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Acta Crystallogr Sect E Struct Rep Online. 2010 May 1; 66(Pt 5): m545.
Published online 2010 April 21. doi:  10.1107/S1600536810013747
PMCID: PMC2979230

{1,3-Bis[(diphenyl­phosphanyl-κP)­oxy]prop-2-yl-κC 2}iodido(trimethyl­phosphane)cobalt(II)

Abstract

The title compound, [Co(C27H25O2P2)I(C3H9P)], was synthesized by the addition of 1-iodo­butane to a solution of the parent cobalt complex {1,3-bis­[(diphenyl­phosphan­yl)­oxy]prop-2-yl}bis­(trimethyl­phosphane)cobalt(II). Two five-membered cobaltocycles with considerable ring bending (sum of inter­nal angles = 516.4 and 517.7°) are formed through two P atoms of the PPh2 groups and a metallated Csp 3 atom. The CoII atom is centered in a trigonal-bipyramidal configuration.

Related literature

For general background to transition metal complexes with PCP pincer ligands and their preparation, see: Boom & Milstein (2003 [triangle]); Pandarus et al. (2008 [triangle]); Xu et al. (2009 [triangle]); Zheng et al. (2009 [triangle]). For Co—Csp 3 bond lengths, see: Klein et al. (2003 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m545-scheme1.jpg

Experimental

Crystal data

  • [Co(C27H25O2P2)I(C3H9P)]
  • M r = 705.31
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m545-efi1.jpg
  • a = 15.161 (3) Å
  • b = 18.194 (4) Å
  • c = 21.410 (4) Å
  • V = 5906 (2) Å3
  • Z = 8
  • Mo Kα radiation
  • μ = 1.82 mm−1
  • T = 293 K
  • 0.20 × 0.15 × 0.10 mm

Data collection

  • Bruker SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 2004 [triangle]) T min = 0.713, T max = 0.876
  • 35496 measured reflections
  • 6237 independent reflections
  • 5551 reflections with I > 2σ(I)
  • R int = 0.071

Refinement

  • R[F 2 > 2σ(F 2)] = 0.024
  • wR(F 2) = 0.061
  • S = 1.04
  • 6237 reflections
  • 357 parameters
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.57 e Å−3
  • Δρmin = −0.54 e Å−3

Data collection: SMART (Bruker, 1997 [triangle]); cell refinement: SAINT (Bruker, 1997 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810013747/zq2034sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810013747/zq2034Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We gratefully acknowledge support by NSF China (No. 20872080/20772072).

supplementary crystallographic information

Comment

Transition metal complexes with PCP pincer ligands have attracted a substantial amount of interest (Boom et al. 2003). We previously reported that the central sp3 C—H bond of (Ph2POCH2)2CH2 could be activated by Co(PMe3)4Me to afford metallated PCP pincer compounds at room temperature (Xu et al., 2009) and the subsequent reaction with CH3I gave rise to iodomethylcobalt(III) complex. Here we explored the reaction of Co(C27H25O2P2)(C3H9P)2 with n-C4H9I, which afforded the title compound via one-electron oxidative addition. The rest part of products might be C,C-coupling product (Zheng et al., 2009), despite it has not been isolated.

The molecular structure is shown in Fig. 1. The CoII atom is five coordinated in a trigonal bipyramidal configuration. The Co—C bond distance of 2.068 (18) Å is within the range of Co—C (sp3) bonds (2.03-2.15 Å) (Klein et al., 2003).

Experimental

Standard vacuum techniques were used in manipulations of volatile and air sensitive material. The title compound was synthesized by combining a solution of {1,3-bis[(diphenylphosphanyl)oxy]prop-2-yl}bis(trimethylphosphane)cobalt(II) (733 mg, 1.12 mmol) in 30 ml of diethyl ether with a sample of n-C4H9I (203 mg, 1.12 mmol) in 30 ml of diethyl ether at 273 K. After kept stirring for 16 h at room temperature, the color changed from red to brown. Volatiles were concentrated and filtrated. Red crystals, which were suitable for X-ray diffraction, could be obtained from diethyl ether at 255 K.

Refinement

The H atoms bound to C16-C18 were located in a difference Fourier map and refined isotropically. The remaining H atoms were included in calculated positions, with C—H = 0.93 Å (aromatic) and 0.96 Å (alkyl), and with Uiso(H) = 1.2 (1.5 for alkyl groups) times Ueq(C).

Figures

Fig. 1.
The molecular structure of the title molecule showing the atom-labelling scheme. Thermal ellipsoids are drawn at the 30% probability level. All hydrogen atoms are omitted for clarity.

Crystal data

[Co(C27H25O2P2)I(C3H9P)]F(000) = 2840
Mr = 705.31Dx = 1.587 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 13063 reflections
a = 15.161 (3) Åθ = 2.0–26.9°
b = 18.194 (4) ŵ = 1.82 mm1
c = 21.410 (4) ÅT = 293 K
V = 5906 (2) Å3Block, red
Z = 80.20 × 0.15 × 0.10 mm

Data collection

Bruker SMART CCD area-detector diffractometer6237 independent reflections
Radiation source: fine-focus sealed tube5551 reflections with I > 2σ(I)
graphiteRint = 0.071
phi and ω scansθmax = 26.7°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)h = −19→18
Tmin = 0.713, Tmax = 0.876k = −23→23
35496 measured reflectionsl = −27→20

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.061H atoms treated by a mixture of independent and constrained refinement
S = 1.04w = 1/[σ2(Fo2) + (0.0293P)2 + 1.1856P] where P = (Fo2 + 2Fc2)/3
6237 reflections(Δ/σ)max = 0.004
357 parametersΔρmax = 0.57 e Å3
0 restraintsΔρmin = −0.54 e Å3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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)

xyzUiso*/Ueq
I10.657194 (9)0.086157 (8)0.506996 (6)0.02926 (5)
Co20.644969 (16)0.062554 (12)0.387635 (11)0.01625 (6)
P10.75443 (3)0.14172 (2)0.37052 (2)0.02092 (10)
P20.54174 (3)0.10487 (2)0.32815 (2)0.01924 (10)
P30.70421 (3)−0.03885 (2)0.35418 (2)0.01858 (10)
O10.48603 (9)0.03615 (7)0.30021 (7)0.0249 (3)
O20.65551 (9)−0.10523 (7)0.39172 (7)0.0247 (3)
C10.79921 (15)0.15169 (11)0.29188 (10)0.0300 (4)
H1A0.84270.19000.29160.045*
H1B0.75250.16400.26350.045*
H1C0.82600.10630.27920.045*
C20.85631 (13)0.12727 (12)0.41438 (11)0.0302 (4)
H2A0.88330.08210.40120.045*
H2B0.84310.12470.45820.045*
H2C0.89600.16740.40680.045*
C30.72818 (15)0.23686 (10)0.39039 (10)0.0291 (4)
H3A0.78130.26550.39060.044*
H3B0.70140.23850.43100.044*
H3C0.68800.25650.36000.044*
C40.55196 (12)0.16068 (10)0.25779 (9)0.0235 (4)
C50.56173 (14)0.12717 (12)0.20005 (10)0.0297 (4)
H50.55820.07630.19680.036*
C60.57680 (15)0.16956 (14)0.14697 (11)0.0380 (5)
H60.58250.14690.10830.046*
C70.58336 (16)0.24521 (14)0.15141 (13)0.0437 (6)
H70.59420.27330.11600.052*
C80.57375 (18)0.27844 (13)0.20852 (13)0.0424 (6)
H80.57880.32920.21170.051*
C90.55662 (16)0.23727 (11)0.26161 (11)0.0330 (5)
H90.54820.26060.29980.040*
C100.45903 (13)0.15345 (10)0.37462 (9)0.0240 (4)
C110.48287 (15)0.20811 (11)0.41667 (11)0.0327 (5)
H110.54160.22240.41960.039*
C120.42052 (18)0.24143 (12)0.45408 (12)0.0417 (6)
H120.43720.27860.48150.050*
C130.33319 (18)0.21962 (14)0.45081 (13)0.0458 (7)
H130.29100.24200.47600.055*
C140.30906 (17)0.16476 (15)0.41022 (14)0.0449 (6)
H140.25050.14970.40840.054*
C150.37125 (15)0.13148 (12)0.37182 (11)0.0332 (5)
H150.35420.09460.34430.040*
C160.49139 (13)−0.02708 (10)0.34158 (10)0.0236 (4)
C170.54239 (12)−0.01073 (9)0.40104 (9)0.0207 (4)
C180.57921 (13)−0.08121 (10)0.42799 (10)0.0243 (4)
C190.81877 (13)−0.05789 (9)0.37445 (10)0.0229 (4)
C200.88739 (14)−0.05669 (10)0.33109 (10)0.0261 (4)
H200.8749−0.05010.28890.031*
C210.97401 (14)−0.06518 (12)0.35030 (12)0.0337 (5)
H211.0193−0.06440.32110.040*
C220.99311 (16)−0.07482 (13)0.41270 (13)0.0400 (5)
H221.0513−0.08060.42540.048*
C230.92562 (17)−0.07593 (14)0.45670 (12)0.0428 (6)
H230.9387−0.08200.49880.051*
C240.83859 (15)−0.06791 (12)0.43761 (12)0.0333 (5)
H240.7934−0.06920.46700.040*
C250.69869 (13)−0.07007 (10)0.27348 (9)0.0216 (4)
C260.71675 (14)−0.02226 (10)0.22455 (10)0.0272 (4)
H260.72650.02730.23280.033*
C270.72045 (14)−0.04749 (12)0.16343 (10)0.0313 (4)
H270.7343−0.01530.13120.038*
C280.70351 (14)−0.12086 (12)0.15053 (10)0.0299 (4)
H280.7070−0.13820.10970.036*
C290.68137 (16)−0.16818 (11)0.19879 (11)0.0336 (5)
H290.6677−0.21690.19010.040*
C300.67953 (16)−0.14335 (10)0.25967 (11)0.0302 (4)
H300.6654−0.17570.29180.036*
H180.5970 (16)−0.0751 (11)0.4712 (12)0.021 (5)*
H310.5038 (15)0.0134 (12)0.4328 (11)0.023 (5)*
H160.5197 (16)−0.0676 (12)0.3174 (11)0.025 (6)*
H170.4303 (17)−0.0420 (13)0.3517 (12)0.029 (6)*
H190.5380 (17)−0.1227 (13)0.4249 (12)0.032 (6)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
I10.03046 (8)0.03908 (9)0.01822 (7)−0.00978 (5)0.00190 (5)−0.00184 (5)
Co20.01717 (12)0.01357 (11)0.01801 (12)−0.00099 (8)0.00126 (9)−0.00041 (8)
P10.0226 (2)0.0175 (2)0.0227 (2)−0.00525 (17)0.00225 (19)−0.00124 (17)
P20.0203 (2)0.01627 (19)0.0211 (2)0.00030 (16)−0.00108 (18)−0.00069 (16)
P30.0197 (2)0.01471 (19)0.0214 (2)0.00055 (16)0.00333 (18)0.00018 (16)
O10.0270 (7)0.0225 (6)0.0252 (7)−0.0043 (5)−0.0052 (6)−0.0015 (5)
O20.0255 (7)0.0170 (6)0.0317 (8)0.0013 (5)0.0089 (6)0.0035 (5)
C10.0343 (12)0.0263 (9)0.0293 (11)−0.0095 (8)0.0085 (9)−0.0016 (8)
C20.0243 (10)0.0310 (10)0.0353 (12)−0.0068 (8)0.0002 (9)−0.0028 (9)
C30.0342 (11)0.0187 (8)0.0343 (11)−0.0064 (8)0.0039 (9)−0.0033 (8)
C40.0192 (9)0.0259 (9)0.0254 (10)0.0026 (7)−0.0018 (8)0.0041 (7)
C50.0265 (10)0.0345 (10)0.0281 (11)−0.0025 (8)−0.0002 (8)−0.0009 (8)
C60.0299 (12)0.0571 (14)0.0270 (11)−0.0026 (10)0.0011 (9)0.0020 (10)
C70.0361 (13)0.0555 (14)0.0394 (13)0.0018 (11)0.0003 (10)0.0241 (11)
C80.0496 (15)0.0306 (10)0.0470 (15)0.0057 (10)0.0002 (12)0.0160 (10)
C90.0395 (12)0.0258 (9)0.0336 (12)0.0066 (8)0.0006 (9)0.0047 (8)
C100.0228 (9)0.0240 (8)0.0252 (10)0.0056 (7)0.0012 (8)0.0043 (7)
C110.0331 (12)0.0293 (10)0.0357 (12)0.0050 (8)0.0050 (9)−0.0045 (8)
C120.0542 (16)0.0340 (11)0.0369 (13)0.0121 (10)0.0130 (11)−0.0027 (9)
C130.0475 (15)0.0459 (13)0.0439 (15)0.0244 (11)0.0223 (12)0.0124 (11)
C140.0257 (12)0.0579 (15)0.0512 (16)0.0097 (10)0.0101 (11)0.0150 (13)
C150.0258 (11)0.0377 (11)0.0362 (12)0.0044 (9)0.0003 (9)0.0065 (9)
C160.0218 (9)0.0185 (8)0.0304 (10)−0.0045 (7)0.0002 (8)−0.0020 (7)
C170.0202 (9)0.0171 (7)0.0249 (9)−0.0031 (7)0.0048 (7)−0.0006 (7)
C180.0243 (10)0.0193 (8)0.0293 (11)−0.0020 (7)0.0073 (8)0.0035 (7)
C190.0239 (9)0.0159 (8)0.0290 (10)0.0026 (7)0.0016 (8)0.0015 (7)
C200.0253 (10)0.0263 (9)0.0268 (10)0.0023 (7)0.0020 (8)0.0006 (8)
C210.0251 (11)0.0352 (11)0.0409 (13)0.0045 (8)0.0074 (9)0.0023 (9)
C220.0263 (11)0.0475 (13)0.0462 (15)0.0067 (9)−0.0053 (10)0.0096 (11)
C230.0346 (13)0.0601 (15)0.0339 (13)0.0081 (11)−0.0046 (10)0.0128 (11)
C240.0295 (12)0.0401 (11)0.0302 (11)0.0053 (9)0.0034 (9)0.0080 (9)
C250.0193 (9)0.0213 (8)0.0243 (10)0.0019 (7)0.0022 (7)−0.0034 (7)
C260.0305 (11)0.0245 (9)0.0266 (10)−0.0063 (8)0.0024 (8)−0.0025 (7)
C270.0300 (11)0.0371 (11)0.0268 (11)−0.0089 (9)0.0038 (9)−0.0008 (8)
C280.0270 (10)0.0357 (10)0.0269 (11)0.0002 (8)0.0013 (8)−0.0096 (8)
C290.0428 (13)0.0224 (9)0.0355 (12)0.0005 (8)−0.0020 (10)−0.0074 (8)
C300.0424 (12)0.0182 (9)0.0300 (11)0.0015 (8)0.0000 (9)−0.0002 (8)

Geometric parameters (Å, °)

I1—Co22.5980 (6)C11—C121.379 (3)
Co2—C172.0685 (18)C11—H110.9300
Co2—P22.1597 (6)C12—C131.384 (4)
Co2—P32.1734 (6)C12—H120.9300
Co2—P12.2278 (6)C13—C141.373 (4)
P1—C11.824 (2)C13—H130.9300
P1—C31.8263 (19)C14—C151.390 (3)
P1—C21.827 (2)C14—H140.9300
P2—O11.6231 (13)C15—H150.9300
P2—C41.823 (2)C16—C171.519 (3)
P2—C101.829 (2)C16—H161.00 (2)
P3—O21.6278 (14)C16—H170.99 (2)
P3—C251.821 (2)C17—C181.513 (3)
P3—C191.823 (2)C17—H311.00 (2)
O1—C161.454 (2)C18—H180.97 (3)
O2—C181.460 (2)C18—H190.98 (2)
C1—H1A0.9600C19—C201.394 (3)
C1—H1B0.9600C19—C241.397 (3)
C1—H1C0.9600C20—C211.385 (3)
C2—H2A0.9600C20—H200.9300
C2—H2B0.9600C21—C221.378 (4)
C2—H2C0.9600C21—H210.9300
C3—H3A0.9600C22—C231.391 (4)
C3—H3B0.9600C22—H220.9300
C3—H3C0.9600C23—C241.389 (3)
C4—C51.386 (3)C23—H230.9300
C4—C91.398 (3)C24—H240.9300
C5—C61.392 (3)C25—C261.389 (3)
C5—H50.9300C25—C301.396 (3)
C6—C71.383 (4)C26—C271.388 (3)
C6—H60.9300C26—H260.9300
C7—C81.372 (4)C27—C281.387 (3)
C7—H70.9300C27—H270.9300
C8—C91.386 (3)C28—C291.386 (3)
C8—H80.9300C28—H280.9300
C9—H90.9300C29—C301.380 (3)
C10—C111.389 (3)C29—H290.9300
C10—C151.391 (3)C30—H300.9300
C17—Co2—P276.51 (6)C12—C11—C10120.8 (2)
C17—Co2—P379.01 (5)C12—C11—H11119.6
P2—Co2—P3114.06 (2)C10—C11—H11119.6
C17—Co2—P1178.47 (6)C11—C12—C13120.0 (2)
P2—Co2—P1102.26 (2)C11—C12—H12120.0
P3—Co2—P1100.77 (2)C13—C12—H12120.0
C17—Co2—I191.36 (6)C14—C13—C12119.7 (2)
P2—Co2—I1124.951 (18)C14—C13—H13120.2
P3—Co2—I1115.788 (17)C12—C13—H13120.2
P1—Co2—I190.104 (16)C13—C14—C15120.7 (2)
C1—P1—C3101.64 (10)C13—C14—H14119.7
C1—P1—C2100.03 (11)C15—C14—H14119.7
C3—P1—C2101.59 (10)C14—C15—C10119.9 (2)
C1—P1—Co2119.56 (7)C14—C15—H15120.0
C3—P1—Co2114.34 (7)C10—C15—H15120.0
C2—P1—Co2116.88 (7)O1—C16—C17112.58 (14)
O1—P2—C499.72 (8)O1—C16—H16107.0 (14)
O1—P2—C10102.47 (9)C17—C16—H16111.2 (14)
C4—P2—C10103.81 (9)O1—C16—H17107.3 (14)
O1—P2—Co2108.65 (5)C17—C16—H17110.3 (15)
C4—P2—Co2128.62 (7)H16—C16—H17108.3 (19)
C10—P2—Co2110.39 (7)C18—C17—C16109.96 (15)
O2—P3—C25102.49 (8)C18—C17—Co2108.77 (13)
O2—P3—C1999.99 (8)C16—C17—Co2113.12 (13)
C25—P3—C19102.15 (9)C18—C17—H31109.3 (13)
O2—P3—Co2106.24 (5)C16—C17—H31111.0 (13)
C25—P3—Co2123.96 (6)Co2—C17—H31104.6 (12)
C19—P3—Co2118.45 (6)O2—C18—C17110.07 (15)
C16—O1—P2110.85 (12)O2—C18—H18108.7 (14)
C18—O2—P3113.57 (11)C17—C18—H18111.6 (13)
P1—C1—H1A109.5O2—C18—H19103.7 (15)
P1—C1—H1B109.5C17—C18—H19113.0 (14)
H1A—C1—H1B109.5H18—C18—H19109 (2)
P1—C1—H1C109.5C20—C19—C24119.07 (19)
H1A—C1—H1C109.5C20—C19—P3123.31 (16)
H1B—C1—H1C109.5C24—C19—P3117.39 (16)
P1—C2—H2A109.5C21—C20—C19120.5 (2)
P1—C2—H2B109.5C21—C20—H20119.7
H2A—C2—H2B109.5C19—C20—H20119.7
P1—C2—H2C109.5C22—C21—C20120.1 (2)
H2A—C2—H2C109.5C22—C21—H21120.0
H2B—C2—H2C109.5C20—C21—H21120.0
P1—C3—H3A109.5C21—C22—C23120.2 (2)
P1—C3—H3B109.5C21—C22—H22119.9
H3A—C3—H3B109.5C23—C22—H22119.9
P1—C3—H3C109.5C24—C23—C22119.9 (2)
H3A—C3—H3C109.5C24—C23—H23120.1
H3B—C3—H3C109.5C22—C23—H23120.1
C5—C4—C9119.02 (19)C23—C24—C19120.2 (2)
C5—C4—P2120.07 (15)C23—C24—H24119.9
C9—C4—P2120.74 (17)C19—C24—H24119.9
C4—C5—C6120.1 (2)C26—C25—C30118.65 (19)
C4—C5—H5119.9C26—C25—P3120.75 (14)
C6—C5—H5119.9C30—C25—P3120.55 (16)
C7—C6—C5120.4 (2)C27—C26—C25120.79 (18)
C7—C6—H6119.8C27—C26—H26119.6
C5—C6—H6119.8C25—C26—H26119.6
C8—C7—C6119.5 (2)C28—C27—C26119.9 (2)
C8—C7—H7120.3C28—C27—H27120.1
C6—C7—H7120.3C26—C27—H27120.1
C7—C8—C9120.8 (2)C29—C28—C27119.6 (2)
C7—C8—H8119.6C29—C28—H28120.2
C9—C8—H8119.6C27—C28—H28120.2
C8—C9—C4120.0 (2)C30—C29—C28120.38 (19)
C8—C9—H9120.0C30—C29—H29119.8
C4—C9—H9120.0C28—C29—H29119.8
C11—C10—C15118.9 (2)C29—C30—C25120.6 (2)
C11—C10—P2121.34 (16)C29—C30—H30119.7
C15—C10—P2119.59 (16)C25—C30—H30119.7
P2—Co2—P1—C1−60.80 (9)C4—P2—C10—C11−89.34 (18)
P3—Co2—P1—C156.98 (9)Co2—P2—C10—C1151.66 (18)
I1—Co2—P1—C1173.28 (9)O1—P2—C10—C15−7.46 (18)
P2—Co2—P1—C359.95 (8)C4—P2—C10—C1595.97 (17)
P3—Co2—P1—C3177.72 (8)Co2—P2—C10—C15−123.03 (16)
I1—Co2—P1—C3−65.97 (8)C15—C10—C11—C12−1.5 (3)
P2—Co2—P1—C2178.41 (8)P2—C10—C11—C12−176.23 (18)
P3—Co2—P1—C2−63.81 (9)C10—C11—C12—C131.1 (4)
I1—Co2—P1—C252.49 (8)C11—C12—C13—C140.0 (4)
C17—Co2—P2—O1−34.20 (8)C12—C13—C14—C15−0.8 (4)
P3—Co2—P2—O137.03 (6)C13—C14—C15—C100.4 (4)
P1—Co2—P2—O1144.87 (6)C11—C10—C15—C140.7 (3)
I1—Co2—P2—O1−116.27 (6)P2—C10—C15—C14175.55 (18)
C17—Co2—P2—C4−154.04 (10)P2—O1—C16—C173.5 (2)
P3—Co2—P2—C4−82.82 (9)O1—C16—C17—C18−155.92 (16)
P1—Co2—P2—C425.02 (9)O1—C16—C17—Co2−34.09 (19)
I1—Co2—P2—C4123.89 (8)P2—Co2—C17—C18160.80 (14)
C17—Co2—P2—C1077.43 (9)P3—Co2—C17—C1842.53 (12)
P3—Co2—P2—C10148.66 (7)I1—Co2—C17—C18−73.49 (13)
P1—Co2—P2—C10−103.50 (7)P2—Co2—C17—C1638.31 (12)
I1—Co2—P2—C10−4.64 (7)P3—Co2—C17—C16−79.97 (13)
C17—Co2—P3—O2−27.71 (8)I1—Co2—C17—C16164.01 (12)
P2—Co2—P3—O2−97.41 (6)P3—O2—C18—C1723.9 (2)
P1—Co2—P3—O2153.84 (6)C16—C17—C18—O275.7 (2)
I1—Co2—P3—O258.45 (6)Co2—C17—C18—O2−48.69 (18)
C17—Co2—P3—C2590.18 (10)O2—P3—C19—C20135.14 (16)
P2—Co2—P3—C2520.48 (8)C25—P3—C19—C2029.91 (18)
P1—Co2—P3—C25−88.28 (8)Co2—P3—C19—C20−110.13 (16)
I1—Co2—P3—C25176.33 (7)O2—P3—C19—C24−50.42 (17)
C17—Co2—P3—C19−139.02 (9)C25—P3—C19—C24−155.65 (16)
P2—Co2—P3—C19151.28 (7)Co2—P3—C19—C2464.31 (17)
P1—Co2—P3—C1942.53 (8)C24—C19—C20—C21−0.1 (3)
I1—Co2—P3—C19−52.86 (8)P3—C19—C20—C21174.23 (15)
C4—P2—O1—C16162.61 (13)C19—C20—C21—C22−0.1 (3)
C10—P2—O1—C16−90.78 (14)C20—C21—C22—C23−0.1 (4)
Co2—P2—O1—C1626.04 (13)C21—C22—C23—C240.5 (4)
C25—P3—O2—C18−122.07 (14)C22—C23—C24—C19−0.7 (4)
C19—P3—O2—C18132.99 (14)C20—C19—C24—C230.5 (3)
Co2—P3—O2—C189.27 (15)P3—C19—C24—C23−174.15 (18)
O1—P2—C4—C5−35.28 (18)O2—P3—C25—C26166.52 (16)
C10—P2—C4—C5−140.81 (17)C19—P3—C25—C26−90.21 (17)
Co2—P2—C4—C588.23 (17)Co2—P3—C25—C2646.88 (19)
O1—P2—C4—C9149.46 (17)O2—P3—C25—C30−15.99 (19)
C10—P2—C4—C943.93 (19)C19—P3—C25—C3087.28 (18)
Co2—P2—C4—C9−87.03 (18)Co2—P3—C25—C30−135.62 (15)
C9—C4—C5—C60.6 (3)C30—C25—C26—C27−3.5 (3)
P2—C4—C5—C6−174.71 (17)P3—C25—C26—C27174.08 (17)
C4—C5—C6—C70.9 (3)C25—C26—C27—C281.8 (3)
C5—C6—C7—C8−0.8 (4)C26—C27—C28—C291.2 (3)
C6—C7—C8—C9−0.7 (4)C27—C28—C29—C30−2.6 (3)
C7—C8—C9—C42.2 (4)C28—C29—C30—C250.9 (4)
C5—C4—C9—C8−2.2 (3)C26—C25—C30—C292.1 (3)
P2—C4—C9—C8173.15 (18)P3—C25—C30—C29−175.47 (18)
O1—P2—C10—C11167.23 (17)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: ZQ2034).

References

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