Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804017507/lh6249sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804017507/lh6249Isup2.hkl |
CCDC reference: 248752
Data collection: SMART-W2K/NT (Bruker, 2003); cell refinement: SAINT-W2K/NT (Bruker, 2003); data reduction: SAINT-W2K/NT; program(s) used to solve structure: SHELXTL-NT (Bruker, 2003); program(s) used to refine structure: SHELXTL-NT; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL-NT.
[RuCl2(C12H8N2O4)2]·H2O | F(000) = 1360 |
Mr = 678.39 | Dx = 1.795 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5415 reflections |
a = 12.2172 (7) Å | θ = 2.3–27.9° |
b = 11.0152 (7) Å | µ = 0.90 mm−1 |
c = 19.5064 (12) Å | T = 173 K |
β = 106.999 (1)° | Plate, black |
V = 2510.4 (3) Å3 | 0.26 × 0.23 × 0.21 mm |
Z = 4 |
Bruker SMART APEX CCD area-detector diffractometer | 5983 independent reflections |
Radiation source: fine-focus sealed tube | 5466 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
Detector resolution: 8.366 pixels mm-1 | θmax = 27.9°, θmin = 1.8° |
φ and ω scans | h = −16→15 |
Absorption correction: multi-scan (SADABS; Scheldrick, 1996) | k = −14→14 |
Tmin = 0.800, Tmax = 0.833 | l = −19→25 |
17958 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0407P)2 + 1.3308P] where P = (Fo2 + 2Fc2)/3 |
5983 reflections | (Δ/σ)max = 0.001 |
387 parameters | Δρmax = 0.68 e Å−3 |
0 restraints | Δρmin = −0.43 e Å−3 |
Experimental. none |
Geometry. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 5.0552 (0.0133) x + 9.0634 (0.0185) y + 4.9075 (0.0474) z = 6.4469 (0.0287) * 0.0000 (0.0000) C11 * 0.0000 (0.0000) O1 * 0.0000 (0.0000) O2 Rms deviation of fitted atoms = 0.0000 4.4379 (0.0082) x + 8.9784 (0.0043) y + 6.3473 (0.0127) z = 6.7378 (0.0035) Angle to previous plane (with approximate e.s.d.) = 4.59 (0.26) * 0.0093 (0.0011) N1 * -0.0043 (0.0012) C1 * -0.0046 (0.0013) C2 * 0.0084 (0.0012) C3 * -0.0035 (0.0012) C4 * -0.0053 (0.0011) C5 Rms deviation of fitted atoms = 0.0063 3.1503 (0.0078) x + 9.3619 (0.0042) y + 7.1016 (0.0123) z = 6.7018 (0.0023) Angle to previous plane (with approximate e.s.d.) = 6.38 (0.09) * 0.0099 (0.0010) N2 * -0.0127 (0.0011) C6 * 0.0047 (0.0011) C7 * 0.0059 (0.0012) C8 * -0.0088 (0.0012) C9 * 0.0010 (0.0012) C10 Rms deviation of fitted atoms = 0.0081 3.4444 (0.0419) x + 9.3708 (0.0073) y + 6.6675 (0.0589) z = 6.5628 (0.0231) Angle to previous plane (with approximate e.s.d.) = 1.65 (0.26) * 0.0000 (0.0000) C12 * 0.0000 (0.0000) O3 * 0.0000 (0.0000) O4 Rms deviation of fitted atoms = 0.0000 3.7624 (0.0134) x - 9.2224 (0.0203) y + 6.6730 (0.0538) z = 0.0459 (0.0030) Angle to previous plane (with approximate e.s.d.) = 64.85 (0.17) * 0.0000 (0.0000) C23 * 0.0000 (0.0000) O5 * 0.0000 (0.0000) O6 Rms deviation of fitted atoms = 0.0000 3.5180 (0.0081) x - 8.7665 (0.0043) y + 8.2936 (0.0117) z = 0.0896 (0.0030) Angle to previous plane (with approximate e.s.d.) = 5.33 (0.30) * -0.0251 (0.0011) N3 * 0.0077 (0.0011) C13 * 0.0160 (0.0012) C14 * -0.0225 (0.0012) C15 * 0.0055 (0.0012) C16 * 0.0183 (0.0011) C17 Rms deviation of fitted atoms = 0.0174 - 1.3653 (0.0088) x + 8.6389 (0.0054) y - 10.7468 (0.0122) z = 0.5754 (0.0064) Angle to previous plane (with approximate e.s.d.) = 11.07 (0.10) * 0.0027 (0.0012) N4 * -0.0053 (0.0012) C18 * 0.0019 (0.0013) C19 * 0.0039 (0.0013) C20 * -0.0064 (0.0014) C21 * 0.0032 (0.0013) C22 Rms deviation of fitted atoms = 0.0042 - 1.7697 (0.0391) x + 8.7386 (0.0079) y - 10.2045 (0.0453) z = 0.3661 (0.0280) Angle to previous plane (with approximate e.s.d.) = 2.25 (0.24) * 0.0000 (0.0000) C24 * 0.0000 (0.0000) O7 * 0.0000 (0.0000) O8 Rms deviation of fitted atoms = 0.0000 3.7550 (0.0028) x + 9.1500 (0.0016) y + 6.9072 (0.0067) z = 6.6526 (0.0015) Angle to previous plane (with approximate e.s.d.) = 70.13 (0.10) * 0.0004 (0.0013) N1 * -0.0842 (0.0015) C1 * -0.0922 (0.0016) C2 * -0.0105 (0.0015) C3 * 0.0514 (0.0016) C4 * 0.0535 (0.0015) C5 * 0.0349 (0.0013) C11 * 0.0863 (0.0012) N2 * 0.0763 (0.0015) C6 * 0.0385 (0.0015) C7 * -0.0301 (0.0015) C8 * -0.0574 (0.0016) C9 * 0.0095 (0.0015) C10 * -0.0765 (0.0013) C12 3.0730 (0.0020) N3_$3 3.1214 (0.0022) C13_$3 3.2294 (0.0020) C14_$3 3.2794 (0.0019) C15_$3 3.2920 (0.0020) C16_$3 3.2026 (0.0021) C17_$3 3.2956 (0.0019) C23_$3 3.0390 (0.0023) N4_$3 3.2656 (0.0023) C18_$3 3.5969 (0.0024) C19_$3 3.7131 (0.0026) C20_$3 3.4984 (0.0029) C21_$3 3.1562 (0.0029) C22_$3 4.0469 (0.0027) C24_$3 Rms deviation of fitted atoms = 0.0581 [$3 = symmetry transformation (x + 1/2,-y + 1/2, z + 1/2)] |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ru1 | 0.411752 (11) | 0.412693 (12) | 0.233999 (7) | 0.01680 (6) | |
Cl1 | 0.33489 (4) | 0.56866 (4) | 0.14632 (2) | 0.02382 (9) | |
Cl2 | 0.49439 (4) | 0.57685 (4) | 0.31602 (2) | 0.02208 (9) | |
N1 | 0.47078 (12) | 0.29585 (13) | 0.31534 (7) | 0.0192 (3) | |
N2 | 0.27878 (12) | 0.41250 (12) | 0.27763 (8) | 0.0182 (3) | |
N3 | 0.35091 (12) | 0.28330 (12) | 0.15838 (7) | 0.0176 (3) | |
N4 | 0.54696 (12) | 0.39383 (13) | 0.19329 (8) | 0.0198 (3) | |
C1 | 0.57049 (15) | 0.23567 (16) | 0.32862 (9) | 0.0241 (3) | |
C2 | 0.61569 (15) | 0.16976 (16) | 0.39020 (9) | 0.0239 (3) | |
C3 | 0.55563 (14) | 0.16486 (15) | 0.44117 (9) | 0.0204 (3) | |
C4 | 0.45128 (14) | 0.22490 (15) | 0.42732 (9) | 0.0209 (3) | |
C5 | 0.41002 (14) | 0.28988 (15) | 0.36398 (9) | 0.0189 (3) | |
C6 | 0.29984 (14) | 0.35426 (14) | 0.34188 (8) | 0.0183 (3) | |
C7 | 0.22075 (14) | 0.35352 (15) | 0.38039 (9) | 0.0202 (3) | |
C8 | 0.11605 (15) | 0.41078 (15) | 0.35153 (9) | 0.0207 (3) | |
C9 | 0.09364 (14) | 0.46723 (16) | 0.28498 (10) | 0.0232 (3) | |
C10 | 0.17668 (15) | 0.46692 (16) | 0.24993 (9) | 0.0222 (3) | |
C11 | 0.60507 (15) | 0.09795 (15) | 0.50950 (9) | 0.0205 (3) | |
C12 | 0.03060 (16) | 0.40952 (16) | 0.39293 (10) | 0.0255 (4) | |
C13 | 0.24909 (14) | 0.22645 (15) | 0.14544 (9) | 0.0199 (3) | |
C14 | 0.20595 (14) | 0.15249 (15) | 0.08656 (9) | 0.0203 (3) | |
C15 | 0.26901 (14) | 0.13625 (15) | 0.03800 (9) | 0.0199 (3) | |
C16 | 0.37642 (14) | 0.19000 (15) | 0.05262 (9) | 0.0212 (3) | |
C17 | 0.41588 (14) | 0.26176 (15) | 0.11328 (9) | 0.0192 (3) | |
C18 | 0.52974 (14) | 0.31851 (15) | 0.13568 (9) | 0.0203 (3) | |
C19 | 0.61579 (15) | 0.29394 (16) | 0.10433 (9) | 0.0229 (3) | |
C20 | 0.72256 (14) | 0.34668 (16) | 0.13298 (9) | 0.0228 (3) | |
C21 | 0.74029 (16) | 0.42238 (17) | 0.19254 (10) | 0.0274 (4) | |
C22 | 0.65110 (16) | 0.44446 (18) | 0.22072 (10) | 0.0263 (4) | |
C23 | 0.22296 (15) | 0.06469 (16) | −0.02942 (10) | 0.0219 (3) | |
C24 | 0.81493 (15) | 0.32232 (16) | 0.09881 (9) | 0.0233 (3) | |
O1 | 0.70141 (11) | 0.04331 (13) | 0.51116 (7) | 0.0285 (3) | |
O2 | 0.56231 (11) | 0.09528 (11) | 0.55848 (7) | 0.0253 (3) | |
O3 | −0.06527 (12) | 0.46813 (17) | 0.36008 (8) | 0.0406 (4) | |
O4 | 0.04845 (13) | 0.36221 (18) | 0.45021 (9) | 0.0482 (4) | |
O5 | 0.12117 (11) | 0.01857 (13) | −0.03576 (7) | 0.0281 (3) | |
O6 | 0.27282 (12) | 0.05265 (15) | −0.07417 (8) | 0.0354 (3) | |
O7 | 0.91114 (11) | 0.38004 (13) | 0.13156 (7) | 0.0276 (3) | |
O8 | 0.80164 (11) | 0.25868 (13) | 0.04662 (7) | 0.0319 (3) | |
H1 | 0.6114 | 0.2388 | 0.2940 | 0.029* | |
H2 | 0.6865 | 0.1283 | 0.3980 | 0.029* | |
H4 | 0.4086 | 0.2215 | 0.4609 | 0.025* | |
H7 | 0.2379 | 0.3145 | 0.4257 | 0.024* | |
H9 | 0.0220 | 0.5055 | 0.2640 | 0.028* | |
H10 | 0.1614 | 0.5064 | 0.2048 | 0.027* | |
H13 | 0.2054 | 0.2377 | 0.1780 | 0.024* | |
H14 | 0.1342 | 0.1131 | 0.0792 | 0.024* | |
H16 | 0.4223 | 0.1777 | 0.0214 | 0.025* | |
H19 | 0.6018 | 0.2418 | 0.0639 | 0.028* | |
H21 | 0.8131 | 0.4584 | 0.2135 | 0.033* | |
H22 | 0.6634 | 0.4971 | 0.2608 | 0.032* | |
H51 | 0.732 (2) | 0.007 (2) | 0.5529 (15) | 0.053 (8)* | |
H52 | −0.114 (2) | 0.460 (3) | 0.3843 (14) | 0.052 (8)* | |
H53 | 0.098 (2) | −0.018 (2) | −0.0756 (13) | 0.039 (7)* | |
H54 | 0.957 (2) | 0.378 (2) | 0.1070 (13) | 0.039 (7)* | |
O10A | 0.5347 (4) | 0.5949 (3) | 0.0574 (2) | 0.0933 (16) | 0.710 (5) |
O10B | 0.6317 (11) | 0.7128 (7) | 0.1944 (5) | 0.120 (5) | 0.290 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.01690 (8) | 0.01976 (8) | 0.01514 (8) | 0.00012 (4) | 0.00689 (6) | 0.00008 (4) |
Cl1 | 0.0273 (2) | 0.02253 (19) | 0.0197 (2) | −0.00075 (15) | 0.00396 (16) | 0.00264 (14) |
Cl2 | 0.0228 (2) | 0.0242 (2) | 0.01894 (19) | 0.00024 (14) | 0.00568 (16) | −0.00272 (14) |
N1 | 0.0196 (6) | 0.0234 (7) | 0.0162 (6) | −0.0006 (5) | 0.0075 (5) | 0.0000 (5) |
N2 | 0.0186 (7) | 0.0200 (7) | 0.0171 (7) | −0.0009 (5) | 0.0066 (5) | −0.0010 (5) |
N3 | 0.0177 (6) | 0.0191 (6) | 0.0174 (6) | 0.0013 (5) | 0.0074 (5) | 0.0023 (5) |
N4 | 0.0200 (7) | 0.0241 (7) | 0.0169 (7) | −0.0012 (5) | 0.0080 (6) | −0.0013 (5) |
C1 | 0.0241 (8) | 0.0282 (9) | 0.0238 (8) | 0.0033 (7) | 0.0129 (7) | 0.0012 (7) |
C2 | 0.0219 (8) | 0.0253 (8) | 0.0262 (9) | 0.0046 (6) | 0.0096 (7) | 0.0019 (7) |
C3 | 0.0205 (8) | 0.0207 (8) | 0.0202 (8) | −0.0002 (6) | 0.0063 (6) | 0.0003 (6) |
C4 | 0.0209 (8) | 0.0232 (8) | 0.0203 (8) | −0.0013 (6) | 0.0087 (6) | 0.0006 (6) |
C5 | 0.0190 (7) | 0.0201 (7) | 0.0190 (7) | −0.0016 (6) | 0.0081 (6) | −0.0015 (6) |
C6 | 0.0193 (7) | 0.0183 (7) | 0.0178 (7) | −0.0008 (6) | 0.0060 (6) | −0.0005 (6) |
C7 | 0.0222 (8) | 0.0206 (8) | 0.0186 (7) | −0.0005 (6) | 0.0072 (6) | 0.0008 (6) |
C8 | 0.0191 (8) | 0.0226 (8) | 0.0218 (8) | −0.0016 (6) | 0.0083 (7) | −0.0010 (6) |
C9 | 0.0179 (8) | 0.0275 (9) | 0.0240 (8) | 0.0022 (6) | 0.0057 (6) | 0.0013 (7) |
C10 | 0.0230 (8) | 0.0250 (8) | 0.0190 (8) | 0.0020 (7) | 0.0068 (6) | 0.0023 (6) |
C11 | 0.0183 (8) | 0.0204 (8) | 0.0226 (8) | −0.0017 (6) | 0.0058 (6) | −0.0001 (6) |
C12 | 0.0220 (8) | 0.0304 (9) | 0.0264 (9) | −0.0001 (7) | 0.0105 (7) | 0.0008 (7) |
C13 | 0.0192 (7) | 0.0226 (8) | 0.0205 (8) | 0.0002 (6) | 0.0097 (6) | 0.0021 (6) |
C14 | 0.0192 (7) | 0.0202 (8) | 0.0220 (8) | −0.0013 (6) | 0.0070 (6) | 0.0013 (6) |
C15 | 0.0197 (8) | 0.0204 (8) | 0.0204 (8) | −0.0005 (6) | 0.0071 (6) | −0.0006 (6) |
C16 | 0.0198 (8) | 0.0246 (8) | 0.0210 (8) | −0.0008 (6) | 0.0090 (6) | −0.0013 (6) |
C17 | 0.0166 (7) | 0.0225 (8) | 0.0204 (8) | 0.0006 (6) | 0.0082 (6) | 0.0006 (6) |
C18 | 0.0198 (8) | 0.0240 (8) | 0.0178 (7) | −0.0029 (6) | 0.0064 (6) | −0.0017 (6) |
C19 | 0.0228 (8) | 0.0276 (8) | 0.0203 (8) | −0.0028 (7) | 0.0093 (7) | −0.0050 (7) |
C20 | 0.0208 (8) | 0.0287 (9) | 0.0208 (8) | −0.0019 (7) | 0.0092 (7) | −0.0010 (7) |
C21 | 0.0216 (9) | 0.0377 (10) | 0.0244 (9) | −0.0078 (7) | 0.0090 (7) | −0.0073 (7) |
C22 | 0.0252 (9) | 0.0336 (9) | 0.0217 (8) | −0.0073 (7) | 0.0094 (7) | −0.0083 (7) |
C23 | 0.0186 (8) | 0.0238 (8) | 0.0232 (8) | −0.0009 (6) | 0.0061 (7) | −0.0016 (6) |
C24 | 0.0222 (8) | 0.0275 (8) | 0.0219 (8) | −0.0015 (7) | 0.0094 (7) | 0.0003 (7) |
O1 | 0.0249 (7) | 0.0382 (7) | 0.0238 (6) | 0.0111 (6) | 0.0091 (5) | 0.0075 (6) |
O2 | 0.0223 (6) | 0.0317 (7) | 0.0236 (6) | 0.0016 (5) | 0.0096 (5) | 0.0033 (5) |
O3 | 0.0227 (7) | 0.0685 (11) | 0.0357 (8) | 0.0135 (7) | 0.0163 (6) | 0.0170 (8) |
O4 | 0.0355 (8) | 0.0784 (12) | 0.0388 (9) | 0.0213 (8) | 0.0237 (7) | 0.0291 (9) |
O5 | 0.0231 (6) | 0.0363 (7) | 0.0268 (7) | −0.0101 (5) | 0.0105 (5) | −0.0099 (6) |
O6 | 0.0250 (7) | 0.0558 (9) | 0.0300 (7) | −0.0125 (6) | 0.0151 (6) | −0.0163 (7) |
O7 | 0.0203 (6) | 0.0384 (7) | 0.0271 (7) | −0.0053 (5) | 0.0117 (5) | −0.0072 (6) |
O8 | 0.0274 (7) | 0.0422 (8) | 0.0302 (7) | −0.0072 (6) | 0.0150 (6) | −0.0121 (6) |
O10A | 0.147 (4) | 0.072 (2) | 0.076 (2) | 0.035 (2) | 0.056 (3) | 0.0312 (17) |
O10B | 0.183 (12) | 0.046 (5) | 0.100 (7) | −0.016 (6) | −0.007 (7) | 0.016 (5) |
Cl2—Ru1 | 2.4299 (4) | C2—C3 | 1.399 (2) |
Cl1—Ru1 | 2.4123 (4) | C2—H2 | 0.9500 |
N1—Ru1 | 2.0063 (14) | C8—C7 | 1.389 (2) |
N2—Ru1 | 2.0426 (14) | C8—C9 | 1.393 (2) |
N3—Ru1 | 2.0295 (14) | C8—C12 | 1.495 (2) |
N4—Ru1 | 2.0419 (14) | C21—C22 | 1.378 (3) |
O1—C11 | 1.314 (2) | C21—C20 | 1.394 (2) |
O2—C11 | 1.216 (2) | C21—H21 | 0.9500 |
O3—C12 | 1.327 (2) | C14—C15 | 1.396 (2) |
O4—C12 | 1.194 (2) | C14—H14 | 0.9500 |
O5—C23 | 1.315 (2) | C16—C17 | 1.387 (2) |
O6—C23 | 1.209 (2) | C16—C15 | 1.391 (2) |
O7—C24 | 1.325 (2) | C16—H16 | 0.9500 |
O8—C24 | 1.207 (2) | C23—C15 | 1.495 (2) |
N4—C22 | 1.348 (2) | C10—C9 | 1.379 (2) |
N4—C18 | 1.363 (2) | C10—H10 | 0.9500 |
N3—C13 | 1.349 (2) | C1—H1 | 0.9500 |
N3—C17 | 1.367 (2) | C6—C7 | 1.387 (2) |
N2—C10 | 1.347 (2) | C6—C5 | 1.470 (2) |
N2—C6 | 1.364 (2) | C7—H7 | 0.9500 |
N1—C1 | 1.344 (2) | C17—C18 | 1.470 (2) |
N1—C5 | 1.366 (2) | C3—C4 | 1.391 (2) |
O7—H54 | 0.84 (3) | C18—C19 | 1.389 (2) |
O5—H53 | 0.85 (3) | C5—C4 | 1.389 (2) |
O3—H52 | 0.87 (3) | C24—C20 | 1.493 (2) |
O1—H51 | 0.89 (3) | C22—H22 | 0.9500 |
C13—C14 | 1.381 (2) | C4—H4 | 0.9500 |
C13—H13 | 0.9500 | C19—C20 | 1.387 (2) |
C11—C3 | 1.488 (2) | C19—H19 | 0.9500 |
C2—C1 | 1.374 (2) | C9—H9 | 0.9500 |
C22—N4—C18 | 118.64 (15) | N3—C17—C16 | 121.70 (15) |
C22—N4—Ru1 | 125.48 (12) | N3—C17—C18 | 114.33 (14) |
C18—N4—Ru1 | 115.80 (11) | C16—C17—C18 | 123.96 (14) |
C13—N3—C17 | 118.44 (14) | C16—C15—C14 | 118.75 (15) |
C13—N3—Ru1 | 125.72 (11) | C16—C15—C23 | 119.65 (15) |
C17—N3—Ru1 | 115.56 (11) | C14—C15—C23 | 121.60 (15) |
C10—N2—C6 | 118.82 (14) | C4—C3—C2 | 119.02 (15) |
C10—N2—Ru1 | 126.06 (12) | C4—C3—C11 | 121.23 (15) |
C6—N2—Ru1 | 115.09 (11) | C2—C3—C11 | 119.73 (15) |
C1—N1—C5 | 119.23 (14) | O4—C12—O3 | 123.94 (18) |
C1—N1—Ru1 | 124.39 (11) | O4—C12—C8 | 122.97 (17) |
C5—N1—Ru1 | 115.93 (11) | O3—C12—C8 | 113.08 (16) |
C24—O7—H54 | 111.0 (17) | N4—C18—C19 | 121.84 (15) |
C23—O5—H53 | 109.1 (16) | N4—C18—C17 | 114.11 (14) |
C12—O3—H52 | 109.8 (18) | C19—C18—C17 | 123.96 (15) |
C11—O1—H51 | 111.2 (17) | N1—C5—C4 | 120.86 (15) |
N3—C13—C14 | 122.44 (15) | N1—C5—C6 | 114.19 (14) |
N3—C13—H13 | 118.8 | C4—C5—C6 | 124.93 (14) |
C14—C13—H13 | 118.8 | O8—C24—O7 | 124.54 (16) |
O2—C11—O1 | 123.86 (16) | O8—C24—C20 | 123.22 (16) |
O2—C11—C3 | 124.10 (16) | O7—C24—C20 | 112.23 (15) |
O1—C11—C3 | 112.03 (15) | N4—C22—C21 | 122.22 (16) |
C1—C2—C3 | 118.79 (16) | N4—C22—H22 | 118.9 |
C1—C2—H2 | 120.6 | C21—C22—H22 | 118.9 |
C3—C2—H2 | 120.6 | C5—C4—C3 | 119.44 (15) |
C7—C8—C9 | 119.16 (16) | C5—C4—H4 | 120.3 |
C7—C8—C12 | 118.86 (15) | C3—C4—H4 | 120.3 |
C9—C8—C12 | 121.98 (16) | C20—C19—C18 | 118.99 (15) |
C22—C21—C20 | 119.31 (17) | C20—C19—H19 | 120.5 |
C22—C21—H21 | 120.3 | C18—C19—H19 | 120.5 |
C20—C21—H21 | 120.3 | C10—C9—C8 | 119.24 (16) |
C13—C14—C15 | 119.19 (15) | C10—C9—H9 | 120.4 |
C13—C14—H14 | 120.4 | C8—C9—H9 | 120.4 |
C15—C14—H14 | 120.4 | C19—C20—C21 | 118.99 (16) |
C17—C16—C15 | 119.29 (15) | C19—C20—C24 | 119.29 (15) |
C17—C16—H16 | 120.4 | C21—C20—C24 | 121.72 (16) |
C15—C16—H16 | 120.4 | N1—Ru1—N3 | 95.44 (6) |
O6—C23—O5 | 123.49 (17) | N1—Ru1—N4 | 95.60 (6) |
O6—C23—C15 | 123.61 (16) | N3—Ru1—N4 | 79.16 (6) |
O5—C23—C15 | 112.88 (15) | N1—Ru1—N2 | 79.37 (6) |
N2—C10—C9 | 122.10 (16) | N3—Ru1—N2 | 97.77 (5) |
N2—C10—H10 | 118.9 | N4—Ru1—N2 | 173.90 (6) |
C9—C10—H10 | 118.9 | N1—Ru1—Cl1 | 173.21 (4) |
N1—C1—C2 | 122.63 (16) | N3—Ru1—Cl1 | 90.05 (4) |
N1—C1—H1 | 118.7 | N4—Ru1—Cl1 | 89.33 (4) |
C2—C1—H1 | 118.7 | N2—Ru1—Cl1 | 95.97 (4) |
N2—C6—C7 | 121.76 (15) | N1—Ru1—Cl2 | 88.43 (4) |
N2—C6—C5 | 114.02 (14) | N3—Ru1—Cl2 | 174.04 (4) |
C7—C6—C5 | 124.17 (15) | N4—Ru1—Cl2 | 95.98 (4) |
C6—C7—C8 | 118.87 (15) | N2—Ru1—Cl2 | 87.39 (4) |
C6—C7—H7 | 120.6 | Cl1—Ru1—Cl2 | 86.420 (16) |
C8—C7—H7 | 120.6 | ||
C17—N3—C13—C14 | −3.3 (2) | N2—C6—C5—C4 | 179.42 (15) |
Ru1—N3—C13—C14 | 170.29 (12) | C7—C6—C5—C4 | −3.0 (3) |
N3—C13—C14—C15 | −0.6 (3) | C18—N4—C22—C21 | −0.1 (3) |
C6—N2—C10—C9 | 1.1 (2) | Ru1—N4—C22—C21 | 176.43 (15) |
Ru1—N2—C10—C9 | −176.67 (13) | C20—C21—C22—N4 | 1.0 (3) |
C5—N1—C1—C2 | −1.4 (3) | N1—C5—C4—C3 | −0.2 (2) |
Ru1—N1—C1—C2 | 170.63 (14) | C6—C5—C4—C3 | 178.14 (15) |
C3—C2—C1—N1 | 0.1 (3) | C2—C3—C4—C5 | −1.1 (3) |
C10—N2—C6—C7 | −2.4 (2) | C11—C3—C4—C5 | 177.75 (15) |
Ru1—N2—C6—C7 | 175.58 (12) | N4—C18—C19—C20 | 0.7 (3) |
C10—N2—C6—C5 | 175.25 (14) | C17—C18—C19—C20 | −175.70 (16) |
Ru1—N2—C6—C5 | −6.78 (17) | N2—C10—C9—C8 | 0.7 (3) |
N2—C6—C7—C8 | 1.9 (2) | C7—C8—C9—C10 | −1.2 (3) |
C5—C6—C7—C8 | −175.50 (15) | C12—C8—C9—C10 | 178.99 (16) |
C9—C8—C7—C6 | −0.1 (2) | C18—C19—C20—C21 | 0.2 (3) |
C12—C8—C7—C6 | 179.75 (15) | C18—C19—C20—C24 | −178.99 (16) |
C13—N3—C17—C16 | 4.3 (2) | C22—C21—C20—C19 | −1.0 (3) |
Ru1—N3—C17—C16 | −169.91 (13) | C22—C21—C20—C24 | 178.18 (18) |
C13—N3—C17—C18 | −174.45 (14) | O8—C24—C20—C19 | 0.3 (3) |
Ru1—N3—C17—C18 | 11.32 (18) | O7—C24—C20—C19 | 179.19 (16) |
C15—C16—C17—N3 | −1.4 (3) | O8—C24—C20—C21 | −178.88 (18) |
C15—C16—C17—C18 | 177.20 (16) | O7—C24—C20—C21 | 0.0 (2) |
C17—C16—C15—C14 | −2.5 (2) | C1—N1—Ru1—N3 | 80.10 (14) |
C17—C16—C15—C23 | 176.48 (15) | C5—N1—Ru1—N3 | −107.65 (12) |
C13—C14—C15—C16 | 3.5 (2) | C1—N1—Ru1—N4 | 0.50 (15) |
C13—C14—C15—C23 | −175.47 (15) | C5—N1—Ru1—N4 | 172.75 (12) |
O6—C23—C15—C16 | −2.0 (3) | C1—N1—Ru1—N2 | 177.01 (15) |
O5—C23—C15—C16 | 179.51 (16) | C5—N1—Ru1—N2 | −10.74 (11) |
O6—C23—C15—C14 | 176.89 (18) | C1—N1—Ru1—Cl2 | −95.35 (14) |
O5—C23—C15—C14 | −1.6 (2) | C5—N1—Ru1—Cl2 | 76.90 (11) |
C1—C2—C3—C4 | 1.2 (3) | C13—N3—Ru1—N1 | 82.42 (14) |
C1—C2—C3—C11 | −177.67 (16) | C17—N3—Ru1—N1 | −103.82 (12) |
O2—C11—C3—C4 | −3.5 (3) | C13—N3—Ru1—N4 | 177.10 (14) |
O1—C11—C3—C4 | 177.37 (16) | C17—N3—Ru1—N4 | −9.14 (11) |
O2—C11—C3—C2 | 175.29 (17) | C13—N3—Ru1—N2 | 2.44 (14) |
O1—C11—C3—C2 | −3.8 (2) | C17—N3—Ru1—N2 | 176.20 (11) |
C7—C8—C12—O4 | 0.6 (3) | C13—N3—Ru1—Cl1 | −93.59 (13) |
C9—C8—C12—O4 | −179.6 (2) | C17—N3—Ru1—Cl1 | 80.16 (11) |
C7—C8—C12—O3 | 179.37 (16) | C22—N4—Ru1—N1 | −76.85 (15) |
C9—C8—C12—O3 | −0.8 (2) | C18—N4—Ru1—N1 | 99.78 (12) |
C22—N4—C18—C19 | −0.7 (3) | C22—N4—Ru1—N3 | −171.34 (16) |
Ru1—N4—C18—C19 | −177.60 (13) | C18—N4—Ru1—N3 | 5.29 (12) |
C22—N4—C18—C17 | 175.97 (15) | C22—N4—Ru1—Cl1 | 98.48 (15) |
Ru1—N4—C18—C17 | −0.90 (19) | C18—N4—Ru1—Cl1 | −84.89 (12) |
N3—C17—C18—N4 | −6.8 (2) | C22—N4—Ru1—Cl2 | 12.15 (15) |
C16—C17—C18—N4 | 174.50 (16) | C18—N4—Ru1—Cl2 | −171.22 (11) |
N3—C17—C18—C19 | 169.85 (16) | C10—N2—Ru1—N1 | −172.74 (14) |
C16—C17—C18—C19 | −8.9 (3) | C6—N2—Ru1—N1 | 9.47 (11) |
C1—N1—C5—C4 | 1.5 (2) | C10—N2—Ru1—N3 | −78.62 (14) |
Ru1—N1—C5—C4 | −171.22 (12) | C6—N2—Ru1—N3 | 103.59 (11) |
C1—N1—C5—C6 | −177.08 (15) | C10—N2—Ru1—Cl1 | 12.25 (14) |
Ru1—N1—C5—C6 | 10.24 (18) | C6—N2—Ru1—Cl1 | −165.54 (11) |
N2—C6—C5—N1 | −2.1 (2) | C10—N2—Ru1—Cl2 | 98.38 (13) |
C7—C6—C5—N1 | 175.47 (15) | C6—N2—Ru1—Cl2 | −79.42 (11) |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H52···O6i | 0.87 (3) | 1.80 (3) | 2.6634 (19) | 174 (3) |
O1—H51···Cl1ii | 0.89 (3) | 2.06 (3) | 2.9355 (14) | 168 (2) |
O7—H54···O2iii | 0.84 (3) | 1.83 (3) | 2.6564 (18) | 168 (3) |
O5—H53···Cl2iv | 0.85 (3) | 2.22 (3) | 3.0404 (14) | 164 (2) |
Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) x−1/2, −y+1/2, z−1/2. |