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In the title compound, [Re(C9H9N)(C14H12N2)(CO)3]PF6, the complex cation adopts a distorted octahedral geometry, with the Re atom at the center and a facial disposition of the three carbonyl ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805004678/fl6138sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805004678/fl6138Isup2.hkl
Contains datablock I

CCDC reference: 269555

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.021
  • wR factor = 0.051
  • Data-to-parameter ratio = 12.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............ 24.97 Deg.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.91 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for O3 - C3 .. 6.65 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Re1 - C2 .. 6.20 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Re1 - C3 .. 8.87 su
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

fac-Tricarbonyl(2,9-dimethyl-1,10-phenanthroline)(2,6-dimethylphenyl isocyanide)rhenium(I) hexafluorophosphate top
Crystal data top
[Re(C9H9N)(C14H12N2)(CO)3]PF6F(000) = 1464
Mr = 754.63Dx = 1.877 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 24 reflections
a = 14.510 (4) Åθ = 1–25°
b = 11.223 (4) ŵ = 4.69 mm1
c = 17.887 (5) ÅT = 100 K
β = 113.53 (2)°Prism, yellow
V = 2670.6 (14) Å30.5 × 0.3 × 0.3 mm
Z = 4
Data collection top
Enraf Nonius CAD4
diffractometer
Rint = 0.026
non–profiled ω/2θ scansθmax = 25.0°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements)
(refined from ΔF; Walker & Stuart, 1983)
h = 017
Tmin = 0.198, Tmax = 0.245k = 013
4871 measured reflectionsl = 2119
4682 independent reflections3 standard reflections every 60 min
3991 reflections with I > 2σ(I) intensity decay: none
Refinement top
Refinement on F2396 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.021 w = 1/[σ2(Fo2) + (0.0226P)2 + 4.1906P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.051(Δ/σ)max = 0.002
S = 1.09Δρmax = 0.57 e Å3
4682 reflectionsΔρmin = 0.60 e Å3
365 parameters
Special details top

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*/Ueq
Re10.123071 (10)0.894497 (12)0.291446 (8)0.00968 (5)
P10.65276 (7)0.06428 (9)0.16381 (6)0.0156 (2)
F30.73794 (18)0.0364 (2)0.19099 (14)0.0291 (6)
F50.73090 (17)0.1576 (2)0.22299 (14)0.0259 (5)
N10.1352 (2)0.8233 (3)0.40936 (17)0.0107 (6)
C120.2961 (3)1.2494 (4)0.4683 (3)0.0308 (10)
H12A0.24411.24880.41420.046*
H12B0.29951.32690.4920.046*
H12C0.28141.19090.50110.046*
F20.57434 (18)0.0283 (2)0.10403 (14)0.0282 (6)
F10.68484 (16)0.1031 (2)0.09122 (13)0.0217 (5)
N20.0591 (2)1.0354 (3)0.34206 (17)0.0115 (6)
C80.5786 (3)1.1632 (4)0.4574 (2)0.0222 (9)
H80.64071.14480.45650.027*
F40.61992 (19)0.0254 (2)0.23578 (14)0.0301 (6)
C110.3956 (3)1.2207 (3)0.4643 (2)0.0178 (8)
F60.56676 (15)0.1647 (2)0.13602 (14)0.0220 (5)
C100.4793 (3)1.2925 (4)0.5008 (2)0.0217 (9)
H100.47411.36140.52780.026*
C150.0340 (3)1.1452 (4)0.2158 (2)0.0230 (9)
H15A0.01571.17490.19780.034*
H15B0.09021.19890.1990.034*
H15C0.05631.06810.19230.034*
O30.1147 (2)1.0077 (2)0.13274 (15)0.0200 (6)
O10.0857 (2)0.7758 (3)0.19786 (17)0.0266 (7)
C140.0931 (2)1.0246 (3)0.4254 (2)0.0116 (7)
N30.3247 (2)1.0444 (3)0.38721 (18)0.0147 (7)
C60.5047 (3)0.9827 (4)0.3695 (3)0.0270 (10)
H6A0.46160.99440.31320.041*
H6B0.4840.91260.38940.041*
H6C0.57280.97320.3750.041*
C130.1322 (2)0.9121 (3)0.4608 (2)0.0106 (7)
C30.1158 (3)0.9684 (3)0.1926 (2)0.0161 (8)
O20.2505 (2)0.7087 (2)0.25044 (18)0.0244 (6)
C240.1861 (3)0.6898 (3)0.5226 (2)0.0151 (8)
H240.20180.61230.54190.018*
C40.2542 (3)0.9870 (3)0.3544 (2)0.0122 (7)
C230.1910 (3)0.7788 (3)0.5753 (2)0.0148 (8)
H230.21320.76340.63090.018*
C190.0849 (2)1.1169 (3)0.4752 (2)0.0137 (7)
C70.4977 (3)1.0891 (3)0.4182 (2)0.0175 (8)
C220.1622 (2)0.8947 (3)0.5451 (2)0.0130 (7)
C160.0107 (3)1.1352 (3)0.3069 (2)0.0154 (8)
C200.1222 (3)1.0989 (4)0.5618 (2)0.0170 (8)
H200.12081.16150.59530.02*
C20.1992 (3)0.7738 (3)0.2652 (2)0.0164 (8)
C250.1575 (2)0.7132 (3)0.4388 (2)0.0120 (7)
C260.1501 (3)0.6103 (3)0.3829 (2)0.0173 (8)
H26A0.09380.62210.3320.026*
H26B0.14110.53770.40760.026*
H26C0.21060.60540.37350.026*
C170.0003 (3)1.2308 (3)0.3541 (2)0.0180 (8)
H170.03361.29930.32840.022*
C10.0101 (3)0.8170 (3)0.2325 (2)0.0168 (8)
C210.1590 (3)0.9929 (3)0.5948 (2)0.0163 (8)
H210.18280.98310.6510.02*
C180.0396 (3)1.2238 (3)0.4373 (2)0.0177 (8)
H180.03641.28890.46840.021*
C90.5692 (3)1.2639 (4)0.4979 (2)0.0234 (9)
H90.62461.31290.52350.028*
C50.4075 (3)1.1197 (3)0.4241 (2)0.0147 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.00960 (7)0.00964 (7)0.00964 (7)0.00029 (6)0.00369 (5)0.00098 (6)
P10.0205 (5)0.0131 (5)0.0147 (5)0.0011 (4)0.0086 (4)0.0006 (4)
F30.0390 (14)0.0240 (14)0.0233 (13)0.0153 (11)0.0116 (11)0.0050 (10)
F50.0239 (12)0.0289 (13)0.0228 (12)0.0040 (10)0.0073 (10)0.0105 (10)
N10.0063 (13)0.0126 (16)0.0134 (15)0.0017 (12)0.0040 (12)0.0017 (13)
C120.024 (2)0.033 (3)0.039 (3)0.0040 (19)0.017 (2)0.016 (2)
F20.0348 (14)0.0182 (13)0.0307 (13)0.0093 (11)0.0119 (11)0.0048 (11)
F10.0251 (12)0.0259 (12)0.0179 (11)0.0009 (11)0.0126 (9)0.0031 (10)
N20.0105 (14)0.0118 (16)0.0127 (15)0.0002 (12)0.0051 (12)0.0001 (12)
C80.0133 (18)0.030 (2)0.025 (2)0.0002 (17)0.0101 (17)0.0071 (18)
F40.0465 (15)0.0281 (14)0.0260 (13)0.0032 (12)0.0253 (12)0.0083 (11)
C110.0175 (19)0.018 (2)0.0174 (19)0.0043 (16)0.0067 (16)0.0012 (16)
F60.0180 (11)0.0183 (12)0.0321 (13)0.0042 (10)0.0123 (10)0.0051 (10)
C100.020 (2)0.021 (2)0.022 (2)0.0062 (17)0.0065 (17)0.0009 (17)
C150.024 (2)0.022 (2)0.020 (2)0.0090 (17)0.0062 (17)0.0048 (17)
O30.0255 (15)0.0222 (15)0.0138 (14)0.0008 (12)0.0094 (11)0.0028 (12)
O10.0181 (15)0.0377 (18)0.0200 (15)0.0111 (14)0.0036 (12)0.0042 (13)
C140.0036 (15)0.0159 (19)0.0156 (18)0.0017 (14)0.0041 (14)0.0005 (15)
N30.0140 (16)0.0163 (17)0.0131 (15)0.0019 (14)0.0047 (13)0.0023 (13)
C60.028 (2)0.029 (2)0.030 (2)0.0017 (19)0.0171 (19)0.0005 (19)
C130.0051 (15)0.0128 (19)0.0147 (17)0.0011 (14)0.0050 (13)0.0022 (14)
C30.0125 (18)0.0111 (19)0.025 (2)0.0014 (14)0.0073 (16)0.0059 (16)
O20.0294 (15)0.0224 (16)0.0246 (15)0.0088 (13)0.0140 (13)0.0047 (13)
C240.0120 (17)0.0145 (18)0.021 (2)0.0015 (15)0.0092 (15)0.0051 (16)
C40.0140 (18)0.0123 (18)0.0120 (18)0.0028 (16)0.0070 (15)0.0006 (15)
C230.0093 (17)0.023 (2)0.0145 (19)0.0003 (15)0.0071 (15)0.0056 (16)
C190.0081 (16)0.0158 (19)0.0197 (19)0.0050 (15)0.0082 (14)0.0057 (16)
C70.0165 (18)0.021 (2)0.0160 (19)0.0003 (16)0.0076 (15)0.0078 (16)
C220.0073 (15)0.0183 (18)0.0157 (18)0.0001 (16)0.0069 (14)0.0016 (16)
C160.0128 (18)0.0136 (19)0.020 (2)0.0006 (14)0.0068 (16)0.0025 (15)
C200.0133 (17)0.021 (2)0.0198 (19)0.0022 (16)0.0099 (15)0.0083 (17)
C20.021 (2)0.0131 (19)0.0147 (19)0.0053 (16)0.0072 (16)0.0009 (15)
C250.0069 (16)0.0132 (19)0.0174 (19)0.0002 (14)0.0064 (14)0.0030 (15)
C260.0199 (19)0.0101 (18)0.023 (2)0.0006 (16)0.0093 (16)0.0007 (16)
C170.0145 (18)0.016 (2)0.024 (2)0.0028 (16)0.0086 (16)0.0014 (16)
C10.020 (2)0.0150 (19)0.0157 (19)0.0002 (17)0.0078 (16)0.0006 (16)
C210.0138 (18)0.024 (2)0.0142 (18)0.0035 (16)0.0084 (15)0.0032 (16)
C180.0137 (18)0.016 (2)0.026 (2)0.0001 (15)0.0109 (17)0.0044 (16)
C90.018 (2)0.024 (2)0.023 (2)0.0091 (17)0.0025 (17)0.0025 (18)
C50.0143 (17)0.017 (2)0.0104 (17)0.0034 (15)0.0024 (14)0.0046 (15)
Geometric parameters (Å, º) top
Re1—C31.918 (4)O1—C11.122 (5)
Re1—C21.920 (4)C14—C191.401 (5)
Re1—C11.994 (4)C14—C131.426 (5)
Re1—C42.063 (4)N3—C41.152 (5)
Re1—N12.196 (3)N3—C51.401 (5)
Re1—N22.203 (3)C6—C71.504 (6)
P1—F21.595 (2)C6—H6A0.96
P1—F51.595 (2)C6—H6B0.96
P1—F31.600 (2)C6—H6C0.96
P1—F41.601 (2)C13—C221.406 (5)
P1—F11.605 (2)O2—C21.147 (5)
P1—F61.606 (2)C24—C231.356 (5)
N1—C251.332 (5)C24—C251.411 (5)
N1—C131.368 (4)C24—H240.93
C12—C111.509 (5)C23—C221.407 (5)
C12—H12A0.96C23—H230.93
C12—H12B0.96C19—C181.405 (5)
C12—H12C0.96C19—C201.435 (5)
N2—C161.338 (5)C7—C51.397 (5)
N2—C141.376 (4)C22—C211.428 (5)
C8—C91.379 (6)C16—C171.410 (5)
C8—C71.380 (6)C20—C211.341 (6)
C8—H80.93C20—H200.93
C11—C101.384 (5)C25—C261.503 (5)
C11—C51.389 (5)C26—H26A0.96
C10—C91.364 (6)C26—H26B0.96
C10—H100.93C26—H26C0.96
C15—C161.498 (5)C17—C181.367 (5)
C15—H15A0.96C17—H170.93
C15—H15B0.96C21—H210.93
C15—H15C0.96C18—H180.93
O3—C31.151 (5)C9—H90.93
C3—Re1—C284.56 (15)C4—N3—C5176.7 (4)
C3—Re1—C190.93 (15)C7—C6—H6A109.5
C2—Re1—C195.39 (16)C7—C6—H6B109.5
C3—Re1—C489.12 (15)H6A—C6—H6B109.5
C2—Re1—C489.59 (15)C7—C6—H6C109.5
C1—Re1—C4175.01 (14)H6A—C6—H6C109.5
C3—Re1—N1175.53 (13)H6B—C6—H6C109.5
C2—Re1—N198.32 (13)N1—C13—C22122.7 (3)
C1—Re1—N192.21 (13)N1—C13—C14117.5 (3)
C4—Re1—N187.48 (12)C22—C13—C14119.7 (3)
C3—Re1—N2101.03 (13)O3—C3—Re1176.2 (3)
C2—Re1—N2169.88 (13)C23—C24—C25120.9 (4)
C1—Re1—N292.98 (13)C23—C24—H24119.6
C4—Re1—N282.12 (12)C25—C24—H24119.6
N1—Re1—N275.63 (11)N3—C4—Re1176.1 (3)
F2—P1—F5179.51 (14)C24—C23—C22119.2 (3)
F2—P1—F390.10 (14)C24—C23—H23120.4
F5—P1—F390.23 (14)C22—C23—H23120.4
F2—P1—F490.00 (14)C14—C19—C18117.8 (3)
F5—P1—F490.36 (14)C14—C19—C20119.3 (3)
F3—P1—F490.29 (13)C18—C19—C20122.9 (3)
F2—P1—F189.65 (13)C8—C7—C5116.4 (4)
F5—P1—F189.98 (13)C8—C7—C6122.2 (4)
F3—P1—F189.95 (13)C5—C7—C6121.3 (3)
F4—P1—F1179.58 (15)C13—C22—C23117.2 (3)
F2—P1—F689.50 (13)C13—C22—C21119.2 (3)
F5—P1—F690.16 (13)C23—C22—C21123.6 (3)
F3—P1—F6179.60 (16)N2—C16—C17121.1 (3)
F4—P1—F689.79 (13)N2—C16—C15119.5 (3)
F1—P1—F689.97 (12)C17—C16—C15119.4 (3)
C25—N1—C13118.5 (3)C21—C20—C19120.8 (3)
C25—N1—Re1129.1 (2)C21—C20—H20119.6
C13—N1—Re1111.7 (2)C19—C20—H20119.6
C11—C12—H12A109.5O2—C2—Re1174.4 (3)
C11—C12—H12B109.5N1—C25—C24121.0 (3)
H12A—C12—H12B109.5N1—C25—C26120.5 (3)
C11—C12—H12C109.5C24—C25—C26118.4 (3)
H12A—C12—H12C109.5C25—C26—H26A109.5
H12B—C12—H12C109.5C25—C26—H26B109.5
C16—N2—C14118.5 (3)H26A—C26—H26B109.5
C16—N2—Re1129.5 (2)C25—C26—H26C109.5
C14—N2—Re1110.8 (2)H26A—C26—H26C109.5
C9—C8—C7121.2 (4)H26B—C26—H26C109.5
C9—C8—H8119.4C18—C17—C16120.7 (4)
C7—C8—H8119.4C18—C17—H17119.6
C10—C11—C5116.9 (4)C16—C17—H17119.6
C10—C11—C12121.9 (4)O1—C1—Re1178.1 (4)
C5—C11—C12121.2 (3)C20—C21—C22121.1 (3)
C9—C10—C11121.1 (4)C20—C21—H21119.4
C9—C10—H10119.5C22—C21—H21119.4
C11—C10—H10119.5C17—C18—C19119.1 (3)
C16—C15—H15A109.5C17—C18—H18120.5
C16—C15—H15B109.5C19—C18—H18120.5
H15A—C15—H15B109.5C10—C9—C8120.7 (4)
C16—C15—H15C109.5C10—C9—H9119.7
H15A—C15—H15C109.5C8—C9—H9119.7
H15B—C15—H15C109.5C11—C5—C7123.6 (3)
N2—C14—C19122.6 (3)C11—C5—N3118.4 (3)
N2—C14—C13117.7 (3)C7—C5—N3118.0 (3)
C19—C14—C13119.5 (3)
 

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