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The title compound, D-(+)-glucosa­mmonium potassium tetra­thio­cyanato­cobaltate(II) dihydrate, K(C6H14NO5)[Co(NCS)4]·2H2O or (GlcNH)(K)[Co(NCS)4]·2H2O, has been obtained as a side product of an incomplete salt metathesis reaction of D-(+)-glucosa­mine hydro­chloride (GlcN·HCl) and K2[Co(NCS)4]. The asymmetric unit contains a D-(+)-glucos­ammonium cation, a potassium cation, a tetra­iso­thio­cyanato­cobalt(II) complex anion and two water mol­ecules. The water mol­ecules coordinate to the potassium cation, which is further coordinated via three short K+...SCN contacts involving three [Co(NCS)4]2− complex anions and via three O atoms of two D-(+)-glucosa­mmonium cations, leading to an overall eightfold coordination around the potassium cation. Hydrogen-bonding inter­actions between the building blocks consolidate the three-dimensional arrangement.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314619011428/wm4108sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2414314619011428/wm4108Isup3.hkl
Contains datablock I

CCDC reference: 1947086

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.038
  • wR factor = 0.058
  • Data-to-parameter ratio = 34.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O6 --H6B . Please Check PLAT780_ALERT_1_B Coordinates do not Form a Properly Connected Set Please Do !
Alert level C PLAT222_ALERT_3_C Non-Solv. Resd 1 H Uiso(max)/Uiso(min) Range 6.7 Ratio
Author Response: The O-H distances of the H-atoms attached to O are restrained in order to keep them at resonable ranges.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H6B      ..N3       .       2.69 Ang.
Author Response: This is structurally caused
PLAT480_ALERT_4_C Long H...A H-Bond Reported H5E      ..S4       .       2.93 Ang.
Author Response: This is structurally caused
PLAT480_ALERT_4_C Long H...A H-Bond Reported H9A      ..O3       .       2.63 Ang.
Author Response: This is structurally caused
PLAT480_ALERT_4_C Long H...A H-Bond Reported H8A      ..S3       .       2.90 Ang.
Author Response: This is structurally caused
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
Author Response: These reflections have low 2Th values and are affected by the beamstop, therefore they are eleiminated

Alert level G PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 14 Note PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension 3 Info PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 3 Report PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings Differ Please Check PLAT063_ALERT_4_G Crystal Size Likely too Large for Beam Size .... 0.65 mm PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 3 Report PLAT230_ALERT_2_G Hirshfeld Test Diff for S1 --C1 . 7.4 s.u. PLAT230_ALERT_2_G Hirshfeld Test Diff for S2 --C2 . 7.5 s.u. PLAT230_ALERT_2_G Hirshfeld Test Diff for S3 --C3 . 5.1 s.u. PLAT230_ALERT_2_G Hirshfeld Test Diff for S4 --C4 . 6.3 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Co1 --N3 . 6.0 s.u. PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.19 Ratio PLAT791_ALERT_4_G Model has Chirality at C5 (Chiral SPGR) S Verify PLAT791_ALERT_4_G Model has Chirality at C6 (Chiral SPGR) R Verify PLAT791_ALERT_4_G Model has Chirality at C7 (Chiral SPGR) R Verify PLAT791_ALERT_4_G Model has Chirality at C8 (Chiral SPGR) S Verify PLAT791_ALERT_4_G Model has Chirality at C9 (Chiral SPGR) R Verify PLAT794_ALERT_5_G Tentative Bond Valency for Co1 (II) . 1.73 Info PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 10 Note PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 2 Note PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 26 Note PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ... 9 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 2 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 2 ALERT level B = A potentially serious problem, consider carefully 6 ALERT level C = Check. Ensure it is not caused by an omission or oversight 23 ALERT level G = General information/check it is not something unexpected 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 13 ALERT type 4 Improvement, methodology, query or suggestion 3 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: DIAMOND (Crystal Impact, 2014); software used to prepare material for publication: ciftab2016 (Köckerling, 2016).

Poly[diaqua[µ-D-(+)-glucosammonium]tri-µ-thiocyanato-thiocyanatocobalt(II)potassium(I)] top
Crystal data top
[KCo(C6H14NO5)(NCS)4(H2O)2]Dx = 1.745 Mg m3
Mr = 546.56Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 9954 reflections
a = 9.3713 (2) Åθ = 2.6–36.0°
b = 14.1059 (3) ŵ = 1.47 mm1
c = 15.7347 (4) ÅT = 173 K
V = 2079.98 (8) Å3Block, blue
Z = 40.65 × 0.07 × 0.05 mm
F(000) = 1116
Data collection top
Bruker APEX-X8 CCD
diffractometer
7503 reflections with I > 2σ(I)
Radiation source: sealed tubeRint = 0.031
φ and ω scansθmax = 36.4°, θmin = 2.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2005)
h = 1415
k = 2313
24428 measured reflectionsl = 2616
9699 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.038H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.058 w = 1/[σ2(Fo2) + (0.0187P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.001
9699 reflectionsΔρmax = 0.59 e Å3
285 parametersΔρmin = 0.68 e Å3
10 restraintsAbsolute structure: Flack x determined using 2715 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.004 (5)
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
Co10.62109 (3)0.76616 (2)0.48158 (2)0.01938 (7)
N10.7606 (2)0.8376 (1)0.4133 (1)0.0268 (4)
C10.8322 (2)0.8742 (2)0.3636 (1)0.0191 (4)
S10.93387 (6)0.92611 (4)0.29276 (4)0.0223 (1)
N20.5171 (2)0.8625 (1)0.5476 (1)0.0232 (4)
C20.4283 (2)0.8943 (2)0.5915 (1)0.0189 (4)
S20.30724 (6)0.94110 (5)0.65107 (4)0.0305 (1)
N30.4981 (2)0.6893 (1)0.4099 (1)0.0274 (4)
C30.4293 (2)0.6383 (2)0.3688 (1)0.0200 (4)
S30.33187 (6)0.56658 (4)0.31185 (4)0.0257 (1)
N40.7071 (2)0.6805 (1)0.5650 (1)0.0250 (4)
C40.7734 (2)0.6367 (1)0.6135 (1)0.0185 (4)
S40.86663 (6)0.57317 (4)0.67975 (3)0.0233 (1)
K10.37801 (5)0.88532 (3)0.85226 (3)0.02172 (9)
O10.5999 (1)0.6576 (1)0.09269 (9)0.0165 (3)
O20.5319 (2)0.6440 (1)0.05053 (9)0.0199 (3)
H2A0.615 (1)0.635 (2)0.070 (2)0.06 (1)*
O30.1598 (1)0.6684 (1)0.0965 (1)0.0196 (3)
H3A0.150 (3)0.693 (2)0.1456 (7)0.049 (9)*
O40.3236 (2)0.8390 (1)0.12991 (9)0.0170 (3)
H4A0.324 (3)0.865 (2)0.1788 (7)0.039 (8)*
O50.7725 (1)0.8081 (1)0.14516 (9)0.0189 (3)
H5A0.819 (2)0.839 (2)0.182 (1)0.030 (7)*
N50.2920 (2)0.5419 (1)0.0135 (1)0.0168 (3)
H5B0.33220.48430.02420.025*
H5C0.29420.57770.06160.025*
H5D0.19990.53380.00330.025*
C50.5299 (2)0.6025 (2)0.0295 (1)0.0161 (4)
H5E0.57590.53860.02630.019*
C60.3738 (2)0.5909 (1)0.0554 (1)0.0141 (3)
H6A0.36840.55240.10860.017*
C70.3019 (2)0.6859 (1)0.0699 (1)0.0136 (4)
H7A0.29830.72020.01440.016*
C80.3854 (2)0.7460 (1)0.1321 (1)0.0126 (3)
H8A0.37680.71890.19060.015*
C90.5425 (2)0.7510 (1)0.1063 (1)0.0130 (4)
H9A0.55220.78920.05300.016*
C100.6299 (2)0.7957 (1)0.1758 (1)0.0169 (4)
H10A0.58860.85770.19190.020*
H10B0.63010.75430.22670.020*
O60.4544 (2)0.9728 (1)1.0028 (1)0.0300 (4)
H6B0.437 (3)1.0320 (4)1.001 (2)0.048 (9)*
H6C0.411 (3)0.948 (2)1.045 (1)0.10 (2)*
O70.5753 (2)0.7830 (1)0.7483 (1)0.0294 (4)
H7B0.635 (2)0.811 (1)0.716 (1)0.07 (1)*
H7C0.559 (3)0.7274 (8)0.730 (2)0.06 (1)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0206 (1)0.0181 (1)0.0194 (1)0.0007 (1)0.0012 (1)0.0005 (1)
N10.028 (1)0.027 (1)0.026 (1)0.0017 (9)0.0034 (8)0.0009 (9)
C10.0209 (9)0.017 (1)0.019 (1)0.0008 (8)0.0048 (8)0.0036 (8)
S10.0236 (2)0.0243 (3)0.0191 (2)0.0077 (2)0.0008 (2)0.0002 (2)
N20.0247 (9)0.022 (1)0.0229 (9)0.0007 (8)0.0002 (8)0.0010 (8)
C20.0215 (9)0.018 (1)0.018 (1)0.0027 (8)0.0057 (8)0.0033 (9)
S20.0288 (3)0.0370 (3)0.0257 (3)0.0123 (3)0.0029 (2)0.0007 (3)
N30.027 (1)0.023 (1)0.032 (1)0.0023 (8)0.0017 (9)0.0026 (9)
C30.0221 (9)0.018 (1)0.020 (1)0.0030 (8)0.0028 (8)0.0033 (9)
S30.0340 (3)0.0222 (3)0.0210 (3)0.0055 (2)0.0040 (2)0.0022 (2)
N40.0235 (9)0.026 (1)0.025 (1)0.0006 (8)0.0017 (8)0.0020 (8)
C40.0188 (9)0.017 (1)0.020 (1)0.0031 (8)0.0052 (8)0.0037 (8)
S40.0280 (3)0.0238 (3)0.0180 (2)0.0046 (2)0.0015 (2)0.0023 (2)
K10.0173 (2)0.0256 (2)0.0223 (2)0.0020 (2)0.0021 (2)0.0012 (2)
O10.0141 (6)0.0158 (7)0.0196 (7)0.0024 (5)0.0052 (5)0.0050 (6)
O20.0163 (7)0.0268 (9)0.0164 (7)0.0006 (6)0.0022 (6)0.0016 (6)
O30.0133 (6)0.0248 (8)0.0207 (8)0.0039 (6)0.0027 (6)0.0065 (7)
O40.0200 (7)0.0124 (7)0.0187 (7)0.0028 (6)0.0009 (6)0.0040 (6)
O50.0130 (6)0.0270 (8)0.0168 (7)0.0062 (6)0.0004 (6)0.0045 (6)
N50.0175 (7)0.0137 (8)0.0191 (8)0.0017 (6)0.0013 (7)0.0029 (7)
C50.0156 (8)0.0164 (9)0.016 (1)0.0025 (7)0.0039 (7)0.0040 (8)
C60.0175 (8)0.0123 (9)0.0125 (8)0.0011 (8)0.0028 (8)0.0001 (7)
C70.0111 (8)0.0145 (9)0.0153 (9)0.0009 (7)0.0007 (7)0.0011 (7)
C80.0138 (7)0.0113 (9)0.0126 (8)0.0002 (7)0.0008 (7)0.0002 (6)
C90.0145 (8)0.0111 (9)0.0134 (8)0.0003 (7)0.0011 (7)0.0012 (7)
C100.0137 (8)0.022 (1)0.0149 (9)0.0027 (8)0.0001 (8)0.0043 (8)
O60.0395 (9)0.0252 (9)0.025 (1)0.0058 (8)0.0028 (8)0.0036 (7)
O70.0303 (8)0.035 (1)0.0233 (8)0.0009 (8)0.0002 (7)0.0037 (8)
Geometric parameters (Å, º) top
Co1—N31.944 (2)O3—H3A0.850 (1)
Co1—N41.958 (2)O4—C81.434 (2)
Co1—N21.968 (2)O4—H4A0.850 (1)
Co1—N11.970 (2)O5—C101.432 (2)
N1—C11.153 (3)O5—K1iv2.902 (2)
C1—S11.638 (2)O5—H5A0.850 (1)
N2—C21.171 (3)N5—C61.497 (2)
C2—S21.613 (2)N5—H5B0.9100
N3—C31.163 (3)N5—H5C0.9100
C3—S31.630 (2)N5—H5D0.9100
N4—C41.162 (3)C5—C61.527 (3)
C4—S41.629 (2)C5—H5E1.0000
S1—K1i3.3256 (7)C6—C71.517 (3)
S2—K13.3287 (8)C6—H6A1.0000
S4—K1ii3.5399 (7)C7—C81.513 (2)
K1—O62.765 (2)C7—H7A1.0000
K1—O1iii2.812 (1)C8—C91.529 (2)
K1—O72.860 (2)C8—H8A1.0000
K1—O3iv2.864 (1)C9—C101.505 (3)
K1—O5iii2.902 (2)C9—H9A1.0000
K1—C10iii3.481 (2)C10—K1iv3.481 (2)
O1—C51.422 (2)C10—H10A0.9900
O1—C91.440 (2)C10—H10B0.9900
O1—K1iv2.812 (1)O6—H6B0.850 (1)
O2—C51.389 (2)O6—H6C0.850 (1)
O2—H2A0.850 (1)O7—H7B0.850 (1)
O3—C71.417 (2)O7—H7C0.850 (1)
O3—K1iii2.864 (1)
N3—Co1—N4106.83 (9)C7—O3—H3A108 (2)
N3—Co1—N2113.43 (8)K1iii—O3—H3A75 (2)
N4—Co1—N2106.02 (8)C8—O4—H4A111 (2)
N3—Co1—N1111.26 (9)C10—O5—K1iv101.4 (1)
N4—Co1—N1114.08 (8)C10—O5—H5A108 (2)
N2—Co1—N1105.25 (8)K1iv—O5—H5A108 (2)
C1—N1—Co1170.3 (2)C6—N5—H5B109.5
N1—C1—S1179.9 (2)C6—N5—H5C109.5
C1—S1—K1i118.29 (7)H5B—N5—H5C109.5
C2—N2—Co1158.1 (2)C6—N5—H5D109.5
N2—C2—S2178.4 (2)H5B—N5—H5D109.5
C2—S2—K1108.43 (8)H5C—N5—H5D109.5
C3—N3—Co1175.6 (2)O2—C5—O1113.4 (2)
N3—C3—S3179.5 (2)O2—C5—C6107.4 (2)
C4—N4—Co1171.4 (2)O1—C5—C6108.3 (2)
N4—C4—S4178.6 (2)O2—C5—H5E109.2
C4—S4—K1ii88.48 (7)O1—C5—H5E109.2
O6—K1—O1iii94.13 (5)C6—C5—H5E109.2
O6—K1—O7123.22 (5)N5—C6—C7106.8 (2)
O1iii—K1—O7131.81 (5)N5—C6—C5110.3 (2)
O6—K1—O3iv68.80 (5)C7—C6—C5111.8 (2)
O1iii—K1—O3iv135.31 (4)N5—C6—H6A109.3
O7—K1—O3iv55.32 (5)C7—C6—H6A109.3
O6—K1—O5iii119.72 (5)C5—C6—H6A109.3
O1iii—K1—O5iii58.51 (4)O3—C7—C8113.1 (2)
O7—K1—O5iii75.74 (5)O3—C7—C6108.0 (2)
O3iv—K1—O5iii93.51 (4)C8—C7—C6111.3 (2)
O6—K1—S1v75.35 (4)O3—C7—H7A108.1
O1iii—K1—S1v138.60 (3)C8—C7—H7A108.1
O7—K1—S1v84.26 (4)C6—C7—H7A108.1
O3iv—K1—S1v78.59 (3)O4—C8—C7106.8 (1)
O5iii—K1—S1v159.46 (3)O4—C8—C9109.9 (1)
O6—K1—S2139.53 (4)C7—C8—C9110.6 (1)
O1iii—K1—S299.16 (3)O4—C8—H8A109.9
O7—K1—S272.81 (4)C7—C8—H8A109.9
O3iv—K1—S2120.94 (3)C9—C8—H8A109.9
O5iii—K1—S299.65 (3)O1—C9—C10106.7 (2)
S1v—K1—S269.44 (2)O1—C9—C8110.9 (2)
O6—K1—C10iii127.51 (5)C10—C9—C8110.5 (2)
O1iii—K1—C10iii42.47 (4)O1—C9—H9A109.6
O7—K1—C10iii89.37 (5)C10—C9—H9A109.6
O3iv—K1—C10iii117.23 (5)C8—C9—H9A109.6
O5iii—K1—C10iii23.78 (4)O5—C10—C9108.3 (2)
S1v—K1—C10iii154.80 (4)O5—C10—K1iv54.79 (9)
S2—K1—C10iii85.38 (4)C9—C10—K1iv88.0 (1)
O6—K1—S4vi87.44 (4)O5—C10—H10A110.0
O1iii—K1—S4vi66.72 (3)C9—C10—H10A110.0
O7—K1—S4vi135.67 (4)K1iv—C10—H10A160.4
O3iv—K1—S4vi146.68 (3)O5—C10—H10B110.0
O5iii—K1—S4vi119.02 (3)C9—C10—H10B110.0
S1v—K1—S4vi72.82 (2)K1iv—C10—H10B70.7
S2—K1—S4vi63.81 (2)H10A—C10—H10B108.4
C10iii—K1—S4vi95.64 (3)K1—O6—H6B111 (2)
C5—O1—C9115.6 (1)K1—O6—H6C111 (2)
C5—O1—K1iv121.7 (1)H6B—O6—H6C109.5 (2)
C9—O1—K1iv119.9 (1)K1—O7—H7B122 (2)
C5—O2—H2A107 (2)K1—O7—H7C123 (2)
C7—O3—K1iii174.6 (1)H7B—O7—H7C109.5 (2)
C9—O1—C5—O259.7 (2)C6—C7—C8—C950.5 (2)
K1iv—O1—C5—O2101.0 (2)C5—O1—C9—C10179.1 (2)
C9—O1—C5—C659.5 (2)K1iv—O1—C9—C1019.9 (2)
K1iv—O1—C5—C6139.9 (1)C5—O1—C9—C858.7 (2)
O2—C5—C6—N551.3 (2)K1iv—O1—C9—C8140.2 (1)
O1—C5—C6—N5174.2 (2)O4—C8—C9—O1169.3 (1)
O2—C5—C6—C767.4 (2)C7—C8—C9—O151.7 (2)
O1—C5—C6—C755.5 (2)O4—C8—C9—C1072.6 (2)
N5—C6—C7—O361.3 (2)C7—C8—C9—C10169.8 (2)
C5—C6—C7—O3177.9 (1)K1iv—O5—C10—C973.8 (2)
N5—C6—C7—C8174.0 (2)O1—C9—C10—O565.5 (2)
C5—C6—C7—C853.2 (2)C8—C9—C10—O5173.8 (2)
O3—C7—C8—O468.2 (2)O1—C9—C10—K1iv13.8 (1)
C6—C7—C8—O4170.0 (2)C8—C9—C10—K1iv134.4 (1)
O3—C7—C8—C9172.3 (2)
Symmetry codes: (i) x+3/2, y+2, z1/2; (ii) x+1, y1/2, z+3/2; (iii) x1/2, y+3/2, z+1; (iv) x+1/2, y+3/2, z+1; (v) x+3/2, y+2, z+1/2; (vi) x+1, y+1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3A···O7iii0.85 (1)1.84 (1)2.657 (2)160 (3)
N5—H5C···O5vii0.912.092.967 (2)162
O6—H6C···O4viii0.85 (1)2.20 (1)3.010 (2)160 (2)
O2—H2A···O4ix0.85 (1)2.20 (1)3.015 (2)162 (3)
N5—H5B···N2x0.912.263.145 (2)166
N5—H5D···O6iii0.912.303.175 (2)160
O5—H5A···S10.85 (1)2.38 (1)3.233 (2)176 (2)
O4—H4A···S4iii0.85 (1)2.42 (1)3.266 (2)170 (3)
O7—H7C···S1iii0.85 (1)2.49 (1)3.298 (2)159 (2)
O7—H7B···S3iv0.85 (1)2.57 (1)3.344 (2)152 (2)
O6—H6B···N3vi0.85 (1)2.69 (2)3.378 (3)139 (2)
C7—H7A···O5vii1.002.553.397 (2)142
C5—H5E···S4xi1.002.933.560 (2)122
C9—H9A···O3ix1.002.633.560 (2)155
C8—H8A···S31.002.903.828 (2)154
Symmetry codes: (iii) x1/2, y+3/2, z+1; (iv) x+1/2, y+3/2, z+1; (vi) x+1, y+1/2, z+3/2; (vii) x1/2, y+3/2, z; (viii) x, y, z+1; (ix) x+1/2, y+3/2, z; (x) x+1, y1/2, z+1/2; (xi) x+3/2, y+1, z1/2.
 

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