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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

cif

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

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105100K_harsup2.hkl
Contains datablock 100K_har

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105125K_harsup3.hkl
Contains datablock 125K_har

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105150K_harsup4.hkl
Contains datablock 150K_har

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105175K_anhsup5.hkl
Contains datablock 175K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105200K_anhsup6.hkl
Contains datablock 200K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105225K_anhsup7.hkl
Contains datablock 225K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105243K_anhsup8.hkl
Contains datablock 243K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105253K_anhsup9.hkl
Contains datablock 253K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105256K_anhsup10.hkl
Contains datablock 256K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105266K_anhsup11.hkl
Contains datablock 266K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105276K_anhsup12.hkl
Contains datablock 276K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105296K_anhsup14.hkl
Contains datablock 296K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105298K_anhsup15.hkl
Contains datablock 298K_anh

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205252062400115X/xk5105308K_anhsup16.hkl
Contains datablock 308K_anh

pdf

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

Computing details top

Sodium potassium L(+)-tartrate tetrahydrate (100K_har) top
Crystal data top
C4H12KNaO10Dx = 1.817 Mg m3
Mr = 282.23Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 8586 reflections
a = 11.7658 (6) Åθ = 3.6–29.3°
b = 14.1879 (8) ŵ = 0.60 mm1
c = 6.1811 (3) ÅT = 100 K
V = 1031.83 (9) Å3Prism, clear colourless
Z = 40.48 × 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 Source2399 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.762, Tmax = 1.000l = 88
18029 measured reflections
Refinement top
Refinement on F2Hydrogen site location: difference Fourier map
Least-squares matrix: fullOnly 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 = 1.11Δρmax = 0.40 e Å3
2647 reflectionsΔρmin = 0.28 e Å3
182 parametersAbsolute structure: Flack x determined using 911 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
1 restraintAbsolute 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
xyzUiso*/Ueq
K10.0000000.0000000.04233 (12)0.02088 (17)
K20.5000000.0000000.16108 (11)0.01464 (16)
Na0.23246 (7)0.00700 (7)0.51491 (14)0.01230 (19)
O10.12017 (13)0.10863 (11)0.3478 (3)0.0123 (3)
O20.21258 (14)0.20354 (12)0.1178 (3)0.0142 (4)
O30.22782 (15)0.40732 (12)0.8205 (3)0.0162 (4)
O40.04753 (14)0.35882 (12)0.8495 (3)0.0155 (4)
O50.16538 (15)0.35811 (12)0.3248 (3)0.0126 (4)
H50.193 (3)0.342 (2)0.221 (5)0.019*
O60.29621 (14)0.24864 (12)0.6343 (3)0.0130 (4)
H60.326 (3)0.291 (2)0.595 (5)0.019*
O70.39590 (15)0.08339 (13)0.4854 (3)0.0156 (4)
H170.367 (3)0.132 (2)0.525 (5)0.023*
H270.434 (3)0.092 (2)0.384 (5)0.023*
O80.23648 (18)0.04169 (14)0.8784 (3)0.0213 (4)
H180.256 (3)0.001 (3)0.972 (5)0.032*
H280.232 (3)0.092 (3)0.943 (6)0.032*
O90.05881 (16)0.19148 (14)0.0303 (3)0.0198 (4)
H190.117 (3)0.204 (2)0.032 (6)0.030*
H290.031 (3)0.250 (2)0.059 (5)0.030*
O100.07869 (15)0.10785 (14)0.5700 (3)0.0184 (4)
H1100.017 (3)0.106 (2)0.513 (5)0.028*
H2100.072 (3)0.138 (2)0.687 (6)0.028*
C10.15518 (19)0.18782 (17)0.2828 (4)0.0104 (5)
C20.12508 (19)0.27352 (17)0.4230 (4)0.0105 (4)
H20.039 (2)0.2777 (19)0.433 (4)0.013*
C30.17721 (19)0.26336 (16)0.6481 (4)0.0109 (4)
H30.146 (2)0.209 (2)0.726 (5)0.013*
C40.1487 (2)0.35058 (17)0.7853 (4)0.0125 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0258 (4)0.0186 (4)0.0182 (4)0.0084 (4)0.0000.000
K20.0155 (3)0.0163 (3)0.0121 (3)0.0024 (3)0.0000.000
Na0.0118 (4)0.0126 (5)0.0124 (4)0.0004 (4)0.0001 (3)0.0001 (4)
O10.0133 (8)0.0109 (8)0.0127 (8)0.0001 (6)0.0013 (7)0.0006 (7)
O20.0167 (8)0.0141 (8)0.0117 (9)0.0001 (7)0.0020 (7)0.0009 (6)
O30.0215 (9)0.0137 (8)0.0133 (8)0.0043 (7)0.0008 (7)0.0021 (7)
O40.0161 (8)0.0186 (9)0.0119 (8)0.0047 (7)0.0001 (7)0.0013 (7)
O50.0178 (9)0.0114 (8)0.0087 (8)0.0006 (7)0.0011 (7)0.0001 (7)
O60.0113 (8)0.0120 (9)0.0156 (9)0.0002 (6)0.0009 (7)0.0008 (7)
O70.0148 (9)0.0147 (9)0.0173 (9)0.0006 (7)0.0038 (7)0.0008 (7)
O80.0402 (12)0.0129 (9)0.0109 (9)0.0046 (8)0.0001 (9)0.0004 (7)
O90.0148 (9)0.0261 (10)0.0185 (10)0.0001 (8)0.0035 (8)0.0003 (8)
O100.0116 (8)0.0212 (10)0.0223 (10)0.0032 (7)0.0030 (8)0.0054 (8)
C10.0091 (11)0.0121 (11)0.0099 (11)0.0016 (9)0.0034 (9)0.0000 (9)
C20.0115 (11)0.0094 (11)0.0105 (11)0.0003 (9)0.0006 (9)0.0005 (9)
C30.0110 (10)0.0110 (11)0.0107 (11)0.0012 (9)0.0004 (9)0.0013 (10)
C40.0183 (12)0.0119 (12)0.0073 (11)0.0024 (9)0.0015 (9)0.0012 (9)
Geometric parameters (Å, º) top
K1—O1i2.8178 (17)Na—C4iv3.080 (3)
K1—O12.8178 (17)O1—C11.262 (3)
K1—O8ii3.020 (2)O2—C11.244 (3)
K1—O8iii3.020 (2)O3—C41.250 (3)
K1—O9i2.839 (2)O4—C41.260 (3)
K1—O92.839 (2)O5—H50.75 (3)
K1—O10iii3.424 (2)O5—C21.426 (3)
K1—O10ii3.424 (2)O6—H60.74 (3)
K2—O4iv2.8344 (18)O6—C31.418 (3)
K2—O4v2.8344 (18)O7—H170.80 (4)
K2—O5vi2.9771 (17)O7—H270.78 (3)
K2—O5vii2.9771 (17)O8—H180.85 (4)
K2—O7iii2.7703 (19)O8—H280.82 (4)
K2—O7viii2.7703 (19)O9—H190.80 (4)
K2—O8iii3.166 (2)O9—H290.91 (3)
K2—O8viii3.166 (2)O10—H1100.80 (3)
Na—O12.3459 (18)O10—H2100.84 (4)
Na—O3iv2.4484 (19)C1—C21.535 (3)
Na—O5iv2.468 (2)C2—H21.02 (3)
Na—O72.319 (2)C2—C31.527 (3)
Na—H172.53 (3)C3—H30.98 (3)
Na—O82.351 (2)C3—C41.537 (3)
Na—O102.332 (2)
Naii—K1—Naiii80.03 (3)O1—Na—H1779.6 (7)
O1i—K1—Naii101.75 (4)O1—Na—O8103.09 (7)
O1—K1—Naiii101.75 (4)O1—Na—C4iv116.70 (7)
O1—K1—Naii145.38 (4)O3iv—Na—K1ix141.51 (5)
O1i—K1—Naiii145.38 (4)O3iv—Na—K2ix107.86 (5)
O1—K1—O1i95.84 (7)O3iv—Na—O5iv82.07 (6)
O1—K1—O8iii69.85 (5)O3iv—Na—H17106.8 (8)
O1—K1—O8ii142.60 (5)O3iv—Na—C4iv22.66 (6)
O1i—K1—O8ii69.85 (5)O5iv—Na—K1ix91.35 (5)
O1i—K1—O8iii142.60 (5)O5iv—Na—K2ix52.72 (4)
O1—K1—O9120.47 (5)O5iv—Na—H17106.8 (7)
O1i—K1—O9i120.47 (5)O5iv—Na—C4iv60.78 (6)
O1—K1—O9i72.83 (5)O7—Na—K1ix125.47 (6)
O1i—K1—O972.84 (5)O7—Na—K2ix47.78 (5)
O1i—K1—O10iii117.56 (5)O7—Na—O192.62 (7)
O1—K1—O10iii132.86 (4)O7—Na—O3iv92.85 (7)
O1i—K1—O10ii132.86 (4)O7—Na—O5iv93.24 (7)
O1—K1—O10ii117.56 (5)O7—Na—H1718.4 (8)
O8ii—K1—Naii32.38 (4)O7—Na—O884.02 (7)
O8iii—K1—Naiii32.38 (4)O7—Na—O10173.97 (8)
O8ii—K1—Naiii109.29 (4)O7—Na—C4iv86.50 (7)
O8iii—K1—Naii109.29 (4)O8—Na—K1ix43.46 (5)
O8ii—K1—O8iii140.78 (8)O8—Na—K2ix57.48 (5)
O8ii—K1—O10iii82.84 (5)O8—Na—O3iv162.04 (8)
O8iii—K1—O10iii63.39 (5)O8—Na—O5iv80.46 (7)
O8iii—K1—O10ii82.84 (5)O8—Na—H1774.6 (8)
O8ii—K1—O10ii63.39 (5)O8—Na—C4iv139.43 (8)
O9i—K1—Naii72.54 (4)O10—Na—K1ix53.41 (5)
O9—K1—Naiii72.54 (4)O10—Na—K2ix126.33 (6)
O9—K1—Naii93.32 (4)O10—Na—O193.23 (7)
O9i—K1—Naiii93.32 (4)O10—Na—O3iv88.11 (7)
O9i—K1—O8ii84.82 (5)O10—Na—O5iv80.99 (7)
O9i—K1—O8iii89.09 (6)O10—Na—H17163.9 (8)
O9—K1—O8ii89.09 (6)O10—Na—O893.23 (8)
O9—K1—O8iii84.82 (5)O10—Na—C4iv92.16 (7)
O9—K1—O9i161.81 (9)C4iv—Na—K1ix140.24 (5)
O9—K1—O10ii111.02 (6)C4iv—Na—K2ix87.58 (5)
O9i—K1—O10ii51.07 (5)C4iv—Na—H17104.0 (8)
O9—K1—O10iii51.07 (5)Na—O1—K1101.25 (6)
O9i—K1—O10iii111.02 (6)C1—O1—K1115.93 (15)
O10iii—K1—Naiii33.15 (3)C1—O1—Na125.36 (14)
O10ii—K1—Naii33.15 (3)C4—O3—Nax108.34 (15)
O10iii—K1—Naii62.04 (4)C4—O4—K2x117.77 (15)
O10ii—K1—Naiii62.04 (4)K2xi—O5—H5101 (2)
O10iii—K1—O10ii62.98 (7)Nax—O5—K2xi86.01 (5)
Naiii—K2—Naviii115.09 (3)Nax—O5—H5112 (2)
O4v—K2—Naiii123.35 (4)C2—O5—K2xi119.77 (13)
O4iv—K2—Naiii100.33 (4)C2—O5—Nax130.05 (14)
O4v—K2—Naviii100.33 (4)C2—O5—H5104 (2)
O4iv—K2—Naviii123.35 (4)C3—O6—H6112 (2)
O4v—K2—O4iv94.40 (7)K2ix—O7—H17108 (2)
O4iv—K2—O5vi146.91 (5)K2ix—O7—H27116 (2)
O4v—K2—O5vi67.92 (5)Na—O7—K2ix93.93 (6)
O4iv—K2—O5vii67.92 (5)Na—O7—H1796 (2)
O4v—K2—O5vii146.91 (5)Na—O7—H27129 (2)
O4iv—K2—O8viii90.51 (5)H17—O7—H27111 (3)
O4v—K2—O8viii83.48 (5)K1ix—O8—K2ix153.08 (7)
O4iv—K2—O8iii83.48 (5)K1ix—O8—H1883 (2)
O4v—K2—O8iii90.51 (5)K1ix—O8—H2887 (2)
O5vi—K2—Naviii41.27 (4)K2ix—O8—H1870 (2)
O5vii—K2—Naviii112.76 (4)K2ix—O8—H28105 (2)
O5vi—K2—Naiii112.76 (4)Na—O8—K1ix104.16 (7)
O5vii—K2—Naiii41.27 (4)Na—O8—K2ix83.76 (6)
O5vii—K2—O5vi140.27 (7)Na—O8—H18117 (2)
O5vii—K2—O8viii122.68 (5)Na—O8—H28136 (2)
O5vii—K2—O8iii60.81 (5)H18—O8—H28106 (3)
O5vi—K2—O8viii60.81 (5)K1—O9—H19110 (2)
O5vi—K2—O8iii122.68 (5)K1—O9—H29144 (2)
O7iii—K2—Naiii38.30 (4)H19—O9—H29102 (3)
O7viii—K2—Naiii86.46 (4)K1ix—O10—H11097 (2)
O7iii—K2—Naviii86.46 (4)K1ix—O10—H21058 (2)
O7viii—K2—Naviii38.30 (4)Na—O10—K1ix93.45 (6)
O7iii—K2—O4iv138.63 (5)Na—O10—H110128 (2)
O7viii—K2—O4iv108.74 (5)Na—O10—H210121 (2)
O7viii—K2—O4v138.63 (5)H110—O10—H210108 (3)
O7iii—K2—O4v108.74 (5)O1—C1—C2116.8 (2)
O7viii—K2—O5vii74.46 (5)O2—C1—O1126.7 (2)
O7iii—K2—O5vii74.44 (5)O2—C1—C2116.5 (2)
O7iii—K2—O5vi74.46 (5)O5—C2—C1110.46 (18)
O7viii—K2—O5vi74.44 (5)O5—C2—H2108.0 (15)
O7viii—K2—O7iii75.87 (8)O5—C2—C3109.51 (18)
O7viii—K2—O8iii125.00 (5)C1—C2—H2108.2 (15)
O7viii—K2—O8viii63.12 (5)C3—C2—C1110.30 (19)
O7iii—K2—O8iii63.12 (5)C3—C2—H2110.4 (15)
O7iii—K2—O8viii125.00 (5)O6—C3—C2110.82 (19)
O8viii—K2—Naviii38.76 (4)O6—C3—H3106.7 (16)
O8iii—K2—Naiii38.76 (4)O6—C3—C4111.56 (19)
O8viii—K2—Naiii149.58 (4)C2—C3—H3111.6 (16)
O8iii—K2—Naviii149.58 (4)C2—C3—C4109.81 (18)
O8viii—K2—O8iii171.17 (7)C4—C3—H3106.3 (16)
K1ix—Na—H17111.4 (8)O3—C4—Nax49.00 (12)
K2ix—Na—K1ix97.49 (2)O3—C4—O4126.1 (2)
K2ix—Na—H1755.7 (7)O3—C4—C3116.8 (2)
O1—Na—K1ix87.65 (5)O4—C4—Nax123.91 (16)
O1—Na—K2ix133.84 (5)O4—C4—C3117.1 (2)
O1—Na—O3iv94.70 (6)C3—C4—Nax95.54 (14)
O1—Na—O5iv173.44 (7)
K1—O1—C1—O252.3 (3)O1—C1—C2—C361.5 (3)
K1—O1—C1—C2128.43 (17)O2—C1—C2—O53.4 (3)
K2x—O4—C4—Nax72.19 (19)O2—C1—C2—C3117.8 (2)
K2x—O4—C4—O311.4 (3)O5—C2—C3—O666.7 (2)
K2x—O4—C4—C3169.52 (14)O5—C2—C3—C457.0 (2)
K2xi—O5—C2—C1113.26 (17)O6—C3—C4—Nax62.77 (18)
K2xi—O5—C2—C3125.07 (15)O6—C3—C4—O316.4 (3)
Na—O1—C1—O275.3 (3)O6—C3—C4—O4164.5 (2)
Na—O1—C1—C2103.9 (2)C1—C2—C3—O655.1 (2)
Nax—O3—C4—O4106.3 (2)C1—C2—C3—C4178.77 (19)
Nax—O3—C4—C372.7 (2)C2—C3—C4—Nax60.49 (17)
Nax—O5—C2—C1134.65 (16)C2—C3—C4—O3106.9 (2)
Nax—O5—C2—C313.0 (3)C2—C3—C4—O472.3 (3)
O1—C1—C2—O5177.26 (19)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y1/2, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y+1/2, z; (vii) x+1/2, y1/2, z; (viii) x+1, y, z1; (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···AD—HH···AD···AD—H···A
O5—H5···O20.75 (3)2.08 (3)2.599 (2)127 (3)
O5—H5···O3iii0.75 (3)2.68 (3)3.277 (2)138 (3)
O5—H5···O4iii0.75 (3)2.87 (3)3.248 (2)114 (3)
O6—H6···O10x0.74 (3)2.08 (3)2.812 (3)168 (3)
O7—H17···O60.80 (4)1.97 (4)2.778 (2)178 (3)
O7—H27···O4v0.78 (3)2.08 (3)2.853 (3)168 (3)
O8—H18···O3xii0.85 (4)1.86 (4)2.697 (3)171 (3)
O8—H28···O1ix0.82 (4)2.84 (3)3.346 (2)122 (3)
O8—H28···O2ix0.82 (4)1.93 (4)2.746 (3)174 (3)
O9—H19···O2vii0.80 (4)2.57 (3)3.122 (3)127 (3)
O9—H19···O3iv0.80 (4)2.58 (4)3.154 (3)130 (3)
O9—H19···O6iv0.80 (4)2.40 (4)3.102 (3)147 (3)
O9—H29···O4ii0.91 (3)1.89 (4)2.785 (3)170 (3)
O10—H110···O1i0.80 (3)1.91 (3)2.713 (2)173 (3)
O10—H210···O9ix0.84 (4)1.91 (4)2.751 (3)172 (3)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y1/2, z+1; (v) x+1/2, y+1/2, z+1; (vii) x+1/2, y1/2, z; (ix) x, y, z+1; (x) x+1/2, y+1/2, z+1; (xii) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (125K_har) top
Crystal data top
C4H12KNaO10Dx = 1.813 Mg m3
Mr = 282.23Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 8346 reflections
a = 11.7769 (6) Åθ = 3.6–29.2°
b = 14.1930 (8) ŵ = 0.60 mm1
c = 6.1849 (3) ÅT = 125 K
V = 1033.80 (10) Å3Prism, clear colourless
Z = 40.48 × 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 Source2389 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.766, Tmax = 1.000l = 88
18069 measured reflections
Refinement top
Refinement on F2Hydrogen site location: difference Fourier map
Least-squares matrix: fullOnly 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 = 1.08Δρmax = 0.34 e Å3
2653 reflectionsΔρmin = 0.25 e Å3
182 parametersAbsolute structure: Flack x determined using 892 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
1 restraintAbsolute 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
xyzUiso*/Ueq
K10.0000000.0000000.04286 (13)0.02478 (19)
K20.5000000.0000000.16099 (12)0.01693 (16)
Na0.23242 (8)0.00693 (7)0.51540 (14)0.0141 (2)
O10.12012 (14)0.10870 (12)0.3477 (3)0.0137 (3)
O20.21246 (15)0.20348 (12)0.1181 (3)0.0158 (4)
O30.22817 (16)0.40726 (12)0.8200 (3)0.0190 (4)
O40.04783 (15)0.35905 (13)0.8489 (3)0.0178 (4)
O50.16518 (15)0.35796 (12)0.3247 (3)0.0143 (4)
H50.194 (3)0.340 (2)0.221 (6)0.021*
O60.29620 (15)0.24856 (12)0.6340 (3)0.0146 (4)
H60.326 (3)0.292 (2)0.593 (5)0.022*
O70.39597 (16)0.08324 (13)0.4858 (3)0.0176 (4)
H170.369 (3)0.132 (3)0.523 (6)0.026*
H270.433 (3)0.094 (2)0.381 (6)0.026*
O80.23692 (19)0.04161 (15)0.8791 (3)0.0246 (5)
H180.255 (3)0.002 (3)0.974 (6)0.037*
H280.234 (3)0.092 (3)0.944 (6)0.037*
O90.05879 (17)0.19184 (15)0.0310 (3)0.0228 (4)
H190.116 (3)0.204 (3)0.030 (6)0.034*
H290.030 (3)0.251 (3)0.059 (5)0.034*
O100.07852 (16)0.10751 (14)0.5703 (4)0.0215 (4)
H1100.016 (3)0.107 (2)0.508 (5)0.032*
H2100.073 (3)0.134 (3)0.690 (6)0.032*
C10.1551 (2)0.18777 (17)0.2829 (4)0.0114 (5)
C20.1253 (2)0.27355 (17)0.4229 (4)0.0117 (5)
H20.042 (2)0.278 (2)0.437 (4)0.014*
C30.17718 (19)0.26350 (17)0.6480 (4)0.0125 (5)
H30.146 (2)0.210 (2)0.726 (5)0.015*
C40.1488 (2)0.35069 (18)0.7850 (4)0.0139 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0305 (4)0.0225 (4)0.0213 (4)0.0105 (4)0.0000.000
K20.0175 (3)0.0190 (4)0.0143 (3)0.0024 (3)0.0000.000
Na0.0140 (4)0.0138 (5)0.0144 (4)0.0003 (4)0.0000 (3)0.0002 (4)
O10.0145 (8)0.0118 (8)0.0149 (8)0.0005 (6)0.0013 (7)0.0005 (7)
O20.0186 (8)0.0157 (9)0.0130 (9)0.0003 (7)0.0023 (7)0.0015 (7)
O30.0256 (9)0.0164 (9)0.0148 (9)0.0043 (8)0.0007 (8)0.0026 (7)
O40.0177 (8)0.0215 (9)0.0141 (8)0.0050 (7)0.0006 (7)0.0019 (8)
O50.0199 (9)0.0117 (8)0.0113 (8)0.0005 (7)0.0006 (7)0.0007 (7)
O60.0125 (8)0.0133 (9)0.0179 (9)0.0014 (7)0.0012 (7)0.0002 (7)
O70.0166 (9)0.0160 (9)0.0202 (10)0.0000 (7)0.0037 (8)0.0006 (8)
O80.0467 (13)0.0152 (9)0.0119 (9)0.0055 (9)0.0008 (9)0.0000 (7)
O90.0162 (9)0.0308 (11)0.0215 (10)0.0004 (8)0.0044 (8)0.0008 (9)
O100.0150 (9)0.0239 (10)0.0255 (10)0.0033 (8)0.0039 (8)0.0060 (8)
C10.0090 (11)0.0140 (12)0.0113 (11)0.0015 (9)0.0034 (9)0.0007 (9)
C20.0117 (11)0.0118 (11)0.0116 (11)0.0005 (9)0.0005 (9)0.0000 (9)
C30.0129 (11)0.0121 (11)0.0126 (11)0.0008 (9)0.0012 (10)0.0010 (10)
C40.0201 (13)0.0123 (12)0.0093 (11)0.0023 (9)0.0030 (10)0.0015 (9)
Geometric parameters (Å, º) top
K1—O12.8172 (17)Na—C4iv3.081 (3)
K1—O1i2.8172 (17)O1—C11.261 (3)
K1—O8ii3.026 (2)O2—C11.243 (3)
K1—O8iii3.026 (2)O3—C41.251 (3)
K1—O9i2.846 (2)O4—C41.259 (3)
K1—O92.846 (2)O5—H50.77 (3)
K1—O10ii3.424 (2)O5—C21.423 (3)
K1—O10iii3.424 (2)O6—H60.75 (3)
K2—O4iv2.8362 (18)O6—C31.420 (3)
K2—O4v2.8362 (18)O7—H170.79 (4)
K2—O5vi2.9789 (18)O7—H270.80 (3)
K2—O5vii2.9789 (18)O8—H180.84 (4)
K2—O7iii2.769 (2)O8—H280.82 (4)
K2—O7viii2.769 (2)O9—H190.79 (4)
K2—O8iii3.164 (2)O9—H290.92 (4)
K2—O8viii3.164 (2)O10—H1100.83 (4)
Na—O12.3491 (19)O10—H2100.83 (4)
Na—O3iv2.450 (2)C1—C21.535 (3)
Na—O5iv2.472 (2)C2—H20.99 (3)
Na—O72.320 (2)C2—C31.527 (3)
Na—H172.54 (3)C3—H30.97 (3)
Na—O82.353 (2)C3—C41.537 (3)
Na—O102.332 (2)
Naii—K1—Naiii80.03 (3)O1—Na—H1780.0 (8)
O1i—K1—Naii101.69 (4)O1—Na—O8103.31 (8)
O1—K1—Naiii101.69 (4)O1—Na—C4iv116.59 (7)
O1—K1—Naii145.35 (4)O3iv—Na—K1ix141.42 (6)
O1i—K1—Naiii145.35 (4)O3iv—Na—K2ix107.88 (5)
O1—K1—O1i95.98 (7)O3iv—Na—O5iv81.99 (7)
O1i—K1—O8iii142.54 (5)O3iv—Na—H17106.3 (8)
O1i—K1—O8ii69.77 (5)O3iv—Na—C4iv22.67 (6)
O1—K1—O8iii69.77 (5)O5iv—Na—K1ix91.44 (5)
O1—K1—O8ii142.54 (5)O5iv—Na—K2ix52.72 (4)
O1—K1—O9120.61 (6)O5iv—Na—H17106.4 (8)
O1i—K1—O9i120.61 (6)O5iv—Na—C4iv60.72 (6)
O1—K1—O9i72.88 (5)O7—Na—K1ix125.54 (6)
O1i—K1—O972.88 (5)O7—Na—K2ix47.72 (5)
O1i—K1—O10iii117.57 (5)O7—Na—O192.70 (7)
O1i—K1—O10ii132.82 (5)O7—Na—O3iv92.87 (7)
O1—K1—O10iii132.82 (5)O7—Na—O5iv93.13 (7)
O1—K1—O10ii117.57 (5)O7—Na—H1717.9 (8)
O8ii—K1—Naii32.41 (4)O7—Na—O883.99 (8)
O8iii—K1—Naii109.37 (5)O7—Na—O10174.01 (9)
O8ii—K1—Naiii109.37 (5)O7—Na—C4iv86.41 (7)
O8iii—K1—Naiii32.41 (4)O8—Na—K1ix43.58 (6)
O8ii—K1—O8iii140.90 (8)O8—Na—K2ix57.38 (6)
O8iii—K1—O10ii82.90 (5)O8—Na—O3iv161.93 (8)
O8ii—K1—O10ii63.41 (5)O8—Na—O5iv80.43 (7)
O8ii—K1—O10iii82.90 (5)O8—Na—H1775.0 (8)
O8iii—K1—O10iii63.41 (5)O8—Na—C4iv139.31 (8)
O9i—K1—Naii72.46 (4)O10—Na—K1ix53.36 (6)
O9—K1—Naii93.18 (5)O10—Na—K2ix126.44 (6)
O9—K1—Naiii72.46 (4)O10—Na—O193.12 (7)
O9i—K1—Naiii93.18 (5)O10—Na—O3iv88.07 (8)
O9i—K1—O8ii84.76 (6)O10—Na—O5iv81.14 (7)
O9—K1—O8iii84.76 (6)O10—Na—H17164.4 (8)
O9—K1—O8ii89.08 (6)O10—Na—O893.29 (8)
O9i—K1—O8iii89.08 (6)O10—Na—C4iv92.24 (8)
O9—K1—O9i161.53 (9)C4iv—Na—K1ix140.24 (6)
O9—K1—O10iii51.03 (5)C4iv—Na—K2ix87.56 (5)
O9i—K1—O10iii110.79 (6)C4iv—Na—H17103.3 (8)
O9—K1—O10ii110.79 (6)Na—O1—K1101.28 (6)
O9i—K1—O10ii51.03 (5)C1—O1—K1116.02 (15)
O10iii—K1—Naiii33.12 (4)C1—O1—Na125.32 (15)
O10ii—K1—Naii33.12 (4)C4—O3—Nax108.31 (15)
O10iii—K1—Naii61.98 (4)C4—O4—K2x117.90 (16)
O10ii—K1—Naiii61.98 (4)K2xi—O5—H5103 (2)
O10iii—K1—O10ii62.81 (7)Nax—O5—K2xi85.96 (6)
Naiii—K2—Naviii115.18 (3)Nax—O5—H5112 (2)
O4v—K2—Naviii100.29 (4)C2—O5—K2xi119.95 (13)
O4iv—K2—Naviii123.43 (4)C2—O5—Nax130.05 (15)
O4v—K2—Naiii123.43 (4)C2—O5—H5103 (2)
O4iv—K2—Naiii100.29 (4)C3—O6—H6111 (2)
O4v—K2—O4iv94.24 (8)K2ix—O7—H17108 (2)
O4iv—K2—O5vi67.93 (5)K2ix—O7—H27118 (2)
O4iv—K2—O5vii146.96 (5)Na—O7—K2ix93.99 (7)
O4v—K2—O5vi146.97 (5)Na—O7—H1797 (2)
O4v—K2—O5vii67.93 (5)Na—O7—H27129 (2)
O4iv—K2—O8viii90.54 (5)H17—O7—H27107 (3)
O4v—K2—O8viii83.33 (5)K1ix—O8—K2ix153.21 (8)
O4iv—K2—O8iii83.33 (5)K1ix—O8—H1883 (2)
O4v—K2—O8iii90.54 (5)K1ix—O8—H2888 (3)
O5vii—K2—Naviii41.32 (4)K2ix—O8—H1871 (2)
O5vii—K2—Naiii112.75 (4)K2ix—O8—H28104 (3)
O5vi—K2—Naviii112.75 (4)Na—O8—K1ix104.01 (8)
O5vi—K2—Naiii41.32 (4)Na—O8—K2ix83.83 (6)
O5vi—K2—O5vii140.26 (8)Na—O8—H18119 (3)
O5vii—K2—O8viii60.89 (5)Na—O8—H28136 (3)
O5vi—K2—O8viii122.67 (5)H18—O8—H28104 (4)
O5vii—K2—O8iii122.67 (5)K1—O9—H19110 (3)
O5vi—K2—O8iii60.89 (5)K1—O9—H29144 (2)
O7iii—K2—Naiii38.29 (4)H19—O9—H29102 (3)
O7viii—K2—Naiii86.52 (5)K1ix—O10—H11098 (2)
O7iii—K2—Naviii86.52 (5)K1ix—O10—H21055 (2)
O7viii—K2—Naviii38.29 (4)Na—O10—K1ix93.52 (7)
O7iii—K2—O4iv138.58 (5)Na—O10—H110128 (2)
O7viii—K2—O4iv108.89 (6)Na—O10—H210118 (2)
O7viii—K2—O4v138.58 (5)H110—O10—H210110 (3)
O7iii—K2—O4v108.89 (6)O1—C1—C2116.8 (2)
O7viii—K2—O5vi74.46 (5)O2—C1—O1126.7 (2)
O7iii—K2—O5vii74.46 (5)O2—C1—C2116.4 (2)
O7iii—K2—O5vi74.44 (5)O5—C2—C1110.56 (19)
O7viii—K2—O5vii74.44 (5)O5—C2—H2108.5 (16)
O7viii—K2—O7iii75.84 (9)O5—C2—C3109.61 (19)
O7iii—K2—O8viii125.08 (6)C1—C2—H2108.8 (16)
O7iii—K2—O8iii63.19 (5)C3—C2—C1110.4 (2)
O7viii—K2—O8iii125.08 (6)C3—C2—H2108.8 (16)
O7viii—K2—O8viii63.19 (5)O6—C3—C2110.7 (2)
O8viii—K2—Naviii38.79 (4)O6—C3—H3106.8 (17)
O8iii—K2—Naiii38.79 (4)O6—C3—C4111.6 (2)
O8viii—K2—Naiii149.71 (4)C2—C3—H3112.0 (17)
O8iii—K2—Naviii149.71 (4)C2—C3—C4109.91 (19)
O8viii—K2—O8iii171.01 (7)C4—C3—H3105.7 (17)
K1ix—Na—H17112.0 (8)O3—C4—Nax49.02 (12)
K2ix—Na—K1ix97.54 (2)O3—C4—O4126.2 (2)
K2ix—Na—H1755.5 (8)O3—C4—C3116.7 (2)
O1—Na—K1ix87.72 (5)O4—C4—Nax123.81 (17)
O1—Na—K2ix133.89 (5)O4—C4—C3117.0 (2)
O1—Na—O3iv94.60 (7)C3—C4—Nax95.57 (14)
O1—Na—O5iv173.39 (7)
K1—O1—C1—O252.3 (3)O1—C1—C2—C361.4 (3)
K1—O1—C1—C2128.50 (17)O2—C1—C2—O53.7 (3)
K2x—O4—C4—Nax72.4 (2)O2—C1—C2—C3117.8 (2)
K2x—O4—C4—O311.6 (3)O5—C2—C3—O667.0 (2)
K2x—O4—C4—C3169.42 (15)O5—C2—C3—C456.8 (2)
K2xi—O5—C2—C1113.15 (17)O6—C3—C4—Nax62.83 (19)
K2xi—O5—C2—C3124.90 (15)O6—C3—C4—O316.4 (3)
Na—O1—C1—O275.4 (3)O6—C3—C4—O4164.5 (2)
Na—O1—C1—C2103.7 (2)C1—C2—C3—O655.1 (3)
Nax—O3—C4—O4106.1 (2)C1—C2—C3—C4178.8 (2)
Nax—O3—C4—C372.9 (2)C2—C3—C4—Nax60.39 (18)
Nax—O5—C2—C1134.63 (17)C2—C3—C4—O3106.9 (2)
Nax—O5—C2—C312.7 (3)C2—C3—C4—O472.3 (3)
O1—C1—C2—O5177.08 (19)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y1/2, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y1/2, z; (vii) x+1/2, y+1/2, z; (viii) x+1, y, z1; (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···AD—HH···AD···AD—H···A
O5—H5···O20.77 (3)2.06 (3)2.598 (2)128 (3)
O5—H5···O3iii0.77 (3)2.69 (3)3.284 (3)136 (3)
O5—H5···O4iii0.77 (3)2.89 (3)3.251 (3)112 (3)
O6—H6···O10x0.75 (3)2.08 (3)2.819 (3)168 (3)
O7—H17···O60.79 (4)1.99 (4)2.780 (3)176 (4)
O7—H27···O4v0.80 (3)2.07 (3)2.856 (3)168 (3)
O8—H18···O3xii0.84 (4)1.86 (4)2.696 (3)171 (4)
O8—H28···O1ix0.82 (4)2.84 (4)3.346 (3)122 (3)
O8—H28···O2ix0.82 (4)1.93 (4)2.747 (3)173 (4)
O9—H19···O2vi0.79 (4)2.58 (4)3.123 (3)128 (3)
O9—H19···O3iv0.79 (4)2.60 (4)3.159 (3)129 (3)
O9—H19···O6iv0.79 (4)2.42 (4)3.108 (3)147 (3)
O9—H29···O4ii0.92 (4)1.88 (4)2.786 (3)169 (3)
O10—H110···O1i0.83 (4)1.88 (4)2.714 (3)175 (3)
O10—H210···O9ix0.83 (4)1.92 (4)2.751 (3)178 (4)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y1/2, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y1/2, z; (ix) x, y, z+1; (x) x+1/2, y+1/2, z+1; (xii) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (150K_har) top
Crystal data top
C4H12KNaO10Dx = 1.808 Mg m3
Mr = 282.23Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 8154 reflections
a = 11.7916 (6) Åθ = 3.6–29.2°
b = 14.2002 (8) ŵ = 0.60 mm1
c = 6.1907 (3) ÅT = 150 K
V = 1036.60 (10) Å3Prism, clear colourless
Z = 40.48 × 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 Source2383 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.810, Tmax = 1.000l = 88
18107 measured reflections
Refinement top
Refinement on F2Hydrogen site location: difference Fourier map
Least-squares matrix: fullOnly 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 = 1.09Δρmax = 0.30 e Å3
2664 reflectionsΔρmin = 0.28 e Å3
182 parametersAbsolute structure: Flack x determined using 880 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
1 restraintAbsolute 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
xyzUiso*/Ueq
K10.0000000.0000000.04316 (13)0.0287 (2)
K20.5000000.0000000.16073 (12)0.01920 (17)
Na0.23237 (8)0.00687 (7)0.51606 (14)0.0158 (2)
O10.12025 (13)0.10875 (12)0.3481 (3)0.0154 (3)
O20.21218 (15)0.20344 (12)0.1181 (3)0.0180 (4)
O30.22848 (16)0.40731 (12)0.8197 (3)0.0217 (4)
O40.04848 (15)0.35928 (13)0.8485 (3)0.0202 (4)
O50.16502 (15)0.35790 (12)0.3247 (3)0.0158 (4)
H50.195 (3)0.342 (2)0.221 (6)0.024*
O60.29608 (15)0.24862 (12)0.6334 (3)0.0171 (4)
H60.326 (3)0.290 (2)0.593 (5)0.026*
O70.39610 (16)0.08322 (13)0.4855 (3)0.0201 (4)
H170.368 (3)0.129 (3)0.527 (6)0.030*
H270.434 (3)0.093 (2)0.377 (6)0.030*
O80.2375 (2)0.04155 (15)0.8799 (3)0.0279 (5)
H180.257 (3)0.001 (3)0.977 (6)0.042*
H280.233 (3)0.091 (3)0.945 (6)0.042*
O90.05899 (17)0.19228 (16)0.0314 (3)0.0267 (5)
H190.117 (3)0.207 (3)0.029 (6)0.040*
H290.028 (3)0.250 (3)0.062 (5)0.040*
O100.07839 (16)0.10705 (15)0.5713 (4)0.0250 (4)
H1100.017 (3)0.105 (2)0.509 (5)0.037*
H2100.071 (3)0.138 (3)0.688 (6)0.037*
C10.1552 (2)0.18783 (17)0.2828 (4)0.0126 (5)
C20.12523 (19)0.27330 (17)0.4230 (4)0.0128 (5)
H20.039 (2)0.2778 (19)0.436 (4)0.015*
C30.17730 (19)0.26351 (17)0.6476 (4)0.0139 (5)
H30.146 (2)0.210 (2)0.725 (5)0.017*
C40.1493 (2)0.35064 (18)0.7842 (4)0.0161 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0358 (4)0.0258 (4)0.0246 (4)0.0130 (4)0.0000.000
K20.0201 (3)0.0211 (4)0.0163 (3)0.0027 (3)0.0000.000
Na0.0151 (4)0.0156 (5)0.0166 (4)0.0003 (4)0.0002 (3)0.0004 (4)
O10.0165 (8)0.0137 (8)0.0161 (8)0.0007 (6)0.0016 (7)0.0011 (7)
O20.0214 (9)0.0175 (9)0.0151 (9)0.0001 (7)0.0035 (7)0.0009 (7)
O30.0292 (10)0.0179 (9)0.0180 (9)0.0057 (8)0.0009 (8)0.0034 (7)
O40.0204 (9)0.0243 (9)0.0159 (8)0.0067 (7)0.0002 (8)0.0024 (8)
O50.0222 (9)0.0140 (8)0.0114 (8)0.0002 (7)0.0015 (7)0.0007 (7)
O60.0150 (8)0.0160 (9)0.0203 (9)0.0013 (7)0.0018 (8)0.0005 (7)
O70.0183 (9)0.0192 (10)0.0227 (10)0.0002 (7)0.0040 (8)0.0012 (8)
O80.0535 (14)0.0162 (9)0.0141 (9)0.0055 (9)0.0009 (9)0.0005 (7)
O90.0176 (9)0.0372 (12)0.0253 (11)0.0007 (9)0.0055 (8)0.0011 (9)
O100.0156 (9)0.0278 (11)0.0314 (11)0.0044 (8)0.0042 (8)0.0074 (9)
C10.0108 (11)0.0143 (11)0.0126 (11)0.0005 (9)0.0042 (9)0.0013 (9)
C20.0135 (11)0.0120 (11)0.0127 (11)0.0002 (9)0.0010 (9)0.0003 (9)
C30.0151 (11)0.0127 (11)0.0138 (11)0.0015 (9)0.0012 (10)0.0005 (10)
C40.0228 (13)0.0158 (12)0.0097 (11)0.0027 (10)0.0022 (10)0.0017 (9)
Geometric parameters (Å, º) top
K1—O1i2.8212 (17)Na—C4iv3.081 (3)
K1—O12.8212 (17)O1—C11.263 (3)
K1—O8ii3.036 (2)O2—C11.241 (3)
K1—O8iii3.036 (2)O3—C41.252 (3)
K1—O92.855 (2)O4—C41.260 (3)
K1—O9i2.855 (2)O5—H50.77 (3)
K1—O10ii3.420 (2)O5—C21.426 (3)
K1—O10iii3.420 (2)O6—H60.73 (3)
K2—O4iv2.8382 (18)O6—C31.419 (3)
K2—O4v2.8383 (18)O7—H170.78 (4)
K2—O5vi2.9814 (18)O7—H270.82 (3)
K2—O5vii2.9814 (18)O8—H180.86 (4)
K2—O7ii2.774 (2)O8—H280.82 (4)
K2—O7viii2.774 (2)O9—H190.81 (4)
K2—O8ii3.161 (2)O9—H290.92 (4)
K2—O8viii3.161 (2)O10—H1100.82 (4)
Na—O12.3505 (19)O10—H2100.85 (4)
Na—O3iv2.453 (2)C1—C21.533 (3)
Na—O5iv2.474 (2)C2—H21.02 (3)
Na—O72.324 (2)C2—C31.526 (3)
Na—H172.51 (3)C3—H30.98 (3)
Na—O82.356 (2)C3—C41.534 (3)
Na—O102.332 (2)
Naiii—K1—Naii80.08 (3)O1—Na—H1780.3 (8)
O1i—K1—Naiii101.64 (4)O1—Na—O8103.51 (8)
O1—K1—Naii101.64 (4)O1—Na—C4iv116.52 (7)
O1—K1—Naiii145.38 (4)O3iv—Na—K1ix141.35 (6)
O1i—K1—Naii145.38 (4)O3iv—Na—K2ix107.92 (5)
O1—K1—O1i96.00 (7)O3iv—Na—O5iv81.95 (6)
O1i—K1—O8ii142.46 (5)O3iv—Na—H17106.6 (9)
O1i—K1—O8iii69.68 (5)O3iv—Na—C4iv22.72 (6)
O1—K1—O8ii69.68 (5)O5iv—Na—K1ix91.55 (5)
O1—K1—O8iii142.46 (5)O5iv—Na—K2ix52.72 (4)
O1—K1—O9i72.98 (5)O5iv—Na—H17106.0 (8)
O1i—K1—O972.98 (5)O5iv—Na—C4iv60.61 (6)
O1—K1—O9120.61 (6)O7—Na—K1ix125.72 (6)
O1i—K1—O9i120.61 (6)O7—Na—K2ix47.76 (5)
O1i—K1—O10ii117.65 (5)O7—Na—O192.68 (7)
O1i—K1—O10iii132.76 (5)O7—Na—O3iv92.76 (7)
O1—K1—O10ii132.76 (5)O7—Na—O5iv93.06 (7)
O1—K1—O10iii117.65 (5)O7—Na—H1718.0 (8)
O8iii—K1—Naiii32.47 (4)O7—Na—O884.01 (8)
O8ii—K1—Naiii109.50 (5)O7—Na—O10174.12 (9)
O8iii—K1—Naii109.50 (5)O7—Na—C4iv86.35 (7)
O8ii—K1—Naii32.47 (4)O8—Na—K1ix43.77 (6)
O8iii—K1—O8ii141.09 (8)O8—Na—K2ix57.23 (6)
O8ii—K1—O10iii83.02 (5)O8—Na—O3iv161.84 (8)
O8iii—K1—O10iii63.42 (5)O8—Na—O5iv80.39 (7)
O8iii—K1—O10ii83.02 (5)O8—Na—H1774.5 (8)
O8ii—K1—O10ii63.42 (5)O8—Na—C4iv139.17 (8)
O9—K1—Naiii93.13 (5)O10—Na—K1ix53.21 (6)
O9i—K1—Naiii72.40 (5)O10—Na—K2ix126.50 (6)
O9i—K1—Naii93.13 (5)O10—Na—O193.04 (7)
O9—K1—Naii72.40 (5)O10—Na—O3iv88.15 (8)
O9—K1—O8iii89.14 (6)O10—Na—O5iv81.31 (7)
O9i—K1—O8ii89.15 (6)O10—Na—H17164.2 (9)
O9i—K1—O8iii84.67 (6)O10—Na—O893.32 (8)
O9—K1—O8ii84.67 (6)O10—Na—C4iv92.32 (8)
O9i—K1—O9161.38 (9)C4iv—Na—K1ix140.17 (6)
O9i—K1—O10ii110.65 (6)C4iv—Na—K2ix87.58 (5)
O9—K1—O10ii51.02 (6)C4iv—Na—H17103.5 (9)
O9i—K1—O10iii51.02 (6)Na—O1—K1101.32 (6)
O9—K1—O10iii110.65 (6)C1—O1—K1115.89 (15)
O10ii—K1—Naii33.09 (4)C1—O1—Na125.39 (14)
O10iii—K1—Naiii33.09 (4)C4—O3—Nax108.11 (15)
O10ii—K1—Naiii61.97 (4)C4—O4—K2x118.29 (16)
O10iii—K1—Naii61.97 (4)K2xi—O5—H5102 (2)
O10ii—K1—O10iii62.68 (7)Nax—O5—K2xi85.96 (6)
Naii—K2—Naviii115.27 (3)Nax—O5—H5110 (2)
O4iv—K2—Naviii123.57 (4)C2—O5—K2xi120.05 (13)
O4v—K2—Naviii100.14 (4)C2—O5—Nax130.15 (14)
O4iv—K2—Naii100.15 (4)C2—O5—H5105 (2)
O4v—K2—Naii123.57 (4)C3—O6—H6112 (3)
O4iv—K2—O4v94.16 (8)K2ix—O7—H17107 (3)
O4v—K2—O5vi147.12 (5)K2ix—O7—H27119 (2)
O4v—K2—O5vii67.91 (5)Na—O7—K2ix93.91 (7)
O4iv—K2—O5vi67.91 (5)Na—O7—H1795 (3)
O4iv—K2—O5vii147.12 (5)Na—O7—H27128 (2)
O4v—K2—O8viii83.11 (5)H17—O7—H27111 (3)
O4iv—K2—O8viii90.67 (5)K1ix—O8—K2ix153.34 (8)
O4v—K2—O8ii90.67 (5)K1ix—O8—H1883 (2)
O4iv—K2—O8ii83.11 (5)K1ix—O8—H2887 (3)
O5vii—K2—Naviii41.33 (4)K2ix—O8—H1871 (2)
O5vii—K2—Naii112.73 (4)K2ix—O8—H28105 (3)
O5vi—K2—Naviii112.73 (4)Na—O8—K1ix103.76 (8)
O5vi—K2—Naii41.33 (4)Na—O8—K2ix83.96 (6)
O5vi—K2—O5vii140.18 (8)Na—O8—H18119 (3)
O5vii—K2—O8viii60.94 (5)Na—O8—H28137 (3)
O5vi—K2—O8viii122.67 (5)H18—O8—H28104 (4)
O5vii—K2—O8ii122.67 (5)K1—O9—H19112 (3)
O5vi—K2—O8ii60.94 (5)K1—O9—H29142 (2)
O7ii—K2—Naii38.33 (4)H19—O9—H29102 (3)
O7viii—K2—Naii86.51 (5)K1ix—O10—H11098 (2)
O7ii—K2—Naviii86.51 (5)K1ix—O10—H21058 (2)
O7viii—K2—Naviii38.33 (4)Na—O10—K1ix93.70 (7)
O7ii—K2—O4v109.07 (6)Na—O10—H110127 (2)
O7viii—K2—O4v138.48 (5)Na—O10—H210122 (2)
O7viii—K2—O4iv109.07 (6)H110—O10—H210109 (3)
O7ii—K2—O4iv138.48 (5)O1—C1—C2116.6 (2)
O7viii—K2—O5vi74.40 (5)O2—C1—O1126.8 (2)
O7ii—K2—O5vii74.40 (5)O2—C1—C2116.7 (2)
O7ii—K2—O5vi74.41 (5)O5—C2—C1110.45 (18)
O7viii—K2—O5vii74.41 (5)O5—C2—H2108.0 (15)
O7viii—K2—O7ii75.71 (9)O5—C2—C3109.45 (19)
O7ii—K2—O8viii125.09 (6)C1—C2—H2108.9 (16)
O7ii—K2—O8ii63.30 (5)C3—C2—C1110.53 (19)
O7viii—K2—O8ii125.09 (6)C3—C2—H2109.4 (15)
O7viii—K2—O8viii63.30 (5)O6—C3—C2110.7 (2)
O8viii—K2—Naviii38.80 (4)O6—C3—H3106.8 (16)
O8ii—K2—Naii38.80 (4)O6—C3—C4111.5 (2)
O8viii—K2—Naii149.81 (4)C2—C3—H3111.5 (17)
O8ii—K2—Naviii149.81 (4)C2—C3—C4110.00 (19)
O8viii—K2—O8ii170.88 (7)C4—C3—H3106.2 (17)
K1ix—Na—H17111.8 (9)O3—C4—Nax49.17 (12)
K2ix—Na—K1ix97.60 (2)O3—C4—O4125.8 (2)
K2ix—Na—H1755.1 (8)O3—C4—C3117.1 (2)
O1—Na—K1ix87.77 (5)O4—C4—Nax123.65 (17)
O1—Na—K2ix133.90 (5)O4—C4—C3117.1 (2)
O1—Na—O3iv94.48 (7)C3—C4—Nax95.73 (14)
O1—Na—O5iv173.37 (7)
K1—O1—C1—O252.2 (3)O1—C1—C2—C361.6 (3)
K1—O1—C1—C2128.49 (17)O2—C1—C2—O53.5 (3)
K2x—O4—C4—Nax72.3 (2)O2—C1—C2—C3117.8 (2)
K2x—O4—C4—O311.5 (3)O5—C2—C3—O667.1 (2)
K2x—O4—C4—C3169.32 (15)O5—C2—C3—C456.6 (2)
K2xi—O5—C2—C1113.12 (17)O6—C3—C4—Nax62.81 (19)
K2xi—O5—C2—C3124.96 (15)O6—C3—C4—O316.2 (3)
Na—O1—C1—O275.6 (3)O6—C3—C4—O4164.6 (2)
Na—O1—C1—C2103.7 (2)C1—C2—C3—O654.8 (3)
Nax—O3—C4—O4106.2 (2)C1—C2—C3—C4178.5 (2)
Nax—O3—C4—C373.0 (2)C2—C3—C4—Nax60.44 (18)
Nax—O5—C2—C1134.45 (17)C2—C3—C4—O3107.1 (2)
Nax—O5—C2—C312.5 (3)C2—C3—C4—O472.2 (3)
O1—C1—C2—O5177.10 (19)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y1/2, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y1/2, z; (vii) x+1/2, y+1/2, z; (viii) x+1, y, z1; (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···AD—HH···AD···AD—H···A
O5—H5···O20.77 (3)2.08 (3)2.599 (2)125 (3)
O5—H5···O3ii0.77 (3)2.68 (3)3.291 (3)138 (3)
O5—H5···O4ii0.77 (3)2.89 (3)3.253 (3)112 (3)
O6—H6···O10x0.73 (3)2.11 (3)2.828 (3)169 (4)
O7—H17···O60.78 (4)2.00 (4)2.783 (3)180 (4)
O7—H27···O4v0.82 (3)2.06 (3)2.859 (3)166 (3)
O8—H18···O3xii0.86 (4)1.84 (4)2.693 (3)170 (4)
O8—H28···O1ix0.82 (4)2.84 (4)3.351 (3)123 (3)
O8—H28···O2ix0.82 (4)1.93 (4)2.748 (3)174 (4)
O9—H19···O2vi0.81 (4)2.55 (4)3.124 (3)129 (3)
O9—H19···O3iv0.81 (4)2.61 (4)3.162 (3)127 (3)
O9—H19···O6iv0.81 (4)2.41 (4)3.114 (3)146 (3)
O9—H29···O4iii0.92 (4)1.88 (4)2.790 (3)172 (3)
O10—H110···O1i0.82 (4)1.90 (4)2.720 (3)175 (3)
O10—H210···O9ix0.85 (4)1.91 (4)2.751 (3)173 (3)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y1/2, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y1/2, z; (ix) x, y, z+1; (x) x+1/2, y+1/2, z+1; (xii) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (175K_anh) top
Crystal data top
C4H12KNaO10Dx = 1.804 Mg m3
Mr = 282.22Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 7792 reflections
a = 11.8046 (7) Åθ = 3.6–29.2°
b = 14.2075 (9) ŵ = 0.59 mm1
c = 6.1957 (3) ÅT = 175 K
V = 1039.1 (1) Å3Prism, clear colourless
Z = 40.48 × 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 Source2357 reflections with I 2u(I)
Graphite monochromatorRint = 0.052
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.799, Tmax = 1.000l = 88
18179 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.07Δρmax = 0.30 e Å3
2672 reflectionsΔρmin = 0.30 e Å3
195 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
1 restraintAbsolute structure parameter: 0.03 (2)
12 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00.00.0437 (2)0.0354 (5)
K20.50.00.16034 (9)0.02184 (14)
Na0.23229 (6)0.00681 (6)0.51684 (11)0.01789 (16)
O10.12026 (11)0.10884 (9)0.3482 (2)0.0172 (3)
O20.21185 (12)0.20331 (9)0.1183 (2)0.0202 (3)
O30.22904 (13)0.40708 (10)0.8186 (2)0.0246 (3)
O40.04894 (12)0.35956 (10)0.8477 (2)0.0230 (3)
O50.16496 (12)0.35792 (10)0.3244 (2)0.0178 (3)
H50.193 (2)0.3387 (17)0.218 (4)0.0267 (4)*
O60.29604 (12)0.24846 (10)0.6329 (2)0.0191 (3)
H60.325 (2)0.2905 (17)0.593 (4)0.0286 (5)*
O70.39595 (12)0.08318 (11)0.4854 (3)0.0223 (3)
H170.368 (2)0.133 (2)0.527 (4)0.0335 (5)*
H270.434 (2)0.0929 (19)0.380 (4)0.0335 (5)*
O80.23835 (16)0.04152 (12)0.8803 (2)0.0316 (4)
H180.256 (2)0.002 (2)0.976 (5)0.0474 (6)*
H280.234 (2)0.093 (2)0.942 (5)0.0474 (6)*
O90.05924 (14)0.19267 (13)0.0319 (3)0.0312 (4)
H190.117 (3)0.205 (2)0.029 (5)0.0468 (6)*
H290.032 (2)0.249 (2)0.064 (4)0.0468 (6)*
O100.07789 (13)0.10646 (12)0.5718 (3)0.0294 (4)
H1100.015 (3)0.106 (2)0.513 (4)0.0440 (6)*
H2100.071 (2)0.137 (2)0.691 (5)0.0440 (6)*
C10.15525 (15)0.18782 (13)0.2831 (3)0.0142 (4)
C20.12536 (15)0.27338 (14)0.4229 (3)0.0150 (4)
H20.0409 (18)0.2764 (15)0.435 (3)0.0180 (4)*
C30.17743 (15)0.26353 (13)0.6473 (3)0.0151 (4)
H30.1461 (18)0.2092 (16)0.725 (4)0.0181 (4)*
C40.14973 (18)0.35089 (14)0.7840 (3)0.0183 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0414 (10)0.0340 (11)0.0306 (10)0.0175 (9)0.0000000.000000
K20.0225 (3)0.0243 (3)0.0186 (3)0.0032 (3)0.0000000.000000
Na0.0172 (3)0.0171 (4)0.0193 (3)0.0005 (3)0.0003 (3)0.0006 (3)
O10.0183 (6)0.0149 (6)0.0185 (6)0.0009 (5)0.0012 (6)0.0005 (6)
O20.0244 (7)0.0195 (7)0.0168 (7)0.0005 (6)0.0036 (6)0.0011 (5)
O30.0337 (8)0.0194 (7)0.0208 (7)0.0066 (6)0.0013 (7)0.0044 (6)
O40.0235 (7)0.0274 (8)0.0181 (7)0.0071 (6)0.0007 (6)0.0035 (6)
O50.0251 (7)0.0146 (7)0.0137 (7)0.0000 (5)0.0006 (6)0.0000 (5)
O60.0166 (7)0.0182 (7)0.0225 (7)0.0015 (5)0.0018 (6)0.0007 (6)
O70.0200 (7)0.0199 (8)0.0270 (8)0.0004 (6)0.0049 (6)0.0013 (6)
O80.0604 (11)0.0185 (8)0.0159 (8)0.0072 (8)0.0022 (8)0.0006 (6)
O90.0211 (8)0.0441 (10)0.0285 (9)0.0008 (7)0.0061 (7)0.0017 (8)
O100.0185 (7)0.0322 (9)0.0375 (9)0.0053 (7)0.0054 (7)0.0101 (7)
C10.0124 (9)0.0169 (9)0.0132 (9)0.0011 (7)0.0036 (7)0.0004 (7)
C20.0153 (9)0.0149 (9)0.0148 (9)0.0002 (7)0.0000 (8)0.0011 (7)
C30.0163 (9)0.0137 (9)0.0153 (9)0.0007 (7)0.0009 (8)0.0008 (8)
C40.0267 (11)0.0168 (10)0.0115 (9)0.0030 (8)0.0023 (8)0.0008 (7)
Geometric parameters (Å, º) top
K1—O12.8223 (16)Na—O72.3249 (16)
K1—O1i2.8223 (16)Na—O82.3556 (16)
K1—O8ii3.0477 (19)Na—O102.3328 (17)
K1—O8iii3.0477 (19)Na—C4v3.082 (2)
K1—H18ii3.05 (3)O1—C11.262 (2)
K1—H18iii3.05 (3)O2—C11.240 (2)
K1—O9i2.8639 (19)O3—C41.249 (2)
K1—O92.8639 (19)O4—C41.260 (2)
K1—O10ii3.418 (2)O5—H50.79 (3)
K1—O10iii3.418 (2)O5—C21.426 (2)
K1—H210iii3.04 (3)O6—H60.73 (2)
K1—H210ii3.04 (3)O6—C31.419 (2)
K2—O4iv2.8402 (14)O7—H170.82 (3)
K2—O4v2.8402 (14)O7—H270.80 (3)
K2—O5vi2.9833 (14)O8—H180.84 (3)
K2—O5vii2.9833 (14)O8—H280.83 (3)
K2—O7viii2.7789 (16)O9—H190.80 (3)
K2—O7ii2.7789 (16)O9—H290.89 (3)
K2—O8ii3.1546 (19)O10—H1100.83 (3)
K2—O8viii3.1546 (19)O10—H2100.86 (3)
K2—H18ii3.01 (3)C1—C21.534 (3)
K2—H18viii3.01 (3)C2—H21.00 (2)
Na—O12.3538 (15)C2—C31.526 (3)
Na—O3v2.4545 (16)C3—H30.98 (2)
Na—O5v2.4764 (16)C3—C41.538 (3)
Naiii—K1—Naii80.10 (3)O8ii—K2—O5vi122.67 (4)
O1—K1—Naii101.57 (3)O8ii—K2—O5vii60.97 (4)
O1—K1—Naiii145.36 (3)O8viii—K2—O5vii122.67 (4)
O1i—K1—Naii145.36 (3)O8ii—K2—O7ii63.31 (4)
O1i—K1—Naiii101.57 (3)O8ii—K2—O7viii125.13 (4)
O1i—K1—O196.11 (7)O8viii—K2—O7viii63.31 (4)
O8iii—K1—Naiii32.49 (3)O8viii—K2—O7ii125.13 (4)
O8ii—K1—Naii32.49 (3)O8viii—K2—O8ii170.83 (6)
O8iii—K1—Naii109.57 (5)H18viii—K2—Naviii48.6 (5)
O8ii—K1—Naiii109.57 (5)H18viii—K2—Naii163.8 (6)
O8iii—K1—O1142.41 (5)H18ii—K2—Naviii163.8 (6)
O8ii—K1—O169.61 (4)H18ii—K2—Naii48.6 (5)
O8ii—K1—O1i142.41 (5)H18ii—K2—O4iv89.9 (6)
O8iii—K1—O1i69.61 (4)H18ii—K2—O4v67.6 (6)
O8iii—K1—O8ii141.21 (8)H18viii—K2—O4v89.9 (6)
H18ii—K1—Naii42.0 (5)H18viii—K2—O4iv67.6 (6)
H18iii—K1—Naii122.0 (5)H18ii—K2—O5vii58.3 (6)
H18iii—K1—Naiii42.0 (5)H18ii—K2—O5vi135.8 (7)
H18ii—K1—Naiii122.0 (5)H18viii—K2—O5vi58.3 (6)
H18ii—K1—O1i126.5 (6)H18viii—K2—O5vii135.8 (7)
H18iii—K1—O1126.5 (6)H18ii—K2—O7ii78.1 (6)
H18iii—K1—O1i65.8 (6)H18ii—K2—O7viii130.4 (6)
H18ii—K1—O165.8 (6)H18viii—K2—O7viii78.1 (6)
H18iii—K1—O8iii15.9 (6)H18viii—K2—O7ii130.4 (6)
H18ii—K1—O8iii150.4 (5)H18ii—K2—O8viii156.8 (6)
H18iii—K1—O8ii150.4 (5)H18ii—K2—O8ii15.5 (6)
H18ii—K1—O8ii15.9 (6)H18viii—K2—O8ii156.8 (6)
H18iii—K1—H18ii164.1 (11)H18viii—K2—O8viii15.5 (6)
O9—K1—Naiii93.07 (5)H18viii—K2—H18ii147.5 (11)
O9—K1—Naii72.31 (4)K2ix—Na—K1x97.66 (2)
O9i—K1—Naiii72.31 (4)O1—Na—K1x87.86 (4)
O9i—K1—Naii93.07 (5)O1—Na—K2ix133.93 (4)
O9—K1—O1i73.05 (5)O3v—Na—K1x141.18 (5)
O9—K1—O1120.68 (5)O3v—Na—K2ix107.97 (4)
O9i—K1—O173.05 (5)O3v—Na—O194.39 (5)
O9i—K1—O1i120.68 (5)O5v—Na—K1x91.64 (4)
O9—K1—O8ii84.56 (5)O5v—Na—K2ix52.70 (3)
O9—K1—O8iii89.20 (5)O5v—Na—O1173.35 (6)
O9i—K1—O8ii89.20 (5)O5v—Na—O3v81.86 (5)
O9i—K1—O8iii84.56 (5)O7—Na—K1x125.87 (5)
O9—K1—H18ii75.1 (6)O7—Na—K2ix47.82 (4)
O9—K1—H18iii102.2 (7)O7—Na—O192.62 (6)
O9i—K1—H18iii75.1 (6)O7—Na—O3v92.79 (6)
O9i—K1—H18ii102.2 (7)O7—Na—O5v93.04 (6)
O9i—K1—O9161.17 (9)O8—Na—K1x44.03 (5)
O10ii—K1—Naii33.08 (3)O8—Na—K2ix57.02 (5)
O10ii—K1—Naiii61.85 (4)O8—Na—O1103.77 (6)
O10iii—K1—Naiii33.08 (3)O8—Na—O3v161.66 (6)
O10iii—K1—Naii61.85 (4)O8—Na—O5v80.31 (6)
O10ii—K1—O1i117.69 (4)O8—Na—O783.95 (6)
O10iii—K1—O1117.69 (4)O10—Na—K1x53.11 (5)
O10iii—K1—O1i132.76 (4)O10—Na—K2ix126.70 (5)
O10ii—K1—O1132.76 (4)O10—Na—O192.84 (6)
O10ii—K1—O8iii83.03 (5)O10—Na—O3v88.07 (6)
O10iii—K1—O8ii83.03 (5)O10—Na—O5v81.59 (6)
O10ii—K1—O8ii63.46 (5)O10—Na—O7174.39 (7)
O10iii—K1—O8iii63.46 (5)O10—Na—O893.51 (7)
O10ii—K1—H18ii67.6 (5)C4v—Na—K1x140.20 (4)
O10ii—K1—H18iii98.3 (6)C4v—Na—K2ix87.63 (4)
O10iii—K1—H18iii67.6 (5)C4v—Na—O1116.31 (6)
O10iii—K1—H18ii98.3 (6)C4v—Na—O3v22.64 (5)
O10ii—K1—O951.05 (5)C4v—Na—O5v60.65 (5)
O10ii—K1—O9i110.41 (6)C4v—Na—O786.25 (6)
O10iii—K1—O9i51.05 (5)C4v—Na—O8139.08 (6)
O10iii—K1—O9110.41 (6)C4v—Na—O1092.47 (6)
O10iii—K1—O10ii62.38 (6)Na—O1—K1101.35 (5)
H210iii—K1—Naiii42.1 (5)C1—O1—K1115.99 (12)
H210iii—K1—Naii69.1 (6)C1—O1—Na125.36 (11)
H210ii—K1—Naiii69.1 (6)C4—O3—Naxi108.22 (12)
H210ii—K1—Naii42.1 (5)C4—O4—K2xii118.34 (12)
H210ii—K1—O1i105.6 (6)Naxi—O5—K2xiii85.98 (4)
H210iii—K1—O1i133.7 (5)H5—O5—K2xiii102.8 (18)
H210iii—K1—O1105.6 (6)H5—O5—Naxi113.4 (18)
H210ii—K1—O1133.7 (5)C2—O5—K2xiii120.12 (10)
H210iii—K1—O8ii83.9 (5)C2—O5—Naxi130.11 (11)
H210ii—K1—O8iii83.9 (5)C2—O5—H5101.8 (18)
H210ii—K1—O8ii68.3 (5)C3—O6—H6111 (2)
H210iii—K1—O8iii68.3 (5)Na—O7—K2xiv93.86 (5)
H210iii—K1—H18iii68.4 (8)H17—O7—K2xiv107.4 (19)
H210iii—K1—H18ii99.8 (8)H17—O7—Na96.5 (19)
H210ii—K1—H18ii68.4 (8)H27—O7—K2xiv117.8 (19)
H210ii—K1—H18iii99.8 (8)H27—O7—Na128.9 (19)
H210iii—K1—O9124.1 (6)H27—O7—H17109 (3)
H210ii—K1—O9i124.1 (6)K2xiv—O8—K1xiv153.41 (6)
H210ii—K1—O937.3 (6)Na—O8—K1xiv103.48 (7)
H210iii—K1—O9i37.3 (6)Na—O8—K2xiv84.19 (5)
H210ii—K1—O10iii75.1 (6)H18—O8—K1xiv82 (2)
H210iii—K1—O10iii13.8 (6)H18—O8—K2xiv72.2 (19)
H210ii—K1—O10ii13.8 (6)H18—O8—Na119 (2)
H210iii—K1—O10ii75.1 (6)H28—O8—K1xiv87 (2)
H210iii—K1—H210ii88.3 (12)H28—O8—K2xiv106 (2)
Naviii—K2—Naii115.37 (3)H28—O8—Na134 (2)
O4iv—K2—Naii123.68 (3)H28—O8—H18107 (3)
O4v—K2—Naii100.05 (3)K2xiv—H18—K1xiv171.7 (11)
O4iv—K2—Naviii100.05 (3)O8—H18—K1xiv82 (2)
O4v—K2—Naviii123.68 (3)O8—H18—K2xiv92 (2)
O4v—K2—O4iv94.00 (6)H19—O9—K1i110 (2)
O5vi—K2—Naviii41.32 (3)H29—O9—K1i144.1 (18)
O5vi—K2—Naii112.75 (3)H29—O9—H19103 (3)
O5vii—K2—Naviii112.75 (3)Na—O10—K1x93.81 (6)
O5vii—K2—Naii41.32 (3)H110—O10—K1x97.6 (18)
O5vii—K2—O4v67.93 (4)H110—O10—Na128.9 (19)
O5vi—K2—O4v147.20 (4)H210—O10—K1x57.3 (19)
O5vii—K2—O4iv147.20 (4)H210—O10—Na120.1 (19)
O5vi—K2—O4iv67.93 (4)H210—O10—H110108 (3)
O5vii—K2—O5vi140.16 (6)O10—H210—K1x109 (2)
O7viii—K2—Naii86.57 (4)O2—C1—O1126.68 (18)
O7viii—K2—Naviii38.32 (3)C2—C1—O1116.67 (16)
O7ii—K2—Naii38.32 (3)C2—C1—O2116.64 (17)
O7ii—K2—Naviii86.57 (4)C1—C2—O5110.51 (15)
O7ii—K2—O4iv109.25 (4)H2—C2—O5108.8 (12)
O7viii—K2—O4iv138.37 (4)H2—C2—C1107.8 (12)
O7ii—K2—O4v138.37 (4)C3—C2—O5109.57 (15)
O7viii—K2—O4v109.25 (4)C3—C2—C1110.44 (15)
O7ii—K2—O5vii74.34 (4)C3—C2—H2109.7 (12)
O7viii—K2—O5vii74.43 (4)C2—C3—O6110.73 (16)
O7ii—K2—O5vi74.43 (4)H3—C3—O6106.5 (13)
O7viii—K2—O5vi74.34 (4)H3—C3—C2111.4 (13)
O7viii—K2—O7ii75.67 (7)C4—C3—O6111.48 (16)
O8viii—K2—Naviii38.78 (3)C4—C3—C2110.00 (15)
O8viii—K2—Naii149.88 (3)C4—C3—H3106.6 (13)
O8ii—K2—Naviii149.88 (3)O3—C4—Naxi49.15 (10)
O8ii—K2—Naii38.78 (3)O4—C4—Naxi123.51 (13)
O8viii—K2—O4iv82.97 (4)O4—C4—O3126.27 (19)
O8ii—K2—O4iv90.76 (4)C3—C4—Naxi95.75 (11)
O8ii—K2—O4v82.97 (4)C3—C4—O3116.82 (18)
O8viii—K2—O4v90.76 (4)C3—C4—O4116.90 (17)
O8viii—K2—O5vi60.97 (4)
K1—O1—C1—O251.99 (13)Naxi—O3—C4—C373.22 (12)
K1i—O1—C1—O251.99 (13)Naxi—O5—C2—C1134.38 (15)
K1—O1—C1—C2128.44 (11)Naxi—O5—C2—C312.47 (13)
K1i—O1—C1—C2128.44 (11)Naxi—C4—C3—O662.92 (11)
K2xii—O4—C4—Naxi72.67 (11)Naxi—C4—C3—C260.31 (11)
K2—O4v—C4v—Na72.67 (11)O1—C1—C2—O5176.94 (16)
K2xii—O4—C4—O311.83 (14)O1—C1—C2—C361.66 (18)
K2xi—O4—C4—O311.83 (14)O2—C1—C2—O53.44 (18)
K2xii—O4—C4—C3169.24 (12)O2—C1—C2—C3117.96 (17)
K2xi—O4—C4—C3169.24 (12)O3—C4—C3—O616.22 (19)
K2xv—O5—C2—C1113.12 (12)O3—C4—C3—C2107.01 (18)
K2xiii—O5—C2—C1113.12 (12)O4—C4—C3—O6164.75 (17)
K2xiii—O5—C2—C3124.97 (12)O4—C4—C3—C272.02 (18)
K2xv—O5—C2—C3124.97 (12)O5—C2—C3—O667.18 (15)
Na—O1—C1—O275.93 (15)O5—C2—C3—C456.48 (16)
Na—O1—C1—C2103.64 (14)O6—C3—C2—C154.77 (17)
Naxi—O3—C4—O4105.71 (12)C1—C2—C3—C4178.44 (15)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y+1/2, z; (vii) x+1/2, y1/2, z; (viii) x+1, y, z1; (ix) x+1, y, z+1; (x) x, y, z+1; (xi) x+1/2, y+1/2, z+1; (xii) x1/2, y+1/2, z+1; (xiii) x1/2, 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···AD—HH···AD···AD—H···A
O5—H5···O20.79 (3)2.03 (2)2.6005 (19)129 (2)
O5—H5···O3ii0.79 (3)2.69 (3)3.299 (2)135 (2)
O5—H5···O4ii0.79 (3)2.87 (3)3.256 (2)113 (2)
O6—H6···O10xi0.73 (2)2.12 (2)2.841 (2)169 (3)
O7—H17···O60.82 (3)1.96 (3)2.782 (2)177 (3)
O7—H27···O4iv0.80 (3)2.07 (3)2.861 (2)167 (3)
O8—H18···O3xvi0.84 (3)1.86 (3)2.697 (2)171 (3)
O8—H28···O1xiv0.83 (3)2.86 (3)3.356 (2)121 (2)
O8—H28···O2xiv0.83 (3)1.93 (3)2.749 (2)172 (3)
O9—H19···O2vii0.80 (3)2.57 (3)3.126 (2)128 (3)
O9—H19···O3v0.80 (3)2.59 (3)3.162 (2)130 (3)
O9—H19···O6v0.80 (3)2.43 (3)3.119 (2)146 (3)
O9—H29···O4iii0.89 (3)1.92 (3)2.794 (2)171 (3)
O10—H110···O1i0.83 (3)1.89 (3)2.719 (2)173 (3)
O10—H210···O9xiv0.86 (3)1.89 (3)2.753 (2)175 (3)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vii) x+1/2, y1/2, z; (xi) x+1/2, y+1/2, z+1; (xiv) x, y, z+1; (xvi) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (200K_anh) top
Crystal data top
C4H12KNaO10Dx = 1.800 Mg m3
Mr = 282.22Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 7450 reflections
a = 11.8172 (7) Åθ = 3.5–29.2°
b = 14.2126 (9) ŵ = 0.59 mm1
c = 6.2012 (3) ÅT = 200 K
V = 1041.52 (10) Å3Prism, clear colourless
Z = 40.48 × 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 Source2350 reflections with I 2u(I)
Graphite monochromatorRint = 0.054
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1819
Tmin = 0.798, Tmax = 1.000l = 88
18257 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.08Δρmax = 0.34 e Å3
2678 reflectionsΔρmin = 0.32 e Å3
195 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
1 restraintAbsolute structure parameter: 0.04 (2)
12 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00.00.0441 (3)0.0406 (5)
K20.50.00.16016 (10)0.02474 (15)
Na0.23217 (6)0.00677 (6)0.51782 (12)0.02024 (18)
O10.12034 (11)0.10885 (10)0.3486 (2)0.0195 (3)
O20.21150 (12)0.20330 (10)0.1182 (2)0.0229 (3)
O30.22987 (13)0.40693 (10)0.8178 (2)0.0275 (3)
O40.04988 (13)0.36003 (11)0.8471 (2)0.0259 (3)
O50.16471 (13)0.35770 (10)0.3244 (2)0.0200 (3)
H50.191 (2)0.3425 (18)0.211 (5)0.0299 (5)*
O60.29584 (12)0.24837 (10)0.6316 (3)0.0216 (3)
H60.326 (2)0.2919 (18)0.600 (5)0.0323 (5)*
O70.39594 (13)0.08303 (11)0.4852 (3)0.0252 (3)
H170.367 (2)0.132 (2)0.525 (5)0.0378 (5)*
H270.431 (2)0.095 (2)0.378 (5)0.0378 (5)*
O80.23925 (17)0.04151 (13)0.8813 (3)0.0356 (4)
H180.256 (3)0.003 (3)0.980 (5)0.0533 (7)*
H280.233 (3)0.094 (2)0.945 (5)0.0533 (7)*
O90.05967 (15)0.19347 (15)0.0327 (3)0.0365 (4)
H190.118 (3)0.207 (2)0.026 (5)0.0548 (6)*
H290.032 (3)0.248 (2)0.069 (5)0.0548 (6)*
O100.07759 (14)0.10576 (13)0.5728 (3)0.0349 (4)
H1100.016 (3)0.106 (2)0.512 (4)0.0523 (6)*
H2100.068 (3)0.136 (2)0.693 (5)0.0523 (6)*
C10.15499 (16)0.18789 (14)0.2828 (3)0.0164 (4)
C20.12531 (16)0.27334 (14)0.4225 (3)0.0163 (4)
H20.0411 (19)0.2780 (16)0.438 (3)0.0195 (5)*
C30.17744 (16)0.26356 (14)0.6471 (3)0.0174 (4)
H30.1465 (19)0.2099 (17)0.726 (4)0.0208 (5)*
C40.15028 (19)0.35095 (15)0.7826 (3)0.0203 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0471 (11)0.0385 (12)0.0361 (11)0.0210 (10)0.0000000.000000
K20.0250 (3)0.0275 (3)0.0217 (3)0.0034 (3)0.0000000.000000
Na0.0190 (4)0.0196 (4)0.0221 (4)0.0005 (3)0.0004 (3)0.0005 (4)
O10.0198 (7)0.0175 (7)0.0213 (7)0.0006 (5)0.0010 (6)0.0001 (6)
O20.0275 (8)0.0221 (8)0.0190 (8)0.0005 (6)0.0057 (6)0.0013 (6)
O30.0367 (8)0.0227 (8)0.0231 (8)0.0072 (7)0.0015 (7)0.0045 (6)
O40.0254 (7)0.0318 (8)0.0204 (7)0.0085 (6)0.0004 (7)0.0039 (7)
O50.0281 (8)0.0165 (7)0.0154 (7)0.0003 (6)0.0002 (6)0.0004 (6)
O60.0182 (7)0.0201 (8)0.0264 (8)0.0025 (6)0.0027 (6)0.0003 (6)
O70.0221 (8)0.0226 (8)0.0309 (9)0.0000 (6)0.0047 (7)0.0021 (7)
O80.0667 (12)0.0211 (8)0.0189 (8)0.0077 (8)0.0026 (8)0.0002 (6)
O90.0239 (9)0.0522 (12)0.0335 (10)0.0023 (8)0.0068 (7)0.0030 (9)
O100.0215 (8)0.0379 (10)0.0452 (11)0.0076 (7)0.0073 (8)0.0133 (8)
C10.0140 (9)0.0179 (10)0.0173 (9)0.0018 (8)0.0044 (8)0.0008 (8)
C20.0170 (9)0.0155 (10)0.0163 (9)0.0009 (8)0.0005 (8)0.0012 (7)
C30.0193 (9)0.0162 (9)0.0166 (9)0.0014 (8)0.0015 (8)0.0003 (8)
C40.0296 (12)0.0176 (10)0.0135 (9)0.0030 (8)0.0030 (8)0.0020 (8)
Geometric parameters (Å, º) top
K1—O12.8252 (17)Na—O72.3271 (17)
K1—O1i2.8252 (17)Na—O82.3576 (17)
K1—O8ii3.060 (2)Na—O102.3308 (18)
K1—O8iii3.060 (2)Na—C4v3.080 (2)
K1—H18ii3.06 (3)O1—C11.263 (2)
K1—H18iii3.06 (3)O2—C11.240 (2)
K1—O9i2.878 (2)O3—C41.251 (3)
K1—O92.878 (2)O4—C41.259 (3)
K1—O10ii3.412 (2)O5—H50.80 (3)
K1—O10iii3.412 (2)O5—C21.423 (2)
K1—H210iii3.02 (3)O6—H60.74 (2)
K1—H210ii3.02 (3)O6—C31.419 (2)
K2—O4iv2.8416 (15)O7—H170.81 (3)
K2—O4v2.8416 (15)O7—H270.80 (3)
K2—O5vi2.9859 (15)O8—H180.85 (3)
K2—O5vii2.9859 (15)O8—H280.85 (3)
K2—O7viii2.7824 (17)O9—H190.80 (3)
K2—O7ii2.7824 (17)O9—H290.87 (3)
K2—O8ii3.148 (2)O10—H1100.82 (3)
K2—O8viii3.148 (2)O10—H2100.86 (3)
K2—H18ii3.01 (3)C1—C21.532 (3)
K2—H18viii3.01 (3)C2—H21.00 (2)
Na—O12.3554 (16)C2—C31.529 (3)
Na—O3v2.4569 (17)C3—H30.98 (2)
Na—O5v2.4805 (17)C3—C41.533 (3)
Naiii—K1—Naii80.14 (4)O8ii—K2—O5vi122.62 (4)
O1—K1—Naii101.54 (3)O8ii—K2—O5vii61.10 (4)
O1—K1—Naiii145.38 (3)O8viii—K2—O5vii122.62 (4)
O1i—K1—Naii145.38 (3)O8ii—K2—O7ii63.41 (4)
O1i—K1—Naiii101.54 (3)O8ii—K2—O7viii125.22 (5)
O1i—K1—O196.11 (8)O8viii—K2—O7viii63.41 (4)
O8iii—K1—Naiii32.58 (4)O8viii—K2—O7ii125.22 (5)
O8ii—K1—Naii32.58 (4)O8viii—K2—O8ii170.63 (6)
O8iii—K1—Naii109.73 (6)H18viii—K2—Naviii49.1 (6)
O8ii—K1—Naiii109.73 (6)H18viii—K2—Naii164.4 (6)
O8iii—K1—O1142.31 (5)H18ii—K2—Naviii164.4 (6)
O8ii—K1—O169.50 (4)H18ii—K2—Naii49.1 (6)
O8ii—K1—O1i142.31 (5)H18ii—K2—O4iv89.5 (6)
O8iii—K1—O1i69.50 (4)H18ii—K2—O4v67.2 (7)
O8iii—K1—O8ii141.46 (9)H18viii—K2—O4v89.5 (6)
H18ii—K1—Naii42.5 (6)H18viii—K2—O4iv67.2 (7)
H18iii—K1—Naii122.6 (6)H18ii—K2—O5vii58.9 (6)
H18iii—K1—Naiii42.5 (6)H18ii—K2—O5vi135.6 (7)
H18ii—K1—Naiii122.6 (6)H18viii—K2—O5vi58.9 (6)
H18ii—K1—O1i126.4 (6)H18viii—K2—O5vii135.6 (7)
H18iii—K1—O1126.4 (6)H18ii—K2—O7ii78.5 (6)
H18iii—K1—O1i65.2 (6)H18ii—K2—O7viii131.1 (6)
H18ii—K1—O165.2 (6)H18viii—K2—O7viii78.5 (6)
H18iii—K1—O8iii16.0 (6)H18viii—K2—O7ii131.1 (6)
H18ii—K1—O8iii151.1 (6)H18ii—K2—O8viii156.3 (6)
H18iii—K1—O8ii151.1 (6)H18ii—K2—O8ii15.6 (6)
H18ii—K1—O8ii16.0 (6)H18viii—K2—O8ii156.3 (6)
H18iii—K1—H18ii165.1 (11)H18viii—K2—O8viii15.6 (6)
O9—K1—Naiii93.01 (5)H18viii—K2—H18ii146.4 (12)
O9—K1—Naii72.19 (5)K2ix—Na—K1x97.76 (2)
O9i—K1—Naiii72.19 (5)O1—Na—K1x87.95 (4)
O9i—K1—Naii93.01 (5)O1—Na—K2ix133.95 (4)
O9—K1—O1i73.19 (5)O3v—Na—K1x140.98 (5)
O9—K1—O1120.69 (6)O3v—Na—K2ix108.08 (4)
O9i—K1—O173.19 (5)O3v—Na—O194.21 (5)
O9i—K1—O1i120.69 (6)O5v—Na—K1x91.81 (4)
O9—K1—O8ii84.45 (5)O5v—Na—K2ix52.71 (4)
O9—K1—O8iii89.29 (5)O5v—Na—O1173.29 (6)
O9i—K1—O8ii89.29 (5)O5v—Na—O3v81.77 (5)
O9i—K1—O8iii84.45 (5)O7—Na—K1x126.10 (5)
O9—K1—H18ii75.4 (7)O7—Na—K2ix47.87 (4)
O9—K1—H18iii102.1 (7)O7—Na—O192.59 (6)
O9i—K1—H18iii75.4 (7)O7—Na—O3v92.77 (6)
O9i—K1—H18ii102.1 (7)O7—Na—O5v92.96 (6)
O9i—K1—O9160.95 (10)O8—Na—K1x44.33 (5)
O10ii—K1—Naii33.04 (3)O8—Na—K2ix56.81 (5)
O10ii—K1—Naiii61.79 (4)O8—Na—O1104.04 (6)
O10iii—K1—Naiii33.04 (3)O8—Na—O3v161.56 (7)
O10iii—K1—Naii61.79 (4)O8—Na—O5v80.29 (6)
O10ii—K1—O1i117.81 (4)O8—Na—O783.92 (7)
O10iii—K1—O1117.81 (4)O10—Na—K1x52.95 (5)
O10iii—K1—O1i132.73 (4)O10—Na—K2ix126.88 (5)
O10ii—K1—O1132.73 (4)O10—Na—O192.67 (6)
O10ii—K1—O8iii83.15 (5)O10—Na—O3v88.03 (7)
O10iii—K1—O8ii83.15 (5)O10—Na—O5v81.87 (6)
O10ii—K1—O8ii63.51 (5)O10—Na—O7174.61 (7)
O10iii—K1—O8iii63.51 (5)O10—Na—O893.65 (7)
O10ii—K1—H18ii68.2 (6)C4v—Na—K1x140.15 (5)
O10ii—K1—H18iii98.6 (6)C4v—Na—K2ix87.60 (4)
O10iii—K1—H18iii68.2 (6)C4v—Na—O1116.21 (6)
O10iii—K1—H18ii98.6 (6)C4v—Na—O3v22.74 (5)
O10ii—K1—O951.07 (5)C4v—Na—O5v60.48 (5)
O10ii—K1—O9i110.18 (7)C4v—Na—O786.13 (6)
O10iii—K1—O9i51.07 (5)C4v—Na—O8138.87 (7)
O10iii—K1—O9110.18 (7)C4v—Na—O1092.61 (7)
O10iii—K1—O10ii62.13 (7)Na—O1—K1101.43 (5)
H210iii—K1—Naiii42.4 (6)C1—O1—K1115.73 (13)
H210iii—K1—Naii68.4 (6)C1—O1—Na125.62 (12)
H210ii—K1—Naiii68.4 (6)C4—O3—Naxi107.87 (13)
H210ii—K1—Naii42.4 (6)C4—O4—K2xii118.98 (13)
H210ii—K1—O1i105.5 (6)Naxi—O5—K2xiii85.92 (5)
H210iii—K1—O1i134.3 (6)H5—O5—K2xiii97.9 (19)
H210iii—K1—O1105.5 (6)H5—O5—Naxi111.5 (19)
H210ii—K1—O1134.3 (6)C2—O5—K2xiii120.21 (11)
H210iii—K1—O8ii83.3 (6)C2—O5—Naxi130.26 (12)
H210ii—K1—O8iii83.3 (6)C2—O5—H5106.0 (18)
H210ii—K1—O8ii68.9 (6)C3—O6—H6111 (2)
H210iii—K1—O8iii68.9 (6)Na—O7—K2xiv93.79 (6)
H210iii—K1—H18iii69.6 (8)H17—O7—K2xiv108 (2)
H210iii—K1—H18ii99.3 (9)H17—O7—Na96 (2)
H210ii—K1—H18ii69.6 (8)H27—O7—K2xiv121 (2)
H210ii—K1—H18iii99.3 (9)H27—O7—Na128 (2)
H210iii—K1—O9123.7 (6)H27—O7—H17107 (3)
H210ii—K1—O9i123.7 (6)K2xiv—O8—K1xiv153.55 (6)
H210ii—K1—O937.4 (6)Na—O8—K1xiv103.10 (7)
H210iii—K1—O9i37.4 (6)Na—O8—K2xiv84.38 (6)
H210ii—K1—O10iii74.6 (6)H18—O8—K1xiv82 (2)
H210iii—K1—O10iii13.7 (6)H18—O8—K2xiv73 (2)
H210ii—K1—O10ii13.7 (6)H18—O8—Na121 (2)
H210iii—K1—O10ii74.6 (6)H28—O8—K1xiv86 (2)
H210iii—K1—H210ii87.5 (13)H28—O8—K2xiv107 (2)
Naviii—K2—Naii115.52 (3)H28—O8—Na135 (2)
O4iv—K2—Naii123.91 (3)H28—O8—H18105 (3)
O4v—K2—Naii99.85 (3)K2xiv—H18—K1xiv170.5 (11)
O4iv—K2—Naviii99.85 (3)O8—H18—K1xiv82 (2)
O4v—K2—Naviii123.91 (3)O8—H18—K2xiv92 (2)
O4v—K2—O4iv93.81 (7)H19—O9—K1i111 (2)
O5vi—K2—Naviii41.37 (3)H29—O9—K1i144 (2)
O5vi—K2—Naii112.75 (4)H29—O9—H19103 (3)
O5vii—K2—Naviii112.75 (4)Na—O10—K1x94.01 (6)
O5vii—K2—Naii41.37 (3)H110—O10—K1x99 (2)
O5vii—K2—O4v67.89 (4)H110—O10—Na129 (2)
O5vi—K2—O4v147.40 (4)H210—O10—K1x56 (2)
O5vii—K2—O4iv147.40 (4)H210—O10—Na122 (2)
O5vi—K2—O4iv67.89 (4)H210—O10—H110106 (3)
O5vii—K2—O5vi140.12 (6)O10—H210—K1x110 (2)
O7viii—K2—Naii86.62 (4)O2—C1—O1126.72 (19)
O7viii—K2—Naviii38.34 (3)C2—C1—O1116.61 (17)
O7ii—K2—Naii38.34 (3)C2—C1—O2116.68 (18)
O7ii—K2—Naviii86.62 (4)C1—C2—O5110.55 (15)
O7ii—K2—O4iv109.56 (5)H2—C2—O5108.0 (13)
O7viii—K2—O4iv138.19 (4)H2—C2—C1109.4 (13)
O7ii—K2—O4v138.19 (4)C3—C2—O5109.53 (16)
O7viii—K2—O4v109.56 (5)C3—C2—C1110.53 (16)
O7ii—K2—O5vii74.31 (4)C3—C2—H2108.7 (12)
O7viii—K2—O5vii74.41 (4)C2—C3—O6110.44 (16)
O7ii—K2—O5vi74.41 (4)H3—C3—O6106.5 (13)
O7viii—K2—O5vi74.31 (4)H3—C3—C2112.0 (13)
O7viii—K2—O7ii75.55 (7)C4—C3—O6111.53 (17)
O8viii—K2—Naviii38.81 (3)C4—C3—C2109.93 (16)
O8viii—K2—Naii150.04 (4)C4—C3—H3106.3 (13)
O8ii—K2—Naviii150.04 (4)O3—C4—Naxi49.39 (10)
O8ii—K2—Naii38.81 (3)O4—C4—Naxi123.37 (14)
O8viii—K2—O4iv82.67 (5)O4—C4—O3126.0 (2)
O8ii—K2—O4iv90.92 (4)C3—C4—Naxi96.10 (12)
O8ii—K2—O4v82.67 (5)C3—C4—O3116.96 (19)
O8viii—K2—O4v90.92 (4)C3—C4—O4117.03 (18)
O8viii—K2—O5vi61.10 (4)
K1—O1—C1—O252.24 (13)Naxi—O3—C4—C373.79 (12)
K1i—O1—C1—O252.24 (13)Naxi—O5—C2—C1134.31 (15)
K1—O1—C1—C2128.57 (12)Naxi—O5—C2—C312.29 (14)
K1i—O1—C1—C2128.57 (12)Naxi—C4—C3—O662.66 (12)
K2xii—O4—C4—Naxi72.53 (12)Naxi—C4—C3—C260.18 (12)
K2—O4v—C4v—Na72.53 (12)O1—C1—C2—O5177.21 (17)
K2xii—O4—C4—O311.53 (15)O1—C1—C2—C361.35 (19)
K2xi—O4—C4—O311.53 (15)O2—C1—C2—O53.52 (19)
K2xii—O4—C4—C3168.87 (13)O2—C1—C2—C3117.92 (18)
K2xi—O4—C4—C3168.87 (13)O3—C4—C3—O615.5 (2)
K2xv—O5—C2—C1113.03 (13)O3—C4—C3—C2107.32 (19)
K2xiii—O5—C2—C1113.03 (13)O4—C4—C3—O6164.85 (18)
K2xiii—O5—C2—C3124.94 (13)O4—C4—C3—C272.32 (19)
K2xv—O5—C2—C3124.94 (13)O5—C2—C3—O667.34 (16)
Na—O1—C1—O275.77 (16)O5—C2—C3—C456.14 (17)
Na—O1—C1—C2103.42 (15)O6—C3—C2—C154.70 (18)
Naxi—O3—C4—O4105.81 (13)C1—C2—C3—C4178.17 (16)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y+1/2, z; (vii) x+1/2, y1/2, z; (viii) x+1, y, z1; (ix) x+1, y, z+1; (x) x, y, z+1; (xi) x+1/2, y+1/2, z+1; (xii) x1/2, y+1/2, z+1; (xiii) x1/2, 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···AD—HH···AD···AD—H···A
O5—H5···O20.80 (3)2.07 (3)2.599 (2)123 (2)
O5—H5···O3ii0.80 (3)2.65 (3)3.309 (2)142 (2)
O5—H5···O4ii0.80 (3)2.82 (3)3.256 (2)117 (2)
O6—H6···O10xi0.74 (2)2.14 (2)2.853 (3)163 (3)
O7—H17···O60.81 (3)1.97 (3)2.783 (2)178 (3)
O7—H27···O4iv0.80 (3)2.08 (3)2.865 (2)166 (3)
O8—H18···O3xvi0.85 (3)1.86 (3)2.697 (2)170 (3)
O8—H28···O1xiv0.85 (3)2.84 (3)3.360 (2)121 (3)
O8—H28···O2xiv0.85 (3)1.90 (3)2.748 (2)173 (3)
O9—H19···O2vii0.80 (3)2.55 (3)3.122 (2)130 (3)
O9—H19···O3v0.80 (3)2.60 (3)3.162 (2)128 (3)
O9—H19···O6v0.80 (3)2.44 (3)3.128 (2)145 (3)
O9—H29···O4iii0.87 (3)1.93 (3)2.799 (3)171 (3)
O10—H110···O1i0.82 (3)1.90 (3)2.721 (2)175 (3)
O10—H210···O9xiv0.86 (3)1.89 (3)2.754 (3)174 (3)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vii) x+1/2, y1/2, z; (xi) x+1/2, y+1/2, z+1; (xiv) x, y, z+1; (xvi) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (225K_anh) top
Crystal data top
C4H12KNaO10Dx = 1.794 Mg m3
Mr = 282.22Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 7210 reflections
a = 11.8339 (7) Åθ = 3.6–29.1°
b = 14.2248 (10) ŵ = 0.59 mm1
c = 6.2075 (4) ÅT = 225 K
V = 1044.95 (11) Å3Prism, clear colourless
Z = 40.48 × 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 Source2296 reflections with I 2u(I)
Graphite monochromatorRint = 0.054
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1819
Tmin = 0.813, Tmax = 1.000l = 88
18297 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.09Δρmax = 0.34 e Å3
2683 reflectionsΔρmin = 0.29 e Å3
195 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
1 restraintAbsolute structure parameter: 0.02 (2)
12 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00.00.0447 (3)0.0464 (6)
K20.50.00.15996 (10)0.02742 (16)
Na0.23198 (6)0.00678 (6)0.51893 (12)0.02257 (18)
O10.12022 (12)0.10904 (10)0.3487 (2)0.0217 (3)
O20.21106 (13)0.20321 (10)0.1184 (2)0.0256 (3)
O30.23056 (14)0.40678 (11)0.8164 (2)0.0308 (4)
O40.05075 (13)0.36049 (11)0.8464 (3)0.0290 (4)
O50.16440 (13)0.35756 (10)0.3243 (2)0.0222 (3)
H50.191 (2)0.3412 (18)0.216 (5)0.0334 (5)*
O60.29562 (13)0.24833 (11)0.6309 (3)0.0242 (3)
H60.326 (2)0.2911 (18)0.596 (5)0.0364 (5)*
O70.39599 (13)0.08277 (12)0.4853 (3)0.0277 (4)
H170.368 (2)0.132 (2)0.524 (5)0.0415 (5)*
H270.432 (2)0.094 (2)0.376 (5)0.0415 (5)*
O80.24058 (19)0.04148 (13)0.8821 (3)0.0402 (5)
H180.256 (3)0.003 (3)0.980 (5)0.0603 (7)*
H280.233 (3)0.093 (3)0.945 (5)0.0603 (7)*
O90.06010 (16)0.19468 (16)0.0333 (3)0.0423 (5)
H190.116 (3)0.209 (3)0.022 (6)0.0635 (7)*
H290.033 (3)0.253 (3)0.076 (5)0.0635 (7)*
O100.07703 (15)0.10474 (14)0.5747 (4)0.0410 (5)
H1100.016 (3)0.104 (2)0.515 (5)0.0615 (7)*
H2100.068 (3)0.136 (2)0.697 (6)0.0615 (7)*
C10.15477 (17)0.18783 (14)0.2835 (3)0.0175 (4)
C20.12525 (17)0.27350 (14)0.4229 (3)0.0179 (4)
H20.0399 (19)0.2789 (16)0.435 (3)0.0215 (5)*
C30.17758 (17)0.26360 (14)0.6464 (3)0.0187 (4)
H30.1462 (19)0.2079 (17)0.726 (4)0.0224 (5)*
C40.1508 (2)0.35089 (15)0.7822 (3)0.0224 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0544 (12)0.0455 (13)0.0393 (12)0.0248 (11)0.0000000.000000
K20.0276 (3)0.0305 (3)0.0241 (3)0.0037 (3)0.0000000.000000
Na0.0218 (4)0.0209 (4)0.0250 (4)0.0005 (3)0.0010 (3)0.0004 (4)
O10.0234 (7)0.0186 (7)0.0231 (7)0.0014 (6)0.0016 (6)0.0010 (6)
O20.0314 (8)0.0238 (8)0.0217 (8)0.0000 (7)0.0049 (7)0.0019 (6)
O30.0414 (9)0.0233 (8)0.0276 (8)0.0066 (7)0.0028 (8)0.0047 (7)
O40.0296 (8)0.0348 (9)0.0226 (8)0.0101 (7)0.0005 (7)0.0057 (7)
O50.0323 (9)0.0177 (7)0.0168 (7)0.0006 (6)0.0002 (7)0.0004 (6)
O60.0214 (8)0.0229 (8)0.0285 (8)0.0029 (6)0.0024 (7)0.0004 (7)
O70.0246 (8)0.0247 (9)0.0337 (9)0.0003 (6)0.0052 (7)0.0030 (7)
O80.0770 (14)0.0233 (8)0.0203 (9)0.0095 (9)0.0034 (9)0.0003 (7)
O90.0281 (9)0.0610 (13)0.0379 (11)0.0033 (9)0.0075 (8)0.0046 (10)
O100.0252 (8)0.0443 (11)0.0535 (12)0.0098 (8)0.0089 (8)0.0172 (9)
C10.0167 (10)0.0181 (10)0.0175 (10)0.0020 (8)0.0039 (8)0.0009 (8)
C20.0204 (10)0.0149 (10)0.0184 (9)0.0016 (8)0.0002 (8)0.0002 (8)
C30.0211 (10)0.0165 (10)0.0185 (10)0.0016 (8)0.0014 (8)0.0001 (8)
C40.0325 (12)0.0196 (10)0.0150 (10)0.0027 (9)0.0031 (9)0.0016 (8)
Geometric parameters (Å, º) top
K1—O12.8269 (18)Na—O72.3310 (17)
K1—O1i2.8269 (18)Na—O82.3586 (18)
K1—O8ii3.078 (2)Na—O102.3289 (19)
K1—O8iii3.078 (2)Na—C4v3.085 (2)
K1—H18iii3.06 (3)O1—C11.260 (2)
K1—H18ii3.06 (3)O2—C11.242 (2)
K1—O9i2.900 (2)O3—C41.252 (3)
K1—O92.900 (2)O4—C41.257 (3)
K1—O10ii3.400 (3)O5—H50.78 (3)
K1—O10iii3.400 (3)O5—C21.421 (3)
K1—H210ii3.01 (3)O6—H60.74 (2)
K1—H210iii3.01 (3)O6—C31.417 (2)
K2—O4iv2.8440 (16)O7—H170.81 (3)
K2—O4v2.8440 (16)O7—H270.82 (3)
K2—O5vi2.9885 (15)O8—H180.84 (4)
K2—O5vii2.9885 (15)O8—H280.84 (4)
K2—O7iii2.7840 (18)O9—H190.77 (4)
K2—O7viii2.7840 (18)O9—H290.92 (4)
K2—O8iii3.137 (2)O10—H1100.81 (3)
K2—O8viii3.137 (2)O10—H2100.89 (4)
K2—H18viii3.02 (3)C1—C21.535 (3)
K2—H18iii3.02 (3)C2—H21.02 (2)
Na—O12.3623 (17)C2—C31.526 (3)
Na—O3v2.4581 (18)C3—H31.00 (2)
Na—O5v2.4848 (17)C3—C41.534 (3)
Naii—K1—Naiii80.17 (4)O8viii—K2—O5vi122.54 (5)
O1—K1—Naii145.31 (3)O8iii—K2—O5vi61.24 (4)
O1i—K1—Naiii145.31 (3)O8viii—K2—O5vii61.24 (4)
O1—K1—Naiii101.50 (3)O8iii—K2—O7iii63.49 (5)
O1i—K1—Naii101.50 (3)O8viii—K2—O7viii63.49 (5)
O1i—K1—O196.24 (8)O8iii—K2—O7viii125.31 (5)
O8ii—K1—Naiii109.87 (6)O8viii—K2—O7iii125.31 (5)
O8ii—K1—Naii32.66 (4)O8viii—K2—O8iii170.46 (6)
O8iii—K1—Naii109.87 (6)H18iii—K2—Naviii164.5 (6)
O8iii—K1—Naiii32.66 (4)H18viii—K2—Naviii49.0 (6)
O8ii—K1—O1142.16 (5)H18iii—K2—Naiii49.0 (6)
O8iii—K1—O1i142.16 (5)H18viii—K2—Naiii164.5 (6)
O8iii—K1—O169.41 (4)H18iii—K2—O4iv89.6 (7)
O8ii—K1—O1i69.41 (4)H18viii—K2—O4v89.6 (7)
O8ii—K1—O8iii141.70 (9)H18iii—K2—O4v67.1 (7)
H18iii—K1—Naii122.5 (6)H18viii—K2—O4iv67.1 (7)
H18ii—K1—Naii42.5 (6)H18iii—K2—O5vi59.1 (7)
H18iii—K1—Naiii42.5 (6)H18viii—K2—O5vi135.3 (7)
H18ii—K1—Naiii122.5 (6)H18viii—K2—O5vii59.1 (7)
H18iii—K1—O1i126.5 (7)H18iii—K2—O5vii135.3 (7)
H18ii—K1—O1i65.2 (6)H18iii—K2—O7iii78.4 (7)
H18ii—K1—O1126.5 (7)H18viii—K2—O7viii78.4 (7)
H18iii—K1—O165.2 (6)H18iii—K2—O7viii131.2 (6)
H18ii—K1—O8ii15.7 (7)H18viii—K2—O7iii131.2 (6)
H18iii—K1—O8iii15.7 (7)H18iii—K2—O8viii156.3 (7)
H18ii—K1—O8iii151.3 (6)H18viii—K2—O8viii15.5 (7)
H18iii—K1—O8ii151.3 (6)H18iii—K2—O8iii15.5 (7)
H18ii—K1—H18iii165.0 (12)H18viii—K2—O8iii156.3 (7)
O9—K1—Naiii72.11 (5)H18viii—K2—H18iii146.4 (12)
O9i—K1—Naii72.11 (5)K2ix—Na—K1x97.88 (2)
O9—K1—Naii92.96 (5)O1—Na—K1x88.06 (4)
O9i—K1—Naiii92.96 (5)O1—Na—K2ix133.93 (5)
O9—K1—O1i73.20 (5)O3v—Na—K1x140.84 (5)
O9i—K1—O173.20 (5)O3v—Na—K2ix108.11 (5)
O9—K1—O1120.80 (6)O3v—Na—O194.07 (6)
O9i—K1—O1i120.80 (6)O5v—Na—K1x92.04 (4)
O9—K1—O8iii84.34 (5)O5v—Na—K2ix52.70 (4)
O9i—K1—O8iii89.37 (5)O5v—Na—O1173.28 (6)
O9—K1—O8ii89.37 (5)O5v—Na—O3v81.62 (6)
O9i—K1—O8ii84.34 (5)O7—Na—K1x126.30 (5)
O9—K1—H18iii75.5 (7)O7—Na—K2ix47.84 (4)
O9i—K1—H18ii75.5 (7)O7—Na—O192.57 (6)
O9—K1—H18ii101.9 (7)O7—Na—O3v92.71 (7)
O9i—K1—H18iii101.9 (7)O7—Na—O5v92.78 (6)
O9i—K1—O9160.77 (11)O8—Na—K1x44.76 (6)
O10ii—K1—Naii32.98 (3)O8—Na—K2ix56.47 (6)
O10iii—K1—Naiii32.98 (3)O8—Na—O1104.39 (7)
O10ii—K1—Naiii61.71 (4)O8—Na—O3v161.31 (7)
O10iii—K1—Naii61.71 (4)O8—Na—O5v80.24 (6)
O10iii—K1—O1i117.86 (5)O8—Na—O783.72 (7)
O10ii—K1—O1i132.71 (4)O10—Na—K1x52.63 (6)
O10ii—K1—O1117.86 (5)O10—Na—K2ix127.06 (6)
O10iii—K1—O1132.71 (4)O10—Na—O192.47 (7)
O10iii—K1—O8ii83.25 (6)O10—Na—O3v88.21 (8)
O10iii—K1—O8iii63.55 (5)O10—Na—O5v82.28 (7)
O10ii—K1—O8iii83.25 (6)O10—Na—O7174.80 (8)
O10ii—K1—O8ii63.55 (5)O10—Na—O893.78 (8)
O10iii—K1—H18iii68.2 (6)C4v—Na—K1x140.15 (5)
O10ii—K1—H18ii68.2 (6)C4v—Na—K2ix87.63 (5)
O10iii—K1—H18ii98.4 (6)C4v—Na—O1116.01 (6)
O10ii—K1—H18iii98.4 (6)C4v—Na—O3v22.70 (5)
O10iii—K1—O951.13 (6)C4v—Na—O5v60.38 (5)
O10ii—K1—O9i51.13 (6)C4v—Na—O785.99 (7)
O10iii—K1—O9i109.93 (7)C4v—Na—O8138.65 (7)
O10ii—K1—O9109.93 (7)C4v—Na—O1092.95 (7)
O10ii—K1—O10iii61.82 (7)Na—O1—K1101.40 (5)
H210iii—K1—Naii68.9 (7)C1—O1—K1115.91 (13)
H210ii—K1—Naii42.7 (6)C1—O1—Na125.63 (12)
H210iii—K1—Naiii42.7 (6)C4—O3—Naxi108.03 (13)
H210ii—K1—Naiii68.9 (7)C4—O4—K2xii119.46 (14)
H210ii—K1—O1i134.2 (6)Naxi—O5—K2xiii85.90 (5)
H210iii—K1—O1134.2 (6)H5—O5—K2xiii100 (2)
H210ii—K1—O1105.0 (7)H5—O5—Naxi112 (2)
H210iii—K1—O1i105.0 (7)C2—O5—K2xiii120.35 (11)
H210iii—K1—O8ii83.7 (6)C2—O5—Naxi130.23 (12)
H210ii—K1—O8ii68.9 (6)C2—O5—H5105 (2)
H210iii—K1—O8iii68.9 (6)C3—O6—H6112 (2)
H210ii—K1—O8iii83.7 (6)Na—O7—K2xiv93.79 (6)
H210ii—K1—H18ii69.5 (9)H17—O7—K2xiv108 (2)
H210iii—K1—H18iii69.5 (9)H17—O7—Na96 (2)
H210ii—K1—H18iii99.3 (9)H27—O7—K2xiv121 (2)
H210iii—K1—H18ii99.3 (9)H27—O7—Na128 (2)
H210iii—K1—O9i124.2 (7)H27—O7—H17107 (3)
H210ii—K1—O9i36.8 (7)K2xiv—O8—K1xiv153.69 (7)
H210iii—K1—O936.8 (7)Na—O8—K1xiv102.58 (8)
H210ii—K1—O9124.2 (7)Na—O8—K2xiv84.72 (6)
H210iii—K1—O10ii74.9 (7)H18—O8—K1xiv81 (2)
H210iii—K1—O10iii14.4 (7)H18—O8—K2xiv74 (2)
H210ii—K1—O10iii74.9 (7)H18—O8—Na121 (2)
H210ii—K1—O10ii14.4 (7)H28—O8—K1xiv85 (2)
H210ii—K1—H210iii88.5 (14)H28—O8—K2xiv108 (2)
Naviii—K2—Naiii115.73 (3)H28—O8—Na134 (2)
O4v—K2—Naviii124.11 (4)H28—O8—H18105 (3)
O4iv—K2—Naviii99.63 (3)K2xiv—H18—K1xiv170.6 (12)
O4iv—K2—Naiii124.11 (4)O8—H18—K1xiv84 (2)
O4v—K2—Naiii99.63 (3)O8—H18—K2xiv90 (2)
O4v—K2—O4iv93.61 (7)H19—O9—K1i112 (3)
O5vi—K2—Naiii41.40 (3)H29—O9—K1i145 (2)
O5vi—K2—Naviii112.76 (4)H29—O9—H19101 (3)
O5vii—K2—Naviii41.40 (3)Na—O10—K1x94.39 (7)
O5vii—K2—Naiii112.76 (4)H110—O10—K1x99 (2)
O5vi—K2—O4v67.86 (4)H110—O10—Na129 (2)
O5vi—K2—O4iv147.59 (5)H210—O10—K1x57 (2)
O5vii—K2—O4v147.59 (5)H210—O10—Na121 (2)
O5vii—K2—O4iv67.86 (4)H210—O10—H110107 (3)
O5vi—K2—O5vii140.08 (7)O10—H210—K1x108 (2)
O7iii—K2—Naiii38.37 (3)O2—C1—O1126.6 (2)
O7viii—K2—Naiii86.71 (4)C2—C1—O1116.83 (18)
O7iii—K2—Naviii86.71 (4)C2—C1—O2116.58 (18)
O7viii—K2—Naviii38.37 (3)C1—C2—O5110.57 (16)
O7iii—K2—O4iv109.86 (5)H2—C2—O5106.9 (13)
O7iii—K2—O4v138.00 (5)H2—C2—C1109.1 (13)
O7viii—K2—O4iv138.00 (5)C3—C2—O5109.68 (16)
O7viii—K2—O4v109.86 (5)C3—C2—C1110.30 (16)
O7iii—K2—O5vi74.27 (5)C3—C2—H2110.2 (12)
O7viii—K2—O5vii74.27 (5)C2—C3—O6110.66 (17)
O7iii—K2—O5vii74.40 (5)H3—C3—O6106.1 (13)
O7viii—K2—O5vi74.40 (5)H3—C3—C2111.6 (13)
O7viii—K2—O7iii75.44 (7)C4—C3—O6111.40 (17)
O8iii—K2—Naviii150.19 (4)C4—C3—C2109.95 (16)
O8viii—K2—Naviii38.81 (3)C4—C3—H3107.1 (13)
O8iii—K2—Naiii38.81 (3)O3—C4—Naxi49.26 (11)
O8viii—K2—Naiii150.19 (4)O4—C4—Naxi122.99 (15)
O8iii—K2—O4iv91.06 (5)O4—C4—O3126.0 (2)
O8viii—K2—O4v91.06 (5)C3—C4—Naxi96.06 (12)
O8iii—K2—O4v82.40 (5)C3—C4—O3116.9 (2)
O8viii—K2—O4iv82.40 (5)C3—C4—O4117.17 (19)
O8iii—K2—O5vii122.54 (5)
K1—O1—C1—O251.98 (14)Naxi—O3—C4—C373.73 (13)
K1i—O1—C1—O251.98 (14)Naxi—O5—C2—C1134.18 (16)
K1—O1—C1—C2128.55 (12)Naxi—O5—C2—C312.33 (15)
K1i—O1—C1—C2128.55 (12)Naxi—C4—C3—O662.88 (12)
K2xii—O4—C4—Naxi72.79 (12)Naxi—C4—C3—C260.17 (12)
K2—O4v—C4v—Na72.79 (12)O1—C1—C2—O5176.99 (18)
K2xii—O4—C4—O312.15 (16)O1—C1—C2—C361.52 (19)
K2xi—O4—C4—O312.15 (16)O2—C1—C2—O53.49 (19)
K2xii—O4—C4—C3168.87 (13)O2—C1—C2—C3118.00 (19)
K2xi—O4—C4—C3168.87 (13)O3—C4—C3—O615.9 (2)
K2xv—O5—C2—C1113.07 (13)O3—C4—C3—C2107.2 (2)
K2xiii—O5—C2—C1113.07 (13)O4—C4—C3—O6165.06 (19)
K2xiii—O5—C2—C3125.08 (13)O4—C4—C3—C271.9 (2)
K2xv—O5—C2—C3125.08 (13)O5—C2—C3—O667.28 (17)
Na—O1—C1—O276.22 (16)O5—C2—C3—C456.20 (18)
Na—O1—C1—C2103.25 (15)O6—C3—C2—C154.74 (18)
Naxi—O3—C4—O4105.24 (14)C1—C2—C3—C4178.22 (16)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y1/2, z; (vii) x+1/2, y+1/2, z; (viii) x+1, y, z1; (ix) x+1, y, z+1; (x) x, y, z+1; (xi) x+1/2, y+1/2, z+1; (xii) x1/2, y+1/2, z+1; (xiii) x1/2, 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···AD—HH···AD···AD—H···A
O5—H5···O20.78 (3)2.07 (3)2.600 (2)126 (2)
O5—H5···O3iii0.78 (3)2.69 (3)3.323 (2)140 (2)
O5—H5···O4iii0.78 (3)2.85 (3)3.258 (2)115 (2)
O6—H6···O10xi0.74 (2)2.16 (2)2.876 (3)166 (3)
O7—H17···O60.81 (3)1.98 (3)2.788 (2)177 (3)
O7—H27···O4iv0.82 (3)2.07 (3)2.871 (2)165 (3)
O8—H18···O3xvi0.84 (4)1.87 (4)2.700 (2)170 (3)
O8—H28···O1xiv0.84 (4)2.85 (3)3.368 (2)122 (3)
O8—H28···O2xiv0.84 (4)1.92 (4)2.751 (2)173 (3)
O9—H19···O2vi0.77 (4)2.55 (4)3.118 (3)131 (3)
O9—H19···O3v0.77 (4)2.64 (4)3.168 (3)127 (3)
O9—H19···O6v0.77 (4)2.47 (4)3.132 (2)145 (3)
O9—H29···O4ii0.92 (4)1.89 (4)2.800 (3)169 (3)
O10—H110···O1i0.81 (3)1.92 (3)2.724 (2)174 (3)
O10—H210···O9xiv0.89 (4)1.87 (4)2.756 (3)174 (3)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y1/2, z; (xi) x+1/2, y+1/2, z+1; (xiv) x, y, z+1; (xvi) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (243K_anh) top
Crystal data top
C4H12KNaO10Dx = 1.790 Mg m3
Mr = 282.22Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 6951 reflections
a = 11.8443 (8) Åθ = 3.6–28.8°
b = 14.2331 (10) ŵ = 0.59 mm1
c = 6.2124 (4) ÅT = 243 K
V = 1047.29 (12) Å3Prism, clear colourless
Z = 40.48 × 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 Source2274 reflections with I 2u(I)
Graphite monochromatorRint = 0.054
Detector resolution: 10.3457 pixels mm-1θmax = 29.5°, θmin = 3.3°
ω scansh = 1616
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 = 1819
Tmin = 0.811, Tmax = 1.000l = 88
18296 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.08Δρmax = 0.34 e Å3
2687 reflectionsΔρmin = 0.29 e Å3
195 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
1 restraintAbsolute structure parameter: 0.05 (2)
12 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00.00.0451 (3)0.0500 (6)
K20.50.00.15966 (11)0.02969 (17)
Na0.23187 (7)0.00679 (7)0.51990 (13)0.02440 (19)
O10.12024 (12)0.10902 (10)0.3492 (3)0.0233 (3)
O20.21069 (14)0.20309 (11)0.1184 (2)0.0274 (4)
O30.23130 (15)0.40654 (11)0.8157 (3)0.0329 (4)
O40.05150 (14)0.36101 (12)0.8458 (3)0.0313 (4)
O50.16404 (14)0.35750 (11)0.3243 (3)0.0242 (3)
H50.192 (2)0.3414 (19)0.216 (5)0.0363 (5)*
O60.29559 (13)0.24821 (11)0.6299 (3)0.0264 (4)
H60.325 (2)0.2918 (19)0.603 (5)0.0396 (5)*
O70.39591 (14)0.08259 (12)0.4849 (3)0.0300 (4)
H170.372 (3)0.131 (2)0.522 (5)0.0451 (6)*
H270.432 (2)0.093 (2)0.374 (5)0.0451 (6)*
O80.24132 (19)0.04137 (14)0.8827 (3)0.0423 (5)
H180.257 (3)0.003 (3)0.982 (5)0.0634 (8)*
H280.235 (3)0.095 (3)0.948 (5)0.0634 (8)*
O90.06040 (16)0.19537 (17)0.0337 (4)0.0470 (5)
H190.117 (3)0.213 (3)0.020 (6)0.0705 (8)*
H290.032 (3)0.253 (3)0.082 (5)0.0705 (8)*
O100.07659 (16)0.10432 (15)0.5760 (4)0.0457 (5)
H1100.016 (3)0.105 (3)0.517 (5)0.0685 (8)*
H2100.068 (3)0.135 (3)0.697 (6)0.0685 (8)*
C10.15470 (18)0.18783 (15)0.2835 (3)0.0195 (4)
C20.12510 (18)0.27339 (15)0.4227 (3)0.0193 (4)
H20.0398 (19)0.2778 (17)0.436 (4)0.0231 (5)*
C30.17773 (17)0.26371 (15)0.6463 (4)0.0203 (4)
H30.147 (2)0.2090 (18)0.723 (4)0.0244 (5)*
C40.1515 (2)0.35106 (16)0.7811 (3)0.0240 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0580 (13)0.0491 (14)0.0429 (13)0.0267 (12)0.0000000.000000
K20.0296 (3)0.0331 (4)0.0263 (3)0.0038 (3)0.0000000.000000
Na0.0235 (4)0.0227 (4)0.0270 (4)0.0009 (4)0.0008 (3)0.0007 (4)
O10.0257 (8)0.0190 (7)0.0252 (8)0.0005 (6)0.0013 (7)0.0011 (7)
O20.0357 (9)0.0247 (8)0.0218 (8)0.0008 (7)0.0060 (7)0.0017 (6)
O30.0431 (10)0.0260 (8)0.0298 (9)0.0072 (7)0.0034 (8)0.0057 (7)
O40.0320 (8)0.0370 (9)0.0249 (8)0.0104 (7)0.0010 (7)0.0058 (8)
O50.0350 (9)0.0185 (8)0.0190 (8)0.0005 (6)0.0007 (7)0.0005 (6)
O60.0231 (8)0.0234 (8)0.0328 (9)0.0033 (6)0.0039 (7)0.0004 (7)
O70.0265 (9)0.0265 (9)0.0372 (10)0.0011 (7)0.0058 (8)0.0013 (8)
O80.0792 (15)0.0247 (9)0.0229 (9)0.0094 (10)0.0036 (10)0.0008 (7)
O90.0299 (10)0.0697 (15)0.0413 (12)0.0051 (10)0.0090 (9)0.0054 (11)
O100.0279 (9)0.0492 (12)0.0599 (14)0.0119 (9)0.0111 (9)0.0218 (10)
C10.0192 (10)0.0196 (11)0.0198 (10)0.0017 (8)0.0050 (8)0.0010 (8)
C20.0220 (10)0.0166 (10)0.0191 (10)0.0007 (8)0.0013 (9)0.0009 (8)
C30.0216 (10)0.0190 (10)0.0204 (10)0.0016 (8)0.0012 (9)0.0024 (9)
C40.0347 (13)0.0218 (11)0.0156 (10)0.0040 (10)0.0039 (9)0.0003 (8)
Geometric parameters (Å, º) top
K1—O12.8293 (19)Na—O72.3325 (18)
K1—O1i2.8293 (19)Na—O82.3586 (19)
K1—O8ii3.088 (2)Na—O102.330 (2)
K1—O8iii3.088 (2)Na—C4v3.082 (2)
K1—H18ii3.07 (3)O1—C11.261 (3)
K1—H18iii3.07 (3)O2—C11.241 (3)
K1—O9i2.913 (3)O3—C41.250 (3)
K1—O92.913 (3)O4—C41.259 (3)
K1—O10ii3.394 (3)O5—H50.78 (3)
K1—O10iii3.394 (3)O5—C21.421 (3)
K1—H210iii3.01 (3)O6—H60.73 (2)
K1—H210ii3.01 (3)O6—C31.417 (3)
K2—O4iv2.8438 (17)O7—H170.78 (3)
K2—O4v2.8438 (17)O7—H270.82 (3)
K2—O5vi2.9890 (16)O8—H180.84 (4)
K2—O5vii2.9890 (16)O8—H280.87 (4)
K2—O7ii2.7890 (19)O9—H190.78 (4)
K2—O7viii2.7890 (19)O9—H290.93 (4)
K2—O8ii3.131 (2)O10—H1100.80 (4)
K2—O8viii3.131 (2)O10—H2100.88 (4)
K2—H18ii3.01 (3)C1—C21.534 (3)
K2—H18viii3.01 (3)C2—H21.02 (2)
Na—O12.3643 (17)C2—C31.529 (3)
Na—O3v2.4612 (19)C3—H30.98 (3)
Na—O5v2.4876 (18)C3—C41.531 (3)
Naiii—K1—Naii80.22 (4)O8ii—K2—O5vi122.50 (5)
O1—K1—Naii101.48 (3)O8ii—K2—O5vii61.33 (5)
O1—K1—Naiii145.32 (3)O8viii—K2—O5vii122.50 (5)
O1i—K1—Naii145.32 (3)O8ii—K2—O7ii63.56 (5)
O1i—K1—Naiii101.48 (3)O8ii—K2—O7viii125.34 (5)
O1i—K1—O196.22 (8)O8viii—K2—O7viii63.56 (5)
O8iii—K1—Naiii32.70 (4)O8viii—K2—O7ii125.34 (5)
O8ii—K1—Naii32.70 (4)O8viii—K2—O8ii170.35 (7)
O8iii—K1—Naii109.99 (6)H18viii—K2—Naviii49.2 (6)
O8ii—K1—Naiii109.99 (6)H18viii—K2—Naii164.8 (7)
O8iii—K1—O1142.06 (6)H18ii—K2—Naviii164.8 (7)
O8ii—K1—O169.36 (5)H18ii—K2—Naii49.2 (6)
O8ii—K1—O1i142.06 (6)H18ii—K2—O4iv89.6 (7)
O8iii—K1—O1i69.36 (5)H18ii—K2—O4v66.7 (7)
O8iii—K1—O8ii141.87 (9)H18viii—K2—O4v89.6 (7)
H18ii—K1—Naii42.7 (6)H18viii—K2—O4iv66.7 (7)
H18iii—K1—Naii122.7 (6)H18ii—K2—O5vii59.3 (7)
H18iii—K1—Naiii42.7 (6)H18ii—K2—O5vi135.3 (8)
H18ii—K1—Naiii122.7 (6)H18viii—K2—O5vi59.3 (7)
H18ii—K1—O1i126.3 (7)H18viii—K2—O5vii135.3 (8)
H18iii—K1—O1126.3 (7)H18ii—K2—O7ii78.6 (7)
H18iii—K1—O1i65.0 (7)H18ii—K2—O7viii131.4 (7)
H18ii—K1—O165.0 (7)H18viii—K2—O7viii78.6 (7)
H18iii—K1—O8iii15.7 (7)H18viii—K2—O7ii131.4 (7)
H18ii—K1—O8iii151.6 (6)H18ii—K2—O8viii156.0 (7)
H18iii—K1—O8ii151.6 (6)H18ii—K2—O8ii15.6 (7)
H18ii—K1—O8ii15.7 (7)H18viii—K2—O8ii156.0 (7)
H18iii—K1—H18ii165.4 (13)H18viii—K2—O8viii15.6 (7)
O9—K1—Naiii92.94 (6)H18viii—K2—H18ii146.0 (13)
O9—K1—Naii72.05 (5)K2ix—Na—K1x97.97 (3)
O9i—K1—Naiii72.05 (5)O1—Na—K1x88.12 (4)
O9i—K1—Naii92.94 (6)O1—Na—K2ix133.94 (5)
O9—K1—O1i73.27 (5)O3v—Na—K1x140.65 (5)
O9—K1—O1120.80 (6)O3v—Na—K2ix108.21 (5)
O9i—K1—O173.27 (5)O3v—Na—O193.93 (6)
O9i—K1—O1i120.80 (6)O5v—Na—K1x92.24 (5)
O9—K1—O8ii84.25 (6)O5v—Na—K2ix52.67 (4)
O9—K1—O8iii89.46 (6)O5v—Na—O1173.25 (6)
O9i—K1—O8ii89.46 (6)O5v—Na—O3v81.52 (6)
O9i—K1—O8iii84.25 (6)O7—Na—K1x126.54 (6)
O9—K1—H18ii75.5 (7)O7—Na—K2ix47.93 (5)
O9—K1—H18iii102.0 (7)O7—Na—O192.51 (7)
O9i—K1—H18iii75.5 (7)O7—Na—O3v92.67 (7)
O9i—K1—H18ii102.0 (7)O7—Na—O5v92.69 (6)
O9i—K1—O9160.67 (12)O8—Na—K1x45.01 (6)
O10ii—K1—Naii33.00 (4)O8—Na—K2ix56.28 (6)
O10ii—K1—Naiii61.66 (4)O8—Na—O1104.64 (7)
O10iii—K1—Naiii33.00 (4)O8—Na—O3v161.20 (7)
O10iii—K1—Naii61.66 (4)O8—Na—O5v80.22 (7)
O10ii—K1—O1i117.90 (5)O8—Na—O783.75 (8)
O10iii—K1—O1117.90 (5)O10—Na—K1x52.49 (6)
O10iii—K1—O1i132.74 (5)O10—Na—K2ix127.19 (6)
O10ii—K1—O1132.74 (5)O10—Na—O192.35 (7)
O10ii—K1—O8iii83.31 (6)O10—Na—O3v88.16 (8)
O10iii—K1—O8ii83.31 (6)O10—Na—O5v82.56 (7)
O10ii—K1—O8ii63.61 (5)O10—Na—O7175.00 (8)
O10iii—K1—O8iii63.61 (5)O10—Na—O893.89 (8)
O10ii—K1—H18ii68.4 (6)C4v—Na—K1x140.13 (5)
O10ii—K1—H18iii98.6 (7)C4v—Na—K2ix87.67 (5)
O10iii—K1—H18iii68.4 (6)C4v—Na—O1115.86 (6)
O10iii—K1—H18ii98.6 (7)C4v—Na—O3v22.73 (6)
O10ii—K1—O951.14 (6)C4v—Na—O5v60.27 (6)
O10ii—K1—O9i109.82 (8)C4v—Na—O785.87 (7)
O10iii—K1—O9i51.14 (6)C4v—Na—O8138.53 (7)
O10iii—K1—O9109.82 (8)C4v—Na—O1093.06 (8)
O10iii—K1—O10ii61.68 (8)Na—O1—K1101.46 (6)
H210iii—K1—Naiii42.5 (7)C1—O1—K1115.76 (14)
H210iii—K1—Naii68.8 (7)C1—O1—Na125.74 (13)
H210ii—K1—Naiii68.8 (7)C4—O3—Naxi107.76 (14)
H210ii—K1—Naii42.5 (7)C4—O4—K2xii119.94 (14)
H210ii—K1—O1i105.3 (7)Naxi—O5—K2xiii85.90 (5)
H210iii—K1—O1i134.1 (7)H5—O5—K2xiii100 (2)
H210iii—K1—O1105.3 (7)H5—O5—Naxi111 (2)
H210ii—K1—O1134.1 (7)C2—O5—K2xiii120.52 (12)
H210iii—K1—O8ii83.8 (7)C2—O5—Naxi130.37 (13)
H210ii—K1—O8iii83.8 (7)C2—O5—H5105 (2)
H210ii—K1—O8ii68.8 (7)C3—O6—H6111 (2)
H210iii—K1—O8iii68.8 (7)Na—O7—K2xiv93.70 (6)
H210iii—K1—H18iii69.6 (9)H17—O7—K2xiv107 (2)
H210iii—K1—H18ii99.6 (10)H17—O7—Na98 (2)
H210ii—K1—H18ii69.6 (9)H27—O7—K2xiv120 (2)
H210ii—K1—H18iii99.6 (10)H27—O7—Na127 (2)
H210iii—K1—O9123.9 (7)H27—O7—H17107 (3)
H210ii—K1—O9i123.9 (7)K2xiv—O8—K1xiv153.83 (7)
H210ii—K1—O937.0 (7)Na—O8—K1xiv102.29 (8)
H210iii—K1—O9i37.0 (7)Na—O8—K2xiv84.92 (6)
H210ii—K1—O10iii74.6 (7)H18—O8—K1xiv81 (2)
H210iii—K1—O10iii14.2 (7)H18—O8—K2xiv74 (2)
H210ii—K1—O10ii14.2 (7)H18—O8—Na122 (2)
H210iii—K1—O10ii74.6 (7)H28—O8—K1xiv86 (2)
H210iii—K1—H210ii88.1 (15)H28—O8—K2xiv107 (2)
Naviii—K2—Naii115.86 (3)H28—O8—Na134 (2)
O4iv—K2—Naii124.31 (4)H28—O8—H18104 (3)
O4v—K2—Naii99.46 (4)K2xiv—H18—K1xiv170.1 (13)
O4iv—K2—Naviii99.46 (4)O8—H18—K1xiv83 (2)
O4v—K2—Naviii124.31 (4)O8—H18—K2xiv90 (2)
O4v—K2—O4iv93.43 (7)H19—O9—K1i116 (3)
O5vi—K2—Naviii41.43 (3)H29—O9—K1i143 (2)
O5vi—K2—Naii112.73 (4)H29—O9—H19100 (4)
O5vii—K2—Naviii112.73 (4)Na—O10—K1x94.51 (8)
O5vii—K2—Naii41.43 (3)H110—O10—K1x99 (2)
O5vii—K2—O4v67.86 (5)H110—O10—Na130 (2)
O5vi—K2—O4v147.78 (5)H210—O10—K1x57 (2)
O5vii—K2—O4iv147.78 (5)H210—O10—Na121 (2)
O5vi—K2—O4iv67.86 (5)H210—O10—H110106 (3)
O5vii—K2—O5vi139.99 (7)O10—H210—K1x109 (3)
O7viii—K2—Naii86.74 (4)O2—C1—O1126.6 (2)
O7viii—K2—Naviii38.37 (4)C2—C1—O1116.72 (19)
O7ii—K2—Naii38.37 (4)C2—C1—O2116.69 (19)
O7ii—K2—Naviii86.74 (4)C1—C2—O5110.62 (17)
O7ii—K2—O4iv110.15 (5)H2—C2—O5107.8 (13)
O7viii—K2—O4iv137.84 (5)H2—C2—C1108.8 (13)
O7ii—K2—O4v137.84 (5)C3—C2—O5109.53 (17)
O7viii—K2—O4v110.15 (5)C3—C2—C1110.33 (17)
O7ii—K2—O5vii74.20 (5)C3—C2—H2109.7 (13)
O7viii—K2—O5vii74.36 (5)C2—C3—O6110.50 (18)
O7ii—K2—O5vi74.36 (5)H3—C3—O6105.8 (14)
O7viii—K2—O5vi74.20 (5)H3—C3—C2111.2 (14)
O7viii—K2—O7ii75.29 (8)C4—C3—O6111.46 (18)
O8viii—K2—Naviii38.80 (3)C4—C3—C2109.93 (17)
O8viii—K2—Naii150.31 (4)C4—C3—H3107.8 (14)
O8ii—K2—Naviii150.31 (4)O3—C4—Naxi49.51 (11)
O8ii—K2—Naii38.80 (3)O4—C4—Naxi122.80 (15)
O8viii—K2—O4iv82.14 (5)O4—C4—O3125.8 (2)
O8ii—K2—O4iv91.23 (5)C3—C4—Naxi96.34 (13)
O8ii—K2—O4v82.14 (5)C3—C4—O3117.0 (2)
O8viii—K2—O4v91.23 (5)C3—C4—O4117.2 (2)
O8viii—K2—O5vi61.33 (5)
K1—O1—C1—O251.92 (15)Naxi—O3—C4—C374.26 (13)
K1i—O1—C1—O251.92 (15)Naxi—O5—C2—C1133.88 (17)
K1—O1—C1—C2128.54 (13)Naxi—O5—C2—C312.06 (15)
K1i—O1—C1—C2128.54 (13)Naxi—C4—C3—O662.75 (13)
K2xii—O4—C4—Naxi72.84 (13)Naxi—C4—C3—C260.13 (13)
K2—O4v—C4v—Na72.84 (13)O1—C1—C2—O5177.04 (18)
K2xii—O4—C4—O312.01 (17)O1—C1—C2—C361.6 (2)
K2xi—O4—C4—O312.01 (17)O2—C1—C2—O53.4 (2)
K2xii—O4—C4—C3168.54 (14)O2—C1—C2—C3118.0 (2)
K2xi—O4—C4—C3168.54 (14)O3—C4—C3—O615.3 (2)
K2xv—O5—C2—C1113.04 (14)O3—C4—C3—C2107.6 (2)
K2xiii—O5—C2—C1113.04 (14)O4—C4—C3—O6165.2 (2)
K2xiii—O5—C2—C3125.13 (14)O4—C4—C3—C271.9 (2)
K2xv—O5—C2—C3125.13 (14)O5—C2—C3—O667.58 (17)
Na—O1—C1—O276.32 (17)O5—C2—C3—C455.86 (18)
Na—O1—C1—C2103.22 (16)O6—C3—C2—C154.42 (19)
Naxi—O3—C4—O4105.20 (14)C1—C2—C3—C4177.86 (17)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y+1/2, z; (vii) x+1/2, y1/2, z; (viii) x+1, y, z1; (ix) x+1, y, z+1; (x) x, y, z+1; (xi) x+1/2, y+1/2, z+1; (xii) x1/2, y+1/2, z+1; (xiii) x1/2, 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···AD—HH···AD···AD—H···A
O5—H5···O20.78 (3)2.07 (3)2.602 (2)125 (3)
O5—H5···O3ii0.78 (3)2.69 (3)3.333 (2)140 (2)
O5—H5···O4ii0.78 (3)2.85 (3)3.258 (2)115 (2)
O6—H6···O10xi0.73 (2)2.19 (3)2.887 (3)161 (3)
O7—H17···O60.78 (3)2.02 (3)2.789 (2)174 (3)
O7—H27···O4iv0.82 (3)2.08 (3)2.874 (2)164 (3)
O8—H18···O3xvi0.84 (4)1.87 (4)2.702 (2)170 (3)
O8—H28···O1xiv0.87 (4)2.85 (3)3.373 (2)121 (3)
O8—H28···O2xiv0.87 (4)1.89 (4)2.752 (2)172 (3)
O9—H19···O2vii0.78 (4)2.52 (4)3.117 (3)134 (3)
O9—H19···O3v0.78 (4)2.67 (4)3.166 (3)122 (3)
O9—H19···O6v0.78 (4)2.47 (4)3.138 (3)143 (4)
O9—H29···O4iii0.93 (4)1.89 (4)2.806 (3)169 (3)
O10—H110···O1i0.80 (4)1.93 (4)2.725 (2)174 (3)
O10—H210···O9xiv0.88 (4)1.88 (4)2.756 (3)175 (3)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vii) x+1/2, y1/2, z; (xi) x+1/2, y+1/2, z+1; (xiv) x, y, z+1; (xvi) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (253K_anh) top
Crystal data top
C4H12KNaO10Dx = 1.788 Mg m3
Mr = 282.22Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 6895 reflections
a = 11.8510 (8) Åθ = 3.6–28.8°
b = 14.239 (1) ŵ = 0.59 mm1
c = 6.2146 (4) ÅT = 253 K
V = 1048.70 (12) Å3Prism, clear colourless
Z = 40.48 × 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 Source2260 reflections with I 2u(I)
Graphite monochromatorRint = 0.055
Detector resolution: 10.3457 pixels mm-1θmax = 29.5°, θmin = 3.3°
ω scansh = 1616
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 = 1819
Tmin = 0.787, Tmax = 1.000l = 88
18338 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.08Δρmax = 0.36 e Å3
2690 reflectionsΔρmin = 0.30 e Å3
195 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
1 restraintAbsolute structure parameter: 0.05 (2)
12 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00.00.0455 (3)0.0523 (6)
K20.50.00.15963 (11)0.03088 (17)
Na0.23176 (7)0.00680 (7)0.52026 (13)0.02556 (19)
O10.12015 (12)0.10898 (10)0.3495 (3)0.0243 (3)
O20.21038 (14)0.20310 (11)0.1184 (2)0.0290 (4)
O30.23176 (15)0.40646 (11)0.8152 (3)0.0346 (4)
O40.05192 (14)0.36127 (12)0.8454 (3)0.0331 (4)
O50.16381 (14)0.35756 (11)0.3242 (3)0.0254 (3)
H50.191 (2)0.3417 (19)0.214 (5)0.0381 (5)*
O60.29556 (13)0.24818 (11)0.6295 (3)0.0273 (4)
H60.326 (2)0.2918 (19)0.604 (5)0.0409 (5)*
O70.39576 (14)0.08270 (12)0.4846 (3)0.0312 (4)
H170.368 (3)0.131 (2)0.524 (5)0.0468 (6)*
H270.432 (2)0.092 (2)0.376 (5)0.0468 (6)*
O80.2418 (2)0.04136 (14)0.8833 (3)0.0448 (5)
H180.255 (3)0.004 (3)0.982 (5)0.0672 (8)*
H280.234 (3)0.096 (3)0.948 (5)0.0672 (8)*
O90.06062 (16)0.19594 (18)0.0342 (4)0.0494 (5)
H190.116 (3)0.215 (3)0.014 (6)0.0740 (8)*
H290.033 (3)0.253 (3)0.080 (5)0.0740 (8)*
O100.07634 (16)0.10383 (15)0.5769 (4)0.0488 (5)
H1100.015 (3)0.103 (3)0.520 (5)0.0732 (8)*
H2100.067 (3)0.137 (3)0.697 (6)0.0732 (8)*
C10.15472 (17)0.18782 (15)0.2841 (3)0.0206 (4)
C20.12520 (17)0.27337 (15)0.4228 (3)0.0200 (4)
H20.0401 (19)0.2768 (16)0.439 (4)0.0240 (5)*
C30.17788 (17)0.26401 (15)0.6460 (4)0.0212 (4)
H30.146 (2)0.2091 (17)0.722 (4)0.0255 (5)*
C40.1518 (2)0.35109 (16)0.7808 (3)0.0252 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0611 (13)0.0520 (14)0.0438 (12)0.0274 (12)0.0000000.000000
K20.0303 (3)0.0349 (4)0.0274 (3)0.0036 (3)0.0000000.000000
Na0.0244 (4)0.0240 (4)0.0283 (4)0.0009 (4)0.0013 (3)0.0008 (4)
O10.0253 (7)0.0206 (7)0.0269 (8)0.0012 (6)0.0008 (7)0.0008 (7)
O20.0368 (9)0.0267 (8)0.0234 (8)0.0004 (7)0.0065 (7)0.0011 (6)
O30.0449 (10)0.0272 (8)0.0316 (9)0.0076 (7)0.0032 (8)0.0059 (7)
O40.0338 (8)0.0394 (9)0.0260 (8)0.0120 (7)0.0004 (7)0.0068 (8)
O50.0378 (9)0.0192 (7)0.0192 (7)0.0004 (6)0.0003 (7)0.0010 (6)
O60.0238 (8)0.0244 (8)0.0336 (9)0.0038 (6)0.0038 (7)0.0006 (7)
O70.0266 (8)0.0283 (9)0.0387 (10)0.0001 (7)0.0069 (7)0.0026 (8)
O80.0844 (15)0.0255 (9)0.0243 (9)0.0101 (10)0.0048 (10)0.0000 (7)
O90.0311 (10)0.0732 (15)0.0438 (12)0.0054 (10)0.0084 (9)0.0049 (11)
O100.0287 (9)0.0523 (12)0.0654 (14)0.0128 (9)0.0128 (9)0.0235 (10)
C10.0187 (10)0.0227 (11)0.0203 (10)0.0017 (8)0.0038 (8)0.0008 (8)
C20.0210 (10)0.0178 (10)0.0212 (10)0.0005 (8)0.0009 (9)0.0005 (8)
C30.0230 (10)0.0203 (10)0.0205 (10)0.0014 (8)0.0012 (9)0.0012 (9)
C40.0355 (13)0.0232 (11)0.0169 (10)0.0042 (10)0.0051 (9)0.0004 (8)
Geometric parameters (Å, º) top
K1—O12.8294 (19)Na—O72.3347 (18)
K1—O1i2.8294 (19)Na—O82.3612 (19)
K1—O8ii3.094 (2)Na—O102.329 (2)
K1—O8iii3.094 (2)Na—C4iv3.082 (2)
K1—H18ii3.05 (3)O1—C11.262 (3)
K1—H18iii3.05 (3)O2—C11.242 (3)
K1—O9i2.923 (3)O3—C41.251 (3)
K1—O92.923 (3)O4—C41.258 (3)
K1—O10iii3.389 (3)O5—H50.79 (3)
K1—O10ii3.389 (3)O5—C21.422 (3)
K1—H210iii3.03 (4)O6—H60.73 (2)
K1—H210ii3.03 (4)O6—C31.417 (3)
K2—O4iv2.8451 (16)O7—H170.80 (3)
K2—O4v2.8451 (16)O7—H270.81 (3)
K2—O5vi2.9881 (16)O8—H180.82 (4)
K2—O5vii2.9881 (16)O8—H280.88 (4)
K2—O7iii2.7931 (19)O9—H190.78 (4)
K2—O7viii2.7931 (19)O9—H290.92 (4)
K2—O8viii3.128 (2)O10—H1100.81 (4)
K2—O8iii3.128 (2)O10—H2100.89 (4)
K2—H18viii3.03 (3)C1—C21.533 (3)
K2—H18iii3.03 (3)C2—H21.01 (2)
Na—O12.3651 (17)C2—C31.527 (3)
Na—O3iv2.4613 (19)C3—H30.99 (3)
Na—O5iv2.4893 (18)C3—C41.528 (3)
Naii—K1—Naiii80.19 (4)O8viii—K2—O5vii61.40 (5)
O1i—K1—Naiii145.32 (3)O8iii—K2—O5vi61.40 (5)
O1—K1—Naiii101.50 (3)O8iii—K2—O5vii122.48 (5)
O1—K1—Naii145.32 (3)O8iii—K2—O7iii63.60 (5)
O1i—K1—Naii101.50 (3)O8iii—K2—O7viii125.43 (5)
O1i—K1—O196.21 (8)O8viii—K2—O7viii63.60 (5)
O8ii—K1—Naii32.76 (4)O8viii—K2—O7iii125.43 (5)
O8iii—K1—Naiii32.76 (4)O8viii—K2—O8iii170.21 (7)
O8ii—K1—Naiii110.04 (6)H18viii—K2—Naviii49.0 (6)
O8iii—K1—Naii110.04 (6)H18viii—K2—Naiii164.6 (7)
O8ii—K1—O1142.00 (6)H18iii—K2—Naviii164.6 (7)
O8iii—K1—O169.33 (5)H18iii—K2—Naiii49.0 (6)
O8iii—K1—O1i142.00 (6)H18iii—K2—O4v89.6 (7)
O8ii—K1—O1i69.33 (5)H18iii—K2—O4iv66.9 (7)
O8ii—K1—O8iii141.98 (9)H18viii—K2—O4iv89.6 (7)
H18iii—K1—Naiii42.5 (6)H18viii—K2—O4v66.9 (7)
H18ii—K1—Naiii122.6 (6)H18iii—K2—O5vi59.4 (7)
H18ii—K1—Naii42.5 (6)H18iii—K2—O5vii135.0 (8)
H18iii—K1—Naii122.6 (6)H18viii—K2—O5vii59.4 (7)
H18iii—K1—O1i126.6 (7)H18viii—K2—O5vi135.0 (8)
H18ii—K1—O1126.6 (7)H18iii—K2—O7iii78.3 (7)
H18ii—K1—O1i65.0 (7)H18iii—K2—O7viii131.4 (7)
H18iii—K1—O165.0 (7)H18viii—K2—O7viii78.3 (7)
H18ii—K1—O8ii15.4 (7)H18viii—K2—O7iii131.4 (7)
H18iii—K1—O8ii151.6 (7)H18iii—K2—O8viii156.2 (7)
H18ii—K1—O8iii151.6 (7)H18viii—K2—O8iii156.2 (7)
H18iii—K1—O8iii15.4 (7)H18viii—K2—O8viii15.3 (7)
H18ii—K1—H18iii165.1 (13)H18iii—K2—O8iii15.3 (7)
O9i—K1—Naii71.98 (5)H18viii—K2—H18iii146.3 (13)
O9—K1—Naii92.88 (6)K2ix—Na—K1x98.00 (3)
O9—K1—Naiii71.98 (5)O1—Na—K1x88.14 (4)
O9i—K1—Naiii92.88 (6)O1—Na—K2ix133.94 (5)
O9—K1—O1i73.34 (5)O3iv—Na—K1x140.56 (5)
O9—K1—O1120.86 (6)O3iv—Na—K2ix108.25 (5)
O9i—K1—O173.34 (5)O3iv—Na—O193.90 (6)
O9i—K1—O1i120.86 (6)O5iv—Na—K1x92.33 (5)
O9—K1—O8iii84.20 (6)O5iv—Na—K2ix52.61 (4)
O9—K1—O8ii89.47 (5)O5iv—Na—O1173.28 (6)
O9i—K1—O8iii89.47 (5)O5iv—Na—O3iv81.49 (6)
O9i—K1—O8ii84.20 (6)O7—Na—K1x126.59 (6)
O9—K1—H18iii75.7 (7)O7—Na—K2ix47.99 (5)
O9—K1—H18ii101.7 (8)O7—Na—O192.43 (6)
O9i—K1—H18ii75.7 (7)O7—Na—O3iv92.71 (7)
O9i—K1—H18iii101.7 (8)O7—Na—O5iv92.66 (6)
O9i—K1—O9160.49 (12)O8—Na—K1x45.15 (6)
O10iii—K1—Naiii32.96 (4)O8—Na—K2ix56.17 (6)
O10iii—K1—Naii61.60 (4)O8—Na—O1104.74 (7)
O10ii—K1—Naii32.96 (4)O8—Na—O3iv161.13 (7)
O10ii—K1—Naiii61.60 (4)O8—Na—O5iv80.18 (7)
O10iii—K1—O1i117.96 (5)O8—Na—O783.71 (8)
O10ii—K1—O1117.96 (5)O10—Na—K1x52.33 (7)
O10ii—K1—O1i132.75 (5)O10—Na—K2ix127.25 (6)
O10iii—K1—O1132.75 (5)O10—Na—O192.24 (7)
O10iii—K1—O8ii83.36 (6)O10—Na—O3iv88.24 (8)
O10ii—K1—O8iii83.36 (6)O10—Na—O5iv82.77 (7)
O10iii—K1—O8iii63.64 (5)O10—Na—O7175.16 (8)
O10ii—K1—O8ii63.64 (5)O10—Na—O893.87 (9)
O10iii—K1—H18iii68.5 (7)C4iv—Na—K1x140.12 (5)
O10iii—K1—H18ii98.3 (7)C4iv—Na—K2ix87.68 (5)
O10ii—K1—H18ii68.5 (7)C4iv—Na—O1115.82 (6)
O10ii—K1—H18iii98.3 (7)C4iv—Na—O3iv22.74 (6)
O10iii—K1—O951.13 (6)C4iv—Na—O5iv60.24 (6)
O10iii—K1—O9i109.66 (8)C4iv—Na—O785.88 (7)
O10ii—K1—O9i51.13 (6)C4iv—Na—O8138.44 (7)
O10ii—K1—O9109.66 (8)C4iv—Na—O1093.23 (8)
O10ii—K1—O10iii61.52 (8)Na—O1—K1101.47 (6)
H210ii—K1—Naii42.9 (7)C1—O1—K1115.85 (14)
H210ii—K1—Naiii68.7 (7)C1—O1—Na125.66 (13)
H210iii—K1—Naii68.7 (7)C4—O3—Naxi107.75 (14)
H210iii—K1—Naiii42.9 (7)C4—O4—K2xii120.15 (14)
H210iii—K1—O1134.4 (7)Naxi—O5—K2xiii85.94 (5)
H210iii—K1—O1i104.9 (7)H5—O5—K2xiii99 (2)
H210ii—K1—O1104.9 (7)H5—O5—Naxi111 (2)
H210ii—K1—O1i134.4 (7)C2—O5—K2xiii120.71 (11)
H210ii—K1—O8ii69.2 (7)C2—O5—Naxi130.32 (13)
H210ii—K1—O8iii83.6 (7)C2—O5—H5105 (2)
H210iii—K1—O8iii69.2 (7)C3—O6—H6111 (2)
H210iii—K1—O8ii83.6 (7)Na—O7—K2xiv93.61 (6)
H210ii—K1—H18ii70.0 (9)H17—O7—K2xiv107 (2)
H210ii—K1—H18iii99.0 (10)H17—O7—Na96 (2)
H210iii—K1—H18iii70.0 (9)H27—O7—K2xiv120 (2)
H210iii—K1—H18ii99.0 (10)H27—O7—Na128 (2)
H210ii—K1—O9i36.6 (7)H27—O7—H17109 (3)
H210ii—K1—O9124.0 (7)K2xiv—O8—K1xiv153.90 (7)
H210iii—K1—O936.6 (7)Na—O8—K1xiv102.09 (8)
H210iii—K1—O9i124.0 (7)Na—O8—K2xiv85.00 (6)
H210iii—K1—O10ii74.7 (7)H18—O8—K1xiv79 (2)
H210ii—K1—O10iii74.7 (7)H18—O8—K2xiv76 (2)
H210ii—K1—O10ii14.6 (7)H18—O8—Na122 (3)
H210iii—K1—O10iii14.6 (7)H28—O8—K1xiv85 (2)
H210ii—K1—H210iii88.5 (15)H28—O8—K2xiv108 (2)
Naviii—K2—Naiii115.95 (3)H28—O8—Na134 (2)
O4v—K2—Naiii124.42 (4)H28—O8—H18104 (3)
O4iv—K2—Naiii99.37 (4)K2xiv—H18—K1xiv170.3 (13)
O4v—K2—Naviii99.37 (4)O8—H18—K1xiv85 (2)
O4iv—K2—Naviii124.42 (4)O8—H18—K2xiv89 (2)
O4iv—K2—O4v93.31 (7)H19—O9—K1i119 (3)
O5vii—K2—Naviii41.44 (3)H29—O9—K1i144 (2)
O5vii—K2—Naiii112.74 (4)H29—O9—H1996 (4)
O5vi—K2—Naviii112.74 (4)Na—O10—K1x94.71 (8)
O5vi—K2—Naiii41.44 (3)H110—O10—K1x97 (2)
O5vi—K2—O4iv67.86 (5)H110—O10—Na130 (2)
O5vii—K2—O4iv147.86 (5)H210—O10—K1x59 (2)
O5vi—K2—O4v147.86 (5)H210—O10—Na123 (2)
O5vii—K2—O4v67.86 (5)H210—O10—H110105 (3)
O5vi—K2—O5vii139.96 (7)O10—H210—K1x107 (3)
O7viii—K2—Naiii86.80 (4)O2—C1—O1126.5 (2)
O7viii—K2—Naviii38.40 (4)C2—C1—O1116.85 (18)
O7iii—K2—Naiii38.40 (4)C2—C1—O2116.63 (19)
O7iii—K2—Naviii86.80 (4)C1—C2—O5110.76 (16)
O7iii—K2—O4v110.26 (5)H2—C2—O5108.8 (13)
O7viii—K2—O4v137.77 (5)H2—C2—C1108.7 (13)
O7iii—K2—O4iv137.77 (5)C3—C2—O5109.47 (16)
O7viii—K2—O4iv110.26 (5)C3—C2—C1110.38 (17)
O7iii—K2—O5vi74.21 (5)C3—C2—H2108.7 (13)
O7viii—K2—O5vi74.35 (5)C2—C3—O6110.51 (17)
O7iii—K2—O5vii74.35 (5)H3—C3—O6106.6 (14)
O7viii—K2—O5vii74.21 (5)H3—C3—C2110.2 (14)
O7viii—K2—O7iii75.33 (8)C4—C3—O6111.59 (18)
O8viii—K2—Naviii38.83 (3)C4—C3—C2110.16 (17)
O8viii—K2—Naiii150.40 (4)C4—C3—H3107.7 (14)
O8iii—K2—Naviii150.40 (4)O3—C4—Naxi49.51 (11)
O8iii—K2—Naiii38.83 (3)O4—C4—Naxi122.62 (15)
O8viii—K2—O4iv91.28 (5)O4—C4—O3125.8 (2)
O8viii—K2—O4v81.98 (5)C3—C4—Naxi96.28 (13)
O8iii—K2—O4iv81.98 (5)C3—C4—O3116.9 (2)
O8iii—K2—O4v91.28 (5)C3—C4—O4117.3 (2)
O8viii—K2—O5vi122.48 (5)
K1—O1—C1—O251.54 (14)Naxi—O3—C4—C374.26 (13)
K1i—O1—C1—O251.54 (14)Naxi—O5—C2—C1133.65 (16)
K1—O1—C1—C2128.48 (13)Naxi—O5—C2—C311.72 (15)
K1i—O1—C1—C2128.48 (13)Naxi—C4—C3—O662.93 (12)
K2xii—O4—C4—Naxi72.98 (13)Naxi—C4—C3—C260.21 (13)
K2—O4iv—C4iv—Na72.98 (13)O1—C1—C2—O5176.76 (18)
K2xii—O4—C4—O312.24 (17)O1—C1—C2—C361.8 (2)
K2xi—O4—C4—O312.24 (17)O2—C1—C2—O53.3 (2)
K2xii—O4—C4—C3168.57 (14)O2—C1—C2—C3118.14 (19)
K2xi—O4—C4—C3168.57 (14)O3—C4—C3—O615.5 (2)
K2xv—O5—C2—C1113.01 (14)O3—C4—C3—C2107.6 (2)
K2xiii—O5—C2—C1113.01 (14)O4—C4—C3—O6165.2 (2)
K2xiii—O5—C2—C3125.06 (14)O4—C4—C3—C271.6 (2)
K2xv—O5—C2—C3125.06 (14)O5—C2—C3—O668.00 (17)
Na—O1—C1—O276.73 (17)O5—C2—C3—C455.77 (18)
Na—O1—C1—C2103.24 (15)O6—C3—C2—C154.16 (19)
Naxi—O3—C4—O4104.94 (14)C1—C2—C3—C4177.93 (17)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y1/2, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y1/2, z; (vii) x+1/2, y+1/2, z; (viii) x+1, y, z1; (ix) x+1, y, z+1; (x) x, y, z+1; (xi) x+1/2, y+1/2, z+1; (xii) x1/2, y+1/2, z+1; (xiii) x1/2, 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···AD—HH···AD···AD—H···A
O5—H5···O20.79 (3)2.07 (3)2.603 (2)124 (3)
O5—H5···O3iii0.79 (3)2.69 (3)3.338 (2)141 (2)
O5—H5···O4iii0.79 (3)2.83 (3)3.258 (2)116 (2)
O6—H6···O10xi0.73 (2)2.20 (3)2.897 (3)160 (3)
O7—H17···O60.80 (3)1.99 (3)2.788 (2)178 (3)
O7—H27···O4v0.81 (3)2.09 (3)2.875 (2)164 (3)
O8—H18···O3xvi0.82 (4)1.89 (4)2.702 (2)170 (4)
O8—H28···O1xiv0.88 (4)2.84 (3)3.376 (2)121 (3)
O8—H28···O2xiv0.88 (4)1.88 (4)2.753 (2)172 (3)
O9—H19···O2vi0.78 (4)2.50 (4)3.115 (3)138 (4)
O9—H19···O3iv0.78 (4)2.72 (4)3.168 (3)119 (3)
O9—H19···O6iv0.78 (4)2.51 (4)3.141 (3)140 (4)
O9—H29···O4ii0.92 (4)1.89 (4)2.807 (3)169 (3)
O10—H110···O1i0.81 (4)1.92 (4)2.725 (2)172 (3)
O10—H210···O9xiv0.89 (4)1.87 (4)2.756 (3)173 (3)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y1/2, z+1; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y1/2, z; (xi) x+1/2, y+1/2, z+1; (xiv) x, y, z+1; (xvi) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (256K_anh) top
Crystal data top
C4H12KNaO10F(000) = 585.519
Mr = 282.22Dx = 1.787 Mg m3
Monoclinic, P2111Mo Kα radiation, λ = 0.71073 Å
a = 11.8513 (8) ÅCell parameters from 6823 reflections
b = 14.2386 (11) Åθ = 3.5–28.7°
c = 6.2155 (4) ŵ = 0.59 mm1
β = 90°T = 256 K
V = 1048.84 (13) Å3Prism, clear colourless
Z = 40.48 × 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 Source4145 reflections with I 2u(I)
Graphite monochromatorRint = 0.051
Detector resolution: 10.3457 pixels mm-1θmax = 29.5°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.758, Tmax = 1.000l = 88
18315 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.09Δρmax = 0.33 e Å3
5147 reflectionsΔρmin = 0.34 e Å3
386 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
3 restraintsAbsolute structure parameter: 0.09 (2)
24 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00032 (18)0.00041 (13)0.0454 (2)0.0536 (5)
K20.50001 (7)0.00022 (5)0.15958 (9)0.03172 (14)
Na10.23165 (10)0.00672 (7)0.52105 (17)0.0262 (3)
Na20.23179 (10)0.00678 (8)0.51995 (17)0.0261 (2)
O110.12003 (16)0.10899 (13)0.3498 (3)0.0247 (4)
O120.12019 (16)0.10901 (13)0.3492 (3)0.0246 (4)
O210.21061 (18)0.20295 (14)0.1191 (3)0.0295 (4)
O220.21005 (18)0.20298 (14)0.1180 (3)0.0296 (4)
O310.23136 (19)0.40638 (14)0.8155 (3)0.0352 (5)
O320.23222 (19)0.40644 (14)0.8142 (3)0.0352 (5)
O410.05168 (18)0.36105 (15)0.8454 (3)0.0336 (5)
O420.05239 (18)0.36159 (15)0.8451 (3)0.0330 (5)
O510.16398 (17)0.35744 (13)0.3243 (3)0.0261 (4)
H510.194 (3)0.341 (2)0.218 (5)0.0391 (7)*
O520.16377 (18)0.35736 (13)0.3239 (3)0.0260 (4)
H520.191 (3)0.344 (2)0.212 (5)0.0390 (7)*
O610.29535 (17)0.24792 (14)0.6298 (3)0.0279 (4)
H610.324 (3)0.295 (2)0.609 (6)0.0419 (7)*
O620.29561 (17)0.24822 (14)0.6289 (3)0.0277 (4)
H620.329 (3)0.289 (2)0.603 (6)0.0416 (7)*
O710.39587 (18)0.08241 (16)0.4845 (4)0.0321 (5)
H170.371 (3)0.129 (3)0.525 (6)0.0482 (7)*
H270.433 (3)0.089 (3)0.373 (6)0.0482 (7)*
O720.39596 (18)0.08272 (16)0.4846 (4)0.0322 (5)
H470.434 (3)0.095 (3)0.371 (6)0.0483 (7)*
H370.366 (3)0.130 (3)0.530 (6)0.0483 (7)*
O810.2421 (2)0.04151 (17)0.8840 (3)0.0452 (6)
H180.240 (4)0.099 (3)0.948 (6)0.0678 (10)*
H280.257 (4)0.002 (3)0.983 (8)0.0678 (10)*
O820.2414 (2)0.04115 (17)0.8834 (3)0.0458 (7)
H480.258 (4)0.001 (3)0.985 (8)0.0687 (10)*
H380.231 (4)0.094 (3)0.941 (7)0.0687 (10)*
O910.0612 (2)0.1963 (2)0.0343 (4)0.0511 (7)
H290.036 (4)0.251 (3)0.080 (6)0.0766 (10)*
H190.118 (4)0.232 (3)0.009 (7)0.0766 (10)*
O920.0607 (2)0.1956 (2)0.0337 (4)0.0507 (7)
H390.118 (4)0.211 (3)0.014 (7)0.0761 (10)*
H490.032 (4)0.251 (3)0.082 (6)0.0761 (10)*
O1010.0758 (2)0.1033 (2)0.5784 (5)0.0513 (7)
H2100.073 (4)0.141 (3)0.693 (7)0.0769 (10)*
H1100.014 (4)0.104 (3)0.523 (6)0.0769 (10)*
O1020.0766 (2)0.10383 (19)0.5764 (5)0.0486 (7)
H4100.069 (4)0.134 (3)0.698 (7)0.0729 (10)*
H3100.018 (4)0.103 (3)0.518 (6)0.0729 (10)*
C110.1547 (2)0.18781 (19)0.2840 (4)0.0206 (6)
C210.1254 (2)0.27330 (18)0.4237 (4)0.0207 (5)
H210.045 (3)0.278 (2)0.437 (4)0.0248 (6)*
C310.1778 (2)0.2640 (2)0.6466 (4)0.0218 (6)
H310.146 (3)0.205 (2)0.723 (4)0.0262 (7)*
C410.1517 (3)0.3509 (2)0.7814 (4)0.0259 (6)
C120.1541 (2)0.18772 (19)0.2841 (4)0.0205 (5)
C220.1254 (2)0.27323 (18)0.4227 (4)0.0204 (5)
H220.038 (3)0.2771 (19)0.437 (4)0.0245 (6)*
C320.1778 (2)0.26405 (19)0.6453 (4)0.0219 (6)
H320.144 (3)0.210 (2)0.724 (4)0.0263 (7)*
C420.1519 (3)0.35140 (19)0.7804 (4)0.0256 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0632 (10)0.0516 (11)0.0460 (10)0.0301 (10)0.0001 (12)0.0012 (9)
K20.0317 (3)0.0358 (3)0.0277 (3)0.0035 (3)0.0000 (3)0.0002 (2)
Na10.0257 (6)0.0239 (6)0.0291 (5)0.0009 (4)0.0017 (5)0.0006 (4)
Na20.0249 (6)0.0242 (6)0.0291 (5)0.0008 (4)0.0015 (5)0.0006 (4)
O110.0267 (10)0.0203 (11)0.0270 (10)0.0013 (8)0.0020 (8)0.0014 (7)
O120.0272 (10)0.0207 (11)0.0260 (10)0.0013 (8)0.0007 (8)0.0007 (7)
O210.0378 (11)0.0272 (11)0.0236 (10)0.0003 (9)0.0077 (9)0.0005 (8)
O220.0377 (12)0.0278 (11)0.0232 (10)0.0013 (9)0.0069 (9)0.0017 (8)
O310.0459 (13)0.0276 (12)0.0321 (10)0.0079 (10)0.0031 (10)0.0065 (8)
O320.0467 (13)0.0266 (12)0.0323 (10)0.0084 (10)0.0024 (10)0.0066 (8)
O410.0357 (11)0.0394 (13)0.0256 (10)0.0127 (10)0.0000 (9)0.0067 (9)
O420.0326 (11)0.0404 (13)0.0261 (10)0.0112 (9)0.0009 (8)0.0069 (9)
O510.0379 (12)0.0190 (10)0.0213 (9)0.0011 (8)0.0014 (8)0.0012 (8)
O520.0377 (12)0.0202 (10)0.0202 (9)0.0007 (8)0.0001 (8)0.0001 (8)
O610.0251 (11)0.0250 (12)0.0337 (11)0.0045 (9)0.0044 (9)0.0002 (9)
O620.0217 (11)0.0255 (12)0.0359 (11)0.0032 (8)0.0034 (9)0.0019 (9)
O710.0285 (11)0.0297 (12)0.0382 (12)0.0005 (9)0.0064 (9)0.0018 (9)
O720.0273 (11)0.0293 (12)0.0400 (12)0.0000 (9)0.0077 (9)0.0019 (9)
O810.0845 (19)0.0257 (13)0.0254 (11)0.0117 (12)0.0044 (12)0.0001 (8)
O820.0850 (19)0.0269 (13)0.0255 (11)0.0122 (13)0.0035 (12)0.0006 (9)
O910.0347 (14)0.075 (2)0.0431 (14)0.0058 (13)0.0069 (11)0.0073 (13)
O920.0326 (14)0.074 (2)0.0450 (14)0.0051 (13)0.0080 (11)0.0048 (13)
O1010.0322 (14)0.0536 (17)0.0681 (18)0.0148 (11)0.0139 (12)0.0257 (13)
O1020.0292 (13)0.0521 (16)0.0645 (17)0.0128 (11)0.0128 (12)0.0226 (13)
C110.0199 (13)0.0220 (15)0.0198 (12)0.0019 (11)0.0055 (11)0.0004 (10)
C210.0223 (15)0.0185 (14)0.0212 (12)0.0000 (11)0.0003 (11)0.0004 (10)
C310.0225 (14)0.0221 (15)0.0209 (13)0.0015 (11)0.0005 (10)0.0003 (10)
C410.0381 (17)0.0221 (15)0.0176 (12)0.0044 (13)0.0055 (12)0.0010 (10)
C120.0178 (13)0.0237 (15)0.0199 (12)0.0019 (11)0.0043 (11)0.0012 (10)
C220.0203 (14)0.0182 (13)0.0227 (13)0.0004 (10)0.0012 (11)0.0019 (10)
C320.0237 (14)0.0196 (14)0.0225 (13)0.0023 (11)0.0019 (10)0.0008 (10)
C420.0382 (17)0.0228 (15)0.0158 (12)0.0038 (13)0.0039 (12)0.0009 (10)
Geometric parameters (Å, º) top
K1—O112.831 (2)O31—C411.249 (4)
K1—O122.828 (2)O32—C421.251 (4)
K1—O81i3.094 (3)O41—C411.258 (4)
K1—H28i3.07 (5)O42—C421.254 (4)
K1—O82i3.091 (4)O51—H510.78 (3)
K1—O912.922 (4)O51—C211.424 (3)
K1—O922.926 (4)O52—H520.79 (3)
K1—O101i3.371 (3)O52—C221.421 (3)
K1—H210i3.09 (4)O61—H610.76 (3)
K1—O102i3.397 (3)O61—C311.416 (3)
K1—H410i3.00 (4)O62—H620.73 (3)
K2—O41ii2.844 (2)O62—C321.418 (3)
K2—O42iii2.847 (2)O71—H170.77 (4)
K2—O51iv2.989 (2)O71—H270.83 (4)
K2—O52v2.991 (2)O72—H470.85 (4)
K2—O71i2.791 (2)O72—H370.82 (4)
K2—O72vi2.793 (2)O81—H180.91 (4)
K2—O81i3.125 (3)O81—H280.85 (5)
K2—H28i3.01 (5)O82—H480.89 (5)
K2—O82vi3.133 (3)O82—H380.85 (4)
K2—H48vi3.00 (5)O91—H290.89 (4)
Na1—O112.366 (2)O91—H190.89 (5)
Na1—O32iii2.460 (2)O92—H390.78 (5)
Na1—O52iii2.492 (2)O92—H490.91 (5)
Na1—O712.335 (2)O101—H2100.90 (5)
Na1—O812.361 (2)O101—H1100.81 (5)
Na1—O1012.330 (3)O102—H4100.88 (4)
Na1—C42iii3.081 (3)O102—H3100.78 (5)
Na2—O122.365 (2)C11—C211.535 (4)
Na2—O31vii2.463 (2)C21—H210.96 (3)
Na2—O51vii2.490 (2)C21—C311.524 (4)
Na2—O722.336 (2)C31—H311.04 (3)
Na2—O822.363 (2)C31—C411.526 (4)
Na2—O1022.327 (3)C12—C221.530 (4)
Na2—C41vii3.086 (3)C22—H221.04 (3)
O11—C111.263 (3)C22—C321.522 (4)
O12—C121.257 (3)C32—H321.00 (3)
O21—C111.239 (3)C32—C421.532 (4)
O22—C121.246 (3)
Na2i—K1—Na1i80.21 (3)O101—Na1—O52iii82.91 (9)
O11—K1—Na1i101.54 (7)O101—Na1—O71175.22 (10)
O11—K1—Na2i145.11 (8)O101—Na1—O8193.81 (10)
O12—K1—Na1i145.54 (8)C42iii—Na1—K1viii140.10 (7)
O12—K1—Na2i101.46 (7)C42iii—Na1—K2viii87.65 (6)
O12—K1—O1196.19 (7)C42iii—Na1—O11115.68 (8)
O81i—K1—Na1i32.84 (5)C42iii—Na1—O32iii22.75 (7)
O81i—K1—Na2i110.10 (6)C42iii—Na1—O52iii60.22 (7)
O81i—K1—O1169.30 (7)C42iii—Na1—O7185.61 (8)
O81i—K1—O12142.17 (10)C42iii—Na1—O81138.41 (9)
H28i—K1—Na1i42.7 (9)C42iii—Na1—O10193.53 (10)
H28i—K1—Na2i122.8 (9)K2ix—Na2—K1viii97.99 (4)
H28i—K1—O1165.2 (8)O12—Na2—K1viii88.05 (6)
H28i—K1—O12126.3 (9)O12—Na2—K2ix133.99 (6)
H28i—K1—O81i15.8 (9)O31vii—Na2—K1viii140.67 (7)
O82i—K1—Na1i110.07 (6)O31vii—Na2—K2ix108.16 (6)
O82i—K1—Na2i32.72 (5)O31vii—Na2—O1293.99 (7)
O82i—K1—O11141.74 (10)O51vii—Na2—K1viii92.36 (6)
O82i—K1—O1269.33 (7)O51vii—Na2—K2ix52.62 (5)
O82i—K1—O81i142.06 (7)O51vii—Na2—O12173.24 (8)
O82i—K1—H28i151.6 (9)O51vii—Na2—O31vii81.44 (7)
O91—K1—Na1i72.05 (7)O72—Na2—K1viii126.51 (7)
O91—K1—Na2i93.01 (7)O72—Na2—K2ix47.98 (6)
O91—K1—O11120.95 (10)O72—Na2—O1292.50 (8)
O91—K1—O1273.49 (8)O72—Na2—O31vii92.69 (9)
O91—K1—O81i84.31 (9)O72—Na2—O51vii92.68 (8)
O91—K1—H28i75.3 (8)O82—Na2—K1viii45.00 (7)
O91—K1—O82i89.68 (8)O82—Na2—K2ix56.26 (7)
O92—K1—Na1i92.88 (7)O82—Na2—O12104.73 (9)
O92—K1—Na2i71.87 (7)O82—Na2—O31vii161.07 (9)
O92—K1—O1173.24 (8)O82—Na2—O51vii80.16 (8)
O92—K1—O12120.63 (10)O82—Na2—O7283.80 (9)
O92—K1—O81i89.44 (8)O102—Na2—K1viii52.42 (8)
O92—K1—H28i102.2 (9)O102—Na2—K2ix127.18 (7)
O92—K1—O82i83.97 (9)O102—Na2—O1292.26 (9)
O92—K1—O91160.56 (9)O102—Na2—O31vii88.25 (10)
O101i—K1—Na1i33.01 (5)O102—Na2—O51vii82.67 (9)
O101i—K1—Na2i61.53 (5)O102—Na2—O72175.07 (10)
O101i—K1—O11132.91 (9)O102—Na2—O8293.76 (11)
O101i—K1—O12118.13 (8)C41vii—Na2—K1viii140.19 (7)
O101i—K1—O81i63.81 (7)C41vii—Na2—K2ix87.69 (6)
O101i—K1—H28i68.4 (9)C41vii—Na2—O12115.84 (8)
O101i—K1—O82i83.35 (7)C41vii—Na2—O31vii22.65 (7)
O101i—K1—O9151.29 (7)C41vii—Na2—O51vii60.26 (7)
O101i—K1—O92109.56 (8)C41vii—Na2—O7285.90 (9)
H210i—K1—Na1i42.7 (9)C41vii—Na2—O82138.48 (9)
H210i—K1—Na2i69.8 (9)C41vii—Na2—O10293.16 (10)
H210i—K1—O11133.6 (9)Na1—O11—K1101.41 (8)
H210i—K1—O12105.0 (9)C11—O11—K1115.81 (15)
H210i—K1—O81i68.7 (9)C11—O11—Na1125.63 (16)
H210i—K1—H28i68.9 (12)Na2—O12—K1101.58 (8)
H210i—K1—O82i84.7 (9)C12—O12—K1115.72 (15)
H210i—K1—O9136.1 (9)C12—O12—Na2125.94 (16)
H210i—K1—O92124.7 (9)C41—O31—Na2ii107.95 (16)
H210i—K1—O101i15.1 (9)C42—O32—Na1x107.75 (16)
O102i—K1—Na1i61.65 (5)C41—O41—K2vii119.97 (18)
O102i—K1—Na2i32.88 (5)C42—O42—K2x120.36 (18)
O102i—K1—O11117.87 (8)Na2ii—O51—K2xi85.94 (6)
O102i—K1—O12132.59 (9)H51—O51—K2xi102 (3)
O102i—K1—O81i83.44 (7)H51—O51—Na2ii110 (3)
O102i—K1—H28i98.7 (9)C21—O51—K2xi120.70 (15)
O102i—K1—O82i63.49 (7)C21—O51—Na2ii130.09 (15)
O102i—K1—O91109.77 (8)C21—O51—H51105 (3)
O102i—K1—O9251.08 (7)Na1x—O52—K2xii85.79 (6)
O102i—K1—O101i61.46 (6)H52—O52—K2xii98 (2)
O102i—K1—H210i75.6 (9)H52—O52—Na1x109 (3)
H410i—K1—Na1i68.8 (9)C22—O52—K2xii120.85 (15)
H410i—K1—Na2i42.2 (9)C22—O52—Na1x130.32 (15)
H410i—K1—O11105.4 (9)C22—O52—H52108 (3)
H410i—K1—O12133.8 (9)C31—O61—H61108 (3)
H410i—K1—O81i84.0 (9)C32—O62—H62115 (3)
H410i—K1—H28i99.9 (13)Na1—O71—K2viii93.63 (8)
H410i—K1—O82i68.5 (9)H17—O71—K2viii106 (3)
H410i—K1—O91123.8 (9)H17—O71—Na197 (3)
H410i—K1—O9237.0 (9)H27—O71—K2viii118 (3)
H410i—K1—O101i74.4 (8)H27—O71—Na1126 (3)
H410i—K1—H210i89.0 (11)H27—O71—H17112 (4)
H410i—K1—O102i14.1 (8)Na2—O72—K2ix93.60 (8)
Na2vi—K2—Na1i115.98 (2)H47—O72—K2ix120 (2)
O41ii—K2—Na1i124.35 (5)H47—O72—Na2129 (2)
O41ii—K2—Na2vi99.48 (5)H37—O72—K2ix105 (3)
O42iii—K2—Na1i99.23 (5)H37—O72—Na293 (3)
O42iii—K2—Na2vi124.52 (5)H37—O72—H47111 (4)
O42iii—K2—O41ii93.27 (6)K2viii—O81—K1viii153.86 (9)
O51iv—K2—Na1i112.81 (5)Na1—O81—K1viii101.86 (10)
O51iv—K2—Na2vi41.44 (4)Na1—O81—K2viii85.05 (7)
O51iv—K2—O41ii67.93 (6)H18—O81—K1viii90 (3)
O51iv—K2—O42iii147.93 (6)H18—O81—K2viii103 (3)
O52v—K2—Na1i41.51 (4)H18—O81—Na1133 (3)
O52v—K2—Na2vi112.68 (5)H28—O81—K1viii80 (3)
O52v—K2—O41ii147.81 (6)H28—O81—K2viii74 (3)
O52v—K2—O42iii67.75 (6)H28—O81—Na1121 (3)
O52v—K2—O51iv140.00 (6)H28—O81—H18106 (4)
O71i—K2—Na1i38.41 (5)K2viii—H28—K1viii170.2 (18)
O71i—K2—Na2vi86.75 (5)O81—H28—K1viii84 (4)
O71i—K2—O41ii110.38 (7)O81—H28—K2viii90 (4)
O71i—K2—O42iii137.64 (7)K2ix—O82—K1viii154.05 (9)
O71i—K2—O51iv74.41 (6)Na2—O82—K1viii102.28 (10)
O71i—K2—O52v74.20 (6)Na2—O82—K2ix84.90 (8)
O72vi—K2—Na1i86.80 (5)H48—O82—K1viii82 (3)
O72vi—K2—Na2vi38.41 (5)H48—O82—K2ix73 (3)
O72vi—K2—O41ii137.89 (7)H48—O82—Na2120 (3)
O72vi—K2—O42iii110.30 (7)H38—O82—K1viii84 (3)
O72vi—K2—O51iv74.24 (6)H38—O82—K2ix110 (3)
O72vi—K2—O52v74.27 (6)H38—O82—Na2131 (3)
O72vi—K2—O71i75.22 (6)H38—O82—H48109 (4)
O81i—K2—Na1i38.84 (4)O82—H48—K2ix90 (3)
O81i—K2—Na2vi150.45 (5)H29—O91—K1145 (3)
O81i—K2—O41ii91.18 (6)H19—O91—K1133 (3)
O81i—K2—O42iii81.82 (6)H19—O91—H2981 (4)
O81i—K2—O51iv122.56 (6)H39—O92—K1115 (4)
O81i—K2—O52v61.48 (6)H49—O92—K1142 (3)
O81i—K2—O71i63.71 (6)H49—O92—H39103 (5)
O81i—K2—O72vi125.44 (6)Na1—O101—K1viii94.95 (10)
H28i—K2—Na1i49.1 (9)H210—O101—K1viii64 (3)
H28i—K2—Na2vi164.9 (10)H210—O101—Na1120 (3)
H28i—K2—O41ii89.9 (8)H110—O101—K1viii97 (3)
H28i—K2—O42iii66.2 (9)H110—O101—Na1131 (3)
H28i—K2—O51iv135.7 (9)H110—O101—H210108 (4)
H28i—K2—O52v59.1 (8)O101—H210—K1viii101 (3)
H28i—K2—O71i78.8 (10)Na2—O102—K1viii94.70 (10)
H28i—K2—O72vi131.2 (9)H410—O102—K1viii57 (3)
H28i—K2—O81i15.8 (9)H410—O102—Na2121 (3)
O82vi—K2—Na1i150.46 (5)H310—O102—K1viii99 (3)
O82vi—K2—Na2vi38.85 (4)H310—O102—Na2128 (3)
O82vi—K2—O41ii82.03 (6)H310—O102—H410109 (4)
O82vi—K2—O42iii91.40 (6)O102—H410—K1viii109 (3)
O82vi—K2—O51iv61.36 (6)O21—C11—O11126.6 (2)
O82vi—K2—O52v122.42 (6)C21—C11—O11116.6 (2)
O82vi—K2—O71i125.39 (6)C21—C11—O21116.8 (2)
O82vi—K2—O72vi63.65 (6)C11—C21—O51110.4 (2)
O82vi—K2—O81i170.14 (5)H21—C21—O51107.3 (17)
O82vi—K2—H28i155.8 (10)H21—C21—C11109.4 (17)
H48vi—K2—Na1i165.4 (10)C31—C21—O51109.7 (2)
H48vi—K2—Na2vi49.5 (9)C31—C21—C11110.6 (2)
H48vi—K2—O41ii65.7 (9)C31—C21—H21109.3 (16)
H48vi—K2—O42iii90.2 (9)C21—C31—O61110.4 (2)
H48vi—K2—O51iv58.7 (8)H31—C31—O61105.2 (17)
H48vi—K2—O52v136.2 (9)H31—C31—C21109.9 (16)
H48vi—K2—O71i131.2 (9)C41—C31—O61111.8 (2)
H48vi—K2—O72vi79.4 (10)C41—C31—C21110.2 (2)
H48vi—K2—O81i155.2 (10)C41—C31—H31109.2 (16)
H48vi—K2—H28i145.5 (10)O31—C41—Na2ii49.41 (13)
H48vi—K2—O82vi16.5 (9)O41—C41—Na2ii122.55 (19)
K2viii—Na1—K1viii98.06 (4)O41—C41—O31125.9 (3)
O11—Na1—K1viii88.29 (6)C31—C41—Na2ii96.23 (16)
O11—Na1—K2viii133.95 (6)C31—C41—O31116.9 (3)
O32iii—Na1—K1viii140.40 (7)C31—C41—O41117.2 (3)
O32iii—Na1—K2viii108.29 (6)O22—C12—O12126.3 (2)
O32iii—Na1—O1193.78 (7)C22—C12—O12117.2 (2)
O52iii—Na1—K1viii92.31 (6)C22—C12—O22116.5 (2)
O52iii—Na1—K2viii52.69 (5)C12—C22—O52110.9 (2)
O52iii—Na1—O11173.16 (8)H22—C22—O52108.2 (15)
O52iii—Na1—O32iii81.42 (7)H22—C22—C12108.2 (15)
O71—Na1—K1viii126.85 (7)C32—C22—O52109.5 (2)
O71—Na1—K2viii47.96 (6)C32—C22—C12110.7 (2)
O71—Na1—O1192.50 (8)C32—C22—H22109.3 (14)
O71—Na1—O32iii92.60 (8)C22—C32—O62110.5 (2)
O71—Na1—O52iii92.60 (8)H32—C32—O62107.7 (18)
O81—Na1—K1viii45.30 (7)H32—C32—C22110.6 (16)
O81—Na1—K2viii56.11 (7)C42—C32—O62111.5 (2)
O81—Na1—O11104.89 (8)C42—C32—C22110.3 (2)
O81—Na1—O32iii161.10 (9)C42—C32—H32106.2 (17)
O81—Na1—O52iii80.22 (8)O32—C42—Na1x49.50 (13)
O81—Na1—O7183.78 (9)O42—C42—Na1x122.70 (19)
O101—Na1—K1viii52.04 (8)O42—C42—O32126.1 (3)
O101—Na1—K2viii127.34 (8)C32—C42—Na1x96.27 (15)
O101—Na1—O1192.11 (9)C32—C42—O32116.6 (3)
O101—Na1—O32iii88.36 (10)C32—C42—O42117.3 (3)
K1—O11—C11—O2151.6 (2)Na2ii—O51—C21—C3111.9 (2)
K1—O11—C11—C21128.89 (17)Na2ii—C41—C31—O6163.01 (15)
K1—O12—C12—O2252.13 (19)Na2ii—C41—C31—C2160.18 (16)
K1—O12—C12—C22128.67 (16)O11—C11—C21—O51176.7 (2)
K2vii—O41—C41—Na2ii73.15 (15)O11—C11—C21—C3161.7 (2)
K2vii—O41—C41—O3112.6 (2)O12—C12—C22—O52177.0 (2)
K2vii—O41—C41—C31168.60 (17)O12—C12—C22—C3261.3 (2)
K2—O42iii—C42iii—Na172.99 (15)O21—C11—C21—O513.8 (2)
K2x—O42—C42—O3212.1 (2)O21—C11—C21—C31117.8 (2)
K2x—O42—C42—C32168.53 (16)O22—C12—C22—O523.7 (2)
K2xi—O51—C21—C11112.88 (17)O22—C12—C22—C32118.0 (2)
K2xi—O51—C21—C31124.94 (17)O31—C41—C31—O6115.7 (3)
K2xii—O52—C22—C12112.76 (17)O31—C41—C31—C21107.5 (3)
K2xii—O52—C22—C32124.82 (18)O32—C42—C32—O6215.5 (3)
Na1—O11—C11—O2176.5 (2)O32—C42—C32—C22107.7 (2)
Na1—O11—C11—C21103.01 (19)O41—C41—C31—O61165.3 (2)
Na1x—O32—C42—O42104.86 (17)O41—C41—C31—C2171.5 (3)
Na1x—O32—C42—C3274.47 (16)O42—C42—C32—O62165.1 (2)
Na1x—O52—C22—C12134.0 (2)O42—C42—C32—C2271.7 (2)
Na1x—O52—C22—C3211.6 (2)O51—C21—C31—O6168.1 (2)
Na1x—C42—C32—O6262.96 (15)O51—C21—C31—C4155.9 (2)
Na1x—C42—C32—C2260.17 (16)O52—C22—C32—O6268.1 (2)
Na2—O12—C12—O2276.5 (2)O52—C22—C32—C4255.6 (2)
Na2—O12—C12—C22102.68 (19)O61—C31—C21—C1154.0 (2)
Na2ii—O31—C41—O41104.76 (17)O62—C32—C22—C1254.5 (2)
Na2ii—O31—C41—C3174.08 (17)C11—C21—C31—C41178.0 (2)
Na2ii—O51—C21—C11134.0 (2)C12—C22—C32—C42178.1 (2)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (iv) x+1/2, y+1/2, z; (v) x+1/2, y1/2, z; (vi) x+1, y, z1; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (ix) x1, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xii) x1/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O51—H51···O210.78 (3)2.07 (4)2.601 (3)125 (3)
O51—H51···O31i0.78 (3)2.71 (3)3.336 (3)139 (3)
O51—H51···O41i0.78 (3)2.88 (3)3.261 (3)113 (3)
O52—H52···O220.79 (3)2.10 (4)2.603 (3)121 (3)
O52—H52···O32i0.79 (3)2.67 (3)3.344 (3)144 (3)
O52—H52···O42i0.79 (3)2.82 (3)3.256 (3)117 (3)
O61—H61···O102ii0.76 (3)2.19 (3)2.899 (4)155 (4)
O62—H62···O101x0.73 (3)2.21 (3)2.907 (4)162 (4)
O71—H17···O610.77 (4)2.02 (4)2.790 (3)176 (4)
O71—H27···O41ii0.83 (4)2.08 (4)2.875 (3)161 (4)
O72—H47···O42x0.85 (4)2.04 (4)2.874 (3)166 (3)
O72—H37···O620.82 (4)1.97 (4)2.788 (3)177 (4)
O81—H18···O11viii0.91 (4)2.88 (4)3.375 (3)116 (3)
O81—H18···O21viii0.91 (4)1.85 (4)2.749 (3)167 (4)
O81—H28···O32xiii0.85 (5)1.86 (5)2.705 (3)170 (5)
O82—H48···O31xiv0.89 (5)1.82 (5)2.699 (3)170 (5)
O82—H38···O12viii0.85 (4)2.87 (4)3.374 (3)120 (3)
O82—H38···O22viii0.85 (4)1.92 (5)2.753 (3)170 (4)
O91—H29···O42i0.89 (4)1.94 (5)2.813 (4)166 (4)
O91—H19···O22v0.89 (5)2.37 (5)3.111 (3)141 (4)
O91—H19···O32iii0.89 (5)2.88 (5)3.163 (3)101 (3)
O91—H19···O62iii0.89 (5)2.49 (5)3.140 (3)131 (4)
O92—H39···O21xi0.78 (5)2.51 (5)3.116 (3)136 (4)
O92—H39···O31vii0.78 (5)2.66 (5)3.166 (3)124 (4)
O92—H39···O61vii0.78 (5)2.51 (5)3.139 (3)140 (4)
O92—H49···O41i0.91 (5)1.91 (5)2.809 (4)170 (4)
O101—H210···O91viii0.90 (5)1.87 (5)2.753 (4)168 (4)
O101—H110···O120.81 (5)1.92 (5)2.727 (3)171 (4)
O102—H410···O92viii0.88 (4)1.88 (4)2.759 (4)176 (4)
O102—H310···O110.78 (5)1.95 (5)2.724 (3)174 (4)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (v) x+1/2, y1/2, z; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xiii) x+1/2, y1/2, z+2; (xiv) x1/2, y+1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (266K_anh) top
Crystal data top
C4H12KNaO10F(000) = 585.519
Mr = 282.22Dx = 1.785 Mg m3
Monoclinic, P2111Mo Kα radiation, λ = 0.71073 Å
a = 11.8565 (8) ÅCell parameters from 6756 reflections
b = 14.2444 (11) Åθ = 3.5–28.7°
c = 6.2171 (4) ŵ = 0.59 mm1
β = 90°T = 266 K
V = 1050.00 (13) Å3Prism, clear colourless
Z = 40.48 × 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 Source4178 reflections with I 2u(I)
Graphite monochromatorRint = 0.051
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.770, Tmax = 1.000l = 88
18373 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.08Δρmax = 0.32 e Å3
5157 reflectionsΔρmin = 0.38 e Å3
386 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
3 restraintsAbsolute structure parameter: 0.02 (2)
24 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00071 (19)0.00025 (14)0.0459 (2)0.0554 (5)
K20.50010 (7)0.00022 (5)0.15947 (9)0.03272 (15)
Na10.23142 (10)0.00689 (8)0.52173 (18)0.0274 (3)
Na20.23172 (10)0.00687 (8)0.52034 (18)0.0270 (3)
O110.12014 (17)0.10898 (14)0.3501 (3)0.0256 (4)
O120.12011 (17)0.10912 (14)0.3495 (3)0.0261 (4)
O210.21020 (19)0.20293 (14)0.1188 (3)0.0306 (5)
O220.21030 (19)0.20281 (14)0.1183 (3)0.0309 (5)
O310.2315 (2)0.40640 (15)0.8149 (3)0.0368 (5)
O320.2329 (2)0.40640 (15)0.8141 (3)0.0363 (5)
O410.05214 (19)0.36130 (16)0.8448 (3)0.0351 (5)
O420.05297 (19)0.36191 (16)0.8447 (3)0.0354 (5)
O510.16378 (18)0.35722 (14)0.3246 (3)0.0264 (5)
H510.188 (3)0.342 (3)0.216 (6)0.0396 (7)*
O520.16373 (19)0.35729 (14)0.3238 (3)0.0269 (5)
H520.190 (3)0.344 (3)0.204 (6)0.0404 (7)*
O610.29535 (18)0.24816 (15)0.6301 (3)0.0285 (5)
H610.327 (3)0.285 (2)0.587 (6)0.0428 (7)*
O620.29555 (18)0.24831 (15)0.6280 (3)0.0296 (5)
H620.328 (3)0.295 (2)0.600 (6)0.0444 (7)*
O710.39566 (19)0.08237 (17)0.4844 (4)0.0333 (5)
H170.371 (4)0.127 (3)0.522 (7)0.0500 (8)*
H270.436 (4)0.090 (3)0.376 (6)0.0500 (8)*
O720.39570 (19)0.08231 (17)0.4851 (4)0.0336 (5)
H470.429 (3)0.096 (3)0.369 (6)0.0505 (8)*
H370.372 (4)0.131 (3)0.532 (6)0.0505 (8)*
O810.2429 (2)0.04159 (18)0.8850 (3)0.0461 (7)
H180.236 (4)0.096 (3)0.945 (7)0.0692 (10)*
H280.255 (5)0.001 (3)0.984 (8)0.0692 (10)*
O820.2416 (3)0.04120 (18)0.8832 (3)0.0469 (7)
H480.255 (5)0.001 (3)0.982 (8)0.0704 (10)*
H380.236 (4)0.093 (3)0.948 (7)0.0704 (10)*
O910.0611 (2)0.1971 (2)0.0348 (5)0.0547 (8)
H290.034 (5)0.254 (4)0.081 (7)0.0820 (11)*
H190.113 (5)0.209 (4)0.021 (8)0.0820 (11)*
O920.0610 (2)0.1959 (2)0.0339 (4)0.0517 (7)
H390.118 (5)0.231 (4)0.005 (8)0.0776 (11)*
H490.032 (5)0.250 (3)0.081 (7)0.0776 (11)*
O1010.0758 (2)0.1032 (2)0.5802 (5)0.0544 (7)
H2100.070 (4)0.142 (4)0.700 (8)0.0815 (11)*
H1100.017 (5)0.108 (3)0.519 (7)0.0815 (11)*
O1020.0769 (2)0.1044 (2)0.5757 (5)0.0508 (7)
H4100.052 (4)0.088 (4)0.682 (7)0.0762 (11)*
H3100.012 (5)0.103 (3)0.525 (7)0.0762 (11)*
C110.1544 (2)0.1878 (2)0.2846 (4)0.0217 (6)
C210.1249 (2)0.27288 (19)0.4233 (4)0.0213 (6)
H210.042 (3)0.273 (2)0.434 (4)0.0255 (7)*
C310.1778 (2)0.2640 (2)0.6468 (4)0.0227 (6)
H310.147 (3)0.211 (2)0.725 (5)0.0272 (7)*
C410.1518 (3)0.3512 (2)0.7809 (4)0.0271 (6)
C120.1543 (2)0.1876 (2)0.2845 (4)0.0215 (6)
C220.1251 (2)0.27343 (19)0.4226 (4)0.0209 (6)
H220.038 (3)0.276 (2)0.438 (4)0.0251 (7)*
C320.1782 (2)0.2644 (2)0.6453 (4)0.0229 (6)
H320.146 (3)0.206 (2)0.722 (5)0.0275 (7)*
C420.1523 (3)0.3512 (2)0.7791 (4)0.0272 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0667 (11)0.0552 (12)0.0442 (10)0.0309 (11)0.0019 (12)0.0005 (9)
K20.0320 (3)0.0377 (3)0.0285 (3)0.0036 (3)0.0004 (3)0.0003 (2)
Na10.0261 (6)0.0252 (6)0.0310 (6)0.0007 (5)0.0009 (5)0.0013 (4)
Na20.0260 (6)0.0249 (6)0.0302 (6)0.0005 (5)0.0014 (5)0.0005 (4)
O110.0280 (11)0.0206 (11)0.0281 (10)0.0019 (8)0.0010 (8)0.0007 (8)
O120.0288 (11)0.0218 (11)0.0277 (10)0.0018 (8)0.0007 (8)0.0010 (8)
O210.0396 (12)0.0289 (12)0.0231 (10)0.0004 (10)0.0074 (9)0.0010 (8)
O220.0400 (12)0.0276 (11)0.0251 (10)0.0001 (10)0.0071 (9)0.0019 (8)
O310.0487 (14)0.0277 (12)0.0338 (11)0.0082 (11)0.0040 (10)0.0066 (9)
O320.0476 (14)0.0274 (12)0.0340 (11)0.0071 (11)0.0034 (10)0.0068 (8)
O410.0344 (12)0.0441 (14)0.0267 (10)0.0125 (10)0.0001 (9)0.0065 (9)
O420.0361 (12)0.0420 (14)0.0280 (11)0.0128 (10)0.0012 (9)0.0084 (9)
O510.0391 (12)0.0198 (11)0.0204 (10)0.0014 (9)0.0011 (9)0.0002 (8)
O520.0401 (12)0.0213 (11)0.0194 (9)0.0002 (9)0.0006 (9)0.0003 (8)
O610.0239 (12)0.0270 (13)0.0347 (12)0.0042 (9)0.0041 (9)0.0014 (9)
O620.0244 (11)0.0269 (12)0.0376 (12)0.0035 (9)0.0038 (9)0.0012 (9)
O710.0274 (12)0.0320 (13)0.0406 (13)0.0011 (10)0.0084 (10)0.0018 (10)
O720.0308 (12)0.0295 (13)0.0406 (13)0.0007 (10)0.0065 (10)0.0015 (10)
O810.085 (2)0.0267 (13)0.0264 (11)0.0097 (13)0.0059 (12)0.0002 (9)
O820.089 (2)0.0256 (13)0.0257 (11)0.0109 (13)0.0044 (13)0.0008 (9)
O910.0346 (15)0.084 (2)0.0453 (16)0.0075 (15)0.0097 (12)0.0083 (14)
O920.0328 (14)0.076 (2)0.0460 (15)0.0034 (13)0.0081 (11)0.0062 (14)
O1010.0321 (14)0.0588 (18)0.072 (2)0.0145 (12)0.0142 (13)0.0263 (14)
O1020.0291 (14)0.0560 (17)0.0672 (19)0.0126 (12)0.0106 (13)0.0201 (15)
C110.0190 (13)0.0245 (16)0.0215 (13)0.0030 (11)0.0055 (11)0.0013 (10)
C210.0229 (15)0.0191 (14)0.0218 (13)0.0013 (11)0.0008 (11)0.0008 (10)
C310.0243 (15)0.0218 (15)0.0219 (13)0.0017 (11)0.0007 (11)0.0023 (11)
C410.0387 (17)0.0251 (16)0.0176 (13)0.0044 (13)0.0054 (12)0.0006 (10)
C120.0213 (14)0.0224 (15)0.0207 (13)0.0022 (11)0.0049 (11)0.0001 (10)
C220.0243 (15)0.0188 (14)0.0197 (13)0.0006 (11)0.0001 (11)0.0002 (10)
C320.0227 (14)0.0232 (15)0.0229 (13)0.0007 (11)0.0008 (11)0.0002 (11)
C420.0393 (18)0.0241 (16)0.0182 (13)0.0031 (13)0.0052 (12)0.0018 (10)
Geometric parameters (Å, º) top
K1—O112.828 (3)O21—C111.244 (3)
K1—O122.832 (3)O22—C121.247 (3)
K1—O81i3.099 (4)O31—C411.248 (4)
K1—H28i3.04 (5)O32—C421.257 (4)
K1—O82i3.101 (4)O41—C411.255 (4)
K1—H48i3.06 (6)O42—C421.255 (4)
K1—O912.937 (4)O51—H510.76 (4)
K1—O922.931 (4)O51—C211.426 (3)
K1—O101i3.365 (4)O52—H520.83 (4)
K1—H210i3.07 (5)O52—C221.419 (3)
K1—O102i3.409 (4)O61—H610.70 (3)
K1—H410i2.66 (5)O61—C311.416 (4)
K2—O41ii2.845 (2)O62—H620.78 (3)
K2—O42iii2.848 (2)O62—C321.414 (4)
K2—O51iv2.991 (2)O71—H170.74 (4)
K2—O52v2.993 (2)O71—H270.83 (4)
K2—O71i2.794 (2)O72—H470.84 (4)
K2—H17i3.09 (4)O72—H370.80 (4)
K2—O72vi2.791 (2)O81—H180.86 (5)
K2—H37vi3.08 (4)O81—H280.86 (5)
K2—O81i3.118 (3)O82—H480.87 (5)
K2—H28i3.04 (5)O82—H380.85 (5)
K2—O82vi3.130 (3)O91—H290.91 (5)
K2—H48vi3.03 (6)O91—H190.72 (5)
Na1—O112.368 (2)O92—H390.87 (5)
Na1—O32iii2.462 (2)O92—H490.90 (5)
Na1—O52iii2.493 (2)O101—H2100.93 (5)
Na1—O712.337 (3)O101—H1100.79 (5)
Na1—O812.365 (2)O102—H4100.76 (4)
Na1—O1012.328 (3)O102—H3100.83 (5)
Na1—C42iii3.079 (3)C11—C211.528 (4)
Na2—O122.368 (2)C21—H210.98 (3)
Na2—O31vii2.463 (2)C21—C311.529 (4)
Na2—O51vii2.492 (2)C31—H310.98 (3)
Na2—O722.333 (3)C31—C411.527 (4)
Na2—O822.361 (2)C12—C221.534 (4)
Na2—O1022.327 (3)C22—H221.04 (3)
Na2—C41vii3.083 (3)C22—C321.526 (4)
O11—C111.261 (3)C32—H321.03 (3)
O12—C121.256 (3)C32—C421.522 (4)
Na2i—K1—Na1i80.19 (3)O52iii—Na1—O11173.23 (8)
O11—K1—Na1i101.66 (7)O52iii—Na1—O32iii81.49 (8)
O11—K1—Na2i145.12 (8)O71—Na1—K1viii126.85 (8)
O12—K1—Na1i145.43 (8)O71—Na1—K2viii47.99 (6)
O12—K1—Na2i101.33 (7)O71—Na1—O1192.30 (8)
O12—K1—O1196.25 (7)O71—Na1—O32iii92.60 (9)
O81i—K1—Na1i33.00 (5)O71—Na1—O52iii92.59 (9)
O81i—K1—Na2i110.24 (6)O81—Na1—K1viii45.53 (8)
O81i—K1—O1169.27 (8)O81—Na1—K2viii55.88 (7)
O81i—K1—O12142.11 (11)O81—Na1—O11105.02 (9)
H28i—K1—Na1i42.8 (10)O81—Na1—O32iii161.09 (10)
H28i—K1—Na2i122.9 (10)O81—Na1—O52iii80.19 (9)
H28i—K1—O1165.5 (9)O81—Na1—O7183.59 (10)
H28i—K1—O12126.0 (10)O101—Na1—K1viii51.96 (9)
H28i—K1—O81i16.1 (10)O101—Na1—K2viii127.31 (8)
O82i—K1—Na1i109.98 (6)O101—Na1—O1192.26 (9)
O82i—K1—Na2i32.67 (5)O101—Na1—O32iii88.46 (10)
O82i—K1—O11141.74 (11)O101—Na1—O52iii82.98 (9)
O82i—K1—O1269.26 (8)O101—Na1—O71175.24 (11)
O82i—K1—O81i142.13 (8)O101—Na1—O8193.92 (11)
O82i—K1—H28i151.5 (9)C42iii—Na1—K1viii140.11 (7)
H48i—K1—Na1i122.5 (10)C42iii—Na1—K2viii87.60 (6)
H48i—K1—Na2i42.4 (10)C42iii—Na1—O11115.68 (8)
H48i—K1—O11125.5 (10)C42iii—Na1—O32iii22.94 (7)
H48i—K1—O1265.7 (9)C42iii—Na1—O52iii60.08 (7)
H48i—K1—O81i151.1 (10)C42iii—Na1—O7185.61 (9)
H48i—K1—H28i165.2 (10)C42iii—Na1—O81138.19 (10)
H48i—K1—O82i16.3 (10)C42iii—Na1—O10193.63 (11)
O91—K1—Na1i72.04 (7)K2ix—Na2—K1viii98.05 (4)
O91—K1—Na2i92.84 (7)O12—Na2—K1viii88.04 (7)
O91—K1—O11121.14 (11)O12—Na2—K2ix133.92 (6)
O91—K1—O1273.39 (8)O31vii—Na2—K1viii140.63 (7)
O91—K1—O81i84.42 (10)O31vii—Na2—K2ix108.17 (7)
O91—K1—H28i75.0 (9)O31vii—Na2—O1293.99 (8)
O91—K1—O82i89.47 (9)O51vii—Na2—K1viii92.50 (7)
O91—K1—H48i103.0 (9)O51vii—Na2—K2ix52.65 (5)
O92—K1—Na1i92.96 (7)O51vii—Na2—O12173.24 (8)
O92—K1—Na2i71.74 (7)O51vii—Na2—O31vii81.33 (7)
O92—K1—O1173.39 (8)O72—Na2—K1viii126.58 (8)
O92—K1—O12120.59 (11)O72—Na2—K2ix47.91 (6)
O92—K1—O81i89.61 (9)O72—Na2—O1292.51 (8)
O92—K1—H28i102.8 (9)O72—Na2—O31vii92.66 (9)
O92—K1—O82i83.83 (10)O72—Na2—O51vii92.57 (9)
O92—K1—H48i74.0 (9)O82—Na2—K1viii45.14 (8)
O92—K1—O91160.41 (10)O82—Na2—K2ix56.20 (8)
O101i—K1—Na1i33.02 (5)O82—Na2—O12104.69 (9)
O101i—K1—Na2i61.53 (6)O82—Na2—O31vii161.08 (10)
O101i—K1—O11133.02 (10)O82—Na2—O51vii80.30 (8)
O101i—K1—O12117.95 (9)O82—Na2—O7283.71 (10)
O101i—K1—O81i63.95 (8)O102—Na2—K1viii52.63 (9)
O101i—K1—H28i68.3 (9)O102—Na2—K2ix127.24 (8)
O101i—K1—O82i83.25 (7)O102—Na2—O1292.39 (9)
O101i—K1—H48i98.8 (10)O102—Na2—O31vii88.00 (10)
O101i—K1—O9151.16 (8)O102—Na2—O51vii82.62 (9)
O101i—K1—O92109.59 (9)O102—Na2—O72175.00 (11)
H210i—K1—Na1i43.5 (9)O102—Na2—O8294.08 (11)
H210i—K1—Na2i69.7 (9)C41vii—Na2—K1viii140.25 (7)
H210i—K1—O11134.2 (9)C41vii—Na2—K2ix87.67 (6)
H210i—K1—O12104.1 (10)C41vii—Na2—O12115.81 (8)
H210i—K1—O81i69.5 (9)C41vii—Na2—O31vii22.65 (7)
H210i—K1—H28i69.3 (13)C41vii—Na2—O51vii60.18 (7)
H210i—K1—O82i84.1 (9)C41vii—Na2—O7285.79 (9)
H210i—K1—H48i100.3 (14)C41vii—Na2—O82138.49 (10)
H210i—K1—O9135.4 (10)C41vii—Na2—O10292.97 (11)
H210i—K1—O92125.2 (10)Na1—O11—K1101.36 (8)
H210i—K1—O101i15.7 (9)C11—O11—K1115.77 (16)
O102i—K1—Na1i61.73 (5)C11—O11—Na1125.94 (17)
O102i—K1—Na2i32.86 (5)Na2—O12—K1101.50 (9)
O102i—K1—O11117.91 (9)C12—O12—K1115.89 (16)
O102i—K1—O12132.44 (10)C12—O12—Na2125.79 (17)
O102i—K1—O81i83.63 (7)C41—O31—Na2ii107.87 (17)
O102i—K1—H28i99.1 (10)C42—O32—Na1x107.30 (17)
O102i—K1—O82i63.41 (8)C41—O41—K2vii120.07 (19)
O102i—K1—H48i67.5 (9)C42—O42—K2x120.97 (19)
O102i—K1—O91109.69 (9)Na2ii—O51—K2xi85.87 (7)
O102i—K1—O9250.96 (8)H51—O51—K2xi98 (3)
O102i—K1—O101i61.56 (7)H51—O51—Na2ii112 (3)
O102i—K1—H210i76.0 (9)C21—O51—K2xi120.68 (16)
H410i—K1—Na1i60.8 (11)C21—O51—Na2ii130.46 (15)
H410i—K1—Na2i35.8 (11)C21—O51—H51105 (3)
H410i—K1—O11115.1 (11)Na1x—O52—K2xii85.83 (7)
H410i—K1—O12135.0 (11)H52—O52—K2xii96 (3)
H410i—K1—O81i81.5 (11)H52—O52—Na1x109 (3)
H410i—K1—H28i97.1 (15)C22—O52—K2xii120.70 (16)
H410i—K1—O82i66.1 (11)C22—O52—Na1x130.36 (15)
H410i—K1—H48i69.8 (15)C22—O52—H52109 (3)
H410i—K1—O91111.4 (11)C31—O61—H61116 (3)
H410i—K1—O9249.1 (11)C32—O62—H62111 (3)
H410i—K1—O101i62.5 (11)Na1—O71—K2viii93.58 (9)
H410i—K1—H210i77.3 (14)H17—O71—K2viii107 (3)
H410i—K1—O102i3.0 (11)H17—O71—Na196 (4)
Na2vi—K2—Na1i116.09 (3)H27—O71—K2viii116 (3)
O41ii—K2—Na1i124.45 (6)H27—O71—Na1129 (3)
O41ii—K2—Na2vi99.40 (5)H27—O71—H17112 (4)
O42iii—K2—Na1i99.03 (5)O71—H17—K2viii60 (3)
O42iii—K2—Na2vi124.71 (6)Na2—O72—K2ix93.75 (8)
O42iii—K2—O41ii93.15 (6)H47—O72—K2ix124 (3)
O51iv—K2—Na1i112.80 (5)H47—O72—Na2126 (3)
O51iv—K2—Na2vi41.48 (4)H37—O72—K2ix103 (3)
O51iv—K2—O41ii67.96 (6)H37—O72—Na298 (3)
O51iv—K2—O42iii148.13 (7)H37—O72—H47106 (4)
O52v—K2—Na1i41.48 (4)O72—H37—K2ix62 (3)
O52v—K2—Na2vi112.72 (5)K2viii—O81—K1viii153.96 (10)
O52v—K2—O41ii147.84 (7)Na1—O81—K1viii101.47 (10)
O52v—K2—O42iii67.70 (6)Na1—O81—K2viii85.22 (8)
O52v—K2—O51iv139.96 (6)H18—O81—K1viii87 (3)
O71i—K2—Na1i38.43 (5)H18—O81—K2viii108 (3)
O71i—K2—Na2vi86.82 (5)H18—O81—Na1132 (3)
O71i—K2—O41ii110.52 (7)H28—O81—K1viii78 (4)
O71i—K2—O42iii137.45 (7)H28—O81—K2viii77 (4)
O71i—K2—O51iv74.38 (6)H28—O81—Na1120 (3)
O71i—K2—O52v74.16 (6)H28—O81—H18108 (4)
H17i—K2—Na1i42.0 (8)K2viii—H28—K1viii170 (2)
H17i—K2—Na2vi93.6 (8)O81—H28—K1viii86 (4)
H17i—K2—O41ii98.2 (8)O81—H28—K2viii87 (4)
H17i—K2—O42iii137.5 (8)K2ix—O82—K1viii153.98 (10)
H17i—K2—O51iv72.7 (8)Na2—O82—K1viii102.19 (11)
H17i—K2—O52v81.8 (8)Na2—O82—K2ix84.99 (8)
H17i—K2—O71i13.2 (8)H48—O82—K1viii79 (4)
O72vi—K2—Na1i86.92 (5)H48—O82—K2ix76 (4)
O72vi—K2—Na2vi38.34 (5)H48—O82—Na2119 (3)
O72vi—K2—O41ii137.74 (7)H38—O82—K1viii86 (3)
O72vi—K2—O42iii110.53 (7)H38—O82—K2ix106 (3)
O72vi—K2—O51iv74.14 (6)H38—O82—Na2135 (3)
O72vi—K2—O52v74.39 (6)H38—O82—H48107 (4)
O72vi—K2—O71i75.23 (7)K2ix—H48—K1viii171 (2)
O72vi—K2—H17i87.5 (8)O82—H48—K1viii85 (4)
H37vi—K2—Na1i94.2 (8)O82—H48—K2ix88 (4)
H37vi—K2—Na2vi42.9 (8)H29—O91—K1144 (3)
H37vi—K2—O41ii137.9 (8)H19—O91—K1111 (4)
H37vi—K2—O42iii96.7 (8)H19—O91—H29103 (6)
H37vi—K2—O51iv83.0 (8)H39—O92—K1134 (3)
H37vi—K2—O52v72.2 (8)H49—O92—K1142 (3)
H37vi—K2—O71i88.8 (8)H49—O92—H3983 (5)
H37vi—K2—H17i101.5 (10)Na1—O101—K1viii95.02 (11)
H37vi—K2—O72vi14.7 (8)H210—O101—K1viii64 (3)
O81i—K2—Na1i38.90 (5)H210—O101—Na1122 (3)
O81i—K2—Na2vi150.56 (5)H110—O101—K1viii103 (3)
O81i—K2—O41ii91.16 (7)H110—O101—Na1132 (3)
O81i—K2—O42iii81.59 (7)H110—O101—H210106 (4)
O81i—K2—O51iv122.46 (7)O101—H210—K1viii101 (3)
O81i—K2—O52v61.58 (6)Na2—O102—K1viii94.51 (11)
O81i—K2—O71i63.74 (7)H410—O102—Na2105 (4)
O81i—K2—H17i57.5 (8)H310—O102—K1viii94 (3)
O81i—K2—O72vi125.63 (7)H310—O102—Na2131 (3)
O81i—K2—H37vi130.7 (8)H310—O102—H41088 (4)
H28i—K2—Na1i49.0 (10)O102—H410—K1viii167 (5)
H28i—K2—Na2vi164.9 (10)O21—C11—O11126.4 (3)
H28i—K2—O41ii90.2 (9)C21—C11—O11116.8 (2)
H28i—K2—O42iii65.7 (10)C21—C11—O21116.9 (2)
H28i—K2—O51iv136.0 (9)C11—C21—O51110.6 (2)
H28i—K2—O52v58.7 (9)H21—C21—O51110.1 (17)
H28i—K2—O71i78.9 (10)H21—C21—C11105.7 (17)
H28i—K2—H17i73.4 (13)C31—C21—O51109.2 (2)
H28i—K2—O72vi131.0 (9)C31—C21—C11110.7 (2)
H28i—K2—H37vi131.0 (12)C31—C21—H21110.5 (16)
H28i—K2—O81i16.0 (10)C21—C31—O61110.5 (2)
O82vi—K2—Na1i150.48 (5)H31—C31—O61106 (2)
O82vi—K2—Na2vi38.81 (5)H31—C31—C21111.5 (18)
O82vi—K2—O41ii81.96 (7)C41—C31—O61111.6 (2)
O82vi—K2—O42iii91.57 (7)C41—C31—C21110.2 (2)
O82vi—K2—O51iv61.47 (6)C41—C31—H31106.7 (18)
O82vi—K2—O52v122.39 (7)O31—C41—Na2ii49.48 (14)
O82vi—K2—O71i125.44 (7)O41—C41—Na2ii122.6 (2)
O82vi—K2—H17i130.5 (8)O41—C41—O31126.0 (3)
O82vi—K2—O72vi63.56 (7)C31—C41—Na2ii96.41 (17)
O82vi—K2—H37vi57.0 (8)C31—C41—O31116.9 (3)
O82vi—K2—O81i170.05 (6)C31—C41—O41117.1 (3)
O82vi—K2—H28i155.6 (10)O22—C12—O12126.3 (3)
H48vi—K2—Na1i164.9 (10)C22—C12—O12117.2 (2)
H48vi—K2—Na2vi48.9 (10)C22—C12—O22116.5 (2)
H48vi—K2—O41ii65.9 (10)C12—C22—O52110.8 (2)
H48vi—K2—O42iii90.9 (9)H22—C22—O52109.0 (16)
H48vi—K2—O51iv58.4 (9)H22—C22—C12107.9 (16)
H48vi—K2—O52v136.2 (9)C32—C22—O52109.3 (2)
H48vi—K2—O71i130.7 (9)C32—C22—C12110.4 (2)
H48vi—K2—H17i131.1 (12)C32—C22—H22109.4 (15)
H48vi—K2—O72vi78.9 (10)C22—C32—O62110.5 (2)
H48vi—K2—H37vi73.2 (13)H32—C32—O62105.6 (19)
H48vi—K2—O81i155.5 (10)H32—C32—C22109.5 (17)
H48vi—K2—H28i146.1 (10)C42—C32—O62111.8 (2)
H48vi—K2—O82vi16.2 (10)C42—C32—C22110.1 (2)
K2viii—Na1—K1viii98.08 (4)C42—C32—H32109.2 (17)
O11—Na1—K1viii88.38 (7)O32—C42—Na1x49.76 (14)
O11—Na1—K2viii133.82 (6)O42—C42—Na1x122.53 (19)
O32iii—Na1—K1viii140.42 (7)O42—C42—O32125.6 (3)
O32iii—Na1—K2viii108.39 (7)C32—C42—Na1x96.37 (16)
O32iii—Na1—O1193.61 (8)C32—C42—O32116.7 (3)
O52iii—Na1—K1viii92.43 (7)C32—C42—O42117.8 (3)
O52iii—Na1—K2viii52.70 (5)
K1—O11—C11—O2151.6 (2)Na2ii—O51—C21—C3111.7 (2)
K1—O11—C11—C21128.74 (17)Na2ii—C41—C31—O6162.82 (16)
K1—O12—C12—O2251.9 (2)Na2ii—C41—C31—C2160.34 (17)
K1—O12—C12—C22128.32 (17)O11—C11—C21—O51177.1 (2)
K2vii—O41—C41—Na2ii73.26 (16)O11—C11—C21—C3161.8 (3)
K2vii—O41—C41—O3112.5 (2)O12—C12—C22—O52176.8 (2)
K2vii—O41—C41—C31168.28 (18)O12—C12—C22—C3261.9 (3)
K2—O42iii—C42iii—Na172.74 (16)O21—C11—C21—O513.3 (3)
K2x—O42—C42—O3211.8 (2)O21—C11—C21—C31117.8 (3)
K2x—O42—C42—C32168.28 (18)O22—C12—C22—O523.4 (3)
K2xi—O51—C21—C11112.94 (17)O22—C12—C22—C32117.8 (3)
K2xi—O51—C21—C31125.07 (18)O31—C41—C31—O6115.4 (3)
K2xii—O52—C22—C12113.15 (18)O31—C41—C31—C21107.8 (3)
K2xii—O52—C22—C32125.01 (18)O32—C42—C32—O6214.9 (3)
Na1—O11—C11—O2176.7 (2)O32—C42—C32—C22108.3 (3)
Na1—O11—C11—C21102.9 (2)O41—C41—C31—O61165.3 (3)
Na1x—O32—C42—O42105.14 (18)O41—C41—C31—C2171.5 (3)
Na1x—O32—C42—C3274.77 (17)O42—C42—C32—O62165.1 (2)
Na1x—O52—C22—C12133.7 (2)O42—C42—C32—C2271.6 (3)
Na1x—O52—C22—C3211.8 (2)O51—C21—C31—O6168.0 (2)
Na1x—C42—C32—O6262.78 (16)O51—C21—C31—C4155.7 (3)
Na1x—C42—C32—C2260.50 (17)O52—C22—C32—O6268.1 (2)
Na2—O12—C12—O2276.6 (2)O52—C22—C32—C4256.0 (3)
Na2—O12—C12—C22103.1 (2)O61—C31—C21—C1153.9 (3)
Na2ii—O31—C41—O41104.82 (18)O62—C32—C22—C1254.0 (3)
Na2ii—O31—C41—C3174.41 (17)C11—C21—C31—C41177.7 (2)
Na2ii—O51—C21—C11133.7 (2)C12—C22—C32—C42178.1 (2)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (iv) x+1/2, y+1/2, z; (v) x+1/2, y1/2, z; (vi) x+1, y, z1; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (ix) x1, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xii) x1/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O51—H51···O210.76 (4)2.09 (4)2.601 (3)125 (4)
O51—H51···O31i0.76 (4)2.71 (4)3.344 (3)142 (4)
O51—H51···O41i0.76 (4)2.83 (4)3.264 (3)119 (3)
O52—H52···O220.83 (4)2.09 (4)2.604 (3)119 (3)
O52—H52···O32i0.83 (4)2.63 (4)3.347 (3)145 (3)
O52—H52···O42i0.83 (4)2.78 (4)3.256 (3)119 (3)
O61—H61···O102ii0.70 (3)2.19 (3)2.889 (4)175 (4)
O62—H62···O101x0.78 (3)2.16 (3)2.911 (4)160 (4)
O71—H17···O610.74 (4)2.06 (4)2.794 (3)177 (5)
O71—H27···O41ii0.83 (4)2.07 (4)2.877 (3)164 (4)
O72—H47···O42x0.84 (4)2.07 (4)2.883 (3)161 (4)
O72—H37···O620.80 (4)1.99 (5)2.792 (3)173 (4)
O81—H18···O11viii0.86 (5)2.87 (5)3.376 (3)119 (4)
O81—H18···O21viii0.86 (5)1.89 (5)2.746 (3)170 (4)
O81—H28···O32xiii0.86 (5)1.84 (5)2.701 (3)174 (5)
O82—H48···O31xiv0.87 (5)1.83 (5)2.703 (3)174 (5)
O82—H38···O12viii0.85 (5)2.86 (5)3.379 (3)121 (4)
O82—H38···O22viii0.85 (5)1.91 (5)2.753 (3)173 (5)
O91—H29···O42i0.91 (5)1.92 (5)2.811 (4)167 (5)
O91—H19···O22v0.72 (5)2.59 (6)3.106 (4)130 (5)
O91—H19···O32iii0.72 (5)2.67 (6)3.165 (4)128 (5)
O91—H19···O62iii0.72 (5)2.51 (5)3.146 (3)147 (5)
O92—H39···O21xi0.87 (5)2.37 (5)3.117 (4)143 (4)
O92—H39···O31vii0.87 (5)2.88 (5)3.167 (4)101 (4)
O92—H39···O61vii0.87 (5)2.51 (5)3.136 (3)129 (4)
O92—H49···O41i0.90 (5)1.93 (5)2.815 (4)170 (5)
O101—H210···O91viii0.93 (5)1.83 (5)2.748 (4)169 (5)
O101—H110···O120.79 (5)1.94 (5)2.731 (3)174 (5)
O102—H410···O92viii0.76 (4)2.34 (5)2.761 (4)116 (5)
O102—H310···O110.83 (5)1.91 (5)2.726 (3)167 (5)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (v) x+1/2, y1/2, z; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xiii) x+1/2, y1/2, z+2; (xiv) x1/2, y+1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (276K_anh) top
Crystal data top
C4H12KNaO10F(000) = 585.519
Mr = 282.22Dx = 1.783 Mg m3
Monoclinic, P2111Mo Kα radiation, λ = 0.71073 Å
a = 11.8629 (9) ÅCell parameters from 6656 reflections
b = 14.2500 (11) Åθ = 3.6–28.7°
c = 6.2199 (4) ŵ = 0.59 mm1
β = 90°T = 276 K
V = 1051.45 (13) Å3Prism, clear colourless
Z = 40.48 × 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 Source4009 reflections with I 2u(I)
Graphite monochromatorRint = 0.053
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.752, Tmax = 1.000l = 88
18369 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.09Δρmax = 0.36 e Å3
5168 reflectionsΔρmin = 0.38 e Å3
386 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
3 restraintsAbsolute structure parameter: 0.09 (3)
24 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.0009 (2)0.00035 (15)0.0460 (3)0.0593 (6)
K20.49999 (8)0.00023 (5)0.15928 (10)0.03526 (16)
Na10.23142 (11)0.00679 (8)0.52233 (19)0.0295 (3)
Na20.23151 (11)0.00682 (9)0.52071 (19)0.0295 (3)
O110.11993 (18)0.10889 (15)0.3506 (3)0.0275 (5)
O120.12008 (18)0.10902 (15)0.3500 (3)0.0283 (5)
O210.2103 (2)0.20285 (15)0.1191 (3)0.0330 (5)
O220.2097 (2)0.20295 (15)0.1180 (3)0.0327 (5)
O310.2318 (2)0.40641 (16)0.8145 (3)0.0391 (6)
O320.2334 (2)0.40611 (16)0.8131 (3)0.0391 (6)
O410.0526 (2)0.36146 (17)0.8445 (3)0.0373 (6)
O420.0533 (2)0.36215 (17)0.8447 (3)0.0376 (6)
O510.1635 (2)0.35704 (15)0.3246 (3)0.0282 (5)
H510.191 (3)0.340 (3)0.221 (6)0.0423 (8)*
O520.1633 (2)0.35732 (15)0.3238 (3)0.0289 (5)
H520.191 (3)0.344 (3)0.206 (6)0.0433 (8)*
O610.29519 (19)0.24801 (16)0.6294 (4)0.0310 (5)
H610.328 (3)0.289 (3)0.597 (7)0.0465 (8)*
O620.29572 (19)0.24827 (16)0.6274 (4)0.0311 (5)
H620.328 (3)0.293 (2)0.603 (6)0.0467 (8)*
O710.3954 (2)0.08225 (18)0.4845 (4)0.0354 (6)
H170.375 (4)0.127 (3)0.516 (7)0.0531 (9)*
H270.438 (4)0.092 (3)0.373 (7)0.0531 (9)*
O720.3958 (2)0.08223 (18)0.4851 (4)0.0354 (6)
H470.431 (4)0.094 (3)0.368 (7)0.0531 (8)*
H370.369 (4)0.131 (3)0.527 (7)0.0531 (8)*
O810.2433 (3)0.0416 (2)0.8849 (4)0.0488 (7)
H180.237 (4)0.097 (3)0.955 (7)0.0732 (11)*
H280.254 (5)0.004 (4)0.988 (9)0.0732 (11)*
O820.2422 (3)0.04122 (19)0.8841 (4)0.0500 (8)
H480.255 (5)0.001 (4)0.986 (9)0.0750 (11)*
H380.235 (5)0.095 (4)0.949 (7)0.0750 (11)*
O910.0615 (2)0.1975 (3)0.0347 (5)0.0586 (8)
H290.035 (5)0.252 (4)0.081 (8)0.0879 (12)*
H190.119 (5)0.223 (4)0.003 (9)0.0879 (12)*
O920.0610 (2)0.1963 (3)0.0340 (5)0.0559 (8)
H390.115 (5)0.221 (4)0.004 (9)0.0839 (12)*
H490.039 (5)0.258 (4)0.084 (7)0.0839 (12)*
O1010.0754 (2)0.1025 (2)0.5815 (5)0.0587 (8)
H2100.073 (5)0.143 (4)0.693 (8)0.0880 (13)*
H1100.015 (5)0.107 (4)0.520 (7)0.0880 (13)*
O1020.0768 (2)0.1042 (2)0.5771 (5)0.0546 (8)
H4100.047 (5)0.086 (4)0.681 (8)0.0818 (12)*
H3100.010 (5)0.101 (3)0.527 (7)0.0818 (12)*
C110.1542 (2)0.1878 (2)0.2849 (4)0.0229 (6)
C210.1248 (3)0.2732 (2)0.4234 (4)0.0230 (6)
H210.043 (3)0.275 (2)0.438 (5)0.0276 (7)*
C310.1778 (3)0.2641 (2)0.6466 (5)0.0250 (7)
H310.145 (3)0.205 (2)0.727 (5)0.0300 (8)*
C410.1516 (3)0.3512 (2)0.7810 (5)0.0298 (7)
C120.1543 (2)0.1877 (2)0.2839 (4)0.0236 (6)
C220.1252 (3)0.2729 (2)0.4224 (4)0.0224 (6)
H220.039 (3)0.277 (2)0.439 (4)0.0269 (7)*
C320.1783 (3)0.2642 (2)0.6458 (5)0.0241 (6)
H320.147 (3)0.212 (2)0.725 (5)0.0290 (8)*
C420.1525 (3)0.3514 (2)0.7798 (5)0.0294 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0698 (12)0.0605 (14)0.0474 (11)0.0335 (12)0.0022 (14)0.0004 (10)
K20.0346 (3)0.0402 (4)0.0310 (3)0.0034 (3)0.0003 (3)0.0002 (3)
Na10.0286 (7)0.0265 (7)0.0336 (6)0.0002 (5)0.0013 (5)0.0008 (5)
Na20.0281 (7)0.0276 (7)0.0329 (6)0.0010 (5)0.0016 (5)0.0004 (5)
O110.0307 (12)0.0226 (12)0.0292 (11)0.0029 (9)0.0014 (9)0.0007 (8)
O120.0311 (12)0.0248 (13)0.0290 (11)0.0014 (9)0.0008 (9)0.0009 (9)
O210.0425 (13)0.0306 (13)0.0259 (11)0.0002 (11)0.0082 (10)0.0013 (9)
O220.0416 (13)0.0309 (13)0.0256 (11)0.0003 (11)0.0075 (10)0.0013 (9)
O310.0502 (15)0.0321 (14)0.0349 (12)0.0072 (12)0.0047 (11)0.0081 (9)
O320.0512 (15)0.0293 (13)0.0367 (12)0.0089 (12)0.0038 (11)0.0070 (9)
O410.0382 (13)0.0452 (15)0.0285 (11)0.0131 (11)0.0007 (10)0.0079 (10)
O420.0379 (13)0.0457 (15)0.0293 (12)0.0112 (11)0.0010 (10)0.0072 (10)
O510.0404 (14)0.0211 (12)0.0231 (11)0.0001 (9)0.0005 (9)0.0004 (8)
O520.0422 (14)0.0218 (12)0.0227 (10)0.0010 (10)0.0001 (9)0.0006 (9)
O610.0263 (13)0.0296 (14)0.0371 (12)0.0040 (10)0.0049 (10)0.0002 (10)
O620.0259 (13)0.0284 (13)0.0390 (13)0.0045 (10)0.0053 (10)0.0016 (10)
O710.0306 (13)0.0323 (14)0.0433 (14)0.0002 (11)0.0073 (10)0.0026 (11)
O720.0297 (13)0.0329 (14)0.0436 (14)0.0003 (10)0.0079 (11)0.0023 (11)
O810.090 (2)0.0305 (15)0.0263 (12)0.0100 (14)0.0053 (14)0.0000 (10)
O820.095 (2)0.0281 (14)0.0272 (12)0.0112 (15)0.0035 (14)0.0001 (10)
O910.0381 (16)0.089 (3)0.0484 (17)0.0077 (16)0.0073 (13)0.0074 (16)
O920.0366 (16)0.082 (2)0.0496 (16)0.0045 (15)0.0083 (13)0.0054 (15)
O1010.0341 (16)0.064 (2)0.078 (2)0.0162 (13)0.0175 (14)0.0307 (16)
O1020.0308 (15)0.0588 (19)0.074 (2)0.0124 (13)0.0113 (14)0.0211 (16)
C110.0204 (15)0.0258 (17)0.0225 (14)0.0026 (12)0.0054 (12)0.0017 (11)
C210.0268 (17)0.0210 (16)0.0213 (14)0.0002 (12)0.0005 (12)0.0010 (11)
C310.0267 (16)0.0257 (17)0.0226 (14)0.0045 (13)0.0004 (12)0.0008 (12)
C410.042 (2)0.0280 (18)0.0199 (14)0.0046 (15)0.0049 (14)0.0001 (12)
C120.0222 (15)0.0260 (17)0.0228 (14)0.0031 (12)0.0045 (12)0.0001 (12)
C220.0238 (16)0.0212 (16)0.0223 (14)0.0004 (12)0.0014 (12)0.0007 (11)
C320.0261 (16)0.0240 (17)0.0223 (14)0.0010 (13)0.0021 (12)0.0013 (12)
C420.042 (2)0.0274 (18)0.0192 (14)0.0041 (15)0.0051 (14)0.0003 (11)
Geometric parameters (Å, º) top
K1—O112.829 (3)O22—C121.243 (4)
K1—O122.835 (3)O31—C411.252 (4)
K1—O81i3.104 (4)O32—C421.254 (4)
K1—H28i3.03 (6)O41—C411.248 (4)
K1—O82i3.109 (4)O42—C421.253 (4)
K1—H48i3.06 (6)O51—H510.76 (4)
K1—O912.943 (4)O51—C211.421 (4)
K1—O922.939 (4)O52—H520.83 (4)
K1—O101i3.353 (4)O52—C221.423 (4)
K1—O102i3.403 (4)O61—H610.73 (3)
K1—H410i2.64 (5)O61—C311.416 (4)
K2—O41ii2.847 (2)O62—H620.76 (3)
K2—O42iii2.847 (2)O62—C321.416 (4)
K2—O51iv2.993 (2)O71—H170.70 (5)
K2—O52v2.990 (2)O71—H270.87 (4)
K2—O71i2.796 (3)O72—H470.86 (4)
K2—H17i3.08 (5)O72—H370.81 (5)
K2—O72vi2.793 (3)O81—H180.91 (5)
K2—O81i3.114 (3)O81—H280.84 (6)
K2—H28i3.06 (6)O82—H480.87 (6)
K2—O82vi3.126 (3)O82—H380.87 (5)
K2—H48vi3.04 (6)O91—H290.89 (5)
Na1—O112.368 (2)O91—H190.81 (6)
Na1—O32iii2.463 (3)O92—H390.76 (6)
Na1—O52iii2.496 (3)O92—H490.97 (5)
Na1—O712.335 (3)O101—H2100.90 (5)
Na1—O812.362 (3)O101—H1100.81 (6)
Na1—O1012.329 (3)O102—H4100.78 (5)
Na1—C42iii3.083 (3)O102—H3100.85 (6)
Na2—O122.366 (2)C11—C211.531 (4)
Na2—O31vii2.463 (3)C21—H210.97 (3)
Na2—O51vii2.498 (2)C21—C311.530 (4)
Na2—O722.336 (3)C31—H311.05 (4)
Na2—O822.365 (3)C31—C411.528 (4)
Na2—O1022.327 (3)C12—C221.529 (4)
Na2—C41vii3.089 (4)C22—H221.03 (3)
O11—C111.263 (4)C22—C321.531 (4)
O12—C121.261 (4)C32—H320.97 (4)
O21—C111.246 (4)C32—C421.528 (4)
Na2i—K1—Na1i80.21 (3)O81—Na1—O7183.59 (11)
O11—K1—Na1i101.73 (8)O101—Na1—K1viii51.71 (10)
O11—K1—Na2i145.10 (9)O101—Na1—K2viii127.37 (9)
O12—K1—Na1i145.55 (9)O101—Na1—O1192.01 (10)
O12—K1—Na2i101.35 (8)O101—Na1—O32iii88.50 (11)
O12—K1—O1196.12 (7)O101—Na1—O52iii83.27 (10)
O81i—K1—Na1i32.97 (5)O101—Na1—O71175.37 (12)
O81i—K1—Na2i110.23 (7)O101—Na1—O8193.85 (12)
O81i—K1—O1169.37 (8)C42iii—Na1—K1viii140.15 (8)
O81i—K1—O12142.16 (12)C42iii—Na1—K2viii87.68 (7)
H28i—K1—Na1i43.1 (11)C42iii—Na1—O11115.51 (9)
H28i—K1—Na2i123.2 (11)C42iii—Na1—O32iii22.80 (8)
H28i—K1—O1164.7 (10)C42iii—Na1—O52iii60.11 (8)
H28i—K1—O12126.4 (11)C42iii—Na1—O7185.54 (10)
H28i—K1—O81i15.7 (11)C42iii—Na1—O81138.26 (10)
O82i—K1—Na1i110.14 (7)C42iii—Na1—O10193.89 (12)
O82i—K1—Na2i32.78 (5)K2ix—Na2—K1viii98.11 (4)
O82i—K1—O11141.52 (11)O12—Na2—K1viii88.04 (7)
O82i—K1—O1269.17 (8)O12—Na2—K2ix133.93 (7)
O82i—K1—O81i142.25 (8)O31vii—Na2—K1viii140.60 (8)
O82i—K1—H28i152.3 (10)O31vii—Na2—K2ix108.14 (7)
H48i—K1—Na1i123.0 (11)O31vii—Na2—O1293.97 (8)
H48i—K1—Na2i42.9 (11)O51vii—Na2—K1viii92.63 (7)
H48i—K1—O11125.3 (11)O51vii—Na2—K2ix52.62 (6)
H48i—K1—O1265.1 (10)O51vii—Na2—O12173.24 (9)
H48i—K1—O81i151.7 (10)O51vii—Na2—O31vii81.25 (8)
H48i—K1—H28i166.1 (11)O72—Na2—K1viii126.66 (8)
H48i—K1—O82i16.2 (10)O72—Na2—K2ix47.88 (7)
O91—K1—Na1i72.05 (8)O72—Na2—O1292.56 (9)
O91—K1—Na2i92.90 (8)O72—Na2—O31vii92.60 (10)
O91—K1—O11121.12 (12)O72—Na2—O51vii92.43 (9)
O91—K1—O1273.49 (9)O82—Na2—K1viii45.37 (9)
O91—K1—O81i84.38 (11)O82—Na2—K2ix56.00 (8)
O91—K1—H28i75.9 (9)O82—Na2—O12104.87 (10)
O91—K1—O82i89.60 (9)O82—Na2—O31vii160.90 (10)
O91—K1—H48i102.8 (10)O82—Na2—O51vii80.22 (9)
O92—K1—Na1i92.92 (8)O82—Na2—O7283.59 (11)
O92—K1—Na2i71.72 (8)O102—Na2—K1viii52.49 (10)
O92—K1—O1173.38 (9)O102—Na2—K2ix127.13 (9)
O92—K1—O12120.52 (11)O102—Na2—O1292.47 (10)
O92—K1—O81i89.59 (9)O102—Na2—O31vii88.11 (11)
O92—K1—H28i102.0 (10)O102—Na2—O51vii82.64 (10)
O92—K1—O82i83.80 (11)O102—Na2—O72174.86 (11)
O92—K1—H48i74.5 (9)O102—Na2—O8294.09 (12)
O92—K1—O91160.42 (10)C41vii—Na2—K1viii140.30 (8)
O101i—K1—Na1i33.03 (6)C41vii—Na2—K2ix87.59 (7)
O101i—K1—Na2i61.45 (6)C41vii—Na2—O12115.80 (9)
O101i—K1—O11133.14 (11)C41vii—Na2—O31vii22.67 (8)
O101i—K1—O12118.11 (10)C41vii—Na2—O51vii60.09 (8)
O101i—K1—O81i63.96 (8)C41vii—Na2—O7285.64 (10)
O101i—K1—H28i69.1 (10)C41vii—Na2—O82138.28 (10)
O101i—K1—O82i83.35 (8)C41vii—Na2—O10293.12 (12)
O101i—K1—H48i99.0 (11)Na1—O11—K1101.42 (9)
O101i—K1—O9151.29 (9)C11—O11—K1115.68 (17)
O101i—K1—O92109.46 (9)C11—O11—Na1125.86 (18)
O102i—K1—Na1i61.79 (6)Na2—O12—K1101.59 (9)
O102i—K1—Na2i32.85 (6)C12—O12—K1115.57 (17)
O102i—K1—O11117.90 (9)C12—O12—Na2125.90 (18)
O102i—K1—O12132.40 (11)C41—O31—Na2ii108.01 (19)
O102i—K1—O81i83.66 (8)C42—O32—Na1x107.63 (18)
O102i—K1—H28i99.0 (11)C41—O41—K2vii120.3 (2)
O102i—K1—O82i63.47 (8)C42—O42—K2x121.0 (2)
O102i—K1—H48i68.1 (10)Na2ii—O51—K2xi85.86 (7)
O102i—K1—O91109.79 (9)H51—O51—K2xi102 (3)
O102i—K1—O9250.89 (8)H51—O51—Na2ii111 (3)
O102i—K1—O101i61.51 (7)C21—O51—K2xi120.72 (17)
H410i—K1—Na1i59.4 (12)C21—O51—Na2ii130.41 (17)
H410i—K1—Na2i36.3 (12)C21—O51—H51104 (3)
H410i—K1—O11115.3 (12)Na1x—O52—K2xii85.82 (7)
H410i—K1—O12135.9 (12)H52—O52—K2xii97 (3)
H410i—K1—O81i80.4 (12)H52—O52—Na1x109 (3)
H410i—K1—H28i95.8 (16)C22—O52—K2xii121.12 (17)
H410i—K1—O82i67.0 (12)C22—O52—Na1x130.50 (17)
H410i—K1—H48i71.5 (16)C22—O52—H52108 (3)
H410i—K1—O91110.5 (12)C31—O61—H61115 (3)
H410i—K1—O9250.0 (12)C32—O62—H62112 (3)
H410i—K1—O101i61.2 (12)Na1—O71—K2viii93.58 (9)
H410i—K1—O102i3.5 (12)H17—O71—K2viii108 (4)
Na2vi—K2—Na1i116.16 (3)H17—O71—Na1100 (4)
O41ii—K2—Na1i124.57 (6)H27—O71—K2viii116 (3)
O41ii—K2—Na2vi99.26 (6)H27—O71—Na1130 (3)
O42iii—K2—Na1i98.97 (6)H27—O71—H17107 (5)
O42iii—K2—Na2vi124.74 (6)O71—H17—K2viii60 (3)
O42iii—K2—O41ii93.12 (6)Na2—O72—K2ix93.78 (9)
O51iv—K2—Na1i112.76 (5)H47—O72—K2ix122 (3)
O51iv—K2—Na2vi41.53 (5)H47—O72—Na2126 (3)
O51iv—K2—O41ii67.90 (7)H37—O72—K2ix106 (3)
O51iv—K2—O42iii148.22 (7)H37—O72—Na296 (3)
O52v—K2—Na1i41.55 (5)H37—O72—H47108 (4)
O52v—K2—Na2vi112.64 (5)K2viii—O81—K1viii153.92 (11)
O52v—K2—O41ii148.05 (7)Na1—O81—K1viii101.36 (11)
O52v—K2—O42iii67.70 (7)Na1—O81—K2viii85.35 (8)
O52v—K2—O51iv139.90 (6)H18—O81—K1viii87 (3)
O71i—K2—Na1i38.38 (6)H18—O81—K2viii106 (3)
O71i—K2—Na2vi86.89 (6)H18—O81—Na1135 (3)
O71i—K2—O41ii110.66 (8)H28—O81—K1viii77 (4)
O71i—K2—O42iii137.35 (8)H28—O81—K2viii78 (4)
O71i—K2—O51iv74.39 (7)H28—O81—Na1123 (3)
O71i—K2—O52v74.12 (7)H28—O81—H18102 (4)
H17i—K2—Na1i42.5 (9)K2viii—H28—K1viii169 (2)
H17i—K2—Na2vi92.6 (9)O81—H28—K1viii87 (4)
H17i—K2—O41ii98.7 (9)O81—H28—K2viii86 (4)
H17i—K2—O42iii138.4 (9)K2ix—O82—K1viii154.12 (10)
H17i—K2—O51iv71.9 (9)Na2—O82—K1viii101.85 (11)
H17i—K2—O52v82.2 (9)Na2—O82—K2ix85.15 (9)
H17i—K2—O71i12.6 (8)H48—O82—K1viii79 (4)
O72vi—K2—Na1i86.95 (6)H48—O82—K2ix76 (4)
O72vi—K2—Na2vi38.34 (5)H48—O82—Na2121 (3)
O72vi—K2—O41ii137.60 (8)H38—O82—K1viii85 (4)
O72vi—K2—O42iii110.62 (8)H38—O82—K2ix108 (4)
O72vi—K2—O51iv74.13 (7)H38—O82—Na2134 (3)
O72vi—K2—O52v74.31 (7)H38—O82—H48105 (5)
O72vi—K2—O71i75.20 (7)K2ix—H48—K1viii170 (2)
O72vi—K2—H17i86.6 (8)O82—H48—K1viii85 (4)
O81i—K2—Na1i38.85 (5)O82—H48—K2ix87 (4)
O81i—K2—Na2vi150.58 (5)H29—O91—K1144 (4)
O81i—K2—O41ii91.31 (7)H19—O91—K1126 (4)
O81i—K2—O42iii81.55 (7)H19—O91—H2989 (6)
O81i—K2—O51iv122.38 (7)H39—O92—K1128 (5)
O81i—K2—O52v61.68 (7)H49—O92—K1148 (3)
O81i—K2—O71i63.69 (7)H49—O92—H3983 (5)
O81i—K2—H17i58.5 (9)Na1—O101—K1viii95.27 (12)
O81i—K2—O72vi125.62 (7)H210—O101—K1viii67 (3)
H28i—K2—Na1i49.3 (11)H210—O101—Na1122 (3)
H28i—K2—Na2vi165.2 (11)H110—O101—K1viii102 (4)
H28i—K2—O41ii89.5 (10)H110—O101—Na1132 (4)
H28i—K2—O42iii66.1 (10)H110—O101—H210106 (5)
H28i—K2—O51iv135.1 (10)Na2—O102—K1viii94.65 (12)
H28i—K2—O52v59.8 (9)H410—O102—Na2106 (4)
H28i—K2—O71i78.8 (11)H310—O102—K1viii92 (3)
H28i—K2—H17i74.2 (14)H310—O102—Na2131 (3)
H28i—K2—O72vi131.8 (10)H310—O102—H41082 (4)
H28i—K2—O81i15.7 (10)O102—H410—K1viii164 (5)
O82vi—K2—Na1i150.58 (5)O21—C11—O11126.4 (3)
O82vi—K2—Na2vi38.85 (5)C21—C11—O11116.9 (3)
O82vi—K2—O41ii81.78 (7)C21—C11—O21116.7 (3)
O82vi—K2—O42iii91.57 (7)C11—C21—O51110.6 (2)
O82vi—K2—O51iv61.58 (7)H21—C21—O51110.0 (18)
O82vi—K2—O52v122.30 (7)H21—C21—C11107.3 (18)
O82vi—K2—O71i125.55 (7)C31—C21—O51109.4 (2)
O82vi—K2—H17i129.5 (9)C31—C21—C11110.4 (2)
O82vi—K2—O72vi63.63 (7)C31—C21—H21109.0 (17)
O82vi—K2—O81i170.00 (6)C21—C31—O61110.4 (2)
O82vi—K2—H28i155.6 (11)H31—C31—O61105.6 (19)
H48vi—K2—Na1i165.3 (11)H31—C31—C21110.4 (17)
H48vi—K2—Na2vi49.3 (11)C41—C31—O61111.8 (3)
H48vi—K2—O41ii65.7 (10)C41—C31—C21110.1 (2)
H48vi—K2—O42iii90.3 (10)C41—C31—H31108.3 (17)
H48vi—K2—O51iv59.1 (10)O31—C41—Na2ii49.32 (15)
H48vi—K2—O52v135.9 (10)O41—C41—Na2ii122.5 (2)
H48vi—K2—O71i131.4 (10)O41—C41—O31126.1 (3)
H48vi—K2—H17i130.9 (13)C31—C41—Na2ii96.26 (18)
H48vi—K2—O72vi79.1 (11)C31—C41—O31116.6 (3)
H48vi—K2—O81i155.3 (11)C31—C41—O41117.3 (3)
H48vi—K2—H28i145.3 (11)O22—C12—O12126.6 (3)
H48vi—K2—O82vi16.2 (10)C22—C12—O12116.8 (3)
K2viii—Na1—K1viii98.12 (4)C22—C12—O22116.7 (3)
O11—Na1—K1viii88.37 (7)C12—C22—O52110.9 (2)
O11—Na1—K2viii133.93 (7)H22—C22—O52108.4 (17)
O32iii—Na1—K1viii140.20 (8)H22—C22—C12108.7 (17)
O32iii—Na1—K2viii108.45 (7)C32—C22—O52109.2 (2)
O32iii—Na1—O1193.62 (8)C32—C22—C12110.7 (2)
O52iii—Na1—K1viii92.56 (7)C32—C22—H22108.9 (16)
O52iii—Na1—K2viii52.63 (6)C22—C32—O62110.2 (2)
O52iii—Na1—O11173.15 (9)H32—C32—O62107 (2)
O52iii—Na1—O32iii81.33 (8)H32—C32—C22111.7 (19)
O71—Na1—K1viii126.97 (8)C42—C32—O62111.8 (3)
O71—Na1—K2viii48.04 (7)C42—C32—C22110.3 (2)
O71—Na1—O1192.38 (9)C42—C32—H32106 (2)
O71—Na1—O32iii92.69 (9)O32—C42—Na1x49.57 (15)
O71—Na1—O52iii92.48 (9)O42—C42—Na1x122.4 (2)
O81—Na1—K1viii45.66 (8)O42—C42—O32126.1 (3)
O81—Na1—K2viii55.80 (8)C32—C42—Na1x96.37 (17)
O81—Na1—O11105.13 (10)C32—C42—O32116.3 (3)
O81—Na1—O32iii160.99 (10)C32—C42—O42117.6 (3)
O81—Na1—O52iii80.23 (9)
K1—O11—C11—O2151.7 (2)Na2ii—O51—C21—C3111.8 (2)
K1—O11—C11—C21128.82 (19)Na2ii—C41—C31—O6162.75 (17)
K1—O12—C12—O2251.8 (2)Na2ii—C41—C31—C2160.43 (19)
K1—O12—C12—C22128.50 (19)O11—C11—C21—O51177.0 (3)
K2vii—O41—C41—Na2ii73.32 (17)O11—C11—C21—C3161.8 (3)
K2vii—O41—C41—O3112.8 (2)O12—C12—C22—O52176.8 (3)
K2vii—O41—C41—C31168.31 (19)O12—C12—C22—C3261.8 (3)
K2—O42iii—C42iii—Na173.12 (17)O21—C11—C21—O513.4 (3)
K2x—O42—C42—O3212.3 (2)O21—C11—C21—C31117.8 (3)
K2x—O42—C42—C32168.18 (19)O22—C12—C22—O523.5 (3)
K2xi—O51—C21—C11113.04 (19)O22—C12—C22—C32117.9 (3)
K2xi—O51—C21—C31125.12 (19)O31—C41—C31—O6115.5 (3)
K2xii—O52—C22—C12112.82 (19)O31—C41—C31—C21107.7 (3)
K2xii—O52—C22—C32124.9 (2)O32—C42—C32—O6214.8 (3)
Na1—O11—C11—O2176.5 (2)O32—C42—C32—C22108.1 (3)
Na1—O11—C11—C21103.0 (2)O41—C41—C31—O61165.5 (3)
Na1x—O32—C42—O42104.43 (19)O41—C41—C31—C2171.3 (3)
Na1x—O32—C42—C3275.06 (18)O42—C42—C32—O62165.6 (3)
Na1x—O52—C22—C12133.4 (2)O42—C42—C32—C2271.4 (3)
Na1x—O52—C22—C3211.1 (2)O51—C21—C31—O6168.0 (3)
Na1x—C42—C32—O6262.55 (17)O51—C21—C31—C4156.0 (3)
Na1x—C42—C32—C2260.39 (18)O52—C22—C32—O6268.5 (3)
Na2—O12—C12—O2276.6 (2)O52—C22—C32—C4255.4 (3)
Na2—O12—C12—C22103.1 (2)O61—C31—C21—C1153.9 (3)
Na2ii—O31—C41—O41104.5 (2)O62—C32—C22—C1253.9 (3)
Na2ii—O31—C41—C3174.38 (19)C11—C21—C31—C41177.9 (3)
Na2ii—O51—C21—C11133.7 (2)C12—C22—C32—C42177.8 (2)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (iv) x+1/2, y+1/2, z; (v) x+1/2, y1/2, z; (vi) x+1, y, z1; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (ix) x1, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xii) x1/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O51—H51···O210.76 (4)2.07 (4)2.601 (3)127 (4)
O51—H51···O31i0.76 (4)2.74 (4)3.350 (3)139 (4)
O51—H51···O41i0.76 (4)2.88 (4)3.264 (3)114 (3)
O52—H52···O220.83 (4)2.09 (4)2.605 (3)120 (3)
O52—H52···O32i0.83 (4)2.64 (4)3.356 (3)145 (3)
O52—H52···O42i0.83 (4)2.79 (4)3.254 (3)117 (3)
O61—H61···O102ii0.73 (3)2.18 (3)2.896 (4)166 (4)
O62—H62···O101x0.76 (3)2.20 (3)2.923 (4)159 (4)
O71—H17···O610.70 (5)2.09 (5)2.793 (3)172 (5)
O71—H27···O41ii0.87 (4)2.03 (4)2.883 (4)166 (4)
O72—H47···O42x0.86 (4)2.06 (4)2.885 (3)162 (4)
O72—H37···O620.81 (5)1.98 (5)2.792 (3)178 (5)
O81—H18···O11viii0.91 (5)2.83 (5)3.384 (3)120 (4)
O81—H18···O21viii0.91 (5)1.85 (5)2.748 (3)172 (5)
O81—H28···O32xiii0.84 (6)1.87 (6)2.709 (3)171 (5)
O82—H48···O31xiv0.87 (6)1.83 (6)2.701 (3)173 (5)
O82—H38···O12viii0.87 (5)2.84 (5)3.382 (3)122 (4)
O82—H38···O22viii0.87 (5)1.89 (5)2.754 (3)173 (5)
O91—H29···O42i0.89 (5)1.94 (6)2.815 (4)167 (5)
O91—H19···O22v0.81 (6)2.41 (6)3.105 (4)145 (5)
O91—H19···O32iii0.81 (6)2.79 (6)3.161 (4)110 (5)
O91—H19···O62iii0.81 (6)2.55 (6)3.144 (4)132 (5)
O92—H39···O21xi0.76 (6)2.44 (6)3.116 (4)149 (5)
O92—H39···O31vii0.76 (6)2.83 (6)3.170 (4)110 (5)
O92—H39···O61vii0.76 (6)2.60 (5)3.142 (4)130 (5)
O92—H49···O41i0.97 (5)1.88 (5)2.816 (4)161 (5)
O101—H210···O91viii0.90 (5)1.87 (5)2.750 (4)165 (5)
O101—H110···O120.81 (6)1.92 (6)2.731 (4)174 (5)
O102—H410···O92viii0.78 (5)2.37 (5)2.757 (4)111 (5)
O102—H310···O110.85 (6)1.89 (5)2.727 (4)165 (5)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (v) x+1/2, y1/2, z; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xiii) x+1/2, y1/2, z+2; (xiv) x1/2, y+1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (286K_anh) top
Crystal data top
C4H12KNaO10F(000) = 585.519
Mr = 282.22Dx = 1.781 Mg m3
Monoclinic, P2111Mo Kα radiation, λ = 0.71073 Å
a = 11.8694 (9) ÅCell parameters from 6523 reflections
b = 14.2539 (12) Åθ = 3.5–28.7°
c = 6.2229 (4) ŵ = 0.59 mm1
β = 90°T = 286 K
V = 1052.82 (14) Å3Prism, clear colourless
Z = 40.48 × 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 Source4022 reflections with I 2u(I)
Graphite monochromatorRint = 0.051
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.752, Tmax = 1.000l = 88
18433 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.08Δρmax = 0.34 e Å3
5179 reflectionsΔρmin = 0.35 e Å3
386 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
3 restraintsAbsolute structure parameter: 0.03 (3)
24 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.0006 (2)0.00029 (15)0.0466 (3)0.0604 (6)
K20.50005 (7)0.00033 (5)0.15923 (10)0.03550 (16)
Na10.23140 (11)0.00677 (8)0.52275 (19)0.0299 (3)
Na20.23151 (11)0.00679 (8)0.52126 (19)0.0296 (3)
O110.11995 (18)0.10895 (15)0.3507 (3)0.0284 (5)
O120.11998 (18)0.10912 (15)0.3501 (3)0.0282 (5)
O210.2097 (2)0.20283 (15)0.1195 (3)0.0339 (5)
O220.2094 (2)0.20277 (15)0.1185 (3)0.0330 (5)
O310.2321 (2)0.40621 (16)0.8140 (3)0.0401 (6)
O320.2336 (2)0.40628 (16)0.8128 (3)0.0391 (5)
O410.0528 (2)0.36199 (17)0.8440 (3)0.0386 (6)
O420.0537 (2)0.36231 (17)0.8440 (3)0.0388 (6)
O510.16340 (19)0.35714 (15)0.3242 (3)0.0292 (5)
H510.192 (3)0.339 (3)0.223 (6)0.0438 (7)*
O520.1634 (2)0.35715 (14)0.3231 (3)0.0290 (5)
H520.190 (3)0.345 (3)0.198 (6)0.0435 (7)*
O610.29518 (19)0.24813 (16)0.6294 (4)0.0312 (5)
H610.329 (3)0.287 (3)0.592 (7)0.0468 (7)*
O620.29532 (19)0.24840 (16)0.6275 (3)0.0316 (5)
H620.332 (3)0.295 (2)0.604 (6)0.0473 (7)*
O710.3956 (2)0.08222 (18)0.4844 (4)0.0355 (5)
H170.370 (4)0.130 (3)0.517 (7)0.0533 (8)*
H270.437 (4)0.093 (3)0.376 (6)0.0533 (8)*
O720.3955 (2)0.08219 (18)0.4847 (4)0.0358 (5)
H470.429 (4)0.095 (3)0.376 (7)0.0538 (8)*
H370.369 (4)0.134 (3)0.535 (6)0.0538 (8)*
O810.2438 (3)0.04171 (19)0.8856 (4)0.0501 (7)
H180.237 (4)0.096 (3)0.957 (7)0.0751 (11)*
H280.254 (5)0.002 (3)0.985 (9)0.0751 (11)*
O820.2425 (3)0.04121 (19)0.8849 (4)0.0505 (7)
H480.257 (5)0.001 (3)0.985 (9)0.0757 (11)*
H380.233 (5)0.094 (3)0.946 (7)0.0757 (11)*
O910.0617 (2)0.1981 (3)0.0346 (5)0.0608 (9)
H290.035 (5)0.248 (4)0.078 (8)0.0912 (13)*
H190.116 (5)0.218 (4)0.017 (9)0.0912 (13)*
O920.0613 (2)0.1966 (2)0.0343 (5)0.0568 (8)
H390.120 (5)0.228 (4)0.011 (8)0.0852 (12)*
H490.038 (5)0.256 (4)0.082 (7)0.0852 (12)*
O1010.0750 (2)0.1024 (2)0.5821 (5)0.0600 (8)
H2100.074 (4)0.145 (4)0.701 (8)0.0900 (12)*
H1100.016 (5)0.105 (4)0.519 (8)0.0900 (12)*
O1020.0766 (2)0.1035 (2)0.5785 (5)0.0563 (8)
H4100.046 (5)0.090 (4)0.681 (8)0.0844 (12)*
H3100.017 (5)0.104 (4)0.526 (8)0.0844 (12)*
C110.1542 (2)0.1879 (2)0.2856 (4)0.0229 (6)
C210.1251 (3)0.2727 (2)0.4235 (4)0.0229 (6)
H210.045 (3)0.277 (2)0.433 (5)0.0275 (7)*
C310.1780 (3)0.2640 (2)0.6459 (4)0.0248 (6)
H310.146 (3)0.208 (2)0.729 (5)0.0298 (7)*
C410.1520 (3)0.3511 (2)0.7805 (4)0.0296 (7)
C120.1540 (2)0.1878 (2)0.2850 (4)0.0231 (6)
C220.1252 (3)0.2731 (2)0.4228 (4)0.0230 (6)
H220.037 (3)0.278 (2)0.439 (4)0.0276 (7)*
C320.1783 (3)0.2644 (2)0.6455 (4)0.0244 (6)
H320.145 (3)0.209 (2)0.720 (5)0.0293 (7)*
C420.1526 (3)0.3515 (2)0.7791 (4)0.0302 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0719 (12)0.0605 (13)0.0486 (11)0.0342 (11)0.0017 (14)0.0004 (10)
K20.0348 (3)0.0405 (4)0.0312 (3)0.0040 (3)0.0002 (3)0.0004 (3)
Na10.0289 (7)0.0280 (7)0.0329 (6)0.0012 (5)0.0013 (5)0.0011 (5)
Na20.0280 (7)0.0282 (7)0.0326 (6)0.0009 (5)0.0013 (5)0.0006 (5)
O110.0314 (12)0.0242 (12)0.0294 (11)0.0002 (9)0.0010 (9)0.0016 (8)
O120.0310 (12)0.0235 (12)0.0299 (11)0.0025 (9)0.0015 (9)0.0008 (8)
O210.0440 (13)0.0302 (12)0.0275 (11)0.0003 (10)0.0083 (10)0.0004 (8)
O220.0429 (13)0.0296 (12)0.0264 (11)0.0000 (10)0.0074 (10)0.0021 (8)
O310.0538 (15)0.0306 (13)0.0359 (12)0.0088 (11)0.0034 (11)0.0081 (9)
O320.0507 (15)0.0302 (13)0.0363 (12)0.0073 (11)0.0033 (11)0.0077 (9)
O410.0371 (13)0.0478 (15)0.0308 (11)0.0141 (11)0.0001 (10)0.0083 (10)
O420.0393 (13)0.0462 (15)0.0309 (11)0.0135 (11)0.0007 (10)0.0078 (10)
O510.0411 (13)0.0227 (11)0.0238 (10)0.0006 (9)0.0004 (9)0.0009 (8)
O520.0440 (13)0.0213 (11)0.0217 (10)0.0013 (9)0.0004 (9)0.0003 (8)
O610.0259 (12)0.0297 (13)0.0381 (12)0.0039 (9)0.0045 (10)0.0000 (9)
O620.0265 (12)0.0293 (13)0.0389 (12)0.0053 (9)0.0042 (10)0.0037 (9)
O710.0309 (13)0.0307 (13)0.0450 (14)0.0000 (10)0.0076 (10)0.0043 (10)
O720.0298 (12)0.0332 (14)0.0445 (14)0.0000 (10)0.0067 (10)0.0025 (11)
O810.092 (2)0.0315 (14)0.0268 (12)0.0116 (14)0.0053 (13)0.0005 (9)
O820.093 (2)0.0301 (14)0.0279 (12)0.0109 (14)0.0040 (14)0.0003 (9)
O910.0393 (16)0.091 (3)0.0524 (17)0.0083 (16)0.0090 (13)0.0079 (16)
O920.0372 (15)0.082 (2)0.0514 (16)0.0057 (15)0.0086 (13)0.0045 (15)
O1010.0361 (16)0.064 (2)0.079 (2)0.0176 (13)0.0188 (14)0.0314 (16)
O1020.0335 (16)0.0600 (19)0.075 (2)0.0148 (13)0.0127 (14)0.0216 (16)
C110.0225 (14)0.0239 (16)0.0223 (13)0.0014 (12)0.0033 (12)0.0018 (11)
C210.0226 (16)0.0215 (15)0.0247 (14)0.0003 (12)0.0001 (12)0.0000 (11)
C310.0277 (16)0.0249 (16)0.0219 (14)0.0023 (12)0.0018 (11)0.0011 (11)
C410.0437 (19)0.0272 (17)0.0178 (13)0.0035 (14)0.0056 (13)0.0005 (11)
C120.0221 (14)0.0258 (16)0.0214 (13)0.0024 (12)0.0041 (12)0.0002 (11)
C220.0258 (16)0.0209 (15)0.0222 (13)0.0001 (12)0.0001 (12)0.0019 (11)
C320.0257 (16)0.0242 (16)0.0234 (14)0.0003 (12)0.0028 (11)0.0010 (11)
C420.0435 (19)0.0269 (17)0.0202 (14)0.0062 (15)0.0067 (14)0.0021 (11)
Geometric parameters (Å, º) top
K1—O112.830 (3)O31—C411.251 (4)
K1—O122.833 (3)O32—C421.256 (4)
K1—O81i3.114 (4)O41—C411.252 (4)
K1—H28i3.03 (6)O42—C421.251 (4)
K1—O82i3.112 (4)O51—H510.76 (4)
K1—H48i3.08 (6)O51—C211.428 (4)
K1—O912.954 (5)O52—H520.86 (4)
K1—O922.945 (4)O52—C221.423 (4)
K1—O101i3.354 (4)O61—H610.73 (3)
K1—O102i3.394 (4)O61—C311.412 (4)
K1—H410i2.68 (5)O62—H620.81 (3)
K2—O41ii2.843 (2)O62—C321.412 (4)
K2—O42iii2.852 (2)O71—H170.77 (4)
K2—O51iv2.991 (2)O71—H270.85 (4)
K2—O52v2.994 (2)O72—H470.80 (4)
K2—O71i2.797 (3)O72—H370.86 (5)
K2—O72vi2.797 (2)O81—H180.90 (5)
K2—O81i3.110 (3)O81—H280.85 (5)
K2—H28i3.06 (6)O82—H480.88 (5)
K2—O82vi3.124 (3)O82—H380.85 (5)
K2—H48vi3.02 (6)O91—H290.83 (5)
Na1—O112.370 (2)O91—H190.77 (6)
Na1—O32iii2.463 (2)O92—H390.85 (6)
Na1—O52iii2.499 (2)O92—H490.94 (5)
Na1—O712.337 (3)O101—H2100.96 (5)
Na1—O812.365 (3)O101—H1100.80 (6)
Na1—O1012.333 (3)O102—H4100.76 (5)
Na1—C42iii3.082 (3)O102—H3100.78 (6)
Na2—O122.369 (2)H410—H3101.04 (6)
Na2—O31vii2.466 (3)C11—C211.522 (4)
Na2—O51vii2.498 (2)C21—H210.96 (3)
Na2—O722.335 (3)C21—C311.525 (4)
Na2—O822.368 (3)C31—H311.02 (4)
Na2—O1022.325 (3)C31—C411.529 (4)
Na2—C41vii3.090 (3)C12—C221.527 (4)
O11—C111.263 (4)C22—H221.05 (3)
O12—C121.259 (4)C22—C321.528 (4)
O21—C111.244 (4)C32—H321.00 (3)
O22—C121.245 (3)C32—C421.526 (4)
Na2i—K1—Na1i80.19 (3)O101—Na1—O8193.96 (12)
O11—K1—Na1i101.63 (8)C42iii—Na1—K1viii140.14 (8)
O11—K1—Na2i145.12 (9)C42iii—Na1—K2viii87.67 (7)
O12—K1—Na1i145.45 (9)C42iii—Na1—O11115.47 (8)
O12—K1—Na2i101.37 (8)C42iii—Na1—O32iii22.88 (8)
O12—K1—O1196.23 (7)C42iii—Na1—O52iii60.14 (8)
O81i—K1—Na1i33.02 (5)C42iii—Na1—O7185.47 (9)
O81i—K1—Na2i110.27 (6)C42iii—Na1—O81138.14 (10)
O81i—K1—O1169.24 (8)C42iii—Na1—O10193.95 (11)
O81i—K1—O12142.04 (11)K2ix—Na2—K1viii98.12 (4)
H28i—K1—Na1i42.7 (11)O12—Na2—K1viii88.10 (7)
H28i—K1—Na2i122.8 (11)O12—Na2—K2ix133.98 (7)
H28i—K1—O1165.3 (10)O31vii—Na2—K1viii140.51 (8)
H28i—K1—O12126.2 (11)O31vii—Na2—K2ix108.16 (7)
H28i—K1—O81i15.8 (10)O31vii—Na2—O1293.92 (8)
O82i—K1—Na1i110.18 (6)O51vii—Na2—K1viii92.64 (7)
O82i—K1—Na2i32.83 (5)O51vii—Na2—K2ix52.56 (6)
O82i—K1—O11141.58 (11)O51vii—Na2—O12173.23 (9)
O82i—K1—O1269.16 (8)O51vii—Na2—O31vii81.23 (8)
O82i—K1—O81i142.35 (8)O72—Na2—K1viii126.78 (8)
O82i—K1—H28i151.8 (10)O72—Na2—K2ix47.99 (6)
H48i—K1—Na1i122.9 (10)O72—Na2—O1292.50 (9)
H48i—K1—Na2i42.8 (10)O72—Na2—O31vii92.58 (10)
H48i—K1—O11125.2 (10)O72—Na2—O51vii92.45 (9)
H48i—K1—O1265.4 (10)O82—Na2—K1viii45.43 (8)
H48i—K1—O81i151.5 (10)O82—Na2—K2ix55.96 (8)
H48i—K1—H28i165.6 (11)O82—Na2—O12104.99 (10)
H48i—K1—O82i16.3 (10)O82—Na2—O31vii160.83 (10)
O91—K1—Na1i72.00 (8)O82—Na2—O51vii80.17 (9)
O91—K1—Na2i92.88 (8)O82—Na2—O7283.67 (11)
O91—K1—O11121.08 (12)O102—Na2—K1viii52.25 (10)
O91—K1—O1273.45 (9)O102—Na2—K2ix127.19 (9)
O91—K1—O81i84.32 (11)O102—Na2—O1292.29 (10)
O91—K1—H28i75.2 (9)O102—Na2—O31vii88.27 (11)
O91—K1—O82i89.63 (9)O102—Na2—O51vii82.88 (10)
O91—K1—H48i103.1 (9)O102—Na2—O72175.07 (11)
O92—K1—Na1i92.85 (7)O102—Na2—O8293.96 (12)
O92—K1—Na2i71.68 (8)C41vii—Na2—K1viii140.23 (7)
O92—K1—O1173.44 (9)C41vii—Na2—K2ix87.62 (7)
O92—K1—O12120.68 (11)C41vii—Na2—O12115.73 (8)
O92—K1—O81i89.58 (9)C41vii—Na2—O31vii22.65 (8)
O92—K1—H28i102.5 (10)C41vii—Na2—O51vii60.09 (7)
O92—K1—O82i83.79 (10)C41vii—Na2—O7285.64 (10)
O92—K1—H48i74.1 (9)C41vii—Na2—O82138.24 (10)
O92—K1—O91160.30 (10)C41vii—Na2—O10293.33 (12)
O101i—K1—Na1i33.05 (6)Na1—O11—K1101.45 (9)
O101i—K1—Na2i61.40 (6)C11—O11—K1115.85 (17)
O101i—K1—O11133.07 (11)C11—O11—Na1125.84 (18)
O101i—K1—O12118.03 (9)Na2—O12—K1101.54 (9)
O101i—K1—O81i64.02 (8)C12—O12—K1115.85 (17)
O101i—K1—H28i68.6 (10)C12—O12—Na2125.88 (18)
O101i—K1—O82i83.36 (8)C41—O31—Na2ii107.96 (18)
O101i—K1—H48i99.0 (11)C42—O32—Na1x107.45 (18)
O101i—K1—O9151.26 (9)C41—O41—K2vii120.7 (2)
O101i—K1—O92109.37 (9)C42—O42—K2x121.2 (2)
O102i—K1—Na1i61.70 (6)Na2ii—O51—K2xi85.90 (7)
O102i—K1—Na2i32.80 (6)H51—O51—K2xi103 (3)
O102i—K1—O11117.98 (9)H51—O51—Na2ii111 (3)
O102i—K1—O12132.44 (11)C21—O51—K2xi120.99 (17)
O102i—K1—O81i83.68 (8)C21—O51—Na2ii130.32 (16)
O102i—K1—H28i98.9 (11)C21—O51—H51102 (3)
O102i—K1—O82i63.49 (8)Na1x—O52—K2xii85.72 (7)
O102i—K1—H48i67.9 (10)H52—O52—K2xii94 (3)
O102i—K1—O91109.61 (9)H52—O52—Na1x109 (3)
O102i—K1—O9250.95 (8)C22—O52—K2xii121.03 (17)
O102i—K1—O101i61.35 (7)C22—O52—Na1x130.21 (16)
H410i—K1—Na1i59.4 (12)C22—O52—H52110 (3)
H410i—K1—Na2i37.3 (12)C31—O61—H61117 (3)
H410i—K1—O11114.1 (12)C32—O62—H62114 (3)
H410i—K1—O12136.6 (12)Na1—O71—K2viii93.55 (9)
H410i—K1—O81i79.9 (12)H17—O71—K2viii110 (3)
H410i—K1—H28i95.3 (16)H17—O71—Na197 (3)
H410i—K1—O82i67.8 (12)H27—O71—K2viii116 (3)
H410i—K1—H48i71.7 (16)H27—O71—Na1131 (3)
H410i—K1—O91111.4 (12)H27—O71—H17107 (4)
H410i—K1—O9249.0 (12)Na2—O72—K2ix93.68 (9)
H410i—K1—O101i61.9 (12)H47—O72—K2ix123 (3)
H410i—K1—O102i4.5 (12)H47—O72—Na2128 (3)
Na2vi—K2—Na1i116.23 (3)H37—O72—K2ix104 (3)
O41ii—K2—Na1i124.67 (6)H37—O72—Na297 (3)
O41ii—K2—Na2vi99.28 (6)H37—O72—H47107 (4)
O42iii—K2—Na1i98.86 (6)K2viii—O81—K1viii154.00 (11)
O42iii—K2—Na2vi124.83 (6)Na1—O81—K1viii101.14 (11)
O42iii—K2—O41ii92.91 (6)Na1—O81—K2viii85.42 (8)
O51iv—K2—Na1i112.82 (5)H18—O81—K1viii86 (3)
O51iv—K2—Na2vi41.55 (5)H18—O81—K2viii107 (3)
O51iv—K2—O41ii68.00 (6)H18—O81—Na1136 (3)
O51iv—K2—O42iii148.26 (7)H28—O81—K1viii76 (4)
O52v—K2—Na1i41.59 (4)H28—O81—K2viii79 (4)
O52v—K2—Na2vi112.71 (5)H28—O81—Na1121 (3)
O52v—K2—O41ii147.94 (7)H28—O81—H18103 (4)
O52v—K2—O42iii67.60 (6)K2viii—H28—K1viii170 (2)
O52v—K2—O51iv140.01 (6)O81—H28—K1viii88 (4)
O71i—K2—Na1i38.42 (5)O81—H28—K2viii85 (4)
O71i—K2—Na2vi86.91 (6)K2ix—O82—K1viii154.16 (10)
O71i—K2—O41ii110.88 (8)Na2—O82—K1viii101.75 (11)
O71i—K2—O42iii137.28 (8)Na2—O82—K2ix85.14 (9)
O71i—K2—O51iv74.42 (7)H48—O82—K1viii80 (4)
O71i—K2—O52v74.18 (7)H48—O82—K2ix75 (4)
O72vi—K2—Na1i86.99 (6)H48—O82—Na2119 (3)
O72vi—K2—Na2vi38.33 (5)H38—O82—K1viii84 (4)
O72vi—K2—O41ii137.61 (7)H38—O82—K2ix110 (4)
O72vi—K2—O42iii110.75 (8)H38—O82—Na2132 (3)
O72vi—K2—O51iv74.12 (7)H38—O82—H48108 (5)
O72vi—K2—O52v74.40 (7)K2ix—H48—K1viii170 (2)
O72vi—K2—O71i75.16 (7)O82—H48—K1viii84 (4)
O81i—K2—Na1i38.90 (5)O82—H48—K2ix88 (4)
O81i—K2—Na2vi150.69 (5)H29—O91—K1142 (4)
O81i—K2—O41ii91.29 (7)H19—O91—K1119 (4)
O81i—K2—O42iii81.39 (7)H19—O91—H2998 (6)
O81i—K2—O51iv122.40 (7)H39—O92—K1133 (4)
O81i—K2—O52v61.72 (7)H49—O92—K1147 (3)
O81i—K2—O71i63.78 (7)H49—O92—H3979 (5)
O81i—K2—O72vi125.71 (7)Na1—O101—K1viii95.30 (12)
H28i—K2—Na1i48.9 (11)H210—O101—K1viii67 (3)
H28i—K2—Na2vi165.0 (11)H210—O101—Na1120 (3)
H28i—K2—O41ii90.2 (10)H110—O101—K1viii102 (4)
H28i—K2—O42iii65.7 (10)H110—O101—Na1130 (4)
H28i—K2—O51iv135.7 (10)H110—O101—H210110 (5)
H28i—K2—O52v59.1 (9)Na2—O102—K1viii94.95 (12)
H28i—K2—O71i78.8 (11)H410—O102—Na2111 (4)
H28i—K2—O72vi131.2 (10)H310—O102—K1viii97 (4)
H28i—K2—O81i15.8 (10)H310—O102—Na2131 (4)
O82vi—K2—Na1i150.68 (5)H310—O102—H41085 (5)
O82vi—K2—Na2vi38.91 (5)O102—H410—K1viii160 (6)
O82vi—K2—O41ii81.66 (7)H310—H410—K1viii144 (6)
O82vi—K2—O42iii91.58 (7)H310—H410—O10248 (4)
O82vi—K2—O51iv61.64 (7)H410—H310—O10246 (4)
O82vi—K2—O52v122.30 (7)O21—C11—O11126.2 (3)
O82vi—K2—O71i125.63 (7)C21—C11—O11116.9 (2)
O82vi—K2—O72vi63.69 (7)C21—C11—O21116.9 (3)
O82vi—K2—O81i169.82 (6)C11—C21—O51110.7 (2)
O82vi—K2—H28i155.6 (11)H21—C21—O51107.2 (19)
H48vi—K2—Na1i165.4 (11)H21—C21—C11107.9 (18)
H48vi—K2—Na2vi49.3 (11)C31—C21—O51109.3 (2)
H48vi—K2—O41ii65.4 (10)C31—C21—C11110.6 (2)
H48vi—K2—O42iii90.6 (10)C31—C21—H21111.1 (18)
H48vi—K2—O51iv58.8 (10)C21—C31—O61110.7 (2)
H48vi—K2—O52v136.1 (10)H31—C31—O61106.1 (19)
H48vi—K2—O71i131.2 (10)H31—C31—C21112.0 (18)
H48vi—K2—O72vi79.2 (11)C41—C31—O61111.6 (2)
H48vi—K2—O81i155.0 (11)C41—C31—C21110.3 (2)
H48vi—K2—H28i145.6 (11)C41—C31—H31106.0 (18)
H48vi—K2—O82vi16.4 (10)O31—C41—Na2ii49.39 (15)
K2viii—Na1—K1viii98.17 (4)O41—C41—Na2ii122.1 (2)
O11—Na1—K1viii88.40 (7)O41—C41—O31125.8 (3)
O11—Na1—K2viii133.91 (7)C31—C41—Na2ii96.26 (17)
O32iii—Na1—K1viii140.19 (8)C31—C41—O31116.6 (3)
O32iii—Na1—K2viii108.48 (7)C31—C41—O41117.6 (3)
O32iii—Na1—O1193.51 (8)O22—C12—O12126.1 (3)
O52iii—Na1—K1viii92.53 (7)C22—C12—O12117.2 (2)
O52iii—Na1—K2viii52.69 (6)C22—C12—O22116.7 (3)
O52iii—Na1—O11173.11 (9)C12—C22—O52110.7 (2)
O52iii—Na1—O32iii81.42 (8)H22—C22—O52107.7 (16)
O71—Na1—K1viii127.07 (8)H22—C22—C12109.0 (17)
O71—Na1—K2viii48.03 (6)C32—C22—O52109.4 (2)
O71—Na1—O1192.36 (9)C32—C22—C12110.6 (2)
O71—Na1—O32iii92.61 (9)C32—C22—H22109.3 (15)
O71—Na1—O52iii92.52 (9)C22—C32—O62110.3 (2)
O81—Na1—K1viii45.84 (8)H32—C32—O62107 (2)
O81—Na1—K2viii55.67 (8)H32—C32—C22108.8 (18)
O81—Na1—O11105.24 (9)C42—C32—O62111.8 (3)
O81—Na1—O32iii160.97 (10)C42—C32—C22110.3 (2)
O81—Na1—O52iii80.14 (9)C42—C32—H32108.4 (18)
O81—Na1—O7183.52 (10)O32—C42—Na1x49.68 (15)
O101—Na1—K1viii51.65 (10)O42—C42—Na1x122.4 (2)
O101—Na1—K2viii127.43 (8)O42—C42—O32126.0 (3)
O101—Na1—O1191.98 (10)C32—C42—Na1x96.46 (17)
O101—Na1—O32iii88.54 (11)C32—C42—O32116.4 (3)
O101—Na1—O52iii83.27 (10)C32—C42—O42117.6 (3)
O101—Na1—O71175.43 (11)
K1—O11—C11—O2151.4 (2)Na2ii—O51—C21—C3111.4 (2)
K1—O11—C11—C21128.76 (18)Na2ii—C41—C31—O6162.96 (17)
K1—O12—C12—O2251.6 (2)Na2ii—C41—C31—C2160.53 (18)
K1—O12—C12—C22128.49 (18)O11—C11—C21—O51176.7 (3)
K2vii—O41—C41—Na2ii73.57 (17)O11—C11—C21—C3162.0 (3)
K2vii—O41—C41—O3113.2 (2)O12—C12—C22—O52176.7 (2)
K2vii—O41—C41—C31168.15 (19)O12—C12—C22—C3261.9 (3)
K2—O42iii—C42iii—Na173.13 (17)O21—C11—C21—O513.5 (3)
K2x—O42—C42—O3212.3 (2)O21—C11—C21—C31117.9 (3)
K2x—O42—C42—C32168.07 (18)O22—C12—C22—O523.5 (3)
K2xi—O51—C21—C11112.87 (18)O22—C12—C22—C32118.0 (3)
K2xi—O51—C21—C31125.04 (19)O31—C41—C31—O6115.6 (3)
K2xii—O52—C22—C12113.09 (18)O31—C41—C31—C21107.9 (3)
K2xii—O52—C22—C32124.71 (19)O32—C42—C32—O6214.8 (3)
Na1—O11—C11—O2177.1 (2)O32—C42—C32—C22108.3 (3)
Na1—O11—C11—C21102.8 (2)O41—C41—C31—O61165.7 (3)
Na1x—O32—C42—O42104.55 (18)O41—C41—C31—C2170.8 (3)
Na1x—O32—C42—C3275.12 (18)O42—C42—C32—O62165.5 (3)
Na1x—O52—C22—C12133.7 (2)O42—C42—C32—C2271.4 (3)
Na1x—O52—C22—C3211.5 (2)O51—C21—C31—O6168.2 (2)
Na1x—C42—C32—O6262.64 (16)O51—C21—C31—C4155.8 (3)
Na1x—C42—C32—C2260.40 (18)O52—C22—C32—O6268.3 (2)
Na2—O12—C12—O2277.0 (2)O52—C22—C32—C4255.6 (3)
Na2—O12—C12—C22102.9 (2)O61—C31—C21—C1153.9 (3)
Na2ii—O31—C41—O41104.19 (19)O62—C32—C22—C1254.0 (3)
Na2ii—O31—C41—C3174.42 (18)C11—C21—C31—C41177.9 (2)
Na2ii—O51—C21—C11133.5 (2)C12—C22—C32—C42177.9 (2)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (iv) x+1/2, y+1/2, z; (v) x+1/2, y1/2, z; (vi) x+1, y, z1; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (ix) x1, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xii) x1/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O51—H51···O210.76 (4)2.06 (4)2.600 (3)129 (4)
O51—H51···O31i0.76 (4)2.76 (4)3.352 (3)136 (4)
O51—H51···O41i0.76 (4)2.90 (4)3.265 (3)113 (3)
O52—H52···O220.86 (4)2.10 (4)2.601 (3)117 (3)
O52—H52···O32i0.86 (4)2.60 (4)3.357 (3)147 (3)
O52—H52···O42i0.86 (4)2.75 (4)3.254 (3)119 (3)
O61—H61···O102ii0.73 (3)2.19 (3)2.910 (4)170 (4)
O62—H62···O101x0.81 (3)2.16 (3)2.930 (4)158 (4)
O71—H17···O610.77 (4)2.03 (5)2.797 (3)174 (4)
O71—H27···O41ii0.85 (4)2.05 (4)2.880 (3)168 (4)
O72—H47···O42x0.80 (4)2.11 (4)2.887 (3)163 (4)
O72—H37···O620.86 (5)1.94 (5)2.796 (3)174 (4)
O81—H18···O11viii0.90 (5)2.82 (5)3.385 (3)122 (4)
O81—H18···O21viii0.90 (5)1.85 (5)2.748 (3)174 (5)
O81—H28···O32xiii0.85 (5)1.86 (6)2.707 (3)174 (5)
O82—H48···O31xiv0.88 (5)1.83 (5)2.702 (3)172 (5)
O82—H38···O12viii0.85 (5)2.86 (5)3.382 (3)122 (4)
O82—H38···O22viii0.85 (5)1.90 (5)2.753 (3)172 (4)
O91—H29···O42i0.83 (5)2.00 (6)2.816 (4)170 (6)
O91—H19···O22v0.77 (6)2.51 (6)3.107 (4)135 (5)
O91—H19···O32iii0.77 (6)2.73 (6)3.165 (4)118 (5)
O91—H19···O62iii0.77 (6)2.50 (6)3.144 (4)142 (5)
O92—H39···O21xi0.85 (6)2.34 (6)3.118 (4)152 (5)
O92—H39···O31vii0.85 (6)2.87 (6)3.170 (4)103 (4)
O92—H39···O61vii0.85 (6)2.60 (5)3.142 (4)123 (4)
O92—H49···O41i0.94 (5)1.91 (5)2.822 (4)162 (5)
O101—H210···O91viii0.96 (5)1.82 (5)2.752 (4)165 (5)
O101—H110···O120.80 (6)1.93 (6)2.730 (3)176 (5)
O102—H410···O92viii0.76 (5)2.34 (5)2.757 (4)116 (5)
O102—H310···O110.78 (6)1.96 (6)2.730 (4)171 (5)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (v) x+1/2, y1/2, z; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xiii) x+1/2, y1/2, z+2; (xiv) x1/2, y+1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (296K_anh) top
Crystal data top
C4H12KNaO10F(000) = 585.519
Mr = 282.22Dx = 1.777 Mg m3
Monoclinic, P2111Mo Kα radiation, λ = 0.71073 Å
a = 11.8822 (9) ÅCell parameters from 6349 reflections
b = 14.2635 (12) Åθ = 3.6–28.7°
c = 6.2260 (4) ŵ = 0.59 mm1
β = 90°T = 296 K
V = 1055.19 (14) Å3Prism, clear colourless
Z = 40.48 × 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 Source3995 reflections with I 2u(I)
Graphite monochromatorRint = 0.052
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.669, Tmax = 1.000l = 88
18450 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.08Δρmax = 0.36 e Å3
5199 reflectionsΔρmin = 0.37 e Å3
386 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
3 restraintsAbsolute structure parameter: 0.06 (3)
24 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.0006 (2)0.00018 (15)0.0470 (3)0.0620 (6)
K20.50002 (8)0.00018 (5)0.15896 (10)0.03674 (16)
Na10.23125 (11)0.00672 (8)0.52288 (19)0.0309 (3)
Na20.23159 (11)0.00681 (8)0.52202 (19)0.0307 (3)
O110.12007 (18)0.10923 (15)0.3513 (3)0.0286 (5)
O120.11999 (18)0.10903 (15)0.3507 (3)0.0292 (5)
O210.2095 (2)0.20281 (15)0.1194 (3)0.0341 (5)
O220.2096 (2)0.20276 (15)0.1191 (3)0.0345 (5)
O310.2325 (2)0.40625 (16)0.8134 (3)0.0398 (5)
O320.2336 (2)0.40615 (16)0.8127 (3)0.0407 (6)
O410.0532 (2)0.36219 (17)0.8436 (3)0.0392 (6)
O420.0536 (2)0.36248 (17)0.8440 (3)0.0397 (6)
O510.1631 (2)0.35721 (15)0.3241 (3)0.0302 (5)
H510.187 (3)0.341 (3)0.219 (6)0.0454 (8)*
O520.1635 (2)0.35710 (15)0.3231 (3)0.0298 (5)
H520.191 (3)0.343 (3)0.203 (6)0.0446 (7)*
O610.29533 (19)0.24814 (15)0.6285 (4)0.0321 (5)
H610.325 (3)0.291 (2)0.607 (7)0.0481 (8)*
O620.29545 (19)0.24813 (16)0.6273 (4)0.0334 (5)
H620.328 (3)0.294 (2)0.604 (6)0.0500 (8)*
O710.3957 (2)0.08191 (18)0.4836 (4)0.0371 (6)
H170.374 (4)0.125 (3)0.519 (7)0.0557 (9)*
H270.437 (4)0.091 (3)0.370 (7)0.0557 (9)*
O720.3957 (2)0.08223 (18)0.4853 (4)0.0371 (6)
H470.428 (4)0.092 (3)0.372 (7)0.0556 (8)*
H370.361 (4)0.133 (3)0.527 (7)0.0556 (8)*
O810.2442 (3)0.0414 (2)0.8862 (4)0.0517 (8)
H180.236 (5)0.094 (4)0.952 (8)0.0776 (11)*
H280.252 (5)0.002 (4)0.983 (9)0.0776 (11)*
O820.2434 (3)0.04129 (19)0.8854 (4)0.0504 (8)
H480.260 (5)0.004 (3)0.981 (9)0.0756 (11)*
H380.235 (4)0.098 (4)0.941 (7)0.0756 (11)*
O910.0615 (3)0.1985 (3)0.0348 (5)0.0620 (9)
H290.048 (5)0.252 (4)0.089 (8)0.0930 (13)*
H190.115 (5)0.216 (4)0.013 (9)0.0930 (13)*
O920.0614 (2)0.1978 (3)0.0346 (5)0.0595 (8)
H390.115 (5)0.227 (4)0.005 (9)0.0893 (12)*
H490.029 (5)0.259 (4)0.085 (7)0.0893 (12)*
O1010.0750 (2)0.1023 (2)0.5828 (6)0.0621 (9)
H2100.071 (5)0.140 (4)0.705 (8)0.0931 (13)*
H1100.014 (5)0.107 (4)0.518 (8)0.0931 (13)*
O1020.0759 (2)0.1033 (2)0.5794 (5)0.0593 (9)
H4100.053 (5)0.086 (4)0.682 (8)0.0889 (13)*
H3100.014 (5)0.103 (4)0.528 (8)0.0889 (13)*
C110.1542 (2)0.1879 (2)0.2851 (4)0.0245 (6)
C210.1249 (3)0.2728 (2)0.4234 (4)0.0240 (6)
H210.041 (3)0.277 (2)0.432 (5)0.0287 (7)*
C310.1780 (3)0.2637 (2)0.6461 (5)0.0264 (6)
H310.145 (3)0.207 (2)0.730 (5)0.0317 (8)*
C410.1520 (3)0.3514 (2)0.7798 (4)0.0303 (7)
C120.1540 (2)0.1876 (2)0.2852 (4)0.0233 (6)
C220.1253 (3)0.2731 (2)0.4225 (4)0.0241 (6)
H220.042 (3)0.279 (2)0.439 (5)0.0289 (7)*
C320.1779 (3)0.2643 (2)0.6446 (5)0.0249 (6)
H320.147 (3)0.209 (2)0.720 (5)0.0299 (7)*
C420.1530 (3)0.3518 (2)0.7792 (4)0.0290 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0720 (12)0.0638 (13)0.0503 (12)0.0355 (11)0.0011 (13)0.0010 (10)
K20.0364 (3)0.0416 (4)0.0322 (3)0.0043 (3)0.0001 (3)0.0005 (3)
Na10.0295 (7)0.0287 (7)0.0344 (6)0.0015 (5)0.0014 (5)0.0019 (5)
Na20.0301 (7)0.0276 (7)0.0343 (6)0.0013 (5)0.0014 (5)0.0010 (5)
O110.0312 (12)0.0234 (12)0.0312 (11)0.0021 (9)0.0010 (9)0.0008 (8)
O120.0330 (12)0.0241 (12)0.0303 (11)0.0020 (9)0.0018 (9)0.0024 (8)
O210.0438 (13)0.0320 (12)0.0264 (11)0.0001 (10)0.0087 (10)0.0014 (9)
O220.0452 (13)0.0301 (12)0.0281 (11)0.0000 (10)0.0072 (10)0.0017 (9)
O310.0523 (15)0.0307 (13)0.0363 (12)0.0074 (11)0.0049 (11)0.0067 (9)
O320.0525 (15)0.0324 (13)0.0372 (12)0.0082 (12)0.0045 (11)0.0085 (9)
O410.0389 (13)0.0485 (15)0.0302 (11)0.0132 (11)0.0010 (10)0.0084 (10)
O420.0403 (13)0.0462 (15)0.0326 (12)0.0126 (11)0.0008 (10)0.0071 (10)
O510.0442 (14)0.0226 (11)0.0240 (10)0.0001 (10)0.0008 (10)0.0009 (8)
O520.0441 (13)0.0226 (11)0.0226 (10)0.0002 (9)0.0000 (9)0.0006 (8)
O610.0289 (13)0.0269 (13)0.0405 (12)0.0036 (9)0.0052 (10)0.0008 (10)
O620.0288 (13)0.0312 (13)0.0401 (12)0.0045 (10)0.0045 (10)0.0026 (10)
O710.0328 (13)0.0326 (14)0.0460 (14)0.0006 (11)0.0074 (11)0.0021 (11)
O720.0315 (13)0.0348 (14)0.0450 (14)0.0002 (10)0.0069 (11)0.0030 (11)
O810.096 (2)0.0321 (14)0.0269 (12)0.0118 (15)0.0076 (14)0.0009 (10)
O820.092 (2)0.0297 (14)0.0294 (12)0.0123 (14)0.0056 (14)0.0005 (10)
O910.0412 (16)0.092 (3)0.0527 (18)0.0076 (17)0.0087 (13)0.0061 (16)
O920.0394 (16)0.087 (2)0.0523 (17)0.0065 (15)0.0089 (13)0.0074 (15)
O1010.0367 (16)0.068 (2)0.082 (2)0.0175 (14)0.0192 (14)0.0317 (16)
O1020.0360 (16)0.065 (2)0.077 (2)0.0128 (14)0.0136 (15)0.0230 (17)
C110.0250 (15)0.0253 (17)0.0231 (14)0.0020 (12)0.0052 (12)0.0012 (11)
C210.0263 (17)0.0224 (15)0.0231 (13)0.0001 (12)0.0023 (12)0.0002 (11)
C310.0296 (16)0.0267 (17)0.0229 (14)0.0041 (13)0.0010 (12)0.0008 (12)
C410.045 (2)0.0269 (17)0.0193 (14)0.0057 (14)0.0066 (13)0.0012 (11)
C120.0235 (15)0.0240 (16)0.0223 (13)0.0025 (12)0.0039 (12)0.0002 (11)
C220.0250 (16)0.0230 (15)0.0242 (14)0.0005 (12)0.0018 (12)0.0001 (11)
C320.0268 (16)0.0237 (16)0.0243 (14)0.0012 (12)0.0012 (12)0.0012 (11)
C420.0396 (18)0.0276 (17)0.0196 (14)0.0040 (14)0.0060 (13)0.0006 (11)
Geometric parameters (Å, º) top
K1—O112.835 (3)O31—C411.254 (4)
K1—O122.835 (3)O32—C421.250 (4)
K1—O81i3.119 (4)O41—C411.248 (4)
K1—H28i3.02 (6)O42—C421.257 (4)
K1—O82i3.125 (4)O51—H510.75 (4)
K1—O912.964 (5)O51—C211.428 (4)
K1—O922.963 (4)O52—H520.84 (4)
K1—O101i3.355 (4)O52—C221.423 (4)
K1—H210i3.04 (5)O61—H610.72 (3)
K1—O102i3.389 (4)O61—C311.417 (4)
K1—H410i2.66 (5)O62—H620.77 (3)
K2—O41ii2.847 (2)O62—C321.420 (4)
K2—O42iii2.848 (2)O71—H170.70 (5)
K2—O51iv2.992 (2)O71—H270.87 (4)
K2—O52v2.997 (2)O72—H470.81 (4)
K2—O71i2.802 (3)O72—H370.87 (5)
K2—H17i3.07 (5)O81—H180.87 (5)
K2—O72vi2.797 (3)O81—H280.83 (6)
K2—O81i3.109 (3)O82—H480.83 (5)
K2—H28i3.07 (6)O82—H380.88 (5)
K2—O82vi3.118 (3)O91—H290.85 (5)
K2—H48vi2.99 (6)O91—H190.75 (6)
Na1—O112.371 (2)O92—H390.78 (6)
Na1—O32iii2.466 (3)O92—H491.00 (5)
Na1—O52iii2.501 (2)O101—H2100.93 (5)
Na1—O712.340 (3)O101—H1100.83 (6)
Na1—O812.369 (3)O102—H4100.74 (5)
Na1—O1012.333 (3)O102—H3100.80 (6)
Na1—C42iii3.082 (3)H410—H3101.09 (7)
Na2—O122.372 (2)C11—C211.525 (4)
Na2—O31vii2.466 (3)C21—H211.01 (3)
Na2—O51vii2.499 (2)C21—C311.528 (4)
Na2—O722.338 (3)C31—H311.05 (4)
Na2—O822.368 (3)C31—C411.533 (4)
Na2—O1022.333 (3)C12—C221.528 (4)
Na2—C41vii3.088 (3)C22—H221.00 (3)
O11—C111.262 (4)C22—C321.523 (4)
O12—C121.259 (4)C32—H320.99 (4)
O21—C111.242 (4)C32—C421.532 (4)
O22—C121.246 (4)
Na2i—K1—Na1i80.23 (3)O81—Na1—O7183.65 (11)
O11—K1—Na1i101.64 (8)O101—Na1—K1viii51.59 (10)
O11—K1—Na2i145.12 (9)O101—Na1—K2viii127.37 (9)
O12—K1—Na1i145.44 (9)O101—Na1—O1192.07 (10)
O12—K1—Na2i101.31 (8)O101—Na1—O32iii88.63 (11)
O12—K1—O1196.26 (7)O101—Na1—O52iii83.28 (10)
O81i—K1—Na1i33.05 (5)O101—Na1—O71175.36 (12)
O81i—K1—Na2i110.40 (7)O101—Na1—O8193.90 (12)
O81i—K1—O1169.24 (8)C42iii—Na1—K1viii140.20 (8)
O81i—K1—O12141.93 (12)C42iii—Na1—K2viii87.68 (7)
H28i—K1—Na1i42.5 (11)C42iii—Na1—O11115.49 (8)
H28i—K1—Na2i122.6 (11)C42iii—Na1—O32iii22.74 (8)
H28i—K1—O1165.6 (10)C42iii—Na1—O52iii60.15 (8)
H28i—K1—O12126.4 (11)C42iii—Na1—O7185.25 (9)
H28i—K1—O81i15.5 (11)C42iii—Na1—O81138.01 (10)
O82i—K1—Na1i110.24 (7)C42iii—Na1—O10194.02 (12)
O82i—K1—Na2i32.86 (5)K2ix—Na2—K1viii98.22 (4)
O82i—K1—O11141.53 (11)O12—Na2—K1viii88.09 (7)
O82i—K1—O1269.08 (8)O12—Na2—K2ix133.99 (7)
O82i—K1—O81i142.49 (8)O31vii—Na2—K1viii140.37 (8)
O82i—K1—H28i151.6 (11)O31vii—Na2—K2ix108.28 (7)
O91—K1—Na1i71.99 (8)O31vii—Na2—O1293.79 (8)
O91—K1—Na2i92.78 (8)O51vii—Na2—K1viii92.76 (7)
O91—K1—O11121.20 (12)O51vii—Na2—K2ix52.57 (6)
O91—K1—O1273.45 (9)O51vii—Na2—O12173.18 (9)
O91—K1—O81i84.26 (11)O51vii—Na2—O31vii81.24 (8)
O91—K1—H28i75.2 (10)O72—Na2—K1viii126.85 (8)
O91—K1—O82i89.54 (9)O72—Na2—K2ix47.97 (6)
O92—K1—Na1i92.84 (8)O72—Na2—O1292.51 (9)
O92—K1—Na2i71.71 (8)O72—Na2—O31vii92.65 (10)
O92—K1—O1173.41 (9)O72—Na2—O51vii92.39 (9)
O92—K1—O12120.70 (12)O82—Na2—K1viii45.71 (8)
O92—K1—O81i89.69 (9)O82—Na2—K2ix55.77 (8)
O92—K1—H28i102.4 (10)O82—Na2—O12105.12 (10)
O92—K1—O82i83.83 (11)O82—Na2—O31vii160.82 (10)
O92—K1—O91160.23 (11)O82—Na2—O51vii80.16 (9)
O101i—K1—Na1i33.02 (6)O82—Na2—O7283.49 (11)
O101i—K1—Na2i61.44 (6)O102—Na2—K1viii52.09 (10)
O101i—K1—O11133.06 (11)O102—Na2—K2ix127.36 (9)
O101i—K1—O12118.03 (10)O102—Na2—O1292.08 (10)
O101i—K1—O81i63.99 (8)O102—Na2—O31vii88.28 (11)
O101i—K1—H28i68.3 (10)O102—Na2—O51vii83.13 (10)
O101i—K1—O82i83.43 (8)O102—Na2—O72175.24 (12)
O101i—K1—O9151.21 (9)O102—Na2—O8294.11 (12)
O101i—K1—O92109.36 (9)C41vii—Na2—K1viii140.27 (7)
H210i—K1—Na1i43.2 (10)C41vii—Na2—K2ix87.59 (7)
H210i—K1—Na2i70.0 (10)C41vii—Na2—O12115.66 (9)
H210i—K1—O11133.8 (10)C41vii—Na2—O31vii22.75 (8)
H210i—K1—O12104.4 (11)C41vii—Na2—O51vii60.04 (8)
H210i—K1—O81i69.1 (10)C41vii—Na2—O7285.57 (10)
H210i—K1—H28i68.9 (14)C41vii—Na2—O82138.12 (10)
H210i—K1—O82i84.7 (10)C41vii—Na2—O10293.56 (12)
H210i—K1—O9135.4 (11)Na1—O11—K1101.31 (9)
H210i—K1—O92125.1 (11)C11—O11—K1115.59 (17)
H210i—K1—O101i15.8 (10)C11—O11—Na1126.05 (18)
O102i—K1—Na1i61.59 (6)Na2—O12—K1101.60 (9)
O102i—K1—Na2i32.90 (6)C12—O12—K1115.70 (17)
O102i—K1—O11117.95 (9)C12—O12—Na2125.90 (18)
O102i—K1—O12132.51 (11)C41—O31—Na2ii107.73 (18)
O102i—K1—O81i83.70 (8)C42—O32—Na1x107.53 (18)
O102i—K1—H28i98.6 (11)C41—O41—K2vii120.9 (2)
O102i—K1—O82i63.64 (8)C42—O42—K2x121.0 (2)
O102i—K1—O91109.49 (10)Na2ii—O51—K2xi85.89 (7)
O102i—K1—O9250.99 (9)H51—O51—K2xi99 (3)
O102i—K1—O101i61.28 (8)H51—O51—Na2ii112 (3)
O102i—K1—H210i75.9 (10)C21—O51—K2xi121.09 (17)
H410i—K1—Na1i60.7 (13)C21—O51—Na2ii130.38 (16)
H410i—K1—Na2i35.2 (13)C21—O51—H51104 (3)
H410i—K1—O11115.8 (13)Na1x—O52—K2xii85.76 (7)
H410i—K1—O12134.6 (13)H52—O52—K2xii97 (3)
H410i—K1—O81i81.9 (13)H52—O52—Na1x109 (3)
H410i—K1—H28i96.9 (17)C22—O52—K2xii120.99 (17)
H410i—K1—O82i65.8 (13)C22—O52—Na1x130.31 (16)
H410i—K1—O91110.7 (13)C22—O52—H52108 (3)
H410i—K1—O9249.6 (13)C31—O61—H61111 (3)
H410i—K1—O101i61.9 (13)C32—O62—H62112 (3)
H410i—K1—H210i76.8 (16)Na1—O71—K2viii93.52 (9)
H410i—K1—O102i2.4 (13)H17—O71—K2viii106 (4)
Na2vi—K2—Na1i116.30 (3)H17—O71—Na197 (4)
O41ii—K2—Na1i124.75 (6)H27—O71—K2viii117 (3)
O41ii—K2—Na2vi99.13 (6)H27—O71—Na1130 (3)
O42iii—K2—Na1i98.91 (6)H27—O71—H17110 (5)
O42iii—K2—Na2vi124.83 (6)O71—H17—K2viii62 (4)
O42iii—K2—O41ii92.88 (7)Na2—O72—K2ix93.66 (9)
O51iv—K2—Na1i112.76 (5)H47—O72—K2ix123 (3)
O51iv—K2—Na2vi41.54 (5)H47—O72—Na2125 (3)
O51iv—K2—O41ii67.95 (7)H37—O72—K2ix109 (3)
O51iv—K2—O42iii148.27 (7)H37—O72—Na292 (3)
O52v—K2—Na1i41.57 (5)H37—O72—H47110 (4)
O52v—K2—Na2vi112.76 (5)K2viii—O81—K1viii154.19 (11)
O52v—K2—O41ii148.04 (7)Na1—O81—K1viii101.04 (11)
O52v—K2—O42iii67.68 (7)Na1—O81—K2viii85.54 (9)
O52v—K2—O51iv139.96 (6)H18—O81—K1viii85 (4)
O71i—K2—Na1i38.42 (6)H18—O81—K2viii109 (4)
O71i—K2—Na2vi86.85 (6)H18—O81—Na1134 (3)
O71i—K2—O41ii111.04 (8)H28—O81—K1viii75 (4)
O71i—K2—O42iii137.32 (8)H28—O81—K2viii80 (4)
O71i—K2—O51iv74.37 (7)H28—O81—Na1120 (4)
O71i—K2—O52v74.08 (7)H28—O81—H18105 (5)
H17i—K2—Na1i41.9 (9)K2viii—H28—K1viii171 (2)
H17i—K2—Na2vi93.2 (9)O81—H28—K1viii89 (4)
H17i—K2—O41ii99.2 (9)O81—H28—K2viii85 (4)
H17i—K2—O42iii137.7 (9)K2ix—O82—K1viii154.20 (10)
H17i—K2—O51iv72.5 (9)Na2—O82—K1viii101.44 (11)
H17i—K2—O52v81.6 (9)Na2—O82—K2ix85.32 (9)
H17i—K2—O71i12.6 (9)H48—O82—K1viii82 (4)
O72vi—K2—Na1i87.03 (6)H48—O82—K2ix73 (4)
O72vi—K2—Na2vi38.37 (5)H48—O82—Na2121 (4)
O72vi—K2—O41ii137.50 (8)H38—O82—K1viii87 (3)
O72vi—K2—O42iii110.77 (8)H38—O82—K2ix108 (3)
O72vi—K2—O51iv74.12 (7)H38—O82—Na2129 (3)
O72vi—K2—O52v74.40 (7)H38—O82—H48110 (5)
O72vi—K2—O71i75.04 (7)O82—H48—K2ix91 (4)
O72vi—K2—H17i86.7 (9)H29—O91—K1151 (4)
O81i—K2—Na1i38.91 (5)H19—O91—K1118 (5)
O81i—K2—Na2vi150.77 (5)H19—O91—H2991 (6)
O81i—K2—O41ii91.40 (7)H39—O92—K1132 (5)
O81i—K2—O42iii81.34 (7)H49—O92—K1142 (3)
O81i—K2—O51iv122.41 (7)H49—O92—H3986 (5)
O81i—K2—O52v61.69 (7)Na1—O101—K1viii95.39 (12)
O81i—K2—O71i63.93 (7)H210—O101—K1viii62 (3)
O81i—K2—H17i58.1 (9)H210—O101—Na1120 (3)
O81i—K2—O72vi125.76 (7)H110—O101—K1viii103 (4)
H28i—K2—Na1i48.6 (11)H110—O101—Na1132 (4)
H28i—K2—Na2vi164.7 (11)H110—O101—H210108 (5)
H28i—K2—O41ii90.5 (10)O101—H210—K1viii102 (4)
H28i—K2—O42iii65.9 (10)Na2—O102—K1viii95.02 (12)
H28i—K2—O51iv135.6 (10)H410—O102—Na2104 (5)
H28i—K2—O52v58.8 (10)H310—O102—K1viii95 (4)
H28i—K2—O71i78.6 (11)H310—O102—Na2132 (4)
H28i—K2—H17i73.5 (14)H310—O102—H41090 (5)
H28i—K2—O72vi131.0 (10)O102—H410—K1viii169 (6)
H28i—K2—O81i15.5 (10)H310—H410—K1viii139 (6)
O82vi—K2—Na1i150.74 (5)H310—H410—O10247 (4)
O82vi—K2—Na2vi38.91 (5)O21—C11—O11126.4 (3)
O82vi—K2—O41ii81.53 (7)C21—C11—O11116.6 (3)
O82vi—K2—O42iii91.54 (7)C21—C11—O21117.0 (3)
O82vi—K2—O51iv61.70 (7)C11—C21—O51110.6 (2)
O82vi—K2—O52v122.33 (7)H21—C21—O51106.6 (18)
O82vi—K2—O71i125.58 (7)H21—C21—C11107.9 (17)
O82vi—K2—H17i130.2 (9)C31—C21—O51109.5 (2)
O82vi—K2—O72vi63.71 (7)C31—C21—C11110.6 (2)
O82vi—K2—O81i169.73 (6)C31—C21—H21111.6 (17)
O82vi—K2—H28i155.8 (11)C21—C31—O61110.4 (2)
H48vi—K2—Na1i164.9 (11)H31—C31—O61106.8 (19)
H48vi—K2—Na2vi48.9 (11)H31—C31—C21111.3 (18)
H48vi—K2—O41ii66.3 (11)C41—C31—O61111.6 (3)
H48vi—K2—O42iii90.0 (10)C41—C31—C21109.9 (2)
H48vi—K2—O51iv59.5 (10)C41—C31—H31106.8 (17)
H48vi—K2—O52v135.0 (10)O31—C41—Na2ii49.51 (15)
H48vi—K2—O71i131.5 (10)O41—C41—Na2ii122.3 (2)
H48vi—K2—H17i131.9 (13)O41—C41—O31126.0 (3)
H48vi—K2—O72vi78.4 (11)C31—C41—Na2ii96.53 (18)
H48vi—K2—O81i155.8 (11)C31—C41—O31116.5 (3)
H48vi—K2—H28i146.3 (11)C31—C41—O41117.5 (3)
H48vi—K2—O82vi15.3 (11)O22—C12—O12126.4 (3)
K2viii—Na1—K1viii98.17 (4)C22—C12—O12117.2 (2)
O11—Na1—K1viii88.37 (7)C22—C12—O22116.4 (3)
O11—Na1—K2viii133.83 (7)C12—C22—O52110.9 (2)
O32iii—Na1—K1viii140.22 (8)H22—C22—O52106.9 (18)
O32iii—Na1—K2viii108.39 (7)H22—C22—C12110.1 (18)
O32iii—Na1—O1193.68 (8)C32—C22—O52109.4 (2)
O52iii—Na1—K1viii92.58 (7)C32—C22—C12110.5 (2)
O52iii—Na1—K2viii52.67 (6)C32—C22—H22108.8 (17)
O52iii—Na1—O11173.20 (9)C22—C32—O62110.4 (2)
O52iii—Na1—O32iii81.29 (8)H32—C32—O62106 (2)
O71—Na1—K1viii127.24 (8)H32—C32—C22110.1 (19)
O71—Na1—K2viii48.06 (7)C42—C32—O62111.3 (3)
O71—Na1—O1192.37 (9)C42—C32—C22110.5 (2)
O71—Na1—O32iii92.41 (9)C42—C32—H32108.3 (19)
O71—Na1—O52iii92.41 (9)O32—C42—Na1x49.73 (15)
O81—Na1—K1viii45.91 (9)O42—C42—Na1x122.4 (2)
O81—Na1—K2viii55.54 (8)O42—C42—O32126.2 (3)
O81—Na1—O11105.33 (10)C32—C42—Na1x96.52 (17)
O81—Na1—O32iii160.69 (10)C32—C42—O32116.7 (3)
O81—Na1—O52iii80.01 (9)C32—C42—O42117.1 (3)
K1—O11—C11—O2151.5 (2)Na2ii—O51—C21—C3111.3 (2)
K1—O11—C11—C21128.92 (19)Na2ii—C41—C31—O6162.43 (17)
K1—O12—C12—O2251.9 (2)Na2ii—C41—C31—C2160.39 (19)
K1—O12—C12—C22128.51 (19)O11—C11—C21—O51176.8 (3)
K2vii—O41—C41—Na2ii73.48 (17)O11—C11—C21—C3161.7 (3)
K2vii—O41—C41—O3112.9 (2)O12—C12—C22—O52176.8 (3)
K2vii—O41—C41—C31167.77 (19)O12—C12—C22—C3261.6 (3)
K2—O42iii—C42iii—Na173.35 (17)O21—C11—C21—O513.5 (3)
K2x—O42—C42—O3212.3 (2)O21—C11—C21—C31117.9 (3)
K2x—O42—C42—C32168.24 (19)O22—C12—C22—O523.6 (3)
K2xi—O51—C21—C11112.81 (19)O22—C12—C22—C32118.0 (3)
K2xi—O51—C21—C31125.10 (19)O31—C41—C31—O6114.7 (3)
K2xii—O52—C22—C12113.03 (19)O31—C41—C31—C21108.1 (3)
K2xii—O52—C22—C32124.73 (19)O32—C42—C32—O6215.1 (3)
Na1—O11—C11—O2176.6 (2)O32—C42—C32—C22108.0 (3)
Na1—O11—C11—C21103.0 (2)O41—C41—C31—O61165.8 (3)
Na1x—O32—C42—O42104.45 (19)O41—C41—C31—C2171.3 (3)
Na1x—O32—C42—C3274.99 (18)O42—C42—C32—O62165.4 (3)
Na1x—O52—C22—C12133.6 (2)O42—C42—C32—C2271.5 (3)
Na1x—O52—C22—C3211.4 (2)O51—C21—C31—O6168.0 (3)
Na1x—C42—C32—O6262.98 (16)O51—C21—C31—C4155.5 (3)
Na1x—C42—C32—C2260.08 (18)O52—C22—C32—O6268.3 (2)
Na2—O12—C12—O2276.7 (2)O52—C22—C32—C4255.3 (3)
Na2—O12—C12—C22102.9 (2)O61—C31—C21—C1154.1 (3)
Na2ii—O31—C41—O41104.33 (19)O62—C32—C22—C1254.1 (3)
Na2ii—O31—C41—C3175.05 (18)C11—C21—C31—C41177.6 (3)
Na2ii—O51—C21—C11133.4 (2)C12—C22—C32—C42177.7 (2)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (iv) x+1/2, y+1/2, z; (v) x+1/2, y1/2, z; (vi) x+1, y, z1; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (ix) x1, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xii) x1/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O51—H51···O210.75 (4)2.09 (4)2.604 (3)126 (4)
O51—H51···O31i0.75 (4)2.74 (4)3.359 (3)141 (4)
O51—H51···O41i0.75 (4)2.85 (4)3.265 (3)118 (4)
O52—H52···O220.84 (4)2.08 (4)2.600 (3)119 (3)
O52—H52···O32i0.84 (4)2.64 (4)3.359 (3)144 (3)
O52—H52···O42i0.84 (4)2.79 (4)3.257 (3)117 (3)
O61—H61···O102ii0.72 (3)2.24 (3)2.917 (4)158 (4)
O62—H62···O101x0.77 (3)2.21 (3)2.938 (4)158 (4)
O71—H17···O610.70 (5)2.11 (5)2.803 (3)175 (5)
O71—H27···O41ii0.87 (4)2.03 (4)2.879 (4)165 (4)
O72—H47···O42x0.81 (4)2.11 (4)2.889 (3)159 (4)
O72—H37···O620.87 (5)1.92 (5)2.793 (3)176 (4)
O81—H18···O11viii0.87 (5)2.85 (5)3.390 (3)122 (4)
O81—H18···O21viii0.87 (5)1.89 (5)2.753 (3)174 (5)
O81—H28···O32xiii0.83 (6)1.87 (6)2.703 (3)176 (5)
O82—H48···O31xiv0.83 (5)1.89 (5)2.703 (3)168 (6)
O82—H38···O12viii0.88 (5)2.90 (5)3.388 (3)117 (4)
O82—H38···O22viii0.88 (5)1.89 (5)2.754 (3)167 (4)
O91—H29···O42i0.85 (5)2.03 (6)2.813 (4)153 (6)
O91—H19···O22v0.75 (6)2.52 (6)3.107 (4)137 (5)
O91—H19···O32iii0.75 (6)2.73 (6)3.173 (4)120 (6)
O91—H19···O62iii0.75 (6)2.53 (6)3.147 (4)141 (6)
O92—H39···O21xi0.78 (6)2.43 (6)3.114 (4)148 (5)
O92—H39···O31vii0.78 (6)2.88 (6)3.177 (4)105 (5)
O92—H39···O61vii0.78 (6)2.60 (6)3.144 (4)129 (5)
O92—H49···O41i1.00 (5)1.82 (6)2.816 (4)170 (5)
O101—H210···O91viii0.93 (5)1.83 (5)2.753 (5)172 (5)
O101—H110···O120.83 (6)1.90 (6)2.733 (4)174 (5)
O102—H410···O92viii0.74 (5)2.38 (6)2.761 (4)114 (6)
O102—H310···O110.80 (6)1.94 (6)2.729 (4)168 (5)
Symmetry codes: (i) x, y, z1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y1/2, z+1; (v) x+1/2, y1/2, z; (vii) x1/2, y+1/2, z+1; (viii) x, y, z+1; (x) x1/2, y1/2, z+1; (xi) x1/2, y+1/2, z; (xiii) x+1/2, y1/2, z+2; (xiv) x1/2, y+1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (298K_anh) top
Crystal data top
C4H12KNaO10Dx = 1.776 Mg m3
Mr = 282.22Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 6467 reflections
a = 11.8843 (9) Åθ = 3.6–28.7°
b = 14.2668 (12) ŵ = 0.59 mm1
c = 6.2266 (5) ÅT = 298 K
V = 1055.74 (14) Å3Prism, clear colourless
Z = 40.48 × 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 Source2175 reflections with I 2u(I)
Graphite monochromatorRint = 0.057
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1918
Tmin = 0.750, Tmax = 1.000l = 88
18499 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.13Δρmax = 0.39 e Å3
2713 reflectionsΔρmin = 0.29 e Å3
195 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
1 restraintAbsolute structure parameter: 0.06 (3)
12 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00.00.0469 (3)0.0631 (7)
K20.50.00.15886 (12)0.03640 (19)
Na0.23137 (7)0.00679 (7)0.52269 (14)0.0304 (2)
O10.12004 (13)0.10919 (11)0.3507 (3)0.0289 (4)
O20.20945 (15)0.20275 (12)0.1192 (3)0.0345 (4)
O30.23313 (16)0.40623 (12)0.8129 (3)0.0404 (4)
O40.05341 (15)0.36239 (13)0.8440 (3)0.0390 (4)
O50.16324 (15)0.35716 (12)0.3240 (3)0.0298 (4)
H50.189 (2)0.342 (2)0.216 (5)0.0447 (6)*
O60.29523 (14)0.24820 (12)0.6277 (3)0.0329 (4)
H60.327 (3)0.290 (2)0.607 (5)0.0493 (6)*
O70.39556 (15)0.08240 (14)0.4847 (3)0.0370 (5)
H170.368 (3)0.131 (2)0.521 (6)0.0555 (7)*
H270.431 (3)0.091 (2)0.374 (5)0.0555 (7)*
O80.2437 (2)0.04125 (15)0.8852 (3)0.0513 (6)
H180.258 (3)0.003 (3)0.986 (6)0.0770 (9)*
H280.236 (3)0.096 (3)0.947 (6)0.0770 (9)*
O90.06177 (18)0.1981 (2)0.0344 (4)0.0612 (7)
H190.115 (4)0.224 (3)0.009 (7)0.0918 (10)*
H290.034 (3)0.253 (3)0.085 (6)0.0918 (10)*
O100.07534 (19)0.10238 (18)0.5816 (5)0.0615 (7)
H1100.017 (4)0.100 (3)0.523 (6)0.0922 (11)*
H2100.068 (3)0.131 (3)0.701 (7)0.0922 (11)*
C10.15407 (19)0.18764 (16)0.2851 (4)0.0236 (5)
C20.12502 (19)0.27322 (16)0.4227 (4)0.0237 (5)
H20.041 (2)0.2798 (17)0.437 (4)0.0284 (6)*
C30.17776 (19)0.26416 (16)0.6448 (4)0.0246 (5)
H30.148 (2)0.2085 (18)0.719 (4)0.0295 (6)*
C40.1526 (2)0.35159 (17)0.7794 (4)0.0295 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0734 (15)0.0649 (17)0.0511 (14)0.0351 (14)0.0000000.000000
K20.0363 (4)0.0406 (4)0.0323 (4)0.0045 (4)0.0000000.000000
Na0.0293 (4)0.0276 (5)0.0343 (5)0.0008 (4)0.0013 (4)0.0007 (4)
O10.0312 (8)0.0241 (8)0.0314 (8)0.0020 (7)0.0013 (8)0.0009 (7)
O20.0444 (10)0.0306 (9)0.0285 (9)0.0002 (8)0.0077 (8)0.0017 (7)
O30.0526 (11)0.0303 (9)0.0383 (10)0.0082 (8)0.0034 (9)0.0076 (8)
O40.0396 (10)0.0461 (11)0.0314 (9)0.0127 (9)0.0016 (8)0.0075 (9)
O50.0440 (10)0.0224 (8)0.0230 (8)0.0002 (7)0.0001 (8)0.0006 (7)
O60.0283 (9)0.0290 (10)0.0415 (10)0.0042 (7)0.0051 (8)0.0011 (8)
O70.0324 (10)0.0322 (10)0.0464 (12)0.0001 (8)0.0071 (9)0.0025 (9)
O80.0961 (17)0.0295 (10)0.0283 (10)0.0114 (11)0.0052 (11)0.0004 (8)
O90.0394 (12)0.090 (2)0.0543 (14)0.0073 (12)0.0101 (11)0.0074 (13)
O100.0365 (11)0.0654 (15)0.0826 (18)0.0161 (11)0.0181 (12)0.0319 (13)
C10.0233 (11)0.0254 (12)0.0222 (11)0.0014 (9)0.0033 (9)0.0004 (9)
C20.0251 (11)0.0205 (11)0.0253 (11)0.0012 (9)0.0002 (10)0.0001 (9)
C30.0275 (11)0.0228 (11)0.0236 (11)0.0018 (9)0.0008 (10)0.0014 (10)
C40.0426 (15)0.0258 (12)0.0202 (11)0.0043 (11)0.0051 (11)0.0006 (9)
Geometric parameters (Å, º) top
K1—O12.835 (2)Na—O72.342 (2)
K1—O1i2.835 (2)Na—O82.363 (2)
K1—O8ii3.122 (3)Na—O102.331 (2)
K1—O8iii3.122 (3)Na—C4v3.086 (3)
K1—H18iii3.08 (4)O1—C11.258 (3)
K1—H18ii3.08 (4)O2—C11.244 (3)
K1—O9i2.963 (3)O3—C41.252 (3)
K1—O92.963 (3)O4—C41.255 (3)
K1—O10ii3.366 (4)O5—H50.77 (3)
K1—O10iii3.366 (4)O5—C21.420 (3)
K1—H210ii2.96 (4)O6—H60.72 (3)
K1—H210iii2.96 (4)O6—C31.418 (3)
K2—O4iv2.8462 (18)O7—H170.80 (3)
K2—O4v2.8462 (18)O7—H270.81 (3)
K2—O5vi2.9957 (17)O8—H180.85 (4)
K2—O5vii2.9957 (17)O8—H280.87 (4)
K2—O7iii2.802 (2)O9—H190.78 (4)
K2—O7viii2.802 (2)O9—H290.91 (4)
K2—O8iii3.114 (3)O10—H1100.79 (4)
K2—O8viii3.114 (3)O10—H2100.85 (4)
K2—H18viii3.02 (4)C1—C21.531 (3)
K2—H18iii3.02 (4)C2—H21.00 (2)
Na—O12.3740 (19)C2—C31.524 (3)
Na—O3v2.467 (2)C3—H30.99 (3)
Na—O5v2.499 (2)C3—C41.532 (3)
Naii—K1—Naiii80.26 (4)O8iii—K2—O5vii122.35 (5)
O1—K1—Naiii101.44 (4)O8iii—K2—O5vi61.67 (5)
O1—K1—Naii145.25 (4)O8viii—K2—O5vi122.35 (5)
O1i—K1—Naiii145.25 (4)O8iii—K2—O7iii63.72 (5)
O1i—K1—Naii101.44 (4)O8viii—K2—O7viii63.72 (5)
O1i—K1—O196.32 (9)O8iii—K2—O7viii125.61 (6)
O8iii—K1—Naiii32.88 (4)O8viii—K2—O7iii125.61 (6)
O8iii—K1—Naii110.28 (7)O8viii—K2—O8iii169.90 (7)
O8ii—K1—Naii32.88 (4)H18viii—K2—Naiii165.4 (7)
O8ii—K1—Naiii110.28 (7)H18iii—K2—Naiii49.3 (7)
O8ii—K1—O1141.76 (6)H18viii—K2—Naviii49.3 (7)
O8iii—K1—O1i141.76 (6)H18iii—K2—Naviii165.4 (7)
O8iii—K1—O169.20 (5)H18iii—K2—O4iv89.9 (7)
O8ii—K1—O1i69.20 (5)H18viii—K2—O4v89.9 (7)
O8ii—K1—O8iii142.37 (10)H18iii—K2—O4v65.8 (8)
H18ii—K1—Naii42.9 (7)H18viii—K2—O4iv65.8 (8)
H18iii—K1—Naii123.0 (7)H18iii—K2—O5vi59.5 (8)
H18ii—K1—Naiii123.0 (7)H18viii—K2—O5vi135.4 (8)
H18iii—K1—Naiii42.9 (7)H18viii—K2—O5vii59.5 (8)
H18iii—K1—O1i126.0 (8)H18iii—K2—O5vii135.4 (8)
H18ii—K1—O1i64.9 (7)H18iii—K2—O7iii79.0 (7)
H18ii—K1—O1126.0 (8)H18viii—K2—O7viii79.0 (7)
H18iii—K1—O164.9 (7)H18iii—K2—O7viii131.6 (7)
H18ii—K1—O8ii15.8 (7)H18viii—K2—O7iii131.6 (7)
H18iii—K1—O8iii15.8 (7)H18iii—K2—O8viii155.4 (7)
H18ii—K1—O8iii152.0 (7)H18iii—K2—O8iii15.9 (8)
H18iii—K1—O8ii152.0 (7)H18viii—K2—O8iii155.4 (7)
H18ii—K1—H18iii165.9 (14)H18viii—K2—O8viii15.9 (8)
O9—K1—Naii92.90 (6)H18viii—K2—H18iii145.2 (14)
O9—K1—Naiii71.83 (6)K2ix—Na—K1x98.23 (3)
O9i—K1—Naii71.83 (6)O1—Na—K1x88.29 (5)
O9i—K1—Naiii92.90 (6)O1—Na—K2ix133.89 (5)
O9—K1—O1i73.42 (6)O3v—Na—K1x140.29 (6)
O9i—K1—O173.42 (6)O3v—Na—K2ix108.33 (5)
O9—K1—O1120.88 (7)O3v—Na—O193.65 (6)
O9i—K1—O1i120.88 (7)O5v—Na—K1x92.77 (5)
O9—K1—O8iii83.96 (6)O5v—Na—K2ix52.63 (4)
O9i—K1—O8iii89.71 (6)O5v—Na—O1173.15 (7)
O9—K1—O8ii89.71 (6)O5v—Na—O3v81.21 (6)
O9i—K1—O8ii83.96 (6)O7—Na—K1x126.99 (6)
O9—K1—H18iii75.2 (8)O7—Na—K2ix48.06 (5)
O9i—K1—H18ii75.2 (8)O7—Na—O192.29 (7)
O9—K1—H18ii102.3 (8)O7—Na—O3v92.59 (8)
O9i—K1—H18iii102.3 (8)O7—Na—O5v92.47 (7)
O9i—K1—O9160.33 (13)O8—Na—K1x45.83 (7)
O10iii—K1—Naii61.51 (5)O8—Na—K2ix55.68 (6)
O10ii—K1—Naiii61.51 (5)O8—Na—O1105.27 (8)
O10iii—K1—Naiii32.93 (4)O8—Na—O3v160.79 (8)
O10ii—K1—Naii32.93 (4)O8—Na—O5v80.18 (7)
O10iii—K1—O1i118.01 (5)O8—Na—O783.53 (8)
O10ii—K1—O1i132.75 (5)O10—Na—K1x51.72 (8)
O10ii—K1—O1118.01 (5)O10—Na—K2ix127.42 (7)
O10iii—K1—O1132.75 (5)O10—Na—O192.03 (8)
O10iii—K1—O8ii83.53 (6)O10—Na—O3v88.58 (9)
O10iii—K1—O8iii63.73 (6)O10—Na—O5v83.35 (8)
O10ii—K1—O8iii83.53 (6)O10—Na—O7175.44 (9)
O10ii—K1—O8ii63.73 (6)O10—Na—O893.94 (10)
O10iii—K1—H18iii68.6 (7)C4v—Na—K1x140.24 (5)
O10ii—K1—H18ii68.6 (7)C4v—Na—K2ix87.64 (5)
O10iii—K1—H18ii98.8 (7)C4v—Na—O1115.49 (7)
O10ii—K1—H18iii98.8 (7)C4v—Na—O3v22.75 (6)
O10iii—K1—O951.19 (7)C4v—Na—O5v60.03 (6)
O10ii—K1—O9i51.19 (7)C4v—Na—O785.51 (7)
O10iii—K1—O9i109.44 (9)C4v—Na—O8138.10 (8)
O10ii—K1—O9109.44 (9)C4v—Na—O1093.92 (10)
O10ii—K1—O10iii61.20 (9)Na—O1—K1101.45 (6)
H210ii—K1—Naiii68.5 (8)C1—O1—K1115.73 (15)
H210iii—K1—Naiii41.8 (8)C1—O1—Na125.97 (14)
H210ii—K1—Naii41.8 (8)C4—O3—Naxi107.62 (15)
H210iii—K1—Naii68.5 (8)C4—O4—K2xii120.99 (16)
H210iii—K1—O1i106.0 (8)Naxi—O5—K2xiii85.83 (5)
H210ii—K1—O1i134.0 (8)H5—O5—K2xiii98 (2)
H210ii—K1—O1106.0 (8)H5—O5—Naxi111 (2)
H210iii—K1—O1134.0 (8)C2—O5—K2xiii120.99 (13)
H210ii—K1—O8iii84.2 (8)C2—O5—Naxi130.53 (14)
H210iii—K1—O8ii84.2 (8)C2—O5—H5105 (2)
H210iii—K1—O8iii68.4 (8)C3—O6—H6113 (3)
H210ii—K1—O8ii68.4 (8)Na—O7—K2xiv93.50 (7)
H210ii—K1—H18ii69.4 (11)H17—O7—K2xiv109 (2)
H210iii—K1—H18iii69.4 (11)H17—O7—Na95 (2)
H210ii—K1—H18iii99.9 (11)H27—O7—K2xiv121 (2)
H210iii—K1—H18ii99.9 (11)H27—O7—Na126 (2)
H210ii—K1—O9123.0 (9)H27—O7—H17108 (3)
H210iii—K1—O9i123.0 (9)K2xiv—O8—K1xiv154.16 (8)
H210iii—K1—O937.5 (9)Na—O8—K1xiv101.29 (9)
H210ii—K1—O9i37.5 (9)Na—O8—K2xiv85.51 (7)
H210iii—K1—O10ii73.8 (9)H18—O8—K1xiv80 (2)
H210ii—K1—O10ii13.7 (9)H18—O8—K2xiv76 (2)
H210iii—K1—O10iii13.7 (9)H18—O8—Na122 (3)
H210ii—K1—O10iii73.8 (9)H28—O8—K1xiv86 (3)
H210ii—K1—H210iii86.8 (17)H28—O8—K2xiv108 (2)
Naviii—K2—Naiii116.33 (3)H28—O8—Na132 (2)
O4iv—K2—Naviii98.98 (4)H28—O8—H18106 (3)
O4v—K2—Naviii124.78 (4)K2xiv—H18—K1xiv169.6 (14)
O4v—K2—Naiii98.98 (4)O8—H18—K1xiv85 (3)
O4iv—K2—Naiii124.78 (4)O8—H18—K2xiv88 (3)
O4v—K2—O4iv92.93 (8)H19—O9—K1i127 (3)
O5vi—K2—Naviii112.73 (4)H29—O9—K1i143 (3)
O5vi—K2—Naiii41.54 (4)H29—O9—H1990 (4)
O5vii—K2—Naiii112.73 (4)Na—O10—K1x95.35 (9)
O5vii—K2—Naviii41.54 (4)H110—O10—K1x98 (3)
O5vi—K2—O4v67.84 (5)H110—O10—Na128 (3)
O5vi—K2—O4iv148.22 (5)H210—O10—K1x55 (3)
O5vii—K2—O4v148.22 (5)H210—O10—Na120 (3)
O5vii—K2—O4iv67.84 (5)H210—O10—H110109 (4)
O5vi—K2—O5vii139.85 (7)O10—H210—K1x111 (3)
O7viii—K2—Naviii38.44 (4)O2—C1—O1126.4 (2)
O7iii—K2—Naviii86.99 (4)C2—C1—O1117.1 (2)
O7viii—K2—Naiii86.99 (4)C2—C1—O2116.5 (2)
O7iii—K2—Naiii38.44 (4)C1—C2—O5111.00 (18)
O7iii—K2—O4iv110.80 (6)H2—C2—O5106.0 (14)
O7iii—K2—O4v137.42 (5)H2—C2—C1110.3 (14)
O7viii—K2—O4iv137.42 (5)C3—C2—O5109.42 (18)
O7viii—K2—O4v110.80 (6)C3—C2—C1110.32 (19)
O7iii—K2—O5vi74.13 (5)C3—C2—H2109.6 (14)
O7viii—K2—O5vii74.13 (5)C2—C3—O6110.49 (19)
O7iii—K2—O5vii74.31 (5)H3—C3—O6105.1 (14)
O7viii—K2—O5vi74.31 (5)H3—C3—C2110.3 (15)
O7viii—K2—O7iii75.21 (8)C4—C3—O6111.3 (2)
O8viii—K2—Naiii150.70 (4)C4—C3—C2110.30 (18)
O8iii—K2—Naiii38.81 (4)C4—C3—H3109.1 (14)
O8viii—K2—Naviii38.81 (4)O3—C4—Naxi49.63 (12)
O8iii—K2—Naviii150.70 (4)O4—C4—Naxi122.33 (17)
O8viii—K2—O4iv81.47 (5)O4—C4—O3126.0 (2)
O8iii—K2—O4iv91.55 (5)C3—C4—Naxi96.46 (14)
O8iii—K2—O4v81.47 (5)C3—C4—O3116.7 (2)
O8viii—K2—O4v91.55 (5)C3—C4—O4117.3 (2)
O8viii—K2—O5vii61.67 (5)
K1—O1—C1—O251.59 (16)Naxi—O3—C4—C374.82 (14)
K1i—O1—C1—O251.59 (16)Naxi—O5—C2—C1133.35 (18)
K1—O1—C1—C2128.58 (14)Naxi—O5—C2—C311.35 (17)
K1i—O1—C1—C2128.58 (14)Naxi—C4—C3—O662.91 (14)
K2xii—O4—C4—Naxi73.36 (14)Naxi—C4—C3—C260.13 (14)
K2—O4v—C4v—Na73.36 (14)O1—C1—C2—O5176.8 (2)
K2xii—O4—C4—O312.54 (19)O1—C1—C2—C361.7 (2)
K2xi—O4—C4—O312.54 (19)O2—C1—C2—O53.3 (2)
K2xii—O4—C4—C3168.19 (15)O2—C1—C2—C3118.2 (2)
K2xi—O4—C4—C3168.19 (15)O3—C4—C3—O615.2 (2)
K2xv—O5—C2—C1112.95 (15)O3—C4—C3—C2107.9 (2)
K2xiii—O5—C2—C1112.95 (15)O4—C4—C3—O6165.5 (2)
K2xiii—O5—C2—C3125.05 (15)O4—C4—C3—C271.5 (2)
K2xv—O5—C2—C3125.05 (15)O5—C2—C3—O668.19 (19)
Na—O1—C1—O276.86 (19)O5—C2—C3—C455.3 (2)
Na—O1—C1—C2102.96 (17)O6—C3—C2—C154.2 (2)
Naxi—O3—C4—O4104.45 (16)C1—C2—C3—C4177.75 (19)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y1/2, z; (vii) x+1/2, y+1/2, z; (viii) x+1, y, z1; (ix) x+1, y, z+1; (x) x, y, z+1; (xi) x+1/2, y+1/2, z+1; (xii) x1/2, y+1/2, z+1; (xiii) x1/2, 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···AD—HH···AD···AD—H···A
O5—H5···O20.77 (3)2.09 (3)2.604 (2)125 (3)
O5—H5···O3iii0.77 (3)2.72 (3)3.363 (3)142 (3)
O5—H5···O4iii0.77 (3)2.83 (3)3.262 (3)118 (3)
O6—H6···O10xi0.72 (3)2.25 (3)2.934 (4)158 (4)
O7—H17···O60.80 (3)2.00 (4)2.795 (3)176 (4)
O7—H27···O4iv0.81 (3)2.10 (3)2.886 (3)162 (3)
O8—H18···O3xvi0.85 (4)1.86 (4)2.706 (3)170 (4)
O8—H28···O1xiv0.87 (4)2.87 (4)3.391 (3)120 (3)
O8—H28···O2xiv0.87 (4)1.89 (4)2.756 (3)170 (4)
O9—H19···O2vi0.78 (4)2.47 (4)3.110 (3)141 (4)
O9—H19···O3v0.78 (4)2.82 (5)3.171 (3)110 (4)
O9—H19···O6v0.78 (4)2.53 (4)3.144 (3)136 (4)
O9—H29···O4ii0.91 (4)1.92 (4)2.819 (3)167 (4)
O10—H110···O1i0.79 (4)1.95 (4)2.733 (3)172 (4)
O10—H210···O9xiv0.85 (4)1.91 (4)2.758 (4)176 (4)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y1/2, z; (xi) x+1/2, y+1/2, z+1; (xiv) x, y, z+1; (xvi) x+1/2, y1/2, z+2.
Sodium potassium L(+)-tartrate tetrahydrate (308K_anh) top
Crystal data top
C4H12KNaO10Dx = 1.771 Mg m3
Mr = 282.22Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P21212Cell parameters from 6554 reflections
a = 11.8996 (9) Åθ = 3.5–28.7°
b = 14.2713 (11) ŵ = 0.58 mm1
c = 6.2331 (4) ÅT = 308 K
V = 1058.51 (13) Å3Prism, clear colourless
Z = 40.48 × 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 Source2156 reflections with I 2u(I)
Graphite monochromatorRint = 0.064
Detector resolution: 10.3457 pixels mm-1θmax = 29.4°, θmin = 3.3°
ω scansh = 1616
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 = 1819
Tmin = 0.461, Tmax = 1.000l = 88
18474 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullOnly 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 = 1.10Δρmax = 0.29 e Å3
2726 reflectionsΔρmin = 0.32 e Å3
195 parametersAbsolute structure: Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.
1 restraintAbsolute structure parameter: 0.06 (3)
12 constraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
K10.00.00.0473 (4)0.0648 (8)
K20.50.00.15874 (13)0.0375 (2)
Na0.23131 (8)0.00680 (8)0.52312 (15)0.0312 (2)
O10.12004 (14)0.10919 (12)0.3508 (3)0.0301 (4)
O20.20924 (17)0.20259 (13)0.1194 (3)0.0354 (4)
O30.23338 (17)0.40629 (13)0.8127 (3)0.0414 (5)
O40.05368 (17)0.36267 (14)0.8437 (3)0.0402 (5)
O50.16323 (16)0.35709 (12)0.3237 (3)0.0307 (4)
H50.189 (3)0.341 (2)0.205 (6)0.0460 (6)*
O60.29515 (15)0.24816 (13)0.6273 (3)0.0330 (4)
H60.327 (3)0.293 (2)0.614 (6)0.0495 (7)*
O70.39539 (16)0.08229 (15)0.4848 (4)0.0381 (5)
H170.363 (3)0.134 (3)0.526 (6)0.0571 (7)*
H270.434 (3)0.094 (3)0.379 (6)0.0571 (7)*
O80.2440 (2)0.04116 (17)0.8857 (3)0.0528 (6)
H180.261 (3)0.002 (3)0.984 (7)0.0791 (10)*
H280.235 (3)0.094 (3)0.947 (7)0.0791 (10)*
O90.0620 (2)0.1988 (2)0.0347 (5)0.0626 (7)
H190.115 (4)0.228 (4)0.009 (8)0.0939 (11)*
H290.033 (4)0.257 (3)0.078 (7)0.0939 (11)*
O100.0751 (2)0.1019 (2)0.5830 (5)0.0643 (8)
H1100.016 (4)0.100 (3)0.526 (7)0.0964 (12)*
H2100.070 (4)0.137 (3)0.704 (8)0.0964 (12)*
C10.1540 (2)0.18754 (17)0.2845 (4)0.0241 (5)
C20.1249 (2)0.27307 (17)0.4226 (4)0.0247 (5)
H20.041 (2)0.2784 (19)0.436 (4)0.0297 (6)*
C30.1780 (2)0.26408 (17)0.6447 (4)0.0250 (5)
H30.148 (2)0.211 (2)0.723 (5)0.0300 (6)*
C40.1528 (2)0.35170 (18)0.7791 (4)0.0304 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0739 (16)0.0690 (19)0.0516 (15)0.0377 (16)0.0000000.000000
K20.0373 (4)0.0415 (5)0.0336 (4)0.0043 (4)0.0000000.000000
Na0.0299 (5)0.0281 (5)0.0357 (5)0.0008 (4)0.0016 (4)0.0011 (5)
O10.0333 (9)0.0240 (9)0.0330 (9)0.0017 (7)0.0014 (8)0.0008 (8)
O20.0454 (11)0.0317 (10)0.0292 (10)0.0001 (8)0.0077 (9)0.0012 (8)
O30.0530 (12)0.0309 (10)0.0402 (11)0.0089 (9)0.0039 (10)0.0071 (9)
O40.0406 (10)0.0472 (12)0.0327 (10)0.0123 (9)0.0013 (9)0.0085 (10)
O50.0455 (11)0.0220 (9)0.0246 (9)0.0001 (8)0.0001 (8)0.0015 (7)
O60.0284 (10)0.0285 (10)0.0420 (11)0.0046 (7)0.0058 (9)0.0023 (9)
O70.0330 (10)0.0322 (11)0.0489 (13)0.0008 (8)0.0073 (9)0.0031 (10)
O80.0973 (19)0.0304 (11)0.0305 (11)0.0124 (12)0.0057 (12)0.0002 (8)
O90.0416 (13)0.091 (2)0.0548 (15)0.0085 (13)0.0106 (12)0.0070 (14)
O100.0373 (12)0.0674 (17)0.088 (2)0.0182 (11)0.0197 (13)0.0341 (15)
C10.0247 (12)0.0237 (12)0.0240 (12)0.0019 (10)0.0044 (10)0.0008 (9)
C20.0263 (12)0.0214 (12)0.0265 (12)0.0012 (10)0.0009 (10)0.0009 (10)
C30.0287 (12)0.0218 (12)0.0245 (11)0.0025 (10)0.0010 (10)0.0012 (10)
C40.0438 (16)0.0263 (13)0.0211 (12)0.0047 (12)0.0043 (11)0.0009 (10)
Geometric parameters (Å, º) top
K1—O12.837 (2)Na—O82.366 (2)
K1—O1i2.837 (2)Na—O102.332 (2)
K1—O8ii3.129 (3)Na—C4v3.087 (3)
K1—O8iii3.129 (3)O1—C11.259 (3)
K1—O9i2.975 (3)O2—C11.240 (3)
K1—O92.975 (3)O3—C41.253 (3)
K1—O10iii3.360 (4)O4—C41.256 (3)
K1—O10ii3.360 (4)O5—H50.83 (4)
K1—H210ii3.01 (5)O5—C21.423 (3)
K1—H210iii3.01 (5)O6—H60.74 (3)
K2—O4iv2.847 (2)O6—C31.417 (3)
K2—O4v2.847 (2)O7—H170.87 (4)
K2—O5vi2.9983 (18)O7—H270.82 (4)
K2—O5vii2.9983 (18)O8—H180.86 (5)
K2—O7iii2.805 (2)O8—H280.86 (5)
K2—O7viii2.805 (2)O9—H190.80 (5)
K2—O8iii3.115 (3)O9—H290.94 (5)
K2—O8viii3.115 (3)O10—H1100.79 (5)
K2—H18iii2.98 (4)O10—H2100.90 (5)
K2—H18viii2.98 (4)C1—C21.533 (3)
Na—O12.376 (2)C2—H21.00 (3)
Na—O3v2.469 (2)C2—C31.527 (3)
Na—O5v2.502 (2)C3—H30.97 (3)
Na—O72.342 (2)C3—C41.535 (3)
Naii—K1—Naiii80.26 (5)H18viii—K2—Naiii165.5 (8)
O1i—K1—Naiii145.26 (4)H18viii—K2—O4v90.1 (8)
O1—K1—Naiii101.43 (4)H18viii—K2—O4iv65.5 (9)
O1—K1—Naii145.26 (4)H18iii—K2—O4v65.5 (9)
O1i—K1—Naii101.43 (4)H18iii—K2—O4iv90.1 (8)
O1i—K1—O196.34 (10)H18iii—K2—O5vii135.7 (9)
O8ii—K1—Naiii110.32 (7)H18viii—K2—O5vii59.4 (8)
O8ii—K1—Naii32.90 (5)H18iii—K2—O5vi59.4 (8)
O8iii—K1—Naii110.32 (7)H18viii—K2—O5vi135.7 (9)
O8iii—K1—Naiii32.90 (5)H18iii—K2—O7iii79.1 (8)
O8ii—K1—O1i69.17 (5)H18viii—K2—O7iii131.6 (8)
O8iii—K1—O1i141.73 (7)H18iii—K2—O7viii131.6 (8)
O8iii—K1—O169.17 (5)H18viii—K2—O7viii79.1 (8)
O8ii—K1—O1141.73 (7)H18iii—K2—O8viii155.2 (8)
O8ii—K1—O8iii142.44 (11)H18iii—K2—O8iii16.0 (9)
O9—K1—Naii92.87 (7)H18viii—K2—O8iii155.2 (8)
O9i—K1—Naii71.78 (6)H18viii—K2—O8viii16.0 (9)
O9—K1—Naiii71.78 (6)H18viii—K2—H18iii145.1 (16)
O9i—K1—Naiii92.87 (7)K2ix—Na—K1x98.27 (3)
O9—K1—O1i73.49 (7)O1—Na—K1x88.32 (5)
O9i—K1—O173.49 (7)O1—Na—K2ix133.91 (6)
O9—K1—O1120.89 (7)O3v—Na—K1x140.28 (6)
O9i—K1—O1i120.89 (7)O3v—Na—K2ix108.36 (6)
O9i—K1—O8ii83.89 (7)O3v—Na—O193.54 (7)
O9—K1—O8iii83.89 (7)O5v—Na—K1x92.81 (5)
O9i—K1—O8iii89.76 (7)O5v—Na—K2ix52.62 (4)
O9—K1—O8ii89.76 (7)O5v—Na—O1173.12 (8)
O9i—K1—O9160.21 (14)O5v—Na—O3v81.26 (7)
O10ii—K1—Naiii61.48 (5)O7—Na—K1x127.06 (7)
O10ii—K1—Naii32.90 (4)O7—Na—K2ix48.06 (6)
O10iii—K1—Naiii32.90 (4)O7—Na—O192.31 (8)
O10iii—K1—Naii61.48 (5)O7—Na—O3v92.54 (8)
O10iii—K1—O1i118.07 (6)O7—Na—O5v92.42 (7)
O10ii—K1—O1118.07 (6)O8—Na—K1x45.91 (7)
O10iii—K1—O1132.72 (6)O8—Na—K2ix55.61 (7)
O10ii—K1—O1i132.72 (6)O8—Na—O1105.40 (8)
O10iii—K1—O8iii63.72 (6)O8—Na—O3v160.76 (9)
O10ii—K1—O8ii63.72 (6)O8—Na—O5v80.10 (8)
O10iii—K1—O8ii83.58 (7)O8—Na—O783.53 (9)
O10ii—K1—O8iii83.58 (7)O10—Na—K1x51.49 (9)
O10iii—K1—O951.20 (8)O10—Na—K2ix127.44 (8)
O10iii—K1—O9i109.31 (10)O10—Na—O191.92 (8)
O10ii—K1—O9109.31 (10)O10—Na—O3v88.79 (10)
O10ii—K1—O9i51.20 (8)O10—Na—O5v83.51 (9)
O10ii—K1—O10iii61.07 (10)O10—Na—O7175.48 (10)
H210ii—K1—Naiii69.5 (9)O10—Na—O893.80 (11)
H210ii—K1—Naii42.7 (9)C4v—Na—K1x140.28 (6)
H210iii—K1—Naiii42.7 (9)C4v—Na—K2ix87.64 (6)
H210iii—K1—Naii69.5 (9)C4v—Na—O1115.40 (7)
H210ii—K1—O1104.9 (9)C4v—Na—O3v22.78 (7)
H210ii—K1—O1i133.7 (9)C4v—Na—O5v60.05 (7)
H210iii—K1—O1133.7 (9)C4v—Na—O785.43 (8)
H210iii—K1—O1i104.9 (9)C4v—Na—O8138.04 (9)
H210iii—K1—O8iii68.7 (9)C4v—Na—O1094.19 (10)
H210ii—K1—O8ii68.7 (9)Na—O1—K1101.50 (7)
H210iii—K1—O8ii84.6 (9)C1—O1—K1115.49 (16)
H210ii—K1—O8iii84.6 (9)C1—O1—Na126.04 (15)
H210iii—K1—O936.1 (10)C4—O3—Naxi107.51 (16)
H210ii—K1—O9i36.1 (10)C4—O4—K2xii121.17 (17)
H210iii—K1—O9i124.3 (10)Naxi—O5—K2xiii85.85 (6)
H210ii—K1—O9124.3 (10)H5—O5—K2xiii97 (2)
H210iii—K1—O10iii15.1 (10)H5—O5—Naxi111 (2)
H210ii—K1—O10iii75.0 (10)C2—O5—K2xiii120.94 (14)
H210ii—K1—O10ii15.1 (10)C2—O5—Naxi130.50 (15)
H210iii—K1—O10ii75.0 (10)C2—O5—H5106 (2)
H210ii—K1—H210iii89.5 (19)C3—O6—H6112 (3)
Naviii—K2—Naiii116.41 (4)Na—O7—K2xiv93.54 (7)
O4iv—K2—Naiii124.88 (4)H17—O7—K2xiv108 (2)
O4iv—K2—Naviii98.92 (4)H17—O7—Na93 (2)
O4v—K2—Naiii98.92 (4)H27—O7—K2xiv118 (2)
O4v—K2—Naviii124.88 (4)H27—O7—Na131 (3)
O4v—K2—O4iv92.77 (9)H27—O7—H17108 (3)
O5vi—K2—Naviii112.78 (4)K2xiv—O8—K1xiv154.26 (8)
O5vii—K2—Naiii112.78 (4)Na—O8—K1xiv101.19 (10)
O5vi—K2—Naiii41.53 (4)Na—O8—K2xiv85.58 (7)
O5vii—K2—Naviii41.53 (4)H18—O8—K1xiv82 (3)
O5vii—K2—O4iv67.85 (5)H18—O8—K2xiv73 (3)
O5vi—K2—O4v67.85 (5)H18—O8—Na121 (3)
O5vii—K2—O4v148.23 (6)H28—O8—K1xiv84 (3)
O5vi—K2—O4iv148.23 (6)H28—O8—K2xiv109 (3)
O5vi—K2—O5vii139.89 (8)H28—O8—Na133 (3)
O7viii—K2—Naviii38.40 (4)H28—O8—H18107 (4)
O7iii—K2—Naiii38.40 (4)O8—H18—K2xiv91 (3)
O7viii—K2—Naiii87.07 (5)H19—O9—K1i129 (4)
O7iii—K2—Naviii87.07 (5)H29—O9—K1i143 (3)
O7iii—K2—O4iv110.97 (6)H29—O9—H1986 (4)
O7iii—K2—O4v137.32 (6)Na—O10—K1x95.62 (10)
O7viii—K2—O4iv137.32 (6)H110—O10—K1x98 (3)
O7viii—K2—O4v110.97 (6)H110—O10—Na128 (3)
O7iii—K2—O5vi74.07 (6)H210—O10—K1x60 (3)
O7viii—K2—O5vi74.39 (6)H210—O10—Na121 (3)
O7viii—K2—O5vii74.07 (6)H210—O10—H110109 (4)
O7iii—K2—O5vii74.39 (6)O10—H210—K1x105 (3)
O7viii—K2—O7iii75.20 (9)O2—C1—O1126.6 (2)
O8viii—K2—Naiii150.79 (5)C2—C1—O1116.7 (2)
O8viii—K2—Naviii38.81 (4)C2—C1—O2116.6 (2)
O8iii—K2—Naiii38.81 (4)C1—C2—O5110.79 (19)
O8iii—K2—Naviii150.79 (5)H2—C2—O5106.9 (16)
O8iii—K2—O4v81.32 (6)H2—C2—C1109.4 (16)
O8viii—K2—O4iv81.32 (6)C3—C2—O5109.32 (19)
O8iii—K2—O4iv91.63 (6)C3—C2—C1110.4 (2)
O8viii—K2—O4v91.63 (6)C3—C2—H2110.0 (15)
O8iii—K2—O5vii122.40 (6)C2—C3—O6110.6 (2)
O8viii—K2—O5vi122.40 (6)H3—C3—O6105.9 (16)
O8iii—K2—O5vi61.65 (6)H3—C3—C2112.0 (17)
O8viii—K2—O5vii61.65 (6)C4—C3—O6111.4 (2)
O8iii—K2—O7iii63.73 (6)C4—C3—C2110.21 (19)
O8iii—K2—O7viii125.69 (6)C4—C3—H3106.6 (16)
O8viii—K2—O7iii125.69 (6)O3—C4—Naxi49.71 (13)
O8viii—K2—O7viii63.73 (6)O4—C4—Naxi122.25 (18)
O8viii—K2—O8iii169.81 (8)O4—C4—O3126.0 (2)
H18iii—K2—Naviii165.5 (8)C3—C4—Naxi96.47 (15)
H18viii—K2—Naviii49.3 (8)C3—C4—O3116.6 (2)
H18iii—K2—Naiii49.3 (8)C3—C4—O4117.4 (2)
K1—O1—C1—O251.75 (17)Naxi—O3—C4—C374.94 (15)
K1i—O1—C1—O251.75 (17)Naxi—O5—C2—C1133.41 (19)
K1—O1—C1—C2128.74 (15)Naxi—O5—C2—C311.50 (18)
K1i—O1—C1—C2128.74 (15)Naxi—C4—C3—O662.84 (15)
K2xii—O4—C4—Naxi73.51 (16)Naxi—C4—C3—C260.29 (15)
K2—O4v—C4v—Na73.51 (16)O1—C1—C2—O5177.0 (2)
K2xii—O4—C4—O312.6 (2)O1—C1—C2—C361.7 (2)
K2xi—O4—C4—O312.6 (2)O2—C1—C2—O53.4 (2)
K2xii—O4—C4—C3168.01 (16)O2—C1—C2—C3117.8 (2)
K2xi—O4—C4—C3168.01 (16)O3—C4—C3—O615.0 (2)
K2xv—O5—C2—C1112.95 (16)O3—C4—C3—C2108.1 (2)
K2xiii—O5—C2—C1112.95 (16)O4—C4—C3—O6165.6 (2)
K2xiii—O5—C2—C3125.15 (16)O4—C4—C3—C271.3 (2)
K2xv—O5—C2—C3125.15 (16)O5—C2—C3—O668.1 (2)
Na—O1—C1—O276.6 (2)O5—C2—C3—C455.5 (2)
Na—O1—C1—C2102.95 (18)O6—C3—C2—C154.0 (2)
Naxi—O3—C4—O4104.42 (17)C1—C2—C3—C4177.6 (2)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y1/2, z; (vii) x+1/2, y+1/2, z; (viii) x+1, y, z1; (ix) x+1, y, z+1; (x) x, y, z+1; (xi) x+1/2, y+1/2, z+1; (xii) x1/2, y+1/2, z+1; (xiii) x1/2, 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···AD—HH···AD···AD—H···A
O5—H5···O20.83 (4)2.06 (3)2.605 (3)122 (3)
O5—H5···O3iii0.83 (4)2.67 (4)3.367 (3)142 (3)
O5—H5···O4iii0.83 (4)2.79 (4)3.265 (3)118 (3)
O6—H6···O10xi0.74 (3)2.27 (3)2.947 (4)153 (4)
O7—H17···O60.87 (4)1.93 (4)2.796 (3)178 (3)
O7—H27···O4iv0.82 (4)2.08 (4)2.891 (3)168 (3)
O8—H18···O3xvi0.86 (5)1.86 (5)2.704 (3)167 (4)
O8—H28···O1xiv0.86 (5)2.87 (4)3.395 (3)121 (3)
O8—H28···O2xiv0.86 (5)1.91 (5)2.757 (3)172 (4)
O9—H19···O2vi0.80 (5)2.45 (5)3.110 (3)140 (5)
O9—H19···O3v0.80 (5)2.86 (5)3.177 (3)106 (4)
O9—H19···O6v0.80 (5)2.53 (5)3.148 (3)135 (4)
O9—H29···O4ii0.94 (5)1.89 (5)2.818 (4)169 (4)
O10—H110···O1i0.79 (5)1.95 (5)2.738 (3)171 (5)
O10—H210···O9xiv0.90 (5)1.86 (5)2.759 (4)175 (4)
Symmetry codes: (i) x, y, z; (ii) x, y, z1; (iii) x, y, z1; (iv) x+1/2, y+1/2, z+1; (v) x+1/2, y1/2, z+1; (vi) x+1/2, y1/2, z; (xi) x+1/2, y+1/2, z+1; (xiv) x, y, z+1; (xvi) x+1/2, y1/2, z+2.
 

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