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In the title compound, [Co(C3H6NO2S)(C2H8N2)2](ClO4)2·H2O, the central CoIII atom is coordinated by one N,S-bidentate L-cysteine (L-H2cys) and two N,N′-bidentate ethyl­enediamine (en) ligands in a slightly distorted octa­hedral geometry with a Δ configuration. The L-Hcys chelate ring adopts a λ conformation, while the two en chelate rings have a δ conformation.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806050033/ng2163sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806050033/ng2163Isup2.hkl
Contains datablock I

CCDC reference: 630196

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.036
  • wR factor = 0.099
  • Data-to-parameter ratio = 21.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - S1 .. 5.25 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl2 PLAT420_ALERT_2_C D-H Without Acceptor N3 - H6 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N3 - H7 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N4 - H8 ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H7 .. O8 .. 2.67 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H6 .. O8 .. 2.61 Ang. PLAT731_ALERT_1_C Bond Calc 0.81(4), Rep 0.809(19) ...... 2.11 su-Ra O2 -H1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.81(4), Rep 0.809(18) ...... 2.22 su-Ra O11 -H23 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.81(4), Rep 0.809(19) ...... 2.11 su-Ra O2 -H1 1.555 1.555
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 29.99 From the CIF: _reflns_number_total 5431 Count of symmetry unique reflns 3066 Completeness (_total/calc) 177.14% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2365 Fraction of Friedel pairs measured 0.771 Are heavy atom types Z>Si present yes PLAT791_ALERT_1_G Confirm the Absolute Configuration of C2 = . R
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: WinAFC (Rigaku/MSC, 2004); cell refinement: WinAFC; data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

ΔL-(L-Cysteinato-κ2N,S)bis(ethylenediamine-κ2N,N')cobalt(III) bis(perchlorate) monohydrate top
Crystal data top
[Co(C3H6NO2S)(C2H8N2)2](ClO4)2·H2OF(000) = 1064
Mr = 516.21Dx = 1.835 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71069 Å
Hall symbol: P 2ac 2abCell parameters from 25 reflections
a = 11.987 (4) Åθ = 12.5–14.9°
b = 16.926 (6) ŵ = 1.38 mm1
c = 9.209 (3) ÅT = 296 K
V = 1868.5 (12) Å3Prism, dark brown
Z = 40.60 × 0.40 × 0.32 mm
Data collection top
Rigaku AFC-7R
diffractometer
5056 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.027
Graphite monochromatorθmax = 30.0°, θmin = 2.5°
ω–2θ scansh = 716
Absorption correction: ψ scan
(North et al., 1968)
k = 023
Tmin = 0.491, Tmax = 0.666l = 1212
6218 measured reflections3 standard reflections every 150 reflections
5431 independent reflections intensity decay: 1.0%
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.036 w = 1/[σ2(Fo2) + (0.0657P)2 + 0.6912P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.099(Δ/σ)max < 0.001
S = 1.07Δρmax = 0.78 e Å3
5431 reflectionsΔρmin = 0.77 e Å3
255 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
4 restraintsExtinction coefficient: 0.0237 (14)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983), no Friedel pairs
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.004 (12)
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
Co10.47672 (2)0.103004 (16)0.37721 (3)0.02071 (8)
S10.48017 (5)0.00569 (3)0.54160 (6)0.02847 (12)
O10.73762 (19)0.22769 (12)0.6910 (2)0.0368 (4)
O20.7443 (2)0.11823 (15)0.8247 (2)0.0463 (5)
H10.800 (3)0.144 (3)0.841 (6)0.069*
N10.58312 (17)0.16183 (12)0.5033 (2)0.0246 (4)
H20.64960.16400.45810.029*
H30.55840.21170.51350.029*
N20.34975 (16)0.15071 (13)0.4773 (2)0.0261 (4)
H40.36330.15270.57340.031*
H50.33950.20040.44530.031*
N30.36294 (19)0.04459 (13)0.2647 (2)0.0296 (4)
H60.37900.04740.16930.036*
H70.36320.00660.29100.036*
N40.4808 (2)0.18783 (12)0.2231 (2)0.0288 (4)
H80.41100.20020.19530.035*
H90.51340.23170.25860.035*
N50.60096 (19)0.05560 (13)0.2663 (2)0.0303 (4)
H100.65660.04260.32750.036*
H110.57730.01120.22240.036*
C10.6036 (2)0.03793 (15)0.6383 (3)0.0337 (5)
H120.60540.01450.73440.040*
H130.67010.02170.58630.040*
C20.59957 (19)0.12723 (14)0.6499 (2)0.0270 (4)
H250.53500.14100.70820.032*
C30.7027 (2)0.16370 (16)0.7228 (3)0.0288 (4)
C40.2481 (2)0.10318 (17)0.4495 (3)0.0328 (5)
H150.18180.13420.46960.039*
H160.24730.05670.51130.039*
C50.2509 (2)0.07926 (17)0.2920 (3)0.0336 (5)
H170.19300.04070.27200.040*
H180.23890.12490.23020.040*
C60.5454 (2)0.15750 (18)0.0972 (3)0.0366 (6)
H190.57130.20110.03770.044*
H200.49880.12350.03780.044*
C70.6432 (2)0.1117 (2)0.1558 (3)0.0399 (6)
H210.67970.08310.07780.048*
H220.69690.14740.19910.048*
Cl10.43393 (5)0.38458 (4)0.54580 (7)0.03353 (14)
O30.4579 (2)0.31652 (17)0.4617 (4)0.0647 (8)
O40.4796 (3)0.3719 (3)0.6884 (3)0.0772 (9)
O50.31590 (19)0.39700 (19)0.5564 (4)0.0599 (7)
O60.4840 (3)0.45364 (17)0.4913 (4)0.0744 (9)
Cl20.26380 (6)0.16612 (4)0.87287 (8)0.04103 (15)
O70.3542 (3)0.2061 (2)0.8029 (4)0.0763 (10)
O80.3005 (5)0.0894 (2)0.9164 (6)0.1076 (17)
O90.2367 (3)0.20894 (19)1.0015 (3)0.0648 (8)
O100.1703 (4)0.1601 (4)0.7822 (5)0.117 (2)
O110.9151 (2)0.16773 (14)0.9737 (3)0.0442 (5)
H230.956 (4)0.1321 (19)0.998 (5)0.066*
H240.936 (4)0.2133 (12)0.978 (5)0.066*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02155 (13)0.02132 (13)0.01927 (13)0.00031 (10)0.00091 (10)0.00089 (10)
S10.0311 (2)0.0245 (2)0.0298 (3)0.0043 (2)0.0023 (2)0.00591 (19)
O10.0431 (10)0.0327 (9)0.0347 (9)0.0092 (8)0.0045 (8)0.0006 (7)
O20.0498 (12)0.0514 (13)0.0376 (10)0.0178 (10)0.0195 (9)0.0159 (9)
N10.0257 (8)0.0237 (8)0.0243 (8)0.0007 (7)0.0014 (6)0.0035 (7)
N20.0234 (8)0.0313 (10)0.0237 (9)0.0015 (7)0.0002 (7)0.0014 (7)
N30.0336 (10)0.0292 (10)0.0260 (9)0.0057 (8)0.0033 (8)0.0031 (8)
N40.0311 (9)0.0298 (9)0.0255 (8)0.0002 (8)0.0004 (8)0.0054 (7)
N50.0293 (10)0.0330 (10)0.0286 (10)0.0052 (8)0.0044 (8)0.0009 (8)
C10.0338 (11)0.0281 (10)0.0391 (13)0.0034 (9)0.0097 (11)0.0105 (10)
C20.0271 (10)0.0307 (10)0.0231 (10)0.0041 (8)0.0003 (8)0.0026 (8)
C30.0304 (10)0.0357 (12)0.0204 (9)0.0009 (9)0.0016 (8)0.0014 (8)
C40.0222 (9)0.0402 (12)0.0361 (11)0.0035 (9)0.0027 (9)0.0038 (10)
C50.0291 (11)0.0356 (12)0.0362 (12)0.0049 (9)0.0075 (10)0.0019 (10)
C60.0415 (14)0.0449 (14)0.0235 (10)0.0011 (11)0.0064 (9)0.0067 (9)
C70.0352 (12)0.0526 (16)0.0318 (12)0.0035 (11)0.0107 (10)0.0082 (11)
Cl10.0253 (2)0.0316 (3)0.0437 (3)0.0012 (2)0.0003 (2)0.0082 (2)
O30.0596 (16)0.0517 (14)0.083 (2)0.0058 (12)0.0070 (15)0.0282 (14)
O40.0695 (18)0.111 (3)0.0513 (15)0.005 (2)0.0145 (15)0.0040 (17)
O50.0266 (10)0.0783 (19)0.0748 (18)0.0044 (11)0.0018 (11)0.0245 (16)
O60.0655 (17)0.0442 (13)0.113 (3)0.0041 (13)0.010 (2)0.0225 (16)
Cl20.0446 (3)0.0428 (3)0.0357 (3)0.0048 (3)0.0032 (3)0.0117 (3)
O70.089 (2)0.089 (2)0.0513 (16)0.0304 (19)0.0245 (16)0.0117 (16)
O80.142 (4)0.0451 (17)0.135 (4)0.007 (2)0.003 (4)0.008 (2)
O90.093 (2)0.0628 (17)0.0390 (12)0.0042 (16)0.0109 (14)0.0150 (11)
O100.065 (2)0.216 (6)0.070 (2)0.001 (3)0.0267 (18)0.051 (3)
O110.0448 (11)0.0430 (11)0.0449 (12)0.0037 (9)0.0122 (10)0.0022 (10)
Geometric parameters (Å, º) top
Co1—S12.2376 (8)C1—C21.516 (4)
Co1—N11.991 (2)C1—H120.9700
Co1—N21.954 (2)C1—H130.9700
Co1—N31.978 (2)C2—C31.536 (3)
Co1—N42.019 (2)C2—H250.9700
Co1—N51.976 (2)C4—C51.506 (4)
S1—C11.811 (3)C4—H150.9700
O1—C31.198 (3)C4—H160.9700
O2—C31.312 (3)C5—H170.9700
O2—H10.809 (19)C5—H180.9700
N1—C21.485 (3)C6—C71.505 (4)
N1—H20.9000C6—H190.9700
N1—H30.9000C6—H200.9700
N2—C41.482 (3)C7—H210.9700
N2—H40.9000C7—H220.9700
N2—H50.9000Cl1—O61.407 (3)
N3—C51.487 (4)Cl1—O31.417 (3)
N3—H60.9000Cl1—O51.434 (2)
N3—H70.9000Cl1—O41.439 (3)
N4—C61.486 (3)Cl2—O101.401 (4)
N4—H80.9000Cl2—O91.426 (3)
N4—H90.9000Cl2—O81.429 (4)
N5—C71.481 (4)Cl2—O71.431 (3)
N5—H100.9000O11—H230.809 (18)
N5—H110.9000O11—H240.810 (18)
S1—Co1—N4176.78 (7)C2—C1—H13110.1
N2—Co1—N5177.02 (9)S1—C1—H13110.1
N2—Co1—N385.22 (10)H12—C1—H13108.4
N5—Co1—N392.64 (10)N1—C2—C1109.4 (2)
N2—Co1—N190.98 (9)N1—C2—C3110.25 (19)
N5—Co1—N191.23 (10)C1—C2—C3114.0 (2)
N1—Co1—N3175.60 (9)N1—C2—H25107.6
N2—Co1—N493.25 (9)C1—C2—H25107.6
N5—Co1—N484.68 (9)C3—C2—H25107.6
N3—Co1—N490.24 (10)O1—C3—O2124.9 (3)
N1—Co1—N492.20 (9)O1—C3—C2122.5 (2)
N2—Co1—S189.96 (7)O2—C3—C2112.5 (2)
N5—Co1—S192.10 (7)N2—C4—C5107.1 (2)
N3—Co1—S189.96 (7)N2—C4—H15110.3
N1—Co1—S187.81 (6)C5—C4—H15110.3
C1—S1—Co197.23 (8)N2—C4—H16110.3
C3—O2—H198 (4)C5—C4—H16110.3
C2—N1—Co1114.71 (14)H15—C4—H16108.5
C2—N1—H2108.6N3—C5—C4106.8 (2)
Co1—N1—H2108.6N3—C5—H17110.4
C2—N1—H3108.6C4—C5—H17110.4
Co1—N1—H3108.6N3—C5—H18110.4
H2—N1—H3107.6C4—C5—H18110.4
C4—N2—Co1109.53 (16)H17—C5—H18108.6
C4—N2—H4109.8N4—C6—C7107.7 (2)
Co1—N2—H4109.8N4—C6—H19110.2
C4—N2—H5109.8C7—C6—H19110.2
Co1—N2—H5109.8N4—C6—H20110.2
H4—N2—H5108.2C7—C6—H20110.2
C5—N3—Co1109.69 (16)H19—C6—H20108.5
C5—N3—H6109.7N5—C7—C6108.1 (2)
Co1—N3—H6109.7N5—C7—H21110.1
C5—N3—H7109.7C6—C7—H21110.1
Co1—N3—H7109.7N5—C7—H22110.1
H6—N3—H7108.2C6—C7—H22110.1
C6—N4—Co1108.40 (16)H21—C7—H22108.4
C6—N4—H8110.0O6—Cl1—O3113.2 (2)
Co1—N4—H8110.0O6—Cl1—O5108.9 (2)
C6—N4—H9110.0O3—Cl1—O5110.90 (17)
Co1—N4—H9110.0O6—Cl1—O4106.7 (3)
H8—N4—H9108.4O3—Cl1—O4107.5 (2)
C7—N5—Co1110.64 (17)O5—Cl1—O4109.6 (2)
C7—N5—H10109.5O10—Cl2—O9110.5 (3)
Co1—N5—H10109.5O10—Cl2—O8110.3 (4)
C7—N5—H11109.5O9—Cl2—O8107.4 (3)
Co1—N5—H11109.5O10—Cl2—O7111.8 (3)
H10—N5—H11108.1O9—Cl2—O7107.9 (2)
C2—C1—S1108.04 (17)O8—Cl2—O7108.8 (3)
C2—C1—H12110.1H23—O11—H24121 (3)
S1—C1—H12110.1
N2—Co1—S1—C1106.38 (12)N3—Co1—N5—C7101.1 (2)
N5—Co1—S1—C175.76 (12)N1—Co1—N5—C781.03 (19)
N3—Co1—S1—C1168.40 (12)N4—Co1—N5—C711.07 (19)
N1—Co1—S1—C115.39 (12)S1—Co1—N5—C7168.88 (18)
N2—Co1—N1—C279.22 (17)Co1—S1—C1—C239.72 (19)
N5—Co1—N1—C2102.76 (17)Co1—N1—C2—C139.7 (2)
N4—Co1—N1—C2172.51 (16)Co1—N1—C2—C3165.85 (15)
S1—Co1—N1—C210.70 (15)S1—C1—C2—N153.0 (2)
N3—Co1—N2—C416.44 (17)S1—C1—C2—C3176.94 (16)
N1—Co1—N2—C4161.33 (17)N1—C2—C3—O124.7 (3)
N4—Co1—N2—C4106.40 (17)C1—C2—C3—O1148.2 (3)
S1—Co1—N2—C473.52 (16)N1—C2—C3—O2157.3 (2)
N2—Co1—N3—C511.85 (17)C1—C2—C3—O233.8 (3)
N5—Co1—N3—C5166.08 (18)Co1—N2—C4—C540.9 (2)
N4—Co1—N3—C581.39 (18)Co1—N3—C5—C436.9 (2)
S1—Co1—N3—C5101.81 (17)N2—C4—C5—N350.3 (3)
N2—Co1—N4—C6161.58 (18)Co1—N4—C6—C739.8 (3)
N5—Co1—N4—C616.28 (18)Co1—N5—C7—C635.9 (3)
N3—Co1—N4—C676.35 (18)N4—C6—C7—N549.6 (3)
N1—Co1—N4—C6107.31 (18)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H5···O1i0.902.132.906 (3)144
O2—H1···O110.81 (2)1.89 (3)2.603 (3)147 (5)
N1—H3···O30.902.203.042 (4)156
N1—H2···O5ii0.902.253.013 (3)143
N2—H5···O30.902.433.095 (4)131
N2—H4···O70.902.303.141 (4)155
N3—H7···O8iii0.902.673.307 (5)128
N3—H6···O8iv0.902.613.379 (6)144
N4—H9···O30.902.453.106 (3)130
N5—H10···O5ii0.902.423.154 (4)139
N5—H11···O6v0.902.323.106 (4)147
Symmetry codes: (i) x1/2, y+1/2, z+1; (ii) x+1/2, y+1/2, z+1; (iii) x+1/2, y, z1/2; (iv) x, y, z1; (v) x+1, y1/2, z+1/2.
 

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