(1η5-Cyclo­penta­dien­yl)(μ-disulfur dinitrido)(triphenyl­phosphino-2κP)cobalt(II)gold(I) perchlorate

Slawin, A.M.Z.; Woollins, J.D.

doi:10.1107/S1600536806024056

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 62| Part 7| July 2006| Pages m1658-m1659

https://doi.org/10.1107/S1600536806024056

(1η⁵-Cyclopentadienyl)(μ-disulfur dinitrido)(triphenylphosphino-2κP)cobalt(II)gold(I) perchlorate

Alexandra M. Z. Slawin ^a and J. Derek Woollins ^a ^*

^aDepartment of Chemistry, University of St Andrews, St Andrews KY16 9ST, Scotland
^*Correspondence e-mail: jdw3@st-and.ac.uk

(Received 22 May 2006; accepted 22 June 2006; online 28 June 2006)

The title compound, [{Au(C₁₈H₁₅P)}Co(C₅H₅)(N₂S₂)]ClO₄, has a planar CoS₂N₂ ring and a close-to-linear N—Au—P angle [176.54 (11)°].

Comment

The disulfur dinitride dianion is not known as a simple species but can be isolated in metal complexes (Kelly & Woollins, 1986 ; Jones et al., 1985a ,b ; Bates et al., 1986 ). These complexes may be protonated at the metal-coordinated N (Jones et al., 1986 ) and we have previously commented on the structural consequences of this protonation (Jones et al., 1987 , 1988 ). Recently, we developed a new route to disulfur dinitrido complexes (Aucott et al., 2002 ) and we examined the metallation of IrS₂N₂ rings using the AuPR₃ cation as a species which is isolobal with a proton (Aucott et al., 2003 ). A comparison of metallacycle bond lengths for [(η⁵-C₅Me₅)Ir(S₂N₂)] and [(C₅Me₅)₂Ir₂(S₂N₂)Cl(PPh₃)][PF₆] indicates that metallation appears to change the IrS₂N₂ bond lengths and angles in a similar fashion to protonation: both enlarge the M—S2, N1—S1 and N2—S2 distances. We have also recently carried out detailed studies of CpCoS₂N₂ (Van Droogenbroeck et al., 2005 ). This led us to synthesize the title compound, (I), in order to allow us to investigate the effects of metallation on the CoS₂N₂ ring.

Compound (I) (Fig. 1) has a planar CoS₂N₂ ring and a close-to-linear N—Au—P angle [176.54 (11) Å]. Compared with the non-metallated parent, CpCoS₂N₂ (Van Droogenbroeck et al., 2005), we note that (I) has statistically invariant Co—N, Co—S and S2—N2 distances, whilst the N1—S1 distance is longer in (I) than in the parent compound [1.599 (4) versus 1.556 (1) Å] and the S1—N2 distance is slightly shorter in (I) than in the parent molecule [1.580 (4) versus 1.597 (2) Å]. Within the CoS₂N₂ ring, it is noticeable that metallation results in an almost perfect trigonal Co—N—S internal angle [120.1 (2)° in (I) versus 118.32 (8)° in the parent compound]. In general, all internal angles in the CoS₂N₂ ring in (I) are closer to the idealized tetrahedral values at S and trigonal values at N compared with the parent molecule. This work illustrates the difficulties in rationalizing bond lengths in S–N compounds and the continuing need for structural work in this area.

Figure 1
The structure and atom-labelling scheme for (I)

, with displacement ellipsoids drawn at the 50% probability level.

Experimental

Triphenylphosphinogold(disulfur dinitrido)(cyclopentadienyl)cobalt(II) perchlorate was prepared as described in the literature (Aucott et al., 2003) and was crystallized by vapour diffusion of diethyl ether into a dichloromethane solution, to give small dark-reddish–violet plates.

Crystal data

[AuCo(C₅H₅)(N₂N₂)(C₁₈H₁₅P)]ClO₄
M_r = 774.85
Monoclinic, P 2₁ /c
a = 14.646 (3) Å
b = 14.186 (3) Å
c = 13.377 (3) Å
β = 111.20 (3)°
V = 2591.2 (11) Å³
Z = 4
D_x = 1.986 Mg m⁻³
Mo Kα radiation
μ = 6.65 mm⁻¹
T = 133 (2) K
Block, red-violet
0.26 × 0.25 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer
ω scans
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.203, T_max = 0.274
15021 measured reflections
4718 independent reflections
3953 reflections with I > 2σ(I)
R_int = 0.048
θ_max = 25.4°

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.030
wR(F²) = 0.054
S = 1.04
4718 reflections
317 parameters
H-atom parameters constrained
w = 1/[σ²(F_o²) + (0.0176P)² + 3.2524P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max = 0.007
Δρ_max = 0.70 e Å⁻³
Δρ_min = −0.77 e Å⁻³

All H atoms were included in calculated positions and refined as riding, with C—H = 0.95 Å and with U_iso(H) = 1.2U_eq(C).

Data collection: SCXmini Benchtop Crystallography System Software (Rigaku, 2006 ); cell refinement: PROCESS-AUTO (Rigaku, 1998 ); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalStructure (Rigaku/MSC, 2004 ); software used to prepare material for publication: CrystalStructure.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536806024056/ez2007sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536806024056/ez2007Isup2.hkl

Computing details top

Data collection: SCXmini Benchtop Crystallography System Software (Rigaku, 2006); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalStructure (Rigaku/MSC, 2004); software used to prepare material for publication: CrystalStructure.

(η⁵-Cyclopentadienyl)(µ-disulfur dinitrido)(triphenylphosphino)cobalt(II)gold(I) perchlorate top

Crystal data top

[AuCo(C₅H₅)(N₂N₂)(C₁₈H₁₅P)]ClO₄	F(000) = 1496
M_r = 774.85	D_x = 1.986 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 15455 reflections
a = 14.646 (3) Å	θ = 3.1–27.5°
b = 14.186 (3) Å	µ = 6.65 mm⁻¹
c = 13.377 (3) Å	T = 133 K
β = 111.20 (3)°	Platelet, red-violet
V = 2591.2 (11) Å³	0.26 × 0.25 × 0.20 mm
Z = 4

Data collection top

Rigaku SCXmini diffractometer	4718 independent reflections
Radiation source: fine-focus sealed tube	3953 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.048
Detector resolution: 0.83 pixels mm^-1	θ_max = 25.4°, θ_min = 3.2°
ω scans	h = −17→17
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −12→17
T_min = 0.203, T_max = 0.274	l = −11→16
15021 measured reflections

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)] = 0.030	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.054	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0176P)² + 3.2524P] where P = (F_o² + 2F_c²)/3
4718 reflections	(Δ/σ)_max = 0.007
317 parameters	Δρ_max = 0.70 e Å⁻³
0 restraints	Δρ_min = −0.77 e Å⁻³

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
Au1	0.660192 (12)	0.597329 (13)	0.673981 (14)	0.01872 (6)
N1	0.5266 (3)	0.6296 (3)	0.5579 (3)	0.0204 (9)
S1	0.43958 (8)	0.57139 (8)	0.57449 (10)	0.0233 (3)
N2	0.3425 (3)	0.5926 (3)	0.4758 (3)	0.0259 (9)
S2	0.35506 (8)	0.66651 (10)	0.38578 (10)	0.0280 (3)
Co1	0.50197 (4)	0.70466 (4)	0.44071 (5)	0.01958 (15)
C1	0.6283 (4)	0.7851 (4)	0.4798 (4)	0.0347 (13)
H1A	0.6779	0.7932	0.5485	0.042*
C2	0.5432 (4)	0.8416 (4)	0.4351 (4)	0.0328 (13)
H2A	0.5249	0.8930	0.4695	0.039*
C3	0.4904 (4)	0.8081 (4)	0.3307 (4)	0.0351 (13)
H3A	0.4313	0.8340	0.2816	0.042*
C4	0.5411 (4)	0.7293 (4)	0.3121 (4)	0.0345 (13)
H4A	0.5216	0.6923	0.2486	0.041*
C5	0.6262 (4)	0.7151 (4)	0.4045 (4)	0.0341 (13)
H5A	0.6735	0.6668	0.4140	0.041*
P1	0.80157 (8)	0.55420 (8)	0.80220 (9)	0.0163 (3)
C6	0.8391 (3)	0.6366 (3)	0.9134 (3)	0.0175 (10)
C7	0.8577 (3)	0.6081 (3)	1.0179 (3)	0.0210 (11)
H7A	0.8507	0.5436	1.0329	0.025*
C8	0.8864 (3)	0.6732 (4)	1.1007 (4)	0.0281 (12)
H8A	0.8986	0.6537	1.1723	0.034*
C9	0.8974 (3)	0.7670 (3)	1.0782 (4)	0.0283 (12)
H9A	0.9192	0.8116	1.1349	0.034*
C10	0.8767 (3)	0.7961 (3)	0.9735 (4)	0.0262 (12)
H10A	0.8828	0.8608	0.9585	0.031*
C11	0.8471 (3)	0.7315 (3)	0.8908 (4)	0.0233 (11)
H11A	0.8322	0.7515	0.8188	0.028*
C12	0.7903 (3)	0.4395 (3)	0.8568 (4)	0.0184 (10)
C13	0.8595 (3)	0.3692 (3)	0.8686 (4)	0.0244 (11)
H13A	0.9159	0.3820	0.8516	0.029*
C14	0.8470 (4)	0.2808 (4)	0.9050 (4)	0.0325 (13)
H14A	0.8938	0.2325	0.9116	0.039*
C15	0.7661 (4)	0.2632 (4)	0.9315 (4)	0.0362 (14)
H15A	0.7579	0.2027	0.9575	0.043*
C16	0.6973 (4)	0.3317 (4)	0.9209 (4)	0.0376 (14)
H16A	0.6417	0.3183	0.9391	0.045*
C17	0.7084 (3)	0.4210 (3)	0.8835 (4)	0.0258 (12)
H17A	0.6608	0.4686	0.8763	0.031*
C18	0.9053 (3)	0.5441 (3)	0.7591 (3)	0.0155 (10)
C19	0.8910 (3)	0.4966 (3)	0.6622 (4)	0.0207 (11)
H19A	0.8281	0.4724	0.6208	0.025*
C20	0.9685 (3)	0.4852 (3)	0.6272 (4)	0.0248 (11)
H20A	0.9590	0.4514	0.5629	0.030*
C21	1.0592 (3)	0.5224 (4)	0.6850 (4)	0.0286 (12)
H21A	1.1117	0.5152	0.6597	0.034*
C22	1.0743 (3)	0.5710 (3)	0.7809 (4)	0.0274 (12)
H22A	1.1366	0.5970	0.8207	0.033*
C23	0.9968 (3)	0.5805 (3)	0.8172 (4)	0.0214 (11)
H23A	1.0069	0.6125	0.8827	0.026*
Cl1	0.66335 (9)	0.97334 (9)	0.70673 (10)	0.0320 (3)
O1	0.7129 (3)	0.8856 (3)	0.7190 (4)	0.0594 (13)
O2	0.5600 (2)	0.9577 (3)	0.6805 (3)	0.0436 (10)
O3	0.6772 (3)	1.0239 (4)	0.6216 (4)	0.0808 (17)
O4	0.7010 (3)	1.0237 (4)	0.8048 (4)	0.0850 (19)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Au1	0.01501 (9)	0.02417 (11)	0.01521 (10)	0.00228 (8)	0.00334 (7)	0.00008 (8)
N1	0.0154 (19)	0.024 (2)	0.020 (2)	0.0025 (16)	0.0044 (17)	−0.0047 (17)
S1	0.0199 (6)	0.0273 (7)	0.0241 (7)	−0.0013 (5)	0.0097 (5)	−0.0025 (5)
N2	0.017 (2)	0.033 (2)	0.027 (2)	−0.0014 (18)	0.0070 (17)	−0.0092 (19)
S2	0.0163 (6)	0.0442 (8)	0.0193 (7)	0.0009 (6)	0.0014 (5)	−0.0038 (6)
Co1	0.0159 (3)	0.0248 (4)	0.0174 (3)	0.0027 (3)	0.0053 (3)	−0.0007 (3)
C1	0.025 (3)	0.037 (3)	0.039 (3)	−0.014 (2)	0.007 (2)	0.006 (3)
C2	0.043 (3)	0.026 (3)	0.036 (3)	−0.004 (2)	0.022 (3)	0.000 (2)
C3	0.041 (3)	0.037 (3)	0.027 (3)	0.008 (3)	0.013 (3)	0.010 (2)
C4	0.045 (3)	0.037 (3)	0.032 (3)	−0.002 (3)	0.026 (3)	0.003 (3)
C5	0.028 (3)	0.035 (3)	0.046 (4)	0.002 (2)	0.021 (3)	0.008 (3)
P1	0.0146 (6)	0.0198 (7)	0.0143 (6)	0.0012 (5)	0.0049 (5)	0.0011 (5)
C6	0.014 (2)	0.025 (3)	0.013 (2)	−0.0006 (19)	0.0033 (19)	−0.0027 (19)
C7	0.017 (2)	0.023 (3)	0.019 (3)	0.004 (2)	0.0017 (19)	−0.001 (2)
C8	0.022 (3)	0.041 (3)	0.018 (3)	0.003 (2)	0.002 (2)	−0.001 (2)
C9	0.025 (3)	0.028 (3)	0.032 (3)	−0.006 (2)	0.011 (2)	−0.015 (2)
C10	0.027 (3)	0.018 (3)	0.035 (3)	−0.006 (2)	0.012 (2)	−0.006 (2)
C11	0.022 (2)	0.023 (3)	0.024 (3)	0.002 (2)	0.008 (2)	0.002 (2)
C12	0.022 (2)	0.019 (2)	0.014 (2)	−0.006 (2)	0.0058 (19)	−0.0009 (18)
C13	0.019 (2)	0.026 (3)	0.029 (3)	−0.005 (2)	0.008 (2)	0.004 (2)
C14	0.031 (3)	0.026 (3)	0.042 (3)	0.004 (2)	0.015 (3)	0.008 (2)
C15	0.039 (3)	0.027 (3)	0.047 (4)	−0.008 (3)	0.020 (3)	0.011 (3)
C16	0.036 (3)	0.045 (4)	0.040 (4)	−0.006 (3)	0.024 (3)	0.009 (3)
C17	0.027 (3)	0.028 (3)	0.028 (3)	0.002 (2)	0.017 (2)	0.001 (2)
C18	0.018 (2)	0.013 (2)	0.016 (2)	0.0004 (18)	0.0058 (19)	0.0067 (18)
C19	0.022 (2)	0.022 (3)	0.020 (3)	−0.004 (2)	0.009 (2)	−0.001 (2)
C20	0.030 (3)	0.027 (3)	0.020 (3)	0.000 (2)	0.011 (2)	−0.001 (2)
C21	0.027 (3)	0.034 (3)	0.031 (3)	0.006 (2)	0.017 (2)	0.011 (2)
C22	0.018 (2)	0.035 (3)	0.027 (3)	0.002 (2)	0.005 (2)	0.006 (2)
C23	0.023 (2)	0.026 (3)	0.013 (2)	−0.002 (2)	0.004 (2)	0.0029 (19)
Cl1	0.0258 (6)	0.0343 (8)	0.0390 (8)	0.0052 (6)	0.0155 (6)	0.0033 (6)
O1	0.053 (3)	0.050 (3)	0.070 (3)	0.030 (2)	0.015 (2)	0.003 (2)
O2	0.027 (2)	0.042 (2)	0.060 (3)	−0.0032 (18)	0.0146 (19)	0.008 (2)
O3	0.054 (3)	0.097 (4)	0.099 (4)	0.012 (3)	0.036 (3)	0.062 (3)
O4	0.038 (3)	0.134 (5)	0.085 (4)	−0.011 (3)	0.026 (3)	−0.077 (4)

Geometric parameters (Å, º) top

Au1—N1	2.062 (4)	C9—C10	1.385 (7)
Au1—P1	2.2439 (14)	C9—H9A	0.9500
N1—S1	1.599 (4)	C10—C11	1.381 (6)
N1—Co1	1.821 (4)	C10—H10A	0.9500
S1—N2	1.580 (4)	C11—H11A	0.9500
N2—S2	1.657 (4)	C12—C13	1.390 (6)
S2—Co1	2.0782 (14)	C12—C17	1.395 (6)
Co1—C4	2.031 (5)	C13—C14	1.381 (7)
Co1—C2	2.044 (5)	C13—H13A	0.9500
Co1—C3	2.042 (5)	C14—C15	1.376 (7)
Co1—C5	2.050 (5)	C14—H14A	0.9500
Co1—C1	2.073 (5)	C15—C16	1.371 (7)
C1—C5	1.408 (7)	C15—H15A	0.9500
C1—C2	1.419 (7)	C16—C17	1.393 (7)
C1—H1A	0.9500	C16—H16A	0.9500
C2—C3	1.412 (7)	C17—H17A	0.9500
C2—H2A	0.9500	C18—C23	1.383 (6)
C3—C4	1.413 (7)	C18—C19	1.408 (6)
C3—H3A	0.9500	C19—C20	1.385 (6)
C4—C5	1.416 (7)	C19—H19A	0.9500
C4—H4A	0.9500	C20—C21	1.378 (6)
C5—H5A	0.9500	C20—H20A	0.9500
P1—C18	1.814 (4)	C21—C22	1.401 (7)
P1—C6	1.814 (4)	C21—H21A	0.9500
P1—C12	1.816 (5)	C22—C23	1.394 (7)
C6—C7	1.384 (6)	C22—H22A	0.9500
C6—C11	1.394 (6)	C23—H23A	0.9500
C7—C8	1.386 (6)	Cl1—O4	1.419 (4)
C7—H7A	0.9500	Cl1—O1	1.420 (4)
C8—C9	1.386 (7)	Cl1—O3	1.422 (4)
C8—H8A	0.9500	Cl1—O2	1.442 (4)

N1—Au1—P1	176.54 (11)	C6—P1—Au1	111.93 (15)
S1—N1—Co1	120.1 (2)	C12—P1—Au1	111.02 (15)
S1—N1—Au1	111.6 (2)	C7—C6—C11	120.0 (4)
Co1—N1—Au1	128.1 (2)	C7—C6—P1	122.0 (4)
N2—S1—N1	107.9 (2)	C11—C6—P1	117.9 (3)
S1—N2—S2	115.1 (2)	C6—C7—C8	120.2 (5)
N2—S2—Co1	106.31 (14)	C6—C7—H7A	119.9
N1—Co1—C4	143.30 (19)	C8—C7—H7A	119.9
N1—Co1—C2	128.21 (19)	C7—C8—C9	119.5 (5)
C4—Co1—C2	68.1 (2)	C7—C8—H8A	120.2
N1—Co1—C3	168.65 (19)	C9—C8—H8A	120.2
C4—Co1—C3	40.6 (2)	C10—C9—C8	120.4 (4)
C2—Co1—C3	40.4 (2)	C10—C9—H9A	119.8
N1—Co1—C5	109.25 (19)	C8—C9—H9A	119.8
C4—Co1—C5	40.6 (2)	C11—C10—C9	120.2 (5)
C2—Co1—C5	67.9 (2)	C11—C10—H10A	119.9
C3—Co1—C5	68.1 (2)	C9—C10—H10A	119.9
N1—Co1—C1	102.95 (19)	C10—C11—C6	119.6 (5)
C4—Co1—C1	67.6 (2)	C10—C11—H11A	120.2
C2—Co1—C1	40.3 (2)	C6—C11—H11A	120.2
C3—Co1—C1	67.7 (2)	C13—C12—C17	119.7 (4)
C5—Co1—C1	39.9 (2)	C13—C12—P1	121.4 (4)
N1—Co1—S2	90.54 (12)	C17—C12—P1	118.9 (4)
C4—Co1—S2	108.58 (16)	C14—C13—C12	120.5 (4)
C2—Co1—S2	121.08 (16)	C14—C13—H13A	119.8
C3—Co1—S2	97.29 (16)	C12—C13—H13A	119.8
C5—Co1—S2	145.98 (16)	C15—C14—C13	119.4 (5)
C1—Co1—S2	161.40 (15)	C15—C14—H14A	120.3
C5—C1—C2	108.0 (5)	C13—C14—H14A	120.3
C5—C1—Co1	69.2 (3)	C16—C15—C14	120.9 (5)
C2—C1—Co1	68.7 (3)	C16—C15—H15A	119.5
C5—C1—H1A	126.0	C14—C15—H15A	119.5
C2—C1—H1A	126.0	C15—C16—C17	120.3 (5)
Co1—C1—H1A	127.7	C15—C16—H16A	119.8
C3—C2—C1	108.0 (5)	C17—C16—H16A	119.8
C3—C2—Co1	69.7 (3)	C12—C17—C16	119.1 (5)
C1—C2—Co1	71.0 (3)	C12—C17—H17A	120.5
C3—C2—H2A	126.0	C16—C17—H17A	120.5
C1—C2—H2A	126.0	C23—C18—C19	119.1 (4)
Co1—C2—H2A	124.9	C23—C18—P1	123.0 (4)
C2—C3—C4	107.8 (5)	C19—C18—P1	117.9 (3)
C2—C3—Co1	69.8 (3)	C20—C19—C18	120.0 (4)
C4—C3—Co1	69.3 (3)	C20—C19—H19A	120.0
C2—C3—H3A	126.1	C18—C19—H19A	120.0
C4—C3—H3A	126.1	C21—C20—C19	120.5 (4)
Co1—C3—H3A	126.3	C21—C20—H20A	119.7
C3—C4—C5	108.1 (5)	C19—C20—H20A	119.7
C3—C4—Co1	70.1 (3)	C20—C21—C22	120.1 (4)
C5—C4—Co1	70.4 (3)	C20—C21—H21A	119.9
C3—C4—H4A	125.9	C22—C21—H21A	119.9
C5—C4—H4A	125.9	C23—C22—C21	119.2 (4)
Co1—C4—H4A	125.2	C23—C22—H22A	120.4
C1—C5—C4	108.0 (5)	C21—C22—H22A	120.4
C1—C5—Co1	70.9 (3)	C18—C23—C22	121.0 (4)
C4—C5—Co1	69.0 (3)	C18—C23—H23A	119.5
C1—C5—H5A	126.0	C22—C23—H23A	119.5
C4—C5—H5A	126.0	O4—Cl1—O1	108.8 (3)
Co1—C5—H5A	125.7	O4—Cl1—O3	111.4 (4)
C18—P1—C6	105.7 (2)	O1—Cl1—O3	108.7 (3)
C18—P1—C12	105.4 (2)	O4—Cl1—O2	109.0 (3)
C6—P1—C12	107.0 (2)	O1—Cl1—O2	110.0 (2)
C18—P1—Au1	115.20 (14)	O3—Cl1—O2	108.9 (3)

Co1—N1—S1—N2	0.8 (3)	S2—Co1—C4—C3	79.2 (3)
Au1—N1—S1—N2	−174.22 (19)	N1—Co1—C4—C5	−44.2 (5)
N1—S1—N2—S2	−0.5 (3)	C2—Co1—C4—C5	81.1 (3)
S1—N2—S2—Co1	0.0 (3)	C3—Co1—C4—C5	118.7 (5)
S1—N1—Co1—C4	−123.7 (3)	C1—Co1—C4—C5	37.4 (3)
Au1—N1—Co1—C4	50.4 (4)	S2—Co1—C4—C5	−162.0 (3)
S1—N1—Co1—C2	131.0 (3)	C2—C1—C5—C4	1.4 (6)
Au1—N1—Co1—C2	−54.9 (3)	Co1—C1—C5—C4	59.3 (3)
S1—N1—Co1—C3	133.1 (9)	C2—C1—C5—Co1	−57.9 (3)
Au1—N1—Co1—C3	−52.8 (11)	C3—C4—C5—C1	−0.3 (6)
S1—N1—Co1—C5	−152.4 (3)	Co1—C4—C5—C1	−60.5 (3)
Au1—N1—Co1—C5	21.6 (3)	C3—C4—C5—Co1	60.2 (4)
S1—N1—Co1—C1	166.4 (3)	N1—Co1—C5—C1	−87.3 (3)
Au1—N1—Co1—C1	−19.5 (3)	C4—Co1—C5—C1	118.9 (4)
S1—N1—Co1—S2	−0.7 (2)	C2—Co1—C5—C1	37.1 (3)
Au1—N1—Co1—S2	173.4 (2)	C3—Co1—C5—C1	80.9 (3)
N2—S2—Co1—N1	0.32 (19)	S2—Co1—C5—C1	150.4 (3)
N2—S2—Co1—C4	148.4 (2)	N1—Co1—C5—C4	153.8 (3)
N2—S2—Co1—C2	−136.4 (2)	C2—Co1—C5—C4	−81.7 (3)
N2—S2—Co1—C3	−171.4 (2)	C3—Co1—C5—C4	−38.0 (3)
N2—S2—Co1—C5	127.4 (3)	C1—Co1—C5—C4	−118.9 (4)
N2—S2—Co1—C1	−136.6 (5)	S2—Co1—C5—C4	31.5 (5)
N1—Co1—C1—C5	104.6 (3)	C18—P1—C6—C7	−109.5 (4)
C4—Co1—C1—C5	−38.0 (3)	C12—P1—C6—C7	2.5 (4)
C2—Co1—C1—C5	−120.2 (4)	Au1—P1—C6—C7	124.3 (3)
C3—Co1—C1—C5	−82.1 (3)	C18—P1—C6—C11	71.8 (4)
S2—Co1—C1—C5	−119.9 (5)	C12—P1—C6—C11	−176.2 (3)
N1—Co1—C1—C2	−135.2 (3)	Au1—P1—C6—C11	−54.4 (4)
C4—Co1—C1—C2	82.1 (3)	C11—C6—C7—C8	−1.5 (6)
C3—Co1—C1—C2	38.1 (3)	P1—C6—C7—C8	179.8 (3)
C5—Co1—C1—C2	120.2 (4)	C6—C7—C8—C9	−0.6 (7)
S2—Co1—C1—C2	0.3 (7)	C7—C8—C9—C10	2.1 (7)
C5—C1—C2—C3	−2.0 (6)	C8—C9—C10—C11	−1.5 (7)
Co1—C1—C2—C3	−60.1 (4)	C9—C10—C11—C6	−0.6 (7)
C5—C1—C2—Co1	58.1 (3)	C7—C6—C11—C10	2.1 (7)
N1—Co1—C2—C3	179.4 (3)	P1—C6—C11—C10	−179.2 (3)
C4—Co1—C2—C3	37.8 (3)	C18—P1—C12—C13	6.3 (4)
C5—Co1—C2—C3	81.7 (3)	C6—P1—C12—C13	−106.0 (4)
C1—Co1—C2—C3	118.5 (5)	Au1—P1—C12—C13	131.6 (3)
S2—Co1—C2—C3	−61.4 (3)	C18—P1—C12—C17	−171.4 (4)
N1—Co1—C2—C1	60.9 (4)	C6—P1—C12—C17	76.4 (4)
C4—Co1—C2—C1	−80.7 (3)	Au1—P1—C12—C17	−46.0 (4)
C3—Co1—C2—C1	−118.5 (5)	C17—C12—C13—C14	1.1 (7)
C5—Co1—C2—C1	−36.8 (3)	P1—C12—C13—C14	−176.6 (4)
S2—Co1—C2—C1	−179.9 (3)	C12—C13—C14—C15	−1.3 (8)
C1—C2—C3—C4	1.8 (6)	C13—C14—C15—C16	0.9 (8)
Co1—C2—C3—C4	−59.1 (4)	C14—C15—C16—C17	−0.4 (9)
C1—C2—C3—Co1	60.9 (3)	C13—C12—C17—C16	−0.5 (7)
N1—Co1—C3—C2	−2.6 (11)	P1—C12—C17—C16	177.2 (4)
C4—Co1—C3—C2	−119.1 (5)	C15—C16—C17—C12	0.2 (8)
C5—Co1—C3—C2	−81.2 (3)	C6—P1—C18—C23	10.6 (4)
C1—Co1—C3—C2	−37.9 (3)	C12—P1—C18—C23	−102.5 (4)
S2—Co1—C3—C2	130.7 (3)	Au1—P1—C18—C23	134.7 (3)
N1—Co1—C3—C4	116.6 (9)	C6—P1—C18—C19	−169.6 (3)
C2—Co1—C3—C4	119.1 (5)	C12—P1—C18—C19	77.3 (4)
C5—Co1—C3—C4	38.0 (3)	Au1—P1—C18—C19	−45.4 (4)
C1—Co1—C3—C4	81.2 (4)	C23—C18—C19—C20	1.3 (7)
S2—Co1—C3—C4	−110.2 (3)	P1—C18—C19—C20	−178.5 (3)
C2—C3—C4—C5	−1.0 (6)	C18—C19—C20—C21	−1.9 (7)
Co1—C3—C4—C5	−60.4 (4)	C19—C20—C21—C22	1.1 (7)
C2—C3—C4—Co1	59.4 (4)	C20—C21—C22—C23	0.3 (7)
N1—Co1—C4—C3	−162.9 (3)	C19—C18—C23—C22	0.1 (7)
C2—Co1—C4—C3	−37.6 (3)	P1—C18—C23—C22	179.9 (4)
C5—Co1—C4—C3	−118.7 (5)	C21—C22—C23—C18	−1.0 (7)
C1—Co1—C4—C3	−81.3 (3)

References

Aucott, S. M., Bhattacharyya, P., Milton, H. L., Slawin, A. M. Z. & Woollins, J. D. (2003). New J. Chem. 27, 1466–1469. CSD CrossRef CAS Google Scholar
Aucott, S. M., Slawin, A. M. Z. & Woollins, J. D. (2002). Can. J. Chem. 80, 1481–1487. CSD CrossRef CAS Google Scholar
Bates, P. A., Hursthouse, M. B., Kelly, P. F. & Woollins, J. D. (1986). J. Chem. Soc. Dalton Trans. pp. 2367–2370. CSD CrossRef Google Scholar
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Google Scholar
Jones, R., Kelly, P. F., Warrens, C. P., Williams, D. J. & Woollins, J. D. (1986). J. Chem. Soc. Chem. Commun. pp. 711–713. CrossRef Google Scholar
Jones, R., Kelly, P. F., Williams, D. J. & Woollins, J. D. (1985a). J. Chem. Soc. Chem. Commun. pp. 1325–1326. CrossRef Google Scholar
Jones, R., Kelly, P. F., Williams, D. J. & Woollins, J. D. (1985b). Polyhedron, 4, 1947–1950. CSD CrossRef CAS Google Scholar
Jones, R., Kelly, P. F., Williams, D. J. & Woollins, J. D. (1988). J. Chem. Soc. Dalton Trans. pp. 803–807. CSD CrossRef Google Scholar
Jones, R., Warrens, C. P., Williams, D. J. & Woollins, J. D. (1987). J. Chem. Soc. Dalton Trans. pp. 907–914. CSD CrossRef Google Scholar
Kelly, P. F. & Woollins, J. D. (1986). Polyhedron, 5, 607–632. CrossRef CAS Google Scholar
Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, 3-9-12 Matsubara, Akishima, Tokyo 196-8666, Japan. Google Scholar
Rigaku (2006). SCXmini Benchtop Crystallography System Software. Version 1.0. Rigaku Americas Corporation, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Google Scholar
Rigaku/MSC (2004). CrystalStructure. Version 3.6.0. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Google Scholar
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany. Google Scholar
Van Droogenbroeck, J., Van Alsenoy, C., Aucott, S. M., Woollins, J. D., Hunter, A. D. & Blockhuys, F. (2005). Organometallics, 24, 1004–1011. CSD CrossRef CAS Google Scholar

© International Union of Crystallography. Prior permission is not required to reproduce short quotations, tables and figures from this article, provided the original authors and source are cited. For more information, click here.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 62| Part 7| July 2006| Pages m1658-m1659

https://doi.org/10.1107/S1600536806024056

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)