Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536800019498/na6021sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536800019498/na6021Isup2.hkl |
CCDC reference: 155844
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- H-atom completeness 98%
- Disorder in solvent or counterion
- R factor = 0.051
- wR factor = 0.183
- Data-to-parameter ratio = 14.4
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_302 Alert C Anion/Solvent disorder ....................... 25.00 Perc. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C36 H68 Cl10 Ga2 N24 O26 Atom count from the _atom_site data: C36 H66 Cl10 Ga2 N24 O26 CELLZ_01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C36 H68 Cl10 Ga2 N24 O26 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 144.00 144.00 0.00 H 272.00 264.00 8.00 Cl 40.00 40.00 0.00 Ga 8.00 8.00 0.00 N 96.00 96.00 0.00 O 104.00 104.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional?
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
The title compound was prepared by crystallization from an aqueous hydrochloric solution containing Ga3+ and cucurbituril. A mixture of Ga(NO3)3·8H2O (0.07 g, 0.18 mmol) and cucurbituril (0.03 g, 0.03 mmol) was dissolved in 2 M HCl (5 ml) and was heated for 5 min. The mixture was filtered and was kept open for 1–2 weeks in a vial until some crystals appeared. Then the vial was closed and the large colourless parallelepipedal crystals were isolated by filtration after 2 weeks. Yield 96% (0.05 g).
Data collection: XSCANS (Bruker, 1998); cell refinement: XSCANS; data reduction: SHELXTL-Plus (Sheldrick, 1990); program(s) used to solve structure: SHELXTL-Plus; program(s) used to refine structure: SHELXL97 (Sheldrick, 1998); molecular graphics: local program; software used to prepare material for publication: local program.
(H7O3)4[GaCl4]2Cl2·C36H36N24O12·2H2O | Dx = 1.668 Mg m−3 |
Mr = 1747.08 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Cmca | Cell parameters from 24 reflections |
a = 16.5665 (10) Å | θ = 16–22° |
b = 16.7800 (9) Å | µ = 1.25 mm−1 |
c = 25.0342 (10) Å | T = 293 K |
V = 6959.2 (6) Å3 | Parallelepiped, colourless |
Z = 4 | 0.60 × 0.35 × 0.20 mm |
F(000) = 3568 |
Bruker P4 diffractometer | 3008 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 27.5°, θmin = 1.9° |
ω scans | h = −21→0 |
Absorption correction: ψ scan (Sheldrick, 1990) | k = 0→21 |
Tmin = 0.531, Tmax = 0.778 | l = −32→0 |
4092 measured reflections | 3 standard reflections every 97 reflections |
4092 independent reflections | intensity decay: none |
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)] = 0.051 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.183 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.1074P)2 + 10.4226P] where P = (Fo2 + 2Fc2)/3 |
4092 reflections | (Δ/σ)max = 0.001 |
285 parameters | Δρmax = 0.84 e Å−3 |
15 restraints | Δρmin = −0.53 e Å−3 |
(H7O3)4[GaCl4]2Cl2·C36H36N24O12·2H2O | V = 6959.2 (6) Å3 |
Mr = 1747.08 | Z = 4 |
Orthorhombic, Cmca | Mo Kα radiation |
a = 16.5665 (10) Å | µ = 1.25 mm−1 |
b = 16.7800 (9) Å | T = 293 K |
c = 25.0342 (10) Å | 0.60 × 0.35 × 0.20 mm |
Bruker P4 diffractometer | 3008 reflections with I > 2σ(I) |
Absorption correction: ψ scan (Sheldrick, 1990) | Rint = 0.000 |
Tmin = 0.531, Tmax = 0.778 | 3 standard reflections every 97 reflections |
4092 measured reflections | intensity decay: none |
4092 independent reflections |
R[F2 > 2σ(F2)] = 0.051 | 15 restraints |
wR(F2) = 0.183 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.1074P)2 + 10.4226P] where P = (Fo2 + 2Fc2)/3 |
4092 reflections | Δρmax = 0.84 e Å−3 |
285 parameters | Δρmin = −0.53 e Å−3 |
Experimental. none |
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) | |
Ga1 | 0.5000 | 0.02140 (4) | 0.65300 (2) | 0.0475 (2) | |
Cl1 | 0.5000 | 0.02171 (10) | 0.56692 (5) | 0.0526 (4) | |
Cl21 | 0.3949 (7) | 0.0709 (8) | 0.6854 (5) | 0.082 (3) | 0.50 |
Cl22 | 0.3927 (8) | 0.0917 (8) | 0.6798 (5) | 0.076 (2) | 0.50 |
Cl31 | 0.5184 (8) | −0.09959 (17) | 0.67997 (11) | 0.111 (4) | 0.50 |
Cl4 | 0.2500 | −0.30977 (10) | 0.2500 | 0.0600 (4) | |
C111 | 0.04674 (18) | 0.13451 (18) | 0.31787 (12) | 0.0311 (6) | |
H111 | 0.0685 | 0.1574 | 0.2849 | 0.031* | |
C11 | 0.0000 | 0.0033 (3) | 0.32326 (19) | 0.0365 (10) | |
O11 | 0.0000 | −0.0692 (2) | 0.32348 (18) | 0.0513 (10) | |
C12 | 0.0000 | 0.2112 (3) | 0.38920 (18) | 0.0325 (9) | |
O12 | 0.0000 | 0.2573 (2) | 0.42714 (14) | 0.0460 (9) | |
N11 | 0.06654 (17) | 0.05100 (16) | 0.32279 (11) | 0.0350 (6) | |
N12 | 0.06673 (16) | 0.18287 (16) | 0.36401 (11) | 0.0338 (6) | |
C11B | 0.1472 (2) | 0.0199 (2) | 0.31581 (13) | 0.0371 (7) | |
H11A | 0.1754 | 0.0528 | 0.2899 | 0.037* | |
H11B | 0.1436 | −0.0335 | 0.3012 | 0.037* | |
C12B | 0.14743 (19) | 0.20595 (18) | 0.37867 (13) | 0.0335 (7) | |
H12A | 0.1777 | 0.2176 | 0.3464 | 0.034* | |
H12B | 0.1448 | 0.2545 | 0.3996 | 0.034* | |
C211 | 0.23914 (19) | 0.08410 (19) | 0.38539 (13) | 0.0330 (7) | |
H211 | 0.2770 | 0.1054 | 0.3589 | 0.033* | |
C212 | 0.2839 (2) | 0.0484 (2) | 0.43422 (13) | 0.0338 (7) | |
H212 | 0.3425 | 0.0545 | 0.4310 | 0.034* | |
C21 | 0.2086 (2) | −0.0508 (2) | 0.39219 (13) | 0.0378 (7) | |
O21 | 0.18160 (18) | −0.11745 (15) | 0.38188 (11) | 0.0494 (7) | |
C22 | 0.20043 (19) | 0.15193 (19) | 0.46292 (13) | 0.0330 (7) | |
O22 | 0.16922 (16) | 0.20167 (15) | 0.49166 (10) | 0.0446 (6) | |
N21 | 0.19446 (18) | 0.01711 (16) | 0.36461 (12) | 0.0369 (6) | |
N22 | 0.26006 (18) | −0.03444 (17) | 0.43309 (11) | 0.0374 (6) | |
N23 | 0.25235 (17) | 0.09319 (16) | 0.47875 (11) | 0.0351 (6) | |
N24 | 0.19022 (17) | 0.14648 (16) | 0.40885 (11) | 0.0348 (6) | |
C21B | 0.2905 (2) | −0.09390 (19) | 0.46902 (14) | 0.0377 (7) | |
H21A | 0.3481 | −0.0858 | 0.4735 | 0.038* | |
H21B | 0.2828 | −0.1460 | 0.4530 | 0.038* | |
O1W | 0.0000 | −0.2116 (3) | 0.2591 (2) | 0.0662 (12) | |
H1W1 | 0.0000 | −0.162 (3) | 0.238 (2) | 0.066* | |
H2W1 | 0.043 (2) | −0.213 (3) | 0.2857 (15) | 0.066* | |
O2W | 0.1231 (2) | −0.2227 (2) | 0.31466 (17) | 0.0845 (12) | |
H1W2 | 0.146 (3) | −0.175 (2) | 0.331 (2) | 0.084* | |
H2W2 | 0.170 (3) | −0.249 (3) | 0.295 (2) | 0.084* | |
O3W | 0.0000 | 0.3147 (3) | 0.5226 (2) | 0.095 (2) | |
H1W3 | 0.0474 (9) | 0.299 (3) | 0.5448 (15) | 0.095* | |
H2W3 | 0.0000 | 0.282 (4) | 0.4929 (19) | 0.095* | |
O4W | 0.1229 (3) | 0.2866 (2) | 0.57685 (17) | 0.0840 (12) | |
H1W4 | 0.105 (3) | 0.264 (3) | 0.6122 (13) | 0.084* | |
H2W4 | 0.135 (3) | 0.239 (2) | 0.5544 (17) | 0.084* | |
O5W | 0.0000 | −0.1356 (9) | 0.4285 (7) | 0.116 (5) | 0.50 |
H1W5 | −0.0481 (9) | −0.157 (7) | 0.410 (4) | 0.116* | 0.50 |
O1C | 0.0000 | 0.041 (3) | 0.488 (2) | 0.18 (2) | 0.25 |
O2C | −0.050 (2) | 0.0000 | 0.5000 | 0.163 (18) | 0.25 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ga1 | 0.0541 (4) | 0.0537 (4) | 0.0348 (3) | 0.000 | 0.000 | 0.0026 (2) |
Cl1 | 0.0438 (7) | 0.0791 (10) | 0.0349 (6) | 0.000 | 0.000 | 0.0050 (6) |
Cl21 | 0.055 (2) | 0.137 (9) | 0.055 (2) | 0.015 (4) | 0.020 (2) | −0.012 (4) |
Cl22 | 0.062 (2) | 0.093 (4) | 0.072 (4) | 0.018 (2) | −0.002 (2) | −0.016 (3) |
Cl31 | 0.192 (13) | 0.0674 (13) | 0.0730 (14) | 0.022 (3) | 0.001 (3) | 0.0285 (11) |
Cl4 | 0.0621 (9) | 0.0668 (9) | 0.0512 (7) | 0.000 | −0.0169 (7) | 0.000 |
C111 | 0.0331 (16) | 0.0306 (15) | 0.0295 (14) | 0.0006 (12) | 0.0008 (12) | 0.0021 (12) |
C11 | 0.044 (3) | 0.034 (2) | 0.031 (2) | 0.000 | 0.000 | −0.0033 (18) |
O11 | 0.056 (2) | 0.0315 (18) | 0.067 (3) | 0.000 | 0.000 | −0.0068 (17) |
C12 | 0.034 (2) | 0.031 (2) | 0.031 (2) | 0.000 | 0.000 | 0.0010 (18) |
O12 | 0.0473 (19) | 0.049 (2) | 0.0413 (19) | 0.000 | 0.000 | −0.0190 (16) |
N11 | 0.0364 (14) | 0.0286 (13) | 0.0401 (14) | 0.0039 (11) | 0.0002 (12) | −0.0032 (11) |
N12 | 0.0320 (13) | 0.0340 (13) | 0.0355 (13) | −0.0005 (11) | −0.0013 (11) | −0.0058 (11) |
C11B | 0.0417 (17) | 0.0377 (17) | 0.0320 (15) | 0.0062 (14) | 0.0021 (14) | −0.0063 (13) |
C12B | 0.0341 (15) | 0.0273 (14) | 0.0391 (16) | −0.0023 (13) | −0.0017 (13) | 0.0010 (12) |
C211 | 0.0283 (15) | 0.0360 (16) | 0.0346 (15) | −0.0007 (12) | 0.0053 (12) | 0.0016 (13) |
C212 | 0.0279 (14) | 0.0358 (16) | 0.0378 (16) | −0.0006 (13) | 0.0049 (13) | −0.0001 (13) |
C21 | 0.0372 (17) | 0.0397 (17) | 0.0364 (16) | 0.0045 (14) | 0.0063 (13) | −0.0035 (14) |
O21 | 0.0646 (18) | 0.0346 (13) | 0.0491 (14) | −0.0057 (12) | −0.0062 (13) | −0.0042 (11) |
C22 | 0.0278 (14) | 0.0357 (16) | 0.0357 (15) | −0.0045 (12) | 0.0003 (12) | −0.0014 (13) |
O22 | 0.0479 (14) | 0.0453 (13) | 0.0405 (13) | 0.0083 (11) | −0.0023 (11) | −0.0107 (11) |
N21 | 0.0403 (15) | 0.0328 (14) | 0.0377 (14) | 0.0023 (12) | −0.0027 (12) | −0.0007 (11) |
N22 | 0.0416 (15) | 0.0335 (13) | 0.0371 (14) | 0.0016 (12) | 0.0013 (12) | 0.0003 (11) |
N23 | 0.0343 (13) | 0.0377 (14) | 0.0334 (13) | 0.0005 (12) | −0.0025 (11) | −0.0023 (11) |
N24 | 0.0344 (14) | 0.0343 (13) | 0.0357 (14) | 0.0052 (11) | 0.0001 (11) | −0.0028 (11) |
C21B | 0.0369 (17) | 0.0350 (16) | 0.0411 (17) | 0.0083 (14) | 0.0075 (14) | 0.0004 (14) |
O1W | 0.084 (3) | 0.043 (2) | 0.072 (3) | 0.000 | 0.000 | −0.003 (2) |
O2W | 0.081 (3) | 0.077 (2) | 0.095 (3) | −0.004 (2) | −0.006 (2) | −0.039 (2) |
O3W | 0.171 (7) | 0.069 (3) | 0.045 (3) | 0.000 | 0.000 | −0.005 (2) |
O4W | 0.090 (3) | 0.076 (2) | 0.086 (3) | −0.024 (2) | 0.031 (2) | −0.028 (2) |
O5W | 0.096 (9) | 0.095 (9) | 0.156 (14) | 0.000 | 0.000 | 0.065 (10) |
O1C | 0.14 (4) | 0.17 (4) | 0.24 (6) | 0.000 | 0.000 | 0.07 (4) |
O2C | 0.06 (2) | 0.18 (4) | 0.24 (5) | 0.000 | 0.000 | −0.02 (4) |
Ga1—Cl1 | 2.1549 (14) | C211—N24 | 1.448 (4) |
Ga1—Cl21i | 2.093 (9) | C212—H212 | 0.9800 |
Ga1—Cl21 | 2.093 (9) | C212—N22 | 1.445 (4) |
Ga1—Cl22i | 2.236 (11) | C212—N23 | 1.442 (4) |
Ga1—Cl22 | 2.236 (11) | C21—O21 | 1.232 (4) |
Ga1—Cl31i | 2.161 (3) | C21—N21 | 1.353 (5) |
Ga1—Cl31 | 2.161 (3) | C21—N22 | 1.360 (5) |
Cl31—Cl31i | 0.61 (3) | C22—O22 | 1.217 (4) |
C111—C111ii | 1.549 (6) | C22—N23 | 1.367 (4) |
C111—H111 | 0.9800 | C22—N24 | 1.367 (4) |
C111—N11 | 1.444 (4) | N22—C21B | 1.435 (4) |
C111—N12 | 1.450 (4) | N23—C21Biii | 1.452 (4) |
C11—O11 | 1.217 (6) | C21B—N23iii | 1.452 (4) |
C11—N11 | 1.362 (4) | C21B—H21A | 0.9700 |
C11—N11ii | 1.362 (4) | C21B—H21B | 0.9700 |
C12—O12 | 1.226 (6) | O1W—H1W1 | 0.99 (3) |
C12—N12ii | 1.358 (4) | O1W—H2W1 | 0.98 (2) |
C12—N12 | 1.358 (4) | O2W—H1W2 | 0.96 (3) |
N11—C11B | 1.446 (4) | O2W—H2W2 | 1.02 (3) |
N12—C12B | 1.439 (4) | O3W—H1W3 | 1.00 (2) |
C11B—H11A | 0.9700 | O3W—H2W3 | 0.93 (3) |
C11B—H11B | 0.9700 | O4W—H1W4 | 1.01 (3) |
C11B—N21 | 1.451 (4) | O4W—H2W4 | 1.00 (3) |
C12B—H12A | 0.9700 | O5W—H1W5 | 0.99 (3) |
C12B—H12B | 0.9700 | O1C—O1Civ | 1.48 (9) |
C12B—N24 | 1.439 (4) | O1C—O2C | 1.11 (3) |
C211—H211 | 0.9800 | O1C—O2Civ | 1.11 (3) |
C211—C212 | 1.550 (5) | O2C—O1Civ | 1.11 (3) |
C211—N21 | 1.443 (4) | O2C—O2Civ | 1.66 (7) |
Cl1—Ga1—Cl22 | 107.4 (3) | N24—C12B—N12 | 113.9 (3) |
Cl1—Ga1—Cl22i | 107.4 (3) | N24—C12B—H12A | 108.8 |
Cl1—Ga1—Cl31 | 108.34 (10) | N24—C12B—H12B | 108.8 |
Cl1—Ga1—Cl31i | 108.34 (10) | C212—C211—H211 | 111.6 |
Cl21—Ga1—Cl1 | 112.8 (4) | N21—C211—H211 | 111.6 |
Cl21i—Ga1—Cl1 | 112.8 (4) | N21—C211—C212 | 103.2 (3) |
Cl21i—Ga1—Cl21 | 112.5 (8) | N21—C211—N24 | 115.0 (3) |
Cl21i—Ga1—Cl22i | 9.3 (7) | N24—C211—H211 | 111.6 |
Cl21—Ga1—Cl22i | 109.60 (12) | N24—C211—C212 | 103.1 (3) |
Cl21i—Ga1—Cl22 | 109.60 (12) | C211—C212—H212 | 111.6 |
Cl21—Ga1—Cl22 | 9.3 (7) | N22—C212—C211 | 103.0 (3) |
Cl21i—Ga1—Cl31i | 111.7 (5) | N22—C212—H212 | 111.6 |
Cl21—Ga1—Cl31i | 97.7 (5) | N23—C212—C211 | 103.6 (3) |
Cl21i—Ga1—Cl31 | 97.7 (5) | N23—C212—H212 | 111.6 |
Cl21—Ga1—Cl31 | 111.7 (5) | N23—C212—N22 | 114.7 (3) |
Cl22i—Ga1—Cl22 | 105.3 (7) | O21—C21—N21 | 126.5 (3) |
Cl31i—Ga1—Cl22i | 120.9 (5) | O21—C21—N22 | 124.6 (3) |
Cl31—Ga1—Cl22i | 106.9 (5) | N21—C21—N22 | 108.8 (3) |
Cl31i—Ga1—Cl22 | 106.9 (5) | O22—C22—N23 | 126.2 (3) |
Cl31—Ga1—Cl22 | 120.9 (5) | O22—C22—N24 | 125.3 (3) |
Cl31i—Ga1—Cl31 | 16.2 (7) | N23—C22—N24 | 108.5 (3) |
Cl31i—Cl31—Ga1 | 81.9 (4) | C211—N21—C11B | 123.7 (3) |
C111ii—C111—H111 | 111.6 | C21—N21—C11B | 123.4 (3) |
N11—C111—C111ii | 103.12 (17) | C21—N21—C211 | 112.5 (3) |
N11—C111—H111 | 111.6 | C21—N22—C212 | 112.3 (3) |
N11—C111—N12 | 115.0 (3) | C21—N22—C21B | 123.5 (3) |
N12—C111—C111ii | 103.21 (16) | C21B—N22—C212 | 124.1 (3) |
N12—C111—H111 | 111.6 | C212—N23—C21Biii | 122.8 (3) |
O11—C11—N11 | 126.0 (2) | C22—N23—C212 | 112.3 (3) |
O11—C11—N11ii | 126.0 (2) | C22—N23—C21Biii | 121.9 (3) |
N11—C11—N11ii | 108.1 (4) | C12B—N24—C211 | 124.3 (3) |
O12—C12—N12ii | 125.49 (19) | C22—N24—C12B | 122.3 (3) |
O12—C12—N12 | 125.49 (19) | C22—N24—C211 | 112.4 (3) |
N12ii—C12—N12 | 109.0 (4) | N22—C21B—N23iii | 113.9 (3) |
C111—N11—C11B | 123.3 (3) | N22—C21B—H21A | 108.8 |
C11—N11—C111 | 112.8 (3) | N22—C21B—H21B | 108.8 |
C11—N11—C11B | 122.5 (3) | N23iii—C21B—H21A | 108.8 |
C12—N12—C111 | 112.3 (3) | N23iii—C21B—H21B | 108.8 |
C12—N12—C12B | 122.9 (3) | H21A—C21B—H21B | 107.7 |
C12B—N12—C111 | 124.5 (3) | H1W1—O1W—H2W1 | 112 (3) |
N11—C11B—H11A | 108.7 | H1W2—O2W—H2W2 | 105 (3) |
N11—C11B—H11B | 108.7 | H1W3—O3W—H2W3 | 107 (3) |
N11—C11B—N21 | 114.1 (3) | H1W4—O4W—H2W4 | 104 (3) |
H11A—C11B—H11B | 107.6 | O2C—O1C—O1Civ | 48 (2) |
N21—C11B—H11A | 108.7 | O2Civ—O1C—O1Civ | 48 (2) |
N21—C11B—H11B | 108.7 | O2C—O1C—O2Civ | 97 (5) |
N12—C12B—H12A | 108.8 | O1C—O2C—O1Civ | 83 (5) |
N12—C12B—H12B | 108.8 | O1C—O2C—O2Civ | 42 (2) |
H12A—C12B—H12B | 107.7 | O1Civ—O2C—O2Civ | 42 (2) |
Symmetry codes: (i) −x+1, y, z; (ii) −x, y, z; (iii) x, −y, −z+1; (iv) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H2W1···O2W | 0.98 (2) | 1.52 (4) | 2.476 (5) | 165 (3) |
O3W—H1W3···O4W | 1.00 (2) | 1.50 (3) | 2.492 (6) | 172 (4) |
Experimental details
Crystal data | |
Chemical formula | (H7O3)4[GaCl4]2Cl2·C36H36N24O12·2H2O |
Mr | 1747.08 |
Crystal system, space group | Orthorhombic, Cmca |
Temperature (K) | 293 |
a, b, c (Å) | 16.5665 (10), 16.7800 (9), 25.0342 (10) |
V (Å3) | 6959.2 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.25 |
Crystal size (mm) | 0.60 × 0.35 × 0.20 |
Data collection | |
Diffractometer | Bruker P4 diffractometer |
Absorption correction | ψ scan (Sheldrick, 1990) |
Tmin, Tmax | 0.531, 0.778 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4092, 4092, 3008 |
Rint | 0.000 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.051, 0.183, 1.04 |
No. of reflections | 4092 |
No. of parameters | 285 |
No. of restraints | 15 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
w = 1/[σ2(Fo2) + (0.1074P)2 + 10.4226P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.84, −0.53 |
Computer programs: XSCANS (Bruker, 1998), XSCANS, SHELXTL-Plus (Sheldrick, 1990), SHELXTL-Plus, SHELXL97 (Sheldrick, 1998), local program.
Ga1—Cl1 | 2.1549 (14) | Ga1—Cl22 | 2.236 (11) |
Ga1—Cl21 | 2.093 (9) | Ga1—Cl31 | 2.161 (3) |
Cl1—Ga1—Cl22 | 107.4 (3) | Cl21—Ga1—Cl31 | 111.7 (5) |
Cl1—Ga1—Cl31 | 108.34 (10) | Cl31—Ga1—Cl22i | 106.9 (5) |
Cl21—Ga1—Cl1 | 112.8 (4) | Cl31—Ga1—Cl22 | 120.9 (5) |
Cl21i—Ga1—Cl22 | 109.60 (12) | Cl31i—Cl31—Ga1 | 81.9 (4) |
Cl21—Ga1—Cl31i | 97.7 (5) |
Symmetry code: (i) −x+1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H2W1···O2W | 0.98 (2) | 1.52 (4) | 2.476 (5) | 165 (3) |
O3W—H1W3···O4W | 1.00 (2) | 1.50 (3) | 2.492 (6) | 172 (4) |
Recently, during the investigation of the Fe3+–HCl–cucurbituril system, we obtained a supramolecular adduct containing the tetrachloroferrate(III) anion and cucurbituril (Virovets et al., 2001). Using Ga3+ salts, under the same conditions, we have crystallized the isostructural title compound, (I).
The structure of the title compound contains hydroxonium cations, [GaCl4]- anions, chloride anions, cucurbituril and water molecules. Cucurbituril centres are arranged as body-centered packing and [GaCl4]- anions are situated in space between them. One water molecule is situated near to the centre inside the cucurbituril molecule and is disordered over four positions (O1C and O2C).
The [GaCl4]- anion lies on the mirror plane and is disordered over two orientations around the Ga1—Cl1 axis. The central Ga atoms have tetrahedral environments and the Ga—Cl distances correspond to those known from other reports (Buscher et al., 1984; Gearhart et al., 1975).
There are two crystallographically independent hydroxonium cations in the structure (O1W and O3W). They lie on the mirror planes, and each cation is joined with two water molecules by short hydrogen bonds (see Table 2). The O···O···O angles are 109.6 (2) and 110.9 (1)°. This corresponds to formation of H7O3+ cations in the crystal (Wells, 1986).
There is a complicated hydrogen-bound network joining O atoms of the cucurbituril carbonyl groups, water molecules, complex anions and chloride in the structure.