018 (9) |
C27 | 0.106 (17) | 0.078 (14) | 0.079 (15) | −0.010 (12) | 0.066 (13) | −0.007 (11) |
C28 | 0.089 (16) | 0.089 (16) | 0.12 (2) | 0.000 (13) | 0.069 (15) | −0.011 (15) |
C29 | 0.081 (16) | 0.17 (3) | 0.081 (16) | −0.039 (16) | 0.041 (13) | −0.011 (16) |
C30 | 0.065 (11) | 0.069 (11) | 0.062 (11) | 0.008 (9) | 0.017 (9) | 0.004 (9) |
Pb1—I1 | 3.1561 (12) | C6—C7 | 1.38 (2) |
Pb1—I3 | 3.2203 (12) | C7—C8 | 1.37 (2) |
Pb1—I5 | 3.2438 (13) | C7—H7A | 0.930 |
Pb1—I2 | 3.2560 (14) | C8—C9 | 1.38 (2) |
Pb1—I6 | 3.2774 (13) | C8—H8A | 0.930 |
Pb1—I4 | 3.2830 (14) | C9—C10 | 1.34 (2) |
Pb2—I6 | 3.2088 (14) | C9—H9A | 0.930 |
Pb2—I2i | 3.2332 (14) | C10—H10A | 0.930 |
Pb2—I5 | 3.2457 (13) | C11—C12 | 1.45 (2) |
Pb2—I3i | 3.2617 (13) | C11—H11A | 0.930 |
Pb2—I1i | 3.2624 (13) | C12—C13 | 1.30 (3) |
Pb2—I4 | 3.2661 (16) | C12—H12A | 0.930 |
I1—Pb2ii | 3.2624 (13) | C13—C14 | 1.43 (3) |
I2—Pb2ii | 3.2332 (14) | C13—H13A | 0.930 |
I3—Pb2ii | 3.2617 (13) | C14—C15 | 1.39 (3) |
Ni1—N5 | 2.051 (14) | C14—H14A | 0.930 |
Ni1—N4 | 2.071 (12) | C15—C16 | 1.52 (2) |
Ni1—N1 | 2.074 (12) | C16—C17 | 1.37 (2) |
Ni1—N6 | 2.087 (14) | C17—C18 | 1.36 (3) |
Ni1—N2 | 2.098 (11) | C17—H17A | 0.930 |
Ni1—N3 | 2.124 (13) | C18—C19 | 1.39 (3) |
N1—C5 | 1.323 (17) | C18—H18A | 0.930 |
N1—C1 | 1.343 (18) | C19—C20 | 1.44 (2) |
N2—C10 | 1.331 (18) | C19—H19A | 0.930 |
N2—C6 | 1.363 (18) | C20—H20A | 0.930 |
N3—C11 | 1.29 (2) | C21—C22 | 1.38 (3) |
N3—C15 | 1.35 (2) | C21—H21A | 0.930 |
N4—C20 | 1.29 (2) | C22—C23 | 1.37 (3) |
N4—C16 | 1.33 (2) | C22—H22A | 0.930 |
N5—C21 | 1.27 (2) | C23—C24 | 1.40 (3) |
N5—C25 | 1.39 (2) | C23—H23A | 0.930 |
N6—C26 | 1.34 (2) | C24—C25 | 1.32 (3) |
N6—C30 | 1.38 (2) | C24—H24A | 0.930 |
C1—C2 | 1.33 (2) | C25—C26 | 1.54 (3) |
C1—H1A | 0.930 | C26—C27 | 1.34 (3) |
C2—C3 | 1.42 (3) | C27—C28 | 1.34 (3) |
C2—H2A | 0.930 | C27—H27A | 0.930 |
C3—C4 | 1.39 (3) | C28—C29 | 1.35 (3) |
C3—H3A | 0.930 | C28—H28A | 0.930 |
C4—C5 | 1.38 (2) | C29—C30 | 1.38 (3) |
C4—H4A | 0.930 | C29—H29A | 0.930 |
C5—C6 | 1.46 (2) | C30—H30A | 0.930 |
I1—Pb1—I3 | 87.31 (3) | C3—C4—H4A | 120.9 |
I1—Pb1—I5 | 96.73 (4) | N1—C5—C4 | 122.2 (14) |
I3—Pb1—I5 | 90.72 (3) | N1—C5—C6 | 116.4 (12) |
I1—Pb1—I2 | 84.14 (4) | C4—C5—C6 | 121.3 (13) |
I3—Pb1—I2 | 81.63 (3) | N2—C6—C7 | 118.8 (14) |
I5—Pb1—I2 | 172.26 (4) | N2—C6—C5 | 115.6 (12) |
I1—Pb1—I6 | 87.83 (3) | C7—C6—C5 | 125.6 (14) |
I3—Pb1—I6 | 172.92 (4) | C8—C7—C6 | 120.5 (15) |
I5—Pb1—I6 | 84.73 (3) | C8—C7—H7A | 119.8 |
I2—Pb1—I6 | 102.99 (4) | C6—C7—H7A | 119.8 |
I1—Pb1—I4 | 171.49 (4) | C7—C8—C9 | 118.3 (15) |
I3—Pb1—I4 | 101.19 (4) | C7—C8—H8A | 120.9 |
I5—Pb1—I4 | 83.41 (4) | C9—C8—H8A | 120.9 |
I2—Pb1—I4 | 96.88 (4) | C10—C9—C8 | 120.2 (15) |
I6—Pb1—I4 | 83.70 (4) | C10—C9—H9A | 119.9 |
I6—Pb2—I2i | 97.81 (4) | C8—C9—H9A | 119.9 |
I6—Pb2—I5 | 85.82 (3) | N2—C10—C9 | 121.6 (14) |
I2i—Pb2—I5 | 96.84 (4) | N2—C10—H10A | 119.2 |
I6—Pb2—I3i | 178.89 (4) | C9—C10—H10A | 119.2 |
I2i—Pb2—I3i | 81.35 (3) | N3—C11—C12 | 121.7 (19) |
I5—Pb2—I3i | 93.55 (3) | N3—C11—H11A | 119.1 |
I6—Pb2—I1i | 95.76 (3) | C12—C11—H11A | 119.1 |
I2i—Pb2—I1i | 82.83 (3) | C13—C12—C11 | 116.0 (19) |
I5—Pb2—I1i | 178.42 (3) | C13—C12—H12A | 122.0 |
I3i—Pb2—I1i | 84.87 (3) | C11—C12—H12A | 122.0 |
I6—Pb2—I4 | 85.06 (4) | C12—C13—C14 | 123 (2) |
I2i—Pb2—I4 | 177.11 (4) | C12—C13—H13A | 118.4 |
I5—Pb2—I4 | 83.64 (4) | C14—C13—H13A | 118.4 |
I3i—Pb2—I4 | 95.78 (4) | C15—C14—C13 | 116 (2) |
I1i—Pb2—I4 | 96.61 (4) | C15—C14—H14A | 121.8 |
Pb1—I1—Pb2ii | 79.82 (3) | C13—C14—H14A | 121.8 |
Pb2ii—I2—Pb1 | 78.80 (3) | N3—C15—C14 | 120.2 (18) |
Pb1—I3—Pb2ii | 78.90 (3) | N3—C15—C16 | 117.2 (15) |
Pb2—I4—Pb1 | 77.69 (3) | C14—C15—C16 | 122.5 (18) |
Pb1—I5—Pb2 | 78.54 (3) | N4—C16—C17 | 126.0 (17) |
Pb2—I6—Pb1 | 78.58 (3) | N4—C16—C15 | 112.0 (14) |
N5—Ni1—N4 | 94.0 (5) | C17—C16—C15 | 122.0 (16) |
N5—Ni1—N1 | 95.2 (5) | C18—C17—C16 | 115.1 (17) |
N4—Ni1—N1 | 167.7 (5) | C18—C17—H17A | 122.5 |
N5—Ni1—N6 | 79.7 (6) | C16—C17—H17A | 122.5 |
N4—Ni1—N6 | 94.2 (6) | C17—C18—C19 | 123.6 (17) |
N1—Ni1—N6 | 95.5 (5) | C17—C18—H18A | 118.2 |
N5—Ni1—N2 | 171.5 (5) | C19—C18—H18A | 118.2 |
N4—Ni1—N2 | 93.0 (5) | C18—C19—C20 | 114.0 (18) |
N1—Ni1—N2 | 78.7 (5) | C18—C19—H19A | 123.0 |
N6—Ni1—N2 | 94.8 (5) | C20—C19—H19A | 123.0 |
N5—Ni1—N3 | 99.3 (6) | N4—C20—C19 | 123.7 (18) |
N4—Ni1—N3 | 79.0 (5) | N4—C20—H20A | 118.1 |
N1—Ni1—N3 | 91.4 (5) | C19—C20—H20A | 118.1 |
N6—Ni1—N3 | 173.1 (6) | N5—C21—C22 | 130 (2) |
N2—Ni1—N3 | 86.9 (5) | N5—C21—H21A | 115.2 |
C5—N1—C1 | 118.6 (13) | C22—C21—H21A | 115.2 |
C5—N1—Ni1 | 114.3 (10) | C23—C22—C21 | 114 (3) |
C1—N1—Ni1 | 126.3 (10) | C23—C22—H22A | 123.2 |
C10—N2—C6 | 120.5 (12) | C21—C22—H22A | 123.2 |
C10—N2—Ni1 | 126.4 (9) | C22—C23—C24 | 118 (2) |
C6—N2—Ni1 | 113.1 (9) | C22—C23—H23A | 120.9 |
C11—N3—C15 | 121.8 (15) | C24—C23—H23A | 120.9 |
C11—N3—Ni1 | 123.6 (12) | C25—C24—C23 | 123 (2) |
C15—N3—Ni1 | 108.8 (11) | C25—C24—H24A | 118.5 |
C20—N4—C16 | 117.6 (14) | C23—C24—H24A | 118.5 |
C20—N4—Ni1 | 126.1 (12) | C24—C25—N5 | 119 (2) |
C16—N4—Ni1 | 116.3 (11) | C24—C25—C26 | 123.9 (19) |
C21—N5—C25 | 116.3 (18) | N5—C25—C26 | 116.6 (16) |
C21—N5—Ni1 | 129.6 (15) | N6—C26—C27 | 124 (2) |
C25—N5—Ni1 | 113.6 (14) | N6—C26—C25 | 111.4 (16) |
C26—N6—C30 | 116.5 (15) | C27—C26—C25 | 124.6 (19) |
C26—N6—Ni1 | 117.7 (12) | C26—C27—C28 | 120 (2) |
C30—N6—Ni1 | 125.7 (11) | C26—C27—H27A | 120.1 |
C2—C1—N1 | 124.5 (16) | C28—C27—H27A | 120.1 |
C2—C1—H1A | 117.8 | C27—C28—C29 | 120 (2) |
N1—C1—H1A | 117.8 | C27—C28—H28A | 120.1 |
C1—C2—C3 | 117.6 (18) | C29—C28—H28A | 120.1 |
C1—C2—H2A | 121.2 | C28—C29—C30 | 119 (3) |
C3—C2—H2A | 121.2 | C28—C29—H29A | 120.3 |
C4—C3—C2 | 119.0 (17) | C30—C29—H29A | 120.3 |
C4—C3—H3A | 120.5 | N6—C30—C29 | 121 (2) |
C2—C3—H3A | 120.5 | N6—C30—H30A | 119.7 |
C5—C4—C3 | 118.2 (17) | C29—C30—H30A | 119.7 |
C5—C4—H4A | 120.9 |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, −y+1/2, z+1/2. |