metal-organic compounds
Diaquatetrakis(dimethyl sulfoxide-κO)cobalt(II) bis[diamminetetrakis(thiocyanato-κN)chromate(III)] dimethyl sulfoxide hexasolvate dihydrate
aDepartment of Chemistry, Taras Shevchenko National University of Kyiv, 64/13 Volodymyrska Street, Kyiv 01601, Ukraine, and bSSI `Institute for Single Crystals', National Academy of Sciences of Ukraine, 60 Lenina ave., Kharkiv 61072, Ukraine
*Correspondence e-mail: vika@xray.isc.kharkov.com
The solvated title salt, [Co(C2H6OS)4(H2O)2][Cr(NCS)4(NH3)2]·6C2H6OS·2H2O, is build up from a complex [Co(DMSO)4(H2O)2]2+ cation (where DMSO is dimethyl sulfoxide), two Reinecke's Salt anions, i.e. [Cr(NCS)4(NH3)2]−, as the complex counter-ions, together with solvent molecules (six DMSO and two water). The crystal packing consists of a branched three-dimensional system of hydrogen bonds involving the DMSO and water solvent molecules, the S atoms of the thiocyanate ligands, and the coordinating NH3 and H2O molecules.
CCDC reference: 1508512
Structure description
The CoII atom of the complex cation lies on an inversion centre and, as shown in Fig. 1, adopts a slightly distorted octahedral coordination geometry. Four O atoms from DMSO ligands constitute the equatorial plane, with the O atoms of two coordinating water molecules in axial positions.
The CrIII atom of the anion is also six-coordinate involving six N atoms, four from thiocyanate ligands in the equatorial plane and two from ammine ligands in axial positions. The bond lengths and angles in the title complex agree well with those reported in closely related compounds (Schubert et al., 1981; Tang et al., 1993; Foust & Janickis, 1980; Anbalagan et al., 2009; Nikitina et al., 2008). The title complex is most closely related to the salt [Mn(DMSO)4(H2O)2][Cr(NCS)4(NH3)2]·6DMSO·2H2O (Gerasimova et al., 2009).
In the ) generates a three-dimensional network of anions, cations and solvent molecules (Fig. 2).
of the title salt, cations are linked to anions and anions are linked to other anions both directly and through the DMSO and water solvent molecules acting as bridges. The extensive series of hydrogen bonds (Table 1Synthesis and crystallization
Cobalt powder (0.159 g, 2.70 mmol), NH4[Cr(NCS)4(NH3)2]·H2O (1.943 g, 5.4 mmol) and DMSO (20 ml) were heated in air at 323–333 K and stirred magnetically until the metal powder had completely dissolved. 2-Propanol was added dropwise after a few days to obtain a fine-grained red precipitate. Good quality single crystals suitable for X-ray analysis were obtained by recrystallization from DMSO with the addition of a few ml of Et2O. These were filtered off, washed with dry 2-propanol and finally dried in vacuo at room temperature (yield: 0.78 g, 37.5%).
Refinement
Crystal data, data collection and structure .
details are summarized in Table 2
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Structural data
CCDC reference: 1508512
https://doi.org/10.1107/S2414314616015716/sj4061sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314616015716/sj4061Isup2.hkl
Data collection: P3 (Siemens, 1991); cell
P3 (Siemens, 1991); data reduction: XDISK in SHELXTL-Plus (Sheldrick, 1992); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009) and publCIF (Westrip, 2010).[Co(C2H6OS)4(H2O)2][Cr(NCS)4(NH3)2]·6C2H6OS·2H2O | Z = 1 |
Mr = 1549.05 | F(000) = 807 |
Triclinic, P1 | Dx = 1.441 Mg m−3 |
a = 11.752 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.212 (4) Å | Cell parameters from 2015 reflections |
c = 13.257 (3) Å | θ = 3.5–25.0° |
α = 85.95 (2)° | µ = 1.11 mm−1 |
β = 87.98 (2)° | T = 294 K |
γ = 70.17 (2)° | Block, colourless |
V = 1785.3 (9) Å3 | 0.6 × 0.4 × 0.2 mm |
Siemens P3/PC diffractometer | 6138 independent reflections |
Graphite monochromator | 3459 reflections with I > 2σ(I) |
Detector resolution: 16.1827 pixels mm-1 | Rint = 0.056 |
θ–2θ scans | θmax = 25.1°, θmin = 1.8° |
Absorption correction: analytical [analytical correction (Katayama 1986) in WinGX (Farrugia, 2012)] | h = −8→14 |
Tmin = 0.604, Tmax = 0.842 | k = −14→14 |
6478 measured reflections | l = −15→15 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.069 | H-atom parameters constrained |
wR(F2) = 0.195 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
6138 reflections | Δρmax = 1.23 e Å−3 |
352 parameters | Δρmin = −1.03 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.0000 | 0.5000 | 0.0000 | 0.0220 (3) | |
Cr1 | −0.62334 (11) | 0.13962 (9) | 0.24820 (8) | 0.0275 (3) | |
S1 | −0.07654 (17) | 0.28560 (14) | 0.07475 (14) | 0.0304 (4) | |
S2 | 0.12683 (18) | 0.59160 (14) | 0.17553 (13) | 0.0308 (4) | |
S3 | −0.3879 (2) | 0.3817 (2) | 0.2914 (2) | 0.0599 (7) | |
S4 | −0.9581 (2) | 0.3312 (2) | 0.45589 (19) | 0.0635 (7) | |
S5 | −0.8412 (2) | −0.12533 (19) | 0.23569 (18) | 0.0513 (6) | |
S6 | −0.2658 (2) | −0.0376 (2) | 0.05798 (18) | 0.0518 (6) | |
S7 | −0.1953 (2) | 0.01062 (19) | 0.47090 (19) | 0.0531 (6) | |
S8 | −0.4153 (3) | −0.2743 (2) | 0.44568 (18) | 0.0626 (7) | |
S9 | −0.49827 (18) | 0.64195 (18) | 0.07185 (15) | 0.0411 (5) | |
N1 | −0.5327 (5) | 0.2493 (5) | 0.2657 (4) | 0.0300 (14) | |
N2 | −0.7566 (6) | 0.2290 (5) | 0.3392 (5) | 0.0388 (16) | |
N3 | −0.7121 (5) | 0.0272 (5) | 0.2342 (4) | 0.0304 (14) | |
N4 | −0.4888 (6) | 0.0534 (5) | 0.1567 (5) | 0.0375 (16) | |
N5 | −0.7122 (6) | 0.2396 (5) | 0.1241 (4) | 0.0335 (14) | |
H5A | −0.7178 | 0.1931 | 0.0771 | 0.050* | |
H5B | −0.6711 | 0.2848 | 0.0990 | 0.050* | |
H5C | −0.7861 | 0.2840 | 0.1426 | 0.050* | |
N6 | −0.5326 (6) | 0.0345 (5) | 0.3673 (4) | 0.0365 (15) | |
H6A | −0.5855 | 0.0258 | 0.4142 | 0.055* | |
H6B | −0.4840 | 0.0669 | 0.3937 | 0.055* | |
H6C | −0.4887 | −0.0349 | 0.3459 | 0.055* | |
O1W | −0.1997 (6) | 0.7216 (5) | 0.2060 (5) | 0.067 (2) | |
H1WA | −0.2318 | 0.7664 | 0.1551 | 0.100* | |
H1WB | −0.2532 | 0.7245 | 0.2515 | 0.100* | |
O1 | 0.0946 (5) | 0.4937 (4) | 0.1327 (3) | 0.0309 (11) | |
O2 | 0.0271 (4) | 0.3229 (4) | 0.0310 (3) | 0.0271 (11) | |
O3 | −0.1606 (4) | 0.5446 (4) | 0.0842 (3) | 0.0290 (11) | |
H3A | −0.1635 | 0.5746 | 0.1414 | 0.044* | |
H3B | −0.2310 | 0.5814 | 0.0596 | 0.044* | |
O4 | −0.3298 (5) | 0.0593 (5) | 0.4896 (4) | 0.0486 (15) | |
O5 | −0.3876 (4) | 0.5990 (4) | 0.0043 (4) | 0.0362 (12) | |
O6 | −0.3761 (6) | −0.2221 (6) | 0.3498 (5) | 0.068 (2) | |
C1 | 0.0615 (9) | 0.6080 (8) | 0.2977 (6) | 0.062 (3) | |
H1A | −0.0246 | 0.6443 | 0.2925 | 0.093* | |
H1B | 0.0938 | 0.6559 | 0.3341 | 0.093* | |
H1C | 0.0798 | 0.5328 | 0.3330 | 0.093* | |
C2 | 0.2785 (8) | 0.5278 (7) | 0.2116 (7) | 0.050 (2) | |
H2A | 0.3288 | 0.5070 | 0.1524 | 0.076* | |
H2B | 0.2876 | 0.4591 | 0.2550 | 0.076* | |
H2C | 0.3022 | 0.5824 | 0.2470 | 0.076* | |
C3 | −0.0346 (8) | 0.1364 (6) | 0.0480 (7) | 0.049 (2) | |
H3C | −0.0360 | 0.1304 | −0.0237 | 0.074* | |
H3D | −0.0905 | 0.1032 | 0.0808 | 0.074* | |
H3E | 0.0455 | 0.0950 | 0.0725 | 0.074* | |
C4 | −0.0561 (9) | 0.2702 (8) | 0.2070 (6) | 0.061 (3) | |
H4A | −0.0622 | 0.3441 | 0.2315 | 0.091* | |
H4B | 0.0223 | 0.2146 | 0.2225 | 0.091* | |
H4C | −0.1173 | 0.2435 | 0.2391 | 0.091* | |
C5 | −0.4680 (6) | 0.3038 (6) | 0.2776 (5) | 0.0301 (16) | |
C6 | −0.8409 (8) | 0.2721 (7) | 0.3870 (6) | 0.0385 (19) | |
C7 | −0.7661 (7) | −0.0362 (6) | 0.2354 (5) | 0.0291 (16) | |
C8 | −0.3949 (8) | 0.0144 (6) | 0.1159 (5) | 0.0361 (18) | |
C9 | −0.5010 (9) | 0.7771 (8) | 0.1143 (7) | 0.060 (3) | |
H9A | −0.4347 | 0.7643 | 0.1591 | 0.090* | |
H9B | −0.5759 | 0.8128 | 0.1495 | 0.090* | |
H9C | −0.4939 | 0.8276 | 0.0573 | 0.090* | |
C10 | −0.6211 (8) | 0.6956 (7) | −0.0121 (8) | 0.056 (3) | |
H10A | −0.6269 | 0.6328 | −0.0489 | 0.084* | |
H10B | −0.6086 | 0.7544 | −0.0586 | 0.084* | |
H10C | −0.6946 | 0.7286 | 0.0257 | 0.084* | |
C11 | −0.1800 (11) | −0.0291 (14) | 0.3457 (10) | 0.122 (6) | |
H11A | −0.2114 | −0.0913 | 0.3398 | 0.183* | |
H11B | −0.0960 | −0.0546 | 0.3264 | 0.183* | |
H11C | −0.2241 | 0.0368 | 0.3022 | 0.183* | |
C12 | −0.1471 (9) | 0.1326 (8) | 0.4536 (8) | 0.067 (3) | |
H12A | −0.1447 | 0.1632 | 0.5180 | 0.101* | |
H12B | −0.2026 | 0.1915 | 0.4103 | 0.101* | |
H12C | −0.0679 | 0.1095 | 0.4232 | 0.101* | |
C13 | −0.3090 (12) | −0.4163 (9) | 0.4675 (11) | 0.106 (5) | |
H13A | −0.2356 | −0.4111 | 0.4928 | 0.159* | |
H13B | −0.2921 | −0.4549 | 0.4052 | 0.159* | |
H13C | −0.3416 | −0.4600 | 0.5162 | 0.159* | |
C14 | −0.5386 (10) | −0.3128 (8) | 0.4146 (8) | 0.068 (3) | |
H14A | −0.6029 | −0.2444 | 0.3904 | 0.102* | |
H14B | −0.5659 | −0.3477 | 0.4734 | 0.102* | |
H14C | −0.5152 | −0.3675 | 0.3627 | 0.102* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0229 (7) | 0.0162 (6) | 0.0226 (7) | −0.0010 (5) | 0.0027 (5) | −0.0031 (5) |
Cr1 | 0.0321 (7) | 0.0245 (6) | 0.0240 (6) | −0.0068 (5) | 0.0012 (5) | −0.0028 (4) |
S1 | 0.0295 (10) | 0.0218 (8) | 0.0378 (10) | −0.0066 (8) | 0.0001 (8) | 0.0006 (7) |
S2 | 0.0398 (11) | 0.0252 (9) | 0.0263 (9) | −0.0088 (8) | 0.0005 (8) | −0.0054 (7) |
S3 | 0.0625 (16) | 0.0475 (13) | 0.0787 (17) | −0.0294 (12) | −0.0204 (13) | 0.0010 (12) |
S4 | 0.0650 (17) | 0.0701 (16) | 0.0529 (14) | −0.0178 (14) | 0.0334 (13) | −0.0293 (12) |
S5 | 0.0531 (14) | 0.0431 (12) | 0.0645 (15) | −0.0253 (11) | 0.0003 (12) | −0.0022 (10) |
S6 | 0.0393 (13) | 0.0578 (13) | 0.0565 (14) | −0.0125 (11) | 0.0195 (11) | −0.0209 (11) |
S7 | 0.0456 (14) | 0.0470 (12) | 0.0621 (15) | −0.0115 (11) | 0.0013 (11) | 0.0049 (11) |
S8 | 0.096 (2) | 0.0466 (13) | 0.0441 (13) | −0.0210 (14) | −0.0135 (13) | −0.0082 (10) |
S9 | 0.0321 (11) | 0.0432 (11) | 0.0420 (11) | −0.0075 (9) | 0.0049 (9) | 0.0072 (9) |
N1 | 0.018 (3) | 0.036 (3) | 0.025 (3) | 0.004 (3) | 0.002 (2) | 0.001 (3) |
N2 | 0.050 (4) | 0.038 (3) | 0.030 (3) | −0.017 (3) | 0.004 (3) | −0.006 (3) |
N3 | 0.023 (3) | 0.031 (3) | 0.032 (3) | −0.002 (3) | 0.004 (3) | −0.006 (3) |
N4 | 0.038 (4) | 0.030 (3) | 0.036 (4) | −0.002 (3) | 0.004 (3) | −0.001 (3) |
N5 | 0.036 (4) | 0.033 (3) | 0.028 (3) | −0.007 (3) | 0.000 (3) | 0.000 (2) |
N6 | 0.037 (4) | 0.033 (3) | 0.033 (3) | −0.005 (3) | −0.003 (3) | 0.005 (3) |
O1W | 0.073 (5) | 0.056 (4) | 0.057 (4) | 0.000 (4) | −0.002 (4) | −0.020 (3) |
O1 | 0.042 (3) | 0.023 (2) | 0.028 (3) | −0.011 (2) | −0.005 (2) | −0.0024 (19) |
O2 | 0.020 (2) | 0.025 (2) | 0.030 (3) | −0.001 (2) | −0.002 (2) | 0.0054 (19) |
O3 | 0.027 (3) | 0.029 (2) | 0.030 (3) | −0.006 (2) | 0.005 (2) | −0.010 (2) |
O4 | 0.055 (4) | 0.042 (3) | 0.044 (3) | −0.011 (3) | 0.016 (3) | −0.002 (3) |
O5 | 0.024 (3) | 0.043 (3) | 0.036 (3) | −0.003 (2) | 0.001 (2) | −0.008 (2) |
O6 | 0.065 (5) | 0.063 (4) | 0.061 (4) | −0.005 (4) | 0.016 (4) | −0.006 (3) |
C1 | 0.078 (7) | 0.068 (6) | 0.034 (5) | −0.016 (6) | 0.011 (5) | −0.019 (4) |
C2 | 0.050 (5) | 0.048 (5) | 0.059 (6) | −0.020 (4) | 0.007 (4) | −0.025 (4) |
C3 | 0.044 (5) | 0.024 (4) | 0.081 (6) | −0.013 (4) | 0.001 (5) | −0.006 (4) |
C4 | 0.072 (7) | 0.066 (6) | 0.035 (5) | −0.015 (5) | 0.015 (5) | 0.007 (4) |
C5 | 0.025 (4) | 0.023 (3) | 0.041 (4) | −0.005 (3) | −0.016 (3) | −0.002 (3) |
C6 | 0.047 (5) | 0.041 (4) | 0.027 (4) | −0.014 (4) | 0.016 (4) | −0.010 (3) |
C7 | 0.037 (4) | 0.027 (4) | 0.024 (4) | −0.013 (4) | −0.004 (3) | 0.002 (3) |
C8 | 0.046 (5) | 0.032 (4) | 0.029 (4) | −0.011 (4) | 0.004 (4) | −0.005 (3) |
C9 | 0.057 (6) | 0.063 (6) | 0.063 (6) | −0.019 (5) | 0.004 (5) | −0.037 (5) |
C10 | 0.035 (5) | 0.035 (4) | 0.091 (7) | −0.002 (4) | −0.027 (5) | 0.000 (5) |
C11 | 0.073 (8) | 0.218 (17) | 0.098 (10) | −0.065 (10) | 0.027 (7) | −0.097 (11) |
C12 | 0.062 (7) | 0.068 (6) | 0.075 (7) | −0.029 (6) | −0.016 (5) | 0.019 (5) |
C13 | 0.121 (11) | 0.046 (6) | 0.152 (13) | −0.025 (7) | −0.071 (10) | 0.009 (7) |
C14 | 0.085 (8) | 0.059 (6) | 0.074 (7) | −0.041 (6) | 0.003 (6) | −0.012 (5) |
Co1—O1 | 2.097 (5) | N6—H6A | 0.8900 |
Co1—O1i | 2.097 (5) | N6—H6B | 0.8900 |
Co1—O2 | 2.089 (4) | N6—H6C | 0.8900 |
Co1—O2i | 2.088 (4) | O1W—H1WA | 0.8499 |
Co1—O3 | 2.084 (4) | O1W—H1WB | 0.8500 |
Co1—O3i | 2.084 (4) | O3—H3A | 0.8600 |
Cr1—N1 | 2.003 (7) | O3—H3B | 0.8600 |
Cr1—N2 | 1.998 (6) | C1—H1A | 0.9600 |
Cr1—N3 | 2.007 (7) | C1—H1B | 0.9600 |
Cr1—N4 | 1.999 (6) | C1—H1C | 0.9600 |
Cr1—N5 | 2.065 (6) | C2—H2A | 0.9600 |
Cr1—N6 | 2.045 (6) | C2—H2B | 0.9600 |
S1—O2 | 1.523 (5) | C2—H2C | 0.9600 |
S1—C3 | 1.777 (7) | C3—H3C | 0.9600 |
S1—C4 | 1.767 (8) | C3—H3D | 0.9600 |
S2—O1 | 1.521 (5) | C3—H3E | 0.9600 |
S2—C1 | 1.763 (8) | C4—H4A | 0.9600 |
S2—C2 | 1.755 (9) | C4—H4B | 0.9600 |
S3—C5 | 1.571 (8) | C4—H4C | 0.9600 |
S4—C6 | 1.606 (8) | C9—H9A | 0.9600 |
S5—C7 | 1.617 (8) | C9—H9B | 0.9600 |
S6—C8 | 1.620 (8) | C9—H9C | 0.9600 |
S7—O4 | 1.506 (6) | C10—H10A | 0.9600 |
S7—C11 | 1.748 (11) | C10—H10B | 0.9600 |
S7—C12 | 1.762 (10) | C10—H10C | 0.9600 |
S8—O6 | 1.509 (7) | C11—H11A | 0.9600 |
S8—C13 | 1.771 (10) | C11—H11B | 0.9600 |
S8—C14 | 1.739 (10) | C11—H11C | 0.9600 |
S9—O5 | 1.513 (5) | C12—H12A | 0.9600 |
S9—C9 | 1.772 (8) | C12—H12B | 0.9600 |
S9—C10 | 1.766 (8) | C12—H12C | 0.9600 |
N1—C5 | 1.189 (9) | C13—H13A | 0.9600 |
N2—C6 | 1.145 (9) | C13—H13B | 0.9600 |
N3—C7 | 1.154 (9) | C13—H13C | 0.9600 |
N4—C8 | 1.173 (9) | C14—H14A | 0.9600 |
N5—H5A | 0.8900 | C14—H14B | 0.9600 |
N5—H5B | 0.8900 | C14—H14C | 0.9600 |
N5—H5C | 0.8900 | ||
O1i—Co1—O1 | 180.0 | H3A—O3—H3B | 103.1 |
O2—Co1—O1 | 87.58 (18) | S2—C1—H1A | 109.5 |
O2i—Co1—O1i | 87.58 (17) | S2—C1—H1B | 109.5 |
O2i—Co1—O1 | 92.42 (17) | S2—C1—H1C | 109.5 |
O2—Co1—O1i | 92.42 (18) | H1A—C1—H1B | 109.5 |
O2i—Co1—O2 | 180.0 | H1A—C1—H1C | 109.5 |
O3i—Co1—O1i | 89.13 (19) | H1B—C1—H1C | 109.5 |
O3i—Co1—O1 | 90.87 (19) | S2—C2—H2A | 109.5 |
O3—Co1—O1i | 90.87 (19) | S2—C2—H2B | 109.5 |
O3—Co1—O1 | 89.13 (19) | S2—C2—H2C | 109.5 |
O3i—Co1—O2 | 89.38 (17) | H2A—C2—H2B | 109.5 |
O3—Co1—O2 | 90.62 (17) | H2A—C2—H2C | 109.5 |
O3i—Co1—O2i | 90.62 (17) | H2B—C2—H2C | 109.5 |
O3—Co1—O2i | 89.38 (17) | S1—C3—H3C | 109.5 |
O3—Co1—O3i | 180.0 | S1—C3—H3D | 109.5 |
N1—Cr1—N3 | 178.4 (2) | S1—C3—H3E | 109.5 |
N1—Cr1—N5 | 91.4 (2) | H3C—C3—H3D | 109.5 |
N1—Cr1—N6 | 90.0 (2) | H3C—C3—H3E | 109.5 |
N2—Cr1—N1 | 91.1 (2) | H3D—C3—H3E | 109.5 |
N2—Cr1—N3 | 88.7 (2) | S1—C4—H4A | 109.5 |
N2—Cr1—N4 | 178.7 (3) | S1—C4—H4B | 109.5 |
N2—Cr1—N5 | 90.4 (2) | S1—C4—H4C | 109.5 |
N2—Cr1—N6 | 91.7 (2) | H4A—C4—H4B | 109.5 |
N3—Cr1—N5 | 90.2 (2) | H4A—C4—H4C | 109.5 |
N3—Cr1—N6 | 88.4 (3) | H4B—C4—H4C | 109.5 |
N4—Cr1—N1 | 87.6 (2) | N1—C5—S3 | 177.1 (6) |
N4—Cr1—N3 | 92.5 (2) | N2—C6—S4 | 179.0 (8) |
N4—Cr1—N5 | 89.2 (2) | N3—C7—S5 | 179.4 (7) |
N4—Cr1—N6 | 88.8 (2) | N4—C8—S6 | 179.0 (7) |
N6—Cr1—N5 | 177.5 (2) | S9—C9—H9A | 109.5 |
O2—S1—C3 | 104.2 (3) | S9—C9—H9B | 109.5 |
O2—S1—C4 | 105.4 (4) | S9—C9—H9C | 109.5 |
C4—S1—C3 | 99.8 (4) | H9A—C9—H9B | 109.5 |
O1—S2—C1 | 105.9 (4) | H9A—C9—H9C | 109.5 |
O1—S2—C2 | 105.0 (3) | H9B—C9—H9C | 109.5 |
C2—S2—C1 | 97.8 (5) | S9—C10—H10A | 109.5 |
O4—S7—C11 | 104.8 (5) | S9—C10—H10B | 109.5 |
O4—S7—C12 | 105.7 (4) | S9—C10—H10C | 109.5 |
C11—S7—C12 | 98.3 (6) | H10A—C10—H10B | 109.5 |
O6—S8—C13 | 107.0 (6) | H10A—C10—H10C | 109.5 |
O6—S8—C14 | 106.6 (5) | H10B—C10—H10C | 109.5 |
C14—S8—C13 | 98.5 (6) | S7—C11—H11A | 109.5 |
O5—S9—C9 | 106.8 (4) | S7—C11—H11B | 109.5 |
O5—S9—C10 | 104.8 (4) | S7—C11—H11C | 109.5 |
C10—S9—C9 | 98.2 (4) | H11A—C11—H11B | 109.5 |
C5—N1—Cr1 | 172.9 (5) | H11A—C11—H11C | 109.5 |
C6—N2—Cr1 | 171.4 (7) | H11B—C11—H11C | 109.5 |
C7—N3—Cr1 | 173.8 (6) | S7—C12—H12A | 109.5 |
C8—N4—Cr1 | 164.3 (7) | S7—C12—H12B | 109.5 |
Cr1—N5—H5A | 109.5 | S7—C12—H12C | 109.5 |
Cr1—N5—H5B | 109.5 | H12A—C12—H12B | 109.5 |
Cr1—N5—H5C | 109.5 | H12A—C12—H12C | 109.5 |
H5A—N5—H5B | 109.5 | H12B—C12—H12C | 109.5 |
H5A—N5—H5C | 109.5 | S8—C13—H13A | 109.5 |
H5B—N5—H5C | 109.5 | S8—C13—H13B | 109.5 |
Cr1—N6—H6A | 109.5 | S8—C13—H13C | 109.5 |
Cr1—N6—H6B | 109.5 | H13A—C13—H13B | 109.5 |
Cr1—N6—H6C | 109.5 | H13A—C13—H13C | 109.5 |
H6A—N6—H6B | 109.5 | H13B—C13—H13C | 109.5 |
H6A—N6—H6C | 109.5 | S8—C14—H14A | 109.5 |
H6B—N6—H6C | 109.5 | S8—C14—H14B | 109.5 |
H1WA—O1W—H1WB | 109.7 | S8—C14—H14C | 109.5 |
S2—O1—Co1 | 127.9 (3) | H14A—C14—H14B | 109.5 |
S1—O2—Co1 | 119.5 (2) | H14A—C14—H14C | 109.5 |
Co1—O3—H3A | 119.3 | H14B—C14—H14C | 109.5 |
Co1—O3—H3B | 124.5 | ||
C1—S2—O1—Co1 | 122.0 (5) | C3—S1—O2—Co1 | 160.4 (4) |
C2—S2—O1—Co1 | −135.1 (4) | C4—S1—O2—Co1 | −95.1 (4) |
Symmetry code: (i) −x, −y+1, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N5—H5A···S6ii | 0.89 | 2.76 | 3.647 (7) | 176 |
N5—H5B···O5iii | 0.89 | 2.17 | 3.019 (8) | 160 |
N6—H6A···O4iv | 0.89 | 2.03 | 2.874 (8) | 158 |
N6—H6B···O4 | 0.89 | 2.22 | 3.037 (9) | 152 |
N6—H6C···O6 | 0.89 | 2.22 | 3.069 (8) | 160 |
O1W—H1WA···S6v | 0.85 | 2.55 | 3.293 (7) | 147 |
O1W—H1WB···O6v | 0.85 | 1.89 | 2.711 (9) | 163 |
C3—H3E···S6vi | 0.96 | 2.97 | 3.590 (9) | 124 |
Symmetry codes: (ii) −x−1, −y, −z; (iii) −x−1, −y+1, −z; (iv) −x−1, −y, −z+1; (v) x, y+1, z; (vi) −x, −y, −z. |
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