Supporting information
Crystallographic Information File (CIF) |
CCDC reference: 125242
PDB reference: ruthenium-modified azurin, 1bex
%TThe Ru atom position was found from the Patterson map and the remaining heavy atom coordinates were obtained from subsequent structure factor-Fourier calculations. H atoms were positioned by calculation (C-H, 0.95 AA), and assigned $B$ values 1.15 times the $U_{eq}$ of the bonded C atom. H atoms of the water molecules were ignored. The large displacement parameters for the water oxygens may indicate partial occupancy. Two of the larger peaks in the final difference map (1.18 and 1.01 eAA${-3}$) may also indicate partial water molecules, although these peaks are within 1.9 AA\ of other waters. Thus, the exact water content of the crystal is uncertain by $πm 2$ H$_2$O. There is extensive hydrogen bonding among the sulfate oxygen atoms, N7 and N8 of the imidazole groups and the water molecules, but in view of the uncertainties in water content, a detailed description of this network could not be developed. Atoms N7 and N8 of the imidazole groups were assigned based on their heigths in the Fourier maps. A least-squares calculation interchanging N7 and C22, and N8 and C25 gave higher values of R-indices and goodness-of-fit, and gave displacement parameters for those four atoms indicating that the original assignment was correct.
Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software (Enraf-Nonius, 1989); data reduction: CRYM (Duchamp, 1964); program(s) used to refine structure: CRYM (Duchamp, 1964); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: CRYM (Duchamp, 1964).
C26H44N8O14RuS | Dx = 1.49 Mg m−3 |
Mr = 825.81 | Mo Kα radiation, λ = 0.7107 Å |
Monoclinic, P21/n | Cell parameters from 25 reflections |
a = 13.230 (2) Å | θ = 9–13° |
b = 18.197 (4) Å | µ = 0.54 mm−1 |
c = 16.126 (4) Å | T = 297 K |
β = 108.65 (2)° | Needle, red |
V = 3678.4 (15) Å3 | 0.43 × 0.10 × 0.07 mm |
Z = 4 |
CAD-4 diffractometer | Rint = 0.031 |
Radiation source: Normal focus sealed tube | θmax = 20°, θmin = 1° |
Graphite monochromator | h = 0→11 |
Ω scans | k = −15→15 |
3430 measured reflections | l = −13→13 |
7815 independent reflections | 3 standard reflections every 150 minutes min |
7815 reflections with All | intensity decay: 13.8% |
Refinement on F2 | Primary atom site location: Patterson |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.091 | Hydrogen site location: calculated |
wR(F2) = 0.17 | H-atom parameters not refined |
S = 3.53 | Calculated w = 1/σ2(Fo2) |
3429 reflections | (Δ/σ)max = 0.05 |
411 parameters | Δρmax = 1.24 e Å−3 |
0 restraints | Δρmin = −0.89 e Å−3 |
C26H44N8O14RuS | V = 3678.4 (15) Å3 |
Mr = 825.81 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.230 (2) Å | µ = 0.54 mm−1 |
b = 18.197 (4) Å | T = 297 K |
c = 16.126 (4) Å | 0.43 × 0.10 × 0.07 mm |
β = 108.65 (2)° |
CAD-4 diffractometer | Rint = 0.031 |
3430 measured reflections | θmax = 20° |
7815 independent reflections | 3 standard reflections every 150 minutes min |
7815 reflections with All | intensity decay: 13.8% |
R[F2 > 2σ(F2)] = 0.091 | 0 restraints |
wR(F2) = 0.17 | H-atom parameters not refined |
S = 3.53 | Δρmax = 1.24 e Å−3 |
3429 reflections | Δρmin = −0.89 e Å−3 |
411 parameters |
x | y | z | Uiso*/Ueq | ||
Ru | 0.16626 (9) | 0.22528 (6) | 0.16175 (6) | 0.0429 (3) | |
N1 | 0.2801 (8) | 0.3057 (5) | 0.1919 (7) | 0.044 (3) | |
C1 | 0.3210 (12) | 0.3373 (9) | 0.1357 (9) | 0.068 (4) | |
C2 | 0.3927 (13) | 0.3958 (9) | 0.1592 (11) | 0.073 (5) | |
C3 | 0.4211 (13) | 0.4215 (8) | 0.2429 (12) | 0.080 (5) | |
C4 | 0.3794 (13) | 0.3896 (9) | 0.3008 (9) | 0.074 (5) | |
C5 | 0.3074 (11) | 0.3320 (7) | 0.2760 (9) | 0.046 (4) | |
C6 | 0.2587 (11) | 0.2955 (7) | 0.3308 (8) | 0.044 (4) | |
C7 | 0.2840 (12) | 0.3094 (8) | 0.4176 (10) | 0.075 (5) | |
C8 | 0.2358 (14) | 0.2695 (11) | 0.4680 (9) | 0.090 (6) | |
C9 | 0.1646 (12) | 0.2164 (9) | 0.4305 (9) | 0.071 (5) | |
C10 | 0.1402 (10) | 0.2045 (7) | 0.3415 (8) | 0.052 (4) | |
N2 | 0.1871 (8) | 0.2428 (6) | 0.2923 (6) | 0.040 (3) | |
N3 | 0.0540 (8) | 0.3046 (5) | 0.1121 (7) | 0.046 (3) | |
C11 | 0.0071 (13) | 0.3467 (8) | 0.1573 (9) | 0.063 (4) | |
C12 | −0.0689 (13) | 0.4005 (10) | 0.1189 (13) | 0.078 (6) | |
C13 | −0.0949 (15) | 0.4129 (10) | 0.0336 (16) | 0.105 (7) | |
C14 | −0.0460 (15) | 0.3710 (11) | −0.0154 (10) | 0.097 (7) | |
C15 | 0.0278 (12) | 0.3162 (8) | 0.0239 (11) | 0.060 (5) | |
C16 | 0.0792 (11) | 0.2676 (9) | −0.0214 (9) | 0.053 (4) | |
C17 | 0.0595 (13) | 0.2688 (10) | −0.1118 (10) | 0.083 (6) | |
C18 | 0.1082 (16) | 0.2228 (12) | −0.1509 (10) | 0.095 (7) | |
C19 | 0.1785 (14) | 0.1717 (10) | −0.0988 (11) | 0.084 (6) | |
C20 | 0.1976 (11) | 0.1711 (8) | −0.0066 (9) | 0.064 (4) | |
N4 | 0.1485 (8) | 0.2190 (7) | 0.0302 (6) | 0.045 (3) | |
N5 | 0.0447 (9) | 0.1464 (6) | 0.1370 (6) | 0.042 (3) | |
C21 | −0.0458 (13) | 0.1519 (8) | 0.1514 (8) | 0.051 (4) | |
N7 | −0.1096 (9) | 0.0925 (8) | 0.1217 (7) | 0.060 (4) | |
C22 | −0.0558 (14) | 0.0472 (8) | 0.0848 (9) | 0.064 (5) | |
C23 | 0.0383 (12) | 0.0791 (8) | 0.0941 (8) | 0.055 (4) | |
N6 | 0.2815 (9) | 0.1429 (6) | 0.2049 (6) | 0.047 (4) | |
C24 | 0.3771 (15) | 0.1394 (9) | 0.1958 (9) | 0.060 (5) | |
N8 | 0.4290 (10) | 0.0790 (9) | 0.2319 (9) | 0.074 (4) | |
C25 | 0.3653 (17) | 0.0412 (8) | 0.2662 (10) | 0.078 (6) | |
C26 | 0.2732 (12) | 0.0805 (9) | 0.2503 (9) | 0.061 (5) | |
S1 | 0.6914 (5) | 0.0109 (4) | 0.2035 (4) | 0.135 (2) | |
O1 | 0.6903 (11) | 0.0613 (10) | 0.1371 (9) | 0.226 (8) | |
O2 | 0.6387 (10) | 0.0474 (9) | 0.2540 (9) | 0.164 (6) | |
O3 | 0.8027 (11) | −0.0164 (8) | 0.2553 (10) | 0.159 (6) | |
O4 | 0.6212 (19) | −0.0501 (17) | 0.1580 (17) | 0.357 (15) | |
W1 | 0.9745 (9) | 0.0693 (6) | 0.3516 (8) | 0.116 (4) | |
W2 | 0.7327 (10) | 0.0829 (7) | 0.4297 (7) | 0.126 (4) | |
W3 | 0.8790 (11) | 0.1842 (8) | 0.4134 (8) | 0.151 (5)* | |
W4 | 0.1306 (13) | 0.0319 (8) | 0.5050 (10) | 0.184 (6)* | |
W5 | 0.1659 (14) | 0.1409 (9) | 0.6443 (10) | 0.190 (6)* | |
W6 | 0.9990 (15) | 0.2545 (10) | 0.5768 (11) | 0.220 (8)* | |
W7 | 0.3538 (14) | 0.2244 (10) | 0.7707 (11) | 0.210 (7)* | |
W8 | 0.6901 (15) | −0.0060 (11) | 0.9658 (11) | 0.227 (8)* | |
W9 | 0.500 (2) | 0.1086 (14) | 0.0306 (17) | 0.339 (13)* | |
W10 | 0.5488 (19) | 0.1017 (12) | 0.8662 (14) | 0.272 (10)* | |
H1 | 0.301 | 0.319 | 0.077 | 0.077* | |
H2 | 0.421 | 0.417 | 0.118 | 0.082* | |
H3 | 0.470 | 0.461 | 0.261 | 0.092* | |
H4 | 0.400 | 0.407 | 0.359 | 0.084* | |
H7 | 0.335 | 0.347 | 0.444 | 0.085* | |
H8 | 0.252 | 0.279 | 0.529 | 0.104* | |
H9 | 0.132 | 0.188 | 0.464 | 0.081* | |
H10 | 0.089 | 0.168 | 0.314 | 0.058* | |
H11 | 0.026 | 0.340 | 0.219 | 0.071* | |
H12 | −0.102 | 0.428 | 0.154 | 0.089* | |
H13 | −0.146 | 0.450 | 0.007 | 0.119* | |
H14 | −0.063 | 0.380 | −0.077 | 0.110* | |
H17 | 0.010 | 0.303 | −0.147 | 0.094* | |
H18 | 0.097 | 0.225 | −0.212 | 0.109* | |
H19 | 0.214 | 0.137 | −0.124 | 0.095* | |
H20 | 0.247 | 0.137 | 0.029 | 0.072* | |
H21 | −0.066 | 0.193 | 0.180 | 0.058* | |
HN7 | −0.179 | 0.085 | 0.126 | 0.070* | |
H22 | −0.080 | 0.002 | 0.057 | 0.073* | |
H23 | 0.093 | 0.059 | 0.075 | 0.062* | |
H24 | 0.405 | 0.176 | 0.167 | 0.068* | |
HN8 | 0.499 | 0.065 | 0.233 | 0.085* | |
H25 | 0.382 | −0.005 | 0.296 | 0.090* | |
H26 | 0.213 | 0.067 | 0.268 | 0.070* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru | 0.0431 (7) | 0.0529 (7) | 0.0317 (6) | −0.0065 (7) | 0.0106 (5) | −0.0030 (6) |
N1 | 0.038 (7) | 0.044 (7) | 0.051 (7) | −0.003 (5) | 0.017 (6) | 0.000 (6) |
C1 | 0.070 (11) | 0.087 (12) | 0.057 (10) | −0.021 (10) | 0.035 (9) | −0.002 (9) |
C2 | 0.076 (12) | 0.072 (12) | 0.081 (13) | −0.027 (10) | 0.040 (10) | 0.005 (10) |
C3 | 0.084 (13) | 0.079 (13) | 0.073 (12) | −0.028 (10) | 0.019 (11) | −0.006 (10) |
C4 | 0.094 (13) | 0.074 (12) | 0.051 (10) | −0.024 (11) | 0.017 (10) | −0.018 (9) |
C5 | 0.055 (10) | 0.045 (9) | 0.035 (9) | −0.011 (8) | 0.009 (8) | −0.014 (8) |
C6 | 0.056 (10) | 0.047 (10) | 0.031 (9) | −0.008 (8) | 0.019 (8) | −0.013 (7) |
C7 | 0.070 (11) | 0.091 (12) | 0.063 (11) | −0.045 (9) | 0.020 (9) | −0.023 (9) |
C8 | 0.097 (13) | 0.132 (15) | 0.045 (9) | −0.031 (13) | 0.027 (10) | −0.015 (11) |
C9 | 0.083 (12) | 0.094 (13) | 0.048 (10) | −0.028 (10) | 0.036 (9) | −0.006 (9) |
C10 | 0.037 (9) | 0.078 (11) | 0.036 (9) | −0.011 (7) | 0.005 (7) | −0.007 (7) |
N2 | 0.038 (7) | 0.052 (8) | 0.030 (6) | 0.001 (6) | 0.012 (6) | −0.001 (6) |
N3 | 0.048 (7) | 0.047 (8) | 0.045 (8) | −0.009 (6) | 0.019 (7) | −0.003 (6) |
C11 | 0.074 (12) | 0.056 (11) | 0.054 (10) | −0.002 (10) | 0.016 (9) | −0.009 (9) |
C12 | 0.063 (12) | 0.084 (14) | 0.082 (13) | 0.018 (10) | 0.016 (11) | −0.004 (11) |
C13 | 0.089 (15) | 0.096 (15) | 0.116 (18) | 0.043 (12) | 0.012 (14) | 0.011 (13) |
C14 | 0.078 (14) | 0.123 (17) | 0.068 (12) | 0.008 (13) | −0.011 (11) | 0.043 (12) |
C15 | 0.047 (10) | 0.072 (11) | 0.054 (11) | −0.007 (9) | 0.008 (9) | 0.011 (9) |
C16 | 0.056 (10) | 0.071 (10) | 0.034 (9) | −0.011 (10) | 0.016 (8) | 0.001 (9) |
C17 | 0.088 (13) | 0.108 (13) | 0.045 (11) | 0.014 (12) | 0.012 (9) | −0.002 (10) |
C18 | 0.102 (15) | 0.141 (17) | 0.036 (10) | −0.011 (14) | 0.013 (10) | 0.014 (12) |
C19 | 0.090 (14) | 0.129 (16) | 0.051 (12) | −0.034 (12) | 0.047 (10) | −0.034 (10) |
C20 | 0.063 (11) | 0.074 (11) | 0.059 (11) | −0.008 (9) | 0.025 (9) | −0.008 (8) |
N4 | 0.043 (7) | 0.064 (8) | 0.037 (7) | −0.005 (7) | 0.023 (6) | 0.001 (7) |
N5 | 0.040 (8) | 0.056 (9) | 0.035 (6) | −0.004 (6) | 0.017 (6) | 0.005 (6) |
C21 | 0.054 (11) | 0.061 (11) | 0.035 (8) | −0.002 (9) | 0.011 (8) | 0.000 (7) |
N7 | 0.047 (8) | 0.080 (10) | 0.049 (8) | −0.022 (8) | 0.009 (7) | 0.003 (7) |
C22 | 0.059 (12) | 0.065 (11) | 0.064 (11) | −0.022 (10) | 0.012 (10) | 0.001 (8) |
C23 | 0.066 (12) | 0.053 (10) | 0.043 (9) | 0.008 (9) | 0.015 (8) | −0.004 (8) |
N6 | 0.047 (9) | 0.050 (9) | 0.040 (7) | −0.001 (6) | 0.006 (6) | −0.006 (6) |
C24 | 0.055 (12) | 0.070 (13) | 0.055 (10) | 0.001 (10) | 0.016 (9) | −0.017 (9) |
N8 | 0.058 (9) | 0.090 (12) | 0.069 (9) | 0.015 (10) | 0.013 (8) | −0.022 (8) |
C25 | 0.081 (14) | 0.060 (12) | 0.076 (12) | 0.011 (12) | 0.003 (11) | 0.011 (9) |
C26 | 0.056 (11) | 0.064 (11) | 0.054 (10) | 0.002 (10) | 0.004 (8) | 0.001 (9) |
S1 | 0.086 (5) | 0.198 (7) | 0.120 (5) | −0.020 (5) | 0.030 (4) | −0.007 (5) |
O1 | 0.130 (13) | 0.35 (2) | 0.155 (13) | −0.062 (14) | −0.019 (10) | 0.204 (16) |
O2 | 0.091 (10) | 0.263 (18) | 0.137 (11) | 0.090 (11) | 0.036 (9) | −0.046 (11) |
O3 | 0.097 (11) | 0.181 (15) | 0.206 (16) | −0.009 (11) | 0.056 (11) | −0.029 (12) |
O4 | 0.21 (3) | 0.46 (4) | 0.35 (3) | −0.09 (3) | 0.00 (2) | −0.15 (3) |
W1 | 0.107 (9) | 0.110 (9) | 0.133 (10) | −0.003 (8) | 0.042 (8) | 0.011 (7) |
W2 | 0.123 (11) | 0.145 (11) | 0.111 (9) | 0.012 (9) | 0.040 (8) | −0.012 (8) |
Experimental details
Crystal data | |
Chemical formula | C26H44N8O14RuS |
Mr | 825.81 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 297 |
a, b, c (Å) | 13.230 (2), 18.197 (4), 16.126 (4) |
β (°) | 108.65 (2) |
V (Å3) | 3678.4 (15) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.54 |
Crystal size (mm) | 0.43 × 0.10 × 0.07 |
Data collection | |
Diffractometer | CAD-4 diffractometer |
Absorption correction | – |
No. of measured, independent and observed (All) reflections | 3430, 7815, 7815 |
Rint | 0.031 |
θmax (°) | 20 |
(sin θ/λ)max (Å−1) | 0.481 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.091, 0.17, 3.53 |
No. of reflections | 3429 |
No. of parameters | 411 |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 1.24, −0.89 |
Computer programs: CAD-4 Software (Enraf-Nonius, 1989), CRYM (Duchamp, 1964), ORTEPII (Johnson, 1976).