Reacting trimesic acid (H3TMA, C9H6O6) with CaCl2 and MCl2 at 110 °C under hydrothermal conditions gave the isostructural heterobimetallic coordination polymers (CPs) catena-poly[[tetraaquazinc(II)]-μ-5-carboxybenzene-1,3-dicarboxylato-[tetraaquacalcium(II)]-μ-5-carboxybenzene-1,3-dicarboxylato], [CaZn(HTMA)2(H2O)8]n, 1, and catena-poly[[tetraaquacobalt(II)]-μ-5-carboxybenzene-1,3-dicarboxylato-[tetraaquacalcium(II)]-μ-5-carboxybenzene-1,3-dicarboxylato], [CaCo(HTMA)2(H2O)8]n, 2. Compounds 1 and 2 crystallize in the monoclinic space group C2/c. The solid-state structures consist of eight-coordinate CaII ions and six-coordinate MII ions. These ions are connected by a doubly deprotonated HTMA2− ligand to create a one-dimensional (1D) zigzag chain. Poly[[decaaquabis(μ3-benzene-1,3,5-tricarboxylato)calcium(II)dizinc(II)] dihydrate], {[CaZn2(TMA)2(H2O)10]·2H2O}n, 3, was found incidentally as a minor by-product during the synthesis of 1 at a temperature of 140 °C. It forms crystals in the orthorhombic space group Ccce. The structure of 3 consists of a two-dimensional (2D) layer composed of [Zn(TMA)] chains that are interconnected by CaII ions. The presence of aromatic carboxylic acid ligands and water molecules, which can form numerous hydrogen bonds and π–π interactions, increases the stability of the three-dimensional (3D) supramolecular architecture of these CPs. Compounds 1 and 2 exhibit thermal stability up to 420 °C, as indicated by the thermogravimetric analysis (TGA) curves. The powder X-ray diffraction (PXRD) data reveal the formation of unidentified phases in methanol and dimethyl sulfoxide, while 1 exhibits chemical stability in a wide range of solvents. The luminescence properties of 1 dispersed in various low molecular weight organic solvents was also examined. The results demonstrate excellent selectivity, sensitivity and recyclability for detecting acetone molecules in aqueous media. Additionally, a possible sensing mechanism is also outlined.
Supporting information
CCDC references: 2299479; 2299478; 2299477
catena-Poly[[tetraaquazinc(II)]-µ-5-carboxybenzene-1,3-dicarboxylato-[tetraaquacalcium(II)]-µ-5-carboxybenzene-1,3-dicarboxylato] (1)
top
Crystal data top
[CaZn(C6H4O6)2(H2O)8] | F(000) = 1368 |
Mr = 665.82 | Dx = 1.886 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 17.848 (2) Å | Cell parameters from 9954 reflections |
b = 20.106 (2) Å | θ = 3.1–28.2° |
c = 6.5975 (8) Å | µ = 1.37 mm−1 |
β = 97.997 (4)° | T = 296 K |
V = 2344.6 (5) Å3 | Block, light colourless |
Z = 4 | 0.4 × 0.4 × 0.2 mm |
Data collection top
Bruker D8 QUEST CMOS PHOTON II diffractometer | 2927 independent reflections |
Radiation source: sealed x-ray tube, Mo | 2515 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
Detector resolution: 7.39 pixels mm-1 | θmax = 28.4°, θmin = 3.1° |
φ and ω scans | h = −23→23 |
Absorption correction: multi-scan (SADABS; Bruker, 2021) | k = −26→26 |
Tmin = 0.670, Tmax = 0.746 | l = −8→8 |
33766 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: inferred from neighbouring sites |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.044 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.131 | w = 1/[σ2(Fo2) + (0.0666P)2 + 7.9545P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max < 0.001 |
2927 reflections | Δρmax = 1.82 e Å−3 |
207 parameters | Δρmin = −0.66 e Å−3 |
17 restraints | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Zn1 | −0.250000 | −0.250000 | 0.000000 | 0.02274 (15) | |
Ca1 | 0.000000 | 0.12347 (4) | 0.250000 | 0.0267 (2) | |
O1 | −0.26118 (11) | −0.14947 (10) | −0.0196 (3) | 0.0277 (5) | |
O2 | −0.38491 (13) | −0.13984 (11) | −0.0214 (4) | 0.0385 (6) | |
O3 | −0.09102 (13) | 0.04009 (12) | 0.1144 (4) | 0.0397 (6) | |
O4 | −0.13318 (12) | 0.14232 (10) | 0.0626 (4) | 0.0306 (5) | |
O5 | −0.41958 (12) | 0.17737 (11) | −0.0329 (4) | 0.0376 (6) | |
O6 | −0.48724 (13) | 0.08593 (12) | −0.0044 (5) | 0.0478 (7) | |
H6 | −0.5222 (12) | 0.1125 (14) | −0.022 (18) | 0.20 (5)* | |
O7 | −0.35518 (13) | −0.27055 (12) | −0.2084 (4) | 0.0328 (5) | |
H7A | −0.355 (2) | −0.2979 (17) | −0.311 (4) | 0.049* | |
H7B | −0.380 (2) | −0.2392 (13) | −0.278 (5) | 0.049* | |
O8 | −0.19164 (13) | −0.24842 (10) | −0.2530 (4) | 0.0299 (5) | |
H8A | −0.179 (2) | −0.2116 (12) | −0.301 (6) | 0.045* | |
H8B | −0.1523 (17) | −0.2724 (17) | −0.251 (6) | 0.045* | |
O9 | 0.05389 (16) | 0.09054 (14) | −0.0538 (5) | 0.0476 (6) | |
H9A | 0.064134 | 0.052489 | −0.094003 | 0.14 (3)* | |
H9B | 0.072004 | 0.121869 | −0.117603 | 0.7 (2)* | |
O10 | 0.02472 (16) | 0.22086 (14) | 0.0502 (5) | 0.0497 (7) | |
H10A | 0.002 (3) | 0.2600 (13) | 0.051 (8) | 0.075* | |
H10B | 0.059 (2) | 0.2266 (18) | −0.029 (7) | 0.075* | |
C1 | −0.32004 (15) | −0.11523 (13) | −0.0183 (4) | 0.0212 (5) | |
C2 | −0.30924 (15) | −0.04058 (12) | −0.0121 (4) | 0.0193 (5) | |
C3 | −0.23620 (15) | −0.01466 (13) | 0.0152 (4) | 0.0209 (5) | |
H3 | −0.195071 | −0.043497 | 0.028015 | 0.025* | |
C4 | −0.22367 (15) | 0.05379 (13) | 0.0237 (4) | 0.0198 (5) | |
C5 | −0.28557 (15) | 0.09729 (13) | 0.0044 (4) | 0.0205 (5) | |
H5 | −0.277951 | 0.143060 | 0.006864 | 0.025* | |
C6 | −0.35852 (15) | 0.07142 (12) | −0.0186 (4) | 0.0202 (5) | |
C7 | −0.37041 (15) | 0.00283 (13) | −0.0277 (4) | 0.0223 (5) | |
H7 | −0.419456 | −0.013924 | −0.044292 | 0.027* | |
C8 | −0.14446 (15) | 0.07985 (14) | 0.0669 (4) | 0.0236 (5) | |
C9 | −0.42460 (15) | 0.11709 (14) | −0.0210 (5) | 0.0238 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0226 (2) | 0.0145 (2) | 0.0321 (3) | 0.00139 (15) | 0.00695 (18) | 0.00118 (16) |
Ca1 | 0.0137 (3) | 0.0310 (4) | 0.0342 (4) | 0.000 | −0.0004 (3) | 0.000 |
O1 | 0.0235 (10) | 0.0152 (9) | 0.0456 (12) | 0.0039 (7) | 0.0085 (9) | 0.0022 (8) |
O2 | 0.0234 (10) | 0.0165 (10) | 0.0764 (18) | −0.0004 (8) | 0.0095 (11) | −0.0011 (10) |
O3 | 0.0216 (10) | 0.0280 (11) | 0.0666 (17) | 0.0035 (9) | −0.0043 (10) | −0.0032 (11) |
O4 | 0.0234 (10) | 0.0208 (10) | 0.0475 (13) | −0.0042 (8) | 0.0040 (9) | −0.0041 (9) |
O5 | 0.0247 (10) | 0.0156 (10) | 0.0718 (17) | 0.0030 (8) | 0.0040 (11) | 0.0022 (10) |
O6 | 0.0230 (11) | 0.0194 (11) | 0.104 (2) | 0.0014 (9) | 0.0193 (13) | 0.0030 (12) |
O7 | 0.0292 (11) | 0.0281 (11) | 0.0390 (12) | 0.0041 (9) | −0.0018 (9) | −0.0014 (9) |
O8 | 0.0300 (11) | 0.0241 (11) | 0.0384 (12) | 0.0040 (8) | 0.0143 (9) | 0.0039 (8) |
O9 | 0.0494 (16) | 0.0383 (14) | 0.0563 (16) | 0.0072 (12) | 0.0120 (13) | −0.0036 (12) |
O10 | 0.0445 (15) | 0.0367 (14) | 0.0719 (19) | 0.0077 (12) | 0.0220 (13) | 0.0119 (13) |
C1 | 0.0225 (12) | 0.0139 (11) | 0.0270 (13) | 0.0018 (9) | 0.0029 (10) | 0.0019 (9) |
C2 | 0.0216 (12) | 0.0124 (11) | 0.0239 (12) | 0.0007 (9) | 0.0031 (9) | 0.0004 (9) |
C3 | 0.0214 (12) | 0.0169 (12) | 0.0241 (12) | 0.0028 (9) | 0.0024 (10) | −0.0001 (9) |
C4 | 0.0185 (11) | 0.0179 (12) | 0.0229 (12) | −0.0017 (9) | 0.0020 (9) | −0.0003 (9) |
C5 | 0.0208 (12) | 0.0147 (11) | 0.0261 (12) | −0.0001 (9) | 0.0037 (10) | 0.0009 (9) |
C6 | 0.0193 (12) | 0.0138 (11) | 0.0277 (13) | 0.0014 (9) | 0.0038 (10) | 0.0010 (9) |
C7 | 0.0199 (12) | 0.0156 (12) | 0.0316 (13) | −0.0003 (9) | 0.0043 (10) | 0.0002 (10) |
C8 | 0.0181 (12) | 0.0240 (13) | 0.0284 (13) | −0.0008 (10) | 0.0020 (10) | −0.0039 (10) |
C9 | 0.0196 (12) | 0.0179 (12) | 0.0334 (14) | 0.0002 (10) | 0.0020 (10) | −0.0005 (10) |
Geometric parameters (Å, º) top
Zn1—O1 | 2.033 (2) | O7—H7A | 0.872 (18) |
Zn1—O1i | 2.033 (2) | O7—H7B | 0.865 (18) |
Zn1—O7 | 2.206 (2) | O8—H8A | 0.848 (18) |
Zn1—O7i | 2.206 (2) | O8—H8B | 0.851 (18) |
Zn1—O8i | 2.087 (2) | O9—H9A | 0.8383 |
Zn1—O8 | 2.087 (2) | O9—H9B | 0.8465 |
Ca1—O3ii | 2.418 (2) | O10—H10A | 0.886 (18) |
Ca1—O3 | 2.418 (2) | O10—H10B | 0.870 (18) |
Ca1—O4 | 2.551 (2) | C1—C2 | 1.513 (3) |
Ca1—O4ii | 2.551 (2) | C2—C3 | 1.392 (4) |
Ca1—O9 | 2.432 (3) | C2—C7 | 1.390 (4) |
Ca1—O9ii | 2.432 (3) | C3—H3 | 0.9300 |
Ca1—O10 | 2.435 (3) | C3—C4 | 1.394 (4) |
Ca1—O10ii | 2.435 (3) | C4—C5 | 1.401 (4) |
O1—C1 | 1.257 (3) | C4—C8 | 1.497 (4) |
O2—C1 | 1.257 (3) | C5—H5 | 0.9300 |
O3—C8 | 1.250 (4) | C5—C6 | 1.391 (4) |
O4—C8 | 1.273 (4) | C6—C7 | 1.395 (4) |
O5—C9 | 1.219 (4) | C6—C9 | 1.493 (4) |
O6—H6 | 0.82 (2) | C7—H7 | 0.9300 |
O6—C9 | 1.300 (4) | | |
| | | |
O1—Zn1—O1i | 180.0 | C1—O1—Zn1 | 128.22 (18) |
O1—Zn1—O7i | 85.46 (9) | C8—O3—Ca1 | 95.70 (18) |
O1i—Zn1—O7i | 94.54 (9) | C8—O4—Ca1 | 88.97 (17) |
O1—Zn1—O7 | 94.54 (9) | C9—O6—H6 | 108.8 (16) |
O1i—Zn1—O7 | 85.46 (9) | Zn1—O7—H7A | 121 (2) |
O1—Zn1—O8i | 90.60 (8) | Zn1—O7—H7B | 121 (2) |
O1—Zn1—O8 | 89.40 (8) | H7A—O7—H7B | 96 (3) |
O1i—Zn1—O8i | 89.40 (8) | Zn1—O8—H8A | 120 (2) |
O1i—Zn1—O8 | 90.60 (8) | Zn1—O8—H8B | 119 (2) |
O7—Zn1—O7i | 180.0 | H8A—O8—H8B | 104 (3) |
O8i—Zn1—O7i | 88.88 (9) | Ca1—O9—H9A | 129.7 |
O8i—Zn1—O7 | 91.11 (9) | Ca1—O9—H9B | 115.4 |
O8—Zn1—O7 | 88.89 (9) | H9A—O9—H9B | 114.0 |
O8—Zn1—O7i | 91.11 (9) | Ca1—O10—H10A | 126 (2) |
O8i—Zn1—O8 | 180.0 | Ca1—O10—H10B | 129 (2) |
O3ii—Ca1—O3 | 92.20 (11) | H10A—O10—H10B | 104 (4) |
O3—Ca1—O4ii | 144.62 (8) | O1—C1—C2 | 116.1 (2) |
O3ii—Ca1—O4ii | 52.46 (7) | O2—C1—O1 | 123.6 (2) |
O3—Ca1—O4 | 52.46 (7) | O2—C1—C2 | 120.3 (2) |
O3ii—Ca1—O4 | 144.62 (8) | C3—C2—C1 | 119.2 (2) |
O3ii—Ca1—O9 | 78.10 (10) | C7—C2—C1 | 121.7 (2) |
O3—Ca1—O9 | 80.14 (10) | C7—C2—C3 | 119.1 (2) |
O3ii—Ca1—O9ii | 80.14 (10) | C2—C3—H3 | 119.4 |
O3—Ca1—O9ii | 78.09 (10) | C2—C3—C4 | 121.1 (2) |
O3ii—Ca1—O10ii | 121.36 (10) | C4—C3—H3 | 119.4 |
O3—Ca1—O10 | 121.36 (10) | C3—C4—C5 | 119.5 (2) |
O3—Ca1—O10ii | 126.51 (9) | C3—C4—C8 | 119.7 (2) |
O3ii—Ca1—O10 | 126.51 (9) | C5—C4—C8 | 120.7 (2) |
O4ii—Ca1—O4 | 162.91 (10) | C4—C5—H5 | 120.3 |
O9—Ca1—O4ii | 89.49 (9) | C6—C5—C4 | 119.4 (2) |
O9—Ca1—O4 | 95.15 (9) | C6—C5—H5 | 120.3 |
O9ii—Ca1—O4 | 89.49 (9) | C5—C6—C7 | 120.6 (2) |
O9ii—Ca1—O4ii | 95.15 (9) | C5—C6—C9 | 119.8 (2) |
O9—Ca1—O9ii | 148.40 (15) | C7—C6—C9 | 119.5 (2) |
O9ii—Ca1—O10 | 141.92 (10) | C2—C7—C6 | 120.3 (2) |
O9—Ca1—O10 | 69.56 (10) | C2—C7—H7 | 119.9 |
O9—Ca1—O10ii | 141.92 (10) | C6—C7—H7 | 119.9 |
O9ii—Ca1—O10ii | 69.56 (10) | O3—C8—O4 | 121.3 (3) |
O10ii—Ca1—O4 | 85.19 (9) | O3—C8—C4 | 119.4 (3) |
O10—Ca1—O4ii | 85.19 (9) | O4—C8—C4 | 119.3 (2) |
O10—Ca1—O4 | 81.08 (9) | O5—C9—O6 | 123.8 (3) |
O10ii—Ca1—O4ii | 81.08 (9) | O5—C9—C6 | 123.2 (3) |
O10—Ca1—O10ii | 72.92 (15) | O6—C9—C6 | 113.0 (2) |
| | | |
Zn1—O1—C1—O2 | −6.3 (4) | C3—C4—C5—C6 | 1.4 (4) |
Zn1—O1—C1—C2 | 173.57 (17) | C3—C4—C8—O3 | −6.8 (4) |
Ca1—O3—C8—O4 | 13.4 (3) | C3—C4—C8—O4 | 175.9 (3) |
Ca1—O3—C8—C4 | −163.8 (2) | C4—C5—C6—C7 | −1.6 (4) |
Ca1—O4—C8—O3 | −12.6 (3) | C4—C5—C6—C9 | 174.7 (2) |
Ca1—O4—C8—C4 | 164.6 (2) | C5—C4—C8—O3 | 169.1 (3) |
O1—C1—C2—C3 | −7.2 (4) | C5—C4—C8—O4 | −8.1 (4) |
O1—C1—C2—C7 | 174.4 (3) | C5—C6—C7—C2 | 0.6 (4) |
O2—C1—C2—C3 | 172.6 (3) | C5—C6—C9—O5 | 10.7 (4) |
O2—C1—C2—C7 | −5.7 (4) | C5—C6—C9—O6 | −167.7 (3) |
C1—C2—C3—C4 | −179.4 (2) | C7—C2—C3—C4 | −1.1 (4) |
C1—C2—C7—C6 | 179.1 (2) | C7—C6—C9—O5 | −172.9 (3) |
C2—C3—C4—C5 | 0.0 (4) | C7—C6—C9—O6 | 8.7 (4) |
C2—C3—C4—C8 | 176.0 (2) | C8—C4—C5—C6 | −174.6 (2) |
C3—C2—C7—C6 | 0.8 (4) | C9—C6—C7—C2 | −175.8 (3) |
Symmetry codes: (i) −x−1/2, −y−1/2, −z; (ii) −x, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6···O2iii | 0.82 (2) | 1.81 (4) | 2.553 (3) | 151 (6) |
O7—H7A···O4iv | 0.87 (2) | 2.04 (2) | 2.905 (3) | 174 (3) |
O7—H7B···O5v | 0.87 (2) | 2.13 (2) | 2.955 (3) | 159 (4) |
O8—H8A···O4v | 0.85 (2) | 1.90 (2) | 2.734 (3) | 166 (3) |
O8—H8B···O2i | 0.85 (2) | 2.54 (3) | 3.083 (3) | 122 (3) |
O8—H8B···O5iv | 0.85 (2) | 2.28 (3) | 2.990 (3) | 141 (3) |
O9—H9A···O3vi | 0.84 (2) | 1.93 (2) | 2.752 (4) | 166 (1) |
O10—H10A···O5vii | 0.89 (2) | 1.93 (3) | 2.768 (3) | 158 (5) |
O10—H10B···O7viii | 0.87 (2) | 2.06 (2) | 2.925 (4) | 173 (3) |
Symmetry codes: (i) −x−1/2, −y−1/2, −z; (iii) −x−1, −y, −z; (iv) −x−1/2, y−1/2, −z−1/2; (v) x, −y, z−1/2; (vi) −x, −y, −z; (vii) −x−1/2, −y+1/2, −z; (viii) x+1/2, y+1/2, z. |
catena-Poly[[tetraaquacobalt(II)]-µ-5-carboxybenzene-1,3-dicarboxylato-[tetraaquacalcium(II)]-µ-5-carboxybenzene-1,3-dicarboxylato] (2)
top
Crystal data top
[CaCo(C6H4O6)2(H2O)8] | F(000) = 1356 |
Mr = 659.38 | Dx = 1.878 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 17.875 (5) Å | Cell parameters from 1029 reflections |
b = 20.192 (4) Å | θ = 3.1–25.2° |
c = 6.5339 (16) Å | µ = 1.06 mm−1 |
β = 98.557 (9)° | T = 296 K |
V = 2332.0 (9) Å3 | Block, light pink |
Z = 4 | 0.14 × 0.12 × 0.08 mm |
Data collection top
Bruker D8 QUEST CMOS PHOTON II diffractometer | 2391 independent reflections |
Radiation source: sealed x-ray tube, Mo | 1996 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
Detector resolution: 7.39 pixels mm-1 | θmax = 26.4°, θmin = 3.1° |
ω and φ scans | h = −22→22 |
Absorption correction: multi-scan (SADABS; Bruker, 2021) | k = −25→25 |
Tmin = 0.689, Tmax = 0.745 | l = −7→8 |
15563 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: inferred from neighbouring sites |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.068 | w = 1/[σ2(Fo2) + (0.0313P)2 + 2.5603P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
2391 reflections | Δρmax = 0.33 e Å−3 |
207 parameters | Δρmin = −0.28 e Å−3 |
17 restraints | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | −0.250000 | −0.250000 | 0.000000 | 0.01469 (11) | |
Ca1 | 0.000000 | 0.12635 (3) | 0.250000 | 0.01778 (14) | |
O1 | −0.26153 (7) | −0.14844 (6) | −0.0159 (2) | 0.0206 (3) | |
O2 | −0.38504 (8) | −0.13906 (7) | −0.0181 (3) | 0.0313 (4) | |
O3 | −0.09133 (8) | 0.04081 (7) | 0.1066 (3) | 0.0310 (4) | |
O4 | −0.13376 (8) | 0.14265 (6) | 0.0630 (2) | 0.0215 (3) | |
O5 | −0.42037 (8) | 0.17700 (7) | −0.0281 (3) | 0.0297 (4) | |
O6 | −0.48777 (9) | 0.08571 (7) | −0.0039 (3) | 0.0407 (5) | |
H6 | −0.5234 (11) | 0.1125 (10) | 0.002 (6) | 0.087 (13)* | |
O7 | −0.35291 (8) | −0.26895 (7) | −0.2116 (2) | 0.0227 (3) | |
H7A | −0.3494 (13) | −0.2972 (10) | −0.300 (3) | 0.034* | |
H7B | −0.3705 (12) | −0.2350 (9) | −0.276 (3) | 0.034* | |
O8 | −0.19074 (8) | −0.24851 (7) | −0.2501 (2) | 0.0229 (3) | |
H8A | −0.1800 (13) | −0.2130 (9) | −0.301 (3) | 0.034* | |
H8B | −0.1526 (11) | −0.2726 (11) | −0.246 (4) | 0.034* | |
O9 | 0.05539 (10) | 0.08955 (8) | −0.0523 (3) | 0.0356 (4) | |
H9A | 0.065634 | 0.051501 | −0.092519 | 0.073 (11)* | |
H9B | 0.073504 | 0.120881 | −0.116119 | 0.29 (4)* | |
O10 | 0.02452 (9) | 0.22094 (8) | 0.0473 (3) | 0.0334 (4) | |
H10A | 0.0001 (14) | 0.2577 (9) | 0.046 (4) | 0.050* | |
H10B | 0.0613 (13) | 0.2272 (12) | −0.016 (4) | 0.050* | |
C1 | −0.32040 (11) | −0.11426 (9) | −0.0148 (3) | 0.0160 (4) | |
C2 | −0.30970 (11) | −0.03988 (9) | −0.0098 (3) | 0.0147 (4) | |
C3 | −0.23698 (11) | −0.01371 (9) | 0.0155 (3) | 0.0157 (4) | |
H3 | −0.195739 | −0.042261 | 0.027325 | 0.019* | |
C4 | −0.22463 (11) | 0.05446 (9) | 0.0235 (3) | 0.0142 (4) | |
C5 | −0.28623 (11) | 0.09733 (9) | 0.0050 (3) | 0.0145 (4) | |
H5 | −0.278678 | 0.142906 | 0.006890 | 0.017* | |
C6 | −0.35936 (11) | 0.07153 (9) | −0.0162 (3) | 0.0152 (4) | |
C7 | −0.37086 (11) | 0.00333 (9) | −0.0247 (3) | 0.0167 (4) | |
H7 | −0.419827 | −0.013462 | −0.040546 | 0.020* | |
C8 | −0.14511 (11) | 0.08041 (9) | 0.0646 (3) | 0.0174 (4) | |
C9 | −0.42526 (11) | 0.11676 (9) | −0.0183 (3) | 0.0185 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0140 (2) | 0.00937 (18) | 0.0211 (2) | 0.00099 (13) | 0.00395 (15) | 0.00086 (14) |
Ca1 | 0.0118 (3) | 0.0136 (3) | 0.0271 (3) | 0.000 | −0.0001 (2) | 0.000 |
O1 | 0.0165 (7) | 0.0100 (6) | 0.0362 (9) | 0.0026 (5) | 0.0069 (6) | 0.0012 (6) |
O2 | 0.0152 (8) | 0.0116 (7) | 0.0677 (12) | −0.0012 (6) | 0.0083 (7) | −0.0022 (7) |
O3 | 0.0159 (8) | 0.0177 (7) | 0.0563 (11) | 0.0013 (6) | −0.0044 (7) | −0.0065 (7) |
O4 | 0.0172 (7) | 0.0128 (7) | 0.0343 (8) | −0.0026 (5) | 0.0029 (6) | −0.0010 (6) |
O5 | 0.0199 (8) | 0.0102 (7) | 0.0587 (11) | 0.0022 (6) | 0.0046 (7) | 0.0010 (7) |
O6 | 0.0166 (8) | 0.0150 (7) | 0.0939 (15) | 0.0013 (6) | 0.0188 (9) | 0.0009 (8) |
O7 | 0.0234 (8) | 0.0177 (7) | 0.0257 (8) | 0.0022 (6) | −0.0005 (6) | −0.0007 (6) |
O8 | 0.0234 (8) | 0.0177 (7) | 0.0301 (8) | 0.0034 (6) | 0.0119 (6) | 0.0039 (6) |
O9 | 0.0410 (10) | 0.0236 (9) | 0.0443 (10) | 0.0073 (7) | 0.0130 (8) | −0.0057 (8) |
O10 | 0.0291 (9) | 0.0220 (8) | 0.0530 (11) | 0.0070 (7) | 0.0190 (8) | 0.0120 (8) |
C1 | 0.0186 (10) | 0.0117 (9) | 0.0178 (10) | 0.0007 (7) | 0.0029 (8) | 0.0005 (7) |
C2 | 0.0173 (10) | 0.0112 (9) | 0.0158 (10) | 0.0001 (7) | 0.0034 (8) | 0.0005 (7) |
C3 | 0.0164 (10) | 0.0141 (9) | 0.0165 (10) | 0.0029 (7) | 0.0017 (8) | 0.0003 (7) |
C4 | 0.0149 (9) | 0.0131 (9) | 0.0146 (9) | −0.0010 (7) | 0.0019 (7) | −0.0007 (7) |
C5 | 0.0169 (10) | 0.0094 (8) | 0.0175 (10) | −0.0016 (7) | 0.0030 (8) | −0.0001 (7) |
C6 | 0.0138 (10) | 0.0127 (9) | 0.0191 (10) | 0.0015 (7) | 0.0028 (8) | 0.0007 (7) |
C7 | 0.0146 (10) | 0.0131 (9) | 0.0221 (10) | −0.0019 (7) | 0.0025 (8) | −0.0004 (8) |
C8 | 0.0169 (10) | 0.0155 (9) | 0.0199 (10) | 0.0005 (8) | 0.0023 (8) | −0.0028 (8) |
C9 | 0.0157 (10) | 0.0137 (10) | 0.0256 (11) | 0.0008 (7) | 0.0012 (8) | −0.0010 (8) |
Geometric parameters (Å, º) top
Co1—O1 | 2.0620 (13) | O7—H7A | 0.819 (15) |
Co1—O1i | 2.0621 (13) | O7—H7B | 0.839 (15) |
Co1—O7 | 2.1645 (15) | O8—H8A | 0.824 (15) |
Co1—O7i | 2.1646 (15) | O8—H8B | 0.835 (15) |
Co1—O8i | 2.0760 (15) | O9—H9A | 0.8410 |
Co1—O8 | 2.0760 (15) | O9—H9B | 0.8481 |
Ca1—O3ii | 2.4641 (15) | O10—H10A | 0.861 (15) |
Ca1—O3 | 2.4641 (15) | O10—H10B | 0.835 (16) |
Ca1—O4 | 2.5393 (15) | C1—C2 | 1.514 (3) |
Ca1—O4ii | 2.5393 (15) | C2—C3 | 1.390 (3) |
Ca1—O9ii | 2.4526 (17) | C2—C7 | 1.391 (3) |
Ca1—O9 | 2.4526 (17) | C3—H3 | 0.9300 |
Ca1—O10 | 2.4013 (16) | C3—C4 | 1.394 (3) |
Ca1—O10ii | 2.4013 (16) | C4—C5 | 1.392 (3) |
O1—C1 | 1.259 (2) | C4—C8 | 1.501 (3) |
O2—C1 | 1.257 (2) | C5—H5 | 0.9300 |
O3—C8 | 1.249 (2) | C5—C6 | 1.395 (3) |
O4—C8 | 1.273 (2) | C6—C7 | 1.392 (3) |
O5—C9 | 1.222 (2) | C6—C9 | 1.489 (3) |
O6—H6 | 0.841 (18) | C7—H7 | 0.9300 |
O6—C9 | 1.297 (2) | | |
| | | |
O1—Co1—O1i | 180.0 | C1—O1—Co1 | 128.47 (12) |
O1i—Co1—O7 | 85.73 (5) | C8—O3—Ca1 | 94.55 (12) |
O1—Co1—O7i | 85.73 (5) | C8—O4—Ca1 | 90.45 (11) |
O1—Co1—O7 | 94.27 (5) | C9—O6—H6 | 111.1 (13) |
O1i—Co1—O7i | 94.27 (5) | Co1—O7—H7A | 115.2 (16) |
O1—Co1—O8i | 89.72 (5) | Co1—O7—H7B | 113.2 (15) |
O1—Co1—O8 | 90.27 (5) | H7A—O7—H7B | 106 (2) |
O1i—Co1—O8i | 90.28 (5) | Co1—O8—H8A | 120.2 (15) |
O1i—Co1—O8 | 89.73 (5) | Co1—O8—H8B | 118.4 (15) |
O7—Co1—O7i | 180.0 | H8A—O8—H8B | 106 (2) |
O8—Co1—O7 | 89.10 (6) | Ca1—O9—H9A | 131.4 |
O8i—Co1—O7 | 90.90 (6) | Ca1—O9—H9B | 113.5 |
O8—Co1—O7i | 90.90 (6) | H9A—O9—H9B | 114.3 |
O8i—Co1—O7i | 89.10 (6) | Ca1—O10—H10A | 123.9 (15) |
O8i—Co1—O8 | 180.0 | Ca1—O10—H10B | 127.9 (16) |
O3—Ca1—O3ii | 90.98 (7) | H10A—O10—H10B | 107 (2) |
O3ii—Ca1—O4ii | 52.03 (5) | O1—C1—C2 | 116.17 (17) |
O3—Ca1—O4 | 52.03 (5) | O2—C1—O1 | 123.26 (17) |
O3—Ca1—O4ii | 142.83 (5) | O2—C1—C2 | 120.57 (17) |
O3ii—Ca1—O4 | 142.83 (5) | C3—C2—C1 | 119.52 (17) |
O4ii—Ca1—O4 | 165.11 (6) | C3—C2—C7 | 118.76 (17) |
O9—Ca1—O3ii | 76.69 (6) | C7—C2—C1 | 121.70 (17) |
O9ii—Ca1—O3ii | 78.78 (6) | C2—C3—H3 | 119.3 |
O9ii—Ca1—O3 | 76.69 (6) | C2—C3—C4 | 121.34 (17) |
O9—Ca1—O3 | 78.78 (6) | C4—C3—H3 | 119.3 |
O9ii—Ca1—O4ii | 96.66 (5) | C3—C4—C8 | 119.47 (17) |
O9ii—Ca1—O4 | 87.86 (6) | C5—C4—C3 | 119.48 (17) |
O9—Ca1—O4 | 96.66 (5) | C5—C4—C8 | 120.95 (17) |
O9—Ca1—O4ii | 87.86 (6) | C4—C5—H5 | 120.2 |
O9ii—Ca1—O9 | 144.73 (8) | C4—C5—C6 | 119.61 (17) |
O10—Ca1—O3ii | 127.04 (5) | C6—C5—H5 | 120.2 |
O10ii—Ca1—O3ii | 120.85 (6) | C5—C6—C9 | 120.02 (16) |
O10—Ca1—O3 | 120.85 (6) | C7—C6—C5 | 120.26 (17) |
O10ii—Ca1—O3 | 127.04 (5) | C7—C6—C9 | 119.63 (17) |
O10—Ca1—O4ii | 85.77 (5) | C2—C7—C6 | 120.52 (18) |
O10—Ca1—O4 | 82.40 (5) | C2—C7—H7 | 119.7 |
O10ii—Ca1—O4 | 85.77 (5) | C6—C7—H7 | 119.7 |
O10ii—Ca1—O4ii | 82.40 (5) | O3—C8—O4 | 121.02 (18) |
O10ii—Ca1—O9 | 144.47 (6) | O3—C8—C4 | 119.55 (17) |
O10—Ca1—O9ii | 144.47 (6) | O4—C8—C4 | 119.39 (17) |
O10ii—Ca1—O9ii | 70.62 (6) | O5—C9—O6 | 123.65 (18) |
O10—Ca1—O9 | 70.62 (6) | O5—C9—C6 | 123.26 (18) |
O10ii—Ca1—O10 | 74.63 (9) | O6—C9—C6 | 113.07 (16) |
| | | |
Co1—O1—C1—O2 | −5.3 (3) | C3—C4—C5—C6 | 1.5 (3) |
Co1—O1—C1—C2 | 174.87 (12) | C3—C4—C8—O3 | −5.4 (3) |
Ca1—O3—C8—O4 | 14.5 (2) | C3—C4—C8—O4 | 177.01 (18) |
Ca1—O3—C8—C4 | −163.08 (15) | C4—C5—C6—C7 | −1.8 (3) |
Ca1—O4—C8—O3 | −14.0 (2) | C4—C5—C6—C9 | 174.90 (17) |
Ca1—O4—C8—C4 | 163.57 (16) | C5—C4—C8—O3 | 170.90 (19) |
O1—C1—C2—C3 | −6.8 (3) | C5—C4—C8—O4 | −6.7 (3) |
O1—C1—C2—C7 | 174.80 (18) | C5—C6—C7—C2 | 0.8 (3) |
O2—C1—C2—C3 | 173.34 (19) | C5—C6—C9—O5 | 9.4 (3) |
O2—C1—C2—C7 | −5.1 (3) | C5—C6—C9—O6 | −169.1 (2) |
C1—C2—C3—C4 | −179.23 (17) | C7—C2—C3—C4 | −0.8 (3) |
C1—C2—C7—C6 | 178.93 (17) | C7—C6—C9—O5 | −173.9 (2) |
C2—C3—C4—C5 | −0.2 (3) | C7—C6—C9—O6 | 7.6 (3) |
C2—C3—C4—C8 | 176.09 (18) | C8—C4—C5—C6 | −174.76 (17) |
C3—C2—C7—C6 | 0.5 (3) | C9—C6—C7—C2 | −175.93 (18) |
Symmetry codes: (i) −x−1/2, −y−1/2, −z; (ii) −x, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6···O2iii | 0.84 (2) | 1.74 (2) | 2.539 (2) | 158 (2) |
O7—H7A···O4iv | 0.82 (2) | 2.09 (2) | 2.890 (2) | 165 (2) |
O7—H7B···O5v | 0.84 (2) | 2.11 (2) | 2.904 (2) | 158 (2) |
O8—H8A···O4v | 0.82 (2) | 1.93 (2) | 2.732 (2) | 165 (2) |
O8—H8B···O2i | 0.84 (2) | 2.50 (2) | 3.058 (2) | 125 (2) |
O8—H8B···O5iv | 0.84 (2) | 2.34 (2) | 3.027 (2) | 140 (2) |
O9—H9A···O3vi | 0.84 (2) | 1.93 (2) | 2.745 (2) | 165 (1) |
O10—H10A···O5vii | 0.86 (2) | 1.93 (2) | 2.768 (2) | 163 (3) |
O10—H10B···O7viii | 0.84 (2) | 2.14 (2) | 2.968 (2) | 171 (3) |
Symmetry codes: (i) −x−1/2, −y−1/2, −z; (iii) −x−1, −y, −z; (iv) −x−1/2, y−1/2, −z−1/2; (v) x, −y, z−1/2; (vi) −x, −y, −z; (vii) −x−1/2, −y+1/2, −z; (viii) x+1/2, y+1/2, z. |
Poly[[decaaquabis(µ
3-benzene-1,3,5-tricarboxylato)calcium(II)dizinc(II)]
dihydrate] (3)
top
Crystal data top
[CaZn2(C6H3O6)2(H2O)10]·2H2O | Dx = 1.932 Mg m−3 |
Mr = 801.24 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Ccce | Cell parameters from 1824 reflections |
a = 6.9927 (9) Å | θ = 3.3–27.1° |
b = 18.934 (2) Å | µ = 2.04 mm−1 |
c = 20.808 (2) Å | T = 296 K |
V = 2755.0 (6) Å3 | Block, light colourless |
Z = 4 | 0.4 × 0.2 × 0.2 mm |
F(000) = 1640 | |
Data collection top
Bruker D8 QUEST CMOS PHOTON II diffractometer | 1730 independent reflections |
Radiation source: sealed x-ray tube | 1184 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.083 |
Detector resolution: 7.39 pixels mm-1 | θmax = 28.3°, θmin = 2.9° |
φ and ω scans | h = −9→8 |
Absorption correction: multi-scan (SADABS; Bruker, 2021) | k = −25→24 |
Tmin = 0.640, Tmax = 0.746 | l = −27→27 |
12352 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: inferred from neighbouring sites |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.040 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.112 | w = 1/[σ2(Fo2) + (0.0412P)2 + 7.6311P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
1730 reflections | Δρmax = 0.72 e Å−3 |
134 parameters | Δρmin = −0.48 e Å−3 |
15 restraints | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Zn1 | 0.250000 | 0.500000 | 0.63791 (3) | 0.03042 (19) | |
Ca1 | 0.000000 | 0.250000 | 0.250000 | 0.0306 (3) | |
O1 | 0.1624 (4) | 0.42831 (13) | 0.57094 (13) | 0.0408 (7) | |
O2 | 0.0367 (4) | 0.38210 (14) | 0.65775 (12) | 0.0390 (7) | |
O3 | 0.0178 (5) | 0.19294 (13) | 0.35990 (11) | 0.0386 (7) | |
O4 | 0.5142 (5) | 0.44813 (14) | 0.64670 (15) | 0.0450 (7) | |
H4A | 0.577 (5) | 0.461 (2) | 0.6138 (16) | 0.068* | |
H4B | 0.491 (6) | 0.4052 (11) | 0.640 (2) | 0.068* | |
O5 | 0.250000 | 0.500000 | 0.7385 (2) | 0.0506 (11) | |
H5A | 0.261 (18) | 0.5417 (17) | 0.753 (3) | 0.076* | 0.5 |
H5B | 0.351 (10) | 0.481 (6) | 0.753 (3) | 0.076* | 0.5 |
O6 | 0.2492 (5) | 0.3353 (2) | 0.25836 (15) | 0.0640 (10) | |
H6A | 0.327 (6) | 0.342 (3) | 0.2270 (16) | 0.096* | |
H6B | 0.324 (6) | 0.338 (3) | 0.2905 (16) | 0.096* | |
O7 | 0.226 (5) | 0.493 (2) | 0.4497 (3) | 0.055 (5) | 0.5 |
H7A | 0.200 (19) | 0.521 (4) | 0.481 (4) | 0.082* | 0.5 |
H7B | 0.228 (19) | 0.453 (3) | 0.468 (4) | 0.082* | 0.5 |
C1 | 0.0790 (5) | 0.37818 (17) | 0.59974 (17) | 0.0274 (8) | |
C2 | 0.0350 (5) | 0.31241 (16) | 0.56248 (15) | 0.0221 (7) | |
C3 | 0.0339 (5) | 0.31200 (16) | 0.49550 (15) | 0.0237 (7) | |
H3 | 0.056038 | 0.353680 | 0.473065 | 0.028* | |
C4 | 0.000000 | 0.250000 | 0.4621 (2) | 0.0207 (9) | |
C5 | 0.000000 | 0.250000 | 0.5956 (2) | 0.0247 (10) | |
H5 | −0.000001 | 0.249999 | 0.640258 | 0.030* | |
C6 | 0.000000 | 0.250000 | 0.3896 (2) | 0.0237 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0465 (4) | 0.0193 (3) | 0.0255 (3) | −0.0017 (3) | 0.000 | 0.000 |
Ca1 | 0.0312 (8) | 0.0416 (8) | 0.0189 (6) | 0.000 | 0.000 | 0.000 |
O1 | 0.0603 (19) | 0.0231 (12) | 0.0389 (15) | −0.0133 (13) | 0.0042 (14) | −0.0038 (11) |
O2 | 0.062 (2) | 0.0312 (13) | 0.0241 (12) | 0.0019 (13) | −0.0007 (13) | −0.0075 (10) |
O3 | 0.069 (2) | 0.0255 (12) | 0.0211 (12) | 0.0053 (13) | −0.0018 (13) | −0.0042 (10) |
O4 | 0.0502 (19) | 0.0266 (13) | 0.0583 (18) | 0.0004 (13) | 0.0048 (16) | −0.0022 (13) |
O5 | 0.076 (4) | 0.045 (2) | 0.031 (2) | 0.003 (2) | 0.000 | 0.000 |
O6 | 0.053 (2) | 0.108 (3) | 0.0309 (15) | −0.036 (2) | −0.0006 (15) | 0.0057 (18) |
O7 | 0.060 (16) | 0.065 (13) | 0.040 (3) | −0.016 (8) | −0.004 (5) | 0.006 (5) |
C1 | 0.031 (2) | 0.0197 (15) | 0.0313 (18) | 0.0004 (14) | −0.0059 (15) | −0.0017 (13) |
C2 | 0.0258 (18) | 0.0182 (14) | 0.0222 (16) | −0.0002 (13) | −0.0011 (13) | −0.0014 (12) |
C3 | 0.030 (2) | 0.0196 (14) | 0.0214 (15) | −0.0002 (14) | −0.0001 (14) | 0.0022 (12) |
C4 | 0.023 (2) | 0.018 (2) | 0.022 (2) | −0.0015 (17) | 0.000 | 0.000 |
C5 | 0.031 (3) | 0.021 (2) | 0.022 (2) | −0.003 (2) | 0.000 | 0.000 |
C6 | 0.028 (3) | 0.024 (2) | 0.020 (2) | 0.000 (2) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Zn1—O1 | 2.039 (3) | O5—H5A | 0.85 (2) |
Zn1—O1i | 2.039 (3) | O5—H5Ai | 0.85 (2) |
Zn1—O4 | 2.100 (3) | O5—H5Bi | 0.85 (2) |
Zn1—O4i | 2.100 (3) | O5—H5B | 0.85 (2) |
Zn1—O5 | 2.093 (4) | O6—H6A | 0.862 (19) |
Ca1—O3 | 2.532 (2) | O6—H6B | 0.850 (19) |
Ca1—O3ii | 2.532 (2) | O7—H7Ai | 0.87 (8) |
Ca1—O3iii | 2.532 (2) | O7—H7A | 0.85 (2) |
Ca1—O3iv | 2.532 (2) | O7—H7B | 0.85 (2) |
Ca1—O6iv | 2.383 (3) | O7—H7Bi | 1.13 (8) |
Ca1—O6ii | 2.383 (3) | C1—C2 | 1.499 (4) |
Ca1—O6iii | 2.383 (3) | C2—C3 | 1.394 (4) |
Ca1—O6 | 2.383 (3) | C2—C5 | 1.389 (4) |
O1—C1 | 1.265 (4) | C3—H3 | 0.9300 |
O2—C1 | 1.245 (4) | C3—C4 | 1.384 (4) |
O3—C6 | 1.251 (3) | C4—C6 | 1.509 (6) |
O3—C6iii | 1.251 (3) | C4—C6iii | 1.509 (6) |
O4—H4A | 0.850 (19) | C5—H5 | 0.9300 |
O4—H4B | 0.840 (19) | C6—C6iii | 0.000 (9) |
| | | |
O1—Zn1—O1i | 93.81 (15) | H4A—O4—H4B | 104 (4) |
O1i—Zn1—O4i | 90.72 (12) | Zn1—O5—H5A | 111 (4) |
O1—Zn1—O4 | 90.72 (12) | Zn1—O5—H5Ai | 111 (4) |
O1—Zn1—O4i | 96.12 (12) | Zn1—O5—H5B | 111 (4) |
O1i—Zn1—O4 | 96.12 (12) | Zn1—O5—H5Bi | 111 (4) |
O1—Zn1—O5 | 133.10 (7) | H5A—O5—H5Ai | 137 (9) |
O1i—Zn1—O5 | 133.10 (7) | H5A—O5—H5Bi | 63 (7) |
O4i—Zn1—O4 | 170.00 (17) | H5A—O5—H5B | 101 (4) |
O5—Zn1—O4 | 85.00 (8) | H5Ai—O5—H5Bi | 101 (4) |
O5—Zn1—O4i | 85.00 (8) | H5B—O5—H5Ai | 63 (7) |
O3—Ca1—O3ii | 129.49 (11) | H5B—O5—H5Bi | 138 (9) |
O3ii—Ca1—O3iii | 174.38 (15) | Ca1—O6—H6A | 121 (3) |
O3—Ca1—O3iii | 50.87 (11) | Ca1—O6—H6B | 123 (3) |
O3—Ca1—O3iv | 174.38 (15) | H6A—O6—H6B | 101 (4) |
O3iii—Ca1—O3iv | 129.49 (11) | H7A—O7—H7Ai | 76 (10) |
O3ii—Ca1—O3iv | 50.87 (11) | H7Ai—O7—H7Bi | 82 (6) |
O6—Ca1—O3ii | 113.03 (10) | H7A—O7—H7B | 103 (5) |
O6iii—Ca1—O3iv | 113.03 (10) | H7A—O7—H7Bi | 42 (10) |
O6ii—Ca1—O3 | 113.03 (10) | H7B—O7—H7Ai | 52 (10) |
O6iv—Ca1—O3 | 74.98 (10) | H7B—O7—H7Bi | 131 (10) |
O6iv—Ca1—O3iv | 100.80 (10) | O1—C1—C2 | 118.2 (3) |
O6iii—Ca1—O3iii | 100.80 (10) | O2—C1—O1 | 121.6 (3) |
O6iii—Ca1—O3 | 71.37 (10) | O2—C1—C2 | 120.1 (3) |
O6ii—Ca1—O3iii | 74.98 (10) | C3—C2—C1 | 121.5 (3) |
O6ii—Ca1—O3iv | 71.37 (10) | C5—C2—C1 | 119.1 (3) |
O6iv—Ca1—O3iii | 113.03 (10) | C5—C2—C3 | 119.3 (3) |
O6—Ca1—O3iv | 74.98 (10) | C2—C3—H3 | 119.8 |
O6—Ca1—O3iii | 71.37 (10) | C4—C3—C2 | 120.5 (3) |
O6—Ca1—O3 | 100.81 (10) | C4—C3—H3 | 119.8 |
O6iii—Ca1—O3ii | 74.98 (10) | C3iii—C4—C3 | 119.8 (4) |
O6iv—Ca1—O3ii | 71.37 (10) | C3—C4—C6 | 120.1 (2) |
O6ii—Ca1—O3ii | 100.80 (10) | C3iii—C4—C6iii | 120.1 (2) |
O6ii—Ca1—O6iv | 171.62 (15) | C3iii—C4—C6 | 120.1 (2) |
O6iii—Ca1—O6iv | 94.6 (2) | C3—C4—C6iii | 120.1 (2) |
O6iv—Ca1—O6 | 86.0 (2) | C6—C4—C6iii | 0.0 |
O6iii—Ca1—O6 | 171.62 (15) | C2—C5—C2iii | 120.6 (4) |
O6ii—Ca1—O6 | 94.6 (2) | C2—C5—H5 | 119.7 |
O6iii—Ca1—O6ii | 86.0 (2) | C2iii—C5—H5 | 119.7 |
C1—O1—Zn1 | 108.3 (2) | O3iii—C6—O3 | 120.7 (4) |
C6—O3—Ca1 | 94.2 (2) | O3—C6—C4 | 119.6 (2) |
C6iii—O3—Ca1 | 94.2 (2) | O3iii—C6—C4 | 119.6 (2) |
C6iii—O3—C6 | 0.0 (3) | C6iii—C6—O3 | 0 (10) |
Zn1—O4—H4A | 105 (3) | C6iii—C6—O3iii | 0 (10) |
Zn1—O4—H4B | 106 (3) | C6iii—C6—C4 | 0 (10) |
| | | |
Zn1—O1—C1—O2 | 10.3 (4) | C2—C3—C4—C6iii | −179.7 (2) |
Zn1—O1—C1—C2 | −168.4 (3) | C3—C2—C5—C2iii | 0.3 (2) |
Ca1—O3—C6—O3iii | 0.000 (1) | C3—C4—C6—O3 | 162.0 (2) |
Ca1—O3—C6—C4 | 180.000 (1) | C3iii—C4—C6—O3 | −18.0 (2) |
Ca1—O3—C6—C6iii | 0.00 (13) | C3—C4—C6—O3iii | −18.0 (2) |
O1—C1—C2—C3 | −18.0 (5) | C3iii—C4—C6—O3iii | 162.0 (2) |
O1—C1—C2—C5 | 160.1 (3) | C3iii—C4—C6—C6iii | 0.0 (5) |
O2—C1—C2—C3 | 163.3 (3) | C3—C4—C6—C6iii | 0 (100) |
O2—C1—C2—C5 | −18.6 (5) | C5—C2—C3—C4 | −0.6 (5) |
C1—C2—C3—C4 | 177.5 (3) | C6iii—O3—C6—O3iii | 0 (100) |
C1—C2—C5—C2iii | −177.9 (4) | C6iii—O3—C6—C4 | 0 (100) |
C2—C3—C4—C3iii | 0.3 (2) | C6iii—C4—C6—O3iii | 0 (100) |
C2—C3—C4—C6 | −179.7 (2) | C6iii—C4—C6—O3 | 0 (100) |
Symmetry codes: (i) −x+1/2, −y+1, z; (ii) −x, y, −z+1/2; (iii) −x, −y+1/2, z; (iv) x, −y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H4A···O7v | 0.85 (2) | 1.79 (3) | 2.636 (17) | 174 (5) |
O4—H4A···O7vi | 0.85 (2) | 2.09 (3) | 2.926 (19) | 165 (5) |
O4—H4B···O3vii | 0.84 (2) | 1.86 (2) | 2.684 (4) | 167 (4) |
O5—H5A···O6viii | 0.85 (2) | 2.33 (3) | 3.145 (4) | 160 (6) |
O5—H5B···O4ix | 0.85 (2) | 2.37 (4) | 3.065 (5) | 139 (6) |
O6—H6A···O2x | 0.86 (2) | 1.88 (2) | 2.722 (4) | 164 (6) |
O6—H6B···O2v | 0.85 (2) | 2.02 (2) | 2.806 (4) | 153 (4) |
O7—H7A···O1i | 0.85 (2) | 2.32 (9) | 3.030 (17) | 141 (12) |
O7—H7B···O1 | 0.85 (2) | 2.25 (9) | 2.841 (15) | 127 (9) |
Symmetry codes: (i) −x+1/2, −y+1, z; (v) x+1/2, y, −z+1; (vi) −x+1, −y+1, −z+1; (vii) −x+1/2, −y+1/2, −z+1; (viii) x, −y+1, z+1/2; (ix) −x+1, y, −z+3/2; (x) −x+1/2, y, z−1/2. |