Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S205252061901343X/lo5053sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S205252061901343X/lo5053Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S205252061901343X/lo5053sup3.pdf |
CCDC reference: 1956842
Cu6H16O21S2Zn | Dx = 3.474 Mg m−3 Dm = 3.48 Mg m−3 Dm measured by ? |
Mr = 862.86 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3 | Cell parameters from 7472 reflections |
a = 8.1905 (12) Å | θ = 5.7–15.6° |
c = 7.0990 (14) Å | µ = 9.38 mm−1 |
V = 412.43 (15) Å3 | T = 100 K |
Z = 1 | Plate, blue |
F(000) = 420 | 0.03 × 0.02 × 0.004 mm |
ADSC Quantum 210r diffractometer | 1522 reflections with I > 2σ(I) |
φ scans | Rint = 0.052 |
Absorption correction: multi-scan Multi-scan SADABS | θmax = 29.6°, θmin = 2.9° |
Tmin = 0.509, Tmax = 0.746 | h = −10→10 |
7949 measured reflections | k = −11→11 |
1545 independent reflections | l = −9→9 |
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.027 | w = 1/[σ2(Fo2) + (0.0816P)2 + 0.7665P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.080 | (Δ/σ)max < 0.001 |
S = 0.76 | Δρmax = 1.74 e Å−3 |
1545 reflections | Δρmin = −0.98 e Å−3 |
108 parameters | Extinction correction: SHELXL-2018/1 (Sheldrick 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
5 restraints | Extinction coefficient: 0.034 (6) |
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. |
Refinement. Refined as a 2-component inversion twin. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cu1 | 0.37307 (9) | 0.46800 (9) | 0.21533 (9) | 0.0123 (3) | 0.968 (10) |
Cu2 | 0.24679 (8) | 0.05639 (9) | 0.21189 (8) | 0.0118 (3) | 0.952 (10) |
ZN | 0.666667 | 0.333333 | 0.97881 (16) | 0.0116 (4) | |
S1 | 0.666667 | 0.333333 | 0.4807 (4) | 0.0169 (7) | |
S2 | 0.000000 | 0.000000 | 0.7911 (4) | 0.0128 (8) | |
O1 | 0.5184 (8) | 0.1423 (9) | 0.4149 (8) | 0.0287 (11) | |
O2 | 0.666667 | 0.333333 | 0.6953 (15) | 0.027 (2) | |
O3 | 0.1797 (6) | 0.1608 (6) | 0.7238 (6) | 0.0201 (9) | |
O4 | 0.000000 | 0.000000 | 0.0006 (10) | 0.0153 (14) | |
OH1 | 0.4134 (6) | 0.2817 (6) | 0.0521 (8) | 0.0159 (11) | |
OH2 | 0.1119 (6) | 0.4249 (5) | 0.0872 (8) | 0.0167 (9) | |
OH3 | 0.1772 (5) | 0.2276 (5) | 0.3403 (8) | 0.0155 (10) | |
OH4 | 0.333333 | 0.666667 | 0.3540 (12) | 0.0180 (15) | |
OW1 | 0.1111 (7) | 0.5056 (8) | 0.7158 (8) | 0.0345 (12) | |
H1 | 0.349 (17) | 0.256 (16) | −0.062 (12) | 0.050* | |
H2 | 0.123 (16) | 0.443 (17) | −0.039 (10) | 0.050* | |
H3 | 0.183 (17) | 0.201 (19) | 0.458 (11) | 0.050* | |
H4 | 0.333333 | 0.666667 | 0.488 (10) | 0.050* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0095 (4) | 0.0088 (4) | 0.0182 (4) | 0.0043 (2) | −0.0001 (2) | −0.00019 (19) |
Cu2 | 0.0101 (3) | 0.0084 (3) | 0.0163 (4) | 0.0042 (2) | −0.0001 (2) | 0.0005 (2) |
ZN | 0.0091 (4) | 0.0091 (4) | 0.0166 (5) | 0.0046 (2) | 0.000 | 0.000 |
S1 | 0.0149 (8) | 0.0149 (8) | 0.0207 (12) | 0.0075 (4) | 0.000 | 0.000 |
S2 | 0.0123 (9) | 0.0123 (9) | 0.0138 (11) | 0.0062 (4) | 0.000 | 0.000 |
O1 | 0.026 (2) | 0.031 (3) | 0.032 (3) | 0.016 (2) | 0.000 (2) | 0.003 (2) |
O2 | 0.028 (2) | 0.028 (2) | 0.025 (5) | 0.0140 (12) | 0.000 | 0.000 |
O3 | 0.0172 (17) | 0.0183 (19) | 0.0211 (17) | 0.0061 (15) | 0.0013 (14) | 0.0019 (13) |
O4 | 0.018 (2) | 0.018 (2) | 0.010 (3) | 0.0089 (10) | 0.000 | 0.000 |
OH1 | 0.0111 (16) | 0.0135 (18) | 0.023 (3) | 0.0060 (13) | 0.0020 (13) | 0.0027 (12) |
OH2 | 0.0166 (17) | 0.0137 (19) | 0.020 (2) | 0.0079 (14) | 0.0013 (15) | 0.0009 (12) |
OH3 | 0.0110 (16) | 0.018 (2) | 0.018 (2) | 0.0074 (14) | −0.0004 (13) | −0.0010 (13) |
OH4 | 0.017 (2) | 0.017 (2) | 0.020 (4) | 0.0086 (10) | 0.000 | 0.000 |
OW1 | 0.022 (2) | 0.037 (3) | 0.028 (2) | 0.003 (2) | −0.0011 (17) | 0.002 (2) |
Cu1—OH2i | 1.953 (5) | ZN—OH1v | 1.968 (4) |
Cu1—OH3 | 2.019 (4) | ZN—O2 | 2.013 (11) |
Cu1—OH4 | 2.062 (4) | S1—O1vi | 1.497 (6) |
Cu1—OH1 | 2.070 (5) | S1—O1vii | 1.497 (6) |
Cu1—OH2 | 2.185 (5) | S1—O1 | 1.497 (6) |
Cu1—O1 | 2.455 (5) | S1—O2 | 1.523 (13) |
Cu1—Cu2 | 2.9915 (10) | S2—O3ii | 1.480 (4) |
Cu2—OH2ii | 1.930 (4) | S2—O3 | 1.480 (4) |
Cu2—OH3 | 1.980 (4) | S2—O3viii | 1.480 (4) |
Cu2—OH3ii | 2.001 (4) | S2—O4v | 1.487 (7) |
Cu2—OH1 | 2.009 (4) | OH1—H1 | 0.93 (6) |
Cu2—O4 | 2.370 (5) | OH2—H2 | 0.90 (7) |
Cu2—O1 | 2.442 (5) | OH3—H3 | 0.87 (7) |
ZN—OH1iii | 1.968 (4) | OH4—H4 | 0.95 (7) |
ZN—OH1iv | 1.968 (4) | ||
OH2i—Cu1—OH3 | 174.35 (18) | O1vii—S1—O2 | 108.2 (2) |
OH2i—Cu1—OH4 | 83.88 (18) | O1—S1—O2 | 108.2 (2) |
OH3—Cu1—OH4 | 101.4 (2) | O3ii—S2—O3 | 110.12 (18) |
OH2i—Cu1—OH1 | 92.4 (2) | O3ii—S2—O3viii | 110.11 (18) |
OH3—Cu1—OH1 | 82.47 (16) | O3—S2—O3viii | 110.11 (18) |
OH4—Cu1—OH1 | 174.4 (3) | O3ii—S2—O4v | 108.82 (18) |
OH2i—Cu1—OH2 | 105.4 (3) | O3—S2—O4v | 108.82 (18) |
OH3—Cu1—OH2 | 77.83 (15) | O3viii—S2—O4v | 108.82 (18) |
OH4—Cu1—OH2 | 78.35 (16) | S1—O2—ZN | 180.0 |
OH1—Cu1—OH2 | 98.75 (17) | S2ix—O4—Cu2 | 129.27 (14) |
OH2i—Cu1—Cu2 | 133.46 (14) | S2ix—O4—Cu2viii | 129.27 (14) |
OH3—Cu1—Cu2 | 41.09 (12) | Cu2—O4—Cu2viii | 84.2 (2) |
OH4—Cu1—Cu2 | 142.29 (15) | S2ix—O4—Cu2ii | 129.27 (14) |
OH1—Cu1—Cu2 | 42.04 (13) | Cu2—O4—Cu2ii | 84.2 (2) |
OH2—Cu1—Cu2 | 93.19 (10) | Cu2viii—O4—Cu2ii | 84.2 (2) |
OH2ii—Cu2—OH3 | 179.6 (2) | ZNix—OH1—Cu2 | 120.4 (2) |
OH2ii—Cu2—OH3ii | 84.53 (17) | ZNix—OH1—Cu1 | 121.9 (2) |
OH3—Cu2—OH3ii | 95.1 (2) | Cu2—OH1—Cu1 | 94.3 (2) |
OH2ii—Cu2—OH1 | 95.3 (2) | ZNix—OH1—H1 | 104 (8) |
OH3—Cu2—OH1 | 85.03 (18) | Cu2—OH1—H1 | 104 (8) |
OH3ii—Cu2—OH1 | 171.1 (2) | Cu1—OH1—H1 | 112 (7) |
OH2ii—Cu2—O4 | 95.02 (16) | Cu2viii—OH2—Cu1x | 108.2 (3) |
OH3—Cu2—O4 | 84.84 (18) | Cu2viii—OH2—Cu1 | 97.1 (2) |
OH3ii—Cu2—O4 | 84.40 (18) | Cu1x—OH2—Cu1 | 98.5 (2) |
OH1—Cu2—O4 | 86.74 (18) | Cu2viii—OH2—H2 | 126 (7) |
OH2ii—Cu2—Cu1 | 138.26 (15) | Cu1x—OH2—H2 | 111 (9) |
OH3—Cu2—Cu1 | 42.09 (12) | Cu1—OH2—H2 | 112 (8) |
OH3ii—Cu2—Cu1 | 137.20 (12) | Cu2—OH3—Cu2viii | 105.9 (2) |
OH1—Cu2—Cu1 | 43.64 (14) | Cu2—OH3—Cu1 | 96.8 (2) |
O4—Cu2—Cu1 | 90.31 (2) | Cu2viii—OH3—Cu1 | 100.4 (2) |
OH1iii—ZN—OH1iv | 113.28 (14) | Cu2—OH3—H3 | 101 (9) |
OH1iii—ZN—OH1v | 113.28 (14) | Cu2viii—OH3—H3 | 124 (8) |
OH1iv—ZN—OH1v | 113.28 (14) | Cu1—OH3—H3 | 123 (8) |
OH1iii—ZN—O2 | 105.32 (17) | Cu1—OH4—Cu1i | 99.1 (3) |
OH1iv—ZN—O2 | 105.32 (17) | Cu1—OH4—Cu1x | 99.1 (3) |
OH1v—ZN—O2 | 105.32 (17) | Cu1i—OH4—Cu1x | 99.1 (3) |
O1vi—S1—O1vii | 110.7 (2) | Cu1—OH4—H4 | 118.5 (2) |
O1vi—S1—O1 | 110.7 (2) | Cu1i—OH4—H4 | 118.5 (2) |
O1vii—S1—O1 | 110.7 (2) | Cu1x—OH4—H4 | 118.5 (2) |
O1vi—S1—O2 | 108.2 (2) |
Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x+y, −x, z; (iii) −y+1, x−y, z+1; (iv) −x+y+1, −x+1, z+1; (v) x, y, z+1; (vi) −y+1, x−y, z; (vii) −x+y+1, −x+1, z; (viii) −y, x−y, z; (ix) x, y, z−1; (x) −x+y, −x+1, z. |