Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The crystal structure of the title compound, (1,4,7,10,13,16-hexaoxacyclo­octadecane-κ6O)potassium chloro­chromate(VI), [K(C12H24O6)][CrClO3], contains a K+ cation, complexed with one crown ether molecule, and a chloro­chromate anion. The cation is located within the mean plane of the ether O atoms, approximately in the centre of the macrocyclic cavity, and bonded to them with K—O distances in the range 2.785 (5)–2.836 (5) Å. In the crystal structure, polymeric chains of the type K+–CrO{}_{3}^{\,- }–K+ are formed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805000085/cv6410sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805000085/cv6410Isup2.hkl
Contains datablock I

CCDC reference: 263549

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.014 Å
  • R factor = 0.082
  • wR factor = 0.253
  • Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT220_ALERT_2_A Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.32 Ratio PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O8 PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for Cr1
Alert level C RFACR01_ALERT_3_C The value of the weighted R factor is > 0.25 Weighted R factor given 0.253 PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 44 Perc. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293 PLAT213_ALERT_2_C Atom O9 has ADP max/min Ratio ............. 3.40 prolat PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for K1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O3 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 14 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C5 - C6 ... 1.43 Ang. PLAT731_ALERT_1_C Bond Calc 1.597(9), Rep 1.597(4) ...... 2.25 su-Rat CR1 -O7 1.555 1.555
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 25.05 From the CIF: _reflns_number_total 3416 From the CIF: _diffrn_reflns_limit_ max hkl 16. 18. 20. From the CIF: _diffrn_reflns_limit_ min hkl 0. 0. 0. TEST1: Expected hkl limits for theta max Calculated maximum hkl 18. 18. 20. Calculated minimum hkl -18. -18. -20.
3 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: P3 (Siemens, 1989); cell refinement: P3; data reduction: XDISK (Siemens, 1991); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: Please provide missing information.

(1,4,7,10,13,16-hexaoxacyclooctadecane-κ6O)potassium chlorochromate top
Crystal data top
[K(C12H24O6)][CrClO3]Dx = 1.463 Mg m3
Mr = 438.86Melting point: 440 (decomposed) K
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
a = 15.113 (2) ÅCell parameters from 24 reflections
b = 15.692 (2) Åθ = 12–14°
c = 16.806 (2) ŵ = 0.95 mm1
V = 3985.4 (9) Å3T = 293 K
Z = 8Plate, pale orange
F(000) = 18240.2 × 0.2 × 0.1 mm
Data collection top
Siemens P3/PC
diffractometer
θmax = 25.1°, θmin = 2.2°
θ/2θ scansh = 016
3465 measured reflectionsk = 018
3416 independent reflectionsl = 020
1518 reflections with I > 2σ(I)2 standard reflections every 98 reflections
Rint = 0.015 intensity decay: 2%
Refinement top
Refinement on F23 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.082 w = 1/[σ2(Fo2) + (0.153P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.253(Δ/σ)max < 0.001
S = 0.91Δρmax = 0.73 e Å3
3416 reflectionsΔρmin = 0.38 e Å3
217 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cr10.86843 (8)0.20047 (8)0.33981 (8)0.0700 (5)
K10.61765 (11)0.19053 (9)0.24546 (9)0.0623 (5)
Cl10.8563 (2)0.10005 (15)0.42629 (16)0.1270 (12)
O10.6754 (4)0.1758 (4)0.0875 (3)0.0780 (16)
O20.6688 (3)0.3374 (3)0.1646 (3)0.0685 (14)
O30.5646 (3)0.3480 (3)0.3075 (3)0.0598 (12)
O40.5498 (3)0.1994 (3)0.4010 (3)0.0598 (12)
O50.5731 (3)0.0392 (3)0.3261 (3)0.0587 (12)
O60.6735 (3)0.0303 (3)0.1855 (3)0.0708 (14)
O70.9409 (6)0.2664 (5)0.3714 (7)0.240 (7)
O80.7773 (4)0.2509 (6)0.3334 (6)0.186 (4)
O90.8903 (11)0.1577 (7)0.2554 (5)0.313 (10)
C10.7191 (6)0.2496 (8)0.0594 (5)0.103 (3)
H1A0.72640.24660.00210.123*
H1B0.77720.25420.08350.123*
C20.6636 (6)0.3250 (6)0.0813 (6)0.094 (3)
H2A0.68490.37530.05380.113*
H2B0.60270.31520.06570.113*
C30.6190 (6)0.4094 (6)0.1892 (8)0.104 (3)
H3A0.55910.40470.16890.125*
H3B0.64520.46070.16720.125*
C40.6167 (6)0.4158 (5)0.2773 (7)0.098 (3)
H4A0.67630.41220.29850.118*
H4B0.59140.470.29310.118*
C50.5595 (6)0.3468 (5)0.3915 (5)0.083 (3)
H5A0.5350.40020.41060.1*
H5B0.61820.34010.41390.1*
C60.5045 (6)0.2776 (5)0.4156 (5)0.084 (3)
H6A0.44940.27870.3860.101*
H6B0.49070.28260.47180.101*
C70.5012 (5)0.1250 (5)0.4188 (4)0.073 (2)
H7A0.45020.1210.38390.088*
H7B0.48020.12730.47330.088*
C80.5578 (6)0.0508 (5)0.4080 (4)0.078 (2)
H8A0.61360.05930.43550.093*
H8B0.52940.00060.43010.093*
C90.6331 (5)0.0281 (5)0.3088 (6)0.078 (2)
H9A0.61520.07930.33680.094*
H9B0.6920.01270.32670.094*
C100.6342 (5)0.0440 (5)0.2244 (6)0.077 (2)
H10A0.57440.05290.20510.092*
H10B0.66870.09460.21280.092*
C110.6685 (6)0.0250 (6)0.1025 (5)0.089 (3)
H11A0.60740.02850.08510.107*
H11B0.69310.02860.08420.107*
C120.7199 (6)0.0972 (7)0.0701 (5)0.097 (3)
H12A0.77850.09780.09370.116*
H12B0.72640.09080.0130.116*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.0728 (9)0.0671 (8)0.0699 (9)0.0048 (7)0.0084 (7)0.0034 (6)
K10.0902 (12)0.0465 (8)0.0501 (9)0.0006 (8)0.0122 (8)0.0027 (7)
Cl10.228 (4)0.0699 (14)0.0827 (17)0.0107 (17)0.026 (2)0.0125 (12)
O10.068 (3)0.112 (4)0.055 (3)0.011 (3)0.008 (3)0.005 (3)
O20.060 (3)0.066 (3)0.079 (4)0.010 (3)0.015 (3)0.020 (3)
O30.063 (3)0.043 (3)0.074 (3)0.001 (2)0.017 (3)0.005 (2)
O40.068 (3)0.058 (3)0.054 (3)0.001 (3)0.004 (2)0.003 (2)
O50.060 (3)0.047 (3)0.069 (3)0.001 (2)0.004 (2)0.001 (2)
O60.071 (3)0.067 (3)0.075 (4)0.003 (3)0.001 (3)0.019 (3)
O70.217 (9)0.143 (7)0.359 (15)0.100 (7)0.174 (10)0.143 (9)
O80.110 (6)0.238 (10)0.211 (11)0.049 (7)0.013 (6)0.101 (9)
O90.65 (3)0.173 (10)0.113 (8)0.021 (12)0.172 (13)0.001 (7)
C10.072 (6)0.183 (11)0.053 (5)0.044 (7)0.002 (4)0.016 (6)
C20.090 (7)0.112 (7)0.081 (7)0.038 (6)0.025 (5)0.046 (6)
C30.089 (7)0.080 (7)0.144 (10)0.022 (5)0.003 (7)0.047 (7)
C40.095 (7)0.041 (4)0.158 (11)0.003 (4)0.005 (7)0.004 (5)
C50.109 (7)0.056 (5)0.085 (7)0.027 (5)0.021 (6)0.024 (5)
C60.098 (6)0.098 (6)0.057 (5)0.049 (6)0.007 (5)0.007 (5)
C70.068 (5)0.108 (6)0.044 (4)0.005 (5)0.007 (4)0.000 (4)
C80.110 (7)0.068 (5)0.055 (5)0.028 (5)0.004 (5)0.013 (4)
C90.073 (5)0.049 (4)0.113 (7)0.002 (4)0.005 (5)0.009 (5)
C100.072 (5)0.045 (4)0.113 (7)0.002 (4)0.000 (5)0.023 (4)
C110.089 (6)0.104 (7)0.075 (6)0.020 (6)0.007 (5)0.029 (6)
C120.084 (7)0.152 (9)0.055 (5)0.046 (7)0.001 (5)0.020 (6)
Geometric parameters (Å, º) top
Cr1—O81.592 (4)C2—H2A0.97
Cr1—O71.597 (4)C2—H2B0.97
Cr1—O91.604 (5)C3—C41.485 (14)
Cr1—Cl12.151 (3)C3—H3A0.97
K1—O12.804 (5)C3—H3B0.97
K1—O22.785 (5)C4—H4A0.97
K1—O32.800 (5)C4—H4B0.97
K1—O42.811 (5)C5—C61.427 (11)
K1—O52.815 (4)C5—H5A0.97
K1—O62.836 (5)C5—H5B0.97
K1—O82.983 (10)C6—H6A0.97
K1—O7i3.522 (14)C6—H6B0.97
K1—O9i3.474 (16)C7—C81.456 (10)
O1—C11.414 (10)C7—H7A0.97
O1—C121.435 (9)C7—H7B0.97
O2—C21.416 (11)C8—H8A0.97
O2—C31.418 (11)C8—H8B0.97
O3—C51.414 (9)C9—C101.440 (11)
O3—C41.417 (9)C9—H9A0.97
O4—C71.411 (8)C9—H9B0.97
O4—C61.427 (7)C10—H10A0.97
O5—C81.408 (8)C10—H10B0.97
O5—C91.423 (8)C11—C121.477 (12)
O6—C111.400 (9)C11—H11A0.97
O6—C101.462 (9)C11—H11B0.97
C1—C21.497 (13)C12—H12A0.97
C1—H1A0.97C12—H12B0.97
C1—H1B0.97
O8—Cr1—O7107.1 (6)O2—C2—C1108.8 (7)
O8—Cr1—O9109.1 (7)O2—C2—H2A109.9
O7—Cr1—O9115.0 (7)C1—C2—H2A109.9
O8—Cr1—Cl1109.6 (3)O2—C2—H2B109.9
O7—Cr1—Cl1107.9 (3)C1—C2—H2B109.9
O9—Cr1—Cl1108.0 (4)H2A—C2—H2B108.3
O2—K1—O361.99 (17)O2—C3—C4110.9 (8)
O2—K1—O161.31 (17)O2—C3—H3A109.5
O3—K1—O1120.95 (17)C4—C3—H3A109.5
O2—K1—O4120.93 (16)O2—C3—H3B109.5
O3—K1—O460.39 (14)C4—C3—H3B109.5
O1—K1—O4176.27 (16)H3A—C3—H3B108.1
O2—K1—O5177.62 (15)O3—C4—C3108.6 (7)
O3—K1—O5119.79 (15)O3—C4—H4A110
O1—K1—O5117.43 (16)C3—C4—H4A110
O4—K1—O560.45 (13)O3—C4—H4B110
O2—K1—O6118.54 (18)C3—C4—H4B110
O3—K1—O6178.82 (16)H4A—C4—H4B108.3
O1—K1—O659.89 (17)O3—C5—C6109.0 (7)
O4—K1—O6118.83 (15)O3—C5—H5A109.9
O5—K1—O659.64 (15)C6—C5—H5A109.9
O2—K1—O875.80 (19)O3—C5—H5B109.9
O3—K1—O876.54 (19)C6—C5—H5B109.9
O1—K1—O8104.1 (2)H5A—C5—H5B108.3
O4—K1—O879.55 (19)C5—C6—O4109.0 (7)
O5—K1—O8102.88 (19)C5—C6—H6A109.9
O6—K1—O8102.51 (19)O4—C6—H6A109.9
O2—K1—O9i113.27 (17)C5—C6—H6B109.9
O3—K1—O9i81.3 (2)O4—C6—H6B109.9
O1—K1—O9i106.94 (19)H6A—C6—H6B108.3
O4—K1—O9i69.56 (17)O4—C7—C8109.2 (6)
O5—K1—O9i68.91 (16)O4—C7—H7A109.8
O6—K1—O9i99.3 (2)C8—C7—H7A109.8
O8—K1—O9i148.1 (2)O4—C7—H7B109.8
O2—K1—O7i70.04 (13)C8—C7—H7B109.8
O3—K1—O7i72.05 (16)H7A—C7—H7B108.3
O1—K1—O7i74.69 (17)O5—C8—C7108.7 (6)
O4—K1—O7i103.02 (16)O5—C8—H8A110
O5—K1—O7i111.82 (13)C7—C8—H8A110
O6—K1—O7i109.09 (17)O5—C8—H8B110
O8—K1—O7i141.5 (2)C7—C8—H8B110
O9i—K1—O7i45.40 (13)H8A—C8—H8B108.3
C1—O1—C12114.6 (8)O5—C9—C10109.6 (7)
C1—O1—K1113.2 (5)O5—C9—H9A109.7
C12—O1—K1114.1 (5)C10—C9—H9A109.7
C2—O2—C3111.6 (8)O5—C9—H9B109.7
C2—O2—K1110.7 (5)C10—C9—H9B109.7
C3—O2—K1111.7 (5)H9A—C9—H9B108.2
C5—O3—C4113.4 (7)C9—C10—O6107.8 (6)
C5—O3—K1112.0 (4)C9—C10—H10A110.1
C4—O3—K1111.7 (5)O6—C10—H10A110.1
C7—O4—C6115.1 (6)C9—C10—H10B110.1
C7—O4—K1110.2 (4)O6—C10—H10B110.1
C6—O4—K1112.2 (4)H10A—C10—H10B108.5
C8—O5—C9113.5 (6)O6—C11—C12107.1 (7)
C8—O5—K1113.7 (4)O6—C11—H11A110.3
C9—O5—K1112.0 (4)C12—C11—H11A110.3
C11—O6—C10112.1 (6)O6—C11—H11B110.3
C11—O6—K1113.0 (5)C12—C11—H11B110.3
C10—O6—K1115.3 (4)H11A—C11—H11B108.6
Cr1—O8—K1125.2 (6)O1—C12—C11109.7 (7)
O1—C1—C2107.6 (7)O1—C12—H12A109.7
O1—C1—H1A110.2C11—C12—H12A109.7
C2—C1—H1A110.2O1—C12—H12B109.7
O1—C1—H1B110.2C11—C12—H12B109.7
C2—C1—H1B110.2H12A—C12—H12B108.2
H1A—C1—H1B108.5
O2—K1—O1—C114.4 (5)O3—K1—O5—C9154.8 (5)
O3—K1—O1—C132.2 (6)O1—K1—O5—C940.5 (5)
O5—K1—O1—C1163.3 (5)O4—K1—O5—C9143.0 (5)
O6—K1—O1—C1146.8 (6)O6—K1—O5—C924.0 (5)
O8—K1—O1—C150.4 (6)O8—K1—O5—C973.1 (5)
O9i—K1—O1—C1122.1 (6)O9i—K1—O5—C9139.2 (5)
O7i—K1—O1—C189.7 (6)O7i—K1—O5—C9124.0 (5)
O2—K1—O1—C12148.0 (6)O2—K1—O6—C1141.1 (6)
O3—K1—O1—C12165.7 (5)O1—K1—O6—C1122.4 (5)
O5—K1—O1—C1229.8 (6)O4—K1—O6—C11153.6 (5)
O6—K1—O1—C1213.3 (5)O5—K1—O6—C11140.6 (6)
O8—K1—O1—C1283.1 (6)O8—K1—O6—C11121.6 (6)
O9i—K1—O1—C12104.3 (6)O9i—K1—O6—C1181.9 (5)
O7i—K1—O1—C12136.7 (5)O7i—K1—O6—C1136.0 (5)
O3—K1—O2—C2140.8 (6)O2—K1—O6—C10171.8 (4)
O1—K1—O2—C222.0 (5)O1—K1—O6—C10153.1 (5)
O4—K1—O2—C2154.6 (5)O4—K1—O6—C1022.8 (5)
O6—K1—O2—C240.4 (6)O5—K1—O6—C109.9 (4)
O8—K1—O2—C2137.1 (6)O8—K1—O6—C10107.7 (5)
O9i—K1—O2—C275.3 (6)O9i—K1—O6—C1048.9 (5)
O7i—K1—O2—C261.0 (6)O7i—K1—O6—C1094.7 (5)
O3—K1—O2—C315.7 (6)O7—Cr1—O8—K1165.1 (5)
O1—K1—O2—C3147.0 (6)O9—Cr1—O8—K140.0 (7)
O4—K1—O2—C329.5 (6)Cl1—Cr1—O8—K178.0 (5)
O6—K1—O2—C3165.5 (6)O2—K1—O8—Cr1115.8 (5)
O8—K1—O2—C397.8 (6)O3—K1—O8—Cr1179.9 (5)
O9i—K1—O2—C349.8 (6)O1—K1—O8—Cr160.9 (5)
O7i—K1—O2—C364.0 (6)O4—K1—O8—Cr1118.3 (5)
O2—K1—O3—C5147.4 (5)O5—K1—O8—Cr162.1 (5)
O1—K1—O3—C5165.1 (5)O6—K1—O8—Cr10.8 (5)
O4—K1—O3—C519.0 (5)O9i—K1—O8—Cr1132.8 (5)
O5—K1—O3—C530.8 (5)O7i—K1—O8—Cr1143.9 (4)
O8—K1—O3—C566.5 (5)C12—O1—C1—C2179.2 (7)
O9i—K1—O3—C590.3 (5)K1—O1—C1—C247.5 (8)
O7i—K1—O3—C5136.1 (5)C3—O2—C2—C1178.7 (7)
O2—K1—O3—C418.9 (5)K1—O2—C2—C156.2 (8)
O1—K1—O3—C436.6 (6)C2—O2—C3—C4173.6 (7)
O4—K1—O3—C4147.5 (6)K1—O2—C3—C449.0 (8)
O5—K1—O3—C4159.3 (5)C5—O3—C4—C3178.7 (7)
O8—K1—O3—C462.0 (6)K1—O3—C4—C350.9 (8)
O9i—K1—O3—C4141.2 (6)C4—O3—C5—C6178.9 (6)
O7i—K1—O3—C495.4 (6)K1—O3—C5—C653.5 (7)
O2—K1—O4—C7159.6 (4)C7—O4—C6—C5177.2 (6)
O3—K1—O4—C7145.6 (5)K1—O4—C6—C550.0 (7)
O5—K1—O4—C722.6 (4)C6—O4—C7—C8174.9 (6)
O6—K1—O4—C735.4 (5)K1—O4—C7—C857.0 (6)
O8—K1—O4—C7134.0 (5)C9—O5—C8—C7175.7 (6)
O9i—K1—O4—C754.1 (4)K1—O5—C8—C746.0 (7)
O7i—K1—O4—C785.3 (4)C8—O5—C9—C10171.1 (6)
O2—K1—O4—C629.9 (5)K1—O5—C9—C1058.4 (7)
O3—K1—O4—C615.9 (5)C11—O6—C10—C9173.4 (7)
O5—K1—O4—C6152.3 (5)K1—O6—C10—C942.3 (7)
O6—K1—O4—C6165.1 (5)C10—O6—C11—C12172.9 (6)
O8—K1—O4—C696.2 (5)K1—O6—C11—C1254.8 (8)
O9i—K1—O4—C675.7 (5)C1—O1—C12—C11179.8 (7)
O7i—K1—O4—C644.4 (5)K1—O1—C12—C1146.9 (8)
O3—K1—O5—C824.4 (5)O1—C1—C2—O271.3 (8)
O1—K1—O5—C8170.9 (5)O2—C3—C4—O369.4 (9)
O4—K1—O5—C812.6 (5)O3—C5—C6—O470.9 (8)
O6—K1—O5—C8154.4 (5)O4—C7—C8—O571.0 (7)
O8—K1—O5—C857.3 (5)O5—C9—C10—O667.4 (8)
O9i—K1—O5—C890.4 (5)O6—C11—C12—O168.7 (9)
O7i—K1—O5—C8105.6 (5)
Symmetry code: (i) x1/2, y, z+1/2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds