Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806012712/gk2003sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806012712/gk2003Isup2.hkl |
CCDC reference: 608334
Key indicators
- Single-crystal X-ray study
- T = 123 K
- Mean (C-C) = 0.003 Å
- R factor = 0.023
- wR factor = 0.056
- Data-to-parameter ratio = 21.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 5 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru - Br .. 5.91 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SHELXTL (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[RuBr(C5H5)(C3H7)(C18H16NP)]PF6 | F(000) = 2816 |
Mr = 709.40 | Dx = 1.787 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 1001 reflections |
a = 15.384 (2) Å | θ = 2.7–29.8° |
b = 17.603 (2) Å | µ = 2.29 mm−1 |
c = 19.469 (2) Å | T = 123 K |
V = 5272.4 (11) Å3 | Block, orange |
Z = 8 | 0.38 × 0.31 × 0.25 mm |
Bruker SMART CCD area-detector diffractometer | 7663 independent reflections |
Radiation source: fine-focus sealed tube | 6108 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
ω scans | θmax = 30.0°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −21→21 |
Tmin = 0.458, Tmax = 0.564 | k = −24→24 |
59992 measured reflections | l = −27→26 |
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.056 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0224P)2 + 3.5883P] where P = (Fo2 + 2Fc2)/3 |
7663 reflections | (Δ/σ)max = 0.002 |
352 parameters | Δρmax = 0.50 e Å−3 |
0 restraints | Δρmin = −0.28 e Å−3 |
Experimental. Smart old, 4 x 606 omega scan frames, 0.3 ° and 20 sec per frame |
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. |
Refinement. 1) 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. 2) N-bound and allyl-bound hydrogen atoms refined unrestrained. All other hydrogen refined with the riding model. |
x | y | z | Uiso*/Ueq | ||
Ru | 0.148779 (9) | 0.134798 (8) | 0.605796 (7) | 0.01689 (4) | |
Br | 0.029085 (12) | 0.189698 (12) | 0.531800 (10) | 0.02634 (5) | |
P1 | 0.24155 (3) | 0.21871 (2) | 0.54451 (2) | 0.01549 (8) | |
N | 0.19318 (10) | 0.30321 (8) | 0.53603 (8) | 0.0191 (3) | |
H | 0.1447 (15) | 0.3000 (12) | 0.5461 (11) | 0.023* | |
C1 | 0.08118 (13) | 0.19397 (12) | 0.69272 (10) | 0.0268 (4) | |
H1 | 0.0331 | 0.2273 | 0.6871 | 0.032* | |
C2 | 0.16914 (13) | 0.21552 (11) | 0.69175 (9) | 0.0254 (4) | |
H2 | 0.1907 | 0.2656 | 0.6853 | 0.030* | |
C3 | 0.22009 (14) | 0.14913 (12) | 0.70221 (9) | 0.0286 (4) | |
H3 | 0.2817 | 0.1468 | 0.7040 | 0.034* | |
C4 | 0.16225 (16) | 0.08720 (12) | 0.70954 (10) | 0.0331 (5) | |
H4 | 0.1783 | 0.0358 | 0.7173 | 0.040* | |
C5 | 0.07585 (15) | 0.11517 (12) | 0.70334 (10) | 0.0317 (5) | |
H5 | 0.0240 | 0.0859 | 0.7059 | 0.038* | |
C6 | 0.08673 (16) | 0.02695 (12) | 0.57282 (12) | 0.0323 (5) | |
H6A | 0.0302 (17) | 0.0321 (14) | 0.5551 (13) | 0.039* | |
H6B | 0.0950 (16) | −0.0037 (14) | 0.6121 (12) | 0.039* | |
C7 | 0.15826 (15) | 0.04358 (11) | 0.53082 (11) | 0.0286 (4) | |
H7 | 0.1506 (15) | 0.0607 (13) | 0.4847 (13) | 0.034* | |
C8 | 0.23949 (15) | 0.04690 (11) | 0.56311 (11) | 0.0269 (4) | |
H8A | 0.2460 (15) | 0.0159 (13) | 0.6016 (12) | 0.032* | |
H8B | 0.2888 (15) | 0.0640 (13) | 0.5360 (12) | 0.032* | |
C9 | 0.34123 (11) | 0.23882 (10) | 0.59094 (9) | 0.0191 (3) | |
C10 | 0.40091 (12) | 0.18133 (11) | 0.60605 (10) | 0.0238 (4) | |
H10 | 0.3899 | 0.1307 | 0.5915 | 0.029* | |
C11 | 0.47605 (13) | 0.19814 (12) | 0.64218 (10) | 0.0281 (4) | |
H11 | 0.5170 | 0.1591 | 0.6517 | 0.034* | |
C12 | 0.49168 (13) | 0.27098 (13) | 0.66431 (10) | 0.0290 (4) | |
H12 | 0.5436 | 0.2822 | 0.6887 | 0.035* | |
C13 | 0.43227 (14) | 0.32786 (12) | 0.65127 (10) | 0.0278 (4) | |
H13 | 0.4429 | 0.3779 | 0.6674 | 0.033* | |
C14 | 0.35713 (12) | 0.31228 (11) | 0.61467 (9) | 0.0222 (4) | |
H14 | 0.3164 | 0.3516 | 0.6057 | 0.027* | |
C15 | 0.27440 (11) | 0.19074 (10) | 0.45869 (9) | 0.0177 (3) | |
C16 | 0.21067 (12) | 0.19012 (11) | 0.40794 (9) | 0.0223 (4) | |
H16 | 0.1519 | 0.2007 | 0.4194 | 0.027* | |
C17 | 0.23355 (14) | 0.17401 (11) | 0.34056 (10) | 0.0273 (4) | |
H17 | 0.1902 | 0.1736 | 0.3058 | 0.033* | |
C18 | 0.31866 (14) | 0.15867 (12) | 0.32380 (10) | 0.0294 (4) | |
H18 | 0.3338 | 0.1480 | 0.2775 | 0.035* | |
C19 | 0.38196 (14) | 0.15869 (12) | 0.37387 (10) | 0.0275 (4) | |
H19 | 0.4405 | 0.1477 | 0.3621 | 0.033* | |
C20 | 0.36014 (12) | 0.17477 (10) | 0.44135 (10) | 0.0226 (4) | |
H20 | 0.4038 | 0.1749 | 0.4758 | 0.027* | |
C21 | 0.20837 (12) | 0.35822 (10) | 0.48411 (9) | 0.0197 (3) | |
C22 | 0.13944 (13) | 0.40404 (10) | 0.46374 (10) | 0.0258 (4) | |
H22 | 0.0842 | 0.3985 | 0.4849 | 0.031* | |
C23 | 0.15124 (16) | 0.45765 (12) | 0.41279 (12) | 0.0342 (5) | |
H23 | 0.1040 | 0.4889 | 0.3991 | 0.041* | |
C24 | 0.23166 (16) | 0.46618 (12) | 0.38148 (10) | 0.0333 (5) | |
H24 | 0.2395 | 0.5027 | 0.3461 | 0.040* | |
C25 | 0.30009 (15) | 0.42118 (11) | 0.40223 (10) | 0.0291 (4) | |
H25 | 0.3553 | 0.4269 | 0.3810 | 0.035* | |
C26 | 0.28925 (13) | 0.36774 (10) | 0.45377 (10) | 0.0229 (4) | |
H26 | 0.3371 | 0.3377 | 0.4683 | 0.027* | |
P2 | 0.08985 (3) | 0.45969 (3) | 0.71205 (3) | 0.02291 (10) | |
F1 | 0.09284 (9) | 0.45228 (8) | 0.79356 (6) | 0.0389 (3) | |
F2 | 0.08631 (10) | 0.46776 (10) | 0.63130 (7) | 0.0523 (4) | |
F3 | 0.10440 (9) | 0.54896 (7) | 0.71982 (9) | 0.0504 (4) | |
F4 | 0.07580 (8) | 0.37021 (7) | 0.70614 (8) | 0.0392 (3) | |
F5 | −0.01296 (7) | 0.47169 (7) | 0.71596 (7) | 0.0329 (3) | |
F6 | 0.19293 (8) | 0.44701 (8) | 0.70859 (7) | 0.0373 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru | 0.01981 (7) | 0.01607 (6) | 0.01479 (6) | 0.00108 (5) | 0.00204 (5) | 0.00094 (5) |
Br | 0.01704 (8) | 0.03527 (10) | 0.02670 (10) | 0.00016 (8) | −0.00174 (7) | 0.00550 (8) |
P1 | 0.0164 (2) | 0.01586 (19) | 0.01421 (19) | 0.00133 (16) | −0.00037 (16) | 0.00038 (15) |
N | 0.0165 (7) | 0.0195 (7) | 0.0212 (7) | 0.0030 (6) | 0.0035 (6) | 0.0030 (6) |
C1 | 0.0317 (10) | 0.0315 (10) | 0.0173 (9) | 0.0078 (8) | 0.0072 (8) | −0.0007 (8) |
C2 | 0.0353 (11) | 0.0269 (9) | 0.0141 (8) | 0.0013 (8) | 0.0036 (8) | −0.0050 (7) |
C3 | 0.0308 (10) | 0.0411 (12) | 0.0139 (8) | 0.0069 (9) | −0.0016 (7) | −0.0017 (8) |
C4 | 0.0515 (14) | 0.0284 (10) | 0.0193 (9) | 0.0097 (10) | 0.0040 (9) | 0.0067 (8) |
C5 | 0.0381 (12) | 0.0353 (11) | 0.0218 (10) | −0.0058 (9) | 0.0107 (9) | 0.0028 (8) |
C6 | 0.0376 (12) | 0.0220 (9) | 0.0374 (12) | −0.0071 (9) | 0.0013 (10) | −0.0050 (9) |
C7 | 0.0411 (12) | 0.0178 (8) | 0.0268 (10) | −0.0011 (8) | 0.0029 (9) | −0.0069 (8) |
C8 | 0.0368 (11) | 0.0181 (8) | 0.0258 (10) | 0.0054 (8) | 0.0049 (9) | −0.0021 (7) |
C9 | 0.0180 (8) | 0.0238 (8) | 0.0155 (8) | −0.0002 (7) | −0.0003 (6) | 0.0003 (6) |
C10 | 0.0230 (9) | 0.0261 (9) | 0.0224 (9) | 0.0028 (7) | −0.0033 (7) | −0.0006 (7) |
C11 | 0.0223 (9) | 0.0399 (11) | 0.0222 (9) | 0.0048 (8) | −0.0025 (8) | 0.0051 (8) |
C12 | 0.0224 (9) | 0.0472 (12) | 0.0174 (9) | −0.0098 (9) | −0.0046 (7) | 0.0060 (8) |
C13 | 0.0341 (11) | 0.0303 (10) | 0.0190 (9) | −0.0111 (8) | −0.0036 (8) | 0.0016 (8) |
C14 | 0.0254 (9) | 0.0236 (8) | 0.0177 (8) | −0.0026 (8) | −0.0014 (7) | 0.0012 (7) |
C15 | 0.0197 (8) | 0.0168 (7) | 0.0165 (8) | −0.0003 (6) | 0.0028 (6) | 0.0010 (6) |
C16 | 0.0234 (9) | 0.0266 (9) | 0.0170 (8) | −0.0001 (7) | 0.0001 (7) | 0.0002 (7) |
C17 | 0.0342 (11) | 0.0293 (10) | 0.0183 (9) | −0.0026 (8) | −0.0012 (8) | −0.0012 (7) |
C18 | 0.0409 (12) | 0.0279 (10) | 0.0193 (9) | −0.0035 (9) | 0.0093 (8) | −0.0042 (8) |
C19 | 0.0258 (10) | 0.0281 (9) | 0.0286 (10) | −0.0028 (8) | 0.0111 (8) | −0.0056 (8) |
C20 | 0.0219 (9) | 0.0221 (9) | 0.0239 (9) | −0.0016 (7) | 0.0023 (7) | −0.0019 (7) |
C21 | 0.0256 (9) | 0.0161 (8) | 0.0175 (8) | −0.0015 (7) | −0.0034 (7) | 0.0003 (6) |
C22 | 0.0256 (10) | 0.0204 (9) | 0.0314 (10) | 0.0008 (7) | −0.0056 (8) | 0.0012 (8) |
C23 | 0.0452 (13) | 0.0224 (9) | 0.0350 (11) | 0.0016 (9) | −0.0166 (10) | 0.0047 (8) |
C24 | 0.0546 (14) | 0.0232 (9) | 0.0220 (9) | −0.0076 (9) | −0.0080 (9) | 0.0059 (8) |
C25 | 0.0412 (12) | 0.0235 (9) | 0.0227 (10) | −0.0094 (9) | 0.0034 (9) | −0.0011 (8) |
C26 | 0.0271 (9) | 0.0198 (8) | 0.0218 (9) | −0.0013 (7) | −0.0002 (7) | 0.0000 (7) |
P2 | 0.0220 (2) | 0.0202 (2) | 0.0266 (3) | −0.00144 (19) | −0.00109 (19) | 0.00317 (19) |
F1 | 0.0370 (7) | 0.0528 (8) | 0.0267 (7) | −0.0061 (6) | −0.0023 (5) | 0.0005 (6) |
F2 | 0.0458 (8) | 0.0857 (11) | 0.0256 (7) | 0.0094 (8) | −0.0007 (6) | 0.0139 (7) |
F3 | 0.0448 (8) | 0.0215 (6) | 0.0849 (12) | −0.0077 (6) | −0.0016 (8) | 0.0074 (7) |
F4 | 0.0365 (7) | 0.0206 (6) | 0.0606 (9) | 0.0010 (5) | −0.0089 (6) | −0.0060 (6) |
F5 | 0.0229 (6) | 0.0314 (6) | 0.0445 (7) | 0.0034 (5) | −0.0020 (5) | −0.0048 (5) |
F6 | 0.0213 (6) | 0.0469 (8) | 0.0436 (8) | 0.0005 (5) | 0.0026 (5) | 0.0074 (6) |
Ru—C1 | 2.243 (2) | C11—C12 | 1.374 (3) |
Ru—C2 | 2.218 (2) | C11—H11 | 0.9500 |
Ru—C3 | 2.189 (2) | C12—C13 | 1.379 (3) |
Ru—C4 | 2.196 (2) | C12—H12 | 0.9500 |
Ru—C5 | 2.233 (2) | C13—C14 | 1.385 (3) |
Ru—C6 | 2.220 (2) | C13—H13 | 0.9500 |
Ru—C7 | 2.175 (2) | C14—H14 | 0.9500 |
Ru—C8 | 2.243 (2) | C15—C20 | 1.390 (2) |
Ru—P1 | 2.3754 (5) | C15—C16 | 1.392 (2) |
Ru—Br | 2.5298 (3) | C16—C17 | 1.387 (3) |
C6—C7 | 1.402 (3) | C16—H16 | 0.9500 |
C7—C8 | 1.400 (3) | C17—C18 | 1.376 (3) |
P1—C9 | 1.815 (2) | C17—H17 | 0.9500 |
P1—C15 | 1.814 (2) | C18—C19 | 1.378 (3) |
P1—N | 1.6714 (15) | C18—H18 | 0.9500 |
N—C21 | 1.419 (2) | C19—C20 | 1.385 (3) |
N—H | 0.77 (2) | C19—H19 | 0.9500 |
C1—C2 | 1.406 (3) | C20—H20 | 0.9500 |
C1—C5 | 1.405 (3) | C21—C26 | 1.387 (3) |
C1—H1 | 0.9500 | C21—C22 | 1.390 (3) |
C2—C3 | 1.422 (3) | C22—C23 | 1.381 (3) |
C2—H2 | 0.9500 | C22—H22 | 0.9500 |
C3—C4 | 1.414 (3) | C23—C24 | 1.387 (3) |
C3—H3 | 0.9500 | C23—H23 | 0.9500 |
C4—C5 | 1.423 (3) | C24—C25 | 1.378 (3) |
C4—H4 | 0.9500 | C24—H24 | 0.9500 |
C5—H5 | 0.9500 | C25—C26 | 1.385 (3) |
C6—H6A | 0.94 (3) | C25—H25 | 0.9500 |
C6—H6B | 0.94 (2) | C26—H26 | 0.9500 |
C7—H7 | 0.95 (2) | P2—F2 | 1.5795 (14) |
C8—H8A | 0.93 (2) | P2—F1 | 1.5929 (13) |
C8—H8B | 0.97 (2) | P2—F3 | 1.5944 (14) |
C9—C14 | 1.395 (3) | P2—F4 | 1.5941 (13) |
C9—C10 | 1.398 (3) | P2—F5 | 1.5974 (13) |
C10—C11 | 1.385 (3) | P2—F6 | 1.6029 (13) |
C10—H10 | 0.9500 | ||
C7—Ru—P1 | 94.68 (6) | C7—C6—H6A | 119.4 (16) |
C7—Ru—Br | 87.06 (6) | Ru—C6—H6A | 115.0 (15) |
P1—Ru—Br | 85.053 (15) | C7—C6—H6B | 119.1 (16) |
C6—C7—C8 | 116.6 (2) | Ru—C6—H6B | 101.3 (15) |
P1—N—C21 | 127.17 (13) | H6A—C6—H6B | 119 (2) |
C7—Ru—C3 | 128.83 (8) | C8—C7—Ru | 74.19 (11) |
C7—Ru—C4 | 109.22 (8) | C6—C7—Ru | 73.14 (12) |
C3—Ru—C4 | 37.63 (8) | C8—C7—H7 | 121.3 (14) |
C7—Ru—C2 | 165.94 (8) | C6—C7—H7 | 121.2 (14) |
C3—Ru—C2 | 37.64 (7) | Ru—C7—H7 | 113.0 (14) |
C4—Ru—C2 | 62.43 (8) | C7—C8—Ru | 68.89 (11) |
C7—Ru—C6 | 37.19 (8) | C7—C8—H8A | 115.6 (15) |
C3—Ru—C6 | 124.20 (9) | Ru—C8—H8A | 99.9 (14) |
C4—Ru—C6 | 88.87 (9) | C7—C8—H8B | 117.8 (14) |
C2—Ru—C6 | 145.79 (8) | Ru—C8—H8B | 118.2 (14) |
C7—Ru—C5 | 119.36 (8) | H8A—C8—H8B | 122 (2) |
C3—Ru—C5 | 62.63 (8) | C14—C9—C10 | 119.10 (17) |
C4—Ru—C5 | 37.46 (8) | C14—C9—P1 | 119.60 (14) |
C2—Ru—C5 | 61.85 (8) | C10—C9—P1 | 121.24 (14) |
C6—Ru—C5 | 84.12 (8) | C11—C10—C9 | 120.03 (18) |
C7—Ru—C1 | 151.69 (8) | C11—C10—H10 | 120.0 |
C3—Ru—C1 | 62.08 (8) | C9—C10—H10 | 120.0 |
C4—Ru—C1 | 61.77 (8) | C12—C11—C10 | 120.31 (19) |
C2—Ru—C1 | 36.73 (7) | C12—C11—H11 | 119.8 |
C6—Ru—C1 | 114.58 (8) | C10—C11—H11 | 119.8 |
C5—Ru—C1 | 36.59 (8) | C11—C12—C13 | 120.26 (18) |
C7—Ru—C8 | 36.91 (8) | C11—C12—H12 | 119.9 |
C3—Ru—C8 | 94.90 (8) | C13—C12—H12 | 119.9 |
C4—Ru—C8 | 91.08 (8) | C12—C13—C14 | 120.26 (19) |
C2—Ru—C8 | 129.32 (8) | C12—C13—H13 | 119.9 |
C6—Ru—C8 | 64.56 (8) | C14—C13—H13 | 119.9 |
C5—Ru—C8 | 121.40 (8) | C13—C14—C9 | 120.02 (18) |
C1—Ru—C8 | 152.66 (7) | C13—C14—H14 | 120.0 |
C3—Ru—P1 | 93.32 (6) | C9—C14—H14 | 120.0 |
C4—Ru—P1 | 129.97 (7) | C20—C15—C16 | 119.63 (17) |
C2—Ru—P1 | 84.01 (5) | C20—C15—P1 | 122.88 (14) |
C6—Ru—P1 | 130.16 (6) | C16—C15—P1 | 117.37 (13) |
C5—Ru—P1 | 145.63 (6) | C17—C16—C15 | 119.61 (18) |
C1—Ru—P1 | 111.64 (6) | C17—C16—H16 | 120.2 |
C8—Ru—P1 | 82.47 (6) | C15—C16—H16 | 120.2 |
C3—Ru—Br | 144.02 (5) | C18—C17—C16 | 120.37 (19) |
C4—Ru—Br | 137.56 (6) | C18—C17—H17 | 119.8 |
C2—Ru—Br | 106.73 (5) | C16—C17—H17 | 119.8 |
C6—Ru—Br | 81.31 (7) | C17—C18—C19 | 120.30 (18) |
C5—Ru—Br | 100.24 (6) | C17—C18—H18 | 119.8 |
C1—Ru—Br | 85.11 (5) | C19—C18—H18 | 119.8 |
C8—Ru—Br | 120.36 (6) | C18—C19—C20 | 119.99 (19) |
N—P1—C15 | 105.95 (8) | C18—C19—H19 | 120.0 |
N—P1—C9 | 104.59 (8) | C20—C19—H19 | 120.0 |
C15—P1—C9 | 106.04 (8) | C19—C20—C15 | 120.09 (18) |
N—P1—Ru | 109.60 (6) | C19—C20—H20 | 120.0 |
C15—P1—Ru | 117.47 (6) | C15—C20—H20 | 120.0 |
C9—P1—Ru | 112.26 (6) | C26—C21—C22 | 119.51 (17) |
C21—N—H | 112.9 (17) | C26—C21—N | 122.24 (16) |
P1—N—H | 109.9 (16) | C22—C21—N | 118.26 (17) |
C2—C1—C5 | 108.95 (18) | C23—C22—C21 | 120.1 (2) |
C2—C1—Ru | 70.66 (11) | C23—C22—H22 | 120.0 |
C5—C1—Ru | 71.32 (11) | C21—C22—H22 | 120.0 |
C2—C1—H1 | 125.5 | C22—C23—C24 | 120.4 (2) |
C5—C1—H1 | 125.5 | C22—C23—H23 | 119.8 |
Ru—C1—H1 | 124.1 | C24—C23—H23 | 119.8 |
C1—C2—C3 | 107.87 (18) | C25—C24—C23 | 119.36 (19) |
C1—C2—Ru | 72.61 (11) | C25—C24—H24 | 120.3 |
C3—C2—Ru | 70.08 (11) | C23—C24—H24 | 120.3 |
C1—C2—H2 | 126.1 | C24—C25—C26 | 120.7 (2) |
C3—C2—H2 | 126.1 | C24—C25—H25 | 119.6 |
Ru—C2—H2 | 122.9 | C26—C25—H25 | 119.6 |
C4—C3—C2 | 107.53 (19) | C25—C26—C21 | 119.89 (18) |
C4—C3—Ru | 71.48 (12) | C25—C26—H26 | 120.1 |
C2—C3—Ru | 72.28 (11) | C21—C26—H26 | 120.1 |
C4—C3—H3 | 126.2 | F2—P2—F1 | 179.44 (9) |
C2—C3—H3 | 126.2 | F2—P2—F3 | 90.61 (9) |
Ru—C3—H3 | 121.7 | F1—P2—F3 | 88.98 (8) |
C3—C4—C5 | 108.21 (18) | F2—P2—F4 | 90.70 (9) |
C3—C4—Ru | 70.89 (11) | F1—P2—F4 | 89.71 (8) |
C5—C4—Ru | 72.66 (11) | F3—P2—F4 | 178.67 (9) |
C3—C4—H4 | 125.9 | F2—P2—F5 | 90.08 (8) |
C5—C4—H4 | 125.9 | F1—P2—F5 | 89.54 (7) |
Ru—C4—H4 | 122.2 | F3—P2—F5 | 90.24 (7) |
C1—C5—C4 | 107.43 (19) | F4—P2—F5 | 89.99 (7) |
C1—C5—Ru | 72.10 (11) | F2—P2—F6 | 90.27 (8) |
C4—C5—Ru | 69.88 (11) | F1—P2—F6 | 90.11 (7) |
C1—C5—H5 | 126.3 | F3—P2—F6 | 90.13 (8) |
C4—C5—H5 | 126.3 | F4—P2—F6 | 89.63 (7) |
Ru—C5—H5 | 123.4 | F5—P2—F6 | 179.49 (8) |
C7—C6—Ru | 69.67 (11) | ||
C7—Ru—P1—N | 129.18 (9) | C1—Ru—C4—C5 | 37.08 (12) |
C3—Ru—P1—N | −101.40 (8) | C8—Ru—C4—C5 | −146.33 (13) |
C4—Ru—P1—N | −110.84 (9) | P1—Ru—C4—C5 | 132.60 (11) |
C2—Ru—P1—N | −64.87 (8) | Br—Ru—C4—C5 | −6.00 (17) |
C6—Ru—P1—N | 116.81 (11) | C2—C1—C5—C4 | 0.4 (2) |
C5—Ru—P1—N | −58.36 (13) | Ru—C1—C5—C4 | 61.30 (14) |
C1—Ru—P1—N | −40.18 (8) | C2—C1—C5—Ru | −60.94 (13) |
C8—Ru—P1—N | 164.10 (8) | C3—C4—C5—C1 | −0.4 (2) |
Br—Ru—P1—N | 42.56 (6) | Ru—C4—C5—C1 | −62.73 (14) |
C7—Ru—P1—C15 | 8.26 (9) | C3—C4—C5—Ru | 62.36 (14) |
C3—Ru—P1—C15 | 137.68 (8) | C7—Ru—C5—C1 | −159.53 (13) |
C4—Ru—P1—C15 | 128.24 (10) | C3—Ru—C5—C1 | 79.21 (14) |
C2—Ru—P1—C15 | 174.21 (8) | C4—Ru—C5—C1 | 116.98 (19) |
C6—Ru—P1—C15 | −4.11 (11) | C2—Ru—C5—C1 | 36.46 (12) |
C5—Ru—P1—C15 | −179.29 (12) | C6—Ru—C5—C1 | −147.18 (14) |
C1—Ru—P1—C15 | −161.11 (9) | C8—Ru—C5—C1 | 157.48 (12) |
C8—Ru—P1—C15 | 43.17 (8) | P1—Ru—C5—C1 | 29.11 (19) |
Br—Ru—P1—C15 | −78.37 (7) | Br—Ru—C5—C1 | −67.14 (13) |
C7—Ru—P1—C9 | −115.06 (9) | C7—Ru—C5—C4 | 83.50 (15) |
C3—Ru—P1—C9 | 14.36 (8) | C3—Ru—C5—C4 | −37.76 (13) |
C4—Ru—P1—C9 | 4.92 (10) | C2—Ru—C5—C4 | −80.52 (14) |
C2—Ru—P1—C9 | 50.89 (8) | C6—Ru—C5—C4 | 95.84 (14) |
C6—Ru—P1—C9 | −127.43 (11) | C1—Ru—C5—C4 | −116.98 (19) |
C5—Ru—P1—C9 | 57.40 (13) | C8—Ru—C5—C4 | 40.50 (16) |
C1—Ru—P1—C9 | 75.58 (9) | P1—Ru—C5—C4 | −87.86 (15) |
C8—Ru—P1—C9 | −80.14 (8) | Br—Ru—C5—C4 | 175.89 (12) |
Br—Ru—P1—C9 | 158.32 (6) | C3—Ru—C6—C7 | −111.01 (14) |
C15—P1—N—C21 | −26.98 (17) | C4—Ru—C6—C7 | −124.81 (14) |
C9—P1—N—C21 | 84.82 (17) | C2—Ru—C6—C7 | −156.33 (14) |
Ru—P1—N—C21 | −154.64 (14) | C5—Ru—C6—C7 | −162.05 (15) |
C7—Ru—C1—C2 | 158.82 (16) | C1—Ru—C6—C7 | 177.15 (13) |
C3—Ru—C1—C2 | 37.97 (12) | C8—Ru—C6—C7 | −33.07 (13) |
C4—Ru—C1—C2 | 80.85 (13) | P1—Ru—C6—C7 | 20.69 (17) |
C6—Ru—C1—C2 | 155.18 (12) | Br—Ru—C6—C7 | 96.62 (13) |
C5—Ru—C1—C2 | 118.82 (18) | Ru—C6—C7—C8 | 61.98 (15) |
C8—Ru—C1—C2 | 73.4 (2) | C3—Ru—C7—C8 | −27.22 (16) |
P1—Ru—C1—C2 | −44.00 (12) | C4—Ru—C7—C8 | −64.47 (14) |
Br—Ru—C1—C2 | −126.70 (11) | C2—Ru—C7—C8 | −13.2 (4) |
C7—Ru—C1—C5 | 40.0 (2) | C6—Ru—C7—C8 | −124.9 (2) |
C3—Ru—C1—C5 | −80.85 (14) | C5—Ru—C7—C8 | −104.26 (14) |
C4—Ru—C1—C5 | −37.96 (13) | C1—Ru—C7—C8 | −130.34 (17) |
C2—Ru—C1—C5 | −118.82 (18) | P1—Ru—C7—C8 | 70.86 (12) |
C6—Ru—C1—C5 | 36.36 (16) | Br—Ru—C7—C8 | 155.65 (12) |
C8—Ru—C1—C5 | −45.4 (2) | C3—Ru—C7—C6 | 97.64 (16) |
P1—Ru—C1—C5 | −162.81 (12) | C4—Ru—C7—C6 | 60.39 (16) |
Br—Ru—C1—C5 | 114.49 (13) | C2—Ru—C7—C6 | 111.7 (3) |
C5—C1—C2—C3 | −0.2 (2) | C5—Ru—C7—C6 | 20.60 (17) |
Ru—C1—C2—C3 | −61.57 (13) | C1—Ru—C7—C6 | −5.5 (2) |
C5—C1—C2—Ru | 61.35 (14) | C8—Ru—C7—C6 | 124.86 (19) |
C7—Ru—C2—C1 | −135.1 (3) | P1—Ru—C7—C6 | −164.28 (13) |
C3—Ru—C2—C1 | −117.10 (17) | Br—Ru—C7—C6 | −79.49 (13) |
C4—Ru—C2—C1 | −78.90 (13) | C6—C7—C8—Ru | −61.41 (16) |
C6—Ru—C2—C1 | −42.8 (2) | C3—Ru—C8—C7 | 159.05 (13) |
C5—Ru—C2—C1 | −36.32 (12) | C4—Ru—C8—C7 | 121.55 (13) |
C8—Ru—C2—C1 | −145.32 (12) | C2—Ru—C8—C7 | 175.89 (12) |
P1—Ru—C2—C1 | 139.52 (11) | C6—Ru—C8—C7 | 33.31 (13) |
Br—Ru—C2—C1 | 56.53 (12) | C5—Ru—C8—C7 | 98.27 (14) |
C7—Ru—C2—C3 | −18.0 (4) | C1—Ru—C8—C7 | 128.08 (17) |
C4—Ru—C2—C3 | 38.20 (12) | P1—Ru—C8—C7 | −108.24 (12) |
C6—Ru—C2—C3 | 74.34 (19) | Br—Ru—C8—C7 | −28.50 (14) |
C5—Ru—C2—C3 | 80.79 (14) | N—P1—C9—C14 | 4.67 (17) |
C1—Ru—C2—C3 | 117.10 (17) | C15—P1—C9—C14 | 116.40 (15) |
C8—Ru—C2—C3 | −28.21 (16) | Ru—P1—C9—C14 | −114.09 (14) |
P1—Ru—C2—C3 | −103.38 (12) | N—P1—C9—C10 | −178.12 (15) |
Br—Ru—C2—C3 | 173.63 (11) | C15—P1—C9—C10 | −66.39 (16) |
C1—C2—C3—C4 | 0.0 (2) | Ru—P1—C9—C10 | 63.13 (16) |
Ru—C2—C3—C4 | −63.21 (13) | C14—C9—C10—C11 | −2.1 (3) |
C1—C2—C3—Ru | 63.20 (13) | P1—C9—C10—C11 | −179.32 (15) |
C7—Ru—C3—C4 | −69.40 (15) | C9—C10—C11—C12 | 1.0 (3) |
C2—Ru—C3—C4 | 116.14 (17) | C10—C11—C12—C13 | 0.6 (3) |
C6—Ru—C3—C4 | −22.98 (16) | C11—C12—C13—C14 | −1.2 (3) |
C5—Ru—C3—C4 | 37.59 (12) | C12—C13—C14—C9 | 0.1 (3) |
C1—Ru—C3—C4 | 79.09 (13) | C10—C9—C14—C13 | 1.5 (3) |
C8—Ru—C3—C4 | −85.40 (13) | P1—C9—C14—C13 | 178.80 (14) |
P1—Ru—C3—C4 | −168.12 (12) | N—P1—C15—C20 | 122.11 (15) |
Br—Ru—C3—C4 | 105.72 (13) | C9—P1—C15—C20 | 11.34 (17) |
C7—Ru—C3—C2 | 174.47 (12) | Ru—P1—C15—C20 | −115.08 (14) |
C4—Ru—C3—C2 | −116.14 (17) | N—P1—C15—C16 | −53.90 (16) |
C6—Ru—C3—C2 | −139.12 (13) | C9—P1—C15—C16 | −164.67 (14) |
C5—Ru—C3—C2 | −78.55 (13) | Ru—P1—C15—C16 | 68.91 (15) |
C1—Ru—C3—C2 | −37.05 (12) | C20—C15—C16—C17 | −0.4 (3) |
C8—Ru—C3—C2 | 158.46 (12) | P1—C15—C16—C17 | 175.78 (14) |
P1—Ru—C3—C2 | 75.74 (11) | C15—C16—C17—C18 | 0.0 (3) |
Br—Ru—C3—C2 | −10.41 (18) | C16—C17—C18—C19 | 0.4 (3) |
C2—C3—C4—C5 | 0.2 (2) | C17—C18—C19—C20 | −0.5 (3) |
Ru—C3—C4—C5 | −63.50 (14) | C18—C19—C20—C15 | 0.1 (3) |
C2—C3—C4—Ru | 63.74 (13) | C16—C15—C20—C19 | 0.3 (3) |
C7—Ru—C4—C3 | 129.45 (13) | P1—C15—C20—C19 | −175.64 (14) |
C2—Ru—C4—C3 | −38.21 (12) | P1—N—C21—C26 | −31.9 (3) |
C6—Ru—C4—C3 | 161.16 (13) | P1—N—C21—C22 | 148.45 (15) |
C5—Ru—C4—C3 | −117.05 (18) | C26—C21—C22—C23 | 1.2 (3) |
C1—Ru—C4—C3 | −79.97 (13) | N—C21—C22—C23 | −179.21 (18) |
C8—Ru—C4—C3 | 96.63 (13) | C21—C22—C23—C24 | 0.1 (3) |
P1—Ru—C4—C3 | 15.55 (15) | C22—C23—C24—C25 | −0.7 (3) |
Br—Ru—C4—C3 | −123.05 (12) | C23—C24—C25—C26 | 0.1 (3) |
C7—Ru—C4—C5 | −113.50 (13) | C24—C25—C26—C21 | 1.2 (3) |
C3—Ru—C4—C5 | 117.05 (18) | C22—C21—C26—C25 | −1.8 (3) |
C2—Ru—C4—C5 | 78.84 (13) | N—C21—C26—C25 | 178.59 (17) |
C6—Ru—C4—C5 | −81.79 (14) |
D—H···A | D—H | H···A | D···A | D—H···A |
N—H···Br | 0.77 (2) | 2.65 (2) | 3.2206 (16) | 132 (2) |
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