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The title compound, [Co(C4H7N2O2)2(NO2)(H2O)]·H2O, is a distorted octa­hedral CoIII complex with two dimethyl­glyoximate ligands in the equatorial plane and nitro and aqua substituents in the axial positions. The two dimethyl­glyoximate ligands are involved in intra­molecular hydrogen bonds. Coordinated and uncoordinated water mol­ecules participate in O—H...O hydrogen bonds, linking the cobalt complexes into a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806037226/kp2048sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806037226/kp2048Isup2.hkl
Contains datablock I

CCDC reference: 624897

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.013 Å
  • R factor = 0.087
  • wR factor = 0.173
  • Data-to-parameter ratio = 14.3

checkCIF/PLATON results

No syntax errors found



Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.134 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.13 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N5 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 2 N3 -CO1 -N1 -C1 -116.00 3.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 7 N3 -CO1 -N1 -O1 61.00 3.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 14 N4 -CO1 -N2 -C3 -127.00 9.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 19 N4 -CO1 -N2 -O2 54.00 10.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 22 N1 -CO1 -N3 -C5 -63.00 3.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 27 N1 -CO1 -N3 -O3 111.00 3.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 31 N2 -CO1 -N4 -C7 -57.00 10.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 36 N2 -CO1 -N4 -O4 120.00 9.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 45 O7 -CO1 -N5 -O6 -84.00 5.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 50 O7 -CO1 -N5 -O5 98.00 5.00 1.555 1.555 1.555 1.555
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 15 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 11 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXTL (Sheldrick, 1998).

Aquabis(dimethylyglyoximato-κ2N,N')nitrocobalt (III) monohydrate top
Crystal data top
[Co(C4H7N2O2)2(NO2)(H2O)]·H2OF(000) = 768
Mr = 371.20Dx = 1.650 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 8.0846 (12) ÅCell parameters from 452 reflections
b = 17.213 (2) Åθ = 2.8–17.8°
c = 13.1945 (15) ŵ = 1.20 mm1
β = 125.521 (7)°T = 293 K
V = 1494.5 (4) Å3Rod, orange
Z = 40.20 × 0.07 × 0.05 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2908 independent reflections
Radiation source: fine-focus sealed tube1594 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.135
ω scansθmax = 26.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 99
Tmin = 0.80, Tmax = 0.94k = 2121
10278 measured reflectionsl = 1316
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)] = 0.087Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.173H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.06P)2]
where P = (Fo2 + 2Fc2)/3
2908 reflections(Δ/σ)max = 0.001
203 parametersΔρmax = 0.64 e Å3
0 restraintsΔρmin = 0.51 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
Co10.73713 (14)0.11370 (5)0.28861 (10)0.0273 (3)
O10.7732 (7)0.0381 (3)0.3790 (5)0.0369 (13)
O20.8808 (8)0.1769 (3)0.1562 (5)0.0501 (15)
O30.7397 (8)0.2742 (3)0.2311 (5)0.0542 (17)
H30.78550.24250.20700.065*
O40.5570 (8)0.0519 (3)0.4086 (5)0.0466 (15)
H40.62650.02250.39890.056*
O50.4223 (9)0.0245 (4)0.1110 (6)0.083 (2)
O60.3885 (9)0.1404 (3)0.0597 (6)0.072 (2)
O71.0004 (7)0.1376 (3)0.4432 (5)0.0401 (14)
H7X1.00970.18090.47200.048*
H7Y1.04730.10500.49860.048*
N10.8132 (8)0.0081 (3)0.3151 (6)0.0319 (15)
N20.8671 (9)0.1130 (4)0.2076 (6)0.0381 (16)
N30.6753 (8)0.2210 (3)0.2771 (6)0.0353 (16)
N40.5982 (8)0.1157 (4)0.3666 (6)0.0343 (15)
N50.4868 (9)0.0901 (4)0.1339 (6)0.0392 (17)
C10.9133 (11)0.0140 (4)0.2709 (7)0.037 (2)
C20.9902 (12)0.0953 (4)0.2829 (8)0.053 (2)
H2A0.94830.12720.32380.079*
H2B1.13590.09460.33100.079*
H2C0.93570.11590.20160.079*
C30.9442 (11)0.0465 (5)0.2071 (7)0.038 (2)
C41.0509 (13)0.0341 (5)0.1463 (9)0.060 (3)
H4A0.97840.06050.06760.091*
H4B1.05610.02040.13340.091*
H4C1.18660.05440.19890.091*
C50.5857 (11)0.2455 (4)0.3247 (7)0.037 (2)
C60.5484 (12)0.3294 (4)0.3318 (9)0.060 (3)
H6A0.64080.36020.32530.090*
H6B0.56920.33980.41000.090*
H6C0.41120.34230.26480.090*
C70.5304 (11)0.1822 (4)0.3745 (7)0.040 (2)
C80.4057 (11)0.1929 (5)0.4223 (8)0.053 (2)
H8A0.26810.20430.35430.079*
H8B0.45940.23510.48070.079*
H8C0.40860.14610.46300.079*
O81.0945 (9)0.2669 (3)0.5676 (6)0.079 (2)
H8X1.03080.28330.59390.094*
H8Y1.17710.29270.56490.094*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0256 (5)0.0267 (5)0.0309 (6)0.0028 (5)0.0172 (4)0.0034 (5)
O10.042 (3)0.030 (3)0.039 (3)0.006 (2)0.024 (3)0.014 (2)
O20.052 (3)0.064 (4)0.050 (4)0.003 (3)0.039 (3)0.014 (3)
O30.067 (4)0.037 (3)0.065 (5)0.003 (3)0.042 (4)0.010 (3)
O40.055 (4)0.049 (3)0.055 (4)0.001 (3)0.043 (3)0.004 (3)
O50.056 (4)0.055 (4)0.078 (5)0.009 (3)0.005 (4)0.002 (4)
O60.066 (4)0.062 (4)0.052 (5)0.008 (3)0.014 (4)0.008 (3)
O70.041 (3)0.030 (3)0.044 (4)0.004 (2)0.022 (3)0.003 (2)
N10.025 (3)0.030 (3)0.033 (4)0.000 (3)0.013 (3)0.002 (3)
N20.034 (3)0.053 (4)0.031 (4)0.009 (4)0.021 (3)0.008 (4)
N30.032 (4)0.024 (3)0.045 (5)0.003 (3)0.020 (3)0.006 (3)
N40.032 (3)0.035 (3)0.042 (4)0.004 (3)0.025 (3)0.001 (3)
N50.030 (4)0.042 (4)0.045 (5)0.002 (3)0.022 (4)0.004 (3)
C10.040 (5)0.038 (4)0.027 (5)0.005 (4)0.016 (4)0.004 (4)
C20.051 (5)0.047 (5)0.055 (6)0.013 (4)0.028 (5)0.009 (4)
C30.028 (4)0.050 (5)0.036 (5)0.006 (4)0.019 (4)0.005 (4)
C40.057 (6)0.088 (7)0.060 (7)0.002 (5)0.047 (5)0.011 (5)
C50.032 (4)0.041 (5)0.031 (5)0.011 (4)0.014 (4)0.001 (4)
C60.057 (6)0.039 (5)0.067 (7)0.011 (4)0.026 (5)0.006 (5)
C70.034 (5)0.040 (5)0.032 (5)0.001 (4)0.011 (4)0.007 (4)
C80.044 (5)0.063 (6)0.060 (7)0.001 (4)0.034 (5)0.016 (5)
O80.084 (5)0.068 (4)0.113 (6)0.023 (4)0.075 (5)0.034 (4)
Geometric parameters (Å, º) top
Co1—N21.885 (6)C1—C31.450 (10)
Co1—N11.886 (6)C1—C21.502 (9)
Co1—N31.897 (6)C2—H2A0.9600
Co1—N51.904 (7)C2—H2B0.9600
Co1—N41.915 (6)C2—H2C0.9600
Co1—O71.953 (5)C3—C41.495 (10)
O1—N11.328 (7)C4—H4A0.9600
O2—N21.330 (7)C4—H4B0.9600
O3—N31.359 (7)C4—H4C0.9600
O3—H30.8201C5—C71.469 (11)
O4—N41.356 (7)C5—C61.490 (9)
O4—H40.8201C6—H6A0.9600
O5—N51.207 (7)C6—H6B0.9600
O6—N51.198 (8)C6—H6C0.9600
O7—H7X0.8197C7—C81.479 (11)
O7—H7Y0.8199C8—H8A0.9600
N1—C11.299 (9)C8—H8B0.9600
N2—C31.305 (9)C8—H8C0.9600
N3—C51.274 (9)O8—H8X0.8200
N4—C71.299 (8)O8—H8Y0.8192
N2—Co1—N182.5 (3)N1—C1—C2123.6 (7)
N2—Co1—N399.7 (3)C3—C1—C2121.9 (7)
N1—Co1—N3175.0 (3)C1—C2—H2A109.5
N2—Co1—N589.2 (3)C1—C2—H2B109.5
N1—Co1—N591.3 (3)H2A—C2—H2B109.5
N3—Co1—N593.2 (3)C1—C2—H2C109.5
N2—Co1—N4178.3 (3)H2A—C2—H2C109.5
N1—Co1—N498.5 (3)H2B—C2—H2C109.5
N3—Co1—N479.4 (3)N2—C3—C1112.4 (7)
N5—Co1—N489.4 (3)N2—C3—C4123.6 (7)
N2—Co1—O788.0 (2)C1—C3—C4123.9 (7)
N1—Co1—O788.2 (2)C3—C4—H4A109.5
N3—Co1—O787.4 (2)C3—C4—H4B109.5
N5—Co1—O7177.2 (2)H4A—C4—H4B109.5
N4—Co1—O793.4 (2)C3—C4—H4C109.5
N3—O3—H395.8H4A—C4—H4C109.5
N4—O4—H494.8H4B—C4—H4C109.5
Co1—O7—H7X115.3N3—C5—C7112.5 (7)
Co1—O7—H7Y116.4N3—C5—C6123.0 (8)
H7X—O7—H7Y109.7C7—C5—C6124.4 (8)
C1—N1—O1123.7 (6)C5—C6—H6A109.5
C1—N1—Co1114.8 (5)C5—C6—H6B109.5
O1—N1—Co1121.5 (5)H6A—C6—H6B109.5
C3—N2—O2122.7 (6)C5—C6—H6C109.5
C3—N2—Co1115.8 (5)H6A—C6—H6C109.5
O2—N2—Co1121.5 (5)H6B—C6—H6C109.5
C5—N3—O3118.2 (6)N4—C7—C5111.4 (7)
C5—N3—Co1118.8 (5)N4—C7—C8124.6 (7)
O3—N3—Co1122.7 (5)C5—C7—C8124.0 (7)
C7—N4—O4117.7 (6)C7—C8—H8A109.5
C7—N4—Co1117.8 (5)C7—C8—H8B109.5
O4—N4—Co1124.4 (5)H8A—C8—H8B109.5
O6—N5—O5119.1 (7)C7—C8—H8C109.5
O6—N5—Co1120.6 (5)H8A—C8—H8C109.5
O5—N5—Co1120.2 (6)H8B—C8—H8C109.5
N1—C1—C3114.5 (7)H8X—O8—H8Y124.1
N2—Co1—N1—C10.9 (5)N3—Co1—N4—O4177.1 (6)
N3—Co1—N1—C1116 (3)N5—Co1—N4—O483.8 (5)
N5—Co1—N1—C189.9 (5)O7—Co1—N4—O496.2 (5)
N4—Co1—N1—C1179.5 (5)N2—Co1—N5—O681.4 (7)
O7—Co1—N1—C187.3 (5)N1—Co1—N5—O6163.9 (7)
N2—Co1—N1—O1178.2 (5)N3—Co1—N5—O618.3 (7)
N3—Co1—N1—O161 (3)N4—Co1—N5—O697.6 (7)
N5—Co1—N1—O192.8 (5)O7—Co1—N5—O684 (5)
N4—Co1—N1—O13.2 (5)N2—Co1—N5—O5100.7 (7)
O7—Co1—N1—O190.0 (5)N1—Co1—N5—O518.3 (7)
N1—Co1—N2—C30.3 (6)N3—Co1—N5—O5159.6 (7)
N3—Co1—N2—C3175.2 (5)N4—Co1—N5—O580.2 (7)
N5—Co1—N2—C391.7 (6)O7—Co1—N5—O598 (5)
N4—Co1—N2—C3127 (9)O1—N1—C1—C3178.4 (6)
O7—Co1—N2—C388.2 (6)Co1—N1—C1—C31.2 (8)
N1—Co1—N2—O2179.4 (6)O1—N1—C1—C22.1 (11)
N3—Co1—N2—O23.8 (6)Co1—N1—C1—C2179.3 (6)
N5—Co1—N2—O289.3 (6)O2—N2—C3—C1178.8 (6)
N4—Co1—N2—O254 (10)Co1—N2—C3—C10.2 (8)
O7—Co1—N2—O290.9 (5)O2—N2—C3—C41.7 (12)
N2—Co1—N3—C5179.1 (6)Co1—N2—C3—C4179.3 (6)
N1—Co1—N3—C563 (3)N1—C1—C3—N20.9 (10)
N5—Co1—N3—C591.2 (6)C2—C1—C3—N2179.6 (7)
N4—Co1—N3—C52.3 (6)N1—C1—C3—C4178.6 (7)
O7—Co1—N3—C591.6 (6)C2—C1—C3—C40.9 (12)
N2—Co1—N3—O35.7 (6)O3—N3—C5—C7178.1 (6)
N1—Co1—N3—O3111 (3)Co1—N3—C5—C74.4 (9)
N5—Co1—N3—O395.4 (6)O3—N3—C5—C60.1 (11)
N4—Co1—N3—O3175.7 (6)Co1—N3—C5—C6173.8 (6)
O7—Co1—N3—O381.8 (5)O4—N4—C7—C5179.6 (6)
N2—Co1—N4—C757 (10)Co1—N4—C7—C52.8 (8)
N1—Co1—N4—C7176.0 (5)O4—N4—C7—C82.1 (11)
N3—Co1—N4—C70.5 (6)Co1—N4—C7—C8174.7 (6)
N5—Co1—N4—C792.8 (6)N3—C5—C7—N44.5 (10)
O7—Co1—N4—C787.3 (6)C6—C5—C7—N4173.7 (7)
N2—Co1—N4—O4120 (9)N3—C5—C7—C8173.0 (7)
N1—Co1—N4—O47.4 (6)C6—C5—C7—C88.8 (12)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O20.821.712.528 (9)180
O)—H4···O10.821.712.530 (9)179
O7—H7X···O80.821.802.603 (8)165
O7—H7Y···O1i0.821.822.607 (8)160
O8—H8X···O2ii0.821.942.763 (11)179
O8—H8Y···O6iii0.822.092.915 (11)179
Symmetry codes: (i) x+2, y, z+1; (ii) x, y+1/2, z+1/2; (iii) x+1, y+1/2, z+1/2.
 

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