Phase transitions in Rochelle salt [sodium potassium L(+)-tartrate tetrahydrate] are revisited in a single-crystal X-ray diffraction multi-temperature study on cooling from 308 to 100 K across the high-temperature paraelectric (PE) ↔ ferroelectric ↔ low-temperature PE phase transition points. The results of structure refinement using three different models (a harmonic with and without disorder, and an anharmonic) were compared. The temperature dependencies of anisotropic displacement parameters (ADPs) and Ueq, which can be calculated directly from ADPs, for the low-temperature PE phase indicate clearly the dynamic nature of disorder of the K1 atoms. The structures of the low-temperature and the high-temperature PE phases are compared for the first time at multiple temperatures for each phase based on diffraction data collected from the same single crystal. The data indicate that the high-temperature and the low-temperature paraelectric phases are probably not two different phases, as was assumed in earlier works, but are structurally the same phase at different temperatures.
Supporting information
| Crystallographic Information File (CIF) https://doi.org/10.1107/S205252062400115X/xk5105sup1.cif Contains datablocks global, 100K_har, 125K_har, 150K_har, 175K_anh, 200K_anh, 225K_anh, 243K_anh, 253K_anh, 256K_anh, 266K_anh, 276K_anh, 286K_anh, 296K_anh, 298K_anh, 308K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105100K_harsup2.hkl Contains datablock 100K_har |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105125K_harsup3.hkl Contains datablock 125K_har |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105150K_harsup4.hkl Contains datablock 150K_har |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105175K_anhsup5.hkl Contains datablock 175K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105200K_anhsup6.hkl Contains datablock 200K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105225K_anhsup7.hkl Contains datablock 225K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105243K_anhsup8.hkl Contains datablock 243K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105253K_anhsup9.hkl Contains datablock 253K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105256K_anhsup10.hkl Contains datablock 256K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105266K_anhsup11.hkl Contains datablock 266K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105276K_anhsup12.hkl Contains datablock 276K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105296K_anhsup14.hkl Contains datablock 296K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105298K_anhsup15.hkl Contains datablock 298K_anh |
| Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105308K_anhsup16.hkl Contains datablock 308K_anh |
| Portable Document Format (PDF) file https://doi.org/10.1107/S205252062400115X/xk5105sup17.pdf Supplementary material |
CCDC references: 2330587; 2330588; 2330589; 2330590; 2330591; 2330592; 2330593; 2330594; 2330595; 2330596; 2330597; 2330598; 2330599; 2330600; 2330601
Sodium potassium L(+)-tartrate tetrahydrate (100K_har)
top
Crystal data top
C4H12KNaO10 | Dx = 1.817 Mg m−3 |
Mr = 282.23 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 8586 reflections |
a = 11.7658 (6) Å | θ = 3.6–29.3° |
b = 14.1879 (8) Å | µ = 0.60 mm−1 |
c = 6.1811 (3) Å | T = 100 K |
V = 1031.83 (9) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 584 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2647 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2399 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.762, Tmax = 1.000 | l = −8→8 |
18029 measured reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.029 | w = 1/[σ2(Fo2) + (0.0192P)2 + 0.3649P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.060 | (Δ/σ)max < 0.001 |
S = 1.11 | Δρmax = 0.40 e Å−3 |
2647 reflections | Δρmin = −0.28 e Å−3 |
182 parameters | Absolute structure: Flack x determined using 911 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). |
1 restraint | Absolute structure parameter: −0.02 (2) |
Primary atom site location: iterative | |
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 | |
K1 | 0.000000 | 0.000000 | 0.04233 (12) | 0.02088 (17) | |
K2 | 0.500000 | 0.000000 | −0.16108 (11) | 0.01464 (16) | |
Na | 0.23246 (7) | −0.00700 (7) | 0.51491 (14) | 0.01230 (19) | |
O1 | 0.12017 (13) | 0.10863 (11) | 0.3478 (3) | 0.0123 (3) | |
O2 | 0.21258 (14) | 0.20354 (12) | 0.1178 (3) | 0.0142 (4) | |
O3 | 0.22782 (15) | 0.40732 (12) | 0.8205 (3) | 0.0162 (4) | |
O4 | 0.04753 (14) | 0.35882 (12) | 0.8495 (3) | 0.0155 (4) | |
O5 | 0.16538 (15) | 0.35811 (12) | 0.3248 (3) | 0.0126 (4) | |
H5 | 0.193 (3) | 0.342 (2) | 0.221 (5) | 0.019* | |
O6 | 0.29621 (14) | 0.24864 (12) | 0.6343 (3) | 0.0130 (4) | |
H6 | 0.326 (3) | 0.291 (2) | 0.595 (5) | 0.019* | |
O7 | 0.39590 (15) | 0.08339 (13) | 0.4854 (3) | 0.0156 (4) | |
H17 | 0.367 (3) | 0.132 (2) | 0.525 (5) | 0.023* | |
H27 | 0.434 (3) | 0.092 (2) | 0.384 (5) | 0.023* | |
O8 | 0.23648 (18) | 0.04169 (14) | 0.8784 (3) | 0.0213 (4) | |
H18 | 0.256 (3) | 0.001 (3) | 0.972 (5) | 0.032* | |
H28 | 0.232 (3) | 0.092 (3) | 0.943 (6) | 0.032* | |
O9 | 0.05881 (16) | −0.19148 (14) | −0.0303 (3) | 0.0198 (4) | |
H19 | 0.117 (3) | −0.204 (2) | 0.032 (6) | 0.030* | |
H29 | 0.031 (3) | −0.250 (2) | −0.059 (5) | 0.030* | |
O10 | 0.07869 (15) | −0.10785 (14) | 0.5700 (3) | 0.0184 (4) | |
H110 | 0.017 (3) | −0.106 (2) | 0.513 (5) | 0.028* | |
H210 | 0.072 (3) | −0.138 (2) | 0.687 (6) | 0.028* | |
C1 | 0.15518 (19) | 0.18782 (17) | 0.2828 (4) | 0.0104 (5) | |
C2 | 0.12508 (19) | 0.27352 (17) | 0.4230 (4) | 0.0105 (4) | |
H2 | 0.039 (2) | 0.2777 (19) | 0.433 (4) | 0.013* | |
C3 | 0.17721 (19) | 0.26336 (16) | 0.6481 (4) | 0.0109 (4) | |
H3 | 0.146 (2) | 0.209 (2) | 0.726 (5) | 0.013* | |
C4 | 0.1487 (2) | 0.35058 (17) | 0.7853 (4) | 0.0125 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0258 (4) | 0.0186 (4) | 0.0182 (4) | −0.0084 (4) | 0.000 | 0.000 |
K2 | 0.0155 (3) | 0.0163 (3) | 0.0121 (3) | −0.0024 (3) | 0.000 | 0.000 |
Na | 0.0118 (4) | 0.0126 (5) | 0.0124 (4) | −0.0004 (4) | 0.0001 (3) | 0.0001 (4) |
O1 | 0.0133 (8) | 0.0109 (8) | 0.0127 (8) | −0.0001 (6) | −0.0013 (7) | −0.0006 (7) |
O2 | 0.0167 (8) | 0.0141 (8) | 0.0117 (9) | −0.0001 (7) | 0.0020 (7) | −0.0009 (6) |
O3 | 0.0215 (9) | 0.0137 (8) | 0.0133 (8) | −0.0043 (7) | −0.0008 (7) | −0.0021 (7) |
O4 | 0.0161 (8) | 0.0186 (9) | 0.0119 (8) | 0.0047 (7) | 0.0001 (7) | −0.0013 (7) |
O5 | 0.0178 (9) | 0.0114 (8) | 0.0087 (8) | −0.0006 (7) | 0.0011 (7) | 0.0001 (7) |
O6 | 0.0113 (8) | 0.0120 (9) | 0.0156 (9) | 0.0002 (6) | −0.0009 (7) | 0.0008 (7) |
O7 | 0.0148 (9) | 0.0147 (9) | 0.0173 (9) | 0.0006 (7) | 0.0038 (7) | 0.0008 (7) |
O8 | 0.0402 (12) | 0.0129 (9) | 0.0109 (9) | 0.0046 (8) | 0.0001 (9) | 0.0004 (7) |
O9 | 0.0148 (9) | 0.0261 (10) | 0.0185 (10) | −0.0001 (8) | −0.0035 (8) | 0.0003 (8) |
O10 | 0.0116 (8) | 0.0212 (10) | 0.0223 (10) | −0.0032 (7) | −0.0030 (8) | 0.0054 (8) |
C1 | 0.0091 (11) | 0.0121 (11) | 0.0099 (11) | 0.0016 (9) | −0.0034 (9) | 0.0000 (9) |
C2 | 0.0115 (11) | 0.0094 (11) | 0.0105 (11) | 0.0003 (9) | −0.0006 (9) | 0.0005 (9) |
C3 | 0.0110 (10) | 0.0110 (11) | 0.0107 (11) | 0.0012 (9) | 0.0004 (9) | 0.0013 (10) |
C4 | 0.0183 (12) | 0.0119 (12) | 0.0073 (11) | 0.0024 (9) | −0.0015 (9) | 0.0012 (9) |
Geometric parameters (Å, º) top
K1—O1i | 2.8178 (17) | Na—C4iv | 3.080 (3) |
K1—O1 | 2.8178 (17) | O1—C1 | 1.262 (3) |
K1—O8ii | 3.020 (2) | O2—C1 | 1.244 (3) |
K1—O8iii | 3.020 (2) | O3—C4 | 1.250 (3) |
K1—O9i | 2.839 (2) | O4—C4 | 1.260 (3) |
K1—O9 | 2.839 (2) | O5—H5 | 0.75 (3) |
K1—O10iii | 3.424 (2) | O5—C2 | 1.426 (3) |
K1—O10ii | 3.424 (2) | O6—H6 | 0.74 (3) |
K2—O4iv | 2.8344 (18) | O6—C3 | 1.418 (3) |
K2—O4v | 2.8344 (18) | O7—H17 | 0.80 (4) |
K2—O5vi | 2.9771 (17) | O7—H27 | 0.78 (3) |
K2—O5vii | 2.9771 (17) | O8—H18 | 0.85 (4) |
K2—O7iii | 2.7703 (19) | O8—H28 | 0.82 (4) |
K2—O7viii | 2.7703 (19) | O9—H19 | 0.80 (4) |
K2—O8iii | 3.166 (2) | O9—H29 | 0.91 (3) |
K2—O8viii | 3.166 (2) | O10—H110 | 0.80 (3) |
Na—O1 | 2.3459 (18) | O10—H210 | 0.84 (4) |
Na—O3iv | 2.4484 (19) | C1—C2 | 1.535 (3) |
Na—O5iv | 2.468 (2) | C2—H2 | 1.02 (3) |
Na—O7 | 2.319 (2) | C2—C3 | 1.527 (3) |
Na—H17 | 2.53 (3) | C3—H3 | 0.98 (3) |
Na—O8 | 2.351 (2) | C3—C4 | 1.537 (3) |
Na—O10 | 2.332 (2) | | |
| | | |
Naii—K1—Naiii | 80.03 (3) | O1—Na—H17 | 79.6 (7) |
O1i—K1—Naii | 101.75 (4) | O1—Na—O8 | 103.09 (7) |
O1—K1—Naiii | 101.75 (4) | O1—Na—C4iv | 116.70 (7) |
O1—K1—Naii | 145.38 (4) | O3iv—Na—K1ix | 141.51 (5) |
O1i—K1—Naiii | 145.38 (4) | O3iv—Na—K2ix | 107.86 (5) |
O1—K1—O1i | 95.84 (7) | O3iv—Na—O5iv | 82.07 (6) |
O1—K1—O8iii | 69.85 (5) | O3iv—Na—H17 | 106.8 (8) |
O1—K1—O8ii | 142.60 (5) | O3iv—Na—C4iv | 22.66 (6) |
O1i—K1—O8ii | 69.85 (5) | O5iv—Na—K1ix | 91.35 (5) |
O1i—K1—O8iii | 142.60 (5) | O5iv—Na—K2ix | 52.72 (4) |
O1—K1—O9 | 120.47 (5) | O5iv—Na—H17 | 106.8 (7) |
O1i—K1—O9i | 120.47 (5) | O5iv—Na—C4iv | 60.78 (6) |
O1—K1—O9i | 72.83 (5) | O7—Na—K1ix | 125.47 (6) |
O1i—K1—O9 | 72.84 (5) | O7—Na—K2ix | 47.78 (5) |
O1i—K1—O10iii | 117.56 (5) | O7—Na—O1 | 92.62 (7) |
O1—K1—O10iii | 132.86 (4) | O7—Na—O3iv | 92.85 (7) |
O1i—K1—O10ii | 132.86 (4) | O7—Na—O5iv | 93.24 (7) |
O1—K1—O10ii | 117.56 (5) | O7—Na—H17 | 18.4 (8) |
O8ii—K1—Naii | 32.38 (4) | O7—Na—O8 | 84.02 (7) |
O8iii—K1—Naiii | 32.38 (4) | O7—Na—O10 | 173.97 (8) |
O8ii—K1—Naiii | 109.29 (4) | O7—Na—C4iv | 86.50 (7) |
O8iii—K1—Naii | 109.29 (4) | O8—Na—K1ix | 43.46 (5) |
O8ii—K1—O8iii | 140.78 (8) | O8—Na—K2ix | 57.48 (5) |
O8ii—K1—O10iii | 82.84 (5) | O8—Na—O3iv | 162.04 (8) |
O8iii—K1—O10iii | 63.39 (5) | O8—Na—O5iv | 80.46 (7) |
O8iii—K1—O10ii | 82.84 (5) | O8—Na—H17 | 74.6 (8) |
O8ii—K1—O10ii | 63.39 (5) | O8—Na—C4iv | 139.43 (8) |
O9i—K1—Naii | 72.54 (4) | O10—Na—K1ix | 53.41 (5) |
O9—K1—Naiii | 72.54 (4) | O10—Na—K2ix | 126.33 (6) |
O9—K1—Naii | 93.32 (4) | O10—Na—O1 | 93.23 (7) |
O9i—K1—Naiii | 93.32 (4) | O10—Na—O3iv | 88.11 (7) |
O9i—K1—O8ii | 84.82 (5) | O10—Na—O5iv | 80.99 (7) |
O9i—K1—O8iii | 89.09 (6) | O10—Na—H17 | 163.9 (8) |
O9—K1—O8ii | 89.09 (6) | O10—Na—O8 | 93.23 (8) |
O9—K1—O8iii | 84.82 (5) | O10—Na—C4iv | 92.16 (7) |
O9—K1—O9i | 161.81 (9) | C4iv—Na—K1ix | 140.24 (5) |
O9—K1—O10ii | 111.02 (6) | C4iv—Na—K2ix | 87.58 (5) |
O9i—K1—O10ii | 51.07 (5) | C4iv—Na—H17 | 104.0 (8) |
O9—K1—O10iii | 51.07 (5) | Na—O1—K1 | 101.25 (6) |
O9i—K1—O10iii | 111.02 (6) | C1—O1—K1 | 115.93 (15) |
O10iii—K1—Naiii | 33.15 (3) | C1—O1—Na | 125.36 (14) |
O10ii—K1—Naii | 33.15 (3) | C4—O3—Nax | 108.34 (15) |
O10iii—K1—Naii | 62.04 (4) | C4—O4—K2x | 117.77 (15) |
O10ii—K1—Naiii | 62.04 (4) | K2xi—O5—H5 | 101 (2) |
O10iii—K1—O10ii | 62.98 (7) | Nax—O5—K2xi | 86.01 (5) |
Naiii—K2—Naviii | 115.09 (3) | Nax—O5—H5 | 112 (2) |
O4v—K2—Naiii | 123.35 (4) | C2—O5—K2xi | 119.77 (13) |
O4iv—K2—Naiii | 100.33 (4) | C2—O5—Nax | 130.05 (14) |
O4v—K2—Naviii | 100.33 (4) | C2—O5—H5 | 104 (2) |
O4iv—K2—Naviii | 123.35 (4) | C3—O6—H6 | 112 (2) |
O4v—K2—O4iv | 94.40 (7) | K2ix—O7—H17 | 108 (2) |
O4iv—K2—O5vi | 146.91 (5) | K2ix—O7—H27 | 116 (2) |
O4v—K2—O5vi | 67.92 (5) | Na—O7—K2ix | 93.93 (6) |
O4iv—K2—O5vii | 67.92 (5) | Na—O7—H17 | 96 (2) |
O4v—K2—O5vii | 146.91 (5) | Na—O7—H27 | 129 (2) |
O4iv—K2—O8viii | 90.51 (5) | H17—O7—H27 | 111 (3) |
O4v—K2—O8viii | 83.48 (5) | K1ix—O8—K2ix | 153.08 (7) |
O4iv—K2—O8iii | 83.48 (5) | K1ix—O8—H18 | 83 (2) |
O4v—K2—O8iii | 90.51 (5) | K1ix—O8—H28 | 87 (2) |
O5vi—K2—Naviii | 41.27 (4) | K2ix—O8—H18 | 70 (2) |
O5vii—K2—Naviii | 112.76 (4) | K2ix—O8—H28 | 105 (2) |
O5vi—K2—Naiii | 112.76 (4) | Na—O8—K1ix | 104.16 (7) |
O5vii—K2—Naiii | 41.27 (4) | Na—O8—K2ix | 83.76 (6) |
O5vii—K2—O5vi | 140.27 (7) | Na—O8—H18 | 117 (2) |
O5vii—K2—O8viii | 122.68 (5) | Na—O8—H28 | 136 (2) |
O5vii—K2—O8iii | 60.81 (5) | H18—O8—H28 | 106 (3) |
O5vi—K2—O8viii | 60.81 (5) | K1—O9—H19 | 110 (2) |
O5vi—K2—O8iii | 122.68 (5) | K1—O9—H29 | 144 (2) |
O7iii—K2—Naiii | 38.30 (4) | H19—O9—H29 | 102 (3) |
O7viii—K2—Naiii | 86.46 (4) | K1ix—O10—H110 | 97 (2) |
O7iii—K2—Naviii | 86.46 (4) | K1ix—O10—H210 | 58 (2) |
O7viii—K2—Naviii | 38.30 (4) | Na—O10—K1ix | 93.45 (6) |
O7iii—K2—O4iv | 138.63 (5) | Na—O10—H110 | 128 (2) |
O7viii—K2—O4iv | 108.74 (5) | Na—O10—H210 | 121 (2) |
O7viii—K2—O4v | 138.63 (5) | H110—O10—H210 | 108 (3) |
O7iii—K2—O4v | 108.74 (5) | O1—C1—C2 | 116.8 (2) |
O7viii—K2—O5vii | 74.46 (5) | O2—C1—O1 | 126.7 (2) |
O7iii—K2—O5vii | 74.44 (5) | O2—C1—C2 | 116.5 (2) |
O7iii—K2—O5vi | 74.46 (5) | O5—C2—C1 | 110.46 (18) |
O7viii—K2—O5vi | 74.44 (5) | O5—C2—H2 | 108.0 (15) |
O7viii—K2—O7iii | 75.87 (8) | O5—C2—C3 | 109.51 (18) |
O7viii—K2—O8iii | 125.00 (5) | C1—C2—H2 | 108.2 (15) |
O7viii—K2—O8viii | 63.12 (5) | C3—C2—C1 | 110.30 (19) |
O7iii—K2—O8iii | 63.12 (5) | C3—C2—H2 | 110.4 (15) |
O7iii—K2—O8viii | 125.00 (5) | O6—C3—C2 | 110.82 (19) |
O8viii—K2—Naviii | 38.76 (4) | O6—C3—H3 | 106.7 (16) |
O8iii—K2—Naiii | 38.76 (4) | O6—C3—C4 | 111.56 (19) |
O8viii—K2—Naiii | 149.58 (4) | C2—C3—H3 | 111.6 (16) |
O8iii—K2—Naviii | 149.58 (4) | C2—C3—C4 | 109.81 (18) |
O8viii—K2—O8iii | 171.17 (7) | C4—C3—H3 | 106.3 (16) |
K1ix—Na—H17 | 111.4 (8) | O3—C4—Nax | 49.00 (12) |
K2ix—Na—K1ix | 97.49 (2) | O3—C4—O4 | 126.1 (2) |
K2ix—Na—H17 | 55.7 (7) | O3—C4—C3 | 116.8 (2) |
O1—Na—K1ix | 87.65 (5) | O4—C4—Nax | 123.91 (16) |
O1—Na—K2ix | 133.84 (5) | O4—C4—C3 | 117.1 (2) |
O1—Na—O3iv | 94.70 (6) | C3—C4—Nax | 95.54 (14) |
O1—Na—O5iv | 173.44 (7) | | |
| | | |
K1—O1—C1—O2 | −52.3 (3) | O1—C1—C2—C3 | 61.5 (3) |
K1—O1—C1—C2 | 128.43 (17) | O2—C1—C2—O5 | 3.4 (3) |
K2x—O4—C4—Nax | −72.19 (19) | O2—C1—C2—C3 | −117.8 (2) |
K2x—O4—C4—O3 | −11.4 (3) | O5—C2—C3—O6 | −66.7 (2) |
K2x—O4—C4—C3 | 169.52 (14) | O5—C2—C3—C4 | 57.0 (2) |
K2xi—O5—C2—C1 | 113.26 (17) | O6—C3—C4—Nax | 62.77 (18) |
K2xi—O5—C2—C3 | −125.07 (15) | O6—C3—C4—O3 | 16.4 (3) |
Na—O1—C1—O2 | 75.3 (3) | O6—C3—C4—O4 | −164.5 (2) |
Na—O1—C1—C2 | −103.9 (2) | C1—C2—C3—O6 | 55.1 (2) |
Nax—O3—C4—O4 | −106.3 (2) | C1—C2—C3—C4 | 178.77 (19) |
Nax—O3—C4—C3 | 72.7 (2) | C2—C3—C4—Nax | −60.49 (17) |
Nax—O5—C2—C1 | −134.65 (16) | C2—C3—C4—O3 | −106.9 (2) |
Nax—O5—C2—C3 | −13.0 (3) | C2—C3—C4—O4 | 72.3 (3) |
O1—C1—C2—O5 | −177.26 (19) | | |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x+1/2, −y+1/2, −z+1; (vi) x+1/2, −y+1/2, −z; (vii) −x+1/2, y−1/2, −z; (viii) −x+1, −y, z−1; (ix) x, y, z+1; (x) −x+1/2, y+1/2, −z+1; (xi) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.75 (3) | 2.08 (3) | 2.599 (2) | 127 (3) |
O5—H5···O3iii | 0.75 (3) | 2.68 (3) | 3.277 (2) | 138 (3) |
O5—H5···O4iii | 0.75 (3) | 2.87 (3) | 3.248 (2) | 114 (3) |
O6—H6···O10x | 0.74 (3) | 2.08 (3) | 2.812 (3) | 168 (3) |
O7—H17···O6 | 0.80 (4) | 1.97 (4) | 2.778 (2) | 178 (3) |
O7—H27···O4v | 0.78 (3) | 2.08 (3) | 2.853 (3) | 168 (3) |
O8—H18···O3xii | 0.85 (4) | 1.86 (4) | 2.697 (3) | 171 (3) |
O8—H28···O1ix | 0.82 (4) | 2.84 (3) | 3.346 (2) | 122 (3) |
O8—H28···O2ix | 0.82 (4) | 1.93 (4) | 2.746 (3) | 174 (3) |
O9—H19···O2vii | 0.80 (4) | 2.57 (3) | 3.122 (3) | 127 (3) |
O9—H19···O3iv | 0.80 (4) | 2.58 (4) | 3.154 (3) | 130 (3) |
O9—H19···O6iv | 0.80 (4) | 2.40 (4) | 3.102 (3) | 147 (3) |
O9—H29···O4ii | 0.91 (3) | 1.89 (4) | 2.785 (3) | 170 (3) |
O10—H110···O1i | 0.80 (3) | 1.91 (3) | 2.713 (2) | 173 (3) |
O10—H210···O9ix | 0.84 (4) | 1.91 (4) | 2.751 (3) | 172 (3) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x+1/2, −y+1/2, −z+1; (vii) −x+1/2, y−1/2, −z; (ix) x, y, z+1; (x) −x+1/2, y+1/2, −z+1; (xii) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (125K_har)
top
Crystal data top
C4H12KNaO10 | Dx = 1.813 Mg m−3 |
Mr = 282.23 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 8346 reflections |
a = 11.7769 (6) Å | θ = 3.6–29.2° |
b = 14.1930 (8) Å | µ = 0.60 mm−1 |
c = 6.1849 (3) Å | T = 125 K |
V = 1033.80 (10) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 584 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2653 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2389 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.766, Tmax = 1.000 | l = −8→8 |
18069 measured reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.030 | w = 1/[σ2(Fo2) + (0.0208P)2 + 0.4259P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.063 | (Δ/σ)max < 0.001 |
S = 1.08 | Δρmax = 0.34 e Å−3 |
2653 reflections | Δρmin = −0.25 e Å−3 |
182 parameters | Absolute structure: Flack x determined using 892 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). |
1 restraint | Absolute structure parameter: −0.02 (2) |
Primary atom site location: structure-invariant direct methods | |
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 | |
K1 | 0.000000 | 0.000000 | 0.04286 (13) | 0.02478 (19) | |
K2 | 0.500000 | 0.000000 | −0.16099 (12) | 0.01693 (16) | |
Na | 0.23242 (8) | −0.00693 (7) | 0.51540 (14) | 0.0141 (2) | |
O1 | 0.12012 (14) | 0.10870 (12) | 0.3477 (3) | 0.0137 (3) | |
O2 | 0.21246 (15) | 0.20348 (12) | 0.1181 (3) | 0.0158 (4) | |
O3 | 0.22817 (16) | 0.40726 (12) | 0.8200 (3) | 0.0190 (4) | |
O4 | 0.04783 (15) | 0.35905 (13) | 0.8489 (3) | 0.0178 (4) | |
O5 | 0.16518 (15) | 0.35796 (12) | 0.3247 (3) | 0.0143 (4) | |
H5 | 0.194 (3) | 0.340 (2) | 0.221 (6) | 0.021* | |
O6 | 0.29620 (15) | 0.24856 (12) | 0.6340 (3) | 0.0146 (4) | |
H6 | 0.326 (3) | 0.292 (2) | 0.593 (5) | 0.022* | |
O7 | 0.39597 (16) | 0.08324 (13) | 0.4858 (3) | 0.0176 (4) | |
H17 | 0.369 (3) | 0.132 (3) | 0.523 (6) | 0.026* | |
H27 | 0.433 (3) | 0.094 (2) | 0.381 (6) | 0.026* | |
O8 | 0.23692 (19) | 0.04161 (15) | 0.8791 (3) | 0.0246 (5) | |
H18 | 0.255 (3) | 0.002 (3) | 0.974 (6) | 0.037* | |
H28 | 0.234 (3) | 0.092 (3) | 0.944 (6) | 0.037* | |
O9 | 0.05879 (17) | −0.19184 (15) | −0.0310 (3) | 0.0228 (4) | |
H19 | 0.116 (3) | −0.204 (3) | 0.030 (6) | 0.034* | |
H29 | 0.030 (3) | −0.251 (3) | −0.059 (5) | 0.034* | |
O10 | 0.07852 (16) | −0.10751 (14) | 0.5703 (4) | 0.0215 (4) | |
H110 | 0.016 (3) | −0.107 (2) | 0.508 (5) | 0.032* | |
H210 | 0.073 (3) | −0.134 (3) | 0.690 (6) | 0.032* | |
C1 | 0.1551 (2) | 0.18777 (17) | 0.2829 (4) | 0.0114 (5) | |
C2 | 0.1253 (2) | 0.27355 (17) | 0.4229 (4) | 0.0117 (5) | |
H2 | 0.042 (2) | 0.278 (2) | 0.437 (4) | 0.014* | |
C3 | 0.17718 (19) | 0.26350 (17) | 0.6480 (4) | 0.0125 (5) | |
H3 | 0.146 (2) | 0.210 (2) | 0.726 (5) | 0.015* | |
C4 | 0.1488 (2) | 0.35069 (18) | 0.7850 (4) | 0.0139 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0305 (4) | 0.0225 (4) | 0.0213 (4) | −0.0105 (4) | 0.000 | 0.000 |
K2 | 0.0175 (3) | 0.0190 (4) | 0.0143 (3) | −0.0024 (3) | 0.000 | 0.000 |
Na | 0.0140 (4) | 0.0138 (5) | 0.0144 (4) | −0.0003 (4) | 0.0000 (3) | 0.0002 (4) |
O1 | 0.0145 (8) | 0.0118 (8) | 0.0149 (8) | −0.0005 (6) | −0.0013 (7) | −0.0005 (7) |
O2 | 0.0186 (8) | 0.0157 (9) | 0.0130 (9) | −0.0003 (7) | 0.0023 (7) | −0.0015 (7) |
O3 | 0.0256 (9) | 0.0164 (9) | 0.0148 (9) | −0.0043 (8) | −0.0007 (8) | −0.0026 (7) |
O4 | 0.0177 (8) | 0.0215 (9) | 0.0141 (8) | 0.0050 (7) | −0.0006 (7) | −0.0019 (8) |
O5 | 0.0199 (9) | 0.0117 (8) | 0.0113 (8) | −0.0005 (7) | 0.0006 (7) | 0.0007 (7) |
O6 | 0.0125 (8) | 0.0133 (9) | 0.0179 (9) | 0.0014 (7) | −0.0012 (7) | 0.0002 (7) |
O7 | 0.0166 (9) | 0.0160 (9) | 0.0202 (10) | 0.0000 (7) | 0.0037 (8) | 0.0006 (8) |
O8 | 0.0467 (13) | 0.0152 (9) | 0.0119 (9) | 0.0055 (9) | 0.0008 (9) | 0.0000 (7) |
O9 | 0.0162 (9) | 0.0308 (11) | 0.0215 (10) | −0.0004 (8) | −0.0044 (8) | 0.0008 (9) |
O10 | 0.0150 (9) | 0.0239 (10) | 0.0255 (10) | −0.0033 (8) | −0.0039 (8) | 0.0060 (8) |
C1 | 0.0090 (11) | 0.0140 (12) | 0.0113 (11) | 0.0015 (9) | −0.0034 (9) | −0.0007 (9) |
C2 | 0.0117 (11) | 0.0118 (11) | 0.0116 (11) | 0.0005 (9) | 0.0005 (9) | 0.0000 (9) |
C3 | 0.0129 (11) | 0.0121 (11) | 0.0126 (11) | 0.0008 (9) | 0.0012 (10) | 0.0010 (10) |
C4 | 0.0201 (13) | 0.0123 (12) | 0.0093 (11) | 0.0023 (9) | −0.0030 (10) | 0.0015 (9) |
Geometric parameters (Å, º) top
K1—O1 | 2.8172 (17) | Na—C4iv | 3.081 (3) |
K1—O1i | 2.8172 (17) | O1—C1 | 1.261 (3) |
K1—O8ii | 3.026 (2) | O2—C1 | 1.243 (3) |
K1—O8iii | 3.026 (2) | O3—C4 | 1.251 (3) |
K1—O9i | 2.846 (2) | O4—C4 | 1.259 (3) |
K1—O9 | 2.846 (2) | O5—H5 | 0.77 (3) |
K1—O10ii | 3.424 (2) | O5—C2 | 1.423 (3) |
K1—O10iii | 3.424 (2) | O6—H6 | 0.75 (3) |
K2—O4iv | 2.8362 (18) | O6—C3 | 1.420 (3) |
K2—O4v | 2.8362 (18) | O7—H17 | 0.79 (4) |
K2—O5vi | 2.9789 (18) | O7—H27 | 0.80 (3) |
K2—O5vii | 2.9789 (18) | O8—H18 | 0.84 (4) |
K2—O7iii | 2.769 (2) | O8—H28 | 0.82 (4) |
K2—O7viii | 2.769 (2) | O9—H19 | 0.79 (4) |
K2—O8iii | 3.164 (2) | O9—H29 | 0.92 (4) |
K2—O8viii | 3.164 (2) | O10—H110 | 0.83 (4) |
Na—O1 | 2.3491 (19) | O10—H210 | 0.83 (4) |
Na—O3iv | 2.450 (2) | C1—C2 | 1.535 (3) |
Na—O5iv | 2.472 (2) | C2—H2 | 0.99 (3) |
Na—O7 | 2.320 (2) | C2—C3 | 1.527 (3) |
Na—H17 | 2.54 (3) | C3—H3 | 0.97 (3) |
Na—O8 | 2.353 (2) | C3—C4 | 1.537 (3) |
Na—O10 | 2.332 (2) | | |
| | | |
Naii—K1—Naiii | 80.03 (3) | O1—Na—H17 | 80.0 (8) |
O1i—K1—Naii | 101.69 (4) | O1—Na—O8 | 103.31 (8) |
O1—K1—Naiii | 101.69 (4) | O1—Na—C4iv | 116.59 (7) |
O1—K1—Naii | 145.35 (4) | O3iv—Na—K1ix | 141.42 (6) |
O1i—K1—Naiii | 145.35 (4) | O3iv—Na—K2ix | 107.88 (5) |
O1—K1—O1i | 95.98 (7) | O3iv—Na—O5iv | 81.99 (7) |
O1i—K1—O8iii | 142.54 (5) | O3iv—Na—H17 | 106.3 (8) |
O1i—K1—O8ii | 69.77 (5) | O3iv—Na—C4iv | 22.67 (6) |
O1—K1—O8iii | 69.77 (5) | O5iv—Na—K1ix | 91.44 (5) |
O1—K1—O8ii | 142.54 (5) | O5iv—Na—K2ix | 52.72 (4) |
O1—K1—O9 | 120.61 (6) | O5iv—Na—H17 | 106.4 (8) |
O1i—K1—O9i | 120.61 (6) | O5iv—Na—C4iv | 60.72 (6) |
O1—K1—O9i | 72.88 (5) | O7—Na—K1ix | 125.54 (6) |
O1i—K1—O9 | 72.88 (5) | O7—Na—K2ix | 47.72 (5) |
O1i—K1—O10iii | 117.57 (5) | O7—Na—O1 | 92.70 (7) |
O1i—K1—O10ii | 132.82 (5) | O7—Na—O3iv | 92.87 (7) |
O1—K1—O10iii | 132.82 (5) | O7—Na—O5iv | 93.13 (7) |
O1—K1—O10ii | 117.57 (5) | O7—Na—H17 | 17.9 (8) |
O8ii—K1—Naii | 32.41 (4) | O7—Na—O8 | 83.99 (8) |
O8iii—K1—Naii | 109.37 (5) | O7—Na—O10 | 174.01 (9) |
O8ii—K1—Naiii | 109.37 (5) | O7—Na—C4iv | 86.41 (7) |
O8iii—K1—Naiii | 32.41 (4) | O8—Na—K1ix | 43.58 (6) |
O8ii—K1—O8iii | 140.90 (8) | O8—Na—K2ix | 57.38 (6) |
O8iii—K1—O10ii | 82.90 (5) | O8—Na—O3iv | 161.93 (8) |
O8ii—K1—O10ii | 63.41 (5) | O8—Na—O5iv | 80.43 (7) |
O8ii—K1—O10iii | 82.90 (5) | O8—Na—H17 | 75.0 (8) |
O8iii—K1—O10iii | 63.41 (5) | O8—Na—C4iv | 139.31 (8) |
O9i—K1—Naii | 72.46 (4) | O10—Na—K1ix | 53.36 (6) |
O9—K1—Naii | 93.18 (5) | O10—Na—K2ix | 126.44 (6) |
O9—K1—Naiii | 72.46 (4) | O10—Na—O1 | 93.12 (7) |
O9i—K1—Naiii | 93.18 (5) | O10—Na—O3iv | 88.07 (8) |
O9i—K1—O8ii | 84.76 (6) | O10—Na—O5iv | 81.14 (7) |
O9—K1—O8iii | 84.76 (6) | O10—Na—H17 | 164.4 (8) |
O9—K1—O8ii | 89.08 (6) | O10—Na—O8 | 93.29 (8) |
O9i—K1—O8iii | 89.08 (6) | O10—Na—C4iv | 92.24 (8) |
O9—K1—O9i | 161.53 (9) | C4iv—Na—K1ix | 140.24 (6) |
O9—K1—O10iii | 51.03 (5) | C4iv—Na—K2ix | 87.56 (5) |
O9i—K1—O10iii | 110.79 (6) | C4iv—Na—H17 | 103.3 (8) |
O9—K1—O10ii | 110.79 (6) | Na—O1—K1 | 101.28 (6) |
O9i—K1—O10ii | 51.03 (5) | C1—O1—K1 | 116.02 (15) |
O10iii—K1—Naiii | 33.12 (4) | C1—O1—Na | 125.32 (15) |
O10ii—K1—Naii | 33.12 (4) | C4—O3—Nax | 108.31 (15) |
O10iii—K1—Naii | 61.98 (4) | C4—O4—K2x | 117.90 (16) |
O10ii—K1—Naiii | 61.98 (4) | K2xi—O5—H5 | 103 (2) |
O10iii—K1—O10ii | 62.81 (7) | Nax—O5—K2xi | 85.96 (6) |
Naiii—K2—Naviii | 115.18 (3) | Nax—O5—H5 | 112 (2) |
O4v—K2—Naviii | 100.29 (4) | C2—O5—K2xi | 119.95 (13) |
O4iv—K2—Naviii | 123.43 (4) | C2—O5—Nax | 130.05 (15) |
O4v—K2—Naiii | 123.43 (4) | C2—O5—H5 | 103 (2) |
O4iv—K2—Naiii | 100.29 (4) | C3—O6—H6 | 111 (2) |
O4v—K2—O4iv | 94.24 (8) | K2ix—O7—H17 | 108 (2) |
O4iv—K2—O5vi | 67.93 (5) | K2ix—O7—H27 | 118 (2) |
O4iv—K2—O5vii | 146.96 (5) | Na—O7—K2ix | 93.99 (7) |
O4v—K2—O5vi | 146.97 (5) | Na—O7—H17 | 97 (2) |
O4v—K2—O5vii | 67.93 (5) | Na—O7—H27 | 129 (2) |
O4iv—K2—O8viii | 90.54 (5) | H17—O7—H27 | 107 (3) |
O4v—K2—O8viii | 83.33 (5) | K1ix—O8—K2ix | 153.21 (8) |
O4iv—K2—O8iii | 83.33 (5) | K1ix—O8—H18 | 83 (2) |
O4v—K2—O8iii | 90.54 (5) | K1ix—O8—H28 | 88 (3) |
O5vii—K2—Naviii | 41.32 (4) | K2ix—O8—H18 | 71 (2) |
O5vii—K2—Naiii | 112.75 (4) | K2ix—O8—H28 | 104 (3) |
O5vi—K2—Naviii | 112.75 (4) | Na—O8—K1ix | 104.01 (8) |
O5vi—K2—Naiii | 41.32 (4) | Na—O8—K2ix | 83.83 (6) |
O5vi—K2—O5vii | 140.26 (8) | Na—O8—H18 | 119 (3) |
O5vii—K2—O8viii | 60.89 (5) | Na—O8—H28 | 136 (3) |
O5vi—K2—O8viii | 122.67 (5) | H18—O8—H28 | 104 (4) |
O5vii—K2—O8iii | 122.67 (5) | K1—O9—H19 | 110 (3) |
O5vi—K2—O8iii | 60.89 (5) | K1—O9—H29 | 144 (2) |
O7iii—K2—Naiii | 38.29 (4) | H19—O9—H29 | 102 (3) |
O7viii—K2—Naiii | 86.52 (5) | K1ix—O10—H110 | 98 (2) |
O7iii—K2—Naviii | 86.52 (5) | K1ix—O10—H210 | 55 (2) |
O7viii—K2—Naviii | 38.29 (4) | Na—O10—K1ix | 93.52 (7) |
O7iii—K2—O4iv | 138.58 (5) | Na—O10—H110 | 128 (2) |
O7viii—K2—O4iv | 108.89 (6) | Na—O10—H210 | 118 (2) |
O7viii—K2—O4v | 138.58 (5) | H110—O10—H210 | 110 (3) |
O7iii—K2—O4v | 108.89 (6) | O1—C1—C2 | 116.8 (2) |
O7viii—K2—O5vi | 74.46 (5) | O2—C1—O1 | 126.7 (2) |
O7iii—K2—O5vii | 74.46 (5) | O2—C1—C2 | 116.4 (2) |
O7iii—K2—O5vi | 74.44 (5) | O5—C2—C1 | 110.56 (19) |
O7viii—K2—O5vii | 74.44 (5) | O5—C2—H2 | 108.5 (16) |
O7viii—K2—O7iii | 75.84 (9) | O5—C2—C3 | 109.61 (19) |
O7iii—K2—O8viii | 125.08 (6) | C1—C2—H2 | 108.8 (16) |
O7iii—K2—O8iii | 63.19 (5) | C3—C2—C1 | 110.4 (2) |
O7viii—K2—O8iii | 125.08 (6) | C3—C2—H2 | 108.8 (16) |
O7viii—K2—O8viii | 63.19 (5) | O6—C3—C2 | 110.7 (2) |
O8viii—K2—Naviii | 38.79 (4) | O6—C3—H3 | 106.8 (17) |
O8iii—K2—Naiii | 38.79 (4) | O6—C3—C4 | 111.6 (2) |
O8viii—K2—Naiii | 149.71 (4) | C2—C3—H3 | 112.0 (17) |
O8iii—K2—Naviii | 149.71 (4) | C2—C3—C4 | 109.91 (19) |
O8viii—K2—O8iii | 171.01 (7) | C4—C3—H3 | 105.7 (17) |
K1ix—Na—H17 | 112.0 (8) | O3—C4—Nax | 49.02 (12) |
K2ix—Na—K1ix | 97.54 (2) | O3—C4—O4 | 126.2 (2) |
K2ix—Na—H17 | 55.5 (8) | O3—C4—C3 | 116.7 (2) |
O1—Na—K1ix | 87.72 (5) | O4—C4—Nax | 123.81 (17) |
O1—Na—K2ix | 133.89 (5) | O4—C4—C3 | 117.0 (2) |
O1—Na—O3iv | 94.60 (7) | C3—C4—Nax | 95.57 (14) |
O1—Na—O5iv | 173.39 (7) | | |
| | | |
K1—O1—C1—O2 | −52.3 (3) | O1—C1—C2—C3 | 61.4 (3) |
K1—O1—C1—C2 | 128.50 (17) | O2—C1—C2—O5 | 3.7 (3) |
K2x—O4—C4—Nax | −72.4 (2) | O2—C1—C2—C3 | −117.8 (2) |
K2x—O4—C4—O3 | −11.6 (3) | O5—C2—C3—O6 | −67.0 (2) |
K2x—O4—C4—C3 | 169.42 (15) | O5—C2—C3—C4 | 56.8 (2) |
K2xi—O5—C2—C1 | 113.15 (17) | O6—C3—C4—Nax | 62.83 (19) |
K2xi—O5—C2—C3 | −124.90 (15) | O6—C3—C4—O3 | 16.4 (3) |
Na—O1—C1—O2 | 75.4 (3) | O6—C3—C4—O4 | −164.5 (2) |
Na—O1—C1—C2 | −103.7 (2) | C1—C2—C3—O6 | 55.1 (3) |
Nax—O3—C4—O4 | −106.1 (2) | C1—C2—C3—C4 | 178.8 (2) |
Nax—O3—C4—C3 | 72.9 (2) | C2—C3—C4—Nax | −60.39 (18) |
Nax—O5—C2—C1 | −134.63 (17) | C2—C3—C4—O3 | −106.9 (2) |
Nax—O5—C2—C3 | −12.7 (3) | C2—C3—C4—O4 | 72.3 (3) |
O1—C1—C2—O5 | −177.08 (19) | | |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x+1/2, −y+1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (vii) x+1/2, −y+1/2, −z; (viii) −x+1, −y, z−1; (ix) x, y, z+1; (x) −x+1/2, y+1/2, −z+1; (xi) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.77 (3) | 2.06 (3) | 2.598 (2) | 128 (3) |
O5—H5···O3iii | 0.77 (3) | 2.69 (3) | 3.284 (3) | 136 (3) |
O5—H5···O4iii | 0.77 (3) | 2.89 (3) | 3.251 (3) | 112 (3) |
O6—H6···O10x | 0.75 (3) | 2.08 (3) | 2.819 (3) | 168 (3) |
O7—H17···O6 | 0.79 (4) | 1.99 (4) | 2.780 (3) | 176 (4) |
O7—H27···O4v | 0.80 (3) | 2.07 (3) | 2.856 (3) | 168 (3) |
O8—H18···O3xii | 0.84 (4) | 1.86 (4) | 2.696 (3) | 171 (4) |
O8—H28···O1ix | 0.82 (4) | 2.84 (4) | 3.346 (3) | 122 (3) |
O8—H28···O2ix | 0.82 (4) | 1.93 (4) | 2.747 (3) | 173 (4) |
O9—H19···O2vi | 0.79 (4) | 2.58 (4) | 3.123 (3) | 128 (3) |
O9—H19···O3iv | 0.79 (4) | 2.60 (4) | 3.159 (3) | 129 (3) |
O9—H19···O6iv | 0.79 (4) | 2.42 (4) | 3.108 (3) | 147 (3) |
O9—H29···O4ii | 0.92 (4) | 1.88 (4) | 2.786 (3) | 169 (3) |
O10—H110···O1i | 0.83 (4) | 1.88 (4) | 2.714 (3) | 175 (3) |
O10—H210···O9ix | 0.83 (4) | 1.92 (4) | 2.751 (3) | 178 (4) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x+1/2, −y+1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (ix) x, y, z+1; (x) −x+1/2, y+1/2, −z+1; (xii) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (150K_har)
top
Crystal data top
C4H12KNaO10 | Dx = 1.808 Mg m−3 |
Mr = 282.23 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 8154 reflections |
a = 11.7916 (6) Å | θ = 3.6–29.2° |
b = 14.2002 (8) Å | µ = 0.60 mm−1 |
c = 6.1907 (3) Å | T = 150 K |
V = 1036.60 (10) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 584 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2664 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2383 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.810, Tmax = 1.000 | l = −8→8 |
18107 measured reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.030 | w = 1/[σ2(Fo2) + (0.0222P)2 + 0.3393P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.063 | (Δ/σ)max < 0.001 |
S = 1.09 | Δρmax = 0.30 e Å−3 |
2664 reflections | Δρmin = −0.28 e Å−3 |
182 parameters | Absolute structure: Flack x determined using 880 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). |
1 restraint | Absolute structure parameter: 0.01 (2) |
Primary atom site location: structure-invariant direct methods | |
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 | |
K1 | 0.000000 | 0.000000 | 0.04316 (13) | 0.0287 (2) | |
K2 | 0.500000 | 0.000000 | −0.16073 (12) | 0.01920 (17) | |
Na | 0.23237 (8) | −0.00687 (7) | 0.51606 (14) | 0.0158 (2) | |
O1 | 0.12025 (13) | 0.10875 (12) | 0.3481 (3) | 0.0154 (3) | |
O2 | 0.21218 (15) | 0.20344 (12) | 0.1181 (3) | 0.0180 (4) | |
O3 | 0.22848 (16) | 0.40731 (12) | 0.8197 (3) | 0.0217 (4) | |
O4 | 0.04848 (15) | 0.35928 (13) | 0.8485 (3) | 0.0202 (4) | |
O5 | 0.16502 (15) | 0.35790 (12) | 0.3247 (3) | 0.0158 (4) | |
H5 | 0.195 (3) | 0.342 (2) | 0.221 (6) | 0.024* | |
O6 | 0.29608 (15) | 0.24862 (12) | 0.6334 (3) | 0.0171 (4) | |
H6 | 0.326 (3) | 0.290 (2) | 0.593 (5) | 0.026* | |
O7 | 0.39610 (16) | 0.08322 (13) | 0.4855 (3) | 0.0201 (4) | |
H17 | 0.368 (3) | 0.129 (3) | 0.527 (6) | 0.030* | |
H27 | 0.434 (3) | 0.093 (2) | 0.377 (6) | 0.030* | |
O8 | 0.2375 (2) | 0.04155 (15) | 0.8799 (3) | 0.0279 (5) | |
H18 | 0.257 (3) | 0.001 (3) | 0.977 (6) | 0.042* | |
H28 | 0.233 (3) | 0.091 (3) | 0.945 (6) | 0.042* | |
O9 | 0.05899 (17) | −0.19228 (16) | −0.0314 (3) | 0.0267 (5) | |
H19 | 0.117 (3) | −0.207 (3) | 0.029 (6) | 0.040* | |
H29 | 0.028 (3) | −0.250 (3) | −0.062 (5) | 0.040* | |
O10 | 0.07839 (16) | −0.10705 (15) | 0.5713 (4) | 0.0250 (4) | |
H110 | 0.017 (3) | −0.105 (2) | 0.509 (5) | 0.037* | |
H210 | 0.071 (3) | −0.138 (3) | 0.688 (6) | 0.037* | |
C1 | 0.1552 (2) | 0.18783 (17) | 0.2828 (4) | 0.0126 (5) | |
C2 | 0.12523 (19) | 0.27330 (17) | 0.4230 (4) | 0.0128 (5) | |
H2 | 0.039 (2) | 0.2778 (19) | 0.436 (4) | 0.015* | |
C3 | 0.17730 (19) | 0.26351 (17) | 0.6476 (4) | 0.0139 (5) | |
H3 | 0.146 (2) | 0.210 (2) | 0.725 (5) | 0.017* | |
C4 | 0.1493 (2) | 0.35064 (18) | 0.7842 (4) | 0.0161 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0358 (4) | 0.0258 (4) | 0.0246 (4) | −0.0130 (4) | 0.000 | 0.000 |
K2 | 0.0201 (3) | 0.0211 (4) | 0.0163 (3) | −0.0027 (3) | 0.000 | 0.000 |
Na | 0.0151 (4) | 0.0156 (5) | 0.0166 (4) | −0.0003 (4) | −0.0002 (3) | 0.0004 (4) |
O1 | 0.0165 (8) | 0.0137 (8) | 0.0161 (8) | −0.0007 (6) | −0.0016 (7) | −0.0011 (7) |
O2 | 0.0214 (9) | 0.0175 (9) | 0.0151 (9) | 0.0001 (7) | 0.0035 (7) | −0.0009 (7) |
O3 | 0.0292 (10) | 0.0179 (9) | 0.0180 (9) | −0.0057 (8) | −0.0009 (8) | −0.0034 (7) |
O4 | 0.0204 (9) | 0.0243 (9) | 0.0159 (8) | 0.0067 (7) | 0.0002 (8) | −0.0024 (8) |
O5 | 0.0222 (9) | 0.0140 (8) | 0.0114 (8) | −0.0002 (7) | 0.0015 (7) | 0.0007 (7) |
O6 | 0.0150 (8) | 0.0160 (9) | 0.0203 (9) | 0.0013 (7) | −0.0018 (8) | 0.0005 (7) |
O7 | 0.0183 (9) | 0.0192 (10) | 0.0227 (10) | 0.0002 (7) | 0.0040 (8) | 0.0012 (8) |
O8 | 0.0535 (14) | 0.0162 (9) | 0.0141 (9) | 0.0055 (9) | 0.0009 (9) | 0.0005 (7) |
O9 | 0.0176 (9) | 0.0372 (12) | 0.0253 (11) | −0.0007 (9) | −0.0055 (8) | 0.0011 (9) |
O10 | 0.0156 (9) | 0.0278 (11) | 0.0314 (11) | −0.0044 (8) | −0.0042 (8) | 0.0074 (9) |
C1 | 0.0108 (11) | 0.0143 (11) | 0.0126 (11) | 0.0005 (9) | −0.0042 (9) | −0.0013 (9) |
C2 | 0.0135 (11) | 0.0120 (11) | 0.0127 (11) | 0.0002 (9) | −0.0010 (9) | 0.0003 (9) |
C3 | 0.0151 (11) | 0.0127 (11) | 0.0138 (11) | 0.0015 (9) | 0.0012 (10) | 0.0005 (10) |
C4 | 0.0228 (13) | 0.0158 (12) | 0.0097 (11) | 0.0027 (10) | −0.0022 (10) | 0.0017 (9) |
Geometric parameters (Å, º) top
K1—O1i | 2.8212 (17) | Na—C4iv | 3.081 (3) |
K1—O1 | 2.8212 (17) | O1—C1 | 1.263 (3) |
K1—O8ii | 3.036 (2) | O2—C1 | 1.241 (3) |
K1—O8iii | 3.036 (2) | O3—C4 | 1.252 (3) |
K1—O9 | 2.855 (2) | O4—C4 | 1.260 (3) |
K1—O9i | 2.855 (2) | O5—H5 | 0.77 (3) |
K1—O10ii | 3.420 (2) | O5—C2 | 1.426 (3) |
K1—O10iii | 3.420 (2) | O6—H6 | 0.73 (3) |
K2—O4iv | 2.8382 (18) | O6—C3 | 1.419 (3) |
K2—O4v | 2.8383 (18) | O7—H17 | 0.78 (4) |
K2—O5vi | 2.9814 (18) | O7—H27 | 0.82 (3) |
K2—O5vii | 2.9814 (18) | O8—H18 | 0.86 (4) |
K2—O7ii | 2.774 (2) | O8—H28 | 0.82 (4) |
K2—O7viii | 2.774 (2) | O9—H19 | 0.81 (4) |
K2—O8ii | 3.161 (2) | O9—H29 | 0.92 (4) |
K2—O8viii | 3.161 (2) | O10—H110 | 0.82 (4) |
Na—O1 | 2.3505 (19) | O10—H210 | 0.85 (4) |
Na—O3iv | 2.453 (2) | C1—C2 | 1.533 (3) |
Na—O5iv | 2.474 (2) | C2—H2 | 1.02 (3) |
Na—O7 | 2.324 (2) | C2—C3 | 1.526 (3) |
Na—H17 | 2.51 (3) | C3—H3 | 0.98 (3) |
Na—O8 | 2.356 (2) | C3—C4 | 1.534 (3) |
Na—O10 | 2.332 (2) | | |
| | | |
Naiii—K1—Naii | 80.08 (3) | O1—Na—H17 | 80.3 (8) |
O1i—K1—Naiii | 101.64 (4) | O1—Na—O8 | 103.51 (8) |
O1—K1—Naii | 101.64 (4) | O1—Na—C4iv | 116.52 (7) |
O1—K1—Naiii | 145.38 (4) | O3iv—Na—K1ix | 141.35 (6) |
O1i—K1—Naii | 145.38 (4) | O3iv—Na—K2ix | 107.92 (5) |
O1—K1—O1i | 96.00 (7) | O3iv—Na—O5iv | 81.95 (6) |
O1i—K1—O8ii | 142.46 (5) | O3iv—Na—H17 | 106.6 (9) |
O1i—K1—O8iii | 69.68 (5) | O3iv—Na—C4iv | 22.72 (6) |
O1—K1—O8ii | 69.68 (5) | O5iv—Na—K1ix | 91.55 (5) |
O1—K1—O8iii | 142.46 (5) | O5iv—Na—K2ix | 52.72 (4) |
O1—K1—O9i | 72.98 (5) | O5iv—Na—H17 | 106.0 (8) |
O1i—K1—O9 | 72.98 (5) | O5iv—Na—C4iv | 60.61 (6) |
O1—K1—O9 | 120.61 (6) | O7—Na—K1ix | 125.72 (6) |
O1i—K1—O9i | 120.61 (6) | O7—Na—K2ix | 47.76 (5) |
O1i—K1—O10ii | 117.65 (5) | O7—Na—O1 | 92.68 (7) |
O1i—K1—O10iii | 132.76 (5) | O7—Na—O3iv | 92.76 (7) |
O1—K1—O10ii | 132.76 (5) | O7—Na—O5iv | 93.06 (7) |
O1—K1—O10iii | 117.65 (5) | O7—Na—H17 | 18.0 (8) |
O8iii—K1—Naiii | 32.47 (4) | O7—Na—O8 | 84.01 (8) |
O8ii—K1—Naiii | 109.50 (5) | O7—Na—O10 | 174.12 (9) |
O8iii—K1—Naii | 109.50 (5) | O7—Na—C4iv | 86.35 (7) |
O8ii—K1—Naii | 32.47 (4) | O8—Na—K1ix | 43.77 (6) |
O8iii—K1—O8ii | 141.09 (8) | O8—Na—K2ix | 57.23 (6) |
O8ii—K1—O10iii | 83.02 (5) | O8—Na—O3iv | 161.84 (8) |
O8iii—K1—O10iii | 63.42 (5) | O8—Na—O5iv | 80.39 (7) |
O8iii—K1—O10ii | 83.02 (5) | O8—Na—H17 | 74.5 (8) |
O8ii—K1—O10ii | 63.42 (5) | O8—Na—C4iv | 139.17 (8) |
O9—K1—Naiii | 93.13 (5) | O10—Na—K1ix | 53.21 (6) |
O9i—K1—Naiii | 72.40 (5) | O10—Na—K2ix | 126.50 (6) |
O9i—K1—Naii | 93.13 (5) | O10—Na—O1 | 93.04 (7) |
O9—K1—Naii | 72.40 (5) | O10—Na—O3iv | 88.15 (8) |
O9—K1—O8iii | 89.14 (6) | O10—Na—O5iv | 81.31 (7) |
O9i—K1—O8ii | 89.15 (6) | O10—Na—H17 | 164.2 (9) |
O9i—K1—O8iii | 84.67 (6) | O10—Na—O8 | 93.32 (8) |
O9—K1—O8ii | 84.67 (6) | O10—Na—C4iv | 92.32 (8) |
O9i—K1—O9 | 161.38 (9) | C4iv—Na—K1ix | 140.17 (6) |
O9i—K1—O10ii | 110.65 (6) | C4iv—Na—K2ix | 87.58 (5) |
O9—K1—O10ii | 51.02 (6) | C4iv—Na—H17 | 103.5 (9) |
O9i—K1—O10iii | 51.02 (6) | Na—O1—K1 | 101.32 (6) |
O9—K1—O10iii | 110.65 (6) | C1—O1—K1 | 115.89 (15) |
O10ii—K1—Naii | 33.09 (4) | C1—O1—Na | 125.39 (14) |
O10iii—K1—Naiii | 33.09 (4) | C4—O3—Nax | 108.11 (15) |
O10ii—K1—Naiii | 61.97 (4) | C4—O4—K2x | 118.29 (16) |
O10iii—K1—Naii | 61.97 (4) | K2xi—O5—H5 | 102 (2) |
O10ii—K1—O10iii | 62.68 (7) | Nax—O5—K2xi | 85.96 (6) |
Naii—K2—Naviii | 115.27 (3) | Nax—O5—H5 | 110 (2) |
O4iv—K2—Naviii | 123.57 (4) | C2—O5—K2xi | 120.05 (13) |
O4v—K2—Naviii | 100.14 (4) | C2—O5—Nax | 130.15 (14) |
O4iv—K2—Naii | 100.15 (4) | C2—O5—H5 | 105 (2) |
O4v—K2—Naii | 123.57 (4) | C3—O6—H6 | 112 (3) |
O4iv—K2—O4v | 94.16 (8) | K2ix—O7—H17 | 107 (3) |
O4v—K2—O5vi | 147.12 (5) | K2ix—O7—H27 | 119 (2) |
O4v—K2—O5vii | 67.91 (5) | Na—O7—K2ix | 93.91 (7) |
O4iv—K2—O5vi | 67.91 (5) | Na—O7—H17 | 95 (3) |
O4iv—K2—O5vii | 147.12 (5) | Na—O7—H27 | 128 (2) |
O4v—K2—O8viii | 83.11 (5) | H17—O7—H27 | 111 (3) |
O4iv—K2—O8viii | 90.67 (5) | K1ix—O8—K2ix | 153.34 (8) |
O4v—K2—O8ii | 90.67 (5) | K1ix—O8—H18 | 83 (2) |
O4iv—K2—O8ii | 83.11 (5) | K1ix—O8—H28 | 87 (3) |
O5vii—K2—Naviii | 41.33 (4) | K2ix—O8—H18 | 71 (2) |
O5vii—K2—Naii | 112.73 (4) | K2ix—O8—H28 | 105 (3) |
O5vi—K2—Naviii | 112.73 (4) | Na—O8—K1ix | 103.76 (8) |
O5vi—K2—Naii | 41.33 (4) | Na—O8—K2ix | 83.96 (6) |
O5vi—K2—O5vii | 140.18 (8) | Na—O8—H18 | 119 (3) |
O5vii—K2—O8viii | 60.94 (5) | Na—O8—H28 | 137 (3) |
O5vi—K2—O8viii | 122.67 (5) | H18—O8—H28 | 104 (4) |
O5vii—K2—O8ii | 122.67 (5) | K1—O9—H19 | 112 (3) |
O5vi—K2—O8ii | 60.94 (5) | K1—O9—H29 | 142 (2) |
O7ii—K2—Naii | 38.33 (4) | H19—O9—H29 | 102 (3) |
O7viii—K2—Naii | 86.51 (5) | K1ix—O10—H110 | 98 (2) |
O7ii—K2—Naviii | 86.51 (5) | K1ix—O10—H210 | 58 (2) |
O7viii—K2—Naviii | 38.33 (4) | Na—O10—K1ix | 93.70 (7) |
O7ii—K2—O4v | 109.07 (6) | Na—O10—H110 | 127 (2) |
O7viii—K2—O4v | 138.48 (5) | Na—O10—H210 | 122 (2) |
O7viii—K2—O4iv | 109.07 (6) | H110—O10—H210 | 109 (3) |
O7ii—K2—O4iv | 138.48 (5) | O1—C1—C2 | 116.6 (2) |
O7viii—K2—O5vi | 74.40 (5) | O2—C1—O1 | 126.8 (2) |
O7ii—K2—O5vii | 74.40 (5) | O2—C1—C2 | 116.7 (2) |
O7ii—K2—O5vi | 74.41 (5) | O5—C2—C1 | 110.45 (18) |
O7viii—K2—O5vii | 74.41 (5) | O5—C2—H2 | 108.0 (15) |
O7viii—K2—O7ii | 75.71 (9) | O5—C2—C3 | 109.45 (19) |
O7ii—K2—O8viii | 125.09 (6) | C1—C2—H2 | 108.9 (16) |
O7ii—K2—O8ii | 63.30 (5) | C3—C2—C1 | 110.53 (19) |
O7viii—K2—O8ii | 125.09 (6) | C3—C2—H2 | 109.4 (15) |
O7viii—K2—O8viii | 63.30 (5) | O6—C3—C2 | 110.7 (2) |
O8viii—K2—Naviii | 38.80 (4) | O6—C3—H3 | 106.8 (16) |
O8ii—K2—Naii | 38.80 (4) | O6—C3—C4 | 111.5 (2) |
O8viii—K2—Naii | 149.81 (4) | C2—C3—H3 | 111.5 (17) |
O8ii—K2—Naviii | 149.81 (4) | C2—C3—C4 | 110.00 (19) |
O8viii—K2—O8ii | 170.88 (7) | C4—C3—H3 | 106.2 (17) |
K1ix—Na—H17 | 111.8 (9) | O3—C4—Nax | 49.17 (12) |
K2ix—Na—K1ix | 97.60 (2) | O3—C4—O4 | 125.8 (2) |
K2ix—Na—H17 | 55.1 (8) | O3—C4—C3 | 117.1 (2) |
O1—Na—K1ix | 87.77 (5) | O4—C4—Nax | 123.65 (17) |
O1—Na—K2ix | 133.90 (5) | O4—C4—C3 | 117.1 (2) |
O1—Na—O3iv | 94.48 (7) | C3—C4—Nax | 95.73 (14) |
O1—Na—O5iv | 173.37 (7) | | |
| | | |
K1—O1—C1—O2 | −52.2 (3) | O1—C1—C2—C3 | 61.6 (3) |
K1—O1—C1—C2 | 128.49 (17) | O2—C1—C2—O5 | 3.5 (3) |
K2x—O4—C4—Nax | −72.3 (2) | O2—C1—C2—C3 | −117.8 (2) |
K2x—O4—C4—O3 | −11.5 (3) | O5—C2—C3—O6 | −67.1 (2) |
K2x—O4—C4—C3 | 169.32 (15) | O5—C2—C3—C4 | 56.6 (2) |
K2xi—O5—C2—C1 | 113.12 (17) | O6—C3—C4—Nax | 62.81 (19) |
K2xi—O5—C2—C3 | −124.96 (15) | O6—C3—C4—O3 | 16.2 (3) |
Na—O1—C1—O2 | 75.6 (3) | O6—C3—C4—O4 | −164.6 (2) |
Na—O1—C1—C2 | −103.7 (2) | C1—C2—C3—O6 | 54.8 (3) |
Nax—O3—C4—O4 | −106.2 (2) | C1—C2—C3—C4 | 178.5 (2) |
Nax—O3—C4—C3 | 73.0 (2) | C2—C3—C4—Nax | −60.44 (18) |
Nax—O5—C2—C1 | −134.45 (17) | C2—C3—C4—O3 | −107.1 (2) |
Nax—O5—C2—C3 | −12.5 (3) | C2—C3—C4—O4 | 72.2 (3) |
O1—C1—C2—O5 | −177.10 (19) | | |
Symmetry codes: (i) −x, −y, z; (ii) x, y, z−1; (iii) −x, −y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x+1/2, −y+1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (vii) x+1/2, −y+1/2, −z; (viii) −x+1, −y, z−1; (ix) x, y, z+1; (x) −x+1/2, y+1/2, −z+1; (xi) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.77 (3) | 2.08 (3) | 2.599 (2) | 125 (3) |
O5—H5···O3ii | 0.77 (3) | 2.68 (3) | 3.291 (3) | 138 (3) |
O5—H5···O4ii | 0.77 (3) | 2.89 (3) | 3.253 (3) | 112 (3) |
O6—H6···O10x | 0.73 (3) | 2.11 (3) | 2.828 (3) | 169 (4) |
O7—H17···O6 | 0.78 (4) | 2.00 (4) | 2.783 (3) | 180 (4) |
O7—H27···O4v | 0.82 (3) | 2.06 (3) | 2.859 (3) | 166 (3) |
O8—H18···O3xii | 0.86 (4) | 1.84 (4) | 2.693 (3) | 170 (4) |
O8—H28···O1ix | 0.82 (4) | 2.84 (4) | 3.351 (3) | 123 (3) |
O8—H28···O2ix | 0.82 (4) | 1.93 (4) | 2.748 (3) | 174 (4) |
O9—H19···O2vi | 0.81 (4) | 2.55 (4) | 3.124 (3) | 129 (3) |
O9—H19···O3iv | 0.81 (4) | 2.61 (4) | 3.162 (3) | 127 (3) |
O9—H19···O6iv | 0.81 (4) | 2.41 (4) | 3.114 (3) | 146 (3) |
O9—H29···O4iii | 0.92 (4) | 1.88 (4) | 2.790 (3) | 172 (3) |
O10—H110···O1i | 0.82 (4) | 1.90 (4) | 2.720 (3) | 175 (3) |
O10—H210···O9ix | 0.85 (4) | 1.91 (4) | 2.751 (3) | 173 (3) |
Symmetry codes: (i) −x, −y, z; (ii) x, y, z−1; (iii) −x, −y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x+1/2, −y+1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (ix) x, y, z+1; (x) −x+1/2, y+1/2, −z+1; (xii) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (175K_anh)
top
Crystal data top
C4H12KNaO10 | Dx = 1.804 Mg m−3 |
Mr = 282.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 7792 reflections |
a = 11.8046 (7) Å | θ = 3.6–29.2° |
b = 14.2075 (9) Å | µ = 0.59 mm−1 |
c = 6.1957 (3) Å | T = 175 K |
V = 1039.1 (1) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 585.519 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2672 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2357 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.052 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.799, Tmax = 1.000 | l = −8→8 |
18179 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.030 | w = 1/[σ2(Fo2) + (0.0186P)2 + 0.4847P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.063 | (Δ/σ)max = 0.0001 |
S = 1.07 | Δρmax = 0.30 e Å−3 |
2672 reflections | Δρmin = −0.30 e Å−3 |
195 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
1 restraint | Absolute structure parameter: 0.03 (2) |
12 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0 | 0.0 | 0.0437 (2) | 0.0354 (5) | |
K2 | 0.5 | 0.0 | −0.16034 (9) | 0.02184 (14) | |
Na | 0.23229 (6) | −0.00681 (6) | 0.51684 (11) | 0.01789 (16) | |
O1 | 0.12026 (11) | 0.10884 (9) | 0.3482 (2) | 0.0172 (3) | |
O2 | 0.21185 (12) | 0.20331 (9) | 0.1183 (2) | 0.0202 (3) | |
O3 | 0.22904 (13) | 0.40708 (10) | 0.8186 (2) | 0.0246 (3) | |
O4 | 0.04894 (12) | 0.35956 (10) | 0.8477 (2) | 0.0230 (3) | |
O5 | 0.16496 (12) | 0.35792 (10) | 0.3244 (2) | 0.0178 (3) | |
H5 | 0.193 (2) | 0.3387 (17) | 0.218 (4) | 0.0267 (4)* | |
O6 | 0.29604 (12) | 0.24846 (10) | 0.6329 (2) | 0.0191 (3) | |
H6 | 0.325 (2) | 0.2905 (17) | 0.593 (4) | 0.0286 (5)* | |
O7 | 0.39595 (12) | 0.08318 (11) | 0.4854 (3) | 0.0223 (3) | |
H17 | 0.368 (2) | 0.133 (2) | 0.527 (4) | 0.0335 (5)* | |
H27 | 0.434 (2) | 0.0929 (19) | 0.380 (4) | 0.0335 (5)* | |
O8 | 0.23835 (16) | 0.04152 (12) | 0.8803 (2) | 0.0316 (4) | |
H18 | 0.256 (2) | 0.002 (2) | 0.976 (5) | 0.0474 (6)* | |
H28 | 0.234 (2) | 0.093 (2) | 0.942 (5) | 0.0474 (6)* | |
O9 | 0.05924 (14) | −0.19267 (13) | −0.0319 (3) | 0.0312 (4) | |
H19 | 0.117 (3) | −0.205 (2) | 0.029 (5) | 0.0468 (6)* | |
H29 | 0.032 (2) | −0.249 (2) | −0.064 (4) | 0.0468 (6)* | |
O10 | 0.07789 (13) | −0.10646 (12) | 0.5718 (3) | 0.0294 (4) | |
H110 | 0.015 (3) | −0.106 (2) | 0.513 (4) | 0.0440 (6)* | |
H210 | 0.071 (2) | −0.137 (2) | 0.691 (5) | 0.0440 (6)* | |
C1 | 0.15525 (15) | 0.18782 (13) | 0.2831 (3) | 0.0142 (4) | |
C2 | 0.12536 (15) | 0.27338 (14) | 0.4229 (3) | 0.0150 (4) | |
H2 | 0.0409 (18) | 0.2764 (15) | 0.435 (3) | 0.0180 (4)* | |
C3 | 0.17743 (15) | 0.26353 (13) | 0.6473 (3) | 0.0151 (4) | |
H3 | 0.1461 (18) | 0.2092 (16) | 0.725 (4) | 0.0181 (4)* | |
C4 | 0.14973 (18) | 0.35089 (14) | 0.7840 (3) | 0.0183 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0414 (10) | 0.0340 (11) | 0.0306 (10) | −0.0175 (9) | −0.000000 | 0.000000 |
K2 | 0.0225 (3) | 0.0243 (3) | 0.0186 (3) | −0.0032 (3) | −0.000000 | 0.000000 |
Na | 0.0172 (3) | 0.0171 (4) | 0.0193 (3) | −0.0005 (3) | −0.0003 (3) | 0.0006 (3) |
O1 | 0.0183 (6) | 0.0149 (6) | 0.0185 (6) | −0.0009 (5) | −0.0012 (6) | −0.0005 (6) |
O2 | 0.0244 (7) | 0.0195 (7) | 0.0168 (7) | −0.0005 (6) | 0.0036 (6) | −0.0011 (5) |
O3 | 0.0337 (8) | 0.0194 (7) | 0.0208 (7) | −0.0066 (6) | −0.0013 (7) | −0.0044 (6) |
O4 | 0.0235 (7) | 0.0274 (8) | 0.0181 (7) | 0.0071 (6) | 0.0007 (6) | −0.0035 (6) |
O5 | 0.0251 (7) | 0.0146 (7) | 0.0137 (7) | 0.0000 (5) | 0.0006 (6) | 0.0000 (5) |
O6 | 0.0166 (7) | 0.0182 (7) | 0.0225 (7) | 0.0015 (5) | −0.0018 (6) | 0.0007 (6) |
O7 | 0.0200 (7) | 0.0199 (8) | 0.0270 (8) | −0.0004 (6) | 0.0049 (6) | 0.0013 (6) |
O8 | 0.0604 (11) | 0.0185 (8) | 0.0159 (8) | 0.0072 (8) | 0.0022 (8) | 0.0006 (6) |
O9 | 0.0211 (8) | 0.0441 (10) | 0.0285 (9) | −0.0008 (7) | −0.0061 (7) | 0.0017 (8) |
O10 | 0.0185 (7) | 0.0322 (9) | 0.0375 (9) | −0.0053 (7) | −0.0054 (7) | 0.0101 (7) |
C1 | 0.0124 (9) | 0.0169 (9) | 0.0132 (9) | 0.0011 (7) | −0.0036 (7) | −0.0004 (7) |
C2 | 0.0153 (9) | 0.0149 (9) | 0.0148 (9) | −0.0002 (7) | 0.0000 (8) | −0.0011 (7) |
C3 | 0.0163 (9) | 0.0137 (9) | 0.0153 (9) | 0.0007 (7) | 0.0009 (8) | 0.0008 (8) |
C4 | 0.0267 (11) | 0.0168 (10) | 0.0115 (9) | 0.0030 (8) | −0.0023 (8) | 0.0008 (7) |
Geometric parameters (Å, º) top
K1—O1 | 2.8223 (16) | Na—O7 | 2.3249 (16) |
K1—O1i | 2.8223 (16) | Na—O8 | 2.3556 (16) |
K1—O8ii | 3.0477 (19) | Na—O10 | 2.3328 (17) |
K1—O8iii | 3.0477 (19) | Na—C4v | 3.082 (2) |
K1—H18ii | 3.05 (3) | O1—C1 | 1.262 (2) |
K1—H18iii | 3.05 (3) | O2—C1 | 1.240 (2) |
K1—O9i | 2.8639 (19) | O3—C4 | 1.249 (2) |
K1—O9 | 2.8639 (19) | O4—C4 | 1.260 (2) |
K1—O10ii | 3.418 (2) | O5—H5 | 0.79 (3) |
K1—O10iii | 3.418 (2) | O5—C2 | 1.426 (2) |
K1—H210iii | 3.04 (3) | O6—H6 | 0.73 (2) |
K1—H210ii | 3.04 (3) | O6—C3 | 1.419 (2) |
K2—O4iv | 2.8402 (14) | O7—H17 | 0.82 (3) |
K2—O4v | 2.8402 (14) | O7—H27 | 0.80 (3) |
K2—O5vi | 2.9833 (14) | O8—H18 | 0.84 (3) |
K2—O5vii | 2.9833 (14) | O8—H28 | 0.83 (3) |
K2—O7viii | 2.7789 (16) | O9—H19 | 0.80 (3) |
K2—O7ii | 2.7789 (16) | O9—H29 | 0.89 (3) |
K2—O8ii | 3.1546 (19) | O10—H110 | 0.83 (3) |
K2—O8viii | 3.1546 (19) | O10—H210 | 0.86 (3) |
K2—H18ii | 3.01 (3) | C1—C2 | 1.534 (3) |
K2—H18viii | 3.01 (3) | C2—H2 | 1.00 (2) |
Na—O1 | 2.3538 (15) | C2—C3 | 1.526 (3) |
Na—O3v | 2.4545 (16) | C3—H3 | 0.98 (2) |
Na—O5v | 2.4764 (16) | C3—C4 | 1.538 (3) |
| | | |
Naiii—K1—Naii | 80.10 (3) | O8ii—K2—O5vi | 122.67 (4) |
O1—K1—Naii | 101.57 (3) | O8ii—K2—O5vii | 60.97 (4) |
O1—K1—Naiii | 145.36 (3) | O8viii—K2—O5vii | 122.67 (4) |
O1i—K1—Naii | 145.36 (3) | O8ii—K2—O7ii | 63.31 (4) |
O1i—K1—Naiii | 101.57 (3) | O8ii—K2—O7viii | 125.13 (4) |
O1i—K1—O1 | 96.11 (7) | O8viii—K2—O7viii | 63.31 (4) |
O8iii—K1—Naiii | 32.49 (3) | O8viii—K2—O7ii | 125.13 (4) |
O8ii—K1—Naii | 32.49 (3) | O8viii—K2—O8ii | 170.83 (6) |
O8iii—K1—Naii | 109.57 (5) | H18viii—K2—Naviii | 48.6 (5) |
O8ii—K1—Naiii | 109.57 (5) | H18viii—K2—Naii | 163.8 (6) |
O8iii—K1—O1 | 142.41 (5) | H18ii—K2—Naviii | 163.8 (6) |
O8ii—K1—O1 | 69.61 (4) | H18ii—K2—Naii | 48.6 (5) |
O8ii—K1—O1i | 142.41 (5) | H18ii—K2—O4iv | 89.9 (6) |
O8iii—K1—O1i | 69.61 (4) | H18ii—K2—O4v | 67.6 (6) |
O8iii—K1—O8ii | 141.21 (8) | H18viii—K2—O4v | 89.9 (6) |
H18ii—K1—Naii | 42.0 (5) | H18viii—K2—O4iv | 67.6 (6) |
H18iii—K1—Naii | 122.0 (5) | H18ii—K2—O5vii | 58.3 (6) |
H18iii—K1—Naiii | 42.0 (5) | H18ii—K2—O5vi | 135.8 (7) |
H18ii—K1—Naiii | 122.0 (5) | H18viii—K2—O5vi | 58.3 (6) |
H18ii—K1—O1i | 126.5 (6) | H18viii—K2—O5vii | 135.8 (7) |
H18iii—K1—O1 | 126.5 (6) | H18ii—K2—O7ii | 78.1 (6) |
H18iii—K1—O1i | 65.8 (6) | H18ii—K2—O7viii | 130.4 (6) |
H18ii—K1—O1 | 65.8 (6) | H18viii—K2—O7viii | 78.1 (6) |
H18iii—K1—O8iii | 15.9 (6) | H18viii—K2—O7ii | 130.4 (6) |
H18ii—K1—O8iii | 150.4 (5) | H18ii—K2—O8viii | 156.8 (6) |
H18iii—K1—O8ii | 150.4 (5) | H18ii—K2—O8ii | 15.5 (6) |
H18ii—K1—O8ii | 15.9 (6) | H18viii—K2—O8ii | 156.8 (6) |
H18iii—K1—H18ii | 164.1 (11) | H18viii—K2—O8viii | 15.5 (6) |
O9—K1—Naiii | 93.07 (5) | H18viii—K2—H18ii | 147.5 (11) |
O9—K1—Naii | 72.31 (4) | K2ix—Na—K1x | 97.66 (2) |
O9i—K1—Naiii | 72.31 (4) | O1—Na—K1x | 87.86 (4) |
O9i—K1—Naii | 93.07 (5) | O1—Na—K2ix | 133.93 (4) |
O9—K1—O1i | 73.05 (5) | O3v—Na—K1x | 141.18 (5) |
O9—K1—O1 | 120.68 (5) | O3v—Na—K2ix | 107.97 (4) |
O9i—K1—O1 | 73.05 (5) | O3v—Na—O1 | 94.39 (5) |
O9i—K1—O1i | 120.68 (5) | O5v—Na—K1x | 91.64 (4) |
O9—K1—O8ii | 84.56 (5) | O5v—Na—K2ix | 52.70 (3) |
O9—K1—O8iii | 89.20 (5) | O5v—Na—O1 | 173.35 (6) |
O9i—K1—O8ii | 89.20 (5) | O5v—Na—O3v | 81.86 (5) |
O9i—K1—O8iii | 84.56 (5) | O7—Na—K1x | 125.87 (5) |
O9—K1—H18ii | 75.1 (6) | O7—Na—K2ix | 47.82 (4) |
O9—K1—H18iii | 102.2 (7) | O7—Na—O1 | 92.62 (6) |
O9i—K1—H18iii | 75.1 (6) | O7—Na—O3v | 92.79 (6) |
O9i—K1—H18ii | 102.2 (7) | O7—Na—O5v | 93.04 (6) |
O9i—K1—O9 | 161.17 (9) | O8—Na—K1x | 44.03 (5) |
O10ii—K1—Naii | 33.08 (3) | O8—Na—K2ix | 57.02 (5) |
O10ii—K1—Naiii | 61.85 (4) | O8—Na—O1 | 103.77 (6) |
O10iii—K1—Naiii | 33.08 (3) | O8—Na—O3v | 161.66 (6) |
O10iii—K1—Naii | 61.85 (4) | O8—Na—O5v | 80.31 (6) |
O10ii—K1—O1i | 117.69 (4) | O8—Na—O7 | 83.95 (6) |
O10iii—K1—O1 | 117.69 (4) | O10—Na—K1x | 53.11 (5) |
O10iii—K1—O1i | 132.76 (4) | O10—Na—K2ix | 126.70 (5) |
O10ii—K1—O1 | 132.76 (4) | O10—Na—O1 | 92.84 (6) |
O10ii—K1—O8iii | 83.03 (5) | O10—Na—O3v | 88.07 (6) |
O10iii—K1—O8ii | 83.03 (5) | O10—Na—O5v | 81.59 (6) |
O10ii—K1—O8ii | 63.46 (5) | O10—Na—O7 | 174.39 (7) |
O10iii—K1—O8iii | 63.46 (5) | O10—Na—O8 | 93.51 (7) |
O10ii—K1—H18ii | 67.6 (5) | C4v—Na—K1x | 140.20 (4) |
O10ii—K1—H18iii | 98.3 (6) | C4v—Na—K2ix | 87.63 (4) |
O10iii—K1—H18iii | 67.6 (5) | C4v—Na—O1 | 116.31 (6) |
O10iii—K1—H18ii | 98.3 (6) | C4v—Na—O3v | 22.64 (5) |
O10ii—K1—O9 | 51.05 (5) | C4v—Na—O5v | 60.65 (5) |
O10ii—K1—O9i | 110.41 (6) | C4v—Na—O7 | 86.25 (6) |
O10iii—K1—O9i | 51.05 (5) | C4v—Na—O8 | 139.08 (6) |
O10iii—K1—O9 | 110.41 (6) | C4v—Na—O10 | 92.47 (6) |
O10iii—K1—O10ii | 62.38 (6) | Na—O1—K1 | 101.35 (5) |
H210iii—K1—Naiii | 42.1 (5) | C1—O1—K1 | 115.99 (12) |
H210iii—K1—Naii | 69.1 (6) | C1—O1—Na | 125.36 (11) |
H210ii—K1—Naiii | 69.1 (6) | C4—O3—Naxi | 108.22 (12) |
H210ii—K1—Naii | 42.1 (5) | C4—O4—K2xii | 118.34 (12) |
H210ii—K1—O1i | 105.6 (6) | Naxi—O5—K2xiii | 85.98 (4) |
H210iii—K1—O1i | 133.7 (5) | H5—O5—K2xiii | 102.8 (18) |
H210iii—K1—O1 | 105.6 (6) | H5—O5—Naxi | 113.4 (18) |
H210ii—K1—O1 | 133.7 (5) | C2—O5—K2xiii | 120.12 (10) |
H210iii—K1—O8ii | 83.9 (5) | C2—O5—Naxi | 130.11 (11) |
H210ii—K1—O8iii | 83.9 (5) | C2—O5—H5 | 101.8 (18) |
H210ii—K1—O8ii | 68.3 (5) | C3—O6—H6 | 111 (2) |
H210iii—K1—O8iii | 68.3 (5) | Na—O7—K2xiv | 93.86 (5) |
H210iii—K1—H18iii | 68.4 (8) | H17—O7—K2xiv | 107.4 (19) |
H210iii—K1—H18ii | 99.8 (8) | H17—O7—Na | 96.5 (19) |
H210ii—K1—H18ii | 68.4 (8) | H27—O7—K2xiv | 117.8 (19) |
H210ii—K1—H18iii | 99.8 (8) | H27—O7—Na | 128.9 (19) |
H210iii—K1—O9 | 124.1 (6) | H27—O7—H17 | 109 (3) |
H210ii—K1—O9i | 124.1 (6) | K2xiv—O8—K1xiv | 153.41 (6) |
H210ii—K1—O9 | 37.3 (6) | Na—O8—K1xiv | 103.48 (7) |
H210iii—K1—O9i | 37.3 (6) | Na—O8—K2xiv | 84.19 (5) |
H210ii—K1—O10iii | 75.1 (6) | H18—O8—K1xiv | 82 (2) |
H210iii—K1—O10iii | 13.8 (6) | H18—O8—K2xiv | 72.2 (19) |
H210ii—K1—O10ii | 13.8 (6) | H18—O8—Na | 119 (2) |
H210iii—K1—O10ii | 75.1 (6) | H28—O8—K1xiv | 87 (2) |
H210iii—K1—H210ii | 88.3 (12) | H28—O8—K2xiv | 106 (2) |
Naviii—K2—Naii | 115.37 (3) | H28—O8—Na | 134 (2) |
O4iv—K2—Naii | 123.68 (3) | H28—O8—H18 | 107 (3) |
O4v—K2—Naii | 100.05 (3) | K2xiv—H18—K1xiv | 171.7 (11) |
O4iv—K2—Naviii | 100.05 (3) | O8—H18—K1xiv | 82 (2) |
O4v—K2—Naviii | 123.68 (3) | O8—H18—K2xiv | 92 (2) |
O4v—K2—O4iv | 94.00 (6) | H19—O9—K1i | 110 (2) |
O5vi—K2—Naviii | 41.32 (3) | H29—O9—K1i | 144.1 (18) |
O5vi—K2—Naii | 112.75 (3) | H29—O9—H19 | 103 (3) |
O5vii—K2—Naviii | 112.75 (3) | Na—O10—K1x | 93.81 (6) |
O5vii—K2—Naii | 41.32 (3) | H110—O10—K1x | 97.6 (18) |
O5vii—K2—O4v | 67.93 (4) | H110—O10—Na | 128.9 (19) |
O5vi—K2—O4v | 147.20 (4) | H210—O10—K1x | 57.3 (19) |
O5vii—K2—O4iv | 147.20 (4) | H210—O10—Na | 120.1 (19) |
O5vi—K2—O4iv | 67.93 (4) | H210—O10—H110 | 108 (3) |
O5vii—K2—O5vi | 140.16 (6) | O10—H210—K1x | 109 (2) |
O7viii—K2—Naii | 86.57 (4) | O2—C1—O1 | 126.68 (18) |
O7viii—K2—Naviii | 38.32 (3) | C2—C1—O1 | 116.67 (16) |
O7ii—K2—Naii | 38.32 (3) | C2—C1—O2 | 116.64 (17) |
O7ii—K2—Naviii | 86.57 (4) | C1—C2—O5 | 110.51 (15) |
O7ii—K2—O4iv | 109.25 (4) | H2—C2—O5 | 108.8 (12) |
O7viii—K2—O4iv | 138.37 (4) | H2—C2—C1 | 107.8 (12) |
O7ii—K2—O4v | 138.37 (4) | C3—C2—O5 | 109.57 (15) |
O7viii—K2—O4v | 109.25 (4) | C3—C2—C1 | 110.44 (15) |
O7ii—K2—O5vii | 74.34 (4) | C3—C2—H2 | 109.7 (12) |
O7viii—K2—O5vii | 74.43 (4) | C2—C3—O6 | 110.73 (16) |
O7ii—K2—O5vi | 74.43 (4) | H3—C3—O6 | 106.5 (13) |
O7viii—K2—O5vi | 74.34 (4) | H3—C3—C2 | 111.4 (13) |
O7viii—K2—O7ii | 75.67 (7) | C4—C3—O6 | 111.48 (16) |
O8viii—K2—Naviii | 38.78 (3) | C4—C3—C2 | 110.00 (15) |
O8viii—K2—Naii | 149.88 (3) | C4—C3—H3 | 106.6 (13) |
O8ii—K2—Naviii | 149.88 (3) | O3—C4—Naxi | 49.15 (10) |
O8ii—K2—Naii | 38.78 (3) | O4—C4—Naxi | 123.51 (13) |
O8viii—K2—O4iv | 82.97 (4) | O4—C4—O3 | 126.27 (19) |
O8ii—K2—O4iv | 90.76 (4) | C3—C4—Naxi | 95.75 (11) |
O8ii—K2—O4v | 82.97 (4) | C3—C4—O3 | 116.82 (18) |
O8viii—K2—O4v | 90.76 (4) | C3—C4—O4 | 116.90 (17) |
O8viii—K2—O5vi | 60.97 (4) | | |
| | | |
K1—O1—C1—O2 | −51.99 (13) | Naxi—O3—C4—C3 | 73.22 (12) |
K1i—O1—C1—O2 | −51.99 (13) | Naxi—O5—C2—C1 | −134.38 (15) |
K1—O1—C1—C2 | 128.44 (11) | Naxi—O5—C2—C3 | −12.47 (13) |
K1i—O1—C1—C2 | 128.44 (11) | Naxi—C4—C3—O6 | 62.92 (11) |
K2xii—O4—C4—Naxi | −72.67 (11) | Naxi—C4—C3—C2 | −60.31 (11) |
K2—O4v—C4v—Na | −72.67 (11) | O1—C1—C2—O5 | −176.94 (16) |
K2xii—O4—C4—O3 | −11.83 (14) | O1—C1—C2—C3 | 61.66 (18) |
K2xi—O4—C4—O3 | −11.83 (14) | O2—C1—C2—O5 | 3.44 (18) |
K2xii—O4—C4—C3 | 169.24 (12) | O2—C1—C2—C3 | −117.96 (17) |
K2xi—O4—C4—C3 | 169.24 (12) | O3—C4—C3—O6 | 16.22 (19) |
K2xv—O5—C2—C1 | 113.12 (12) | O3—C4—C3—C2 | −107.01 (18) |
K2xiii—O5—C2—C1 | 113.12 (12) | O4—C4—C3—O6 | −164.75 (17) |
K2xiii—O5—C2—C3 | −124.97 (12) | O4—C4—C3—C2 | 72.02 (18) |
K2xv—O5—C2—C3 | −124.97 (12) | O5—C2—C3—O6 | −67.18 (15) |
Na—O1—C1—O2 | 75.93 (15) | O5—C2—C3—C4 | 56.48 (16) |
Na—O1—C1—C2 | −103.64 (14) | O6—C3—C2—C1 | 54.77 (17) |
Naxi—O3—C4—O4 | −105.71 (12) | C1—C2—C3—C4 | 178.44 (15) |
Symmetry codes: (i) −x, −y, z; (ii) x, y, z−1; (iii) −x, −y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) x+1/2, −y+1/2, −z; (vii) −x+1/2, y−1/2, −z; (viii) −x+1, −y, z−1; (ix) −x+1, −y, z+1; (x) −x, −y, z+1; (xi) −x+1/2, y+1/2, −z+1; (xii) x−1/2, −y+1/2, −z+1; (xiii) x−1/2, −y+1/2, −z; (xiv) x, y, z+1; (xv) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.79 (3) | 2.03 (2) | 2.6005 (19) | 129 (2) |
O5—H5···O3ii | 0.79 (3) | 2.69 (3) | 3.299 (2) | 135 (2) |
O5—H5···O4ii | 0.79 (3) | 2.87 (3) | 3.256 (2) | 113 (2) |
O6—H6···O10xi | 0.73 (2) | 2.12 (2) | 2.841 (2) | 169 (3) |
O7—H17···O6 | 0.82 (3) | 1.96 (3) | 2.782 (2) | 177 (3) |
O7—H27···O4iv | 0.80 (3) | 2.07 (3) | 2.861 (2) | 167 (3) |
O8—H18···O3xvi | 0.84 (3) | 1.86 (3) | 2.697 (2) | 171 (3) |
O8—H28···O1xiv | 0.83 (3) | 2.86 (3) | 3.356 (2) | 121 (2) |
O8—H28···O2xiv | 0.83 (3) | 1.93 (3) | 2.749 (2) | 172 (3) |
O9—H19···O2vii | 0.80 (3) | 2.57 (3) | 3.126 (2) | 128 (3) |
O9—H19···O3v | 0.80 (3) | 2.59 (3) | 3.162 (2) | 130 (3) |
O9—H19···O6v | 0.80 (3) | 2.43 (3) | 3.119 (2) | 146 (3) |
O9—H29···O4iii | 0.89 (3) | 1.92 (3) | 2.794 (2) | 171 (3) |
O10—H110···O1i | 0.83 (3) | 1.89 (3) | 2.719 (2) | 173 (3) |
O10—H210···O9xiv | 0.86 (3) | 1.89 (3) | 2.753 (2) | 175 (3) |
Symmetry codes: (i) −x, −y, z; (ii) x, y, z−1; (iii) −x, −y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vii) −x+1/2, y−1/2, −z; (xi) −x+1/2, y+1/2, −z+1; (xiv) x, y, z+1; (xvi) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (200K_anh)
top
Crystal data top
C4H12KNaO10 | Dx = 1.800 Mg m−3 |
Mr = 282.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 7450 reflections |
a = 11.8172 (7) Å | θ = 3.5–29.2° |
b = 14.2126 (9) Å | µ = 0.59 mm−1 |
c = 6.2012 (3) Å | T = 200 K |
V = 1041.52 (10) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 585.519 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2678 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2350 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.054 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −18→19 |
Tmin = 0.798, Tmax = 1.000 | l = −8→8 |
18257 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.032 | w = 1/[σ2(Fo2) + (0.0192P)2 + 0.4814P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.067 | (Δ/σ)max = 0.001 |
S = 1.08 | Δρmax = 0.34 e Å−3 |
2678 reflections | Δρmin = −0.32 e Å−3 |
195 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
1 restraint | Absolute structure parameter: 0.04 (2) |
12 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0 | 0.0 | 0.0441 (3) | 0.0406 (5) | |
K2 | 0.5 | 0.0 | −0.16016 (10) | 0.02474 (15) | |
Na | 0.23217 (6) | −0.00677 (6) | 0.51782 (12) | 0.02024 (18) | |
O1 | 0.12034 (11) | 0.10885 (10) | 0.3486 (2) | 0.0195 (3) | |
O2 | 0.21150 (12) | 0.20330 (10) | 0.1182 (2) | 0.0229 (3) | |
O3 | 0.22987 (13) | 0.40693 (10) | 0.8178 (2) | 0.0275 (3) | |
O4 | 0.04988 (13) | 0.36003 (11) | 0.8471 (2) | 0.0259 (3) | |
O5 | 0.16471 (13) | 0.35770 (10) | 0.3244 (2) | 0.0200 (3) | |
H5 | 0.191 (2) | 0.3425 (18) | 0.211 (5) | 0.0299 (5)* | |
O6 | 0.29584 (12) | 0.24837 (10) | 0.6316 (3) | 0.0216 (3) | |
H6 | 0.326 (2) | 0.2919 (18) | 0.600 (5) | 0.0323 (5)* | |
O7 | 0.39594 (13) | 0.08303 (11) | 0.4852 (3) | 0.0252 (3) | |
H17 | 0.367 (2) | 0.132 (2) | 0.525 (5) | 0.0378 (5)* | |
H27 | 0.431 (2) | 0.095 (2) | 0.378 (5) | 0.0378 (5)* | |
O8 | 0.23925 (17) | 0.04151 (13) | 0.8813 (3) | 0.0356 (4) | |
H18 | 0.256 (3) | 0.003 (3) | 0.980 (5) | 0.0533 (7)* | |
H28 | 0.233 (3) | 0.094 (2) | 0.945 (5) | 0.0533 (7)* | |
O9 | 0.05967 (15) | −0.19347 (15) | −0.0327 (3) | 0.0365 (4) | |
H19 | 0.118 (3) | −0.207 (2) | 0.026 (5) | 0.0548 (6)* | |
H29 | 0.032 (3) | −0.248 (2) | −0.069 (5) | 0.0548 (6)* | |
O10 | 0.07759 (14) | −0.10576 (13) | 0.5728 (3) | 0.0349 (4) | |
H110 | 0.016 (3) | −0.106 (2) | 0.512 (4) | 0.0523 (6)* | |
H210 | 0.068 (3) | −0.136 (2) | 0.693 (5) | 0.0523 (6)* | |
C1 | 0.15499 (16) | 0.18789 (14) | 0.2828 (3) | 0.0164 (4) | |
C2 | 0.12531 (16) | 0.27334 (14) | 0.4225 (3) | 0.0163 (4) | |
H2 | 0.0411 (19) | 0.2780 (16) | 0.438 (3) | 0.0195 (5)* | |
C3 | 0.17744 (16) | 0.26356 (14) | 0.6471 (3) | 0.0174 (4) | |
H3 | 0.1465 (19) | 0.2099 (17) | 0.726 (4) | 0.0208 (5)* | |
C4 | 0.15028 (19) | 0.35095 (15) | 0.7826 (3) | 0.0203 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0471 (11) | 0.0385 (12) | 0.0361 (11) | −0.0210 (10) | −0.000000 | 0.000000 |
K2 | 0.0250 (3) | 0.0275 (3) | 0.0217 (3) | −0.0034 (3) | −0.000000 | 0.000000 |
Na | 0.0190 (4) | 0.0196 (4) | 0.0221 (4) | −0.0005 (3) | −0.0004 (3) | 0.0005 (4) |
O1 | 0.0198 (7) | 0.0175 (7) | 0.0213 (7) | −0.0006 (5) | −0.0010 (6) | −0.0001 (6) |
O2 | 0.0275 (8) | 0.0221 (8) | 0.0190 (8) | −0.0005 (6) | 0.0057 (6) | −0.0013 (6) |
O3 | 0.0367 (8) | 0.0227 (8) | 0.0231 (8) | −0.0072 (7) | −0.0015 (7) | −0.0045 (6) |
O4 | 0.0254 (7) | 0.0318 (8) | 0.0204 (7) | 0.0085 (6) | 0.0004 (7) | −0.0039 (7) |
O5 | 0.0281 (8) | 0.0165 (7) | 0.0154 (7) | −0.0003 (6) | −0.0002 (6) | 0.0004 (6) |
O6 | 0.0182 (7) | 0.0201 (8) | 0.0264 (8) | 0.0025 (6) | −0.0027 (6) | 0.0003 (6) |
O7 | 0.0221 (8) | 0.0226 (8) | 0.0309 (9) | 0.0000 (6) | 0.0047 (7) | 0.0021 (7) |
O8 | 0.0667 (12) | 0.0211 (8) | 0.0189 (8) | 0.0077 (8) | 0.0026 (8) | −0.0002 (6) |
O9 | 0.0239 (9) | 0.0522 (12) | 0.0335 (10) | −0.0023 (8) | −0.0068 (7) | 0.0030 (9) |
O10 | 0.0215 (8) | 0.0379 (10) | 0.0452 (11) | −0.0076 (7) | −0.0073 (8) | 0.0133 (8) |
C1 | 0.0140 (9) | 0.0179 (10) | 0.0173 (9) | 0.0018 (8) | −0.0044 (8) | −0.0008 (8) |
C2 | 0.0170 (9) | 0.0155 (10) | 0.0163 (9) | 0.0009 (8) | −0.0005 (8) | −0.0012 (7) |
C3 | 0.0193 (9) | 0.0162 (9) | 0.0166 (9) | 0.0014 (8) | 0.0015 (8) | 0.0003 (8) |
C4 | 0.0296 (12) | 0.0176 (10) | 0.0135 (9) | 0.0030 (8) | −0.0030 (8) | 0.0020 (8) |
Geometric parameters (Å, º) top
K1—O1 | 2.8252 (17) | Na—O7 | 2.3271 (17) |
K1—O1i | 2.8252 (17) | Na—O8 | 2.3576 (17) |
K1—O8ii | 3.060 (2) | Na—O10 | 2.3308 (18) |
K1—O8iii | 3.060 (2) | Na—C4v | 3.080 (2) |
K1—H18ii | 3.06 (3) | O1—C1 | 1.263 (2) |
K1—H18iii | 3.06 (3) | O2—C1 | 1.240 (2) |
K1—O9i | 2.878 (2) | O3—C4 | 1.251 (3) |
K1—O9 | 2.878 (2) | O4—C4 | 1.259 (3) |
K1—O10ii | 3.412 (2) | O5—H5 | 0.80 (3) |
K1—O10iii | 3.412 (2) | O5—C2 | 1.423 (2) |
K1—H210iii | 3.02 (3) | O6—H6 | 0.74 (2) |
K1—H210ii | 3.02 (3) | O6—C3 | 1.419 (2) |
K2—O4iv | 2.8416 (15) | O7—H17 | 0.81 (3) |
K2—O4v | 2.8416 (15) | O7—H27 | 0.80 (3) |
K2—O5vi | 2.9859 (15) | O8—H18 | 0.85 (3) |
K2—O5vii | 2.9859 (15) | O8—H28 | 0.85 (3) |
K2—O7viii | 2.7824 (17) | O9—H19 | 0.80 (3) |
K2—O7ii | 2.7824 (17) | O9—H29 | 0.87 (3) |
K2—O8ii | 3.148 (2) | O10—H110 | 0.82 (3) |
K2—O8viii | 3.148 (2) | O10—H210 | 0.86 (3) |
K2—H18ii | 3.01 (3) | C1—C2 | 1.532 (3) |
K2—H18viii | 3.01 (3) | C2—H2 | 1.00 (2) |
Na—O1 | 2.3554 (16) | C2—C3 | 1.529 (3) |
Na—O3v | 2.4569 (17) | C3—H3 | 0.98 (2) |
Na—O5v | 2.4805 (17) | C3—C4 | 1.533 (3) |
| | | |
Naiii—K1—Naii | 80.14 (4) | O8ii—K2—O5vi | 122.62 (4) |
O1—K1—Naii | 101.54 (3) | O8ii—K2—O5vii | 61.10 (4) |
O1—K1—Naiii | 145.38 (3) | O8viii—K2—O5vii | 122.62 (4) |
O1i—K1—Naii | 145.38 (3) | O8ii—K2—O7ii | 63.41 (4) |
O1i—K1—Naiii | 101.54 (3) | O8ii—K2—O7viii | 125.22 (5) |
O1i—K1—O1 | 96.11 (8) | O8viii—K2—O7viii | 63.41 (4) |
O8iii—K1—Naiii | 32.58 (4) | O8viii—K2—O7ii | 125.22 (5) |
O8ii—K1—Naii | 32.58 (4) | O8viii—K2—O8ii | 170.63 (6) |
O8iii—K1—Naii | 109.73 (6) | H18viii—K2—Naviii | 49.1 (6) |
O8ii—K1—Naiii | 109.73 (6) | H18viii—K2—Naii | 164.4 (6) |
O8iii—K1—O1 | 142.31 (5) | H18ii—K2—Naviii | 164.4 (6) |
O8ii—K1—O1 | 69.50 (4) | H18ii—K2—Naii | 49.1 (6) |
O8ii—K1—O1i | 142.31 (5) | H18ii—K2—O4iv | 89.5 (6) |
O8iii—K1—O1i | 69.50 (4) | H18ii—K2—O4v | 67.2 (7) |
O8iii—K1—O8ii | 141.46 (9) | H18viii—K2—O4v | 89.5 (6) |
H18ii—K1—Naii | 42.5 (6) | H18viii—K2—O4iv | 67.2 (7) |
H18iii—K1—Naii | 122.6 (6) | H18ii—K2—O5vii | 58.9 (6) |
H18iii—K1—Naiii | 42.5 (6) | H18ii—K2—O5vi | 135.6 (7) |
H18ii—K1—Naiii | 122.6 (6) | H18viii—K2—O5vi | 58.9 (6) |
H18ii—K1—O1i | 126.4 (6) | H18viii—K2—O5vii | 135.6 (7) |
H18iii—K1—O1 | 126.4 (6) | H18ii—K2—O7ii | 78.5 (6) |
H18iii—K1—O1i | 65.2 (6) | H18ii—K2—O7viii | 131.1 (6) |
H18ii—K1—O1 | 65.2 (6) | H18viii—K2—O7viii | 78.5 (6) |
H18iii—K1—O8iii | 16.0 (6) | H18viii—K2—O7ii | 131.1 (6) |
H18ii—K1—O8iii | 151.1 (6) | H18ii—K2—O8viii | 156.3 (6) |
H18iii—K1—O8ii | 151.1 (6) | H18ii—K2—O8ii | 15.6 (6) |
H18ii—K1—O8ii | 16.0 (6) | H18viii—K2—O8ii | 156.3 (6) |
H18iii—K1—H18ii | 165.1 (11) | H18viii—K2—O8viii | 15.6 (6) |
O9—K1—Naiii | 93.01 (5) | H18viii—K2—H18ii | 146.4 (12) |
O9—K1—Naii | 72.19 (5) | K2ix—Na—K1x | 97.76 (2) |
O9i—K1—Naiii | 72.19 (5) | O1—Na—K1x | 87.95 (4) |
O9i—K1—Naii | 93.01 (5) | O1—Na—K2ix | 133.95 (4) |
O9—K1—O1i | 73.19 (5) | O3v—Na—K1x | 140.98 (5) |
O9—K1—O1 | 120.69 (6) | O3v—Na—K2ix | 108.08 (4) |
O9i—K1—O1 | 73.19 (5) | O3v—Na—O1 | 94.21 (5) |
O9i—K1—O1i | 120.69 (6) | O5v—Na—K1x | 91.81 (4) |
O9—K1—O8ii | 84.45 (5) | O5v—Na—K2ix | 52.71 (4) |
O9—K1—O8iii | 89.29 (5) | O5v—Na—O1 | 173.29 (6) |
O9i—K1—O8ii | 89.29 (5) | O5v—Na—O3v | 81.77 (5) |
O9i—K1—O8iii | 84.45 (5) | O7—Na—K1x | 126.10 (5) |
O9—K1—H18ii | 75.4 (7) | O7—Na—K2ix | 47.87 (4) |
O9—K1—H18iii | 102.1 (7) | O7—Na—O1 | 92.59 (6) |
O9i—K1—H18iii | 75.4 (7) | O7—Na—O3v | 92.77 (6) |
O9i—K1—H18ii | 102.1 (7) | O7—Na—O5v | 92.96 (6) |
O9i—K1—O9 | 160.95 (10) | O8—Na—K1x | 44.33 (5) |
O10ii—K1—Naii | 33.04 (3) | O8—Na—K2ix | 56.81 (5) |
O10ii—K1—Naiii | 61.79 (4) | O8—Na—O1 | 104.04 (6) |
O10iii—K1—Naiii | 33.04 (3) | O8—Na—O3v | 161.56 (7) |
O10iii—K1—Naii | 61.79 (4) | O8—Na—O5v | 80.29 (6) |
O10ii—K1—O1i | 117.81 (4) | O8—Na—O7 | 83.92 (7) |
O10iii—K1—O1 | 117.81 (4) | O10—Na—K1x | 52.95 (5) |
O10iii—K1—O1i | 132.73 (4) | O10—Na—K2ix | 126.88 (5) |
O10ii—K1—O1 | 132.73 (4) | O10—Na—O1 | 92.67 (6) |
O10ii—K1—O8iii | 83.15 (5) | O10—Na—O3v | 88.03 (7) |
O10iii—K1—O8ii | 83.15 (5) | O10—Na—O5v | 81.87 (6) |
O10ii—K1—O8ii | 63.51 (5) | O10—Na—O7 | 174.61 (7) |
O10iii—K1—O8iii | 63.51 (5) | O10—Na—O8 | 93.65 (7) |
O10ii—K1—H18ii | 68.2 (6) | C4v—Na—K1x | 140.15 (5) |
O10ii—K1—H18iii | 98.6 (6) | C4v—Na—K2ix | 87.60 (4) |
O10iii—K1—H18iii | 68.2 (6) | C4v—Na—O1 | 116.21 (6) |
O10iii—K1—H18ii | 98.6 (6) | C4v—Na—O3v | 22.74 (5) |
O10ii—K1—O9 | 51.07 (5) | C4v—Na—O5v | 60.48 (5) |
O10ii—K1—O9i | 110.18 (7) | C4v—Na—O7 | 86.13 (6) |
O10iii—K1—O9i | 51.07 (5) | C4v—Na—O8 | 138.87 (7) |
O10iii—K1—O9 | 110.18 (7) | C4v—Na—O10 | 92.61 (7) |
O10iii—K1—O10ii | 62.13 (7) | Na—O1—K1 | 101.43 (5) |
H210iii—K1—Naiii | 42.4 (6) | C1—O1—K1 | 115.73 (13) |
H210iii—K1—Naii | 68.4 (6) | C1—O1—Na | 125.62 (12) |
H210ii—K1—Naiii | 68.4 (6) | C4—O3—Naxi | 107.87 (13) |
H210ii—K1—Naii | 42.4 (6) | C4—O4—K2xii | 118.98 (13) |
H210ii—K1—O1i | 105.5 (6) | Naxi—O5—K2xiii | 85.92 (5) |
H210iii—K1—O1i | 134.3 (6) | H5—O5—K2xiii | 97.9 (19) |
H210iii—K1—O1 | 105.5 (6) | H5—O5—Naxi | 111.5 (19) |
H210ii—K1—O1 | 134.3 (6) | C2—O5—K2xiii | 120.21 (11) |
H210iii—K1—O8ii | 83.3 (6) | C2—O5—Naxi | 130.26 (12) |
H210ii—K1—O8iii | 83.3 (6) | C2—O5—H5 | 106.0 (18) |
H210ii—K1—O8ii | 68.9 (6) | C3—O6—H6 | 111 (2) |
H210iii—K1—O8iii | 68.9 (6) | Na—O7—K2xiv | 93.79 (6) |
H210iii—K1—H18iii | 69.6 (8) | H17—O7—K2xiv | 108 (2) |
H210iii—K1—H18ii | 99.3 (9) | H17—O7—Na | 96 (2) |
H210ii—K1—H18ii | 69.6 (8) | H27—O7—K2xiv | 121 (2) |
H210ii—K1—H18iii | 99.3 (9) | H27—O7—Na | 128 (2) |
H210iii—K1—O9 | 123.7 (6) | H27—O7—H17 | 107 (3) |
H210ii—K1—O9i | 123.7 (6) | K2xiv—O8—K1xiv | 153.55 (6) |
H210ii—K1—O9 | 37.4 (6) | Na—O8—K1xiv | 103.10 (7) |
H210iii—K1—O9i | 37.4 (6) | Na—O8—K2xiv | 84.38 (6) |
H210ii—K1—O10iii | 74.6 (6) | H18—O8—K1xiv | 82 (2) |
H210iii—K1—O10iii | 13.7 (6) | H18—O8—K2xiv | 73 (2) |
H210ii—K1—O10ii | 13.7 (6) | H18—O8—Na | 121 (2) |
H210iii—K1—O10ii | 74.6 (6) | H28—O8—K1xiv | 86 (2) |
H210iii—K1—H210ii | 87.5 (13) | H28—O8—K2xiv | 107 (2) |
Naviii—K2—Naii | 115.52 (3) | H28—O8—Na | 135 (2) |
O4iv—K2—Naii | 123.91 (3) | H28—O8—H18 | 105 (3) |
O4v—K2—Naii | 99.85 (3) | K2xiv—H18—K1xiv | 170.5 (11) |
O4iv—K2—Naviii | 99.85 (3) | O8—H18—K1xiv | 82 (2) |
O4v—K2—Naviii | 123.91 (3) | O8—H18—K2xiv | 92 (2) |
O4v—K2—O4iv | 93.81 (7) | H19—O9—K1i | 111 (2) |
O5vi—K2—Naviii | 41.37 (3) | H29—O9—K1i | 144 (2) |
O5vi—K2—Naii | 112.75 (4) | H29—O9—H19 | 103 (3) |
O5vii—K2—Naviii | 112.75 (4) | Na—O10—K1x | 94.01 (6) |
O5vii—K2—Naii | 41.37 (3) | H110—O10—K1x | 99 (2) |
O5vii—K2—O4v | 67.89 (4) | H110—O10—Na | 129 (2) |
O5vi—K2—O4v | 147.40 (4) | H210—O10—K1x | 56 (2) |
O5vii—K2—O4iv | 147.40 (4) | H210—O10—Na | 122 (2) |
O5vi—K2—O4iv | 67.89 (4) | H210—O10—H110 | 106 (3) |
O5vii—K2—O5vi | 140.12 (6) | O10—H210—K1x | 110 (2) |
O7viii—K2—Naii | 86.62 (4) | O2—C1—O1 | 126.72 (19) |
O7viii—K2—Naviii | 38.34 (3) | C2—C1—O1 | 116.61 (17) |
O7ii—K2—Naii | 38.34 (3) | C2—C1—O2 | 116.68 (18) |
O7ii—K2—Naviii | 86.62 (4) | C1—C2—O5 | 110.55 (15) |
O7ii—K2—O4iv | 109.56 (5) | H2—C2—O5 | 108.0 (13) |
O7viii—K2—O4iv | 138.19 (4) | H2—C2—C1 | 109.4 (13) |
O7ii—K2—O4v | 138.19 (4) | C3—C2—O5 | 109.53 (16) |
O7viii—K2—O4v | 109.56 (5) | C3—C2—C1 | 110.53 (16) |
O7ii—K2—O5vii | 74.31 (4) | C3—C2—H2 | 108.7 (12) |
O7viii—K2—O5vii | 74.41 (4) | C2—C3—O6 | 110.44 (16) |
O7ii—K2—O5vi | 74.41 (4) | H3—C3—O6 | 106.5 (13) |
O7viii—K2—O5vi | 74.31 (4) | H3—C3—C2 | 112.0 (13) |
O7viii—K2—O7ii | 75.55 (7) | C4—C3—O6 | 111.53 (17) |
O8viii—K2—Naviii | 38.81 (3) | C4—C3—C2 | 109.93 (16) |
O8viii—K2—Naii | 150.04 (4) | C4—C3—H3 | 106.3 (13) |
O8ii—K2—Naviii | 150.04 (4) | O3—C4—Naxi | 49.39 (10) |
O8ii—K2—Naii | 38.81 (3) | O4—C4—Naxi | 123.37 (14) |
O8viii—K2—O4iv | 82.67 (5) | O4—C4—O3 | 126.0 (2) |
O8ii—K2—O4iv | 90.92 (4) | C3—C4—Naxi | 96.10 (12) |
O8ii—K2—O4v | 82.67 (5) | C3—C4—O3 | 116.96 (19) |
O8viii—K2—O4v | 90.92 (4) | C3—C4—O4 | 117.03 (18) |
O8viii—K2—O5vi | 61.10 (4) | | |
| | | |
K1—O1—C1—O2 | −52.24 (13) | Naxi—O3—C4—C3 | 73.79 (12) |
K1i—O1—C1—O2 | −52.24 (13) | Naxi—O5—C2—C1 | −134.31 (15) |
K1—O1—C1—C2 | 128.57 (12) | Naxi—O5—C2—C3 | −12.29 (14) |
K1i—O1—C1—C2 | 128.57 (12) | Naxi—C4—C3—O6 | 62.66 (12) |
K2xii—O4—C4—Naxi | −72.53 (12) | Naxi—C4—C3—C2 | −60.18 (12) |
K2—O4v—C4v—Na | −72.53 (12) | O1—C1—C2—O5 | −177.21 (17) |
K2xii—O4—C4—O3 | −11.53 (15) | O1—C1—C2—C3 | 61.35 (19) |
K2xi—O4—C4—O3 | −11.53 (15) | O2—C1—C2—O5 | 3.52 (19) |
K2xii—O4—C4—C3 | 168.87 (13) | O2—C1—C2—C3 | −117.92 (18) |
K2xi—O4—C4—C3 | 168.87 (13) | O3—C4—C3—O6 | 15.5 (2) |
K2xv—O5—C2—C1 | 113.03 (13) | O3—C4—C3—C2 | −107.32 (19) |
K2xiii—O5—C2—C1 | 113.03 (13) | O4—C4—C3—O6 | −164.85 (18) |
K2xiii—O5—C2—C3 | −124.94 (13) | O4—C4—C3—C2 | 72.32 (19) |
K2xv—O5—C2—C3 | −124.94 (13) | O5—C2—C3—O6 | −67.34 (16) |
Na—O1—C1—O2 | 75.77 (16) | O5—C2—C3—C4 | 56.14 (17) |
Na—O1—C1—C2 | −103.42 (15) | O6—C3—C2—C1 | 54.70 (18) |
Naxi—O3—C4—O4 | −105.81 (13) | C1—C2—C3—C4 | 178.17 (16) |
Symmetry codes: (i) −x, −y, z; (ii) x, y, z−1; (iii) −x, −y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) x+1/2, −y+1/2, −z; (vii) −x+1/2, y−1/2, −z; (viii) −x+1, −y, z−1; (ix) −x+1, −y, z+1; (x) −x, −y, z+1; (xi) −x+1/2, y+1/2, −z+1; (xii) x−1/2, −y+1/2, −z+1; (xiii) x−1/2, −y+1/2, −z; (xiv) x, y, z+1; (xv) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.80 (3) | 2.07 (3) | 2.599 (2) | 123 (2) |
O5—H5···O3ii | 0.80 (3) | 2.65 (3) | 3.309 (2) | 142 (2) |
O5—H5···O4ii | 0.80 (3) | 2.82 (3) | 3.256 (2) | 117 (2) |
O6—H6···O10xi | 0.74 (2) | 2.14 (2) | 2.853 (3) | 163 (3) |
O7—H17···O6 | 0.81 (3) | 1.97 (3) | 2.783 (2) | 178 (3) |
O7—H27···O4iv | 0.80 (3) | 2.08 (3) | 2.865 (2) | 166 (3) |
O8—H18···O3xvi | 0.85 (3) | 1.86 (3) | 2.697 (2) | 170 (3) |
O8—H28···O1xiv | 0.85 (3) | 2.84 (3) | 3.360 (2) | 121 (3) |
O8—H28···O2xiv | 0.85 (3) | 1.90 (3) | 2.748 (2) | 173 (3) |
O9—H19···O2vii | 0.80 (3) | 2.55 (3) | 3.122 (2) | 130 (3) |
O9—H19···O3v | 0.80 (3) | 2.60 (3) | 3.162 (2) | 128 (3) |
O9—H19···O6v | 0.80 (3) | 2.44 (3) | 3.128 (2) | 145 (3) |
O9—H29···O4iii | 0.87 (3) | 1.93 (3) | 2.799 (3) | 171 (3) |
O10—H110···O1i | 0.82 (3) | 1.90 (3) | 2.721 (2) | 175 (3) |
O10—H210···O9xiv | 0.86 (3) | 1.89 (3) | 2.754 (3) | 174 (3) |
Symmetry codes: (i) −x, −y, z; (ii) x, y, z−1; (iii) −x, −y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vii) −x+1/2, y−1/2, −z; (xi) −x+1/2, y+1/2, −z+1; (xiv) x, y, z+1; (xvi) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (225K_anh)
top
Crystal data top
C4H12KNaO10 | Dx = 1.794 Mg m−3 |
Mr = 282.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 7210 reflections |
a = 11.8339 (7) Å | θ = 3.6–29.1° |
b = 14.2248 (10) Å | µ = 0.59 mm−1 |
c = 6.2075 (4) Å | T = 225 K |
V = 1044.95 (11) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 585.519 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2683 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2296 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.054 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −18→19 |
Tmin = 0.813, Tmax = 1.000 | l = −8→8 |
18297 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.033 | w = 1/[σ2(Fo2) + (0.0191P)2 + 0.4812P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.068 | (Δ/σ)max = −0.0001 |
S = 1.09 | Δρmax = 0.34 e Å−3 |
2683 reflections | Δρmin = −0.29 e Å−3 |
195 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
1 restraint | Absolute structure parameter: 0.02 (2) |
12 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0 | 0.0 | 0.0447 (3) | 0.0464 (6) | |
K2 | 0.5 | 0.0 | −0.15996 (10) | 0.02742 (16) | |
Na | 0.23198 (6) | −0.00678 (6) | 0.51893 (12) | 0.02257 (18) | |
O1 | 0.12022 (12) | 0.10904 (10) | 0.3487 (2) | 0.0217 (3) | |
O2 | 0.21106 (13) | 0.20321 (10) | 0.1184 (2) | 0.0256 (3) | |
O3 | 0.23056 (14) | 0.40678 (11) | 0.8164 (2) | 0.0308 (4) | |
O4 | 0.05075 (13) | 0.36049 (11) | 0.8464 (3) | 0.0290 (4) | |
O5 | 0.16440 (13) | 0.35756 (10) | 0.3243 (2) | 0.0222 (3) | |
H5 | 0.191 (2) | 0.3412 (18) | 0.216 (5) | 0.0334 (5)* | |
O6 | 0.29562 (13) | 0.24833 (11) | 0.6309 (3) | 0.0242 (3) | |
H6 | 0.326 (2) | 0.2911 (18) | 0.596 (5) | 0.0364 (5)* | |
O7 | 0.39599 (13) | 0.08277 (12) | 0.4853 (3) | 0.0277 (4) | |
H17 | 0.368 (2) | 0.132 (2) | 0.524 (5) | 0.0415 (5)* | |
H27 | 0.432 (2) | 0.094 (2) | 0.376 (5) | 0.0415 (5)* | |
O8 | 0.24058 (19) | 0.04148 (13) | 0.8821 (3) | 0.0402 (5) | |
H18 | 0.256 (3) | 0.003 (3) | 0.980 (5) | 0.0603 (7)* | |
H28 | 0.233 (3) | 0.093 (3) | 0.945 (5) | 0.0603 (7)* | |
O9 | 0.06010 (16) | −0.19468 (16) | −0.0333 (3) | 0.0423 (5) | |
H19 | 0.116 (3) | −0.209 (3) | 0.022 (6) | 0.0635 (7)* | |
H29 | 0.033 (3) | −0.253 (3) | −0.076 (5) | 0.0635 (7)* | |
O10 | 0.07703 (15) | −0.10474 (14) | 0.5747 (4) | 0.0410 (5) | |
H110 | 0.016 (3) | −0.104 (2) | 0.515 (5) | 0.0615 (7)* | |
H210 | 0.068 (3) | −0.136 (2) | 0.697 (6) | 0.0615 (7)* | |
C1 | 0.15477 (17) | 0.18783 (14) | 0.2835 (3) | 0.0175 (4) | |
C2 | 0.12525 (17) | 0.27350 (14) | 0.4229 (3) | 0.0179 (4) | |
H2 | 0.0399 (19) | 0.2789 (16) | 0.435 (3) | 0.0215 (5)* | |
C3 | 0.17758 (17) | 0.26360 (14) | 0.6464 (3) | 0.0187 (4) | |
H3 | 0.1462 (19) | 0.2079 (17) | 0.726 (4) | 0.0224 (5)* | |
C4 | 0.1508 (2) | 0.35089 (15) | 0.7822 (3) | 0.0224 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0544 (12) | 0.0455 (13) | 0.0393 (12) | −0.0248 (11) | −0.000000 | 0.000000 |
K2 | 0.0276 (3) | 0.0305 (3) | 0.0241 (3) | −0.0037 (3) | −0.000000 | 0.000000 |
Na | 0.0218 (4) | 0.0209 (4) | 0.0250 (4) | −0.0005 (3) | −0.0010 (3) | 0.0004 (4) |
O1 | 0.0234 (7) | 0.0186 (7) | 0.0231 (7) | −0.0014 (6) | −0.0016 (6) | −0.0010 (6) |
O2 | 0.0314 (8) | 0.0238 (8) | 0.0217 (8) | 0.0000 (7) | 0.0049 (7) | −0.0019 (6) |
O3 | 0.0414 (9) | 0.0233 (8) | 0.0276 (8) | −0.0066 (7) | −0.0028 (8) | −0.0047 (7) |
O4 | 0.0296 (8) | 0.0348 (9) | 0.0226 (8) | 0.0101 (7) | 0.0005 (7) | −0.0057 (7) |
O5 | 0.0323 (9) | 0.0177 (7) | 0.0168 (7) | 0.0006 (6) | 0.0002 (7) | −0.0004 (6) |
O6 | 0.0214 (8) | 0.0229 (8) | 0.0285 (8) | 0.0029 (6) | −0.0024 (7) | 0.0004 (7) |
O7 | 0.0246 (8) | 0.0247 (9) | 0.0337 (9) | −0.0003 (6) | 0.0052 (7) | 0.0030 (7) |
O8 | 0.0770 (14) | 0.0233 (8) | 0.0203 (9) | 0.0095 (9) | 0.0034 (9) | 0.0003 (7) |
O9 | 0.0281 (9) | 0.0610 (13) | 0.0379 (11) | −0.0033 (9) | −0.0075 (8) | 0.0046 (10) |
O10 | 0.0252 (8) | 0.0443 (11) | 0.0535 (12) | −0.0098 (8) | −0.0089 (8) | 0.0172 (9) |
C1 | 0.0167 (10) | 0.0181 (10) | 0.0175 (10) | 0.0020 (8) | −0.0039 (8) | −0.0009 (8) |
C2 | 0.0204 (10) | 0.0149 (10) | 0.0184 (9) | 0.0016 (8) | −0.0002 (8) | −0.0002 (8) |
C3 | 0.0211 (10) | 0.0165 (10) | 0.0185 (10) | 0.0016 (8) | 0.0014 (8) | −0.0001 (8) |
C4 | 0.0325 (12) | 0.0196 (10) | 0.0150 (10) | 0.0027 (9) | −0.0031 (9) | 0.0016 (8) |
Geometric parameters (Å, º) top
K1—O1 | 2.8269 (18) | Na—O7 | 2.3310 (17) |
K1—O1i | 2.8269 (18) | Na—O8 | 2.3586 (18) |
K1—O8ii | 3.078 (2) | Na—O10 | 2.3289 (19) |
K1—O8iii | 3.078 (2) | Na—C4v | 3.085 (2) |
K1—H18iii | 3.06 (3) | O1—C1 | 1.260 (2) |
K1—H18ii | 3.06 (3) | O2—C1 | 1.242 (2) |
K1—O9i | 2.900 (2) | O3—C4 | 1.252 (3) |
K1—O9 | 2.900 (2) | O4—C4 | 1.257 (3) |
K1—O10ii | 3.400 (3) | O5—H5 | 0.78 (3) |
K1—O10iii | 3.400 (3) | O5—C2 | 1.421 (3) |
K1—H210ii | 3.01 (3) | O6—H6 | 0.74 (2) |
K1—H210iii | 3.01 (3) | O6—C3 | 1.417 (2) |
K2—O4iv | 2.8440 (16) | O7—H17 | 0.81 (3) |
K2—O4v | 2.8440 (16) | O7—H27 | 0.82 (3) |
K2—O5vi | 2.9885 (15) | O8—H18 | 0.84 (4) |
K2—O5vii | 2.9885 (15) | O8—H28 | 0.84 (4) |
K2—O7iii | 2.7840 (18) | O9—H19 | 0.77 (4) |
K2—O7viii | 2.7840 (18) | O9—H29 | 0.92 (4) |
K2—O8iii | 3.137 (2) | O10—H110 | 0.81 (3) |
K2—O8viii | 3.137 (2) | O10—H210 | 0.89 (4) |
K2—H18viii | 3.02 (3) | C1—C2 | 1.535 (3) |
K2—H18iii | 3.02 (3) | C2—H2 | 1.02 (2) |
Na—O1 | 2.3623 (17) | C2—C3 | 1.526 (3) |
Na—O3v | 2.4581 (18) | C3—H3 | 1.00 (2) |
Na—O5v | 2.4848 (17) | C3—C4 | 1.534 (3) |
| | | |
Naii—K1—Naiii | 80.17 (4) | O8viii—K2—O5vi | 122.54 (5) |
O1—K1—Naii | 145.31 (3) | O8iii—K2—O5vi | 61.24 (4) |
O1i—K1—Naiii | 145.31 (3) | O8viii—K2—O5vii | 61.24 (4) |
O1—K1—Naiii | 101.50 (3) | O8iii—K2—O7iii | 63.49 (5) |
O1i—K1—Naii | 101.50 (3) | O8viii—K2—O7viii | 63.49 (5) |
O1i—K1—O1 | 96.24 (8) | O8iii—K2—O7viii | 125.31 (5) |
O8ii—K1—Naiii | 109.87 (6) | O8viii—K2—O7iii | 125.31 (5) |
O8ii—K1—Naii | 32.66 (4) | O8viii—K2—O8iii | 170.46 (6) |
O8iii—K1—Naii | 109.87 (6) | H18iii—K2—Naviii | 164.5 (6) |
O8iii—K1—Naiii | 32.66 (4) | H18viii—K2—Naviii | 49.0 (6) |
O8ii—K1—O1 | 142.16 (5) | H18iii—K2—Naiii | 49.0 (6) |
O8iii—K1—O1i | 142.16 (5) | H18viii—K2—Naiii | 164.5 (6) |
O8iii—K1—O1 | 69.41 (4) | H18iii—K2—O4iv | 89.6 (7) |
O8ii—K1—O1i | 69.41 (4) | H18viii—K2—O4v | 89.6 (7) |
O8ii—K1—O8iii | 141.70 (9) | H18iii—K2—O4v | 67.1 (7) |
H18iii—K1—Naii | 122.5 (6) | H18viii—K2—O4iv | 67.1 (7) |
H18ii—K1—Naii | 42.5 (6) | H18iii—K2—O5vi | 59.1 (7) |
H18iii—K1—Naiii | 42.5 (6) | H18viii—K2—O5vi | 135.3 (7) |
H18ii—K1—Naiii | 122.5 (6) | H18viii—K2—O5vii | 59.1 (7) |
H18iii—K1—O1i | 126.5 (7) | H18iii—K2—O5vii | 135.3 (7) |
H18ii—K1—O1i | 65.2 (6) | H18iii—K2—O7iii | 78.4 (7) |
H18ii—K1—O1 | 126.5 (7) | H18viii—K2—O7viii | 78.4 (7) |
H18iii—K1—O1 | 65.2 (6) | H18iii—K2—O7viii | 131.2 (6) |
H18ii—K1—O8ii | 15.7 (7) | H18viii—K2—O7iii | 131.2 (6) |
H18iii—K1—O8iii | 15.7 (7) | H18iii—K2—O8viii | 156.3 (7) |
H18ii—K1—O8iii | 151.3 (6) | H18viii—K2—O8viii | 15.5 (7) |
H18iii—K1—O8ii | 151.3 (6) | H18iii—K2—O8iii | 15.5 (7) |
H18ii—K1—H18iii | 165.0 (12) | H18viii—K2—O8iii | 156.3 (7) |
O9—K1—Naiii | 72.11 (5) | H18viii—K2—H18iii | 146.4 (12) |
O9i—K1—Naii | 72.11 (5) | K2ix—Na—K1x | 97.88 (2) |
O9—K1—Naii | 92.96 (5) | O1—Na—K1x | 88.06 (4) |
O9i—K1—Naiii | 92.96 (5) | O1—Na—K2ix | 133.93 (5) |
O9—K1—O1i | 73.20 (5) | O3v—Na—K1x | 140.84 (5) |
O9i—K1—O1 | 73.20 (5) | O3v—Na—K2ix | 108.11 (5) |
O9—K1—O1 | 120.80 (6) | O3v—Na—O1 | 94.07 (6) |
O9i—K1—O1i | 120.80 (6) | O5v—Na—K1x | 92.04 (4) |
O9—K1—O8iii | 84.34 (5) | O5v—Na—K2ix | 52.70 (4) |
O9i—K1—O8iii | 89.37 (5) | O5v—Na—O1 | 173.28 (6) |
O9—K1—O8ii | 89.37 (5) | O5v—Na—O3v | 81.62 (6) |
O9i—K1—O8ii | 84.34 (5) | O7—Na—K1x | 126.30 (5) |
O9—K1—H18iii | 75.5 (7) | O7—Na—K2ix | 47.84 (4) |
O9i—K1—H18ii | 75.5 (7) | O7—Na—O1 | 92.57 (6) |
O9—K1—H18ii | 101.9 (7) | O7—Na—O3v | 92.71 (7) |
O9i—K1—H18iii | 101.9 (7) | O7—Na—O5v | 92.78 (6) |
O9i—K1—O9 | 160.77 (11) | O8—Na—K1x | 44.76 (6) |
O10ii—K1—Naii | 32.98 (3) | O8—Na—K2ix | 56.47 (6) |
O10iii—K1—Naiii | 32.98 (3) | O8—Na—O1 | 104.39 (7) |
O10ii—K1—Naiii | 61.71 (4) | O8—Na—O3v | 161.31 (7) |
O10iii—K1—Naii | 61.71 (4) | O8—Na—O5v | 80.24 (6) |
O10iii—K1—O1i | 117.86 (5) | O8—Na—O7 | 83.72 (7) |
O10ii—K1—O1i | 132.71 (4) | O10—Na—K1x | 52.63 (6) |
O10ii—K1—O1 | 117.86 (5) | O10—Na—K2ix | 127.06 (6) |
O10iii—K1—O1 | 132.71 (4) | O10—Na—O1 | 92.47 (7) |
O10iii—K1—O8ii | 83.25 (6) | O10—Na—O3v | 88.21 (8) |
O10iii—K1—O8iii | 63.55 (5) | O10—Na—O5v | 82.28 (7) |
O10ii—K1—O8iii | 83.25 (6) | O10—Na—O7 | 174.80 (8) |
O10ii—K1—O8ii | 63.55 (5) | O10—Na—O8 | 93.78 (8) |
O10iii—K1—H18iii | 68.2 (6) | C4v—Na—K1x | 140.15 (5) |
O10ii—K1—H18ii | 68.2 (6) | C4v—Na—K2ix | 87.63 (5) |
O10iii—K1—H18ii | 98.4 (6) | C4v—Na—O1 | 116.01 (6) |
O10ii—K1—H18iii | 98.4 (6) | C4v—Na—O3v | 22.70 (5) |
O10iii—K1—O9 | 51.13 (6) | C4v—Na—O5v | 60.38 (5) |
O10ii—K1—O9i | 51.13 (6) | C4v—Na—O7 | 85.99 (7) |
O10iii—K1—O9i | 109.93 (7) | C4v—Na—O8 | 138.65 (7) |
O10ii—K1—O9 | 109.93 (7) | C4v—Na—O10 | 92.95 (7) |
O10ii—K1—O10iii | 61.82 (7) | Na—O1—K1 | 101.40 (5) |
H210iii—K1—Naii | 68.9 (7) | C1—O1—K1 | 115.91 (13) |
H210ii—K1—Naii | 42.7 (6) | C1—O1—Na | 125.63 (12) |
H210iii—K1—Naiii | 42.7 (6) | C4—O3—Naxi | 108.03 (13) |
H210ii—K1—Naiii | 68.9 (7) | C4—O4—K2xii | 119.46 (14) |
H210ii—K1—O1i | 134.2 (6) | Naxi—O5—K2xiii | 85.90 (5) |
H210iii—K1—O1 | 134.2 (6) | H5—O5—K2xiii | 100 (2) |
H210ii—K1—O1 | 105.0 (7) | H5—O5—Naxi | 112 (2) |
H210iii—K1—O1i | 105.0 (7) | C2—O5—K2xiii | 120.35 (11) |
H210iii—K1—O8ii | 83.7 (6) | C2—O5—Naxi | 130.23 (12) |
H210ii—K1—O8ii | 68.9 (6) | C2—O5—H5 | 105 (2) |
H210iii—K1—O8iii | 68.9 (6) | C3—O6—H6 | 112 (2) |
H210ii—K1—O8iii | 83.7 (6) | Na—O7—K2xiv | 93.79 (6) |
H210ii—K1—H18ii | 69.5 (9) | H17—O7—K2xiv | 108 (2) |
H210iii—K1—H18iii | 69.5 (9) | H17—O7—Na | 96 (2) |
H210ii—K1—H18iii | 99.3 (9) | H27—O7—K2xiv | 121 (2) |
H210iii—K1—H18ii | 99.3 (9) | H27—O7—Na | 128 (2) |
H210iii—K1—O9i | 124.2 (7) | H27—O7—H17 | 107 (3) |
H210ii—K1—O9i | 36.8 (7) | K2xiv—O8—K1xiv | 153.69 (7) |
H210iii—K1—O9 | 36.8 (7) | Na—O8—K1xiv | 102.58 (8) |
H210ii—K1—O9 | 124.2 (7) | Na—O8—K2xiv | 84.72 (6) |
H210iii—K1—O10ii | 74.9 (7) | H18—O8—K1xiv | 81 (2) |
H210iii—K1—O10iii | 14.4 (7) | H18—O8—K2xiv | 74 (2) |
H210ii—K1—O10iii | 74.9 (7) | H18—O8—Na | 121 (2) |
H210ii—K1—O10ii | 14.4 (7) | H28—O8—K1xiv | 85 (2) |
H210ii—K1—H210iii | 88.5 (14) | H28—O8—K2xiv | 108 (2) |
Naviii—K2—Naiii | 115.73 (3) | H28—O8—Na | 134 (2) |
O4v—K2—Naviii | 124.11 (4) | H28—O8—H18 | 105 (3) |
O4iv—K2—Naviii | 99.63 (3) | K2xiv—H18—K1xiv | 170.6 (12) |
O4iv—K2—Naiii | 124.11 (4) | O8—H18—K1xiv | 84 (2) |
O4v—K2—Naiii | 99.63 (3) | O8—H18—K2xiv | 90 (2) |
O4v—K2—O4iv | 93.61 (7) | H19—O9—K1i | 112 (3) |
O5vi—K2—Naiii | 41.40 (3) | H29—O9—K1i | 145 (2) |
O5vi—K2—Naviii | 112.76 (4) | H29—O9—H19 | 101 (3) |
O5vii—K2—Naviii | 41.40 (3) | Na—O10—K1x | 94.39 (7) |
O5vii—K2—Naiii | 112.76 (4) | H110—O10—K1x | 99 (2) |
O5vi—K2—O4v | 67.86 (4) | H110—O10—Na | 129 (2) |
O5vi—K2—O4iv | 147.59 (5) | H210—O10—K1x | 57 (2) |
O5vii—K2—O4v | 147.59 (5) | H210—O10—Na | 121 (2) |
O5vii—K2—O4iv | 67.86 (4) | H210—O10—H110 | 107 (3) |
O5vi—K2—O5vii | 140.08 (7) | O10—H210—K1x | 108 (2) |
O7iii—K2—Naiii | 38.37 (3) | O2—C1—O1 | 126.6 (2) |
O7viii—K2—Naiii | 86.71 (4) | C2—C1—O1 | 116.83 (18) |
O7iii—K2—Naviii | 86.71 (4) | C2—C1—O2 | 116.58 (18) |
O7viii—K2—Naviii | 38.37 (3) | C1—C2—O5 | 110.57 (16) |
O7iii—K2—O4iv | 109.86 (5) | H2—C2—O5 | 106.9 (13) |
O7iii—K2—O4v | 138.00 (5) | H2—C2—C1 | 109.1 (13) |
O7viii—K2—O4iv | 138.00 (5) | C3—C2—O5 | 109.68 (16) |
O7viii—K2—O4v | 109.86 (5) | C3—C2—C1 | 110.30 (16) |
O7iii—K2—O5vi | 74.27 (5) | C3—C2—H2 | 110.2 (12) |
O7viii—K2—O5vii | 74.27 (5) | C2—C3—O6 | 110.66 (17) |
O7iii—K2—O5vii | 74.40 (5) | H3—C3—O6 | 106.1 (13) |
O7viii—K2—O5vi | 74.40 (5) | H3—C3—C2 | 111.6 (13) |
O7viii—K2—O7iii | 75.44 (7) | C4—C3—O6 | 111.40 (17) |
O8iii—K2—Naviii | 150.19 (4) | C4—C3—C2 | 109.95 (16) |
O8viii—K2—Naviii | 38.81 (3) | C4—C3—H3 | 107.1 (13) |
O8iii—K2—Naiii | 38.81 (3) | O3—C4—Naxi | 49.26 (11) |
O8viii—K2—Naiii | 150.19 (4) | O4—C4—Naxi | 122.99 (15) |
O8iii—K2—O4iv | 91.06 (5) | O4—C4—O3 | 126.0 (2) |
O8viii—K2—O4v | 91.06 (5) | C3—C4—Naxi | 96.06 (12) |
O8iii—K2—O4v | 82.40 (5) | C3—C4—O3 | 116.9 (2) |
O8viii—K2—O4iv | 82.40 (5) | C3—C4—O4 | 117.17 (19) |
O8iii—K2—O5vii | 122.54 (5) | | |
| | | |
K1—O1—C1—O2 | −51.98 (14) | Naxi—O3—C4—C3 | 73.73 (13) |
K1i—O1—C1—O2 | −51.98 (14) | Naxi—O5—C2—C1 | −134.18 (16) |
K1—O1—C1—C2 | 128.55 (12) | Naxi—O5—C2—C3 | −12.33 (15) |
K1i—O1—C1—C2 | 128.55 (12) | Naxi—C4—C3—O6 | 62.88 (12) |
K2xii—O4—C4—Naxi | −72.79 (12) | Naxi—C4—C3—C2 | −60.17 (12) |
K2—O4v—C4v—Na | −72.79 (12) | O1—C1—C2—O5 | −176.99 (18) |
K2xii—O4—C4—O3 | −12.15 (16) | O1—C1—C2—C3 | 61.52 (19) |
K2xi—O4—C4—O3 | −12.15 (16) | O2—C1—C2—O5 | 3.49 (19) |
K2xii—O4—C4—C3 | 168.87 (13) | O2—C1—C2—C3 | −118.00 (19) |
K2xi—O4—C4—C3 | 168.87 (13) | O3—C4—C3—O6 | 15.9 (2) |
K2xv—O5—C2—C1 | 113.07 (13) | O3—C4—C3—C2 | −107.2 (2) |
K2xiii—O5—C2—C1 | 113.07 (13) | O4—C4—C3—O6 | −165.06 (19) |
K2xiii—O5—C2—C3 | −125.08 (13) | O4—C4—C3—C2 | 71.9 (2) |
K2xv—O5—C2—C3 | −125.08 (13) | O5—C2—C3—O6 | −67.28 (17) |
Na—O1—C1—O2 | 76.22 (16) | O5—C2—C3—C4 | 56.20 (18) |
Na—O1—C1—C2 | −103.25 (15) | O6—C3—C2—C1 | 54.74 (18) |
Naxi—O3—C4—O4 | −105.24 (14) | C1—C2—C3—C4 | 178.22 (16) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (vii) x+1/2, −y+1/2, −z; (viii) −x+1, −y, z−1; (ix) −x+1, −y, z+1; (x) −x, −y, z+1; (xi) −x+1/2, y+1/2, −z+1; (xii) x−1/2, −y+1/2, −z+1; (xiii) x−1/2, −y+1/2, −z; (xiv) x, y, z+1; (xv) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.78 (3) | 2.07 (3) | 2.600 (2) | 126 (2) |
O5—H5···O3iii | 0.78 (3) | 2.69 (3) | 3.323 (2) | 140 (2) |
O5—H5···O4iii | 0.78 (3) | 2.85 (3) | 3.258 (2) | 115 (2) |
O6—H6···O10xi | 0.74 (2) | 2.16 (2) | 2.876 (3) | 166 (3) |
O7—H17···O6 | 0.81 (3) | 1.98 (3) | 2.788 (2) | 177 (3) |
O7—H27···O4iv | 0.82 (3) | 2.07 (3) | 2.871 (2) | 165 (3) |
O8—H18···O3xvi | 0.84 (4) | 1.87 (4) | 2.700 (2) | 170 (3) |
O8—H28···O1xiv | 0.84 (4) | 2.85 (3) | 3.368 (2) | 122 (3) |
O8—H28···O2xiv | 0.84 (4) | 1.92 (4) | 2.751 (2) | 173 (3) |
O9—H19···O2vi | 0.77 (4) | 2.55 (4) | 3.118 (3) | 131 (3) |
O9—H19···O3v | 0.77 (4) | 2.64 (4) | 3.168 (3) | 127 (3) |
O9—H19···O6v | 0.77 (4) | 2.47 (4) | 3.132 (2) | 145 (3) |
O9—H29···O4ii | 0.92 (4) | 1.89 (4) | 2.800 (3) | 169 (3) |
O10—H110···O1i | 0.81 (3) | 1.92 (3) | 2.724 (2) | 174 (3) |
O10—H210···O9xiv | 0.89 (4) | 1.87 (4) | 2.756 (3) | 174 (3) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (xi) −x+1/2, y+1/2, −z+1; (xiv) x, y, z+1; (xvi) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (243K_anh)
top
Crystal data top
C4H12KNaO10 | Dx = 1.790 Mg m−3 |
Mr = 282.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 6951 reflections |
a = 11.8443 (8) Å | θ = 3.6–28.8° |
b = 14.2331 (10) Å | µ = 0.59 mm−1 |
c = 6.2124 (4) Å | T = 243 K |
V = 1047.29 (12) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 585.519 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2687 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2274 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.054 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.5°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −18→19 |
Tmin = 0.811, Tmax = 1.000 | l = −8→8 |
18296 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.035 | w = 1/[σ2(Fo2) + (0.0207P)2 + 0.4837P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.071 | (Δ/σ)max = −0.0005 |
S = 1.08 | Δρmax = 0.34 e Å−3 |
2687 reflections | Δρmin = −0.29 e Å−3 |
195 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
1 restraint | Absolute structure parameter: 0.05 (2) |
12 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0 | 0.0 | 0.0451 (3) | 0.0500 (6) | |
K2 | 0.5 | 0.0 | −0.15966 (11) | 0.02969 (17) | |
Na | 0.23187 (7) | −0.00679 (7) | 0.51990 (13) | 0.02440 (19) | |
O1 | 0.12024 (12) | 0.10902 (10) | 0.3492 (3) | 0.0233 (3) | |
O2 | 0.21069 (14) | 0.20309 (11) | 0.1184 (2) | 0.0274 (4) | |
O3 | 0.23130 (15) | 0.40654 (11) | 0.8157 (3) | 0.0329 (4) | |
O4 | 0.05150 (14) | 0.36101 (12) | 0.8458 (3) | 0.0313 (4) | |
O5 | 0.16404 (14) | 0.35750 (11) | 0.3243 (3) | 0.0242 (3) | |
H5 | 0.192 (2) | 0.3414 (19) | 0.216 (5) | 0.0363 (5)* | |
O6 | 0.29559 (13) | 0.24821 (11) | 0.6299 (3) | 0.0264 (4) | |
H6 | 0.325 (2) | 0.2918 (19) | 0.603 (5) | 0.0396 (5)* | |
O7 | 0.39591 (14) | 0.08259 (12) | 0.4849 (3) | 0.0300 (4) | |
H17 | 0.372 (3) | 0.131 (2) | 0.522 (5) | 0.0451 (6)* | |
H27 | 0.432 (2) | 0.093 (2) | 0.374 (5) | 0.0451 (6)* | |
O8 | 0.24132 (19) | 0.04137 (14) | 0.8827 (3) | 0.0423 (5) | |
H18 | 0.257 (3) | 0.003 (3) | 0.982 (5) | 0.0634 (8)* | |
H28 | 0.235 (3) | 0.095 (3) | 0.948 (5) | 0.0634 (8)* | |
O9 | 0.06040 (16) | −0.19537 (17) | −0.0337 (4) | 0.0470 (5) | |
H19 | 0.117 (3) | −0.213 (3) | 0.020 (6) | 0.0705 (8)* | |
H29 | 0.032 (3) | −0.253 (3) | −0.082 (5) | 0.0705 (8)* | |
O10 | 0.07659 (16) | −0.10432 (15) | 0.5760 (4) | 0.0457 (5) | |
H110 | 0.016 (3) | −0.105 (3) | 0.517 (5) | 0.0685 (8)* | |
H210 | 0.068 (3) | −0.135 (3) | 0.697 (6) | 0.0685 (8)* | |
C1 | 0.15470 (18) | 0.18783 (15) | 0.2835 (3) | 0.0195 (4) | |
C2 | 0.12510 (18) | 0.27339 (15) | 0.4227 (3) | 0.0193 (4) | |
H2 | 0.0398 (19) | 0.2778 (17) | 0.436 (4) | 0.0231 (5)* | |
C3 | 0.17773 (17) | 0.26371 (15) | 0.6463 (4) | 0.0203 (4) | |
H3 | 0.147 (2) | 0.2090 (18) | 0.723 (4) | 0.0244 (5)* | |
C4 | 0.1515 (2) | 0.35106 (16) | 0.7811 (3) | 0.0240 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0580 (13) | 0.0491 (14) | 0.0429 (13) | −0.0267 (12) | −0.000000 | 0.000000 |
K2 | 0.0296 (3) | 0.0331 (4) | 0.0263 (3) | −0.0038 (3) | −0.000000 | 0.000000 |
Na | 0.0235 (4) | 0.0227 (4) | 0.0270 (4) | −0.0009 (4) | −0.0008 (3) | 0.0007 (4) |
O1 | 0.0257 (8) | 0.0190 (7) | 0.0252 (8) | −0.0005 (6) | −0.0013 (7) | −0.0011 (7) |
O2 | 0.0357 (9) | 0.0247 (8) | 0.0218 (8) | 0.0008 (7) | 0.0060 (7) | −0.0017 (6) |
O3 | 0.0431 (10) | 0.0260 (8) | 0.0298 (9) | −0.0072 (7) | −0.0034 (8) | −0.0057 (7) |
O4 | 0.0320 (8) | 0.0370 (9) | 0.0249 (8) | 0.0104 (7) | 0.0010 (7) | −0.0058 (8) |
O5 | 0.0350 (9) | 0.0185 (8) | 0.0190 (8) | −0.0005 (6) | 0.0007 (7) | 0.0005 (6) |
O6 | 0.0231 (8) | 0.0234 (8) | 0.0328 (9) | 0.0033 (6) | −0.0039 (7) | −0.0004 (7) |
O7 | 0.0265 (9) | 0.0265 (9) | 0.0372 (10) | −0.0011 (7) | 0.0058 (8) | 0.0013 (8) |
O8 | 0.0792 (15) | 0.0247 (9) | 0.0229 (9) | 0.0094 (10) | 0.0036 (10) | 0.0008 (7) |
O9 | 0.0299 (10) | 0.0697 (15) | 0.0413 (12) | −0.0051 (10) | −0.0090 (9) | 0.0054 (11) |
O10 | 0.0279 (9) | 0.0492 (12) | 0.0599 (14) | −0.0119 (9) | −0.0111 (9) | 0.0218 (10) |
C1 | 0.0192 (10) | 0.0196 (11) | 0.0198 (10) | 0.0017 (8) | −0.0050 (8) | −0.0010 (8) |
C2 | 0.0220 (10) | 0.0166 (10) | 0.0191 (10) | 0.0007 (8) | −0.0013 (9) | −0.0009 (8) |
C3 | 0.0216 (10) | 0.0190 (10) | 0.0204 (10) | 0.0016 (8) | 0.0012 (9) | 0.0024 (9) |
C4 | 0.0347 (13) | 0.0218 (11) | 0.0156 (10) | 0.0040 (10) | −0.0039 (9) | 0.0003 (8) |
Geometric parameters (Å, º) top
K1—O1 | 2.8293 (19) | Na—O7 | 2.3325 (18) |
K1—O1i | 2.8293 (19) | Na—O8 | 2.3586 (19) |
K1—O8ii | 3.088 (2) | Na—O10 | 2.330 (2) |
K1—O8iii | 3.088 (2) | Na—C4v | 3.082 (2) |
K1—H18ii | 3.07 (3) | O1—C1 | 1.261 (3) |
K1—H18iii | 3.07 (3) | O2—C1 | 1.241 (3) |
K1—O9i | 2.913 (3) | O3—C4 | 1.250 (3) |
K1—O9 | 2.913 (3) | O4—C4 | 1.259 (3) |
K1—O10ii | 3.394 (3) | O5—H5 | 0.78 (3) |
K1—O10iii | 3.394 (3) | O5—C2 | 1.421 (3) |
K1—H210iii | 3.01 (3) | O6—H6 | 0.73 (2) |
K1—H210ii | 3.01 (3) | O6—C3 | 1.417 (3) |
K2—O4iv | 2.8438 (17) | O7—H17 | 0.78 (3) |
K2—O4v | 2.8438 (17) | O7—H27 | 0.82 (3) |
K2—O5vi | 2.9890 (16) | O8—H18 | 0.84 (4) |
K2—O5vii | 2.9890 (16) | O8—H28 | 0.87 (4) |
K2—O7ii | 2.7890 (19) | O9—H19 | 0.78 (4) |
K2—O7viii | 2.7890 (19) | O9—H29 | 0.93 (4) |
K2—O8ii | 3.131 (2) | O10—H110 | 0.80 (4) |
K2—O8viii | 3.131 (2) | O10—H210 | 0.88 (4) |
K2—H18ii | 3.01 (3) | C1—C2 | 1.534 (3) |
K2—H18viii | 3.01 (3) | C2—H2 | 1.02 (2) |
Na—O1 | 2.3643 (17) | C2—C3 | 1.529 (3) |
Na—O3v | 2.4612 (19) | C3—H3 | 0.98 (3) |
Na—O5v | 2.4876 (18) | C3—C4 | 1.531 (3) |
| | | |
Naiii—K1—Naii | 80.22 (4) | O8ii—K2—O5vi | 122.50 (5) |
O1—K1—Naii | 101.48 (3) | O8ii—K2—O5vii | 61.33 (5) |
O1—K1—Naiii | 145.32 (3) | O8viii—K2—O5vii | 122.50 (5) |
O1i—K1—Naii | 145.32 (3) | O8ii—K2—O7ii | 63.56 (5) |
O1i—K1—Naiii | 101.48 (3) | O8ii—K2—O7viii | 125.34 (5) |
O1i—K1—O1 | 96.22 (8) | O8viii—K2—O7viii | 63.56 (5) |
O8iii—K1—Naiii | 32.70 (4) | O8viii—K2—O7ii | 125.34 (5) |
O8ii—K1—Naii | 32.70 (4) | O8viii—K2—O8ii | 170.35 (7) |
O8iii—K1—Naii | 109.99 (6) | H18viii—K2—Naviii | 49.2 (6) |
O8ii—K1—Naiii | 109.99 (6) | H18viii—K2—Naii | 164.8 (7) |
O8iii—K1—O1 | 142.06 (6) | H18ii—K2—Naviii | 164.8 (7) |
O8ii—K1—O1 | 69.36 (5) | H18ii—K2—Naii | 49.2 (6) |
O8ii—K1—O1i | 142.06 (6) | H18ii—K2—O4iv | 89.6 (7) |
O8iii—K1—O1i | 69.36 (5) | H18ii—K2—O4v | 66.7 (7) |
O8iii—K1—O8ii | 141.87 (9) | H18viii—K2—O4v | 89.6 (7) |
H18ii—K1—Naii | 42.7 (6) | H18viii—K2—O4iv | 66.7 (7) |
H18iii—K1—Naii | 122.7 (6) | H18ii—K2—O5vii | 59.3 (7) |
H18iii—K1—Naiii | 42.7 (6) | H18ii—K2—O5vi | 135.3 (8) |
H18ii—K1—Naiii | 122.7 (6) | H18viii—K2—O5vi | 59.3 (7) |
H18ii—K1—O1i | 126.3 (7) | H18viii—K2—O5vii | 135.3 (8) |
H18iii—K1—O1 | 126.3 (7) | H18ii—K2—O7ii | 78.6 (7) |
H18iii—K1—O1i | 65.0 (7) | H18ii—K2—O7viii | 131.4 (7) |
H18ii—K1—O1 | 65.0 (7) | H18viii—K2—O7viii | 78.6 (7) |
H18iii—K1—O8iii | 15.7 (7) | H18viii—K2—O7ii | 131.4 (7) |
H18ii—K1—O8iii | 151.6 (6) | H18ii—K2—O8viii | 156.0 (7) |
H18iii—K1—O8ii | 151.6 (6) | H18ii—K2—O8ii | 15.6 (7) |
H18ii—K1—O8ii | 15.7 (7) | H18viii—K2—O8ii | 156.0 (7) |
H18iii—K1—H18ii | 165.4 (13) | H18viii—K2—O8viii | 15.6 (7) |
O9—K1—Naiii | 92.94 (6) | H18viii—K2—H18ii | 146.0 (13) |
O9—K1—Naii | 72.05 (5) | K2ix—Na—K1x | 97.97 (3) |
O9i—K1—Naiii | 72.05 (5) | O1—Na—K1x | 88.12 (4) |
O9i—K1—Naii | 92.94 (6) | O1—Na—K2ix | 133.94 (5) |
O9—K1—O1i | 73.27 (5) | O3v—Na—K1x | 140.65 (5) |
O9—K1—O1 | 120.80 (6) | O3v—Na—K2ix | 108.21 (5) |
O9i—K1—O1 | 73.27 (5) | O3v—Na—O1 | 93.93 (6) |
O9i—K1—O1i | 120.80 (6) | O5v—Na—K1x | 92.24 (5) |
O9—K1—O8ii | 84.25 (6) | O5v—Na—K2ix | 52.67 (4) |
O9—K1—O8iii | 89.46 (6) | O5v—Na—O1 | 173.25 (6) |
O9i—K1—O8ii | 89.46 (6) | O5v—Na—O3v | 81.52 (6) |
O9i—K1—O8iii | 84.25 (6) | O7—Na—K1x | 126.54 (6) |
O9—K1—H18ii | 75.5 (7) | O7—Na—K2ix | 47.93 (5) |
O9—K1—H18iii | 102.0 (7) | O7—Na—O1 | 92.51 (7) |
O9i—K1—H18iii | 75.5 (7) | O7—Na—O3v | 92.67 (7) |
O9i—K1—H18ii | 102.0 (7) | O7—Na—O5v | 92.69 (6) |
O9i—K1—O9 | 160.67 (12) | O8—Na—K1x | 45.01 (6) |
O10ii—K1—Naii | 33.00 (4) | O8—Na—K2ix | 56.28 (6) |
O10ii—K1—Naiii | 61.66 (4) | O8—Na—O1 | 104.64 (7) |
O10iii—K1—Naiii | 33.00 (4) | O8—Na—O3v | 161.20 (7) |
O10iii—K1—Naii | 61.66 (4) | O8—Na—O5v | 80.22 (7) |
O10ii—K1—O1i | 117.90 (5) | O8—Na—O7 | 83.75 (8) |
O10iii—K1—O1 | 117.90 (5) | O10—Na—K1x | 52.49 (6) |
O10iii—K1—O1i | 132.74 (5) | O10—Na—K2ix | 127.19 (6) |
O10ii—K1—O1 | 132.74 (5) | O10—Na—O1 | 92.35 (7) |
O10ii—K1—O8iii | 83.31 (6) | O10—Na—O3v | 88.16 (8) |
O10iii—K1—O8ii | 83.31 (6) | O10—Na—O5v | 82.56 (7) |
O10ii—K1—O8ii | 63.61 (5) | O10—Na—O7 | 175.00 (8) |
O10iii—K1—O8iii | 63.61 (5) | O10—Na—O8 | 93.89 (8) |
O10ii—K1—H18ii | 68.4 (6) | C4v—Na—K1x | 140.13 (5) |
O10ii—K1—H18iii | 98.6 (7) | C4v—Na—K2ix | 87.67 (5) |
O10iii—K1—H18iii | 68.4 (6) | C4v—Na—O1 | 115.86 (6) |
O10iii—K1—H18ii | 98.6 (7) | C4v—Na—O3v | 22.73 (6) |
O10ii—K1—O9 | 51.14 (6) | C4v—Na—O5v | 60.27 (6) |
O10ii—K1—O9i | 109.82 (8) | C4v—Na—O7 | 85.87 (7) |
O10iii—K1—O9i | 51.14 (6) | C4v—Na—O8 | 138.53 (7) |
O10iii—K1—O9 | 109.82 (8) | C4v—Na—O10 | 93.06 (8) |
O10iii—K1—O10ii | 61.68 (8) | Na—O1—K1 | 101.46 (6) |
H210iii—K1—Naiii | 42.5 (7) | C1—O1—K1 | 115.76 (14) |
H210iii—K1—Naii | 68.8 (7) | C1—O1—Na | 125.74 (13) |
H210ii—K1—Naiii | 68.8 (7) | C4—O3—Naxi | 107.76 (14) |
H210ii—K1—Naii | 42.5 (7) | C4—O4—K2xii | 119.94 (14) |
H210ii—K1—O1i | 105.3 (7) | Naxi—O5—K2xiii | 85.90 (5) |
H210iii—K1—O1i | 134.1 (7) | H5—O5—K2xiii | 100 (2) |
H210iii—K1—O1 | 105.3 (7) | H5—O5—Naxi | 111 (2) |
H210ii—K1—O1 | 134.1 (7) | C2—O5—K2xiii | 120.52 (12) |
H210iii—K1—O8ii | 83.8 (7) | C2—O5—Naxi | 130.37 (13) |
H210ii—K1—O8iii | 83.8 (7) | C2—O5—H5 | 105 (2) |
H210ii—K1—O8ii | 68.8 (7) | C3—O6—H6 | 111 (2) |
H210iii—K1—O8iii | 68.8 (7) | Na—O7—K2xiv | 93.70 (6) |
H210iii—K1—H18iii | 69.6 (9) | H17—O7—K2xiv | 107 (2) |
H210iii—K1—H18ii | 99.6 (10) | H17—O7—Na | 98 (2) |
H210ii—K1—H18ii | 69.6 (9) | H27—O7—K2xiv | 120 (2) |
H210ii—K1—H18iii | 99.6 (10) | H27—O7—Na | 127 (2) |
H210iii—K1—O9 | 123.9 (7) | H27—O7—H17 | 107 (3) |
H210ii—K1—O9i | 123.9 (7) | K2xiv—O8—K1xiv | 153.83 (7) |
H210ii—K1—O9 | 37.0 (7) | Na—O8—K1xiv | 102.29 (8) |
H210iii—K1—O9i | 37.0 (7) | Na—O8—K2xiv | 84.92 (6) |
H210ii—K1—O10iii | 74.6 (7) | H18—O8—K1xiv | 81 (2) |
H210iii—K1—O10iii | 14.2 (7) | H18—O8—K2xiv | 74 (2) |
H210ii—K1—O10ii | 14.2 (7) | H18—O8—Na | 122 (2) |
H210iii—K1—O10ii | 74.6 (7) | H28—O8—K1xiv | 86 (2) |
H210iii—K1—H210ii | 88.1 (15) | H28—O8—K2xiv | 107 (2) |
Naviii—K2—Naii | 115.86 (3) | H28—O8—Na | 134 (2) |
O4iv—K2—Naii | 124.31 (4) | H28—O8—H18 | 104 (3) |
O4v—K2—Naii | 99.46 (4) | K2xiv—H18—K1xiv | 170.1 (13) |
O4iv—K2—Naviii | 99.46 (4) | O8—H18—K1xiv | 83 (2) |
O4v—K2—Naviii | 124.31 (4) | O8—H18—K2xiv | 90 (2) |
O4v—K2—O4iv | 93.43 (7) | H19—O9—K1i | 116 (3) |
O5vi—K2—Naviii | 41.43 (3) | H29—O9—K1i | 143 (2) |
O5vi—K2—Naii | 112.73 (4) | H29—O9—H19 | 100 (4) |
O5vii—K2—Naviii | 112.73 (4) | Na—O10—K1x | 94.51 (8) |
O5vii—K2—Naii | 41.43 (3) | H110—O10—K1x | 99 (2) |
O5vii—K2—O4v | 67.86 (5) | H110—O10—Na | 130 (2) |
O5vi—K2—O4v | 147.78 (5) | H210—O10—K1x | 57 (2) |
O5vii—K2—O4iv | 147.78 (5) | H210—O10—Na | 121 (2) |
O5vi—K2—O4iv | 67.86 (5) | H210—O10—H110 | 106 (3) |
O5vii—K2—O5vi | 139.99 (7) | O10—H210—K1x | 109 (3) |
O7viii—K2—Naii | 86.74 (4) | O2—C1—O1 | 126.6 (2) |
O7viii—K2—Naviii | 38.37 (4) | C2—C1—O1 | 116.72 (19) |
O7ii—K2—Naii | 38.37 (4) | C2—C1—O2 | 116.69 (19) |
O7ii—K2—Naviii | 86.74 (4) | C1—C2—O5 | 110.62 (17) |
O7ii—K2—O4iv | 110.15 (5) | H2—C2—O5 | 107.8 (13) |
O7viii—K2—O4iv | 137.84 (5) | H2—C2—C1 | 108.8 (13) |
O7ii—K2—O4v | 137.84 (5) | C3—C2—O5 | 109.53 (17) |
O7viii—K2—O4v | 110.15 (5) | C3—C2—C1 | 110.33 (17) |
O7ii—K2—O5vii | 74.20 (5) | C3—C2—H2 | 109.7 (13) |
O7viii—K2—O5vii | 74.36 (5) | C2—C3—O6 | 110.50 (18) |
O7ii—K2—O5vi | 74.36 (5) | H3—C3—O6 | 105.8 (14) |
O7viii—K2—O5vi | 74.20 (5) | H3—C3—C2 | 111.2 (14) |
O7viii—K2—O7ii | 75.29 (8) | C4—C3—O6 | 111.46 (18) |
O8viii—K2—Naviii | 38.80 (3) | C4—C3—C2 | 109.93 (17) |
O8viii—K2—Naii | 150.31 (4) | C4—C3—H3 | 107.8 (14) |
O8ii—K2—Naviii | 150.31 (4) | O3—C4—Naxi | 49.51 (11) |
O8ii—K2—Naii | 38.80 (3) | O4—C4—Naxi | 122.80 (15) |
O8viii—K2—O4iv | 82.14 (5) | O4—C4—O3 | 125.8 (2) |
O8ii—K2—O4iv | 91.23 (5) | C3—C4—Naxi | 96.34 (13) |
O8ii—K2—O4v | 82.14 (5) | C3—C4—O3 | 117.0 (2) |
O8viii—K2—O4v | 91.23 (5) | C3—C4—O4 | 117.2 (2) |
O8viii—K2—O5vi | 61.33 (5) | | |
| | | |
K1—O1—C1—O2 | −51.92 (15) | Naxi—O3—C4—C3 | 74.26 (13) |
K1i—O1—C1—O2 | −51.92 (15) | Naxi—O5—C2—C1 | −133.88 (17) |
K1—O1—C1—C2 | 128.54 (13) | Naxi—O5—C2—C3 | −12.06 (15) |
K1i—O1—C1—C2 | 128.54 (13) | Naxi—C4—C3—O6 | 62.75 (13) |
K2xii—O4—C4—Naxi | −72.84 (13) | Naxi—C4—C3—C2 | −60.13 (13) |
K2—O4v—C4v—Na | −72.84 (13) | O1—C1—C2—O5 | −177.04 (18) |
K2xii—O4—C4—O3 | −12.01 (17) | O1—C1—C2—C3 | 61.6 (2) |
K2xi—O4—C4—O3 | −12.01 (17) | O2—C1—C2—O5 | 3.4 (2) |
K2xii—O4—C4—C3 | 168.54 (14) | O2—C1—C2—C3 | −118.0 (2) |
K2xi—O4—C4—C3 | 168.54 (14) | O3—C4—C3—O6 | 15.3 (2) |
K2xv—O5—C2—C1 | 113.04 (14) | O3—C4—C3—C2 | −107.6 (2) |
K2xiii—O5—C2—C1 | 113.04 (14) | O4—C4—C3—O6 | −165.2 (2) |
K2xiii—O5—C2—C3 | −125.13 (14) | O4—C4—C3—C2 | 71.9 (2) |
K2xv—O5—C2—C3 | −125.13 (14) | O5—C2—C3—O6 | −67.58 (17) |
Na—O1—C1—O2 | 76.32 (17) | O5—C2—C3—C4 | 55.86 (18) |
Na—O1—C1—C2 | −103.22 (16) | O6—C3—C2—C1 | 54.42 (19) |
Naxi—O3—C4—O4 | −105.20 (14) | C1—C2—C3—C4 | 177.86 (17) |
Symmetry codes: (i) −x, −y, z; (ii) x, y, z−1; (iii) −x, −y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) x+1/2, −y+1/2, −z; (vii) −x+1/2, y−1/2, −z; (viii) −x+1, −y, z−1; (ix) −x+1, −y, z+1; (x) −x, −y, z+1; (xi) −x+1/2, y+1/2, −z+1; (xii) x−1/2, −y+1/2, −z+1; (xiii) x−1/2, −y+1/2, −z; (xiv) x, y, z+1; (xv) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.78 (3) | 2.07 (3) | 2.602 (2) | 125 (3) |
O5—H5···O3ii | 0.78 (3) | 2.69 (3) | 3.333 (2) | 140 (2) |
O5—H5···O4ii | 0.78 (3) | 2.85 (3) | 3.258 (2) | 115 (2) |
O6—H6···O10xi | 0.73 (2) | 2.19 (3) | 2.887 (3) | 161 (3) |
O7—H17···O6 | 0.78 (3) | 2.02 (3) | 2.789 (2) | 174 (3) |
O7—H27···O4iv | 0.82 (3) | 2.08 (3) | 2.874 (2) | 164 (3) |
O8—H18···O3xvi | 0.84 (4) | 1.87 (4) | 2.702 (2) | 170 (3) |
O8—H28···O1xiv | 0.87 (4) | 2.85 (3) | 3.373 (2) | 121 (3) |
O8—H28···O2xiv | 0.87 (4) | 1.89 (4) | 2.752 (2) | 172 (3) |
O9—H19···O2vii | 0.78 (4) | 2.52 (4) | 3.117 (3) | 134 (3) |
O9—H19···O3v | 0.78 (4) | 2.67 (4) | 3.166 (3) | 122 (3) |
O9—H19···O6v | 0.78 (4) | 2.47 (4) | 3.138 (3) | 143 (4) |
O9—H29···O4iii | 0.93 (4) | 1.89 (4) | 2.806 (3) | 169 (3) |
O10—H110···O1i | 0.80 (4) | 1.93 (4) | 2.725 (2) | 174 (3) |
O10—H210···O9xiv | 0.88 (4) | 1.88 (4) | 2.756 (3) | 175 (3) |
Symmetry codes: (i) −x, −y, z; (ii) x, y, z−1; (iii) −x, −y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vii) −x+1/2, y−1/2, −z; (xi) −x+1/2, y+1/2, −z+1; (xiv) x, y, z+1; (xvi) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (253K_anh)
top
Crystal data top
C4H12KNaO10 | Dx = 1.788 Mg m−3 |
Mr = 282.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 6895 reflections |
a = 11.8510 (8) Å | θ = 3.6–28.8° |
b = 14.239 (1) Å | µ = 0.59 mm−1 |
c = 6.2146 (4) Å | T = 253 K |
V = 1048.70 (12) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 585.519 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2690 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2260 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.055 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.5°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −18→19 |
Tmin = 0.787, Tmax = 1.000 | l = −8→8 |
18338 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.034 | w = 1/[σ2(Fo2) + (0.0203P)2 + 0.4656P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.071 | (Δ/σ)max = −0.0001 |
S = 1.08 | Δρmax = 0.36 e Å−3 |
2690 reflections | Δρmin = −0.30 e Å−3 |
195 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
1 restraint | Absolute structure parameter: 0.05 (2) |
12 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0 | 0.0 | 0.0455 (3) | 0.0523 (6) | |
K2 | 0.5 | 0.0 | −0.15963 (11) | 0.03088 (17) | |
Na | 0.23176 (7) | −0.00680 (7) | 0.52026 (13) | 0.02556 (19) | |
O1 | 0.12015 (12) | 0.10898 (10) | 0.3495 (3) | 0.0243 (3) | |
O2 | 0.21038 (14) | 0.20310 (11) | 0.1184 (2) | 0.0290 (4) | |
O3 | 0.23176 (15) | 0.40646 (11) | 0.8152 (3) | 0.0346 (4) | |
O4 | 0.05192 (14) | 0.36127 (12) | 0.8454 (3) | 0.0331 (4) | |
O5 | 0.16381 (14) | 0.35756 (11) | 0.3242 (3) | 0.0254 (3) | |
H5 | 0.191 (2) | 0.3417 (19) | 0.214 (5) | 0.0381 (5)* | |
O6 | 0.29556 (13) | 0.24818 (11) | 0.6295 (3) | 0.0273 (4) | |
H6 | 0.326 (2) | 0.2918 (19) | 0.604 (5) | 0.0409 (5)* | |
O7 | 0.39576 (14) | 0.08270 (12) | 0.4846 (3) | 0.0312 (4) | |
H17 | 0.368 (3) | 0.131 (2) | 0.524 (5) | 0.0468 (6)* | |
H27 | 0.432 (2) | 0.092 (2) | 0.376 (5) | 0.0468 (6)* | |
O8 | 0.2418 (2) | 0.04136 (14) | 0.8833 (3) | 0.0448 (5) | |
H18 | 0.255 (3) | 0.004 (3) | 0.982 (5) | 0.0672 (8)* | |
H28 | 0.234 (3) | 0.096 (3) | 0.948 (5) | 0.0672 (8)* | |
O9 | 0.06062 (16) | −0.19594 (18) | −0.0342 (4) | 0.0494 (5) | |
H19 | 0.116 (3) | −0.215 (3) | 0.014 (6) | 0.0740 (8)* | |
H29 | 0.033 (3) | −0.253 (3) | −0.080 (5) | 0.0740 (8)* | |
O10 | 0.07634 (16) | −0.10383 (15) | 0.5769 (4) | 0.0488 (5) | |
H110 | 0.015 (3) | −0.103 (3) | 0.520 (5) | 0.0732 (8)* | |
H210 | 0.067 (3) | −0.137 (3) | 0.697 (6) | 0.0732 (8)* | |
C1 | 0.15472 (17) | 0.18782 (15) | 0.2841 (3) | 0.0206 (4) | |
C2 | 0.12520 (17) | 0.27337 (15) | 0.4228 (3) | 0.0200 (4) | |
H2 | 0.0401 (19) | 0.2768 (16) | 0.439 (4) | 0.0240 (5)* | |
C3 | 0.17788 (17) | 0.26401 (15) | 0.6460 (4) | 0.0212 (4) | |
H3 | 0.146 (2) | 0.2091 (17) | 0.722 (4) | 0.0255 (5)* | |
C4 | 0.1518 (2) | 0.35109 (16) | 0.7808 (3) | 0.0252 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0611 (13) | 0.0520 (14) | 0.0438 (12) | −0.0274 (12) | −0.000000 | 0.000000 |
K2 | 0.0303 (3) | 0.0349 (4) | 0.0274 (3) | −0.0036 (3) | −0.000000 | 0.000000 |
Na | 0.0244 (4) | 0.0240 (4) | 0.0283 (4) | −0.0009 (4) | −0.0013 (3) | 0.0008 (4) |
O1 | 0.0253 (7) | 0.0206 (7) | 0.0269 (8) | −0.0012 (6) | −0.0008 (7) | −0.0008 (7) |
O2 | 0.0368 (9) | 0.0267 (8) | 0.0234 (8) | −0.0004 (7) | 0.0065 (7) | −0.0011 (6) |
O3 | 0.0449 (10) | 0.0272 (8) | 0.0316 (9) | −0.0076 (7) | −0.0032 (8) | −0.0059 (7) |
O4 | 0.0338 (8) | 0.0394 (9) | 0.0260 (8) | 0.0120 (7) | −0.0004 (7) | −0.0068 (8) |
O5 | 0.0378 (9) | 0.0192 (7) | 0.0192 (7) | −0.0004 (6) | 0.0003 (7) | 0.0010 (6) |
O6 | 0.0238 (8) | 0.0244 (8) | 0.0336 (9) | 0.0038 (6) | −0.0038 (7) | −0.0006 (7) |
O7 | 0.0266 (8) | 0.0283 (9) | 0.0387 (10) | 0.0001 (7) | 0.0069 (7) | 0.0026 (8) |
O8 | 0.0844 (15) | 0.0255 (9) | 0.0243 (9) | 0.0101 (10) | 0.0048 (10) | 0.0000 (7) |
O9 | 0.0311 (10) | 0.0732 (15) | 0.0438 (12) | −0.0054 (10) | −0.0084 (9) | 0.0049 (11) |
O10 | 0.0287 (9) | 0.0523 (12) | 0.0654 (14) | −0.0128 (9) | −0.0128 (9) | 0.0235 (10) |
C1 | 0.0187 (10) | 0.0227 (11) | 0.0203 (10) | 0.0017 (8) | −0.0038 (8) | −0.0008 (8) |
C2 | 0.0210 (10) | 0.0178 (10) | 0.0212 (10) | −0.0005 (8) | −0.0009 (9) | −0.0005 (8) |
C3 | 0.0230 (10) | 0.0203 (10) | 0.0205 (10) | 0.0014 (8) | 0.0012 (9) | 0.0012 (9) |
C4 | 0.0355 (13) | 0.0232 (11) | 0.0169 (10) | 0.0042 (10) | −0.0051 (9) | 0.0004 (8) |
Geometric parameters (Å, º) top
K1—O1 | 2.8294 (19) | Na—O7 | 2.3347 (18) |
K1—O1i | 2.8294 (19) | Na—O8 | 2.3612 (19) |
K1—O8ii | 3.094 (2) | Na—O10 | 2.329 (2) |
K1—O8iii | 3.094 (2) | Na—C4iv | 3.082 (2) |
K1—H18ii | 3.05 (3) | O1—C1 | 1.262 (3) |
K1—H18iii | 3.05 (3) | O2—C1 | 1.242 (3) |
K1—O9i | 2.923 (3) | O3—C4 | 1.251 (3) |
K1—O9 | 2.923 (3) | O4—C4 | 1.258 (3) |
K1—O10iii | 3.389 (3) | O5—H5 | 0.79 (3) |
K1—O10ii | 3.389 (3) | O5—C2 | 1.422 (3) |
K1—H210iii | 3.03 (4) | O6—H6 | 0.73 (2) |
K1—H210ii | 3.03 (4) | O6—C3 | 1.417 (3) |
K2—O4iv | 2.8451 (16) | O7—H17 | 0.80 (3) |
K2—O4v | 2.8451 (16) | O7—H27 | 0.81 (3) |
K2—O5vi | 2.9881 (16) | O8—H18 | 0.82 (4) |
K2—O5vii | 2.9881 (16) | O8—H28 | 0.88 (4) |
K2—O7iii | 2.7931 (19) | O9—H19 | 0.78 (4) |
K2—O7viii | 2.7931 (19) | O9—H29 | 0.92 (4) |
K2—O8viii | 3.128 (2) | O10—H110 | 0.81 (4) |
K2—O8iii | 3.128 (2) | O10—H210 | 0.89 (4) |
K2—H18viii | 3.03 (3) | C1—C2 | 1.533 (3) |
K2—H18iii | 3.03 (3) | C2—H2 | 1.01 (2) |
Na—O1 | 2.3651 (17) | C2—C3 | 1.527 (3) |
Na—O3iv | 2.4613 (19) | C3—H3 | 0.99 (3) |
Na—O5iv | 2.4893 (18) | C3—C4 | 1.528 (3) |
| | | |
Naii—K1—Naiii | 80.19 (4) | O8viii—K2—O5vii | 61.40 (5) |
O1i—K1—Naiii | 145.32 (3) | O8iii—K2—O5vi | 61.40 (5) |
O1—K1—Naiii | 101.50 (3) | O8iii—K2—O5vii | 122.48 (5) |
O1—K1—Naii | 145.32 (3) | O8iii—K2—O7iii | 63.60 (5) |
O1i—K1—Naii | 101.50 (3) | O8iii—K2—O7viii | 125.43 (5) |
O1i—K1—O1 | 96.21 (8) | O8viii—K2—O7viii | 63.60 (5) |
O8ii—K1—Naii | 32.76 (4) | O8viii—K2—O7iii | 125.43 (5) |
O8iii—K1—Naiii | 32.76 (4) | O8viii—K2—O8iii | 170.21 (7) |
O8ii—K1—Naiii | 110.04 (6) | H18viii—K2—Naviii | 49.0 (6) |
O8iii—K1—Naii | 110.04 (6) | H18viii—K2—Naiii | 164.6 (7) |
O8ii—K1—O1 | 142.00 (6) | H18iii—K2—Naviii | 164.6 (7) |
O8iii—K1—O1 | 69.33 (5) | H18iii—K2—Naiii | 49.0 (6) |
O8iii—K1—O1i | 142.00 (6) | H18iii—K2—O4v | 89.6 (7) |
O8ii—K1—O1i | 69.33 (5) | H18iii—K2—O4iv | 66.9 (7) |
O8ii—K1—O8iii | 141.98 (9) | H18viii—K2—O4iv | 89.6 (7) |
H18iii—K1—Naiii | 42.5 (6) | H18viii—K2—O4v | 66.9 (7) |
H18ii—K1—Naiii | 122.6 (6) | H18iii—K2—O5vi | 59.4 (7) |
H18ii—K1—Naii | 42.5 (6) | H18iii—K2—O5vii | 135.0 (8) |
H18iii—K1—Naii | 122.6 (6) | H18viii—K2—O5vii | 59.4 (7) |
H18iii—K1—O1i | 126.6 (7) | H18viii—K2—O5vi | 135.0 (8) |
H18ii—K1—O1 | 126.6 (7) | H18iii—K2—O7iii | 78.3 (7) |
H18ii—K1—O1i | 65.0 (7) | H18iii—K2—O7viii | 131.4 (7) |
H18iii—K1—O1 | 65.0 (7) | H18viii—K2—O7viii | 78.3 (7) |
H18ii—K1—O8ii | 15.4 (7) | H18viii—K2—O7iii | 131.4 (7) |
H18iii—K1—O8ii | 151.6 (7) | H18iii—K2—O8viii | 156.2 (7) |
H18ii—K1—O8iii | 151.6 (7) | H18viii—K2—O8iii | 156.2 (7) |
H18iii—K1—O8iii | 15.4 (7) | H18viii—K2—O8viii | 15.3 (7) |
H18ii—K1—H18iii | 165.1 (13) | H18iii—K2—O8iii | 15.3 (7) |
O9i—K1—Naii | 71.98 (5) | H18viii—K2—H18iii | 146.3 (13) |
O9—K1—Naii | 92.88 (6) | K2ix—Na—K1x | 98.00 (3) |
O9—K1—Naiii | 71.98 (5) | O1—Na—K1x | 88.14 (4) |
O9i—K1—Naiii | 92.88 (6) | O1—Na—K2ix | 133.94 (5) |
O9—K1—O1i | 73.34 (5) | O3iv—Na—K1x | 140.56 (5) |
O9—K1—O1 | 120.86 (6) | O3iv—Na—K2ix | 108.25 (5) |
O9i—K1—O1 | 73.34 (5) | O3iv—Na—O1 | 93.90 (6) |
O9i—K1—O1i | 120.86 (6) | O5iv—Na—K1x | 92.33 (5) |
O9—K1—O8iii | 84.20 (6) | O5iv—Na—K2ix | 52.61 (4) |
O9—K1—O8ii | 89.47 (5) | O5iv—Na—O1 | 173.28 (6) |
O9i—K1—O8iii | 89.47 (5) | O5iv—Na—O3iv | 81.49 (6) |
O9i—K1—O8ii | 84.20 (6) | O7—Na—K1x | 126.59 (6) |
O9—K1—H18iii | 75.7 (7) | O7—Na—K2ix | 47.99 (5) |
O9—K1—H18ii | 101.7 (8) | O7—Na—O1 | 92.43 (6) |
O9i—K1—H18ii | 75.7 (7) | O7—Na—O3iv | 92.71 (7) |
O9i—K1—H18iii | 101.7 (8) | O7—Na—O5iv | 92.66 (6) |
O9i—K1—O9 | 160.49 (12) | O8—Na—K1x | 45.15 (6) |
O10iii—K1—Naiii | 32.96 (4) | O8—Na—K2ix | 56.17 (6) |
O10iii—K1—Naii | 61.60 (4) | O8—Na—O1 | 104.74 (7) |
O10ii—K1—Naii | 32.96 (4) | O8—Na—O3iv | 161.13 (7) |
O10ii—K1—Naiii | 61.60 (4) | O8—Na—O5iv | 80.18 (7) |
O10iii—K1—O1i | 117.96 (5) | O8—Na—O7 | 83.71 (8) |
O10ii—K1—O1 | 117.96 (5) | O10—Na—K1x | 52.33 (7) |
O10ii—K1—O1i | 132.75 (5) | O10—Na—K2ix | 127.25 (6) |
O10iii—K1—O1 | 132.75 (5) | O10—Na—O1 | 92.24 (7) |
O10iii—K1—O8ii | 83.36 (6) | O10—Na—O3iv | 88.24 (8) |
O10ii—K1—O8iii | 83.36 (6) | O10—Na—O5iv | 82.77 (7) |
O10iii—K1—O8iii | 63.64 (5) | O10—Na—O7 | 175.16 (8) |
O10ii—K1—O8ii | 63.64 (5) | O10—Na—O8 | 93.87 (9) |
O10iii—K1—H18iii | 68.5 (7) | C4iv—Na—K1x | 140.12 (5) |
O10iii—K1—H18ii | 98.3 (7) | C4iv—Na—K2ix | 87.68 (5) |
O10ii—K1—H18ii | 68.5 (7) | C4iv—Na—O1 | 115.82 (6) |
O10ii—K1—H18iii | 98.3 (7) | C4iv—Na—O3iv | 22.74 (6) |
O10iii—K1—O9 | 51.13 (6) | C4iv—Na—O5iv | 60.24 (6) |
O10iii—K1—O9i | 109.66 (8) | C4iv—Na—O7 | 85.88 (7) |
O10ii—K1—O9i | 51.13 (6) | C4iv—Na—O8 | 138.44 (7) |
O10ii—K1—O9 | 109.66 (8) | C4iv—Na—O10 | 93.23 (8) |
O10ii—K1—O10iii | 61.52 (8) | Na—O1—K1 | 101.47 (6) |
H210ii—K1—Naii | 42.9 (7) | C1—O1—K1 | 115.85 (14) |
H210ii—K1—Naiii | 68.7 (7) | C1—O1—Na | 125.66 (13) |
H210iii—K1—Naii | 68.7 (7) | C4—O3—Naxi | 107.75 (14) |
H210iii—K1—Naiii | 42.9 (7) | C4—O4—K2xii | 120.15 (14) |
H210iii—K1—O1 | 134.4 (7) | Naxi—O5—K2xiii | 85.94 (5) |
H210iii—K1—O1i | 104.9 (7) | H5—O5—K2xiii | 99 (2) |
H210ii—K1—O1 | 104.9 (7) | H5—O5—Naxi | 111 (2) |
H210ii—K1—O1i | 134.4 (7) | C2—O5—K2xiii | 120.71 (11) |
H210ii—K1—O8ii | 69.2 (7) | C2—O5—Naxi | 130.32 (13) |
H210ii—K1—O8iii | 83.6 (7) | C2—O5—H5 | 105 (2) |
H210iii—K1—O8iii | 69.2 (7) | C3—O6—H6 | 111 (2) |
H210iii—K1—O8ii | 83.6 (7) | Na—O7—K2xiv | 93.61 (6) |
H210ii—K1—H18ii | 70.0 (9) | H17—O7—K2xiv | 107 (2) |
H210ii—K1—H18iii | 99.0 (10) | H17—O7—Na | 96 (2) |
H210iii—K1—H18iii | 70.0 (9) | H27—O7—K2xiv | 120 (2) |
H210iii—K1—H18ii | 99.0 (10) | H27—O7—Na | 128 (2) |
H210ii—K1—O9i | 36.6 (7) | H27—O7—H17 | 109 (3) |
H210ii—K1—O9 | 124.0 (7) | K2xiv—O8—K1xiv | 153.90 (7) |
H210iii—K1—O9 | 36.6 (7) | Na—O8—K1xiv | 102.09 (8) |
H210iii—K1—O9i | 124.0 (7) | Na—O8—K2xiv | 85.00 (6) |
H210iii—K1—O10ii | 74.7 (7) | H18—O8—K1xiv | 79 (2) |
H210ii—K1—O10iii | 74.7 (7) | H18—O8—K2xiv | 76 (2) |
H210ii—K1—O10ii | 14.6 (7) | H18—O8—Na | 122 (3) |
H210iii—K1—O10iii | 14.6 (7) | H28—O8—K1xiv | 85 (2) |
H210ii—K1—H210iii | 88.5 (15) | H28—O8—K2xiv | 108 (2) |
Naviii—K2—Naiii | 115.95 (3) | H28—O8—Na | 134 (2) |
O4v—K2—Naiii | 124.42 (4) | H28—O8—H18 | 104 (3) |
O4iv—K2—Naiii | 99.37 (4) | K2xiv—H18—K1xiv | 170.3 (13) |
O4v—K2—Naviii | 99.37 (4) | O8—H18—K1xiv | 85 (2) |
O4iv—K2—Naviii | 124.42 (4) | O8—H18—K2xiv | 89 (2) |
O4iv—K2—O4v | 93.31 (7) | H19—O9—K1i | 119 (3) |
O5vii—K2—Naviii | 41.44 (3) | H29—O9—K1i | 144 (2) |
O5vii—K2—Naiii | 112.74 (4) | H29—O9—H19 | 96 (4) |
O5vi—K2—Naviii | 112.74 (4) | Na—O10—K1x | 94.71 (8) |
O5vi—K2—Naiii | 41.44 (3) | H110—O10—K1x | 97 (2) |
O5vi—K2—O4iv | 67.86 (5) | H110—O10—Na | 130 (2) |
O5vii—K2—O4iv | 147.86 (5) | H210—O10—K1x | 59 (2) |
O5vi—K2—O4v | 147.86 (5) | H210—O10—Na | 123 (2) |
O5vii—K2—O4v | 67.86 (5) | H210—O10—H110 | 105 (3) |
O5vi—K2—O5vii | 139.96 (7) | O10—H210—K1x | 107 (3) |
O7viii—K2—Naiii | 86.80 (4) | O2—C1—O1 | 126.5 (2) |
O7viii—K2—Naviii | 38.40 (4) | C2—C1—O1 | 116.85 (18) |
O7iii—K2—Naiii | 38.40 (4) | C2—C1—O2 | 116.63 (19) |
O7iii—K2—Naviii | 86.80 (4) | C1—C2—O5 | 110.76 (16) |
O7iii—K2—O4v | 110.26 (5) | H2—C2—O5 | 108.8 (13) |
O7viii—K2—O4v | 137.77 (5) | H2—C2—C1 | 108.7 (13) |
O7iii—K2—O4iv | 137.77 (5) | C3—C2—O5 | 109.47 (16) |
O7viii—K2—O4iv | 110.26 (5) | C3—C2—C1 | 110.38 (17) |
O7iii—K2—O5vi | 74.21 (5) | C3—C2—H2 | 108.7 (13) |
O7viii—K2—O5vi | 74.35 (5) | C2—C3—O6 | 110.51 (17) |
O7iii—K2—O5vii | 74.35 (5) | H3—C3—O6 | 106.6 (14) |
O7viii—K2—O5vii | 74.21 (5) | H3—C3—C2 | 110.2 (14) |
O7viii—K2—O7iii | 75.33 (8) | C4—C3—O6 | 111.59 (18) |
O8viii—K2—Naviii | 38.83 (3) | C4—C3—C2 | 110.16 (17) |
O8viii—K2—Naiii | 150.40 (4) | C4—C3—H3 | 107.7 (14) |
O8iii—K2—Naviii | 150.40 (4) | O3—C4—Naxi | 49.51 (11) |
O8iii—K2—Naiii | 38.83 (3) | O4—C4—Naxi | 122.62 (15) |
O8viii—K2—O4iv | 91.28 (5) | O4—C4—O3 | 125.8 (2) |
O8viii—K2—O4v | 81.98 (5) | C3—C4—Naxi | 96.28 (13) |
O8iii—K2—O4iv | 81.98 (5) | C3—C4—O3 | 116.9 (2) |
O8iii—K2—O4v | 91.28 (5) | C3—C4—O4 | 117.3 (2) |
O8viii—K2—O5vi | 122.48 (5) | | |
| | | |
K1—O1—C1—O2 | −51.54 (14) | Naxi—O3—C4—C3 | 74.26 (13) |
K1i—O1—C1—O2 | −51.54 (14) | Naxi—O5—C2—C1 | −133.65 (16) |
K1—O1—C1—C2 | 128.48 (13) | Naxi—O5—C2—C3 | −11.72 (15) |
K1i—O1—C1—C2 | 128.48 (13) | Naxi—C4—C3—O6 | 62.93 (12) |
K2xii—O4—C4—Naxi | −72.98 (13) | Naxi—C4—C3—C2 | −60.21 (13) |
K2—O4iv—C4iv—Na | −72.98 (13) | O1—C1—C2—O5 | −176.76 (18) |
K2xii—O4—C4—O3 | −12.24 (17) | O1—C1—C2—C3 | 61.8 (2) |
K2xi—O4—C4—O3 | −12.24 (17) | O2—C1—C2—O5 | 3.3 (2) |
K2xii—O4—C4—C3 | 168.57 (14) | O2—C1—C2—C3 | −118.14 (19) |
K2xi—O4—C4—C3 | 168.57 (14) | O3—C4—C3—O6 | 15.5 (2) |
K2xv—O5—C2—C1 | 113.01 (14) | O3—C4—C3—C2 | −107.6 (2) |
K2xiii—O5—C2—C1 | 113.01 (14) | O4—C4—C3—O6 | −165.2 (2) |
K2xiii—O5—C2—C3 | −125.06 (14) | O4—C4—C3—C2 | 71.6 (2) |
K2xv—O5—C2—C3 | −125.06 (14) | O5—C2—C3—O6 | −68.00 (17) |
Na—O1—C1—O2 | 76.73 (17) | O5—C2—C3—C4 | 55.77 (18) |
Na—O1—C1—C2 | −103.24 (15) | O6—C3—C2—C1 | 54.16 (19) |
Naxi—O3—C4—O4 | −104.94 (14) | C1—C2—C3—C4 | 177.93 (17) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x+1/2, −y+1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (vii) x+1/2, −y+1/2, −z; (viii) −x+1, −y, z−1; (ix) −x+1, −y, z+1; (x) −x, −y, z+1; (xi) −x+1/2, y+1/2, −z+1; (xii) x−1/2, −y+1/2, −z+1; (xiii) x−1/2, −y+1/2, −z; (xiv) x, y, z+1; (xv) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.79 (3) | 2.07 (3) | 2.603 (2) | 124 (3) |
O5—H5···O3iii | 0.79 (3) | 2.69 (3) | 3.338 (2) | 141 (2) |
O5—H5···O4iii | 0.79 (3) | 2.83 (3) | 3.258 (2) | 116 (2) |
O6—H6···O10xi | 0.73 (2) | 2.20 (3) | 2.897 (3) | 160 (3) |
O7—H17···O6 | 0.80 (3) | 1.99 (3) | 2.788 (2) | 178 (3) |
O7—H27···O4v | 0.81 (3) | 2.09 (3) | 2.875 (2) | 164 (3) |
O8—H18···O3xvi | 0.82 (4) | 1.89 (4) | 2.702 (2) | 170 (4) |
O8—H28···O1xiv | 0.88 (4) | 2.84 (3) | 3.376 (2) | 121 (3) |
O8—H28···O2xiv | 0.88 (4) | 1.88 (4) | 2.753 (2) | 172 (3) |
O9—H19···O2vi | 0.78 (4) | 2.50 (4) | 3.115 (3) | 138 (4) |
O9—H19···O3iv | 0.78 (4) | 2.72 (4) | 3.168 (3) | 119 (3) |
O9—H19···O6iv | 0.78 (4) | 2.51 (4) | 3.141 (3) | 140 (4) |
O9—H29···O4ii | 0.92 (4) | 1.89 (4) | 2.807 (3) | 169 (3) |
O10—H110···O1i | 0.81 (4) | 1.92 (4) | 2.725 (2) | 172 (3) |
O10—H210···O9xiv | 0.89 (4) | 1.87 (4) | 2.756 (3) | 173 (3) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x+1/2, −y+1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (xi) −x+1/2, y+1/2, −z+1; (xiv) x, y, z+1; (xvi) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (256K_anh)
top
Crystal data top
C4H12KNaO10 | F(000) = 585.519 |
Mr = 282.22 | Dx = 1.787 Mg m−3 |
Monoclinic, P2111 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.8513 (8) Å | Cell parameters from 6823 reflections |
b = 14.2386 (11) Å | θ = 3.5–28.7° |
c = 6.2155 (4) Å | µ = 0.59 mm−1 |
β = 90° | T = 256 K |
V = 1048.84 (13) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 5147 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 4145 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.5°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.758, Tmax = 1.000 | l = −8→8 |
18315 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.037 | w = 1/[σ2(Fo2) + (0.0232P)2 + 0.1644P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.077 | (Δ/σ)max = 0.001 |
S = 1.09 | Δρmax = 0.33 e Å−3 |
5147 reflections | Δρmin = −0.34 e Å−3 |
386 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
3 restraints | Absolute structure parameter: 0.09 (2) |
24 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.00032 (18) | −0.00041 (13) | 0.0454 (2) | 0.0536 (5) | |
K2 | 0.50001 (7) | 0.00022 (5) | −0.15958 (9) | 0.03172 (14) | |
Na1 | 0.23165 (10) | −0.00672 (7) | 0.52105 (17) | 0.0262 (3) | |
Na2 | −0.23179 (10) | 0.00678 (8) | 0.51995 (17) | 0.0261 (2) | |
O11 | 0.12003 (16) | 0.10899 (13) | 0.3498 (3) | 0.0247 (4) | |
O12 | −0.12019 (16) | −0.10901 (13) | 0.3492 (3) | 0.0246 (4) | |
O21 | 0.21061 (18) | 0.20295 (14) | 0.1191 (3) | 0.0295 (4) | |
O22 | −0.21005 (18) | −0.20298 (14) | 0.1180 (3) | 0.0296 (4) | |
O31 | 0.23136 (19) | 0.40638 (14) | 0.8155 (3) | 0.0352 (5) | |
O32 | −0.23222 (19) | −0.40644 (14) | 0.8142 (3) | 0.0352 (5) | |
O41 | 0.05168 (18) | 0.36105 (15) | 0.8454 (3) | 0.0336 (5) | |
O42 | −0.05239 (18) | −0.36159 (15) | 0.8451 (3) | 0.0330 (5) | |
O51 | 0.16398 (17) | 0.35744 (13) | 0.3243 (3) | 0.0261 (4) | |
H51 | 0.194 (3) | 0.341 (2) | 0.218 (5) | 0.0391 (7)* | |
O52 | −0.16377 (18) | −0.35736 (13) | 0.3239 (3) | 0.0260 (4) | |
H52 | −0.191 (3) | −0.344 (2) | 0.212 (5) | 0.0390 (7)* | |
O61 | 0.29535 (17) | 0.24792 (14) | 0.6298 (3) | 0.0279 (4) | |
H61 | 0.324 (3) | 0.295 (2) | 0.609 (6) | 0.0419 (7)* | |
O62 | −0.29561 (17) | −0.24822 (14) | 0.6289 (3) | 0.0277 (4) | |
H62 | −0.329 (3) | −0.289 (2) | 0.603 (6) | 0.0416 (7)* | |
O71 | 0.39587 (18) | 0.08241 (16) | 0.4845 (4) | 0.0321 (5) | |
H17 | 0.371 (3) | 0.129 (3) | 0.525 (6) | 0.0482 (7)* | |
H27 | 0.433 (3) | 0.089 (3) | 0.373 (6) | 0.0482 (7)* | |
O72 | −0.39596 (18) | −0.08272 (16) | 0.4846 (4) | 0.0322 (5) | |
H47 | −0.434 (3) | −0.095 (3) | 0.371 (6) | 0.0483 (7)* | |
H37 | −0.366 (3) | −0.130 (3) | 0.530 (6) | 0.0483 (7)* | |
O81 | 0.2421 (2) | 0.04151 (17) | 0.8840 (3) | 0.0452 (6) | |
H18 | 0.240 (4) | 0.099 (3) | 0.948 (6) | 0.0678 (10)* | |
H28 | 0.257 (4) | 0.002 (3) | 0.983 (8) | 0.0678 (10)* | |
O82 | −0.2414 (2) | −0.04115 (17) | 0.8834 (3) | 0.0458 (7) | |
H48 | −0.258 (4) | 0.001 (3) | 0.985 (8) | 0.0687 (10)* | |
H38 | −0.231 (4) | −0.094 (3) | 0.941 (7) | 0.0687 (10)* | |
O91 | 0.0612 (2) | −0.1963 (2) | −0.0343 (4) | 0.0511 (7) | |
H29 | 0.036 (4) | −0.251 (3) | −0.080 (6) | 0.0766 (10)* | |
H19 | 0.118 (4) | −0.232 (3) | 0.009 (7) | 0.0766 (10)* | |
O92 | −0.0607 (2) | 0.1956 (2) | −0.0337 (4) | 0.0507 (7) | |
H39 | −0.118 (4) | 0.211 (3) | 0.014 (7) | 0.0761 (10)* | |
H49 | −0.032 (4) | 0.251 (3) | −0.082 (6) | 0.0761 (10)* | |
O101 | 0.0758 (2) | −0.1033 (2) | 0.5784 (5) | 0.0513 (7) | |
H210 | 0.073 (4) | −0.141 (3) | 0.693 (7) | 0.0769 (10)* | |
H110 | 0.014 (4) | −0.104 (3) | 0.523 (6) | 0.0769 (10)* | |
O102 | −0.0766 (2) | 0.10383 (19) | 0.5764 (5) | 0.0486 (7) | |
H410 | −0.069 (4) | 0.134 (3) | 0.698 (7) | 0.0729 (10)* | |
H310 | −0.018 (4) | 0.103 (3) | 0.518 (6) | 0.0729 (10)* | |
C11 | 0.1547 (2) | 0.18781 (19) | 0.2840 (4) | 0.0206 (6) | |
C21 | 0.1254 (2) | 0.27330 (18) | 0.4237 (4) | 0.0207 (5) | |
H21 | 0.045 (3) | 0.278 (2) | 0.437 (4) | 0.0248 (6)* | |
C31 | 0.1778 (2) | 0.2640 (2) | 0.6466 (4) | 0.0218 (6) | |
H31 | 0.146 (3) | 0.205 (2) | 0.723 (4) | 0.0262 (7)* | |
C41 | 0.1517 (3) | 0.3509 (2) | 0.7814 (4) | 0.0259 (6) | |
C12 | −0.1541 (2) | −0.18772 (19) | 0.2841 (4) | 0.0205 (5) | |
C22 | −0.1254 (2) | −0.27323 (18) | 0.4227 (4) | 0.0204 (5) | |
H22 | −0.038 (3) | −0.2771 (19) | 0.437 (4) | 0.0245 (6)* | |
C32 | −0.1778 (2) | −0.26405 (19) | 0.6453 (4) | 0.0219 (6) | |
H32 | −0.144 (3) | −0.210 (2) | 0.724 (4) | 0.0263 (7)* | |
C42 | −0.1519 (3) | −0.35140 (19) | 0.7804 (4) | 0.0256 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0632 (10) | 0.0516 (11) | 0.0460 (10) | −0.0301 (10) | 0.0001 (12) | 0.0012 (9) |
K2 | 0.0317 (3) | 0.0358 (3) | 0.0277 (3) | −0.0035 (3) | 0.0000 (3) | 0.0002 (2) |
Na1 | 0.0257 (6) | 0.0239 (6) | 0.0291 (5) | −0.0009 (4) | −0.0017 (5) | 0.0006 (4) |
Na2 | 0.0249 (6) | 0.0242 (6) | 0.0291 (5) | −0.0008 (4) | 0.0015 (5) | −0.0006 (4) |
O11 | 0.0267 (10) | 0.0203 (11) | 0.0270 (10) | −0.0013 (8) | −0.0020 (8) | −0.0014 (7) |
O12 | 0.0272 (10) | 0.0207 (11) | 0.0260 (10) | −0.0013 (8) | 0.0007 (8) | 0.0007 (7) |
O21 | 0.0378 (11) | 0.0272 (11) | 0.0236 (10) | 0.0003 (9) | 0.0077 (9) | −0.0005 (8) |
O22 | 0.0377 (12) | 0.0278 (11) | 0.0232 (10) | −0.0013 (9) | −0.0069 (9) | 0.0017 (8) |
O31 | 0.0459 (13) | 0.0276 (12) | 0.0321 (10) | −0.0079 (10) | −0.0031 (10) | −0.0065 (8) |
O32 | 0.0467 (13) | 0.0266 (12) | 0.0323 (10) | −0.0084 (10) | 0.0024 (10) | 0.0066 (8) |
O41 | 0.0357 (11) | 0.0394 (13) | 0.0256 (10) | 0.0127 (10) | 0.0000 (9) | −0.0067 (9) |
O42 | 0.0326 (11) | 0.0404 (13) | 0.0261 (10) | 0.0112 (9) | −0.0009 (8) | 0.0069 (9) |
O51 | 0.0379 (12) | 0.0190 (10) | 0.0213 (9) | −0.0011 (8) | 0.0014 (8) | 0.0012 (8) |
O52 | 0.0377 (12) | 0.0202 (10) | 0.0202 (9) | −0.0007 (8) | 0.0001 (8) | −0.0001 (8) |
O61 | 0.0251 (11) | 0.0250 (12) | 0.0337 (11) | 0.0045 (9) | −0.0044 (9) | −0.0002 (9) |
O62 | 0.0217 (11) | 0.0255 (12) | 0.0359 (11) | 0.0032 (8) | 0.0034 (9) | 0.0019 (9) |
O71 | 0.0285 (11) | 0.0297 (12) | 0.0382 (12) | −0.0005 (9) | 0.0064 (9) | 0.0018 (9) |
O72 | 0.0273 (11) | 0.0293 (12) | 0.0400 (12) | 0.0000 (9) | −0.0077 (9) | −0.0019 (9) |
O81 | 0.0845 (19) | 0.0257 (13) | 0.0254 (11) | 0.0117 (12) | 0.0044 (12) | 0.0001 (8) |
O82 | 0.0850 (19) | 0.0269 (13) | 0.0255 (11) | 0.0122 (13) | −0.0035 (12) | −0.0006 (9) |
O91 | 0.0347 (14) | 0.075 (2) | 0.0431 (14) | −0.0058 (13) | −0.0069 (11) | 0.0073 (13) |
O92 | 0.0326 (14) | 0.074 (2) | 0.0450 (14) | −0.0051 (13) | 0.0080 (11) | −0.0048 (13) |
O101 | 0.0322 (14) | 0.0536 (17) | 0.0681 (18) | −0.0148 (11) | −0.0139 (12) | 0.0257 (13) |
O102 | 0.0292 (13) | 0.0521 (16) | 0.0645 (17) | −0.0128 (11) | 0.0128 (12) | −0.0226 (13) |
C11 | 0.0199 (13) | 0.0220 (15) | 0.0198 (12) | 0.0019 (11) | −0.0055 (11) | −0.0004 (10) |
C21 | 0.0223 (15) | 0.0185 (14) | 0.0212 (12) | 0.0000 (11) | 0.0003 (11) | 0.0004 (10) |
C31 | 0.0225 (14) | 0.0221 (15) | 0.0209 (13) | 0.0015 (11) | 0.0005 (10) | −0.0003 (10) |
C41 | 0.0381 (17) | 0.0221 (15) | 0.0176 (12) | 0.0044 (13) | −0.0055 (12) | 0.0010 (10) |
C12 | 0.0178 (13) | 0.0237 (15) | 0.0199 (12) | 0.0019 (11) | 0.0043 (11) | 0.0012 (10) |
C22 | 0.0203 (14) | 0.0182 (13) | 0.0227 (13) | −0.0004 (10) | −0.0012 (11) | −0.0019 (10) |
C32 | 0.0237 (14) | 0.0196 (14) | 0.0225 (13) | 0.0023 (11) | −0.0019 (10) | −0.0008 (10) |
C42 | 0.0382 (17) | 0.0228 (15) | 0.0158 (12) | 0.0038 (13) | 0.0039 (12) | 0.0009 (10) |
Geometric parameters (Å, º) top
K1—O11 | 2.831 (2) | O31—C41 | 1.249 (4) |
K1—O12 | 2.828 (2) | O32—C42 | 1.251 (4) |
K1—O81i | 3.094 (3) | O41—C41 | 1.258 (4) |
K1—H28i | 3.07 (5) | O42—C42 | 1.254 (4) |
K1—O82i | 3.091 (4) | O51—H51 | 0.78 (3) |
K1—O91 | 2.922 (4) | O51—C21 | 1.424 (3) |
K1—O92 | 2.926 (4) | O52—H52 | 0.79 (3) |
K1—O101i | 3.371 (3) | O52—C22 | 1.421 (3) |
K1—H210i | 3.09 (4) | O61—H61 | 0.76 (3) |
K1—O102i | 3.397 (3) | O61—C31 | 1.416 (3) |
K1—H410i | 3.00 (4) | O62—H62 | 0.73 (3) |
K2—O41ii | 2.844 (2) | O62—C32 | 1.418 (3) |
K2—O42iii | 2.847 (2) | O71—H17 | 0.77 (4) |
K2—O51iv | 2.989 (2) | O71—H27 | 0.83 (4) |
K2—O52v | 2.991 (2) | O72—H47 | 0.85 (4) |
K2—O71i | 2.791 (2) | O72—H37 | 0.82 (4) |
K2—O72vi | 2.793 (2) | O81—H18 | 0.91 (4) |
K2—O81i | 3.125 (3) | O81—H28 | 0.85 (5) |
K2—H28i | 3.01 (5) | O82—H48 | 0.89 (5) |
K2—O82vi | 3.133 (3) | O82—H38 | 0.85 (4) |
K2—H48vi | 3.00 (5) | O91—H29 | 0.89 (4) |
Na1—O11 | 2.366 (2) | O91—H19 | 0.89 (5) |
Na1—O32iii | 2.460 (2) | O92—H39 | 0.78 (5) |
Na1—O52iii | 2.492 (2) | O92—H49 | 0.91 (5) |
Na1—O71 | 2.335 (2) | O101—H210 | 0.90 (5) |
Na1—O81 | 2.361 (2) | O101—H110 | 0.81 (5) |
Na1—O101 | 2.330 (3) | O102—H410 | 0.88 (4) |
Na1—C42iii | 3.081 (3) | O102—H310 | 0.78 (5) |
Na2—O12 | 2.365 (2) | C11—C21 | 1.535 (4) |
Na2—O31vii | 2.463 (2) | C21—H21 | 0.96 (3) |
Na2—O51vii | 2.490 (2) | C21—C31 | 1.524 (4) |
Na2—O72 | 2.336 (2) | C31—H31 | 1.04 (3) |
Na2—O82 | 2.363 (2) | C31—C41 | 1.526 (4) |
Na2—O102 | 2.327 (3) | C12—C22 | 1.530 (4) |
Na2—C41vii | 3.086 (3) | C22—H22 | 1.04 (3) |
O11—C11 | 1.263 (3) | C22—C32 | 1.522 (4) |
O12—C12 | 1.257 (3) | C32—H32 | 1.00 (3) |
O21—C11 | 1.239 (3) | C32—C42 | 1.532 (4) |
O22—C12 | 1.246 (3) | | |
| | | |
Na2i—K1—Na1i | 80.21 (3) | O101—Na1—O52iii | 82.91 (9) |
O11—K1—Na1i | 101.54 (7) | O101—Na1—O71 | 175.22 (10) |
O11—K1—Na2i | 145.11 (8) | O101—Na1—O81 | 93.81 (10) |
O12—K1—Na1i | 145.54 (8) | C42iii—Na1—K1viii | 140.10 (7) |
O12—K1—Na2i | 101.46 (7) | C42iii—Na1—K2viii | 87.65 (6) |
O12—K1—O11 | 96.19 (7) | C42iii—Na1—O11 | 115.68 (8) |
O81i—K1—Na1i | 32.84 (5) | C42iii—Na1—O32iii | 22.75 (7) |
O81i—K1—Na2i | 110.10 (6) | C42iii—Na1—O52iii | 60.22 (7) |
O81i—K1—O11 | 69.30 (7) | C42iii—Na1—O71 | 85.61 (8) |
O81i—K1—O12 | 142.17 (10) | C42iii—Na1—O81 | 138.41 (9) |
H28i—K1—Na1i | 42.7 (9) | C42iii—Na1—O101 | 93.53 (10) |
H28i—K1—Na2i | 122.8 (9) | K2ix—Na2—K1viii | 97.99 (4) |
H28i—K1—O11 | 65.2 (8) | O12—Na2—K1viii | 88.05 (6) |
H28i—K1—O12 | 126.3 (9) | O12—Na2—K2ix | 133.99 (6) |
H28i—K1—O81i | 15.8 (9) | O31vii—Na2—K1viii | 140.67 (7) |
O82i—K1—Na1i | 110.07 (6) | O31vii—Na2—K2ix | 108.16 (6) |
O82i—K1—Na2i | 32.72 (5) | O31vii—Na2—O12 | 93.99 (7) |
O82i—K1—O11 | 141.74 (10) | O51vii—Na2—K1viii | 92.36 (6) |
O82i—K1—O12 | 69.33 (7) | O51vii—Na2—K2ix | 52.62 (5) |
O82i—K1—O81i | 142.06 (7) | O51vii—Na2—O12 | 173.24 (8) |
O82i—K1—H28i | 151.6 (9) | O51vii—Na2—O31vii | 81.44 (7) |
O91—K1—Na1i | 72.05 (7) | O72—Na2—K1viii | 126.51 (7) |
O91—K1—Na2i | 93.01 (7) | O72—Na2—K2ix | 47.98 (6) |
O91—K1—O11 | 120.95 (10) | O72—Na2—O12 | 92.50 (8) |
O91—K1—O12 | 73.49 (8) | O72—Na2—O31vii | 92.69 (9) |
O91—K1—O81i | 84.31 (9) | O72—Na2—O51vii | 92.68 (8) |
O91—K1—H28i | 75.3 (8) | O82—Na2—K1viii | 45.00 (7) |
O91—K1—O82i | 89.68 (8) | O82—Na2—K2ix | 56.26 (7) |
O92—K1—Na1i | 92.88 (7) | O82—Na2—O12 | 104.73 (9) |
O92—K1—Na2i | 71.87 (7) | O82—Na2—O31vii | 161.07 (9) |
O92—K1—O11 | 73.24 (8) | O82—Na2—O51vii | 80.16 (8) |
O92—K1—O12 | 120.63 (10) | O82—Na2—O72 | 83.80 (9) |
O92—K1—O81i | 89.44 (8) | O102—Na2—K1viii | 52.42 (8) |
O92—K1—H28i | 102.2 (9) | O102—Na2—K2ix | 127.18 (7) |
O92—K1—O82i | 83.97 (9) | O102—Na2—O12 | 92.26 (9) |
O92—K1—O91 | 160.56 (9) | O102—Na2—O31vii | 88.25 (10) |
O101i—K1—Na1i | 33.01 (5) | O102—Na2—O51vii | 82.67 (9) |
O101i—K1—Na2i | 61.53 (5) | O102—Na2—O72 | 175.07 (10) |
O101i—K1—O11 | 132.91 (9) | O102—Na2—O82 | 93.76 (11) |
O101i—K1—O12 | 118.13 (8) | C41vii—Na2—K1viii | 140.19 (7) |
O101i—K1—O81i | 63.81 (7) | C41vii—Na2—K2ix | 87.69 (6) |
O101i—K1—H28i | 68.4 (9) | C41vii—Na2—O12 | 115.84 (8) |
O101i—K1—O82i | 83.35 (7) | C41vii—Na2—O31vii | 22.65 (7) |
O101i—K1—O91 | 51.29 (7) | C41vii—Na2—O51vii | 60.26 (7) |
O101i—K1—O92 | 109.56 (8) | C41vii—Na2—O72 | 85.90 (9) |
H210i—K1—Na1i | 42.7 (9) | C41vii—Na2—O82 | 138.48 (9) |
H210i—K1—Na2i | 69.8 (9) | C41vii—Na2—O102 | 93.16 (10) |
H210i—K1—O11 | 133.6 (9) | Na1—O11—K1 | 101.41 (8) |
H210i—K1—O12 | 105.0 (9) | C11—O11—K1 | 115.81 (15) |
H210i—K1—O81i | 68.7 (9) | C11—O11—Na1 | 125.63 (16) |
H210i—K1—H28i | 68.9 (12) | Na2—O12—K1 | 101.58 (8) |
H210i—K1—O82i | 84.7 (9) | C12—O12—K1 | 115.72 (15) |
H210i—K1—O91 | 36.1 (9) | C12—O12—Na2 | 125.94 (16) |
H210i—K1—O92 | 124.7 (9) | C41—O31—Na2ii | 107.95 (16) |
H210i—K1—O101i | 15.1 (9) | C42—O32—Na1x | 107.75 (16) |
O102i—K1—Na1i | 61.65 (5) | C41—O41—K2vii | 119.97 (18) |
O102i—K1—Na2i | 32.88 (5) | C42—O42—K2x | 120.36 (18) |
O102i—K1—O11 | 117.87 (8) | Na2ii—O51—K2xi | 85.94 (6) |
O102i—K1—O12 | 132.59 (9) | H51—O51—K2xi | 102 (3) |
O102i—K1—O81i | 83.44 (7) | H51—O51—Na2ii | 110 (3) |
O102i—K1—H28i | 98.7 (9) | C21—O51—K2xi | 120.70 (15) |
O102i—K1—O82i | 63.49 (7) | C21—O51—Na2ii | 130.09 (15) |
O102i—K1—O91 | 109.77 (8) | C21—O51—H51 | 105 (3) |
O102i—K1—O92 | 51.08 (7) | Na1x—O52—K2xii | 85.79 (6) |
O102i—K1—O101i | 61.46 (6) | H52—O52—K2xii | 98 (2) |
O102i—K1—H210i | 75.6 (9) | H52—O52—Na1x | 109 (3) |
H410i—K1—Na1i | 68.8 (9) | C22—O52—K2xii | 120.85 (15) |
H410i—K1—Na2i | 42.2 (9) | C22—O52—Na1x | 130.32 (15) |
H410i—K1—O11 | 105.4 (9) | C22—O52—H52 | 108 (3) |
H410i—K1—O12 | 133.8 (9) | C31—O61—H61 | 108 (3) |
H410i—K1—O81i | 84.0 (9) | C32—O62—H62 | 115 (3) |
H410i—K1—H28i | 99.9 (13) | Na1—O71—K2viii | 93.63 (8) |
H410i—K1—O82i | 68.5 (9) | H17—O71—K2viii | 106 (3) |
H410i—K1—O91 | 123.8 (9) | H17—O71—Na1 | 97 (3) |
H410i—K1—O92 | 37.0 (9) | H27—O71—K2viii | 118 (3) |
H410i—K1—O101i | 74.4 (8) | H27—O71—Na1 | 126 (3) |
H410i—K1—H210i | 89.0 (11) | H27—O71—H17 | 112 (4) |
H410i—K1—O102i | 14.1 (8) | Na2—O72—K2ix | 93.60 (8) |
Na2vi—K2—Na1i | 115.98 (2) | H47—O72—K2ix | 120 (2) |
O41ii—K2—Na1i | 124.35 (5) | H47—O72—Na2 | 129 (2) |
O41ii—K2—Na2vi | 99.48 (5) | H37—O72—K2ix | 105 (3) |
O42iii—K2—Na1i | 99.23 (5) | H37—O72—Na2 | 93 (3) |
O42iii—K2—Na2vi | 124.52 (5) | H37—O72—H47 | 111 (4) |
O42iii—K2—O41ii | 93.27 (6) | K2viii—O81—K1viii | 153.86 (9) |
O51iv—K2—Na1i | 112.81 (5) | Na1—O81—K1viii | 101.86 (10) |
O51iv—K2—Na2vi | 41.44 (4) | Na1—O81—K2viii | 85.05 (7) |
O51iv—K2—O41ii | 67.93 (6) | H18—O81—K1viii | 90 (3) |
O51iv—K2—O42iii | 147.93 (6) | H18—O81—K2viii | 103 (3) |
O52v—K2—Na1i | 41.51 (4) | H18—O81—Na1 | 133 (3) |
O52v—K2—Na2vi | 112.68 (5) | H28—O81—K1viii | 80 (3) |
O52v—K2—O41ii | 147.81 (6) | H28—O81—K2viii | 74 (3) |
O52v—K2—O42iii | 67.75 (6) | H28—O81—Na1 | 121 (3) |
O52v—K2—O51iv | 140.00 (6) | H28—O81—H18 | 106 (4) |
O71i—K2—Na1i | 38.41 (5) | K2viii—H28—K1viii | 170.2 (18) |
O71i—K2—Na2vi | 86.75 (5) | O81—H28—K1viii | 84 (4) |
O71i—K2—O41ii | 110.38 (7) | O81—H28—K2viii | 90 (4) |
O71i—K2—O42iii | 137.64 (7) | K2ix—O82—K1viii | 154.05 (9) |
O71i—K2—O51iv | 74.41 (6) | Na2—O82—K1viii | 102.28 (10) |
O71i—K2—O52v | 74.20 (6) | Na2—O82—K2ix | 84.90 (8) |
O72vi—K2—Na1i | 86.80 (5) | H48—O82—K1viii | 82 (3) |
O72vi—K2—Na2vi | 38.41 (5) | H48—O82—K2ix | 73 (3) |
O72vi—K2—O41ii | 137.89 (7) | H48—O82—Na2 | 120 (3) |
O72vi—K2—O42iii | 110.30 (7) | H38—O82—K1viii | 84 (3) |
O72vi—K2—O51iv | 74.24 (6) | H38—O82—K2ix | 110 (3) |
O72vi—K2—O52v | 74.27 (6) | H38—O82—Na2 | 131 (3) |
O72vi—K2—O71i | 75.22 (6) | H38—O82—H48 | 109 (4) |
O81i—K2—Na1i | 38.84 (4) | O82—H48—K2ix | 90 (3) |
O81i—K2—Na2vi | 150.45 (5) | H29—O91—K1 | 145 (3) |
O81i—K2—O41ii | 91.18 (6) | H19—O91—K1 | 133 (3) |
O81i—K2—O42iii | 81.82 (6) | H19—O91—H29 | 81 (4) |
O81i—K2—O51iv | 122.56 (6) | H39—O92—K1 | 115 (4) |
O81i—K2—O52v | 61.48 (6) | H49—O92—K1 | 142 (3) |
O81i—K2—O71i | 63.71 (6) | H49—O92—H39 | 103 (5) |
O81i—K2—O72vi | 125.44 (6) | Na1—O101—K1viii | 94.95 (10) |
H28i—K2—Na1i | 49.1 (9) | H210—O101—K1viii | 64 (3) |
H28i—K2—Na2vi | 164.9 (10) | H210—O101—Na1 | 120 (3) |
H28i—K2—O41ii | 89.9 (8) | H110—O101—K1viii | 97 (3) |
H28i—K2—O42iii | 66.2 (9) | H110—O101—Na1 | 131 (3) |
H28i—K2—O51iv | 135.7 (9) | H110—O101—H210 | 108 (4) |
H28i—K2—O52v | 59.1 (8) | O101—H210—K1viii | 101 (3) |
H28i—K2—O71i | 78.8 (10) | Na2—O102—K1viii | 94.70 (10) |
H28i—K2—O72vi | 131.2 (9) | H410—O102—K1viii | 57 (3) |
H28i—K2—O81i | 15.8 (9) | H410—O102—Na2 | 121 (3) |
O82vi—K2—Na1i | 150.46 (5) | H310—O102—K1viii | 99 (3) |
O82vi—K2—Na2vi | 38.85 (4) | H310—O102—Na2 | 128 (3) |
O82vi—K2—O41ii | 82.03 (6) | H310—O102—H410 | 109 (4) |
O82vi—K2—O42iii | 91.40 (6) | O102—H410—K1viii | 109 (3) |
O82vi—K2—O51iv | 61.36 (6) | O21—C11—O11 | 126.6 (2) |
O82vi—K2—O52v | 122.42 (6) | C21—C11—O11 | 116.6 (2) |
O82vi—K2—O71i | 125.39 (6) | C21—C11—O21 | 116.8 (2) |
O82vi—K2—O72vi | 63.65 (6) | C11—C21—O51 | 110.4 (2) |
O82vi—K2—O81i | 170.14 (5) | H21—C21—O51 | 107.3 (17) |
O82vi—K2—H28i | 155.8 (10) | H21—C21—C11 | 109.4 (17) |
H48vi—K2—Na1i | 165.4 (10) | C31—C21—O51 | 109.7 (2) |
H48vi—K2—Na2vi | 49.5 (9) | C31—C21—C11 | 110.6 (2) |
H48vi—K2—O41ii | 65.7 (9) | C31—C21—H21 | 109.3 (16) |
H48vi—K2—O42iii | 90.2 (9) | C21—C31—O61 | 110.4 (2) |
H48vi—K2—O51iv | 58.7 (8) | H31—C31—O61 | 105.2 (17) |
H48vi—K2—O52v | 136.2 (9) | H31—C31—C21 | 109.9 (16) |
H48vi—K2—O71i | 131.2 (9) | C41—C31—O61 | 111.8 (2) |
H48vi—K2—O72vi | 79.4 (10) | C41—C31—C21 | 110.2 (2) |
H48vi—K2—O81i | 155.2 (10) | C41—C31—H31 | 109.2 (16) |
H48vi—K2—H28i | 145.5 (10) | O31—C41—Na2ii | 49.41 (13) |
H48vi—K2—O82vi | 16.5 (9) | O41—C41—Na2ii | 122.55 (19) |
K2viii—Na1—K1viii | 98.06 (4) | O41—C41—O31 | 125.9 (3) |
O11—Na1—K1viii | 88.29 (6) | C31—C41—Na2ii | 96.23 (16) |
O11—Na1—K2viii | 133.95 (6) | C31—C41—O31 | 116.9 (3) |
O32iii—Na1—K1viii | 140.40 (7) | C31—C41—O41 | 117.2 (3) |
O32iii—Na1—K2viii | 108.29 (6) | O22—C12—O12 | 126.3 (2) |
O32iii—Na1—O11 | 93.78 (7) | C22—C12—O12 | 117.2 (2) |
O52iii—Na1—K1viii | 92.31 (6) | C22—C12—O22 | 116.5 (2) |
O52iii—Na1—K2viii | 52.69 (5) | C12—C22—O52 | 110.9 (2) |
O52iii—Na1—O11 | 173.16 (8) | H22—C22—O52 | 108.2 (15) |
O52iii—Na1—O32iii | 81.42 (7) | H22—C22—C12 | 108.2 (15) |
O71—Na1—K1viii | 126.85 (7) | C32—C22—O52 | 109.5 (2) |
O71—Na1—K2viii | 47.96 (6) | C32—C22—C12 | 110.7 (2) |
O71—Na1—O11 | 92.50 (8) | C32—C22—H22 | 109.3 (14) |
O71—Na1—O32iii | 92.60 (8) | C22—C32—O62 | 110.5 (2) |
O71—Na1—O52iii | 92.60 (8) | H32—C32—O62 | 107.7 (18) |
O81—Na1—K1viii | 45.30 (7) | H32—C32—C22 | 110.6 (16) |
O81—Na1—K2viii | 56.11 (7) | C42—C32—O62 | 111.5 (2) |
O81—Na1—O11 | 104.89 (8) | C42—C32—C22 | 110.3 (2) |
O81—Na1—O32iii | 161.10 (9) | C42—C32—H32 | 106.2 (17) |
O81—Na1—O52iii | 80.22 (8) | O32—C42—Na1x | 49.50 (13) |
O81—Na1—O71 | 83.78 (9) | O42—C42—Na1x | 122.70 (19) |
O101—Na1—K1viii | 52.04 (8) | O42—C42—O32 | 126.1 (3) |
O101—Na1—K2viii | 127.34 (8) | C32—C42—Na1x | 96.27 (15) |
O101—Na1—O11 | 92.11 (9) | C32—C42—O32 | 116.6 (3) |
O101—Na1—O32iii | 88.36 (10) | C32—C42—O42 | 117.3 (3) |
| | | |
K1—O11—C11—O21 | −51.6 (2) | Na2ii—O51—C21—C31 | −11.9 (2) |
K1—O11—C11—C21 | 128.89 (17) | Na2ii—C41—C31—O61 | 63.01 (15) |
K1—O12—C12—O22 | −52.13 (19) | Na2ii—C41—C31—C21 | −60.18 (16) |
K1—O12—C12—C22 | 128.67 (16) | O11—C11—C21—O51 | −176.7 (2) |
K2vii—O41—C41—Na2ii | −73.15 (15) | O11—C11—C21—C31 | 61.7 (2) |
K2vii—O41—C41—O31 | −12.6 (2) | O12—C12—C22—O52 | −177.0 (2) |
K2vii—O41—C41—C31 | 168.60 (17) | O12—C12—C22—C32 | 61.3 (2) |
K2—O42iii—C42iii—Na1 | −72.99 (15) | O21—C11—C21—O51 | 3.8 (2) |
K2x—O42—C42—O32 | −12.1 (2) | O21—C11—C21—C31 | −117.8 (2) |
K2x—O42—C42—C32 | 168.53 (16) | O22—C12—C22—O52 | 3.7 (2) |
K2xi—O51—C21—C11 | 112.88 (17) | O22—C12—C22—C32 | −118.0 (2) |
K2xi—O51—C21—C31 | −124.94 (17) | O31—C41—C31—O61 | 15.7 (3) |
K2xii—O52—C22—C12 | 112.76 (17) | O31—C41—C31—C21 | −107.5 (3) |
K2xii—O52—C22—C32 | −124.82 (18) | O32—C42—C32—O62 | 15.5 (3) |
Na1—O11—C11—O21 | 76.5 (2) | O32—C42—C32—C22 | −107.7 (2) |
Na1—O11—C11—C21 | −103.01 (19) | O41—C41—C31—O61 | −165.3 (2) |
Na1x—O32—C42—O42 | −104.86 (17) | O41—C41—C31—C21 | 71.5 (3) |
Na1x—O32—C42—C32 | 74.47 (16) | O42—C42—C32—O62 | −165.1 (2) |
Na1x—O52—C22—C12 | −134.0 (2) | O42—C42—C32—C22 | 71.7 (2) |
Na1x—O52—C22—C32 | −11.6 (2) | O51—C21—C31—O61 | −68.1 (2) |
Na1x—C42—C32—O62 | 62.96 (15) | O51—C21—C31—C41 | 55.9 (2) |
Na1x—C42—C32—C22 | −60.17 (16) | O52—C22—C32—O62 | −68.1 (2) |
Na2—O12—C12—O22 | 76.5 (2) | O52—C22—C32—C42 | 55.6 (2) |
Na2—O12—C12—C22 | −102.68 (19) | O61—C31—C21—C11 | 54.0 (2) |
Na2ii—O31—C41—O41 | −104.76 (17) | O62—C32—C22—C12 | 54.5 (2) |
Na2ii—O31—C41—C31 | 74.08 (17) | C11—C21—C31—C41 | 178.0 (2) |
Na2ii—O51—C21—C11 | −134.0 (2) | C12—C22—C32—C42 | 178.1 (2) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (iv) x+1/2, −y+1/2, −z; (v) x+1/2, −y−1/2, −z; (vi) x+1, y, z−1; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (ix) x−1, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xii) x−1/2, −y−1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O51—H51···O21 | 0.78 (3) | 2.07 (4) | 2.601 (3) | 125 (3) |
O51—H51···O31i | 0.78 (3) | 2.71 (3) | 3.336 (3) | 139 (3) |
O51—H51···O41i | 0.78 (3) | 2.88 (3) | 3.261 (3) | 113 (3) |
O52—H52···O22 | 0.79 (3) | 2.10 (4) | 2.603 (3) | 121 (3) |
O52—H52···O32i | 0.79 (3) | 2.67 (3) | 3.344 (3) | 144 (3) |
O52—H52···O42i | 0.79 (3) | 2.82 (3) | 3.256 (3) | 117 (3) |
O61—H61···O102ii | 0.76 (3) | 2.19 (3) | 2.899 (4) | 155 (4) |
O62—H62···O101x | 0.73 (3) | 2.21 (3) | 2.907 (4) | 162 (4) |
O71—H17···O61 | 0.77 (4) | 2.02 (4) | 2.790 (3) | 176 (4) |
O71—H27···O41ii | 0.83 (4) | 2.08 (4) | 2.875 (3) | 161 (4) |
O72—H47···O42x | 0.85 (4) | 2.04 (4) | 2.874 (3) | 166 (3) |
O72—H37···O62 | 0.82 (4) | 1.97 (4) | 2.788 (3) | 177 (4) |
O81—H18···O11viii | 0.91 (4) | 2.88 (4) | 3.375 (3) | 116 (3) |
O81—H18···O21viii | 0.91 (4) | 1.85 (4) | 2.749 (3) | 167 (4) |
O81—H28···O32xiii | 0.85 (5) | 1.86 (5) | 2.705 (3) | 170 (5) |
O82—H48···O31xiv | 0.89 (5) | 1.82 (5) | 2.699 (3) | 170 (5) |
O82—H38···O12viii | 0.85 (4) | 2.87 (4) | 3.374 (3) | 120 (3) |
O82—H38···O22viii | 0.85 (4) | 1.92 (5) | 2.753 (3) | 170 (4) |
O91—H29···O42i | 0.89 (4) | 1.94 (5) | 2.813 (4) | 166 (4) |
O91—H19···O22v | 0.89 (5) | 2.37 (5) | 3.111 (3) | 141 (4) |
O91—H19···O32iii | 0.89 (5) | 2.88 (5) | 3.163 (3) | 101 (3) |
O91—H19···O62iii | 0.89 (5) | 2.49 (5) | 3.140 (3) | 131 (4) |
O92—H39···O21xi | 0.78 (5) | 2.51 (5) | 3.116 (3) | 136 (4) |
O92—H39···O31vii | 0.78 (5) | 2.66 (5) | 3.166 (3) | 124 (4) |
O92—H39···O61vii | 0.78 (5) | 2.51 (5) | 3.139 (3) | 140 (4) |
O92—H49···O41i | 0.91 (5) | 1.91 (5) | 2.809 (4) | 170 (4) |
O101—H210···O91viii | 0.90 (5) | 1.87 (5) | 2.753 (4) | 168 (4) |
O101—H110···O12 | 0.81 (5) | 1.92 (5) | 2.727 (3) | 171 (4) |
O102—H410···O92viii | 0.88 (4) | 1.88 (4) | 2.759 (4) | 176 (4) |
O102—H310···O11 | 0.78 (5) | 1.95 (5) | 2.724 (3) | 174 (4) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (v) x+1/2, −y−1/2, −z; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xiii) x+1/2, −y−1/2, −z+2; (xiv) x−1/2, −y+1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (266K_anh)
top
Crystal data top
C4H12KNaO10 | F(000) = 585.519 |
Mr = 282.22 | Dx = 1.785 Mg m−3 |
Monoclinic, P2111 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.8565 (8) Å | Cell parameters from 6756 reflections |
b = 14.2444 (11) Å | θ = 3.5–28.7° |
c = 6.2171 (4) Å | µ = 0.59 mm−1 |
β = 90° | T = 266 K |
V = 1050.00 (13) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 5157 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 4178 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.770, Tmax = 1.000 | l = −8→8 |
18373 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.040 | w = 1/[σ2(Fo2) + (0.0248P)2 + 0.3311P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.082 | (Δ/σ)max = −0.001 |
S = 1.08 | Δρmax = 0.32 e Å−3 |
5157 reflections | Δρmin = −0.38 e Å−3 |
386 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
3 restraints | Absolute structure parameter: 0.02 (2) |
24 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.00071 (19) | −0.00025 (14) | 0.0459 (2) | 0.0554 (5) | |
K2 | 0.50010 (7) | 0.00022 (5) | −0.15947 (9) | 0.03272 (15) | |
Na1 | 0.23142 (10) | −0.00689 (8) | 0.52173 (18) | 0.0274 (3) | |
Na2 | −0.23172 (10) | 0.00687 (8) | 0.52034 (18) | 0.0270 (3) | |
O11 | 0.12014 (17) | 0.10898 (14) | 0.3501 (3) | 0.0256 (4) | |
O12 | −0.12011 (17) | −0.10912 (14) | 0.3495 (3) | 0.0261 (4) | |
O21 | 0.21020 (19) | 0.20293 (14) | 0.1188 (3) | 0.0306 (5) | |
O22 | −0.21030 (19) | −0.20281 (14) | 0.1183 (3) | 0.0309 (5) | |
O31 | 0.2315 (2) | 0.40640 (15) | 0.8149 (3) | 0.0368 (5) | |
O32 | −0.2329 (2) | −0.40640 (15) | 0.8141 (3) | 0.0363 (5) | |
O41 | 0.05214 (19) | 0.36130 (16) | 0.8448 (3) | 0.0351 (5) | |
O42 | −0.05297 (19) | −0.36191 (16) | 0.8447 (3) | 0.0354 (5) | |
O51 | 0.16378 (18) | 0.35722 (14) | 0.3246 (3) | 0.0264 (5) | |
H51 | 0.188 (3) | 0.342 (3) | 0.216 (6) | 0.0396 (7)* | |
O52 | −0.16373 (19) | −0.35729 (14) | 0.3238 (3) | 0.0269 (5) | |
H52 | −0.190 (3) | −0.344 (3) | 0.204 (6) | 0.0404 (7)* | |
O61 | 0.29535 (18) | 0.24816 (15) | 0.6301 (3) | 0.0285 (5) | |
H61 | 0.327 (3) | 0.285 (2) | 0.587 (6) | 0.0428 (7)* | |
O62 | −0.29555 (18) | −0.24831 (15) | 0.6280 (3) | 0.0296 (5) | |
H62 | −0.328 (3) | −0.295 (2) | 0.600 (6) | 0.0444 (7)* | |
O71 | 0.39566 (19) | 0.08237 (17) | 0.4844 (4) | 0.0333 (5) | |
H17 | 0.371 (4) | 0.127 (3) | 0.522 (7) | 0.0500 (8)* | |
H27 | 0.436 (4) | 0.090 (3) | 0.376 (6) | 0.0500 (8)* | |
O72 | −0.39570 (19) | −0.08231 (17) | 0.4851 (4) | 0.0336 (5) | |
H47 | −0.429 (3) | −0.096 (3) | 0.369 (6) | 0.0505 (8)* | |
H37 | −0.372 (4) | −0.131 (3) | 0.532 (6) | 0.0505 (8)* | |
O81 | 0.2429 (2) | 0.04159 (18) | 0.8850 (3) | 0.0461 (7) | |
H18 | 0.236 (4) | 0.096 (3) | 0.945 (7) | 0.0692 (10)* | |
H28 | 0.255 (5) | 0.001 (3) | 0.984 (8) | 0.0692 (10)* | |
O82 | −0.2416 (3) | −0.04120 (18) | 0.8832 (3) | 0.0469 (7) | |
H48 | −0.255 (5) | 0.001 (3) | 0.982 (8) | 0.0704 (10)* | |
H38 | −0.236 (4) | −0.093 (3) | 0.948 (7) | 0.0704 (10)* | |
O91 | 0.0611 (2) | −0.1971 (2) | −0.0348 (5) | 0.0547 (8) | |
H29 | 0.034 (5) | −0.254 (4) | −0.081 (7) | 0.0820 (11)* | |
H19 | 0.113 (5) | −0.209 (4) | 0.021 (8) | 0.0820 (11)* | |
O92 | −0.0610 (2) | 0.1959 (2) | −0.0339 (4) | 0.0517 (7) | |
H39 | −0.118 (5) | 0.231 (4) | 0.005 (8) | 0.0776 (11)* | |
H49 | −0.032 (5) | 0.250 (3) | −0.081 (7) | 0.0776 (11)* | |
O101 | 0.0758 (2) | −0.1032 (2) | 0.5802 (5) | 0.0544 (7) | |
H210 | 0.070 (4) | −0.142 (4) | 0.700 (8) | 0.0815 (11)* | |
H110 | 0.017 (5) | −0.108 (3) | 0.519 (7) | 0.0815 (11)* | |
O102 | −0.0769 (2) | 0.1044 (2) | 0.5757 (5) | 0.0508 (7) | |
H410 | −0.052 (4) | 0.088 (4) | 0.682 (7) | 0.0762 (11)* | |
H310 | −0.012 (5) | 0.103 (3) | 0.525 (7) | 0.0762 (11)* | |
C11 | 0.1544 (2) | 0.1878 (2) | 0.2846 (4) | 0.0217 (6) | |
C21 | 0.1249 (2) | 0.27288 (19) | 0.4233 (4) | 0.0213 (6) | |
H21 | 0.042 (3) | 0.273 (2) | 0.434 (4) | 0.0255 (7)* | |
C31 | 0.1778 (2) | 0.2640 (2) | 0.6468 (4) | 0.0227 (6) | |
H31 | 0.147 (3) | 0.211 (2) | 0.725 (5) | 0.0272 (7)* | |
C41 | 0.1518 (3) | 0.3512 (2) | 0.7809 (4) | 0.0271 (6) | |
C12 | −0.1543 (2) | −0.1876 (2) | 0.2845 (4) | 0.0215 (6) | |
C22 | −0.1251 (2) | −0.27343 (19) | 0.4226 (4) | 0.0209 (6) | |
H22 | −0.038 (3) | −0.276 (2) | 0.438 (4) | 0.0251 (7)* | |
C32 | −0.1782 (2) | −0.2644 (2) | 0.6453 (4) | 0.0229 (6) | |
H32 | −0.146 (3) | −0.206 (2) | 0.722 (5) | 0.0275 (7)* | |
C42 | −0.1523 (3) | −0.3512 (2) | 0.7791 (4) | 0.0272 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0667 (11) | 0.0552 (12) | 0.0442 (10) | −0.0309 (11) | 0.0019 (12) | 0.0005 (9) |
K2 | 0.0320 (3) | 0.0377 (3) | 0.0285 (3) | −0.0036 (3) | −0.0004 (3) | 0.0003 (2) |
Na1 | 0.0261 (6) | 0.0252 (6) | 0.0310 (6) | −0.0007 (5) | −0.0009 (5) | 0.0013 (4) |
Na2 | 0.0260 (6) | 0.0249 (6) | 0.0302 (6) | −0.0005 (5) | 0.0014 (5) | −0.0005 (4) |
O11 | 0.0280 (11) | 0.0206 (11) | 0.0281 (10) | −0.0019 (8) | −0.0010 (8) | −0.0007 (8) |
O12 | 0.0288 (11) | 0.0218 (11) | 0.0277 (10) | −0.0018 (8) | 0.0007 (8) | 0.0010 (8) |
O21 | 0.0396 (12) | 0.0289 (12) | 0.0231 (10) | −0.0004 (10) | 0.0074 (9) | −0.0010 (8) |
O22 | 0.0400 (12) | 0.0276 (11) | 0.0251 (10) | 0.0001 (10) | −0.0071 (9) | 0.0019 (8) |
O31 | 0.0487 (14) | 0.0277 (12) | 0.0338 (11) | −0.0082 (11) | −0.0040 (10) | −0.0066 (9) |
O32 | 0.0476 (14) | 0.0274 (12) | 0.0340 (11) | −0.0071 (11) | 0.0034 (10) | 0.0068 (8) |
O41 | 0.0344 (12) | 0.0441 (14) | 0.0267 (10) | 0.0125 (10) | −0.0001 (9) | −0.0065 (9) |
O42 | 0.0361 (12) | 0.0420 (14) | 0.0280 (11) | 0.0128 (10) | −0.0012 (9) | 0.0084 (9) |
O51 | 0.0391 (12) | 0.0198 (11) | 0.0204 (10) | −0.0014 (9) | 0.0011 (9) | −0.0002 (8) |
O52 | 0.0401 (12) | 0.0213 (11) | 0.0194 (9) | 0.0002 (9) | −0.0006 (9) | −0.0003 (8) |
O61 | 0.0239 (12) | 0.0270 (13) | 0.0347 (12) | 0.0042 (9) | −0.0041 (9) | 0.0014 (9) |
O62 | 0.0244 (11) | 0.0269 (12) | 0.0376 (12) | 0.0035 (9) | 0.0038 (9) | 0.0012 (9) |
O71 | 0.0274 (12) | 0.0320 (13) | 0.0406 (13) | 0.0011 (10) | 0.0084 (10) | 0.0018 (10) |
O72 | 0.0308 (12) | 0.0295 (13) | 0.0406 (13) | −0.0007 (10) | −0.0065 (10) | −0.0015 (10) |
O81 | 0.085 (2) | 0.0267 (13) | 0.0264 (11) | 0.0097 (13) | 0.0059 (12) | 0.0002 (9) |
O82 | 0.089 (2) | 0.0256 (13) | 0.0257 (11) | 0.0109 (13) | −0.0044 (13) | −0.0008 (9) |
O91 | 0.0346 (15) | 0.084 (2) | 0.0453 (16) | −0.0075 (15) | −0.0097 (12) | 0.0083 (14) |
O92 | 0.0328 (14) | 0.076 (2) | 0.0460 (15) | −0.0034 (13) | 0.0081 (11) | −0.0062 (14) |
O101 | 0.0321 (14) | 0.0588 (18) | 0.072 (2) | −0.0145 (12) | −0.0142 (13) | 0.0263 (14) |
O102 | 0.0291 (14) | 0.0560 (17) | 0.0672 (19) | −0.0126 (12) | 0.0106 (13) | −0.0201 (15) |
C11 | 0.0190 (13) | 0.0245 (16) | 0.0215 (13) | 0.0030 (11) | −0.0055 (11) | −0.0013 (10) |
C21 | 0.0229 (15) | 0.0191 (14) | 0.0218 (13) | −0.0013 (11) | −0.0008 (11) | 0.0008 (10) |
C31 | 0.0243 (15) | 0.0218 (15) | 0.0219 (13) | 0.0017 (11) | 0.0007 (11) | 0.0023 (11) |
C41 | 0.0387 (17) | 0.0251 (16) | 0.0176 (13) | 0.0044 (13) | −0.0054 (12) | 0.0006 (10) |
C12 | 0.0213 (14) | 0.0224 (15) | 0.0207 (13) | 0.0022 (11) | 0.0049 (11) | −0.0001 (10) |
C22 | 0.0243 (15) | 0.0188 (14) | 0.0197 (13) | 0.0006 (11) | 0.0001 (11) | −0.0002 (10) |
C32 | 0.0227 (14) | 0.0232 (15) | 0.0229 (13) | 0.0007 (11) | −0.0008 (11) | 0.0002 (11) |
C42 | 0.0393 (18) | 0.0241 (16) | 0.0182 (13) | 0.0031 (13) | 0.0052 (12) | −0.0018 (10) |
Geometric parameters (Å, º) top
K1—O11 | 2.828 (3) | O21—C11 | 1.244 (3) |
K1—O12 | 2.832 (3) | O22—C12 | 1.247 (3) |
K1—O81i | 3.099 (4) | O31—C41 | 1.248 (4) |
K1—H28i | 3.04 (5) | O32—C42 | 1.257 (4) |
K1—O82i | 3.101 (4) | O41—C41 | 1.255 (4) |
K1—H48i | 3.06 (6) | O42—C42 | 1.255 (4) |
K1—O91 | 2.937 (4) | O51—H51 | 0.76 (4) |
K1—O92 | 2.931 (4) | O51—C21 | 1.426 (3) |
K1—O101i | 3.365 (4) | O52—H52 | 0.83 (4) |
K1—H210i | 3.07 (5) | O52—C22 | 1.419 (3) |
K1—O102i | 3.409 (4) | O61—H61 | 0.70 (3) |
K1—H410i | 2.66 (5) | O61—C31 | 1.416 (4) |
K2—O41ii | 2.845 (2) | O62—H62 | 0.78 (3) |
K2—O42iii | 2.848 (2) | O62—C32 | 1.414 (4) |
K2—O51iv | 2.991 (2) | O71—H17 | 0.74 (4) |
K2—O52v | 2.993 (2) | O71—H27 | 0.83 (4) |
K2—O71i | 2.794 (2) | O72—H47 | 0.84 (4) |
K2—H17i | 3.09 (4) | O72—H37 | 0.80 (4) |
K2—O72vi | 2.791 (2) | O81—H18 | 0.86 (5) |
K2—H37vi | 3.08 (4) | O81—H28 | 0.86 (5) |
K2—O81i | 3.118 (3) | O82—H48 | 0.87 (5) |
K2—H28i | 3.04 (5) | O82—H38 | 0.85 (5) |
K2—O82vi | 3.130 (3) | O91—H29 | 0.91 (5) |
K2—H48vi | 3.03 (6) | O91—H19 | 0.72 (5) |
Na1—O11 | 2.368 (2) | O92—H39 | 0.87 (5) |
Na1—O32iii | 2.462 (2) | O92—H49 | 0.90 (5) |
Na1—O52iii | 2.493 (2) | O101—H210 | 0.93 (5) |
Na1—O71 | 2.337 (3) | O101—H110 | 0.79 (5) |
Na1—O81 | 2.365 (2) | O102—H410 | 0.76 (4) |
Na1—O101 | 2.328 (3) | O102—H310 | 0.83 (5) |
Na1—C42iii | 3.079 (3) | C11—C21 | 1.528 (4) |
Na2—O12 | 2.368 (2) | C21—H21 | 0.98 (3) |
Na2—O31vii | 2.463 (2) | C21—C31 | 1.529 (4) |
Na2—O51vii | 2.492 (2) | C31—H31 | 0.98 (3) |
Na2—O72 | 2.333 (3) | C31—C41 | 1.527 (4) |
Na2—O82 | 2.361 (2) | C12—C22 | 1.534 (4) |
Na2—O102 | 2.327 (3) | C22—H22 | 1.04 (3) |
Na2—C41vii | 3.083 (3) | C22—C32 | 1.526 (4) |
O11—C11 | 1.261 (3) | C32—H32 | 1.03 (3) |
O12—C12 | 1.256 (3) | C32—C42 | 1.522 (4) |
| | | |
Na2i—K1—Na1i | 80.19 (3) | O52iii—Na1—O11 | 173.23 (8) |
O11—K1—Na1i | 101.66 (7) | O52iii—Na1—O32iii | 81.49 (8) |
O11—K1—Na2i | 145.12 (8) | O71—Na1—K1viii | 126.85 (8) |
O12—K1—Na1i | 145.43 (8) | O71—Na1—K2viii | 47.99 (6) |
O12—K1—Na2i | 101.33 (7) | O71—Na1—O11 | 92.30 (8) |
O12—K1—O11 | 96.25 (7) | O71—Na1—O32iii | 92.60 (9) |
O81i—K1—Na1i | 33.00 (5) | O71—Na1—O52iii | 92.59 (9) |
O81i—K1—Na2i | 110.24 (6) | O81—Na1—K1viii | 45.53 (8) |
O81i—K1—O11 | 69.27 (8) | O81—Na1—K2viii | 55.88 (7) |
O81i—K1—O12 | 142.11 (11) | O81—Na1—O11 | 105.02 (9) |
H28i—K1—Na1i | 42.8 (10) | O81—Na1—O32iii | 161.09 (10) |
H28i—K1—Na2i | 122.9 (10) | O81—Na1—O52iii | 80.19 (9) |
H28i—K1—O11 | 65.5 (9) | O81—Na1—O71 | 83.59 (10) |
H28i—K1—O12 | 126.0 (10) | O101—Na1—K1viii | 51.96 (9) |
H28i—K1—O81i | 16.1 (10) | O101—Na1—K2viii | 127.31 (8) |
O82i—K1—Na1i | 109.98 (6) | O101—Na1—O11 | 92.26 (9) |
O82i—K1—Na2i | 32.67 (5) | O101—Na1—O32iii | 88.46 (10) |
O82i—K1—O11 | 141.74 (11) | O101—Na1—O52iii | 82.98 (9) |
O82i—K1—O12 | 69.26 (8) | O101—Na1—O71 | 175.24 (11) |
O82i—K1—O81i | 142.13 (8) | O101—Na1—O81 | 93.92 (11) |
O82i—K1—H28i | 151.5 (9) | C42iii—Na1—K1viii | 140.11 (7) |
H48i—K1—Na1i | 122.5 (10) | C42iii—Na1—K2viii | 87.60 (6) |
H48i—K1—Na2i | 42.4 (10) | C42iii—Na1—O11 | 115.68 (8) |
H48i—K1—O11 | 125.5 (10) | C42iii—Na1—O32iii | 22.94 (7) |
H48i—K1—O12 | 65.7 (9) | C42iii—Na1—O52iii | 60.08 (7) |
H48i—K1—O81i | 151.1 (10) | C42iii—Na1—O71 | 85.61 (9) |
H48i—K1—H28i | 165.2 (10) | C42iii—Na1—O81 | 138.19 (10) |
H48i—K1—O82i | 16.3 (10) | C42iii—Na1—O101 | 93.63 (11) |
O91—K1—Na1i | 72.04 (7) | K2ix—Na2—K1viii | 98.05 (4) |
O91—K1—Na2i | 92.84 (7) | O12—Na2—K1viii | 88.04 (7) |
O91—K1—O11 | 121.14 (11) | O12—Na2—K2ix | 133.92 (6) |
O91—K1—O12 | 73.39 (8) | O31vii—Na2—K1viii | 140.63 (7) |
O91—K1—O81i | 84.42 (10) | O31vii—Na2—K2ix | 108.17 (7) |
O91—K1—H28i | 75.0 (9) | O31vii—Na2—O12 | 93.99 (8) |
O91—K1—O82i | 89.47 (9) | O51vii—Na2—K1viii | 92.50 (7) |
O91—K1—H48i | 103.0 (9) | O51vii—Na2—K2ix | 52.65 (5) |
O92—K1—Na1i | 92.96 (7) | O51vii—Na2—O12 | 173.24 (8) |
O92—K1—Na2i | 71.74 (7) | O51vii—Na2—O31vii | 81.33 (7) |
O92—K1—O11 | 73.39 (8) | O72—Na2—K1viii | 126.58 (8) |
O92—K1—O12 | 120.59 (11) | O72—Na2—K2ix | 47.91 (6) |
O92—K1—O81i | 89.61 (9) | O72—Na2—O12 | 92.51 (8) |
O92—K1—H28i | 102.8 (9) | O72—Na2—O31vii | 92.66 (9) |
O92—K1—O82i | 83.83 (10) | O72—Na2—O51vii | 92.57 (9) |
O92—K1—H48i | 74.0 (9) | O82—Na2—K1viii | 45.14 (8) |
O92—K1—O91 | 160.41 (10) | O82—Na2—K2ix | 56.20 (8) |
O101i—K1—Na1i | 33.02 (5) | O82—Na2—O12 | 104.69 (9) |
O101i—K1—Na2i | 61.53 (6) | O82—Na2—O31vii | 161.08 (10) |
O101i—K1—O11 | 133.02 (10) | O82—Na2—O51vii | 80.30 (8) |
O101i—K1—O12 | 117.95 (9) | O82—Na2—O72 | 83.71 (10) |
O101i—K1—O81i | 63.95 (8) | O102—Na2—K1viii | 52.63 (9) |
O101i—K1—H28i | 68.3 (9) | O102—Na2—K2ix | 127.24 (8) |
O101i—K1—O82i | 83.25 (7) | O102—Na2—O12 | 92.39 (9) |
O101i—K1—H48i | 98.8 (10) | O102—Na2—O31vii | 88.00 (10) |
O101i—K1—O91 | 51.16 (8) | O102—Na2—O51vii | 82.62 (9) |
O101i—K1—O92 | 109.59 (9) | O102—Na2—O72 | 175.00 (11) |
H210i—K1—Na1i | 43.5 (9) | O102—Na2—O82 | 94.08 (11) |
H210i—K1—Na2i | 69.7 (9) | C41vii—Na2—K1viii | 140.25 (7) |
H210i—K1—O11 | 134.2 (9) | C41vii—Na2—K2ix | 87.67 (6) |
H210i—K1—O12 | 104.1 (10) | C41vii—Na2—O12 | 115.81 (8) |
H210i—K1—O81i | 69.5 (9) | C41vii—Na2—O31vii | 22.65 (7) |
H210i—K1—H28i | 69.3 (13) | C41vii—Na2—O51vii | 60.18 (7) |
H210i—K1—O82i | 84.1 (9) | C41vii—Na2—O72 | 85.79 (9) |
H210i—K1—H48i | 100.3 (14) | C41vii—Na2—O82 | 138.49 (10) |
H210i—K1—O91 | 35.4 (10) | C41vii—Na2—O102 | 92.97 (11) |
H210i—K1—O92 | 125.2 (10) | Na1—O11—K1 | 101.36 (8) |
H210i—K1—O101i | 15.7 (9) | C11—O11—K1 | 115.77 (16) |
O102i—K1—Na1i | 61.73 (5) | C11—O11—Na1 | 125.94 (17) |
O102i—K1—Na2i | 32.86 (5) | Na2—O12—K1 | 101.50 (9) |
O102i—K1—O11 | 117.91 (9) | C12—O12—K1 | 115.89 (16) |
O102i—K1—O12 | 132.44 (10) | C12—O12—Na2 | 125.79 (17) |
O102i—K1—O81i | 83.63 (7) | C41—O31—Na2ii | 107.87 (17) |
O102i—K1—H28i | 99.1 (10) | C42—O32—Na1x | 107.30 (17) |
O102i—K1—O82i | 63.41 (8) | C41—O41—K2vii | 120.07 (19) |
O102i—K1—H48i | 67.5 (9) | C42—O42—K2x | 120.97 (19) |
O102i—K1—O91 | 109.69 (9) | Na2ii—O51—K2xi | 85.87 (7) |
O102i—K1—O92 | 50.96 (8) | H51—O51—K2xi | 98 (3) |
O102i—K1—O101i | 61.56 (7) | H51—O51—Na2ii | 112 (3) |
O102i—K1—H210i | 76.0 (9) | C21—O51—K2xi | 120.68 (16) |
H410i—K1—Na1i | 60.8 (11) | C21—O51—Na2ii | 130.46 (15) |
H410i—K1—Na2i | 35.8 (11) | C21—O51—H51 | 105 (3) |
H410i—K1—O11 | 115.1 (11) | Na1x—O52—K2xii | 85.83 (7) |
H410i—K1—O12 | 135.0 (11) | H52—O52—K2xii | 96 (3) |
H410i—K1—O81i | 81.5 (11) | H52—O52—Na1x | 109 (3) |
H410i—K1—H28i | 97.1 (15) | C22—O52—K2xii | 120.70 (16) |
H410i—K1—O82i | 66.1 (11) | C22—O52—Na1x | 130.36 (15) |
H410i—K1—H48i | 69.8 (15) | C22—O52—H52 | 109 (3) |
H410i—K1—O91 | 111.4 (11) | C31—O61—H61 | 116 (3) |
H410i—K1—O92 | 49.1 (11) | C32—O62—H62 | 111 (3) |
H410i—K1—O101i | 62.5 (11) | Na1—O71—K2viii | 93.58 (9) |
H410i—K1—H210i | 77.3 (14) | H17—O71—K2viii | 107 (3) |
H410i—K1—O102i | 3.0 (11) | H17—O71—Na1 | 96 (4) |
Na2vi—K2—Na1i | 116.09 (3) | H27—O71—K2viii | 116 (3) |
O41ii—K2—Na1i | 124.45 (6) | H27—O71—Na1 | 129 (3) |
O41ii—K2—Na2vi | 99.40 (5) | H27—O71—H17 | 112 (4) |
O42iii—K2—Na1i | 99.03 (5) | O71—H17—K2viii | 60 (3) |
O42iii—K2—Na2vi | 124.71 (6) | Na2—O72—K2ix | 93.75 (8) |
O42iii—K2—O41ii | 93.15 (6) | H47—O72—K2ix | 124 (3) |
O51iv—K2—Na1i | 112.80 (5) | H47—O72—Na2 | 126 (3) |
O51iv—K2—Na2vi | 41.48 (4) | H37—O72—K2ix | 103 (3) |
O51iv—K2—O41ii | 67.96 (6) | H37—O72—Na2 | 98 (3) |
O51iv—K2—O42iii | 148.13 (7) | H37—O72—H47 | 106 (4) |
O52v—K2—Na1i | 41.48 (4) | O72—H37—K2ix | 62 (3) |
O52v—K2—Na2vi | 112.72 (5) | K2viii—O81—K1viii | 153.96 (10) |
O52v—K2—O41ii | 147.84 (7) | Na1—O81—K1viii | 101.47 (10) |
O52v—K2—O42iii | 67.70 (6) | Na1—O81—K2viii | 85.22 (8) |
O52v—K2—O51iv | 139.96 (6) | H18—O81—K1viii | 87 (3) |
O71i—K2—Na1i | 38.43 (5) | H18—O81—K2viii | 108 (3) |
O71i—K2—Na2vi | 86.82 (5) | H18—O81—Na1 | 132 (3) |
O71i—K2—O41ii | 110.52 (7) | H28—O81—K1viii | 78 (4) |
O71i—K2—O42iii | 137.45 (7) | H28—O81—K2viii | 77 (4) |
O71i—K2—O51iv | 74.38 (6) | H28—O81—Na1 | 120 (3) |
O71i—K2—O52v | 74.16 (6) | H28—O81—H18 | 108 (4) |
H17i—K2—Na1i | 42.0 (8) | K2viii—H28—K1viii | 170 (2) |
H17i—K2—Na2vi | 93.6 (8) | O81—H28—K1viii | 86 (4) |
H17i—K2—O41ii | 98.2 (8) | O81—H28—K2viii | 87 (4) |
H17i—K2—O42iii | 137.5 (8) | K2ix—O82—K1viii | 153.98 (10) |
H17i—K2—O51iv | 72.7 (8) | Na2—O82—K1viii | 102.19 (11) |
H17i—K2—O52v | 81.8 (8) | Na2—O82—K2ix | 84.99 (8) |
H17i—K2—O71i | 13.2 (8) | H48—O82—K1viii | 79 (4) |
O72vi—K2—Na1i | 86.92 (5) | H48—O82—K2ix | 76 (4) |
O72vi—K2—Na2vi | 38.34 (5) | H48—O82—Na2 | 119 (3) |
O72vi—K2—O41ii | 137.74 (7) | H38—O82—K1viii | 86 (3) |
O72vi—K2—O42iii | 110.53 (7) | H38—O82—K2ix | 106 (3) |
O72vi—K2—O51iv | 74.14 (6) | H38—O82—Na2 | 135 (3) |
O72vi—K2—O52v | 74.39 (6) | H38—O82—H48 | 107 (4) |
O72vi—K2—O71i | 75.23 (7) | K2ix—H48—K1viii | 171 (2) |
O72vi—K2—H17i | 87.5 (8) | O82—H48—K1viii | 85 (4) |
H37vi—K2—Na1i | 94.2 (8) | O82—H48—K2ix | 88 (4) |
H37vi—K2—Na2vi | 42.9 (8) | H29—O91—K1 | 144 (3) |
H37vi—K2—O41ii | 137.9 (8) | H19—O91—K1 | 111 (4) |
H37vi—K2—O42iii | 96.7 (8) | H19—O91—H29 | 103 (6) |
H37vi—K2—O51iv | 83.0 (8) | H39—O92—K1 | 134 (3) |
H37vi—K2—O52v | 72.2 (8) | H49—O92—K1 | 142 (3) |
H37vi—K2—O71i | 88.8 (8) | H49—O92—H39 | 83 (5) |
H37vi—K2—H17i | 101.5 (10) | Na1—O101—K1viii | 95.02 (11) |
H37vi—K2—O72vi | 14.7 (8) | H210—O101—K1viii | 64 (3) |
O81i—K2—Na1i | 38.90 (5) | H210—O101—Na1 | 122 (3) |
O81i—K2—Na2vi | 150.56 (5) | H110—O101—K1viii | 103 (3) |
O81i—K2—O41ii | 91.16 (7) | H110—O101—Na1 | 132 (3) |
O81i—K2—O42iii | 81.59 (7) | H110—O101—H210 | 106 (4) |
O81i—K2—O51iv | 122.46 (7) | O101—H210—K1viii | 101 (3) |
O81i—K2—O52v | 61.58 (6) | Na2—O102—K1viii | 94.51 (11) |
O81i—K2—O71i | 63.74 (7) | H410—O102—Na2 | 105 (4) |
O81i—K2—H17i | 57.5 (8) | H310—O102—K1viii | 94 (3) |
O81i—K2—O72vi | 125.63 (7) | H310—O102—Na2 | 131 (3) |
O81i—K2—H37vi | 130.7 (8) | H310—O102—H410 | 88 (4) |
H28i—K2—Na1i | 49.0 (10) | O102—H410—K1viii | 167 (5) |
H28i—K2—Na2vi | 164.9 (10) | O21—C11—O11 | 126.4 (3) |
H28i—K2—O41ii | 90.2 (9) | C21—C11—O11 | 116.8 (2) |
H28i—K2—O42iii | 65.7 (10) | C21—C11—O21 | 116.9 (2) |
H28i—K2—O51iv | 136.0 (9) | C11—C21—O51 | 110.6 (2) |
H28i—K2—O52v | 58.7 (9) | H21—C21—O51 | 110.1 (17) |
H28i—K2—O71i | 78.9 (10) | H21—C21—C11 | 105.7 (17) |
H28i—K2—H17i | 73.4 (13) | C31—C21—O51 | 109.2 (2) |
H28i—K2—O72vi | 131.0 (9) | C31—C21—C11 | 110.7 (2) |
H28i—K2—H37vi | 131.0 (12) | C31—C21—H21 | 110.5 (16) |
H28i—K2—O81i | 16.0 (10) | C21—C31—O61 | 110.5 (2) |
O82vi—K2—Na1i | 150.48 (5) | H31—C31—O61 | 106 (2) |
O82vi—K2—Na2vi | 38.81 (5) | H31—C31—C21 | 111.5 (18) |
O82vi—K2—O41ii | 81.96 (7) | C41—C31—O61 | 111.6 (2) |
O82vi—K2—O42iii | 91.57 (7) | C41—C31—C21 | 110.2 (2) |
O82vi—K2—O51iv | 61.47 (6) | C41—C31—H31 | 106.7 (18) |
O82vi—K2—O52v | 122.39 (7) | O31—C41—Na2ii | 49.48 (14) |
O82vi—K2—O71i | 125.44 (7) | O41—C41—Na2ii | 122.6 (2) |
O82vi—K2—H17i | 130.5 (8) | O41—C41—O31 | 126.0 (3) |
O82vi—K2—O72vi | 63.56 (7) | C31—C41—Na2ii | 96.41 (17) |
O82vi—K2—H37vi | 57.0 (8) | C31—C41—O31 | 116.9 (3) |
O82vi—K2—O81i | 170.05 (6) | C31—C41—O41 | 117.1 (3) |
O82vi—K2—H28i | 155.6 (10) | O22—C12—O12 | 126.3 (3) |
H48vi—K2—Na1i | 164.9 (10) | C22—C12—O12 | 117.2 (2) |
H48vi—K2—Na2vi | 48.9 (10) | C22—C12—O22 | 116.5 (2) |
H48vi—K2—O41ii | 65.9 (10) | C12—C22—O52 | 110.8 (2) |
H48vi—K2—O42iii | 90.9 (9) | H22—C22—O52 | 109.0 (16) |
H48vi—K2—O51iv | 58.4 (9) | H22—C22—C12 | 107.9 (16) |
H48vi—K2—O52v | 136.2 (9) | C32—C22—O52 | 109.3 (2) |
H48vi—K2—O71i | 130.7 (9) | C32—C22—C12 | 110.4 (2) |
H48vi—K2—H17i | 131.1 (12) | C32—C22—H22 | 109.4 (15) |
H48vi—K2—O72vi | 78.9 (10) | C22—C32—O62 | 110.5 (2) |
H48vi—K2—H37vi | 73.2 (13) | H32—C32—O62 | 105.6 (19) |
H48vi—K2—O81i | 155.5 (10) | H32—C32—C22 | 109.5 (17) |
H48vi—K2—H28i | 146.1 (10) | C42—C32—O62 | 111.8 (2) |
H48vi—K2—O82vi | 16.2 (10) | C42—C32—C22 | 110.1 (2) |
K2viii—Na1—K1viii | 98.08 (4) | C42—C32—H32 | 109.2 (17) |
O11—Na1—K1viii | 88.38 (7) | O32—C42—Na1x | 49.76 (14) |
O11—Na1—K2viii | 133.82 (6) | O42—C42—Na1x | 122.53 (19) |
O32iii—Na1—K1viii | 140.42 (7) | O42—C42—O32 | 125.6 (3) |
O32iii—Na1—K2viii | 108.39 (7) | C32—C42—Na1x | 96.37 (16) |
O32iii—Na1—O11 | 93.61 (8) | C32—C42—O32 | 116.7 (3) |
O52iii—Na1—K1viii | 92.43 (7) | C32—C42—O42 | 117.8 (3) |
O52iii—Na1—K2viii | 52.70 (5) | | |
| | | |
K1—O11—C11—O21 | −51.6 (2) | Na2ii—O51—C21—C31 | −11.7 (2) |
K1—O11—C11—C21 | 128.74 (17) | Na2ii—C41—C31—O61 | 62.82 (16) |
K1—O12—C12—O22 | −51.9 (2) | Na2ii—C41—C31—C21 | −60.34 (17) |
K1—O12—C12—C22 | 128.32 (17) | O11—C11—C21—O51 | −177.1 (2) |
K2vii—O41—C41—Na2ii | −73.26 (16) | O11—C11—C21—C31 | 61.8 (3) |
K2vii—O41—C41—O31 | −12.5 (2) | O12—C12—C22—O52 | −176.8 (2) |
K2vii—O41—C41—C31 | 168.28 (18) | O12—C12—C22—C32 | 61.9 (3) |
K2—O42iii—C42iii—Na1 | −72.74 (16) | O21—C11—C21—O51 | 3.3 (3) |
K2x—O42—C42—O32 | −11.8 (2) | O21—C11—C21—C31 | −117.8 (3) |
K2x—O42—C42—C32 | 168.28 (18) | O22—C12—C22—O52 | 3.4 (3) |
K2xi—O51—C21—C11 | 112.94 (17) | O22—C12—C22—C32 | −117.8 (3) |
K2xi—O51—C21—C31 | −125.07 (18) | O31—C41—C31—O61 | 15.4 (3) |
K2xii—O52—C22—C12 | 113.15 (18) | O31—C41—C31—C21 | −107.8 (3) |
K2xii—O52—C22—C32 | −125.01 (18) | O32—C42—C32—O62 | 14.9 (3) |
Na1—O11—C11—O21 | 76.7 (2) | O32—C42—C32—C22 | −108.3 (3) |
Na1—O11—C11—C21 | −102.9 (2) | O41—C41—C31—O61 | −165.3 (3) |
Na1x—O32—C42—O42 | −105.14 (18) | O41—C41—C31—C21 | 71.5 (3) |
Na1x—O32—C42—C32 | 74.77 (17) | O42—C42—C32—O62 | −165.1 (2) |
Na1x—O52—C22—C12 | −133.7 (2) | O42—C42—C32—C22 | 71.6 (3) |
Na1x—O52—C22—C32 | −11.8 (2) | O51—C21—C31—O61 | −68.0 (2) |
Na1x—C42—C32—O62 | 62.78 (16) | O51—C21—C31—C41 | 55.7 (3) |
Na1x—C42—C32—C22 | −60.50 (17) | O52—C22—C32—O62 | −68.1 (2) |
Na2—O12—C12—O22 | 76.6 (2) | O52—C22—C32—C42 | 56.0 (3) |
Na2—O12—C12—C22 | −103.1 (2) | O61—C31—C21—C11 | 53.9 (3) |
Na2ii—O31—C41—O41 | −104.82 (18) | O62—C32—C22—C12 | 54.0 (3) |
Na2ii—O31—C41—C31 | 74.41 (17) | C11—C21—C31—C41 | 177.7 (2) |
Na2ii—O51—C21—C11 | −133.7 (2) | C12—C22—C32—C42 | 178.1 (2) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (iv) x+1/2, −y+1/2, −z; (v) x+1/2, −y−1/2, −z; (vi) x+1, y, z−1; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (ix) x−1, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xii) x−1/2, −y−1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O51—H51···O21 | 0.76 (4) | 2.09 (4) | 2.601 (3) | 125 (4) |
O51—H51···O31i | 0.76 (4) | 2.71 (4) | 3.344 (3) | 142 (4) |
O51—H51···O41i | 0.76 (4) | 2.83 (4) | 3.264 (3) | 119 (3) |
O52—H52···O22 | 0.83 (4) | 2.09 (4) | 2.604 (3) | 119 (3) |
O52—H52···O32i | 0.83 (4) | 2.63 (4) | 3.347 (3) | 145 (3) |
O52—H52···O42i | 0.83 (4) | 2.78 (4) | 3.256 (3) | 119 (3) |
O61—H61···O102ii | 0.70 (3) | 2.19 (3) | 2.889 (4) | 175 (4) |
O62—H62···O101x | 0.78 (3) | 2.16 (3) | 2.911 (4) | 160 (4) |
O71—H17···O61 | 0.74 (4) | 2.06 (4) | 2.794 (3) | 177 (5) |
O71—H27···O41ii | 0.83 (4) | 2.07 (4) | 2.877 (3) | 164 (4) |
O72—H47···O42x | 0.84 (4) | 2.07 (4) | 2.883 (3) | 161 (4) |
O72—H37···O62 | 0.80 (4) | 1.99 (5) | 2.792 (3) | 173 (4) |
O81—H18···O11viii | 0.86 (5) | 2.87 (5) | 3.376 (3) | 119 (4) |
O81—H18···O21viii | 0.86 (5) | 1.89 (5) | 2.746 (3) | 170 (4) |
O81—H28···O32xiii | 0.86 (5) | 1.84 (5) | 2.701 (3) | 174 (5) |
O82—H48···O31xiv | 0.87 (5) | 1.83 (5) | 2.703 (3) | 174 (5) |
O82—H38···O12viii | 0.85 (5) | 2.86 (5) | 3.379 (3) | 121 (4) |
O82—H38···O22viii | 0.85 (5) | 1.91 (5) | 2.753 (3) | 173 (5) |
O91—H29···O42i | 0.91 (5) | 1.92 (5) | 2.811 (4) | 167 (5) |
O91—H19···O22v | 0.72 (5) | 2.59 (6) | 3.106 (4) | 130 (5) |
O91—H19···O32iii | 0.72 (5) | 2.67 (6) | 3.165 (4) | 128 (5) |
O91—H19···O62iii | 0.72 (5) | 2.51 (5) | 3.146 (3) | 147 (5) |
O92—H39···O21xi | 0.87 (5) | 2.37 (5) | 3.117 (4) | 143 (4) |
O92—H39···O31vii | 0.87 (5) | 2.88 (5) | 3.167 (4) | 101 (4) |
O92—H39···O61vii | 0.87 (5) | 2.51 (5) | 3.136 (3) | 129 (4) |
O92—H49···O41i | 0.90 (5) | 1.93 (5) | 2.815 (4) | 170 (5) |
O101—H210···O91viii | 0.93 (5) | 1.83 (5) | 2.748 (4) | 169 (5) |
O101—H110···O12 | 0.79 (5) | 1.94 (5) | 2.731 (3) | 174 (5) |
O102—H410···O92viii | 0.76 (4) | 2.34 (5) | 2.761 (4) | 116 (5) |
O102—H310···O11 | 0.83 (5) | 1.91 (5) | 2.726 (3) | 167 (5) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (v) x+1/2, −y−1/2, −z; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xiii) x+1/2, −y−1/2, −z+2; (xiv) x−1/2, −y+1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (276K_anh)
top
Crystal data top
C4H12KNaO10 | F(000) = 585.519 |
Mr = 282.22 | Dx = 1.783 Mg m−3 |
Monoclinic, P2111 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.8629 (9) Å | Cell parameters from 6656 reflections |
b = 14.2500 (11) Å | θ = 3.6–28.7° |
c = 6.2199 (4) Å | µ = 0.59 mm−1 |
β = 90° | T = 276 K |
V = 1051.45 (13) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 5168 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 4009 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.053 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.752, Tmax = 1.000 | l = −8→8 |
18369 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.042 | w = 1/[σ2(Fo2) + (0.0265P)2 + 0.227P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.087 | (Δ/σ)max = −0.001 |
S = 1.09 | Δρmax = 0.36 e Å−3 |
5168 reflections | Δρmin = −0.38 e Å−3 |
386 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
3 restraints | Absolute structure parameter: 0.09 (3) |
24 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0009 (2) | −0.00035 (15) | 0.0460 (3) | 0.0593 (6) | |
K2 | 0.49999 (8) | 0.00023 (5) | −0.15928 (10) | 0.03526 (16) | |
Na1 | 0.23142 (11) | −0.00679 (8) | 0.52233 (19) | 0.0295 (3) | |
Na2 | −0.23151 (11) | 0.00682 (9) | 0.52071 (19) | 0.0295 (3) | |
O11 | 0.11993 (18) | 0.10889 (15) | 0.3506 (3) | 0.0275 (5) | |
O12 | −0.12008 (18) | −0.10902 (15) | 0.3500 (3) | 0.0283 (5) | |
O21 | 0.2103 (2) | 0.20285 (15) | 0.1191 (3) | 0.0330 (5) | |
O22 | −0.2097 (2) | −0.20295 (15) | 0.1180 (3) | 0.0327 (5) | |
O31 | 0.2318 (2) | 0.40641 (16) | 0.8145 (3) | 0.0391 (6) | |
O32 | −0.2334 (2) | −0.40611 (16) | 0.8131 (3) | 0.0391 (6) | |
O41 | 0.0526 (2) | 0.36146 (17) | 0.8445 (3) | 0.0373 (6) | |
O42 | −0.0533 (2) | −0.36215 (17) | 0.8447 (3) | 0.0376 (6) | |
O51 | 0.1635 (2) | 0.35704 (15) | 0.3246 (3) | 0.0282 (5) | |
H51 | 0.191 (3) | 0.340 (3) | 0.221 (6) | 0.0423 (8)* | |
O52 | −0.1633 (2) | −0.35732 (15) | 0.3238 (3) | 0.0289 (5) | |
H52 | −0.191 (3) | −0.344 (3) | 0.206 (6) | 0.0433 (8)* | |
O61 | 0.29519 (19) | 0.24801 (16) | 0.6294 (4) | 0.0310 (5) | |
H61 | 0.328 (3) | 0.289 (3) | 0.597 (7) | 0.0465 (8)* | |
O62 | −0.29572 (19) | −0.24827 (16) | 0.6274 (4) | 0.0311 (5) | |
H62 | −0.328 (3) | −0.293 (2) | 0.603 (6) | 0.0467 (8)* | |
O71 | 0.3954 (2) | 0.08225 (18) | 0.4845 (4) | 0.0354 (6) | |
H17 | 0.375 (4) | 0.127 (3) | 0.516 (7) | 0.0531 (9)* | |
H27 | 0.438 (4) | 0.092 (3) | 0.373 (7) | 0.0531 (9)* | |
O72 | −0.3958 (2) | −0.08223 (18) | 0.4851 (4) | 0.0354 (6) | |
H47 | −0.431 (4) | −0.094 (3) | 0.368 (7) | 0.0531 (8)* | |
H37 | −0.369 (4) | −0.131 (3) | 0.527 (7) | 0.0531 (8)* | |
O81 | 0.2433 (3) | 0.0416 (2) | 0.8849 (4) | 0.0488 (7) | |
H18 | 0.237 (4) | 0.097 (3) | 0.955 (7) | 0.0732 (11)* | |
H28 | 0.254 (5) | 0.004 (4) | 0.988 (9) | 0.0732 (11)* | |
O82 | −0.2422 (3) | −0.04122 (19) | 0.8841 (4) | 0.0500 (8) | |
H48 | −0.255 (5) | −0.001 (4) | 0.986 (9) | 0.0750 (11)* | |
H38 | −0.235 (5) | −0.095 (4) | 0.949 (7) | 0.0750 (11)* | |
O91 | 0.0615 (2) | −0.1975 (3) | −0.0347 (5) | 0.0586 (8) | |
H29 | 0.035 (5) | −0.252 (4) | −0.081 (8) | 0.0879 (12)* | |
H19 | 0.119 (5) | −0.223 (4) | 0.003 (9) | 0.0879 (12)* | |
O92 | −0.0610 (2) | 0.1963 (3) | −0.0340 (5) | 0.0559 (8) | |
H39 | −0.115 (5) | 0.221 (4) | −0.004 (9) | 0.0839 (12)* | |
H49 | −0.039 (5) | 0.258 (4) | −0.084 (7) | 0.0839 (12)* | |
O101 | 0.0754 (2) | −0.1025 (2) | 0.5815 (5) | 0.0587 (8) | |
H210 | 0.073 (5) | −0.143 (4) | 0.693 (8) | 0.0880 (13)* | |
H110 | 0.015 (5) | −0.107 (4) | 0.520 (7) | 0.0880 (13)* | |
O102 | −0.0768 (2) | 0.1042 (2) | 0.5771 (5) | 0.0546 (8) | |
H410 | −0.047 (5) | 0.086 (4) | 0.681 (8) | 0.0818 (12)* | |
H310 | −0.010 (5) | 0.101 (3) | 0.527 (7) | 0.0818 (12)* | |
C11 | 0.1542 (2) | 0.1878 (2) | 0.2849 (4) | 0.0229 (6) | |
C21 | 0.1248 (3) | 0.2732 (2) | 0.4234 (4) | 0.0230 (6) | |
H21 | 0.043 (3) | 0.275 (2) | 0.438 (5) | 0.0276 (7)* | |
C31 | 0.1778 (3) | 0.2641 (2) | 0.6466 (5) | 0.0250 (7) | |
H31 | 0.145 (3) | 0.205 (2) | 0.727 (5) | 0.0300 (8)* | |
C41 | 0.1516 (3) | 0.3512 (2) | 0.7810 (5) | 0.0298 (7) | |
C12 | −0.1543 (2) | −0.1877 (2) | 0.2839 (4) | 0.0236 (6) | |
C22 | −0.1252 (3) | −0.2729 (2) | 0.4224 (4) | 0.0224 (6) | |
H22 | −0.039 (3) | −0.277 (2) | 0.439 (4) | 0.0269 (7)* | |
C32 | −0.1783 (3) | −0.2642 (2) | 0.6458 (5) | 0.0241 (6) | |
H32 | −0.147 (3) | −0.212 (2) | 0.725 (5) | 0.0290 (8)* | |
C42 | −0.1525 (3) | −0.3514 (2) | 0.7798 (5) | 0.0294 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0698 (12) | 0.0605 (14) | 0.0474 (11) | −0.0335 (12) | 0.0022 (14) | 0.0004 (10) |
K2 | 0.0346 (3) | 0.0402 (4) | 0.0310 (3) | −0.0034 (3) | −0.0003 (3) | 0.0002 (3) |
Na1 | 0.0286 (7) | 0.0265 (7) | 0.0336 (6) | −0.0002 (5) | −0.0013 (5) | 0.0008 (5) |
Na2 | 0.0281 (7) | 0.0276 (7) | 0.0329 (6) | −0.0010 (5) | 0.0016 (5) | −0.0004 (5) |
O11 | 0.0307 (12) | 0.0226 (12) | 0.0292 (11) | −0.0029 (9) | −0.0014 (9) | −0.0007 (8) |
O12 | 0.0311 (12) | 0.0248 (13) | 0.0290 (11) | −0.0014 (9) | 0.0008 (9) | 0.0009 (9) |
O21 | 0.0425 (13) | 0.0306 (13) | 0.0259 (11) | 0.0002 (11) | 0.0082 (10) | −0.0013 (9) |
O22 | 0.0416 (13) | 0.0309 (13) | 0.0256 (11) | −0.0003 (11) | −0.0075 (10) | 0.0013 (9) |
O31 | 0.0502 (15) | 0.0321 (14) | 0.0349 (12) | −0.0072 (12) | −0.0047 (11) | −0.0081 (9) |
O32 | 0.0512 (15) | 0.0293 (13) | 0.0367 (12) | −0.0089 (12) | 0.0038 (11) | 0.0070 (9) |
O41 | 0.0382 (13) | 0.0452 (15) | 0.0285 (11) | 0.0131 (11) | −0.0007 (10) | −0.0079 (10) |
O42 | 0.0379 (13) | 0.0457 (15) | 0.0293 (12) | 0.0112 (11) | −0.0010 (10) | 0.0072 (10) |
O51 | 0.0404 (14) | 0.0211 (12) | 0.0231 (11) | 0.0001 (9) | 0.0005 (9) | 0.0004 (8) |
O52 | 0.0422 (14) | 0.0218 (12) | 0.0227 (10) | 0.0010 (10) | 0.0001 (9) | −0.0006 (9) |
O61 | 0.0263 (13) | 0.0296 (14) | 0.0371 (12) | 0.0040 (10) | −0.0049 (10) | −0.0002 (10) |
O62 | 0.0259 (13) | 0.0284 (13) | 0.0390 (13) | 0.0045 (10) | 0.0053 (10) | 0.0016 (10) |
O71 | 0.0306 (13) | 0.0323 (14) | 0.0433 (14) | −0.0002 (11) | 0.0073 (10) | 0.0026 (11) |
O72 | 0.0297 (13) | 0.0329 (14) | 0.0436 (14) | 0.0003 (10) | −0.0079 (11) | −0.0023 (11) |
O81 | 0.090 (2) | 0.0305 (15) | 0.0263 (12) | 0.0100 (14) | 0.0053 (14) | 0.0000 (10) |
O82 | 0.095 (2) | 0.0281 (14) | 0.0272 (12) | 0.0112 (15) | −0.0035 (14) | 0.0001 (10) |
O91 | 0.0381 (16) | 0.089 (3) | 0.0484 (17) | −0.0077 (16) | −0.0073 (13) | 0.0074 (16) |
O92 | 0.0366 (16) | 0.082 (2) | 0.0496 (16) | −0.0045 (15) | 0.0083 (13) | −0.0054 (15) |
O101 | 0.0341 (16) | 0.064 (2) | 0.078 (2) | −0.0162 (13) | −0.0175 (14) | 0.0307 (16) |
O102 | 0.0308 (15) | 0.0588 (19) | 0.074 (2) | −0.0124 (13) | 0.0113 (14) | −0.0211 (16) |
C11 | 0.0204 (15) | 0.0258 (17) | 0.0225 (14) | 0.0026 (12) | −0.0054 (12) | −0.0017 (11) |
C21 | 0.0268 (17) | 0.0210 (16) | 0.0213 (14) | −0.0002 (12) | 0.0005 (12) | −0.0010 (11) |
C31 | 0.0267 (16) | 0.0257 (17) | 0.0226 (14) | 0.0045 (13) | 0.0004 (12) | −0.0008 (12) |
C41 | 0.042 (2) | 0.0280 (18) | 0.0199 (14) | 0.0046 (15) | −0.0049 (14) | −0.0001 (12) |
C12 | 0.0222 (15) | 0.0260 (17) | 0.0228 (14) | 0.0031 (12) | 0.0045 (12) | −0.0001 (12) |
C22 | 0.0238 (16) | 0.0212 (16) | 0.0223 (14) | 0.0004 (12) | −0.0014 (12) | −0.0007 (11) |
C32 | 0.0261 (16) | 0.0240 (17) | 0.0223 (14) | 0.0010 (13) | −0.0021 (12) | −0.0013 (12) |
C42 | 0.042 (2) | 0.0274 (18) | 0.0192 (14) | 0.0041 (15) | 0.0051 (14) | −0.0003 (11) |
Geometric parameters (Å, º) top
K1—O11 | 2.829 (3) | O22—C12 | 1.243 (4) |
K1—O12 | 2.835 (3) | O31—C41 | 1.252 (4) |
K1—O81i | 3.104 (4) | O32—C42 | 1.254 (4) |
K1—H28i | 3.03 (6) | O41—C41 | 1.248 (4) |
K1—O82i | 3.109 (4) | O42—C42 | 1.253 (4) |
K1—H48i | 3.06 (6) | O51—H51 | 0.76 (4) |
K1—O91 | 2.943 (4) | O51—C21 | 1.421 (4) |
K1—O92 | 2.939 (4) | O52—H52 | 0.83 (4) |
K1—O101i | 3.353 (4) | O52—C22 | 1.423 (4) |
K1—O102i | 3.403 (4) | O61—H61 | 0.73 (3) |
K1—H410i | 2.64 (5) | O61—C31 | 1.416 (4) |
K2—O41ii | 2.847 (2) | O62—H62 | 0.76 (3) |
K2—O42iii | 2.847 (2) | O62—C32 | 1.416 (4) |
K2—O51iv | 2.993 (2) | O71—H17 | 0.70 (5) |
K2—O52v | 2.990 (2) | O71—H27 | 0.87 (4) |
K2—O71i | 2.796 (3) | O72—H47 | 0.86 (4) |
K2—H17i | 3.08 (5) | O72—H37 | 0.81 (5) |
K2—O72vi | 2.793 (3) | O81—H18 | 0.91 (5) |
K2—O81i | 3.114 (3) | O81—H28 | 0.84 (6) |
K2—H28i | 3.06 (6) | O82—H48 | 0.87 (6) |
K2—O82vi | 3.126 (3) | O82—H38 | 0.87 (5) |
K2—H48vi | 3.04 (6) | O91—H29 | 0.89 (5) |
Na1—O11 | 2.368 (2) | O91—H19 | 0.81 (6) |
Na1—O32iii | 2.463 (3) | O92—H39 | 0.76 (6) |
Na1—O52iii | 2.496 (3) | O92—H49 | 0.97 (5) |
Na1—O71 | 2.335 (3) | O101—H210 | 0.90 (5) |
Na1—O81 | 2.362 (3) | O101—H110 | 0.81 (6) |
Na1—O101 | 2.329 (3) | O102—H410 | 0.78 (5) |
Na1—C42iii | 3.083 (3) | O102—H310 | 0.85 (6) |
Na2—O12 | 2.366 (2) | C11—C21 | 1.531 (4) |
Na2—O31vii | 2.463 (3) | C21—H21 | 0.97 (3) |
Na2—O51vii | 2.498 (2) | C21—C31 | 1.530 (4) |
Na2—O72 | 2.336 (3) | C31—H31 | 1.05 (4) |
Na2—O82 | 2.365 (3) | C31—C41 | 1.528 (4) |
Na2—O102 | 2.327 (3) | C12—C22 | 1.529 (4) |
Na2—C41vii | 3.089 (4) | C22—H22 | 1.03 (3) |
O11—C11 | 1.263 (4) | C22—C32 | 1.531 (4) |
O12—C12 | 1.261 (4) | C32—H32 | 0.97 (4) |
O21—C11 | 1.246 (4) | C32—C42 | 1.528 (4) |
| | | |
Na2i—K1—Na1i | 80.21 (3) | O81—Na1—O71 | 83.59 (11) |
O11—K1—Na1i | 101.73 (8) | O101—Na1—K1viii | 51.71 (10) |
O11—K1—Na2i | 145.10 (9) | O101—Na1—K2viii | 127.37 (9) |
O12—K1—Na1i | 145.55 (9) | O101—Na1—O11 | 92.01 (10) |
O12—K1—Na2i | 101.35 (8) | O101—Na1—O32iii | 88.50 (11) |
O12—K1—O11 | 96.12 (7) | O101—Na1—O52iii | 83.27 (10) |
O81i—K1—Na1i | 32.97 (5) | O101—Na1—O71 | 175.37 (12) |
O81i—K1—Na2i | 110.23 (7) | O101—Na1—O81 | 93.85 (12) |
O81i—K1—O11 | 69.37 (8) | C42iii—Na1—K1viii | 140.15 (8) |
O81i—K1—O12 | 142.16 (12) | C42iii—Na1—K2viii | 87.68 (7) |
H28i—K1—Na1i | 43.1 (11) | C42iii—Na1—O11 | 115.51 (9) |
H28i—K1—Na2i | 123.2 (11) | C42iii—Na1—O32iii | 22.80 (8) |
H28i—K1—O11 | 64.7 (10) | C42iii—Na1—O52iii | 60.11 (8) |
H28i—K1—O12 | 126.4 (11) | C42iii—Na1—O71 | 85.54 (10) |
H28i—K1—O81i | 15.7 (11) | C42iii—Na1—O81 | 138.26 (10) |
O82i—K1—Na1i | 110.14 (7) | C42iii—Na1—O101 | 93.89 (12) |
O82i—K1—Na2i | 32.78 (5) | K2ix—Na2—K1viii | 98.11 (4) |
O82i—K1—O11 | 141.52 (11) | O12—Na2—K1viii | 88.04 (7) |
O82i—K1—O12 | 69.17 (8) | O12—Na2—K2ix | 133.93 (7) |
O82i—K1—O81i | 142.25 (8) | O31vii—Na2—K1viii | 140.60 (8) |
O82i—K1—H28i | 152.3 (10) | O31vii—Na2—K2ix | 108.14 (7) |
H48i—K1—Na1i | 123.0 (11) | O31vii—Na2—O12 | 93.97 (8) |
H48i—K1—Na2i | 42.9 (11) | O51vii—Na2—K1viii | 92.63 (7) |
H48i—K1—O11 | 125.3 (11) | O51vii—Na2—K2ix | 52.62 (6) |
H48i—K1—O12 | 65.1 (10) | O51vii—Na2—O12 | 173.24 (9) |
H48i—K1—O81i | 151.7 (10) | O51vii—Na2—O31vii | 81.25 (8) |
H48i—K1—H28i | 166.1 (11) | O72—Na2—K1viii | 126.66 (8) |
H48i—K1—O82i | 16.2 (10) | O72—Na2—K2ix | 47.88 (7) |
O91—K1—Na1i | 72.05 (8) | O72—Na2—O12 | 92.56 (9) |
O91—K1—Na2i | 92.90 (8) | O72—Na2—O31vii | 92.60 (10) |
O91—K1—O11 | 121.12 (12) | O72—Na2—O51vii | 92.43 (9) |
O91—K1—O12 | 73.49 (9) | O82—Na2—K1viii | 45.37 (9) |
O91—K1—O81i | 84.38 (11) | O82—Na2—K2ix | 56.00 (8) |
O91—K1—H28i | 75.9 (9) | O82—Na2—O12 | 104.87 (10) |
O91—K1—O82i | 89.60 (9) | O82—Na2—O31vii | 160.90 (10) |
O91—K1—H48i | 102.8 (10) | O82—Na2—O51vii | 80.22 (9) |
O92—K1—Na1i | 92.92 (8) | O82—Na2—O72 | 83.59 (11) |
O92—K1—Na2i | 71.72 (8) | O102—Na2—K1viii | 52.49 (10) |
O92—K1—O11 | 73.38 (9) | O102—Na2—K2ix | 127.13 (9) |
O92—K1—O12 | 120.52 (11) | O102—Na2—O12 | 92.47 (10) |
O92—K1—O81i | 89.59 (9) | O102—Na2—O31vii | 88.11 (11) |
O92—K1—H28i | 102.0 (10) | O102—Na2—O51vii | 82.64 (10) |
O92—K1—O82i | 83.80 (11) | O102—Na2—O72 | 174.86 (11) |
O92—K1—H48i | 74.5 (9) | O102—Na2—O82 | 94.09 (12) |
O92—K1—O91 | 160.42 (10) | C41vii—Na2—K1viii | 140.30 (8) |
O101i—K1—Na1i | 33.03 (6) | C41vii—Na2—K2ix | 87.59 (7) |
O101i—K1—Na2i | 61.45 (6) | C41vii—Na2—O12 | 115.80 (9) |
O101i—K1—O11 | 133.14 (11) | C41vii—Na2—O31vii | 22.67 (8) |
O101i—K1—O12 | 118.11 (10) | C41vii—Na2—O51vii | 60.09 (8) |
O101i—K1—O81i | 63.96 (8) | C41vii—Na2—O72 | 85.64 (10) |
O101i—K1—H28i | 69.1 (10) | C41vii—Na2—O82 | 138.28 (10) |
O101i—K1—O82i | 83.35 (8) | C41vii—Na2—O102 | 93.12 (12) |
O101i—K1—H48i | 99.0 (11) | Na1—O11—K1 | 101.42 (9) |
O101i—K1—O91 | 51.29 (9) | C11—O11—K1 | 115.68 (17) |
O101i—K1—O92 | 109.46 (9) | C11—O11—Na1 | 125.86 (18) |
O102i—K1—Na1i | 61.79 (6) | Na2—O12—K1 | 101.59 (9) |
O102i—K1—Na2i | 32.85 (6) | C12—O12—K1 | 115.57 (17) |
O102i—K1—O11 | 117.90 (9) | C12—O12—Na2 | 125.90 (18) |
O102i—K1—O12 | 132.40 (11) | C41—O31—Na2ii | 108.01 (19) |
O102i—K1—O81i | 83.66 (8) | C42—O32—Na1x | 107.63 (18) |
O102i—K1—H28i | 99.0 (11) | C41—O41—K2vii | 120.3 (2) |
O102i—K1—O82i | 63.47 (8) | C42—O42—K2x | 121.0 (2) |
O102i—K1—H48i | 68.1 (10) | Na2ii—O51—K2xi | 85.86 (7) |
O102i—K1—O91 | 109.79 (9) | H51—O51—K2xi | 102 (3) |
O102i—K1—O92 | 50.89 (8) | H51—O51—Na2ii | 111 (3) |
O102i—K1—O101i | 61.51 (7) | C21—O51—K2xi | 120.72 (17) |
H410i—K1—Na1i | 59.4 (12) | C21—O51—Na2ii | 130.41 (17) |
H410i—K1—Na2i | 36.3 (12) | C21—O51—H51 | 104 (3) |
H410i—K1—O11 | 115.3 (12) | Na1x—O52—K2xii | 85.82 (7) |
H410i—K1—O12 | 135.9 (12) | H52—O52—K2xii | 97 (3) |
H410i—K1—O81i | 80.4 (12) | H52—O52—Na1x | 109 (3) |
H410i—K1—H28i | 95.8 (16) | C22—O52—K2xii | 121.12 (17) |
H410i—K1—O82i | 67.0 (12) | C22—O52—Na1x | 130.50 (17) |
H410i—K1—H48i | 71.5 (16) | C22—O52—H52 | 108 (3) |
H410i—K1—O91 | 110.5 (12) | C31—O61—H61 | 115 (3) |
H410i—K1—O92 | 50.0 (12) | C32—O62—H62 | 112 (3) |
H410i—K1—O101i | 61.2 (12) | Na1—O71—K2viii | 93.58 (9) |
H410i—K1—O102i | 3.5 (12) | H17—O71—K2viii | 108 (4) |
Na2vi—K2—Na1i | 116.16 (3) | H17—O71—Na1 | 100 (4) |
O41ii—K2—Na1i | 124.57 (6) | H27—O71—K2viii | 116 (3) |
O41ii—K2—Na2vi | 99.26 (6) | H27—O71—Na1 | 130 (3) |
O42iii—K2—Na1i | 98.97 (6) | H27—O71—H17 | 107 (5) |
O42iii—K2—Na2vi | 124.74 (6) | O71—H17—K2viii | 60 (3) |
O42iii—K2—O41ii | 93.12 (6) | Na2—O72—K2ix | 93.78 (9) |
O51iv—K2—Na1i | 112.76 (5) | H47—O72—K2ix | 122 (3) |
O51iv—K2—Na2vi | 41.53 (5) | H47—O72—Na2 | 126 (3) |
O51iv—K2—O41ii | 67.90 (7) | H37—O72—K2ix | 106 (3) |
O51iv—K2—O42iii | 148.22 (7) | H37—O72—Na2 | 96 (3) |
O52v—K2—Na1i | 41.55 (5) | H37—O72—H47 | 108 (4) |
O52v—K2—Na2vi | 112.64 (5) | K2viii—O81—K1viii | 153.92 (11) |
O52v—K2—O41ii | 148.05 (7) | Na1—O81—K1viii | 101.36 (11) |
O52v—K2—O42iii | 67.70 (7) | Na1—O81—K2viii | 85.35 (8) |
O52v—K2—O51iv | 139.90 (6) | H18—O81—K1viii | 87 (3) |
O71i—K2—Na1i | 38.38 (6) | H18—O81—K2viii | 106 (3) |
O71i—K2—Na2vi | 86.89 (6) | H18—O81—Na1 | 135 (3) |
O71i—K2—O41ii | 110.66 (8) | H28—O81—K1viii | 77 (4) |
O71i—K2—O42iii | 137.35 (8) | H28—O81—K2viii | 78 (4) |
O71i—K2—O51iv | 74.39 (7) | H28—O81—Na1 | 123 (3) |
O71i—K2—O52v | 74.12 (7) | H28—O81—H18 | 102 (4) |
H17i—K2—Na1i | 42.5 (9) | K2viii—H28—K1viii | 169 (2) |
H17i—K2—Na2vi | 92.6 (9) | O81—H28—K1viii | 87 (4) |
H17i—K2—O41ii | 98.7 (9) | O81—H28—K2viii | 86 (4) |
H17i—K2—O42iii | 138.4 (9) | K2ix—O82—K1viii | 154.12 (10) |
H17i—K2—O51iv | 71.9 (9) | Na2—O82—K1viii | 101.85 (11) |
H17i—K2—O52v | 82.2 (9) | Na2—O82—K2ix | 85.15 (9) |
H17i—K2—O71i | 12.6 (8) | H48—O82—K1viii | 79 (4) |
O72vi—K2—Na1i | 86.95 (6) | H48—O82—K2ix | 76 (4) |
O72vi—K2—Na2vi | 38.34 (5) | H48—O82—Na2 | 121 (3) |
O72vi—K2—O41ii | 137.60 (8) | H38—O82—K1viii | 85 (4) |
O72vi—K2—O42iii | 110.62 (8) | H38—O82—K2ix | 108 (4) |
O72vi—K2—O51iv | 74.13 (7) | H38—O82—Na2 | 134 (3) |
O72vi—K2—O52v | 74.31 (7) | H38—O82—H48 | 105 (5) |
O72vi—K2—O71i | 75.20 (7) | K2ix—H48—K1viii | 170 (2) |
O72vi—K2—H17i | 86.6 (8) | O82—H48—K1viii | 85 (4) |
O81i—K2—Na1i | 38.85 (5) | O82—H48—K2ix | 87 (4) |
O81i—K2—Na2vi | 150.58 (5) | H29—O91—K1 | 144 (4) |
O81i—K2—O41ii | 91.31 (7) | H19—O91—K1 | 126 (4) |
O81i—K2—O42iii | 81.55 (7) | H19—O91—H29 | 89 (6) |
O81i—K2—O51iv | 122.38 (7) | H39—O92—K1 | 128 (5) |
O81i—K2—O52v | 61.68 (7) | H49—O92—K1 | 148 (3) |
O81i—K2—O71i | 63.69 (7) | H49—O92—H39 | 83 (5) |
O81i—K2—H17i | 58.5 (9) | Na1—O101—K1viii | 95.27 (12) |
O81i—K2—O72vi | 125.62 (7) | H210—O101—K1viii | 67 (3) |
H28i—K2—Na1i | 49.3 (11) | H210—O101—Na1 | 122 (3) |
H28i—K2—Na2vi | 165.2 (11) | H110—O101—K1viii | 102 (4) |
H28i—K2—O41ii | 89.5 (10) | H110—O101—Na1 | 132 (4) |
H28i—K2—O42iii | 66.1 (10) | H110—O101—H210 | 106 (5) |
H28i—K2—O51iv | 135.1 (10) | Na2—O102—K1viii | 94.65 (12) |
H28i—K2—O52v | 59.8 (9) | H410—O102—Na2 | 106 (4) |
H28i—K2—O71i | 78.8 (11) | H310—O102—K1viii | 92 (3) |
H28i—K2—H17i | 74.2 (14) | H310—O102—Na2 | 131 (3) |
H28i—K2—O72vi | 131.8 (10) | H310—O102—H410 | 82 (4) |
H28i—K2—O81i | 15.7 (10) | O102—H410—K1viii | 164 (5) |
O82vi—K2—Na1i | 150.58 (5) | O21—C11—O11 | 126.4 (3) |
O82vi—K2—Na2vi | 38.85 (5) | C21—C11—O11 | 116.9 (3) |
O82vi—K2—O41ii | 81.78 (7) | C21—C11—O21 | 116.7 (3) |
O82vi—K2—O42iii | 91.57 (7) | C11—C21—O51 | 110.6 (2) |
O82vi—K2—O51iv | 61.58 (7) | H21—C21—O51 | 110.0 (18) |
O82vi—K2—O52v | 122.30 (7) | H21—C21—C11 | 107.3 (18) |
O82vi—K2—O71i | 125.55 (7) | C31—C21—O51 | 109.4 (2) |
O82vi—K2—H17i | 129.5 (9) | C31—C21—C11 | 110.4 (2) |
O82vi—K2—O72vi | 63.63 (7) | C31—C21—H21 | 109.0 (17) |
O82vi—K2—O81i | 170.00 (6) | C21—C31—O61 | 110.4 (2) |
O82vi—K2—H28i | 155.6 (11) | H31—C31—O61 | 105.6 (19) |
H48vi—K2—Na1i | 165.3 (11) | H31—C31—C21 | 110.4 (17) |
H48vi—K2—Na2vi | 49.3 (11) | C41—C31—O61 | 111.8 (3) |
H48vi—K2—O41ii | 65.7 (10) | C41—C31—C21 | 110.1 (2) |
H48vi—K2—O42iii | 90.3 (10) | C41—C31—H31 | 108.3 (17) |
H48vi—K2—O51iv | 59.1 (10) | O31—C41—Na2ii | 49.32 (15) |
H48vi—K2—O52v | 135.9 (10) | O41—C41—Na2ii | 122.5 (2) |
H48vi—K2—O71i | 131.4 (10) | O41—C41—O31 | 126.1 (3) |
H48vi—K2—H17i | 130.9 (13) | C31—C41—Na2ii | 96.26 (18) |
H48vi—K2—O72vi | 79.1 (11) | C31—C41—O31 | 116.6 (3) |
H48vi—K2—O81i | 155.3 (11) | C31—C41—O41 | 117.3 (3) |
H48vi—K2—H28i | 145.3 (11) | O22—C12—O12 | 126.6 (3) |
H48vi—K2—O82vi | 16.2 (10) | C22—C12—O12 | 116.8 (3) |
K2viii—Na1—K1viii | 98.12 (4) | C22—C12—O22 | 116.7 (3) |
O11—Na1—K1viii | 88.37 (7) | C12—C22—O52 | 110.9 (2) |
O11—Na1—K2viii | 133.93 (7) | H22—C22—O52 | 108.4 (17) |
O32iii—Na1—K1viii | 140.20 (8) | H22—C22—C12 | 108.7 (17) |
O32iii—Na1—K2viii | 108.45 (7) | C32—C22—O52 | 109.2 (2) |
O32iii—Na1—O11 | 93.62 (8) | C32—C22—C12 | 110.7 (2) |
O52iii—Na1—K1viii | 92.56 (7) | C32—C22—H22 | 108.9 (16) |
O52iii—Na1—K2viii | 52.63 (6) | C22—C32—O62 | 110.2 (2) |
O52iii—Na1—O11 | 173.15 (9) | H32—C32—O62 | 107 (2) |
O52iii—Na1—O32iii | 81.33 (8) | H32—C32—C22 | 111.7 (19) |
O71—Na1—K1viii | 126.97 (8) | C42—C32—O62 | 111.8 (3) |
O71—Na1—K2viii | 48.04 (7) | C42—C32—C22 | 110.3 (2) |
O71—Na1—O11 | 92.38 (9) | C42—C32—H32 | 106 (2) |
O71—Na1—O32iii | 92.69 (9) | O32—C42—Na1x | 49.57 (15) |
O71—Na1—O52iii | 92.48 (9) | O42—C42—Na1x | 122.4 (2) |
O81—Na1—K1viii | 45.66 (8) | O42—C42—O32 | 126.1 (3) |
O81—Na1—K2viii | 55.80 (8) | C32—C42—Na1x | 96.37 (17) |
O81—Na1—O11 | 105.13 (10) | C32—C42—O32 | 116.3 (3) |
O81—Na1—O32iii | 160.99 (10) | C32—C42—O42 | 117.6 (3) |
O81—Na1—O52iii | 80.23 (9) | | |
| | | |
K1—O11—C11—O21 | −51.7 (2) | Na2ii—O51—C21—C31 | −11.8 (2) |
K1—O11—C11—C21 | 128.82 (19) | Na2ii—C41—C31—O61 | 62.75 (17) |
K1—O12—C12—O22 | −51.8 (2) | Na2ii—C41—C31—C21 | −60.43 (19) |
K1—O12—C12—C22 | 128.50 (19) | O11—C11—C21—O51 | −177.0 (3) |
K2vii—O41—C41—Na2ii | −73.32 (17) | O11—C11—C21—C31 | 61.8 (3) |
K2vii—O41—C41—O31 | −12.8 (2) | O12—C12—C22—O52 | −176.8 (3) |
K2vii—O41—C41—C31 | 168.31 (19) | O12—C12—C22—C32 | 61.8 (3) |
K2—O42iii—C42iii—Na1 | −73.12 (17) | O21—C11—C21—O51 | 3.4 (3) |
K2x—O42—C42—O32 | −12.3 (2) | O21—C11—C21—C31 | −117.8 (3) |
K2x—O42—C42—C32 | 168.18 (19) | O22—C12—C22—O52 | 3.5 (3) |
K2xi—O51—C21—C11 | 113.04 (19) | O22—C12—C22—C32 | −117.9 (3) |
K2xi—O51—C21—C31 | −125.12 (19) | O31—C41—C31—O61 | 15.5 (3) |
K2xii—O52—C22—C12 | 112.82 (19) | O31—C41—C31—C21 | −107.7 (3) |
K2xii—O52—C22—C32 | −124.9 (2) | O32—C42—C32—O62 | 14.8 (3) |
Na1—O11—C11—O21 | 76.5 (2) | O32—C42—C32—C22 | −108.1 (3) |
Na1—O11—C11—C21 | −103.0 (2) | O41—C41—C31—O61 | −165.5 (3) |
Na1x—O32—C42—O42 | −104.43 (19) | O41—C41—C31—C21 | 71.3 (3) |
Na1x—O32—C42—C32 | 75.06 (18) | O42—C42—C32—O62 | −165.6 (3) |
Na1x—O52—C22—C12 | −133.4 (2) | O42—C42—C32—C22 | 71.4 (3) |
Na1x—O52—C22—C32 | −11.1 (2) | O51—C21—C31—O61 | −68.0 (3) |
Na1x—C42—C32—O62 | 62.55 (17) | O51—C21—C31—C41 | 56.0 (3) |
Na1x—C42—C32—C22 | −60.39 (18) | O52—C22—C32—O62 | −68.5 (3) |
Na2—O12—C12—O22 | 76.6 (2) | O52—C22—C32—C42 | 55.4 (3) |
Na2—O12—C12—C22 | −103.1 (2) | O61—C31—C21—C11 | 53.9 (3) |
Na2ii—O31—C41—O41 | −104.5 (2) | O62—C32—C22—C12 | 53.9 (3) |
Na2ii—O31—C41—C31 | 74.38 (19) | C11—C21—C31—C41 | 177.9 (3) |
Na2ii—O51—C21—C11 | −133.7 (2) | C12—C22—C32—C42 | 177.8 (2) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (iv) x+1/2, −y+1/2, −z; (v) x+1/2, −y−1/2, −z; (vi) x+1, y, z−1; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (ix) x−1, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xii) x−1/2, −y−1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O51—H51···O21 | 0.76 (4) | 2.07 (4) | 2.601 (3) | 127 (4) |
O51—H51···O31i | 0.76 (4) | 2.74 (4) | 3.350 (3) | 139 (4) |
O51—H51···O41i | 0.76 (4) | 2.88 (4) | 3.264 (3) | 114 (3) |
O52—H52···O22 | 0.83 (4) | 2.09 (4) | 2.605 (3) | 120 (3) |
O52—H52···O32i | 0.83 (4) | 2.64 (4) | 3.356 (3) | 145 (3) |
O52—H52···O42i | 0.83 (4) | 2.79 (4) | 3.254 (3) | 117 (3) |
O61—H61···O102ii | 0.73 (3) | 2.18 (3) | 2.896 (4) | 166 (4) |
O62—H62···O101x | 0.76 (3) | 2.20 (3) | 2.923 (4) | 159 (4) |
O71—H17···O61 | 0.70 (5) | 2.09 (5) | 2.793 (3) | 172 (5) |
O71—H27···O41ii | 0.87 (4) | 2.03 (4) | 2.883 (4) | 166 (4) |
O72—H47···O42x | 0.86 (4) | 2.06 (4) | 2.885 (3) | 162 (4) |
O72—H37···O62 | 0.81 (5) | 1.98 (5) | 2.792 (3) | 178 (5) |
O81—H18···O11viii | 0.91 (5) | 2.83 (5) | 3.384 (3) | 120 (4) |
O81—H18···O21viii | 0.91 (5) | 1.85 (5) | 2.748 (3) | 172 (5) |
O81—H28···O32xiii | 0.84 (6) | 1.87 (6) | 2.709 (3) | 171 (5) |
O82—H48···O31xiv | 0.87 (6) | 1.83 (6) | 2.701 (3) | 173 (5) |
O82—H38···O12viii | 0.87 (5) | 2.84 (5) | 3.382 (3) | 122 (4) |
O82—H38···O22viii | 0.87 (5) | 1.89 (5) | 2.754 (3) | 173 (5) |
O91—H29···O42i | 0.89 (5) | 1.94 (6) | 2.815 (4) | 167 (5) |
O91—H19···O22v | 0.81 (6) | 2.41 (6) | 3.105 (4) | 145 (5) |
O91—H19···O32iii | 0.81 (6) | 2.79 (6) | 3.161 (4) | 110 (5) |
O91—H19···O62iii | 0.81 (6) | 2.55 (6) | 3.144 (4) | 132 (5) |
O92—H39···O21xi | 0.76 (6) | 2.44 (6) | 3.116 (4) | 149 (5) |
O92—H39···O31vii | 0.76 (6) | 2.83 (6) | 3.170 (4) | 110 (5) |
O92—H39···O61vii | 0.76 (6) | 2.60 (5) | 3.142 (4) | 130 (5) |
O92—H49···O41i | 0.97 (5) | 1.88 (5) | 2.816 (4) | 161 (5) |
O101—H210···O91viii | 0.90 (5) | 1.87 (5) | 2.750 (4) | 165 (5) |
O101—H110···O12 | 0.81 (6) | 1.92 (6) | 2.731 (4) | 174 (5) |
O102—H410···O92viii | 0.78 (5) | 2.37 (5) | 2.757 (4) | 111 (5) |
O102—H310···O11 | 0.85 (6) | 1.89 (5) | 2.727 (4) | 165 (5) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (v) x+1/2, −y−1/2, −z; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xiii) x+1/2, −y−1/2, −z+2; (xiv) x−1/2, −y+1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (286K_anh)
top
Crystal data top
C4H12KNaO10 | F(000) = 585.519 |
Mr = 282.22 | Dx = 1.781 Mg m−3 |
Monoclinic, P2111 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.8694 (9) Å | Cell parameters from 6523 reflections |
b = 14.2539 (12) Å | θ = 3.5–28.7° |
c = 6.2229 (4) Å | µ = 0.59 mm−1 |
β = 90° | T = 286 K |
V = 1052.82 (14) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 5179 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 4022 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.752, Tmax = 1.000 | l = −8→8 |
18433 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.040 | w = 1/[σ2(Fo2) + (0.028P)2 + 0.2216P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.087 | (Δ/σ)max = −0.001 |
S = 1.08 | Δρmax = 0.34 e Å−3 |
5179 reflections | Δρmin = −0.35 e Å−3 |
386 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
3 restraints | Absolute structure parameter: 0.03 (3) |
24 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0006 (2) | −0.00029 (15) | 0.0466 (3) | 0.0604 (6) | |
K2 | 0.50005 (7) | 0.00033 (5) | −0.15923 (10) | 0.03550 (16) | |
Na1 | 0.23140 (11) | −0.00677 (8) | 0.52275 (19) | 0.0299 (3) | |
Na2 | −0.23151 (11) | 0.00679 (8) | 0.52126 (19) | 0.0296 (3) | |
O11 | 0.11995 (18) | 0.10895 (15) | 0.3507 (3) | 0.0284 (5) | |
O12 | −0.11998 (18) | −0.10912 (15) | 0.3501 (3) | 0.0282 (5) | |
O21 | 0.2097 (2) | 0.20283 (15) | 0.1195 (3) | 0.0339 (5) | |
O22 | −0.2094 (2) | −0.20277 (15) | 0.1185 (3) | 0.0330 (5) | |
O31 | 0.2321 (2) | 0.40621 (16) | 0.8140 (3) | 0.0401 (6) | |
O32 | −0.2336 (2) | −0.40628 (16) | 0.8128 (3) | 0.0391 (5) | |
O41 | 0.0528 (2) | 0.36199 (17) | 0.8440 (3) | 0.0386 (6) | |
O42 | −0.0537 (2) | −0.36231 (17) | 0.8440 (3) | 0.0388 (6) | |
O51 | 0.16340 (19) | 0.35714 (15) | 0.3242 (3) | 0.0292 (5) | |
H51 | 0.192 (3) | 0.339 (3) | 0.223 (6) | 0.0438 (7)* | |
O52 | −0.1634 (2) | −0.35715 (14) | 0.3231 (3) | 0.0290 (5) | |
H52 | −0.190 (3) | −0.345 (3) | 0.198 (6) | 0.0435 (7)* | |
O61 | 0.29518 (19) | 0.24813 (16) | 0.6294 (4) | 0.0312 (5) | |
H61 | 0.329 (3) | 0.287 (3) | 0.592 (7) | 0.0468 (7)* | |
O62 | −0.29532 (19) | −0.24840 (16) | 0.6275 (3) | 0.0316 (5) | |
H62 | −0.332 (3) | −0.295 (2) | 0.604 (6) | 0.0473 (7)* | |
O71 | 0.3956 (2) | 0.08222 (18) | 0.4844 (4) | 0.0355 (5) | |
H17 | 0.370 (4) | 0.130 (3) | 0.517 (7) | 0.0533 (8)* | |
H27 | 0.437 (4) | 0.093 (3) | 0.376 (6) | 0.0533 (8)* | |
O72 | −0.3955 (2) | −0.08219 (18) | 0.4847 (4) | 0.0358 (5) | |
H47 | −0.429 (4) | −0.095 (3) | 0.376 (7) | 0.0538 (8)* | |
H37 | −0.369 (4) | −0.134 (3) | 0.535 (6) | 0.0538 (8)* | |
O81 | 0.2438 (3) | 0.04171 (19) | 0.8856 (4) | 0.0501 (7) | |
H18 | 0.237 (4) | 0.096 (3) | 0.957 (7) | 0.0751 (11)* | |
H28 | 0.254 (5) | 0.002 (3) | 0.985 (9) | 0.0751 (11)* | |
O82 | −0.2425 (3) | −0.04121 (19) | 0.8849 (4) | 0.0505 (7) | |
H48 | −0.257 (5) | 0.001 (3) | 0.985 (9) | 0.0757 (11)* | |
H38 | −0.233 (5) | −0.094 (3) | 0.946 (7) | 0.0757 (11)* | |
O91 | 0.0617 (2) | −0.1981 (3) | −0.0346 (5) | 0.0608 (9) | |
H29 | 0.035 (5) | −0.248 (4) | −0.078 (8) | 0.0912 (13)* | |
H19 | 0.116 (5) | −0.218 (4) | 0.017 (9) | 0.0912 (13)* | |
O92 | −0.0613 (2) | 0.1966 (2) | −0.0343 (5) | 0.0568 (8) | |
H39 | −0.120 (5) | 0.228 (4) | −0.011 (8) | 0.0852 (12)* | |
H49 | −0.038 (5) | 0.256 (4) | −0.082 (7) | 0.0852 (12)* | |
O101 | 0.0750 (2) | −0.1024 (2) | 0.5821 (5) | 0.0600 (8) | |
H210 | 0.074 (4) | −0.145 (4) | 0.701 (8) | 0.0900 (12)* | |
H110 | 0.016 (5) | −0.105 (4) | 0.519 (8) | 0.0900 (12)* | |
O102 | −0.0766 (2) | 0.1035 (2) | 0.5785 (5) | 0.0563 (8) | |
H410 | −0.046 (5) | 0.090 (4) | 0.681 (8) | 0.0844 (12)* | |
H310 | −0.017 (5) | 0.104 (4) | 0.526 (8) | 0.0844 (12)* | |
C11 | 0.1542 (2) | 0.1879 (2) | 0.2856 (4) | 0.0229 (6) | |
C21 | 0.1251 (3) | 0.2727 (2) | 0.4235 (4) | 0.0229 (6) | |
H21 | 0.045 (3) | 0.277 (2) | 0.433 (5) | 0.0275 (7)* | |
C31 | 0.1780 (3) | 0.2640 (2) | 0.6459 (4) | 0.0248 (6) | |
H31 | 0.146 (3) | 0.208 (2) | 0.729 (5) | 0.0298 (7)* | |
C41 | 0.1520 (3) | 0.3511 (2) | 0.7805 (4) | 0.0296 (7) | |
C12 | −0.1540 (2) | −0.1878 (2) | 0.2850 (4) | 0.0231 (6) | |
C22 | −0.1252 (3) | −0.2731 (2) | 0.4228 (4) | 0.0230 (6) | |
H22 | −0.037 (3) | −0.278 (2) | 0.439 (4) | 0.0276 (7)* | |
C32 | −0.1783 (3) | −0.2644 (2) | 0.6455 (4) | 0.0244 (6) | |
H32 | −0.145 (3) | −0.209 (2) | 0.720 (5) | 0.0293 (7)* | |
C42 | −0.1526 (3) | −0.3515 (2) | 0.7791 (4) | 0.0302 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0719 (12) | 0.0605 (13) | 0.0486 (11) | −0.0342 (11) | 0.0017 (14) | 0.0004 (10) |
K2 | 0.0348 (3) | 0.0405 (4) | 0.0312 (3) | −0.0040 (3) | −0.0002 (3) | 0.0004 (3) |
Na1 | 0.0289 (7) | 0.0280 (7) | 0.0329 (6) | −0.0012 (5) | −0.0013 (5) | 0.0011 (5) |
Na2 | 0.0280 (7) | 0.0282 (7) | 0.0326 (6) | −0.0009 (5) | 0.0013 (5) | −0.0006 (5) |
O11 | 0.0314 (12) | 0.0242 (12) | 0.0294 (11) | −0.0002 (9) | −0.0010 (9) | −0.0016 (8) |
O12 | 0.0310 (12) | 0.0235 (12) | 0.0299 (11) | −0.0025 (9) | 0.0015 (9) | 0.0008 (8) |
O21 | 0.0440 (13) | 0.0302 (12) | 0.0275 (11) | −0.0003 (10) | 0.0083 (10) | −0.0004 (8) |
O22 | 0.0429 (13) | 0.0296 (12) | 0.0264 (11) | 0.0000 (10) | −0.0074 (10) | 0.0021 (8) |
O31 | 0.0538 (15) | 0.0306 (13) | 0.0359 (12) | −0.0088 (11) | −0.0034 (11) | −0.0081 (9) |
O32 | 0.0507 (15) | 0.0302 (13) | 0.0363 (12) | −0.0073 (11) | 0.0033 (11) | 0.0077 (9) |
O41 | 0.0371 (13) | 0.0478 (15) | 0.0308 (11) | 0.0141 (11) | 0.0001 (10) | −0.0083 (10) |
O42 | 0.0393 (13) | 0.0462 (15) | 0.0309 (11) | 0.0135 (11) | −0.0007 (10) | 0.0078 (10) |
O51 | 0.0411 (13) | 0.0227 (11) | 0.0238 (10) | 0.0006 (9) | 0.0004 (9) | 0.0009 (8) |
O52 | 0.0440 (13) | 0.0213 (11) | 0.0217 (10) | −0.0013 (9) | −0.0004 (9) | 0.0003 (8) |
O61 | 0.0259 (12) | 0.0297 (13) | 0.0381 (12) | 0.0039 (9) | −0.0045 (10) | 0.0000 (9) |
O62 | 0.0265 (12) | 0.0293 (13) | 0.0389 (12) | 0.0053 (9) | 0.0042 (10) | 0.0037 (9) |
O71 | 0.0309 (13) | 0.0307 (13) | 0.0450 (14) | 0.0000 (10) | 0.0076 (10) | 0.0043 (10) |
O72 | 0.0298 (12) | 0.0332 (14) | 0.0445 (14) | 0.0000 (10) | −0.0067 (10) | −0.0025 (11) |
O81 | 0.092 (2) | 0.0315 (14) | 0.0268 (12) | 0.0116 (14) | 0.0053 (13) | 0.0005 (9) |
O82 | 0.093 (2) | 0.0301 (14) | 0.0279 (12) | 0.0109 (14) | −0.0040 (14) | −0.0003 (9) |
O91 | 0.0393 (16) | 0.091 (3) | 0.0524 (17) | −0.0083 (16) | −0.0090 (13) | 0.0079 (16) |
O92 | 0.0372 (15) | 0.082 (2) | 0.0514 (16) | −0.0057 (15) | 0.0086 (13) | −0.0045 (15) |
O101 | 0.0361 (16) | 0.064 (2) | 0.079 (2) | −0.0176 (13) | −0.0188 (14) | 0.0314 (16) |
O102 | 0.0335 (16) | 0.0600 (19) | 0.075 (2) | −0.0148 (13) | 0.0127 (14) | −0.0216 (16) |
C11 | 0.0225 (14) | 0.0239 (16) | 0.0223 (13) | 0.0014 (12) | −0.0033 (12) | −0.0018 (11) |
C21 | 0.0226 (16) | 0.0215 (15) | 0.0247 (14) | −0.0003 (12) | 0.0001 (12) | 0.0000 (11) |
C31 | 0.0277 (16) | 0.0249 (16) | 0.0219 (14) | 0.0023 (12) | 0.0018 (11) | 0.0011 (11) |
C41 | 0.0437 (19) | 0.0272 (17) | 0.0178 (13) | 0.0035 (14) | −0.0056 (13) | 0.0005 (11) |
C12 | 0.0221 (14) | 0.0258 (16) | 0.0214 (13) | 0.0024 (12) | 0.0041 (12) | −0.0002 (11) |
C22 | 0.0258 (16) | 0.0209 (15) | 0.0222 (13) | −0.0001 (12) | −0.0001 (12) | −0.0019 (11) |
C32 | 0.0257 (16) | 0.0242 (16) | 0.0234 (14) | −0.0003 (12) | −0.0028 (11) | −0.0010 (11) |
C42 | 0.0435 (19) | 0.0269 (17) | 0.0202 (14) | 0.0062 (15) | 0.0067 (14) | −0.0021 (11) |
Geometric parameters (Å, º) top
K1—O11 | 2.830 (3) | O31—C41 | 1.251 (4) |
K1—O12 | 2.833 (3) | O32—C42 | 1.256 (4) |
K1—O81i | 3.114 (4) | O41—C41 | 1.252 (4) |
K1—H28i | 3.03 (6) | O42—C42 | 1.251 (4) |
K1—O82i | 3.112 (4) | O51—H51 | 0.76 (4) |
K1—H48i | 3.08 (6) | O51—C21 | 1.428 (4) |
K1—O91 | 2.954 (5) | O52—H52 | 0.86 (4) |
K1—O92 | 2.945 (4) | O52—C22 | 1.423 (4) |
K1—O101i | 3.354 (4) | O61—H61 | 0.73 (3) |
K1—O102i | 3.394 (4) | O61—C31 | 1.412 (4) |
K1—H410i | 2.68 (5) | O62—H62 | 0.81 (3) |
K2—O41ii | 2.843 (2) | O62—C32 | 1.412 (4) |
K2—O42iii | 2.852 (2) | O71—H17 | 0.77 (4) |
K2—O51iv | 2.991 (2) | O71—H27 | 0.85 (4) |
K2—O52v | 2.994 (2) | O72—H47 | 0.80 (4) |
K2—O71i | 2.797 (3) | O72—H37 | 0.86 (5) |
K2—O72vi | 2.797 (2) | O81—H18 | 0.90 (5) |
K2—O81i | 3.110 (3) | O81—H28 | 0.85 (5) |
K2—H28i | 3.06 (6) | O82—H48 | 0.88 (5) |
K2—O82vi | 3.124 (3) | O82—H38 | 0.85 (5) |
K2—H48vi | 3.02 (6) | O91—H29 | 0.83 (5) |
Na1—O11 | 2.370 (2) | O91—H19 | 0.77 (6) |
Na1—O32iii | 2.463 (2) | O92—H39 | 0.85 (6) |
Na1—O52iii | 2.499 (2) | O92—H49 | 0.94 (5) |
Na1—O71 | 2.337 (3) | O101—H210 | 0.96 (5) |
Na1—O81 | 2.365 (3) | O101—H110 | 0.80 (6) |
Na1—O101 | 2.333 (3) | O102—H410 | 0.76 (5) |
Na1—C42iii | 3.082 (3) | O102—H310 | 0.78 (6) |
Na2—O12 | 2.369 (2) | H410—H310 | 1.04 (6) |
Na2—O31vii | 2.466 (3) | C11—C21 | 1.522 (4) |
Na2—O51vii | 2.498 (2) | C21—H21 | 0.96 (3) |
Na2—O72 | 2.335 (3) | C21—C31 | 1.525 (4) |
Na2—O82 | 2.368 (3) | C31—H31 | 1.02 (4) |
Na2—O102 | 2.325 (3) | C31—C41 | 1.529 (4) |
Na2—C41vii | 3.090 (3) | C12—C22 | 1.527 (4) |
O11—C11 | 1.263 (4) | C22—H22 | 1.05 (3) |
O12—C12 | 1.259 (4) | C22—C32 | 1.528 (4) |
O21—C11 | 1.244 (4) | C32—H32 | 1.00 (3) |
O22—C12 | 1.245 (3) | C32—C42 | 1.526 (4) |
| | | |
Na2i—K1—Na1i | 80.19 (3) | O101—Na1—O81 | 93.96 (12) |
O11—K1—Na1i | 101.63 (8) | C42iii—Na1—K1viii | 140.14 (8) |
O11—K1—Na2i | 145.12 (9) | C42iii—Na1—K2viii | 87.67 (7) |
O12—K1—Na1i | 145.45 (9) | C42iii—Na1—O11 | 115.47 (8) |
O12—K1—Na2i | 101.37 (8) | C42iii—Na1—O32iii | 22.88 (8) |
O12—K1—O11 | 96.23 (7) | C42iii—Na1—O52iii | 60.14 (8) |
O81i—K1—Na1i | 33.02 (5) | C42iii—Na1—O71 | 85.47 (9) |
O81i—K1—Na2i | 110.27 (6) | C42iii—Na1—O81 | 138.14 (10) |
O81i—K1—O11 | 69.24 (8) | C42iii—Na1—O101 | 93.95 (11) |
O81i—K1—O12 | 142.04 (11) | K2ix—Na2—K1viii | 98.12 (4) |
H28i—K1—Na1i | 42.7 (11) | O12—Na2—K1viii | 88.10 (7) |
H28i—K1—Na2i | 122.8 (11) | O12—Na2—K2ix | 133.98 (7) |
H28i—K1—O11 | 65.3 (10) | O31vii—Na2—K1viii | 140.51 (8) |
H28i—K1—O12 | 126.2 (11) | O31vii—Na2—K2ix | 108.16 (7) |
H28i—K1—O81i | 15.8 (10) | O31vii—Na2—O12 | 93.92 (8) |
O82i—K1—Na1i | 110.18 (6) | O51vii—Na2—K1viii | 92.64 (7) |
O82i—K1—Na2i | 32.83 (5) | O51vii—Na2—K2ix | 52.56 (6) |
O82i—K1—O11 | 141.58 (11) | O51vii—Na2—O12 | 173.23 (9) |
O82i—K1—O12 | 69.16 (8) | O51vii—Na2—O31vii | 81.23 (8) |
O82i—K1—O81i | 142.35 (8) | O72—Na2—K1viii | 126.78 (8) |
O82i—K1—H28i | 151.8 (10) | O72—Na2—K2ix | 47.99 (6) |
H48i—K1—Na1i | 122.9 (10) | O72—Na2—O12 | 92.50 (9) |
H48i—K1—Na2i | 42.8 (10) | O72—Na2—O31vii | 92.58 (10) |
H48i—K1—O11 | 125.2 (10) | O72—Na2—O51vii | 92.45 (9) |
H48i—K1—O12 | 65.4 (10) | O82—Na2—K1viii | 45.43 (8) |
H48i—K1—O81i | 151.5 (10) | O82—Na2—K2ix | 55.96 (8) |
H48i—K1—H28i | 165.6 (11) | O82—Na2—O12 | 104.99 (10) |
H48i—K1—O82i | 16.3 (10) | O82—Na2—O31vii | 160.83 (10) |
O91—K1—Na1i | 72.00 (8) | O82—Na2—O51vii | 80.17 (9) |
O91—K1—Na2i | 92.88 (8) | O82—Na2—O72 | 83.67 (11) |
O91—K1—O11 | 121.08 (12) | O102—Na2—K1viii | 52.25 (10) |
O91—K1—O12 | 73.45 (9) | O102—Na2—K2ix | 127.19 (9) |
O91—K1—O81i | 84.32 (11) | O102—Na2—O12 | 92.29 (10) |
O91—K1—H28i | 75.2 (9) | O102—Na2—O31vii | 88.27 (11) |
O91—K1—O82i | 89.63 (9) | O102—Na2—O51vii | 82.88 (10) |
O91—K1—H48i | 103.1 (9) | O102—Na2—O72 | 175.07 (11) |
O92—K1—Na1i | 92.85 (7) | O102—Na2—O82 | 93.96 (12) |
O92—K1—Na2i | 71.68 (8) | C41vii—Na2—K1viii | 140.23 (7) |
O92—K1—O11 | 73.44 (9) | C41vii—Na2—K2ix | 87.62 (7) |
O92—K1—O12 | 120.68 (11) | C41vii—Na2—O12 | 115.73 (8) |
O92—K1—O81i | 89.58 (9) | C41vii—Na2—O31vii | 22.65 (8) |
O92—K1—H28i | 102.5 (10) | C41vii—Na2—O51vii | 60.09 (7) |
O92—K1—O82i | 83.79 (10) | C41vii—Na2—O72 | 85.64 (10) |
O92—K1—H48i | 74.1 (9) | C41vii—Na2—O82 | 138.24 (10) |
O92—K1—O91 | 160.30 (10) | C41vii—Na2—O102 | 93.33 (12) |
O101i—K1—Na1i | 33.05 (6) | Na1—O11—K1 | 101.45 (9) |
O101i—K1—Na2i | 61.40 (6) | C11—O11—K1 | 115.85 (17) |
O101i—K1—O11 | 133.07 (11) | C11—O11—Na1 | 125.84 (18) |
O101i—K1—O12 | 118.03 (9) | Na2—O12—K1 | 101.54 (9) |
O101i—K1—O81i | 64.02 (8) | C12—O12—K1 | 115.85 (17) |
O101i—K1—H28i | 68.6 (10) | C12—O12—Na2 | 125.88 (18) |
O101i—K1—O82i | 83.36 (8) | C41—O31—Na2ii | 107.96 (18) |
O101i—K1—H48i | 99.0 (11) | C42—O32—Na1x | 107.45 (18) |
O101i—K1—O91 | 51.26 (9) | C41—O41—K2vii | 120.7 (2) |
O101i—K1—O92 | 109.37 (9) | C42—O42—K2x | 121.2 (2) |
O102i—K1—Na1i | 61.70 (6) | Na2ii—O51—K2xi | 85.90 (7) |
O102i—K1—Na2i | 32.80 (6) | H51—O51—K2xi | 103 (3) |
O102i—K1—O11 | 117.98 (9) | H51—O51—Na2ii | 111 (3) |
O102i—K1—O12 | 132.44 (11) | C21—O51—K2xi | 120.99 (17) |
O102i—K1—O81i | 83.68 (8) | C21—O51—Na2ii | 130.32 (16) |
O102i—K1—H28i | 98.9 (11) | C21—O51—H51 | 102 (3) |
O102i—K1—O82i | 63.49 (8) | Na1x—O52—K2xii | 85.72 (7) |
O102i—K1—H48i | 67.9 (10) | H52—O52—K2xii | 94 (3) |
O102i—K1—O91 | 109.61 (9) | H52—O52—Na1x | 109 (3) |
O102i—K1—O92 | 50.95 (8) | C22—O52—K2xii | 121.03 (17) |
O102i—K1—O101i | 61.35 (7) | C22—O52—Na1x | 130.21 (16) |
H410i—K1—Na1i | 59.4 (12) | C22—O52—H52 | 110 (3) |
H410i—K1—Na2i | 37.3 (12) | C31—O61—H61 | 117 (3) |
H410i—K1—O11 | 114.1 (12) | C32—O62—H62 | 114 (3) |
H410i—K1—O12 | 136.6 (12) | Na1—O71—K2viii | 93.55 (9) |
H410i—K1—O81i | 79.9 (12) | H17—O71—K2viii | 110 (3) |
H410i—K1—H28i | 95.3 (16) | H17—O71—Na1 | 97 (3) |
H410i—K1—O82i | 67.8 (12) | H27—O71—K2viii | 116 (3) |
H410i—K1—H48i | 71.7 (16) | H27—O71—Na1 | 131 (3) |
H410i—K1—O91 | 111.4 (12) | H27—O71—H17 | 107 (4) |
H410i—K1—O92 | 49.0 (12) | Na2—O72—K2ix | 93.68 (9) |
H410i—K1—O101i | 61.9 (12) | H47—O72—K2ix | 123 (3) |
H410i—K1—O102i | 4.5 (12) | H47—O72—Na2 | 128 (3) |
Na2vi—K2—Na1i | 116.23 (3) | H37—O72—K2ix | 104 (3) |
O41ii—K2—Na1i | 124.67 (6) | H37—O72—Na2 | 97 (3) |
O41ii—K2—Na2vi | 99.28 (6) | H37—O72—H47 | 107 (4) |
O42iii—K2—Na1i | 98.86 (6) | K2viii—O81—K1viii | 154.00 (11) |
O42iii—K2—Na2vi | 124.83 (6) | Na1—O81—K1viii | 101.14 (11) |
O42iii—K2—O41ii | 92.91 (6) | Na1—O81—K2viii | 85.42 (8) |
O51iv—K2—Na1i | 112.82 (5) | H18—O81—K1viii | 86 (3) |
O51iv—K2—Na2vi | 41.55 (5) | H18—O81—K2viii | 107 (3) |
O51iv—K2—O41ii | 68.00 (6) | H18—O81—Na1 | 136 (3) |
O51iv—K2—O42iii | 148.26 (7) | H28—O81—K1viii | 76 (4) |
O52v—K2—Na1i | 41.59 (4) | H28—O81—K2viii | 79 (4) |
O52v—K2—Na2vi | 112.71 (5) | H28—O81—Na1 | 121 (3) |
O52v—K2—O41ii | 147.94 (7) | H28—O81—H18 | 103 (4) |
O52v—K2—O42iii | 67.60 (6) | K2viii—H28—K1viii | 170 (2) |
O52v—K2—O51iv | 140.01 (6) | O81—H28—K1viii | 88 (4) |
O71i—K2—Na1i | 38.42 (5) | O81—H28—K2viii | 85 (4) |
O71i—K2—Na2vi | 86.91 (6) | K2ix—O82—K1viii | 154.16 (10) |
O71i—K2—O41ii | 110.88 (8) | Na2—O82—K1viii | 101.75 (11) |
O71i—K2—O42iii | 137.28 (8) | Na2—O82—K2ix | 85.14 (9) |
O71i—K2—O51iv | 74.42 (7) | H48—O82—K1viii | 80 (4) |
O71i—K2—O52v | 74.18 (7) | H48—O82—K2ix | 75 (4) |
O72vi—K2—Na1i | 86.99 (6) | H48—O82—Na2 | 119 (3) |
O72vi—K2—Na2vi | 38.33 (5) | H38—O82—K1viii | 84 (4) |
O72vi—K2—O41ii | 137.61 (7) | H38—O82—K2ix | 110 (4) |
O72vi—K2—O42iii | 110.75 (8) | H38—O82—Na2 | 132 (3) |
O72vi—K2—O51iv | 74.12 (7) | H38—O82—H48 | 108 (5) |
O72vi—K2—O52v | 74.40 (7) | K2ix—H48—K1viii | 170 (2) |
O72vi—K2—O71i | 75.16 (7) | O82—H48—K1viii | 84 (4) |
O81i—K2—Na1i | 38.90 (5) | O82—H48—K2ix | 88 (4) |
O81i—K2—Na2vi | 150.69 (5) | H29—O91—K1 | 142 (4) |
O81i—K2—O41ii | 91.29 (7) | H19—O91—K1 | 119 (4) |
O81i—K2—O42iii | 81.39 (7) | H19—O91—H29 | 98 (6) |
O81i—K2—O51iv | 122.40 (7) | H39—O92—K1 | 133 (4) |
O81i—K2—O52v | 61.72 (7) | H49—O92—K1 | 147 (3) |
O81i—K2—O71i | 63.78 (7) | H49—O92—H39 | 79 (5) |
O81i—K2—O72vi | 125.71 (7) | Na1—O101—K1viii | 95.30 (12) |
H28i—K2—Na1i | 48.9 (11) | H210—O101—K1viii | 67 (3) |
H28i—K2—Na2vi | 165.0 (11) | H210—O101—Na1 | 120 (3) |
H28i—K2—O41ii | 90.2 (10) | H110—O101—K1viii | 102 (4) |
H28i—K2—O42iii | 65.7 (10) | H110—O101—Na1 | 130 (4) |
H28i—K2—O51iv | 135.7 (10) | H110—O101—H210 | 110 (5) |
H28i—K2—O52v | 59.1 (9) | Na2—O102—K1viii | 94.95 (12) |
H28i—K2—O71i | 78.8 (11) | H410—O102—Na2 | 111 (4) |
H28i—K2—O72vi | 131.2 (10) | H310—O102—K1viii | 97 (4) |
H28i—K2—O81i | 15.8 (10) | H310—O102—Na2 | 131 (4) |
O82vi—K2—Na1i | 150.68 (5) | H310—O102—H410 | 85 (5) |
O82vi—K2—Na2vi | 38.91 (5) | O102—H410—K1viii | 160 (6) |
O82vi—K2—O41ii | 81.66 (7) | H310—H410—K1viii | 144 (6) |
O82vi—K2—O42iii | 91.58 (7) | H310—H410—O102 | 48 (4) |
O82vi—K2—O51iv | 61.64 (7) | H410—H310—O102 | 46 (4) |
O82vi—K2—O52v | 122.30 (7) | O21—C11—O11 | 126.2 (3) |
O82vi—K2—O71i | 125.63 (7) | C21—C11—O11 | 116.9 (2) |
O82vi—K2—O72vi | 63.69 (7) | C21—C11—O21 | 116.9 (3) |
O82vi—K2—O81i | 169.82 (6) | C11—C21—O51 | 110.7 (2) |
O82vi—K2—H28i | 155.6 (11) | H21—C21—O51 | 107.2 (19) |
H48vi—K2—Na1i | 165.4 (11) | H21—C21—C11 | 107.9 (18) |
H48vi—K2—Na2vi | 49.3 (11) | C31—C21—O51 | 109.3 (2) |
H48vi—K2—O41ii | 65.4 (10) | C31—C21—C11 | 110.6 (2) |
H48vi—K2—O42iii | 90.6 (10) | C31—C21—H21 | 111.1 (18) |
H48vi—K2—O51iv | 58.8 (10) | C21—C31—O61 | 110.7 (2) |
H48vi—K2—O52v | 136.1 (10) | H31—C31—O61 | 106.1 (19) |
H48vi—K2—O71i | 131.2 (10) | H31—C31—C21 | 112.0 (18) |
H48vi—K2—O72vi | 79.2 (11) | C41—C31—O61 | 111.6 (2) |
H48vi—K2—O81i | 155.0 (11) | C41—C31—C21 | 110.3 (2) |
H48vi—K2—H28i | 145.6 (11) | C41—C31—H31 | 106.0 (18) |
H48vi—K2—O82vi | 16.4 (10) | O31—C41—Na2ii | 49.39 (15) |
K2viii—Na1—K1viii | 98.17 (4) | O41—C41—Na2ii | 122.1 (2) |
O11—Na1—K1viii | 88.40 (7) | O41—C41—O31 | 125.8 (3) |
O11—Na1—K2viii | 133.91 (7) | C31—C41—Na2ii | 96.26 (17) |
O32iii—Na1—K1viii | 140.19 (8) | C31—C41—O31 | 116.6 (3) |
O32iii—Na1—K2viii | 108.48 (7) | C31—C41—O41 | 117.6 (3) |
O32iii—Na1—O11 | 93.51 (8) | O22—C12—O12 | 126.1 (3) |
O52iii—Na1—K1viii | 92.53 (7) | C22—C12—O12 | 117.2 (2) |
O52iii—Na1—K2viii | 52.69 (6) | C22—C12—O22 | 116.7 (3) |
O52iii—Na1—O11 | 173.11 (9) | C12—C22—O52 | 110.7 (2) |
O52iii—Na1—O32iii | 81.42 (8) | H22—C22—O52 | 107.7 (16) |
O71—Na1—K1viii | 127.07 (8) | H22—C22—C12 | 109.0 (17) |
O71—Na1—K2viii | 48.03 (6) | C32—C22—O52 | 109.4 (2) |
O71—Na1—O11 | 92.36 (9) | C32—C22—C12 | 110.6 (2) |
O71—Na1—O32iii | 92.61 (9) | C32—C22—H22 | 109.3 (15) |
O71—Na1—O52iii | 92.52 (9) | C22—C32—O62 | 110.3 (2) |
O81—Na1—K1viii | 45.84 (8) | H32—C32—O62 | 107 (2) |
O81—Na1—K2viii | 55.67 (8) | H32—C32—C22 | 108.8 (18) |
O81—Na1—O11 | 105.24 (9) | C42—C32—O62 | 111.8 (3) |
O81—Na1—O32iii | 160.97 (10) | C42—C32—C22 | 110.3 (2) |
O81—Na1—O52iii | 80.14 (9) | C42—C32—H32 | 108.4 (18) |
O81—Na1—O71 | 83.52 (10) | O32—C42—Na1x | 49.68 (15) |
O101—Na1—K1viii | 51.65 (10) | O42—C42—Na1x | 122.4 (2) |
O101—Na1—K2viii | 127.43 (8) | O42—C42—O32 | 126.0 (3) |
O101—Na1—O11 | 91.98 (10) | C32—C42—Na1x | 96.46 (17) |
O101—Na1—O32iii | 88.54 (11) | C32—C42—O32 | 116.4 (3) |
O101—Na1—O52iii | 83.27 (10) | C32—C42—O42 | 117.6 (3) |
O101—Na1—O71 | 175.43 (11) | | |
| | | |
K1—O11—C11—O21 | −51.4 (2) | Na2ii—O51—C21—C31 | −11.4 (2) |
K1—O11—C11—C21 | 128.76 (18) | Na2ii—C41—C31—O61 | 62.96 (17) |
K1—O12—C12—O22 | −51.6 (2) | Na2ii—C41—C31—C21 | −60.53 (18) |
K1—O12—C12—C22 | 128.49 (18) | O11—C11—C21—O51 | −176.7 (3) |
K2vii—O41—C41—Na2ii | −73.57 (17) | O11—C11—C21—C31 | 62.0 (3) |
K2vii—O41—C41—O31 | −13.2 (2) | O12—C12—C22—O52 | −176.7 (2) |
K2vii—O41—C41—C31 | 168.15 (19) | O12—C12—C22—C32 | 61.9 (3) |
K2—O42iii—C42iii—Na1 | −73.13 (17) | O21—C11—C21—O51 | 3.5 (3) |
K2x—O42—C42—O32 | −12.3 (2) | O21—C11—C21—C31 | −117.9 (3) |
K2x—O42—C42—C32 | 168.07 (18) | O22—C12—C22—O52 | 3.5 (3) |
K2xi—O51—C21—C11 | 112.87 (18) | O22—C12—C22—C32 | −118.0 (3) |
K2xi—O51—C21—C31 | −125.04 (19) | O31—C41—C31—O61 | 15.6 (3) |
K2xii—O52—C22—C12 | 113.09 (18) | O31—C41—C31—C21 | −107.9 (3) |
K2xii—O52—C22—C32 | −124.71 (19) | O32—C42—C32—O62 | 14.8 (3) |
Na1—O11—C11—O21 | 77.1 (2) | O32—C42—C32—C22 | −108.3 (3) |
Na1—O11—C11—C21 | −102.8 (2) | O41—C41—C31—O61 | −165.7 (3) |
Na1x—O32—C42—O42 | −104.55 (18) | O41—C41—C31—C21 | 70.8 (3) |
Na1x—O32—C42—C32 | 75.12 (18) | O42—C42—C32—O62 | −165.5 (3) |
Na1x—O52—C22—C12 | −133.7 (2) | O42—C42—C32—C22 | 71.4 (3) |
Na1x—O52—C22—C32 | −11.5 (2) | O51—C21—C31—O61 | −68.2 (2) |
Na1x—C42—C32—O62 | 62.64 (16) | O51—C21—C31—C41 | 55.8 (3) |
Na1x—C42—C32—C22 | −60.40 (18) | O52—C22—C32—O62 | −68.3 (2) |
Na2—O12—C12—O22 | 77.0 (2) | O52—C22—C32—C42 | 55.6 (3) |
Na2—O12—C12—C22 | −102.9 (2) | O61—C31—C21—C11 | 53.9 (3) |
Na2ii—O31—C41—O41 | −104.19 (19) | O62—C32—C22—C12 | 54.0 (3) |
Na2ii—O31—C41—C31 | 74.42 (18) | C11—C21—C31—C41 | 177.9 (2) |
Na2ii—O51—C21—C11 | −133.5 (2) | C12—C22—C32—C42 | 177.9 (2) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (iv) x+1/2, −y+1/2, −z; (v) x+1/2, −y−1/2, −z; (vi) x+1, y, z−1; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (ix) x−1, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xii) x−1/2, −y−1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O51—H51···O21 | 0.76 (4) | 2.06 (4) | 2.600 (3) | 129 (4) |
O51—H51···O31i | 0.76 (4) | 2.76 (4) | 3.352 (3) | 136 (4) |
O51—H51···O41i | 0.76 (4) | 2.90 (4) | 3.265 (3) | 113 (3) |
O52—H52···O22 | 0.86 (4) | 2.10 (4) | 2.601 (3) | 117 (3) |
O52—H52···O32i | 0.86 (4) | 2.60 (4) | 3.357 (3) | 147 (3) |
O52—H52···O42i | 0.86 (4) | 2.75 (4) | 3.254 (3) | 119 (3) |
O61—H61···O102ii | 0.73 (3) | 2.19 (3) | 2.910 (4) | 170 (4) |
O62—H62···O101x | 0.81 (3) | 2.16 (3) | 2.930 (4) | 158 (4) |
O71—H17···O61 | 0.77 (4) | 2.03 (5) | 2.797 (3) | 174 (4) |
O71—H27···O41ii | 0.85 (4) | 2.05 (4) | 2.880 (3) | 168 (4) |
O72—H47···O42x | 0.80 (4) | 2.11 (4) | 2.887 (3) | 163 (4) |
O72—H37···O62 | 0.86 (5) | 1.94 (5) | 2.796 (3) | 174 (4) |
O81—H18···O11viii | 0.90 (5) | 2.82 (5) | 3.385 (3) | 122 (4) |
O81—H18···O21viii | 0.90 (5) | 1.85 (5) | 2.748 (3) | 174 (5) |
O81—H28···O32xiii | 0.85 (5) | 1.86 (6) | 2.707 (3) | 174 (5) |
O82—H48···O31xiv | 0.88 (5) | 1.83 (5) | 2.702 (3) | 172 (5) |
O82—H38···O12viii | 0.85 (5) | 2.86 (5) | 3.382 (3) | 122 (4) |
O82—H38···O22viii | 0.85 (5) | 1.90 (5) | 2.753 (3) | 172 (4) |
O91—H29···O42i | 0.83 (5) | 2.00 (6) | 2.816 (4) | 170 (6) |
O91—H19···O22v | 0.77 (6) | 2.51 (6) | 3.107 (4) | 135 (5) |
O91—H19···O32iii | 0.77 (6) | 2.73 (6) | 3.165 (4) | 118 (5) |
O91—H19···O62iii | 0.77 (6) | 2.50 (6) | 3.144 (4) | 142 (5) |
O92—H39···O21xi | 0.85 (6) | 2.34 (6) | 3.118 (4) | 152 (5) |
O92—H39···O31vii | 0.85 (6) | 2.87 (6) | 3.170 (4) | 103 (4) |
O92—H39···O61vii | 0.85 (6) | 2.60 (5) | 3.142 (4) | 123 (4) |
O92—H49···O41i | 0.94 (5) | 1.91 (5) | 2.822 (4) | 162 (5) |
O101—H210···O91viii | 0.96 (5) | 1.82 (5) | 2.752 (4) | 165 (5) |
O101—H110···O12 | 0.80 (6) | 1.93 (6) | 2.730 (3) | 176 (5) |
O102—H410···O92viii | 0.76 (5) | 2.34 (5) | 2.757 (4) | 116 (5) |
O102—H310···O11 | 0.78 (6) | 1.96 (6) | 2.730 (4) | 171 (5) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (v) x+1/2, −y−1/2, −z; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xiii) x+1/2, −y−1/2, −z+2; (xiv) x−1/2, −y+1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (296K_anh)
top
Crystal data top
C4H12KNaO10 | F(000) = 585.519 |
Mr = 282.22 | Dx = 1.777 Mg m−3 |
Monoclinic, P2111 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.8822 (9) Å | Cell parameters from 6349 reflections |
b = 14.2635 (12) Å | θ = 3.6–28.7° |
c = 6.2260 (4) Å | µ = 0.59 mm−1 |
β = 90° | T = 296 K |
V = 1055.19 (14) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 5199 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 3995 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.052 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.669, Tmax = 1.000 | l = −8→8 |
18450 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.040 | w = 1/[σ2(Fo2) + (0.0287P)2 + 0.2309P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.089 | (Δ/σ)max = −0.0004 |
S = 1.08 | Δρmax = 0.36 e Å−3 |
5199 reflections | Δρmin = −0.37 e Å−3 |
386 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
3 restraints | Absolute structure parameter: 0.06 (3) |
24 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0006 (2) | −0.00018 (15) | 0.0470 (3) | 0.0620 (6) | |
K2 | 0.50002 (8) | 0.00018 (5) | −0.15896 (10) | 0.03674 (16) | |
Na1 | 0.23125 (11) | −0.00672 (8) | 0.52288 (19) | 0.0309 (3) | |
Na2 | −0.23159 (11) | 0.00681 (8) | 0.52202 (19) | 0.0307 (3) | |
O11 | 0.12007 (18) | 0.10923 (15) | 0.3513 (3) | 0.0286 (5) | |
O12 | −0.11999 (18) | −0.10903 (15) | 0.3507 (3) | 0.0292 (5) | |
O21 | 0.2095 (2) | 0.20281 (15) | 0.1194 (3) | 0.0341 (5) | |
O22 | −0.2096 (2) | −0.20276 (15) | 0.1191 (3) | 0.0345 (5) | |
O31 | 0.2325 (2) | 0.40625 (16) | 0.8134 (3) | 0.0398 (5) | |
O32 | −0.2336 (2) | −0.40615 (16) | 0.8127 (3) | 0.0407 (6) | |
O41 | 0.0532 (2) | 0.36219 (17) | 0.8436 (3) | 0.0392 (6) | |
O42 | −0.0536 (2) | −0.36248 (17) | 0.8440 (3) | 0.0397 (6) | |
O51 | 0.1631 (2) | 0.35721 (15) | 0.3241 (3) | 0.0302 (5) | |
H51 | 0.187 (3) | 0.341 (3) | 0.219 (6) | 0.0454 (8)* | |
O52 | −0.1635 (2) | −0.35710 (15) | 0.3231 (3) | 0.0298 (5) | |
H52 | −0.191 (3) | −0.343 (3) | 0.203 (6) | 0.0446 (7)* | |
O61 | 0.29533 (19) | 0.24814 (15) | 0.6285 (4) | 0.0321 (5) | |
H61 | 0.325 (3) | 0.291 (2) | 0.607 (7) | 0.0481 (8)* | |
O62 | −0.29545 (19) | −0.24813 (16) | 0.6273 (4) | 0.0334 (5) | |
H62 | −0.328 (3) | −0.294 (2) | 0.604 (6) | 0.0500 (8)* | |
O71 | 0.3957 (2) | 0.08191 (18) | 0.4836 (4) | 0.0371 (6) | |
H17 | 0.374 (4) | 0.125 (3) | 0.519 (7) | 0.0557 (9)* | |
H27 | 0.437 (4) | 0.091 (3) | 0.370 (7) | 0.0557 (9)* | |
O72 | −0.3957 (2) | −0.08223 (18) | 0.4853 (4) | 0.0371 (6) | |
H47 | −0.428 (4) | −0.092 (3) | 0.372 (7) | 0.0556 (8)* | |
H37 | −0.361 (4) | −0.133 (3) | 0.527 (7) | 0.0556 (8)* | |
O81 | 0.2442 (3) | 0.0414 (2) | 0.8862 (4) | 0.0517 (8) | |
H18 | 0.236 (5) | 0.094 (4) | 0.952 (8) | 0.0776 (11)* | |
H28 | 0.252 (5) | 0.002 (4) | 0.983 (9) | 0.0776 (11)* | |
O82 | −0.2434 (3) | −0.04129 (19) | 0.8854 (4) | 0.0504 (8) | |
H48 | −0.260 (5) | −0.004 (3) | 0.981 (9) | 0.0756 (11)* | |
H38 | −0.235 (4) | −0.098 (4) | 0.941 (7) | 0.0756 (11)* | |
O91 | 0.0615 (3) | −0.1985 (3) | −0.0348 (5) | 0.0620 (9) | |
H29 | 0.048 (5) | −0.252 (4) | −0.089 (8) | 0.0930 (13)* | |
H19 | 0.115 (5) | −0.216 (4) | 0.013 (9) | 0.0930 (13)* | |
O92 | −0.0614 (2) | 0.1978 (3) | −0.0346 (5) | 0.0595 (8) | |
H39 | −0.115 (5) | 0.227 (4) | −0.005 (9) | 0.0893 (12)* | |
H49 | −0.029 (5) | 0.259 (4) | −0.085 (7) | 0.0893 (12)* | |
O101 | 0.0750 (2) | −0.1023 (2) | 0.5828 (6) | 0.0621 (9) | |
H210 | 0.071 (5) | −0.140 (4) | 0.705 (8) | 0.0931 (13)* | |
H110 | 0.014 (5) | −0.107 (4) | 0.518 (8) | 0.0931 (13)* | |
O102 | −0.0759 (2) | 0.1033 (2) | 0.5794 (5) | 0.0593 (9) | |
H410 | −0.053 (5) | 0.086 (4) | 0.682 (8) | 0.0889 (13)* | |
H310 | −0.014 (5) | 0.103 (4) | 0.528 (8) | 0.0889 (13)* | |
C11 | 0.1542 (2) | 0.1879 (2) | 0.2851 (4) | 0.0245 (6) | |
C21 | 0.1249 (3) | 0.2728 (2) | 0.4234 (4) | 0.0240 (6) | |
H21 | 0.041 (3) | 0.277 (2) | 0.432 (5) | 0.0287 (7)* | |
C31 | 0.1780 (3) | 0.2637 (2) | 0.6461 (5) | 0.0264 (6) | |
H31 | 0.145 (3) | 0.207 (2) | 0.730 (5) | 0.0317 (8)* | |
C41 | 0.1520 (3) | 0.3514 (2) | 0.7798 (4) | 0.0303 (7) | |
C12 | −0.1540 (2) | −0.1876 (2) | 0.2852 (4) | 0.0233 (6) | |
C22 | −0.1253 (3) | −0.2731 (2) | 0.4225 (4) | 0.0241 (6) | |
H22 | −0.042 (3) | −0.279 (2) | 0.439 (5) | 0.0289 (7)* | |
C32 | −0.1779 (3) | −0.2643 (2) | 0.6446 (5) | 0.0249 (6) | |
H32 | −0.147 (3) | −0.209 (2) | 0.720 (5) | 0.0299 (7)* | |
C42 | −0.1530 (3) | −0.3518 (2) | 0.7792 (4) | 0.0290 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0720 (12) | 0.0638 (13) | 0.0503 (12) | −0.0355 (11) | 0.0011 (13) | 0.0010 (10) |
K2 | 0.0364 (3) | 0.0416 (4) | 0.0322 (3) | −0.0043 (3) | −0.0001 (3) | 0.0005 (3) |
Na1 | 0.0295 (7) | 0.0287 (7) | 0.0344 (6) | −0.0015 (5) | −0.0014 (5) | 0.0019 (5) |
Na2 | 0.0301 (7) | 0.0276 (7) | 0.0343 (6) | −0.0013 (5) | 0.0014 (5) | −0.0010 (5) |
O11 | 0.0312 (12) | 0.0234 (12) | 0.0312 (11) | −0.0021 (9) | −0.0010 (9) | −0.0008 (8) |
O12 | 0.0330 (12) | 0.0241 (12) | 0.0303 (11) | −0.0020 (9) | 0.0018 (9) | 0.0024 (8) |
O21 | 0.0438 (13) | 0.0320 (12) | 0.0264 (11) | −0.0001 (10) | 0.0087 (10) | −0.0014 (9) |
O22 | 0.0452 (13) | 0.0301 (12) | 0.0281 (11) | 0.0000 (10) | −0.0072 (10) | 0.0017 (9) |
O31 | 0.0523 (15) | 0.0307 (13) | 0.0363 (12) | −0.0074 (11) | −0.0049 (11) | −0.0067 (9) |
O32 | 0.0525 (15) | 0.0324 (13) | 0.0372 (12) | −0.0082 (12) | 0.0045 (11) | 0.0085 (9) |
O41 | 0.0389 (13) | 0.0485 (15) | 0.0302 (11) | 0.0132 (11) | 0.0010 (10) | −0.0084 (10) |
O42 | 0.0403 (13) | 0.0462 (15) | 0.0326 (12) | 0.0126 (11) | −0.0008 (10) | 0.0071 (10) |
O51 | 0.0442 (14) | 0.0226 (11) | 0.0240 (10) | 0.0001 (10) | −0.0008 (10) | 0.0009 (8) |
O52 | 0.0441 (13) | 0.0226 (11) | 0.0226 (10) | −0.0002 (9) | 0.0000 (9) | 0.0006 (8) |
O61 | 0.0289 (13) | 0.0269 (13) | 0.0405 (12) | 0.0036 (9) | −0.0052 (10) | −0.0008 (10) |
O62 | 0.0288 (13) | 0.0312 (13) | 0.0401 (12) | 0.0045 (10) | 0.0045 (10) | 0.0026 (10) |
O71 | 0.0328 (13) | 0.0326 (14) | 0.0460 (14) | −0.0006 (11) | 0.0074 (11) | 0.0021 (11) |
O72 | 0.0315 (13) | 0.0348 (14) | 0.0450 (14) | 0.0002 (10) | −0.0069 (11) | −0.0030 (11) |
O81 | 0.096 (2) | 0.0321 (14) | 0.0269 (12) | 0.0118 (15) | 0.0076 (14) | 0.0009 (10) |
O82 | 0.092 (2) | 0.0297 (14) | 0.0294 (12) | 0.0123 (14) | −0.0056 (14) | −0.0005 (10) |
O91 | 0.0412 (16) | 0.092 (3) | 0.0527 (18) | −0.0076 (17) | −0.0087 (13) | 0.0061 (16) |
O92 | 0.0394 (16) | 0.087 (2) | 0.0523 (17) | −0.0065 (15) | 0.0089 (13) | −0.0074 (15) |
O101 | 0.0367 (16) | 0.068 (2) | 0.082 (2) | −0.0175 (14) | −0.0192 (14) | 0.0317 (16) |
O102 | 0.0360 (16) | 0.065 (2) | 0.077 (2) | −0.0128 (14) | 0.0136 (15) | −0.0230 (17) |
C11 | 0.0250 (15) | 0.0253 (17) | 0.0231 (14) | 0.0020 (12) | −0.0052 (12) | −0.0012 (11) |
C21 | 0.0263 (17) | 0.0224 (15) | 0.0231 (13) | −0.0001 (12) | −0.0023 (12) | 0.0002 (11) |
C31 | 0.0296 (16) | 0.0267 (17) | 0.0229 (14) | 0.0041 (13) | 0.0010 (12) | −0.0008 (12) |
C41 | 0.045 (2) | 0.0269 (17) | 0.0193 (14) | 0.0057 (14) | −0.0066 (13) | −0.0012 (11) |
C12 | 0.0235 (15) | 0.0240 (16) | 0.0223 (13) | 0.0025 (12) | 0.0039 (12) | 0.0002 (11) |
C22 | 0.0250 (16) | 0.0230 (15) | 0.0242 (14) | 0.0005 (12) | −0.0018 (12) | −0.0001 (11) |
C32 | 0.0268 (16) | 0.0237 (16) | 0.0243 (14) | 0.0012 (12) | −0.0012 (12) | −0.0012 (11) |
C42 | 0.0396 (18) | 0.0276 (17) | 0.0196 (14) | 0.0040 (14) | 0.0060 (13) | 0.0006 (11) |
Geometric parameters (Å, º) top
K1—O11 | 2.835 (3) | O31—C41 | 1.254 (4) |
K1—O12 | 2.835 (3) | O32—C42 | 1.250 (4) |
K1—O81i | 3.119 (4) | O41—C41 | 1.248 (4) |
K1—H28i | 3.02 (6) | O42—C42 | 1.257 (4) |
K1—O82i | 3.125 (4) | O51—H51 | 0.75 (4) |
K1—O91 | 2.964 (5) | O51—C21 | 1.428 (4) |
K1—O92 | 2.963 (4) | O52—H52 | 0.84 (4) |
K1—O101i | 3.355 (4) | O52—C22 | 1.423 (4) |
K1—H210i | 3.04 (5) | O61—H61 | 0.72 (3) |
K1—O102i | 3.389 (4) | O61—C31 | 1.417 (4) |
K1—H410i | 2.66 (5) | O62—H62 | 0.77 (3) |
K2—O41ii | 2.847 (2) | O62—C32 | 1.420 (4) |
K2—O42iii | 2.848 (2) | O71—H17 | 0.70 (5) |
K2—O51iv | 2.992 (2) | O71—H27 | 0.87 (4) |
K2—O52v | 2.997 (2) | O72—H47 | 0.81 (4) |
K2—O71i | 2.802 (3) | O72—H37 | 0.87 (5) |
K2—H17i | 3.07 (5) | O81—H18 | 0.87 (5) |
K2—O72vi | 2.797 (3) | O81—H28 | 0.83 (6) |
K2—O81i | 3.109 (3) | O82—H48 | 0.83 (5) |
K2—H28i | 3.07 (6) | O82—H38 | 0.88 (5) |
K2—O82vi | 3.118 (3) | O91—H29 | 0.85 (5) |
K2—H48vi | 2.99 (6) | O91—H19 | 0.75 (6) |
Na1—O11 | 2.371 (2) | O92—H39 | 0.78 (6) |
Na1—O32iii | 2.466 (3) | O92—H49 | 1.00 (5) |
Na1—O52iii | 2.501 (2) | O101—H210 | 0.93 (5) |
Na1—O71 | 2.340 (3) | O101—H110 | 0.83 (6) |
Na1—O81 | 2.369 (3) | O102—H410 | 0.74 (5) |
Na1—O101 | 2.333 (3) | O102—H310 | 0.80 (6) |
Na1—C42iii | 3.082 (3) | H410—H310 | 1.09 (7) |
Na2—O12 | 2.372 (2) | C11—C21 | 1.525 (4) |
Na2—O31vii | 2.466 (3) | C21—H21 | 1.01 (3) |
Na2—O51vii | 2.499 (2) | C21—C31 | 1.528 (4) |
Na2—O72 | 2.338 (3) | C31—H31 | 1.05 (4) |
Na2—O82 | 2.368 (3) | C31—C41 | 1.533 (4) |
Na2—O102 | 2.333 (3) | C12—C22 | 1.528 (4) |
Na2—C41vii | 3.088 (3) | C22—H22 | 1.00 (3) |
O11—C11 | 1.262 (4) | C22—C32 | 1.523 (4) |
O12—C12 | 1.259 (4) | C32—H32 | 0.99 (4) |
O21—C11 | 1.242 (4) | C32—C42 | 1.532 (4) |
O22—C12 | 1.246 (4) | | |
| | | |
Na2i—K1—Na1i | 80.23 (3) | O81—Na1—O71 | 83.65 (11) |
O11—K1—Na1i | 101.64 (8) | O101—Na1—K1viii | 51.59 (10) |
O11—K1—Na2i | 145.12 (9) | O101—Na1—K2viii | 127.37 (9) |
O12—K1—Na1i | 145.44 (9) | O101—Na1—O11 | 92.07 (10) |
O12—K1—Na2i | 101.31 (8) | O101—Na1—O32iii | 88.63 (11) |
O12—K1—O11 | 96.26 (7) | O101—Na1—O52iii | 83.28 (10) |
O81i—K1—Na1i | 33.05 (5) | O101—Na1—O71 | 175.36 (12) |
O81i—K1—Na2i | 110.40 (7) | O101—Na1—O81 | 93.90 (12) |
O81i—K1—O11 | 69.24 (8) | C42iii—Na1—K1viii | 140.20 (8) |
O81i—K1—O12 | 141.93 (12) | C42iii—Na1—K2viii | 87.68 (7) |
H28i—K1—Na1i | 42.5 (11) | C42iii—Na1—O11 | 115.49 (8) |
H28i—K1—Na2i | 122.6 (11) | C42iii—Na1—O32iii | 22.74 (8) |
H28i—K1—O11 | 65.6 (10) | C42iii—Na1—O52iii | 60.15 (8) |
H28i—K1—O12 | 126.4 (11) | C42iii—Na1—O71 | 85.25 (9) |
H28i—K1—O81i | 15.5 (11) | C42iii—Na1—O81 | 138.01 (10) |
O82i—K1—Na1i | 110.24 (7) | C42iii—Na1—O101 | 94.02 (12) |
O82i—K1—Na2i | 32.86 (5) | K2ix—Na2—K1viii | 98.22 (4) |
O82i—K1—O11 | 141.53 (11) | O12—Na2—K1viii | 88.09 (7) |
O82i—K1—O12 | 69.08 (8) | O12—Na2—K2ix | 133.99 (7) |
O82i—K1—O81i | 142.49 (8) | O31vii—Na2—K1viii | 140.37 (8) |
O82i—K1—H28i | 151.6 (11) | O31vii—Na2—K2ix | 108.28 (7) |
O91—K1—Na1i | 71.99 (8) | O31vii—Na2—O12 | 93.79 (8) |
O91—K1—Na2i | 92.78 (8) | O51vii—Na2—K1viii | 92.76 (7) |
O91—K1—O11 | 121.20 (12) | O51vii—Na2—K2ix | 52.57 (6) |
O91—K1—O12 | 73.45 (9) | O51vii—Na2—O12 | 173.18 (9) |
O91—K1—O81i | 84.26 (11) | O51vii—Na2—O31vii | 81.24 (8) |
O91—K1—H28i | 75.2 (10) | O72—Na2—K1viii | 126.85 (8) |
O91—K1—O82i | 89.54 (9) | O72—Na2—K2ix | 47.97 (6) |
O92—K1—Na1i | 92.84 (8) | O72—Na2—O12 | 92.51 (9) |
O92—K1—Na2i | 71.71 (8) | O72—Na2—O31vii | 92.65 (10) |
O92—K1—O11 | 73.41 (9) | O72—Na2—O51vii | 92.39 (9) |
O92—K1—O12 | 120.70 (12) | O82—Na2—K1viii | 45.71 (8) |
O92—K1—O81i | 89.69 (9) | O82—Na2—K2ix | 55.77 (8) |
O92—K1—H28i | 102.4 (10) | O82—Na2—O12 | 105.12 (10) |
O92—K1—O82i | 83.83 (11) | O82—Na2—O31vii | 160.82 (10) |
O92—K1—O91 | 160.23 (11) | O82—Na2—O51vii | 80.16 (9) |
O101i—K1—Na1i | 33.02 (6) | O82—Na2—O72 | 83.49 (11) |
O101i—K1—Na2i | 61.44 (6) | O102—Na2—K1viii | 52.09 (10) |
O101i—K1—O11 | 133.06 (11) | O102—Na2—K2ix | 127.36 (9) |
O101i—K1—O12 | 118.03 (10) | O102—Na2—O12 | 92.08 (10) |
O101i—K1—O81i | 63.99 (8) | O102—Na2—O31vii | 88.28 (11) |
O101i—K1—H28i | 68.3 (10) | O102—Na2—O51vii | 83.13 (10) |
O101i—K1—O82i | 83.43 (8) | O102—Na2—O72 | 175.24 (12) |
O101i—K1—O91 | 51.21 (9) | O102—Na2—O82 | 94.11 (12) |
O101i—K1—O92 | 109.36 (9) | C41vii—Na2—K1viii | 140.27 (7) |
H210i—K1—Na1i | 43.2 (10) | C41vii—Na2—K2ix | 87.59 (7) |
H210i—K1—Na2i | 70.0 (10) | C41vii—Na2—O12 | 115.66 (9) |
H210i—K1—O11 | 133.8 (10) | C41vii—Na2—O31vii | 22.75 (8) |
H210i—K1—O12 | 104.4 (11) | C41vii—Na2—O51vii | 60.04 (8) |
H210i—K1—O81i | 69.1 (10) | C41vii—Na2—O72 | 85.57 (10) |
H210i—K1—H28i | 68.9 (14) | C41vii—Na2—O82 | 138.12 (10) |
H210i—K1—O82i | 84.7 (10) | C41vii—Na2—O102 | 93.56 (12) |
H210i—K1—O91 | 35.4 (11) | Na1—O11—K1 | 101.31 (9) |
H210i—K1—O92 | 125.1 (11) | C11—O11—K1 | 115.59 (17) |
H210i—K1—O101i | 15.8 (10) | C11—O11—Na1 | 126.05 (18) |
O102i—K1—Na1i | 61.59 (6) | Na2—O12—K1 | 101.60 (9) |
O102i—K1—Na2i | 32.90 (6) | C12—O12—K1 | 115.70 (17) |
O102i—K1—O11 | 117.95 (9) | C12—O12—Na2 | 125.90 (18) |
O102i—K1—O12 | 132.51 (11) | C41—O31—Na2ii | 107.73 (18) |
O102i—K1—O81i | 83.70 (8) | C42—O32—Na1x | 107.53 (18) |
O102i—K1—H28i | 98.6 (11) | C41—O41—K2vii | 120.9 (2) |
O102i—K1—O82i | 63.64 (8) | C42—O42—K2x | 121.0 (2) |
O102i—K1—O91 | 109.49 (10) | Na2ii—O51—K2xi | 85.89 (7) |
O102i—K1—O92 | 50.99 (9) | H51—O51—K2xi | 99 (3) |
O102i—K1—O101i | 61.28 (8) | H51—O51—Na2ii | 112 (3) |
O102i—K1—H210i | 75.9 (10) | C21—O51—K2xi | 121.09 (17) |
H410i—K1—Na1i | 60.7 (13) | C21—O51—Na2ii | 130.38 (16) |
H410i—K1—Na2i | 35.2 (13) | C21—O51—H51 | 104 (3) |
H410i—K1—O11 | 115.8 (13) | Na1x—O52—K2xii | 85.76 (7) |
H410i—K1—O12 | 134.6 (13) | H52—O52—K2xii | 97 (3) |
H410i—K1—O81i | 81.9 (13) | H52—O52—Na1x | 109 (3) |
H410i—K1—H28i | 96.9 (17) | C22—O52—K2xii | 120.99 (17) |
H410i—K1—O82i | 65.8 (13) | C22—O52—Na1x | 130.31 (16) |
H410i—K1—O91 | 110.7 (13) | C22—O52—H52 | 108 (3) |
H410i—K1—O92 | 49.6 (13) | C31—O61—H61 | 111 (3) |
H410i—K1—O101i | 61.9 (13) | C32—O62—H62 | 112 (3) |
H410i—K1—H210i | 76.8 (16) | Na1—O71—K2viii | 93.52 (9) |
H410i—K1—O102i | 2.4 (13) | H17—O71—K2viii | 106 (4) |
Na2vi—K2—Na1i | 116.30 (3) | H17—O71—Na1 | 97 (4) |
O41ii—K2—Na1i | 124.75 (6) | H27—O71—K2viii | 117 (3) |
O41ii—K2—Na2vi | 99.13 (6) | H27—O71—Na1 | 130 (3) |
O42iii—K2—Na1i | 98.91 (6) | H27—O71—H17 | 110 (5) |
O42iii—K2—Na2vi | 124.83 (6) | O71—H17—K2viii | 62 (4) |
O42iii—K2—O41ii | 92.88 (7) | Na2—O72—K2ix | 93.66 (9) |
O51iv—K2—Na1i | 112.76 (5) | H47—O72—K2ix | 123 (3) |
O51iv—K2—Na2vi | 41.54 (5) | H47—O72—Na2 | 125 (3) |
O51iv—K2—O41ii | 67.95 (7) | H37—O72—K2ix | 109 (3) |
O51iv—K2—O42iii | 148.27 (7) | H37—O72—Na2 | 92 (3) |
O52v—K2—Na1i | 41.57 (5) | H37—O72—H47 | 110 (4) |
O52v—K2—Na2vi | 112.76 (5) | K2viii—O81—K1viii | 154.19 (11) |
O52v—K2—O41ii | 148.04 (7) | Na1—O81—K1viii | 101.04 (11) |
O52v—K2—O42iii | 67.68 (7) | Na1—O81—K2viii | 85.54 (9) |
O52v—K2—O51iv | 139.96 (6) | H18—O81—K1viii | 85 (4) |
O71i—K2—Na1i | 38.42 (6) | H18—O81—K2viii | 109 (4) |
O71i—K2—Na2vi | 86.85 (6) | H18—O81—Na1 | 134 (3) |
O71i—K2—O41ii | 111.04 (8) | H28—O81—K1viii | 75 (4) |
O71i—K2—O42iii | 137.32 (8) | H28—O81—K2viii | 80 (4) |
O71i—K2—O51iv | 74.37 (7) | H28—O81—Na1 | 120 (4) |
O71i—K2—O52v | 74.08 (7) | H28—O81—H18 | 105 (5) |
H17i—K2—Na1i | 41.9 (9) | K2viii—H28—K1viii | 171 (2) |
H17i—K2—Na2vi | 93.2 (9) | O81—H28—K1viii | 89 (4) |
H17i—K2—O41ii | 99.2 (9) | O81—H28—K2viii | 85 (4) |
H17i—K2—O42iii | 137.7 (9) | K2ix—O82—K1viii | 154.20 (10) |
H17i—K2—O51iv | 72.5 (9) | Na2—O82—K1viii | 101.44 (11) |
H17i—K2—O52v | 81.6 (9) | Na2—O82—K2ix | 85.32 (9) |
H17i—K2—O71i | 12.6 (9) | H48—O82—K1viii | 82 (4) |
O72vi—K2—Na1i | 87.03 (6) | H48—O82—K2ix | 73 (4) |
O72vi—K2—Na2vi | 38.37 (5) | H48—O82—Na2 | 121 (4) |
O72vi—K2—O41ii | 137.50 (8) | H38—O82—K1viii | 87 (3) |
O72vi—K2—O42iii | 110.77 (8) | H38—O82—K2ix | 108 (3) |
O72vi—K2—O51iv | 74.12 (7) | H38—O82—Na2 | 129 (3) |
O72vi—K2—O52v | 74.40 (7) | H38—O82—H48 | 110 (5) |
O72vi—K2—O71i | 75.04 (7) | O82—H48—K2ix | 91 (4) |
O72vi—K2—H17i | 86.7 (9) | H29—O91—K1 | 151 (4) |
O81i—K2—Na1i | 38.91 (5) | H19—O91—K1 | 118 (5) |
O81i—K2—Na2vi | 150.77 (5) | H19—O91—H29 | 91 (6) |
O81i—K2—O41ii | 91.40 (7) | H39—O92—K1 | 132 (5) |
O81i—K2—O42iii | 81.34 (7) | H49—O92—K1 | 142 (3) |
O81i—K2—O51iv | 122.41 (7) | H49—O92—H39 | 86 (5) |
O81i—K2—O52v | 61.69 (7) | Na1—O101—K1viii | 95.39 (12) |
O81i—K2—O71i | 63.93 (7) | H210—O101—K1viii | 62 (3) |
O81i—K2—H17i | 58.1 (9) | H210—O101—Na1 | 120 (3) |
O81i—K2—O72vi | 125.76 (7) | H110—O101—K1viii | 103 (4) |
H28i—K2—Na1i | 48.6 (11) | H110—O101—Na1 | 132 (4) |
H28i—K2—Na2vi | 164.7 (11) | H110—O101—H210 | 108 (5) |
H28i—K2—O41ii | 90.5 (10) | O101—H210—K1viii | 102 (4) |
H28i—K2—O42iii | 65.9 (10) | Na2—O102—K1viii | 95.02 (12) |
H28i—K2—O51iv | 135.6 (10) | H410—O102—Na2 | 104 (5) |
H28i—K2—O52v | 58.8 (10) | H310—O102—K1viii | 95 (4) |
H28i—K2—O71i | 78.6 (11) | H310—O102—Na2 | 132 (4) |
H28i—K2—H17i | 73.5 (14) | H310—O102—H410 | 90 (5) |
H28i—K2—O72vi | 131.0 (10) | O102—H410—K1viii | 169 (6) |
H28i—K2—O81i | 15.5 (10) | H310—H410—K1viii | 139 (6) |
O82vi—K2—Na1i | 150.74 (5) | H310—H410—O102 | 47 (4) |
O82vi—K2—Na2vi | 38.91 (5) | O21—C11—O11 | 126.4 (3) |
O82vi—K2—O41ii | 81.53 (7) | C21—C11—O11 | 116.6 (3) |
O82vi—K2—O42iii | 91.54 (7) | C21—C11—O21 | 117.0 (3) |
O82vi—K2—O51iv | 61.70 (7) | C11—C21—O51 | 110.6 (2) |
O82vi—K2—O52v | 122.33 (7) | H21—C21—O51 | 106.6 (18) |
O82vi—K2—O71i | 125.58 (7) | H21—C21—C11 | 107.9 (17) |
O82vi—K2—H17i | 130.2 (9) | C31—C21—O51 | 109.5 (2) |
O82vi—K2—O72vi | 63.71 (7) | C31—C21—C11 | 110.6 (2) |
O82vi—K2—O81i | 169.73 (6) | C31—C21—H21 | 111.6 (17) |
O82vi—K2—H28i | 155.8 (11) | C21—C31—O61 | 110.4 (2) |
H48vi—K2—Na1i | 164.9 (11) | H31—C31—O61 | 106.8 (19) |
H48vi—K2—Na2vi | 48.9 (11) | H31—C31—C21 | 111.3 (18) |
H48vi—K2—O41ii | 66.3 (11) | C41—C31—O61 | 111.6 (3) |
H48vi—K2—O42iii | 90.0 (10) | C41—C31—C21 | 109.9 (2) |
H48vi—K2—O51iv | 59.5 (10) | C41—C31—H31 | 106.8 (17) |
H48vi—K2—O52v | 135.0 (10) | O31—C41—Na2ii | 49.51 (15) |
H48vi—K2—O71i | 131.5 (10) | O41—C41—Na2ii | 122.3 (2) |
H48vi—K2—H17i | 131.9 (13) | O41—C41—O31 | 126.0 (3) |
H48vi—K2—O72vi | 78.4 (11) | C31—C41—Na2ii | 96.53 (18) |
H48vi—K2—O81i | 155.8 (11) | C31—C41—O31 | 116.5 (3) |
H48vi—K2—H28i | 146.3 (11) | C31—C41—O41 | 117.5 (3) |
H48vi—K2—O82vi | 15.3 (11) | O22—C12—O12 | 126.4 (3) |
K2viii—Na1—K1viii | 98.17 (4) | C22—C12—O12 | 117.2 (2) |
O11—Na1—K1viii | 88.37 (7) | C22—C12—O22 | 116.4 (3) |
O11—Na1—K2viii | 133.83 (7) | C12—C22—O52 | 110.9 (2) |
O32iii—Na1—K1viii | 140.22 (8) | H22—C22—O52 | 106.9 (18) |
O32iii—Na1—K2viii | 108.39 (7) | H22—C22—C12 | 110.1 (18) |
O32iii—Na1—O11 | 93.68 (8) | C32—C22—O52 | 109.4 (2) |
O52iii—Na1—K1viii | 92.58 (7) | C32—C22—C12 | 110.5 (2) |
O52iii—Na1—K2viii | 52.67 (6) | C32—C22—H22 | 108.8 (17) |
O52iii—Na1—O11 | 173.20 (9) | C22—C32—O62 | 110.4 (2) |
O52iii—Na1—O32iii | 81.29 (8) | H32—C32—O62 | 106 (2) |
O71—Na1—K1viii | 127.24 (8) | H32—C32—C22 | 110.1 (19) |
O71—Na1—K2viii | 48.06 (7) | C42—C32—O62 | 111.3 (3) |
O71—Na1—O11 | 92.37 (9) | C42—C32—C22 | 110.5 (2) |
O71—Na1—O32iii | 92.41 (9) | C42—C32—H32 | 108.3 (19) |
O71—Na1—O52iii | 92.41 (9) | O32—C42—Na1x | 49.73 (15) |
O81—Na1—K1viii | 45.91 (9) | O42—C42—Na1x | 122.4 (2) |
O81—Na1—K2viii | 55.54 (8) | O42—C42—O32 | 126.2 (3) |
O81—Na1—O11 | 105.33 (10) | C32—C42—Na1x | 96.52 (17) |
O81—Na1—O32iii | 160.69 (10) | C32—C42—O32 | 116.7 (3) |
O81—Na1—O52iii | 80.01 (9) | C32—C42—O42 | 117.1 (3) |
| | | |
K1—O11—C11—O21 | −51.5 (2) | Na2ii—O51—C21—C31 | −11.3 (2) |
K1—O11—C11—C21 | 128.92 (19) | Na2ii—C41—C31—O61 | 62.43 (17) |
K1—O12—C12—O22 | −51.9 (2) | Na2ii—C41—C31—C21 | −60.39 (19) |
K1—O12—C12—C22 | 128.51 (19) | O11—C11—C21—O51 | −176.8 (3) |
K2vii—O41—C41—Na2ii | −73.48 (17) | O11—C11—C21—C31 | 61.7 (3) |
K2vii—O41—C41—O31 | −12.9 (2) | O12—C12—C22—O52 | −176.8 (3) |
K2vii—O41—C41—C31 | 167.77 (19) | O12—C12—C22—C32 | 61.6 (3) |
K2—O42iii—C42iii—Na1 | −73.35 (17) | O21—C11—C21—O51 | 3.5 (3) |
K2x—O42—C42—O32 | −12.3 (2) | O21—C11—C21—C31 | −117.9 (3) |
K2x—O42—C42—C32 | 168.24 (19) | O22—C12—C22—O52 | 3.6 (3) |
K2xi—O51—C21—C11 | 112.81 (19) | O22—C12—C22—C32 | −118.0 (3) |
K2xi—O51—C21—C31 | −125.10 (19) | O31—C41—C31—O61 | 14.7 (3) |
K2xii—O52—C22—C12 | 113.03 (19) | O31—C41—C31—C21 | −108.1 (3) |
K2xii—O52—C22—C32 | −124.73 (19) | O32—C42—C32—O62 | 15.1 (3) |
Na1—O11—C11—O21 | 76.6 (2) | O32—C42—C32—C22 | −108.0 (3) |
Na1—O11—C11—C21 | −103.0 (2) | O41—C41—C31—O61 | −165.8 (3) |
Na1x—O32—C42—O42 | −104.45 (19) | O41—C41—C31—C21 | 71.3 (3) |
Na1x—O32—C42—C32 | 74.99 (18) | O42—C42—C32—O62 | −165.4 (3) |
Na1x—O52—C22—C12 | −133.6 (2) | O42—C42—C32—C22 | 71.5 (3) |
Na1x—O52—C22—C32 | −11.4 (2) | O51—C21—C31—O61 | −68.0 (3) |
Na1x—C42—C32—O62 | 62.98 (16) | O51—C21—C31—C41 | 55.5 (3) |
Na1x—C42—C32—C22 | −60.08 (18) | O52—C22—C32—O62 | −68.3 (2) |
Na2—O12—C12—O22 | 76.7 (2) | O52—C22—C32—C42 | 55.3 (3) |
Na2—O12—C12—C22 | −102.9 (2) | O61—C31—C21—C11 | 54.1 (3) |
Na2ii—O31—C41—O41 | −104.33 (19) | O62—C32—C22—C12 | 54.1 (3) |
Na2ii—O31—C41—C31 | 75.05 (18) | C11—C21—C31—C41 | 177.6 (3) |
Na2ii—O51—C21—C11 | −133.4 (2) | C12—C22—C32—C42 | 177.7 (2) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (iv) x+1/2, −y+1/2, −z; (v) x+1/2, −y−1/2, −z; (vi) x+1, y, z−1; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (ix) x−1, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xii) x−1/2, −y−1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O51—H51···O21 | 0.75 (4) | 2.09 (4) | 2.604 (3) | 126 (4) |
O51—H51···O31i | 0.75 (4) | 2.74 (4) | 3.359 (3) | 141 (4) |
O51—H51···O41i | 0.75 (4) | 2.85 (4) | 3.265 (3) | 118 (4) |
O52—H52···O22 | 0.84 (4) | 2.08 (4) | 2.600 (3) | 119 (3) |
O52—H52···O32i | 0.84 (4) | 2.64 (4) | 3.359 (3) | 144 (3) |
O52—H52···O42i | 0.84 (4) | 2.79 (4) | 3.257 (3) | 117 (3) |
O61—H61···O102ii | 0.72 (3) | 2.24 (3) | 2.917 (4) | 158 (4) |
O62—H62···O101x | 0.77 (3) | 2.21 (3) | 2.938 (4) | 158 (4) |
O71—H17···O61 | 0.70 (5) | 2.11 (5) | 2.803 (3) | 175 (5) |
O71—H27···O41ii | 0.87 (4) | 2.03 (4) | 2.879 (4) | 165 (4) |
O72—H47···O42x | 0.81 (4) | 2.11 (4) | 2.889 (3) | 159 (4) |
O72—H37···O62 | 0.87 (5) | 1.92 (5) | 2.793 (3) | 176 (4) |
O81—H18···O11viii | 0.87 (5) | 2.85 (5) | 3.390 (3) | 122 (4) |
O81—H18···O21viii | 0.87 (5) | 1.89 (5) | 2.753 (3) | 174 (5) |
O81—H28···O32xiii | 0.83 (6) | 1.87 (6) | 2.703 (3) | 176 (5) |
O82—H48···O31xiv | 0.83 (5) | 1.89 (5) | 2.703 (3) | 168 (6) |
O82—H38···O12viii | 0.88 (5) | 2.90 (5) | 3.388 (3) | 117 (4) |
O82—H38···O22viii | 0.88 (5) | 1.89 (5) | 2.754 (3) | 167 (4) |
O91—H29···O42i | 0.85 (5) | 2.03 (6) | 2.813 (4) | 153 (6) |
O91—H19···O22v | 0.75 (6) | 2.52 (6) | 3.107 (4) | 137 (5) |
O91—H19···O32iii | 0.75 (6) | 2.73 (6) | 3.173 (4) | 120 (6) |
O91—H19···O62iii | 0.75 (6) | 2.53 (6) | 3.147 (4) | 141 (6) |
O92—H39···O21xi | 0.78 (6) | 2.43 (6) | 3.114 (4) | 148 (5) |
O92—H39···O31vii | 0.78 (6) | 2.88 (6) | 3.177 (4) | 105 (5) |
O92—H39···O61vii | 0.78 (6) | 2.60 (6) | 3.144 (4) | 129 (5) |
O92—H49···O41i | 1.00 (5) | 1.82 (6) | 2.816 (4) | 170 (5) |
O101—H210···O91viii | 0.93 (5) | 1.83 (5) | 2.753 (5) | 172 (5) |
O101—H110···O12 | 0.83 (6) | 1.90 (6) | 2.733 (4) | 174 (5) |
O102—H410···O92viii | 0.74 (5) | 2.38 (6) | 2.761 (4) | 114 (6) |
O102—H310···O11 | 0.80 (6) | 1.94 (6) | 2.729 (4) | 168 (5) |
Symmetry codes: (i) x, y, z−1; (ii) x+1/2, −y+1/2, −z+1; (iii) x+1/2, −y−1/2, −z+1; (v) x+1/2, −y−1/2, −z; (vii) x−1/2, −y+1/2, −z+1; (viii) x, y, z+1; (x) x−1/2, −y−1/2, −z+1; (xi) x−1/2, −y+1/2, −z; (xiii) x+1/2, −y−1/2, −z+2; (xiv) x−1/2, −y+1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (298K_anh)
top
Crystal data top
C4H12KNaO10 | Dx = 1.776 Mg m−3 |
Mr = 282.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 6467 reflections |
a = 11.8843 (9) Å | θ = 3.6–28.7° |
b = 14.2668 (12) Å | µ = 0.59 mm−1 |
c = 6.2266 (5) Å | T = 298 K |
V = 1055.74 (14) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 585.519 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2713 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2175 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.057 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −19→18 |
Tmin = 0.750, Tmax = 1.000 | l = −8→8 |
18499 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.037 | w = 1/[σ2(Fo2) + (0.0187P)2 + 0.4246P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.075 | (Δ/σ)max = 0.001 |
S = 1.13 | Δρmax = 0.39 e Å−3 |
2713 reflections | Δρmin = −0.29 e Å−3 |
195 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
1 restraint | Absolute structure parameter: 0.06 (3) |
12 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0 | 0.0 | 0.0469 (3) | 0.0631 (7) | |
K2 | 0.5 | 0.0 | −0.15886 (12) | 0.03640 (19) | |
Na | 0.23137 (7) | −0.00679 (7) | 0.52269 (14) | 0.0304 (2) | |
O1 | 0.12004 (13) | 0.10919 (11) | 0.3507 (3) | 0.0289 (4) | |
O2 | 0.20945 (15) | 0.20275 (12) | 0.1192 (3) | 0.0345 (4) | |
O3 | 0.23313 (16) | 0.40623 (12) | 0.8129 (3) | 0.0404 (4) | |
O4 | 0.05341 (15) | 0.36239 (13) | 0.8440 (3) | 0.0390 (4) | |
O5 | 0.16324 (15) | 0.35716 (12) | 0.3240 (3) | 0.0298 (4) | |
H5 | 0.189 (2) | 0.342 (2) | 0.216 (5) | 0.0447 (6)* | |
O6 | 0.29523 (14) | 0.24820 (12) | 0.6277 (3) | 0.0329 (4) | |
H6 | 0.327 (3) | 0.290 (2) | 0.607 (5) | 0.0493 (6)* | |
O7 | 0.39556 (15) | 0.08240 (14) | 0.4847 (3) | 0.0370 (5) | |
H17 | 0.368 (3) | 0.131 (2) | 0.521 (6) | 0.0555 (7)* | |
H27 | 0.431 (3) | 0.091 (2) | 0.374 (5) | 0.0555 (7)* | |
O8 | 0.2437 (2) | 0.04125 (15) | 0.8852 (3) | 0.0513 (6) | |
H18 | 0.258 (3) | 0.003 (3) | 0.986 (6) | 0.0770 (9)* | |
H28 | 0.236 (3) | 0.096 (3) | 0.947 (6) | 0.0770 (9)* | |
O9 | 0.06177 (18) | −0.1981 (2) | −0.0344 (4) | 0.0612 (7) | |
H19 | 0.115 (4) | −0.224 (3) | 0.009 (7) | 0.0918 (10)* | |
H29 | 0.034 (3) | −0.253 (3) | −0.085 (6) | 0.0918 (10)* | |
O10 | 0.07534 (19) | −0.10238 (18) | 0.5816 (5) | 0.0615 (7) | |
H110 | 0.017 (4) | −0.100 (3) | 0.523 (6) | 0.0922 (11)* | |
H210 | 0.068 (3) | −0.131 (3) | 0.701 (7) | 0.0922 (11)* | |
C1 | 0.15407 (19) | 0.18764 (16) | 0.2851 (4) | 0.0236 (5) | |
C2 | 0.12502 (19) | 0.27322 (16) | 0.4227 (4) | 0.0237 (5) | |
H2 | 0.041 (2) | 0.2798 (17) | 0.437 (4) | 0.0284 (6)* | |
C3 | 0.17776 (19) | 0.26416 (16) | 0.6448 (4) | 0.0246 (5) | |
H3 | 0.148 (2) | 0.2085 (18) | 0.719 (4) | 0.0295 (6)* | |
C4 | 0.1526 (2) | 0.35159 (17) | 0.7794 (4) | 0.0295 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0734 (15) | 0.0649 (17) | 0.0511 (14) | −0.0351 (14) | −0.000000 | 0.000000 |
K2 | 0.0363 (4) | 0.0406 (4) | 0.0323 (4) | −0.0045 (4) | −0.000000 | 0.000000 |
Na | 0.0293 (4) | 0.0276 (5) | 0.0343 (5) | −0.0008 (4) | −0.0013 (4) | 0.0007 (4) |
O1 | 0.0312 (8) | 0.0241 (8) | 0.0314 (8) | −0.0020 (7) | −0.0013 (8) | −0.0009 (7) |
O2 | 0.0444 (10) | 0.0306 (9) | 0.0285 (9) | −0.0002 (8) | 0.0077 (8) | −0.0017 (7) |
O3 | 0.0526 (11) | 0.0303 (9) | 0.0383 (10) | −0.0082 (8) | −0.0034 (9) | −0.0076 (8) |
O4 | 0.0396 (10) | 0.0461 (11) | 0.0314 (9) | 0.0127 (9) | 0.0016 (8) | −0.0075 (9) |
O5 | 0.0440 (10) | 0.0224 (8) | 0.0230 (8) | −0.0002 (7) | −0.0001 (8) | 0.0006 (7) |
O6 | 0.0283 (9) | 0.0290 (10) | 0.0415 (10) | 0.0042 (7) | −0.0051 (8) | −0.0011 (8) |
O7 | 0.0324 (10) | 0.0322 (10) | 0.0464 (12) | −0.0001 (8) | 0.0071 (9) | 0.0025 (9) |
O8 | 0.0961 (17) | 0.0295 (10) | 0.0283 (10) | 0.0114 (11) | 0.0052 (11) | −0.0004 (8) |
O9 | 0.0394 (12) | 0.090 (2) | 0.0543 (14) | −0.0073 (12) | −0.0101 (11) | 0.0074 (13) |
O10 | 0.0365 (11) | 0.0654 (15) | 0.0826 (18) | −0.0161 (11) | −0.0181 (12) | 0.0319 (13) |
C1 | 0.0233 (11) | 0.0254 (12) | 0.0222 (11) | 0.0014 (9) | −0.0033 (9) | 0.0004 (9) |
C2 | 0.0251 (11) | 0.0205 (11) | 0.0253 (11) | 0.0012 (9) | −0.0002 (10) | −0.0001 (9) |
C3 | 0.0275 (11) | 0.0228 (11) | 0.0236 (11) | 0.0018 (9) | 0.0008 (10) | 0.0014 (10) |
C4 | 0.0426 (15) | 0.0258 (12) | 0.0202 (11) | 0.0043 (11) | −0.0051 (11) | 0.0006 (9) |
Geometric parameters (Å, º) top
K1—O1 | 2.835 (2) | Na—O7 | 2.342 (2) |
K1—O1i | 2.835 (2) | Na—O8 | 2.363 (2) |
K1—O8ii | 3.122 (3) | Na—O10 | 2.331 (2) |
K1—O8iii | 3.122 (3) | Na—C4v | 3.086 (3) |
K1—H18iii | 3.08 (4) | O1—C1 | 1.258 (3) |
K1—H18ii | 3.08 (4) | O2—C1 | 1.244 (3) |
K1—O9i | 2.963 (3) | O3—C4 | 1.252 (3) |
K1—O9 | 2.963 (3) | O4—C4 | 1.255 (3) |
K1—O10ii | 3.366 (4) | O5—H5 | 0.77 (3) |
K1—O10iii | 3.366 (4) | O5—C2 | 1.420 (3) |
K1—H210ii | 2.96 (4) | O6—H6 | 0.72 (3) |
K1—H210iii | 2.96 (4) | O6—C3 | 1.418 (3) |
K2—O4iv | 2.8462 (18) | O7—H17 | 0.80 (3) |
K2—O4v | 2.8462 (18) | O7—H27 | 0.81 (3) |
K2—O5vi | 2.9957 (17) | O8—H18 | 0.85 (4) |
K2—O5vii | 2.9957 (17) | O8—H28 | 0.87 (4) |
K2—O7iii | 2.802 (2) | O9—H19 | 0.78 (4) |
K2—O7viii | 2.802 (2) | O9—H29 | 0.91 (4) |
K2—O8iii | 3.114 (3) | O10—H110 | 0.79 (4) |
K2—O8viii | 3.114 (3) | O10—H210 | 0.85 (4) |
K2—H18viii | 3.02 (4) | C1—C2 | 1.531 (3) |
K2—H18iii | 3.02 (4) | C2—H2 | 1.00 (2) |
Na—O1 | 2.3740 (19) | C2—C3 | 1.524 (3) |
Na—O3v | 2.467 (2) | C3—H3 | 0.99 (3) |
Na—O5v | 2.499 (2) | C3—C4 | 1.532 (3) |
| | | |
Naii—K1—Naiii | 80.26 (4) | O8iii—K2—O5vii | 122.35 (5) |
O1—K1—Naiii | 101.44 (4) | O8iii—K2—O5vi | 61.67 (5) |
O1—K1—Naii | 145.25 (4) | O8viii—K2—O5vi | 122.35 (5) |
O1i—K1—Naiii | 145.25 (4) | O8iii—K2—O7iii | 63.72 (5) |
O1i—K1—Naii | 101.44 (4) | O8viii—K2—O7viii | 63.72 (5) |
O1i—K1—O1 | 96.32 (9) | O8iii—K2—O7viii | 125.61 (6) |
O8iii—K1—Naiii | 32.88 (4) | O8viii—K2—O7iii | 125.61 (6) |
O8iii—K1—Naii | 110.28 (7) | O8viii—K2—O8iii | 169.90 (7) |
O8ii—K1—Naii | 32.88 (4) | H18viii—K2—Naiii | 165.4 (7) |
O8ii—K1—Naiii | 110.28 (7) | H18iii—K2—Naiii | 49.3 (7) |
O8ii—K1—O1 | 141.76 (6) | H18viii—K2—Naviii | 49.3 (7) |
O8iii—K1—O1i | 141.76 (6) | H18iii—K2—Naviii | 165.4 (7) |
O8iii—K1—O1 | 69.20 (5) | H18iii—K2—O4iv | 89.9 (7) |
O8ii—K1—O1i | 69.20 (5) | H18viii—K2—O4v | 89.9 (7) |
O8ii—K1—O8iii | 142.37 (10) | H18iii—K2—O4v | 65.8 (8) |
H18ii—K1—Naii | 42.9 (7) | H18viii—K2—O4iv | 65.8 (8) |
H18iii—K1—Naii | 123.0 (7) | H18iii—K2—O5vi | 59.5 (8) |
H18ii—K1—Naiii | 123.0 (7) | H18viii—K2—O5vi | 135.4 (8) |
H18iii—K1—Naiii | 42.9 (7) | H18viii—K2—O5vii | 59.5 (8) |
H18iii—K1—O1i | 126.0 (8) | H18iii—K2—O5vii | 135.4 (8) |
H18ii—K1—O1i | 64.9 (7) | H18iii—K2—O7iii | 79.0 (7) |
H18ii—K1—O1 | 126.0 (8) | H18viii—K2—O7viii | 79.0 (7) |
H18iii—K1—O1 | 64.9 (7) | H18iii—K2—O7viii | 131.6 (7) |
H18ii—K1—O8ii | 15.8 (7) | H18viii—K2—O7iii | 131.6 (7) |
H18iii—K1—O8iii | 15.8 (7) | H18iii—K2—O8viii | 155.4 (7) |
H18ii—K1—O8iii | 152.0 (7) | H18iii—K2—O8iii | 15.9 (8) |
H18iii—K1—O8ii | 152.0 (7) | H18viii—K2—O8iii | 155.4 (7) |
H18ii—K1—H18iii | 165.9 (14) | H18viii—K2—O8viii | 15.9 (8) |
O9—K1—Naii | 92.90 (6) | H18viii—K2—H18iii | 145.2 (14) |
O9—K1—Naiii | 71.83 (6) | K2ix—Na—K1x | 98.23 (3) |
O9i—K1—Naii | 71.83 (6) | O1—Na—K1x | 88.29 (5) |
O9i—K1—Naiii | 92.90 (6) | O1—Na—K2ix | 133.89 (5) |
O9—K1—O1i | 73.42 (6) | O3v—Na—K1x | 140.29 (6) |
O9i—K1—O1 | 73.42 (6) | O3v—Na—K2ix | 108.33 (5) |
O9—K1—O1 | 120.88 (7) | O3v—Na—O1 | 93.65 (6) |
O9i—K1—O1i | 120.88 (7) | O5v—Na—K1x | 92.77 (5) |
O9—K1—O8iii | 83.96 (6) | O5v—Na—K2ix | 52.63 (4) |
O9i—K1—O8iii | 89.71 (6) | O5v—Na—O1 | 173.15 (7) |
O9—K1—O8ii | 89.71 (6) | O5v—Na—O3v | 81.21 (6) |
O9i—K1—O8ii | 83.96 (6) | O7—Na—K1x | 126.99 (6) |
O9—K1—H18iii | 75.2 (8) | O7—Na—K2ix | 48.06 (5) |
O9i—K1—H18ii | 75.2 (8) | O7—Na—O1 | 92.29 (7) |
O9—K1—H18ii | 102.3 (8) | O7—Na—O3v | 92.59 (8) |
O9i—K1—H18iii | 102.3 (8) | O7—Na—O5v | 92.47 (7) |
O9i—K1—O9 | 160.33 (13) | O8—Na—K1x | 45.83 (7) |
O10iii—K1—Naii | 61.51 (5) | O8—Na—K2ix | 55.68 (6) |
O10ii—K1—Naiii | 61.51 (5) | O8—Na—O1 | 105.27 (8) |
O10iii—K1—Naiii | 32.93 (4) | O8—Na—O3v | 160.79 (8) |
O10ii—K1—Naii | 32.93 (4) | O8—Na—O5v | 80.18 (7) |
O10iii—K1—O1i | 118.01 (5) | O8—Na—O7 | 83.53 (8) |
O10ii—K1—O1i | 132.75 (5) | O10—Na—K1x | 51.72 (8) |
O10ii—K1—O1 | 118.01 (5) | O10—Na—K2ix | 127.42 (7) |
O10iii—K1—O1 | 132.75 (5) | O10—Na—O1 | 92.03 (8) |
O10iii—K1—O8ii | 83.53 (6) | O10—Na—O3v | 88.58 (9) |
O10iii—K1—O8iii | 63.73 (6) | O10—Na—O5v | 83.35 (8) |
O10ii—K1—O8iii | 83.53 (6) | O10—Na—O7 | 175.44 (9) |
O10ii—K1—O8ii | 63.73 (6) | O10—Na—O8 | 93.94 (10) |
O10iii—K1—H18iii | 68.6 (7) | C4v—Na—K1x | 140.24 (5) |
O10ii—K1—H18ii | 68.6 (7) | C4v—Na—K2ix | 87.64 (5) |
O10iii—K1—H18ii | 98.8 (7) | C4v—Na—O1 | 115.49 (7) |
O10ii—K1—H18iii | 98.8 (7) | C4v—Na—O3v | 22.75 (6) |
O10iii—K1—O9 | 51.19 (7) | C4v—Na—O5v | 60.03 (6) |
O10ii—K1—O9i | 51.19 (7) | C4v—Na—O7 | 85.51 (7) |
O10iii—K1—O9i | 109.44 (9) | C4v—Na—O8 | 138.10 (8) |
O10ii—K1—O9 | 109.44 (9) | C4v—Na—O10 | 93.92 (10) |
O10ii—K1—O10iii | 61.20 (9) | Na—O1—K1 | 101.45 (6) |
H210ii—K1—Naiii | 68.5 (8) | C1—O1—K1 | 115.73 (15) |
H210iii—K1—Naiii | 41.8 (8) | C1—O1—Na | 125.97 (14) |
H210ii—K1—Naii | 41.8 (8) | C4—O3—Naxi | 107.62 (15) |
H210iii—K1—Naii | 68.5 (8) | C4—O4—K2xii | 120.99 (16) |
H210iii—K1—O1i | 106.0 (8) | Naxi—O5—K2xiii | 85.83 (5) |
H210ii—K1—O1i | 134.0 (8) | H5—O5—K2xiii | 98 (2) |
H210ii—K1—O1 | 106.0 (8) | H5—O5—Naxi | 111 (2) |
H210iii—K1—O1 | 134.0 (8) | C2—O5—K2xiii | 120.99 (13) |
H210ii—K1—O8iii | 84.2 (8) | C2—O5—Naxi | 130.53 (14) |
H210iii—K1—O8ii | 84.2 (8) | C2—O5—H5 | 105 (2) |
H210iii—K1—O8iii | 68.4 (8) | C3—O6—H6 | 113 (3) |
H210ii—K1—O8ii | 68.4 (8) | Na—O7—K2xiv | 93.50 (7) |
H210ii—K1—H18ii | 69.4 (11) | H17—O7—K2xiv | 109 (2) |
H210iii—K1—H18iii | 69.4 (11) | H17—O7—Na | 95 (2) |
H210ii—K1—H18iii | 99.9 (11) | H27—O7—K2xiv | 121 (2) |
H210iii—K1—H18ii | 99.9 (11) | H27—O7—Na | 126 (2) |
H210ii—K1—O9 | 123.0 (9) | H27—O7—H17 | 108 (3) |
H210iii—K1—O9i | 123.0 (9) | K2xiv—O8—K1xiv | 154.16 (8) |
H210iii—K1—O9 | 37.5 (9) | Na—O8—K1xiv | 101.29 (9) |
H210ii—K1—O9i | 37.5 (9) | Na—O8—K2xiv | 85.51 (7) |
H210iii—K1—O10ii | 73.8 (9) | H18—O8—K1xiv | 80 (2) |
H210ii—K1—O10ii | 13.7 (9) | H18—O8—K2xiv | 76 (2) |
H210iii—K1—O10iii | 13.7 (9) | H18—O8—Na | 122 (3) |
H210ii—K1—O10iii | 73.8 (9) | H28—O8—K1xiv | 86 (3) |
H210ii—K1—H210iii | 86.8 (17) | H28—O8—K2xiv | 108 (2) |
Naviii—K2—Naiii | 116.33 (3) | H28—O8—Na | 132 (2) |
O4iv—K2—Naviii | 98.98 (4) | H28—O8—H18 | 106 (3) |
O4v—K2—Naviii | 124.78 (4) | K2xiv—H18—K1xiv | 169.6 (14) |
O4v—K2—Naiii | 98.98 (4) | O8—H18—K1xiv | 85 (3) |
O4iv—K2—Naiii | 124.78 (4) | O8—H18—K2xiv | 88 (3) |
O4v—K2—O4iv | 92.93 (8) | H19—O9—K1i | 127 (3) |
O5vi—K2—Naviii | 112.73 (4) | H29—O9—K1i | 143 (3) |
O5vi—K2—Naiii | 41.54 (4) | H29—O9—H19 | 90 (4) |
O5vii—K2—Naiii | 112.73 (4) | Na—O10—K1x | 95.35 (9) |
O5vii—K2—Naviii | 41.54 (4) | H110—O10—K1x | 98 (3) |
O5vi—K2—O4v | 67.84 (5) | H110—O10—Na | 128 (3) |
O5vi—K2—O4iv | 148.22 (5) | H210—O10—K1x | 55 (3) |
O5vii—K2—O4v | 148.22 (5) | H210—O10—Na | 120 (3) |
O5vii—K2—O4iv | 67.84 (5) | H210—O10—H110 | 109 (4) |
O5vi—K2—O5vii | 139.85 (7) | O10—H210—K1x | 111 (3) |
O7viii—K2—Naviii | 38.44 (4) | O2—C1—O1 | 126.4 (2) |
O7iii—K2—Naviii | 86.99 (4) | C2—C1—O1 | 117.1 (2) |
O7viii—K2—Naiii | 86.99 (4) | C2—C1—O2 | 116.5 (2) |
O7iii—K2—Naiii | 38.44 (4) | C1—C2—O5 | 111.00 (18) |
O7iii—K2—O4iv | 110.80 (6) | H2—C2—O5 | 106.0 (14) |
O7iii—K2—O4v | 137.42 (5) | H2—C2—C1 | 110.3 (14) |
O7viii—K2—O4iv | 137.42 (5) | C3—C2—O5 | 109.42 (18) |
O7viii—K2—O4v | 110.80 (6) | C3—C2—C1 | 110.32 (19) |
O7iii—K2—O5vi | 74.13 (5) | C3—C2—H2 | 109.6 (14) |
O7viii—K2—O5vii | 74.13 (5) | C2—C3—O6 | 110.49 (19) |
O7iii—K2—O5vii | 74.31 (5) | H3—C3—O6 | 105.1 (14) |
O7viii—K2—O5vi | 74.31 (5) | H3—C3—C2 | 110.3 (15) |
O7viii—K2—O7iii | 75.21 (8) | C4—C3—O6 | 111.3 (2) |
O8viii—K2—Naiii | 150.70 (4) | C4—C3—C2 | 110.30 (18) |
O8iii—K2—Naiii | 38.81 (4) | C4—C3—H3 | 109.1 (14) |
O8viii—K2—Naviii | 38.81 (4) | O3—C4—Naxi | 49.63 (12) |
O8iii—K2—Naviii | 150.70 (4) | O4—C4—Naxi | 122.33 (17) |
O8viii—K2—O4iv | 81.47 (5) | O4—C4—O3 | 126.0 (2) |
O8iii—K2—O4iv | 91.55 (5) | C3—C4—Naxi | 96.46 (14) |
O8iii—K2—O4v | 81.47 (5) | C3—C4—O3 | 116.7 (2) |
O8viii—K2—O4v | 91.55 (5) | C3—C4—O4 | 117.3 (2) |
O8viii—K2—O5vii | 61.67 (5) | | |
| | | |
K1—O1—C1—O2 | −51.59 (16) | Naxi—O3—C4—C3 | 74.82 (14) |
K1i—O1—C1—O2 | −51.59 (16) | Naxi—O5—C2—C1 | −133.35 (18) |
K1—O1—C1—C2 | 128.58 (14) | Naxi—O5—C2—C3 | −11.35 (17) |
K1i—O1—C1—C2 | 128.58 (14) | Naxi—C4—C3—O6 | 62.91 (14) |
K2xii—O4—C4—Naxi | −73.36 (14) | Naxi—C4—C3—C2 | −60.13 (14) |
K2—O4v—C4v—Na | −73.36 (14) | O1—C1—C2—O5 | −176.8 (2) |
K2xii—O4—C4—O3 | −12.54 (19) | O1—C1—C2—C3 | 61.7 (2) |
K2xi—O4—C4—O3 | −12.54 (19) | O2—C1—C2—O5 | 3.3 (2) |
K2xii—O4—C4—C3 | 168.19 (15) | O2—C1—C2—C3 | −118.2 (2) |
K2xi—O4—C4—C3 | 168.19 (15) | O3—C4—C3—O6 | 15.2 (2) |
K2xv—O5—C2—C1 | 112.95 (15) | O3—C4—C3—C2 | −107.9 (2) |
K2xiii—O5—C2—C1 | 112.95 (15) | O4—C4—C3—O6 | −165.5 (2) |
K2xiii—O5—C2—C3 | −125.05 (15) | O4—C4—C3—C2 | 71.5 (2) |
K2xv—O5—C2—C3 | −125.05 (15) | O5—C2—C3—O6 | −68.19 (19) |
Na—O1—C1—O2 | 76.86 (19) | O5—C2—C3—C4 | 55.3 (2) |
Na—O1—C1—C2 | −102.96 (17) | O6—C3—C2—C1 | 54.2 (2) |
Naxi—O3—C4—O4 | −104.45 (16) | C1—C2—C3—C4 | 177.75 (19) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (vii) x+1/2, −y+1/2, −z; (viii) −x+1, −y, z−1; (ix) −x+1, −y, z+1; (x) −x, −y, z+1; (xi) −x+1/2, y+1/2, −z+1; (xii) x−1/2, −y+1/2, −z+1; (xiii) x−1/2, −y+1/2, −z; (xiv) x, y, z+1; (xv) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.77 (3) | 2.09 (3) | 2.604 (2) | 125 (3) |
O5—H5···O3iii | 0.77 (3) | 2.72 (3) | 3.363 (3) | 142 (3) |
O5—H5···O4iii | 0.77 (3) | 2.83 (3) | 3.262 (3) | 118 (3) |
O6—H6···O10xi | 0.72 (3) | 2.25 (3) | 2.934 (4) | 158 (4) |
O7—H17···O6 | 0.80 (3) | 2.00 (4) | 2.795 (3) | 176 (4) |
O7—H27···O4iv | 0.81 (3) | 2.10 (3) | 2.886 (3) | 162 (3) |
O8—H18···O3xvi | 0.85 (4) | 1.86 (4) | 2.706 (3) | 170 (4) |
O8—H28···O1xiv | 0.87 (4) | 2.87 (4) | 3.391 (3) | 120 (3) |
O8—H28···O2xiv | 0.87 (4) | 1.89 (4) | 2.756 (3) | 170 (4) |
O9—H19···O2vi | 0.78 (4) | 2.47 (4) | 3.110 (3) | 141 (4) |
O9—H19···O3v | 0.78 (4) | 2.82 (5) | 3.171 (3) | 110 (4) |
O9—H19···O6v | 0.78 (4) | 2.53 (4) | 3.144 (3) | 136 (4) |
O9—H29···O4ii | 0.91 (4) | 1.92 (4) | 2.819 (3) | 167 (4) |
O10—H110···O1i | 0.79 (4) | 1.95 (4) | 2.733 (3) | 172 (4) |
O10—H210···O9xiv | 0.85 (4) | 1.91 (4) | 2.758 (4) | 176 (4) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (xi) −x+1/2, y+1/2, −z+1; (xiv) x, y, z+1; (xvi) −x+1/2, y−1/2, −z+2. |
Sodium potassium L(+)-tartrate tetrahydrate (308K_anh)
top
Crystal data top
C4H12KNaO10 | Dx = 1.771 Mg m−3 |
Mr = 282.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P21212 | Cell parameters from 6554 reflections |
a = 11.8996 (9) Å | θ = 3.5–28.7° |
b = 14.2713 (11) Å | µ = 0.58 mm−1 |
c = 6.2331 (4) Å | T = 308 K |
V = 1058.51 (13) Å3 | Prism, clear colourless |
Z = 4 | 0.48 × 0.45 × 0.3 mm |
F(000) = 585.519 | |
Data collection top
Xcalibur, Ruby, Gemini ultra diffractometer | 2726 independent reflections |
Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2156 reflections with I ≥ 2u(I) |
Graphite monochromator | Rint = 0.064 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 29.4°, θmin = 3.3° |
ω scans | h = −16→16 |
Absorption correction: multi-scan CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | k = −18→19 |
Tmin = 0.461, Tmax = 1.000 | l = −8→8 |
18474 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.038 | w = 1/[σ2(Fo2) + (0.0306P)2 + 0.4128P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.090 | (Δ/σ)max = −0.0003 |
S = 1.10 | Δρmax = 0.29 e Å−3 |
2726 reflections | Δρmin = −0.32 e Å−3 |
195 parameters | Absolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668. |
1 restraint | Absolute structure parameter: 0.06 (3) |
12 constraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.0 | 0.0 | 0.0473 (4) | 0.0648 (8) | |
K2 | 0.5 | 0.0 | −0.15874 (13) | 0.0375 (2) | |
Na | 0.23131 (8) | −0.00680 (8) | 0.52312 (15) | 0.0312 (2) | |
O1 | 0.12004 (14) | 0.10919 (12) | 0.3508 (3) | 0.0301 (4) | |
O2 | 0.20924 (17) | 0.20259 (13) | 0.1194 (3) | 0.0354 (4) | |
O3 | 0.23338 (17) | 0.40629 (13) | 0.8127 (3) | 0.0414 (5) | |
O4 | 0.05368 (17) | 0.36267 (14) | 0.8437 (3) | 0.0402 (5) | |
O5 | 0.16323 (16) | 0.35709 (12) | 0.3237 (3) | 0.0307 (4) | |
H5 | 0.189 (3) | 0.341 (2) | 0.205 (6) | 0.0460 (6)* | |
O6 | 0.29515 (15) | 0.24816 (13) | 0.6273 (3) | 0.0330 (4) | |
H6 | 0.327 (3) | 0.293 (2) | 0.614 (6) | 0.0495 (7)* | |
O7 | 0.39539 (16) | 0.08229 (15) | 0.4848 (4) | 0.0381 (5) | |
H17 | 0.363 (3) | 0.134 (3) | 0.526 (6) | 0.0571 (7)* | |
H27 | 0.434 (3) | 0.094 (3) | 0.379 (6) | 0.0571 (7)* | |
O8 | 0.2440 (2) | 0.04116 (17) | 0.8857 (3) | 0.0528 (6) | |
H18 | 0.261 (3) | 0.002 (3) | 0.984 (7) | 0.0791 (10)* | |
H28 | 0.235 (3) | 0.094 (3) | 0.947 (7) | 0.0791 (10)* | |
O9 | 0.0620 (2) | −0.1988 (2) | −0.0347 (5) | 0.0626 (7) | |
H19 | 0.115 (4) | −0.228 (4) | 0.009 (8) | 0.0939 (11)* | |
H29 | 0.033 (4) | −0.257 (3) | −0.078 (7) | 0.0939 (11)* | |
O10 | 0.0751 (2) | −0.1019 (2) | 0.5830 (5) | 0.0643 (8) | |
H110 | 0.016 (4) | −0.100 (3) | 0.526 (7) | 0.0964 (12)* | |
H210 | 0.070 (4) | −0.137 (3) | 0.704 (8) | 0.0964 (12)* | |
C1 | 0.1540 (2) | 0.18754 (17) | 0.2845 (4) | 0.0241 (5) | |
C2 | 0.1249 (2) | 0.27307 (17) | 0.4226 (4) | 0.0247 (5) | |
H2 | 0.041 (2) | 0.2784 (19) | 0.436 (4) | 0.0297 (6)* | |
C3 | 0.1780 (2) | 0.26408 (17) | 0.6447 (4) | 0.0250 (5) | |
H3 | 0.148 (2) | 0.211 (2) | 0.723 (5) | 0.0300 (6)* | |
C4 | 0.1528 (2) | 0.35170 (18) | 0.7791 (4) | 0.0304 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0739 (16) | 0.0690 (19) | 0.0516 (15) | −0.0377 (16) | −0.000000 | 0.000000 |
K2 | 0.0373 (4) | 0.0415 (5) | 0.0336 (4) | −0.0043 (4) | −0.000000 | 0.000000 |
Na | 0.0299 (5) | 0.0281 (5) | 0.0357 (5) | −0.0008 (4) | −0.0016 (4) | 0.0011 (5) |
O1 | 0.0333 (9) | 0.0240 (9) | 0.0330 (9) | −0.0017 (7) | −0.0014 (8) | −0.0008 (8) |
O2 | 0.0454 (11) | 0.0317 (10) | 0.0292 (10) | −0.0001 (8) | 0.0077 (9) | −0.0012 (8) |
O3 | 0.0530 (12) | 0.0309 (10) | 0.0402 (11) | −0.0089 (9) | −0.0039 (10) | −0.0071 (9) |
O4 | 0.0406 (10) | 0.0472 (12) | 0.0327 (10) | 0.0123 (9) | 0.0013 (9) | −0.0085 (10) |
O5 | 0.0455 (11) | 0.0220 (9) | 0.0246 (9) | −0.0001 (8) | −0.0001 (8) | 0.0015 (7) |
O6 | 0.0284 (10) | 0.0285 (10) | 0.0420 (11) | 0.0046 (7) | −0.0058 (9) | −0.0023 (9) |
O7 | 0.0330 (10) | 0.0322 (11) | 0.0489 (13) | −0.0008 (8) | 0.0073 (9) | 0.0031 (10) |
O8 | 0.0973 (19) | 0.0304 (11) | 0.0305 (11) | 0.0124 (12) | 0.0057 (12) | −0.0002 (8) |
O9 | 0.0416 (13) | 0.091 (2) | 0.0548 (15) | −0.0085 (13) | −0.0106 (12) | 0.0070 (14) |
O10 | 0.0373 (12) | 0.0674 (17) | 0.088 (2) | −0.0182 (11) | −0.0197 (13) | 0.0341 (15) |
C1 | 0.0247 (12) | 0.0237 (12) | 0.0240 (12) | 0.0019 (10) | −0.0044 (10) | −0.0008 (9) |
C2 | 0.0263 (12) | 0.0214 (12) | 0.0265 (12) | 0.0012 (10) | −0.0009 (10) | −0.0009 (10) |
C3 | 0.0287 (12) | 0.0218 (12) | 0.0245 (11) | 0.0025 (10) | 0.0010 (10) | 0.0012 (10) |
C4 | 0.0438 (16) | 0.0263 (13) | 0.0211 (12) | 0.0047 (12) | −0.0043 (11) | 0.0009 (10) |
Geometric parameters (Å, º) top
K1—O1 | 2.837 (2) | Na—O8 | 2.366 (2) |
K1—O1i | 2.837 (2) | Na—O10 | 2.332 (2) |
K1—O8ii | 3.129 (3) | Na—C4v | 3.087 (3) |
K1—O8iii | 3.129 (3) | O1—C1 | 1.259 (3) |
K1—O9i | 2.975 (3) | O2—C1 | 1.240 (3) |
K1—O9 | 2.975 (3) | O3—C4 | 1.253 (3) |
K1—O10iii | 3.360 (4) | O4—C4 | 1.256 (3) |
K1—O10ii | 3.360 (4) | O5—H5 | 0.83 (4) |
K1—H210ii | 3.01 (5) | O5—C2 | 1.423 (3) |
K1—H210iii | 3.01 (5) | O6—H6 | 0.74 (3) |
K2—O4iv | 2.847 (2) | O6—C3 | 1.417 (3) |
K2—O4v | 2.847 (2) | O7—H17 | 0.87 (4) |
K2—O5vi | 2.9983 (18) | O7—H27 | 0.82 (4) |
K2—O5vii | 2.9983 (18) | O8—H18 | 0.86 (5) |
K2—O7iii | 2.805 (2) | O8—H28 | 0.86 (5) |
K2—O7viii | 2.805 (2) | O9—H19 | 0.80 (5) |
K2—O8iii | 3.115 (3) | O9—H29 | 0.94 (5) |
K2—O8viii | 3.115 (3) | O10—H110 | 0.79 (5) |
K2—H18iii | 2.98 (4) | O10—H210 | 0.90 (5) |
K2—H18viii | 2.98 (4) | C1—C2 | 1.533 (3) |
Na—O1 | 2.376 (2) | C2—H2 | 1.00 (3) |
Na—O3v | 2.469 (2) | C2—C3 | 1.527 (3) |
Na—O5v | 2.502 (2) | C3—H3 | 0.97 (3) |
Na—O7 | 2.342 (2) | C3—C4 | 1.535 (3) |
| | | |
Naii—K1—Naiii | 80.26 (5) | H18viii—K2—Naiii | 165.5 (8) |
O1i—K1—Naiii | 145.26 (4) | H18viii—K2—O4v | 90.1 (8) |
O1—K1—Naiii | 101.43 (4) | H18viii—K2—O4iv | 65.5 (9) |
O1—K1—Naii | 145.26 (4) | H18iii—K2—O4v | 65.5 (9) |
O1i—K1—Naii | 101.43 (4) | H18iii—K2—O4iv | 90.1 (8) |
O1i—K1—O1 | 96.34 (10) | H18iii—K2—O5vii | 135.7 (9) |
O8ii—K1—Naiii | 110.32 (7) | H18viii—K2—O5vii | 59.4 (8) |
O8ii—K1—Naii | 32.90 (5) | H18iii—K2—O5vi | 59.4 (8) |
O8iii—K1—Naii | 110.32 (7) | H18viii—K2—O5vi | 135.7 (9) |
O8iii—K1—Naiii | 32.90 (5) | H18iii—K2—O7iii | 79.1 (8) |
O8ii—K1—O1i | 69.17 (5) | H18viii—K2—O7iii | 131.6 (8) |
O8iii—K1—O1i | 141.73 (7) | H18iii—K2—O7viii | 131.6 (8) |
O8iii—K1—O1 | 69.17 (5) | H18viii—K2—O7viii | 79.1 (8) |
O8ii—K1—O1 | 141.73 (7) | H18iii—K2—O8viii | 155.2 (8) |
O8ii—K1—O8iii | 142.44 (11) | H18iii—K2—O8iii | 16.0 (9) |
O9—K1—Naii | 92.87 (7) | H18viii—K2—O8iii | 155.2 (8) |
O9i—K1—Naii | 71.78 (6) | H18viii—K2—O8viii | 16.0 (9) |
O9—K1—Naiii | 71.78 (6) | H18viii—K2—H18iii | 145.1 (16) |
O9i—K1—Naiii | 92.87 (7) | K2ix—Na—K1x | 98.27 (3) |
O9—K1—O1i | 73.49 (7) | O1—Na—K1x | 88.32 (5) |
O9i—K1—O1 | 73.49 (7) | O1—Na—K2ix | 133.91 (6) |
O9—K1—O1 | 120.89 (7) | O3v—Na—K1x | 140.28 (6) |
O9i—K1—O1i | 120.89 (7) | O3v—Na—K2ix | 108.36 (6) |
O9i—K1—O8ii | 83.89 (7) | O3v—Na—O1 | 93.54 (7) |
O9—K1—O8iii | 83.89 (7) | O5v—Na—K1x | 92.81 (5) |
O9i—K1—O8iii | 89.76 (7) | O5v—Na—K2ix | 52.62 (4) |
O9—K1—O8ii | 89.76 (7) | O5v—Na—O1 | 173.12 (8) |
O9i—K1—O9 | 160.21 (14) | O5v—Na—O3v | 81.26 (7) |
O10ii—K1—Naiii | 61.48 (5) | O7—Na—K1x | 127.06 (7) |
O10ii—K1—Naii | 32.90 (4) | O7—Na—K2ix | 48.06 (6) |
O10iii—K1—Naiii | 32.90 (4) | O7—Na—O1 | 92.31 (8) |
O10iii—K1—Naii | 61.48 (5) | O7—Na—O3v | 92.54 (8) |
O10iii—K1—O1i | 118.07 (6) | O7—Na—O5v | 92.42 (7) |
O10ii—K1—O1 | 118.07 (6) | O8—Na—K1x | 45.91 (7) |
O10iii—K1—O1 | 132.72 (6) | O8—Na—K2ix | 55.61 (7) |
O10ii—K1—O1i | 132.72 (6) | O8—Na—O1 | 105.40 (8) |
O10iii—K1—O8iii | 63.72 (6) | O8—Na—O3v | 160.76 (9) |
O10ii—K1—O8ii | 63.72 (6) | O8—Na—O5v | 80.10 (8) |
O10iii—K1—O8ii | 83.58 (7) | O8—Na—O7 | 83.53 (9) |
O10ii—K1—O8iii | 83.58 (7) | O10—Na—K1x | 51.49 (9) |
O10iii—K1—O9 | 51.20 (8) | O10—Na—K2ix | 127.44 (8) |
O10iii—K1—O9i | 109.31 (10) | O10—Na—O1 | 91.92 (8) |
O10ii—K1—O9 | 109.31 (10) | O10—Na—O3v | 88.79 (10) |
O10ii—K1—O9i | 51.20 (8) | O10—Na—O5v | 83.51 (9) |
O10ii—K1—O10iii | 61.07 (10) | O10—Na—O7 | 175.48 (10) |
H210ii—K1—Naiii | 69.5 (9) | O10—Na—O8 | 93.80 (11) |
H210ii—K1—Naii | 42.7 (9) | C4v—Na—K1x | 140.28 (6) |
H210iii—K1—Naiii | 42.7 (9) | C4v—Na—K2ix | 87.64 (6) |
H210iii—K1—Naii | 69.5 (9) | C4v—Na—O1 | 115.40 (7) |
H210ii—K1—O1 | 104.9 (9) | C4v—Na—O3v | 22.78 (7) |
H210ii—K1—O1i | 133.7 (9) | C4v—Na—O5v | 60.05 (7) |
H210iii—K1—O1 | 133.7 (9) | C4v—Na—O7 | 85.43 (8) |
H210iii—K1—O1i | 104.9 (9) | C4v—Na—O8 | 138.04 (9) |
H210iii—K1—O8iii | 68.7 (9) | C4v—Na—O10 | 94.19 (10) |
H210ii—K1—O8ii | 68.7 (9) | Na—O1—K1 | 101.50 (7) |
H210iii—K1—O8ii | 84.6 (9) | C1—O1—K1 | 115.49 (16) |
H210ii—K1—O8iii | 84.6 (9) | C1—O1—Na | 126.04 (15) |
H210iii—K1—O9 | 36.1 (10) | C4—O3—Naxi | 107.51 (16) |
H210ii—K1—O9i | 36.1 (10) | C4—O4—K2xii | 121.17 (17) |
H210iii—K1—O9i | 124.3 (10) | Naxi—O5—K2xiii | 85.85 (6) |
H210ii—K1—O9 | 124.3 (10) | H5—O5—K2xiii | 97 (2) |
H210iii—K1—O10iii | 15.1 (10) | H5—O5—Naxi | 111 (2) |
H210ii—K1—O10iii | 75.0 (10) | C2—O5—K2xiii | 120.94 (14) |
H210ii—K1—O10ii | 15.1 (10) | C2—O5—Naxi | 130.50 (15) |
H210iii—K1—O10ii | 75.0 (10) | C2—O5—H5 | 106 (2) |
H210ii—K1—H210iii | 89.5 (19) | C3—O6—H6 | 112 (3) |
Naviii—K2—Naiii | 116.41 (4) | Na—O7—K2xiv | 93.54 (7) |
O4iv—K2—Naiii | 124.88 (4) | H17—O7—K2xiv | 108 (2) |
O4iv—K2—Naviii | 98.92 (4) | H17—O7—Na | 93 (2) |
O4v—K2—Naiii | 98.92 (4) | H27—O7—K2xiv | 118 (2) |
O4v—K2—Naviii | 124.88 (4) | H27—O7—Na | 131 (3) |
O4v—K2—O4iv | 92.77 (9) | H27—O7—H17 | 108 (3) |
O5vi—K2—Naviii | 112.78 (4) | K2xiv—O8—K1xiv | 154.26 (8) |
O5vii—K2—Naiii | 112.78 (4) | Na—O8—K1xiv | 101.19 (10) |
O5vi—K2—Naiii | 41.53 (4) | Na—O8—K2xiv | 85.58 (7) |
O5vii—K2—Naviii | 41.53 (4) | H18—O8—K1xiv | 82 (3) |
O5vii—K2—O4iv | 67.85 (5) | H18—O8—K2xiv | 73 (3) |
O5vi—K2—O4v | 67.85 (5) | H18—O8—Na | 121 (3) |
O5vii—K2—O4v | 148.23 (6) | H28—O8—K1xiv | 84 (3) |
O5vi—K2—O4iv | 148.23 (6) | H28—O8—K2xiv | 109 (3) |
O5vi—K2—O5vii | 139.89 (8) | H28—O8—Na | 133 (3) |
O7viii—K2—Naviii | 38.40 (4) | H28—O8—H18 | 107 (4) |
O7iii—K2—Naiii | 38.40 (4) | O8—H18—K2xiv | 91 (3) |
O7viii—K2—Naiii | 87.07 (5) | H19—O9—K1i | 129 (4) |
O7iii—K2—Naviii | 87.07 (5) | H29—O9—K1i | 143 (3) |
O7iii—K2—O4iv | 110.97 (6) | H29—O9—H19 | 86 (4) |
O7iii—K2—O4v | 137.32 (6) | Na—O10—K1x | 95.62 (10) |
O7viii—K2—O4iv | 137.32 (6) | H110—O10—K1x | 98 (3) |
O7viii—K2—O4v | 110.97 (6) | H110—O10—Na | 128 (3) |
O7iii—K2—O5vi | 74.07 (6) | H210—O10—K1x | 60 (3) |
O7viii—K2—O5vi | 74.39 (6) | H210—O10—Na | 121 (3) |
O7viii—K2—O5vii | 74.07 (6) | H210—O10—H110 | 109 (4) |
O7iii—K2—O5vii | 74.39 (6) | O10—H210—K1x | 105 (3) |
O7viii—K2—O7iii | 75.20 (9) | O2—C1—O1 | 126.6 (2) |
O8viii—K2—Naiii | 150.79 (5) | C2—C1—O1 | 116.7 (2) |
O8viii—K2—Naviii | 38.81 (4) | C2—C1—O2 | 116.6 (2) |
O8iii—K2—Naiii | 38.81 (4) | C1—C2—O5 | 110.79 (19) |
O8iii—K2—Naviii | 150.79 (5) | H2—C2—O5 | 106.9 (16) |
O8iii—K2—O4v | 81.32 (6) | H2—C2—C1 | 109.4 (16) |
O8viii—K2—O4iv | 81.32 (6) | C3—C2—O5 | 109.32 (19) |
O8iii—K2—O4iv | 91.63 (6) | C3—C2—C1 | 110.4 (2) |
O8viii—K2—O4v | 91.63 (6) | C3—C2—H2 | 110.0 (15) |
O8iii—K2—O5vii | 122.40 (6) | C2—C3—O6 | 110.6 (2) |
O8viii—K2—O5vi | 122.40 (6) | H3—C3—O6 | 105.9 (16) |
O8iii—K2—O5vi | 61.65 (6) | H3—C3—C2 | 112.0 (17) |
O8viii—K2—O5vii | 61.65 (6) | C4—C3—O6 | 111.4 (2) |
O8iii—K2—O7iii | 63.73 (6) | C4—C3—C2 | 110.21 (19) |
O8iii—K2—O7viii | 125.69 (6) | C4—C3—H3 | 106.6 (16) |
O8viii—K2—O7iii | 125.69 (6) | O3—C4—Naxi | 49.71 (13) |
O8viii—K2—O7viii | 63.73 (6) | O4—C4—Naxi | 122.25 (18) |
O8viii—K2—O8iii | 169.81 (8) | O4—C4—O3 | 126.0 (2) |
H18iii—K2—Naviii | 165.5 (8) | C3—C4—Naxi | 96.47 (15) |
H18viii—K2—Naviii | 49.3 (8) | C3—C4—O3 | 116.6 (2) |
H18iii—K2—Naiii | 49.3 (8) | C3—C4—O4 | 117.4 (2) |
| | | |
K1—O1—C1—O2 | −51.75 (17) | Naxi—O3—C4—C3 | 74.94 (15) |
K1i—O1—C1—O2 | −51.75 (17) | Naxi—O5—C2—C1 | −133.41 (19) |
K1—O1—C1—C2 | 128.74 (15) | Naxi—O5—C2—C3 | −11.50 (18) |
K1i—O1—C1—C2 | 128.74 (15) | Naxi—C4—C3—O6 | 62.84 (15) |
K2xii—O4—C4—Naxi | −73.51 (16) | Naxi—C4—C3—C2 | −60.29 (15) |
K2—O4v—C4v—Na | −73.51 (16) | O1—C1—C2—O5 | −177.0 (2) |
K2xii—O4—C4—O3 | −12.6 (2) | O1—C1—C2—C3 | 61.7 (2) |
K2xi—O4—C4—O3 | −12.6 (2) | O2—C1—C2—O5 | 3.4 (2) |
K2xii—O4—C4—C3 | 168.01 (16) | O2—C1—C2—C3 | −117.8 (2) |
K2xi—O4—C4—C3 | 168.01 (16) | O3—C4—C3—O6 | 15.0 (2) |
K2xv—O5—C2—C1 | 112.95 (16) | O3—C4—C3—C2 | −108.1 (2) |
K2xiii—O5—C2—C1 | 112.95 (16) | O4—C4—C3—O6 | −165.6 (2) |
K2xiii—O5—C2—C3 | −125.15 (16) | O4—C4—C3—C2 | 71.3 (2) |
K2xv—O5—C2—C3 | −125.15 (16) | O5—C2—C3—O6 | −68.1 (2) |
Na—O1—C1—O2 | 76.6 (2) | O5—C2—C3—C4 | 55.5 (2) |
Na—O1—C1—C2 | −102.95 (18) | O6—C3—C2—C1 | 54.0 (2) |
Naxi—O3—C4—O4 | −104.42 (17) | C1—C2—C3—C4 | 177.6 (2) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (vii) x+1/2, −y+1/2, −z; (viii) −x+1, −y, z−1; (ix) −x+1, −y, z+1; (x) −x, −y, z+1; (xi) −x+1/2, y+1/2, −z+1; (xii) x−1/2, −y+1/2, −z+1; (xiii) x−1/2, −y+1/2, −z; (xiv) x, y, z+1; (xv) −x+1/2, y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O2 | 0.83 (4) | 2.06 (3) | 2.605 (3) | 122 (3) |
O5—H5···O3iii | 0.83 (4) | 2.67 (4) | 3.367 (3) | 142 (3) |
O5—H5···O4iii | 0.83 (4) | 2.79 (4) | 3.265 (3) | 118 (3) |
O6—H6···O10xi | 0.74 (3) | 2.27 (3) | 2.947 (4) | 153 (4) |
O7—H17···O6 | 0.87 (4) | 1.93 (4) | 2.796 (3) | 178 (3) |
O7—H27···O4iv | 0.82 (4) | 2.08 (4) | 2.891 (3) | 168 (3) |
O8—H18···O3xvi | 0.86 (5) | 1.86 (5) | 2.704 (3) | 167 (4) |
O8—H28···O1xiv | 0.86 (5) | 2.87 (4) | 3.395 (3) | 121 (3) |
O8—H28···O2xiv | 0.86 (5) | 1.91 (5) | 2.757 (3) | 172 (4) |
O9—H19···O2vi | 0.80 (5) | 2.45 (5) | 3.110 (3) | 140 (5) |
O9—H19···O3v | 0.80 (5) | 2.86 (5) | 3.177 (3) | 106 (4) |
O9—H19···O6v | 0.80 (5) | 2.53 (5) | 3.148 (3) | 135 (4) |
O9—H29···O4ii | 0.94 (5) | 1.89 (5) | 2.818 (4) | 169 (4) |
O10—H110···O1i | 0.79 (5) | 1.95 (5) | 2.738 (3) | 171 (5) |
O10—H210···O9xiv | 0.90 (5) | 1.86 (5) | 2.759 (4) | 175 (4) |
Symmetry codes: (i) −x, −y, z; (ii) −x, −y, z−1; (iii) x, y, z−1; (iv) x+1/2, −y+1/2, −z+1; (v) −x+1/2, y−1/2, −z+1; (vi) −x+1/2, y−1/2, −z; (xi) −x+1/2, y+1/2, −z+1; (xiv) x, y, z+1; (xvi) −x+1/2, y−1/2, −z+2. |