Download citation
Download citation
link to html
In ([eta]6-p-cymene)(difluorophosphinato-[kappa]O){2-[(1H-pyrazol-1-yl)methyl-[kappa]N2]pyridine-[kappa]N}ruthenium(II) 0.85-hexafluoro­phosphate 0.15-tetrafluoroborate, [Ru(PO2F2)(C10H14)(C9H9N3)](PF6)0.85(BF4)0.15, (I), the [PO2F2]- ligand exhibits positional disorder due to one F atom and one O atom sharing the same two positions related by a mirror reflection across the O-P-F plane. The correct composition of this coordinated anion was successfully determined to be [PO2F2]- by refining the complex with various tetrahedral anions in which terminal atoms have similar atomic form factors. The noncoordinated counter-ion is compositionally disordered between [PF6]- and [BF4]-. The difficulty in determining the correct composition of this anion illustrates the importance of a crystallographer remaining impartial and open to encountering unexpected moieties in the process of elucidating a structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113017605/wq3041sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270113017605/wq3041Isup2.hkl
Contains datablock I

CCDC reference: 962896

Computing details top

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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
(η6-p-Cymene)(difluorophosphinato-κO){2-[(1H-pyrazol-1-yl-κN2)methyl]pyridine-κN}ruthenium(II) hexafluorophosphate tetrafluoroborate (1/0.86/0.14) top
Crystal data top
[Ru(C10H14)(C9H9N3)(PO2F2)](PF6)0.86(BF4)0.14F(000) = 1264
Mr = 631.92Dx = 1.823 Mg m3
Monoclinic, P21/nCu Kα radiation, λ = 1.54178 Å
a = 15.6531 (17) ÅCell parameters from 9902 reflections
b = 8.7619 (9) Åθ = 4.5–71.7°
c = 17.4895 (18) ŵ = 7.54 mm1
β = 106.316 (5)°T = 100 K
V = 2302.1 (4) Å3Slab, orange
Z = 40.16 × 0.10 × 0.06 mm
Data collection top
Bruker SMART APEXII area-detector
diffractometer
4479 independent reflections
Radiation source: sealed X-ray tube, Siemens, K FFCU 2K 904065 reflections with I > 2σ(I)
Equatorially mounted graphite monochromatorRint = 0.039
Detector resolution: 7.9 pixels mm-1θmax = 72.3°, θmin = 3.4°
0.60° ω and 0.6° ϕ scansh = 1918
Absorption correction: analytical
(SADABS; Bruker, 2012)
k = 1010
Tmin = 0.429, Tmax = 0.735l = 1921
32407 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H-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 reflectionsΔρmax = 0.47 e Å3
327 parametersΔρmin = 0.33 e Å3
Crystal data top
[Ru(C10H14)(C9H9N3)(PO2F2)](PF6)0.86(BF4)0.14V = 2302.1 (4) Å3
Mr = 631.92Z = 4
Monoclinic, P21/nCu Kα radiation
a = 15.6531 (17) ŵ = 7.54 mm1
b = 8.7619 (9) ÅT = 100 K
c = 17.4895 (18) Å0.16 × 0.10 × 0.06 mm
β = 106.316 (5)°
Data collection top
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 = 0.735Rint = 0.039
32407 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.057H-atom parameters constrained
S = 1.02Δρmax = 0.47 e Å3
4479 reflectionsΔρmin = 0.33 e Å3
327 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ru10.55217 (2)0.90161 (2)0.27953 (2)0.01267 (6)
P10.48184 (4)1.25979 (7)0.24813 (4)0.02103 (13)
F10.40442 (12)1.22266 (19)0.17430 (10)0.0436 (4)
F2A0.44888 (11)1.38720 (17)0.28842 (10)0.0287 (4)0.5
O2B0.44888 (11)1.38720 (17)0.28842 (10)0.0287 (4)0.5
F2B0.55436 (12)1.31092 (19)0.21382 (11)0.0350 (4)0.5
O2A0.55436 (12)1.31092 (19)0.21382 (11)0.0350 (4)0.5
O10.50252 (11)1.11911 (17)0.29711 (10)0.0185 (3)
N10.57552 (12)0.8956 (2)0.40467 (11)0.0145 (4)
N20.40768 (13)0.7363 (2)0.33223 (11)0.0193 (4)
N30.42432 (12)0.8334 (2)0.27798 (11)0.0165 (4)
C10.62923 (15)1.0027 (3)0.44785 (14)0.0192 (5)
H10.65271.07880.42070.023*
C20.65186 (16)1.0071 (3)0.52975 (15)0.0247 (5)
H20.69251.08140.55860.030*
C30.61440 (16)0.9018 (3)0.56913 (15)0.0254 (5)
H30.62820.90310.62560.031*
C40.55660 (16)0.7943 (3)0.52536 (14)0.0217 (5)
H40.52880.72260.55140.026*
C50.53934 (14)0.7917 (3)0.44333 (13)0.0167 (4)
C60.48156 (16)0.6703 (3)0.39366 (14)0.0211 (5)
H6A0.51800.60640.36820.025*
H6B0.45780.60360.42850.025*
C70.34528 (15)0.8783 (3)0.23143 (14)0.0217 (5)
H70.33660.94680.18780.026*
C80.27713 (17)0.8096 (3)0.25642 (16)0.0296 (6)
H80.21480.82220.23400.036*
C90.31937 (16)0.7198 (3)0.32029 (15)0.0266 (5)
H90.29130.65730.35050.032*
C100.58083 (16)0.6985 (3)0.22017 (14)0.0215 (5)
H100.55590.59940.21920.026*
C110.65646 (16)0.7385 (3)0.28218 (14)0.0224 (5)
H110.68180.66540.32230.027*
C120.69611 (15)0.8863 (3)0.28628 (14)0.0230 (5)
C130.65426 (15)0.9930 (3)0.22829 (14)0.0209 (5)
H130.67731.09370.23090.025*
C140.57733 (15)0.9527 (3)0.16514 (13)0.0182 (5)
H140.55021.02760.12670.022*
C150.54095 (15)0.8053 (3)0.15862 (13)0.0183 (5)
C160.77689 (16)0.9271 (4)0.35332 (16)0.0344 (7)
H16A0.77681.03690.36380.052*
H16B0.83080.90010.33840.052*
H16C0.77560.87070.40140.052*
C170.46174 (17)0.7656 (3)0.08834 (14)0.0241 (5)
H170.42010.85470.07780.029*
C180.4099 (2)0.6252 (3)0.10075 (16)0.0333 (6)
H18A0.44710.53420.10360.050*
H18B0.35600.61520.05610.050*
H18C0.39340.63600.15050.050*
C190.49747 (19)0.7442 (3)0.01539 (15)0.0315 (6)
H19A0.53070.83540.00840.047*
H19B0.44750.72840.03230.047*
H19C0.53690.65510.02370.047*
P20.73404 (5)0.43580 (8)0.46735 (4)0.0192 (2)0.854 (3)
F30.77516 (16)0.4669 (3)0.56018 (11)0.0372 (6)0.854 (3)
F40.64455 (13)0.3736 (3)0.48429 (13)0.0471 (6)0.854 (3)
F50.77414 (14)0.2683 (2)0.47753 (16)0.0464 (6)0.854 (3)
F60.82175 (13)0.5013 (2)0.45011 (12)0.0390 (5)0.854 (3)
F70.69530 (15)0.6044 (2)0.45747 (13)0.0444 (6)0.854 (3)
F80.69105 (15)0.4060 (3)0.37410 (12)0.0475 (6)0.854 (3)
F90.7598 (11)0.5712 (15)0.4432 (10)0.085 (4)*0.146 (3)
F110.6396 (9)0.443 (2)0.4615 (12)0.085 (4)*0.146 (3)
F120.7521 (11)0.3111 (16)0.4312 (11)0.085 (4)*0.146 (3)
F100.7755 (14)0.422 (2)0.5539 (8)0.085 (4)*0.146 (3)
B10.7317 (8)0.4369 (13)0.4725 (7)0.085 (4)*0.146 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01457 (9)0.01302 (9)0.01117 (9)0.00064 (6)0.00483 (6)0.00039 (6)
P10.0220 (3)0.0138 (3)0.0249 (3)0.0008 (2)0.0029 (2)0.0009 (2)
F10.0535 (11)0.0359 (9)0.0280 (9)0.0111 (8)0.0103 (7)0.0029 (7)
F2A0.0342 (9)0.0191 (8)0.0331 (9)0.0040 (7)0.0098 (7)0.0038 (7)
O2B0.0342 (9)0.0191 (8)0.0331 (9)0.0040 (7)0.0098 (7)0.0038 (7)
F2B0.0377 (10)0.0280 (9)0.0470 (11)0.0002 (7)0.0247 (8)0.0064 (8)
O2A0.0377 (10)0.0280 (9)0.0470 (11)0.0002 (7)0.0247 (8)0.0064 (8)
O10.0242 (8)0.0138 (7)0.0210 (9)0.0011 (6)0.0119 (7)0.0001 (6)
N10.0152 (9)0.0169 (9)0.0121 (9)0.0028 (7)0.0052 (7)0.0002 (7)
N20.0231 (10)0.0198 (10)0.0155 (10)0.0075 (8)0.0062 (8)0.0002 (8)
N30.0190 (9)0.0166 (9)0.0149 (10)0.0034 (7)0.0064 (7)0.0005 (7)
C10.0162 (11)0.0225 (11)0.0189 (12)0.0006 (9)0.0052 (9)0.0034 (9)
C20.0222 (12)0.0308 (13)0.0198 (13)0.0012 (10)0.0040 (9)0.0058 (10)
C30.0260 (12)0.0333 (14)0.0166 (12)0.0080 (11)0.0053 (9)0.0019 (10)
C40.0227 (12)0.0253 (12)0.0188 (12)0.0062 (10)0.0086 (9)0.0045 (10)
C50.0174 (11)0.0178 (11)0.0156 (11)0.0041 (9)0.0057 (9)0.0015 (9)
C60.0299 (13)0.0164 (11)0.0175 (12)0.0014 (9)0.0075 (10)0.0037 (9)
C70.0198 (11)0.0245 (12)0.0190 (12)0.0031 (9)0.0026 (9)0.0019 (9)
C80.0201 (12)0.0412 (15)0.0266 (14)0.0095 (11)0.0050 (10)0.0063 (11)
C90.0254 (13)0.0336 (14)0.0228 (13)0.0149 (11)0.0099 (10)0.0063 (11)
C100.0327 (13)0.0169 (11)0.0175 (12)0.0062 (10)0.0114 (10)0.0008 (9)
C110.0247 (12)0.0274 (12)0.0169 (12)0.0150 (10)0.0089 (9)0.0036 (9)
C120.0169 (11)0.0367 (14)0.0193 (12)0.0050 (10)0.0111 (9)0.0007 (10)
C130.0206 (11)0.0267 (12)0.0204 (12)0.0029 (9)0.0141 (9)0.0016 (9)
C140.0237 (11)0.0199 (11)0.0142 (11)0.0029 (9)0.0106 (9)0.0031 (9)
C150.0239 (12)0.0206 (11)0.0124 (11)0.0047 (9)0.0084 (9)0.0018 (9)
C160.0162 (12)0.0614 (19)0.0259 (14)0.0022 (12)0.0063 (10)0.0045 (13)
C170.0285 (13)0.0256 (12)0.0167 (12)0.0037 (10)0.0037 (10)0.0015 (9)
C180.0403 (15)0.0352 (15)0.0226 (14)0.0099 (12)0.0058 (11)0.0086 (11)
C190.0399 (15)0.0375 (15)0.0161 (13)0.0036 (12)0.0059 (11)0.0042 (11)
P20.0174 (4)0.0221 (4)0.0177 (4)0.0016 (3)0.0044 (3)0.0038 (3)
F30.0456 (11)0.0441 (13)0.0164 (10)0.0177 (10)0.0004 (8)0.0066 (8)
F40.0286 (10)0.0758 (17)0.0405 (13)0.0239 (10)0.0153 (9)0.0016 (11)
F50.0417 (12)0.0219 (10)0.0706 (16)0.0021 (8)0.0077 (11)0.0020 (10)
F60.0395 (11)0.0390 (11)0.0487 (13)0.0150 (9)0.0290 (9)0.0114 (9)
F70.0558 (13)0.0350 (11)0.0429 (12)0.0200 (10)0.0151 (10)0.0073 (9)
F80.0582 (14)0.0574 (14)0.0238 (11)0.0168 (11)0.0066 (9)0.0050 (9)
Geometric parameters (Å, º) top
Ru1—O12.1130 (15)C10—H100.9500
Ru1—N12.1160 (18)C10—C111.407 (3)
Ru1—N32.0815 (18)C10—C151.430 (3)
Ru1—C102.169 (2)C11—H110.9500
Ru1—C112.161 (2)C11—C121.430 (4)
Ru1—C122.227 (2)C12—C131.399 (3)
Ru1—C132.191 (2)C12—C161.506 (3)
Ru1—C142.191 (2)C13—H130.9500
Ru1—C152.237 (2)C13—C141.431 (3)
P1—F11.5371 (17)C14—H140.9500
P1—F2A1.4877 (16)C14—C151.403 (3)
P1—F2B1.4940 (17)C15—C171.521 (3)
P1—O11.4840 (16)C16—H16A0.9800
N1—C11.342 (3)C16—H16B0.9800
N1—C51.350 (3)C16—H16C0.9800
N2—N31.353 (3)C17—H171.0000
N2—C61.459 (3)C17—C181.522 (4)
N2—C91.347 (3)C17—C191.542 (3)
N3—C71.335 (3)C18—H18A0.9800
C1—H10.9500C18—H18B0.9800
C1—C21.376 (3)C18—H18C0.9800
C2—H20.9500C19—H19A0.9800
C2—C31.377 (4)C19—H19B0.9800
C3—H30.9500C19—H19C0.9800
C3—C41.379 (4)P2—F31.5930 (19)
C4—H40.9500P2—F41.6064 (19)
C4—C51.383 (3)P2—F51.587 (2)
C5—C61.504 (3)P2—F61.5931 (18)
C6—H6A0.9900P2—F71.5875 (19)
C6—H6B0.9900P2—F81.601 (2)
C7—H70.9500F9—B11.4030
C7—C81.398 (3)F11—B11.4016
C8—H80.9500F12—B11.4027
C8—C91.374 (4)F10—B11.4017
C9—H90.9500
O1—Ru1—N180.54 (6)Ru1—C10—H10128.3
O1—Ru1—C10160.62 (8)C11—C10—Ru170.70 (13)
O1—Ru1—C11154.19 (8)C11—C10—H10119.6
O1—Ru1—C12117.04 (8)C11—C10—C15120.8 (2)
O1—Ru1—C1394.04 (8)C15—C10—Ru173.66 (13)
O1—Ru1—C1496.69 (7)C15—C10—H10119.6
O1—Ru1—C15122.92 (7)Ru1—C11—H11128.1
N1—Ru1—C10118.41 (8)C10—C11—Ru171.39 (13)
N1—Ru1—C1192.95 (8)C10—C11—H11119.2
N1—Ru1—C1293.76 (8)C10—C11—C12121.6 (2)
N1—Ru1—C13119.88 (8)C12—C11—Ru173.51 (13)
N1—Ru1—C14157.89 (8)C12—C11—H11119.2
N1—Ru1—C15155.93 (8)C11—C12—Ru168.49 (13)
N3—Ru1—O182.48 (7)C11—C12—C16120.8 (2)
N3—Ru1—N183.82 (7)C13—C12—Ru170.17 (13)
N3—Ru1—C1094.91 (8)C13—C12—C11117.4 (2)
N3—Ru1—C11121.88 (9)C13—C12—C16121.7 (2)
N3—Ru1—C12159.75 (9)C16—C12—Ru1130.00 (16)
N3—Ru1—C13155.30 (8)Ru1—C13—H13129.1
N3—Ru1—C14117.75 (8)C12—C13—Ru172.92 (13)
N3—Ru1—C1593.41 (8)C12—C13—H13119.5
C10—Ru1—C1268.52 (9)C12—C13—C14121.1 (2)
C10—Ru1—C1380.29 (9)C14—C13—Ru170.93 (12)
C10—Ru1—C1467.44 (9)C14—C13—H13119.5
C10—Ru1—C1537.84 (8)Ru1—C14—H14128.9
C11—Ru1—C1037.91 (9)C13—C14—Ru170.96 (12)
C11—Ru1—C1238.00 (10)C13—C14—H14119.2
C11—Ru1—C1367.48 (9)C15—C14—Ru173.33 (13)
C11—Ru1—C1479.99 (9)C15—C14—C13121.6 (2)
C11—Ru1—C1568.21 (9)C15—C14—H14119.2
C12—Ru1—C1580.62 (9)C10—C15—Ru168.51 (12)
C13—Ru1—C1236.91 (9)C10—C15—C17122.9 (2)
C13—Ru1—C1567.91 (9)C14—C15—Ru169.73 (12)
C14—Ru1—C1267.79 (9)C14—C15—C10117.3 (2)
C14—Ru1—C1338.11 (9)C14—C15—C17119.7 (2)
C14—Ru1—C1536.93 (8)C17—C15—Ru1132.83 (16)
F2A—P1—F1105.08 (10)C12—C16—H16A109.5
F2B—P1—F1103.58 (11)C12—C16—H16B109.5
O1—P1—F1107.56 (10)C12—C16—H16C109.5
O1—P1—F2A113.47 (10)H16A—C16—H16B109.5
O1—P1—F2B114.44 (10)H16A—C16—H16C109.5
P1—O1—Ru1134.00 (10)H16B—C16—H16C109.5
C1—N1—Ru1117.61 (15)C15—C17—H17108.2
C1—N1—C5118.34 (19)C15—C17—C18114.5 (2)
C5—N1—Ru1124.06 (15)C15—C17—C19107.1 (2)
N3—N2—C6119.81 (18)C18—C17—H17108.2
C9—N2—N3110.5 (2)C18—C17—C19110.6 (2)
C9—N2—C6129.6 (2)C19—C17—H17108.2
N2—N3—Ru1123.04 (14)C17—C18—H18A109.5
C7—N3—Ru1130.26 (16)C17—C18—H18B109.5
C7—N3—N2106.55 (18)C17—C18—H18C109.5
N1—C1—H1118.6H18A—C18—H18B109.5
N1—C1—C2122.9 (2)H18A—C18—H18C109.5
C2—C1—H1118.6H18B—C18—H18C109.5
C1—C2—H2120.6C17—C19—H19A109.5
C1—C2—C3118.7 (2)C17—C19—H19B109.5
C3—C2—H2120.6C17—C19—H19C109.5
C2—C3—H3120.5H19A—C19—H19B109.5
C2—C3—C4119.0 (2)H19A—C19—H19C109.5
C4—C3—H3120.5H19B—C19—H19C109.5
C3—C4—H4120.2F3—P2—F489.64 (11)
C3—C4—C5119.6 (2)F3—P2—F690.47 (12)
C5—C4—H4120.2F3—P2—F8178.95 (14)
N1—C5—C4121.4 (2)F5—P2—F390.58 (13)
N1—C5—C6117.16 (19)F5—P2—F490.19 (13)
C4—C5—C6121.4 (2)F5—P2—F691.13 (11)
N2—C6—C5111.60 (18)F5—P2—F7179.19 (12)
N2—C6—H6A109.3F5—P2—F890.18 (13)
N2—C6—H6B109.3F6—P2—F4178.68 (13)
C5—C6—H6A109.3F6—P2—F890.23 (11)
C5—C6—H6B109.3F7—P2—F389.10 (12)
H6A—C6—H6B108.0F7—P2—F490.55 (13)
N3—C7—H7125.0F7—P2—F688.13 (12)
N3—C7—C8109.9 (2)F7—P2—F890.14 (12)
C8—C7—H7125.0F8—P2—F489.65 (12)
C7—C8—H8127.3F11—B1—F9109.5
C9—C8—C7105.4 (2)F11—B1—F12109.5
C9—C8—H8127.3F11—B1—F10109.5
N2—C9—C8107.6 (2)F12—B1—F9109.4
N2—C9—H9126.2F10—B1—F9109.5
C8—C9—H9126.2F10—B1—F12109.6
Ru1—N1—C1—C2177.60 (18)C4—C5—C6—N2124.4 (2)
Ru1—N1—C5—C4179.49 (16)C5—N1—C1—C22.8 (3)
Ru1—N1—C5—C62.2 (3)C6—N2—N3—Ru12.3 (3)
Ru1—N3—C7—C8175.32 (17)C6—N2—N3—C7178.3 (2)
Ru1—C10—C11—C1256.06 (19)C6—N2—C9—C8177.8 (2)
Ru1—C10—C15—C1451.48 (18)C7—C8—C9—N20.4 (3)
Ru1—C10—C15—C17128.0 (2)C9—N2—N3—Ru1176.00 (15)
Ru1—C11—C12—C1352.02 (18)C9—N2—N3—C70.0 (3)
Ru1—C11—C12—C16124.7 (2)C9—N2—C6—C5119.8 (3)
Ru1—C12—C13—C1454.26 (18)C10—C11—C12—Ru155.08 (19)
Ru1—C13—C14—C1555.35 (19)C10—C11—C12—C133.1 (3)
Ru1—C14—C15—C1050.90 (18)C10—C11—C12—C16179.8 (2)
Ru1—C14—C15—C17128.6 (2)C10—C15—C17—C1818.5 (3)
Ru1—C15—C17—C1871.8 (3)C10—C15—C17—C19104.5 (3)
Ru1—C15—C17—C19165.26 (18)C11—C10—C15—Ru154.82 (19)
F1—P1—O1—Ru165.24 (16)C11—C10—C15—C143.3 (3)
F2A—P1—O1—Ru1178.98 (12)C11—C10—C15—C17177.2 (2)
F2B—P1—O1—Ru149.24 (17)C11—C12—C13—Ru151.22 (18)
N1—C1—C2—C33.3 (4)C11—C12—C13—C143.0 (3)
N1—C5—C6—N257.3 (3)C12—C13—C14—Ru155.18 (19)
N2—N3—C7—C80.3 (3)C12—C13—C14—C150.2 (3)
N3—N2—C6—C558.2 (3)C13—C14—C15—Ru154.27 (18)
N3—N2—C9—C80.3 (3)C13—C14—C15—C103.4 (3)
N3—C7—C8—C90.4 (3)C13—C14—C15—C17177.1 (2)
C1—N1—C5—C40.0 (3)C14—C15—C17—C18160.9 (2)
C1—N1—C5—C6178.27 (19)C14—C15—C17—C1976.1 (3)
C1—C2—C3—C40.9 (4)C15—C10—C11—Ru156.20 (19)
C2—C3—C4—C51.8 (3)C15—C10—C11—C120.1 (3)
C3—C4—C5—N12.3 (3)C16—C12—C13—Ru1125.5 (2)
C3—C4—C5—C6175.9 (2)C16—C12—C13—C14179.7 (2)

Experimental details

Crystal data
Chemical formula[Ru(C10H14)(C9H9N3)(PO2F2)](PF6)0.86(BF4)0.14
Mr631.92
Crystal system, space groupMonoclinic, P21/n
Temperature (K)100
a, b, c (Å)15.6531 (17), 8.7619 (9), 17.4895 (18)
β (°) 106.316 (5)
V3)2302.1 (4)
Z4
Radiation typeCu Kα
µ (mm1)7.54
Crystal size (mm)0.16 × 0.10 × 0.06
Data collection
DiffractometerBruker SMART APEXII area-detector
diffractometer
Absorption correctionAnalytical
(SADABS; Bruker, 2012)
Tmin, Tmax0.429, 0.735
No. of measured, independent and
observed [I > 2σ(I)] reflections
32407, 4479, 4065
Rint0.039
(sin θ/λ)max1)0.618
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.057, 1.02
No. of reflections4479
No. of parameters327
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.47, 0.33

Computer programs: APEX2 (Bruker, 2013), SAINT-Plus (Bruker, 2013), SHELXTL (Sheldrick, 2013), OLEX2 (Dolomanov et al., 2009).

 

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds