Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100005552/qa0274sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100005552/qa0274Isup2.hkl |
CCDC reference: 145638
The title compound, [Mn2(salen)2(CH3COO)]ClO4, was synthesized as described previously by Suzuki et al. (1997).
The positional parameters of all the H atoms were calculated geometrically and fixed with U(H) = 1.2Ueq(parent atom).
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: DIRDIF94 (Beurskens et al., 1994); program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.
[Mn2(C16H14N2O2)2(C2H3O2)]ClO4 | Z = 2 |
Mr = 800.97 | Dx = 1.583 Mg m−3 |
Triclinic, P1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.990 (4) Å | Cell parameters from 25 reflections |
b = 12.988 (4) Å | θ = 10–15° |
c = 11.296 (5) Å | µ = 0.90 mm−1 |
α = 106.52 (3)° | T = 298 K |
β = 94.31 (3)° | Prism, black |
γ = 90.79 (3)° | 0.5 × 0.5 × 0.3 mm |
V = 1680.5 (9) Å3 |
Rigaku AFC-5S diffractometer | Rint = 0.011 |
θ–2θ scans | θmax = 27.5° |
Absorption correction: integration (Coppens et al., 1965) | h = 0→16 |
Tmin = 0.670, Tmax = 0.789 | k = −17→17 |
8092 measured reflections | l = −15→15 |
7723 independent reflections | 3 standard reflections every 100 reflections |
6237 reflections with I > 2σ(I) | intensity decay: none |
Refinement on F2 | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.039 | w = 1/[σ2(Fo2) + (0.05(Fo2 + 2Fc2)/3)2] |
wR(F2) = 0.106 | (Δ/σ)max = 0.001 |
S = 1.37 | Δρmax = 0.53 e Å−3 |
7723 reflections | Δρmin = −0.66 e Å−3 |
460 parameters |
[Mn2(C16H14N2O2)2(C2H3O2)]ClO4 | γ = 90.79 (3)° |
Mr = 800.97 | V = 1680.5 (9) Å3 |
Triclinic, P1 | Z = 2 |
a = 11.990 (4) Å | Mo Kα radiation |
b = 12.988 (4) Å | µ = 0.90 mm−1 |
c = 11.296 (5) Å | T = 298 K |
α = 106.52 (3)° | 0.5 × 0.5 × 0.3 mm |
β = 94.31 (3)° |
Rigaku AFC-5S diffractometer | 6237 reflections with I > 2σ(I) |
Absorption correction: integration (Coppens et al., 1965) | Rint = 0.011 |
Tmin = 0.670, Tmax = 0.789 | 3 standard reflections every 100 reflections |
8092 measured reflections | intensity decay: none |
7723 independent reflections |
R[F2 > 2σ(F2)] = 0.039 | 460 parameters |
wR(F2) = 0.106 | H-atom parameters not refined |
S = 1.37 | Δρmax = 0.53 e Å−3 |
7723 reflections | Δρmin = −0.66 e Å−3 |
Refinement. Refinement using reflections with F2 > 0.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.00387 (3) | 0.46031 (3) | 0.34269 (3) | 0.02548 (8) | |
Mn2 | −0.35940 (3) | 0.48464 (3) | 0.04533 (3) | 0.02727 (8) | |
Cl1 | −0.48912 (7) | 0.22137 (7) | 0.40514 (6) | 0.0617 (2) | |
O1 | −0.0807 (1) | 0.5607 (1) | 0.4584 (1) | 0.0293 (4) | |
O2 | −0.0884 (1) | 0.3388 (1) | 0.3269 (1) | 0.0345 (4) | |
O3 | −0.4264 (1) | 0.5849 (1) | −0.0291 (1) | 0.0324 (4) | |
O4 | −0.3411 (1) | 0.3819 (1) | −0.1063 (1) | 0.0355 (4) | |
O5 | −0.0808 (1) | 0.5022 (1) | 0.1913 (2) | 0.0425 (5) | |
O6 | −0.1991 (1) | 0.5607 (1) | 0.0677 (2) | 0.0425 (5) | |
O7 | −0.4440 (3) | 0.1738 (2) | 0.2936 (2) | 0.0923 (10) | |
O8 | −0.5757 (4) | 0.2880 (5) | 0.3794 (4) | 0.190 (2) | |
O9 | −0.4076 (4) | 0.2916 (3) | 0.4854 (3) | 0.148 (2) | |
O10 | −0.5290 (3) | 0.1514 (3) | 0.4684 (3) | 0.110 (1) | |
N1 | 0.1250 (1) | 0.5727 (2) | 0.3706 (2) | 0.0330 (5) | |
N2 | 0.1189 (2) | 0.3699 (2) | 0.2491 (2) | 0.0364 (5) | |
N3 | −0.4018 (1) | 0.5736 (2) | 0.2085 (2) | 0.0326 (5) | |
N4 | −0.3272 (1) | 0.3801 (2) | 0.1395 (2) | 0.0317 (5) | |
C1 | −0.0882 (2) | 0.6631 (2) | 0.4546 (2) | 0.0314 (5) | |
C2 | −0.1864 (2) | 0.7167 (2) | 0.4857 (2) | 0.0405 (6) | |
C3 | −0.1958 (2) | 0.8229 (2) | 0.4866 (3) | 0.0528 (8) | |
C4 | −0.1075 (3) | 0.8786 (2) | 0.4567 (3) | 0.0585 (9) | |
C5 | −0.0101 (3) | 0.8282 (2) | 0.4288 (3) | 0.0509 (8) | |
C6 | 0.0022 (2) | 0.7203 (2) | 0.4263 (2) | 0.0365 (6) | |
C7 | 0.1095 (2) | 0.6734 (2) | 0.4004 (2) | 0.0391 (6) | |
C8 | 0.2356 (2) | 0.5272 (2) | 0.3464 (2) | 0.0432 (7) | |
C9 | 0.2178 (2) | 0.4318 (2) | 0.2334 (3) | 0.0487 (7) | |
C10 | 0.1129 (2) | 0.2674 (2) | 0.2032 (2) | 0.0482 (7) | |
C11 | 0.0238 (2) | 0.1974 (2) | 0.2134 (3) | 0.0488 (7) | |
C12 | 0.0337 (3) | 0.0850 (3) | 0.1621 (4) | 0.075 (1) | |
C13 | −0.0447 (4) | 0.0134 (3) | 0.1752 (4) | 0.085 (1) | |
C14 | −0.1366 (3) | 0.0506 (2) | 0.2390 (3) | 0.070 (1) | |
C15 | −0.1508 (2) | 0.1593 (2) | 0.2898 (3) | 0.0491 (7) | |
C16 | −0.0712 (2) | 0.2352 (2) | 0.2775 (2) | 0.0383 (6) | |
C17 | −0.4148 (2) | 0.6914 (2) | 0.0230 (2) | 0.0305 (5) | |
C18 | −0.4189 (2) | 0.7586 (2) | −0.0542 (2) | 0.0376 (6) | |
C19 | −0.4140 (2) | 0.8693 (2) | −0.0050 (3) | 0.0482 (7) | |
C20 | −0.4067 (2) | 0.9162 (2) | 0.1230 (3) | 0.0550 (8) | |
C21 | −0.4041 (2) | 0.8516 (2) | 0.2000 (2) | 0.0465 (7) | |
C22 | −0.4062 (2) | 0.7390 (2) | 0.1526 (2) | 0.0356 (6) | |
C23 | −0.4120 (2) | 0.6756 (2) | 0.2382 (2) | 0.0365 (6) | |
C24 | −0.4181 (2) | 0.5103 (2) | 0.2957 (2) | 0.0380 (6) | |
C25 | −0.3295 (2) | 0.4267 (2) | 0.2750 (2) | 0.0383 (6) | |
C26 | −0.3056 (2) | 0.2812 (2) | 0.0936 (2) | 0.0382 (6) | |
C27 | −0.3007 (2) | 0.2270 (2) | −0.0354 (2) | 0.0387 (6) | |
C28 | −0.2831 (3) | 0.1148 (2) | −0.0706 (3) | 0.0575 (9) | |
C29 | −0.2870 (3) | 0.0560 (2) | −0.1917 (3) | 0.0661 (10) | |
C30 | −0.3101 (3) | 0.1060 (2) | −0.2840 (3) | 0.0560 (8) | |
C31 | −0.3267 (2) | 0.2153 (2) | −0.2537 (2) | 0.0426 (7) | |
C32 | −0.3218 (2) | 0.2782 (2) | −0.1295 (2) | 0.0330 (5) | |
C33 | −0.1049 (2) | 0.5608 (2) | 0.1233 (2) | 0.0323 (5) | |
C34 | −0.0168 (2) | 0.6367 (2) | 0.1026 (2) | 0.0514 (8) | |
H1 | −0.2483 | 0.6795 | 0.5068 | 0.0487* | |
H2 | −0.2642 | 0.8586 | 0.5080 | 0.0634* | |
H3 | −0.1151 | 0.9518 | 0.4557 | 0.0703* | |
H4 | 0.0516 | 0.8674 | 0.4104 | 0.0611* | |
H5 | 0.1729 | 0.7210 | 0.4059 | 0.0470* | |
H6 | 0.2857 | 0.5795 | 0.3313 | 0.0519* | |
H7 | 0.2661 | 0.5050 | 0.4159 | 0.0519* | |
H8 | 0.2823 | 0.3881 | 0.2260 | 0.0585* | |
H9 | 0.2051 | 0.4555 | 0.1605 | 0.0585* | |
H10 | 0.1740 | 0.2348 | 0.1577 | 0.0579* | |
H11 | 0.0972 | 0.0590 | 0.1170 | 0.0897* | |
H12 | −0.0363 | −0.0624 | 0.1405 | 0.1022* | |
H13 | −0.1919 | −0.0001 | 0.2484 | 0.0839* | |
H14 | −0.2155 | 0.1830 | 0.3338 | 0.0589* | |
H15 | −0.4252 | 0.7277 | −0.1425 | 0.0451* | |
H16 | −0.4157 | 0.9142 | −0.0595 | 0.0579* | |
H17 | −0.4036 | 0.9930 | 0.1567 | 0.0660* | |
H18 | −0.4007 | 0.8838 | 0.2880 | 0.0559* | |
H19 | −0.4243 | 0.7121 | 0.3227 | 0.0438* | |
H20 | −0.4093 | 0.5560 | 0.3795 | 0.0456* | |
H21 | −0.4914 | 0.4761 | 0.2795 | 0.0456* | |
H22 | −0.3478 | 0.3716 | 0.3124 | 0.0459* | |
H23 | −0.2578 | 0.4596 | 0.3103 | 0.0459* | |
H24 | −0.2914 | 0.2396 | 0.1507 | 0.0458* | |
H25 | −0.2680 | 0.0796 | −0.0073 | 0.0690* | |
H26 | −0.2739 | −0.0196 | −0.2132 | 0.0794* | |
H27 | −0.3144 | 0.0644 | −0.3695 | 0.0672* | |
H28 | −0.3419 | 0.2487 | −0.3186 | 0.0511* | |
H29 | 0.0521 | 0.6307 | 0.1489 | 0.0617* | |
H30 | −0.0053 | 0.6186 | 0.0160 | 0.0617* | |
H31 | −0.0412 | 0.7092 | 0.1298 | 0.0617* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0234 (2) | 0.0286 (2) | 0.0259 (2) | 0.0013 (1) | 0.0031 (1) | 0.0099 (1) |
Mn2 | 0.0327 (2) | 0.0273 (2) | 0.0237 (2) | 0.0053 (1) | 0.0002 (1) | 0.0106 (1) |
Cl1 | 0.0737 (5) | 0.0704 (5) | 0.0372 (3) | −0.0129 (4) | 0.0143 (3) | 0.0074 (3) |
O1 | 0.0302 (7) | 0.0295 (7) | 0.0306 (7) | 0.0027 (6) | 0.0050 (6) | 0.0120 (6) |
O2 | 0.0329 (8) | 0.0306 (8) | 0.0409 (9) | 0.0006 (6) | 0.0013 (6) | 0.0122 (7) |
O3 | 0.0395 (8) | 0.0274 (7) | 0.0295 (7) | 0.0048 (6) | −0.0044 (6) | 0.0087 (6) |
O4 | 0.0473 (9) | 0.0299 (8) | 0.0316 (8) | 0.0083 (7) | 0.0070 (7) | 0.0114 (6) |
O5 | 0.0449 (9) | 0.052 (1) | 0.0351 (8) | −0.0001 (8) | −0.0063 (7) | 0.0216 (8) |
O6 | 0.0352 (8) | 0.054 (1) | 0.0430 (9) | −0.0018 (7) | −0.0059 (7) | 0.0250 (8) |
O7 | 0.122 (2) | 0.086 (2) | 0.062 (2) | 0.018 (2) | 0.032 (2) | 0.004 (1) |
O8 | 0.159 (4) | 0.303 (6) | 0.173 (4) | 0.148 (4) | 0.097 (3) | 0.146 (4) |
O9 | 0.224 (4) | 0.148 (3) | 0.061 (2) | −0.105 (3) | −0.036 (2) | 0.029 (2) |
O10 | 0.117 (2) | 0.122 (3) | 0.105 (2) | −0.033 (2) | 0.018 (2) | 0.055 (2) |
N1 | 0.0286 (9) | 0.041 (1) | 0.0330 (9) | −0.0030 (7) | 0.0019 (7) | 0.0164 (8) |
N2 | 0.0308 (9) | 0.048 (1) | 0.0303 (9) | 0.0068 (8) | 0.0045 (7) | 0.0096 (8) |
N3 | 0.0321 (9) | 0.038 (1) | 0.0273 (9) | 0.0005 (7) | −0.0002 (7) | 0.0100 (8) |
N4 | 0.0285 (9) | 0.039 (1) | 0.0319 (9) | 0.0018 (7) | −0.0006 (7) | 0.0172 (8) |
C1 | 0.038 (1) | 0.030 (1) | 0.0251 (10) | 0.0019 (9) | −0.0020 (8) | 0.0086 (8) |
C2 | 0.042 (1) | 0.036 (1) | 0.042 (1) | 0.0057 (10) | −0.0033 (10) | 0.0097 (10) |
C3 | 0.055 (2) | 0.039 (1) | 0.060 (2) | 0.015 (1) | −0.007 (1) | 0.009 (1) |
C4 | 0.079 (2) | 0.029 (1) | 0.068 (2) | 0.005 (1) | −0.005 (2) | 0.015 (1) |
C5 | 0.065 (2) | 0.035 (1) | 0.054 (2) | −0.008 (1) | 0.000 (1) | 0.017 (1) |
C6 | 0.044 (1) | 0.034 (1) | 0.033 (1) | −0.0031 (9) | −0.0024 (9) | 0.0128 (9) |
C7 | 0.039 (1) | 0.043 (1) | 0.038 (1) | −0.0101 (10) | 0.0031 (10) | 0.017 (1) |
C8 | 0.027 (1) | 0.056 (2) | 0.051 (1) | −0.003 (1) | 0.0028 (10) | 0.023 (1) |
C9 | 0.035 (1) | 0.067 (2) | 0.047 (1) | 0.007 (1) | 0.016 (1) | 0.019 (1) |
C10 | 0.044 (1) | 0.051 (2) | 0.042 (1) | 0.014 (1) | 0.004 (1) | 0.001 (1) |
C11 | 0.049 (1) | 0.038 (1) | 0.050 (1) | 0.008 (1) | −0.008 (1) | 0.000 (1) |
C12 | 0.076 (2) | 0.045 (2) | 0.084 (2) | 0.017 (2) | −0.005 (2) | −0.010 (2) |
C13 | 0.090 (3) | 0.035 (2) | 0.113 (3) | 0.003 (2) | −0.022 (2) | 0.000 (2) |
C14 | 0.082 (2) | 0.040 (2) | 0.084 (2) | −0.016 (2) | −0.037 (2) | 0.025 (2) |
C15 | 0.051 (1) | 0.040 (1) | 0.057 (2) | −0.008 (1) | −0.018 (1) | 0.022 (1) |
C16 | 0.042 (1) | 0.034 (1) | 0.038 (1) | −0.0002 (9) | −0.0136 (10) | 0.0116 (9) |
C17 | 0.0251 (10) | 0.028 (1) | 0.038 (1) | 0.0014 (8) | −0.0025 (8) | 0.0095 (9) |
C18 | 0.036 (1) | 0.035 (1) | 0.044 (1) | 0.0033 (9) | 0.0012 (10) | 0.0155 (10) |
C19 | 0.050 (1) | 0.033 (1) | 0.065 (2) | 0.000 (1) | −0.002 (1) | 0.021 (1) |
C20 | 0.058 (2) | 0.027 (1) | 0.074 (2) | 0.000 (1) | −0.010 (1) | 0.008 (1) |
C21 | 0.048 (1) | 0.035 (1) | 0.048 (1) | 0.001 (1) | −0.006 (1) | 0.001 (1) |
C22 | 0.033 (1) | 0.031 (1) | 0.038 (1) | 0.0006 (9) | −0.0028 (9) | 0.0057 (9) |
C23 | 0.036 (1) | 0.040 (1) | 0.028 (1) | 0.0027 (9) | 0.0004 (9) | 0.0020 (9) |
C24 | 0.039 (1) | 0.049 (1) | 0.028 (1) | −0.0024 (10) | 0.0027 (9) | 0.0141 (10) |
C25 | 0.041 (1) | 0.048 (1) | 0.031 (1) | −0.001 (1) | −0.0028 (9) | 0.021 (1) |
C26 | 0.036 (1) | 0.041 (1) | 0.044 (1) | 0.0056 (9) | −0.0029 (10) | 0.024 (1) |
C27 | 0.037 (1) | 0.035 (1) | 0.046 (1) | 0.0086 (9) | 0.0031 (10) | 0.017 (1) |
C28 | 0.073 (2) | 0.039 (1) | 0.065 (2) | 0.020 (1) | 0.004 (1) | 0.022 (1) |
C29 | 0.089 (2) | 0.032 (1) | 0.075 (2) | 0.020 (1) | 0.011 (2) | 0.010 (1) |
C30 | 0.068 (2) | 0.041 (1) | 0.055 (2) | 0.010 (1) | 0.017 (1) | 0.004 (1) |
C31 | 0.047 (1) | 0.038 (1) | 0.043 (1) | 0.004 (1) | 0.011 (1) | 0.011 (1) |
C32 | 0.030 (1) | 0.031 (1) | 0.040 (1) | 0.0043 (8) | 0.0058 (9) | 0.0115 (9) |
C33 | 0.034 (1) | 0.039 (1) | 0.0237 (10) | 0.0016 (9) | 0.0033 (8) | 0.0084 (9) |
C34 | 0.052 (2) | 0.063 (2) | 0.042 (1) | −0.016 (1) | −0.003 (1) | 0.022 (1) |
Mn1—O1 | 1.924 (2) | C10—C11 | 1.425 (4) |
Mn1—O2 | 1.873 (2) | C10—H10 | 0.960 |
Mn1—O5 | 2.129 (2) | C11—C12 | 1.419 (4) |
Mn1—N1 | 1.987 (2) | C11—C16 | 1.414 (4) |
Mn1—N2 | 1.989 (2) | C12—C13 | 1.359 (6) |
Mn2—O3 | 1.897 (1) | C12—H11 | 0.960 |
Mn2—O4 | 1.878 (2) | C13—C14 | 1.380 (6) |
Mn2—O6 | 2.113 (2) | C13—H12 | 0.960 |
Mn2—N3 | 1.984 (2) | C14—C15 | 1.383 (4) |
Mn2—N4 | 1.975 (2) | C14—H13 | 0.960 |
Cl1—O7 | 1.389 (2) | C15—C16 | 1.406 (4) |
Cl1—O8 | 1.426 (4) | C15—H14 | 0.960 |
Cl1—O9 | 1.407 (3) | C17—C18 | 1.397 (3) |
Cl1—O10 | 1.405 (3) | C17—C22 | 1.413 (3) |
O1—C1 | 1.348 (3) | C18—C19 | 1.384 (3) |
O2—C16 | 1.328 (3) | C18—H15 | 0.960 |
O3—C17 | 1.340 (3) | C19—C20 | 1.396 (4) |
O4—C32 | 1.323 (3) | C19—H16 | 0.960 |
O5—C33 | 1.248 (3) | C20—C21 | 1.369 (4) |
O6—C33 | 1.250 (3) | C20—H17 | 0.960 |
N1—C7 | 1.274 (3) | C21—C22 | 1.407 (3) |
N1—C8 | 1.473 (3) | C21—H18 | 0.960 |
N2—C9 | 1.474 (3) | C22—C23 | 1.442 (3) |
N2—C10 | 1.283 (3) | C23—H19 | 0.960 |
N3—C23 | 1.280 (3) | C24—C25 | 1.512 (4) |
N3—C24 | 1.473 (3) | C24—H20 | 0.960 |
N4—C25 | 1.480 (3) | C24—H21 | 0.960 |
N4—C26 | 1.279 (3) | C25—H22 | 0.960 |
C1—C2 | 1.393 (3) | C25—H23 | 0.960 |
C1—C6 | 1.411 (3) | C26—C27 | 1.433 (4) |
C2—C3 | 1.384 (4) | C26—H24 | 0.960 |
C2—H1 | 0.960 | C27—C28 | 1.421 (3) |
C3—C4 | 1.388 (4) | C27—C32 | 1.414 (3) |
C3—H2 | 0.960 | C28—C29 | 1.361 (4) |
C4—C5 | 1.360 (4) | C28—H25 | 0.960 |
C4—H3 | 0.960 | C29—C30 | 1.391 (4) |
C5—C6 | 1.404 (3) | C29—H26 | 0.960 |
C5—H4 | 0.960 | C30—C31 | 1.384 (4) |
C6—C7 | 1.445 (4) | C30—H27 | 0.960 |
C7—H5 | 0.960 | C31—C32 | 1.405 (3) |
C8—C9 | 1.503 (4) | C31—H28 | 0.960 |
C8—H6 | 0.960 | C33—C34 | 1.510 (3) |
C8—H7 | 0.960 | C34—H29 | 0.960 |
C9—H8 | 0.960 | C34—H30 | 0.960 |
C9—H9 | 0.960 | C34—H31 | 0.960 |
Mn1···C1i | 3.259 (2) | O7···C26 | 3.477 (4) |
Mn1···Mn1i | 3.4161 (6) | O7···C15 | 3.526 (4) |
Mn2···O3ii | 2.686 (2) | O8···C2v | 3.341 (5) |
Mn2···C17ii | 3.414 (2) | O8···C18ii | 3.544 (5) |
Mn2···Mn2ii | 3.510 (1) | O9···C8i | 3.183 (4) |
O1···O1i | 2.786 (3) | O9···C31vi | 3.445 (4) |
O1···N1i | 3.008 (2) | O9···C25 | 3.503 (4) |
O1···O2i | 3.013 (2) | O10···C3v | 3.383 (5) |
O1···N2i | 3.239 (2) | O10···C23v | 3.563 (4) |
O1···C8i | 3.407 (3) | N2···C2i | 3.531 (3) |
O2···C1i | 3.134 (3) | N2···C1i | 3.538 (3) |
O2···C7i | 3.158 (3) | N4···C18ii | 3.443 (3) |
O2···C6i | 3.199 (3) | N4···C17ii | 3.448 (3) |
O2···N1i | 3.345 (2) | C1···C16i | 3.366 (3) |
O3···O3ii | 3.050 (3) | C2···C10i | 3.505 (4) |
O3···N3ii | 3.077 (2) | C5···C15i | 3.553 (4) |
O3···N4ii | 3.209 (2) | C6···C16i | 3.268 (3) |
O3···O4ii | 3.256 (2) | C6···C15i | 3.480 (3) |
O3···C24ii | 3.324 (3) | C7···C15i | 3.549 (4) |
O3···C9iii | 3.496 (3) | C7···C16i | 3.559 (3) |
O4···C23ii | 3.191 (3) | C17···C32ii | 3.452 (3) |
O4···N3ii | 3.326 (3) | C17···C26ii | 3.568 (3) |
O4···C22ii | 3.328 (3) | C17···C27ii | 3.586 (3) |
O4···C17ii | 3.347 (3) | C18···C26ii | 3.312 (3) |
O4···C9iii | 3.507 (3) | C18···C27ii | 3.575 (4) |
O4···C8iii | 3.556 (3) | C21···C31ii | 3.472 (4) |
O5···C34iii | 3.590 (3) | C22···C32ii | 3.251 (3) |
O6···C9iii | 3.421 (3) | C22···C31ii | 3.483 (4) |
O7···C18ii | 3.392 (4) | C23···C31ii | 3.452 (4) |
O7···C20iv | 3.407 (4) | C23···C32ii | 3.455 (3) |
O7···C19ii | 3.455 (4) | C33···C34iii | 3.489 (4) |
O1—Mn1—O2 | 96.7 (1) | C10—C11—C16 | 122.6 (2) |
O1—Mn1—O5 | 91.0 (1) | C12—C11—C16 | 118.9 (3) |
O1—Mn1—N1 | 89.1 (1) | C11—C12—C13 | 121.5 (3) |
O1—Mn1—N2 | 167.7 (1) | C11—C12—H11 | 119.2 |
O2—Mn1—O5 | 94.9 (1) | C13—C12—H11 | 119.2 |
O2—Mn1—N1 | 168.8 (1) | C12—C13—C14 | 119.3 (3) |
O2—Mn1—N2 | 91.2 (1) | C12—C13—H12 | 120.3 |
O5—Mn1—N1 | 94.6 (1) | C14—C13—H12 | 120.3 |
O5—Mn1—N2 | 97.7 (1) | C13—C14—C15 | 121.4 (3) |
N1—Mn1—N2 | 81.6 (1) | C13—C14—H13 | 119.3 |
O3—Mn2—O4 | 94.3 (1) | C15—C14—H13 | 119.3 |
O3—Mn2—O6 | 93.1 (1) | C14—C15—C16 | 120.5 (3) |
O3—Mn2—N3 | 89.1 (1) | C14—C15—H14 | 119.8 |
O3—Mn2—N4 | 165.4 (1) | C16—C15—H14 | 119.8 |
O4—Mn2—O6 | 96.9 (1) | O2—C16—C11 | 123.2 (2) |
O4—Mn2—N3 | 168.9 (1) | O2—C16—C15 | 118.5 (2) |
O4—Mn2—N4 | 92.1 (1) | C11—C16—C15 | 118.3 (2) |
O6—Mn2—N3 | 93.5 (1) | O3—C17—C18 | 118.6 (2) |
O6—Mn2—N4 | 99.1 (1) | O3—C17—C22 | 122.8 (2) |
N3—Mn2—N4 | 82.3 (1) | C18—C17—C22 | 118.5 (2) |
O7—Cl1—O8 | 106.8 (2) | C17—C18—C19 | 120.9 (2) |
O7—Cl1—O9 | 108.9 (2) | C17—C18—H15 | 119.6 |
O7—Cl1—O10 | 116.4 (2) | C19—C18—H15 | 119.6 |
O8—Cl1—O9 | 105.7 (3) | C18—C19—C20 | 120.7 (2) |
O8—Cl1—O10 | 110.8 (3) | C18—C19—H16 | 119.7 |
O9—Cl1—O10 | 107.7 (2) | C20—C19—H16 | 119.7 |
Mn1—O1—C1 | 120.6 (1) | C19—C20—C21 | 119.3 (2) |
Mn1—O2—C16 | 130.5 (2) | C19—C20—H17 | 120.4 |
Mn2—O3—C17 | 122.5 (1) | C21—C20—H17 | 120.4 |
Mn2—O4—C32 | 129.6 (1) | C20—C21—C22 | 121.2 (2) |
Mn1—O5—C33 | 155.9 (2) | C20—C21—H18 | 119.4 |
Mn2—O6—C33 | 140.1 (1) | C22—C21—H18 | 119.4 |
Mn1—N1—C7 | 124.5 (2) | C17—C22—C21 | 119.5 (2) |
Mn1—N1—C8 | 112.6 (2) | C17—C22—C23 | 121.9 (2) |
C7—N1—C8 | 122.8 (2) | C21—C22—C23 | 118.3 (2) |
Mn1—N2—C9 | 113.7 (2) | N3—C23—C22 | 124.0 (2) |
Mn1—N2—C10 | 126.3 (2) | N3—C23—H19 | 118.0 |
C9—N2—C10 | 119.9 (2) | C22—C23—H19 | 118.0 |
Mn2—N3—C23 | 124.8 (2) | N3—C24—C25 | 106.4 (2) |
Mn2—N3—C24 | 112.9 (1) | N3—C24—H20 | 110.2 |
C23—N3—C24 | 122.4 (2) | N3—C24—H21 | 110.2 |
Mn2—N4—C25 | 113.3 (1) | C25—C24—H20 | 110.2 |
Mn2—N4—C26 | 126.1 (2) | C25—C24—H21 | 110.2 |
C25—N4—C26 | 120.6 (2) | H20—C24—H21 | 109.5 |
O1—C1—C2 | 119.1 (2) | N4—C25—C24 | 107.3 (2) |
O1—C1—C6 | 122.3 (2) | N4—C25—H22 | 110.0 |
C2—C1—C6 | 118.5 (2) | N4—C25—H23 | 110.0 |
C1—C2—C3 | 120.7 (2) | C24—C25—H22 | 110.0 |
C1—C2—H1 | 119.7 | C24—C25—H23 | 110.0 |
C3—C2—H1 | 119.7 | H22—C25—H23 | 109.5 |
C2—C3—C4 | 120.7 (3) | N4—C26—C27 | 125.8 (2) |
C2—C3—H2 | 119.6 | N4—C26—H24 | 117.1 |
C4—C3—H2 | 119.6 | C27—C26—H24 | 117.1 |
C3—C4—C5 | 119.4 (2) | C26—C27—C28 | 118.2 (2) |
C3—C4—H3 | 120.3 | C26—C27—C32 | 123.0 (2) |
C5—C4—H3 | 120.3 | C28—C27—C32 | 118.6 (2) |
C4—C5—C6 | 121.4 (3) | C27—C28—C29 | 121.7 (3) |
C4—C5—H4 | 119.3 | C27—C28—H25 | 119.1 |
C6—C5—H4 | 119.3 | C29—C28—H25 | 119.1 |
C1—C6—C5 | 119.2 (2) | C28—C29—C30 | 119.6 (3) |
C1—C6—C7 | 122.4 (2) | C28—C29—H26 | 120.2 |
C5—C6—C7 | 118.3 (2) | C30—C29—H26 | 120.2 |
N1—C7—C6 | 124.0 (2) | C29—C30—C31 | 120.5 (3) |
N1—C7—H5 | 118.0 | C29—C30—H27 | 119.8 |
C6—C7—H5 | 118.0 | C31—C30—H27 | 119.7 |
N1—C8—C9 | 106.6 (2) | C30—C31—C32 | 121.1 (2) |
N1—C8—H6 | 110.2 | C30—C31—H28 | 119.5 |
N1—C8—H7 | 110.2 | C32—C31—H28 | 119.5 |
C9—C8—H6 | 110.2 | O4—C32—C27 | 123.2 (2) |
C9—C8—H7 | 110.2 | O4—C32—C31 | 118.2 (2) |
H6—C8—H7 | 109.5 | C27—C32—C31 | 118.5 (2) |
N2—C9—C8 | 107.3 (2) | O5—C33—O6 | 124.1 (2) |
N2—C9—H8 | 110.0 | O5—C33—C34 | 119.9 (2) |
N2—C9—H9 | 110.0 | O6—C33—C34 | 116.0 (2) |
C8—C9—H8 | 110.0 | C33—C34—H29 | 109.5 |
C8—C9—H9 | 110.0 | C33—C34—H30 | 109.5 |
H8—C9—H9 | 109.5 | C33—C34—H31 | 109.5 |
N2—C10—C11 | 126.0 (2) | H29—C34—H30 | 109.5 |
N2—C10—H10 | 117.0 | H29—C34—H31 | 109.5 |
C11—C10—H10 | 117.0 | H30—C34—H31 | 109.5 |
C10—C11—C12 | 118.4 (3) | ||
Mn1—O5—C33—O6 | −148.6 (3) | Mn2—O6—C33—O5 | 0.9 (4) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x−1, −y+1, −z; (iii) −x, −y+1, −z; (iv) x, y−1, z; (v) −x−1, −y+1, −z+1; (vi) x, y, z+1. |
Experimental details
Crystal data | |
Chemical formula | [Mn2(C16H14N2O2)2(C2H3O2)]ClO4 |
Mr | 800.97 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 11.990 (4), 12.988 (4), 11.296 (5) |
α, β, γ (°) | 106.52 (3), 94.31 (3), 90.79 (3) |
V (Å3) | 1680.5 (9) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.90 |
Crystal size (mm) | 0.5 × 0.5 × 0.3 |
Data collection | |
Diffractometer | Rigaku AFC-5S diffractometer |
Absorption correction | Integration (Coppens et al., 1965) |
Tmin, Tmax | 0.670, 0.789 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8092, 7723, 6237 |
Rint | 0.011 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.106, 1.37 |
No. of reflections | 7723 |
No. of parameters | 460 |
No. of restraints | ? |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.53, −0.66 |
Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), DIRDIF94 (Beurskens et al., 1994), TEXSAN.
Mn1—O1 | 1.924 (2) | Mn2—O3 | 1.897 (1) |
Mn1—O2 | 1.873 (2) | Mn2—O4 | 1.878 (2) |
Mn1—O5 | 2.129 (2) | Mn2—O6 | 2.113 (2) |
Mn1—N1 | 1.987 (2) | Mn2—N3 | 1.984 (2) |
Mn1—N2 | 1.989 (2) | Mn2—N4 | 1.975 (2) |
Mn1—O5—C33 | 155.9 (2) | Mn2—O6—C33 | 140.1 (1) |
Mn1—O5—C33—O6 | −148.6 (3) | Mn2—O6—C33—O5 | 0.9 (4) |
The X-ray structure analysis of [Mn2(7-Me-salen)2(CH3COO)]ClO4 gave an unsatisfactory R value of 0.140 due to the poor crystalinity (Suzuki et al., 1997). The structure of [Mn2(salen)2(CH3COO)]ClO4, (I), is presented here.