Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807028152/dn2188sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807028152/dn2188Isup2.hkl |
CCDC reference: 634333
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.001 Å
- R factor = 0.024
- wR factor = 0.064
- Data-to-parameter ratio = 22.3
checkCIF/PLATON results
No syntax errors found Datablock: I
Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H32 .. H91 .. 2.08 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT417_ALERT_2_C Short Inter D-H..H-D H51 .. H71 .. 2.13 Ang. PLAT417_ALERT_2_C Short Inter D-H..H-D H72 .. H101 .. 2.13 Ang.
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Al1 (3) 2.98
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For the crystal structure of the title compound at 293 K, see: Bataille (2003). For related literature, see: Aghabozorg et al. (2006).
A solution of Al2(SO4)3.18H2O (333 mg, 0.5 mmol) in water (10 ml) was added to an aqueous solution of the proton-transfer compound (pipzH2)(pydc) (Aghabozorg et al., 2006) (506 mg, 2 mmol) in water (20 ml). Colorless crystals of (I) were obtained after allowing the mixture to stand for seven weeks at room temperature.
All H atoms were located in difference Fourier maps but they were treated in the refinement as riding on their parent atoms with Uiso(H) = 1.2Ueq(C or N). H or Uiso(H) = 1.5Ueq(O).
In this work, our goal was the generation of the self-assembling coordination compound using a self-assembling ligand. The structure of the Al(III) complex was reported recently (Bataille, 2003), but the goal and method of synthesis were completely different from ours. The data collection temperature in our work was 100 K, whereas, the previous work was conducted at room temperature. For our complex, the final R value was 0.0237, whereas in the reported structure it was 0.0384. In the present study the measured reflections was 4639, while in the earlier work it was 2991.
As previously observed (Bataille, 2003), the structure of (I) consists of Al3+ ions octahedrally coordinated to six water molecules, together with sulfate tetrahedra, piperazinium cations (lying about inversion centres) and non-bonded water molecules, linked by hydrogen bonds only (Fig. 1, Table 1). All the O—H···O and N—H···O hydrogen bonds build up a three dimensionnal network as previously reported (Table 1).
For the crystal structure of the title compound at 293 K, see: Bataille (2003). For related literature, see: Aghabozorg et al. (2006).
Data collection: APEX2 (Bruker, 2005); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXTL (Sheldrick, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL.
(C4H12N2)0.5[Al(H2O)6](SO4)2·4H2O | F(000) = 936 |
Mr = 443.34 | Dx = 1.746 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 9176 reflections |
a = 6.5438 (3) Å | θ = 3.1–33.5° |
b = 11.9938 (5) Å | µ = 0.46 mm−1 |
c = 21.4916 (9) Å | T = 100 K |
β = 90.164 (1)° | Needle, colourless |
V = 1686.76 (13) Å3 | 0.55 × 0.50 × 0.45 mm |
Z = 4 |
Bruker APEXII CCD area-detector diffractometer | 4639 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.017 |
Graphite monochromator | θmax = 30.0°, θmin = 1.9° |
ω scans | h = −9→9 |
21192 measured reflections | k = −16→16 |
4847 independent reflections | l = −30→30 |
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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0314P)2 + 0.8179P] where P = (Fo2 + 2Fc2)/3 |
4847 reflections | (Δ/σ)max = 0.002 |
217 parameters | Δρmax = 0.45 e Å−3 |
0 restraints | Δρmin = −0.43 e Å−3 |
(C4H12N2)0.5[Al(H2O)6](SO4)2·4H2O | V = 1686.76 (13) Å3 |
Mr = 443.34 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 6.5438 (3) Å | µ = 0.46 mm−1 |
b = 11.9938 (5) Å | T = 100 K |
c = 21.4916 (9) Å | 0.55 × 0.50 × 0.45 mm |
β = 90.164 (1)° |
Bruker APEXII CCD area-detector diffractometer | 4639 reflections with I > 2σ(I) |
21192 measured reflections | Rint = 0.017 |
4847 independent reflections |
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.12 | Δρmax = 0.45 e Å−3 |
4847 reflections | Δρmin = −0.43 e Å−3 |
217 parameters |
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 | ||
Al1 | 0.46318 (4) | 0.06332 (2) | 0.367174 (13) | 0.00638 (6) | |
S1 | −0.04729 (3) | −0.026950 (19) | 0.191802 (10) | 0.00698 (6) | |
S2 | −0.03384 (3) | 0.191544 (19) | 0.543172 (10) | 0.00664 (6) | |
O11 | 0.15644 (11) | 0.00561 (7) | 0.21597 (3) | 0.01263 (14) | |
O12 | −0.16492 (11) | −0.08210 (6) | 0.24163 (3) | 0.01111 (13) | |
O13 | −0.15781 (11) | 0.07318 (6) | 0.16977 (3) | 0.01059 (13) | |
O14 | −0.02011 (11) | −0.10239 (6) | 0.13764 (3) | 0.01058 (13) | |
O21 | 0.03790 (11) | 0.10582 (6) | 0.58850 (3) | 0.01070 (13) | |
O22 | −0.23346 (11) | 0.15446 (6) | 0.51731 (3) | 0.01083 (13) | |
O23 | −0.06166 (12) | 0.29846 (6) | 0.57654 (3) | 0.01124 (14) | |
O24 | 0.11598 (12) | 0.20524 (6) | 0.49313 (4) | 0.01263 (14) | |
O91 | 0.70177 (11) | 0.13100 (6) | 0.39764 (3) | 0.00987 (13) | |
H11 | 0.7381 | 0.1366 | 0.4396 | 0.015* | |
H12 | 0.7911 | 0.1736 | 0.3719 | 0.015* | |
O92 | 0.58088 (11) | −0.07843 (6) | 0.37551 (3) | 0.00921 (13) | |
H21 | 0.5367 | −0.1358 | 0.3490 | 0.014* | |
H22 | 0.7117 | −0.0898 | 0.3904 | 0.014* | |
O93 | 0.34321 (11) | 0.20329 (6) | 0.35718 (3) | 0.00985 (13) | |
H31 | 0.4107 | 0.2713 | 0.3579 | 0.015* | |
H32 | 0.2067 | 0.2122 | 0.3475 | 0.015* | |
O94 | 0.22216 (11) | −0.00281 (6) | 0.33634 (3) | 0.00985 (13) | |
H41 | 0.1923 | −0.0035 | 0.2948 | 0.015* | |
H42 | 0.1263 | −0.0395 | 0.3618 | 0.015* | |
O95 | 0.56726 (11) | 0.07184 (6) | 0.28547 (3) | 0.00972 (13) | |
H51 | 0.5402 | 0.1244 | 0.2538 | 0.015* | |
H52 | 0.6632 | 0.0199 | 0.2693 | 0.015* | |
O96 | 0.36145 (11) | 0.05062 (6) | 0.44869 (3) | 0.00899 (13) | |
H61 | 0.2661 | 0.1014 | 0.4637 | 0.013* | |
H62 | 0.3291 | −0.0208 | 0.4604 | 0.013* | |
C1 | 0.21352 (15) | −0.03328 (9) | −0.00316 (5) | 0.01139 (17) | |
H1A | 0.3297 | −0.0764 | 0.0140 | 0.014* | |
H1B | 0.2622 | 0.0082 | −0.0401 | 0.014* | |
N2 | 0.13773 (13) | 0.04702 (7) | 0.04474 (4) | 0.01019 (15) | |
H21N | 0.2469 | 0.0966 | 0.0571 | 0.012* | |
H22N | 0.0929 | 0.0036 | 0.0808 | 0.012* | |
C3 | 0.04290 (15) | −0.11226 (8) | −0.02208 (5) | 0.01135 (17) | |
H3A | 0.0914 | −0.1625 | −0.0555 | 0.014* | |
H3B | 0.0028 | −0.1586 | 0.0140 | 0.014* | |
O97 | 0.46083 (11) | 0.23332 (6) | 0.20641 (3) | 0.01154 (14) | |
H71 | 0.5473 | 0.2917 | 0.2201 | 0.017* | |
H72 | 0.4663 | 0.2247 | 0.1630 | 0.017* | |
O98 | 0.46950 (11) | −0.03204 (6) | 0.13234 (3) | 0.01213 (14) | |
H81 | 0.3761 | −0.0178 | 0.1645 | 0.018* | |
H82 | 0.5871 | 0.0082 | 0.1394 | 0.018* | |
O99 | −0.03940 (11) | 0.25482 (6) | 0.33251 (3) | 0.01119 (13) | |
H91 | −0.0342 | 0.3254 | 0.3500 | 0.017* | |
H92 | −0.0442 | 0.2657 | 0.2883 | 0.017* | |
O910 | 0.02956 (12) | 0.26417 (6) | 0.20367 (4) | 0.01238 (14) | |
H101 | 0.1734 | 0.2544 | 0.2030 | 0.019* | |
H102 | −0.0246 | 0.1950 | 0.1915 | 0.019* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al1 | 0.00647 (12) | 0.00660 (13) | 0.00607 (12) | −0.00009 (9) | 0.00003 (9) | 0.00003 (9) |
S1 | 0.00685 (10) | 0.00767 (10) | 0.00641 (10) | 0.00039 (7) | 0.00017 (7) | 0.00016 (7) |
S2 | 0.00686 (10) | 0.00652 (10) | 0.00655 (10) | 0.00020 (7) | 0.00028 (7) | 0.00008 (7) |
O11 | 0.0081 (3) | 0.0195 (4) | 0.0103 (3) | −0.0020 (3) | −0.0016 (2) | −0.0005 (3) |
O12 | 0.0118 (3) | 0.0117 (3) | 0.0099 (3) | 0.0006 (3) | 0.0035 (2) | 0.0028 (2) |
O13 | 0.0119 (3) | 0.0073 (3) | 0.0126 (3) | 0.0018 (2) | −0.0009 (2) | 0.0012 (2) |
O14 | 0.0139 (3) | 0.0095 (3) | 0.0083 (3) | 0.0017 (3) | 0.0005 (2) | −0.0017 (2) |
O21 | 0.0089 (3) | 0.0105 (3) | 0.0127 (3) | 0.0008 (2) | −0.0013 (2) | 0.0045 (2) |
O22 | 0.0099 (3) | 0.0129 (3) | 0.0097 (3) | −0.0026 (3) | −0.0030 (2) | 0.0013 (3) |
O23 | 0.0142 (3) | 0.0085 (3) | 0.0110 (3) | 0.0025 (3) | −0.0014 (3) | −0.0031 (2) |
O24 | 0.0135 (3) | 0.0111 (3) | 0.0133 (3) | −0.0001 (3) | 0.0069 (3) | 0.0009 (3) |
O91 | 0.0095 (3) | 0.0125 (3) | 0.0076 (3) | −0.0034 (2) | −0.0011 (2) | 0.0007 (2) |
O92 | 0.0087 (3) | 0.0080 (3) | 0.0109 (3) | 0.0013 (2) | −0.0018 (2) | −0.0008 (2) |
O93 | 0.0083 (3) | 0.0070 (3) | 0.0142 (3) | 0.0001 (2) | −0.0004 (2) | 0.0008 (2) |
O94 | 0.0089 (3) | 0.0126 (3) | 0.0081 (3) | −0.0030 (2) | −0.0014 (2) | 0.0008 (2) |
O95 | 0.0110 (3) | 0.0110 (3) | 0.0071 (3) | 0.0025 (2) | 0.0016 (2) | 0.0014 (2) |
O96 | 0.0107 (3) | 0.0081 (3) | 0.0082 (3) | 0.0000 (2) | 0.0017 (2) | 0.0005 (2) |
C1 | 0.0094 (4) | 0.0137 (4) | 0.0110 (4) | 0.0004 (3) | 0.0003 (3) | −0.0022 (3) |
N2 | 0.0103 (4) | 0.0112 (4) | 0.0091 (4) | −0.0012 (3) | −0.0011 (3) | −0.0004 (3) |
C3 | 0.0122 (4) | 0.0102 (4) | 0.0117 (4) | 0.0008 (3) | −0.0021 (3) | −0.0008 (3) |
O97 | 0.0146 (3) | 0.0111 (3) | 0.0089 (3) | −0.0003 (3) | −0.0001 (2) | 0.0011 (2) |
O98 | 0.0106 (3) | 0.0126 (3) | 0.0131 (3) | −0.0005 (3) | 0.0006 (3) | 0.0000 (3) |
O99 | 0.0110 (3) | 0.0104 (3) | 0.0122 (3) | 0.0001 (3) | 0.0002 (2) | 0.0014 (3) |
O910 | 0.0129 (3) | 0.0086 (3) | 0.0156 (3) | −0.0001 (3) | −0.0009 (3) | 0.0006 (3) |
Al1—O93 | 1.8654 (8) | O95—H51 | 0.9440 |
Al1—O92 | 1.8748 (8) | O95—H52 | 0.9504 |
Al1—O91 | 1.8760 (8) | O96—H61 | 0.9304 |
Al1—O96 | 1.8820 (8) | O96—H62 | 0.9177 |
Al1—O94 | 1.8841 (8) | C1—N2 | 1.4954 (13) |
Al1—O95 | 1.8880 (8) | C1—C3 | 1.5187 (14) |
S1—O12 | 1.4770 (7) | C1—H1A | 0.9900 |
S1—O13 | 1.4791 (7) | C1—H1B | 0.9900 |
S1—O11 | 1.4818 (7) | N2—C3i | 1.4977 (13) |
S1—O14 | 1.4854 (7) | N2—H21N | 0.9666 |
S2—O24 | 1.4666 (7) | N2—H22N | 0.9802 |
S2—O23 | 1.4808 (7) | C3—N2i | 1.4977 (13) |
S2—O22 | 1.4862 (7) | C3—H3A | 0.9900 |
S2—O21 | 1.4913 (7) | C3—H3B | 0.9900 |
O91—H11 | 0.9343 | O97—H71 | 0.9466 |
O91—H12 | 0.9543 | O97—H72 | 0.9395 |
O92—H21 | 0.9386 | O98—H81 | 0.9403 |
O92—H22 | 0.9229 | O98—H82 | 0.9208 |
O93—H31 | 0.9273 | O99—H91 | 0.9268 |
O93—H32 | 0.9227 | O99—H92 | 0.9595 |
O94—H41 | 0.9126 | O910—H101 | 0.9484 |
O94—H42 | 0.9433 | O910—H102 | 0.9390 |
O93—Al1—O92 | 178.68 (4) | Al1—O93—H32 | 122.5 |
O93—Al1—O91 | 90.02 (3) | H31—O93—H32 | 111.3 |
O92—Al1—O91 | 91.02 (3) | Al1—O94—H41 | 121.6 |
O93—Al1—O96 | 91.73 (3) | Al1—O94—H42 | 123.3 |
O92—Al1—O96 | 89.08 (3) | H41—O94—H42 | 115.0 |
O91—Al1—O96 | 90.36 (3) | Al1—O95—H51 | 129.7 |
O93—Al1—O94 | 89.24 (3) | Al1—O95—H52 | 123.0 |
O92—Al1—O94 | 89.72 (3) | H51—O95—H52 | 107.3 |
O91—Al1—O94 | 179.26 (4) | Al1—O96—H61 | 120.6 |
O96—Al1—O94 | 89.73 (3) | Al1—O96—H62 | 114.4 |
O93—Al1—O95 | 89.83 (3) | H61—O96—H62 | 111.1 |
O92—Al1—O95 | 89.36 (3) | N2—C1—C3 | 109.93 (8) |
O91—Al1—O95 | 89.95 (3) | N2—C1—H1A | 109.7 |
O96—Al1—O95 | 178.41 (4) | C3—C1—H1A | 109.7 |
O94—Al1—O95 | 89.97 (3) | N2—C1—H1B | 109.7 |
O12—S1—O13 | 109.90 (4) | C3—C1—H1B | 109.7 |
O12—S1—O11 | 109.52 (4) | H1A—C1—H1B | 108.2 |
O13—S1—O11 | 109.68 (5) | C1—N2—C3i | 112.06 (7) |
O12—S1—O14 | 111.05 (4) | C1—N2—H21N | 109.9 |
O13—S1—O14 | 107.65 (4) | C3i—N2—H21N | 110.5 |
O11—S1—O14 | 109.00 (4) | C1—N2—H22N | 107.7 |
O24—S2—O23 | 109.97 (5) | C3i—N2—H22N | 107.3 |
O24—S2—O22 | 110.36 (4) | H21N—N2—H22N | 109.3 |
O23—S2—O22 | 109.34 (4) | N2i—C3—C1 | 109.88 (8) |
O24—S2—O21 | 110.27 (4) | N2i—C3—H3A | 109.7 |
O23—S2—O21 | 108.64 (4) | C1—C3—H3A | 109.7 |
O22—S2—O21 | 108.22 (4) | N2i—C3—H3B | 109.7 |
Al1—O91—H11 | 125.3 | C1—C3—H3B | 109.7 |
Al1—O91—H12 | 122.7 | H3A—C3—H3B | 108.2 |
H11—O91—H12 | 111.5 | H71—O97—H72 | 111.4 |
Al1—O92—H21 | 118.7 | H81—O98—H82 | 109.1 |
Al1—O92—H22 | 123.2 | H91—O99—H92 | 106.2 |
H21—O92—H22 | 112.7 | H101—O910—H102 | 105.1 |
Al1—O93—H31 | 126.1 |
Symmetry code: (i) −x, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O91—H11···O22ii | 0.93 | 1.69 | 2.6205 (10) | 171 |
O91—H12···O99ii | 0.95 | 1.70 | 2.6546 (10) | 174 |
O92—H21···O910iii | 0.94 | 1.70 | 2.6411 (10) | 175 |
O92—H22···O21iv | 0.92 | 1.71 | 2.6302 (10) | 175 |
O93—H31···O14v | 0.93 | 1.68 | 2.6046 (10) | 176 |
O93—H32···O99 | 0.92 | 1.72 | 2.6313 (10) | 169 |
O94—H41···O11 | 0.91 | 1.71 | 2.6232 (10) | 174 |
O94—H42···O21vi | 0.94 | 1.71 | 2.6547 (10) | 177 |
O95—H51···O97 | 0.94 | 1.74 | 2.6677 (10) | 169 |
O95—H52···O12ii | 0.95 | 1.77 | 2.7161 (10) | 177 |
O96—H61···O24 | 0.93 | 1.71 | 2.6345 (10) | 173 |
O96—H62···O22vi | 0.92 | 1.79 | 2.6997 (10) | 173 |
N2—H21N···O23vii | 0.97 | 1.82 | 2.7864 (11) | 174 |
N2—H22N···O14 | 0.98 | 1.91 | 2.8769 (11) | 167 |
O97—H71···O12v | 0.95 | 1.89 | 2.8149 (10) | 166 |
O97—H72···O23vii | 0.94 | 1.89 | 2.8203 (10) | 172 |
O98—H81···O11 | 0.94 | 1.84 | 2.7663 (10) | 169 |
O98—H82···O13ii | 0.92 | 1.95 | 2.8594 (11) | 168 |
O99—H91···O98v | 0.93 | 1.80 | 2.7042 (11) | 164 |
O99—H92···O910 | 0.96 | 1.88 | 2.8091 (11) | 161 |
O910—H101···O97 | 0.95 | 1.90 | 2.8468 (11) | 177 |
O910—H102···O13 | 0.94 | 1.76 | 2.6974 (10) | 173 |
Symmetry codes: (ii) x+1, y, z; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x+1, −y, −z+1; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x, −y, −z+1; (vii) x+1/2, −y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | (C4H12N2)0.5[Al(H2O)6](SO4)2·4H2O |
Mr | 443.34 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 100 |
a, b, c (Å) | 6.5438 (3), 11.9938 (5), 21.4916 (9) |
β (°) | 90.164 (1) |
V (Å3) | 1686.76 (13) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.46 |
Crystal size (mm) | 0.55 × 0.50 × 0.45 |
Data collection | |
Diffractometer | Bruker APEXII CCD area-detector |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 21192, 4847, 4639 |
Rint | 0.017 |
(sin θ/λ)max (Å−1) | 0.703 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.065, 1.12 |
No. of reflections | 4847 |
No. of parameters | 217 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.45, −0.43 |
Computer programs: APEX2 (Bruker, 2005), APEX2, SHELXTL (Sheldrick, 1998), SHELXTL, ORTEP-3 for Windows (Farrugia, 1997).
D—H···A | D—H | H···A | D···A | D—H···A |
O91—H11···O22i | 0.93 | 1.69 | 2.6205 (10) | 171.1 |
O91—H12···O99i | 0.95 | 1.70 | 2.6546 (10) | 174.4 |
O92—H21···O910ii | 0.94 | 1.70 | 2.6411 (10) | 175.2 |
O92—H22···O21iii | 0.92 | 1.71 | 2.6302 (10) | 174.6 |
O93—H31···O14iv | 0.93 | 1.68 | 2.6046 (10) | 176.1 |
O93—H32···O99 | 0.92 | 1.72 | 2.6313 (10) | 169.2 |
O94—H41···O11 | 0.91 | 1.71 | 2.6232 (10) | 173.9 |
O94—H42···O21v | 0.94 | 1.71 | 2.6547 (10) | 176.7 |
O95—H51···O97 | 0.94 | 1.74 | 2.6677 (10) | 168.9 |
O95—H52···O12i | 0.95 | 1.77 | 2.7161 (10) | 177.0 |
O96—H61···O24 | 0.93 | 1.71 | 2.6345 (10) | 173.0 |
O96—H62···O22v | 0.92 | 1.79 | 2.6997 (10) | 172.8 |
N2—H21N···O23vi | 0.97 | 1.82 | 2.7864 (11) | 174.1 |
N2—H22N···O14 | 0.98 | 1.91 | 2.8769 (11) | 167.3 |
O97—H71···O12iv | 0.95 | 1.89 | 2.8149 (10) | 166.4 |
O97—H72···O23vi | 0.94 | 1.89 | 2.8203 (10) | 171.9 |
O98—H81···O11 | 0.94 | 1.84 | 2.7663 (10) | 169.1 |
O98—H82···O13i | 0.92 | 1.95 | 2.8594 (11) | 167.9 |
O99—H91···O98iv | 0.93 | 1.80 | 2.7042 (11) | 163.9 |
O99—H92···O910 | 0.96 | 1.88 | 2.8091 (11) | 161.3 |
O910—H101···O97 | 0.95 | 1.90 | 2.8468 (11) | 176.8 |
O910—H102···O13 | 0.94 | 1.76 | 2.6974 (10) | 172.6 |
Symmetry codes: (i) x+1, y, z; (ii) −x+1/2, y−1/2, −z+1/2; (iii) −x+1, −y, −z+1; (iv) −x+1/2, y+1/2, −z+1/2; (v) −x, −y, −z+1; (vi) x+1/2, −y+1/2, z−1/2. |
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In this work, our goal was the generation of the self-assembling coordination compound using a self-assembling ligand. The structure of the Al(III) complex was reported recently (Bataille, 2003), but the goal and method of synthesis were completely different from ours. The data collection temperature in our work was 100 K, whereas, the previous work was conducted at room temperature. For our complex, the final R value was 0.0237, whereas in the reported structure it was 0.0384. In the present study the measured reflections was 4639, while in the earlier work it was 2991.
As previously observed (Bataille, 2003), the structure of (I) consists of Al3+ ions octahedrally coordinated to six water molecules, together with sulfate tetrahedra, piperazinium cations (lying about inversion centres) and non-bonded water molecules, linked by hydrogen bonds only (Fig. 1, Table 1). All the O—H···O and N—H···O hydrogen bonds build up a three dimensionnal network as previously reported (Table 1).