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The title compound, [CoCl(tren)(dmso)](ClO4)2 [tren is tris-(2-aminoethyl)amine, C6H18N4; dmso is dimethyl sulfoxide, C2H6OS], is the first crystal structure reported with dmso coordinated to CoIII. It crystallizes with two independent molecules in the asymmetric unit. A localized non-crystallographic inversion centre is observed between the two cations.
Supporting information
CCDC reference: 150730
Data collection: SMART (Bruker, 1998); cell refinement: SMART (Bruker, 1998); data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXTL (Bruker, 1998).
chloro tris-(2-aminoethyl)amine (dimethyl sulfoxide-O)- cobalt (III) perchlorate
top
Crystal data top
[CoCl(C6H18N4)(C2H6OS)](ClO4)2 | F(000) = 2128 |
Mr = 517.65 | Dx = 1.739 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 20.0177 (10) Å | Cell parameters from 8192 reflections |
b = 15.7193 (8) Å | θ = 1.7–27.0° |
c = 12.9074 (7) Å | µ = 1.43 mm−1 |
β = 103.235 (1)° | T = 293 K |
V = 3953.6 (4) Å3 | Column, red |
Z = 8 | 0.3 × 0.2 × 0.15 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 8616 independent reflections |
Radiation source: fine-focus sealed tube | 6484 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
φ and ω scans | θmax = 27.0°, θmin = 1.7° |
Absorption correction: empirical (using intensity measurements) (Blessing, 1995) | h = −25→25 |
Tmin = 0.674, Tmax = 0.814 | k = −15→20 |
23159 measured reflections | l = −16→15 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.044 | w = 1/[σ2(Fo2) + (0.0977P)2 + 1.2289P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.130 | (Δ/σ)max = 0.002 |
S = 1.04 | Δρmax = 0.99 e Å−3 |
8616 reflections | Δρmin = −0.84 e Å−3 |
466 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.41961 (2) | 0.41694 (3) | 0.82622 (3) | 0.02703 (11) | |
Cl1 | 0.44355 (4) | 0.39637 (6) | 1.00340 (6) | 0.0384 (2) | |
C1 | 0.4004 (2) | 0.2793 (2) | 0.6763 (3) | 0.0474 (9) | |
H1A | 0.4407 | 0.2685 | 0.6484 | 0.057* | |
H1B | 0.3706 | 0.2300 | 0.6616 | 0.057* | |
C2 | 0.3634 (2) | 0.3571 (2) | 0.6244 (3) | 0.0432 (9) | |
H2A | 0.3603 | 0.3557 | 0.5483 | 0.052* | |
H2B | 0.3173 | 0.3589 | 0.6361 | 0.052* | |
C3 | 0.3624 (2) | 0.5142 (2) | 0.6485 (3) | 0.0420 (8) | |
H3A | 0.3151 | 0.5044 | 0.6520 | 0.050* | |
H3B | 0.3629 | 0.5341 | 0.5776 | 0.050* | |
C4 | 0.3948 (2) | 0.5798 (2) | 0.7303 (3) | 0.0449 (9) | |
H4A | 0.4384 | 0.5984 | 0.7174 | 0.054* | |
H4B | 0.3650 | 0.6289 | 0.7262 | 0.054* | |
C5 | 0.47061 (19) | 0.4408 (2) | 0.6397 (3) | 0.0411 (8) | |
H5A | 0.4677 | 0.4106 | 0.5732 | 0.049* | |
H5B | 0.4804 | 0.5001 | 0.6285 | 0.049* | |
C6 | 0.52769 (19) | 0.4037 (2) | 0.7242 (3) | 0.0428 (8) | |
H6A | 0.5276 | 0.3421 | 0.7188 | 0.051* | |
H6B | 0.5717 | 0.4247 | 0.7158 | 0.051* | |
C7 | 0.2072 (2) | 0.3338 (4) | 0.8163 (4) | 0.0817 (17) | |
H7A | 0.2121 | 0.2889 | 0.7681 | 0.123* | |
H7B | 0.1875 | 0.3828 | 0.7765 | 0.123* | |
H7C | 0.1778 | 0.3151 | 0.8610 | 0.123* | |
C8 | 0.2643 (3) | 0.4418 (4) | 0.9745 (4) | 0.0879 (19) | |
H8A | 0.3043 | 0.4635 | 1.0232 | 0.132* | |
H8B | 0.2330 | 0.4192 | 1.0137 | 0.132* | |
H8C | 0.2424 | 0.4869 | 0.9290 | 0.132* | |
N1 | 0.40288 (14) | 0.43391 (17) | 0.6723 (2) | 0.0326 (6) | |
N2 | 0.42128 (15) | 0.29496 (17) | 0.7944 (2) | 0.0351 (6) | |
H2C | 0.4638 | 0.2745 | 0.8200 | 0.042* | |
H2D | 0.3924 | 0.2672 | 0.8268 | 0.042* | |
N3 | 0.40533 (15) | 0.53916 (18) | 0.8373 (2) | 0.0374 (6) | |
H3C | 0.3684 | 0.5485 | 0.8645 | 0.045* | |
H3D | 0.4421 | 0.5625 | 0.8816 | 0.045* | |
N4 | 0.51570 (14) | 0.43012 (18) | 0.8288 (2) | 0.0354 (6) | |
H4C | 0.5282 | 0.4848 | 0.8418 | 0.042* | |
H4D | 0.5410 | 0.3978 | 0.8808 | 0.042* | |
O1 | 0.32101 (12) | 0.40697 (16) | 0.81506 (18) | 0.0398 (6) | |
S1 | 0.28878 (5) | 0.36036 (7) | 0.89622 (7) | 0.0460 (2) | |
Co2 | 0.90425 (2) | 0.47537 (3) | 0.80758 (3) | 0.02916 (12) | |
Cl2 | 0.90154 (4) | 0.50517 (6) | 0.97645 (6) | 0.0403 (2) | |
C9 | 0.9334 (2) | 0.3643 (2) | 0.6580 (3) | 0.0459 (9) | |
H9A | 0.9473 | 0.3540 | 0.5919 | 0.055* | |
H9B | 0.8974 | 0.3243 | 0.6630 | 0.055* | |
C10 | 0.9940 (2) | 0.3534 (3) | 0.7517 (3) | 0.0490 (10) | |
H10A | 1.0062 | 0.2937 | 0.7615 | 0.059* | |
H10B | 1.0334 | 0.3844 | 0.7396 | 0.059* | |
C11 | 0.8368 (2) | 0.4649 (3) | 0.5963 (3) | 0.0524 (10) | |
H11A | 0.8080 | 0.4183 | 0.6091 | 0.063* | |
H11B | 0.8367 | 0.4658 | 0.5211 | 0.063* | |
C12 | 0.8097 (2) | 0.5480 (3) | 0.6284 (3) | 0.0561 (11) | |
H12A | 0.8299 | 0.5953 | 0.5981 | 0.067* | |
H12B | 0.7603 | 0.5505 | 0.6026 | 0.067* | |
C13 | 0.9575 (2) | 0.5150 (3) | 0.6277 (3) | 0.0492 (10) | |
H13A | 1.0015 | 0.4875 | 0.6330 | 0.059* | |
H13B | 0.9399 | 0.5317 | 0.5542 | 0.059* | |
C14 | 0.9667 (2) | 0.5927 (3) | 0.6976 (3) | 0.0513 (10) | |
H14A | 1.0080 | 0.6230 | 0.6924 | 0.062* | |
H14B | 0.9278 | 0.6306 | 0.6761 | 0.062* | |
C15 | 0.7205 (2) | 0.3111 (3) | 0.7826 (4) | 0.0580 (11) | |
H15A | 0.6968 | 0.3444 | 0.7232 | 0.087* | |
H15B | 0.6884 | 0.2911 | 0.8221 | 0.087* | |
H15C | 0.7421 | 0.2634 | 0.7573 | 0.087* | |
C16 | 0.8177 (3) | 0.2996 (3) | 0.9678 (3) | 0.0641 (12) | |
H16A | 0.8537 | 0.3253 | 1.0205 | 0.096* | |
H16B | 0.8357 | 0.2517 | 0.9368 | 0.096* | |
H16C | 0.7818 | 0.2809 | 1.0006 | 0.096* | |
N5 | 0.90814 (14) | 0.4532 (2) | 0.6607 (2) | 0.0373 (6) | |
N6 | 0.97329 (15) | 0.38707 (19) | 0.8475 (2) | 0.0391 (7) | |
H6C | 1.0103 | 0.4085 | 0.8933 | 0.047* | |
H6D | 0.9564 | 0.3445 | 0.8805 | 0.047* | |
N7 | 0.82847 (15) | 0.5530 (2) | 0.7481 (2) | 0.0398 (7) | |
H7D | 0.7917 | 0.5395 | 0.7737 | 0.048* | |
H7E | 0.8408 | 0.6067 | 0.7682 | 0.048* | |
N8 | 0.97208 (15) | 0.56278 (19) | 0.8081 (2) | 0.0400 (7) | |
H8D | 0.9650 | 0.6065 | 0.8493 | 0.048* | |
H8E | 1.0144 | 0.5418 | 0.8348 | 0.048* | |
O2 | 0.83867 (13) | 0.38252 (17) | 0.79914 (19) | 0.0428 (6) | |
S2 | 0.78427 (5) | 0.37518 (6) | 0.86688 (7) | 0.0412 (2) | |
Cl3 | 0.63998 (4) | 0.57897 (5) | 0.69409 (7) | 0.0394 (2) | |
O3 | 0.57936 (18) | 0.5972 (2) | 0.7279 (4) | 0.0917 (13) | |
O4 | 0.6244 (3) | 0.5306 (3) | 0.5990 (3) | 0.1090 (16) | |
O5 | 0.67627 (18) | 0.6541 (2) | 0.6797 (4) | 0.0849 (12) | |
O6 | 0.6813 (2) | 0.5265 (3) | 0.7703 (3) | 0.1044 (15) | |
Cl4 | 0.60941 (5) | 0.25236 (7) | 0.50364 (8) | 0.0533 (3) | |
O7 | 0.66763 (17) | 0.3058 (2) | 0.5081 (3) | 0.0751 (10) | |
O8 | 0.5887 (2) | 0.2502 (3) | 0.6005 (3) | 0.0995 (14) | |
O9 | 0.6279 (2) | 0.1649 (3) | 0.4860 (4) | 0.1038 (14) | |
O10 | 0.5582 (2) | 0.2712 (4) | 0.4144 (4) | 0.141 (2) | |
Cl5 | 0.15410 (7) | 0.59792 (9) | 0.72736 (11) | 0.0735 (4) | |
O11 | 0.1238 (2) | 0.5341 (3) | 0.7779 (4) | 0.1129 (16) | |
O12 | 0.1346 (3) | 0.6767 (3) | 0.7586 (5) | 0.139 (2) | |
O13 | 0.1225 (5) | 0.5972 (6) | 0.6194 (4) | 0.212 (4) | |
O14A | 0.2292 (5) | 0.6009 (7) | 0.7868 (9) | 0.116 (3)* | 0.50 |
O14B | 0.2160 (5) | 0.5861 (6) | 0.7149 (9) | 0.110 (3)* | 0.50 |
Cl6 | 0.09721 (9) | 0.26153 (7) | 0.55487 (9) | 0.0785 (4) | |
O15 | 0.0967 (2) | 0.3497 (2) | 0.5750 (3) | 0.0935 (13) | |
O16 | 0.0947 (3) | 0.2385 (3) | 0.4540 (4) | 0.136 (2) | |
O18A | 0.1324 (5) | 0.2133 (6) | 0.6380 (8) | 0.101 (3)* | 0.50 |
O17B | 0.0953 (3) | 0.2205 (4) | 0.6478 (5) | 0.0554 (15)* | 0.50 |
O18B | 0.1790 (6) | 0.2393 (8) | 0.5681 (10) | 0.139 (4)* | 0.50 |
O17A | 0.0192 (4) | 0.2251 (5) | 0.5427 (6) | 0.089 (2)* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0336 (2) | 0.0256 (2) | 0.0221 (2) | −0.00252 (16) | 0.00670 (16) | −0.00156 (16) |
Cl1 | 0.0451 (5) | 0.0443 (5) | 0.0240 (4) | −0.0050 (4) | 0.0043 (3) | −0.0005 (3) |
C1 | 0.076 (3) | 0.0323 (19) | 0.0350 (19) | −0.0116 (18) | 0.0154 (18) | −0.0083 (15) |
C2 | 0.059 (2) | 0.044 (2) | 0.0251 (16) | −0.0161 (17) | 0.0067 (15) | −0.0051 (15) |
C3 | 0.049 (2) | 0.042 (2) | 0.0331 (18) | 0.0040 (16) | 0.0056 (15) | 0.0089 (15) |
C4 | 0.065 (2) | 0.0305 (18) | 0.0396 (19) | 0.0058 (16) | 0.0120 (17) | 0.0069 (15) |
C5 | 0.053 (2) | 0.043 (2) | 0.0321 (17) | −0.0031 (16) | 0.0199 (16) | 0.0014 (15) |
C6 | 0.047 (2) | 0.041 (2) | 0.047 (2) | −0.0001 (16) | 0.0246 (17) | −0.0005 (16) |
C7 | 0.047 (3) | 0.126 (5) | 0.068 (3) | −0.036 (3) | 0.005 (2) | 0.000 (3) |
C8 | 0.068 (3) | 0.145 (5) | 0.056 (3) | 0.026 (3) | 0.023 (2) | −0.028 (3) |
N1 | 0.0416 (15) | 0.0331 (15) | 0.0236 (13) | −0.0044 (12) | 0.0084 (11) | 0.0001 (11) |
N2 | 0.0474 (16) | 0.0270 (14) | 0.0315 (14) | −0.0056 (12) | 0.0102 (12) | −0.0034 (11) |
N3 | 0.0473 (17) | 0.0297 (15) | 0.0347 (15) | 0.0013 (12) | 0.0085 (13) | −0.0031 (12) |
N4 | 0.0367 (15) | 0.0334 (15) | 0.0349 (15) | −0.0003 (12) | 0.0062 (12) | 0.0010 (12) |
O1 | 0.0353 (12) | 0.0535 (16) | 0.0313 (12) | −0.0054 (11) | 0.0092 (10) | 0.0009 (11) |
S1 | 0.0371 (5) | 0.0663 (7) | 0.0361 (5) | −0.0060 (4) | 0.0112 (4) | 0.0044 (4) |
Co2 | 0.0309 (2) | 0.0324 (2) | 0.0241 (2) | 0.00308 (17) | 0.00624 (16) | −0.00085 (17) |
Cl2 | 0.0405 (4) | 0.0530 (5) | 0.0274 (4) | −0.0001 (4) | 0.0081 (3) | −0.0078 (3) |
C9 | 0.062 (2) | 0.042 (2) | 0.0378 (19) | 0.0069 (17) | 0.0180 (17) | −0.0091 (16) |
C10 | 0.061 (2) | 0.047 (2) | 0.042 (2) | 0.0207 (18) | 0.0184 (18) | 0.0010 (17) |
C11 | 0.045 (2) | 0.084 (3) | 0.0251 (17) | 0.010 (2) | 0.0034 (15) | −0.0011 (18) |
C12 | 0.048 (2) | 0.085 (3) | 0.035 (2) | 0.026 (2) | 0.0081 (17) | 0.013 (2) |
C13 | 0.056 (2) | 0.057 (2) | 0.041 (2) | 0.0089 (19) | 0.0237 (18) | 0.0117 (18) |
C14 | 0.058 (2) | 0.045 (2) | 0.058 (2) | 0.0021 (18) | 0.027 (2) | 0.0109 (19) |
C15 | 0.049 (2) | 0.065 (3) | 0.058 (3) | −0.020 (2) | 0.010 (2) | −0.012 (2) |
C16 | 0.081 (3) | 0.066 (3) | 0.044 (2) | −0.008 (2) | 0.012 (2) | 0.012 (2) |
N5 | 0.0401 (16) | 0.0472 (17) | 0.0254 (13) | 0.0075 (13) | 0.0094 (12) | 0.0002 (12) |
N6 | 0.0457 (17) | 0.0368 (16) | 0.0333 (15) | 0.0096 (13) | 0.0058 (13) | 0.0008 (12) |
N7 | 0.0371 (15) | 0.0470 (17) | 0.0355 (15) | 0.0110 (13) | 0.0086 (12) | 0.0012 (13) |
N8 | 0.0406 (16) | 0.0358 (16) | 0.0452 (17) | 0.0003 (12) | 0.0130 (13) | −0.0016 (13) |
O2 | 0.0490 (15) | 0.0455 (15) | 0.0370 (13) | −0.0116 (11) | 0.0159 (11) | −0.0091 (11) |
S2 | 0.0431 (5) | 0.0446 (5) | 0.0374 (5) | −0.0059 (4) | 0.0127 (4) | −0.0045 (4) |
Cl3 | 0.0411 (5) | 0.0369 (5) | 0.0416 (5) | 0.0051 (3) | 0.0121 (4) | 0.0007 (4) |
O3 | 0.067 (2) | 0.057 (2) | 0.171 (4) | −0.0099 (16) | 0.068 (3) | −0.027 (2) |
O4 | 0.156 (4) | 0.125 (4) | 0.057 (2) | −0.053 (3) | 0.048 (2) | −0.030 (2) |
O5 | 0.072 (2) | 0.0446 (18) | 0.157 (4) | −0.0041 (15) | 0.065 (2) | −0.005 (2) |
O6 | 0.071 (2) | 0.143 (4) | 0.091 (3) | 0.013 (2) | 0.002 (2) | 0.061 (3) |
Cl4 | 0.0612 (6) | 0.0568 (6) | 0.0400 (5) | −0.0162 (5) | 0.0077 (4) | −0.0032 (4) |
O7 | 0.071 (2) | 0.072 (2) | 0.078 (2) | −0.0262 (17) | 0.0068 (17) | 0.0026 (18) |
O8 | 0.111 (3) | 0.125 (4) | 0.075 (3) | −0.034 (3) | 0.045 (2) | −0.034 (2) |
O9 | 0.128 (4) | 0.068 (3) | 0.130 (4) | −0.020 (2) | 0.061 (3) | −0.028 (2) |
O10 | 0.108 (3) | 0.169 (5) | 0.111 (4) | −0.067 (3) | −0.049 (3) | 0.076 (3) |
Cl5 | 0.0898 (9) | 0.0703 (8) | 0.0717 (8) | −0.0073 (6) | 0.0420 (7) | −0.0020 (6) |
O11 | 0.094 (3) | 0.121 (4) | 0.130 (4) | 0.000 (3) | 0.039 (3) | 0.058 (3) |
O12 | 0.153 (5) | 0.088 (3) | 0.177 (5) | 0.006 (3) | 0.038 (4) | −0.047 (3) |
O13 | 0.303 (10) | 0.285 (10) | 0.066 (3) | −0.061 (8) | 0.078 (5) | −0.017 (4) |
Cl6 | 0.1522 (13) | 0.0433 (6) | 0.0406 (6) | 0.0138 (7) | 0.0233 (7) | 0.0044 (5) |
O15 | 0.162 (4) | 0.0413 (18) | 0.073 (2) | 0.007 (2) | 0.019 (2) | 0.0079 (17) |
O16 | 0.241 (7) | 0.094 (3) | 0.073 (3) | 0.004 (4) | 0.038 (3) | −0.009 (2) |
Geometric parameters (Å, º) top
Co1—N4 | 1.927 (3) | C11—C12 | 1.508 (6) |
Co1—O1 | 1.952 (2) | C12—N7 | 1.506 (4) |
Co1—N3 | 1.952 (3) | C13—C14 | 1.504 (6) |
Co1—N1 | 1.956 (3) | C13—N5 | 1.515 (5) |
Co1—N2 | 1.963 (3) | C14—N8 | 1.482 (5) |
Co1—Cl1 | 2.2500 (9) | C15—S2 | 1.786 (4) |
C1—C2 | 1.505 (5) | C16—S2 | 1.777 (4) |
C1—N2 | 1.506 (4) | O2—S2 | 1.549 (3) |
C2—N1 | 1.497 (4) | Cl3—O6 | 1.400 (4) |
C3—N1 | 1.494 (4) | Cl3—O3 | 1.410 (3) |
C3—C4 | 1.510 (5) | Cl3—O4 | 1.416 (4) |
C4—N3 | 1.493 (4) | Cl3—O5 | 1.421 (3) |
C5—C6 | 1.505 (5) | Cl4—O10 | 1.386 (4) |
C5—N1 | 1.513 (4) | Cl4—O8 | 1.406 (4) |
C6—N4 | 1.484 (4) | Cl4—O7 | 1.427 (3) |
C7—S1 | 1.770 (4) | Cl4—O9 | 1.455 (4) |
C8—S1 | 1.768 (5) | Cl5—O14B | 1.299 (10) |
O1—S1 | 1.536 (2) | Cl5—O12 | 1.386 (5) |
Co2—N8 | 1.931 (3) | Cl5—O13 | 1.393 (6) |
Co2—N6 | 1.943 (3) | Cl5—O11 | 1.407 (4) |
Co2—N5 | 1.947 (3) | Cl5—O14A | 1.523 (11) |
Co2—O2 | 1.949 (2) | Cl6—O16 | 1.341 (4) |
Co2—N7 | 1.962 (3) | Cl6—O17B | 1.370 (6) |
Co2—Cl2 | 2.2422 (9) | Cl6—O18A | 1.370 (10) |
C9—N5 | 1.489 (5) | Cl6—O15 | 1.411 (4) |
C9—C10 | 1.514 (5) | Cl6—O17A | 1.637 (8) |
C10—N6 | 1.489 (4) | Cl6—O18B | 1.644 (12) |
C11—N5 | 1.490 (5) | | |
| | | |
N4—Co1—O1 | 176.48 (11) | C14—C13—N5 | 110.5 (3) |
N4—Co1—N3 | 93.17 (12) | N8—C14—C13 | 107.0 (3) |
O1—Co1—N3 | 85.52 (12) | C9—N5—C11 | 113.0 (3) |
N4—Co1—N1 | 86.61 (11) | C9—N5—C13 | 110.4 (3) |
O1—Co1—N1 | 90.05 (11) | C11—N5—C13 | 111.5 (3) |
N3—Co1—N1 | 86.93 (11) | C9—N5—Co2 | 106.3 (2) |
N4—Co1—N2 | 92.51 (12) | C11—N5—Co2 | 105.9 (2) |
O1—Co1—N2 | 88.37 (12) | C13—N5—Co2 | 109.4 (2) |
N3—Co1—N2 | 170.55 (12) | C10—N6—Co2 | 110.5 (2) |
N1—Co1—N2 | 85.87 (11) | C12—N7—Co2 | 111.0 (2) |
N4—Co1—Cl1 | 91.06 (8) | C14—N8—Co2 | 109.1 (2) |
O1—Co1—Cl1 | 92.29 (7) | S2—O2—Co2 | 125.15 (15) |
N3—Co1—Cl1 | 93.87 (9) | O2—S2—C16 | 105.5 (2) |
N1—Co1—Cl1 | 177.57 (9) | O2—S2—C15 | 101.25 (18) |
N2—Co1—Cl1 | 93.57 (8) | C16—S2—C15 | 99.5 (2) |
C2—C1—N2 | 108.2 (3) | O6—Cl3—O3 | 108.4 (3) |
N1—C2—C1 | 108.2 (3) | O6—Cl3—O4 | 105.7 (3) |
N1—C3—C4 | 107.9 (3) | O3—Cl3—O4 | 110.1 (3) |
N3—C4—C3 | 107.6 (3) | O6—Cl3—O5 | 110.1 (3) |
C6—C5—N1 | 110.6 (3) | O3—Cl3—O5 | 111.9 (2) |
N4—C6—C5 | 107.2 (3) | O4—Cl3—O5 | 110.5 (2) |
C3—N1—C2 | 112.7 (3) | O10—Cl4—O8 | 115.6 (3) |
C3—N1—C5 | 111.2 (3) | O10—Cl4—O7 | 110.4 (2) |
C2—N1—C5 | 111.4 (3) | O8—Cl4—O7 | 112.6 (2) |
C3—N1—Co1 | 106.4 (2) | O10—Cl4—O9 | 103.8 (3) |
C2—N1—Co1 | 105.16 (19) | O8—Cl4—O9 | 104.7 (3) |
C5—N1—Co1 | 109.7 (2) | O7—Cl4—O9 | 109.1 (2) |
C1—N2—Co1 | 110.9 (2) | O14B—Cl5—O12 | 120.2 (5) |
C4—N3—Co1 | 110.2 (2) | O14B—Cl5—O13 | 95.9 (6) |
C6—N4—Co1 | 108.8 (2) | O12—Cl5—O13 | 101.8 (5) |
S1—O1—Co1 | 124.29 (15) | O14B—Cl5—O11 | 118.7 (5) |
O1—S1—C8 | 105.0 (2) | O12—Cl5—O11 | 108.8 (3) |
O1—S1—C7 | 101.0 (2) | O13—Cl5—O11 | 108.2 (4) |
C8—S1—C7 | 99.5 (3) | O14B—Cl5—O14A | 37.6 (5) |
N8—Co2—N6 | 92.90 (13) | O12—Cl5—O14A | 97.9 (5) |
N8—Co2—N5 | 86.89 (13) | O13—Cl5—O14A | 132.4 (5) |
N6—Co2—N5 | 86.90 (12) | O11—Cl5—O14A | 105.6 (5) |
N8—Co2—O2 | 175.66 (11) | O16—Cl6—O17B | 136.1 (4) |
N6—Co2—O2 | 84.78 (13) | O16—Cl6—O18A | 120.6 (5) |
N5—Co2—O2 | 89.32 (12) | O17B—Cl6—O18A | 33.4 (4) |
N8—Co2—N7 | 92.21 (13) | O16—Cl6—O15 | 116.3 (3) |
N6—Co2—N7 | 170.99 (13) | O17B—Cl6—O15 | 107.4 (3) |
N5—Co2—N7 | 85.97 (12) | O18A—Cl6—O15 | 115.1 (4) |
O2—Co2—N7 | 89.63 (12) | O16—Cl6—O17A | 89.5 (4) |
N8—Co2—Cl2 | 91.24 (9) | O17B—Cl6—O17A | 72.7 (4) |
N6—Co2—Cl2 | 93.75 (9) | O18A—Cl6—O17A | 100.9 (5) |
N5—Co2—Cl2 | 178.05 (10) | O15—Cl6—O17A | 108.3 (4) |
O2—Co2—Cl2 | 92.57 (7) | O16—Cl6—O18B | 81.8 (5) |
N7—Co2—Cl2 | 93.56 (9) | O17B—Cl6—O18B | 92.0 (5) |
N5—C9—C10 | 107.6 (3) | O18A—Cl6—O18B | 58.7 (6) |
N6—C10—C9 | 107.4 (3) | O15—Cl6—O18B | 103.8 (5) |
N5—C11—C12 | 108.2 (3) | O17A—Cl6—O18B | 147.3 (5) |
N7—C12—C11 | 107.8 (3) | | |
| | | |
N2—C1—C2—N1 | 44.4 (4) | N5—C9—C10—N6 | 48.4 (4) |
N1—C3—C4—N3 | −48.6 (4) | N5—C11—C12—N7 | −44.7 (4) |
N1—C5—C6—N4 | −40.6 (4) | N5—C13—C14—N8 | 41.8 (4) |
C4—C3—N1—C2 | 159.4 (3) | C10—C9—N5—C11 | −161.4 (3) |
C4—C3—N1—C5 | −74.7 (3) | C10—C9—N5—C13 | 72.9 (4) |
C4—C3—N1—Co1 | 44.6 (3) | C10—C9—N5—Co2 | −45.7 (3) |
C1—C2—N1—C3 | −165.0 (3) | C12—C11—N5—C9 | 164.4 (3) |
C1—C2—N1—C5 | 69.3 (3) | C12—C11—N5—C13 | −70.5 (4) |
C1—C2—N1—Co1 | −49.4 (3) | C12—C11—N5—Co2 | 48.5 (4) |
C6—C5—N1—C3 | 136.8 (3) | C14—C13—N5—C9 | −138.5 (3) |
C6—C5—N1—C2 | −96.6 (3) | C14—C13—N5—C11 | 95.0 (4) |
C6—C5—N1—Co1 | 19.3 (3) | C14—C13—N5—Co2 | −21.9 (4) |
N4—Co1—N1—C3 | −116.1 (2) | N8—Co2—N5—C9 | 117.4 (2) |
O1—Co1—N1—C3 | 62.7 (2) | N6—Co2—N5—C9 | 24.3 (2) |
N3—Co1—N1—C3 | −22.8 (2) | O2—Co2—N5—C9 | −60.5 (2) |
N2—Co1—N1—C3 | 151.1 (2) | N7—Co2—N5—C9 | −150.2 (2) |
Cl1—Co1—N1—C3 | −132.2 (19) | Cl2—Co2—N5—C9 | 134 (3) |
N4—Co1—N1—C2 | 124.0 (2) | N8—Co2—N5—C11 | −122.2 (3) |
O1—Co1—N1—C2 | −57.1 (2) | N6—Co2—N5—C11 | 144.7 (3) |
N3—Co1—N1—C2 | −142.6 (2) | O2—Co2—N5—C11 | 59.9 (3) |
N2—Co1—N1—C2 | 31.3 (2) | N7—Co2—N5—C11 | −29.8 (3) |
Cl1—Co1—N1—C2 | 108 (2) | Cl2—Co2—N5—C11 | −106 (3) |
N4—Co1—N1—C5 | 4.2 (2) | N8—Co2—N5—C13 | −1.9 (2) |
O1—Co1—N1—C5 | −176.9 (2) | N6—Co2—N5—C13 | −94.9 (2) |
N3—Co1—N1—C5 | 97.6 (2) | O2—Co2—N5—C13 | −179.7 (2) |
N2—Co1—N1—C5 | −88.6 (2) | N7—Co2—N5—C13 | 90.6 (2) |
Cl1—Co1—N1—C5 | −12 (2) | Cl2—Co2—N5—C13 | 15 (3) |
C2—C1—N2—Co1 | −18.4 (4) | C9—C10—N6—Co2 | −28.1 (4) |
N4—Co1—N2—C1 | −93.9 (2) | N8—Co2—N6—C10 | −84.4 (3) |
O1—Co1—N2—C1 | 82.7 (2) | N5—Co2—N6—C10 | 2.3 (3) |
N3—Co1—N2—C1 | 33.0 (9) | O2—Co2—N6—C10 | 91.9 (3) |
N1—Co1—N2—C1 | −7.5 (2) | N7—Co2—N6—C10 | 40.0 (9) |
Cl1—Co1—N2—C1 | 174.9 (2) | Cl2—Co2—N6—C10 | −175.9 (2) |
C3—C4—N3—Co1 | 29.3 (4) | C11—C12—N7—Co2 | 20.0 (4) |
N4—Co1—N3—C4 | 82.7 (2) | N8—Co2—N7—C12 | 92.3 (3) |
O1—Co1—N3—C4 | −94.1 (2) | N6—Co2—N7—C12 | −32.2 (9) |
N1—Co1—N3—C4 | −3.8 (2) | N5—Co2—N7—C12 | 5.5 (3) |
N2—Co1—N3—C4 | −44.2 (9) | O2—Co2—N7—C12 | −83.8 (3) |
Cl1—Co1—N3—C4 | 173.9 (2) | Cl2—Co2—N7—C12 | −176.4 (3) |
C5—C6—N4—Co1 | 43.5 (3) | C13—C14—N8—Co2 | −42.7 (3) |
O1—Co1—N4—C6 | −46 (2) | N6—Co2—N8—C14 | 112.1 (2) |
N3—Co1—N4—C6 | −113.8 (2) | N5—Co2—N8—C14 | 25.4 (2) |
N1—Co1—N4—C6 | −27.1 (2) | O2—Co2—N8—C14 | 54.6 (17) |
N2—Co1—N4—C6 | 58.6 (2) | N7—Co2—N8—C14 | −60.4 (2) |
Cl1—Co1—N4—C6 | 152.2 (2) | Cl2—Co2—N8—C14 | −154.0 (2) |
N4—Co1—O1—S1 | 174.9 (18) | N8—Co2—O2—S2 | 177.1 (15) |
N3—Co1—O1—S1 | −116.83 (19) | N6—Co2—O2—S2 | 119.3 (2) |
N1—Co1—O1—S1 | 156.25 (19) | N5—Co2—O2—S2 | −153.7 (2) |
N2—Co1—O1—S1 | 70.39 (19) | N7—Co2—O2—S2 | −67.8 (2) |
Cl1—Co1—O1—S1 | −23.13 (18) | Cl2—Co2—O2—S2 | 25.78 (19) |
Co1—O1—S1—C8 | 101.7 (2) | Co2—O2—S2—C16 | −102.4 (2) |
Co1—O1—S1—C7 | −155.3 (3) | Co2—O2—S2—C15 | 154.2 (2) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2C···O10i | 0.90 | 2.13 | 3.009 (5) | 167 |
N2—H2D···O5ii | 0.90 | 2.24 | 3.021 (4) | 145 |
N2—H2D···S1 | 0.90 | 2.85 | 3.379 (3) | 119 |
N3—H3C···O9iii | 0.90 | 2.65 | 3.201 (5) | 121 |
N3—H3D···Cl1iv | 0.90 | 2.51 | 3.399 (3) | 169 |
N4—H4C···O3 | 0.90 | 2.65 | 3.314 (5) | 131 |
N4—H4C···Cl1iv | 0.90 | 2.70 | 3.462 (3) | 143 |
N4—H4D···O9i | 0.90 | 2.18 | 3.051 (5) | 162 |
N6—H6C···Cl2v | 0.90 | 2.53 | 3.421 (3) | 168 |
N6—H6D···O17Avi | 0.90 | 2.44 | 3.040 (9) | 124 |
N7—H7D···O6 | 0.90 | 2.21 | 3.052 (5) | 156 |
N7—H7D···S2 | 0.90 | 2.87 | 3.402 (3) | 120 |
N7—H7E···O18Aiii | 0.90 | 2.07 | 2.932 (10) | 161 |
N8—H8D···O17Biii | 0.90 | 2.17 | 2.940 (7) | 144 |
N8—H8D···O17Biii | 0.90 | 2.17 | 2.940 (7) | 144 |
N8—H8D···O17Aiii | 0.90 | 2.31 | 3.178 (9) | 163 |
N8—H8D···O18Aiii | 0.90 | 2.61 | 3.334 (10) | 139 |
N8—H8E···O11vii | 0.90 | 2.47 | 3.181 (5) | 136 |
N8—H8E···Cl2v | 0.90 | 2.73 | 3.472 (3) | 141 |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) −x+1, y−1/2, −z+3/2; (iii) −x+1, y+1/2, −z+3/2; (iv) −x+1, −y+1, −z+2; (v) −x+2, −y+1, −z+2; (vi) x+1, −y+1/2, z+1/2; (vii) x+1, y, z. |
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