
Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005575/ci6753sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005575/ci6753Isup2.hkl |
CCDC reference: 601144
Data collection: CAD-4 Software (Enraf–Nonius, 1989); cell refinement: CAD-4 Software; data reduction: CAD-4 Software; 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.
(C8H19N2O2)[Al(C4H19NO)6](ClO4)7 | F(000) = 2084 |
Mr = 1970.82 | Dx = 1.369 Mg m−3 |
Monoclinic, P21/n | Cu Kα radiation, λ = 1.54184 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 22.413 (2) Å | θ = 67.2–69.9° |
b = 10.862 (2) Å | µ = 2.86 mm−1 |
c = 22.416 (3) Å | T = 297 K |
β = 118.80 (1)° | Prism, colourless |
V = 4782.2 (12) Å3 | 0.40 × 0.40 × 0.40 mm |
Z = 2 |
Enraf-Nonius CAD-4 diffractometer | 5548 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.034 |
Graphite monochromator | θmax = 69.9°, θmin = 2.3° |
ω–2θ scans | h = −27→23 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→13 |
Tmin = 0.318, Tmax = 0.318 | l = 0→23 |
8959 measured reflections | 3 standard reflections every 60 min |
8716 independent reflections | intensity decay: 2.7% |
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)] = 0.078 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.244 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.1096P)2 + 5.6858P] where P = (Fo2 + 2Fc2)/3 |
8716 reflections | (Δ/σ)max = 0.001 |
623 parameters | Δρmax = 0.58 e Å−3 |
6 restraints | Δρmin = −0.33 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 | Occ. (<1) | |
Al | 0.53181 (5) | 0.04737 (11) | 0.25252 (6) | 0.0482 (3) | |
O1 | 0.45827 (14) | 0.0306 (3) | 0.27000 (15) | 0.0600 (7) | |
O2 | 0.60447 (14) | 0.0604 (3) | 0.23308 (15) | 0.0624 (8) | |
O3 | 0.51902 (12) | −0.1135 (3) | 0.21445 (14) | 0.0539 (7) | |
O4 | 0.47401 (15) | 0.1026 (3) | 0.16404 (15) | 0.0665 (8) | |
O5 | 0.54294 (16) | 0.2093 (3) | 0.28365 (17) | 0.0675 (8) | |
O6 | 0.59197 (14) | −0.0072 (3) | 0.34156 (14) | 0.0578 (7) | |
N1 | 0.3753 (2) | −0.0161 (4) | 0.2932 (2) | 0.0748 (11) | |
N2 | 0.69308 (19) | 0.0830 (4) | 0.2156 (2) | 0.0719 (11) | |
N3 | 0.49329 (19) | −0.2603 (4) | 0.13661 (18) | 0.0668 (10) | |
N4 | 0.4312 (3) | 0.2073 (6) | 0.0678 (3) | 0.124 (2) | |
N5 | 0.5420 (2) | 0.4032 (5) | 0.3141 (3) | 0.1047 (19) | |
N6 | 0.68702 (18) | −0.0354 (4) | 0.44017 (19) | 0.0669 (10) | |
C11 | 0.4315 (2) | −0.0463 (4) | 0.2933 (2) | 0.0586 (11) | |
C12 | 0.4628 (3) | −0.1685 (5) | 0.3200 (3) | 0.0756 (14) | |
H12A | 0.4313 | −0.2322 | 0.2938 | 0.113* | |
H12B | 0.4736 | −0.1756 | 0.3668 | 0.113* | |
H12C | 0.5036 | −0.1766 | 0.3165 | 0.113* | |
C13 | 0.3409 (3) | −0.0965 (7) | 0.3201 (4) | 0.105 (2) | |
H13A | 0.2996 | −0.0579 | 0.3134 | 0.157* | |
H13B | 0.3703 | −0.1100 | 0.3678 | 0.157* | |
H13C | 0.3304 | −0.1739 | 0.2966 | 0.157* | |
C14 | 0.3464 (3) | 0.1056 (7) | 0.2711 (4) | 0.112 (2) | |
H14A | 0.3002 | 0.1060 | 0.2627 | 0.169* | |
H14B | 0.3474 | 0.1268 | 0.2300 | 0.169* | |
H14C | 0.3725 | 0.1645 | 0.3059 | 0.169* | |
C21 | 0.6626 (2) | 0.1065 (4) | 0.2513 (2) | 0.0638 (12) | |
C22 | 0.6970 (3) | 0.1848 (6) | 0.3134 (3) | 0.0847 (16) | |
H22A | 0.7000 | 0.2679 | 0.3004 | 0.127* | |
H22B | 0.7419 | 0.1536 | 0.3424 | 0.127* | |
H22C | 0.6711 | 0.1835 | 0.3373 | 0.127* | |
C23 | 0.7594 (3) | 0.1341 (7) | 0.2312 (4) | 0.106 (2) | |
H23A | 0.7600 | 0.2207 | 0.2399 | 0.159* | |
H23B | 0.7673 | 0.1212 | 0.1932 | 0.159* | |
H23C | 0.7944 | 0.0938 | 0.2707 | 0.159* | |
C24 | 0.6617 (3) | 0.0068 (6) | 0.1553 (3) | 0.0964 (19) | |
H24A | 0.6886 | −0.0660 | 0.1623 | 0.145* | |
H24B | 0.6588 | 0.0518 | 0.1172 | 0.145* | |
H24C | 0.6168 | −0.0162 | 0.1464 | 0.145* | |
C31 | 0.4744 (2) | −0.1727 (4) | 0.1636 (2) | 0.0556 (10) | |
C32 | 0.3996 (2) | −0.1470 (5) | 0.1356 (3) | 0.0792 (15) | |
H32A | 0.3779 | −0.2178 | 0.1422 | 0.119* | |
H32B | 0.3795 | −0.1292 | 0.0878 | 0.119* | |
H32C | 0.3939 | −0.0776 | 0.1588 | 0.119* | |
C33 | 0.5655 (3) | −0.2858 (5) | 0.1611 (3) | 0.0817 (15) | |
H33A | 0.5732 | −0.2980 | 0.1229 | 0.123* | |
H33B | 0.5784 | −0.3587 | 0.1887 | 0.123* | |
H33C | 0.5922 | −0.2175 | 0.1877 | 0.123* | |
C34 | 0.4442 (3) | −0.3388 (7) | 0.0806 (3) | 0.103 (2) | |
H34A | 0.4685 | −0.3988 | 0.0692 | 0.154* | |
H34B | 0.4171 | −0.2886 | 0.0415 | 0.154* | |
H34C | 0.4152 | −0.3799 | 0.0948 | 0.154* | |
C41 | 0.4407 (3) | 0.1800 (6) | 0.1229 (3) | 0.096 (2) | |
C42 | 0.3941 (5) | 0.2671 (8) | 0.1417 (5) | 0.151 (3) | |
H42A | 0.3873 | 0.2285 | 0.1766 | 0.227* | |
H42B | 0.3508 | 0.2797 | 0.1020 | 0.227* | |
H42C | 0.4163 | 0.3450 | 0.1579 | 0.227* | |
C43 | 0.4765 (5) | 0.1141 (10) | 0.0485 (5) | 0.156 (4) | |
H43A | 0.5084 | 0.1609 | 0.0407 | 0.234* | |
H43B | 0.4470 | 0.0689 | 0.0081 | 0.234* | |
H43C | 0.5007 | 0.0578 | 0.0854 | 0.234* | |
C44 | 0.3920 (4) | 0.2930 (8) | 0.0161 (4) | 0.136 (3) | |
H44A | 0.3567 | 0.2503 | −0.0222 | 0.204* | |
H44B | 0.4208 | 0.3354 | 0.0021 | 0.204* | |
H44C | 0.3718 | 0.3514 | 0.0332 | 0.204* | |
C51 | 0.5365 (2) | 0.2926 (6) | 0.3172 (3) | 0.0847 (16) | |
C52 | 0.5200 (4) | 0.2598 (7) | 0.3763 (3) | 0.107 (2) | |
H52A | 0.4761 | 0.2925 | 0.3656 | 0.161* | |
H52B | 0.5541 | 0.2950 | 0.4182 | 0.161* | |
H52C | 0.5196 | 0.1720 | 0.3809 | 0.161* | |
C53 | 0.5358 (4) | 0.5045 (6) | 0.3516 (4) | 0.108 (2) | |
H53A | 0.5409 | 0.5804 | 0.3325 | 0.162* | |
H53B | 0.5706 | 0.4988 | 0.3983 | 0.162* | |
H53C | 0.4919 | 0.5024 | 0.3491 | 0.162* | |
C54 | 0.5586 (4) | 0.4389 (8) | 0.2557 (4) | 0.128 (3) | |
H54A | 0.6005 | 0.4845 | 0.2746 | 0.192* | |
H54B | 0.5224 | 0.4885 | 0.2225 | 0.192* | |
H54C | 0.5631 | 0.3654 | 0.2344 | 0.192* | |
C61 | 0.6468 (2) | −0.0658 (4) | 0.3771 (2) | 0.0598 (11) | |
C62 | 0.6660 (3) | −0.1719 (6) | 0.3476 (3) | 0.098 (2) | |
H62A | 0.6782 | −0.2410 | 0.3779 | 0.147* | |
H62B | 0.7042 | −0.1494 | 0.3414 | 0.147* | |
H62C | 0.6282 | −0.1937 | 0.3044 | 0.147* | |
C63 | 0.7522 (3) | −0.0988 (6) | 0.4836 (3) | 0.0928 (18) | |
H63A | 0.7673 | −0.0793 | 0.5305 | 0.139* | |
H63B | 0.7857 | −0.0722 | 0.4714 | 0.139* | |
H63C | 0.7458 | −0.1862 | 0.4771 | 0.139* | |
C64 | 0.6704 (3) | 0.0689 (7) | 0.4706 (3) | 0.107 (2) | |
H64A | 0.6848 | 0.1439 | 0.4588 | 0.161* | |
H64B | 0.6933 | 0.0598 | 0.5192 | 0.161* | |
H64C | 0.6221 | 0.0715 | 0.4539 | 0.161* | |
Cl1 | 0.16330 (6) | 0.03451 (13) | 0.29394 (7) | 0.0759 (4) | |
O11 | 0.1061 (2) | 0.0656 (5) | 0.3008 (3) | 0.1337 (19) | |
O12 | 0.1864 (3) | 0.1328 (6) | 0.2712 (4) | 0.169 (3) | |
O13 | 0.1452 (3) | −0.0574 (6) | 0.2460 (3) | 0.165 (3) | |
O14 | 0.2133 (3) | −0.0117 (8) | 0.3547 (3) | 0.177 (3) | |
Cl2 | 0.87209 (8) | −0.10474 (14) | 0.38545 (7) | 0.0837 (4) | |
O21 | 0.8603 (3) | −0.2107 (5) | 0.4140 (3) | 0.1360 (19) | |
O22 | 0.8497 (5) | −0.0017 (7) | 0.4040 (4) | 0.190 (3) | |
O231 | 0.8527 (12) | −0.1154 (18) | 0.3211 (7) | 0.150 (9) | 0.50 |
O232 | 0.8238 (13) | −0.107 (2) | 0.3131 (9) | 0.207 (13) | 0.50 |
O241 | 0.9389 (10) | −0.066 (2) | 0.4218 (12) | 0.195 (13) | 0.50 |
O242 | 0.9342 (12) | −0.115 (3) | 0.3871 (16) | 0.224 (14) | 0.50 |
Cl3 | 0.73827 (8) | 0.46792 (17) | 0.46367 (9) | 0.0957 (5) | |
O31 | 0.7046 (8) | 0.3953 (10) | 0.4826 (8) | 0.308 (7) | |
O32 | 0.7174 (6) | 0.5800 (7) | 0.4690 (5) | 0.260 (5) | |
O331 | 0.7941 (10) | 0.4461 (19) | 0.5251 (11) | 0.265 (14) | 0.50 |
O332 | 0.8041 (7) | 0.483 (2) | 0.4787 (7) | 0.198 (9) | 0.50 |
O341 | 0.7087 (7) | 0.4776 (19) | 0.3910 (6) | 0.158 (7) | 0.50 |
O342 | 0.7304 (15) | 0.3894 (19) | 0.4187 (11) | 0.256 (13) | 0.50 |
O7 | 0.0461 (2) | −0.0697 (6) | 0.0144 (3) | 0.1314 (18) | |
N7 | 0.1539 (3) | −0.1210 (7) | 0.0785 (3) | 0.1143 (19) | |
C71 | 0.1064 (4) | −0.0379 (7) | 0.0587 (3) | 0.0964 (19) | |
C72 | 0.1190 (5) | 0.0889 (9) | 0.0844 (4) | 0.141 (3) | |
H72A | 0.1516 | 0.1268 | 0.0739 | 0.211* | |
H72B | 0.1365 | 0.0882 | 0.1328 | 0.211* | |
H72C | 0.0772 | 0.1346 | 0.0632 | 0.211* | |
C73 | 0.2243 (4) | −0.0944 (11) | 0.1278 (4) | 0.163 (4) | |
H73A | 0.2272 | −0.0136 | 0.1464 | 0.245* | |
H73B | 0.2518 | −0.0978 | 0.1057 | 0.245* | |
H73C | 0.2403 | −0.1541 | 0.1637 | 0.245* | |
C74 | 0.1394 (5) | −0.2415 (9) | 0.0474 (7) | 0.179 (4) | |
H74A | 0.1725 | −0.2993 | 0.0778 | 0.268* | |
H74B | 0.1413 | −0.2383 | 0.0056 | 0.268* | |
H74C | 0.0948 | −0.2669 | 0.0383 | 0.268* | |
H7 | 0.0000 | 0.0000 | 0.0000 | 0.25 (8)* | |
Cl4 | 0.5000 | 0.0000 | 0.5000 | 0.1372 (11) | |
O41 | 0.5217 (11) | −0.0331 (16) | 0.4538 (8) | 0.166 (5) | 0.50 |
O42 | 0.5333 (12) | −0.0565 (14) | 0.5617 (5) | 0.166 (6) | 0.50 |
O43 | 0.5303 (8) | 0.1250 (10) | 0.5166 (7) | 0.163 (5) | 0.50 |
O44 | 0.4312 (6) | 0.026 (3) | 0.472 (2) | 0.293 (14) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al | 0.0413 (6) | 0.0569 (7) | 0.0464 (6) | 0.0016 (5) | 0.0212 (5) | −0.0012 (5) |
O1 | 0.0497 (15) | 0.0674 (19) | 0.0689 (19) | 0.0068 (14) | 0.0334 (14) | 0.0051 (15) |
O2 | 0.0478 (15) | 0.077 (2) | 0.0689 (19) | −0.0096 (14) | 0.0330 (14) | −0.0101 (16) |
O3 | 0.0380 (13) | 0.0588 (16) | 0.0530 (16) | −0.0004 (12) | 0.0125 (12) | −0.0076 (13) |
O4 | 0.0615 (18) | 0.075 (2) | 0.0542 (18) | 0.0079 (16) | 0.0213 (15) | 0.0150 (16) |
O5 | 0.072 (2) | 0.0598 (18) | 0.075 (2) | −0.0032 (15) | 0.0392 (17) | −0.0117 (16) |
O6 | 0.0488 (15) | 0.0692 (18) | 0.0486 (16) | 0.0043 (13) | 0.0181 (13) | 0.0011 (14) |
N1 | 0.057 (2) | 0.093 (3) | 0.085 (3) | 0.001 (2) | 0.042 (2) | −0.002 (2) |
N2 | 0.055 (2) | 0.085 (3) | 0.087 (3) | 0.004 (2) | 0.043 (2) | 0.020 (2) |
N3 | 0.064 (2) | 0.077 (3) | 0.051 (2) | −0.0084 (19) | 0.0214 (18) | −0.0148 (19) |
N4 | 0.107 (4) | 0.126 (5) | 0.076 (3) | −0.037 (4) | −0.005 (3) | 0.041 (3) |
N5 | 0.072 (3) | 0.071 (3) | 0.129 (4) | 0.007 (2) | 0.015 (3) | −0.035 (3) |
N6 | 0.052 (2) | 0.087 (3) | 0.053 (2) | 0.0023 (19) | 0.0187 (17) | 0.001 (2) |
C11 | 0.046 (2) | 0.077 (3) | 0.056 (2) | −0.001 (2) | 0.0273 (19) | −0.001 (2) |
C12 | 0.071 (3) | 0.074 (3) | 0.086 (4) | 0.001 (3) | 0.041 (3) | 0.011 (3) |
C13 | 0.078 (4) | 0.146 (6) | 0.118 (5) | −0.019 (4) | 0.070 (4) | −0.004 (4) |
C14 | 0.077 (4) | 0.111 (5) | 0.163 (7) | 0.016 (4) | 0.069 (4) | −0.003 (5) |
C21 | 0.054 (2) | 0.071 (3) | 0.069 (3) | 0.004 (2) | 0.031 (2) | 0.017 (2) |
C22 | 0.069 (3) | 0.092 (4) | 0.081 (4) | −0.017 (3) | 0.027 (3) | −0.009 (3) |
C23 | 0.060 (3) | 0.128 (5) | 0.144 (6) | 0.001 (3) | 0.060 (4) | 0.040 (5) |
C24 | 0.102 (4) | 0.107 (5) | 0.109 (5) | −0.001 (4) | 0.074 (4) | −0.009 (4) |
C31 | 0.049 (2) | 0.067 (3) | 0.046 (2) | 0.0005 (19) | 0.0185 (19) | 0.002 (2) |
C32 | 0.040 (2) | 0.093 (4) | 0.080 (3) | −0.002 (2) | 0.009 (2) | −0.005 (3) |
C33 | 0.071 (3) | 0.091 (4) | 0.087 (4) | 0.006 (3) | 0.042 (3) | −0.014 (3) |
C34 | 0.097 (4) | 0.120 (5) | 0.078 (4) | −0.027 (4) | 0.031 (3) | −0.049 (4) |
C41 | 0.088 (4) | 0.084 (4) | 0.071 (4) | −0.028 (3) | 0.004 (3) | 0.013 (3) |
C42 | 0.145 (7) | 0.132 (7) | 0.186 (9) | 0.036 (6) | 0.087 (7) | −0.040 (6) |
C43 | 0.145 (7) | 0.208 (10) | 0.153 (8) | 0.019 (7) | 0.102 (7) | −0.029 (7) |
C44 | 0.125 (6) | 0.136 (7) | 0.103 (5) | 0.018 (5) | 0.019 (4) | 0.063 (5) |
C51 | 0.050 (3) | 0.084 (4) | 0.089 (4) | −0.002 (3) | 0.009 (3) | −0.023 (3) |
C52 | 0.112 (5) | 0.139 (6) | 0.085 (4) | 0.001 (4) | 0.059 (4) | 0.015 (4) |
C53 | 0.105 (5) | 0.074 (4) | 0.130 (6) | 0.005 (3) | 0.043 (4) | −0.030 (4) |
C54 | 0.108 (5) | 0.167 (8) | 0.121 (6) | 0.016 (5) | 0.064 (5) | 0.070 (5) |
C61 | 0.053 (2) | 0.072 (3) | 0.053 (2) | −0.004 (2) | 0.024 (2) | 0.002 (2) |
C62 | 0.092 (4) | 0.104 (4) | 0.071 (3) | 0.036 (3) | 0.018 (3) | −0.015 (3) |
C63 | 0.055 (3) | 0.129 (5) | 0.065 (3) | 0.017 (3) | 0.005 (2) | 0.011 (3) |
C64 | 0.095 (4) | 0.134 (6) | 0.069 (4) | 0.021 (4) | 0.021 (3) | −0.032 (4) |
Cl1 | 0.0594 (6) | 0.0945 (9) | 0.0761 (8) | 0.0018 (6) | 0.0344 (6) | 0.0055 (7) |
O11 | 0.102 (3) | 0.135 (4) | 0.201 (6) | 0.004 (3) | 0.103 (4) | −0.012 (4) |
O12 | 0.139 (5) | 0.145 (5) | 0.248 (7) | −0.009 (4) | 0.112 (5) | 0.063 (5) |
O13 | 0.173 (6) | 0.177 (6) | 0.159 (5) | −0.028 (5) | 0.090 (5) | −0.081 (5) |
O14 | 0.113 (4) | 0.304 (9) | 0.094 (4) | 0.057 (5) | 0.034 (3) | 0.059 (5) |
Cl2 | 0.1001 (10) | 0.0842 (9) | 0.0680 (8) | −0.0117 (7) | 0.0416 (7) | −0.0049 (7) |
O21 | 0.196 (5) | 0.104 (4) | 0.107 (3) | −0.043 (3) | 0.072 (4) | 0.004 (3) |
O22 | 0.289 (10) | 0.143 (5) | 0.179 (6) | 0.009 (6) | 0.145 (7) | −0.041 (5) |
O231 | 0.28 (3) | 0.135 (12) | 0.069 (9) | −0.014 (13) | 0.117 (15) | −0.024 (8) |
O232 | 0.222 (18) | 0.121 (12) | 0.109 (11) | −0.019 (11) | −0.055 (11) | 0.026 (9) |
O241 | 0.109 (13) | 0.170 (16) | 0.21 (2) | −0.075 (13) | −0.001 (12) | 0.052 (14) |
O242 | 0.123 (18) | 0.30 (3) | 0.29 (4) | 0.030 (17) | 0.13 (2) | 0.02 (2) |
Cl3 | 0.0872 (10) | 0.0997 (11) | 0.0950 (11) | −0.0033 (8) | 0.0397 (8) | −0.0130 (9) |
O31 | 0.46 (2) | 0.223 (10) | 0.377 (17) | −0.062 (11) | 0.307 (17) | 0.050 (10) |
O32 | 0.372 (14) | 0.121 (6) | 0.265 (11) | 0.072 (7) | 0.136 (10) | 0.006 (6) |
O331 | 0.166 (15) | 0.221 (18) | 0.178 (16) | 0.078 (14) | −0.102 (13) | −0.075 (15) |
O332 | 0.095 (9) | 0.39 (3) | 0.100 (9) | −0.024 (12) | 0.035 (8) | 0.006 (13) |
O341 | 0.111 (8) | 0.28 (2) | 0.082 (7) | −0.040 (10) | 0.042 (6) | −0.008 (10) |
O342 | 0.43 (4) | 0.180 (17) | 0.152 (16) | −0.064 (19) | 0.14 (2) | −0.105 (14) |
O7 | 0.076 (3) | 0.156 (5) | 0.148 (5) | 0.008 (3) | 0.042 (3) | −0.001 (4) |
N7 | 0.088 (4) | 0.150 (6) | 0.114 (4) | 0.014 (4) | 0.056 (3) | 0.016 (4) |
C71 | 0.089 (4) | 0.129 (6) | 0.084 (4) | 0.021 (4) | 0.052 (4) | 0.014 (4) |
C72 | 0.162 (8) | 0.144 (8) | 0.107 (6) | 0.011 (6) | 0.057 (5) | −0.023 (5) |
C73 | 0.083 (5) | 0.248 (12) | 0.122 (7) | 0.032 (6) | 0.020 (5) | 0.026 (7) |
C74 | 0.151 (8) | 0.125 (8) | 0.267 (14) | 0.018 (6) | 0.106 (9) | −0.022 (9) |
Cl4 | 0.122 (2) | 0.190 (4) | 0.0860 (19) | 0.020 (2) | 0.0392 (17) | 0.005 (2) |
O41 | 0.228 (17) | 0.193 (16) | 0.099 (9) | −0.030 (13) | 0.095 (11) | −0.014 (10) |
O42 | 0.239 (19) | 0.162 (13) | 0.083 (8) | −0.019 (13) | 0.067 (10) | 0.019 (7) |
O43 | 0.189 (13) | 0.158 (12) | 0.131 (10) | −0.009 (11) | 0.069 (10) | 0.007 (9) |
O44 | 0.105 (12) | 0.32 (3) | 0.37 (4) | 0.005 (15) | 0.045 (18) | −0.02 (3) |
Al—O1 | 1.878 (3) | Cl2—O22 | 1.369 (7) |
Al—O2 | 1.883 (3) | Cl2—O231 | 1.296 (10) |
Al—O3 | 1.905 (3) | Cl2—O232 | 1.453 (18) |
Al—O4 | 1.870 (3) | Cl2—O241 | 1.380 (17) |
Al—O5 | 1.864 (3) | Cl2—O242 | 1.38 (2) |
Al—O6 | 1.887 (3) | O231—O232 | 0.59 (4) |
O1—C11 | 1.277 (5) | O231—O242 | 1.71 (3) |
O2—C21 | 1.265 (5) | O241—O242 | 0.90 (4) |
O3—C31 | 1.271 (5) | Cl3—O31 | 1.296 (9) |
O4—C41 | 1.204 (6) | Cl3—O32 | 1.329 (8) |
O5—C51 | 1.228 (6) | Cl3—O331 | 1.363 (13) |
O6—C61 | 1.267 (5) | Cl3—O332 | 1.357 (14) |
N1—C11 | 1.302 (5) | Cl3—O341 | 1.436 (13) |
N1—C13 | 1.472 (7) | Cl3—O342 | 1.266 (15) |
N1—C14 | 1.450 (8) | O31—O342 | 1.78 (2) |
N2—C21 | 1.304 (6) | O331—O332 | 1.24 (3) |
N2—C23 | 1.462 (6) | O341—O342 | 1.12 (2) |
N2—C24 | 1.446 (7) | O7—C71 | 1.280 (8) |
N3—C31 | 1.303 (6) | O7—H7 | 1.192 |
N3—C33 | 1.463 (6) | N7—C71 | 1.301 (8) |
N3—C34 | 1.477 (6) | N7—C73 | 1.453 (9) |
N4—C41 | 1.186 (8) | N7—C74 | 1.444 (11) |
N4—C43 | 1.633 (10) | C71—C72 | 1.466 (11) |
N4—C44 | 1.414 (8) | Cl4—O41i | 1.388 (10) |
N5—C51 | 1.213 (7) | Cl4—O41 | 1.388 (10) |
N5—C53 | 1.430 (7) | Cl4—O42 | 1.361 (10) |
N5—C54 | 1.574 (9) | Cl4—O42i | 1.361 (10) |
N6—C61 | 1.301 (6) | Cl4—O43 | 1.483 (11) |
N6—C63 | 1.478 (6) | Cl4—O43i | 1.483 (10) |
N6—C64 | 1.461 (7) | Cl4—O44i | 1.385 (11) |
C11—C12 | 1.485 (7) | Cl4—O44 | 1.385 (11) |
C21—C22 | 1.490 (7) | O41—O42i | 1.48 (2) |
C31—C32 | 1.505 (6) | O41—O44i | 1.48 (3) |
C41—C42 | 1.610 (10) | O42—O41i | 1.48 (2) |
C51—C52 | 1.579 (8) | O42—O43i | 1.80 (2) |
C61—C62 | 1.493 (7) | O42—O44i | 1.37 (3) |
Cl1—O11 | 1.404 (4) | O43—O42i | 1.80 (2) |
Cl1—O12 | 1.387 (5) | O43—O44i | 1.81 (3) |
Cl1—O13 | 1.377 (5) | O44—O41i | 1.48 (3) |
Cl1—O14 | 1.376 (5) | O44—O42i | 1.37 (3) |
Cl2—O21 | 1.403 (5) | O44—O43i | 1.81 (3) |
O1—Al—O2 | 178.31 (15) | Cl2—O241—O242 | 71 (2) |
O1—Al—O3 | 92.67 (13) | Cl2—O242—O231 | 48.1 (9) |
O1—Al—O4 | 91.33 (14) | Cl2—O242—O241 | 71 (2) |
O1—Al—O5 | 89.21 (14) | O231—O242—O241 | 112 (3) |
O1—Al—O6 | 90.03 (14) | O31—Cl3—O32 | 104.1 (8) |
O2—Al—O3 | 85.74 (13) | O31—Cl3—O331 | 87.7 (15) |
O2—Al—O4 | 87.98 (14) | O31—Cl3—O332 | 136.9 (11) |
O2—Al—O5 | 92.33 (14) | O31—Cl3—O341 | 113.0 (9) |
O2—Al—O6 | 90.66 (13) | O31—Cl3—O342 | 88.3 (12) |
O3—Al—O4 | 86.65 (14) | O32—Cl3—O331 | 105.1 (9) |
O3—Al—O5 | 175.86 (15) | O32—Cl3—O332 | 104.6 (12) |
O3—Al—O6 | 93.57 (13) | O32—Cl3—O341 | 92.5 (10) |
O4—Al—O5 | 89.63 (16) | O32—Cl3—O342 | 140.1 (13) |
O4—Al—O6 | 178.61 (15) | O331—Cl3—O332 | 54.0 (14) |
O5—Al—O6 | 90.12 (15) | O331—Cl3—O341 | 148.9 (15) |
Al—O1—C11 | 141.3 (3) | O331—Cl3—O342 | 113.3 (15) |
Al—O2—C21 | 145.7 (3) | O332—Cl3—O341 | 97.2 (8) |
Al—O3—C31 | 138.6 (3) | O332—Cl3—O342 | 89.9 (16) |
Al—O4—C41 | 153.3 (4) | O341—Cl3—O342 | 48.3 (11) |
Al—O5—C51 | 152.9 (4) | Cl3—O31—O342 | 45.2 (7) |
Al—O6—C61 | 143.6 (3) | Cl3—O331—O332 | 62.7 (11) |
C11—N1—C13 | 123.2 (5) | Cl3—O332—O331 | 63.3 (11) |
C11—N1—C14 | 120.2 (5) | Cl3—O341—O342 | 57.9 (10) |
C13—N1—C14 | 116.4 (5) | Cl3—O342—O31 | 46.5 (8) |
C21—N2—C23 | 123.5 (5) | Cl3—O342—O341 | 73.8 (14) |
C21—N2—C24 | 121.5 (4) | O31—O342—O341 | 101 (2) |
C23—N2—C24 | 115.0 (5) | C71—O7—H7 | 119.4 |
C31—N3—C33 | 120.8 (4) | C71—N7—C73 | 122.1 (8) |
C31—N3—C34 | 122.7 (4) | C71—N7—C74 | 120.5 (7) |
C33—N3—C34 | 116.4 (4) | C73—N7—C74 | 117.2 (8) |
C41—N4—C43 | 107.3 (7) | O7—C71—N7 | 117.6 (8) |
C41—N4—C44 | 138.4 (9) | O7—C71—C72 | 119.4 (7) |
C43—N4—C44 | 114.3 (7) | N7—C71—C72 | 123.1 (8) |
C51—N5—C53 | 133.5 (7) | O41—Cl4—O41i | 180.0 (6) |
C51—N5—C54 | 111.2 (6) | O41—Cl4—O42 | 115.1 (8) |
C53—N5—C54 | 115.3 (6) | O41—Cl4—O42i | 64.9 (8) |
C61—N6—C63 | 123.0 (4) | O41i—Cl4—O42 | 64.9 (8) |
C61—N6—C64 | 120.3 (4) | O41i—Cl4—O42i | 115.1 (8) |
C63—N6—C64 | 116.6 (4) | O41—Cl4—O43 | 98.1 (8) |
O1—C11—N1 | 118.7 (4) | O41—Cl4—O43i | 81.9 (8) |
O1—C11—C12 | 121.7 (4) | O41i—Cl4—O43 | 81.9 (8) |
N1—C11—C12 | 119.6 (4) | O41i—Cl4—O43i | 98.1 (8) |
O2—C21—N2 | 119.2 (5) | O41—Cl4—O44 | 115.4 (15) |
O2—C21—C22 | 121.0 (4) | O41—Cl4—O44i | 64.6 (15) |
N2—C21—C22 | 119.8 (4) | O41i—Cl4—O44 | 64.6 (15) |
O3—C31—N3 | 119.7 (4) | O41i—Cl4—O44i | 115.4 (15) |
O3—C31—C32 | 121.2 (4) | O42—Cl4—O42i | 180.0 (7) |
N3—C31—C32 | 119.1 (4) | O42—Cl4—O43 | 101.4 (9) |
O4—C41—N4 | 134.9 (8) | O42—Cl4—O43i | 78.6 (9) |
O4—C41—C42 | 116.8 (6) | O42i—Cl4—O43 | 78.6 (9) |
N4—C41—C42 | 108.2 (7) | O42i—Cl4—O43i | 101.4 (9) |
O5—C51—N5 | 130.6 (7) | O42—Cl4—O44 | 119.9 (14) |
O5—C51—C52 | 119.4 (6) | O42—Cl4—O44i | 60.1 (14) |
N5—C51—C52 | 109.9 (6) | O42i—Cl4—O44 | 60.1 (14) |
O6—C61—N6 | 120.7 (4) | O42i—Cl4—O44i | 119.9 (14) |
O6—C61—C62 | 120.6 (4) | O43—Cl4—O43i | 180.0 (13) |
N6—C61—C62 | 118.7 (4) | O43—Cl4—O44 | 101.7 (12) |
O11—Cl1—O12 | 112.2 (4) | O43—Cl4—O44i | 78.3 (12) |
O11—Cl1—O13 | 108.6 (4) | O43i—Cl4—O44 | 78.3 (12) |
O11—Cl1—O14 | 109.2 (4) | O43i—Cl4—O44i | 101.7 (12) |
O12—Cl1—O13 | 107.0 (5) | O44i—Cl4—O44 | 180 (4) |
O12—Cl1—O14 | 112.0 (4) | Cl4—O41—O42i | 56.6 (6) |
O13—Cl1—O14 | 107.6 (5) | Cl4—O41—O44i | 57.6 (9) |
O21—Cl2—O22 | 110.8 (4) | O42i—O41—O44i | 107.0 (12) |
O21—Cl2—O231 | 113.5 (9) | Cl4—O42—O41i | 58.4 (6) |
O21—Cl2—O232 | 107.2 (10) | Cl4—O42—O43i | 53.7 (6) |
O21—Cl2—O241 | 111.6 (9) | Cl4—O42—O44i | 60.8 (9) |
O21—Cl2—O242 | 109.3 (14) | O41i—O42—O43i | 82.1 (10) |
O22—Cl2—O231 | 115.8 (10) | O41i—O42—O44i | 110.6 (13) |
O22—Cl2—O232 | 99.5 (11) | O43i—O42—O44i | 87.7 (14) |
O22—Cl2—O241 | 91.4 (12) | Cl4—O43—O42i | 47.7 (5) |
O22—Cl2—O242 | 124.7 (13) | Cl4—O43—O44i | 48.4 (6) |
O231—Cl2—O241 | 111.9 (14) | O42i—O43—O44i | 82.2 (10) |
O231—Cl2—O242 | 79.4 (15) | Cl4—O44—O41i | 57.8 (9) |
O232—Cl2—O241 | 132.6 (15) | Cl4—O44—O42i | 59.1 (8) |
O232—Cl2—O242 | 103.2 (16) | Cl4—O44—O43i | 53.3 (7) |
Cl2—O231—O232 | 93 (3) | O41i—O44—O42i | 108.5 (12) |
Cl2—O231—O242 | 52.4 (10) | O41i—O44—O43i | 81.7 (13) |
O232—O231—O242 | 145 (3) | O42i—O44—O43i | 86.3 (14) |
Cl2—O232—O231 | 63 (2) | ||
Al—O1—C11—N1 | −177.3 (3) | O242—Cl2—O231—O232 | −174 (4) |
Al—O1—C11—C12 | 2.3 (7) | O242—Cl2—O232—O231 | 6 (4) |
Al—O2—C21—N2 | −180.0 (4) | O242—O231—O232—Cl2 | −8 (6) |
Al—O2—C21—C22 | 1.2 (8) | Cl3—O31—O342—O341 | −54.8 (14) |
Al—O3—C31—N3 | 149.3 (4) | Cl3—O341—O342—O31 | 38.1 (7) |
Al—O3—C31—C32 | −33.1 (7) | O31—Cl3—O331—O332 | 158.8 (17) |
Al—O4—C41—N4 | 138.8 (8) | O31—Cl3—O332—O331 | −32 (2) |
Al—O4—C41—C42 | −44.5 (11) | O31—Cl3—O341—O342 | −65 (2) |
Al—O5—C51—N5 | −164.4 (5) | O31—Cl3—O342—O341 | 123.4 (18) |
Al—O5—C51—C52 | 17.1 (10) | O32—Cl3—O31—O342 | 141.6 (14) |
Al—O6—C61—N6 | 146.8 (4) | O32—Cl3—O331—O332 | −97.2 (16) |
Al—O6—C61—C62 | −33.9 (8) | O32—Cl3—O332—O331 | 98.2 (15) |
O1—Al—O3—C31 | 64.2 (4) | O32—Cl3—O341—O342 | −172 (2) |
O1—Al—O4—C41 | 80.3 (9) | O32—Cl3—O342—O31 | −110.1 (18) |
O1—Al—O5—C51 | 23.7 (8) | O32—Cl3—O342—O341 | 13 (3) |
O1—Al—O6—C61 | 147.9 (5) | O331—Cl3—O31—O342 | −113.4 (15) |
O2—Al—O3—C31 | −115.2 (4) | O331—Cl3—O341—O342 | 63 (3) |
O2—Al—O4—C41 | −101.3 (9) | O331—Cl3—O342—O31 | 86.7 (17) |
O2—Al—O5—C51 | −157.0 (8) | O331—Cl3—O342—O341 | −150 (2) |
O2—Al—O6—C61 | −30.5 (5) | O332—Cl3—O31—O342 | −88.1 (18) |
O3—Al—O1—C11 | 43.6 (5) | O332—Cl3—O341—O342 | 83 (2) |
O3—Al—O2—C21 | −148.2 (6) | O332—Cl3—O342—O31 | 136.9 (11) |
O3—Al—O4—C41 | 172.9 (9) | O332—Cl3—O342—O341 | −99.7 (18) |
O3—Al—O6—C61 | 55.2 (5) | O341—Cl3—O31—O342 | 42.6 (14) |
O4—Al—O1—C11 | 130.3 (5) | O341—Cl3—O331—O332 | 25 (3) |
O4—Al—O2—C21 | 125.0 (6) | O341—Cl3—O332—O331 | −167.2 (15) |
O4—Al—O3—C31 | −27.0 (4) | O341—Cl3—O342—O31 | −123.4 (18) |
O4—Al—O5—C51 | 115.0 (8) | O342—Cl3—O331—O332 | 72 (2) |
O5—Al—O1—C11 | −140.1 (5) | O342—Cl3—O332—O331 | −119.3 (18) |
O5—Al—O2—C21 | 35.5 (6) | C73—N7—C71—O7 | 179.1 (7) |
O5—Al—O4—C41 | −8.9 (9) | C73—N7—C71—C72 | −0.6 (11) |
O5—Al—O6—C61 | −122.9 (5) | C74—N7—C71—O7 | 4.5 (11) |
O6—Al—O1—C11 | −50.0 (5) | C74—N7—C71—C72 | −175.1 (8) |
O6—Al—O2—C21 | −54.6 (6) | H7—O7—C71—N7 | 172.7 |
O6—Al—O3—C31 | 154.4 (4) | H7—O7—C71—C72 | −7.7 |
O6—Al—O5—C51 | −66.3 (8) | O41—Cl4—O42—O41i | 180.000 (9) |
C13—N1—C11—O1 | −178.7 (5) | O41—Cl4—O42—O43i | −75.4 (11) |
C13—N1—C11—C12 | 1.6 (7) | O41i—Cl4—O42—O43i | 104.6 (11) |
C14—N1—C11—O1 | −4.0 (7) | O41—Cl4—O42—O44i | 35.4 (18) |
C14—N1—C11—C12 | 176.3 (5) | O41i—Cl4—O42—O44i | −144.6 (18) |
C23—N2—C21—O2 | 178.4 (5) | O41—Cl4—O43—O42i | 62.3 (9) |
C23—N2—C21—C22 | −2.7 (7) | O41i—Cl4—O43—O42i | −117.7 (9) |
C24—N2—C21—O2 | 0.7 (7) | O41—Cl4—O43—O44i | −61.9 (16) |
C24—N2—C21—C22 | 179.6 (5) | O41i—Cl4—O43—O44i | 118.1 (16) |
C33—N3—C31—O3 | −4.2 (7) | O41—Cl4—O44—O41i | 180.000 (11) |
C33—N3—C31—C32 | 178.2 (5) | O41—Cl4—O44—O42i | −35.5 (17) |
C34—N3—C31—O3 | 175.6 (5) | O41i—Cl4—O44—O42i | 144.5 (17) |
C34—N3—C31—C32 | −2.0 (7) | O41—Cl4—O44—O43i | 75.1 (12) |
C43—N4—C41—O4 | −0.8 (10) | O41i—Cl4—O44—O43i | −104.9 (12) |
C43—N4—C41—C42 | −177.7 (6) | O42—Cl4—O41—O42i | 180.000 (8) |
C44—N4—C41—O4 | 177.6 (7) | O42—Cl4—O41—O44i | −33.7 (17) |
C44—N4—C41—C42 | 0.7 (11) | O42i—Cl4—O41—O44i | 146.3 (17) |
C53—N5—C51—O5 | −179.3 (6) | O42—Cl4—O43—O42i | 180.000 (2) |
C53—N5—C51—C52 | −0.7 (9) | O42—Cl4—O43—O44i | 55.8 (15) |
C54—N5—C51—O5 | 1.3 (8) | O42i—Cl4—O43—O44i | −124.2 (15) |
C54—N5—C51—C52 | 179.9 (5) | O42—Cl4—O44—O41i | 35.5 (17) |
C63—N6—C61—O6 | −178.8 (5) | O42i—Cl4—O44—O41i | −144.5 (17) |
C63—N6—C61—C62 | 1.9 (7) | O42—Cl4—O44—O42i | 180.000 (9) |
C64—N6—C61—O6 | −1.5 (7) | O42—Cl4—O44—O43i | −69.4 (14) |
C64—N6—C61—C62 | 179.2 (6) | O42i—Cl4—O44—O43i | 110.6 (14) |
Cl2—O231—O242—O241 | −33 (3) | O43—Cl4—O41—O42i | −73.4 (11) |
Cl2—O241—O242—O231 | 25 (2) | O43i—Cl4—O41—O42i | 106.6 (11) |
O21—Cl2—O231—O232 | 79 (4) | O43—Cl4—O41—O44i | 72.9 (14) |
O21—Cl2—O231—O242 | −106.6 (14) | O43i—Cl4—O41—O44i | −107.1 (14) |
O21—Cl2—O232—O231 | −109 (4) | O43—Cl4—O42—O41i | 75.4 (11) |
O21—Cl2—O241—O242 | 94 (3) | O43i—Cl4—O42—O41i | −104.6 (11) |
O21—Cl2—O242—O231 | 111.3 (10) | O43—Cl4—O42—O43i | 180.0 |
O21—Cl2—O242—O241 | −101 (3) | O43—Cl4—O42—O44i | −69.3 (16) |
O22—Cl2—O231—O232 | −50 (4) | O43i—Cl4—O42—O44i | 110.7 (16) |
O22—Cl2—O231—O242 | 123.6 (15) | O43—Cl4—O44—O41i | −75.1 (12) |
O22—Cl2—O232—O231 | 135 (4) | O43i—Cl4—O44—O41i | 104.9 (12) |
O22—Cl2—O241—O242 | −153 (3) | O43—Cl4—O44—O42i | 69.4 (14) |
O22—Cl2—O242—O231 | −114.1 (13) | O43i—Cl4—O44—O42i | −110.6 (14) |
O22—Cl2—O242—O241 | 34 (4) | O43—Cl4—O44—O43i | 180.0 |
O231—Cl2—O241—O242 | −34 (3) | O44—Cl4—O41—O42i | 33.7 (17) |
O231—Cl2—O242—O241 | 148 (3) | O44i—Cl4—O41—O42i | −146.3 (17) |
O232—Cl2—O231—O242 | 174 (4) | O44—Cl4—O41—O44i | 180.000 (11) |
O232—Cl2—O241—O242 | −48 (4) | O44—Cl4—O42—O41i | −35.4 (18) |
O232—Cl2—O242—O231 | −2.5 (18) | O44i—Cl4—O42—O41i | 144.6 (18) |
O232—Cl2—O242—O241 | 146 (3) | O44—Cl4—O42—O43i | 69.3 (15) |
O232—O231—O242—Cl2 | 10 (8) | O44i—Cl4—O42—O43i | −110.7 (15) |
O232—O231—O242—O241 | −22 (9) | O44—Cl4—O42—O44i | 180.000 (11) |
O241—Cl2—O231—O232 | −153 (4) | O44—Cl4—O43—O42i | −55.8 (15) |
O241—Cl2—O231—O242 | 21 (2) | O44i—Cl4—O43—O42i | 124.2 (15) |
O241—Cl2—O232—O231 | 34 (5) | O44—Cl4—O43—O44i | 180.0 |
O241—Cl2—O242—O231 | −148 (3) |
Symmetry code: (i) −x+1, −y, −z+1. |