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The title compound, trans-K[Cr(C3H2O4)2(H2O)2]·3H2O, comprises an octahedral coordinated Cr atom, bonded to two malonato ions and two water mol­ecules and a K ion surrounded by nine O atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802013077/ob6153sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802013077/ob6153Isup2.hkl
Contains datablock I

CCDC reference: 193719

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.025
  • wR factor = 0.066
  • Data-to-parameter ratio = 16.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
DIFF_019 Alert A _diffrn_standards_number is missing Number of standards used in measurement.
Author response: The data have been collected on an area detector.
DIFF_020  Alert A _diffrn_standards_interval_count and
          _diffrn_standards_interval_time are missing. Number of measurements
          between standards or time (min) between standards.
Author response: The data have been collected on an area detector.
DIFF_022  Alert A _diffrn_standards_decay_% is missing
          Percentage decrease in standards intensity.
Author response: The data have been collected on an area detector.

3 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991).

; top
Crystal data top
K[Cr(C3H2O4)2(H2O)2](H2O)3F(000) = 788
Mr = 385.27Dx = 1.893 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 7.0279 (5) ÅCell parameters from 34274 reflections
b = 11.6943 (5) Åθ = 3.7–29.7°
c = 16.5623 (12) ŵ = 1.22 mm1
β = 96.791 (6)°T = 173 K
V = 1351.65 (15) Å3Block, purple
Z = 40.48 × 0.24 × 0.22 mm
Data collection top
STOE IPDS-II two-circle
diffractometer
3803 independent reflections
Radiation source: fine-focus sealed tube3536 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
ω scansθmax = 29.7°, θmin = 3.7°
Absorption correction: empirical
(MULABS; Spek, 1990; Blessing, 1995)
h = 99
Tmin = 0.583, Tmax = 0.764k = 1616
25347 measured reflectionsl = 2323
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.066H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0389P)2 + 0.4185P]
where P = (Fo2 + 2Fc2)/3
3803 reflections(Δ/σ)max = 0.002
230 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = 0.70 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cr10.55435 (2)0.600339 (14)0.695396 (9)0.01232 (6)
K10.55847 (4)0.82573 (2)0.508217 (16)0.02319 (7)
C10.38760 (15)0.81433 (9)0.74146 (6)0.01553 (19)
O110.47968 (12)0.76079 (7)0.69157 (5)0.01695 (15)
O120.37073 (14)0.92032 (8)0.73864 (5)0.02202 (17)
C20.28967 (16)0.74680 (10)0.80326 (7)0.0199 (2)
H2A0.25460.80110.84490.024*
H2B0.16870.71560.77510.024*
C30.39948 (15)0.64855 (9)0.84715 (6)0.01531 (18)
O310.51224 (11)0.58641 (7)0.80933 (5)0.01588 (15)
O320.37107 (13)0.62856 (8)0.91810 (5)0.02247 (17)
C40.70021 (16)0.38346 (10)0.63991 (7)0.01712 (19)
O410.62969 (12)0.43866 (7)0.69623 (5)0.01791 (16)
O420.70211 (15)0.27760 (8)0.63612 (6)0.02580 (19)
C50.79681 (19)0.44910 (11)0.57674 (8)0.0255 (2)
H5A0.92480.47340.60240.031*
H5B0.81730.39550.53230.031*
C60.69501 (15)0.55337 (9)0.53898 (6)0.01591 (19)
O610.59623 (12)0.61571 (7)0.58211 (5)0.01722 (15)
O620.71157 (14)0.57934 (8)0.46767 (5)0.02444 (18)
O10.28364 (11)0.55248 (7)0.66045 (5)0.01683 (15)
H1A0.242 (3)0.5098 (17)0.6925 (13)0.033 (5)*
H1B0.281 (3)0.5181 (17)0.6168 (13)0.031 (5)*
O20.82200 (11)0.65416 (8)0.73047 (5)0.01799 (15)
H2C0.826 (3)0.6913 (17)0.7748 (13)0.032 (5)*
H2D0.859 (3)0.7002 (18)0.6972 (13)0.036 (5)*
O30.92215 (17)0.82155 (9)0.63799 (7)0.0327 (2)
H3A1.022 (4)0.830 (2)0.6117 (15)0.053 (6)*
H3B0.921 (4)0.879 (2)0.6706 (17)0.059 (7)*
O40.18756 (14)0.89028 (10)0.53672 (7)0.0286 (2)
H4A0.102 (3)0.8916 (19)0.4946 (15)0.043 (6)*
H4B0.187 (3)0.957 (2)0.5484 (15)0.046 (6)*
O50.57363 (16)1.01361 (9)0.61085 (6)0.02728 (19)
H5C0.675 (4)1.037 (2)0.6317 (17)0.063 (8)*
H5D0.520 (3)0.9918 (19)0.6528 (14)0.043 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.01460 (9)0.01117 (9)0.01154 (9)0.00019 (5)0.00298 (6)0.00077 (5)
K10.02673 (13)0.01761 (13)0.02617 (13)0.00148 (9)0.00701 (9)0.00350 (9)
C10.0157 (4)0.0157 (5)0.0150 (4)0.0010 (3)0.0013 (3)0.0005 (3)
O110.0210 (4)0.0134 (4)0.0173 (3)0.0019 (3)0.0058 (3)0.0009 (3)
O120.0295 (4)0.0151 (4)0.0229 (4)0.0035 (3)0.0096 (3)0.0005 (3)
C20.0194 (5)0.0200 (5)0.0217 (5)0.0037 (4)0.0079 (4)0.0050 (4)
C30.0150 (4)0.0163 (5)0.0147 (4)0.0020 (4)0.0020 (3)0.0006 (3)
O310.0183 (4)0.0165 (4)0.0133 (3)0.0016 (3)0.0039 (3)0.0014 (3)
O320.0255 (4)0.0280 (4)0.0149 (4)0.0029 (3)0.0062 (3)0.0028 (3)
C40.0183 (5)0.0162 (5)0.0167 (5)0.0038 (4)0.0011 (4)0.0019 (4)
O410.0238 (4)0.0135 (4)0.0172 (3)0.0034 (3)0.0053 (3)0.0018 (3)
O420.0395 (5)0.0158 (4)0.0227 (4)0.0066 (4)0.0061 (4)0.0004 (3)
C50.0266 (6)0.0247 (6)0.0276 (6)0.0092 (5)0.0132 (4)0.0073 (5)
C60.0168 (4)0.0158 (5)0.0153 (4)0.0033 (4)0.0023 (3)0.0012 (4)
O610.0225 (4)0.0163 (4)0.0134 (3)0.0012 (3)0.0046 (3)0.0014 (3)
O620.0362 (5)0.0230 (4)0.0153 (4)0.0008 (4)0.0079 (3)0.0003 (3)
O10.0173 (3)0.0184 (4)0.0151 (3)0.0034 (3)0.0030 (3)0.0000 (3)
O20.0162 (3)0.0209 (4)0.0170 (4)0.0023 (3)0.0025 (3)0.0002 (3)
O30.0386 (5)0.0284 (5)0.0336 (5)0.0069 (4)0.0142 (4)0.0012 (4)
O40.0241 (4)0.0327 (6)0.0285 (5)0.0022 (4)0.0007 (4)0.0037 (4)
O50.0350 (5)0.0259 (5)0.0206 (4)0.0065 (4)0.0020 (4)0.0012 (3)
Geometric parameters (Å, º) top
Cr1—O611.9417 (8)C3—O321.2373 (13)
Cr1—O111.9474 (8)C3—O311.2906 (13)
Cr1—O311.9512 (8)O32—K1iv2.8488 (9)
Cr1—O411.9630 (8)C4—O421.2396 (15)
Cr1—O12.0018 (8)C4—O411.2813 (13)
Cr1—O22.0034 (8)C4—C51.5208 (16)
K1—O612.7428 (9)O42—K1iii3.0811 (10)
K1—O52.7723 (10)C5—C61.5112 (16)
K1—O5i2.8014 (10)C5—H5A0.9900
K1—O42.8069 (11)C5—H5B0.9900
K1—O32ii2.8488 (9)C6—O621.2383 (14)
K1—O42iii3.0811 (11)C6—O611.2810 (13)
K1—O33.1394 (13)O1—H1A0.81 (2)
K1—O623.1752 (10)O1—H1B0.83 (2)
K1—O113.2408 (9)O2—H2C0.85 (2)
K1—C63.3480 (12)O2—H2D0.83 (2)
K1—K1i4.1606 (5)O3—H3A0.87 (3)
C1—O121.2455 (14)O3—H3B0.87 (3)
C1—O111.2727 (13)O4—H4A0.86 (2)
C1—C21.5205 (15)O4—H4B0.80 (3)
C2—C31.5203 (15)O5—K1i2.8014 (10)
C2—H2A0.9900O5—H5C0.80 (3)
C2—H2B0.9900O5—H5D0.87 (2)
O61—Cr1—O1187.16 (3)O4—K1—K1i64.36 (2)
O61—Cr1—O31179.48 (3)O32ii—K1—K1i86.59 (2)
O11—Cr1—O3192.34 (3)O42iii—K1—K1i103.81 (2)
O61—Cr1—O4191.40 (3)O3—K1—K1i101.45 (2)
O11—Cr1—O41178.53 (3)O62—K1—K1i160.809 (19)
O31—Cr1—O4189.11 (3)O11—K1—K1i103.682 (17)
O61—Cr1—O189.65 (4)C6—K1—K1i173.11 (2)
O11—Cr1—O190.96 (4)O12—C1—O11121.24 (10)
O31—Cr1—O190.50 (3)O12—C1—C2119.57 (10)
O41—Cr1—O188.80 (4)O11—C1—C2119.14 (10)
O61—Cr1—O290.38 (4)C1—O11—Cr1127.49 (7)
O11—Cr1—O286.96 (4)C1—O11—K1130.50 (7)
O31—Cr1—O289.45 (3)Cr1—O11—K1100.43 (3)
O41—Cr1—O293.29 (4)C3—C2—C1118.02 (9)
O1—Cr1—O2177.91 (4)C3—C2—H2A107.8
O61—K1—O5116.19 (3)C1—C2—H2A107.8
O61—K1—O5i157.09 (3)C3—C2—H2B107.8
O5—K1—O5i83.43 (3)C1—C2—H2B107.8
O61—K1—O4102.04 (3)H2A—C2—H2B107.1
O5—K1—O469.69 (3)O32—C3—O31122.13 (10)
O5i—K1—O472.60 (3)O32—C3—C2117.84 (10)
O61—K1—O32ii111.22 (3)O31—C3—C2119.98 (9)
O5—K1—O32ii101.33 (3)C3—O31—Cr1126.47 (7)
O5i—K1—O32ii73.57 (3)C3—O32—K1iv133.10 (8)
O4—K1—O32ii145.76 (3)O42—C4—O41123.19 (11)
O61—K1—O42iii90.70 (3)O42—C4—C5117.44 (10)
O5—K1—O42iii139.71 (3)O41—C4—C5119.28 (10)
O5i—K1—O42iii66.41 (3)C4—O41—Cr1127.41 (7)
O4—K1—O42iii75.96 (3)C4—O42—K1iii114.96 (7)
O32ii—K1—O42iii95.25 (3)C6—C5—C4117.64 (10)
O61—K1—O369.67 (3)C6—C5—H5A107.9
O5—K1—O367.88 (3)C4—C5—H5A107.9
O5i—K1—O3131.88 (3)C6—C5—H5B107.9
O4—K1—O3125.88 (3)C4—C5—H5B107.9
O32ii—K1—O375.27 (3)H5A—C5—H5B107.2
O42iii—K1—O3152.40 (3)O62—C6—O61120.70 (11)
O61—K1—O6242.65 (2)O62—C6—C5119.95 (10)
O5—K1—O62149.26 (3)O61—C6—C5119.33 (10)
O5i—K1—O62123.51 (3)O62—C6—K171.28 (7)
O4—K1—O62128.63 (3)O61—C6—K151.60 (5)
O32ii—K1—O6275.99 (3)C5—C6—K1160.68 (8)
O42iii—K1—O6270.44 (2)C6—O61—Cr1129.80 (7)
O3—K1—O6282.06 (3)C6—O61—K1106.92 (7)
O61—K1—O1152.44 (2)Cr1—O61—K1119.76 (4)
O5—K1—O1167.02 (3)C6—O62—K187.04 (7)
O5i—K1—O11137.53 (3)Cr1—O1—H1A113.0 (14)
O4—K1—O1168.93 (3)Cr1—O1—H1B108.0 (13)
O32ii—K1—O11139.71 (3)H1A—O1—H1B108 (2)
O42iii—K1—O11118.91 (3)Cr1—O2—H2C110.3 (13)
O3—K1—O1164.55 (3)Cr1—O2—H2D111.6 (14)
O62—K1—O1194.89 (2)H2C—O2—H2D105.0 (19)
O61—K1—C621.47 (2)K1—O3—H3A107.0 (16)
O5—K1—C6132.15 (3)K1—O3—H3B110.2 (18)
O5i—K1—C6144.13 (3)H3A—O3—H3B107 (2)
O4—K1—C6119.04 (3)K1—O4—H4A116.0 (15)
O32ii—K1—C691.91 (3)K1—O4—H4B109.2 (17)
O42iii—K1—C683.01 (3)H4A—O4—H4B99 (2)
O3—K1—C671.67 (3)K1—O5—K1i96.57 (3)
O62—K1—C621.68 (2)K1—O5—H5C120 (2)
O11—K1—C673.27 (2)K1i—O5—H5C106 (2)
O61—K1—K1i156.11 (2)K1—O5—H5D105.6 (15)
O5—K1—K1i41.98 (2)K1i—O5—H5D128.5 (15)
O5i—K1—K1i41.45 (2)H5C—O5—H5D102 (2)
O12—C1—O11—Cr1170.22 (8)O4—K1—C6—O6140.55 (8)
C2—C1—O11—Cr112.35 (14)O32ii—K1—C6—O61154.74 (7)
O12—C1—O11—K127.05 (15)O42iii—K1—C6—O61110.20 (7)
C2—C1—O11—K1150.38 (8)O3—K1—C6—O6180.94 (7)
O61—Cr1—O11—C1163.23 (9)O62—K1—C6—O61162.98 (11)
O31—Cr1—O11—C116.91 (9)O11—K1—C6—O6112.85 (6)
O1—Cr1—O11—C173.62 (9)O61—K1—C6—C568.2 (2)
O2—Cr1—O11—C1106.24 (9)O5—K1—C6—C520.6 (2)
O61—Cr1—O11—K13.51 (3)O5i—K1—C6—C5150.6 (2)
O31—Cr1—O11—K1176.35 (3)O4—K1—C6—C5108.7 (2)
O1—Cr1—O11—K193.11 (3)O32ii—K1—C6—C586.5 (2)
O2—Cr1—O11—K187.03 (3)O42iii—K1—C6—C5178.4 (2)
O61—K1—O11—C1163.02 (10)O3—K1—C6—C512.7 (2)
O5—K1—O11—C138.39 (9)O62—K1—C6—C5128.8 (2)
O5i—K1—O11—C111.27 (11)O11—K1—C6—C555.3 (2)
O4—K1—O11—C137.68 (9)O62—C6—O61—Cr1177.06 (8)
O32ii—K1—O11—C1118.59 (9)C5—C6—O61—Cr11.11 (15)
O42iii—K1—O11—C197.03 (9)K1—C6—O61—Cr1158.26 (11)
O3—K1—O11—C1113.84 (9)O62—C6—O61—K118.81 (12)
O62—K1—O11—C1167.36 (9)C5—C6—O61—K1159.37 (9)
C6—K1—O11—C1168.91 (9)O11—Cr1—O61—C6160.60 (10)
K1i—K1—O11—C117.50 (9)O41—Cr1—O61—C619.63 (10)
O61—K1—O11—Cr13.13 (3)O1—Cr1—O61—C6108.42 (10)
O5—K1—O11—Cr1155.47 (4)O2—Cr1—O61—C673.67 (10)
O5i—K1—O11—Cr1154.87 (4)O11—Cr1—O61—K14.70 (4)
O4—K1—O11—Cr1128.46 (4)O41—Cr1—O61—K1175.53 (4)
O32ii—K1—O11—Cr175.27 (5)O1—Cr1—O61—K195.67 (4)
O42iii—K1—O11—Cr169.11 (4)O2—Cr1—O61—K182.24 (4)
O3—K1—O11—Cr180.02 (4)O5—K1—O61—C6142.43 (7)
O62—K1—O11—Cr11.22 (3)O5i—K1—O61—C670.78 (11)
C6—K1—O11—Cr12.77 (3)O4—K1—O61—C6144.47 (7)
K1i—K1—O11—Cr1176.36 (3)O32ii—K1—O61—C627.23 (7)
O12—C1—C2—C3138.93 (11)O42iii—K1—O61—C668.68 (7)
O11—C1—C2—C343.59 (15)O3—K1—O61—C691.46 (7)
C1—C2—C3—O32147.03 (11)O62—K1—O61—C69.18 (6)
C1—C2—C3—O3135.60 (16)O11—K1—O61—C6164.42 (8)
O32—C3—O31—Cr1174.74 (8)K1i—K1—O61—C6163.19 (6)
C2—C3—O31—Cr12.52 (14)O5—K1—O61—Cr118.44 (6)
O11—Cr1—O31—C324.78 (9)O5i—K1—O61—Cr1128.36 (7)
O41—Cr1—O31—C3155.00 (9)O4—K1—O61—Cr154.67 (5)
O1—Cr1—O31—C366.20 (9)O32ii—K1—O61—Cr1133.64 (4)
O2—Cr1—O31—C3111.71 (9)O42iii—K1—O61—Cr1130.46 (4)
O31—C3—O32—K1iv153.28 (8)O3—K1—O61—Cr169.40 (4)
C2—C3—O32—K1iv24.03 (16)O62—K1—O61—Cr1170.04 (6)
O42—C4—O41—Cr1162.33 (9)O11—K1—O61—Cr13.55 (3)
C5—C4—O41—Cr121.19 (15)C6—K1—O61—Cr1160.86 (10)
O61—Cr1—O41—C47.43 (10)K1i—K1—O61—Cr12.32 (9)
O31—Cr1—O41—C4172.43 (10)O61—C6—O62—K115.47 (10)
O1—Cr1—O41—C497.06 (10)C5—C6—O62—K1162.69 (10)
O2—Cr1—O41—C483.03 (10)O61—K1—O62—C69.10 (6)
O41—C4—O42—K1iii112.13 (10)O5—K1—O62—C647.48 (10)
C5—C4—O42—K1iii71.33 (12)O5i—K1—O62—C6164.85 (7)
O42—C4—C5—C6137.36 (12)O4—K1—O62—C670.83 (8)
O41—C4—C5—C645.96 (17)O32ii—K1—O62—C6136.13 (7)
C4—C5—C6—O62147.63 (12)O42iii—K1—O62—C6122.99 (7)
C4—C5—C6—O6134.18 (17)O3—K1—O62—C659.42 (7)
C4—C5—C6—K190.8 (2)O11—K1—O62—C64.01 (7)
O61—K1—C6—O62162.98 (11)K1i—K1—O62—C6161.49 (6)
O5—K1—C6—O62149.45 (7)O61—K1—O5—K1i167.61 (3)
O5i—K1—C6—O6221.83 (9)O5i—K1—O5—K1i0.0
O4—K1—C6—O62122.44 (7)O4—K1—O5—K1i73.84 (4)
O32ii—K1—C6—O6242.28 (7)O32ii—K1—O5—K1i71.74 (3)
O42iii—K1—C6—O6252.78 (7)O42iii—K1—O5—K1i40.64 (6)
O3—K1—C6—O62116.08 (7)O3—K1—O5—K1i140.55 (4)
O11—K1—C6—O62175.83 (7)O62—K1—O5—K1i153.32 (4)
O5—K1—C6—O6147.56 (8)O11—K1—O5—K1i148.80 (4)
O5i—K1—C6—O61141.16 (7)C6—K1—O5—K1i174.87 (3)
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1/2, y+3/2, z1/2; (iii) x+1, y+1, z+1; (iv) x1/2, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O12v0.81 (2)1.80 (2)2.6054 (12)175 (2)
O1—H1B···O62iii0.83 (2)1.81 (2)2.6262 (12)170 (2)
O2—H2C···O42vi0.85 (2)1.82 (2)2.6614 (13)171.0 (19)
O2—H2D···O30.83 (2)1.81 (2)2.6321 (14)169 (2)
O3—H3A···O4vii0.87 (3)1.94 (3)2.7710 (15)160 (2)
O3—H3B···O41vi0.87 (3)2.38 (3)3.1280 (14)145 (2)
O3—H3B···O31vi0.87 (3)2.48 (3)3.2361 (14)146 (2)
O4—H4A···O32viii0.86 (2)1.95 (2)2.7968 (14)165 (2)
O4—H4B···O32ix0.80 (3)2.14 (3)2.9271 (15)169 (2)
O5—H5C···O31vi0.80 (3)2.37 (3)3.1675 (14)174 (3)
O5—H5D···O120.87 (2)2.04 (2)2.9011 (13)170 (2)
Symmetry codes: (iii) x+1, y+1, z+1; (v) x+1/2, y1/2, z+3/2; (vi) x+3/2, y+1/2, z+3/2; (vii) x+1, y, z; (viii) x1/2, y+3/2, z1/2; (ix) x+1/2, y+1/2, z+3/2.
 

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