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The title compound, [Co(C4H7N2O2)2(C2H9N2)2][Co(C4H6N2O2)Cl2(C4H8N2O2)]Cl2·0.75H2O, contains a Co-centered cation and a Co-centered anion, together with two uncoordin­ated Cl anions and a total of 0.75 uncoordinated water mol­ecules in the asymmetric unit. Both Co atoms are six-coordinated in distorted octahedral configurations, with two di­methyl­glyoximate and two protonated ethyl­enedi­amine ligands attached to the Co atom in the cation; a di­methyl­glyoximate and a di­methyl­glyoxime ligand with two Cl anions are bonded to the Co atom in the anion. The Co atom belonging to the cation lies on a inversion center, while the anion centered on the other Co atom lies on a mirror plane, as does one of the disordered water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805015552/bh6003sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805015552/bh6003Isup2.hkl
Contains datablock I

CCDC reference: 274329

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.014 Å
  • Disorder in solvent or counterion
  • R factor = 0.048
  • wR factor = 0.144
  • Data-to-parameter ratio = 18.7

checkCIF/PLATON results

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Alert level B PLAT220_ALERT_2_B Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.64 Ratio
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.98 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C6 PLAT301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 37.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 14 PLAT420_ALERT_2_C D-H Without Acceptor >N4 - >H4C ... ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2002); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis(2-aminoethylaminium-κN2)bis(dimethylglyoximato-κ2N,N')cobalt(III) dichloro(dimethylglyoximato-κ2N,N')(dimethylglyoxime-κ2N,N')cobalt(III) dichloride 0.75-hydrate top
Crystal data top
[Co(C4H7N2O2)2(C2H9N2)2] [Co(C4H6N2O2)Cl2(C4H8N2O2)]Cl2·0.75H2OF(000) = 1774
Mr = 855.86Dx = 1.499 Mg m3
Monoclinic, C2/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yCell parameters from 4776 reflections
a = 19.531 (2) Åθ = 1.6–28.3°
b = 25.500 (2) ŵ = 1.21 mm1
c = 7.8777 (7) ÅT = 295 K
β = 104.847 (2)°Block, dark-red
V = 3792.4 (6) Å30.33 × 0.25 × 0.21 mm
Z = 4
Data collection top
Bruker APEX area-detector
diffractometer
4774 independent reflections
Radiation source: fine-focus sealed tube2557 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.067
φ and ω scansθmax = 28.3°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 2425
Tmin = 0.692, Tmax = 0.771k = 3330
13650 measured reflectionsl = 910
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)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.144H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0575P)2]
where P = (Fo2 + 2Fc2)/3
4774 reflections(Δ/σ)max < 0.001
255 parametersΔρmax = 0.47 e Å3
6 restraintsΔρmin = 0.43 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*/UeqOcc. (<1)
Co10.75000.75001.00000.0308 (5)
N10.6739 (4)0.7954 (3)1.0044 (9)0.0338 (18)
N20.6986 (4)0.7448 (3)0.7606 (9)0.0329 (18)
N30.8059 (4)0.8105 (3)0.9479 (9)0.0355 (19)
H3D0.77860.83930.94070.043*
H3E0.84320.81491.04140.043*
N40.8855 (9)0.8612 (6)0.5921 (18)0.074 (6)0.656 (19)
H4A0.88660.89380.55290.110*0.656 (19)
H4B0.85740.84170.50910.110*0.656 (19)
H4C0.92910.84780.61910.110*0.656 (19)
N4'0.915 (2)0.8868 (14)0.852 (5)0.114 (17)0.344 (19)
H4'A0.90810.92120.84060.171*0.344 (19)
H4'B0.95450.87800.82420.171*0.344 (19)
H4'C0.91770.87760.96280.171*0.344 (19)
O10.6666 (4)0.8201 (2)1.1527 (8)0.0436 (18)
H10.70060.80751.22490.065*
O20.7187 (4)0.7121 (2)0.6485 (8)0.0434 (18)
C10.6269 (5)0.8035 (3)0.8575 (12)0.034 (2)
C20.6427 (5)0.7742 (4)0.7116 (11)0.034 (2)
C30.5641 (6)0.8386 (4)0.8375 (14)0.051 (3)
H3A0.56560.85510.94790.076*
H3B0.52150.81830.80060.076*
H3C0.56490.86500.75100.076*
C40.5999 (6)0.7769 (4)0.5268 (12)0.049 (3)
H4D0.63050.77420.44940.074*
H4E0.57490.80970.50730.074*
H4F0.56640.74850.50420.074*
C50.8334 (7)0.8095 (4)0.7898 (13)0.053 (3)
H5A0.79630.79710.69110.063*
H5B0.87220.78450.80850.063*
C60.8591 (8)0.8615 (5)0.7436 (17)0.061 (3)
H6A0.82040.88640.72560.073*0.656 (19)
H6B0.89630.87370.84240.073*0.656 (19)
H6C0.87090.85710.63210.073*0.344 (19)
H6D0.81910.88530.72270.073*0.344 (19)
Co20.68886 (10)1.00000.7089 (2)0.0309 (5)
Cl10.5831 (2)1.00000.7681 (4)0.0448 (9)
Cl20.7963 (2)1.00000.6510 (5)0.0504 (10)
N50.6535 (4)0.9521 (3)0.5212 (9)0.0329 (18)
N60.7224 (4)0.9520 (3)0.8923 (9)0.0360 (19)
O30.6575 (4)0.8991 (2)0.5409 (9)0.052 (2)
H30.68000.89850.64430.077*
O40.7164 (4)0.9002 (2)0.8642 (8)0.0472 (19)
C70.6218 (5)0.9710 (3)0.3701 (12)0.034 (2)
C80.5877 (6)0.9392 (4)0.2131 (12)0.045 (3)
H8A0.60060.95290.11210.067*
H8B0.53720.94070.19390.067*
H8C0.60320.90340.23190.067*
C90.7518 (6)0.9712 (4)1.0451 (12)0.038 (2)
C100.7825 (7)0.9383 (4)1.2025 (13)0.057 (3)
H10A0.78540.95851.30690.085*
H10B0.82900.92691.19970.085*
H10C0.75280.90831.20220.085*
Cl30.5488 (7)0.6600 (6)0.7525 (15)0.099 (5)0.58 (4)
Cl3'0.5391 (19)0.684 (2)0.805 (7)0.29 (2)0.42 (4)
O1011.043 (5)1.00000.975 (13)0.18 (4)0.25
H1011.01671.00000.87540.276*0.25
H1021.08591.00000.98370.276*0.25
O1020.960 (4)0.9544 (19)0.554 (10)0.22 (3)0.25
H1030.91940.95870.48110.329*0.25
H1040.98130.92130.53910.329*0.25
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0409 (12)0.0315 (10)0.0204 (9)0.0120 (9)0.0084 (7)0.0003 (7)
N10.043 (5)0.034 (4)0.026 (4)0.012 (4)0.012 (4)0.003 (3)
N20.044 (5)0.035 (4)0.021 (4)0.008 (4)0.009 (3)0.003 (3)
N30.048 (6)0.034 (4)0.024 (4)0.011 (4)0.008 (3)0.000 (3)
N40.106 (16)0.074 (11)0.044 (10)0.017 (10)0.026 (9)0.005 (7)
N4'0.16 (5)0.10 (3)0.11 (3)0.07 (3)0.07 (3)0.02 (2)
O10.053 (5)0.048 (4)0.030 (4)0.019 (4)0.012 (3)0.006 (3)
O20.060 (5)0.045 (4)0.025 (3)0.012 (4)0.013 (3)0.008 (3)
C10.036 (6)0.034 (5)0.033 (5)0.006 (4)0.009 (4)0.002 (4)
C20.039 (6)0.033 (5)0.027 (5)0.007 (5)0.002 (4)0.003 (4)
C30.049 (8)0.051 (7)0.050 (7)0.019 (6)0.010 (5)0.003 (5)
C40.049 (7)0.062 (7)0.031 (6)0.012 (6)0.001 (5)0.001 (5)
C50.075 (9)0.050 (7)0.040 (6)0.003 (6)0.027 (6)0.003 (5)
C60.071 (10)0.056 (8)0.065 (8)0.009 (7)0.033 (7)0.008 (6)
Co20.0413 (12)0.0265 (9)0.0258 (9)0.0000.0100 (8)0.000
Cl10.045 (2)0.051 (2)0.041 (2)0.0000.0162 (17)0.000
Cl20.048 (3)0.065 (3)0.043 (2)0.0000.0193 (17)0.000
N50.045 (5)0.020 (4)0.034 (4)0.000 (4)0.011 (4)0.001 (3)
N60.048 (6)0.029 (4)0.032 (4)0.004 (4)0.011 (4)0.001 (3)
O30.084 (6)0.025 (4)0.041 (4)0.003 (4)0.006 (4)0.002 (3)
O40.069 (6)0.029 (4)0.042 (4)0.009 (3)0.009 (4)0.003 (3)
C70.040 (6)0.031 (5)0.034 (5)0.001 (4)0.014 (4)0.000 (4)
C80.060 (8)0.037 (6)0.033 (5)0.001 (5)0.006 (5)0.005 (4)
C90.045 (7)0.041 (5)0.029 (5)0.005 (5)0.011 (5)0.001 (4)
C100.076 (9)0.056 (7)0.035 (6)0.011 (6)0.007 (6)0.002 (5)
Cl30.065 (6)0.171 (11)0.058 (6)0.024 (6)0.013 (4)0.005 (6)
Cl3'0.14 (2)0.34 (4)0.30 (3)0.14 (2)0.12 (2)0.23 (3)
O1010.21 (12)0.12 (6)0.22 (9)0.0000.05 (9)0.000
O1020.27 (11)0.08 (3)0.33 (10)0.03 (4)0.11 (7)0.05 (5)
Geometric parameters (Å, º) top
Co1—N11.892 (7)C5—H5A0.9700
Co1—N1i1.892 (7)C5—H5B0.9700
Co1—N2i1.900 (7)C6—H6A0.9700
Co1—N21.900 (7)C6—H6B0.9700
Co1—N31.993 (8)C6—H6C0.9700
Co1—N3i1.993 (8)C6—H6D0.9700
N1—C11.296 (11)Co2—N6ii1.879 (7)
N1—O11.366 (8)Co2—N61.879 (7)
N2—C21.299 (11)Co2—N51.906 (7)
N2—O21.344 (9)Co2—N5ii1.906 (7)
N3—C51.478 (11)Co2—Cl12.230 (4)
N3—H3D0.9000Co2—Cl22.258 (4)
N3—H3E0.9000N5—C71.286 (11)
N4—C61.416 (16)N5—O31.362 (8)
N4—H4A0.8900N6—C91.290 (11)
N4—H4B0.8900N6—O41.340 (9)
N4—H4C0.8900O3—H30.8200
N4'—C61.36 (4)C7—C7ii1.478 (17)
N4'—H4'A0.8900C7—C81.486 (12)
N4'—H4'B0.8900C8—H8A0.9600
N4'—H4'C0.8900C8—H8B0.9600
O1—H10.8202C8—H8C0.9600
C1—C21.470 (12)C9—C9ii1.468 (19)
C1—C31.492 (13)C9—C101.490 (13)
C2—C41.483 (12)C10—H10A0.9600
C3—H3A0.9600C10—H10B0.9600
C3—H3B0.9600C10—H10C0.9600
C3—H3C0.9600O101—H1010.8206
C4—H4D0.9600O101—H1020.8203
C4—H4E0.9600O102—H1030.8628
C4—H4F0.9600O102—H1040.9590
C5—C61.496 (15)
N1—Co1—N1i180.000 (2)N4'—C6—N497.4 (18)
N1—Co1—N2i99.0 (3)N4'—C6—C5122.0 (19)
N1i—Co1—N2i81.0 (3)N4—C6—C5114.6 (11)
N1—Co1—N281.0 (3)N4'—C6—H6A104.3
N1i—Co1—N299.0 (3)N4—C6—H6A108.6
N2i—Co1—N2180.000 (2)C5—C6—H6A108.6
N1—Co1—N390.2 (3)N4—C6—H6B108.6
N1i—Co1—N389.8 (3)C5—C6—H6B108.6
N2i—Co1—N388.4 (3)H6A—C6—H6B107.6
N2—Co1—N391.6 (3)N4'—C6—H6C106.8
N1—Co1—N3i89.8 (3)C5—C6—H6C106.8
N1i—Co1—N3i90.2 (3)H6A—C6—H6C107.5
N2i—Co1—N3i91.6 (3)H6B—C6—H6C117.5
N2—Co1—N3i88.4 (3)N4'—C6—H6D106.8
N3—Co1—N3i180.000 (2)N4—C6—H6D108.2
C1—N1—O1119.0 (8)C5—C6—H6D106.8
C1—N1—Co1117.5 (6)H6B—C6—H6D109.9
O1—N1—Co1123.5 (6)H6C—C6—H6D106.7
C2—N2—O2121.8 (7)N6ii—Co2—N681.3 (5)
C2—N2—Co1116.4 (6)N6ii—Co2—N5179.0 (4)
O2—N2—Co1121.8 (6)N6—Co2—N599.5 (3)
C5—N3—Co1119.8 (6)N6ii—Co2—N5ii99.5 (3)
C5—N3—H3D107.4N6—Co2—N5ii179.0 (4)
Co1—N3—H3D107.4N5—Co2—N5ii79.7 (4)
C5—N3—H3E107.4N6ii—Co2—Cl189.9 (3)
Co1—N3—H3E107.4N6—Co2—Cl189.9 (3)
H3D—N3—H3E106.9N5—Co2—Cl189.5 (3)
C6—N4—H4A109.5N5ii—Co2—Cl189.5 (3)
C6—N4—H4B109.5N6ii—Co2—Cl289.8 (3)
C6—N4—H4C109.5N6—Co2—Cl289.8 (3)
C6—N4'—H4'A109.5N5—Co2—Cl290.8 (3)
C6—N4'—H4'B109.5N5ii—Co2—Cl290.8 (3)
H4'A—N4'—H4'B109.5Cl1—Co2—Cl2179.59 (16)
C6—N4'—H4'C109.5C7—N5—O3118.6 (7)
H4'A—N4'—H4'C109.5C7—N5—Co2118.1 (6)
H4'B—N4'—H4'C109.5O3—N5—Co2123.3 (6)
N1—O1—H199.8C9—N6—O4121.9 (7)
N1—C1—C2111.9 (8)C9—N6—Co2117.0 (6)
N1—C1—C3124.4 (8)O4—N6—Co2121.1 (6)
C2—C1—C3123.7 (8)N5—O3—H397.6
N2—C2—C1113.0 (8)N5—C7—C7ii112.0 (5)
N2—C2—C4122.6 (8)N5—C7—C8124.9 (8)
C1—C2—C4124.4 (9)C7ii—C7—C8123.1 (5)
C1—C3—H3A109.5C7—C8—H8A109.5
C1—C3—H3B109.5C7—C8—H8B109.5
H3A—C3—H3B109.5H8A—C8—H8B109.5
C1—C3—H3C109.5C7—C8—H8C109.5
H3A—C3—H3C109.5H8A—C8—H8C109.5
H3B—C3—H3C109.5H8B—C8—H8C109.5
C2—C4—H4D109.5N6—C9—C9ii112.3 (5)
C2—C4—H4E109.5N6—C9—C10123.4 (9)
H4D—C4—H4E109.5C9ii—C9—C10124.3 (6)
C2—C4—H4F109.5C9—C10—H10A109.5
H4D—C4—H4F109.5C9—C10—H10B109.5
H4E—C4—H4F109.5H10A—C10—H10B109.5
N3—C5—C6114.0 (9)C9—C10—H10C109.5
N3—C5—H5A108.8H10A—C10—H10C109.5
C6—C5—H5A108.8H10B—C10—H10C109.5
N3—C5—H5B108.8H101—O101—H102117.3
C6—C5—H5B108.8H103—O102—H104112.4
H5A—C5—H5B107.7
N2i—Co1—N1—C1177.8 (7)N1—C1—C2—C4178.0 (9)
N2—Co1—N1—C12.2 (7)C3—C1—C2—C41.8 (15)
N3—Co1—N1—C189.4 (7)Co1—N3—C5—C6166.4 (8)
N3i—Co1—N1—C190.6 (7)N3—C5—C6—N4'63 (3)
N2i—Co1—N1—O11.6 (7)N3—C5—C6—N4179.8 (12)
N2—Co1—N1—O1178.4 (7)N6—Co2—N5—C7176.4 (7)
N3—Co1—N1—O190.0 (7)N5ii—Co2—N5—C73.0 (9)
N3i—Co1—N1—O190.0 (7)Cl1—Co2—N5—C786.6 (7)
N1—Co1—N2—C23.7 (7)Cl2—Co2—N5—C793.7 (7)
N1i—Co1—N2—C2176.3 (7)N6—Co2—N5—O31.0 (8)
N3—Co1—N2—C286.3 (7)N5ii—Co2—N5—O3179.7 (5)
N3i—Co1—N2—C293.7 (7)Cl1—Co2—N5—O390.8 (7)
N1—Co1—N2—O2175.7 (7)Cl2—Co2—N5—O389.0 (7)
N1i—Co1—N2—O24.3 (7)N6ii—Co2—N6—C91.4 (9)
N3—Co1—N2—O294.3 (7)N5—Co2—N6—C9179.3 (7)
N3i—Co1—N2—O285.7 (7)Cl1—Co2—N6—C991.3 (7)
N1—Co1—N3—C5123.7 (8)Cl2—Co2—N6—C988.5 (7)
N1i—Co1—N3—C556.3 (8)N6ii—Co2—N6—O4179.1 (5)
N2i—Co1—N3—C5137.3 (8)N5—Co2—N6—O40.2 (8)
N2—Co1—N3—C542.7 (8)Cl1—Co2—N6—O489.2 (7)
O1—N1—C1—C2179.9 (7)Cl2—Co2—N6—O491.1 (7)
Co1—N1—C1—C20.5 (11)O3—N5—C7—C7ii179.9 (6)
O1—N1—C1—C30.2 (14)Co2—N5—C7—C7ii2.5 (7)
Co1—N1—C1—C3179.3 (8)O3—N5—C7—C81.1 (15)
O2—N2—C2—C1175.1 (8)Co2—N5—C7—C8176.4 (8)
Co1—N2—C2—C14.3 (10)O4—N6—C9—C9ii179.4 (6)
O2—N2—C2—C44.5 (14)Co2—N6—C9—C9ii1.1 (7)
Co1—N2—C2—C4176.1 (8)O4—N6—C9—C101.0 (15)
N1—C1—C2—N22.5 (12)Co2—N6—C9—C10178.5 (8)
C3—C1—C2—N2177.7 (9)
Symmetry codes: (i) x+3/2, y+3/2, z+2; (ii) x, y+2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H3D···O40.901.972.851 (10)166
N4—H4A···O1020.892.112.85 (5)140
N4—H4B···O2iii0.892.163.041 (17)168
O1—H1···O2i0.821.712.518 (10)168
O1—H1···N2i0.822.363.034 (10)141
O3—H3···O40.821.702.512 (9)172
O3—H3···N60.822.353.048 (10)143
Symmetry codes: (i) x+3/2, y+3/2, z+2; (iii) x+3/2, y+3/2, z+1.
 

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