Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807048404/lh2500sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807048404/lh2500Isup2.hkl |
CCDC reference: 667161
Key indicators
- Single-crystal X-ray study
- T = 297 K
- Mean (C-C) = 0.005 Å
- Disorder in solvent or counterion
- R factor = 0.045
- wR factor = 0.124
- Data-to-parameter ratio = 14.5
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C6 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C9 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 38.00 Perc. PLAT480_ALERT_4_C Long H...A H-Bond Reported H3 .. F1 .. 2.78 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.26 Ratio
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 21
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
The structure of a related compound containing the same cation with a nitrate anion has already been determined (Brasse et al., 2000)
The title compound was obtained by anion exchange of 1,1'-Bis(diphenylphosphino)cobaltocenium chloride with 1.2 equiv of sodium tetrafluoroborate. Crystals appropriate for data collection were obtained by slow diffusion of hexane into a solution of the the title compound in dichloromethane at 293 K.
F1, F3 and F4 are disordered equally over two sites imposed by the crystallographic twofold symmetry. All H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with C—H = 0.93 Å; with Uiso(H) = 1.2Ueq(C).
The molecular structure of the title complex consists of a [(η5-Ph2PC5H4)2Co]+ cation and a BF4- anion (Fig.1), in which the bond length and angles of the cation are similar to those in the cation of the complex 1,1'-Bis(diphenylphosphino)cobaltocenium nitrate (Brasse et al., 2000). The two Ph2P– substituents are trans to each other with respect to the CoIII metal center, and the two substituted cyclopentadienyl rings are exactly staggered with a dihedral angle of 4.62 (18)° between them. The distance between the atom Co1 and the center of the unique cyclopentadienyl ring is 1.6380 (13) Å. In the crystal structutre, molecules are linked by C—H···F hydrogen bonds, as shown in Fig.2.
The structure of a related compound containing the same cation with a nitrate anion has already been determined (Brasse et al., 2000)
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL (Sheldrick, 2001); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL (Sheldrick, 2001).
[Co(C17H14P)2]BF4 | F(000) = 1320 |
Mr = 644.24 | Dx = 1.405 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 5457 reflections |
a = 10.3357 (11) Å | θ = 2.5–27.7° |
b = 13.1659 (14) Å | µ = 0.72 mm−1 |
c = 22.894 (3) Å | T = 297 K |
β = 102.085 (2)° | Block, yellow |
V = 3046.3 (6) Å3 | 0.20 × 0.15 × 0.10 mm |
Z = 4 |
Bruker SMART CCD diffractometer | 2970 independent reflections |
Radiation source: fine-focus sealed tube | 2655 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
φ and ω scans | θmax = 26.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | h = −12→12 |
Tmin = 0.870, Tmax = 0.932 | k = −14→16 |
10252 measured reflections | l = −28→28 |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.125 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0776P)2 + 1.0622P] where P = (Fo2 + 2Fc2)/3 |
2970 reflections | (Δ/σ)max < 0.001 |
205 parameters | Δρmax = 0.49 e Å−3 |
21 restraints | Δρmin = −0.36 e Å−3 |
[Co(C17H14P)2]BF4 | V = 3046.3 (6) Å3 |
Mr = 644.24 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 10.3357 (11) Å | µ = 0.72 mm−1 |
b = 13.1659 (14) Å | T = 297 K |
c = 22.894 (3) Å | 0.20 × 0.15 × 0.10 mm |
β = 102.085 (2)° |
Bruker SMART CCD diffractometer | 2970 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | 2655 reflections with I > 2σ(I) |
Tmin = 0.870, Tmax = 0.932 | Rint = 0.025 |
10252 measured reflections |
R[F2 > 2σ(F2)] = 0.045 | 21 restraints |
wR(F2) = 0.125 | H-atom parameters constrained |
S = 1.08 | Δρmax = 0.49 e Å−3 |
2970 reflections | Δρmin = −0.36 e Å−3 |
205 parameters |
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. 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) | |
Co1 | 1.0000 | 0.60723 (4) | 0.7500 | 0.04454 (19) | |
C1 | 0.8097 (3) | 0.5865 (3) | 0.75876 (13) | 0.0610 (7) | |
H1 | 0.7821 | 0.5677 | 0.7934 | 0.073* | |
C2 | 0.8716 (3) | 0.6816 (2) | 0.68594 (12) | 0.0560 (6) | |
H2 | 0.8923 | 0.7370 | 0.6644 | 0.067* | |
C3 | 0.8290 (3) | 0.6865 (3) | 0.74086 (12) | 0.0625 (8) | |
H3 | 0.8161 | 0.7453 | 0.7614 | 0.075* | |
C4 | 0.8773 (2) | 0.5777 (2) | 0.66922 (11) | 0.0512 (6) | |
C5 | 0.8394 (3) | 0.5192 (2) | 0.71517 (12) | 0.0547 (6) | |
H5 | 0.8350 | 0.4487 | 0.7163 | 0.066* | |
C6 | 0.7918 (3) | 0.5732 (2) | 0.54478 (12) | 0.0550 (6) | |
C7 | 0.8100 (4) | 0.5751 (4) | 0.48680 (15) | 0.0909 (12) | |
H7 | 0.8920 | 0.5583 | 0.4789 | 0.109* | |
C8 | 0.7070 (5) | 0.6020 (4) | 0.44030 (16) | 0.1003 (15) | |
H8 | 0.7202 | 0.6005 | 0.4014 | 0.120* | |
C9 | 0.5890 (4) | 0.6299 (3) | 0.45003 (16) | 0.0822 (10) | |
H9 | 0.5215 | 0.6495 | 0.4184 | 0.099* | |
C10 | 0.5690 (4) | 0.6292 (4) | 0.50737 (16) | 0.0979 (13) | |
H10 | 0.4872 | 0.6479 | 0.5147 | 0.117* | |
C11 | 0.6702 (3) | 0.6007 (3) | 0.55444 (14) | 0.0847 (12) | |
H11 | 0.6553 | 0.6003 | 0.5931 | 0.102* | |
C12 | 0.9059 (3) | 0.3975 (2) | 0.60954 (12) | 0.0565 (7) | |
C13 | 1.0036 (3) | 0.3419 (3) | 0.64705 (15) | 0.0732 (9) | |
H13 | 1.0812 | 0.3741 | 0.6660 | 0.088* | |
C14 | 0.9876 (4) | 0.2396 (3) | 0.65664 (17) | 0.0830 (10) | |
H14 | 1.0526 | 0.2042 | 0.6831 | 0.100* | |
C15 | 0.8761 (4) | 0.1899 (3) | 0.62734 (17) | 0.0826 (10) | |
H15 | 0.8656 | 0.1209 | 0.6336 | 0.099* | |
C16 | 0.7805 (4) | 0.2427 (3) | 0.58887 (19) | 0.0899 (11) | |
H16 | 0.7054 | 0.2091 | 0.5684 | 0.108* | |
C17 | 0.7948 (3) | 0.3462 (3) | 0.58021 (16) | 0.0761 (9) | |
H17 | 0.7286 | 0.3813 | 0.5543 | 0.091* | |
F2 | 0.5000 | 0.5484 (2) | 0.7500 | 0.1305 (15) | |
F1 | 0.5209 (12) | 0.4095 (5) | 0.6985 (2) | 0.185 (6) | 0.50 |
F3 | 0.6174 (8) | 0.4195 (4) | 0.7881 (2) | 0.107 (2) | 0.50 |
P1 | 0.93254 (7) | 0.53398 (6) | 0.60262 (3) | 0.0569 (2) | |
B1 | 0.5000 | 0.4466 (4) | 0.7500 | 0.094 (2) | |
F4 | 0.4042 (9) | 0.4033 (5) | 0.7672 (8) | 0.317 (12) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0398 (3) | 0.0519 (3) | 0.0405 (3) | 0.000 | 0.00524 (19) | 0.000 |
C1 | 0.0407 (13) | 0.090 (2) | 0.0538 (15) | −0.0025 (13) | 0.0125 (11) | −0.0118 (14) |
C2 | 0.0492 (14) | 0.0613 (16) | 0.0508 (13) | 0.0057 (12) | −0.0052 (11) | 0.0007 (12) |
C3 | 0.0472 (14) | 0.076 (2) | 0.0590 (15) | 0.0143 (13) | −0.0010 (12) | −0.0162 (14) |
C4 | 0.0425 (13) | 0.0651 (16) | 0.0431 (12) | −0.0036 (11) | 0.0027 (10) | −0.0061 (11) |
C5 | 0.0462 (14) | 0.0655 (17) | 0.0526 (14) | −0.0099 (12) | 0.0112 (11) | −0.0079 (12) |
C6 | 0.0581 (16) | 0.0617 (16) | 0.0456 (13) | −0.0003 (13) | 0.0119 (11) | 0.0014 (12) |
C7 | 0.095 (3) | 0.127 (3) | 0.0565 (18) | 0.042 (2) | 0.0282 (18) | 0.0230 (19) |
C8 | 0.111 (3) | 0.143 (4) | 0.0494 (17) | 0.035 (3) | 0.0231 (19) | 0.033 (2) |
C9 | 0.081 (2) | 0.100 (3) | 0.0605 (18) | 0.007 (2) | 0.0026 (16) | 0.0174 (18) |
C10 | 0.061 (2) | 0.164 (4) | 0.064 (2) | 0.016 (2) | 0.0030 (16) | −0.006 (2) |
C11 | 0.0602 (19) | 0.147 (4) | 0.0454 (15) | 0.002 (2) | 0.0074 (13) | −0.0117 (17) |
C12 | 0.0556 (16) | 0.0687 (17) | 0.0460 (13) | 0.0071 (13) | 0.0122 (11) | −0.0065 (11) |
C13 | 0.0581 (18) | 0.082 (2) | 0.0757 (19) | 0.0142 (16) | 0.0054 (15) | −0.0075 (17) |
C14 | 0.076 (2) | 0.086 (2) | 0.086 (2) | 0.025 (2) | 0.0140 (18) | 0.0068 (19) |
C15 | 0.101 (3) | 0.068 (2) | 0.085 (2) | 0.0096 (19) | 0.033 (2) | 0.0035 (18) |
C16 | 0.086 (3) | 0.081 (2) | 0.096 (3) | −0.014 (2) | 0.004 (2) | −0.004 (2) |
C17 | 0.072 (2) | 0.074 (2) | 0.0731 (19) | 0.0005 (17) | −0.0060 (16) | 0.0015 (16) |
F2 | 0.108 (3) | 0.0566 (19) | 0.212 (5) | 0.000 | −0.001 (3) | 0.000 |
F1 | 0.324 (16) | 0.137 (6) | 0.061 (3) | 0.028 (7) | −0.039 (5) | −0.030 (3) |
F3 | 0.142 (5) | 0.078 (3) | 0.086 (3) | 0.007 (3) | −0.008 (4) | 0.030 (3) |
P1 | 0.0520 (4) | 0.0738 (5) | 0.0455 (4) | −0.0011 (3) | 0.0112 (3) | −0.0050 (3) |
B1 | 0.084 (4) | 0.048 (3) | 0.147 (7) | 0.000 | 0.020 (4) | 0.000 |
F4 | 0.167 (9) | 0.086 (5) | 0.79 (4) | −0.038 (6) | 0.302 (17) | −0.067 (14) |
Co1—C2i | 2.014 (3) | C10—C11 | 1.387 (5) |
Co1—C2 | 2.014 (2) | C10—H10 | 0.9300 |
Co1—C3i | 2.025 (3) | C11—H11 | 0.9300 |
Co1—C3 | 2.025 (3) | C12—C17 | 1.380 (4) |
Co1—C1i | 2.037 (3) | C12—C13 | 1.390 (4) |
Co1—C1 | 2.037 (3) | C12—P1 | 1.830 (3) |
Co1—C5 | 2.044 (3) | C13—C14 | 1.380 (5) |
Co1—C5i | 2.044 (3) | C13—H13 | 0.9300 |
Co1—C4 | 2.049 (2) | C14—C15 | 1.372 (5) |
Co1—C4i | 2.049 (2) | C14—H14 | 0.9300 |
C1—C3 | 1.406 (5) | C15—C16 | 1.368 (5) |
C1—C5 | 1.415 (4) | C15—H15 | 0.9300 |
C1—H1 | 0.9300 | C16—C17 | 1.388 (6) |
C2—C3 | 1.418 (4) | C16—H16 | 0.9300 |
C2—C4 | 1.424 (4) | C17—H17 | 0.9300 |
C2—H2 | 0.9300 | F2—B1 | 1.341 (5) |
C3—H3 | 0.9300 | F1—F4ii | 0.985 (15) |
C4—C5 | 1.424 (4) | F1—B1 | 1.336 (6) |
C4—P1 | 1.829 (3) | F1—F3ii | 1.529 (11) |
C5—H5 | 0.9300 | F3—F4ii | 1.257 (17) |
C6—C11 | 1.370 (5) | F3—B1 | 1.385 (5) |
C6—C7 | 1.379 (4) | F3—F1ii | 1.529 (11) |
C6—P1 | 1.825 (3) | B1—F4ii | 1.274 (5) |
C7—C8 | 1.385 (5) | B1—F4 | 1.274 (5) |
C7—H7 | 0.9300 | B1—F1ii | 1.336 (6) |
C8—C9 | 1.336 (6) | B1—F3ii | 1.385 (5) |
C8—H8 | 0.9300 | F4—F1ii | 0.985 (14) |
C9—C10 | 1.371 (5) | F4—F3ii | 1.257 (17) |
C9—H9 | 0.9300 | ||
C2i—Co1—C2 | 121.84 (16) | C4—C5—Co1 | 69.82 (15) |
C2i—Co1—C3i | 41.10 (11) | C1—C5—H5 | 125.8 |
C2—Co1—C3i | 104.64 (12) | C4—C5—H5 | 125.8 |
C2i—Co1—C3 | 104.64 (12) | Co1—C5—H5 | 126.6 |
C2—Co1—C3 | 41.10 (11) | C11—C6—C7 | 117.7 (3) |
C3i—Co1—C3 | 118.0 (2) | C11—C6—P1 | 125.2 (2) |
C2i—Co1—C1i | 68.54 (13) | C7—C6—P1 | 117.1 (2) |
C2—Co1—C1i | 119.76 (12) | C6—C7—C8 | 120.5 (4) |
C3i—Co1—C1i | 40.49 (13) | C6—C7—H7 | 119.8 |
C3—Co1—C1i | 154.01 (14) | C8—C7—H7 | 119.8 |
C2i—Co1—C1 | 119.76 (12) | C9—C8—C7 | 121.6 (3) |
C2—Co1—C1 | 68.54 (13) | C9—C8—H8 | 119.2 |
C3i—Co1—C1 | 154.01 (14) | C7—C8—H8 | 119.2 |
C3—Co1—C1 | 40.49 (13) | C8—C9—C10 | 118.9 (3) |
C1i—Co1—C1 | 164.57 (19) | C8—C9—H9 | 120.6 |
C2i—Co1—C5 | 156.51 (11) | C10—C9—H9 | 120.6 |
C2—Co1—C5 | 68.53 (12) | C9—C10—C11 | 120.4 (4) |
C3i—Co1—C5 | 162.18 (11) | C9—C10—H10 | 119.8 |
C3—Co1—C5 | 68.41 (13) | C11—C10—H10 | 119.8 |
C1i—Co1—C5 | 127.39 (13) | C6—C11—C10 | 120.9 (3) |
C1—Co1—C5 | 40.58 (11) | C6—C11—H11 | 119.5 |
C2i—Co1—C5i | 68.53 (12) | C10—C11—H11 | 119.5 |
C2—Co1—C5i | 156.51 (11) | C17—C12—C13 | 117.7 (3) |
C3i—Co1—C5i | 68.41 (13) | C17—C12—P1 | 124.3 (2) |
C3—Co1—C5i | 162.18 (11) | C13—C12—P1 | 117.9 (2) |
C1i—Co1—C5i | 40.58 (11) | C14—C13—C12 | 121.1 (3) |
C1—Co1—C5i | 127.39 (13) | C14—C13—H13 | 119.4 |
C5—Co1—C5i | 110.94 (17) | C12—C13—H13 | 119.4 |
C2i—Co1—C4 | 159.80 (12) | C15—C14—C13 | 120.3 (3) |
C2—Co1—C4 | 41.04 (11) | C15—C14—H14 | 119.9 |
C3i—Co1—C4 | 123.55 (11) | C13—C14—H14 | 119.9 |
C3—Co1—C4 | 69.06 (11) | C16—C15—C14 | 119.4 (4) |
C1i—Co1—C4 | 108.27 (12) | C16—C15—H15 | 120.3 |
C1—Co1—C4 | 68.63 (11) | C14—C15—H15 | 120.3 |
C5—Co1—C4 | 40.71 (11) | C15—C16—C17 | 120.4 (4) |
C5i—Co1—C4 | 122.90 (12) | C15—C16—H16 | 119.8 |
C2i—Co1—C4i | 41.04 (11) | C17—C16—H16 | 119.8 |
C2—Co1—C4i | 159.80 (12) | C12—C17—C16 | 120.9 (3) |
C3i—Co1—C4i | 69.06 (11) | C12—C17—H17 | 119.5 |
C3—Co1—C4i | 123.55 (11) | C16—C17—H17 | 119.5 |
C1i—Co1—C4i | 68.63 (11) | F4ii—F1—B1 | 64.6 (6) |
C1—Co1—C4i | 108.27 (12) | F4ii—F1—F3ii | 117.3 (11) |
C5—Co1—C4i | 122.90 (12) | B1—F1—F3ii | 57.3 (4) |
C5i—Co1—C4i | 40.71 (11) | F4ii—F3—B1 | 57.4 (4) |
C4—Co1—C4i | 158.15 (17) | F4ii—F3—F1ii | 102.2 (7) |
C3—C1—C5 | 108.4 (3) | B1—F3—F1ii | 54.3 (3) |
C3—C1—Co1 | 69.32 (16) | C6—P1—C4 | 100.10 (13) |
C5—C1—Co1 | 69.99 (15) | C6—P1—C12 | 103.26 (13) |
C3—C1—H1 | 125.8 | C4—P1—C12 | 99.10 (13) |
C5—C1—H1 | 125.8 | F4ii—B1—F4 | 126.8 (7) |
Co1—C1—H1 | 126.5 | F4—B1—F1 | 112.9 (5) |
C3—C2—C4 | 108.7 (3) | F4ii—B1—F1ii | 112.9 (5) |
C3—C2—Co1 | 69.89 (15) | F1—B1—F1ii | 137.2 (8) |
C4—C2—Co1 | 70.79 (15) | F4ii—B1—F2 | 116.6 (4) |
C3—C2—H2 | 125.7 | F4—B1—F2 | 116.6 (4) |
C4—C2—H2 | 125.7 | F1—B1—F2 | 111.4 (4) |
Co1—C2—H2 | 125.2 | F1ii—B1—F2 | 111.4 (4) |
C1—C3—C2 | 107.8 (3) | F4ii—B1—F3ii | 109.0 (6) |
C1—C3—Co1 | 70.20 (16) | F4—B1—F3ii | 56.2 (7) |
C2—C3—Co1 | 69.01 (15) | F1—B1—F3ii | 68.4 (4) |
C1—C3—H3 | 126.1 | F1ii—B1—F3ii | 100.4 (4) |
C2—C3—H3 | 126.1 | F2—B1—F3ii | 104.9 (3) |
Co1—C3—H3 | 126.2 | F4ii—B1—F3 | 56.2 (7) |
C5—C4—C2 | 106.7 (2) | F4—B1—F3 | 109.0 (6) |
C5—C4—P1 | 128.9 (2) | F1—B1—F3 | 100.4 (4) |
C2—C4—P1 | 124.4 (2) | F1ii—B1—F3 | 68.4 (4) |
C5—C4—Co1 | 69.48 (14) | F2—B1—F3 | 104.9 (3) |
C2—C4—Co1 | 68.17 (13) | F3ii—B1—F3 | 150.2 (6) |
P1—C4—Co1 | 124.76 (14) | F1ii—F4—F3ii | 137.2 (8) |
C1—C5—C4 | 108.5 (3) | F1ii—F4—B1 | 71.1 (5) |
C1—C5—Co1 | 69.43 (16) | F3ii—F4—B1 | 66.3 (5) |
C2i—Co1—C1—C3 | 77.22 (19) | C3—C1—C5—C4 | −0.2 (3) |
C2—Co1—C1—C3 | −38.13 (16) | Co1—C1—C5—C4 | −59.09 (18) |
C3i—Co1—C1—C3 | 41.1 (4) | C3—C1—C5—Co1 | 58.86 (19) |
C1i—Co1—C1—C3 | −163.60 (16) | C2—C4—C5—C1 | 0.6 (3) |
C5—Co1—C1—C3 | −119.8 (2) | P1—C4—C5—C1 | 177.5 (2) |
C5i—Co1—C1—C3 | 161.84 (16) | Co1—C4—C5—C1 | 58.85 (18) |
C4—Co1—C1—C3 | −82.37 (18) | C2—C4—C5—Co1 | −58.21 (17) |
C4i—Co1—C1—C3 | 120.65 (17) | P1—C4—C5—Co1 | 118.7 (2) |
C2i—Co1—C1—C5 | −163.02 (17) | C2i—Co1—C5—C1 | 39.5 (4) |
C2—Co1—C1—C5 | 81.62 (19) | C2—Co1—C5—C1 | −81.7 (2) |
C3i—Co1—C1—C5 | 160.9 (2) | C3i—Co1—C5—C1 | −152.0 (4) |
C3—Co1—C1—C5 | 119.8 (2) | C3—Co1—C5—C1 | −37.31 (19) |
C1i—Co1—C1—C5 | −43.85 (17) | C1i—Co1—C5—C1 | 166.59 (18) |
C5i—Co1—C1—C5 | −78.4 (3) | C5i—Co1—C5—C1 | 123.6 (2) |
C4—Co1—C1—C5 | 37.39 (18) | C4—Co1—C5—C1 | −119.9 (3) |
C4i—Co1—C1—C5 | −119.60 (18) | C4i—Co1—C5—C1 | 79.6 (2) |
C2i—Co1—C2—C3 | −74.98 (17) | C2i—Co1—C5—C4 | 159.4 (3) |
C3i—Co1—C2—C3 | −116.0 (2) | C2—Co1—C5—C4 | 38.22 (17) |
C1i—Co1—C2—C3 | −156.9 (2) | C3i—Co1—C5—C4 | −32.1 (5) |
C1—Co1—C2—C3 | 37.58 (18) | C3—Co1—C5—C4 | 82.57 (19) |
C5—Co1—C2—C3 | 81.33 (19) | C1i—Co1—C5—C4 | −73.5 (2) |
C5i—Co1—C2—C3 | 174.7 (3) | C1—Co1—C5—C4 | 119.9 (3) |
C4—Co1—C2—C3 | 119.3 (2) | C5i—Co1—C5—C4 | −116.56 (18) |
C4i—Co1—C2—C3 | −47.1 (4) | C4i—Co1—C5—C4 | −160.57 (16) |
C2i—Co1—C2—C4 | 165.76 (18) | C11—C6—C7—C8 | −1.4 (6) |
C3i—Co1—C2—C4 | 124.74 (18) | P1—C6—C7—C8 | 178.6 (4) |
C3—Co1—C2—C4 | −119.3 (2) | C6—C7—C8—C9 | 2.2 (8) |
C1i—Co1—C2—C4 | 83.86 (19) | C7—C8—C9—C10 | −1.7 (7) |
C1—Co1—C2—C4 | −81.68 (18) | C8—C9—C10—C11 | 0.5 (7) |
C5—Co1—C2—C4 | −37.93 (16) | C7—C6—C11—C10 | 0.2 (6) |
C5i—Co1—C2—C4 | 55.4 (4) | P1—C6—C11—C10 | −179.8 (3) |
C4i—Co1—C2—C4 | −166.3 (2) | C9—C10—C11—C6 | 0.3 (7) |
C5—C1—C3—C2 | −0.3 (3) | C17—C12—C13—C14 | −2.8 (5) |
Co1—C1—C3—C2 | 58.99 (18) | P1—C12—C13—C14 | 176.9 (3) |
C5—C1—C3—Co1 | −59.27 (19) | C12—C13—C14—C15 | 2.5 (5) |
C4—C2—C3—C1 | 0.7 (3) | C13—C14—C15—C16 | −0.5 (6) |
Co1—C2—C3—C1 | −59.73 (19) | C14—C15—C16—C17 | −1.1 (6) |
C4—C2—C3—Co1 | 60.42 (17) | C13—C12—C17—C16 | 1.2 (5) |
C2i—Co1—C3—C1 | −118.95 (17) | P1—C12—C17—C16 | −178.5 (3) |
C2—Co1—C3—C1 | 119.1 (2) | C15—C16—C17—C12 | 0.7 (6) |
C3i—Co1—C3—C1 | −160.95 (18) | C11—C6—P1—C4 | −15.3 (3) |
C1i—Co1—C3—C1 | 170.13 (17) | C7—C6—P1—C4 | 164.7 (3) |
C5—Co1—C3—C1 | 37.40 (16) | C11—C6—P1—C12 | 86.7 (3) |
C5i—Co1—C3—C1 | −54.0 (5) | C7—C6—P1—C12 | −93.3 (3) |
C4—Co1—C3—C1 | 81.23 (18) | C5—C4—P1—C6 | 111.3 (2) |
C4i—Co1—C3—C1 | −78.61 (19) | C2—C4—P1—C6 | −72.3 (2) |
C2i—Co1—C3—C2 | 122.0 (2) | Co1—C4—P1—C6 | −158.04 (18) |
C3i—Co1—C3—C2 | 80.00 (17) | C5—C4—P1—C12 | 6.0 (3) |
C1i—Co1—C3—C2 | 51.1 (3) | C2—C4—P1—C12 | −177.6 (2) |
C1—Co1—C3—C2 | −119.1 (2) | Co1—C4—P1—C12 | 96.62 (19) |
C5—Co1—C3—C2 | −81.65 (18) | C17—C12—P1—C6 | −5.8 (3) |
C5i—Co1—C3—C2 | −173.1 (4) | C13—C12—P1—C6 | 174.5 (2) |
C4—Co1—C3—C2 | −37.83 (17) | C17—C12—P1—C4 | 96.9 (3) |
C4i—Co1—C3—C2 | 162.34 (17) | C13—C12—P1—C4 | −82.8 (3) |
C3—C2—C4—C5 | −0.8 (3) | F3ii—F1—B1—F4ii | 155.2 (9) |
Co1—C2—C4—C5 | 59.04 (18) | F4ii—F1—B1—F4 | −119.9 (9) |
C3—C2—C4—P1 | −177.90 (19) | F3ii—F1—B1—F4 | 35.3 (7) |
Co1—C2—C4—P1 | −118.04 (19) | F4ii—F1—B1—F1ii | −73.4 (7) |
C3—C2—C4—Co1 | −59.85 (17) | F3ii—F1—B1—F1ii | 81.8 (4) |
C2i—Co1—C4—C5 | −156.0 (3) | F4ii—F1—B1—F2 | 106.6 (7) |
C2—Co1—C4—C5 | −118.7 (2) | F3ii—F1—B1—F2 | −98.2 (4) |
C3i—Co1—C4—C5 | 168.73 (18) | F4ii—F1—B1—F3ii | −155.2 (9) |
C3—Co1—C4—C5 | −80.83 (19) | F4ii—F1—B1—F3 | −4.0 (8) |
C1i—Co1—C4—C5 | 126.65 (18) | F3ii—F1—B1—F3 | 151.2 (6) |
C1—Co1—C4—C5 | −37.28 (18) | F1ii—F3—B1—F4ii | −140.2 (6) |
C5i—Co1—C4—C5 | 84.3 (2) | F4ii—F3—B1—F4 | 122.2 (9) |
C4i—Co1—C4—C5 | 48.63 (15) | F1ii—F3—B1—F4 | −18.0 (8) |
C2i—Co1—C4—C2 | −37.3 (5) | F4ii—F3—B1—F1 | 3.4 (7) |
C3i—Co1—C4—C2 | −72.6 (2) | F1ii—F3—B1—F1 | −136.8 (8) |
C3—Co1—C4—C2 | 37.89 (18) | F4ii—F3—B1—F1ii | 140.2 (6) |
C1i—Co1—C4—C2 | −114.64 (18) | F4ii—F3—B1—F2 | −112.3 (4) |
C1—Co1—C4—C2 | 81.44 (19) | F1ii—F3—B1—F2 | 107.5 (4) |
C5—Co1—C4—C2 | 118.7 (2) | F4ii—F3—B1—F3ii | 67.7 (4) |
C5i—Co1—C4—C2 | −156.99 (17) | F1ii—F3—B1—F3ii | −72.5 (4) |
C4i—Co1—C4—C2 | 167.35 (16) | F4ii—B1—F4—F1ii | 85.9 (7) |
C2i—Co1—C4—P1 | 80.3 (4) | F1—B1—F4—F1ii | 135.0 (10) |
C2—Co1—C4—P1 | 117.5 (3) | F2—B1—F4—F1ii | −94.1 (7) |
C3i—Co1—C4—P1 | 45.0 (2) | F3ii—B1—F4—F1ii | 175.2 (10) |
C3—Co1—C4—P1 | 155.4 (2) | F3—B1—F4—F1ii | 24.4 (9) |
C1i—Co1—C4—P1 | 2.9 (2) | F4ii—B1—F4—F3ii | −89.4 (5) |
C1—Co1—C4—P1 | −161.0 (2) | F1—B1—F4—F3ii | −40.2 (6) |
C5—Co1—C4—P1 | −123.8 (3) | F1ii—B1—F4—F3ii | −175.2 (10) |
C5i—Co1—C4—P1 | −39.5 (2) | F2—B1—F4—F3ii | 90.6 (5) |
C4i—Co1—C4—P1 | −75.14 (17) | F3—B1—F4—F3ii | −150.9 (6) |
Symmetry codes: (i) −x+2, y, −z+3/2; (ii) −x+1, y, −z+3/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3···F1iii | 0.93 | 2.78 | 3.473 (8) | 132 |
Symmetry code: (iii) −x+3/2, y+1/2, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Co(C17H14P)2]BF4 |
Mr | 644.24 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 297 |
a, b, c (Å) | 10.3357 (11), 13.1659 (14), 22.894 (3) |
β (°) | 102.085 (2) |
V (Å3) | 3046.3 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.72 |
Crystal size (mm) | 0.20 × 0.15 × 0.10 |
Data collection | |
Diffractometer | Bruker SMART CCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2004) |
Tmin, Tmax | 0.870, 0.932 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10252, 2970, 2655 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.125, 1.08 |
No. of reflections | 2970 |
No. of parameters | 205 |
No. of restraints | 21 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.49, −0.36 |
Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2001).
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3···F1i | 0.93 | 2.78 | 3.473 (8) | 132.4 |
Symmetry code: (i) −x+3/2, y+1/2, −z+3/2. |
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The molecular structure of the title complex consists of a [(η5-Ph2PC5H4)2Co]+ cation and a BF4- anion (Fig.1), in which the bond length and angles of the cation are similar to those in the cation of the complex 1,1'-Bis(diphenylphosphino)cobaltocenium nitrate (Brasse et al., 2000). The two Ph2P– substituents are trans to each other with respect to the CoIII metal center, and the two substituted cyclopentadienyl rings are exactly staggered with a dihedral angle of 4.62 (18)° between them. The distance between the atom Co1 and the center of the unique cyclopentadienyl ring is 1.6380 (13) Å. In the crystal structutre, molecules are linked by C—H···F hydrogen bonds, as shown in Fig.2.