1,1′-Bis(diphenyl­phosphino)cobaltocenium tetra­fluoridoborate

Hou, J.-G.; Zhang, P.; Ye, C.; Yu, T.-G.

doi:10.1107/S1600536807048404

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1,1′-Bis(diphenylphosphino)cobaltocenium tetrafluoridoborate

J.-G. Hou, P. Zhang, C. Ye and T.-G. Yu

The title compound, [Co(C₁₇H₁₄P)₂]BF₄, was obtained by the anion exchange of 1,1′-bis(diphenylphosphino)cobaltocenium chloride with sodium tetrafluoroborate. Both the cation and anion lie on crystallographic twofold axes which run through the Co^III ion, and both the B atom and one F atom of the anion, respectively. Three of the F atoms of the BF₄⁻ anion are disordered equally over two sites. The two diphenylphosphine ligands are trans to each other with respect to the Co^III ion. The crystal structure contains weak C—H

F interactions.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807048404/lh2500sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807048404/lh2500Isup2.hkl Contains datablock I

CCDC reference: 667161

checkCIF report

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

Comment top

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 Co^III 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.

Related literature top

The structure of a related compound containing the same cation with a nitrate anion has already been determined (Brasse et al., 2000)

Experimental top

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.

Structure description top

The structure of a related compound containing the same cation with a nitrate anion has already been determined (Brasse et al., 2000)

Computing details top

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).

Figures top

	Fig. 1. The molecular structure with atom labels and 50% probability displacement ellipsoids for non-H atoms. H atoms are represented by circles of arbitrary size [Symmetry codes: (a) -x + 2, y, -z + 3/2; (b) -x + 1, y, -z + 3/2]
	Fig. 2. A partial packing plot showing C—H···F hydrogen bonds as dashed lines.

1,1'-Bis(diphenylphosphino)cobaltocenium tetrafluoridoborate top

Crystal data top

[Co(C₁₇H₁₄P)₂]BF₄	F(000) = 1320
M_r = 644.24	D_x = 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

Data collection top

Bruker SMART CCD diffractometer	2970 independent reflections
Radiation source: fine-focus sealed tube	2655 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.025
φ and ω scans	θ_max = 26.0°, θ_min = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −12→12
T_min = 0.870, T_max = 0.932	k = −14→16
10252 measured reflections	l = −28→28

Refinement top

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(F_o²) + (0.0776P)² + 1.0622P] where P = (F_o² + 2F_c²)/3
2970 reflections	(Δ/σ)_max < 0.001
205 parameters	Δρ_max = 0.49 e Å⁻³
21 restraints	Δρ_min = −0.36 e Å⁻³

Crystal data top

[Co(C₁₇H₁₄P)₂]BF₄	V = 3046.3 (6) Å³
M_r = 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)°

Data collection top

Bruker SMART CCD diffractometer	2970 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	2655 reflections with I > 2σ(I)
T_min = 0.870, T_max = 0.932	R_int = 0.025
10252 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.045	21 restraints
wR(F²) = 0.125	H-atom parameters constrained
S = 1.08	Δρ_max = 0.49 e Å⁻³
2970 reflections	Δρ_min = −0.36 e Å⁻³
205 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.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	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

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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.

Hydrogen-bond geometry (Å, º) top

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
M_r	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)
T_min, T_max	0.870, 0.932
No. of measured, independent and observed [I > 2σ(I)] reflections	10252, 2970, 2655
R_int	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
Δρ_max, Δρ_min (e Å⁻³)	0.49, −0.36

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2001).

Hydrogen-bond geometry (Å, º) top

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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