Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113017605/wq3041sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113017605/wq3041Isup2.hkl |
CCDC reference: 962896
Data collection: APEX2 (Bruker, 2013); cell refinement: SAINT-Plus (Bruker, 2013); data reduction: SAINT-Plus (Bruker, 2013); program(s) used to solve structure: SHELXTL (Sheldrick, 2013); program(s) used to refine structure: SHELXTL (Sheldrick, 2013); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).
[Ru(C10H14)(C9H9N3)(PO2F2)](PF6)0.86(BF4)0.14 | F(000) = 1264 |
Mr = 631.92 | Dx = 1.823 Mg m−3 |
Monoclinic, P21/n | Cu Kα radiation, λ = 1.54178 Å |
a = 15.6531 (17) Å | Cell parameters from 9902 reflections |
b = 8.7619 (9) Å | θ = 4.5–71.7° |
c = 17.4895 (18) Å | µ = 7.54 mm−1 |
β = 106.316 (5)° | T = 100 K |
V = 2302.1 (4) Å3 | Slab, orange |
Z = 4 | 0.16 × 0.10 × 0.06 mm |
Bruker SMART APEXII area-detector diffractometer | 4479 independent reflections |
Radiation source: sealed X-ray tube, Siemens, K FFCU 2K 90 | 4065 reflections with I > 2σ(I) |
Equatorially mounted graphite monochromator | Rint = 0.039 |
Detector resolution: 7.9 pixels mm-1 | θmax = 72.3°, θmin = 3.4° |
0.60° ω and 0.6° ϕ scans | h = −19→18 |
Absorption correction: analytical (SADABS; Bruker, 2012) | k = −10→10 |
Tmin = 0.429, Tmax = 0.735 | l = −19→21 |
32407 measured reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.024 | H-atom parameters constrained |
wR(F2) = 0.057 | w = 1/[σ2(Fo2) + (0.0261P)2 + 2.5316P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.002 |
4479 reflections | Δρmax = 0.47 e Å−3 |
327 parameters | Δρmin = −0.33 e Å−3 |
[Ru(C10H14)(C9H9N3)(PO2F2)](PF6)0.86(BF4)0.14 | V = 2302.1 (4) Å3 |
Mr = 631.92 | Z = 4 |
Monoclinic, P21/n | Cu Kα radiation |
a = 15.6531 (17) Å | µ = 7.54 mm−1 |
b = 8.7619 (9) Å | T = 100 K |
c = 17.4895 (18) Å | 0.16 × 0.10 × 0.06 mm |
β = 106.316 (5)° |
Bruker SMART APEXII area-detector diffractometer | 4479 independent reflections |
Absorption correction: analytical (SADABS; Bruker, 2012) | 4065 reflections with I > 2σ(I) |
Tmin = 0.429, Tmax = 0.735 | Rint = 0.039 |
32407 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.057 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.47 e Å−3 |
4479 reflections | Δρmin = −0.33 e Å−3 |
327 parameters |
Experimental. Absorption correction: SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0580 before and 0.0481 after correction. The Ratio of minimum to maximum transmission is 0.5840. The λ/2 correction factor is 0.0015. |
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 | Occ. (<1) | |
Ru1 | 0.55217 (2) | 0.90161 (2) | 0.27953 (2) | 0.01267 (6) | |
P1 | 0.48184 (4) | 1.25979 (7) | 0.24813 (4) | 0.02103 (13) | |
F1 | 0.40442 (12) | 1.22266 (19) | 0.17430 (10) | 0.0436 (4) | |
F2A | 0.44888 (11) | 1.38720 (17) | 0.28842 (10) | 0.0287 (4) | 0.5 |
O2B | 0.44888 (11) | 1.38720 (17) | 0.28842 (10) | 0.0287 (4) | 0.5 |
F2B | 0.55436 (12) | 1.31092 (19) | 0.21382 (11) | 0.0350 (4) | 0.5 |
O2A | 0.55436 (12) | 1.31092 (19) | 0.21382 (11) | 0.0350 (4) | 0.5 |
O1 | 0.50252 (11) | 1.11911 (17) | 0.29711 (10) | 0.0185 (3) | |
N1 | 0.57552 (12) | 0.8956 (2) | 0.40467 (11) | 0.0145 (4) | |
N2 | 0.40768 (13) | 0.7363 (2) | 0.33223 (11) | 0.0193 (4) | |
N3 | 0.42432 (12) | 0.8334 (2) | 0.27798 (11) | 0.0165 (4) | |
C1 | 0.62923 (15) | 1.0027 (3) | 0.44785 (14) | 0.0192 (5) | |
H1 | 0.6527 | 1.0788 | 0.4207 | 0.023* | |
C2 | 0.65186 (16) | 1.0071 (3) | 0.52975 (15) | 0.0247 (5) | |
H2 | 0.6925 | 1.0814 | 0.5586 | 0.030* | |
C3 | 0.61440 (16) | 0.9018 (3) | 0.56913 (15) | 0.0254 (5) | |
H3 | 0.6282 | 0.9031 | 0.6256 | 0.031* | |
C4 | 0.55660 (16) | 0.7943 (3) | 0.52536 (14) | 0.0217 (5) | |
H4 | 0.5288 | 0.7226 | 0.5514 | 0.026* | |
C5 | 0.53934 (14) | 0.7917 (3) | 0.44333 (13) | 0.0167 (4) | |
C6 | 0.48156 (16) | 0.6703 (3) | 0.39366 (14) | 0.0211 (5) | |
H6A | 0.5180 | 0.6064 | 0.3682 | 0.025* | |
H6B | 0.4578 | 0.6036 | 0.4285 | 0.025* | |
C7 | 0.34528 (15) | 0.8783 (3) | 0.23143 (14) | 0.0217 (5) | |
H7 | 0.3366 | 0.9468 | 0.1878 | 0.026* | |
C8 | 0.27713 (17) | 0.8096 (3) | 0.25642 (16) | 0.0296 (6) | |
H8 | 0.2148 | 0.8222 | 0.2340 | 0.036* | |
C9 | 0.31937 (16) | 0.7198 (3) | 0.32029 (15) | 0.0266 (5) | |
H9 | 0.2913 | 0.6573 | 0.3505 | 0.032* | |
C10 | 0.58083 (16) | 0.6985 (3) | 0.22017 (14) | 0.0215 (5) | |
H10 | 0.5559 | 0.5994 | 0.2192 | 0.026* | |
C11 | 0.65646 (16) | 0.7385 (3) | 0.28218 (14) | 0.0224 (5) | |
H11 | 0.6818 | 0.6654 | 0.3223 | 0.027* | |
C12 | 0.69611 (15) | 0.8863 (3) | 0.28628 (14) | 0.0230 (5) | |
C13 | 0.65426 (15) | 0.9930 (3) | 0.22829 (14) | 0.0209 (5) | |
H13 | 0.6773 | 1.0937 | 0.2309 | 0.025* | |
C14 | 0.57733 (15) | 0.9527 (3) | 0.16514 (13) | 0.0182 (5) | |
H14 | 0.5502 | 1.0276 | 0.1267 | 0.022* | |
C15 | 0.54095 (15) | 0.8053 (3) | 0.15862 (13) | 0.0183 (5) | |
C16 | 0.77689 (16) | 0.9271 (4) | 0.35332 (16) | 0.0344 (7) | |
H16A | 0.7768 | 1.0369 | 0.3638 | 0.052* | |
H16B | 0.8308 | 0.9001 | 0.3384 | 0.052* | |
H16C | 0.7756 | 0.8707 | 0.4014 | 0.052* | |
C17 | 0.46174 (17) | 0.7656 (3) | 0.08834 (14) | 0.0241 (5) | |
H17 | 0.4201 | 0.8547 | 0.0778 | 0.029* | |
C18 | 0.4099 (2) | 0.6252 (3) | 0.10075 (16) | 0.0333 (6) | |
H18A | 0.4471 | 0.5342 | 0.1036 | 0.050* | |
H18B | 0.3560 | 0.6152 | 0.0561 | 0.050* | |
H18C | 0.3934 | 0.6360 | 0.1505 | 0.050* | |
C19 | 0.49747 (19) | 0.7442 (3) | 0.01539 (15) | 0.0315 (6) | |
H19A | 0.5307 | 0.8354 | 0.0084 | 0.047* | |
H19B | 0.4475 | 0.7284 | −0.0323 | 0.047* | |
H19C | 0.5369 | 0.6551 | 0.0237 | 0.047* | |
P2 | 0.73404 (5) | 0.43580 (8) | 0.46735 (4) | 0.0192 (2) | 0.854 (3) |
F3 | 0.77516 (16) | 0.4669 (3) | 0.56018 (11) | 0.0372 (6) | 0.854 (3) |
F4 | 0.64455 (13) | 0.3736 (3) | 0.48429 (13) | 0.0471 (6) | 0.854 (3) |
F5 | 0.77414 (14) | 0.2683 (2) | 0.47753 (16) | 0.0464 (6) | 0.854 (3) |
F6 | 0.82175 (13) | 0.5013 (2) | 0.45011 (12) | 0.0390 (5) | 0.854 (3) |
F7 | 0.69530 (15) | 0.6044 (2) | 0.45747 (13) | 0.0444 (6) | 0.854 (3) |
F8 | 0.69105 (15) | 0.4060 (3) | 0.37410 (12) | 0.0475 (6) | 0.854 (3) |
F9 | 0.7598 (11) | 0.5712 (15) | 0.4432 (10) | 0.085 (4)* | 0.146 (3) |
F11 | 0.6396 (9) | 0.443 (2) | 0.4615 (12) | 0.085 (4)* | 0.146 (3) |
F12 | 0.7521 (11) | 0.3111 (16) | 0.4312 (11) | 0.085 (4)* | 0.146 (3) |
F10 | 0.7755 (14) | 0.422 (2) | 0.5539 (8) | 0.085 (4)* | 0.146 (3) |
B1 | 0.7317 (8) | 0.4369 (13) | 0.4725 (7) | 0.085 (4)* | 0.146 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.01457 (9) | 0.01302 (9) | 0.01117 (9) | 0.00064 (6) | 0.00483 (6) | 0.00039 (6) |
P1 | 0.0220 (3) | 0.0138 (3) | 0.0249 (3) | 0.0008 (2) | 0.0029 (2) | 0.0009 (2) |
F1 | 0.0535 (11) | 0.0359 (9) | 0.0280 (9) | −0.0111 (8) | −0.0103 (7) | 0.0029 (7) |
F2A | 0.0342 (9) | 0.0191 (8) | 0.0331 (9) | 0.0040 (7) | 0.0098 (7) | −0.0038 (7) |
O2B | 0.0342 (9) | 0.0191 (8) | 0.0331 (9) | 0.0040 (7) | 0.0098 (7) | −0.0038 (7) |
F2B | 0.0377 (10) | 0.0280 (9) | 0.0470 (11) | 0.0002 (7) | 0.0247 (8) | 0.0064 (8) |
O2A | 0.0377 (10) | 0.0280 (9) | 0.0470 (11) | 0.0002 (7) | 0.0247 (8) | 0.0064 (8) |
O1 | 0.0242 (8) | 0.0138 (7) | 0.0210 (9) | 0.0011 (6) | 0.0119 (7) | −0.0001 (6) |
N1 | 0.0152 (9) | 0.0169 (9) | 0.0121 (9) | 0.0028 (7) | 0.0052 (7) | −0.0002 (7) |
N2 | 0.0231 (10) | 0.0198 (10) | 0.0155 (10) | −0.0075 (8) | 0.0062 (8) | 0.0002 (8) |
N3 | 0.0190 (9) | 0.0166 (9) | 0.0149 (10) | −0.0034 (7) | 0.0064 (7) | −0.0005 (7) |
C1 | 0.0162 (11) | 0.0225 (11) | 0.0189 (12) | 0.0006 (9) | 0.0052 (9) | −0.0034 (9) |
C2 | 0.0222 (12) | 0.0308 (13) | 0.0198 (13) | 0.0012 (10) | 0.0040 (9) | −0.0058 (10) |
C3 | 0.0260 (12) | 0.0333 (14) | 0.0166 (12) | 0.0080 (11) | 0.0053 (9) | −0.0019 (10) |
C4 | 0.0227 (12) | 0.0253 (12) | 0.0188 (12) | 0.0062 (10) | 0.0086 (9) | 0.0045 (10) |
C5 | 0.0174 (11) | 0.0178 (11) | 0.0156 (11) | 0.0041 (9) | 0.0057 (9) | 0.0015 (9) |
C6 | 0.0299 (13) | 0.0164 (11) | 0.0175 (12) | −0.0014 (9) | 0.0075 (10) | 0.0037 (9) |
C7 | 0.0198 (11) | 0.0245 (12) | 0.0190 (12) | −0.0031 (9) | 0.0026 (9) | −0.0019 (9) |
C8 | 0.0201 (12) | 0.0412 (15) | 0.0266 (14) | −0.0095 (11) | 0.0050 (10) | −0.0063 (11) |
C9 | 0.0254 (13) | 0.0336 (14) | 0.0228 (13) | −0.0149 (11) | 0.0099 (10) | −0.0063 (11) |
C10 | 0.0327 (13) | 0.0169 (11) | 0.0175 (12) | 0.0062 (10) | 0.0114 (10) | −0.0008 (9) |
C11 | 0.0247 (12) | 0.0274 (12) | 0.0169 (12) | 0.0150 (10) | 0.0089 (9) | 0.0036 (9) |
C12 | 0.0169 (11) | 0.0367 (14) | 0.0193 (12) | 0.0050 (10) | 0.0111 (9) | −0.0007 (10) |
C13 | 0.0206 (11) | 0.0267 (12) | 0.0204 (12) | −0.0029 (9) | 0.0141 (9) | −0.0016 (9) |
C14 | 0.0237 (11) | 0.0199 (11) | 0.0142 (11) | 0.0029 (9) | 0.0106 (9) | 0.0031 (9) |
C15 | 0.0239 (12) | 0.0206 (11) | 0.0124 (11) | 0.0047 (9) | 0.0084 (9) | −0.0018 (9) |
C16 | 0.0162 (12) | 0.0614 (19) | 0.0259 (14) | 0.0022 (12) | 0.0063 (10) | −0.0045 (13) |
C17 | 0.0285 (13) | 0.0256 (12) | 0.0167 (12) | 0.0037 (10) | 0.0037 (10) | −0.0015 (9) |
C18 | 0.0403 (15) | 0.0352 (15) | 0.0226 (14) | −0.0099 (12) | 0.0058 (11) | −0.0086 (11) |
C19 | 0.0399 (15) | 0.0375 (15) | 0.0161 (13) | −0.0036 (12) | 0.0059 (11) | −0.0042 (11) |
P2 | 0.0174 (4) | 0.0221 (4) | 0.0177 (4) | −0.0016 (3) | 0.0044 (3) | 0.0038 (3) |
F3 | 0.0456 (11) | 0.0441 (13) | 0.0164 (10) | −0.0177 (10) | −0.0004 (8) | 0.0066 (8) |
F4 | 0.0286 (10) | 0.0758 (17) | 0.0405 (13) | −0.0239 (10) | 0.0153 (9) | −0.0016 (11) |
F5 | 0.0417 (12) | 0.0219 (10) | 0.0706 (16) | −0.0021 (8) | 0.0077 (11) | 0.0020 (10) |
F6 | 0.0395 (11) | 0.0390 (11) | 0.0487 (13) | −0.0150 (9) | 0.0290 (9) | −0.0114 (9) |
F7 | 0.0558 (13) | 0.0350 (11) | 0.0429 (12) | 0.0200 (10) | 0.0151 (10) | 0.0073 (9) |
F8 | 0.0582 (14) | 0.0574 (14) | 0.0238 (11) | −0.0168 (11) | 0.0066 (9) | −0.0050 (9) |
Ru1—O1 | 2.1130 (15) | C10—H10 | 0.9500 |
Ru1—N1 | 2.1160 (18) | C10—C11 | 1.407 (3) |
Ru1—N3 | 2.0815 (18) | C10—C15 | 1.430 (3) |
Ru1—C10 | 2.169 (2) | C11—H11 | 0.9500 |
Ru1—C11 | 2.161 (2) | C11—C12 | 1.430 (4) |
Ru1—C12 | 2.227 (2) | C12—C13 | 1.399 (3) |
Ru1—C13 | 2.191 (2) | C12—C16 | 1.506 (3) |
Ru1—C14 | 2.191 (2) | C13—H13 | 0.9500 |
Ru1—C15 | 2.237 (2) | C13—C14 | 1.431 (3) |
P1—F1 | 1.5371 (17) | C14—H14 | 0.9500 |
P1—F2A | 1.4877 (16) | C14—C15 | 1.403 (3) |
P1—F2B | 1.4940 (17) | C15—C17 | 1.521 (3) |
P1—O1 | 1.4840 (16) | C16—H16A | 0.9800 |
N1—C1 | 1.342 (3) | C16—H16B | 0.9800 |
N1—C5 | 1.350 (3) | C16—H16C | 0.9800 |
N2—N3 | 1.353 (3) | C17—H17 | 1.0000 |
N2—C6 | 1.459 (3) | C17—C18 | 1.522 (4) |
N2—C9 | 1.347 (3) | C17—C19 | 1.542 (3) |
N3—C7 | 1.335 (3) | C18—H18A | 0.9800 |
C1—H1 | 0.9500 | C18—H18B | 0.9800 |
C1—C2 | 1.376 (3) | C18—H18C | 0.9800 |
C2—H2 | 0.9500 | C19—H19A | 0.9800 |
C2—C3 | 1.377 (4) | C19—H19B | 0.9800 |
C3—H3 | 0.9500 | C19—H19C | 0.9800 |
C3—C4 | 1.379 (4) | P2—F3 | 1.5930 (19) |
C4—H4 | 0.9500 | P2—F4 | 1.6064 (19) |
C4—C5 | 1.383 (3) | P2—F5 | 1.587 (2) |
C5—C6 | 1.504 (3) | P2—F6 | 1.5931 (18) |
C6—H6A | 0.9900 | P2—F7 | 1.5875 (19) |
C6—H6B | 0.9900 | P2—F8 | 1.601 (2) |
C7—H7 | 0.9500 | F9—B1 | 1.4030 |
C7—C8 | 1.398 (3) | F11—B1 | 1.4016 |
C8—H8 | 0.9500 | F12—B1 | 1.4027 |
C8—C9 | 1.374 (4) | F10—B1 | 1.4017 |
C9—H9 | 0.9500 | ||
O1—Ru1—N1 | 80.54 (6) | Ru1—C10—H10 | 128.3 |
O1—Ru1—C10 | 160.62 (8) | C11—C10—Ru1 | 70.70 (13) |
O1—Ru1—C11 | 154.19 (8) | C11—C10—H10 | 119.6 |
O1—Ru1—C12 | 117.04 (8) | C11—C10—C15 | 120.8 (2) |
O1—Ru1—C13 | 94.04 (8) | C15—C10—Ru1 | 73.66 (13) |
O1—Ru1—C14 | 96.69 (7) | C15—C10—H10 | 119.6 |
O1—Ru1—C15 | 122.92 (7) | Ru1—C11—H11 | 128.1 |
N1—Ru1—C10 | 118.41 (8) | C10—C11—Ru1 | 71.39 (13) |
N1—Ru1—C11 | 92.95 (8) | C10—C11—H11 | 119.2 |
N1—Ru1—C12 | 93.76 (8) | C10—C11—C12 | 121.6 (2) |
N1—Ru1—C13 | 119.88 (8) | C12—C11—Ru1 | 73.51 (13) |
N1—Ru1—C14 | 157.89 (8) | C12—C11—H11 | 119.2 |
N1—Ru1—C15 | 155.93 (8) | C11—C12—Ru1 | 68.49 (13) |
N3—Ru1—O1 | 82.48 (7) | C11—C12—C16 | 120.8 (2) |
N3—Ru1—N1 | 83.82 (7) | C13—C12—Ru1 | 70.17 (13) |
N3—Ru1—C10 | 94.91 (8) | C13—C12—C11 | 117.4 (2) |
N3—Ru1—C11 | 121.88 (9) | C13—C12—C16 | 121.7 (2) |
N3—Ru1—C12 | 159.75 (9) | C16—C12—Ru1 | 130.00 (16) |
N3—Ru1—C13 | 155.30 (8) | Ru1—C13—H13 | 129.1 |
N3—Ru1—C14 | 117.75 (8) | C12—C13—Ru1 | 72.92 (13) |
N3—Ru1—C15 | 93.41 (8) | C12—C13—H13 | 119.5 |
C10—Ru1—C12 | 68.52 (9) | C12—C13—C14 | 121.1 (2) |
C10—Ru1—C13 | 80.29 (9) | C14—C13—Ru1 | 70.93 (12) |
C10—Ru1—C14 | 67.44 (9) | C14—C13—H13 | 119.5 |
C10—Ru1—C15 | 37.84 (8) | Ru1—C14—H14 | 128.9 |
C11—Ru1—C10 | 37.91 (9) | C13—C14—Ru1 | 70.96 (12) |
C11—Ru1—C12 | 38.00 (10) | C13—C14—H14 | 119.2 |
C11—Ru1—C13 | 67.48 (9) | C15—C14—Ru1 | 73.33 (13) |
C11—Ru1—C14 | 79.99 (9) | C15—C14—C13 | 121.6 (2) |
C11—Ru1—C15 | 68.21 (9) | C15—C14—H14 | 119.2 |
C12—Ru1—C15 | 80.62 (9) | C10—C15—Ru1 | 68.51 (12) |
C13—Ru1—C12 | 36.91 (9) | C10—C15—C17 | 122.9 (2) |
C13—Ru1—C15 | 67.91 (9) | C14—C15—Ru1 | 69.73 (12) |
C14—Ru1—C12 | 67.79 (9) | C14—C15—C10 | 117.3 (2) |
C14—Ru1—C13 | 38.11 (9) | C14—C15—C17 | 119.7 (2) |
C14—Ru1—C15 | 36.93 (8) | C17—C15—Ru1 | 132.83 (16) |
F2A—P1—F1 | 105.08 (10) | C12—C16—H16A | 109.5 |
F2B—P1—F1 | 103.58 (11) | C12—C16—H16B | 109.5 |
O1—P1—F1 | 107.56 (10) | C12—C16—H16C | 109.5 |
O1—P1—F2A | 113.47 (10) | H16A—C16—H16B | 109.5 |
O1—P1—F2B | 114.44 (10) | H16A—C16—H16C | 109.5 |
P1—O1—Ru1 | 134.00 (10) | H16B—C16—H16C | 109.5 |
C1—N1—Ru1 | 117.61 (15) | C15—C17—H17 | 108.2 |
C1—N1—C5 | 118.34 (19) | C15—C17—C18 | 114.5 (2) |
C5—N1—Ru1 | 124.06 (15) | C15—C17—C19 | 107.1 (2) |
N3—N2—C6 | 119.81 (18) | C18—C17—H17 | 108.2 |
C9—N2—N3 | 110.5 (2) | C18—C17—C19 | 110.6 (2) |
C9—N2—C6 | 129.6 (2) | C19—C17—H17 | 108.2 |
N2—N3—Ru1 | 123.04 (14) | C17—C18—H18A | 109.5 |
C7—N3—Ru1 | 130.26 (16) | C17—C18—H18B | 109.5 |
C7—N3—N2 | 106.55 (18) | C17—C18—H18C | 109.5 |
N1—C1—H1 | 118.6 | H18A—C18—H18B | 109.5 |
N1—C1—C2 | 122.9 (2) | H18A—C18—H18C | 109.5 |
C2—C1—H1 | 118.6 | H18B—C18—H18C | 109.5 |
C1—C2—H2 | 120.6 | C17—C19—H19A | 109.5 |
C1—C2—C3 | 118.7 (2) | C17—C19—H19B | 109.5 |
C3—C2—H2 | 120.6 | C17—C19—H19C | 109.5 |
C2—C3—H3 | 120.5 | H19A—C19—H19B | 109.5 |
C2—C3—C4 | 119.0 (2) | H19A—C19—H19C | 109.5 |
C4—C3—H3 | 120.5 | H19B—C19—H19C | 109.5 |
C3—C4—H4 | 120.2 | F3—P2—F4 | 89.64 (11) |
C3—C4—C5 | 119.6 (2) | F3—P2—F6 | 90.47 (12) |
C5—C4—H4 | 120.2 | F3—P2—F8 | 178.95 (14) |
N1—C5—C4 | 121.4 (2) | F5—P2—F3 | 90.58 (13) |
N1—C5—C6 | 117.16 (19) | F5—P2—F4 | 90.19 (13) |
C4—C5—C6 | 121.4 (2) | F5—P2—F6 | 91.13 (11) |
N2—C6—C5 | 111.60 (18) | F5—P2—F7 | 179.19 (12) |
N2—C6—H6A | 109.3 | F5—P2—F8 | 90.18 (13) |
N2—C6—H6B | 109.3 | F6—P2—F4 | 178.68 (13) |
C5—C6—H6A | 109.3 | F6—P2—F8 | 90.23 (11) |
C5—C6—H6B | 109.3 | F7—P2—F3 | 89.10 (12) |
H6A—C6—H6B | 108.0 | F7—P2—F4 | 90.55 (13) |
N3—C7—H7 | 125.0 | F7—P2—F6 | 88.13 (12) |
N3—C7—C8 | 109.9 (2) | F7—P2—F8 | 90.14 (12) |
C8—C7—H7 | 125.0 | F8—P2—F4 | 89.65 (12) |
C7—C8—H8 | 127.3 | F11—B1—F9 | 109.5 |
C9—C8—C7 | 105.4 (2) | F11—B1—F12 | 109.5 |
C9—C8—H8 | 127.3 | F11—B1—F10 | 109.5 |
N2—C9—C8 | 107.6 (2) | F12—B1—F9 | 109.4 |
N2—C9—H9 | 126.2 | F10—B1—F9 | 109.5 |
C8—C9—H9 | 126.2 | F10—B1—F12 | 109.6 |
Ru1—N1—C1—C2 | −177.60 (18) | C4—C5—C6—N2 | 124.4 (2) |
Ru1—N1—C5—C4 | −179.49 (16) | C5—N1—C1—C2 | 2.8 (3) |
Ru1—N1—C5—C6 | 2.2 (3) | C6—N2—N3—Ru1 | −2.3 (3) |
Ru1—N3—C7—C8 | −175.32 (17) | C6—N2—N3—C7 | −178.3 (2) |
Ru1—C10—C11—C12 | −56.06 (19) | C6—N2—C9—C8 | 177.8 (2) |
Ru1—C10—C15—C14 | 51.48 (18) | C7—C8—C9—N2 | 0.4 (3) |
Ru1—C10—C15—C17 | −128.0 (2) | C9—N2—N3—Ru1 | 176.00 (15) |
Ru1—C11—C12—C13 | −52.02 (18) | C9—N2—N3—C7 | 0.0 (3) |
Ru1—C11—C12—C16 | 124.7 (2) | C9—N2—C6—C5 | −119.8 (3) |
Ru1—C12—C13—C14 | −54.26 (18) | C10—C11—C12—Ru1 | 55.08 (19) |
Ru1—C13—C14—C15 | −55.35 (19) | C10—C11—C12—C13 | 3.1 (3) |
Ru1—C14—C15—C10 | −50.90 (18) | C10—C11—C12—C16 | 179.8 (2) |
Ru1—C14—C15—C17 | 128.6 (2) | C10—C15—C17—C18 | 18.5 (3) |
Ru1—C15—C17—C18 | −71.8 (3) | C10—C15—C17—C19 | −104.5 (3) |
Ru1—C15—C17—C19 | 165.26 (18) | C11—C10—C15—Ru1 | −54.82 (19) |
F1—P1—O1—Ru1 | 65.24 (16) | C11—C10—C15—C14 | −3.3 (3) |
F2A—P1—O1—Ru1 | −178.98 (12) | C11—C10—C15—C17 | 177.2 (2) |
F2B—P1—O1—Ru1 | −49.24 (17) | C11—C12—C13—Ru1 | 51.22 (18) |
N1—C1—C2—C3 | −3.3 (4) | C11—C12—C13—C14 | −3.0 (3) |
N1—C5—C6—N2 | −57.3 (3) | C12—C13—C14—Ru1 | 55.18 (19) |
N2—N3—C7—C8 | 0.3 (3) | C12—C13—C14—C15 | −0.2 (3) |
N3—N2—C6—C5 | 58.2 (3) | C13—C14—C15—Ru1 | 54.27 (18) |
N3—N2—C9—C8 | −0.3 (3) | C13—C14—C15—C10 | 3.4 (3) |
N3—C7—C8—C9 | −0.4 (3) | C13—C14—C15—C17 | −177.1 (2) |
C1—N1—C5—C4 | 0.0 (3) | C14—C15—C17—C18 | −160.9 (2) |
C1—N1—C5—C6 | −178.27 (19) | C14—C15—C17—C19 | 76.1 (3) |
C1—C2—C3—C4 | 0.9 (4) | C15—C10—C11—Ru1 | 56.20 (19) |
C2—C3—C4—C5 | 1.8 (3) | C15—C10—C11—C12 | 0.1 (3) |
C3—C4—C5—N1 | −2.3 (3) | C16—C12—C13—Ru1 | −125.5 (2) |
C3—C4—C5—C6 | 175.9 (2) | C16—C12—C13—C14 | −179.7 (2) |
Experimental details
Crystal data | |
Chemical formula | [Ru(C10H14)(C9H9N3)(PO2F2)](PF6)0.86(BF4)0.14 |
Mr | 631.92 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 100 |
a, b, c (Å) | 15.6531 (17), 8.7619 (9), 17.4895 (18) |
β (°) | 106.316 (5) |
V (Å3) | 2302.1 (4) |
Z | 4 |
Radiation type | Cu Kα |
µ (mm−1) | 7.54 |
Crystal size (mm) | 0.16 × 0.10 × 0.06 |
Data collection | |
Diffractometer | Bruker SMART APEXII area-detector diffractometer |
Absorption correction | Analytical (SADABS; Bruker, 2012) |
Tmin, Tmax | 0.429, 0.735 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 32407, 4479, 4065 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.618 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.057, 1.02 |
No. of reflections | 4479 |
No. of parameters | 327 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.47, −0.33 |
Computer programs: APEX2 (Bruker, 2013), SAINT-Plus (Bruker, 2013), SHELXTL (Sheldrick, 2013), OLEX2 (Dolomanov et al., 2009).