Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618010264/ov3111sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229618010264/ov3111Isup2.hkl |
CCDC reference: 1526885
Data collection: CrysAlis PRO (Rigaku OD, 2015); cell refinement: CrysAlis PRO (Rigaku OD, 2015); data reduction: CrysAlis PRO (Rigaku OD, 2015); program(s) used to solve structure: SHELXS2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: Mercury (Macrae et al., 2008) and ORTEP 3 For Windows (Farrugia, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012), publCIF (Westrip, 2010) and TOPOSPRO (Blatov et al., 2016).
K[Zn(C8H3O7S)(H2O)4] | F(000) = 848 |
Mr = 419.7 | Dx = 2.079 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.7107 Å |
Hall symbol: -P 2yn | Cell parameters from 19501 reflections |
a = 6.7891 (1) Å | θ = 3.7–29.0° |
b = 16.7667 (2) Å | µ = 2.36 mm−1 |
c = 11.7793 (1) Å | T = 293 K |
β = 90.752 (1)° | Prismatic, colorless |
V = 1340.73 (3) Å3 | 0.40 × 0.31 × 0.09 mm |
Z = 4 |
Oxford Diffraction SuperNova Dual Source diffractometer with an AtlasS2 detector | 3640 independent reflections |
Radiation source: micro-focus sealed X-ray tube | 3313 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.044 |
Detector resolution: 5.2923 pixels mm-1 | θmax = 29.7°, θmin = 3.2° |
ω scans | h = −8→9 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015) | k = −22→23 |
Tmin = 0.735, Tmax = 1 | l = −16→16 |
41833 measured reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.027 | w = 1/[σ2(Fo2) + (0.0313P)2 + 0.8858P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.065 | (Δ/σ)max < 0.001 |
S = 1.03 | Δρmax = 0.39 e Å−3 |
3640 reflections | Δρmin = −0.53 e Å−3 |
210 parameters |
Experimental. #__ type_ start__ end____ width___ exp.time_ 1 omega -76.00 100.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 0.0000 0.0000 176 #__ type_ start__ end____ width___ exp.time_ 2 omega -20.00 53.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -99.0000 60.0000 73 #__ type_ start__ end____ width___ exp.time_ 3 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 90.0000 49 #__ type_ start__ end____ width___ exp.time_ 4 omega -85.00 16.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -57.0000 159.0000 101 #__ type_ start__ end____ width___ exp.time_ 5 omega -40.00 61.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 57.0000 -60.0000 101 #__ type_ start__ end____ width___ exp.time_ 6 omega -62.00 36.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -38.0000 -180.0000 98 #__ type_ start__ end____ width___ exp.time_ 7 omega -20.00 53.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -99.0000 -180.0000 73 #__ type_ start__ end____ width___ exp.time_ 8 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 -60.0000 49 #__ type_ start__ end____ width___ exp.time_ 9 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 30.0000 49 #__ type_ start__ end____ width___ exp.time_ 10 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 0.0000 49 #__ type_ start__ end____ width___ exp.time_ 11 omega -20.00 53.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -99.0000 -120.0000 73 #__ type_ start__ end____ width___ exp.time_ 12 omega -20.00 53.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 11.79 -99.0000 120.0000 73 #__ type_ start__ end____ width___ exp.time_ 13 omega -45.00 64.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 77.0000 -120.0000 109 #__ type_ start__ end____ width___ exp.time_ 14 omega -88.00 -40.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -77.0000 -30.0000 48 #__ type_ start__ end____ width___ exp.time_ 15 omega -20.00 29.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -12.03 -99.0000 -90.0000 49 |
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. Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. |
x | y | z | Uiso*/Ueq | ||
Zn | 0.32214 (3) | 0.24186 (2) | 0.25221 (2) | 0.02170 (7) | |
K | 0.64311 (6) | 0.06941 (3) | −0.36694 (4) | 0.03651 (11) | |
S1 | 0.17932 (6) | −0.00347 (2) | −0.34264 (3) | 0.01782 (9) | |
O1 | −0.02690 (19) | −0.02261 (8) | −0.36164 (11) | 0.0294 (3) | |
O2 | 0.23130 (18) | 0.07663 (7) | −0.37944 (10) | 0.0229 (2) | |
O3 | 0.3137 (2) | −0.06239 (8) | −0.38961 (11) | 0.0331 (3) | |
O4 | 0.3177 (2) | 0.14336 (7) | 0.14800 (10) | 0.0260 (3) | |
O5 | 0.3302 (2) | 0.20402 (7) | −0.02076 (11) | 0.0315 (3) | |
O6 | 0.20630 (19) | −0.15456 (7) | 0.15212 (10) | 0.0247 (3) | |
O7 | 0.1604 (2) | −0.21618 (8) | −0.01355 (11) | 0.0354 (3) | |
O8 | 0.2021 (3) | 0.17067 (10) | 0.37636 (12) | 0.0603 (6) | |
H8B | 0.159977 | 0.131735 | 0.372871 | 0.090* | |
H8A | 0.223746 | 0.185196 | 0.436560 | 0.090* | |
O9 | 0.6146 (2) | 0.21894 (8) | 0.31278 (11) | 0.0299 (3) | |
H9B | 0.648586 | 0.244628 | 0.361743 | 0.045* | |
H9A | 0.628231 | 0.173398 | 0.331105 | 0.045* | |
O10 | 0.41855 (19) | 0.31583 (7) | 0.12098 (10) | 0.0254 (3) | |
H10B | 0.517963 | 0.338394 | 0.120587 | 0.038* | |
H10A | 0.413573 | 0.287824 | 0.065490 | 0.038* | |
O11 | 0.02081 (19) | 0.27368 (8) | 0.19839 (12) | 0.0306 (3) | |
H11A | −0.027408 | 0.248246 | 0.143978 | 0.046* | |
H11B | −0.033653 | 0.269686 | 0.248681 | 0.046* | |
C1 | 0.2708 (2) | 0.06554 (9) | −0.01814 (13) | 0.0173 (3) | |
C2 | 0.2506 (2) | −0.00558 (9) | 0.04116 (13) | 0.0183 (3) | |
H2 | 0.261025 | −0.005655 | 0.119965 | 0.022* | |
C3 | 0.2149 (2) | −0.07678 (9) | −0.01654 (13) | 0.0179 (3) | |
C4 | 0.1975 (2) | −0.07603 (9) | −0.13446 (13) | 0.0190 (3) | |
H4 | 0.173554 | −0.123245 | −0.173700 | 0.023* | |
C5 | 0.2160 (2) | −0.00484 (9) | −0.19337 (13) | 0.0171 (3) | |
C6 | 0.2538 (2) | 0.06559 (9) | −0.13614 (13) | 0.0187 (3) | |
H6 | 0.267832 | 0.112947 | −0.176340 | 0.022* | |
C7 | 0.3089 (2) | 0.14364 (9) | 0.04129 (14) | 0.0202 (3) | |
C8 | 0.1920 (2) | −0.15534 (10) | 0.04498 (14) | 0.0201 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn | 0.03106 (12) | 0.01702 (11) | 0.01700 (11) | −0.00144 (7) | −0.00039 (8) | −0.00263 (7) |
K | 0.0276 (2) | 0.0373 (2) | 0.0447 (3) | −0.00300 (17) | 0.00112 (18) | −0.00491 (18) |
S1 | 0.0253 (2) | 0.01469 (18) | 0.01347 (17) | 0.00044 (14) | −0.00119 (14) | 0.00050 (13) |
O1 | 0.0321 (7) | 0.0289 (7) | 0.0270 (6) | −0.0093 (5) | −0.0088 (5) | 0.0037 (5) |
O2 | 0.0285 (6) | 0.0201 (6) | 0.0201 (6) | −0.0016 (5) | −0.0003 (5) | 0.0057 (4) |
O3 | 0.0510 (9) | 0.0283 (7) | 0.0201 (6) | 0.0166 (6) | 0.0022 (6) | −0.0029 (5) |
O4 | 0.0410 (7) | 0.0199 (6) | 0.0171 (6) | −0.0006 (5) | −0.0016 (5) | −0.0046 (4) |
O5 | 0.0540 (9) | 0.0165 (6) | 0.0235 (6) | −0.0053 (6) | −0.0097 (6) | −0.0009 (5) |
O6 | 0.0370 (7) | 0.0200 (6) | 0.0171 (6) | 0.0005 (5) | −0.0016 (5) | 0.0060 (4) |
O7 | 0.0620 (10) | 0.0181 (6) | 0.0258 (7) | −0.0075 (6) | −0.0141 (6) | 0.0043 (5) |
O8 | 0.1187 (17) | 0.0398 (9) | 0.0226 (7) | −0.0450 (10) | 0.0058 (8) | −0.0034 (6) |
O9 | 0.0416 (8) | 0.0229 (6) | 0.0251 (6) | 0.0070 (6) | −0.0074 (5) | −0.0057 (5) |
O10 | 0.0327 (7) | 0.0222 (6) | 0.0213 (6) | −0.0063 (5) | 0.0029 (5) | −0.0049 (5) |
O11 | 0.0275 (7) | 0.0318 (7) | 0.0324 (7) | −0.0026 (5) | −0.0036 (5) | −0.0051 (5) |
C1 | 0.0191 (7) | 0.0157 (7) | 0.0170 (7) | 0.0000 (6) | −0.0013 (6) | −0.0020 (5) |
C2 | 0.0202 (7) | 0.0201 (7) | 0.0146 (7) | 0.0014 (6) | −0.0016 (5) | 0.0005 (6) |
C3 | 0.0194 (7) | 0.0174 (7) | 0.0170 (7) | 0.0004 (6) | −0.0002 (6) | 0.0028 (6) |
C4 | 0.0239 (8) | 0.0148 (7) | 0.0182 (7) | −0.0016 (6) | −0.0008 (6) | −0.0004 (5) |
C5 | 0.0209 (7) | 0.0170 (7) | 0.0133 (7) | 0.0006 (6) | −0.0003 (5) | 0.0002 (5) |
C6 | 0.0240 (8) | 0.0145 (7) | 0.0176 (7) | −0.0005 (6) | 0.0006 (6) | 0.0014 (5) |
C7 | 0.0218 (8) | 0.0182 (7) | 0.0204 (8) | 0.0018 (6) | −0.0030 (6) | −0.0033 (6) |
C8 | 0.0211 (8) | 0.0186 (7) | 0.0203 (7) | −0.0008 (6) | −0.0021 (6) | 0.0040 (6) |
Zn—O4 | 2.0578 (12) | O6—C8 | 1.2646 (19) |
Zn—O8 | 2.0637 (15) | O7—C8 | 1.248 (2) |
Zn—O6i | 2.0806 (11) | C1—C2 | 1.390 (2) |
Zn—O10 | 2.0935 (12) | C1—C6 | 1.393 (2) |
Zn—O9 | 2.1360 (13) | C1—C7 | 1.506 (2) |
Zn—O11 | 2.1994 (13) | C2—C3 | 1.393 (2) |
Zn—Kii | 3.6627 (5) | C3—C4 | 1.392 (2) |
K—O10iii | 2.6882 (13) | C3—C8 | 1.513 (2) |
K—O1iv | 2.7202 (14) | C4—C5 | 1.387 (2) |
K—O2 | 2.8004 (13) | C5—C6 | 1.382 (2) |
K—O11iii | 2.8671 (14) | O8—H8A | 0.7600 |
K—O3v | 2.8889 (13) | O8—H8B | 0.7100 |
K—O6vi | 3.0689 (13) | O9—H9A | 0.8000 |
K—O3 | 3.1527 (16) | O9—H9B | 0.7500 |
K—S1 | 3.3931 (6) | O10—H10B | 0.7700 |
K—Kv | 4.3428 (9) | O10—H10A | 0.8100 |
S1—O1 | 1.4509 (13) | O11—H11B | 0.7100 |
S1—O2 | 1.4561 (12) | O11—H11A | 0.8300 |
S1—O3 | 1.4589 (13) | C2—H2 | 0.9300 |
S1—C5 | 1.7726 (15) | C4—H4 | 0.9300 |
O4—C7 | 1.258 (2) | C6—H6 | 0.9300 |
O5—C7 | 1.258 (2) | ||
O4—Zn—O8 | 87.46 (5) | S1—K—Kv | 57.383 (12) |
O4—Zn—O6i | 172.87 (5) | Zniii—K—Kv | 151.97 (2) |
O8—Zn—O6i | 93.37 (6) | O1—S1—O2 | 113.28 (7) |
O4—Zn—O10 | 92.14 (5) | O1—S1—O3 | 113.51 (9) |
O8—Zn—O10 | 174.95 (7) | O2—S1—O3 | 110.88 (8) |
O6i—Zn—O10 | 86.42 (5) | O1—S1—C5 | 105.83 (7) |
O4—Zn—O9 | 93.51 (5) | O2—S1—C5 | 106.02 (7) |
O8—Zn—O9 | 91.90 (7) | O3—S1—C5 | 106.68 (7) |
O6i—Zn—O9 | 93.54 (5) | O1—S1—K | 164.01 (5) |
O10—Zn—O9 | 93.15 (5) | O2—S1—K | 54.12 (5) |
O4—Zn—O11 | 90.94 (5) | O3—S1—K | 68.04 (6) |
O8—Zn—O11 | 88.29 (7) | C5—S1—K | 88.28 (5) |
O6i—Zn—O11 | 82.01 (5) | S1—O1—Kvii | 132.13 (8) |
O10—Zn—O11 | 86.68 (5) | S1—O2—K | 100.96 (6) |
O9—Zn—O11 | 175.55 (5) | S1—O3—Kv | 118.43 (7) |
O4—Zn—Kii | 117.56 (4) | S1—O3—K | 86.54 (6) |
O8—Zn—Kii | 129.73 (6) | Kv—O3—K | 91.81 (4) |
O6i—Zn—Kii | 56.89 (3) | C7—O4—Zn | 126.39 (11) |
O10—Zn—Kii | 46.42 (4) | C8—O6—Znviii | 121.69 (11) |
O9—Zn—Kii | 125.86 (4) | C8—O6—Kvi | 148.01 (10) |
O11—Zn—Kii | 51.49 (4) | Znviii—O6—Kvi | 88.51 (4) |
O10iii—K—O1iv | 80.44 (4) | Zn—O10—Kii | 99.23 (5) |
O10iii—K—O2 | 131.37 (4) | Zn—O11—Kii | 91.63 (4) |
O1iv—K—O2 | 147.90 (4) | C2—C1—C6 | 119.64 (14) |
O10iii—K—O11iii | 63.99 (4) | C2—C1—C7 | 122.01 (14) |
O1iv—K—O11iii | 139.08 (4) | C6—C1—C7 | 118.35 (14) |
O2—K—O11iii | 71.46 (4) | C1—C2—C3 | 120.51 (14) |
O10iii—K—O3v | 84.08 (4) | C4—C3—C2 | 119.39 (14) |
O1iv—K—O3v | 84.58 (4) | C4—C3—C8 | 118.55 (14) |
O2—K—O3v | 93.65 (4) | C2—C3—C8 | 122.06 (14) |
O11iii—K—O3v | 109.71 (4) | C5—C4—C3 | 119.99 (14) |
O10iii—K—O6vi | 59.09 (3) | C6—C5—C4 | 120.57 (14) |
O1iv—K—O6vi | 88.83 (4) | C6—C5—S1 | 119.69 (12) |
O2—K—O6vi | 110.17 (4) | C4—C5—S1 | 119.67 (12) |
O11iii—K—O6vi | 56.38 (4) | C5—C6—C1 | 119.90 (14) |
O3v—K—O6vi | 143.17 (4) | O4—C7—O5 | 125.41 (15) |
O10iii—K—O3 | 172.03 (4) | O4—C7—C1 | 117.84 (14) |
O1iv—K—O3 | 100.80 (4) | O5—C7—C1 | 116.75 (14) |
O2—K—O3 | 47.11 (3) | O7—C8—O6 | 124.76 (15) |
O11iii—K—O3 | 117.28 (4) | O7—C8—C3 | 117.72 (14) |
O3v—K—O3 | 88.19 (4) | O6—C8—C3 | 117.52 (14) |
O6vi—K—O3 | 128.62 (4) | Zn—O8—H8A | 114.00 |
O10iii—K—S1 | 155.39 (3) | Zn—O8—H8B | 131.00 |
O1iv—K—S1 | 123.97 (3) | H8A—O8—H8B | 115.00 |
O2—K—S1 | 24.92 (2) | Zn—O9—H9B | 115.00 |
O11iii—K—S1 | 92.03 (3) | H9A—O9—H9B | 108.00 |
O3v—K—S1 | 100.10 (3) | Zn—O9—H9A | 111.00 |
O6vi—K—S1 | 113.42 (3) | Zn—O10—H10A | 104.00 |
O3—K—S1 | 25.42 (2) | Zn—O10—H10B | 125.00 |
O10iii—K—Zniii | 34.34 (3) | K—O10—H10A | 116.00 |
O1iv—K—Zniii | 102.25 (3) | K—O10—H10B | 105.00 |
O2—K—Zniii | 107.99 (3) | H10A—O10—H10B | 108.00 |
O11iii—K—Zniii | 36.89 (3) | K—O11—H11B | 118.00 |
O3v—K—Zniii | 112.22 (3) | H11A—O11—H11B | 113.00 |
O6vi—K—Zniii | 34.60 (2) | K—O11—H11A | 112.00 |
O3—K—Zniii | 150.40 (3) | Zn—O11—H11A | 117.00 |
S1—K—Zniii | 125.621 (15) | Zn—O11—H11B | 103.00 |
O10iii—K—Kv | 130.57 (3) | C1—C2—H2 | 120.00 |
O1iv—K—Kv | 94.20 (3) | C3—C2—H2 | 120.00 |
O2—K—Kv | 63.14 (3) | C3—C4—H4 | 120.00 |
O11iii—K—Kv | 123.86 (3) | C5—C4—H4 | 120.00 |
O3v—K—Kv | 46.52 (3) | C1—C6—H6 | 120.00 |
O6vi—K—Kv | 170.24 (3) | C5—C6—H6 | 120.00 |
O3—K—Kv | 41.67 (2) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) x+1, y, z; (v) −x+1, −y, −z−1; (vi) −x+1, −y, −z; (vii) x−1, y, z; (viii) −x+1/2, y−1/2, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H8A···O7i | 0.76 | 2.04 | 2.653 (2) | 138 |
O8—H8B···O1ix | 0.71 | 2.05 | 2.759 (2) | 177 |
O9—H9A···O3vi | 0.80 | 2.02 | 2.8166 (19) | 174 |
O9—H9B···O5x | 0.75 | 2.03 | 2.7536 (18) | 160 |
O10—H10A···O5 | 0.81 | 1.82 | 2.5757 (17) | 156 |
O10—H10B···O2x | 0.77 | 2.03 | 2.7854 (17) | 165 |
O11—H11A···O7ix | 0.83 | 1.85 | 2.667 (2) | 166 |
C4—H4···O7 | 0.93 | 2.45 | 2.761 (2) | 100 |
C6—H6···O2 | 0.93 | 2.48 | 2.8741 (19) | 106 |
C6—H6···O5 | 0.93 | 2.42 | 2.7358 (19) | 100 |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (vi) −x+1, −y, −z; (ix) −x, −y, −z; (x) x+1/2, −y+1/2, z+1/2. |