metal-organic compounds
(−)545-fac-Δ-Tris(L-prolinato)cobalt(III) trihydrate
aDepartment of Chemistry, Graduate School of Science and Engineering, Saitama University, Shimo-Okubo 255, Sakura-ku, Saitama 338-8570, Japan, and bMolecular Analysis and Life Science Center, Saitama University, Shimo-Okubo 255, Sakura-ku, Saitama 338-8570, Japan
*Correspondence e-mail: fuji@chem.saitama-u.ac.jp
The fac-CoN3O3 title complex, [Co(C5H8NO2)3]·3H2O, has been determined by single-crystal X-ray analysis. A three-dimensional network of hydrogen bonds is observed between the proline carboxylate groups and the three uncoordinated water molecules.
of the octahedralExperimental
Crystal data
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Data collection: SMART-W2K/NT (Bruker, 2003); cell SAINT-W2K/NT (Bruker, 2003); data reduction: SAINT-W2K/NT; program(s) used to solve structure: SHELXTL-NT (Sheldrick, 2008); program(s) used to refine structure: SHELXTL-NT; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL-NT.
Supporting information
10.1107/S1600536808010246/tk2254sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536808010246/tk2254Isup2.hkl
The title compound was prepared according to the literature method (Denning & Piper, 1965). Single crystals suitable for single-crystal X-ray analysis were obtained by vapor diffusion of ethanol into the aqueous solution of (I) at room temperature. Analysis found: C 39.59, H 6.58, N 9.10; C15H30CoN3O9 C29H34F6O2S2 requires: C 39.57, H 6.64, N 9.23.
The water- and N-bound H atoms were located in difference maps and refined with Uiso(H) = 1.5Ueq(O) or 1.5Ueq(N); see Table 1 for O-H and N-H bond distances. The remaining H atoms were placed in calculated positions, with C—H = 1.00 Å (for CH) and 0.99 Å (for CH2) and refined using a riding model, with Uiso(H) = 1.2Ueq(C).
Data collection: SMART-W2K/NT (Bruker, 2003); cell
SAINT-W2K/NT (Bruker, 2003); data reduction: SAINT-W2K/NT (Bruker, 2003); program(s) used to solve structure: SHELXTL-NT (Bruker, 2003); program(s) used to refine structure: SHELXTL-NT (Bruker, 2003); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL-NT (Bruker, 2003).[Co(C5H8NO2)3]·3H2O | F(000) = 960 |
Mr = 455.35 | Dx = 1.594 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 705 reflections |
a = 10.1673 (9) Å | θ = 2.2–17.1° |
b = 10.8433 (10) Å | µ = 0.96 mm−1 |
c = 17.2157 (14) Å | T = 173 K |
V = 1898.0 (3) Å3 | Block, pink |
Z = 4 | 0.13 × 0.08 × 0.07 mm |
Bruker SMART APEX CCD area-detector diffractometer | 4522 independent reflections |
Radiation source: fine-focus sealed tube | 2969 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.122 |
Detector resolution: 8.366 pixels mm-1 | θmax = 27.9°, θmin = 2.2° |
ϕ and ω scans | h = −13→7 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −14→14 |
Tmin = 0.885, Tmax = 0.936 | l = −22→22 |
13762 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.062 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.107 | w = 1/[σ2(Fo2) + (0.0283P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max < 0.001 |
4522 reflections | Δρmax = 0.85 e Å−3 |
274 parameters | Δρmin = −0.51 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 2596 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.04 (2) |
[Co(C5H8NO2)3]·3H2O | V = 1898.0 (3) Å3 |
Mr = 455.35 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 10.1673 (9) Å | µ = 0.96 mm−1 |
b = 10.8433 (10) Å | T = 173 K |
c = 17.2157 (14) Å | 0.13 × 0.08 × 0.07 mm |
Bruker SMART APEX CCD area-detector diffractometer | 4522 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2969 reflections with I > 2σ(I) |
Tmin = 0.885, Tmax = 0.936 | Rint = 0.122 |
13762 measured reflections |
R[F2 > 2σ(F2)] = 0.062 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.107 | Δρmax = 0.85 e Å−3 |
S = 0.92 | Δρmin = −0.51 e Å−3 |
4522 reflections | Absolute structure: Flack (1983), 2596 Friedel pairs |
274 parameters | Absolute structure parameter: 0.04 (2) |
0 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.3689 (5) | 0.9795 (5) | 0.1401 (3) | 0.0220 (11) | |
H1A | 0.4364 | 0.9396 | 0.1063 | 0.026* | |
C2 | 0.4210 (5) | 1.1046 (5) | 0.1661 (3) | 0.0309 (15) | |
H2A | 0.3940 | 1.1230 | 0.2201 | 0.037* | |
H2B | 0.5182 | 1.1074 | 0.1627 | 0.037* | |
C3 | 0.3589 (5) | 1.1948 (4) | 0.1093 (3) | 0.0248 (11) | |
H3A | 0.3561 | 1.2794 | 0.1309 | 0.030* | |
H3B | 0.4062 | 1.1958 | 0.0591 | 0.030* | |
C4 | 0.2218 (5) | 1.1408 (5) | 0.1008 (3) | 0.0251 (12) | |
H4A | 0.1678 | 1.1576 | 0.1475 | 0.030* | |
H4B | 0.1766 | 1.1749 | 0.0546 | 0.030* | |
C5 | 0.3343 (5) | 0.8910 (5) | 0.2056 (3) | 0.0216 (12) | |
C6 | 0.0485 (5) | 0.7863 (5) | −0.0354 (3) | 0.0168 (11) | |
H6A | −0.0194 | 0.7199 | −0.0309 | 0.020* | |
C7 | 0.0427 (5) | 0.8403 (5) | −0.1185 (3) | 0.0226 (12) | |
H7A | 0.1316 | 0.8630 | −0.1372 | 0.027* | |
H7B | 0.0029 | 0.7809 | −0.1553 | 0.027* | |
C8 | −0.0437 (5) | 0.9539 (4) | −0.1089 (3) | 0.0223 (11) | |
H8A | −0.0286 | 1.0141 | −0.1512 | 0.027* | |
H8B | −0.1381 | 0.9316 | −0.1074 | 0.027* | |
C9 | 0.0024 (5) | 1.0038 (5) | −0.0315 (3) | 0.0213 (12) | |
H9A | 0.0893 | 1.0442 | −0.0364 | 0.026* | |
H9B | −0.0614 | 1.0637 | −0.0101 | 0.026* | |
C10 | 0.1804 (5) | 0.7331 (5) | −0.0136 (3) | 0.0172 (11) | |
C11 | −0.0584 (5) | 0.8563 (5) | 0.2340 (3) | 0.0208 (12) | |
H11A | −0.0041 | 0.8448 | 0.2819 | 0.025* | |
C12 | −0.1937 (5) | 0.9052 (5) | 0.2579 (3) | 0.0311 (15) | |
H12A | −0.2643 | 0.8598 | 0.2305 | 0.037* | |
H12B | −0.2069 | 0.8960 | 0.3146 | 0.037* | |
C13 | −0.1946 (5) | 1.0400 (5) | 0.2351 (3) | 0.0258 (13) | |
H13A | −0.1594 | 1.0925 | 0.2773 | 0.031* | |
H13B | −0.2844 | 1.0681 | 0.2216 | 0.031* | |
C14 | −0.1050 (5) | 1.0419 (5) | 0.1647 (3) | 0.0205 (12) | |
H14A | −0.1523 | 1.0132 | 0.1178 | 0.025* | |
H14B | −0.0710 | 1.1261 | 0.1551 | 0.025* | |
C15 | −0.0597 (5) | 0.7356 (5) | 0.1891 (3) | 0.0180 (11) | |
Co1 | 0.12024 (6) | 0.87354 (6) | 0.11104 (3) | 0.01537 (16) | |
N1 | 0.2469 (4) | 1.0046 (4) | 0.0916 (2) | 0.0190 (10) | |
H1C | 0.2698 | 0.9957 | 0.0470 | 0.023* | |
N2 | 0.0110 (4) | 0.8912 (4) | 0.01862 (19) | 0.0144 (9) | |
H2C | −0.070 | 0.8757 | 0.0338 | 0.017* | |
N3 | 0.0039 (4) | 0.9561 (4) | 0.1851 (2) | 0.0194 (11) | |
H3C | 0.0460 | 0.9900 | 0.2108 | 0.023* | |
O1 | 0.2224 (3) | 0.8373 (3) | 0.20056 (17) | 0.0198 (9) | |
O2 | 0.4133 (3) | 0.8715 (4) | 0.25896 (18) | 0.0321 (9) | |
O3 | 0.2340 (3) | 0.7768 (3) | 0.04792 (18) | 0.0182 (8) | |
O4 | 0.2308 (3) | 0.6524 (3) | −0.05483 (18) | 0.0275 (9) | |
O5 | 0.0152 (3) | 0.7314 (3) | 0.12902 (16) | 0.0189 (8) | |
O6 | −0.1273 (4) | 0.6473 (3) | 0.21062 (17) | 0.0246 (8) | |
O7 | 0.1135 (5) | 0.9744 (5) | 0.4313 (3) | 0.0419 (12) | |
H7C | 0.096 (6) | 1.024 (6) | 0.392 (4) | 0.063* | |
H7D | 0.051 (7) | 0.966 (8) | 0.442 (4) | 0.063* | |
O8 | 0.2893 (4) | 0.7736 (4) | 0.3961 (2) | 0.0383 (11) | |
H8C | 0.227 (6) | 0.835 (6) | 0.404 (3) | 0.057* | |
H8D | 0.328 (6) | 0.796 (6) | 0.360 (3) | 0.057* | |
O9 | 0.3649 (5) | 0.5837 (4) | 0.5018 (3) | 0.0461 (13) | |
H9C | 0.356 (8) | 0.640 (6) | 0.475 (4) | 0.069* | |
H9D | 0.328 (7) | 0.531 (6) | 0.485 (4) | 0.069* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.016 (3) | 0.027 (3) | 0.023 (2) | −0.002 (3) | 0.002 (2) | −0.003 (2) |
C2 | 0.024 (3) | 0.034 (4) | 0.035 (3) | −0.010 (3) | 0.000 (2) | −0.007 (3) |
C3 | 0.029 (3) | 0.019 (3) | 0.027 (2) | −0.006 (2) | 0.009 (3) | −0.002 (3) |
C4 | 0.031 (3) | 0.019 (3) | 0.025 (3) | 0.003 (3) | 0.006 (2) | −0.004 (3) |
C5 | 0.028 (3) | 0.016 (3) | 0.021 (3) | 0.005 (2) | 0.002 (2) | −0.005 (2) |
C6 | 0.018 (3) | 0.018 (3) | 0.015 (2) | −0.005 (2) | 0.004 (2) | −0.008 (2) |
C7 | 0.024 (3) | 0.035 (3) | 0.009 (2) | −0.001 (2) | −0.001 (2) | −0.002 (2) |
C8 | 0.019 (3) | 0.030 (3) | 0.018 (2) | 0.000 (2) | −0.001 (3) | 0.009 (3) |
C9 | 0.022 (3) | 0.018 (3) | 0.024 (3) | 0.000 (2) | 0.000 (2) | 0.003 (2) |
C10 | 0.015 (3) | 0.017 (3) | 0.019 (3) | −0.002 (2) | 0.007 (2) | −0.001 (2) |
C11 | 0.028 (3) | 0.015 (3) | 0.019 (2) | −0.001 (3) | 0.003 (2) | 0.000 (2) |
C12 | 0.031 (3) | 0.025 (4) | 0.037 (3) | −0.006 (3) | 0.014 (3) | 0.001 (3) |
C13 | 0.018 (3) | 0.029 (3) | 0.030 (3) | 0.000 (3) | 0.004 (2) | −0.003 (3) |
C14 | 0.022 (3) | 0.015 (3) | 0.025 (3) | 0.003 (3) | −0.003 (3) | 0.001 (2) |
C15 | 0.017 (3) | 0.018 (3) | 0.019 (3) | −0.002 (2) | −0.006 (2) | −0.002 (2) |
Co1 | 0.0161 (3) | 0.0153 (3) | 0.0147 (3) | −0.0008 (3) | −0.0009 (3) | −0.0009 (3) |
N1 | 0.020 (2) | 0.019 (2) | 0.018 (2) | 0.0016 (19) | −0.0008 (19) | −0.0008 (17) |
N2 | 0.013 (2) | 0.015 (2) | 0.0159 (19) | 0.0001 (19) | −0.0015 (17) | 0.0004 (18) |
N3 | 0.026 (3) | 0.012 (2) | 0.021 (2) | −0.004 (2) | −0.003 (2) | −0.0027 (18) |
O1 | 0.021 (2) | 0.023 (2) | 0.0158 (17) | 0.0023 (17) | −0.0061 (16) | 0.0040 (15) |
O2 | 0.033 (2) | 0.040 (2) | 0.0236 (18) | 0.001 (2) | −0.0133 (16) | 0.003 (2) |
O3 | 0.0158 (18) | 0.019 (2) | 0.0199 (17) | 0.0037 (16) | −0.0049 (15) | −0.0045 (15) |
O4 | 0.0225 (19) | 0.034 (3) | 0.0261 (19) | 0.0057 (18) | 0.0014 (16) | −0.0104 (18) |
O5 | 0.0215 (18) | 0.016 (2) | 0.0194 (19) | −0.0054 (16) | −0.0042 (15) | −0.0002 (14) |
O6 | 0.0259 (18) | 0.021 (2) | 0.0270 (17) | −0.005 (2) | −0.0014 (17) | 0.0053 (15) |
O7 | 0.041 (3) | 0.046 (3) | 0.039 (2) | 0.009 (3) | −0.003 (3) | 0.0153 (19) |
O8 | 0.049 (3) | 0.034 (3) | 0.032 (2) | −0.001 (2) | 0.002 (2) | 0.004 (2) |
O9 | 0.048 (3) | 0.036 (3) | 0.055 (3) | −0.005 (3) | −0.006 (3) | 0.004 (2) |
C1—N1 | 1.520 (6) | C11—N3 | 1.510 (6) |
C1—C5 | 1.521 (7) | C11—C15 | 1.520 (7) |
C1—C2 | 1.523 (7) | C11—C12 | 1.530 (7) |
C1—H1A | 1.0000 | C11—H11A | 1.0000 |
C2—C3 | 1.520 (7) | C12—C13 | 1.514 (7) |
C2—H2A | 0.9900 | C12—H12A | 0.9900 |
C2—H2B | 0.9900 | C12—H12B | 0.9900 |
C3—C4 | 1.518 (6) | C13—C14 | 1.516 (6) |
C3—H3A | 0.9900 | C13—H13A | 0.9900 |
C3—H3B | 0.9900 | C13—H13B | 0.9900 |
C4—N1 | 1.507 (6) | C14—N3 | 1.488 (6) |
C4—H4A | 0.9900 | C14—H14A | 0.9900 |
C4—H4B | 0.9900 | C14—H14B | 0.9900 |
C5—O2 | 1.238 (5) | C15—O6 | 1.235 (6) |
C5—O1 | 1.282 (6) | C15—O5 | 1.285 (5) |
C6—C10 | 1.508 (6) | Co1—O1 | 1.900 (3) |
C6—N2 | 1.518 (6) | Co1—O5 | 1.900 (3) |
C6—C7 | 1.546 (6) | Co1—O3 | 1.903 (3) |
C6—H6A | 1.0000 | Co1—N1 | 1.947 (4) |
C7—C8 | 1.522 (7) | Co1—N2 | 1.950 (3) |
C7—H7A | 0.9900 | Co1—N3 | 1.956 (4) |
C7—H7B | 0.9900 | N1—H1C | 0.8117 |
C8—C9 | 1.513 (6) | N2—H2C | 0.8806 |
C8—H8A | 0.9900 | N3—H3C | 0.7180 |
C8—H8B | 0.9900 | O7—H7C | 0.88 (6) |
C9—N2 | 1.497 (6) | O7—H7D | 0.66 (7) |
C9—H9A | 0.9900 | O8—H8C | 0.93 (6) |
C9—H9B | 0.9900 | O8—H8D | 0.77 (6) |
C10—O4 | 1.237 (6) | O9—H9C | 0.77 (6) |
C10—O3 | 1.282 (5) | O9—H9D | 0.74 (6) |
N1—C1—C5 | 109.4 (4) | C13—C12—C11 | 105.7 (4) |
N1—C1—C2 | 106.6 (4) | C13—C12—H12A | 110.6 |
C5—C1—C2 | 115.2 (4) | C11—C12—H12A | 110.6 |
N1—C1—H1A | 108.5 | C13—C12—H12B | 110.6 |
C5—C1—H1A | 108.5 | C11—C12—H12B | 110.6 |
C2—C1—H1A | 108.5 | H12A—C12—H12B | 108.7 |
C3—C2—C1 | 103.9 (4) | C12—C13—C14 | 102.5 (4) |
C3—C2—H2A | 111.0 | C12—C13—H13A | 111.3 |
C1—C2—H2A | 111.0 | C14—C13—H13A | 111.3 |
C3—C2—H2B | 111.0 | C12—C13—H13B | 111.3 |
C1—C2—H2B | 111.0 | C14—C13—H13B | 111.3 |
H2A—C2—H2B | 109.0 | H13A—C13—H13B | 109.2 |
C4—C3—C2 | 101.3 (4) | N3—C14—C13 | 104.5 (4) |
C4—C3—H3A | 111.5 | N3—C14—H14A | 110.9 |
C2—C3—H3A | 111.5 | C13—C14—H14A | 110.9 |
C4—C3—H3B | 111.5 | N3—C14—H14B | 110.9 |
C2—C3—H3B | 111.5 | C13—C14—H14B | 110.9 |
H3A—C3—H3B | 109.3 | H14A—C14—H14B | 108.9 |
N1—C4—C3 | 103.5 (4) | O6—C15—O5 | 123.0 (5) |
N1—C4—H4A | 111.1 | O6—C15—C11 | 121.3 (4) |
C3—C4—H4A | 111.1 | O5—C15—C11 | 115.8 (4) |
N1—C4—H4B | 111.1 | O1—Co1—O5 | 90.41 (14) |
C3—C4—H4B | 111.1 | O1—Co1—O3 | 90.97 (14) |
H4A—C4—H4B | 109.0 | O5—Co1—O3 | 89.27 (14) |
O2—C5—O1 | 123.3 (5) | O1—Co1—N1 | 85.92 (15) |
O2—C5—C1 | 120.5 (5) | O5—Co1—N1 | 172.63 (16) |
O1—C5—C1 | 116.2 (4) | O3—Co1—N1 | 84.41 (15) |
C10—C6—N2 | 111.0 (4) | O1—Co1—N2 | 173.64 (17) |
C10—C6—C7 | 114.1 (4) | O5—Co1—N2 | 83.85 (15) |
N2—C6—C7 | 105.9 (4) | O3—Co1—N2 | 86.24 (15) |
C10—C6—H6A | 108.6 | N1—Co1—N2 | 99.48 (16) |
N2—C6—H6A | 108.6 | O1—Co1—N3 | 84.07 (15) |
C7—C6—H6A | 108.6 | O5—Co1—N3 | 85.70 (16) |
C8—C7—C6 | 103.2 (4) | O3—Co1—N3 | 172.90 (16) |
C8—C7—H7A | 111.1 | N1—Co1—N3 | 100.25 (17) |
C6—C7—H7A | 111.1 | N2—Co1—N3 | 98.17 (16) |
C8—C7—H7B | 111.1 | C4—N1—C1 | 104.8 (4) |
C6—C7—H7B | 111.1 | C4—N1—Co1 | 125.9 (3) |
H7A—C7—H7B | 109.1 | C1—N1—Co1 | 108.3 (3) |
C9—C8—C7 | 101.9 (4) | C4—N1—H1C | 105.4 |
C9—C8—H8A | 111.4 | C1—N1—H1C | 105.4 |
C7—C8—H8A | 111.4 | Co1—N1—H1C | 105.4 |
C9—C8—H8B | 111.4 | C9—N2—C6 | 105.8 (3) |
C7—C8—H8B | 111.4 | C9—N2—Co1 | 125.7 (3) |
H8A—C8—H8B | 109.3 | C6—N2—Co1 | 106.5 (3) |
N2—C9—C8 | 103.6 (4) | C9—N2—H2C | 105.8 |
N2—C9—H9A | 111.0 | C6—N2—H2C | 105.8 |
C8—C9—H9A | 111.0 | Co1—N2—H2C | 105.8 |
N2—C9—H9B | 111.0 | C14—N3—C11 | 105.5 (4) |
C8—C9—H9B | 111.0 | C14—N3—Co1 | 125.6 (3) |
H9A—C9—H9B | 109.0 | C11—N3—Co1 | 106.8 (3) |
O4—C10—O3 | 124.0 (5) | C14—N3—H3C | 105.8 |
O4—C10—C6 | 119.8 (5) | C11—N3—H3C | 105.8 |
O3—C10—C6 | 116.2 (4) | Co1—N3—H3C | 105.8 |
N3—C11—C15 | 109.7 (4) | C5—O1—Co1 | 116.5 (3) |
N3—C11—C12 | 106.2 (4) | C10—O3—Co1 | 114.7 (3) |
C15—C11—C12 | 115.3 (4) | C15—O5—Co1 | 115.8 (3) |
N3—C11—H11A | 108.5 | H7C—O7—H7D | 95 (7) |
C15—C11—H11A | 108.5 | H8C—O8—H8D | 104 (6) |
C12—C11—H11A | 108.5 | H9C—O9—H9D | 108 (8) |
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H9D···O4i | 0.74 (6) | 2.19 (7) | 2.907 (6) | 164 (8) |
O8—H8D···O2 | 0.77 (6) | 2.11 (6) | 2.880 (5) | 173 (7) |
O7—H7D···O9ii | 0.66 (7) | 2.20 (6) | 2.848 (7) | 167 (9) |
O9—H9C···O8 | 0.77 (6) | 2.09 (7) | 2.853 (6) | 166 (8) |
O8—H8C···O7 | 0.93 (6) | 1.96 (6) | 2.882 (7) | 172 (5) |
Symmetry codes: (i) −x+1/2, −y+1, z+1/2; (ii) x−1/2, −y+3/2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Co(C5H8NO2)3]·3H2O |
Mr | 455.35 |
Crystal system, space group | Orthorhombic, P212121 |
Temperature (K) | 173 |
a, b, c (Å) | 10.1673 (9), 10.8433 (10), 17.2157 (14) |
V (Å3) | 1898.0 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.96 |
Crystal size (mm) | 0.13 × 0.08 × 0.07 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.885, 0.936 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13762, 4522, 2969 |
Rint | 0.122 |
(sin θ/λ)max (Å−1) | 0.658 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.062, 0.107, 0.92 |
No. of reflections | 4522 |
No. of parameters | 274 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.85, −0.51 |
Absolute structure | Flack (1983), 2596 Friedel pairs |
Absolute structure parameter | 0.04 (2) |
Computer programs: SMART-W2K/NT (Bruker, 2003), SAINT-W2K/NT (Bruker, 2003), SHELXTL-NT (Bruker, 2003), ORTEP-3 for Windows (Farrugia, 1997).
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H9D···O4i | 0.74 (6) | 2.19 (7) | 2.907 (6) | 164 (8) |
O8—H8D···O2 | 0.77 (6) | 2.11 (6) | 2.880 (5) | 173 (7) |
O7—H7D···O9ii | 0.66 (7) | 2.20 (6) | 2.848 (7) | 167 (9) |
O9—H9C···O8 | 0.77 (6) | 2.09 (7) | 2.853 (6) | 166 (8) |
O8—H8C···O7 | 0.93 (6) | 1.96 (6) | 2.882 (7) | 172 (5) |
Symmetry codes: (i) −x+1/2, −y+1, z+1/2; (ii) x−1/2, −y+3/2, −z+1. |
References
Bruker (2003). SAINT-W2K/NT and SMART-W2K/NT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Denning, R. G. & Piper, T. S. (1965). Inorg. Chem. 5, 1056–1065. CrossRef Web of Science Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
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The optical activity, absolute configuration, and rearrangement of tris(L-prolinato)cobalt(III) complexes were studied by Denning & Piper (1965), in which the absolute configurations were assigned based on circular dichroism (CD) studies and 1H NMR spectra. In this work, single crystals of the (-)545-fac-[Co(L-pro)3] isomer (I) suitable for single-crystal X-ray analysis have been prepared. This has allowed the determination of the absolute configuration of (I) as Δ. The UV-Vis and CD spectra of (I) in H2O show good agreement with the reported spectra (Denning & Piper, 1965). The molecular structure, Fig. 1, shows three deprotonated proline molecules to chelate the cobalt(III) ion to form octahedral fac-CoN3O3 geometry. The three lattice water form a three-dimensional network of hydrogen bonds with the uncoordinated carbonyl groups of the proline molecules (Table 1 & Fig. 2).