In the title compound, bis[hexakis(N,N-dimethylacetamide)aluminium(III)] bis(N,N-dimethylacetamide)ium heptakis(perchlorate), [H(C4H9NO)2][Al(C4H9NO)6]2(ClO4)7, the AlIII ion has an octahedral coordination environment. The singly charged cation lies on a centre of inversion. One of the anions lies on an inversion centre and is disordered; a second anion is also disordered. Three Al-O-C-N torsion angles deviate significantly from 180°, indicating that the Al-O bonds are displaced from the direction of the lone pair of the sp2 O atom. This is ascribed to the steric hindrance of the ligand in an octahedral environment.
Supporting information
CCDC reference: 601144
Key indicators
- Single-crystal X-ray study
- T = 297 K
- Mean (C-C) = 0.009 Å
- Disorder in solvent or counterion
- R factor = 0.078
- wR factor = 0.244
- Data-to-parameter ratio = 14.0
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT355_ALERT_3_A Long O-H Bond (0.82A) O7 - H7 ... 1.19 Ang.
| Author Response: see _publ_section_comment
|
Alert level B
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for N7
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C71
PLAT420_ALERT_2_B D-H Without Acceptor O7 - H7 ... ?
PLAT432_ALERT_2_B Short Inter X...Y Contact O44 .. C74 .. 2.90 Ang.
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.87
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.80 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N6
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C41
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O232
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O241
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O242
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O331
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O332
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O342
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl4
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl2
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for O231
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl3
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 29.00 Perc.
PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C12
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C72
PLAT432_ALERT_2_C Short Inter X...Y Contact O41 .. C12 .. 3.01 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.16 Ratio
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4
Cl O4
Alert level G
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
From the CIF: _diffrn_reflns_theta_max 69.93
From the CIF: _reflns_number_total 8716
From the CIF: _diffrn_reflns_limit_ max hkl 23. 13. 23.
From the CIF: _diffrn_reflns_limit_ min hkl -27. 0. 0.
TEST1: Expected hkl limits for theta max
Calculated maximum hkl 27. 13. 27.
Calculated minimum hkl -27. -13. -27.
1 ALERT level A = In general: serious problem
4 ALERT level B = Potentially serious problem
26 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
10 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
16 ALERT type 4 Improvement, methodology, query or suggestion
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.
bis[hexakis(
N,
N-dimethylacetamide)aluminium(III)]
bis(
N,
N-dimethylacetamide)ium heptakis(perchlorate)
top
Crystal data top
(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 | |
Data collection top
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 top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.078 | 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 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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 |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |