Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100003504/qa0245sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100003504/qa0245Isup2.hkl |
CCDC reference: 144692
Na3[Co(CO3)3]·3H2O and the ligand C-meso-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-N-acetic acid were prepared according to a literature method (Bauer & Drinkard, 1960; Xu et al., 1988). Na3[Co(CO3)3]·3H2O (1.0 g) and the ligand (1.0 g) were suspended in water (50 ml). The mixture was heated on a water bath for 2 h. An aliqot of aqueous 12 M HCl (4 ml) was added dropwise to the solution. The solution was heated for a further 30 min, NaClO4 (4.0 g) was added, and the solution was cooled. The green powder obtained upon cooling was filtered off, washed with ethanol and diethyl ether, and dried in vacuo. The crystals for X-ray analysis were recrystallized from a 1 M ZnCl2/2M HCl mixture by slow evaporation.
The maximum 2θ for data collection is 50.0°. The data collection would not go beyond this limit, because the crystal quality was not good. The hydrogen atoms were fixed geometrically and refined with constraint.
Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: NRCVAX (Gabe, et al., 1989); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: NRCVAX (Gabe et al., 1989); software used to prepare material for publication: SHELXL93.
[CoZnCl4(C18H37N4O2)] | Z = 4 |
Mr = 607.62 | F(000) = 1256 |
Triclinic, P1 | Dx = 1.608 Mg m−3 |
a = 10.242 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.874 (2) Å | Cell parameters from 25 reflections |
c = 23.168 (5) Å | θ = 6.1–15.3° |
α = 92.50 (2)° | µ = 2.07 mm−1 |
β = 100.39 (2)° | T = 293 K |
γ = 97.60 (2)° | Pillar, green |
V = 2509.6 (8) Å3 | 0.28 × 0.18 × 0.11 mm |
Enraf-Nonius CAD-4 diffractometer | 5321 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.061 |
Graphite monochromator | θmax = 25.0°, θmin = 1.8° |
ω/2θ scans | h = −12→11 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→12 |
Tmin = 0.656, Tmax = 0.798 | l = −27→27 |
9300 measured reflections | 3 standard reflections every 60 min |
8792 independent reflections | intensity decay: 1% |
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.052 | Hydrogen site location: geometrically |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 0.93 | Calculated w = 1/[s2(Fo2) + (0.0689P)2] where P = (Fo2 + 2Fc2)/3 |
8792 reflections | (Δ/σ)max = 0.002 |
541 parameters | Δρmax = 0.86 e Å−3 |
0 restraints | Δρmin = −0.68 e Å−3 |
[CoZnCl4(C18H37N4O2)] | γ = 97.60 (2)° |
Mr = 607.62 | V = 2509.6 (8) Å3 |
Triclinic, P1 | Z = 4 |
a = 10.242 (1) Å | Mo Kα radiation |
b = 10.874 (2) Å | µ = 2.07 mm−1 |
c = 23.168 (5) Å | T = 293 K |
α = 92.50 (2)° | 0.28 × 0.18 × 0.11 mm |
β = 100.39 (2)° |
Enraf-Nonius CAD-4 diffractometer | 5321 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.061 |
Tmin = 0.656, Tmax = 0.798 | 3 standard reflections every 60 min |
9300 measured reflections | intensity decay: 1% |
8792 independent reflections |
R[F2 > 2σ(F2)] = 0.052 | 0 restraints |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 0.93 | Δρmax = 0.86 e Å−3 |
8792 reflections | Δρmin = −0.68 e Å−3 |
541 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Co1A | 0.36747 (8) | 0.24346 (7) | 0.13674 (3) | 0.0245 (2) | |
Cl1A | 0.3612 (2) | 0.43108 (14) | 0.17694 (7) | 0.0395 (4) | |
N1A | 0.5378 (4) | 0.2924 (4) | 0.1065 (2) | 0.0264 (11) | |
N2A | 0.4575 (5) | 0.1863 (4) | 0.2130 (2) | 0.0269 (11) | |
H1A | 0.4653 | 0.1060 | 0.2033 | 0.080* | |
N3A | 0.1970 (5) | 0.1866 (5) | 0.1630 (2) | 0.0294 (11) | |
H2A | 0.1702 | 0.2561 | 0.1776 | 0.080* | |
N4A | 0.2742 (5) | 0.3045 (5) | 0.0620 (2) | 0.0328 (12) | |
H3A | 0.2567 | 0.3799 | 0.0746 | 0.080* | |
O1A | 0.3712 (4) | 0.0800 (4) | 0.1041 (2) | 0.0312 (9) | |
C1A | 0.6533 (6) | 0.3494 (6) | 0.1540 (3) | 0.0366 (15) | |
H4A | 0.6250 | 0.4204 | 0.1735 | 0.080* | |
C2A | 0.6887 (6) | 0.2585 (6) | 0.2001 (3) | 0.040 (2) | |
H5A | 0.7791 | 0.2871 | 0.2213 | 0.080* | |
H6A | 0.6900 | 0.1787 | 0.1800 | 0.080* | |
C3A | 0.5965 (6) | 0.2376 (6) | 0.2456 (2) | 0.0345 (14) | |
C4A | 0.3559 (6) | 0.1732 (6) | 0.2514 (3) | 0.037 (2) | |
H7A | 0.3432 | 0.2542 | 0.2668 | 0.080* | |
H8A | 0.3844 | 0.1244 | 0.2842 | 0.080* | |
C5A | 0.2288 (6) | 0.1092 (6) | 0.2143 (3) | 0.038 (2) | |
H9A | 0.1569 | 0.1025 | 0.2366 | 0.080* | |
H10A | 0.2400 | 0.0262 | 0.2008 | 0.080* | |
C6A | 0.0825 (6) | 0.1266 (6) | 0.1171 (3) | 0.038 (2) | |
H11A | 0.1104 | 0.0553 | 0.0976 | 0.080* | |
C7A | 0.0478 (6) | 0.2189 (7) | 0.0720 (3) | 0.044 (2) | |
H12A | 0.0433 | 0.2969 | 0.0930 | 0.080* | |
H13A | −0.0416 | 0.1894 | 0.0500 | 0.080* | |
C8A | 0.1393 (6) | 0.2466 (7) | 0.0278 (3) | 0.046 (2) | |
C9A | 0.3734 (7) | 0.3398 (6) | 0.0249 (3) | 0.044 (2) | |
H14A | 0.3821 | 0.2682 | 0.0001 | 0.080* | |
H15A | 0.3444 | 0.4038 | −0.0003 | 0.080* | |
C10A | 0.5032 (6) | 0.3863 (5) | 0.0628 (2) | 0.0335 (14) | |
H16A | 0.4981 | 0.4647 | 0.0833 | 0.080* | |
H17A | 0.5721 | 0.4001 | 0.0391 | 0.080* | |
C11A | 0.5694 (7) | 0.1785 (5) | 0.0764 (3) | 0.040 (2) | |
H18A | 0.6618 | 0.1681 | 0.0913 | 0.080* | |
H19A | 0.5602 | 0.1890 | 0.0345 | 0.080* | |
C12A | 0.4785 (7) | 0.0636 (6) | 0.0858 (2) | 0.0341 (15) | |
C13A | 0.7765 (6) | 0.3981 (7) | 0.1288 (3) | 0.052 (2) | |
H20A | 0.7526 | 0.4554 | 0.0996 | 0.080* | |
H21A | 0.8092 | 0.3298 | 0.1111 | 0.080* | |
H22A | 0.8452 | 0.4398 | 0.1598 | 0.080* | |
C14A | 0.6519 (7) | 0.1381 (7) | 0.2841 (3) | 0.050 (2) | |
H23A | 0.6483 | 0.0630 | 0.2602 | 0.080* | |
H24A | 0.5988 | 0.1218 | 0.3139 | 0.080* | |
H25A | 0.7431 | 0.1672 | 0.3025 | 0.080* | |
C15A | 0.6018 (7) | 0.3570 (6) | 0.2835 (3) | 0.048 (2) | |
H26A | 0.5671 | 0.4190 | 0.2593 | 0.080* | |
H27A | 0.6930 | 0.3863 | 0.3019 | 0.080* | |
H28A | 0.5486 | 0.3407 | 0.3132 | 0.080* | |
C16A | −0.0397 (7) | 0.0801 (7) | 0.1439 (3) | 0.052 (2) | |
H29A | −0.0158 | 0.0214 | 0.1723 | 0.080* | |
H30A | −0.1109 | 0.0406 | 0.1133 | 0.080* | |
H31A | −0.0688 | 0.1492 | 0.1627 | 0.080* | |
C17A | 0.1490 (8) | 0.1288 (8) | −0.0085 (3) | 0.065 (2) | |
H32A | 0.2071 | 0.1488 | −0.0359 | 0.080* | |
H33A | 0.0614 | 0.0941 | −0.0295 | 0.080* | |
H34A | 0.1846 | 0.0694 | 0.0172 | 0.080* | |
C18A | 0.0822 (8) | 0.3412 (9) | −0.0135 (3) | 0.080 (3) | |
H35A | 0.1392 | 0.3594 | −0.0416 | 0.080* | |
H36A | 0.0780 | 0.4162 | 0.0091 | 0.080* | |
H37A | −0.0062 | 0.3070 | −0.0338 | 0.080* | |
Zn1A | 0.47081 (8) | −0.20003 (7) | 0.11607 (3) | 0.0362 (2) | |
Cl2A | 0.6652 (2) | −0.2770 (2) | 0.12971 (8) | 0.0586 (5) | |
Cl3A | 0.4359 (2) | −0.1294 (2) | 0.20381 (7) | 0.0470 (4) | |
Cl4A | 0.3048 (2) | −0.3162 (2) | 0.05356 (8) | 0.0612 (5) | |
O2A | 0.5110 (5) | −0.0392 (4) | 0.0743 (2) | 0.0493 (13) | |
Co1B | 0.21427 (8) | 0.75133 (7) | 0.36890 (3) | 0.0250 (2) | |
Cl1B | 0.3095 (2) | 0.94735 (14) | 0.36482 (7) | 0.0376 (4) | |
N1B | 0.2059 (5) | 0.7626 (4) | 0.4553 (2) | 0.0316 (12) | |
N2B | 0.3899 (5) | 0.6827 (4) | 0.3828 (2) | 0.0295 (11) | |
H1B | 0.3643 | 0.6012 | 0.3880 | 0.080* | |
N3B | 0.2164 (5) | 0.7222 (4) | 0.2841 (2) | 0.0280 (11) | |
H2B | 0.2528 | 0.7954 | 0.2721 | 0.080* | |
N4B | 0.0377 (5) | 0.8190 (5) | 0.3556 (2) | 0.0323 (12) | |
H3B | 0.0629 | 0.9013 | 0.3519 | 0.080* | |
O1B | 0.1278 (4) | 0.5870 (3) | 0.3683 (2) | 0.0299 (9) | |
C1B | 0.3388 (7) | 0.8045 (6) | 0.4957 (3) | 0.042 (2) | |
H4B | 0.3734 | 0.8866 | 0.4843 | 0.080* | |
C2B | 0.4425 (7) | 0.7210 (7) | 0.4905 (3) | 0.045 (2) | |
H5B | 0.4022 | 0.6365 | 0.4940 | 0.080* | |
H6B | 0.5150 | 0.7423 | 0.5240 | 0.080* | |
C3B | 0.5050 (7) | 0.7212 (6) | 0.4347 (3) | 0.042 (2) | |
C4B | 0.4341 (6) | 0.6773 (6) | 0.3255 (2) | 0.038 (2) | |
H7B | 0.4990 | 0.6198 | 0.3257 | 0.080* | |
H8B | 0.4754 | 0.7588 | 0.3177 | 0.080* | |
C5B | 0.3115 (6) | 0.6338 (5) | 0.2796 (2) | 0.0335 (14) | |
H9B | 0.3343 | 0.6321 | 0.2408 | 0.080* | |
H10B | 0.2725 | 0.5507 | 0.2865 | 0.080* | |
C6B | 0.0845 (6) | 0.6837 (6) | 0.2433 (2) | 0.0359 (15) | |
H11B | 0.0426 | 0.6048 | 0.2551 | 0.080* | |
C7B | −0.0063 (7) | 0.7796 (6) | 0.2479 (3) | 0.041 (2) | |
H12B | −0.0773 | 0.7671 | 0.2134 | 0.080* | |
H13B | 0.0448 | 0.8608 | 0.2465 | 0.080* | |
C8B | −0.0712 (6) | 0.7825 (6) | 0.3020 (3) | 0.039 (2) | |
C9B | −0.0103 (7) | 0.8192 (6) | 0.4123 (3) | 0.043 (2) | |
H14B | −0.0572 | 0.7379 | 0.4171 | 0.080* | |
H15B | −0.0715 | 0.8798 | 0.4133 | 0.080* | |
C10B | 0.1102 (7) | 0.8519 (6) | 0.4606 (3) | 0.041 (2) | |
H16B | 0.1527 | 0.9359 | 0.4575 | 0.080* | |
H17B | 0.0832 | 0.8479 | 0.4986 | 0.080* | |
C11B | 0.1449 (7) | 0.6368 (5) | 0.4701 (3) | 0.038 (2) | |
H18B | 0.0674 | 0.6461 | 0.4877 | 0.080* | |
H19B | 0.2097 | 0.6033 | 0.4988 | 0.080* | |
C12B | 0.1028 (6) | 0.5474 (5) | 0.4167 (3) | 0.0291 (13) | |
C13B | 0.3242 (8) | 0.8202 (8) | 0.5605 (3) | 0.061 (2) | |
H20B | 0.2581 | 0.8737 | 0.5639 | 0.080* | |
H21B | 0.4087 | 0.8564 | 0.5839 | 0.080* | |
H22B | 0.2966 | 0.7404 | 0.5740 (3) | 0.080* | |
C14B | 0.5981 (7) | 0.6236 (7) | 0.4398 (3) | 0.053 (2) | |
H23B | 0.5481 | 0.5439 | 0.4431 | 0.080* | |
H24B | 0.6672 | 0.6443 | 0.4740 | 0.080* | |
H25B | 0.6379 | 0.6205 | 0.4054 | 0.080* | |
C15B | 0.5842 (7) | 0.8473 (7) | 0.4295 (3) | 0.056 (2) | |
H26B | 0.5251 | 0.9093 | 0.4262 | 0.080* | |
H27B | 0.6243 | 0.8443 | 0.3952 | 0.080* | |
H28B | 0.6531 | 0.8680 | 0.4639 | 0.080* | |
C16B | 0.1028 (7) | 0.6651 (7) | 0.1796 (2) | 0.053 (2) | |
H29B | 0.1610 | 0.6036 | 0.1769 | 0.080* | |
H30B | 0.1417 | 0.7423 | 0.1671 | 0.080* | |
H31B | 0.0172 | 0.6377 | 0.1548 | 0.080* | |
C17B | −0.1552 (7) | 0.6578 (7) | 0.3062 (3) | 0.058 (2) | |
H32B | −0.1954 | 0.6613 | 0.3405 | 0.080* | |
H33B | −0.0989 | 0.5936 | 0.3090 | 0.080* | |
H34B | −0.2243 | 0.6400 | 0.2718 | 0.080* | |
C18B | −0.1641 (7) | 0.8832 (7) | 0.2949 (4) | 0.062 (2) | |
H35B | −0.2067 | 0.8875 | 0.3285 | 0.080* | |
H36B | −0.2313 | 0.8626 | 0.2600 | 0.080* | |
H37B | −0.1124 | 0.9622 | 0.2919 | 0.080* | |
Zn1B | 0.10743 (8) | 0.30893 (7) | 0.36618 (3) | 0.0372 (2) | |
Cl2B | 0.0358 (2) | 0.3264 (2) | 0.27019 (8) | 0.0568 (5) | |
Cl3B | 0.3314 (2) | 0.3666 (2) | 0.38745 (7) | 0.0475 (4) | |
Cl4B | 0.0281 (3) | 0.1367 (2) | 0.40312 (11) | 0.0800 (7) | |
O2B | 0.0516 (5) | 0.4401 (4) | 0.4215 (2) | 0.0476 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1A | 0.0289 (4) | 0.0271 (4) | 0.0196 (4) | 0.0053 (3) | 0.0085 (3) | 0.0043 (3) |
Cl1A | 0.0507 (10) | 0.0314 (8) | 0.0405 (9) | 0.0111 (7) | 0.0160 (8) | 0.0002 (7) |
N1A | 0.023 (3) | 0.033 (3) | 0.024 (2) | −0.002 (2) | 0.010 (2) | 0.005 (2) |
N2A | 0.030 (3) | 0.030 (3) | 0.022 (2) | 0.008 (2) | 0.007 (2) | 0.004 (2) |
N3A | 0.029 (3) | 0.036 (3) | 0.027 (3) | 0.006 (2) | 0.012 (2) | 0.005 (2) |
N4A | 0.033 (3) | 0.037 (3) | 0.026 (3) | 0.002 (2) | 0.002 (2) | 0.008 (2) |
O1A | 0.038 (2) | 0.032 (2) | 0.026 (2) | 0.005 (2) | 0.011 (2) | 0.002 (2) |
C1A | 0.029 (3) | 0.044 (4) | 0.036 (3) | −0.002 (3) | 0.010 (3) | 0.007 (3) |
C2A | 0.026 (3) | 0.057 (4) | 0.038 (4) | 0.007 (3) | 0.005 (3) | 0.012 (3) |
C3A | 0.034 (4) | 0.042 (4) | 0.025 (3) | 0.002 (3) | 0.002 (3) | 0.004 (3) |
C4A | 0.044 (4) | 0.046 (4) | 0.026 (3) | 0.012 (3) | 0.014 (3) | 0.009 (3) |
C5A | 0.039 (4) | 0.045 (4) | 0.034 (3) | 0.005 (3) | 0.015 (3) | 0.011 (3) |
C6A | 0.032 (4) | 0.046 (4) | 0.037 (4) | 0.000 (3) | 0.011 (3) | 0.001 (3) |
C7A | 0.025 (4) | 0.064 (5) | 0.040 (4) | 0.002 (3) | −0.001 (3) | 0.009 (3) |
C8A | 0.034 (4) | 0.065 (5) | 0.035 (4) | 0.001 (4) | 0.001 (3) | 0.016 (3) |
C9A | 0.055 (5) | 0.047 (4) | 0.030 (3) | 0.000 (4) | 0.010 (3) | 0.016 (3) |
C10A | 0.041 (4) | 0.032 (3) | 0.027 (3) | −0.005 (3) | 0.010 (3) | 0.010 (3) |
C11A | 0.055 (4) | 0.032 (3) | 0.042 (4) | 0.016 (3) | 0.024 (3) | 0.008 (3) |
C12A | 0.054 (4) | 0.037 (4) | 0.013 (3) | 0.009 (3) | 0.010 (3) | 0.004 (2) |
C13A | 0.023 (4) | 0.065 (5) | 0.064 (5) | −0.010 (3) | 0.011 (3) | 0.017 (4) |
C14A | 0.046 (4) | 0.064 (5) | 0.038 (4) | 0.010 (4) | 0.001 (3) | 0.017 (3) |
C15A | 0.044 (4) | 0.054 (4) | 0.040 (4) | −0.006 (4) | 0.003 (3) | −0.003 (3) |
C16A | 0.034 (4) | 0.071 (5) | 0.049 (4) | −0.002 (4) | 0.014 (3) | −0.003 (4) |
C17A | 0.077 (6) | 0.079 (6) | 0.032 (4) | −0.028 (5) | 0.018 (4) | −0.002 (4) |
C18A | 0.051 (5) | 0.129 (8) | 0.053 (5) | 0.010 (5) | −0.012 (4) | 0.044 (5) |
Zn1A | 0.0464 (5) | 0.0364 (4) | 0.0287 (4) | 0.0065 (4) | 0.0141 (3) | 0.0045 (3) |
Cl2A | 0.0549 (12) | 0.0732 (13) | 0.0503 (11) | 0.0249 (10) | 0.0069 (9) | 0.0002 (10) |
Cl3A | 0.0752 (13) | 0.0415 (9) | 0.0319 (8) | 0.0116 (9) | 0.0261 (8) | 0.0092 (7) |
Cl4A | 0.0536 (12) | 0.0865 (15) | 0.0382 (10) | −0.0090 (11) | 0.0096 (9) | −0.0031 (10) |
O2A | 0.092 (4) | 0.028 (2) | 0.043 (3) | 0.021 (3) | 0.041 (3) | 0.013 (2) |
Co1B | 0.0324 (5) | 0.0250 (4) | 0.0196 (4) | 0.0039 (4) | 0.0097 (3) | 0.0054 (3) |
Cl1B | 0.0483 (10) | 0.0289 (8) | 0.0364 (8) | −0.0014 (7) | 0.0140 (7) | 0.0063 (6) |
N1B | 0.046 (3) | 0.026 (3) | 0.026 (3) | −0.001 (2) | 0.017 (2) | 0.001 (2) |
N2B | 0.036 (3) | 0.033 (3) | 0.020 (2) | 0.003 (2) | 0.008 (2) | 0.007 (2) |
N3B | 0.034 (3) | 0.030 (3) | 0.020 (2) | −0.002 (2) | 0.006 (2) | 0.008 (2) |
N4B | 0.039 (3) | 0.031 (3) | 0.031 (3) | 0.011 (2) | 0.013 (2) | 0.005 (2) |
O1B | 0.038 (2) | 0.027 (2) | 0.027 (2) | 0.001 (2) | 0.014 (2) | 0.006 (2) |
C1B | 0.057 (5) | 0.040 (4) | 0.026 (3) | 0.001 (3) | 0.006 (3) | −0.002 (3) |
C2B | 0.050 (4) | 0.064 (5) | 0.021 (3) | 0.013 (4) | 0.003 (3) | 0.015 (3) |
C3B | 0.042 (4) | 0.053 (4) | 0.030 (3) | 0.007 (3) | 0.003 (3) | 0.011 (3) |
C4B | 0.041 (4) | 0.049 (4) | 0.030 (3) | 0.013 (3) | 0.014 (3) | 0.010 (3) |
C5B | 0.048 (4) | 0.032 (3) | 0.025 (3) | 0.010 (3) | 0.015 (3) | 0.008 (3) |
C6B | 0.039 (4) | 0.045 (4) | 0.020 (3) | −0.005 (3) | 0.006 (3) | −0.001 (3) |
C7B | 0.045 (4) | 0.048 (4) | 0.030 (3) | 0.006 (3) | 0.006 (3) | 0.014 (3) |
C8B | 0.026 (3) | 0.047 (4) | 0.045 (4) | 0.007 (3) | 0.005 (3) | 0.004 (3) |
C9B | 0.048 (4) | 0.048 (4) | 0.043 (4) | 0.018 (3) | 0.027 (3) | 0.009 (3) |
C10B | 0.064 (5) | 0.037 (4) | 0.031 (3) | 0.016 (3) | 0.021 (3) | −0.002 (3) |
C11B | 0.062 (5) | 0.029 (3) | 0.027 (3) | 0.010 (3) | 0.015 (3) | 0.006 (3) |
C12B | 0.036 (4) | 0.022 (3) | 0.033 (3) | 0.008 (3) | 0.012 (3) | 0.005 (3) |
C13B | 0.077 (6) | 0.072 (5) | 0.029 (4) | −0.002 (5) | 0.007 (4) | −0.001 (4) |
C14B | 0.041 (4) | 0.077 (5) | 0.046 (4) | 0.019 (4) | 0.008 (3) | 0.019 (4) |
C15B | 0.048 (5) | 0.063 (5) | 0.050 (4) | −0.007 (4) | 0.006 (4) | 0.000 (4) |
C16B | 0.059 (5) | 0.082 (6) | 0.016 (3) | 0.006 (4) | 0.004 (3) | 0.003 (3) |
C17B | 0.046 (5) | 0.070 (5) | 0.056 (5) | 0.003 (4) | 0.013 (4) | 0.003 (4) |
C18B | 0.048 (5) | 0.074 (6) | 0.069 (5) | 0.027 (4) | 0.007 (4) | 0.009 (4) |
Zn1B | 0.0461 (5) | 0.0331 (4) | 0.0349 (4) | 0.0047 (4) | 0.0151 (3) | 0.0031 (3) |
Cl2B | 0.0502 (11) | 0.0730 (13) | 0.0405 (10) | 0.0086 (10) | −0.0067 (8) | −0.0067 (9) |
Cl3B | 0.0425 (10) | 0.0542 (11) | 0.0427 (10) | 0.0107 (8) | −0.0036 (8) | 0.0059 (8) |
Cl4B | 0.117 (2) | 0.0380 (11) | 0.107 (2) | 0.0138 (12) | 0.073 (2) | 0.0201 (11) |
O2B | 0.072 (3) | 0.027 (2) | 0.054 (3) | 0.001 (2) | 0.041 (3) | 0.006 (2) |
Co1A—O1A | 1.909 (4) | Co1B—O1B | 1.885 (4) |
Co1A—N3A | 1.983 (4) | Co1B—N3B | 1.981 (4) |
Co1A—N2A | 2.004 (4) | Co1B—N2B | 2.016 (5) |
Co1A—N4A | 2.006 (5) | Co1B—N1B | 2.018 (4) |
Co1A—N1A | 2.012 (4) | Co1B—N4B | 2.020 (5) |
Co1A—Cl1A | 2.219 (2) | Co1B—Cl1B | 2.237 (2) |
N1A—C11A | 1.496 (7) | N1B—C10B | 1.484 (7) |
N1A—C10A | 1.499 (7) | N1B—C11B | 1.507 (7) |
N1A—C1A | 1.508 (7) | N1B—C1B | 1.509 (8) |
N2A—C4A | 1.485 (7) | N2B—C4B | 1.478 (7) |
N2A—C3A | 1.508 (7) | N2B—C3B | 1.526 (8) |
N2A—H1A | 0.91 | N2B—H1B | 0.91 |
N3A—C6A | 1.491 (8) | N3B—C5B | 1.469 (7) |
N3A—C5A | 1.498 (7) | N3B—C6B | 1.500 (7) |
N3A—H2A | 0.91 | N3B—H2B | 0.91 |
N4A—C9A | 1.470 (7) | N4B—C9B | 1.484 (7) |
N4A—C8A | 1.504 (8) | N4B—C8B | 1.510 (8) |
N4A—H3A | 0.91 | N4B—H3B | 0.91 |
O1A—C12A | 1.278 (7) | O1B—C12B | 1.275 (6) |
C1A—C2A | 1.515 (8) | C1B—C2B | 1.503 (9) |
C1A—C13A | 1.527 (8) | C1B—C13B | 1.540 (8) |
C1A—H4A | 0.98 | C1B—H4B | 0.98 |
C2A—C3A | 1.542 (8) | C2B—C3B | 1.541 (8) |
C2A—H5A | 0.97 | C2B—H5B | 0.97 |
C2A—H6A | 0.97 | C2B—H6B | 0.97 |
C3A—C15A | 1.524 (9) | C3B—C14B | 1.513 (9) |
C3A—C14A | 1.534 (8) | C3B—C15B | 1.519 (9) |
C4A—C5A | 1.491 (9) | C4B—C5B | 1.500 (8) |
C4A—H7A | 0.97 | C4B—H7B | 0.97 |
C4A—H8A | 0.97 | C4B—H8B | 0.97 |
C5A—H9A | 0.97 | C5B—H9B | 0.97 |
C5A—H10A | 0.97 | C5B—H10B | 0.97 |
C6A—C7A | 1.510 (9) | C6B—C7B | 1.499 (9) |
C6A—C16A | 1.531 (8) | C6B—C16B | 1.528 (7) |
C6A—H11A | 0.98 | C6B—H11B | 0.98 |
C7A—C8A | 1.521 (9) | C7B—C8B | 1.522 (8) |
C7A—H12A | 0.97 | C7B—H12B | 0.97 |
C7A—H13A | 0.97 | C7B—H13B | 0.97 |
C8A—C17A | 1.526 (10) | C8B—C17B | 1.524 (9) |
C8A—C18A | 1.535 (10) | C8B—C18B | 1.538 (9) |
C9A—C10A | 1.468 (8) | C9B—C10B | 1.501 (9) |
C9A—H14A | 0.97 | C9B—H14B | 0.97 |
C9A—H15A | 0.97 | C9B—H15B | 0.97 |
C10A—H16A | 0.97 | C10B—H16B | 0.97 |
C10A—H17A | 0.97 | C10B—H17B | 0.97 |
C11A—C12A | 1.505 (8) | C11B—C12B | 1.501 (8) |
C11A—H18A | 0.97 | C11B—H18B | 0.97 |
C11A—H19A | 0.97 | C11B—H19B | 0.97 |
C12A—O2A | 1.240 (7) | C12B—O2B | 1.232 (7) |
C13A—H20A | 0.96 | C13B—H20B | 0.96 |
C13A—H21A | 0.96 | C13B—H21B | 0.96 |
C13A—H22A | 0.96 | C13B—H22B | 0.96 |
C14A—H23A | 0.96 | C14B—H23B | 0.96 |
C14A—H24A | 0.96 | C14B—H24B | 0.96 |
C14A—H25A | 0.96 | C14B—H25B | 0.96 |
C15A—H26A | 0.96 | C15B—H26B | 0.96 |
C15A—H27A | 0.96 | C15B—H27B | 0.96 |
C15A—H28A | 0.96 | C15B—H28B | 0.96 |
C16A—H29A | 0.96 | C16B—H29B | 0.96 |
C16A—H30A | 0.96 | C16B—H30B | 0.96 |
C16A—H31A | 0.96 | C16B—H31B | 0.96 |
C17A—H32A | 0.96 | C17B—H32B | 0.96 |
C17A—H33A | 0.96 | C17B—H33B | 0.96 |
C17A—H34A | 0.96 | C17B—H34B | 0.96 |
C18A—H35A | 0.96 | C18B—H35B | 0.96 |
C18A—H36A | 0.96 | C18B—H36B | 0.96 |
C18A—H37A | 0.96 | C18B—H37B | 0.96 |
Zn1A—O2A | 2.066 (4) | Zn1B—O2B | 2.080 (4) |
Zn1A—Cl4A | 2.229 (2) | Zn1B—Cl4B | 2.211 (2) |
Zn1A—Cl2A | 2.237 (2) | Zn1B—Cl2B | 2.237 (2) |
Zn1A—Cl3A | 2.247 (2) | Zn1B—Cl3B | 2.254 (2) |
O1A—Co1A—N3A | 90.8 (2) | O1B—Co1B—N3B | 88.9 (2) |
O1A—Co1A—N2A | 86.2 (2) | O1B—Co1B—N2B | 87.7 (2) |
N3A—Co1A—N2A | 85.7 (2) | N3B—Co1B—N2B | 85.7 (2) |
O1A—Co1A—N4A | 95.5 (2) | O1B—Co1B—N1B | 85.5 (2) |
N3A—Co1A—N4A | 93.3 (2) | N3B—Co1B—N1B | 174.2 (2) |
N2A—Co1A—N4A | 178.0 (2) | N2B—Co1B—N1B | 93.1 (2) |
O1A—Co1A—N1A | 86.0 (2) | O1B—Co1B—N4B | 91.9 (2) |
N3A—Co1A—N1A | 176.6 (2) | N3B—Co1B—N4B | 94.6 (2) |
N2A—Co1A—N1A | 95.4 (2) | N2B—Co1B—N4B | 179.4 (2) |
N4A—Co1A—N1A | 85.8 (2) | N1B—Co1B—N4B | 86.5 (2) |
O1A—Co1A—Cl1A | 178.3 (1) | O1B—Co1B—Cl1B | 176.8 (1) |
N3A—Co1A—Cl1A | 88.0 (1) | N3B—Co1B—Cl1B | 88.8 (1) |
N2A—Co1A—Cl1A | 92.6 (1) | N2B—Co1B—Cl1B | 94.3 (1) |
N4A—Co1A—Cl1A | 85.7 (2) | N1B—Co1B—Cl1B | 96.9 (1) |
N1A—Co1A—Cl1A | 95.2 (1) | N4B—Co1B—Cl1B | 86.1 (2) |
C11A—N1A—C10A | 110.5 (4) | C10B—N1B—C11B | 108.4 (5) |
C11A—N1A—C1A | 111.4 (5) | C10B—N1B—C1B | 110.9 (5) |
C10A—N1A—C1A | 109.8 (4) | C11B—N1B—C1B | 110.6 (5) |
C11A—N1A—Co1A | 107.3 (3) | C10B—N1B—Co1B | 104.4 (4) |
C10A—N1A—Co1A | 104.4 (3) | C11B—N1B—Co1B | 107.5 (3) |
C1A—N1A—Co1A | 113.1 (3) | C1B—N1B—Co1B | 114.7 (4) |
C4A—N2A—C3A | 113.4 (4) | C4B—N2B—C3B | 113.3 (5) |
C4A—N2A—Co1A | 106.6 (3) | C4B—N2B—Co1B | 106.6 (3) |
C3A—N2A—Co1A | 125.4 (3) | C3B—N2B—Co1B | 125.5 (4) |
C4A—N2A—H1A | 102.8 | C4B—N2B—H1B | 102.8 |
C3A—N2A—H1A | 102.8 | C3B—N2B—H1B | 102.8 |
Co1A—N2A—H1A | 102.8 | Co1B—N2B—H1B | 102.8 |
C6A—N3A—C5A | 113.5 (5) | C5B—N3B—C6B | 112.2 (5) |
C6A—N3A—Co1A | 116.9 (3) | C5B—N3B—Co1B | 106.7 (3) |
C5A—N3A—Co1A | 107.7 (3) | C6B—N3B—Co1B | 117.7 (3) |
C6A—N3A—H2A | 106.0 | C5B—N3B—H2B | 106.5 |
C5A—N3A—H2A | 106.0 | C6B—N3B—H2B | 106.5 |
Co1A—N3A—H2A | 106.0 | Co1B—N3B—H2B | 106.5 |
C9A—N4A—C8A | 113.7 (5) | C9B—N4B—C8B | 114.5 (5) |
C9A—N4A—Co1A | 108.9 (4) | C9B—N4B—Co1B | 107.3 (4) |
C8A—N4A—Co1A | 124.8 (4) | C8B—N4B—Co1B | 123.6 (4) |
C9A—N4A—H3A | 101.9 | C9B—N4B—H3B | 102.8 |
C8A—N4A—H3A | 101.9 | C8B—N4B—H3B | 102.8 |
Co1A—N4A—H3A | 101.8 | Co1B—N4B—H3B | 102.8 |
C12A—O1A—Co1A | 115.5 (4) | C12B—O1B—Co1B | 118.2 (4) |
N1A—C1A—C2A | 111.5 (5) | C2B—C1B—N1B | 113.6 (5) |
N1A—C1A—C13A | 111.8 (5) | C2B—C1B—C13B | 109.4 (6) |
C2A—C1A—C13A | 110.4 (5) | N1B—C1B—C13B | 112.1 (6) |
N1A—C1A—H4A | 107.7 | C2B—C1B—H4B | 107.1 |
C2A—C1A—H4A | 107.7 | N1B—C1B—H4B | 107.1 |
C13A—C1A—H4A | 107.7 | C13B—C1B—H4B | 107.1 |
C1A—C2A—C3A | 117.1 (5) | C1B—C2B—C3B | 118.9 (5) |
C1A—C2A—H5A | 108.0 | C1B—C2B—H5B | 107.6 |
C3A—C2A—H5A | 108.0 | C3B—C2B—H5B | 107.6 |
C1A—C2A—H6A | 108.0 | C1B—C2B—H6B | 107.6 |
C3A—C2A—H6A | 108.0 | C3B—C2B—H6B | 107.6 |
H5A—C2A—H6A | 107.3 | H5B—C2B—H6B | 107.0 |
N2A—C3A—C15A | 113.6 (5) | C14B—C3B—C15B | 109.4 (6) |
N2A—C3A—C14A | 108.8 (5) | C14B—C3B—N2B | 109.0 (5) |
C15A—C3A—C14A | 109.7 (5) | C15B—C3B—N2B | 113.0 (5) |
N2A—C3A—C2A | 108.1 (5) | C14B—C3B—C2B | 107.4 (5) |
C15A—C3A—C2A | 110.7 (5) | C15B—C3B—C2B | 111.1 (6) |
C14A—C3A—C2A | 105.6 (5) | N2B—C3B—C2B | 106.7 (5) |
N2A—C4A—C5A | 106.7 (5) | N2B—C4B—C5B | 106.9 (5) |
N2A—C4A—H7A | 110.4 | N2B—C4B—H7B | 110.3 |
C5A—C4A—H7A | 110.4 | C5B—C4B—H7B | 110.3 |
N2A—C4A—H8A | 110.4 | N2B—C4B—H8B | 110.3 |
C5A—C4A—H8A | 110.4 | C5B—C4B—H8B | 110.3 |
H7A—C4A—H8A | 108.6 | H7B—C4B—H8B | 108.6 |
C4A—C5A—N3A | 106.7 (5) | N3B—C5B—C4B | 106.9 (5) |
C4A—C5A—H9A | 110.4 | N3B—C5B—H9B | 110.3 |
N3A—C5A—H9A | 110.4 | C4B—C5B—H9B | 110.3 |
C4A—C5A—H10A | 110.4 | N3B—C5B—H10B | 110.3 |
N3A—C5A—H10A | 110.4 | C4B—C5B—H10B | 110.3 |
H9A—C5A—H10A | 108.6 | H9B—C5B—H10B | 108.6 |
N3A—C6A—C7A | 108.8 (5) | C7B—C6B—N3B | 109.9 (5) |
N3A—C6A—C16A | 111.5 (5) | C7B—C6B—C16B | 109.8 (5) |
C7A—C6A—C16A | 110.6 (6) | N3B—C6B—C16B | 111.5 (5) |
N3A—C6A—H11A | 108.6 | C7B—C6B—H11B | 108.5 |
C7A—C6A—H11A | 108.6 | N3B—C6B—H11B | 108.5 |
C16A—C6A—H11A | 108.6 | C16B—C6B—H11B | 108.5 |
C6A—C7A—C8A | 118.5 (6) | C6B—C7B—C8B | 117.3 (5) |
C6A—C7A—H12A | 107.7 | C6B—C7B—H12B | 108.0 |
C8A—C7A—H12A | 107.7 | C8B—C7B—H12B | 108.0 |
C6A—C7A—H13A | 107.7 | C6B—C7B—H13B | 108.0 |
C8A—C7A—H13A | 107.7 | C8B—C7B—H13B | 108.0 |
H12A—C7A—H13A | 107.1 | H12B—C7B—H13B | 107.2 |
N4A—C8A—C7A | 107.3 (5) | N4B—C8B—C7B | 108.5 (5) |
N4A—C8A—C17A | 111.6 (6) | N4B—C8B—C17B | 112.7 (5) |
C7A—C8A—C17A | 111.1 (6) | C7B—C8B—C17B | 110.6 (6) |
N4A—C8A—C18A | 108.8 (6) | N4B—C8B—C18B | 108.9 (5) |
C7A—C8A—C18A | 108.7 (6) | C7B—C8B—C18B | 107.3 (6) |
C17A—C8A—C18A | 109.2 (6) | C17B—C8B—C18B | 108.7 (6) |
C10A—C9A—N4A | 109.0 (5) | N4B—C9B—C10B | 107.6 (5) |
C10A—C9A—H14A | 109.9 | N4B—C9B—H14B | 110.2 |
N4A—C9A—H14A | 109.9 | C10B—C9B—H14B | 110.2 |
C10A—C9A—H15A | 109.9 | N4B—C9B—H15B | 110.2 |
N4A—C9A—H15A | 109.9 | C10B—C9B—H15B | 110.2 |
H14A—C9A—H15A | 108.3 | H14B—C9B—H15B | 108.5 |
C9A—C10A—N1A | 109.0 (5) | N1B—C10B—C9B | 108.8 (5) |
C9A—C10A—H16A | 109.9 | N1B—C10B—H16B | 109.9 |
N1A—C10A—H16A | 109.9 | C9B—C10B—H16B | 109.9 |
C9A—C10A—H17A | 109.9 | N1B—C10B—H17B | 109.9 |
N1A—C10A—H17A | 109.9 | C9B—C10B—H17B | 109.9 |
H16A—C10A—H17A | 108.3 | H16B—C10B—H17B | 108.3 |
N1A—C11A—C12A | 111.8 (5) | N1B—C11B—C12B | 111.9 (5) |
N1A—C11A—H18A | 109.2 | N1B—C11B—H18B | 109.2 |
C12A—C11A—H18A | 109.2 | C12B—C11B—H18B | 109.2 |
N1A—C11A—H19A | 109.2 | N1B—C11B—H19B | 109.2 |
C12A—C11A—H19A | 109.2 | C12B—C11B—H19B | 109.2 |
H18A—C11A—H19A | 107.9 | H18B—C11B—H19B | 107.9 |
O2A—C12A—O1A | 124.8 (6) | O2B—C12B—O1B | 123.2 (5) |
O2A—C12A—C11A | 118.2 (6) | O2B—C12B—C11B | 120.0 (5) |
O1A—C12A—C11A | 116.9 (5) | O1B—C12B—C11B | 116.7 (5) |
C1A—C13A—H20A | 109.5 | C1B—C13B—H20B | 109.5 |
C1A—C13A—H21A | 109.5 | C1B—C13B—H21B | 109.5 |
H20A—C13A—H21A | 109.5 | H20B—C13B—H21B | 109.5 |
C1A—C13A—H22A | 109.5 | C1B—C13B—H22B | 109.5 |
H20A—C13A—H22A | 109.5 | H20B—C13B—H22B | 109.5 |
H21A—C13A—H22A | 109.5 | H21B—C13B—H22B | 109.5 |
C3A—C14A—H23A | 109.5 | C3B—C14B—H23B | 109.5 |
C3A—C14A—H24A | 109.5 | C3B—C14B—H24B | 109.5 |
H23A—C14A—H24A | 109.5 | H23B—C14B—H24B | 109.5 |
C3A—C14A—H25A | 109.5 | C3B—C14B—H25B | 109.5 |
H23A—C14A—H25A | 109.5 | H23B—C14B—H25B | 109.5 |
H24A—C14A—H25A | 109.5 | H24B—C14B—H25B | 109.5 |
C3A—C15A—H26A | 109.5 | C3B—C15B—H26B | 109.5 |
C3A—C15A—H27A | 109.5 | C3B—C15B—H27B | 109.5 |
H26A—C15A—H27A | 109.5 | H26B—C15B—H27B | 109.5 |
C3A—C15A—H28A | 109.5 | C3B—C15B—H28B | 109.5 |
H26A—C15A—H28A | 109.5 | H26B—C15B—H28B | 109.5 |
H27A—C15A—H28A | 109.5 | H27B—C15B—H28B | 109.5 |
C6A—C16A—H29A | 109.5 | C6B—C16B—H29B | 109.5 |
C6A—C16A—H30A | 109.5 | C6B—C16B—H30B | 109.5 |
H29A—C16A—H30A | 109.5 | H29B—C16B—H30B | 109.5 |
C6A—C16A—H31A | 109.5 | C6B—C16B—H31B | 109.5 |
H29A—C16A—H31A | 109.5 | H29B—C16B—H31B | 109.5 |
H30A—C16A—H31A | 109.5 | H30B—C16B—H31B | 109.5 |
C8A—C17A—H32A | 109.5 | C8B—C17B—H32B | 109.5 |
C8A—C17A—H33A | 109.5 | C8B—C17B—H33B | 109.5 |
H32A—C17A—H33A | 109.5 | H32B—C17B—H33B | 109.5 |
C8A—C17A—H34A | 109.5 | C8B—C17B—H34B | 109.5 |
H32A—C17A—H34A | 109.5 | H32B—C17B—H34B | 109.5 |
H33A—C17A—H34A | 109.5 | H33B—C17B—H34B | 109.5 |
C8A—C18A—H35A | 109.5 | C8B—C18B—H35B | 109.5 |
C8A—C18A—H36A | 109.5 | C8B—C18B—H36B | 109.5 |
H35A—C18A—H36A | 109.5 | H35B—C18B—H36B | 109.5 |
C8A—C18A—H37A | 109.5 | C8B—C18B—H37B | 109.5 |
H35A—C18A—H37A | 109.5 | H35B—C18B—H37B | 109.5 |
H36A—C18A—H37A | 109.5 | H36B—C18B—H37B | 109.5 |
O2A—Zn1A—Cl4A | 104.8 (2) | O2B—Zn1B—Cl4B | 99.7 (1) |
O2A—Zn1A—Cl2A | 103.8 (1) | O2B—Zn1B—Cl2B | 114.6 (1) |
Cl4A—Zn1A—Cl2A | 114.4 (1) | Cl4B—Zn1B—Cl2B | 116.7 (1) |
O2A—Zn1A—Cl3A | 103.3 (1) | O2B—Zn1B—Cl3B | 98.8 (1) |
Cl4A—Zn1A—Cl3A | 120.0 (1) | Cl4B—Zn1B—Cl3B | 116.8 (1) |
Cl2A—Zn1A—Cl3A | 108.6 (1) | Cl2B—Zn1B—Cl3B | 108.7 (1) |
C12A—O2A—Zn1A | 126.5 (4) | C12B—O2B—Zn1B | 113.5 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
N2A—H1A···CL3A | 0.91 | 2.53 | 3.406 (5) | 160 |
N3A—H2A···CL2B | 0.91 | 2.88 | 3.608 (5) | 138 |
N3A—H2A···CL1A | 0.91 | 2.54 | 2.923 (5) | 106 |
N4A—H3A···CL1A | 0.91 | 2.43 | 2.878 (5) | 111 |
N2B—H1B···CL3B | 0.91 | 2.53 | 3.420 (5) | 167 |
N3B—H2B···CL1B | 0.91 | 2.58 | 2.957 (5) | 105 |
N3B—H2B···CL3Ai | 0.91 | 2.73 | 3.454 (5) | 137 |
N4B—H3B···CL4Bi | 0.91 | 2.87 | 3.599 (5) | 139 |
N4B—H3B···CL1B | 0.91 | 2.47 | 2.911 (5) | 110 |
Symmetry code: (i) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [CoZnCl4(C18H37N4O2)] |
Mr | 607.62 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 10.242 (1), 10.874 (2), 23.168 (5) |
α, β, γ (°) | 92.50 (2), 100.39 (2), 97.60 (2) |
V (Å3) | 2509.6 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.07 |
Crystal size (mm) | 0.28 × 0.18 × 0.11 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.656, 0.798 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9300, 8792, 5321 |
Rint | 0.061 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.052, 0.131, 0.93 |
No. of reflections | 8792 |
No. of parameters | 541 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.86, −0.68 |
Computer programs: CAD-4 Software (Enraf-Nonius, 1989), CAD-4 Software, NRCVAX (Gabe, et al., 1989), SHELXS86 (Sheldrick, 1985), SHELXL93 (Sheldrick, 1993), NRCVAX (Gabe et al., 1989), SHELXL93.
Co1A—O1A | 1.909 (4) | Co1B—O1B | 1.885 (4) |
Co1A—N3A | 1.983 (4) | Co1B—N3B | 1.981 (4) |
Co1A—N2A | 2.004 (4) | Co1B—N2B | 2.016 (5) |
Co1A—N4A | 2.006 (5) | Co1B—N1B | 2.018 (4) |
Co1A—N1A | 2.012 (4) | Co1B—N4B | 2.020 (5) |
Co1A—Cl1A | 2.219 (2) | Co1B—Cl1B | 2.237 (2) |
Zn1A—O2A | 2.066 (4) | Zn1B—O2B | 2.080 (4) |
Zn1A—Cl4A | 2.229 (2) | Zn1B—Cl4B | 2.211 (2) |
Zn1A—Cl2A | 2.237 (2) | Zn1B—Cl2B | 2.237 (2) |
Zn1A—Cl3A | 2.247 (2) | Zn1B—Cl3B | 2.254 (2) |
O1A—Co1A—N3A | 90.8 (2) | O1B—Co1B—N3B | 88.9 (2) |
O1A—Co1A—N2A | 86.2 (2) | O1B—Co1B—N2B | 87.7 (2) |
N3A—Co1A—N2A | 85.7 (2) | N3B—Co1B—N2B | 85.7 (2) |
O1A—Co1A—N4A | 95.5 (2) | O1B—Co1B—N1B | 85.5 (2) |
N3A—Co1A—N4A | 93.3 (2) | N3B—Co1B—N1B | 174.2 (2) |
N2A—Co1A—N4A | 178.0 (2) | N2B—Co1B—N1B | 93.1 (2) |
O1A—Co1A—N1A | 86.0 (2) | O1B—Co1B—N4B | 91.9 (2) |
N3A—Co1A—N1A | 176.6 (2) | N3B—Co1B—N4B | 94.6 (2) |
N2A—Co1A—N1A | 95.4 (2) | N2B—Co1B—N4B | 179.4 (2) |
N4A—Co1A—N1A | 85.8 (2) | N1B—Co1B—N4B | 86.5 (2) |
O1A—Co1A—Cl1A | 178.3 (1) | O1B—Co1B—Cl1B | 176.8 (1) |
N3A—Co1A—Cl1A | 88.0 (1) | N3B—Co1B—Cl1B | 88.8 (1) |
N2A—Co1A—Cl1A | 92.6 (1) | N2B—Co1B—Cl1B | 94.3 (1) |
N4A—Co1A—Cl1A | 85.7 (2) | N1B—Co1B—Cl1B | 96.9 (1) |
N1A—Co1A—Cl1A | 95.2 (1) | N4B—Co1B—Cl1B | 86.1 (2) |
O2A—Zn1A—Cl4A | 104.8 (2) | O2B—Zn1B—Cl4B | 99.7 (1) |
O2A—Zn1A—Cl2A | 103.8 (1) | O2B—Zn1B—Cl2B | 114.6 (1) |
Cl4A—Zn1A—Cl2A | 114.4 (1) | Cl4B—Zn1B—Cl2B | 116.7 (1) |
O2A—Zn1A—Cl3A | 103.3 (1) | O2B—Zn1B—Cl3B | 98.8 (1) |
Cl4A—Zn1A—Cl3A | 120.0 (1) | Cl4B—Zn1B—Cl3B | 116.8 (1) |
Cl2A—Zn1A—Cl3A | 108.6 (1) | Cl2B—Zn1B—Cl3B | 108.7 (1) |
D—H···A | D—H | H···A | D···A | D—H···A |
N2A—H1A···CL3A | 0.91 | 2.53 | 3.406 (5) | 159.6 |
N3A—H2A···CL2B | 0.91 | 2.88 | 3.608 (5) | 138.3 |
N3A—H2A···CL1A | 0.91 | 2.54 | 2.923 (5) | 105.5 |
N4A—H3A···CL1A | 0.91 | 2.43 | 2.878 (5) | 110.8 |
N2B—H1B···CL3B | 0.91 | 2.53 | 3.420 (5) | 166.8 |
N3B—H2B···CL1B | 0.91 | 2.58 | 2.957 (5) | 105.4 |
N3B—H2B···CL3Ai | 0.91 | 2.73 | 3.454 (5) | 137.0 |
N4B—H3B···CL4Bi | 0.91 | 2.87 | 3.599 (5) | 138.5 |
N4B—H3B···CL1B | 0.91 | 2.47 | 2.911 (5) | 110.2 |
Symmetry code: (i) x, y+1, z. |
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Metal complexes of polyaza macrocycles with additional pendant functional groups have attracted interest owing to their diverse applications in fundamental and applied science (Bernhardt & Lawrance, 1990; Kaden, 1993). The coordination behaviour of NiII and CuII ions with C-meso-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane- N-acetate has been studied chemically and crystallographically (Panneerselvam et al., 1998; Xu et al., 1988). In this study, we present the crystal structure of the title compound, (I), to expand the knowledge of this area.
The X-ray structure shows that an asymmetric unit contains two independent molecules (denoted as molecules A and B). The two molecules have almost identical bond lengths and angles. In both molecules, the C-meso-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-N-acetate acts as a bridging ligand between the CoIII and ZnII ions. The CoIII ion is six-coordinate in a nearly octahedral environment provided by one Cl atom, four N atoms of the bridging ligand, and one O atom. The macrocyclic moiety adopts a conformation in which the two six-membered rings are in a chair form and the two five-membered rings are in a gauche form. This combination of these four chelate rings has been found in several similar crystal stuctures (Clay et al., 1979; Panneerselvam et al., 1998; Tasker & Sklar, 1975). The Co—N distances [1.981 (4)–2.020 (5) Å] are longer than those in the trans-dichloro(1,4,8,11-tetraazacyclotetradecane)cobalt(III) cation [1.978 (4) Å; Sosa-Torres & Toscano, 1997] and the [1,4-N,N'-bis(carboxymethyl)-1,4,8,11-tetraazacyclotetradecane]cobalt(III) cation [1.969 (4) Å; Ware et al., 1996]. The Co—O distances [1.885 (4) and 1.909 (4) Å] agree with the corresponding values found in the [1,4-N,N'-bis(carboxymethyl)-1,4,8,11-tetraazacyclotetradecane]cobalt(III) cation [1.969 (4) Å; Ware et al., 1996]. The Co—Cl distances [2.219 (2) Å for molecule A and 2.237 (2) Å for molecule B] are shorter than those found in CoIII complexes such as chloro(1,5,8,11,14-pentaazacyclohexadecane)cobalt(III) diperchlorate [2.242 (9) Å; Bombieri et al., 1982], chloro(1,4,7,11,14-pentaazacycloheptadecane)cobalt(III) diperchlorate [2.249 (1) Å; Tahirov et al., 1993] and the trans-dichloro(1,4,8,11-tetraazacyclotetradecane)cobalt(III) cation [2.252 (1) Å; Sosa-Torres & Toscano, 1997].
The ZnII ion is four-coordinate in a distorted tetrahedral environment completed by three Cl atoms and an O atom of the bridging ligand. The Zn—O bond lengths are 2.066 (4) and 2.080 (4) Å, which are shorter than that found in (1,4,8,11-tetraazacyclotetradecane-N,N',N'',N'''-dihydrogentetraactato)zinc(II) tetrahydrate [Zn—O 2.127 (1) Å; Riesen et al. 1991], but longer than that found in dichlorobis(pyridine betaine)zinc(II) [Zn—O 1.988 (3) and 1.964 (2) Å; Chen & Mak, 1991]. The average Zn—Cl bond length [2.236 (3) Å] is shorter than that in the [ZnCl4]2- ion found in bis(2-amino-4,5-dihydro-3H+-1,3-thiazolium) tetrachlorozincate(II) [2.243 (1)–2.301 (1) Å; Kubiak & Glowiak, 1984].
This crystal structure is stabilized by coordination bonds as well as hydrogen bonds. The hydrogen bonds between the complex cations and chloride anions are detailed in Table 2.