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The title compound, [Co(C12H27O3SSi)2(C7H9N)(NH3)], was obtained by the reaction of dimeric [Co{SSi(OtBu)3}2(NH3)]2 with 2-ethyl­pyridine. The CoII atom is coordinated by two S atoms from two silanethiol­ate ligands and two N atoms, one from ammonia and one from a 2-ethyl­pyridine mol­ecule. The arrangement of the ligands around the CoII centre facilitates the formation of an inter­molecular N—H...S hydrogen bond. One of the tert-butyl groups and the 2-ethyl­pyridine ligand are disordered over two positions each, with approximate occupancy ratios of 2:1 and 3:1, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807025421/gk2075sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807025421/gk2075Isup2.hkl
Contains datablock I

CCDC reference: 650540

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.003 Å
  • Disorder in main residue
  • R factor = 0.035
  • wR factor = 0.095
  • Data-to-parameter ratio = 15.2

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.56 Ratio
Alert level C PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.06 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C26A PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C5 PLAT301_ALERT_3_C Main Residue Disorder ......................... 20.00 Perc. PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1A ... ? PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1B ... ?
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

Complexes of transition metals with sulfur and nitrogen ligands serve as biological models of histidine-metal-cysteine centers found in zinc metalloproteins (Corwin et al., 1987; Kimblin et al., 2000). However, "spectroscopic silence" of zinc thiolates prevents the use of spectral experiments for simulation of enzymatic reactions in solution, i.e. direct measurement of the loss of substrate or product concentration increase. Since, cobalt and zinc coordination chemistry is similar and changes in coordination environment of cobalt complexes can be monitored by UV-VIS, we decided to synthesize appropriate cobalt complexes which could replace adequate complexes of zinc in spectral experiments. The objective of our research is exploration of the syntheses, geometrical structures and reactivity of model complexes. We have synthesized and characterized structurally several cobalt (II) silanethiolates with pyridine and pyridine related ligands (Becker et al., 2002 and the references cited therein; Pladzyk & Baranowska, 2006).

The title complex (Fig. 1), with CoN2S2 core and tetrahedrally coordinated cobalt (II), is similar to [Co{SSi(OtBu)3}2(NH3)(2-methylpyridine)], obtained earlier (Becker et al., 2002). However, ethyl substituent on the pyridine ring forces different spatial arrangement of the ligands and, in consequence, intermolecular hydrogen bond can be formed between sulfur atom and ammonia nitrogen with the N···S distance of 3.528 (2) Å, while in [Co{SSi(OtBu)3}2(NH3)(2-methylpyridine)] two N···O hydrogen bonds were present. The reorganization of ligands in the title compound involves mainly changes in the N2–Co1–N2 and S1–Co1–S2 angles, which in comparison with [Co{SSi(OtBu)3}2(NH3)(2-methylpyridine)], are wider by approximately 6–7 ° in (I). The remaining N–Co–S, Si–S–Co angles are slightly smaller than those found in [Co{SSi(OtBu)3}2(NH3)(2-methylpyridine)].

Related literature top

For related literature, see: Corwin et al. (1987); Kimblin et al. (2000); Becker et al. (2002); Pladzyk & Baranowska (2006).

Experimental top

[Co{SSi(OtBu)3}2(NH3)]2 was obtained as described (Becker et al., 2002). All other reagents were obtained commercially. 2-Ethylpyridine was dried by standard methods, and distilled prior to use. To a solution of [Co{SSi(OtBu)3}2(NH3)]2 (0.124 g, 0.2 mmol) in 10 ml of n-hexane, freshly prepared 2-ethylpyridine (22,8µl, 0.2 mmol) was added and blue, well formed crystals of [Co{SSi(OtBu)3}2(2-ethylpyridine)(NH3)] were obtained.

Refinement top

All H atoms were refined in the riding mode approximation with aromatic C—H = 0.95 Å, methyl C—H = 0.98 Å, methylene C—H = 0.99 Å, and Uiso(H) = 1.2Ueq(C) for CH groups, Uiso(H) = 1.3Ueq(C) for CH2 groups, 1.5Ueq(C) for CH3 groups. The disordered tBu group C2—C4 has site-occupancy factors of 0.660 (5) and 0.340 (5) for two orientations. Also 2-ethylpyridine was refined as disordered over two positions with occupancies of 0.736 (5) and 0.264 (5).

Structure description top

Complexes of transition metals with sulfur and nitrogen ligands serve as biological models of histidine-metal-cysteine centers found in zinc metalloproteins (Corwin et al., 1987; Kimblin et al., 2000). However, "spectroscopic silence" of zinc thiolates prevents the use of spectral experiments for simulation of enzymatic reactions in solution, i.e. direct measurement of the loss of substrate or product concentration increase. Since, cobalt and zinc coordination chemistry is similar and changes in coordination environment of cobalt complexes can be monitored by UV-VIS, we decided to synthesize appropriate cobalt complexes which could replace adequate complexes of zinc in spectral experiments. The objective of our research is exploration of the syntheses, geometrical structures and reactivity of model complexes. We have synthesized and characterized structurally several cobalt (II) silanethiolates with pyridine and pyridine related ligands (Becker et al., 2002 and the references cited therein; Pladzyk & Baranowska, 2006).

The title complex (Fig. 1), with CoN2S2 core and tetrahedrally coordinated cobalt (II), is similar to [Co{SSi(OtBu)3}2(NH3)(2-methylpyridine)], obtained earlier (Becker et al., 2002). However, ethyl substituent on the pyridine ring forces different spatial arrangement of the ligands and, in consequence, intermolecular hydrogen bond can be formed between sulfur atom and ammonia nitrogen with the N···S distance of 3.528 (2) Å, while in [Co{SSi(OtBu)3}2(NH3)(2-methylpyridine)] two N···O hydrogen bonds were present. The reorganization of ligands in the title compound involves mainly changes in the N2–Co1–N2 and S1–Co1–S2 angles, which in comparison with [Co{SSi(OtBu)3}2(NH3)(2-methylpyridine)], are wider by approximately 6–7 ° in (I). The remaining N–Co–S, Si–S–Co angles are slightly smaller than those found in [Co{SSi(OtBu)3}2(NH3)(2-methylpyridine)].

For related literature, see: Corwin et al. (1987); Kimblin et al. (2000); Becker et al. (2002); Pladzyk & Baranowska (2006).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); 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).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title compound, showing the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. Only major orientations of the disordered groups are shown. C-bound H atoms have been omitted for clarity.
[Figure 2] Fig. 2. The crystal packing of the title compound, viewed approximately down the a axis.
Ammine(2-ethylpyridine-κN)bis(tri-tert-butoxysilanethiolato- κS)cobalt(II) top
Crystal data top
[Co(C12H27O3SSi)2(C7H9N)(NH3)]Z = 2
Mr = 742.09F(000) = 802
Triclinic, P1Dx = 1.184 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.6939 (4) ÅCell parameters from 12985 reflections
b = 13.7249 (6) Åθ = 2.2–32.4°
c = 16.1266 (6) ŵ = 0.61 mm1
α = 78.605 (4)°T = 120 K
β = 88.106 (3)°Prism, blue
γ = 81.830 (4)°0.26 × 0.11 × 0.04 mm
V = 2081.94 (15) Å3
Data collection top
Kuma KM-4-CCD κ-geometry
diffractometer
7322 independent reflections
Graphite monochromator6247 reflections with I > 2σ(I)
Detector resolution: 8.1883 pixels mm-1Rint = 0.025
ω scansθmax = 25.1°, θmin = 2.2°
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2005)
h = 1111
Tmin = 0.787, Tmax = 0.944k = 1316
13393 measured reflectionsl = 1819
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)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0534P)2 + 0.9644P]
where P = (Fo2 + 2Fc2)/3
7322 reflections(Δ/σ)max = 0.001
482 parametersΔρmax = 0.39 e Å3
0 restraintsΔρmin = 0.31 e Å3
Crystal data top
[Co(C12H27O3SSi)2(C7H9N)(NH3)]γ = 81.830 (4)°
Mr = 742.09V = 2081.94 (15) Å3
Triclinic, P1Z = 2
a = 9.6939 (4) ÅMo Kα radiation
b = 13.7249 (6) ŵ = 0.61 mm1
c = 16.1266 (6) ÅT = 120 K
α = 78.605 (4)°0.26 × 0.11 × 0.04 mm
β = 88.106 (3)°
Data collection top
Kuma KM-4-CCD κ-geometry
diffractometer
7322 independent reflections
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2005)
6247 reflections with I > 2σ(I)
Tmin = 0.787, Tmax = 0.944Rint = 0.025
13393 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0350 restraints
wR(F2) = 0.095H-atom parameters constrained
S = 1.08Δρmax = 0.39 e Å3
7322 reflectionsΔρmin = 0.31 e Å3
482 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.

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)
Co10.56482 (3)0.444200 (19)0.684482 (17)0.02391 (9)
S10.74076 (6)0.39705 (4)0.78226 (3)0.02890 (13)
S20.58041 (6)0.58892 (4)0.58700 (3)0.02917 (13)
Si10.72768 (6)0.24453 (4)0.81741 (3)0.02232 (13)
Si20.56792 (6)0.69859 (4)0.66132 (3)0.02210 (13)
O10.82101 (15)0.19001 (11)0.90026 (9)0.0288 (3)
O20.78130 (14)0.18079 (10)0.74373 (9)0.0251 (3)
O30.56257 (15)0.23304 (10)0.83043 (10)0.0288 (3)
O40.67436 (16)0.65534 (10)0.73988 (9)0.0292 (3)
O50.60382 (15)0.80487 (10)0.60540 (9)0.0270 (3)
O60.41524 (15)0.72489 (10)0.70317 (9)0.0267 (3)
C10.8376 (2)0.21322 (18)0.98232 (14)0.0361 (5)
C20.9411 (5)0.2897 (4)0.9685 (3)0.0587 (14)0.660 (5)
H2A1.02880.260.9460.088*0.660 (5)
H2B0.95850.30821.02240.088*0.660 (5)
H2C0.90210.34960.92810.088*0.660 (5)
C30.8864 (7)0.1205 (4)1.0388 (3)0.0640 (17)0.660 (5)
H3A0.81730.07421.04190.096*0.660 (5)
H3B0.90.13371.09530.096*0.660 (5)
H3C0.9750.09041.01760.096*0.660 (5)
C40.6966 (4)0.2650 (3)1.0095 (2)0.0449 (12)0.660 (5)
H4A0.66480.32410.96620.067*0.660 (5)
H4B0.70750.28571.06340.067*0.660 (5)
H4C0.62790.2181.01620.067*0.660 (5)
C2A0.9997 (8)0.1834 (7)1.0065 (5)0.051 (2)0.340 (5)
H2D1.01180.18481.06630.077*0.340 (5)
H2E1.05390.23130.97150.077*0.340 (5)
H2F1.03230.11570.99650.077*0.340 (5)
C3A0.7689 (12)0.1315 (7)1.0487 (4)0.051 (3)0.340 (5)
H3D0.80010.06471.03660.076*0.340 (5)
H3E0.66720.14611.04440.076*0.340 (5)
H3F0.79730.13361.10610.076*0.340 (5)
C4A0.7904 (10)0.3121 (6)0.9995 (5)0.047 (2)0.340 (5)
H4D0.80980.31291.05860.071*0.340 (5)
H4E0.68990.32890.98940.071*0.340 (5)
H4F0.83960.36150.96220.071*0.340 (5)
C50.9195 (2)0.13754 (17)0.72242 (13)0.0309 (5)
C60.9139 (2)0.13352 (18)0.62931 (14)0.0357 (5)
H6A0.83480.10030.61930.054*
H6B1.00060.09580.61280.054*
H6C0.90280.20190.59570.054*
C71.0277 (3)0.2022 (3)0.7361 (2)0.0624 (9)
H7A1.00330.27010.70270.094*
H7B1.11940.17310.71830.094*
H7C1.03030.20540.79620.094*
C80.9478 (4)0.0324 (2)0.77527 (19)0.0713 (11)
H8A0.94120.03580.83540.107*
H8B1.04150.00150.76260.107*
H8C0.87890.00790.76190.107*
C90.4871 (2)0.14759 (16)0.84083 (14)0.0306 (5)
C100.5736 (3)0.05220 (17)0.88649 (17)0.0406 (6)
H10A0.65910.03840.85420.061*
H10B0.51970.0040.89180.061*
H10C0.59770.06070.94290.061*
C110.4473 (3)0.1358 (2)0.75355 (17)0.0471 (6)
H11A0.39520.19880.72390.071*
H11B0.38910.0820.7590.071*
H11C0.53180.11880.72140.071*
C120.3577 (3)0.1741 (2)0.89199 (19)0.0470 (6)
H12A0.38530.1840.94730.071*
H12B0.30070.11940.89990.071*
H12C0.30350.2360.86180.071*
C130.6934 (2)0.68762 (16)0.81831 (13)0.0315 (5)
C140.8372 (3)0.6369 (2)0.84889 (17)0.0460 (6)
H14A0.84170.5640.85490.069*
H14B0.85530.65290.90380.069*
H14C0.90760.66080.80780.069*
C150.6850 (3)0.80104 (19)0.80386 (17)0.0537 (7)
H15A0.7550.82320.76170.081*
H15B0.70270.8210.85720.081*
H15C0.59190.83210.78340.081*
C160.5838 (3)0.6502 (2)0.88057 (16)0.0526 (7)
H16A0.4910.6780.85760.079*
H16B0.5950.67160.93420.079*
H16C0.59430.57680.89030.079*
C170.7164 (2)0.82932 (17)0.54831 (14)0.0324 (5)
C180.6719 (3)0.82716 (18)0.45958 (14)0.0353 (5)
H18A0.65820.75870.45620.053*
H18B0.74430.84910.41920.053*
H18C0.58450.87230.4460.053*
C190.7370 (3)0.9354 (2)0.55490 (17)0.0538 (8)
H19A0.64990.98070.54060.081*
H19B0.81060.95760.51550.081*
H19C0.76390.93620.61280.081*
C200.8493 (3)0.7557 (2)0.57218 (17)0.0497 (7)
H20A0.87560.75660.63020.075*
H20B0.92470.77540.53330.075*
H20C0.83270.68790.56840.075*
C210.2913 (2)0.79131 (16)0.67126 (13)0.0281 (4)
C220.1732 (2)0.75394 (18)0.72733 (15)0.0366 (5)
H22A0.16110.68680.71910.055*
H22B0.08690.79990.71240.055*
H22C0.19550.7510.78670.055*
C230.3091 (3)0.89734 (16)0.68011 (16)0.0384 (5)
H23A0.32480.89840.73960.058*
H23B0.22470.94330.66030.058*
H23C0.38920.91850.64610.058*
C240.2664 (2)0.78670 (19)0.57969 (14)0.0376 (5)
H24A0.34410.81020.54460.056*
H24B0.17940.82960.56010.056*
H24C0.25960.71730.57530.056*
N10.5957 (2)0.33782 (13)0.60817 (12)0.0359 (4)
H1A0.57760.27760.63840.043*
H1B0.68560.3320.58960.043*
H1C0.53750.35720.5630.043*
N20.3802 (2)0.44899 (16)0.75423 (15)0.0262 (7)0.736 (5)
C250.3889 (6)0.4540 (3)0.8362 (3)0.0312 (9)0.736 (5)
H250.4790.45120.85880.037*0.736 (5)
C260.2760 (6)0.4629 (4)0.8896 (4)0.0490 (13)0.736 (5)
H260.28750.46620.94720.059*0.736 (5)
C270.1466 (4)0.4668 (3)0.8566 (3)0.0498 (11)0.736 (5)
H270.06570.4730.8910.06*0.736 (5)
C280.1354 (6)0.4615 (5)0.7723 (4)0.0406 (13)0.736 (5)
H280.04610.46340.74910.049*0.736 (5)
C290.2525 (4)0.4534 (2)0.7215 (3)0.0328 (9)0.736 (5)
C300.2485 (5)0.4491 (4)0.6297 (4)0.0450 (12)0.736 (5)
H30A0.32270.48550.60.059*0.736 (5)
H30B0.27080.37810.62390.059*0.736 (5)
C310.1151 (5)0.4913 (6)0.5867 (4)0.0664 (15)0.736 (5)
H31A0.04180.45260.61240.1*0.736 (5)
H31B0.12420.4880.52660.1*0.736 (5)
H31C0.09080.56140.59260.1*0.736 (5)
N2A0.3486 (7)0.4540 (4)0.6852 (4)0.0206 (18)*0.264 (5)
C25A0.2872 (14)0.4509 (10)0.6126 (9)0.031 (3)*0.264 (5)
H25A0.34420.44230.56480.037*0.264 (5)
C26A0.149 (2)0.4594 (11)0.6048 (11)0.051 (4)*0.264 (5)
H26A0.11090.45880.55160.062*0.264 (5)
C27A0.0581 (10)0.4694 (7)0.6754 (6)0.040 (2)*0.264 (5)
H27A0.04050.47760.67060.048*0.264 (5)
C28A0.1219 (19)0.4662 (14)0.7485 (10)0.029 (4)*0.264 (5)
H28A0.06760.46660.79860.035*0.264 (5)
C29A0.2690 (11)0.4623 (7)0.7529 (6)0.020 (3)*0.264 (5)
C30A0.3392 (15)0.4674 (12)0.8331 (11)0.042 (4)*0.264 (5)
H30C0.40090.4030.85080.055*0.264 (5)
H30D0.40010.52060.81940.055*0.264 (5)
C31A0.2567 (19)0.4856 (13)0.9038 (11)0.046 (5)*0.264 (5)
H31D0.19690.55030.88890.069*0.264 (5)
H31E0.31740.48720.95080.069*0.264 (5)
H31F0.19860.43210.92080.069*0.264 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02190 (15)0.01971 (15)0.03067 (17)0.00157 (10)0.00152 (11)0.00691 (11)
S10.0379 (3)0.0223 (3)0.0276 (3)0.0090 (2)0.0064 (2)0.0031 (2)
S20.0435 (3)0.0208 (2)0.0240 (3)0.0019 (2)0.0099 (2)0.0064 (2)
Si10.0244 (3)0.0205 (3)0.0218 (3)0.0026 (2)0.0007 (2)0.0038 (2)
Si20.0280 (3)0.0184 (3)0.0206 (3)0.0045 (2)0.0045 (2)0.0038 (2)
O10.0353 (8)0.0297 (8)0.0192 (7)0.0039 (6)0.0014 (6)0.0052 (6)
O20.0241 (7)0.0270 (7)0.0245 (7)0.0018 (6)0.0008 (6)0.0072 (6)
O30.0263 (8)0.0215 (7)0.0388 (9)0.0037 (6)0.0028 (6)0.0062 (6)
O40.0370 (8)0.0263 (7)0.0256 (8)0.0024 (6)0.0095 (6)0.0077 (6)
O50.0337 (8)0.0227 (7)0.0258 (7)0.0078 (6)0.0021 (6)0.0050 (6)
O60.0288 (8)0.0256 (7)0.0247 (7)0.0037 (6)0.0031 (6)0.0017 (6)
C10.0408 (13)0.0453 (13)0.0243 (11)0.0008 (10)0.0040 (10)0.0147 (10)
C20.052 (3)0.084 (3)0.049 (3)0.010 (2)0.019 (2)0.032 (2)
C30.097 (5)0.060 (3)0.025 (2)0.029 (3)0.021 (2)0.0079 (19)
C40.048 (2)0.060 (3)0.0267 (19)0.008 (2)0.0018 (17)0.0206 (18)
C2A0.045 (5)0.073 (6)0.044 (5)0.013 (4)0.009 (4)0.025 (4)
C3A0.078 (7)0.060 (5)0.018 (4)0.033 (5)0.000 (4)0.004 (3)
C4A0.070 (6)0.046 (4)0.023 (4)0.002 (4)0.004 (4)0.007 (3)
C50.0271 (11)0.0400 (12)0.0243 (11)0.0043 (9)0.0007 (9)0.0094 (9)
C60.0371 (12)0.0437 (13)0.0288 (12)0.0053 (10)0.0037 (10)0.0135 (10)
C70.0280 (13)0.114 (3)0.0615 (18)0.0116 (15)0.0048 (12)0.0553 (19)
C80.077 (2)0.0646 (19)0.0452 (17)0.0444 (17)0.0192 (15)0.0118 (14)
C90.0294 (11)0.0270 (11)0.0372 (12)0.0096 (9)0.0029 (9)0.0070 (9)
C100.0467 (14)0.0264 (11)0.0468 (15)0.0097 (10)0.0034 (11)0.0003 (10)
C110.0474 (15)0.0544 (16)0.0437 (15)0.0214 (12)0.0039 (12)0.0089 (12)
C120.0364 (13)0.0441 (14)0.0630 (18)0.0132 (11)0.0158 (12)0.0131 (13)
C130.0413 (13)0.0319 (11)0.0241 (11)0.0065 (9)0.0114 (9)0.0093 (9)
C140.0458 (15)0.0498 (15)0.0453 (15)0.0065 (12)0.0207 (12)0.0133 (12)
C150.089 (2)0.0349 (13)0.0416 (15)0.0073 (13)0.0243 (14)0.0144 (11)
C160.0556 (17)0.079 (2)0.0275 (13)0.0196 (15)0.0058 (11)0.0134 (13)
C170.0364 (12)0.0371 (12)0.0266 (11)0.0181 (10)0.0026 (9)0.0042 (9)
C180.0405 (13)0.0389 (12)0.0277 (12)0.0119 (10)0.0010 (10)0.0052 (10)
C190.085 (2)0.0494 (16)0.0372 (14)0.0435 (15)0.0105 (14)0.0105 (12)
C200.0303 (13)0.0724 (19)0.0436 (15)0.0147 (12)0.0009 (11)0.0009 (13)
C210.0276 (11)0.0297 (11)0.0257 (11)0.0006 (9)0.0027 (8)0.0044 (9)
C220.0326 (12)0.0446 (13)0.0330 (12)0.0068 (10)0.0025 (10)0.0079 (10)
C230.0399 (13)0.0273 (11)0.0465 (14)0.0006 (10)0.0004 (11)0.0076 (10)
C240.0344 (12)0.0472 (14)0.0279 (12)0.0034 (10)0.0069 (9)0.0044 (10)
N10.0492 (12)0.0247 (9)0.0327 (10)0.0067 (8)0.0174 (9)0.0085 (8)
N20.0260 (14)0.0200 (12)0.0311 (15)0.0000 (9)0.0013 (10)0.0031 (10)
C250.036 (2)0.0311 (19)0.0241 (18)0.0022 (19)0.0007 (18)0.0054 (13)
C260.053 (3)0.045 (3)0.039 (3)0.015 (2)0.001 (2)0.000 (2)
C270.042 (2)0.043 (2)0.054 (2)0.0097 (16)0.0165 (17)0.0024 (17)
C280.024 (2)0.038 (2)0.056 (4)0.0007 (15)0.002 (3)0.004 (3)
C290.0278 (19)0.0229 (16)0.048 (2)0.0002 (12)0.0069 (17)0.0090 (16)
C300.026 (3)0.060 (3)0.053 (3)0.009 (2)0.015 (2)0.028 (2)
C310.038 (3)0.092 (4)0.068 (3)0.004 (3)0.017 (2)0.020 (3)
Geometric parameters (Å, º) top
Co1—N12.0730 (17)C14—H14A0.98
Co1—N2A2.081 (6)C14—H14B0.98
Co1—N22.082 (2)C14—H14C0.98
Co1—S12.2967 (6)C15—H15A0.98
Co1—S22.2968 (6)C15—H15B0.98
S1—Si12.0787 (7)C15—H15C0.98
S2—Si22.0899 (7)C16—H16A0.98
Si1—O11.6298 (15)C16—H16B0.98
Si1—O31.6332 (15)C16—H16C0.98
Si1—O21.6395 (14)C17—C181.515 (3)
Si2—O41.6240 (15)C17—C191.522 (3)
Si2—O61.6293 (15)C17—C201.529 (4)
Si2—O51.6328 (14)C18—H18A0.98
O1—C11.440 (2)C18—H18B0.98
O2—C51.446 (2)C18—H18C0.98
O3—C91.448 (2)C19—H19A0.98
O4—C131.446 (2)C19—H19B0.98
O5—C171.438 (3)C19—H19C0.98
O6—C211.444 (2)C20—H20A0.98
C1—C31.440 (5)C20—H20B0.98
C1—C4A1.447 (8)C20—H20C0.98
C1—C21.532 (5)C21—C221.518 (3)
C1—C41.540 (4)C21—C241.519 (3)
C1—C3A1.593 (8)C21—C231.524 (3)
C1—C2A1.608 (8)C22—H22A0.98
C2—H2A0.98C22—H22B0.98
C2—H2B0.98C22—H22C0.98
C2—H2C0.98C23—H23A0.98
C3—H3A0.98C23—H23B0.98
C3—H3B0.98C23—H23C0.98
C3—H3C0.98C24—H24A0.98
C4—H4A0.98C24—H24B0.98
C4—H4B0.98C24—H24C0.98
C4—H4C0.98N1—H1A0.91
C2A—H2D0.98N1—H1B0.91
C2A—H2E0.98N1—H1C0.91
C2A—H2F0.98N2—C251.343 (5)
C3A—H3D0.98N2—C291.350 (5)
C3A—H3E0.98C25—C261.377 (7)
C3A—H3F0.98C25—H250.95
C4A—H4D0.98C26—C271.369 (7)
C4A—H4E0.98C26—H260.95
C4A—H4F0.98C27—C281.384 (8)
C5—C71.514 (4)C27—H270.95
C5—C81.516 (4)C28—C291.382 (7)
C5—C61.516 (3)C28—H280.95
C6—H6A0.98C29—C301.496 (7)
C6—H6B0.98C30—C311.475 (6)
C6—H6C0.98C30—H30A0.99
C7—H7A0.98C30—H30B0.99
C7—H7B0.98C31—H31A0.98
C7—H7C0.98C31—H31B0.98
C8—H8A0.98C31—H31C0.98
C8—H8B0.98N2A—C29A1.330 (12)
C8—H8C0.98N2A—C25A1.343 (17)
C9—C111.517 (3)C25A—C26A1.33 (2)
C9—C101.519 (3)C25A—H25A0.95
C9—C121.519 (3)C26A—C27A1.434 (19)
C10—H10A0.98C26A—H26A0.95
C10—H10B0.98C27A—C28A1.340 (19)
C10—H10C0.98C27A—H27A0.95
C11—H11A0.98C28A—C29A1.42 (2)
C11—H11B0.98C28A—H28A0.95
C11—H11C0.98C29A—C30A1.50 (2)
C12—H12A0.98C30A—C31A1.41 (2)
C12—H12B0.98C30A—H30C0.99
C12—H12C0.98C30A—H30D0.99
C13—C161.511 (4)C31A—H31D0.98
C13—C141.518 (3)C31A—H31E0.98
C13—C151.519 (3)C31A—H31F0.98
N1—Co1—N2A94.65 (18)C13—C14—H14A109.5
N1—Co1—N2116.09 (9)C13—C14—H14B109.5
N2A—Co1—N232.07 (18)H14A—C14—H14B109.5
N1—Co1—S1104.82 (5)C13—C14—H14C109.5
N2A—Co1—S1136.83 (17)H14A—C14—H14C109.5
N2—Co1—S1105.70 (7)H14B—C14—H14C109.5
N1—Co1—S2101.12 (6)C13—C15—H15A109.5
N2A—Co1—S297.03 (17)C13—C15—H15B109.5
N2—Co1—S2113.31 (6)H15A—C15—H15B109.5
S1—Co1—S2115.85 (2)C13—C15—H15C109.5
Si1—S1—Co1100.10 (3)H15A—C15—H15C109.5
Si2—S2—Co1103.26 (3)H15B—C15—H15C109.5
O1—Si1—O3112.92 (8)C13—C16—H16A109.5
O1—Si1—O2105.15 (7)C13—C16—H16B109.5
O3—Si1—O2104.91 (8)H16A—C16—H16B109.5
O1—Si1—S1113.09 (6)C13—C16—H16C109.5
O3—Si1—S1107.06 (6)H16A—C16—H16C109.5
O2—Si1—S1113.54 (6)H16B—C16—H16C109.5
O4—Si2—O6106.16 (8)O5—C17—C18108.30 (17)
O4—Si2—O5112.39 (8)O5—C17—C19105.48 (18)
O6—Si2—O5105.35 (7)C18—C17—C19110.2 (2)
O4—Si2—S2107.19 (6)O5—C17—C20111.37 (18)
O6—Si2—S2114.89 (6)C18—C17—C20110.3 (2)
O5—Si2—S2110.89 (6)C19—C17—C20111.1 (2)
C1—O1—Si1134.13 (13)C17—C18—H18A109.5
C5—O2—Si1130.97 (13)C17—C18—H18B109.5
C9—O3—Si1132.79 (13)H18A—C18—H18B109.5
C13—O4—Si2132.73 (13)C17—C18—H18C109.5
C17—O5—Si2132.12 (13)H18A—C18—H18C109.5
C21—O6—Si2132.54 (13)H18B—C18—H18C109.5
C3—C1—O1107.3 (2)C17—C19—H19A109.5
C3—C1—C4A130.5 (4)C17—C19—H19B109.5
O1—C1—C4A121.5 (3)H19A—C19—H19B109.5
C3—C1—C2114.2 (4)C17—C19—H19C109.5
O1—C1—C2105.0 (2)H19A—C19—H19C109.5
C4A—C1—C262.1 (4)H19B—C19—H19C109.5
C3—C1—C4113.2 (3)C17—C20—H20A109.5
O1—C1—C4108.3 (2)C17—C20—H20B109.5
C2—C1—C4108.3 (3)H20A—C20—H20B109.5
O1—C1—C3A106.4 (3)C17—C20—H20C109.5
C4A—C1—C3A109.6 (5)H20A—C20—H20C109.5
C2—C1—C3A146.3 (4)H20B—C20—H20C109.5
O1—C1—C2A107.3 (3)O6—C21—C22105.35 (17)
C4A—C1—C2A108.7 (5)O6—C21—C24110.69 (17)
C4—C1—C2A144.1 (3)C22—C21—C24110.61 (18)
C3A—C1—C2A101.4 (5)O6—C21—C23108.24 (17)
C1—C2—H2A109.5C22—C21—C23110.73 (18)
C1—C2—H2B109.5C24—C21—C23111.06 (19)
C1—C2—H2C109.5C21—C22—H22A109.5
C1—C3—H3A109.5C21—C22—H22B109.5
C1—C3—H3B109.5H22A—C22—H22B109.5
C1—C3—H3C109.5C21—C22—H22C109.5
C1—C4—H4A109.5H22A—C22—H22C109.5
C1—C4—H4B109.5H22B—C22—H22C109.5
C1—C4—H4C109.5C21—C23—H23A109.5
C1—C2A—H2D109.5C21—C23—H23B109.5
C1—C2A—H2E109.5H23A—C23—H23B109.5
H2D—C2A—H2E109.5C21—C23—H23C109.5
C1—C2A—H2F109.5H23A—C23—H23C109.5
H2D—C2A—H2F109.5H23B—C23—H23C109.5
H2E—C2A—H2F109.5C21—C24—H24A109.5
C1—C3A—H3D109.5C21—C24—H24B109.5
C1—C3A—H3E109.5H24A—C24—H24B109.5
H3D—C3A—H3E109.5C21—C24—H24C109.5
C1—C3A—H3F109.5H24A—C24—H24C109.5
H3D—C3A—H3F109.5H24B—C24—H24C109.5
H3E—C3A—H3F109.5Co1—N1—H1A109.5
C1—C4A—H4D109.5Co1—N1—H1B109.5
C1—C4A—H4E109.5H1A—N1—H1B109.5
H4D—C4A—H4E109.5Co1—N1—H1C109.5
C1—C4A—H4F109.5H1A—N1—H1C109.5
H4D—C4A—H4F109.5H1B—N1—H1C109.5
H4E—C4A—H4F109.5C25—N2—C29118.2 (4)
O2—C5—C7111.27 (18)C25—N2—Co1117.2 (3)
O2—C5—C8107.68 (19)C29—N2—Co1124.5 (2)
C7—C5—C8112.2 (3)N2—C25—C26124.4 (5)
O2—C5—C6105.45 (17)N2—C25—H25117.8
C7—C5—C6109.6 (2)C26—C25—H25117.8
C8—C5—C6110.4 (2)C27—C26—C25117.5 (5)
C5—C6—H6A109.5C27—C26—H26121.3
C5—C6—H6B109.5C25—C26—H26121.3
H6A—C6—H6B109.5C26—C27—C28119.1 (4)
C5—C6—H6C109.5C26—C27—H27120.5
H6A—C6—H6C109.5C28—C27—H27120.5
H6B—C6—H6C109.5C29—C28—C27120.9 (5)
C5—C7—H7A109.5C29—C28—H28119.6
C5—C7—H7B109.5C27—C28—H28119.6
H7A—C7—H7B109.5N2—C29—C28120.1 (5)
C5—C7—H7C109.5N2—C29—C30116.0 (4)
H7A—C7—H7C109.5C28—C29—C30123.9 (5)
H7B—C7—H7C109.5C31—C30—C29115.6 (4)
C5—C8—H8A109.5C31—C30—H30A108.4
C5—C8—H8B109.5C29—C30—H30A108.4
H8A—C8—H8B109.5C31—C30—H30B108.4
C5—C8—H8C109.5C29—C30—H30B108.4
H8A—C8—H8C109.5H30A—C30—H30B107.5
H8B—C8—H8C109.5C29A—N2A—C25A118.7 (9)
O3—C9—C11107.79 (18)C29A—N2A—Co1124.1 (6)
O3—C9—C10111.75 (18)C25A—N2A—Co1117.2 (7)
C11—C9—C10110.4 (2)C26A—C25A—N2A122.5 (13)
O3—C9—C12105.68 (17)C26A—C25A—H25A118.7
C11—C9—C12110.5 (2)N2A—C25A—H25A118.7
C10—C9—C12110.6 (2)C25A—C26A—C27A121.3 (15)
C9—C10—H10A109.5C25A—C26A—H26A119.3
C9—C10—H10B109.5C27A—C26A—H26A119.3
H10A—C10—H10B109.5C28A—C27A—C26A115.1 (13)
C9—C10—H10C109.5C28A—C27A—H27A122.4
H10A—C10—H10C109.5C26A—C27A—H27A122.4
H10B—C10—H10C109.5C27A—C28A—C29A121.6 (15)
C9—C11—H11A109.5C27A—C28A—H28A119.2
C9—C11—H11B109.5C29A—C28A—H28A119.2
H11A—C11—H11B109.5N2A—C29A—C28A120.5 (11)
C9—C11—H11C109.5N2A—C29A—C30A117.9 (10)
H11A—C11—H11C109.5C28A—C29A—C30A121.6 (11)
H11B—C11—H11C109.5C31A—C30A—C29A119.3 (13)
C9—C12—H12A109.5C31A—C30A—H30C107.5
C9—C12—H12B109.5C29A—C30A—H30C107.5
H12A—C12—H12B109.5C31A—C30A—H30D107.5
C9—C12—H12C109.5C29A—C30A—H30D107.5
H12A—C12—H12C109.5H30C—C30A—H30D107
H12B—C12—H12C109.5C30A—C31A—H31D109.5
O4—C13—C16108.31 (18)C30A—C31A—H31E109.5
O4—C13—C14105.12 (18)H31D—C31A—H31E109.5
C16—C13—C14110.0 (2)C30A—C31A—H31F109.5
O4—C13—C15110.79 (18)H31D—C31A—H31F109.5
C16—C13—C15111.4 (2)H31E—C31A—H31F109.5
C14—C13—C15111.0 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···S2i0.912.633.5283 (19)168
Symmetry code: (i) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Co(C12H27O3SSi)2(C7H9N)(NH3)]
Mr742.09
Crystal system, space groupTriclinic, P1
Temperature (K)120
a, b, c (Å)9.6939 (4), 13.7249 (6), 16.1266 (6)
α, β, γ (°)78.605 (4), 88.106 (3), 81.830 (4)
V3)2081.94 (15)
Z2
Radiation typeMo Kα
µ (mm1)0.61
Crystal size (mm)0.26 × 0.11 × 0.04
Data collection
DiffractometerKuma KM-4-CCD κ-geometry
Absorption correctionAnalytical
(CrysAlis RED; Oxford Diffraction, 2005)
Tmin, Tmax0.787, 0.944
No. of measured, independent and
observed [I > 2σ(I)] reflections
13393, 7322, 6247
Rint0.025
(sin θ/λ)max1)0.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.035, 0.095, 1.08
No. of reflections7322
No. of parameters482
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.39, 0.31

Computer programs: CrysAlis CCD (Oxford Diffraction, 2005), CrysAlis RED (Oxford Diffraction, 2005), CrysAlis RED, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···S2i0.912.633.5283 (19)168
Symmetry code: (i) x+1, y+1, z+1.
 

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