N,N-Dimethyl­acetamide complex of aluminium(III) perchlorate

Suzuki, H.; Ishiguro, S.

doi:10.1107/S1600536806005575

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N,N-Dimethylacetamide complex of aluminium(III) perchlorate

H. Suzuki and S. Ishiguro

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 Al^III 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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806005575/ci6753sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806005575/ci6753Isup2.hkl Contains datablock I

CCDC reference: 601144

checkCIF report

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

Computing details top

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
M_r = 1970.82	D_x = 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	R_int = 0.034
Graphite monochromator	θ_max = 69.9°, θ_min = 2.3°
ω–2θ scans	h = −27→23
Absorption correction: ψ scan (North et al., 1968)	k = 0→13
T_min = 0.318, T_max = 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(F_o²) + (0.1096P)² + 5.6858P] where P = (F_o² + 2F_c²)/3
8716 reflections	(Δ/σ)_max = 0.001
623 parameters	Δρ_max = 0.58 e Å⁻³
6 restraints	Δρ_min = −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	U_iso*/U_eq	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.

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