Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100005564/qa0276sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100005564/qa0276Isup2.hkl |
Preparation of the bzpy ligand and its chlorocopper(II) complex was carried out by an analagous method to that described previously by Ito et al. (1998). Crystals of the title compound, [Cu2(bzpy)2Cl3]ClO4.0.5H2O, were grown from an MeOH/CH3CN solution.
The water O atom lies on an inversion centre the water H atoms were not introduced. Positional parameters of all the other 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: SIR92 (Altomare et al., 1994); program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.
[Cu2Cl3(C19H19N3)2]ClO4·0.5H2O | Z = 2 |
Mr = 920.67 | Dx = 1.524 Mg m−3 |
Triclinic, P1 | Mo Kα radiation, λ = 0.71073 Å |
a = 13.799 (2) Å | Cell parameters from 25 reflections |
b = 14.488 (2) Å | θ = 10–15° |
c = 12.608 (2) Å | µ = 1.38 mm−1 |
α = 99.33 (1)° | T = 300 K |
β = 111.86 (1)° | Sphere, blue |
γ = 113.14 (1)° | 0.3 mm (radius) |
V = 2005.9 (6) Å3 |
Rigaku AFC-5S diffractometer | Rint = 0.012 |
θ–2θ scans | θmax = 27.5° |
Absorption correction: for a sphere (International Tables for Crystallography, 1992, Vol.C) | h = 0→18 |
Tmin = 0.545, Tmax = 0.552 | k = −19→19 |
9581 measured reflections | l = −16→16 |
9196 independent reflections | 3 standard reflections every 100 reflections |
6985 reflections with I > 2σ(I) | intensity decay: 4.3% |
Refinement on F2 | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.040 | w = 1/[σ2(Fo2) + (0.1(Fo2 + 2Fc2)/3)2] |
wR(F2) = 0.141 | (Δ/σ)max = 0.004 |
S = 1.02 | Δρmax = 0.42 e Å−3 |
9196 reflections | Δρmin = −0.35 e Å−3 |
493 parameters |
[Cu2Cl3(C19H19N3)2]ClO4·0.5H2O | γ = 113.14 (1)° |
Mr = 920.67 | V = 2005.9 (6) Å3 |
Triclinic, P1 | Z = 2 |
a = 13.799 (2) Å | Mo Kα radiation |
b = 14.488 (2) Å | µ = 1.38 mm−1 |
c = 12.608 (2) Å | T = 300 K |
α = 99.33 (1)° | 0.3 mm (radius) |
β = 111.86 (1)° |
Rigaku AFC-5S diffractometer | 6985 reflections with I > 2σ(I) |
Absorption correction: for a sphere (International Tables for Crystallography, 1992, Vol.C) | Rint = 0.012 |
Tmin = 0.545, Tmax = 0.552 | 3 standard reflections every 100 reflections |
9581 measured reflections | intensity decay: 4.3% |
9196 independent reflections |
R[F2 > 2σ(F2)] = 0.040 | 493 parameters |
wR(F2) = 0.141 | H-atom parameters not refined |
S = 1.02 | Δρmax = 0.42 e Å−3 |
9196 reflections | Δρmin = −0.35 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 | ||
Cu1 | 0.33950 (3) | 0.22173 (3) | 0.19568 (3) | 0.03784 (9) | |
Cu2 | 0.36224 (3) | 0.15547 (3) | −0.19073 (3) | 0.03861 (10) | |
Cl1 | 0.30204 (7) | 0.09911 (7) | 0.28385 (8) | 0.0572 (2) | |
Cl2 | 0.38586 (8) | 0.31866 (6) | −0.18914 (8) | 0.0545 (2) | |
Cl3 | 0.33147 (7) | 0.11426 (6) | −0.00579 (7) | 0.0461 (2) | |
Cl4 | −0.00835 (7) | −0.34483 (7) | −0.66328 (9) | 0.0564 (2) | |
O1 | 0.0894 (3) | −0.2478 (4) | −0.6377 (6) | 0.151 (2) | |
O2 | −0.1165 (3) | −0.3620 (5) | −0.7477 (6) | 0.174 (2) | |
O3 | 0.0050 (6) | −0.4296 (5) | −0.6863 (8) | 0.232 (3) | |
O4 | −0.0073 (7) | −0.3427 (7) | −0.5558 (6) | 0.238 (3) | |
O5 | 1.0000 | 0.5000 | 1.0000 | 0.294 (9) | |
N1 | 0.1713 (2) | 0.1952 (2) | 0.1056 (2) | 0.0432 (6) | |
N2 | 0.3791 (2) | 0.3591 (2) | 0.1548 (2) | 0.0425 (6) | |
N3 | 0.5185 (2) | 0.2893 (2) | 0.2789 (2) | 0.0435 (6) | |
N4 | 0.1840 (2) | 0.0717 (2) | −0.2892 (2) | 0.0447 (7) | |
N5 | 0.3470 (2) | 0.0091 (2) | −0.2641 (2) | 0.0405 (6) | |
N6 | 0.5349 (2) | 0.1999 (2) | −0.0959 (2) | 0.0418 (6) | |
C1 | 0.0740 (3) | 0.1250 (3) | 0.1076 (3) | 0.0492 (8) | |
C2 | −0.0397 (3) | 0.1069 (3) | 0.0328 (4) | 0.061 (1) | |
C3 | −0.0525 (3) | 0.1607 (4) | −0.0466 (4) | 0.068 (1) | |
C4 | 0.0475 (3) | 0.2352 (3) | −0.0460 (3) | 0.060 (1) | |
C5 | 0.1593 (3) | 0.2522 (3) | 0.0322 (3) | 0.0453 (8) | |
C6 | 0.2723 (3) | 0.3304 (3) | 0.0380 (3) | 0.0515 (9) | |
C7 | 0.4886 (3) | 0.3861 (2) | 0.1427 (3) | 0.0485 (8) | |
C8 | 0.5710 (3) | 0.3653 (2) | 0.2391 (3) | 0.0473 (8) | |
C9 | 0.6951 (3) | 0.4179 (3) | 0.2839 (4) | 0.0614 (10) | |
C10 | 0.7640 (3) | 0.3887 (3) | 0.3688 (4) | 0.068 (1) | |
C11 | 0.7090 (3) | 0.3103 (3) | 0.4076 (4) | 0.063 (1) | |
C12 | 0.5866 (3) | 0.2628 (3) | 0.3619 (3) | 0.0517 (8) | |
C13 | 0.4077 (3) | 0.4517 (3) | 0.2569 (3) | 0.0551 (9) | |
C14 | 0.3224 (3) | 0.4257 (3) | 0.3090 (3) | 0.0571 (9) | |
C15 | 0.2274 (4) | 0.4454 (3) | 0.2690 (5) | 0.080 (1) | |
C16 | 0.1518 (5) | 0.4256 (5) | 0.3187 (8) | 0.118 (2) | |
C17 | 0.1711 (8) | 0.3875 (5) | 0.4107 (10) | 0.148 (3) | |
C18 | 0.2664 (7) | 0.3667 (4) | 0.4563 (5) | 0.115 (2) | |
C19 | 0.3438 (5) | 0.3873 (3) | 0.4033 (4) | 0.079 (1) | |
C20 | 0.1090 (3) | 0.1121 (3) | −0.3071 (3) | 0.0554 (10) | |
C21 | −0.0133 (3) | 0.0466 (4) | −0.3542 (4) | 0.067 (1) | |
C22 | −0.0590 (3) | −0.0613 (4) | −0.3859 (4) | 0.070 (1) | |
C23 | 0.0169 (3) | −0.1038 (3) | −0.3707 (4) | 0.063 (1) | |
C24 | 0.1390 (3) | −0.0346 (3) | −0.3199 (3) | 0.0465 (8) | |
C25 | 0.2283 (3) | −0.0746 (2) | −0.2866 (3) | 0.0484 (8) | |
C26 | 0.4488 (3) | 0.0061 (2) | −0.1697 (3) | 0.0465 (8) | |
C27 | 0.5568 (3) | 0.1173 (2) | −0.0968 (3) | 0.0420 (7) | |
C28 | 0.6713 (3) | 0.1330 (3) | −0.0296 (3) | 0.0568 (10) | |
C29 | 0.7645 (3) | 0.2362 (4) | 0.0424 (4) | 0.066 (1) | |
C30 | 0.7424 (3) | 0.3216 (3) | 0.0430 (4) | 0.065 (1) | |
C31 | 0.6269 (3) | 0.3007 (3) | −0.0280 (3) | 0.0537 (9) | |
C32 | 0.3493 (3) | −0.0033 (3) | −0.3841 (3) | 0.0481 (8) | |
C33 | 0.4604 (3) | 0.0853 (3) | −0.3734 (3) | 0.0437 (8) | |
C34 | 0.5607 (3) | 0.0744 (3) | −0.3503 (3) | 0.056 (1) | |
C35 | 0.6644 (4) | 0.1589 (4) | −0.3326 (4) | 0.071 (1) | |
C36 | 0.6678 (4) | 0.2544 (4) | −0.3398 (4) | 0.075 (1) | |
C37 | 0.5671 (4) | 0.2639 (3) | −0.3671 (4) | 0.070 (1) | |
C38 | 0.4641 (3) | 0.1792 (3) | −0.3836 (3) | 0.0545 (10) | |
H1 | 0.0834 | 0.0863 | 0.1623 | 0.0591* | |
H2 | −0.1083 | 0.0575 | 0.0365 | 0.0735* | |
H3 | −0.1310 | 0.1465 | −0.1024 | 0.0818* | |
H4 | 0.0396 | 0.2750 | −0.0995 | 0.0725* | |
H5 | 0.2688 | 0.3944 | 0.0326 | 0.0618* | |
H6 | 0.2797 | 0.2988 | −0.0295 | 0.0618* | |
H7 | 0.4672 | 0.3422 | 0.0632 | 0.0582* | |
H8 | 0.5279 | 0.4606 | 0.1526 | 0.0582* | |
H9 | 0.7322 | 0.4733 | 0.2566 | 0.0737* | |
H10 | 0.8494 | 0.4231 | 0.3999 | 0.0817* | |
H11 | 0.7553 | 0.2889 | 0.4658 | 0.0758* | |
H12 | 0.5484 | 0.2089 | 0.3903 | 0.0620* | |
H13 | 0.4868 | 0.4768 | 0.3220 | 0.0661* | |
H14 | 0.4068 | 0.5080 | 0.2262 | 0.0661* | |
H15 | 0.2139 | 0.4738 | 0.2045 | 0.0959* | |
H16 | 0.0854 | 0.4387 | 0.2882 | 0.1411* | |
H17 | 0.1183 | 0.3743 | 0.4457 | 0.1771* | |
H18 | 0.2792 | 0.3393 | 0.5217 | 0.1379* | |
H19 | 0.4105 | 0.3744 | 0.4330 | 0.0954* | |
H20 | 0.1413 | 0.1884 | −0.2866 | 0.0665* | |
H21 | −0.0651 | 0.0772 | −0.3642 | 0.0805* | |
H22 | −0.1437 | −0.1080 | −0.4188 | 0.0844* | |
H23 | −0.0147 | −0.1802 | −0.3950 | 0.0752* | |
H24 | 0.1992 | −0.1385 | −0.3527 | 0.0581* | |
H25 | 0.2373 | −0.0909 | −0.2138 | 0.0581* | |
H26 | 0.4243 | −0.0230 | −0.1151 | 0.0559* | |
H27 | 0.4702 | −0.0390 | −0.2095 | 0.0559* | |
H28 | 0.6852 | 0.0729 | −0.0332 | 0.0682* | |
H29 | 0.8440 | 0.2489 | 0.0917 | 0.0791* | |
H30 | 0.8065 | 0.3942 | 0.0919 | 0.0782* | |
H31 | 0.6119 | 0.3599 | −0.0288 | 0.0644* | |
H32 | 0.3454 | −0.0708 | −0.4132 | 0.0577* | |
H33 | 0.2804 | −0.0032 | −0.4420 | 0.0577* | |
H34 | 0.5580 | 0.0078 | −0.3465 | 0.0672* | |
H35 | 0.7344 | 0.1517 | −0.3153 | 0.0855* | |
H36 | 0.7406 | 0.3139 | −0.3255 | 0.0895* | |
H37 | 0.5683 | 0.3292 | −0.3747 | 0.0844* | |
H38 | 0.3936 | 0.1860 | −0.4026 | 0.0654* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0334 (2) | 0.0351 (2) | 0.0394 (2) | 0.0130 (1) | 0.0167 (1) | 0.0124 (1) |
Cu2 | 0.0392 (2) | 0.0314 (2) | 0.0411 (2) | 0.0154 (1) | 0.0188 (2) | 0.0099 (1) |
Cl1 | 0.0473 (4) | 0.0572 (5) | 0.0615 (5) | 0.0196 (4) | 0.0225 (4) | 0.0336 (4) |
Cl2 | 0.0686 (5) | 0.0395 (4) | 0.0678 (5) | 0.0287 (4) | 0.0397 (4) | 0.0250 (4) |
Cl3 | 0.0553 (4) | 0.0404 (4) | 0.0435 (4) | 0.0198 (3) | 0.0296 (3) | 0.0125 (3) |
Cl4 | 0.0454 (4) | 0.0578 (5) | 0.0701 (5) | 0.0246 (4) | 0.0299 (4) | 0.0293 (4) |
O1 | 0.064 (2) | 0.130 (4) | 0.246 (6) | 0.026 (2) | 0.067 (3) | 0.110 (4) |
O2 | 0.055 (2) | 0.165 (5) | 0.273 (7) | 0.045 (3) | 0.032 (3) | 0.148 (5) |
O3 | 0.137 (5) | 0.123 (4) | 0.321 (10) | 0.090 (4) | 0.014 (5) | −0.023 (5) |
O4 | 0.196 (7) | 0.266 (9) | 0.145 (5) | 0.002 (6) | 0.118 (5) | 0.035 (5) |
O5 | 0.30 (2) | 0.25 (2) | 0.36 (2) | 0.10 (1) | 0.22 (2) | 0.12 (1) |
N1 | 0.041 (1) | 0.041 (1) | 0.043 (1) | 0.020 (1) | 0.020 (1) | 0.009 (1) |
N2 | 0.048 (1) | 0.037 (1) | 0.044 (1) | 0.019 (1) | 0.026 (1) | 0.014 (1) |
N3 | 0.037 (1) | 0.040 (1) | 0.041 (1) | 0.013 (1) | 0.016 (1) | 0.006 (1) |
N4 | 0.044 (1) | 0.045 (1) | 0.039 (1) | 0.020 (1) | 0.018 (1) | 0.012 (1) |
N5 | 0.043 (1) | 0.036 (1) | 0.040 (1) | 0.016 (1) | 0.022 (1) | 0.0098 (10) |
N6 | 0.043 (1) | 0.040 (1) | 0.039 (1) | 0.015 (1) | 0.023 (1) | 0.0101 (10) |
C1 | 0.041 (2) | 0.044 (2) | 0.056 (2) | 0.017 (1) | 0.024 (1) | 0.012 (1) |
C2 | 0.040 (2) | 0.055 (2) | 0.075 (2) | 0.018 (2) | 0.026 (2) | 0.011 (2) |
C3 | 0.047 (2) | 0.080 (3) | 0.061 (2) | 0.034 (2) | 0.016 (2) | 0.008 (2) |
C4 | 0.062 (2) | 0.075 (2) | 0.052 (2) | 0.043 (2) | 0.024 (2) | 0.024 (2) |
C5 | 0.051 (2) | 0.049 (2) | 0.041 (2) | 0.029 (1) | 0.023 (1) | 0.013 (1) |
C6 | 0.061 (2) | 0.054 (2) | 0.051 (2) | 0.032 (2) | 0.031 (2) | 0.025 (1) |
C7 | 0.052 (2) | 0.039 (2) | 0.054 (2) | 0.015 (1) | 0.033 (1) | 0.015 (1) |
C8 | 0.045 (2) | 0.038 (1) | 0.048 (2) | 0.011 (1) | 0.027 (1) | 0.004 (1) |
C9 | 0.047 (2) | 0.052 (2) | 0.065 (2) | 0.008 (2) | 0.031 (2) | 0.006 (2) |
C10 | 0.036 (2) | 0.071 (2) | 0.067 (2) | 0.014 (2) | 0.019 (2) | 0.001 (2) |
C11 | 0.046 (2) | 0.069 (2) | 0.057 (2) | 0.026 (2) | 0.015 (2) | 0.009 (2) |
C12 | 0.043 (2) | 0.051 (2) | 0.047 (2) | 0.019 (1) | 0.016 (1) | 0.011 (1) |
C13 | 0.064 (2) | 0.035 (2) | 0.063 (2) | 0.018 (1) | 0.037 (2) | 0.009 (1) |
C14 | 0.064 (2) | 0.036 (2) | 0.062 (2) | 0.016 (1) | 0.038 (2) | 0.001 (1) |
C15 | 0.072 (3) | 0.056 (2) | 0.107 (3) | 0.029 (2) | 0.051 (3) | 0.006 (2) |
C16 | 0.091 (4) | 0.073 (3) | 0.179 (7) | 0.024 (3) | 0.093 (5) | −0.004 (4) |
C17 | 0.146 (6) | 0.057 (3) | 0.211 (9) | −0.008 (3) | 0.150 (7) | −0.026 (4) |
C18 | 0.160 (6) | 0.053 (3) | 0.090 (4) | 0.000 (3) | 0.090 (4) | −0.002 (2) |
C19 | 0.106 (3) | 0.049 (2) | 0.062 (2) | 0.014 (2) | 0.051 (2) | 0.006 (2) |
C20 | 0.053 (2) | 0.065 (2) | 0.047 (2) | 0.034 (2) | 0.019 (1) | 0.017 (2) |
C21 | 0.053 (2) | 0.089 (3) | 0.058 (2) | 0.040 (2) | 0.023 (2) | 0.021 (2) |
C22 | 0.041 (2) | 0.082 (3) | 0.068 (2) | 0.020 (2) | 0.022 (2) | 0.020 (2) |
C23 | 0.049 (2) | 0.056 (2) | 0.066 (2) | 0.014 (2) | 0.027 (2) | 0.017 (2) |
C24 | 0.044 (2) | 0.046 (2) | 0.039 (1) | 0.015 (1) | 0.020 (1) | 0.011 (1) |
C25 | 0.046 (2) | 0.034 (1) | 0.057 (2) | 0.013 (1) | 0.026 (1) | 0.012 (1) |
C26 | 0.049 (2) | 0.041 (2) | 0.050 (2) | 0.022 (1) | 0.023 (1) | 0.018 (1) |
C27 | 0.044 (1) | 0.047 (2) | 0.036 (1) | 0.021 (1) | 0.022 (1) | 0.015 (1) |
C28 | 0.052 (2) | 0.067 (2) | 0.056 (2) | 0.031 (2) | 0.028 (2) | 0.023 (2) |
C29 | 0.044 (2) | 0.081 (3) | 0.056 (2) | 0.026 (2) | 0.018 (2) | 0.013 (2) |
C30 | 0.046 (2) | 0.061 (2) | 0.058 (2) | 0.008 (2) | 0.024 (2) | 0.002 (2) |
C31 | 0.048 (2) | 0.044 (2) | 0.057 (2) | 0.013 (1) | 0.029 (2) | 0.008 (1) |
C32 | 0.050 (2) | 0.049 (2) | 0.038 (1) | 0.021 (1) | 0.022 (1) | 0.007 (1) |
C33 | 0.046 (2) | 0.050 (2) | 0.033 (1) | 0.021 (1) | 0.022 (1) | 0.010 (1) |
C34 | 0.064 (2) | 0.068 (2) | 0.053 (2) | 0.038 (2) | 0.037 (2) | 0.026 (2) |
C35 | 0.056 (2) | 0.111 (4) | 0.054 (2) | 0.041 (2) | 0.034 (2) | 0.032 (2) |
C36 | 0.068 (2) | 0.073 (3) | 0.063 (2) | 0.012 (2) | 0.039 (2) | 0.020 (2) |
C37 | 0.095 (3) | 0.057 (2) | 0.070 (2) | 0.032 (2) | 0.054 (2) | 0.029 (2) |
C38 | 0.069 (2) | 0.062 (2) | 0.049 (2) | 0.037 (2) | 0.037 (2) | 0.023 (2) |
Cu1—Cl1 | 2.238 (1) | C13—C14 | 1.506 (5) |
Cu1—Cl3 | 2.695 (1) | C13—H13 | 0.960 |
Cu1—N1 | 2.004 (3) | C13—H14 | 0.960 |
Cu1—N2 | 2.053 (3) | C14—C15 | 1.379 (6) |
Cu1—N3 | 1.999 (3) | C14—C19 | 1.376 (6) |
Cu2—Cl2 | 2.252 (1) | C15—C16 | 1.369 (8) |
Cu2—Cl3 | 2.639 (1) | C15—H15 | 0.960 |
Cu2—N4 | 1.988 (3) | C16—C17 | 1.35 (1) |
Cu2—N5 | 2.066 (2) | C16—H16 | 0.960 |
Cu2—N6 | 1.985 (3) | C17—C18 | 1.40 (1) |
Cl4—O1 | 1.393 (4) | C17—H17 | 0.960 |
Cl4—O2 | 1.364 (4) | C18—C19 | 1.422 (7) |
Cl4—O3 | 1.315 (5) | C18—H18 | 0.960 |
Cl4—O4 | 1.345 (6) | C19—H19 | 0.960 |
N1—C1 | 1.342 (4) | C20—C21 | 1.384 (5) |
N1—C5 | 1.344 (4) | C20—H20 | 0.960 |
N2—C6 | 1.488 (4) | C21—C22 | 1.355 (7) |
N2—C7 | 1.480 (4) | C21—H21 | 0.960 |
N2—C13 | 1.502 (4) | C22—C23 | 1.381 (6) |
N3—C8 | 1.347 (4) | C22—H22 | 0.960 |
N3—C12 | 1.344 (4) | C23—C24 | 1.385 (5) |
N4—C20 | 1.345 (4) | C23—H23 | 0.960 |
N4—C24 | 1.335 (4) | C24—C25 | 1.511 (5) |
N5—C25 | 1.489 (4) | C25—H24 | 0.960 |
N5—C26 | 1.486 (4) | C25—H25 | 0.960 |
N5—C32 | 1.508 (4) | C26—C27 | 1.508 (4) |
N6—C27 | 1.344 (4) | C26—H26 | 0.960 |
N6—C31 | 1.343 (4) | C26—H27 | 0.960 |
C1—C2 | 1.384 (5) | C27—C28 | 1.388 (4) |
C1—H1 | 0.960 | C28—C29 | 1.376 (6) |
C2—C3 | 1.367 (6) | C28—H28 | 0.960 |
C2—H2 | 0.960 | C29—C30 | 1.385 (6) |
C3—C4 | 1.374 (6) | C29—H29 | 0.960 |
C3—H3 | 0.960 | C30—C31 | 1.380 (5) |
C4—C5 | 1.380 (5) | C30—H30 | 0.960 |
C4—H4 | 0.960 | C31—H31 | 0.960 |
C5—C6 | 1.490 (5) | C32—C33 | 1.504 (4) |
C6—H5 | 0.960 | C32—H32 | 0.960 |
C6—H6 | 0.960 | C32—H33 | 0.960 |
C7—C8 | 1.490 (5) | C33—C34 | 1.382 (5) |
C7—H7 | 0.960 | C33—C38 | 1.370 (5) |
C7—H8 | 0.960 | C34—C35 | 1.377 (6) |
C8—C9 | 1.395 (5) | C34—H34 | 0.960 |
C9—C10 | 1.391 (6) | C35—C36 | 1.384 (7) |
C9—H9 | 0.960 | C35—H35 | 0.960 |
C10—C11 | 1.374 (6) | C36—C37 | 1.371 (7) |
C10—H10 | 0.960 | C36—H36 | 0.960 |
C11—C12 | 1.376 (5) | C37—C38 | 1.377 (6) |
C11—H11 | 0.960 | C37—H37 | 0.960 |
C12—H12 | 0.960 | C38—H38 | 0.960 |
Cu1···Cl3 | 2.6946 (8) | C1···C2v | 3.293 (5) |
Cu2···Cl3 | 2.6389 (8) | C1···C1v | 3.394 (6) |
O1···C35i | 3.317 (6) | C3···C29vi | 3.566 (6) |
O1···C21ii | 3.468 (7) | C10···C17vii | 3.463 (7) |
O1···C36i | 3.503 (7) | C11···C36viii | 3.598 (6) |
O2···C9iii | 3.428 (6) | C12···C37viii | 3.523 (5) |
O2···C20ii | 3.527 (7) | C12···C36viii | 3.540 (6) |
O3···C16iv | 3.434 (8) | C20···C22ii | 3.562 (6) |
O4···C17v | 3.346 (8) | C34···C34i | 3.394 (7) |
O4···C10iii | 3.594 (9) | ||
Cl1—Cu1—Cl3 | 102.3 (1) | C11—C12—H12 | 118.9 |
Cl1—Cu1—N1 | 97.6 (1) | N2—C13—C14 | 115.1 (3) |
Cl1—Cu1—N2 | 165.1 (1) | N2—C13—H13 | 108.1 |
Cl1—Cu1—N3 | 98.0 (1) | N2—C13—H14 | 108.1 |
Cl3—Cu1—N1 | 94.1 (1) | C14—C13—H13 | 108.1 |
Cl3—Cu1—N2 | 92.5 (1) | C14—C13—H14 | 108.1 |
Cl3—Cu1—N3 | 88.5 (1) | H13—C13—H14 | 109.5 |
N1—Cu1—N2 | 82.0 (1) | C13—C14—C15 | 121.4 (4) |
N1—Cu1—N3 | 163.3 (1) | C13—C14—C19 | 119.1 (4) |
N2—Cu1—N3 | 81.4 (1) | C15—C14—C19 | 119.4 (4) |
Cl2—Cu2—Cl3 | 111.8 (1) | C14—C15—C16 | 121.9 (6) |
Cl2—Cu2—N4 | 97.8 (1) | C14—C15—H15 | 119.1 |
Cl2—Cu2—N5 | 153.4 (1) | C16—C15—H15 | 119.1 |
Cl2—Cu2—N6 | 97.7 (1) | C15—C16—C17 | 119.5 (7) |
Cl3—Cu2—N4 | 85.9 (1) | C15—C16—H16 | 120.3 |
Cl3—Cu2—N5 | 94.8 (1) | C17—C16—H16 | 120.2 |
Cl3—Cu2—N6 | 89.4 (1) | C16—C17—C18 | 121.6 (5) |
N4—Cu2—N5 | 82.5 (1) | C16—C17—H17 | 119 |
N4—Cu2—N6 | 164.5 (1) | C18—C17—H17 | 119 |
N5—Cu2—N6 | 83.2 (1) | C17—C18—C19 | 118.2 (6) |
Cu1—Cl3—Cu2 | 136.9 (1) | C17—C18—H18 | 120.9 |
O1—Cl4—O2 | 114.2 (3) | C19—C18—H18 | 120.9 |
O1—Cl4—O3 | 114.8 (4) | C14—C19—C18 | 119.4 (6) |
O1—Cl4—O4 | 106.1 (4) | C14—C19—H19 | 120.3 |
O2—Cl4—O3 | 112.1 (4) | C18—C19—H19 | 120.3 |
O2—Cl4—O4 | 110.2 (5) | N4—C20—C21 | 121.8 (4) |
O3—Cl4—O4 | 97.9 (6) | N4—C20—H20 | 119.1 |
Cu1—N1—C1 | 127.0 (2) | C21—C20—H20 | 119.1 |
Cu1—N1—C5 | 113.4 (2) | C20—C21—C22 | 119.0 (4) |
C1—N1—C5 | 119.5 (3) | C20—C21—H21 | 120.5 |
Cu1—N2—C6 | 105.6 (2) | C22—C21—H21 | 120.5 |
Cu1—N2—C7 | 105.6 (2) | C21—C22—C23 | 119.7 (3) |
Cu1—N2—C13 | 111.6 (2) | C21—C22—H22 | 120.2 |
C6—N2—C7 | 113.1 (2) | C23—C22—H22 | 120.2 |
C6—N2—C13 | 112.8 (3) | C22—C23—C24 | 119.1 (4) |
C7—N2—C13 | 107.9 (2) | C22—C23—H23 | 120.5 |
Cu1—N3—C8 | 113.3 (2) | C24—C23—H23 | 120.5 |
Cu1—N3—C12 | 127.2 (2) | N4—C24—C23 | 121.3 (3) |
C8—N3—C12 | 119.5 (3) | N4—C24—C25 | 116.9 (3) |
Cu2—N4—C20 | 126.1 (2) | C23—C24—C25 | 121.6 (3) |
Cu2—N4—C24 | 113.7 (2) | N5—C25—C24 | 110.3 (2) |
C20—N4—C24 | 119.2 (3) | N5—C25—H24 | 109.3 |
Cu2—N5—C25 | 106.0 (2) | N5—C25—H25 | 109.3 |
Cu2—N5—C26 | 105.9 (2) | C24—C25—H24 | 109.3 |
Cu2—N5—C32 | 111.2 (2) | C24—C25—H25 | 109.3 |
C25—N5—C26 | 112.3 (2) | H24—C25—H25 | 109.5 |
C25—N5—C32 | 109.0 (2) | N5—C26—C27 | 111.1 (2) |
C26—N5—C32 | 112.2 (2) | N5—C26—H26 | 109.1 |
Cu2—N6—C27 | 114.1 (2) | N5—C26—H27 | 109.1 |
Cu2—N6—C31 | 127.0 (2) | C27—C26—H26 | 109.1 |
C27—N6—C31 | 118.8 (3) | C27—C26—H27 | 109.1 |
N1—C1—C2 | 121.6 (3) | H26—C26—H27 | 109.5 |
N1—C1—H1 | 119.2 | N6—C27—C26 | 116.2 (3) |
C2—C1—H1 | 119.2 | N6—C27—C28 | 122.0 (3) |
C1—C2—C3 | 118.7 (3) | C26—C27—C28 | 121.7 (3) |
C1—C2—H2 | 120.6 | C27—C28—C29 | 118.8 (3) |
C3—C2—H2 | 120.6 | C27—C28—H28 | 120.6 |
C2—C3—C4 | 119.7 (3) | C29—C28—H28 | 120.6 |
C2—C3—H3 | 120.1 | C28—C29—C30 | 119.4 (3) |
C4—C3—H3 | 120.1 | C28—C29—H29 | 120.3 |
C3—C4—C5 | 119.4 (4) | C30—C29—H29 | 120.3 |
C3—C4—H4 | 120.3 | C29—C30—C31 | 118.9 (3) |
C5—C4—H4 | 120.3 | C29—C30—H30 | 120.5 |
N1—C5—C4 | 120.9 (3) | C31—C30—H30 | 120.5 |
N1—C5—C6 | 116.0 (3) | N6—C31—C30 | 122.1 (3) |
C4—C5—C6 | 123.0 (3) | N6—C31—H31 | 119.0 |
N2—C6—C5 | 111.0 (3) | C30—C31—H31 | 119.0 |
N2—C6—H5 | 109.1 | N5—C32—C33 | 113.1 (2) |
N2—C6—H6 | 109.1 | N5—C32—H32 | 108.6 |
C5—C6—H5 | 109.1 | N5—C32—H33 | 108.6 |
C5—C6—H6 | 109.1 | C33—C32—H32 | 108.6 |
H5—C6—H6 | 109.5 | C33—C32—H33 | 108.6 |
N2—C7—C8 | 108.9 (2) | H32—C32—H33 | 109.5 |
N2—C7—H7 | 109.6 | C32—C33—C34 | 120.8 (3) |
N2—C7—H8 | 109.6 | C32—C33—C38 | 119.9 (3) |
C8—C7—H7 | 109.6 | C34—C33—C38 | 119.3 (3) |
C8—C7—H8 | 109.6 | C33—C34—C35 | 120.1 (4) |
H7—C7—H8 | 109.5 | C33—C34—H34 | 120.0 |
N3—C8—C7 | 116.1 (3) | C35—C34—H34 | 120.0 |
N3—C8—C9 | 121.0 (3) | C34—C35—C36 | 119.9 (4) |
C7—C8—C9 | 122.9 (3) | C34—C35—H35 | 120.0 |
C8—C9—C10 | 118.8 (3) | C36—C35—H35 | 120.0 |
C8—C9—H9 | 120.6 | C35—C36—C37 | 120.0 (4) |
C10—C9—H9 | 120.6 | C35—C36—H36 | 120.0 |
C9—C10—C11 | 119.5 (3) | C37—C36—H36 | 120.0 |
C9—C10—H10 | 120.2 | C36—C37—C38 | 119.5 (4) |
C11—C10—H10 | 120.2 | C36—C37—H37 | 120.2 |
C10—C11—C12 | 119.0 (4) | C38—C37—H37 | 120.2 |
C10—C11—H11 | 120.5 | C33—C38—C37 | 121.1 (4) |
C12—C11—H11 | 120.5 | C33—C38—H38 | 119.5 |
N3—C12—C11 | 122.2 (3) | C37—C38—H38 | 119.5 |
N3—C12—H12 | 118.9 |
Symmetry codes: (i) −x+1, −y, −z−1; (ii) −x, −y, −z−1; (iii) x−1, y−1, z−1; (iv) x, y−1, z−1; (v) −x, −y, −z; (vi) x−1, y, z; (vii) −x+1, −y+1, −z+1; (viii) x, y, z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cu2Cl3(C19H19N3)2]ClO4·0.5H2O |
Mr | 920.67 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 300 |
a, b, c (Å) | 13.799 (2), 14.488 (2), 12.608 (2) |
α, β, γ (°) | 99.33 (1), 111.86 (1), 113.14 (1) |
V (Å3) | 2005.9 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.38 |
Crystal size (mm) | 0.3 (radius) |
Data collection | |
Diffractometer | Rigaku AFC-5S diffractometer |
Absorption correction | For a sphere (International Tables for Crystallography, 1992, Vol.C) |
Tmin, Tmax | 0.545, 0.552 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9581, 9196, 6985 |
Rint | 0.012 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.141, 1.02 |
No. of reflections | 9196 |
No. of parameters | 493 |
No. of restraints | ? |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.42, −0.35 |
Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), SIR92 (Altomare et al., 1994), TEXSAN.
Cu1—Cl1 | 2.238 (1) | Cu2—Cl2 | 2.252 (1) |
Cu1—Cl3 | 2.695 (1) | Cu2—Cl3 | 2.639 (1) |
Cu1—N1 | 2.004 (3) | Cu2—N4 | 1.988 (3) |
Cu1—N2 | 2.053 (3) | Cu2—N5 | 2.066 (2) |
Cu1—N3 | 1.999 (3) | Cu2—N6 | 1.985 (3) |
Cl1—Cu1—N2 | 165.1 (1) | N4—Cu2—N6 | 164.5 (1) |
N1—Cu1—N3 | 163.3 (1) | Cu1—Cl3—Cu2 | 136.9 (1) |
Cl2—Cu2—N5 | 153.4 (1) |
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The abbreviation for the tridentate benzyl(2-pyridylmethyl)amine ligand in the title compound, (I), is bzpy, and that of its 2-hydroxy derivative is phpyH. In the crystals of [Cu(phpyH)Cl]ClO4.CH3OH, which is a model compound for galactose oxidase, a rather long CuII–phenolic oxygen distance of 2.570 (4) Å was observed (Ito et al., 1998).